####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ampt16dyx
_audit_block_doi                 10.5517/ccy2d7m
_database_code_depnum_ccdc_archive 'CCDC 866240'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C3CC45695A 2013
2 10.1021/ja206941e 2011
_audit_update_record             
;
2012-02-09 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C60 H70 Dy2 Fe2 N2 O20, 2(C8 H8 O2), 2(C2 H3 N)'
_chemical_formula_sum            'C80 H92 Dy2 Fe2 N4 O24'
_chemical_formula_weight         1930.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5412(10)
_cell_length_b                   14.2757(13)
_cell_length_c                   14.4870(12)
_cell_angle_alpha                61.979(6)
_cell_angle_beta                 87.646(7)
_cell_angle_gamma                80.384(7)
_cell_volume                     2075.5(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    19893
_cell_measurement_theta_min      1.59
_cell_measurement_theta_max      28.41

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.516
_exptl_absorpt_correction_T_max  0.654
_exptl_absorpt_process_details   
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean 6.667
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24227
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         26.37
_reflns_number_total             8476
_reflns_number_gt                7303
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0708P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8476
_refine_ls_number_parameters     517
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0972
_refine_ls_wR_factor_gt          0.0956
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.565146(15) 0.479869(14) 0.708675(14) 0.02411(7) Uani 1 1 d . . .
Fe1 Fe 0.43405(4) 0.62281(4) 0.46244(4) 0.02479(12) Uani 1 1 d . . .
O1 O 0.5896(2) 0.5198(2) 0.5305(2) 0.0238(5) Uani 1 1 d D . .
H1 H 0.649(3) 0.550(4) 0.500(3) 0.029 Uiso 1 1 d D . .
N1 N 0.3780(3) 0.4060(3) 0.8052(3) 0.0302(7) Uani 1 1 d . . .
C1 C 0.2703(4) 0.4649(3) 0.7362(3) 0.0334(9) Uani 1 1 d . . .
H1A H 0.2032 0.4692 0.7796 0.040 Uiso 1 1 calc R . .
H1B H 0.2522 0.4243 0.7004 0.040 Uiso 1 1 calc R . .
C2 C 0.2845(3) 0.5784(3) 0.6543(3) 0.0295(8) Uani 1 1 d . . .
H2A H 0.2201 0.6085 0.6000 0.035 Uiso 1 1 calc R . .
H2B H 0.2802 0.6255 0.6877 0.035 Uiso 1 1 calc R . .
O2 O 0.3935(2) 0.5756(2) 0.6079(2) 0.0273(6) Uani 1 1 d . . .
C3 C 0.3995(4) 0.2907(3) 0.8300(3) 0.0335(9) Uani 1 1 d . . .
H3A H 0.3277 0.2591 0.8579 0.040 Uiso 1 1 calc R . .
H3B H 0.4638 0.2506 0.8843 0.040 Uiso 1 1 calc R . .
C4 C 0.4327(4) 0.2803(3) 0.7323(3) 0.0319(8) Uani 1 1 d . . .
H4A H 0.4614 0.2038 0.7517 0.038 Uiso 1 1 calc R . .
H4B H 0.3625 0.3057 0.6844 0.038 Uiso 1 1 calc R . .
O3 O 0.5208(2) 0.3416(2) 0.6816(2) 0.0273(5) Uani 1 1 d . . .
C5 C 0.3721(4) 0.4139(4) 0.9031(3) 0.0347(9) Uani 1 1 d . . .
H5A H 0.4381 0.3631 0.9516 0.042 Uiso 1 1 calc R . .
H5B H 0.2976 0.3932 0.9369 0.042 Uiso 1 1 calc R . .
C6 C 0.3787(4) 0.5271(4) 0.8822(4) 0.0353(9) Uani 1 1 d . . .
H6A H 0.3028 0.5751 0.8512 0.042 Uiso 1 1 calc R . .
H6B H 0.3963 0.5277 0.9482 0.042 Uiso 1 1 calc R . .
O4 O 0.4715(3) 0.5629(3) 0.8103(2) 0.0349(6) Uani 1 1 d D . .
H4 H 0.507(4) 0.607(4) 0.829(4) 0.042 Uiso 1 1 d D . .
O5 O 0.5074(2) 0.7420(2) 0.4588(2) 0.0303(6) Uani 1 1 d . . .
O6 O 0.6084(2) 0.6577(2) 0.6147(2) 0.0307(6) Uani 1 1 d . . .
C7 C 0.5749(3) 0.7391(3) 0.5287(3) 0.0302(8) Uani 1 1 d . . .
C8 C 0.6154(3) 0.8424(3) 0.5030(3) 0.0284(8) Uani 1 1 d . . .
C9 C 0.6966(4) 0.8450(4) 0.5704(4) 0.0373(9) Uani 1 1 d . . .
H9A H 0.7293 0.7804 0.6302 0.045 Uiso 1 1 calc R . .
C10 C 0.7294(4) 0.9409(4) 0.5502(4) 0.0421(10) Uani 1 1 d . . .
H10A H 0.7841 0.9418 0.5969 0.051 Uiso 1 1 calc R . .
C11 C 0.6838(4) 1.0367(4) 0.4628(4) 0.0387(10) Uani 1 1 d . . .
C12 C 0.6043(4) 1.0338(3) 0.3951(4) 0.0386(10) Uani 1 1 d . . .
H12A H 0.5727 1.0983 0.3348 0.046 Uiso 1 1 calc R . .
C13 C 0.5710(4) 0.9377(4) 0.4148(4) 0.0348(9) Uani 1 1 d . . .
H13A H 0.5170 0.9368 0.3676 0.042 Uiso 1 1 calc R . .
C14 C 0.7168(5) 1.1424(4) 0.4440(5) 0.0558(14) Uani 1 1 d . . .
H14A H 0.6822 1.1999 0.3763 0.084 Uiso 1 1 calc R . .
H14B H 0.8026 1.1367 0.4436 0.084 Uiso 1 1 calc R . .
H14C H 0.6869 1.1591 0.4998 0.084 Uiso 1 1 calc R . .
O7 O 0.2669(2) 0.6898(2) 0.4109(2) 0.0314(6) Uani 1 1 d . . .
O8 O 0.2478(2) 0.6154(2) 0.3065(2) 0.0315(6) Uani 1 1 d . . .
C15 C 0.2108(3) 0.6775(3) 0.3436(3) 0.0300(8) Uani 1 1 d . . .
C16 C 0.0904(3) 0.7435(3) 0.3087(3) 0.0321(8) Uani 1 1 d . . .
C17 C 0.0373(4) 0.8038(4) 0.3556(4) 0.0418(10) Uani 1 1 d . . .
H17A H 0.0772 0.8032 0.4120 0.050 Uiso 1 1 calc R . .
C18 C -0.0741(4) 0.8652(4) 0.3209(4) 0.0474(12) Uani 1 1 d . . .
H18A H -0.1099 0.9051 0.3546 0.057 Uiso 1 1 calc R . .
C19 C -0.1332(4) 0.8689(4) 0.2381(4) 0.0418(10) Uani 1 1 d . . .
C20 C -0.0788(4) 0.8099(4) 0.1901(4) 0.0461(11) Uani 1 1 d . . .
H20A H -0.1174 0.8128 0.1319 0.055 Uiso 1 1 calc R . .
C21 C 0.0312(4) 0.7467(4) 0.2256(4) 0.0435(11) Uani 1 1 d . . .
H21A H 0.0661 0.7054 0.1929 0.052 Uiso 1 1 calc R . .
C22 C -0.2534(4) 0.9370(5) 0.1991(5) 0.0574(14) Uani 1 1 d . . .
H22A H -0.3078 0.9145 0.2564 0.086 Uiso 1 1 calc R . .
H22B H -0.2825 0.9278 0.1418 0.086 Uiso 1 1 calc R . .
H22C H -0.2478 1.0129 0.1739 0.086 Uiso 1 1 calc R . .
O9 O 0.6402(2) 0.3482(2) 0.8843(2) 0.0320(6) Uani 1 1 d . . .
O10 O 0.7198(2) 0.4949(2) 0.8205(2) 0.0321(6) Uani 1 1 d . . .
C23 C 0.7120(3) 0.3995(3) 0.8938(3) 0.0289(8) Uani 1 1 d . . .
C24 C 0.7876(3) 0.3505(3) 0.9912(3) 0.0322(8) Uani 1 1 d . . .
C25 C 0.7685(4) 0.2552(4) 1.0752(4) 0.0423(10) Uani 1 1 d . . .
H25A H 0.7101 0.2187 1.0688 0.051 Uiso 1 1 calc R . .
C26 C 0.8334(5) 0.2118(4) 1.1692(4) 0.0487(12) Uani 1 1 d . . .
H26A H 0.8193 0.1459 1.2260 0.058 Uiso 1 1 calc R . .
C27 C 0.9190(4) 0.2642(4) 1.1807(4) 0.0418(10) Uani 1 1 d . . .
C28 C 0.9381(4) 0.3583(5) 1.0961(4) 0.0488(12) Uani 1 1 d . . .
H28A H 0.9971 0.3945 1.1022 0.059 Uiso 1 1 calc R . .
C29 C 0.8742(4) 0.4021(4) 1.0023(4) 0.0422(10) Uani 1 1 d . . .
H29A H 0.8895 0.4674 0.9453 0.051 Uiso 1 1 calc R . .
C30 C 0.9853(5) 0.2200(5) 1.2847(4) 0.0567(14) Uani 1 1 d . . .
H30A H 1.0625 0.2427 1.2727 0.085 Uiso 1 1 calc R . .
H30B H 0.9957 0.1412 1.3202 0.085 Uiso 1 1 calc R . .
H30C H 0.9406 0.2475 1.3284 0.085 Uiso 1 1 calc R . .
O11 O 0.7423(3) 0.6663(3) 0.8407(3) 0.0411(7) Uani 1 1 d . . .
H11 H 0.7248 0.6230 0.8218 0.062 Uiso 1 1 calc R . .
O12 O 0.5463(3) 0.7158(3) 0.8332(3) 0.0452(8) Uani 1 1 d . . .
C31 C 0.6450(4) 0.7304(4) 0.8423(3) 0.0356(9) Uani 1 1 d . . .
C32 C 0.6665(4) 0.8214(4) 0.8587(3) 0.0342(9) Uani 1 1 d . . .
C33 C 0.5696(4) 0.8891(4) 0.8675(4) 0.0390(10) Uani 1 1 d . . .
H33A H 0.4924 0.8762 0.8629 0.047 Uiso 1 1 calc R . .
C34 C 0.5850(4) 0.9746(4) 0.8828(4) 0.0440(11) Uani 1 1 d . . .
H34A H 0.5182 1.0189 0.8904 0.053 Uiso 1 1 calc R . .
C35 C 0.6968(5) 0.9969(4) 0.8875(4) 0.0459(11) Uani 1 1 d . . .
C36 C 0.7924(5) 0.9286(5) 0.8807(5) 0.0572(14) Uani 1 1 d . . .
H36A H 0.8694 0.9418 0.8851 0.069 Uiso 1 1 calc R . .
C37 C 0.7782(4) 0.8406(4) 0.8676(5) 0.0480(12) Uani 1 1 d . . .
H37A H 0.8454 0.7936 0.8647 0.058 Uiso 1 1 calc R . .
C38 C 0.7117(6) 1.0948(5) 0.8980(5) 0.0592(14) Uani 1 1 d . . .
H38A H 0.7927 1.0867 0.9218 0.089 Uiso 1 1 calc R . .
H38B H 0.6573 1.1018 0.9489 0.089 Uiso 1 1 calc R . .
H38C H 0.6947 1.1593 0.8299 0.089 Uiso 1 1 calc R . .
N41 N 0.8317(4) 0.5780(5) 0.4612(4) 0.0672(14) Uani 1 1 d . . .
C41 C 0.8760(4) 0.5764(5) 0.5294(5) 0.0520(13) Uani 1 1 d . . .
C42 C 0.9313(6) 0.5718(7) 0.6201(6) 0.0726(19) Uani 1 1 d . . .
H42A H 0.8784 0.5485 0.6786 0.109 Uiso 1 1 calc R . .
H42B H 0.9475 0.6433 0.6030 0.109 Uiso 1 1 calc R . .
H42C H 1.0052 0.5205 0.6399 0.109 Uiso 1 1 calc R . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.320(3) . ?
Dy1 O3 2.322(3) . ?
Dy1 O6 2.381(3) . ?
Dy1 O1 2.384(3) . ?
Dy1 O8 2.413(3) 2_666 ?
Dy1 O4 2.413(3) . ?
Dy1 O9 2.429(3) . ?
Dy1 O10 2.559(3) . ?
Dy1 N1 2.619(3) . ?
Dy1 Fe1 3.4208(6) 2_666 ?
Dy1 Fe1 3.4279(7) . ?
Fe1 O2 1.950(3) . ?
Fe1 O3 1.971(3) 2_666 ?
Fe1 O5 2.002(3) . ?
Fe1 O7 2.006(3) . ?
Fe1 O1 2.054(3) 2_666 ?
Fe1 O1 2.064(3) . ?
Fe1 Dy1 3.4208(6) 2_666 ?
O1 Fe1 2.054(3) 2_666 ?
O1 H1 0.87(3) . ?
N1 C5 1.471(5) . ?
N1 C1 1.488(5) . ?
N1 C3 1.489(5) . ?
C1 C2 1.525(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O2 1.405(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.518(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.405(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O3 Fe1 1.971(3) 2_666 ?
C5 C6 1.514(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O4 1.444(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O4 H4 0.95(3) . ?
O5 C7 1.284(5) . ?
O6 C7 1.257(5) . ?
C7 C8 1.494(5) . ?
C8 C13 1.391(6) . ?
C8 C9 1.398(6) . ?
C9 C10 1.375(6) . ?
C9 H9A 0.9500 . ?
C10 C11 1.393(7) . ?
C10 H10A 0.9500 . ?
C11 C12 1.389(7) . ?
C11 C14 1.514(6) . ?
C12 C13 1.382(6) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O7 C15 1.284(5) . ?
O8 C15 1.249(5) . ?
O8 Dy1 2.413(3) 2_666 ?
C15 C16 1.499(5) . ?
C16 C17 1.385(6) . ?
C16 C21 1.387(6) . ?
C17 C18 1.391(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.379(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.388(7) . ?
C19 C22 1.512(6) . ?
C20 C21 1.387(6) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
O9 C23 1.245(5) . ?
O10 C23 1.289(5) . ?
C23 C24 1.487(6) . ?
C24 C25 1.379(6) . ?
C24 C29 1.392(6) . ?
C25 C26 1.392(7) . ?
C25 H25A 0.9500 . ?
C26 C27 1.393(7) . ?
C26 H26A 0.9500 . ?
C27 C28 1.374(8) . ?
C27 C30 1.514(7) . ?
C28 C29 1.383(7) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O11 C31 1.332(5) . ?
O11 H11 0.8400 . ?
O12 C31 1.216(5) . ?
C31 C32 1.485(6) . ?
C32 C37 1.385(6) . ?
C32 C33 1.395(6) . ?
C33 C34 1.379(7) . ?
C33 H33A 0.9500 . ?
C34 C35 1.391(7) . ?
C34 H34A 0.9500 . ?
C35 C36 1.378(8) . ?
C35 C38 1.512(7) . ?
C36 C37 1.392(7) . ?
C36 H36A 0.9500 . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
N41 C41 1.120(7) . ?
C41 C42 1.453(8) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O3 83.72(10) . . ?
O2 Dy1 O6 77.35(10) . . ?
O3 Dy1 O6 141.01(10) . . ?
O2 Dy1 O1 68.69(9) . . ?
O3 Dy1 O1 69.47(9) . . ?
O6 Dy1 O1 71.94(9) . . ?
O2 Dy1 O8 138.49(10) . 2_666 ?
O3 Dy1 O8 74.52(10) . 2_666 ?
O6 Dy1 O8 97.92(10) . 2_666 ?
O1 Dy1 O8 70.67(9) . 2_666 ?
O2 Dy1 O4 79.20(10) . . ?
O3 Dy1 O4 131.42(10) . . ?
O6 Dy1 O4 78.01(10) . . ?
O1 Dy1 O4 139.76(10) . . ?
O8 Dy1 O4 140.93(10) 2_666 . ?
O2 Dy1 O9 143.27(10) . . ?
O3 Dy1 O9 89.35(10) . . ?
O6 Dy1 O9 125.45(9) . . ?
O1 Dy1 O9 141.04(9) . . ?
O8 Dy1 O9 72.33(10) 2_666 . ?
O4 Dy1 O9 78.70(10) . . ?
O2 Dy1 O10 141.06(9) . . ?
O3 Dy1 O10 134.74(9) . . ?
O6 Dy1 O10 73.49(9) . . ?
O1 Dy1 O10 123.57(9) . . ?
O8 Dy1 O10 71.61(9) 2_666 . ?
O4 Dy1 O10 70.01(10) . . ?
O9 Dy1 O10 52.26(9) . . ?
O2 Dy1 N1 67.88(10) . . ?
O3 Dy1 N1 67.36(10) . . ?
O6 Dy1 N1 131.97(10) . . ?
O1 Dy1 N1 120.61(10) . . ?
O8 Dy1 N1 130.08(10) 2_666 . ?
O4 Dy1 N1 64.06(10) . . ?
O9 Dy1 N1 76.14(10) . . ?
O10 Dy1 N1 115.73(10) . . ?
O2 Fe1 O3 175.45(11) . 2_666 ?
O2 Fe1 O5 91.57(12) . . ?
O3 Fe1 O5 91.74(12) 2_666 . ?
O2 Fe1 O7 92.09(12) . . ?
O3 Fe1 O7 90.10(12) 2_666 . ?
O5 Fe1 O7 104.74(12) . . ?
O2 Fe1 O1 92.40(11) . 2_666 ?
O3 Fe1 O1 83.54(11) 2_666 2_666 ?
O5 Fe1 O1 162.92(11) . 2_666 ?
O7 Fe1 O1 91.71(11) . 2_666 ?
O2 Fe1 O1 82.75(11) . . ?
O3 Fe1 O1 94.22(11) 2_666 . ?
O5 Fe1 O1 88.30(11) . . ?
O7 Fe1 O1 166.15(12) . . ?
O1 Fe1 O1 75.74(11) 2_666 . ?
O2 Fe1 Dy1 135.33(8) . 2_666 ?
O3 Fe1 Dy1 40.88(8) 2_666 2_666 ?
O5 Fe1 Dy1 132.11(9) . 2_666 ?
O7 Fe1 Dy1 85.79(8) . 2_666 ?
O1 Fe1 Dy1 43.23(7) 2_666 2_666 ?
O1 Fe1 Dy1 88.87(7) . 2_666 ?
O2 Fe1 Dy1 40.48(7) . . ?
O3 Fe1 Dy1 137.00(8) 2_666 . ?
O5 Fe1 Dy1 83.44(8) . . ?
O7 Fe1 Dy1 132.51(9) . . ?
O1 Fe1 Dy1 88.84(7) 2_666 . ?
O1 Fe1 Dy1 43.12(7) . . ?
Dy1 Fe1 Dy1 123.336(17) 2_666 . ?
Fe1 O1 Fe1 104.26(11) 2_666 . ?
Fe1 O1 Dy1 100.61(11) 2_666 . ?
Fe1 O1 Dy1 100.60(10) . . ?
Fe1 O1 H1 121(3) 2_666 . ?
Fe1 O1 H1 111(3) . . ?
Dy1 O1 H1 117(3) . . ?
C5 N1 C1 112.4(3) . . ?
C5 N1 C3 109.5(3) . . ?
C1 N1 C3 110.9(3) . . ?
C5 N1 Dy1 108.5(2) . . ?
C1 N1 Dy1 110.7(2) . . ?
C3 N1 Dy1 104.5(2) . . ?
N1 C1 C2 112.2(3) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
O2 C2 C1 109.7(3) . . ?
O2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
O2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C2 O2 Fe1 131.7(2) . . ?
C2 O2 Dy1 121.2(2) . . ?
Fe1 O2 Dy1 106.47(11) . . ?
N1 C3 C4 110.2(3) . . ?
N1 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N1 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.1 . . ?
O3 C4 C3 110.0(3) . . ?
O3 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
O3 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 O3 Fe1 123.6(2) . 2_666 ?
C4 O3 Dy1 124.5(2) . . ?
Fe1 O3 Dy1 105.37(11) 2_666 . ?
N1 C5 C6 111.0(4) . . ?
N1 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N1 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
O4 C6 C5 106.9(3) . . ?
O4 C6 H6A 110.3 . . ?
C5 C6 H6A 110.3 . . ?
O4 C6 H6B 110.3 . . ?
C5 C6 H6B 110.3 . . ?
H6A C6 H6B 108.6 . . ?
C6 O4 Dy1 126.7(2) . . ?
C6 O4 H4 106(3) . . ?
Dy1 O4 H4 124(3) . . ?
C7 O5 Fe1 128.3(3) . . ?
C7 O6 Dy1 136.0(2) . . ?
O6 C7 O5 125.5(4) . . ?
O6 C7 C8 118.9(3) . . ?
O5 C7 C8 115.6(4) . . ?
C13 C8 C9 118.7(4) . . ?
C13 C8 C7 121.4(4) . . ?
C9 C8 C7 119.8(4) . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9A 120.0 . . ?
C8 C9 H9A 120.0 . . ?
C9 C10 C11 121.3(4) . . ?
C9 C10 H10A 119.4 . . ?
C11 C10 H10A 119.4 . . ?
C12 C11 C10 118.6(4) . . ?
C12 C11 C14 120.7(5) . . ?
C10 C11 C14 120.7(5) . . ?
C13 C12 C11 120.5(4) . . ?
C13 C12 H12A 119.8 . . ?
C11 C12 H12A 119.8 . . ?
C12 C13 C8 120.8(4) . . ?
C12 C13 H13A 119.6 . . ?
C8 C13 H13A 119.6 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C15 O7 Fe1 125.1(3) . . ?
C15 O8 Dy1 137.2(2) . 2_666 ?
O8 C15 O7 125.6(4) . . ?
O8 C15 C16 118.3(4) . . ?
O7 C15 C16 116.1(4) . . ?
C17 C16 C21 118.7(4) . . ?
C17 C16 C15 121.7(4) . . ?
C21 C16 C15 119.5(4) . . ?
C16 C17 C18 120.5(4) . . ?
C16 C17 H17A 119.8 . . ?
C18 C17 H17A 119.8 . . ?
C19 C18 C17 121.0(5) . . ?
C19 C18 H18A 119.5 . . ?
C17 C18 H18A 119.5 . . ?
C18 C19 C20 118.3(4) . . ?
C18 C19 C22 121.0(5) . . ?
C20 C19 C22 120.7(5) . . ?
C21 C20 C19 121.1(4) . . ?
C21 C20 H20A 119.5 . . ?
C19 C20 H20A 119.5 . . ?
C16 C21 C20 120.3(4) . . ?
C16 C21 H21A 119.8 . . ?
C20 C21 H21A 119.8 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 O9 Dy1 97.2(2) . . ?
C23 O10 Dy1 90.0(2) . . ?
O9 C23 O10 120.4(4) . . ?
O9 C23 C24 119.3(4) . . ?
O10 C23 C24 120.2(4) . . ?
C25 C24 C29 118.4(4) . . ?
C25 C24 C23 120.3(4) . . ?
C29 C24 C23 121.2(4) . . ?
C24 C25 C26 121.0(4) . . ?
C24 C25 H25A 119.5 . . ?
C26 C25 H25A 119.5 . . ?
C25 C26 C27 120.6(5) . . ?
C25 C26 H26A 119.7 . . ?
C27 C26 H26A 119.7 . . ?
C28 C27 C26 117.8(4) . . ?
C28 C27 C30 121.5(5) . . ?
C26 C27 C30 120.6(5) . . ?
C27 C28 C29 122.0(5) . . ?
C27 C28 H28A 119.0 . . ?
C29 C28 H28A 119.0 . . ?
C28 C29 C24 120.1(5) . . ?
C28 C29 H29A 119.9 . . ?
C24 C29 H29A 119.9 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 O11 H11 109.5 . . ?
O12 C31 O11 123.6(4) . . ?
O12 C31 C32 122.0(4) . . ?
O11 C31 C32 114.4(4) . . ?
C37 C32 C33 118.8(4) . . ?
C37 C32 C31 123.0(4) . . ?
C33 C32 C31 118.3(4) . . ?
C34 C33 C32 120.4(4) . . ?
C34 C33 H33A 119.8 . . ?
C32 C33 H33A 119.8 . . ?
C33 C34 C35 121.1(5) . . ?
C33 C34 H34A 119.5 . . ?
C35 C34 H34A 119.5 . . ?
C36 C35 C34 118.2(5) . . ?
C36 C35 C38 121.4(5) . . ?
C34 C35 C38 120.4(5) . . ?
C35 C36 C37 121.3(5) . . ?
C35 C36 H36A 119.4 . . ?
C37 C36 H36A 119.4 . . ?
C32 C37 C36 120.1(5) . . ?
C32 C37 H37A 119.9 . . ?
C36 C37 H37A 119.9 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N41 C41 C42 178.1(7) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N41 0.87(3) 2.21(3) 3.043(6) 162(4) .
O4 H4 O12 0.95(3) 1.71(4) 2.637(4) 163(5) .
O11 H11 O10 0.84 1.85 2.652(4) 159.9 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.498
_refine_diff_density_min         -2.104
_refine_diff_density_rms         0.146
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_amnb16dy
_audit_block_doi                 10.5517/ccy2d9p
_database_code_depnum_ccdc_archive 'CCDC 866242'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1021/ja206941e 2011
_audit_update_record             
;
2012-02-09 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C54 H52 Dy2 Fe2 N8 O32, 2(C H4 O), 7.7(C2 H3 N), 0.3(H2 O)'
_chemical_formula_sum            'C71.4 H83.7 Dy2 Fe2 N15.7 O34.3'
_chemical_formula_weight         2147.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0959(10)
_cell_length_b                   14.0354(12)
_cell_length_c                   14.3715(11)
_cell_angle_alpha                85.882(7)
_cell_angle_beta                 89.474(7)
_cell_angle_gamma                75.941(7)
_cell_volume                     2165.4(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    19649
_cell_measurement_theta_min      1.42
_cell_measurement_theta_max      27.10

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    2.128
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_process_details   
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean 6.667
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15906
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.42
_diffrn_reflns_theta_max         26.82
_reflns_number_total             9149
_reflns_number_gt                6930
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0167P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9149
_refine_ls_number_parameters     590
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0643
_refine_ls_wR_factor_gt          0.0612
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.59449(2) 0.564644(15) 0.677379(15) 0.02603(6) Uani 1 1 d . . .
Fe1 Fe 0.50656(5) 0.39360(4) 0.55103(4) 0.02735(13) Uani 1 1 d . . .
O1 O 0.4430(2) 0.54008(19) 0.56985(18) 0.0267(6) Uani 1 1 d D . .
H1 H 0.369(3) 0.557(3) 0.584(3) 0.032 Uiso 1 1 d D . .
N1 N 0.8295(3) 0.5115(2) 0.6406(2) 0.0294(7) Uani 1 1 d . . .
C1 C 0.8622(4) 0.4122(3) 0.6026(3) 0.0382(10) Uani 1 1 d . . .
H1A H 0.9465 0.3767 0.6246 0.046 Uiso 1 1 calc R . .
H1B H 0.8637 0.4203 0.5336 0.046 Uiso 1 1 calc R . .
C2 C 0.7709(4) 0.3512(3) 0.6322(3) 0.0332(9) Uani 1 1 d . . .
H2A H 0.7830 0.2936 0.5942 0.040 Uiso 1 1 calc R . .
H2B H 0.7850 0.3271 0.6985 0.040 Uiso 1 1 calc R . .
O2 O 0.6479(2) 0.41093(18) 0.61928(18) 0.0293(6) Uani 1 1 d . . .
C3 C 0.8508(4) 0.5890(3) 0.5711(3) 0.0351(9) Uani 1 1 d . . .
H3A H 0.9362 0.5690 0.5466 0.042 Uiso 1 1 calc R . .
H3B H 0.8427 0.6512 0.6017 0.042 Uiso 1 1 calc R . .
C4 C 0.7585(4) 0.6058(3) 0.4910(3) 0.0335(9) Uani 1 1 d . . .
H4B H 0.7640 0.6656 0.4520 0.040 Uiso 1 1 calc R . .
H4C H 0.7790 0.5492 0.4515 0.040 Uiso 1 1 calc R . .
O3 O 0.6369(2) 0.61700(18) 0.52468(17) 0.0290(6) Uani 1 1 d . . .
C5 C 0.9012(4) 0.5127(3) 0.7270(3) 0.0352(10) Uani 1 1 d . . .
H5A H 0.8875 0.5812 0.7451 0.042 Uiso 1 1 calc R . .
H5B H 0.9910 0.4877 0.7151 0.042 Uiso 1 1 calc R . .
C6 C 0.8622(4) 0.4499(3) 0.8054(3) 0.0402(11) Uani 1 1 d . . .
H6A H 0.8919 0.3793 0.7943 0.048 Uiso 1 1 calc R . .
H6B H 0.8973 0.4615 0.8655 0.048 Uiso 1 1 calc R . .
O4 O 0.7294(3) 0.4778(2) 0.8072(2) 0.0382(7) Uani 1 1 d D . .
H4 H 0.699(4) 0.446(3) 0.847(3) 0.046 Uiso 1 1 d D . .
O5 O 0.4209(3) 0.36281(19) 0.66943(18) 0.0338(6) Uani 1 1 d . . .
O6 O 0.4660(3) 0.4748(2) 0.76041(19) 0.0340(7) Uani 1 1 d . . .
C7 C 0.4114(4) 0.4091(3) 0.7438(3) 0.0320(9) Uani 1 1 d . . .
C8 C 0.3254(4) 0.3831(3) 0.8158(3) 0.0301(9) Uani 1 1 d . . .
C9 C 0.3140(4) 0.4257(3) 0.9011(3) 0.0378(10) Uani 1 1 d . . .
H9A H 0.3643 0.4692 0.9142 0.045 Uiso 1 1 calc R . .
C10 C 0.2308(4) 0.4055(3) 0.9667(3) 0.0410(11) Uani 1 1 d . . .
H10A H 0.2232 0.4346 1.0248 0.049 Uiso 1 1 calc R . .
C11 C 0.1589(4) 0.3423(3) 0.9465(3) 0.0339(9) Uani 1 1 d . . .
C12 C 0.1684(4) 0.2979(3) 0.8627(3) 0.0363(10) Uani 1 1 d . . .
H12A H 0.1186 0.2538 0.8503 0.044 Uiso 1 1 calc R . .
C13 C 0.2520(4) 0.3193(3) 0.7980(3) 0.0358(10) Uani 1 1 d . . .
H13A H 0.2596 0.2898 0.7401 0.043 Uiso 1 1 calc R . .
N2 N 0.0713(4) 0.3184(3) 1.0161(3) 0.0452(9) Uani 1 1 d . . .
O7 O 0.0199(3) 0.2534(3) 1.0030(2) 0.0632(10) Uani 1 1 d . . .
O8 O 0.0554(4) 0.3635(3) 1.0863(2) 0.0684(11) Uani 1 1 d . . .
O9 O 0.6031(3) 0.26147(18) 0.51321(18) 0.0313(6) Uani 1 1 d . . .
O10 O 0.5611(3) 0.28150(19) 0.35880(18) 0.0331(7) Uani 1 1 d . . .
C14 C 0.6139(4) 0.2346(3) 0.4299(3) 0.0300(9) Uani 1 1 d . . .
C15 C 0.6999(4) 0.1347(3) 0.4192(3) 0.0292(9) Uani 1 1 d . . .
C16 C 0.7762(4) 0.0862(3) 0.4918(3) 0.0350(10) Uani 1 1 d . . .
H16A H 0.7776 0.1172 0.5483 0.042 Uiso 1 1 calc R . .
C17 C 0.8508(4) -0.0075(3) 0.4833(3) 0.0328(9) Uani 1 1 d . . .
H17A H 0.9030 -0.0414 0.5332 0.039 Uiso 1 1 calc R . .
C18 C 0.8469(4) -0.0497(3) 0.4006(3) 0.0351(10) Uani 1 1 d . . .
C19 C 0.7733(4) -0.0025(3) 0.3254(3) 0.0388(10) Uani 1 1 d . . .
H19A H 0.7732 -0.0333 0.2686 0.047 Uiso 1 1 calc R . .
C20 C 0.7000(4) 0.0907(3) 0.3361(3) 0.0361(10) Uani 1 1 d . . .
H20A H 0.6491 0.1251 0.2857 0.043 Uiso 1 1 calc R . .
N3 N 0.9196(4) -0.1508(3) 0.3913(3) 0.0441(9) Uani 1 1 d . . .
O11 O 0.9129(4) -0.1889(2) 0.3188(2) 0.0620(10) Uani 1 1 d . . .
O12 O 0.9872(4) -0.1917(2) 0.4571(3) 0.0615(10) Uani 1 1 d . . .
O13 O 0.6782(3) 0.69848(19) 0.72876(18) 0.0330(6) Uani 1 1 d . . .
O14 O 0.5376(3) 0.6536(2) 0.82076(18) 0.0337(6) Uani 1 1 d . . .
C21 C 0.6100(4) 0.7076(3) 0.8013(3) 0.0336(10) Uani 1 1 d . . .
C22 C 0.6211(4) 0.7837(3) 0.8671(3) 0.0325(9) Uani 1 1 d . . .
C23 C 0.5565(4) 0.7899(3) 0.9502(3) 0.0372(10) Uani 1 1 d . . .
H23A H 0.5005 0.7492 0.9630 0.045 Uiso 1 1 calc R . .
C24 C 0.5720(4) 0.8539(3) 1.0147(3) 0.0399(11) Uani 1 1 d . . .
H24A H 0.5274 0.8581 1.0716 0.048 Uiso 1 1 calc R . .
C25 C 0.6545(4) 0.9120(3) 0.9943(3) 0.0395(11) Uani 1 1 d . . .
C26 C 0.7198(5) 0.9099(3) 0.9117(3) 0.0476(12) Uani 1 1 d . . .
H26A H 0.7754 0.9511 0.8993 0.057 Uiso 1 1 calc R . .
C27 C 0.7012(4) 0.8457(3) 0.8477(3) 0.0412(11) Uani 1 1 d . . .
H27A H 0.7433 0.8436 0.7898 0.049 Uiso 1 1 calc R . .
N4 N 0.6788(4) 0.9763(3) 1.0645(3) 0.0527(11) Uani 1 1 d . . .
O15 O 0.6164(4) 0.9801(3) 1.1363(3) 0.0679(11) Uani 1 1 d . . .
O16 O 0.7571(4) 1.0223(3) 1.0499(3) 0.0811(13) Uani 1 1 d . . .
N31 N 0.1878(4) 0.6305(3) 0.6335(3) 0.0545(11) Uani 1 1 d . . .
C31 C 0.1092(4) 0.6916(4) 0.6560(3) 0.0441(11) Uani 1 1 d . . .
C32 C 0.0106(5) 0.7709(4) 0.6870(4) 0.0560(13) Uani 1 1 d . . .
H32A H -0.0140 0.7532 0.7504 0.084 Uiso 1 1 calc R . .
H32B H -0.0611 0.7819 0.6448 0.084 Uiso 1 1 calc R . .
H32C H 0.0403 0.8312 0.6869 0.084 Uiso 1 1 calc R . .
N32A N 0.6943(6) 0.3653(4) 0.9689(4) 0.0745(17) Uani 0.85 1 d P A 1
C33A C 0.7158(6) 0.3251(5) 1.0434(5) 0.0602(18) Uani 0.85 1 d P A 1
C34A C 0.7509(6) 0.2742(6) 1.1298(4) 0.073(2) Uani 0.85 1 d P A 1
H34A H 0.7263 0.2116 1.1328 0.109 Uiso 0.85 1 calc PR A 1
H34B H 0.7098 0.3140 1.1797 0.109 Uiso 0.85 1 calc PR A 1
H34C H 0.8412 0.2614 1.1376 0.109 Uiso 0.85 1 calc PR A 1
O32B O 0.699(2) 0.3191(15) 0.9015(15) 0.046(5) Uiso 0.15 1 d P B 2
N33 N 0.0938(5) 0.9874(4) 0.2747(4) 0.0849(16) Uani 1 1 d . . .
C35 C 0.0836(6) 0.9434(5) 0.2134(5) 0.0709(16) Uani 1 1 d . . .
C36 C 0.0715(8) 0.8880(6) 0.1338(5) 0.098(2) Uani 1 1 d . . .
H36A H -0.0155 0.9044 0.1130 0.147 Uiso 1 1 calc R . .
H36B H 0.0981 0.8173 0.1518 0.147 Uiso 1 1 calc R . .
H36C H 0.1236 0.9048 0.0828 0.147 Uiso 1 1 calc R . .
N34 N 0.3701(7) 0.8179(5) 0.1886(6) 0.109(2) Uani 1 1 d . . .
C37 C 0.4054(8) 0.8579(7) 0.2451(7) 0.092(2) Uani 1 1 d . . .
C38 C 0.4506(9) 0.9050(7) 0.3127(5) 0.114(3) Uani 1 1 d . . .
H38A H 0.5015 0.9469 0.2836 0.170 Uiso 1 1 calc R . .
H38B H 0.5015 0.8560 0.3575 0.170 Uiso 1 1 calc R . .
H38C H 0.3810 0.9458 0.3453 0.170 Uiso 1 1 calc R . .
O41 O 0.7111(5) 0.8492(4) 0.5997(4) 0.1010(16) Uani 1 1 d D . .
H41 H 0.685(8) 0.793(5) 0.638(5) 0.151 Uiso 1 1 d D . .
C41A C 0.6171(7) 0.8750(7) 0.5342(6) 0.085(3) Uani 0.85 1 d PD C 1
H41A H 0.6147 0.8177 0.4998 0.128 Uiso 0.85 1 calc PR C 1
H41B H 0.6322 0.9278 0.4906 0.128 Uiso 0.85 1 calc PR C 1
H41C H 0.5376 0.8980 0.5654 0.128 Uiso 0.85 1 calc PR C 1
C41B C 0.684(4) 0.810(3) 0.5173(19) 0.062(10) Uiso 0.15 1 d PD C 2


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.309(2) . ?
Dy1 O3 2.344(2) . ?
Dy1 O6 2.381(3) . ?
Dy1 O1 2.396(3) . ?
Dy1 O10 2.441(3) 2_666 ?
Dy1 O13 2.448(3) . ?
Dy1 O4 2.459(3) . ?
Dy1 O14 2.483(3) . ?
Dy1 N1 2.592(3) . ?
Fe1 O2 1.931(3) . ?
Fe1 O3 1.977(3) 2_666 ?
Fe1 O5 2.012(3) . ?
Fe1 O9 2.013(3) . ?
Fe1 O1 2.042(3) . ?
Fe1 O1 2.050(3) 2_666 ?
O1 Fe1 2.050(3) 2_666 ?
O1 H1 0.82(3) . ?
N1 C3 1.483(5) . ?
N1 C5 1.485(5) . ?
N1 C1 1.494(5) . ?
C1 C2 1.516(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O2 1.424(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.515(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.405(5) . ?
C4 H4B 0.9900 . ?
C4 H4C 0.9900 . ?
O3 Fe1 1.977(3) 2_666 ?
C5 C6 1.506(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O4 1.430(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O4 H4 0.82(3) . ?
O5 C7 1.280(5) . ?
O6 C7 1.257(5) . ?
C7 C8 1.488(6) . ?
C8 C13 1.387(6) . ?
C8 C9 1.393(5) . ?
C9 C10 1.376(6) . ?
C9 H9A 0.9500 . ?
C10 C11 1.376(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.387(6) . ?
C11 N2 1.467(5) . ?
C12 C13 1.376(6) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
N2 O7 1.213(5) . ?
N2 O8 1.218(5) . ?
O9 C14 1.278(4) . ?
O10 C14 1.244(4) . ?
O10 Dy1 2.441(3) 2_666 ?
C14 C15 1.509(5) . ?
C15 C16 1.380(5) . ?
C15 C20 1.383(5) . ?
C16 C17 1.385(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.372(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.387(6) . ?
C18 N3 1.466(5) . ?
C19 C20 1.381(6) . ?
C19 H19A 0.9500 . ?
C20 H20A 0.9500 . ?
N3 O11 1.215(5) . ?
N3 O12 1.230(5) . ?
O13 C21 1.278(5) . ?
O14 C21 1.248(5) . ?
C21 C22 1.504(6) . ?
C22 C23 1.384(6) . ?
C22 C27 1.400(6) . ?
C23 C24 1.376(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.382(6) . ?
C24 H24A 0.9500 . ?
C25 C26 1.383(6) . ?
C25 N4 1.470(6) . ?
C26 C27 1.383(6) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
N4 O16 1.210(6) . ?
N4 O15 1.235(5) . ?
N31 C31 1.127(6) . ?
C31 C32 1.451(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
N32A C33A 1.172(7) . ?
C33A C34A 1.397(8) . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
N33 C35 1.133(7) . ?
C35 C36 1.454(9) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
N34 C37 1.143(10) . ?
C37 C38 1.377(12) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
O41 C41A 1.375(8) . ?
O41 C41B 1.405(19) . ?
O41 H41 1.03(4) . ?
C41A H41A 0.9800 . ?
C41A H41B 0.9800 . ?
C41A H41C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O3 82.94(9) . . ?
O2 Dy1 O6 75.75(9) . . ?
O3 Dy1 O6 140.68(9) . . ?
O2 Dy1 O1 67.30(9) . . ?
O3 Dy1 O1 69.05(9) . . ?
O6 Dy1 O1 72.31(9) . . ?
O2 Dy1 O10 136.24(9) . 2_666 ?
O3 Dy1 O10 74.59(9) . 2_666 ?
O6 Dy1 O10 98.73(10) . 2_666 ?
O1 Dy1 O10 69.69(9) . 2_666 ?
O2 Dy1 O13 143.86(9) . . ?
O3 Dy1 O13 86.96(9) . . ?
O6 Dy1 O13 128.77(9) . . ?
O1 Dy1 O13 139.29(9) . . ?
O10 Dy1 O13 72.50(9) 2_666 . ?
O2 Dy1 O4 82.10(10) . . ?
O3 Dy1 O4 132.44(10) . . ?
O6 Dy1 O4 77.06(10) . . ?
O1 Dy1 O4 140.86(9) . . ?
O10 Dy1 O4 139.91(9) 2_666 . ?
O13 Dy1 O4 79.47(9) . . ?
O2 Dy1 O14 144.29(9) . . ?
O3 Dy1 O14 132.57(9) . . ?
O6 Dy1 O14 76.00(9) . . ?
O1 Dy1 O14 122.81(9) . . ?
O10 Dy1 O14 69.70(9) 2_666 . ?
O13 Dy1 O14 53.31(9) . . ?
O4 Dy1 O14 70.64(9) . . ?
O2 Dy1 N1 68.18(10) . . ?
O3 Dy1 N1 68.23(9) . . ?
O6 Dy1 N1 129.52(10) . . ?
O1 Dy1 N1 120.54(9) . . ?
O10 Dy1 N1 131.75(10) 2_666 . ?
O13 Dy1 N1 75.83(9) . . ?
O4 Dy1 N1 64.28(10) . . ?
O14 Dy1 N1 116.44(10) . . ?
O2 Fe1 O3 176.25(11) . 2_666 ?
O2 Fe1 O5 91.94(11) . . ?
O3 Fe1 O5 91.05(11) 2_666 . ?
O2 Fe1 O9 91.26(11) . . ?
O3 Fe1 O9 90.16(11) 2_666 . ?
O5 Fe1 O9 104.51(11) . . ?
O2 Fe1 O1 82.02(11) . . ?
O3 Fe1 O1 95.79(11) 2_666 . ?
O5 Fe1 O1 89.00(11) . . ?
O9 Fe1 O1 165.16(11) . . ?
O2 Fe1 O1 92.84(11) . 2_666 ?
O3 Fe1 O1 83.69(10) 2_666 2_666 ?
O5 Fe1 O1 164.39(11) . 2_666 ?
O9 Fe1 O1 90.24(11) . 2_666 ?
O1 Fe1 O1 76.98(11) . 2_666 ?
Fe1 O1 Fe1 103.02(11) . 2_666 ?
Fe1 O1 Dy1 101.20(11) . . ?
Fe1 O1 Dy1 101.19(11) 2_666 . ?
Fe1 O1 H1 115(3) . . ?
Fe1 O1 H1 116(3) 2_666 . ?
Dy1 O1 H1 118(3) . . ?
C3 N1 C5 109.4(3) . . ?
C3 N1 C1 111.6(3) . . ?
C5 N1 C1 111.3(3) . . ?
C3 N1 Dy1 104.6(2) . . ?
C5 N1 Dy1 108.7(2) . . ?
C1 N1 Dy1 111.1(2) . . ?
N1 C1 C2 112.3(3) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
O2 C2 C1 108.9(3) . . ?
O2 C2 H2A 109.9 . . ?
C1 C2 H2A 109.9 . . ?
O2 C2 H2B 109.9 . . ?
C1 C2 H2B 109.9 . . ?
H2A C2 H2B 108.3 . . ?
C2 O2 Fe1 132.0(2) . . ?
C2 O2 Dy1 119.9(2) . . ?
Fe1 O2 Dy1 107.97(11) . . ?
N1 C3 C4 111.0(3) . . ?
N1 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N1 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 C3 110.7(3) . . ?
O3 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
O3 C4 H4C 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4B C4 H4C 108.1 . . ?
C4 O3 Fe1 124.5(2) . 2_666 ?
C4 O3 Dy1 122.6(2) . . ?
Fe1 O3 Dy1 105.30(11) 2_666 . ?
N1 C5 C6 110.8(3) . . ?
N1 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O4 C6 C5 106.5(3) . . ?
O4 C6 H6A 110.4 . . ?
C5 C6 H6A 110.4 . . ?
O4 C6 H6B 110.4 . . ?
C5 C6 H6B 110.4 . . ?
H6A C6 H6B 108.6 . . ?
C6 O4 Dy1 125.3(2) . . ?
C6 O4 H4 114(3) . . ?
Dy1 O4 H4 117(3) . . ?
C7 O5 Fe1 126.5(3) . . ?
C7 O6 Dy1 136.9(3) . . ?
O6 C7 O5 126.2(4) . . ?
O6 C7 C8 117.7(3) . . ?
O5 C7 C8 116.1(4) . . ?
C13 C8 C9 119.0(4) . . ?
C13 C8 C7 120.7(4) . . ?
C9 C8 C7 120.3(4) . . ?
C10 C9 C8 120.8(4) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C9 C10 C11 118.7(4) . . ?
C9 C10 H10A 120.6 . . ?
C11 C10 H10A 120.6 . . ?
C10 C11 C12 122.1(4) . . ?
C10 C11 N2 119.6(4) . . ?
C12 C11 N2 118.3(4) . . ?
C13 C12 C11 118.2(4) . . ?
C13 C12 H12A 120.9 . . ?
C11 C12 H12A 120.9 . . ?
C12 C13 C8 121.2(4) . . ?
C12 C13 H13A 119.4 . . ?
C8 C13 H13A 119.4 . . ?
O7 N2 O8 122.6(4) . . ?
O7 N2 C11 119.2(4) . . ?
O8 N2 C11 118.1(4) . . ?
C14 O9 Fe1 125.4(2) . . ?
C14 O10 Dy1 136.9(3) . 2_666 ?
O10 C14 O9 126.9(4) . . ?
O10 C14 C15 118.2(3) . . ?
O9 C14 C15 114.9(3) . . ?
C16 C15 C20 119.8(4) . . ?
C16 C15 C14 120.8(3) . . ?
C20 C15 C14 119.3(3) . . ?
C15 C16 C17 120.7(4) . . ?
C15 C16 H16A 119.7 . . ?
C17 C16 H16A 119.7 . . ?
C18 C17 C16 118.0(4) . . ?
C18 C17 H17A 121.0 . . ?
C16 C17 H17A 121.0 . . ?
C17 C18 C19 123.0(4) . . ?
C17 C18 N3 119.2(4) . . ?
C19 C18 N3 117.7(4) . . ?
C20 C19 C18 117.6(4) . . ?
C20 C19 H19A 121.2 . . ?
C18 C19 H19A 121.2 . . ?
C19 C20 C15 120.9(4) . . ?
C19 C20 H20A 119.5 . . ?
C15 C20 H20A 119.5 . . ?
O11 N3 O12 123.4(4) . . ?
O11 N3 C18 118.9(4) . . ?
O12 N3 C18 117.7(4) . . ?
C21 O13 Dy1 92.6(2) . . ?
C21 O14 Dy1 91.8(2) . . ?
O14 C21 O13 122.3(4) . . ?
O14 C21 C22 119.1(4) . . ?
O13 C21 C22 118.6(4) . . ?
C23 C22 C27 119.1(4) . . ?
C23 C22 C21 120.1(4) . . ?
C27 C22 C21 120.8(4) . . ?
C24 C23 C22 121.2(4) . . ?
C24 C23 H23A 119.4 . . ?
C22 C23 H23A 119.4 . . ?
C23 C24 C25 118.0(4) . . ?
C23 C24 H24A 121.0 . . ?
C25 C24 H24A 121.0 . . ?
C24 C25 C26 123.1(4) . . ?
C24 C25 N4 119.1(4) . . ?
C26 C25 N4 117.8(4) . . ?
C27 C26 C25 117.6(4) . . ?
C27 C26 H26A 121.2 . . ?
C25 C26 H26A 121.2 . . ?
C26 C27 C22 121.0(4) . . ?
C26 C27 H27A 119.5 . . ?
C22 C27 H27A 119.5 . . ?
O16 N4 O15 123.5(4) . . ?
O16 N4 C25 119.6(5) . . ?
O15 N4 C25 116.9(5) . . ?
N31 C31 C32 178.3(5) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N32A C33A C34A 175.6(8) . . ?
N33 C35 C36 179.1(7) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N34 C37 C38 178.7(10) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C41A O41 C41B 45.2(17) . . ?
C41A O41 H41 101(5) . . ?
C41B O41 H41 89(5) . . ?
O41 C41A H41A 109.5 . . ?
O41 C41A H41B 109.5 . . ?
O41 C41A H41C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N31 0.82(3) 2.16(3) 2.972(5) 166(4) .
O4 H4 N32A 0.82(3) 2.03(3) 2.793(6) 155(5) .
O4 H4 O32B 0.82(3) 1.90(4) 2.62(2) 146(5) .
O41 H41 O13 1.03(4) 1.81(4) 2.801(5) 162(7) .

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.093
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ammt16dyx
_audit_block_doi                 10.5517/cc10352c
_database_code_depnum_ccdc_archive 'CCDC 926561'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C3CC45695A 2013
_audit_update_record             
;
2013-09-05 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(C60 H70 Dy2 Fe2 N2 O20), 2(C2 H3 N), 2(C H4 O)'
_chemical_formula_sum            'C66 H84 Dy2 Fe2 N4 O22'
_chemical_formula_weight         1722.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.4404(8)
_cell_length_b                   21.4830(15)
_cell_length_c                   13.7050(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.532(5)
_cell_angle_gamma                90.00
_cell_volume                     3601.1(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    29823
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      28.23

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    2.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.433
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_process_details   
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean 6.667
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38489
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         26.73
_reflns_number_total             7652
_reflns_number_gt                6012
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 The disordered m-tolyl group of one of the carboxylate ligands was refined
 using two sets of isotropic half-occupancy atoms, with the aromatic rings
 constrained to rigid hexagons.
 O-H distances were restrained: DFIX 0.92 0.04 O1 H1 O4 H4
 The m-toluyl ring of one of the carboxylate ligands was disordered, and
 was refined using 50% occupancy isotropic C-atoms; these aromatic rings
 were refined as rigid hexagons (AFIX 66).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0879P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7652
_refine_ls_number_parameters     415
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0528
_refine_ls_wR_factor_ref         0.1262
_refine_ls_wR_factor_gt          0.1207
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.405200(18) 0.626140(10) 0.536579(16) 0.03849(9) Uani 1 1 d . . .
Fe1 Fe 0.45109(5) 0.50649(3) 0.38239(5) 0.03637(15) Uani 1 1 d . . .
O1 O 0.4079(3) 0.51514(16) 0.5203(2) 0.0354(7) Uani 1 1 d D . .
H1 H 0.336(3) 0.497(2) 0.507(4) 0.042 Uiso 1 1 d D . .
N1 N 0.5769(4) 0.6927(2) 0.5145(3) 0.0452(9) Uani 1 1 d . . .
C1 C 0.5781(5) 0.6919(2) 0.4062(4) 0.0464(11) Uani 1 1 d . . .
H1A H 0.6482 0.7093 0.3941 0.056 Uiso 1 1 calc R . .
H1B H 0.5182 0.7185 0.3712 0.056 Uiso 1 1 calc R . .
C2 C 0.5644(4) 0.6263(2) 0.3653(4) 0.0455(11) Uani 1 1 d . . .
H2A H 0.5535 0.6275 0.2919 0.055 Uiso 1 1 calc R . .
H2B H 0.6313 0.6019 0.3900 0.055 Uiso 1 1 calc R . .
O2 O 0.4735(3) 0.59751(16) 0.3950(2) 0.0384(7) Uani 1 1 d . . .
C3 C 0.6569(5) 0.6223(2) 0.6535(4) 0.0492(12) Uani 1 1 d . . .
H3A H 0.7223 0.5965 0.6778 0.059 Uiso 1 1 calc R . .
H3B H 0.6413 0.6477 0.7096 0.059 Uiso 1 1 calc R . .
C4 C 0.6787(5) 0.6646(3) 0.5707(4) 0.0521(13) Uani 1 1 d . . .
H4A H 0.7291 0.6982 0.5994 0.063 Uiso 1 1 calc R . .
H4B H 0.7150 0.6404 0.5246 0.063 Uiso 1 1 calc R . .
O3 O 0.5672(3) 0.58370(15) 0.6180(2) 0.0398(7) Uani 1 1 d . . .
C5 C 0.5593(5) 0.7567(3) 0.5479(4) 0.0527(13) Uani 1 1 d . . .
H5A H 0.4963 0.7756 0.5031 0.063 Uiso 1 1 calc R . .
H5B H 0.6248 0.7823 0.5448 0.063 Uiso 1 1 calc R . .
C6 C 0.5379(6) 0.7565(3) 0.6521(5) 0.0589(14) Uani 1 1 d . . .
H6A H 0.6062 0.7472 0.6994 0.071 Uiso 1 1 calc R . .
H6B H 0.5108 0.7977 0.6688 0.071 Uiso 1 1 calc R . .
O4 O 0.4572(4) 0.70937(18) 0.6586(3) 0.0542(9) Uani 1 1 d D . .
H4 H 0.413(5) 0.725(3) 0.697(4) 0.065 Uiso 1 1 d D . .
O5 O 0.2962(3) 0.51819(16) 0.3139(3) 0.0429(8) Uani 1 1 d . . .
O6 O 0.2477(3) 0.59043(17) 0.4163(3) 0.0443(8) Uani 1 1 d . . .
C7 C 0.2272(4) 0.5550(2) 0.3432(4) 0.0418(10) Uani 1 1 d . . .
C8 C 0.1143(4) 0.5545(3) 0.2835(4) 0.0436(11) Uani 1 1 d . . .
C10 C 0.0374(4) 0.5967(3) 0.3053(5) 0.0512(12) Uani 1 1 d . . .
H10A H 0.0569 0.6249 0.3590 0.061 Uiso 1 1 calc R . .
C11 C -0.0673(5) 0.5983(4) 0.2497(5) 0.0651(17) Uani 1 1 d . . .
C12 C -0.0937(5) 0.5557(4) 0.1724(5) 0.0723(19) Uani 1 1 d . . .
H12A H -0.1658 0.5554 0.1348 0.087 Uiso 1 1 calc R . .
C13 C -0.0181(5) 0.5139(4) 0.1489(5) 0.073(2) Uani 1 1 d . . .
H13A H -0.0378 0.4862 0.0946 0.088 Uiso 1 1 calc R . .
C14 C 0.0863(5) 0.5126(3) 0.2049(4) 0.0556(14) Uani 1 1 d . . .
H14A H 0.1386 0.4835 0.1900 0.067 Uiso 1 1 calc R . .
C15 C -0.1500(6) 0.6445(4) 0.2734(7) 0.086(2) Uani 1 1 d . . .
H15A H -0.1865 0.6274 0.3251 0.129 Uiso 1 1 calc R . .
H15B H -0.2045 0.6527 0.2135 0.129 Uiso 1 1 calc R . .
H15C H -0.1130 0.6834 0.2969 0.129 Uiso 1 1 calc R . .
O7 O 0.5321(3) 0.50168(17) 0.2688(3) 0.0452(8) Uani 1 1 d . . .
O8 O 0.6376(3) 0.41774(17) 0.3156(3) 0.0461(8) Uani 1 1 d . . .
C16 C 0.6015(4) 0.4605(2) 0.2554(4) 0.0435(11) Uani 1 1 d . . .
C17 C 0.6421(4) 0.4633(3) 0.1587(4) 0.0437(11) Uani 1 1 d . . .
C18 C 0.6174(4) 0.5141(3) 0.0956(4) 0.0478(12) Uani 1 1 d . . .
H18A H 0.5753 0.5473 0.1146 0.057 Uiso 1 1 calc R . .
C19 C 0.6531(5) 0.5172(3) 0.0050(4) 0.0524(13) Uani 1 1 d . . .
C20 C 0.7121(5) 0.4668(3) -0.0222(5) 0.0637(16) Uani 1 1 d . . .
H20A H 0.7345 0.4670 -0.0848 0.076 Uiso 1 1 calc R . .
C21 C 0.7383(6) 0.4166(4) 0.0414(5) 0.0669(17) Uani 1 1 d . . .
H21A H 0.7804 0.3833 0.0228 0.080 Uiso 1 1 calc R . .
C22 C 0.7034(5) 0.4149(3) 0.1314(5) 0.0601(15) Uani 1 1 d . . .
H22A H 0.7216 0.3804 0.1745 0.072 Uiso 1 1 calc R . .
C23 C 0.6302(6) 0.5742(3) -0.0608(5) 0.0655(17) Uani 1 1 d . . .
H23A H 0.6947 0.6012 -0.0505 0.098 Uiso 1 1 calc R . .
H23B H 0.5678 0.5969 -0.0440 0.098 Uiso 1 1 calc R . .
H23C H 0.6134 0.5612 -0.1305 0.098 Uiso 1 1 calc R . .
O9 O 0.2406(4) 0.6804(2) 0.5627(3) 0.0589(10) Uani 1 1 d . A .
O10 O 0.3172(3) 0.71573(18) 0.4418(3) 0.0534(9) Uani 1 1 d . A .
C24 C 0.2362(5) 0.7141(3) 0.4866(5) 0.0599(15) Uani 1 1 d . . .
C25A C 0.1396(6) 0.7521(4) 0.4317(7) 0.052(3) Uiso 0.50 1 d PG A 1
C26A C 0.1286(7) 0.7781(5) 0.3375(6) 0.062(3) Uiso 0.50 1 d PG A 1
H26A H 0.1850 0.7729 0.2999 0.075 Uiso 0.50 1 calc PR A 1
C27A C 0.0352(8) 0.8117(5) 0.2984(6) 0.075(4) Uiso 0.50 1 d PG A 1
H27A H 0.0277 0.8295 0.2341 0.091 Uiso 0.50 1 calc PR A 1
C28A C -0.0472(7) 0.8194(5) 0.3535(8) 0.087(5) Uiso 0.50 1 d PG A 1
H28A H -0.1111 0.8423 0.3268 0.104 Uiso 0.50 1 calc PR A 1
C29A C -0.0363(6) 0.7933(5) 0.4476(7) 0.068(3) Uiso 0.50 1 d PG A 1
C30A C 0.0571(7) 0.7597(4) 0.4867(6) 0.066(3) Uiso 0.50 1 d PG A 1
H30A H 0.0646 0.7419 0.5511 0.079 Uiso 0.50 1 calc PR A 1
C31A C -0.1250(16) 0.8028(10) 0.5089(15) 0.097(5) Uiso 0.50 1 d P A 1
H31A H -0.1563 0.8445 0.4964 0.146 Uiso 0.50 1 calc PR A 1
H31B H -0.0935 0.7985 0.5795 0.146 Uiso 0.50 1 calc PR A 1
H31C H -0.1825 0.7716 0.4902 0.146 Uiso 0.50 1 calc PR A 1
C25B C 0.1313(6) 0.7499(4) 0.4662(7) 0.057(3) Uiso 0.50 1 d PG A 2
C26B C 0.1037(7) 0.7748(4) 0.3713(6) 0.056(3) Uiso 0.50 1 d PG A 2
H26B H 0.1497 0.7678 0.3241 0.067 Uiso 0.50 1 calc PR A 2
C27B C 0.0089(8) 0.8099(4) 0.3454(6) 0.062(3) Uiso 0.50 1 d PG A 2
C28B C -0.0583(7) 0.8201(5) 0.4144(8) 0.084(4) Uiso 0.50 1 d PG A 2
H28B H -0.1231 0.8441 0.3967 0.100 Uiso 0.50 1 calc PR A 2
C29B C -0.0307(8) 0.7952(5) 0.5093(8) 0.091(5) Uiso 0.50 1 d PG A 2
H29A H -0.0767 0.8022 0.5565 0.110 Uiso 0.50 1 calc PR A 2
C30B C 0.0641(9) 0.7601(5) 0.5352(6) 0.077(4) Uiso 0.50 1 d PG A 2
H30B H 0.0829 0.7431 0.6001 0.092 Uiso 0.50 1 calc PR A 2
C31B C -0.0251(16) 0.8353(9) 0.2410(14) 0.088(5) Uiso 0.50 1 d P A 2
H31D H 0.0279 0.8222 0.2003 0.132 Uiso 0.50 1 calc PR A 2
H31E H -0.0276 0.8808 0.2433 0.132 Uiso 0.50 1 calc PR A 2
H31F H -0.0976 0.8192 0.2120 0.132 Uiso 0.50 1 calc PR A 2
N41 N 0.1827(5) 0.4630(3) 0.5354(6) 0.0823(19) Uani 1 1 d . . .
C41 C 0.1435(6) 0.5033(4) 0.5671(6) 0.0722(19) Uani 1 1 d . . .
C42 C 0.0934(6) 0.5571(4) 0.6106(7) 0.082(2) Uani 1 1 d . . .
H42A H 0.1292 0.5957 0.5956 0.122 Uiso 1 1 calc R . .
H42B H 0.1028 0.5519 0.6827 0.122 Uiso 1 1 calc R . .
H42C H 0.0153 0.5592 0.5822 0.122 Uiso 1 1 calc R . .
O41 O 0.3274(5) 0.7741(3) 0.7478(4) 0.0881(18) Uani 1 1 d . . .
H41 H 0.3278 0.7798 0.8085 0.132 Uiso 1 1 calc R . .
C43 C 0.2889(9) 0.8283(5) 0.6945(7) 0.116(4) Uani 1 1 d . . .
H43A H 0.3287 0.8647 0.7259 0.174 Uiso 1 1 calc R . .
H43B H 0.2107 0.8334 0.6946 0.174 Uiso 1 1 calc R . .
H43C H 0.3007 0.8247 0.6260 0.174 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O3 2.306(3) . ?
Dy1 O2 2.339(3) . ?
Dy1 O8 2.381(4) 3_666 ?
Dy1 O1 2.396(3) . ?
Dy1 O9 2.439(4) . ?
Dy1 O6 2.442(3) . ?
Dy1 O4 2.453(4) . ?
Dy1 O10 2.464(4) . ?
Dy1 N1 2.633(5) . ?
Fe1 O3 1.951(3) 3_666 ?
Fe1 O2 1.978(4) . ?
Fe1 O5 1.998(3) . ?
Fe1 O7 2.006(4) . ?
Fe1 O1 2.053(3) 3_666 ?
Fe1 O1 2.066(3) . ?
O1 Fe1 2.053(3) 3_666 ?
O1 H1 0.96(3) . ?
N1 C5 1.479(7) . ?
N1 C4 1.484(7) . ?
N1 C1 1.488(7) . ?
C1 C2 1.515(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O2 1.412(6) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 O3 1.404(6) . ?
C3 C4 1.516(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O3 Fe1 1.951(3) 3_666 ?
C5 C6 1.500(8) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O4 1.439(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O4 H4 0.89(4) . ?
O5 C7 1.284(6) . ?
O6 C7 1.246(6) . ?
C7 C8 1.491(7) . ?
C8 C10 1.390(8) . ?
C8 C14 1.399(8) . ?
C10 C11 1.383(8) . ?
C10 H10A 0.9500 . ?
C11 C12 1.393(11) . ?
C11 C15 1.507(10) . ?
C12 C13 1.380(11) . ?
C12 H12A 0.9500 . ?
C13 C14 1.383(8) . ?
C13 H13A 0.9500 . ?
C14 H14A 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O7 C16 1.273(6) . ?
O8 C16 1.261(6) . ?
O8 Dy1 2.381(4) 3_666 ?
C16 C17 1.504(7) . ?
C17 C22 1.380(8) . ?
C17 C18 1.391(8) . ?
C18 C19 1.395(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.395(9) . ?
C19 C23 1.517(9) . ?
C20 C21 1.387(10) . ?
C20 H20A 0.9500 . ?
C21 C22 1.381(9) . ?
C21 H21A 0.9500 . ?
C22 H22A 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O9 C24 1.263(8) . ?
O10 C24 1.273(8) . ?
C24 C25B 1.497(9) . ?
C24 C25A 1.532(9) . ?
C25A C26A 1.3900 . ?
C25A C30A 1.3900 . ?
C26A C27A 1.3900 . ?
C26A H26A 0.9500 . ?
C27A C28A 1.3900 . ?
C27A H27A 0.9500 . ?
C28A C29A 1.3900 . ?
C28A H28A 0.9500 . ?
C29A C30A 1.3900 . ?
C29A C31A 1.52(2) . ?
C30A H30A 0.9500 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C25B C26B 1.3900 . ?
C25B C30B 1.3900 . ?
C26B C27B 1.3900 . ?
C26B H26B 0.9500 . ?
C27B C28B 1.3900 . ?
C27B C31B 1.517(19) . ?
C28B C29B 1.3900 . ?
C28B H28B 0.9500 . ?
C29B C30B 1.3900 . ?
C29B H29A 0.9500 . ?
C30B H30B 0.9500 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
N41 C41 1.119(10) . ?
C41 C42 1.489(12) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O41 C43 1.412(11) . ?
O41 H41 0.8400 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Dy1 O2 83.06(12) . . ?
O3 Dy1 O8 75.14(13) . 3_666 ?
O2 Dy1 O8 140.67(12) . 3_666 ?
O3 Dy1 O1 68.02(11) . . ?
O2 Dy1 O1 69.37(11) . . ?
O8 Dy1 O1 72.19(11) 3_666 . ?
O3 Dy1 O9 143.24(14) . . ?
O2 Dy1 O9 133.62(14) . . ?
O8 Dy1 O9 74.93(14) 3_666 . ?
O1 Dy1 O9 121.05(13) . . ?
O3 Dy1 O6 136.46(12) . . ?
O2 Dy1 O6 74.08(12) . . ?
O8 Dy1 O6 99.99(13) 3_666 . ?
O1 Dy1 O6 69.37(11) . . ?
O9 Dy1 O6 69.99(14) . . ?
O3 Dy1 O4 81.95(13) . . ?
O2 Dy1 O4 131.81(13) . . ?
O8 Dy1 O4 77.34(13) 3_666 . ?
O1 Dy1 O4 141.49(12) . . ?
O9 Dy1 O4 71.07(15) . . ?
O6 Dy1 O4 140.21(13) . . ?
O3 Dy1 O10 145.98(13) . . ?
O2 Dy1 O10 87.81(13) . . ?
O8 Dy1 O10 127.65(14) 3_666 . ?
O1 Dy1 O10 137.81(12) . . ?
O9 Dy1 O10 53.13(15) . . ?
O6 Dy1 O10 70.44(13) . . ?
O4 Dy1 O10 80.00(14) . . ?
O3 Dy1 N1 67.31(13) . . ?
O2 Dy1 N1 67.79(13) . . ?
O8 Dy1 N1 128.66(13) 3_666 . ?
O1 Dy1 N1 120.28(12) . . ?
O9 Dy1 N1 118.55(15) . . ?
O6 Dy1 N1 131.35(13) . . ?
O4 Dy1 N1 64.14(14) . . ?
O10 Dy1 N1 78.87(14) . . ?
O3 Fe1 O2 175.20(14) 3_666 . ?
O3 Fe1 O5 91.23(14) 3_666 . ?
O2 Fe1 O5 91.45(14) . . ?
O3 Fe1 O7 91.25(15) 3_666 . ?
O2 Fe1 O7 92.04(14) . . ?
O5 Fe1 O7 102.71(15) . . ?
O3 Fe1 O1 82.10(14) 3_666 3_666 ?
O2 Fe1 O1 94.40(14) . 3_666 ?
O5 Fe1 O1 165.74(14) . 3_666 ?
O7 Fe1 O1 90.09(14) . 3_666 ?
O3 Fe1 O1 92.41(14) 3_666 . ?
O2 Fe1 O1 83.54(13) . . ?
O5 Fe1 O1 91.64(14) . . ?
O7 Fe1 O1 165.11(14) . . ?
O1 Fe1 O1 76.14(14) 3_666 . ?
Fe1 O1 Fe1 103.86(14) 3_666 . ?
Fe1 O1 Dy1 100.93(13) 3_666 . ?
Fe1 O1 Dy1 100.67(13) . . ?
Fe1 O1 H1 133(3) 3_666 . ?
Fe1 O1 H1 100(3) . . ?
Dy1 O1 H1 113(3) . . ?
C5 N1 C4 112.2(4) . . ?
C5 N1 C1 110.3(4) . . ?
C4 N1 C1 110.5(5) . . ?
C5 N1 Dy1 107.5(3) . . ?
C4 N1 Dy1 110.7(3) . . ?
C1 N1 Dy1 105.4(3) . . ?
N1 C1 C2 111.0(4) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
O2 C2 C1 110.1(4) . . ?
O2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
O2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
C2 O2 Fe1 121.1(3) . . ?
C2 O2 Dy1 123.7(3) . . ?
Fe1 O2 Dy1 105.38(14) . . ?
O3 C3 C4 109.5(4) . . ?
O3 C3 H3A 109.8 . . ?
C4 C3 H3A 109.8 . . ?
O3 C3 H3B 109.8 . . ?
C4 C3 H3B 109.8 . . ?
H3A C3 H3B 108.2 . . ?
N1 C4 C3 112.3(5) . . ?
N1 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
C3 O3 Fe1 132.3(3) . 3_666 ?
C3 O3 Dy1 120.2(3) . . ?
Fe1 O3 Dy1 107.46(14) 3_666 . ?
N1 C5 C6 110.7(5) . . ?
N1 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.1 . . ?
O4 C6 C5 108.0(5) . . ?
O4 C6 H6A 110.1 . . ?
C5 C6 H6A 110.1 . . ?
O4 C6 H6B 110.1 . . ?
C5 C6 H6B 110.1 . . ?
H6A C6 H6B 108.4 . . ?
C6 O4 Dy1 124.8(3) . . ?
C6 O4 H4 107(4) . . ?
Dy1 O4 H4 124(5) . . ?
C7 O5 Fe1 124.9(3) . . ?
C7 O6 Dy1 139.0(3) . . ?
O6 C7 O5 125.3(5) . . ?
O6 C7 C8 118.6(5) . . ?
O5 C7 C8 116.2(5) . . ?
C10 C8 C14 120.1(5) . . ?
C10 C8 C7 119.7(5) . . ?
C14 C8 C7 120.3(5) . . ?
C11 C10 C8 120.9(6) . . ?
C11 C10 H10A 119.5 . . ?
C8 C10 H10A 119.5 . . ?
C10 C11 C12 118.0(6) . . ?
C10 C11 C15 120.6(7) . . ?
C12 C11 C15 121.3(6) . . ?
C13 C12 C11 121.9(6) . . ?
C13 C12 H12A 119.0 . . ?
C11 C12 H12A 119.0 . . ?
C12 C13 C14 119.6(7) . . ?
C12 C13 H13A 120.2 . . ?
C14 C13 H13A 120.2 . . ?
C13 C14 C8 119.4(6) . . ?
C13 C14 H14A 120.3 . . ?
C8 C14 H14A 120.3 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 O7 Fe1 126.7(3) . . ?
C16 O8 Dy1 137.4(3) . 3_666 ?
O8 C16 O7 125.6(5) . . ?
O8 C16 C17 118.0(5) . . ?
O7 C16 C17 116.4(5) . . ?
C22 C17 C18 119.5(5) . . ?
C22 C17 C16 120.0(5) . . ?
C18 C17 C16 120.5(5) . . ?
C17 C18 C19 121.3(6) . . ?
C17 C18 H18A 119.3 . . ?
C19 C18 H18A 119.3 . . ?
C20 C19 C18 118.0(6) . . ?
C20 C19 C23 121.2(6) . . ?
C18 C19 C23 120.8(6) . . ?
C21 C20 C19 120.6(6) . . ?
C21 C20 H20A 119.7 . . ?
C19 C20 H20A 119.7 . . ?
C22 C21 C20 120.4(6) . . ?
C22 C21 H21A 119.8 . . ?
C20 C21 H21A 119.8 . . ?
C17 C22 C21 120.1(6) . . ?
C17 C22 H22A 120.0 . . ?
C21 C22 H22A 120.0 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C24 O9 Dy1 93.6(4) . . ?
C24 O10 Dy1 92.2(4) . . ?
O9 C24 O10 119.7(5) . . ?
O9 C24 C25B 110.7(7) . . ?
O10 C24 C25B 129.5(7) . . ?
O9 C24 C25A 128.5(7) . . ?
O10 C24 C25A 111.6(6) . . ?
C26A C25A C30A 120.0 . . ?
C26A C25A C24 127.3(6) . . ?
C30A C25A C24 112.7(6) . . ?
C25A C26A C27A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C27A C26A H26A 120.0 . . ?
C28A C27A C26A 120.0 . . ?
C28A C27A H27A 120.0 . . ?
C26A C27A H27A 120.0 . . ?
C27A C28A C29A 120.0 . . ?
C27A C28A H28A 120.0 . . ?
C29A C28A H28A 120.0 . . ?
C30A C29A C28A 120.0 . . ?
C30A C29A C31A 119.9(10) . . ?
C28A C29A C31A 120.1(10) . . ?
C29A C30A C25A 120.0 . . ?
C29A C30A H30A 120.0 . . ?
C25A C30A H30A 120.0 . . ?
C26B C25B C30B 120.0 . . ?
C26B C25B C24 115.5(7) . . ?
C30B C25B C24 124.5(7) . . ?
C25B C26B C27B 120.0 . . ?
C25B C26B H26B 120.0 . . ?
C27B C26B H26B 120.0 . . ?
C28B C27B C26B 120.0 . . ?
C28B C27B C31B 119.1(10) . . ?
C26B C27B C31B 120.9(10) . . ?
C27B C28B C29B 120.0 . . ?
C27B C28B H28B 120.0 . . ?
C29B C28B H28B 120.0 . . ?
C30B C29B C28B 120.0 . . ?
C30B C29B H29A 120.0 . . ?
C28B C29B H29A 120.0 . . ?
C29B C30B C25B 120.0 . . ?
C29B C30B H30B 120.0 . . ?
C25B C30B H30B 120.0 . . ?
C27B C31B H31D 109.5 . . ?
C27B C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C27B C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
N41 C41 C42 178.9(9) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C43 O41 H41 109.5 . . ?
O41 C43 H43A 109.5 . . ?
O41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
O41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N41 0.96(3) 2.14(4) 3.058(7) 158(5) .
O4 H4 O41 0.89(4) 1.74(4) 2.600(6) 162(7) .
O41 H41 O10 0.84 1.86 2.694(7) 173.2 4_576

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.676
_refine_diff_density_min         -2.641
_refine_diff_density_rms         0.159
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_am3cbdy
_audit_block_doi                 10.5517/cc10351b
_database_code_depnum_ccdc_archive 'CCDC 926560'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C3CC45695A 2013
_audit_update_record             
;
2013-09-05 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H52 Dy2 Fe2 N8 O20, 2(C2 H3 N)'
_chemical_formula_sum            'C64 H58 Dy2 Fe2 N10 O20'
_chemical_formula_weight         1723.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.700(2)
_cell_length_b                   12.915(3)
_cell_length_c                   14.427(3)
_cell_angle_alpha                87.159(17)
_cell_angle_beta                 74.068(18)
_cell_angle_gamma                73.135(17)
_cell_volume                     1662.2(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5918
_cell_measurement_theta_min      1.47
_cell_measurement_theta_max      25.65

_exptl_crystal_description       plate
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_absorpt_coefficient_mu    2.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_process_details   
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean 6.667
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15190
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_av_unetI/netI     0.1302
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.35
_reflns_number_total             6039
_reflns_number_gt                3726
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger.
 O-H distances were restrained:
 DFIX 0.92 0.04 O1 H1 O4 H4
 DFIX 2.00 0.04 H4 N31
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0648P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6039
_refine_ls_number_parameters     449
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0616
_refine_ls_wR_factor_ref         0.1467
_refine_ls_wR_factor_gt          0.1311
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.70891(7) 0.32132(4) 0.35603(4) 0.03422(16) Uani 1 1 d . . .
Fe1 Fe 0.55476(17) 0.43057(11) 0.58639(10) 0.0350(4) Uani 1 1 d . . .
O1 O 0.4804(8) 0.4165(5) 0.4679(5) 0.0367(16) Uani 1 1 d D . .
H1 H 0.394(7) 0.401(9) 0.489(7) 0.044 Uiso 1 1 d D . .
N1 N 0.9395(10) 0.3928(6) 0.3129(5) 0.036(2) Uani 1 1 d . . .
C1 C 1.0001(11) 0.3677(8) 0.4003(7) 0.038(2) Uani 1 1 d . . .
H1A H 1.0412 0.2884 0.4039 0.045 Uiso 1 1 calc R . .
H1B H 1.0824 0.4007 0.3939 0.045 Uiso 1 1 calc R . .
C2 C 0.8785(12) 0.4111(9) 0.4912(7) 0.041(3) Uani 1 1 d . . .
H2A H 0.9171 0.3874 0.5479 0.049 Uiso 1 1 calc R . .
H2B H 0.8478 0.4912 0.4919 0.049 Uiso 1 1 calc R . .
O2 O 0.7522(8) 0.3734(5) 0.4973(5) 0.0361(16) Uani 1 1 d . . .
C3 C 0.8986(14) 0.5119(8) 0.2975(8) 0.046(3) Uani 1 1 d . . .
H3A H 0.9787 0.5285 0.2450 0.055 Uiso 1 1 calc R . .
H3B H 0.8915 0.5506 0.3570 0.055 Uiso 1 1 calc R . .
C4 C 0.7511(13) 0.5527(9) 0.2717(8) 0.045(3) Uani 1 1 d . . .
H4A H 0.7142 0.6326 0.2787 0.054 Uiso 1 1 calc R . .
H4B H 0.7647 0.5317 0.2040 0.054 Uiso 1 1 calc R . .
O3 O 0.6464(8) 0.5061(5) 0.3348(5) 0.0381(17) Uani 1 1 d . . .
C5 C 1.0498(13) 0.3312(9) 0.2276(7) 0.045(3) Uani 1 1 d . . .
H5A H 1.0843 0.2541 0.2433 0.054 Uiso 1 1 calc R . .
H5B H 1.1378 0.3595 0.2090 0.054 Uiso 1 1 calc R . .
C6 C 0.9797(14) 0.3406(10) 0.1433(8) 0.055(3) Uani 1 1 d . . .
H6A H 0.9662 0.4142 0.1173 0.066 Uiso 1 1 calc R . .
H6B H 1.0454 0.2875 0.0910 0.066 Uiso 1 1 calc R . .
O4 O 0.8360(9) 0.3193(6) 0.1798(5) 0.0464(19) Uani 1 1 d D . .
H4 H 0.836(13) 0.260(6) 0.144(6) 0.056 Uiso 1 1 d D . .
O5 O 0.6312(9) 0.2001(5) 0.4765(5) 0.0427(18) Uani 1 1 d . . .
O6 O 0.5500(9) 0.2806(5) 0.6268(5) 0.0417(18) Uani 1 1 d . . .
C7 C 0.5900(13) 0.1999(8) 0.5683(8) 0.041(3) Uani 1 1 d . . .
C8 C 0.5886(12) 0.0918(8) 0.6120(8) 0.039(2) Uani 1 1 d . . .
C9 C 0.6417(13) -0.0009(8) 0.5518(8) 0.041(3) Uani 1 1 d . . .
H9A H 0.6796 0.0043 0.4842 0.049 Uiso 1 1 calc R . .
C10 C 0.6387(14) -0.1008(8) 0.5916(8) 0.046(3) Uani 1 1 d . . .
C11 C 0.5893(17) -0.1104(9) 0.6900(9) 0.064(4) Uani 1 1 d . . .
H11A H 0.5896 -0.1793 0.7164 0.076 Uiso 1 1 calc R . .
C12 C 0.5397(19) -0.0196(10) 0.7499(9) 0.073(5) Uani 1 1 d . . .
H12A H 0.5039 -0.0255 0.8176 0.088 Uiso 1 1 calc R . .
C13 C 0.5420(15) 0.0801(8) 0.7113(8) 0.052(3) Uani 1 1 d . . .
H13A H 0.5112 0.1419 0.7532 0.063 Uiso 1 1 calc R . .
C14 C 0.6918(14) -0.1963(8) 0.5285(8) 0.046(3) Uani 1 1 d . . .
N2 N 0.7341(13) -0.2746(8) 0.4820(8) 0.061(3) Uani 1 1 d . . .
O7 O 0.5164(9) 0.3559(5) 0.2758(5) 0.0429(18) Uani 1 1 d . . .
O8 O 0.3685(8) 0.5285(5) 0.3063(5) 0.0394(17) Uani 1 1 d . . .
C15 C 0.4308(13) 0.4405(9) 0.2554(8) 0.040(3) Uani 1 1 d . . .
C16 C 0.3922(12) 0.4385(8) 0.1612(7) 0.035(2) Uani 1 1 d . . .
C17 C 0.4345(12) 0.3384(9) 0.1105(7) 0.041(2) Uani 1 1 d . . .
H17A H 0.4918 0.2748 0.1334 0.049 Uiso 1 1 calc R . .
C18 C 0.3922(16) 0.3334(10) 0.0273(8) 0.055(3) Uani 1 1 d . . .
C19 C 0.3150(16) 0.4261(11) -0.0096(9) 0.062(4) Uani 1 1 d . . .
H19A H 0.2854 0.4216 -0.0664 0.075 Uiso 1 1 calc R . .
C20 C 0.2811(16) 0.5248(11) 0.0364(9) 0.064(4) Uani 1 1 d . . .
H20A H 0.2324 0.5888 0.0093 0.077 Uiso 1 1 calc R . .
C21 C 0.3174(13) 0.5317(9) 0.1223(8) 0.048(3) Uani 1 1 d . . .
H21A H 0.2913 0.6000 0.1544 0.057 Uiso 1 1 calc R . .
C22 C 0.4242(17) 0.2293(11) -0.0191(10) 0.067(4) Uani 1 1 d . . .
N3 N 0.4516(18) 0.1444(11) -0.0508(10) 0.097(5) Uani 1 1 d . . .
O9 O 0.7453(9) 0.1473(5) 0.2787(5) 0.0407(17) Uani 1 1 d . . .
O10 O 0.9170(9) 0.1612(5) 0.3491(6) 0.0469(19) Uani 1 1 d . . .
C23 C 0.8579(14) 0.1054(9) 0.3100(8) 0.044(3) Uani 1 1 d . . .
C24 C 0.9284(13) -0.0145(8) 0.3009(8) 0.041(3) Uani 1 1 d . . .
C25 C 0.8867(13) -0.0751(8) 0.2406(8) 0.044(3) Uani 1 1 d . . .
H25A H 0.8158 -0.0403 0.2065 0.053 Uiso 1 1 calc R . .
C26 C 0.9508(14) -0.1872(8) 0.2315(8) 0.046(3) Uani 1 1 d . . .
C27 C 1.0480(15) -0.2388(9) 0.2865(9) 0.055(3) Uani 1 1 d . . .
H27A H 1.0900 -0.3152 0.2810 0.066 Uiso 1 1 calc R . .
C28 C 1.0832(15) -0.1790(9) 0.3489(10) 0.059(3) Uani 1 1 d . . .
H28A H 1.1486 -0.2139 0.3867 0.071 Uiso 1 1 calc R . .
C29 C 1.0211(14) -0.0662(9) 0.3557(9) 0.055(3) Uani 1 1 d . . .
H29A H 1.0439 -0.0250 0.3991 0.066 Uiso 1 1 calc R . .
C30 C 0.9186(16) -0.2471(9) 0.1637(9) 0.057(3) Uani 1 1 d . . .
N4 N 0.8951(15) -0.2963(9) 0.1074(8) 0.074(3) Uani 1 1 d . . .
N31 N 0.8242(17) 0.1681(12) 0.0381(9) 0.090(4) Uani 1 1 d D . .
C31 C 0.8148(19) 0.0974(15) -0.0036(12) 0.082(5) Uani 1 1 d . . .
C32 C 0.806(2) 0.0070(15) -0.0568(14) 0.102(6) Uani 1 1 d . . .
H32A H 0.7905 0.0312 -0.1196 0.153 Uiso 1 1 calc R . .
H32B H 0.7220 -0.0190 -0.0200 0.153 Uiso 1 1 calc R . .
H32C H 0.8994 -0.0519 -0.0665 0.153 Uiso 1 1 calc R . .


_geom_special_details            
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O3 2.312(6) . ?
Dy1 O2 2.356(6) . ?
Dy1 O7 2.383(7) . ?
Dy1 O1 2.383(7) . ?
Dy1 O5 2.395(7) . ?
Dy1 O10 2.418(7) . ?
Dy1 O9 2.447(6) . ?
Dy1 O4 2.501(7) . ?
Dy1 N1 2.573(8) . ?
Fe1 O3 1.928(7) 2_666 ?
Fe1 O2 1.946(7) . ?
Fe1 O6 2.004(7) . ?
Fe1 O8 2.043(7) 2_666 ?
Fe1 O1 2.058(7) 2_666 ?
Fe1 O1 2.064(7) . ?
O1 Fe1 2.058(7) 2_666 ?
O1 H1 0.89(4) . ?
N1 C5 1.474(12) . ?
N1 C3 1.495(13) . ?
N1 C1 1.515(13) . ?
C1 C2 1.505(14) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 O2 1.424(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.516(16) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.420(12) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O3 Fe1 1.928(7) 2_666 ?
C5 C6 1.532(16) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O4 1.450(14) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O4 H4 0.93(3) . ?
O5 C7 1.275(12) . ?
O6 C7 1.273(12) . ?
C7 C8 1.506(13) . ?
C8 C13 1.393(15) . ?
C8 C9 1.398(14) . ?
C9 C10 1.390(14) . ?
C9 H9A 0.9500 . ?
C10 C11 1.381(16) . ?
C10 C14 1.449(14) . ?
C11 C12 1.378(16) . ?
C11 H11A 0.9500 . ?
C12 C13 1.381(15) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 N2 1.148(13) . ?
O7 C15 1.243(13) . ?
O8 C15 1.278(12) . ?
O8 Fe1 2.043(7) 2_666 ?
C15 C16 1.509(14) . ?
C16 C21 1.393(15) . ?
C16 C17 1.413(14) . ?
C17 C18 1.380(15) . ?
C17 H17A 0.9500 . ?
C18 C19 1.382(18) . ?
C18 C22 1.445(16) . ?
C19 C20 1.376(17) . ?
C19 H19A 0.9500 . ?
C20 C21 1.392(16) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
C22 N3 1.139(16) . ?
O9 C23 1.262(14) . ?
O10 C23 1.274(13) . ?
C23 C24 1.497(14) . ?
C24 C29 1.367(17) . ?
C24 C25 1.406(14) . ?
C25 C26 1.397(14) . ?
C25 H25A 0.9500 . ?
C26 C27 1.399(17) . ?
C26 C30 1.426(16) . ?
C27 C28 1.384(17) . ?
C27 H27A 0.9500 . ?
C28 C29 1.402(16) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 N4 1.162(16) . ?
N31 C31 1.155(18) . ?
C31 C32 1.46(2) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Dy1 O2 82.0(2) . . ?
O3 Dy1 O7 75.4(2) . . ?
O2 Dy1 O7 140.4(2) . . ?
O3 Dy1 O1 67.4(2) . . ?
O2 Dy1 O1 68.8(2) . . ?
O7 Dy1 O1 72.5(2) . . ?
O3 Dy1 O5 137.1(2) . . ?
O2 Dy1 O5 74.5(2) . . ?
O7 Dy1 O5 100.8(3) . . ?
O1 Dy1 O5 70.8(2) . . ?
O3 Dy1 O10 143.6(3) . . ?
O2 Dy1 O10 87.0(2) . . ?
O7 Dy1 O10 129.5(2) . . ?
O1 Dy1 O10 138.9(2) . . ?
O5 Dy1 O10 71.0(3) . . ?
O3 Dy1 O9 143.3(2) . . ?
O2 Dy1 O9 134.4(2) . . ?
O7 Dy1 O9 75.5(2) . . ?
O1 Dy1 O9 123.1(2) . . ?
O5 Dy1 O9 70.7(2) . . ?
O10 Dy1 O9 54.4(2) . . ?
O3 Dy1 O4 81.6(2) . . ?
O2 Dy1 O4 134.6(2) . . ?
O7 Dy1 O4 73.8(3) . . ?
O1 Dy1 O4 138.7(2) . . ?
O5 Dy1 O4 139.5(2) . . ?
O10 Dy1 O4 81.8(3) . . ?
O9 Dy1 O4 69.1(2) . . ?
O3 Dy1 N1 67.8(3) . . ?
O2 Dy1 N1 69.8(2) . . ?
O7 Dy1 N1 127.3(3) . . ?
O1 Dy1 N1 121.7(2) . . ?
O5 Dy1 N1 131.8(3) . . ?
O10 Dy1 N1 75.9(3) . . ?
O9 Dy1 N1 115.2(2) . . ?
O4 Dy1 N1 64.8(2) . . ?
O3 Fe1 O2 174.9(3) 2_666 . ?
O3 Fe1 O6 92.4(3) 2_666 . ?
O2 Fe1 O6 90.7(3) . . ?
O3 Fe1 O8 88.3(3) 2_666 2_666 ?
O2 Fe1 O8 95.2(3) . 2_666 ?
O6 Fe1 O8 98.6(3) . 2_666 ?
O3 Fe1 O1 81.5(3) 2_666 2_666 ?
O2 Fe1 O1 94.6(3) . 2_666 ?
O6 Fe1 O1 166.7(3) . 2_666 ?
O8 Fe1 O1 93.0(3) 2_666 2_666 ?
O3 Fe1 O1 92.0(3) 2_666 . ?
O2 Fe1 O1 83.8(3) . . ?
O6 Fe1 O1 91.9(3) . . ?
O8 Fe1 O1 169.4(3) 2_666 . ?
O1 Fe1 O1 76.6(3) 2_666 . ?
Fe1 O1 Fe1 103.4(3) 2_666 . ?
Fe1 O1 Dy1 101.3(3) 2_666 . ?
Fe1 O1 Dy1 100.8(3) . . ?
Fe1 O1 H1 110(7) 2_666 . ?
Fe1 O1 H1 108(7) . . ?
Dy1 O1 H1 130(7) . . ?
C5 N1 C3 111.9(8) . . ?
C5 N1 C1 109.8(8) . . ?
C3 N1 C1 110.3(8) . . ?
C5 N1 Dy1 108.8(6) . . ?
C3 N1 Dy1 112.0(6) . . ?
C1 N1 Dy1 103.6(5) . . ?
C2 C1 N1 110.6(8) . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
O2 C2 C1 110.7(8) . . ?
O2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
C2 O2 Fe1 125.3(6) . . ?
C2 O2 Dy1 120.1(6) . . ?
Fe1 O2 Dy1 105.5(3) . . ?
N1 C3 C4 112.1(8) . . ?
N1 C3 H3A 109.2 . . ?
C4 C3 H3A 109.2 . . ?
N1 C3 H3B 109.2 . . ?
C4 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
O3 C4 C3 108.2(8) . . ?
O3 C4 H4A 110.1 . . ?
C3 C4 H4A 110.1 . . ?
O3 C4 H4B 110.1 . . ?
C3 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
C4 O3 Fe1 131.7(6) . 2_666 ?
C4 O3 Dy1 120.1(6) . . ?
Fe1 O3 Dy1 108.2(3) 2_666 . ?
N1 C5 C6 110.2(9) . . ?
N1 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
N1 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
O4 C6 C5 107.5(9) . . ?
O4 C6 H6A 110.2 . . ?
C5 C6 H6A 110.2 . . ?
O4 C6 H6B 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
C6 O4 Dy1 122.5(6) . . ?
C6 O4 H4 108(7) . . ?
Dy1 O4 H4 114(6) . . ?
C7 O5 Dy1 136.7(6) . . ?
C7 O6 Fe1 124.0(7) . . ?
O6 C7 O5 127.3(9) . . ?
O6 C7 C8 116.7(9) . . ?
O5 C7 C8 115.9(9) . . ?
C13 C8 C9 118.6(9) . . ?
C13 C8 C7 122.1(9) . . ?
C9 C8 C7 119.2(9) . . ?
C10 C9 C8 119.5(10) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
C11 C10 C9 121.0(10) . . ?
C11 C10 C14 119.8(10) . . ?
C9 C10 C14 119.2(10) . . ?
C12 C11 C10 119.7(10) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.2 . . ?
C11 C12 C13 119.9(11) . . ?
C11 C12 H12A 120.1 . . ?
C13 C12 H12A 120.1 . . ?
C12 C13 C8 121.3(10) . . ?
C12 C13 H13A 119.4 . . ?
C8 C13 H13A 119.4 . . ?
N2 C14 C10 177.1(12) . . ?
C15 O7 Dy1 133.1(6) . . ?
C15 O8 Fe1 123.4(7) . 2_666 ?
O7 C15 O8 127.5(9) . . ?
O7 C15 C16 116.4(9) . . ?
O8 C15 C16 116.0(10) . . ?
C21 C16 C17 119.0(9) . . ?
C21 C16 C15 122.3(9) . . ?
C17 C16 C15 118.7(9) . . ?
C18 C17 C16 119.7(11) . . ?
C18 C17 H17A 120.2 . . ?
C16 C17 H17A 120.2 . . ?
C17 C18 C19 120.8(11) . . ?
C17 C18 C22 119.2(12) . . ?
C19 C18 C22 119.9(11) . . ?
C20 C19 C18 119.8(11) . . ?
C20 C19 H19A 120.1 . . ?
C18 C19 H19A 120.1 . . ?
C19 C20 C21 120.6(12) . . ?
C19 C20 H20A 119.7 . . ?
C21 C20 H20A 119.7 . . ?
C20 C21 C16 119.9(10) . . ?
C20 C21 H21A 120.0 . . ?
C16 C21 H21A 120.0 . . ?
N3 C22 C18 175.8(16) . . ?
C23 O9 Dy1 90.4(6) . . ?
C23 O10 Dy1 91.4(7) . . ?
O9 C23 O10 122.7(10) . . ?
O9 C23 C24 119.9(9) . . ?
O10 C23 C24 117.3(11) . . ?
C29 C24 C25 119.9(10) . . ?
C29 C24 C23 121.5(10) . . ?
C25 C24 C23 118.4(10) . . ?
C26 C25 C24 119.2(11) . . ?
C26 C25 H25A 120.4 . . ?
C24 C25 H25A 120.4 . . ?
C25 C26 C27 120.1(11) . . ?
C25 C26 C30 119.0(12) . . ?
C27 C26 C30 120.9(10) . . ?
C28 C27 C26 120.2(11) . . ?
C28 C27 H27A 119.9 . . ?
C26 C27 H27A 119.9 . . ?
C27 C28 C29 119.2(12) . . ?
C27 C28 H28A 120.4 . . ?
C29 C28 H28A 120.4 . . ?
C24 C29 C28 121.2(12) . . ?
C24 C29 H29A 119.4 . . ?
C28 C29 H29A 119.4 . . ?
N4 C30 C26 178.7(15) . . ?
N31 C31 C32 179(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N2 0.89(4) 2.28(7) 3.076(12) 149(9) 2_656
O4 H4 N31 0.93(3) 2.04(3) 2.942(15) 162(9) .

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.911
_refine_diff_density_min         -2.908
_refine_diff_density_rms         0.191
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_amcb16dyy
_audit_block_doi                 10.5517/ccy2dbq
_database_code_depnum_ccdc_archive 'CCDC 866243'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C3CC45695A 2013
2 10.1021/ja206941e 2011
_audit_update_record             
;
2012-02-09 deposited with the CCDC.	2022-07-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H52 Dy2 Fe2 N8 O20, 6(C2 H3 N)'
_chemical_formula_sum            'C72 H70 Dy2 Fe2 N14 O20'
_chemical_formula_weight         1888.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.9912(6)
_cell_length_b                   12.8733(7)
_cell_length_c                   14.5474(8)
_cell_angle_alpha                70.567(4)
_cell_angle_beta                 79.101(4)
_cell_angle_gamma                67.143(4)
_cell_volume                     1946.78(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    68334
_cell_measurement_theta_min      1.49
_cell_measurement_theta_max      29.56

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    2.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.453
_exptl_absorpt_correction_T_max  0.585
_exptl_absorpt_process_details   
;
XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe IPDS II'
_diffrn_measurement_method       'area detector'
_diffrn_detector_area_resol_mean 6.667
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56533
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         29.21
_reflns_number_total             10469
_reflns_number_gt                9443
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)'
_computing_cell_refinement       'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_data_reduction        'X-Area 1.38 (Stoe & Cie GmbH, 2006)'
_computing_structure_solution    'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_structure_refinement  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'
_computing_molecular_graphics    'Diamond 2.1 (Crystal Impact, 1998)'
_computing_publication_material  'SHELXTL 6.14 (BrukerAXS Inc., 2003)'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0354P)²+0.5276P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10469
_refine_ls_number_parameters     505
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0593
_refine_ls_wR_factor_gt          0.0579
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.278990(8) 0.425652(8) 0.535934(8) 0.02092(3) Uani 1 1 d . . .
Fe1 Fe 0.45040(3) 0.59272(3) 0.39865(2) 0.02139(6) Uani 1 1 d . . .
O1 O 0.39507(13) 0.53786(13) 0.54369(11) 0.0221(3) Uani 1 1 d D . .
H1 H 0.358(3) 0.584(2) 0.573(2) 0.027 Uiso 1 1 d D . .
N1 N 0.37831(17) 0.25864(16) 0.45071(15) 0.0268(4) Uani 1 1 d . . .
C1 C 0.4482(2) 0.2970(2) 0.35765(19) 0.0317(5) Uani 1 1 d . . .
H1B H 0.4428 0.2593 0.3102 0.038 Uiso 1 1 calc R . .
H1C H 0.5347 0.2701 0.3703 0.038 Uiso 1 1 calc R . .
C2 C 0.4017(2) 0.4297(2) 0.31336(17) 0.0287(4) Uani 1 1 d . . .
H2A H 0.4624 0.4532 0.2630 0.034 Uiso 1 1 calc R . .
H2B H 0.3257 0.4546 0.2816 0.034 Uiso 1 1 calc R . .
O2 O 0.37988(14) 0.48512(13) 0.38688(11) 0.0242(3) Uani 1 1 d . . .
C3 C 0.4600(2) 0.15899(19) 0.52164(19) 0.0302(5) Uani 1 1 d . . .
H3A H 0.5103 0.0971 0.4898 0.036 Uiso 1 1 calc R . .
H3B H 0.4109 0.1248 0.5773 0.036 Uiso 1 1 calc R . .
C4 C 0.5421(2) 0.1989(2) 0.5591(2) 0.0301(5) Uani 1 1 d . . .
H4A H 0.5810 0.1371 0.6173 0.036 Uiso 1 1 calc R . .
H4B H 0.6068 0.2117 0.5081 0.036 Uiso 1 1 calc R . .
O3 O 0.47379(13) 0.30433(13) 0.58388(12) 0.0239(3) Uani 1 1 d . . .
C5 C 0.2827(2) 0.2226(2) 0.43439(19) 0.0310(5) Uani 1 1 d . . .
H5A H 0.2494 0.1831 0.4981 0.037 Uiso 1 1 calc R . .
H5B H 0.3180 0.1657 0.3955 0.037 Uiso 1 1 calc R . .
C6 C 0.1817(2) 0.3277(2) 0.38122(19) 0.0323(5) Uani 1 1 d . . .
H6A H 0.2097 0.3580 0.3125 0.039 Uiso 1 1 calc R . .
H6B H 0.1114 0.3052 0.3816 0.039 Uiso 1 1 calc R . .
O4 O 0.14775(15) 0.41576(15) 0.43095(13) 0.0303(3) Uani 1 1 d D . .
H4 H 0.071(2) 0.459(3) 0.424(2) 0.036 Uiso 1 1 d D . .
O5 O 0.29000(14) 0.72233(14) 0.38046(12) 0.0272(3) Uani 1 1 d . . .
O6 O 0.15952(14) 0.63432(14) 0.47310(12) 0.0273(3) Uani 1 1 d . . .
C7 C 0.18607(19) 0.72232(19) 0.42141(16) 0.0245(4) Uani 1 1 d . . .
C8 C 0.08900(19) 0.84310(19) 0.40282(17) 0.0257(4) Uani 1 1 d . . .
C9 C 0.1198(2) 0.9409(2) 0.3520(2) 0.0434(7) Uani 1 1 d . . .
H9A H 0.2009 0.9313 0.3263 0.052 Uiso 1 1 calc R . .
C10 C 0.0333(2) 1.0528(2) 0.3382(3) 0.0475(7) Uani 1 1 d . . .
H10A H 0.0553 1.1199 0.3044 0.057 Uiso 1 1 calc R . .
C11 C -0.0852(2) 1.0662(2) 0.37397(19) 0.0307(5) Uani 1 1 d . . .
C12 C -0.1174(2) 0.9689(2) 0.4230(3) 0.0450(7) Uani 1 1 d . . .
H12A H -0.1991 0.9782 0.4468 0.054 Uiso 1 1 calc R . .
C13 C -0.0293(2) 0.8571(2) 0.4374(2) 0.0405(6) Uani 1 1 d . . .
H13A H -0.0510 0.7899 0.4713 0.049 Uiso 1 1 calc R . .
C14 C -0.1738(2) 1.1836(2) 0.3621(2) 0.0336(5) Uani 1 1 d . . .
N2 N -0.2430(2) 1.2766(2) 0.3545(2) 0.0409(5) Uani 1 1 d . . .
O7 O 0.52875(15) 0.61018(15) 0.26304(12) 0.0292(3) Uani 1 1 d . . .
O8 O 0.71675(14) 0.58388(15) 0.29283(12) 0.0296(3) Uani 1 1 d . . .
C15 C 0.6350(2) 0.6153(2) 0.23743(17) 0.0269(4) Uani 1 1 d . . .
C16 C 0.6592(2) 0.6678(2) 0.13007(17) 0.0294(5) Uani 1 1 d . . .
C17 C 0.5756(3) 0.6924(3) 0.0647(2) 0.0429(6) Uani 1 1 d . . .
H17A H 0.5046 0.6728 0.0875 0.051 Uiso 1 1 calc R . .
C18 C 0.5951(3) 0.7451(3) -0.0335(2) 0.0476(7) Uani 1 1 d . . .
H18A H 0.5390 0.7600 -0.0786 0.057 Uiso 1 1 calc R . .
C19 C 0.6975(3) 0.7761(2) -0.06553(19) 0.0372(5) Uani 1 1 d . . .
C20 C 0.7817(2) 0.7531(2) -0.00086(19) 0.0369(5) Uani 1 1 d . . .
H20A H 0.8514 0.7749 -0.0235 0.044 Uiso 1 1 calc R . .
C21 C 0.7625(2) 0.6978(2) 0.09701(18) 0.0336(5) Uani 1 1 d . . .
H21A H 0.8200 0.6802 0.1418 0.040 Uiso 1 1 calc R . .
C22 C 0.7172(3) 0.8325(3) -0.1682(2) 0.0425(6) Uani 1 1 d . . .
N3 N 0.7305(3) 0.8774(3) -0.24920(19) 0.0535(7) Uani 1 1 d . . .
O9 O 0.21543(14) 0.26408(14) 0.64287(13) 0.0304(3) Uani 1 1 d . . .
O10 O 0.07229(14) 0.43865(14) 0.62550(13) 0.0285(3) Uani 1 1 d . . .
C23 C 0.11010(19) 0.3272(2) 0.66408(17) 0.0260(4) Uani 1 1 d . . .
C24 C 0.0291(2) 0.2700(2) 0.73632(17) 0.0286(4) Uani 1 1 d . . .
C25 C -0.0927(2) 0.3333(2) 0.7529(2) 0.0376(6) Uani 1 1 d . . .
H25A H -0.1244 0.4153 0.7210 0.045 Uiso 1 1 calc R . .
C26 C -0.1686(3) 0.2779(3) 0.8156(2) 0.0457(7) Uani 1 1 d . . .
H26A H -0.2522 0.3213 0.8254 0.055 Uiso 1 1 calc R . .
C27 C -0.1219(3) 0.1592(3) 0.8636(2) 0.0417(6) Uani 1 1 d . . .
C28 C -0.0003(3) 0.0954(3) 0.8487(2) 0.0440(6) Uani 1 1 d . . .
H28A H 0.0316 0.0139 0.8819 0.053 Uiso 1 1 calc R . .
C29 C 0.0744(2) 0.1508(2) 0.7854(2) 0.0397(6) Uani 1 1 d . . .
H29A H 0.1578 0.1069 0.7754 0.048 Uiso 1 1 calc R . .
C30 C -0.2011(3) 0.1018(3) 0.9286(3) 0.0611(10) Uani 1 1 d . . .
N4 N -0.2657(3) 0.0583(3) 0.9787(3) 0.0946(15) Uani 1 1 d . . .
N31 N 0.6152(4) 0.0823(3) 0.2471(4) 0.0884(12) Uani 1 1 d . . .
C31 C 0.5974(4) 0.0171(3) 0.2216(3) 0.0644(10) Uani 1 1 d . . .
C32 C 0.5784(4) -0.0689(3) 0.1889(3) 0.0662(10) Uani 1 1 d . . .
H32A H 0.6192 -0.0688 0.1238 0.099 Uiso 1 1 calc R . .
H32B H 0.4913 -0.0491 0.1860 0.099 Uiso 1 1 calc R . .
H32C H 0.6119 -0.1472 0.2347 0.099 Uiso 1 1 calc R . .
N32 N 0.9320(5) 0.2076(5) 0.0971(4) 0.1126(17) Uani 1 1 d . . .
C33 C 0.8286(6) 0.2634(5) 0.0946(4) 0.0876(14) Uani 1 1 d . . .
C34 C 0.7019(5) 0.3332(6) 0.0936(6) 0.118(2) Uani 1 1 d . . .
H34A H 0.6542 0.2813 0.1161 0.176 Uiso 1 1 calc R . .
H34B H 0.6826 0.3830 0.0270 0.176 Uiso 1 1 calc R . .
H34C H 0.6823 0.3828 0.1371 0.176 Uiso 1 1 calc R . .
N33 N 1.1340(8) 0.5070(6) 0.0851(5) 0.156(3) Uani 1 1 d . . .
C35 C 1.0629(6) 0.4681(4) 0.1267(4) 0.0844(14) Uani 1 1 d . . .
C36 C 0.9760(4) 0.4178(4) 0.1802(4) 0.0804(13) Uani 1 1 d . . .
H36A H 1.0145 0.3319 0.2016 0.121 Uiso 1 1 calc R . .
H36B H 0.9102 0.4394 0.1388 0.121 Uiso 1 1 calc R . .
H36C H 0.9429 0.4470 0.2375 0.121 Uiso 1 1 calc R . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.3183(15) . ?
Dy1 O3 2.3322(15) . ?
Dy1 O1 2.4014(15) . ?
Dy1 O9 2.4407(16) . ?
Dy1 O6 2.4445(16) . ?
Dy1 O4 2.4534(17) . ?
Dy1 O8 2.4622(17) 2_666 ?
Dy1 O10 2.5438(16) . ?
Dy1 N1 2.6084(19) . ?
Dy1 Fe1 3.4442(4) . ?
Dy1 Fe1 3.4516(3) 2_666 ?
Fe1 O2 1.9455(15) . ?
Fe1 O3 1.9735(15) 2_666 ?
Fe1 O5 1.9897(15) . ?
Fe1 O7 1.9982(16) . ?
Fe1 O1 2.0477(15) 2_666 ?
Fe1 O1 2.0576(16) . ?
Fe1 Dy1 3.4516(3) 2_666 ?
O1 Fe1 2.0477(15) 2_666 ?
O1 H1 0.79(2) . ?
N1 C5 1.475(3) . ?
N1 C3 1.482(3) . ?
N1 C1 1.492(3) . ?
C1 C2 1.519(3) . ?
C1 H1B 0.9900 . ?
C1 H1C 0.9900 . ?
C2 O2 1.407(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.521(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 O3 1.411(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O3 Fe1 1.9736(15) 2_666 ?
C5 C6 1.510(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 O4 1.432(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
O4 H4 0.88(3) . ?
O5 C7 1.276(3) . ?
O6 C7 1.254(3) . ?
C7 C8 1.510(3) . ?
C8 C13 1.374(3) . ?
C8 C9 1.380(3) . ?
C9 C10 1.384(3) . ?
C9 H9A 0.9500 . ?
C10 C11 1.382(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.380(4) . ?
C11 C14 1.446(3) . ?
C12 C13 1.391(3) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 N2 1.144(3) . ?
O7 C15 1.279(3) . ?
O8 C15 1.244(3) . ?
O8 Dy1 2.4622(17) 2_666 ?
C15 C16 1.503(3) . ?
C16 C17 1.387(4) . ?
C16 C21 1.392(3) . ?
C17 C18 1.381(4) . ?
C17 H17A 0.9500 . ?
C18 C19 1.387(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.391(4) . ?
C19 C22 1.447(4) . ?
C20 C21 1.384(3) . ?
C20 H20A 0.9500 . ?
C21 H21A 0.9500 . ?
C22 N3 1.137(4) . ?
O9 C23 1.254(3) . ?
O10 C23 1.278(3) . ?
C23 C24 1.498(3) . ?
C24 C25 1.388(3) . ?
C24 C29 1.389(4) . ?
C25 C26 1.388(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.382(4) . ?
C26 H26A 0.9500 . ?
C27 C28 1.384(4) . ?
C27 C30 1.443(4) . ?
C28 C29 1.380(4) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 N4 1.139(4) . ?
N31 C31 1.124(6) . ?
C31 C32 1.447(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
N32 C33 1.167(7) . ?
C33 C34 1.433(8) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
N33 C35 1.132(8) . ?
C35 C36 1.412(8) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O3 83.79(5) . . ?
O2 Dy1 O1 68.06(5) . . ?
O3 Dy1 O1 68.53(5) . . ?
O2 Dy1 O9 143.13(5) . . ?
O3 Dy1 O9 85.73(5) . . ?
O1 Dy1 O9 138.35(6) . . ?
O2 Dy1 O6 76.23(5) . . ?
O3 Dy1 O6 140.00(5) . . ?
O1 Dy1 O6 71.92(5) . . ?
O9 Dy1 O6 129.83(5) . . ?
O2 Dy1 O4 82.11(6) . . ?
O3 Dy1 O4 131.90(5) . . ?
O1 Dy1 O4 142.48(6) . . ?
O9 Dy1 O4 78.97(6) . . ?
O6 Dy1 O4 79.46(6) . . ?
O2 Dy1 O8 137.43(5) . 2_666 ?
O3 Dy1 O8 72.88(5) . 2_666 ?
O1 Dy1 O8 70.37(5) . 2_666 ?
O9 Dy1 O8 71.01(6) . 2_666 ?
O6 Dy1 O8 99.35(6) . 2_666 ?
O4 Dy1 O8 139.53(6) . 2_666 ?
O2 Dy1 O10 144.97(5) . . ?
O3 Dy1 O10 130.80(5) . . ?
O1 Dy1 O10 124.26(5) . . ?
O9 Dy1 O10 52.39(5) . . ?
O6 Dy1 O10 77.75(5) . . ?
O4 Dy1 O10 70.36(6) . . ?
O8 Dy1 O10 69.92(5) 2_666 . ?
O2 Dy1 N1 67.74(6) . . ?
O3 Dy1 N1 67.21(6) . . ?
O1 Dy1 N1 119.24(5) . . ?
O9 Dy1 N1 75.59(6) . . ?
O6 Dy1 N1 131.60(6) . . ?
O4 Dy1 N1 64.87(6) . . ?
O8 Dy1 N1 129.04(6) 2_666 . ?
O10 Dy1 N1 115.98(5) . . ?
O2 Fe1 O3 177.15(7) . 2_666 ?
O2 Fe1 O5 90.32(7) . . ?
O3 Fe1 O5 91.74(6) 2_666 . ?
O2 Fe1 O7 92.45(7) . . ?
O3 Fe1 O7 89.00(7) 2_666 . ?
O5 Fe1 O7 103.28(7) . . ?
O2 Fe1 O1 94.49(6) . 2_666 ?
O3 Fe1 O1 83.02(6) 2_666 2_666 ?
O5 Fe1 O1 164.09(7) . 2_666 ?
O7 Fe1 O1 91.68(7) . 2_666 ?
O2 Fe1 O1 82.55(6) . . ?
O3 Fe1 O1 95.54(6) 2_666 . ?
O5 Fe1 O1 88.09(6) . . ?
O7 Fe1 O1 167.65(7) . . ?
O1 Fe1 O1 77.53(6) 2_666 . ?
Fe1 O1 Fe1 102.47(6) 2_666 . ?
Fe1 O1 Dy1 101.46(6) 2_666 . ?
Fe1 O1 Dy1 100.86(6) . . ?
Fe1 O1 H1 117(2) 2_666 . ?
Fe1 O1 H1 120(2) . . ?
Dy1 O1 H1 112(2) . . ?
C5 N1 C3 108.79(18) . . ?
C5 N1 C1 111.68(19) . . ?
C3 N1 C1 110.64(18) . . ?
C5 N1 Dy1 108.88(13) . . ?
C3 N1 Dy1 105.43(14) . . ?
C1 N1 Dy1 111.20(13) . . ?
N1 C1 C2 112.38(18) . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
N1 C1 H1C 109.1 . . ?
C2 C1 H1C 109.1 . . ?
H1B C1 H1C 107.9 . . ?
O2 C2 C1 109.74(19) . . ?
O2 C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 . . ?
O2 C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C2 O2 Fe1 129.49(13) . . ?
C2 O2 Dy1 121.87(13) . . ?
Fe1 O2 Dy1 107.44(7) . . ?
N1 C3 C4 111.04(18) . . ?
N1 C3 H3A 109.4 . . ?
C4 C3 H3A 109.4 . . ?
N1 C3 H3B 109.4 . . ?
C4 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O3 C4 C3 109.99(18) . . ?
O3 C4 H4A 109.7 . . ?
C3 C4 H4A 109.7 . . ?
O3 C4 H4B 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C4 O3 Fe1 122.56(13) . 2_666 ?
C4 O3 Dy1 124.70(13) . . ?
Fe1 O3 Dy1 106.27(6) 2_666 . ?
N1 C5 C6 110.92(19) . . ?
N1 C5 H5A 109.5 . . ?
C6 C5 H5A 109.5 . . ?
N1 C5 H5B 109.5 . . ?
C6 C5 H5B 109.5 . . ?
H5A C5 H5B 108.0 . . ?
O4 C6 C5 107.41(19) . . ?
O4 C6 H6A 110.2 . . ?
C5 C6 H6A 110.2 . . ?
O4 C6 H6B 110.2 . . ?
C5 C6 H6B 110.2 . . ?
H6A C6 H6B 108.5 . . ?
C6 O4 Dy1 124.43(14) . . ?
C6 O4 H4 109(2) . . ?
Dy1 O4 H4 126(2) . . ?
C7 O5 Fe1 129.31(15) . . ?
C7 O6 Dy1 133.44(14) . . ?
O6 C7 O5 126.7(2) . . ?
O6 C7 C8 119.50(19) . . ?
O5 C7 C8 113.82(19) . . ?
C13 C8 C9 119.6(2) . . ?
C13 C8 C7 120.8(2) . . ?
C9 C8 C7 119.6(2) . . ?
C8 C9 C10 120.6(2) . . ?
C8 C9 H9A 119.7 . . ?
C10 C9 H9A 119.7 . . ?
C11 C10 C9 119.5(2) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 120.3(2) . . ?
C12 C11 C14 120.6(2) . . ?
C10 C11 C14 119.0(2) . . ?
C11 C12 C13 119.5(2) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C8 C13 C12 120.5(2) . . ?
C8 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
N2 C14 C11 178.5(3) . . ?
C15 O7 Fe1 125.10(15) . . ?
C15 O8 Dy1 134.67(15) . 2_666 ?
O8 C15 O7 126.2(2) . . ?
O8 C15 C16 118.4(2) . . ?
O7 C15 C16 115.3(2) . . ?
C17 C16 C21 120.0(2) . . ?
C17 C16 C15 120.1(2) . . ?
C21 C16 C15 119.8(2) . . ?
C18 C17 C16 120.3(2) . . ?
C18 C17 H17A 119.9 . . ?
C16 C17 H17A 119.9 . . ?
C17 C18 C19 119.3(3) . . ?
C17 C18 H18A 120.3 . . ?
C19 C18 H18A 120.3 . . ?
C18 C19 C20 121.2(2) . . ?
C18 C19 C22 119.3(3) . . ?
C20 C19 C22 119.6(2) . . ?
C21 C20 C19 119.0(2) . . ?
C21 C20 H20A 120.5 . . ?
C19 C20 H20A 120.5 . . ?
C20 C21 C16 120.3(2) . . ?
C20 C21 H21A 119.9 . . ?
C16 C21 H21A 119.9 . . ?
N3 C22 C19 178.7(3) . . ?
C23 O9 Dy1 96.07(13) . . ?
C23 O10 Dy1 90.64(13) . . ?
O9 C23 O10 120.8(2) . . ?
O9 C23 C24 118.9(2) . . ?
O10 C23 C24 120.3(2) . . ?
C25 C24 C29 118.8(2) . . ?
C25 C24 C23 121.1(2) . . ?
C29 C24 C23 120.0(2) . . ?
C24 C25 C26 120.6(2) . . ?
C24 C25 H25A 119.7 . . ?
C26 C25 H25A 119.7 . . ?
C27 C26 C25 119.7(3) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C28 120.3(2) . . ?
C26 C27 C30 119.5(3) . . ?
C28 C27 C30 120.2(3) . . ?
C29 C28 C27 119.8(3) . . ?
C29 C28 H28A 120.1 . . ?
C27 C28 H28A 120.1 . . ?
C28 C29 C24 120.8(2) . . ?
C28 C29 H29A 119.6 . . ?
C24 C29 H29A 119.6 . . ?
N4 C30 C27 178.5(5) . . ?
N31 C31 C32 178.3(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N32 C33 C34 178.4(7) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N33 C35 C36 178.7(8) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 N2 0.79(2) 2.24(2) 3.029(3) 175(3) 2_576
O4 H4 O10 0.88(3) 1.81(3) 2.665(2) 164(3) 2_566

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.853
_refine_diff_density_min         -1.083
_refine_diff_density_rms         0.082

