####################################################################### 
# 
# 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_Cu5Gd4final
_audit_block_doi                 10.5517/ccw4vmg
_database_code_depnum_ccdc_archive 'CCDC 809026'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/c1sc00038a 2011
2 10.1002/chem.201100218 2011
_audit_update_record             
;
2011-01-20 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
#TrackingRef '- 1 Cu5Gd4final.CIF'

#==========================================================================

_audit_creation_method           SHELXL-97
_audit_creation_date             '9 November 2005'
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C38 H82 Cu5 Gd4 N8 O34, 2(C4 H10 O), 2(C H4 O)'
_chemical_formula_sum            'C48 H110 Cu5 Gd4 N8 O38'
_chemical_formula_weight         2354.16

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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

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

_cell_length_a                   11.050(2)
_cell_length_b                   13.830(3)
_cell_length_c                   14.030(3)
_cell_angle_alpha                78.80(3)
_cell_angle_beta                 83.81(3)
_cell_angle_gamma                69.28(3)
_cell_volume                     1965.4(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12139
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      25.00

_exptl_crystal_description       plate
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1159
_exptl_absorpt_coefficient_mu    4.737
_exptl_absorpt_correction_type   MULTi-scan
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71082
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         '3BM1 dipole'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12139
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7056
_reflns_number_gt                6876
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'


_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 crystal was run on the Australian synchrotron in which We were
restricted to only one 185 degree phi scan. The asymmetric unit contains
half the cluster which lies upon an inversion centre as well as solvent
MeOH and Et2O molecules. All non H-atoms are refined anisotropically
and H-atoms are placed in calculated positions.
;

_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)+(0.0000P)²+20.5732P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7056
_refine_ls_number_parameters     477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0398
_refine_ls_wR_factor_ref         0.0999
_refine_ls_wR_factor_gt          0.0992
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_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
Gd1 Gd 0.16746(3) 0.47562(2) 0.30188(2) 0.00891(11) Uani 1 1 d . . .
Gd2 Gd 0.13931(3) 0.67966(2) 0.45069(2) 0.01088(11) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.5000 0.5000 0.0076(2) Uani 1 2 d S . .
Cu2 Cu 0.09850(7) 0.58197(6) 0.68482(5) 0.01224(18) Uani 1 1 d . . .
Cu3 Cu -0.14134(7) 0.74542(6) 0.57703(6) 0.01054(18) Uani 1 1 d . . .
O1 O -0.0180(4) 0.6035(3) 0.5833(3) 0.0110(9) Uani 1 1 d . . .
O2 O 0.0045(4) 0.6058(3) 0.3837(3) 0.0106(9) Uani 1 1 d . . .
O3 O 0.2343(4) 0.5041(3) 0.4408(3) 0.0147(9) Uani 1 1 d . . .
O4 O 0.2700(5) 0.4205(4) 0.1422(4) 0.0197(10) Uani 1 1 d . . .
O5 O 0.4032(4) 0.4375(4) 0.2354(3) 0.0172(10) Uani 1 1 d . . .
O6 O 0.4767(5) 0.3737(5) 0.1022(4) 0.0276(12) Uani 1 1 d . . .
O7 O 0.1803(6) 0.6303(4) 0.2116(5) 0.0406(17) Uani 1 1 d . . .
O8 O 0.1322(6) 0.7670(5) 0.2880(4) 0.0359(14) Uani 1 1 d . . .
O9 O 0.3665(5) 0.6782(4) 0.4157(5) 0.0295(13) Uani 1 1 d . . .
O10 O 0.2289(5) 0.8221(4) 0.4517(4) 0.0243(11) Uani 1 1 d . . .
O11 O 0.4318(6) 0.8049(5) 0.4321(6) 0.0478(19) Uani 1 1 d . . .
O12 O -0.0468(4) 0.8090(3) 0.4770(3) 0.0159(10) Uani 1 1 d . . .
O13 O -0.0622(5) 0.7740(4) 0.7215(4) 0.0257(11) Uani 1 1 d . . .
H13 H -0.0818 0.7616 0.7810 0.031 Uiso 1 1 calc R . .
O14 O -0.2717(4) 0.6977(3) 0.6505(3) 0.0148(9) Uani 1 1 d . . .
O15 O 0.0016(4) 0.5168(4) 0.7796(3) 0.0165(10) Uani 1 1 d . . .
O16 O 0.2033(5) 0.6521(4) 0.6041(3) 0.0186(10) Uani 1 1 d . . .
O17 O 0.3899(6) 0.3465(4) 0.9317(4) 0.0329(13) Uani 1 1 d . . .
H17 H 0.4431 0.3229 0.9761 0.040 Uiso 1 1 calc R . .
O1S O 0.5928(14) 0.9838(11) 0.2131(10) 0.119(5) Uani 1 1 d . . .
O2S O -0.1850(6) 0.7395(5) 0.8967(4) 0.0384(15) Uani 1 1 d . . .
H2S H -0.2141 0.6899 0.9042 0.046 Uiso 1 1 calc R . .
N1 N 0.3863(5) 0.4104(4) 0.1591(4) 0.0159(12) Uani 1 1 d . . .
N2 N 0.3441(6) 0.7690(5) 0.4336(5) 0.0279(15) Uani 1 1 d . . .
N3 N -0.2651(5) 0.8920(4) 0.5795(4) 0.0144(11) Uani 1 1 d . . .
N4 N 0.2231(5) 0.5533(5) 0.7885(4) 0.0185(12) Uani 1 1 d . . .
C1 C -0.1161(6) 0.6707(5) 0.3438(5) 0.0167(14) Uani 1 1 d . . .
H1A H -0.1537 0.6283 0.3163 0.025 Uiso 1 1 calc R . .
H1B H -0.1027 0.7256 0.2924 0.025 Uiso 1 1 calc R . .
H1C H -0.1752 0.7032 0.3950 0.025 Uiso 1 1 calc R . .
C2 C 0.3522(7) 0.4405(6) 0.4843(5) 0.0206(15) Uani 1 1 d . . .
H2A H 0.3830 0.3726 0.4621 0.031 Uiso 1 1 calc R . .
H2B H 0.3384 0.4298 0.5552 0.031 Uiso 1 1 calc R . .
H2C H 0.4168 0.4752 0.4658 0.031 Uiso 1 1 calc R . .
C3 C 0.1511(6) 0.7278(6) 0.2128(6) 0.0210(15) Uani 1 1 d . A .
C4 C 0.1352(9) 0.7980(7) 0.1119(6) 0.0322(18) Uani 1 1 d . . .
C5 C 0.1142(13) 0.9088(9) 0.1196(9) 0.061(3) Uani 1 1 d . A 1
H5A H 0.1091 0.9507 0.0543 0.091 Uiso 1 1 calc R A 1
H5B H 0.1865 0.9114 0.1526 0.091 Uiso 1 1 calc R A 1
H5C H 0.0331 0.9370 0.1570 0.091 Uiso 1 1 calc R A 1
C6 C 0.0189(15) 0.7909(11) 0.0646(10) 0.070(4) Uani 1 1 d . A 1
H6A H 0.0152 0.8263 -0.0033 0.104 Uiso 1 1 calc R A 1
H6B H -0.0615 0.8249 0.1002 0.104 Uiso 1 1 calc R A 1
H6C H 0.0295 0.7171 0.0669 0.104 Uiso 1 1 calc R A 1
C7 C 0.2549(15) 0.7552(12) 0.0484(9) 0.083(5) Uani 1 1 d . A 1
H7A H 0.2795 0.6789 0.0562 0.125 Uiso 1 1 calc R A 1
H7B H 0.3261 0.7731 0.0676 0.125 Uiso 1 1 calc R A 1
H7C H 0.2367 0.7862 -0.0198 0.125 Uiso 1 1 calc R A 1
C8 C -0.1051(7) 0.9183(5) 0.4497(5) 0.0179(14) Uani 1 1 d . . .
H8A H -0.0944 0.9384 0.3785 0.021 Uiso 1 1 calc R . .
H8B H -0.0633 0.9552 0.4820 0.021 Uiso 1 1 calc R . .
C9 C -0.2488(7) 0.9490(5) 0.4801(5) 0.0180(14) Uani 1 1 d . . .
H9A H -0.2859 1.0256 0.4796 0.022 Uiso 1 1 calc R . .
H9B H -0.2955 0.9313 0.4335 0.022 Uiso 1 1 calc R . .
C10 C -0.2347(8) 0.9375(5) 0.6577(6) 0.0239(16) Uani 1 1 d . . .
H10A H -0.2944 0.9313 0.7146 0.029 Uiso 1 1 calc R . .
H10B H -0.2508 1.0132 0.6344 0.029 Uiso 1 1 calc R . .
C11 C -0.0963(8) 0.8859(6) 0.6901(6) 0.0272(17) Uani 1 1 d . . .
H11A H -0.0365 0.8994 0.6356 0.033 Uiso 1 1 calc R . .
H11B H -0.0851 0.9179 0.7443 0.033 Uiso 1 1 calc R . .
C12 C -0.3945(7) 0.8786(5) 0.5972(6) 0.0228(16) Uani 1 1 d . . .
H12A H -0.4240 0.8704 0.5360 0.027 Uiso 1 1 calc R . .
H12B H -0.4587 0.9413 0.6198 0.027 Uiso 1 1 calc R . .
C13 C -0.3828(7) 0.7819(5) 0.6738(6) 0.0200(15) Uani 1 1 d . . .
H13A H -0.3748 0.7968 0.7386 0.024 Uiso 1 1 calc R . .
H13B H -0.4613 0.7627 0.6759 0.024 Uiso 1 1 calc R . .
C14 C 0.1445(8) 0.5448(7) 0.8805(5) 0.0255(16) Uani 1 1 d . . .
H14A H 0.0883 0.6154 0.8926 0.031 Uiso 1 1 calc R . .
H14B H 0.2019 0.5105 0.9359 0.031 Uiso 1 1 calc R . .
C15 C 0.0614(7) 0.4789(6) 0.8702(5) 0.0226(16) Uani 1 1 d . . .
H15A H 0.1165 0.4043 0.8737 0.027 Uiso 1 1 calc R . .
H15B H -0.0055 0.4843 0.9238 0.027 Uiso 1 1 calc R . .
C16 C 0.2597(7) 0.6497(6) 0.7665(6) 0.0241(16) Uani 1 1 d . . .
H16A H 0.3360 0.6394 0.8034 0.029 Uiso 1 1 calc R . .
H16B H 0.1872 0.7101 0.7858 0.029 Uiso 1 1 calc R . .
C17 C 0.2916(8) 0.6716(7) 0.6562(5) 0.0265(17) Uani 1 1 d . . .
H17A H 0.2869 0.7455 0.6365 0.032 Uiso 1 1 calc R . .
H17B H 0.3808 0.6260 0.6411 0.032 Uiso 1 1 calc R . .
C18 C 0.3360(7) 0.4584(6) 0.7772(6) 0.0253(16) Uani 1 1 d . . .
H18A H 0.3839 0.4736 0.7156 0.030 Uiso 1 1 calc R . .
H18B H 0.3036 0.4018 0.7708 0.030 Uiso 1 1 calc R . .
C19 C 0.4301(8) 0.4178(6) 0.8582(6) 0.0267(16) Uani 1 1 d . . .
H19A H 0.5180 0.3815 0.8320 0.032 Uiso 1 1 calc R . .
H19B H 0.4330 0.4771 0.8865 0.032 Uiso 1 1 calc R . .
C1S C 0.486(2) 0.8724(18) 0.184(2) 0.146(10) Uani 1 1 d . . .
H1S1 H 0.4339 0.8626 0.2441 0.219 Uiso 1 1 calc R . .
H1S2 H 0.5029 0.8138 0.1495 0.219 Uiso 1 1 calc R . .
H1S3 H 0.4396 0.9383 0.1430 0.219 Uiso 1 1 calc R . .
C2S C 0.597(2) 0.876(2) 0.2069(19) 0.146(11) Uani 1 1 d . . .
H2S1 H 0.6644 0.8475 0.1573 0.175 Uiso 1 1 calc R . .
H2S2 H 0.6224 0.8300 0.2702 0.175 Uiso 1 1 calc R . .
C3S C 0.7042(18) 1.0011(14) 0.1915(12) 0.094(6) Uani 1 1 d . . .
H3S1 H 0.7235 1.0036 0.1206 0.113 Uiso 1 1 calc R . .
H3S2 H 0.7740 0.9410 0.2251 0.113 Uiso 1 1 calc R . .
C4S C 0.7068(14) 1.0938(10) 0.2167(10) 0.070(4) Uani 1 1 d . . .
H4S1 H 0.6563 1.1543 0.1710 0.104 Uiso 1 1 calc R . .
H4S2 H 0.7965 1.0921 0.2139 0.104 Uiso 1 1 calc R . .
H4S3 H 0.6693 1.0998 0.2828 0.104 Uiso 1 1 calc R . .
C5S C -0.2711(12) 0.8210(9) 0.9412(8) 0.054(3) Uani 1 1 d . . .
H5S1 H -0.2806 0.7957 1.0109 0.081 Uiso 1 1 calc R . .
H5S2 H -0.3556 0.8454 0.9119 0.081 Uiso 1 1 calc R . .
H5S3 H -0.2375 0.8791 0.9320 0.081 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
Gd1 O15 2.254(5) 2_566 ?
Gd1 O14 2.260(5) 2_566 ?
Gd1 O3 2.305(5) . ?
Gd1 O7 2.306(5) . ?
Gd1 O2 2.422(4) . ?
Gd1 O4 2.528(5) . ?
Gd1 O1 2.557(4) 2_566 ?
Gd1 O5 2.574(4) . ?
Gd1 N1 2.965(5) . ?
Gd1 Cu2 3.2842(10) 2_566 ?
Gd1 Cu3 3.2887(12) 2_566 ?
Gd2 O12 2.249(5) . ?
Gd2 O16 2.258(5) . ?
Gd2 O3 2.305(4) . ?
Gd2 O8 2.361(6) . ?
Gd2 O2 2.428(4) . ?
Gd2 O9 2.499(5) . ?
Gd2 O10 2.501(5) . ?
Gd2 O1 2.726(4) . ?
Gd2 N2 2.907(6) . ?
Cu1 O1 1.964(4) . ?
Cu1 O1 1.964(4) 2_566 ?
Cu1 O2 1.978(4) 2_566 ?
Cu1 O2 1.978(4) . ?
Cu1 Gd1 3.1747(10) 2_566 ?
Cu1 Gd2 3.2910(9) 2_566 ?
Cu2 O15 1.907(5) . ?
Cu2 O16 1.910(5) . ?
Cu2 O1 1.932(4) . ?
Cu2 N4 1.997(6) . ?
Cu2 Gd1 3.2842(10) 2_566 ?
Cu3 O14 1.914(4) . ?
Cu3 O12 1.920(4) . ?
Cu3 O1 1.945(4) . ?
Cu3 N3 2.009(5) . ?
Cu3 Gd1 3.2887(13) 2_566 ?
O1 Gd1 2.557(4) 2_566 ?
O2 C1 1.419(8) . ?
O3 C2 1.412(9) . ?
O4 N1 1.286(8) . ?
O5 N1 1.253(7) . ?
O6 N1 1.233(7) . ?
O7 C3 1.274(9) . ?
O8 C3 1.243(10) . ?
O9 N2 1.261(8) . ?
O10 N2 1.251(8) . ?
O11 N2 1.232(8) . ?
O12 C8 1.409(8) . ?
O13 C11 1.445(9) . ?
O13 H13 0.8400 . ?
O14 C13 1.421(8) . ?
O14 Gd1 2.260(5) 2_566 ?
O15 C15 1.417(9) . ?
O15 Gd1 2.254(5) 2_566 ?
O16 C17 1.405(9) . ?
O17 C19 1.431(9) . ?
O17 H17 0.8400 . ?
O1S C3S 1.328(19) . ?
O1S C2S 1.50(3) . ?
O2S C5S 1.397(12) . ?
O2S H2S 0.8400 . ?
N3 C10 1.487(9) . ?
N3 C9 1.489(9) . ?
N3 C12 1.494(8) . ?
N4 C18 1.478(10) . ?
N4 C14 1.485(9) . ?
N4 C16 1.494(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.542(10) . ?
C4 C5 1.490(14) . ?
C4 C7 1.513(15) . ?
C4 C6 1.549(16) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.527(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.518(12) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.520(10) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.538(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.545(10) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.510(12) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C1S C2S 1.31(3) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?
C3S C4S 1.406(19) . ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
C5S H5S1 0.9800 . ?
C5S H5S2 0.9800 . ?
C5S H5S3 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
O15 Gd1 O14 104.46(17) 2_566 2_566 ?
O15 Gd1 O3 146.44(16) 2_566 . ?
O14 Gd1 O3 87.97(17) 2_566 . ?
O15 Gd1 O7 92.9(2) 2_566 . ?
O14 Gd1 O7 146.30(17) 2_566 . ?
O3 Gd1 O7 93.2(2) . . ?
O15 Gd1 O2 83.71(16) 2_566 . ?
O14 Gd1 O2 131.81(15) 2_566 . ?
O3 Gd1 O2 65.47(16) . . ?
O7 Gd1 O2 77.95(17) . . ?
O15 Gd1 O4 76.34(16) 2_566 . ?
O14 Gd1 O4 78.78(17) 2_566 . ?
O3 Gd1 O4 137.15(16) . . ?
O7 Gd1 O4 77.6(2) . . ?
O2 Gd1 O4 147.38(16) . . ?
O15 Gd1 O1 70.26(15) 2_566 2_566 ?
O14 Gd1 O1 70.38(14) 2_566 2_566 ?
O3 Gd1 O1 85.51(14) . 2_566 ?
O7 Gd1 O1 143.31(17) . 2_566 ?
O2 Gd1 O1 68.20(13) . 2_566 ?
O4 Gd1 O1 126.04(14) . 2_566 ?
O15 Gd1 O5 126.41(15) 2_566 . ?
O14 Gd1 O5 73.47(16) 2_566 . ?
O3 Gd1 O5 86.85(15) . . ?
O7 Gd1 O5 72.98(18) . . ?
O2 Gd1 O5 138.31(14) . . ?
O4 Gd1 O5 50.35(15) . . ?
O1 Gd1 O5 143.25(15) 2_566 . ?
O15 Gd1 N1 101.84(16) 2_566 . ?
O14 Gd1 N1 73.24(16) 2_566 . ?
O3 Gd1 N1 111.63(16) . . ?
O7 Gd1 N1 75.07(18) . . ?
O2 Gd1 N1 152.66(15) . . ?
O4 Gd1 N1 25.52(16) . . ?
O1 Gd1 N1 138.99(14) 2_566 . ?
O5 Gd1 N1 24.90(15) . . ?
O15 Gd1 Cu2 34.31(11) 2_566 2_566 ?
O14 Gd1 Cu2 86.63(12) 2_566 2_566 ?
O3 Gd1 Cu2 118.64(11) . 2_566 ?
O7 Gd1 Cu2 121.35(17) . 2_566 ?
O2 Gd1 Cu2 73.97(10) . 2_566 ?
O4 Gd1 Cu2 101.21(11) . 2_566 ?
O1 Gd1 Cu2 35.97(10) 2_566 2_566 ?
O5 Gd1 Cu2 147.38(10) . 2_566 ?
N1 Gd1 Cu2 124.71(11) . 2_566 ?
O15 Gd1 Cu3 84.63(13) 2_566 2_566 ?
O14 Gd1 Cu3 34.43(11) 2_566 2_566 ?
O3 Gd1 Cu3 89.23(11) . 2_566 ?
O7 Gd1 Cu3 177.43(19) . 2_566 ?
O2 Gd1 Cu3 102.49(10) . 2_566 ?
O4 Gd1 Cu3 101.04(11) . 2_566 ?
O1 Gd1 Cu3 36.20(9) 2_566 2_566 ?
O5 Gd1 Cu3 107.90(11) . 2_566 ?
N1 Gd1 Cu3 104.67(12) . 2_566 ?
Cu2 Gd1 Cu3 56.62(3) 2_566 2_566 ?
O12 Gd2 O16 93.89(18) . . ?
O12 Gd2 O3 145.52(16) . . ?
O16 Gd2 O3 91.70(18) . . ?
O12 Gd2 O8 86.3(2) . . ?
O16 Gd2 O8 150.38(18) . . ?
O3 Gd2 O8 104.8(2) . . ?
O12 Gd2 O2 85.38(15) . . ?
O16 Gd2 O2 129.90(15) . . ?
O3 Gd2 O2 65.35(15) . . ?
O8 Gd2 O2 79.68(17) . . ?
O12 Gd2 O9 131.72(16) . . ?
O16 Gd2 O9 80.25(19) . . ?
O3 Gd2 O9 82.75(16) . . ?
O8 Gd2 O9 77.7(2) . . ?
O2 Gd2 O9 134.18(17) . . ?
O12 Gd2 O10 81.13(16) . . ?
O16 Gd2 O10 75.70(18) . . ?
O3 Gd2 O10 133.08(16) . . ?
O8 Gd2 O10 75.07(19) . . ?
O2 Gd2 O10 151.99(17) . . ?
O9 Gd2 O10 50.85(17) . . ?
O12 Gd2 O1 69.61(14) . . ?
O16 Gd2 O1 67.96(14) . . ?
O3 Gd2 O1 81.20(14) . . ?
O8 Gd2 O1 137.97(18) . . ?
O2 Gd2 O1 64.98(13) . . ?
O9 Gd2 O1 143.70(17) . . ?
O10 Gd2 O1 130.67(15) . . ?
O12 Gd2 N2 106.46(17) . . ?
O16 Gd2 N2 75.36(19) . . ?
O3 Gd2 N2 107.88(17) . . ?
O8 Gd2 N2 76.2(2) . . ?
O2 Gd2 N2 152.22(18) . . ?
O9 Gd2 N2 25.56(18) . . ?
O10 Gd2 N2 25.35(18) . . ?
O1 Gd2 N2 142.52(17) . . ?
O1 Cu1 O1 180.000(1) . 2_566 ?
O1 Cu1 O2 90.29(17) . 2_566 ?
O1 Cu1 O2 89.71(17) 2_566 2_566 ?
O1 Cu1 O2 89.71(17) . . ?
O1 Cu1 O2 90.29(17) 2_566 . ?
O2 Cu1 O2 180.00(19) 2_566 . ?
O1 Cu1 Gd1 53.62(12) . 2_566 ?
O1 Cu1 Gd1 126.38(12) 2_566 2_566 ?
O2 Cu1 Gd1 49.69(12) 2_566 2_566 ?
O2 Cu1 Gd1 130.31(12) . 2_566 ?
O1 Cu1 Gd2 124.15(12) . 2_566 ?
O1 Cu1 Gd2 55.85(12) 2_566 2_566 ?
O2 Cu1 Gd2 47.20(12) 2_566 2_566 ?
O2 Cu1 Gd2 132.80(12) . 2_566 ?
Gd1 Cu1 Gd2 70.54(3) 2_566 2_566 ?
O15 Cu2 O16 172.4(2) . . ?
O15 Cu2 O1 92.77(19) . . ?
O16 Cu2 O1 94.11(19) . . ?
O15 Cu2 N4 87.0(2) . . ?
O16 Cu2 N4 86.3(2) . . ?
O1 Cu2 N4 177.5(2) . . ?
O15 Cu2 Gd1 41.76(14) . 2_566 ?
O16 Cu2 Gd1 144.85(15) . 2_566 ?
O1 Cu2 Gd1 51.04(12) . 2_566 ?
N4 Cu2 Gd1 128.75(16) . 2_566 ?
O14 Cu3 O12 164.0(2) . . ?
O14 Cu3 O1 92.48(18) . . ?
O12 Cu3 O1 95.75(18) . . ?
O14 Cu3 N3 87.1(2) . . ?
O12 Cu3 N3 85.6(2) . . ?
O1 Cu3 N3 176.1(2) . . ?
O14 Cu3 Gd1 41.90(14) . 2_566 ?
O12 Cu3 Gd1 145.98(14) . 2_566 ?
O1 Cu3 Gd1 50.95(12) . 2_566 ?
N3 Cu3 Gd1 128.09(15) . 2_566 ?
Cu2 O1 Cu3 107.05(19) . . ?
Cu2 O1 Cu1 123.9(2) . . ?
Cu3 O1 Cu1 128.9(2) . . ?
Cu2 O1 Gd1 92.99(16) . 2_566 ?
Cu3 O1 Gd1 92.85(15) . 2_566 ?
Cu1 O1 Gd1 88.20(14) . 2_566 ?
Cu2 O1 Gd2 90.23(15) . . ?
Cu3 O1 Gd2 89.02(15) . . ?
Cu1 O1 Gd2 87.56(14) . . ?
Gd1 O1 Gd2 175.63(17) 2_566 . ?
C1 O2 Cu1 117.0(4) . . ?
C1 O2 Gd1 123.6(4) . . ?
Cu1 O2 Gd1 91.80(16) . . ?
C1 O2 Gd2 121.0(3) . . ?
Cu1 O2 Gd2 96.11(18) . . ?
Gd1 O2 Gd2 100.70(15) . . ?
C2 O3 Gd1 123.5(4) . . ?
C2 O3 Gd2 122.6(4) . . ?
Gd1 O3 Gd2 108.21(19) . . ?
N1 O4 Gd1 96.6(3) . . ?
N1 O5 Gd1 95.2(3) . . ?
C3 O7 Gd1 143.5(5) . . ?
C3 O8 Gd2 127.7(5) . . ?
N2 O9 Gd2 95.6(4) . . ?
N2 O10 Gd2 95.8(4) . . ?
C8 O12 Cu3 114.7(4) . . ?
C8 O12 Gd2 139.6(4) . . ?
Cu3 O12 Gd2 105.4(2) . . ?
C11 O13 H13 109.5 . . ?
C13 O14 Cu3 112.3(4) . . ?
C13 O14 Gd1 141.7(4) . 2_566 ?
Cu3 O14 Gd1 103.67(19) . 2_566 ?
C15 O15 Cu2 112.5(4) . . ?
C15 O15 Gd1 143.5(4) . 2_566 ?
Cu2 O15 Gd1 103.9(2) . 2_566 ?
C17 O16 Cu2 113.3(4) . . ?
C17 O16 Gd2 140.2(4) . . ?
Cu2 O16 Gd2 106.6(2) . . ?
C19 O17 H17 109.5 . . ?
C3S O1S C2S 115.3(14) . . ?
C5S O2S H2S 109.5 . . ?
O6 N1 O5 122.2(5) . . ?
O6 N1 O4 120.2(5) . . ?
O5 N1 O4 117.5(5) . . ?
O6 N1 Gd1 173.8(5) . . ?
O5 N1 Gd1 59.9(3) . . ?
O4 N1 Gd1 57.9(3) . . ?
O11 N2 O10 121.1(6) . . ?
O11 N2 O9 121.5(7) . . ?
O10 N2 O9 117.4(6) . . ?
O11 N2 Gd2 176.3(7) . . ?
O10 N2 Gd2 58.9(3) . . ?
O9 N2 Gd2 58.8(3) . . ?
C10 N3 C9 113.2(5) . . ?
C10 N3 C12 112.1(5) . . ?
C9 N3 C12 112.5(6) . . ?
C10 N3 Cu3 110.9(4) . . ?
C9 N3 Cu3 103.8(4) . . ?
C12 N3 Cu3 103.6(4) . . ?
C18 N4 C14 114.7(6) . . ?
C18 N4 C16 111.4(6) . . ?
C14 N4 C16 114.2(6) . . ?
C18 N4 Cu2 109.9(5) . . ?
C14 N4 Cu2 104.0(4) . . ?
C16 N4 Cu2 101.4(4) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C2 H2A 109.5 . . ?
O3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O8 C3 O7 124.4(7) . . ?
O8 C3 C4 120.6(7) . . ?
O7 C3 C4 115.0(7) . . ?
C5 C4 C7 110.4(10) . . ?
C5 C4 C3 111.2(7) . . ?
C7 C4 C3 108.9(8) . . ?
C5 C4 C6 110.5(9) . . ?
C7 C4 C6 107.5(10) . . ?
C3 C4 C6 108.2(7) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
O12 C8 C9 108.5(5) . . ?
O12 C8 H8A 110.0 . . ?
C9 C8 H8A 110.0 . . ?
O12 C8 H8B 110.0 . . ?
C9 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N3 C9 C8 109.7(6) . . ?
N3 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N3 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N3 C10 C11 114.0(5) . . ?
N3 C10 H10A 108.8 . . ?
C11 C10 H10A 108.8 . . ?
N3 C10 H10B 108.8 . . ?
C11 C10 H10B 108.8 . . ?
H10A C10 H10B 107.6 . . ?
O13 C11 C10 112.6(6) . . ?
O13 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
O13 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N3 C12 C13 108.8(6) . . ?
N3 C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
N3 C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O14 C13 C12 109.2(5) . . ?
O14 C13 H13A 109.8 . . ?
C12 C13 H13A 109.8 . . ?
O14 C13 H13B 109.8 . . ?
C12 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
N4 C14 C15 107.8(6) . . ?
N4 C14 H14A 110.2 . . ?
C15 C14 H14A 110.2 . . ?
N4 C14 H14B 110.2 . . ?
C15 C14 H14B 110.2 . . ?
H14A C14 H14B 108.5 . . ?
O15 C15 C14 108.8(6) . . ?
O15 C15 H15A 109.9 . . ?
C14 C15 H15A 109.9 . . ?
O15 C15 H15B 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
N4 C16 C17 108.6(6) . . ?
N4 C16 H16A 110.0 . . ?
C17 C16 H16A 110.0 . . ?
N4 C16 H16B 110.0 . . ?
C17 C16 H16B 110.0 . . ?
H16A C16 H16B 108.4 . . ?
O16 C17 C16 109.9(5) . . ?
O16 C17 H17A 109.7 . . ?
C16 C17 H17A 109.7 . . ?
O16 C17 H17B 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N4 C18 C19 116.2(7) . . ?
N4 C18 H18A 108.2 . . ?
C19 C18 H18A 108.2 . . ?
N4 C18 H18B 108.2 . . ?
C19 C18 H18B 108.2 . . ?
H18A C18 H18B 107.4 . . ?
O17 C19 C18 109.5(6) . . ?
O17 C19 H19A 109.8 . . ?
C18 C19 H19A 109.8 . . ?
O17 C19 H19B 109.8 . . ?
C18 C19 H19B 109.8 . . ?
H19A C19 H19B 108.2 . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C1S C2S O1S 114(2) . . ?
C1S C2S H2S1 108.8 . . ?
O1S C2S H2S1 108.8 . . ?
C1S C2S H2S2 108.8 . . ?
O1S C2S H2S2 108.8 . . ?
H2S1 C2S H2S2 107.7 . . ?
O1S C3S C4S 114.8(13) . . ?
O1S C3S H3S1 108.6 . . ?
C4S C3S H3S1 108.6 . . ?
O1S C3S H3S2 108.6 . . ?
C4S C3S H3S2 108.6 . . ?
H3S1 C3S H3S2 107.6 . . ?
C3S C4S H4S1 109.5 . . ?
C3S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
C3S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
O2S C5S H5S1 109.5 . . ?
O2S C5S H5S2 109.5 . . ?
H5S1 C5S H5S2 109.5 . . ?
O2S C5S H5S3 109.5 . . ?
H5S1 C5S H5S3 109.5 . . ?
H5S2 C5S H5S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.931
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.931
_refine_diff_density_max         1.095
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.153

####################################################################### 
# 
# 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_Cu5Dy4final
_audit_block_doi                 10.5517/ccw4vpj
_database_code_depnum_ccdc_archive 'CCDC 809028'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/chem.201100218 2011
_audit_update_record             
;
2011-01-20 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
#TrackingRef '3 Cu5Dy4final.CIF'

#==========================================================================

_audit_creation_method           SHELXL-97
_audit_creation_date             '9 November 2005'
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C38 H82 Cu5 N8 O34 Dy4, 2(C4 H10 O), 2(C H4 O)
;
_chemical_formula_sum            'C48 H110 Cu5 Dy4 N8 O38'
_chemical_formula_weight         2375.14

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'
Cu Cu 0.3201 1.2651 '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

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

_cell_length_a                   11.080(2)
_cell_length_b                   13.820(3)
_cell_length_c                   13.990(3)
_cell_angle_alpha                78.90(3)
_cell_angle_beta                 84.10(3)
_cell_angle_gamma                69.04(3)
_cell_volume                     1961.7(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    21274
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      26.24

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1167
_exptl_absorpt_coefficient_mu    5.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7819
_exptl_absorpt_correction_T_max  0.9501
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.77512
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         '3BM1 dipole'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21274
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.17
_diffrn_reflns_theta_max         26.24
_reflns_number_total             5521
_reflns_number_gt                5220
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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 crystal was run on the Australian synchrotron in which only a
wavelength of 0.77 Aand a resolution of ~0.9 A was possible. We were
also restricted to only 360 degree phi scan. The asymmetric unit contains
half the cluster which lies upon an inversion centre as well as solvent
MeOH and Et2O molecules. All non H-atoms are refined anisotropically
and H-atoms are placed in calculated positions. The carbon atoms of the
pivalte are disordered other two positions at 65:35 occupancy. Bond (DFIX)
and thermal (ISOR) restraints are placed on the solvent Et2O
molecule and the disordered pivalate.
;

_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)+(0.0661P)²+14.3510P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5521
_refine_ls_number_parameters     507
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0393
_refine_ls_wR_factor_ref         0.1083
_refine_ls_wR_factor_gt          0.1071
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.040
_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 0.16466(3) 0.47641(2) 0.30200(2) 0.01410(12) Uani 1 1 d . . .
Dy2 Dy 0.13868(3) 0.67810(2) 0.45177(2) 0.01508(13) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.5000 0.5000 0.0125(3) Uani 1 2 d S . .
Cu2 Cu 0.10032(8) 0.57914(7) 0.68481(6) 0.0173(2) Uani 1 1 d . . .
Cu3 Cu -0.13921(8) 0.74422(6) 0.57731(6) 0.0161(2) Uani 1 1 d . . .
O1 O -0.0165(4) 0.6021(3) 0.5830(3) 0.0173(11) Uani 1 1 d . . .
O2 O 0.0053(4) 0.6059(4) 0.3844(3) 0.0156(10) Uani 1 1 d . . .
O3 O 0.2352(5) 0.5059(3) 0.4366(3) 0.0180(10) Uani 1 1 d . . .
O4 O 0.2678(5) 0.4197(4) 0.1445(4) 0.0259(12) Uani 1 1 d . . .
O5 O 0.3979(5) 0.4406(4) 0.2372(3) 0.0209(11) Uani 1 1 d . . .
O6 O 0.4733(6) 0.3797(5) 0.1028(4) 0.0355(14) Uani 1 1 d . . .
O7 O 0.1689(6) 0.6296(4) 0.2057(4) 0.0322(13) Uani 1 1 d . . .
O8 O 0.1347(6) 0.7594(4) 0.2887(3) 0.0299(13) Uani 1 1 d . . .
O9 O 0.3641(5) 0.6754(4) 0.4181(4) 0.0318(13) Uani 1 1 d . . .
O10 O 0.2240(5) 0.8216(4) 0.4518(4) 0.0268(12) Uani 1 1 d . . .
O11 O 0.4285(7) 0.8043(5) 0.4310(6) 0.0528(19) Uani 1 1 d . . .
O12 O -0.0437(5) 0.8071(4) 0.4772(3) 0.0204(11) Uani 1 1 d . . .
O13 O -0.0606(6) 0.7735(4) 0.7227(4) 0.0308(13) Uani 1 1 d . . .
H13 H -0.0947 0.7615 0.7781 0.037 Uiso 1 1 calc R . .
O14 O -0.2697(5) 0.6965(4) 0.6490(4) 0.0204(11) Uani 1 1 d . . .
O15 O 0.0005(5) 0.5171(4) 0.7797(3) 0.0202(11) Uani 1 1 d . . .
O16 O 0.2048(5) 0.6487(4) 0.6044(3) 0.0247(11) Uani 1 1 d . . .
O17 O 0.3956(7) 0.3407(5) 0.9341(4) 0.0429(16) Uani 1 1 d . . .
H17 H 0.4498 0.3176 0.9782 0.052 Uiso 1 1 calc R . .
O1S O 0.5893(15) 0.9890(11) 0.2115(13) 0.161(7) Uani 1 1 d D . .
O2S O -0.1826(7) 0.7371(6) 0.8972(5) 0.0483(17) Uani 1 1 d . . .
H2S H -0.2135 0.6889 0.9023 0.058 Uiso 1 1 calc R . .
N1 N 0.3819(6) 0.4130(5) 0.1617(4) 0.0225(14) Uani 1 1 d . . .
N2 N 0.3403(7) 0.7694(5) 0.4330(5) 0.0323(17) Uani 1 1 d . . .
N3 N -0.2638(6) 0.8910(4) 0.5795(4) 0.0208(13) Uani 1 1 d . . .
N4 N 0.2261(6) 0.5477(5) 0.7889(4) 0.0248(14) Uani 1 1 d . . .
C1 C -0.1162(7) 0.6725(6) 0.3434(5) 0.0238(16) Uani 1 1 d . . .
H1A H -0.1572 0.6297 0.3202 0.036 Uiso 1 1 calc R . .
H1B H -0.1016 0.7237 0.2887 0.036 Uiso 1 1 calc R . .
H1C H -0.1726 0.7096 0.3933 0.036 Uiso 1 1 calc R . .
C2 C 0.3540(8) 0.4403(6) 0.4810(6) 0.0285(18) Uani 1 1 d . . .
H2A H 0.3844 0.3725 0.4581 0.043 Uiso 1 1 calc R . .
H2B H 0.3403 0.4289 0.5520 0.043 Uiso 1 1 calc R . .
H2C H 0.4189 0.4743 0.4634 0.043 Uiso 1 1 calc R . .
C3 C 0.1452(7) 0.7245(6) 0.2108(5) 0.0241(17) Uani 1 1 d . A .
C4 C 0.1279(9) 0.8020(7) 0.1140(6) 0.037(2) Uani 1 1 d D . .
C5 C 0.110(2) 0.9090(11) 0.1264(11) 0.057(6) Uani 0.653(18) 1 d P A 1
H5A H 0.1062 0.9533 0.0623 0.086 Uiso 0.653(18) 1 calc PR A 1
H5B H 0.1817 0.9082 0.1619 0.086 Uiso 0.653(18) 1 calc PR A 1
H5C H 0.0283 0.9371 0.1634 0.086 Uiso 0.653(18) 1 calc PR A 1
C6 C 0.0161(18) 0.7972(13) 0.0615(12) 0.054(5) Uani 0.653(18) 1 d P A 1
H6A H 0.0086 0.8415 -0.0029 0.081 Uiso 0.653(18) 1 calc PR A 1
H6B H -0.0647 0.8225 0.0998 0.081 Uiso 0.653(18) 1 calc PR A 1
H6C H 0.0327 0.7244 0.0540 0.081 Uiso 0.653(18) 1 calc PR A 1
C7 C 0.2455(16) 0.7584(12) 0.0453(10) 0.048(4) Uani 0.653(18) 1 d PU A 1
H7A H 0.2542 0.6870 0.0382 0.072 Uiso 0.653(18) 1 calc PR A 1
H7B H 0.3241 0.7569 0.0729 0.072 Uiso 0.653(18) 1 calc PR A 1
H7C H 0.2329 0.8036 -0.0187 0.072 Uiso 0.653(18) 1 calc PR A 1
C8 C -0.1041(7) 0.9176(5) 0.4508(5) 0.0228(16) Uani 1 1 d . . .
H8A H -0.0931 0.9386 0.3796 0.027 Uiso 1 1 calc R . .
H8B H -0.0631 0.9543 0.4842 0.027 Uiso 1 1 calc R . .
C9 C -0.2467(8) 0.9485(6) 0.4797(6) 0.0282(18) Uani 1 1 d . . .
H9A H -0.2841 1.0252 0.4792 0.034 Uiso 1 1 calc R . .
H9B H -0.2927 0.9309 0.4322 0.034 Uiso 1 1 calc R . .
C10 C -0.2318(9) 0.9357(6) 0.6584(6) 0.0314(19) Uani 1 1 d . . .
H10A H -0.2913 0.9296 0.7153 0.038 Uiso 1 1 calc R . .
H10B H -0.2483 1.0115 0.6352 0.038 Uiso 1 1 calc R . .
C11 C -0.0959(9) 0.8851(7) 0.6914(6) 0.036(2) Uani 1 1 d . . .
H11A H -0.0362 0.8989 0.6372 0.043 Uiso 1 1 calc R . .
H11B H -0.0857 0.9175 0.7460 0.043 Uiso 1 1 calc R . .
C12 C -0.3919(8) 0.8777(6) 0.5966(6) 0.0315(19) Uani 1 1 d . . .
H12A H -0.4218 0.8702 0.5351 0.038 Uiso 1 1 calc R . .
H12B H -0.4561 0.9402 0.6199 0.038 Uiso 1 1 calc R . .
C13 C -0.3796(8) 0.7802(6) 0.6725(6) 0.0281(18) Uani 1 1 d . . .
H13A H -0.3713 0.7944 0.7378 0.034 Uiso 1 1 calc R . .
H13B H -0.4580 0.7613 0.6741 0.034 Uiso 1 1 calc R . .
C14 C 0.1460(8) 0.5407(7) 0.8821(5) 0.0291(18) Uani 1 1 d . . .
H14A H 0.0902 0.6118 0.8936 0.035 Uiso 1 1 calc R . .
H14B H 0.2027 0.5060 0.9381 0.035 Uiso 1 1 calc R . .
C15 C 0.0636(8) 0.4765(7) 0.8702(5) 0.0277(18) Uani 1 1 d . . .
H15A H 0.1189 0.4020 0.8716 0.033 Uiso 1 1 calc R . .
H15B H -0.0016 0.4802 0.9246 0.033 Uiso 1 1 calc R . .
C16 C 0.2619(8) 0.6444(7) 0.7668(5) 0.0295(18) Uani 1 1 d . . .
H16A H 0.3371 0.6347 0.8050 0.035 Uiso 1 1 calc R . .
H16B H 0.1886 0.7052 0.7849 0.035 Uiso 1 1 calc R . .
C17 C 0.2955(9) 0.6649(7) 0.6583(5) 0.034(2) Uani 1 1 d . . .
H17A H 0.2942 0.7380 0.6388 0.041 Uiso 1 1 calc R . .
H17B H 0.3836 0.6168 0.6442 0.041 Uiso 1 1 calc R . .
C18 C 0.3372(9) 0.4512(7) 0.7783(6) 0.035(2) Uani 1 1 d . . .
H18A H 0.3834 0.4646 0.7155 0.042 Uiso 1 1 calc R . .
H18B H 0.3031 0.3951 0.7740 0.042 Uiso 1 1 calc R . .
C19 C 0.4354(9) 0.4096(7) 0.8580(6) 0.035(2) Uani 1 1 d . . .
H19A H 0.5216 0.3712 0.8307 0.042 Uiso 1 1 calc R . .
H19B H 0.4418 0.4689 0.8846 0.042 Uiso 1 1 calc R . .
C5' C 0.222(3) 0.862(2) 0.121(2) 0.052(8) Uani 0.347(18) 1 d PU A 2
H5'1 H 0.3119 0.8135 0.1194 0.079 Uiso 0.347(18) 1 calc PR A 2
H5'2 H 0.2038 0.8906 0.1817 0.079 Uiso 0.347(18) 1 calc PR A 2
H5'3 H 0.2103 0.9198 0.0653 0.079 Uiso 0.347(18) 1 calc PR A 2
C6' C -0.007(2) 0.879(3) 0.126(3) 0.090(14) Uani 0.347(18) 1 d PDU A 2
H6'1 H -0.0353 0.9227 0.0622 0.135 Uiso 0.347(18) 1 calc PR A 2
H6'2 H -0.0069 0.9248 0.1715 0.135 Uiso 0.347(18) 1 calc PR A 2
H6'3 H -0.0662 0.8413 0.1505 0.135 Uiso 0.347(18) 1 calc PR A 2
C7' C 0.139(4) 0.765(3) 0.029(2) 0.063(10) Uani 0.347(18) 1 d PU A 2
H7'1 H 0.0565 0.7584 0.0167 0.095 Uiso 0.347(18) 1 calc PR A 2
H7'2 H 0.2072 0.6956 0.0334 0.095 Uiso 0.347(18) 1 calc PR A 2
H7'3 H 0.1604 0.8135 -0.0250 0.095 Uiso 0.347(18) 1 calc PR A 2
C1S C 0.479(2) 0.885(2) 0.175(2) 0.188(13) Uani 1 1 d D . .
H1S1 H 0.4245 0.8763 0.2335 0.282 Uiso 1 1 calc R . .
H1S2 H 0.4937 0.8273 0.1389 0.282 Uiso 1 1 calc R . .
H1S3 H 0.4347 0.9522 0.1334 0.282 Uiso 1 1 calc R . .
C2S C 0.604(2) 0.8845(15) 0.203(2) 0.203(16) Uani 1 1 d D . .
H2S1 H 0.6296 0.8373 0.2663 0.244 Uiso 1 1 calc R . .
H2S2 H 0.6726 0.8590 0.1533 0.244 Uiso 1 1 calc R . .
C3S C 0.706(2) 1.0061(17) 0.1869(17) 0.171(12) Uani 1 1 d D . .
H3S1 H 0.7231 1.0102 0.1156 0.205 Uiso 1 1 calc R . .
H3S2 H 0.7771 0.9456 0.2194 0.205 Uiso 1 1 calc R . .
C4S C 0.7070(15) 1.1038(11) 0.2154(12) 0.096(5) Uani 1 1 d D . .
H4S1 H 0.6530 1.1649 0.1717 0.144 Uiso 1 1 calc R . .
H4S2 H 0.7958 1.1039 0.2108 0.144 Uiso 1 1 calc R . .
H4S3 H 0.6728 1.1072 0.2826 0.144 Uiso 1 1 calc R . .
C5S C -0.2659(16) 0.8169(10) 0.9431(10) 0.086(4) Uani 1 1 d . . .
H5S1 H -0.2760 0.7897 1.0124 0.128 Uiso 1 1 calc R . .
H5S2 H -0.3503 0.8441 0.9132 0.128 Uiso 1 1 calc R . .
H5S3 H -0.2305 0.8736 0.9364 0.128 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 O15 2.222(5) 2_566 ?
Dy1 O14 2.254(5) 2_566 ?
Dy1 O3 2.269(5) . ?
Dy1 O7 2.293(5) . ?
Dy1 O2 2.402(5) . ?
Dy1 O4 2.506(5) . ?
Dy1 O1 2.553(4) 2_566 ?
Dy1 O5 2.554(5) . ?
Dy1 Cu2 3.2695(11) 2_566 ?
Dy1 Cu3 3.2806(13) 2_566 ?
Dy2 O12 2.215(5) . ?
Dy2 O16 2.245(5) . ?
Dy2 O3 2.275(5) . ?
Dy2 O8 2.338(5) . ?
Dy2 O2 2.402(5) . ?
Dy2 O9 2.482(6) . ?
Dy2 O10 2.484(5) . ?
Dy2 O1 2.708(4) . ?
Dy2 Cu3 3.3004(14) . ?
Dy2 Cu2 3.3308(12) . ?
Cu1 O1 1.943(4) 2_566 ?
Cu1 O1 1.943(4) . ?
Cu1 O2 1.973(4) 2_566 ?
Cu1 O2 1.973(4) . ?
Cu1 Dy1 3.1609(10) 2_566 ?
Cu1 Dy2 3.2752(9) 2_566 ?
Cu2 O16 1.908(5) . ?
Cu2 O15 1.913(5) . ?
Cu2 O1 1.927(5) . ?
Cu2 N4 1.999(6) . ?
Cu2 Dy1 3.2695(11) 2_566 ?
Cu3 O14 1.914(5) . ?
Cu3 O12 1.929(5) . ?
Cu3 O1 1.940(4) . ?
Cu3 N3 2.008(6) . ?
Cu3 Dy1 3.2806(13) 2_566 ?
O1 Dy1 2.553(4) 2_566 ?
O2 C1 1.433(9) . ?
O3 C2 1.428(9) . ?
O4 N1 1.278(9) . ?
O5 N1 1.239(8) . ?
O6 N1 1.248(8) . ?
O7 C3 1.257(9) . ?
O8 C3 1.254(9) . ?
O9 N2 1.284(9) . ?
O10 N2 1.261(9) . ?
O11 N2 1.231(9) . ?
O12 C8 1.422(8) . ?
O13 C11 1.438(10) . ?
O13 H13 0.8400 . ?
O14 C13 1.409(9) . ?
O14 Dy1 2.254(5) 2_566 ?
O15 C15 1.426(9) . ?
O15 Dy1 2.222(5) 2_566 ?
O16 C17 1.417(10) . ?
O17 C19 1.431(10) . ?
O17 H17 0.8400 . ?
O1S C3S 1.396(10) . ?
O1S C2S 1.419(10) . ?
O2S C5S 1.379(14) . ?
O2S H2S 0.8400 . ?
N3 C12 1.485(11) . ?
N3 C10 1.492(10) . ?
N3 C9 1.498(9) . ?
N4 C18 1.476(11) . ?
N4 C16 1.495(10) . ?
N4 C14 1.507(9) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.539(11) . ?
C4 C7' 1.36(4) . ?
C4 C5 1.461(17) . ?
C4 C6' 1.509(10) . ?
C4 C6 1.531(18) . ?
C4 C7 1.546(17) . ?
C4 C5' 1.57(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.515(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.495(13) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.519(11) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.521(11) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.522(11) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.521(12) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C5' H5'1 0.9800 . ?
C5' H5'2 0.9800 . ?
C5' H5'3 0.9800 . ?
C6' H6'1 0.9800 . ?
C6' H6'2 0.9800 . ?
C6' H6'3 0.9800 . ?
C7' H7'1 0.9800 . ?
C7' H7'2 0.9800 . ?
C7' H7'3 0.9800 . ?
C1S C2S 1.484(10) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?
C3S C4S 1.482(10) . ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
C5S H5S1 0.9800 . ?
C5S H5S2 0.9800 . ?
C5S H5S3 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
O15 Dy1 O14 104.51(18) 2_566 2_566 ?
O15 Dy1 O3 148.33(17) 2_566 . ?
O14 Dy1 O3 87.83(17) 2_566 . ?
O15 Dy1 O7 89.8(2) 2_566 . ?
O14 Dy1 O7 147.22(19) 2_566 . ?
O3 Dy1 O7 95.25(19) . . ?
O15 Dy1 O2 85.02(17) 2_566 . ?
O14 Dy1 O2 131.27(16) 2_566 . ?
O3 Dy1 O2 65.56(16) . . ?
O7 Dy1 O2 78.45(17) . . ?
O15 Dy1 O4 76.27(18) 2_566 . ?
O14 Dy1 O4 78.58(17) 2_566 . ?
O3 Dy1 O4 135.29(18) . . ?
O7 Dy1 O4 76.40(18) . . ?
O2 Dy1 O4 148.51(16) . . ?
O15 Dy1 O1 70.63(16) 2_566 2_566 ?
O14 Dy1 O1 70.42(16) 2_566 2_566 ?
O3 Dy1 O1 86.98(16) . 2_566 ?
O7 Dy1 O1 142.25(18) . 2_566 ?
O2 Dy1 O1 68.24(14) . 2_566 ?
O4 Dy1 O1 126.15(16) . 2_566 ?
O15 Dy1 O5 126.45(16) 2_566 . ?
O14 Dy1 O5 74.06(17) 2_566 . ?
O3 Dy1 O5 84.79(16) . . ?
O7 Dy1 O5 73.74(18) . . ?
O2 Dy1 O5 136.91(15) . . ?
O4 Dy1 O5 50.56(17) . . ?
O1 Dy1 O5 143.77(15) 2_566 . ?
O15 Dy1 Cu2 34.55(12) 2_566 2_566 ?
O14 Dy1 Cu2 87.18(13) 2_566 2_566 ?
O3 Dy1 Cu2 120.09(12) . 2_566 ?
O7 Dy1 Cu2 118.39(16) . 2_566 ?
O2 Dy1 Cu2 74.18(11) . 2_566 ?
O4 Dy1 Cu2 101.73(13) . 2_566 ?
O1 Dy1 Cu2 36.08(10) 2_566 2_566 ?
O5 Dy1 Cu2 148.60(11) . 2_566 ?
O15 Dy1 Cu3 84.38(13) 2_566 2_566 ?
O14 Dy1 Cu3 34.55(12) 2_566 2_566 ?
O3 Dy1 Cu3 90.54(12) . 2_566 ?
O7 Dy1 Cu3 173.96(15) . 2_566 ?
O2 Dy1 Cu3 102.48(11) . 2_566 ?
O4 Dy1 Cu3 100.65(12) . 2_566 ?
O1 Dy1 Cu3 36.21(10) 2_566 2_566 ?
O5 Dy1 Cu3 108.61(12) . 2_566 ?
Cu2 Dy1 Cu3 56.71(4) 2_566 2_566 ?
O12 Dy2 O16 94.58(19) . . ?
O12 Dy2 O3 147.02(18) . . ?
O16 Dy2 O3 92.51(18) . . ?
O12 Dy2 O8 87.71(19) . . ?
O16 Dy2 O8 151.24(18) . . ?
O3 Dy2 O8 101.07(18) . . ?
O12 Dy2 O2 85.66(17) . . ?
O16 Dy2 O2 130.04(17) . . ?
O3 Dy2 O2 65.46(17) . . ?
O8 Dy2 O2 78.71(17) . . ?
O12 Dy2 O9 131.41(18) . . ?
O16 Dy2 O9 79.66(19) . . ?
O3 Dy2 O9 81.55(18) . . ?
O8 Dy2 O9 77.5(2) . . ?
O2 Dy2 O9 134.18(17) . . ?
O12 Dy2 O10 79.91(18) . . ?
O16 Dy2 O10 76.60(18) . . ?
O3 Dy2 O10 133.02(18) . . ?
O8 Dy2 O10 75.60(18) . . ?
O2 Dy2 O10 150.89(16) . . ?
O9 Dy2 O10 51.69(18) . . ?
O12 Dy2 O1 70.19(15) . . ?
O16 Dy2 O1 68.28(16) . . ?
O3 Dy2 O1 82.78(15) . . ?
O8 Dy2 O1 138.15(17) . . ?
O2 Dy2 O1 64.96(14) . . ?
O9 Dy2 O1 143.47(16) . . ?
O10 Dy2 O1 130.91(15) . . ?
O12 Dy2 Cu3 34.30(12) . . ?
O16 Dy2 Cu3 78.28(14) . . ?
O3 Dy2 Cu3 117.35(13) . . ?
O8 Dy2 Cu3 116.17(15) . . ?
O2 Dy2 Cu3 74.43(11) . . ?
O9 Dy2 Cu3 151.37(14) . . ?
O10 Dy2 Cu3 105.08(13) . . ?
O1 Dy2 Cu3 36.00(9) . . ?
O12 Dy2 Cu2 85.10(13) . . ?
O16 Dy2 Cu2 33.34(13) . . ?
O3 Dy2 Cu2 83.36(12) . . ?
O8 Dy2 Cu2 172.10(15) . . ?
O2 Dy2 Cu2 97.45(11) . . ?
O9 Dy2 Cu2 109.84(13) . . ?
O10 Dy2 Cu2 106.26(13) . . ?
O1 Dy2 Cu2 35.36(10) . . ?
Cu3 Dy2 Cu2 55.95(4) . . ?
O1 Cu1 O1 180.00(17) 2_566 . ?
O1 Cu1 O2 89.47(18) 2_566 2_566 ?
O1 Cu1 O2 90.53(18) . 2_566 ?
O1 Cu1 O2 90.53(18) 2_566 . ?
O1 Cu1 O2 89.47(18) . . ?
O2 Cu1 O2 180.000(1) 2_566 . ?
O1 Cu1 Dy1 126.17(13) 2_566 2_566 ?
O1 Cu1 Dy1 53.83(13) . 2_566 ?
O2 Cu1 Dy1 49.40(13) 2_566 2_566 ?
O2 Cu1 Dy1 130.60(13) . 2_566 ?
O1 Cu1 Dy2 55.71(13) 2_566 2_566 ?
O1 Cu1 Dy2 124.29(13) . 2_566 ?
O2 Cu1 Dy2 46.79(13) 2_566 2_566 ?
O2 Cu1 Dy2 133.21(13) . 2_566 ?
Dy1 Cu1 Dy2 70.46(3) 2_566 2_566 ?
O16 Cu2 O15 172.1(2) . . ?
O16 Cu2 O1 94.0(2) . . ?
O15 Cu2 O1 92.5(2) . . ?
O16 Cu2 N4 86.5(2) . . ?
O15 Cu2 N4 87.3(2) . . ?
O1 Cu2 N4 177.0(2) . . ?
O16 Cu2 Dy1 145.00(16) . 2_566 ?
O15 Cu2 Dy1 41.21(14) . 2_566 ?
O1 Cu2 Dy1 51.26(13) . 2_566 ?
N4 Cu2 Dy1 128.43(18) . 2_566 ?
O16 Cu2 Dy2 40.29(15) . . ?
O15 Cu2 Dy2 146.73(15) . . ?
O1 Cu2 Dy2 54.39(13) . . ?
N4 Cu2 Dy2 125.67(18) . . ?
Dy1 Cu2 Dy2 105.61(4) 2_566 . ?
O14 Cu3 O12 163.8(2) . . ?
O14 Cu3 O1 92.42(19) . . ?
O12 Cu3 O1 95.3(2) . . ?
O14 Cu3 N3 86.9(2) . . ?
O12 Cu3 N3 86.2(2) . . ?
O1 Cu3 N3 176.6(2) . . ?
O14 Cu3 Dy1 41.90(14) . 2_566 ?
O12 Cu3 Dy1 145.65(14) . 2_566 ?
O1 Cu3 Dy1 51.01(13) . 2_566 ?
N3 Cu3 Dy1 127.85(17) . 2_566 ?
O14 Cu3 Dy2 146.08(14) . . ?
O12 Cu3 Dy2 40.32(14) . . ?
O1 Cu3 Dy2 55.12(13) . . ?
N3 Cu3 Dy2 126.08(17) . . ?
Dy1 Cu3 Dy2 106.05(4) 2_566 . ?
Cu2 O1 Cu3 107.1(2) . . ?
Cu2 O1 Cu1 123.9(2) . . ?
Cu3 O1 Cu1 128.9(2) . . ?
Cu2 O1 Dy1 92.66(17) . 2_566 ?
Cu3 O1 Dy1 92.78(17) . 2_566 ?
Cu1 O1 Dy1 88.25(16) . 2_566 ?
Cu2 O1 Dy2 90.26(17) . . ?
Cu3 O1 Dy2 88.89(16) . . ?
Cu1 O1 Dy2 87.92(15) . . ?
Dy1 O1 Dy2 176.06(18) 2_566 . ?
C1 O2 Cu1 117.0(4) . . ?
C1 O2 Dy1 122.9(4) . . ?
Cu1 O2 Dy1 92.01(17) . . ?
C1 O2 Dy2 120.8(4) . . ?
Cu1 O2 Dy2 96.45(17) . . ?
Dy1 O2 Dy2 101.27(17) . . ?
C2 O3 Dy1 123.5(4) . . ?
C2 O3 Dy2 122.8(4) . . ?
Dy1 O3 Dy2 109.62(19) . . ?
N1 O4 Dy1 96.1(4) . . ?
N1 O5 Dy1 94.9(4) . . ?
C3 O7 Dy1 140.3(5) . . ?
C3 O8 Dy2 131.6(5) . . ?
N2 O9 Dy2 95.5(4) . . ?
N2 O10 Dy2 96.1(4) . . ?
C8 O12 Cu3 113.4(4) . . ?
C8 O12 Dy2 140.9(4) . . ?
Cu3 O12 Dy2 105.4(2) . . ?
C11 O13 H13 109.5 . . ?
C13 O14 Cu3 112.3(4) . . ?
C13 O14 Dy1 141.4(4) . 2_566 ?
Cu3 O14 Dy1 103.5(2) . 2_566 ?
C15 O15 Cu2 111.4(4) . . ?
C15 O15 Dy1 144.0(5) . 2_566 ?
Cu2 O15 Dy1 104.2(2) . 2_566 ?
C17 O16 Cu2 112.5(4) . . ?
C17 O16 Dy2 141.1(4) . . ?
Cu2 O16 Dy2 106.4(2) . . ?
C19 O17 H17 109.5 . . ?
C3S O1S C2S 109.8(15) . . ?
C5S O2S H2S 109.5 . . ?
O5 N1 O6 121.9(7) . . ?
O5 N1 O4 118.2(6) . . ?
O6 N1 O4 119.9(6) . . ?
O11 N2 O10 122.7(7) . . ?
O11 N2 O9 120.7(7) . . ?
O10 N2 O9 116.6(6) . . ?
C12 N3 C10 112.6(6) . . ?
C12 N3 C9 113.1(6) . . ?
C10 N3 C9 112.9(6) . . ?
C12 N3 Cu3 103.7(4) . . ?
C10 N3 Cu3 110.1(5) . . ?
C9 N3 Cu3 103.7(4) . . ?
C18 N4 C16 112.7(7) . . ?
C18 N4 C14 114.7(6) . . ?
C16 N4 C14 113.6(6) . . ?
C18 N4 Cu2 110.3(5) . . ?
C16 N4 Cu2 100.5(4) . . ?
C14 N4 Cu2 103.6(5) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C2 H2A 109.5 . . ?
O3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O8 C3 O7 124.6(7) . . ?
O8 C3 C4 118.5(7) . . ?
O7 C3 C4 116.9(7) . . ?
C7' C4 C5 127.8(17) . . ?
C7' C4 C6' 109(3) . . ?
C5 C4 C6' 60(2) . . ?
C7' C4 C6 54.4(18) . . ?
C5 C4 C6 112.1(12) . . ?
C6' C4 C6 60(2) . . ?
C7' C4 C3 119.0(16) . . ?
C5 C4 C3 113.1(9) . . ?
C6' C4 C3 103.1(17) . . ?
C6 C4 C3 108.4(9) . . ?
C7' C4 C7 48.1(17) . . ?
C5 C4 C7 111.9(11) . . ?
C6' C4 C7 147.8(19) . . ?
C6 C4 C7 102.5(11) . . ?
C3 C4 C7 108.2(8) . . ?
C7' C4 C5' 115(2) . . ?
C5 C4 C5' 45.9(14) . . ?
C6' C4 C5' 106(2) . . ?
C6 C4 C5' 147.3(14) . . ?
C3 C4 C5' 103.4(13) . . ?
C7 C4 C5' 73.8(15) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
O12 C8 C9 109.4(6) . . ?
O12 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
O12 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
N3 C9 C8 109.6(6) . . ?
N3 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N3 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N3 C10 C11 115.2(6) . . ?
N3 C10 H10A 108.5 . . ?
C11 C10 H10A 108.5 . . ?
N3 C10 H10B 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
O13 C11 C10 112.7(7) . . ?
O13 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
O13 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
N3 C12 C13 108.9(7) . . ?
N3 C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
N3 C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O14 C13 C12 109.4(6) . . ?
O14 C13 H13A 109.8 . . ?
C12 C13 H13A 109.8 . . ?
O14 C13 H13B 109.8 . . ?
C12 C13 H13B 109.8 . . ?
H13A C13 H13B 108.2 . . ?
N4 C14 C15 106.9(6) . . ?
N4 C14 H14A 110.3 . . ?
C15 C14 H14A 110.3 . . ?
N4 C14 H14B 110.3 . . ?
C15 C14 H14B 110.3 . . ?
H14A C14 H14B 108.6 . . ?
O15 C15 C14 109.4(6) . . ?
O15 C15 H15A 109.8 . . ?
C14 C15 H15A 109.8 . . ?
O15 C15 H15B 109.8 . . ?
C14 C15 H15B 109.8 . . ?
H15A C15 H15B 108.3 . . ?
N4 C16 C17 108.7(6) . . ?
N4 C16 H16A 109.9 . . ?
C17 C16 H16A 109.9 . . ?
N4 C16 H16B 109.9 . . ?
C17 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
O16 C17 C16 109.7(6) . . ?
O16 C17 H17A 109.7 . . ?
C16 C17 H17A 109.7 . . ?
O16 C17 H17B 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N4 C18 C19 117.1(7) . . ?
N4 C18 H18A 108.0 . . ?
C19 C18 H18A 108.0 . . ?
N4 C18 H18B 108.0 . . ?
C19 C18 H18B 108.0 . . ?
H18A C18 H18B 107.3 . . ?
O17 C19 C18 109.4(7) . . ?
O17 C19 H19A 109.8 . . ?
C18 C19 H19A 109.8 . . ?
O17 C19 H19B 109.8 . . ?
C18 C19 H19B 109.8 . . ?
H19A C19 H19B 108.2 . . ?
C4 C5' H5'1 109.5 . . ?
C4 C5' H5'2 109.5 . . ?
H5'1 C5' H5'2 109.5 . . ?
C4 C5' H5'3 109.5 . . ?
H5'1 C5' H5'3 109.5 . . ?
H5'2 C5' H5'3 109.5 . . ?
C4 C6' H6'1 109.5 . . ?
C4 C6' H6'2 109.5 . . ?
H6'1 C6' H6'2 109.5 . . ?
C4 C6' H6'3 109.5 . . ?
H6'1 C6' H6'3 109.5 . . ?
H6'2 C6' H6'3 109.5 . . ?
C4 C7' H7'1 109.5 . . ?
C4 C7' H7'2 109.5 . . ?
H7'1 C7' H7'2 109.5 . . ?
C4 C7' H7'3 109.5 . . ?
H7'1 C7' H7'3 109.5 . . ?
H7'2 C7' H7'3 109.5 . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
O1S C2S C1S 107.7(17) . . ?
O1S C2S H2S1 110.2 . . ?
C1S C2S H2S1 110.2 . . ?
O1S C2S H2S2 110.2 . . ?
C1S C2S H2S2 110.2 . . ?
H2S1 C2S H2S2 108.5 . . ?
O1S C3S C4S 112.8(15) . . ?
O1S C3S H3S1 109.0 . . ?
C4S C3S H3S1 109.0 . . ?
O1S C3S H3S2 109.0 . . ?
C4S C3S H3S2 109.0 . . ?
H3S1 C3S H3S2 107.8 . . ?
C3S C4S H4S1 109.5 . . ?
C3S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
C3S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
O2S C5S H5S1 109.5 . . ?
O2S C5S H5S2 109.5 . . ?
H5S1 C5S H5S2 109.5 . . ?
O2S C5S H5S3 109.5 . . ?
H5S1 C5S H5S3 109.5 . . ?
H5S2 C5S H5S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.906
_diffrn_reflns_theta_full        26.24
_diffrn_measured_fraction_theta_full 0.906
_refine_diff_density_max         1.498
_refine_diff_density_min         -1.530
_refine_diff_density_rms         0.184
####################################################################### 
# 
# 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_Cu5Ho4final
_audit_block_doi                 10.5517/ccw4vqk
_database_code_depnum_ccdc_archive 'CCDC 809029'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/chem.201100218 2011
_audit_update_record             
;
2011-01-20 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
#TrackingRef '4 Cu5Ho4final.CIF'

#==========================================================================

_audit_creation_method           SHELXL-97
_audit_creation_date             '9 November 2005'
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C38 H82 Cu5 Ho4 N8 O34, 2(C4 H10 O), 2(C H4 O)
;
_chemical_formula_sum            'C48 H110 Cu5 Ho4 N8 O38'
_chemical_formula_weight         2384.86

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 '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

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

_cell_length_a                   11.087(2)
_cell_length_b                   13.803(3)
_cell_length_c                   13.985(3)
_cell_angle_alpha                78.94(3)
_cell_angle_beta                 84.10(3)
_cell_angle_gamma                69.05(3)
_cell_volume                     1960.3(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    24425
_cell_measurement_theta_min      2.00
_cell_measurement_theta_max      25.00

_exptl_crystal_description       blue
_exptl_crystal_colour            needle
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1171
_exptl_absorpt_coefficient_mu    5.403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71253
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         '3BM1 dipole'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_measurement_device_type  synchrotron
_diffrn_measurement_method       'scans in phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            24425
_diffrn_reflns_av_R_equivalents  0.1413
_diffrn_reflns_av_sigmaI/netI    0.1215
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6300
_reflns_number_gt                6093
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Blu-Ice (McPhillips et al, 2002)'
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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 crystal was run on the Australian synchrotron in which We were
restricted to only one 360 degree phi scan. The asymmetric unit contains
half the cluster which lies upon an inversion centre as well as solvent
MeOH and Et2O molecules. All non H-atoms are refined anisotropically
and H-atoms are placed in calculated positions. The carbon atoms of the
pivalte are disordered other two positions at 50:50 occupancy. Bond (DFIX)
and thermal (ISOR) restraints are placed on the solvent Et2O
molecule and the disordered pivalate.
;

_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)+(0.0601P)²+17.9534P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6300
_refine_ls_number_parameters     506
_refine_ls_number_restraints     52
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.1685
_refine_ls_wR_factor_gt          0.1676
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.080
_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
Ho1 Ho 1.16386(3) 0.97650(3) 0.30234(3) 0.01160(17) Uani 1 1 d . . .
Ho2 Ho 1.13953(3) 1.17673(3) 0.45208(3) 0.01296(17) Uani 1 1 d . . .
Cu1 Cu 1.0000 1.0000 0.5000 0.0093(3) Uani 1 2 d S . .
Cu2 Cu 1.10137(9) 1.07769(8) 0.68466(7) 0.0148(3) Uani 1 1 d . . .
Cu3 Cu 0.86215(9) 1.24360(7) 0.57726(7) 0.0135(2) Uani 1 1 d . . .
O1 O 0.9833(5) 1.1017(4) 0.5833(4) 0.0143(12) Uani 1 1 d . . .
O2 O 1.0070(5) 1.1058(4) 0.3843(4) 0.0141(12) Uani 1 1 d . . .
O3 O 1.2351(5) 1.0048(5) 0.4372(4) 0.0180(13) Uani 1 1 d . . .
O4 O 1.2661(6) 0.9201(5) 0.1457(5) 0.0203(13) Uani 1 1 d . . .
O5 O 1.3952(6) 0.9414(5) 0.2389(5) 0.0216(14) Uani 1 1 d . . .
O6 O 1.4701(7) 0.8830(7) 0.1033(5) 0.0389(19) Uani 1 1 d . . .
O7 O 1.1677(7) 1.1294(5) 0.2058(5) 0.0320(17) Uani 1 1 d . . .
O8 O 1.1376(7) 1.2552(6) 0.2907(5) 0.0287(15) Uani 1 1 d . . .
O9 O 1.3632(6) 1.1740(5) 0.4189(6) 0.0329(17) Uani 1 1 d . . .
O10 O 1.2241(6) 1.3198(5) 0.4524(5) 0.0250(14) Uani 1 1 d . . .
O11 O 1.4262(8) 1.3023(7) 0.4292(9) 0.063(3) Uani 1 1 d . . .
O12 O 0.9576(6) 1.3057(4) 0.4765(4) 0.0180(12) Uani 1 1 d . . .
O13 O 0.9416(7) 1.2739(5) 0.7209(6) 0.0313(16) Uani 1 1 d . . .
H13 H 0.8932 1.2607 0.7680 0.038 Uiso 1 1 calc R . .
O14 O 0.7336(5) 1.1953(5) 0.6501(5) 0.0179(12) Uani 1 1 d . . .
O15 O 1.0007(6) 1.0168(5) 0.7797(4) 0.0195(13) Uani 1 1 d . . .
O16 O 1.2067(6) 1.1456(6) 0.6039(5) 0.0248(14) Uani 1 1 d . . .
O17 O 1.3966(9) 0.8406(7) 0.9346(6) 0.044(2) Uani 1 1 d . . .
H17 H 1.4508 0.8184 0.9786 0.053 Uiso 1 1 calc R . .
O1S O 1.595(2) 1.4838(18) 0.2196(17) 0.154(8) Uani 1 1 d DU . .
O2S O 0.8198(10) 1.2351(8) 0.8979(7) 0.052(2) Uani 1 1 d . . .
H2S H 0.8071 1.1788 0.9221 0.062 Uiso 1 1 calc R . .
N1 N 1.3794(7) 0.9151(6) 0.1618(6) 0.0212(17) Uani 1 1 d . . .
N2 N 1.3397(8) 1.2682(7) 0.4333(7) 0.033(2) Uani 1 1 d . . .
N3 N 0.7387(8) 1.3902(6) 0.5786(6) 0.0243(17) Uani 1 1 d . . .
N4 N 1.2270(8) 1.0455(7) 0.7893(6) 0.0255(17) Uani 1 1 d . . .
C1 C 0.8852(8) 1.1730(7) 0.3428(7) 0.0210(19) Uani 1 1 d . . .
H1A H 0.8295 1.1315 0.3433 0.031 Uiso 1 1 calc R . .
H1B H 0.9003 1.2041 0.2756 0.031 Uiso 1 1 calc R . .
H1C H 0.8430 1.2292 0.3814 0.031 Uiso 1 1 calc R . .
C2 C 1.3513(9) 0.9391(7) 0.4808(7) 0.022(2) Uani 1 1 d . . .
H2A H 1.3338 0.9152 0.5497 0.033 Uiso 1 1 calc R . .
H2B H 1.4107 0.9783 0.4757 0.033 Uiso 1 1 calc R . .
H2C H 1.3905 0.8781 0.4476 0.033 Uiso 1 1 calc R . .
C3 C 1.1466(9) 1.2223(7) 0.2127(7) 0.025(2) Uani 1 1 d . A .
C4 C 1.1276(13) 1.3031(9) 0.1153(8) 0.040(3) Uani 1 1 d . . .
C5 C 1.118(3) 1.4075(19) 0.1316(19) 0.052(7) Uani 0.50 1 d P A 1
H5A H 1.1999 1.4039 0.1548 0.078 Uiso 0.50 1 calc PR A 1
H5B H 1.0487 1.4311 0.1806 0.078 Uiso 0.50 1 calc PR A 1
H5C H 1.0980 1.4574 0.0703 0.078 Uiso 0.50 1 calc PR A 1
C6 C 1.014(3) 1.296(2) 0.067(2) 0.063(9) Uani 0.50 1 d P A 1
H6A H 0.9997 1.3440 0.0043 0.094 Uiso 0.50 1 calc PR A 1
H6B H 0.9364 1.3167 0.1094 0.094 Uiso 0.50 1 calc PR A 1
H6C H 1.0338 1.2241 0.0564 0.094 Uiso 0.50 1 calc PR A 1
C7 C 1.250(4) 1.259(2) 0.049(2) 0.069(10) Uani 0.50 1 d P A 1
H7A H 1.2569 1.1891 0.0377 0.103 Uiso 0.50 1 calc PR A 1
H7B H 1.3273 1.2538 0.0804 0.103 Uiso 0.50 1 calc PR A 1
H7C H 1.2423 1.3064 -0.0141 0.103 Uiso 0.50 1 calc PR A 1
C8 C 0.9007(9) 1.4143(7) 0.4511(7) 0.024(2) Uani 1 1 d . . .
H8A H 0.9133 1.4356 0.3801 0.029 Uiso 1 1 calc R . .
H8B H 0.9419 1.4498 0.4858 0.029 Uiso 1 1 calc R . .
C9 C 0.7556(9) 1.4475(7) 0.4787(7) 0.024(2) Uani 1 1 d . . .
H9A H 0.7190 1.5244 0.4779 0.029 Uiso 1 1 calc R . .
H9B H 0.7098 1.4299 0.4311 0.029 Uiso 1 1 calc R . .
C10 C 0.7697(11) 1.4358(7) 0.6588(8) 0.031(2) Uani 1 1 d . . .
H10A H 0.7524 1.5118 0.6360 0.037 Uiso 1 1 calc R . .
H10B H 0.7105 1.4289 0.7157 0.037 Uiso 1 1 calc R . .
C11 C 0.9054(11) 1.3860(8) 0.6916(8) 0.032(2) Uani 1 1 d . . .
H11A H 0.9648 1.4012 0.6378 0.038 Uiso 1 1 calc R . .
H11B H 0.9149 1.4174 0.7471 0.038 Uiso 1 1 calc R . .
C12 C 0.6101(9) 1.3758(7) 0.5949(9) 0.031(2) Uani 1 1 d . . .
H12A H 0.5823 1.3663 0.5333 0.037 Uiso 1 1 calc R . .
H12B H 0.5446 1.4389 0.6164 0.037 Uiso 1 1 calc R . .
C13 C 0.6216(9) 1.2796(7) 0.6722(8) 0.027(2) Uani 1 1 d . . .
H13A H 0.6283 1.2955 0.7372 0.032 Uiso 1 1 calc R . .
H13B H 0.5439 1.2599 0.6736 0.032 Uiso 1 1 calc R . .
C14 C 1.1469(10) 1.0407(10) 0.8815(7) 0.032(2) Uani 1 1 d . . .
H14A H 1.0918 1.1124 0.8921 0.039 Uiso 1 1 calc R . .
H14B H 1.2028 1.0062 0.9379 0.039 Uiso 1 1 calc R . .
C15 C 1.0622(10) 0.9757(8) 0.8691(6) 0.027(2) Uani 1 1 d . . .
H15A H 1.1170 0.9010 0.8702 0.032 Uiso 1 1 calc R . .
H15B H 0.9968 0.9796 0.9233 0.032 Uiso 1 1 calc R . .
C16 C 1.2638(10) 1.1431(8) 0.7654(8) 0.031(2) Uani 1 1 d . . .
H16A H 1.3395 1.1334 0.8029 0.037 Uiso 1 1 calc R . .
H16B H 1.1911 1.2043 0.7835 0.037 Uiso 1 1 calc R . .
C17 C 1.2962(10) 1.1625(9) 0.6564(8) 0.033(2) Uani 1 1 d . . .
H17A H 1.2946 1.2358 0.6361 0.039 Uiso 1 1 calc R . .
H17B H 1.3843 1.1145 0.6422 0.039 Uiso 1 1 calc R . .
C18 C 1.3372(10) 0.9478(10) 0.7788(8) 0.036(2) Uani 1 1 d . . .
H18A H 1.3818 0.9591 0.7149 0.043 Uiso 1 1 calc R . .
H18B H 1.3024 0.8911 0.7779 0.043 Uiso 1 1 calc R . .
C19 C 1.4358(11) 0.9099(10) 0.8568(8) 0.037(3) Uani 1 1 d . . .
H19A H 1.5221 0.8718 0.8294 0.044 Uiso 1 1 calc R . .
H19B H 1.4410 0.9705 0.8820 0.044 Uiso 1 1 calc R . .
C5' C 1.221(3) 1.361(2) 0.116(2) 0.050(6) Uani 0.50 1 d PU A 2
H5'1 H 1.2503 1.3496 0.1820 0.076 Uiso 0.50 1 calc PR A 2
H5'2 H 1.1778 1.4360 0.0933 0.076 Uiso 0.50 1 calc PR A 2
H5'3 H 1.2958 1.3334 0.0720 0.076 Uiso 0.50 1 calc PR A 2
C6' C 0.981(4) 1.384(3) 0.128(3) 0.082(10) Uani 0.50 1 d PU A 2
H6'1 H 0.9502 1.4255 0.0645 0.124 Uiso 0.50 1 calc PR A 2
H6'2 H 0.9792 1.4315 0.1725 0.124 Uiso 0.50 1 calc PR A 2
H6'3 H 0.9239 1.3442 0.1550 0.124 Uiso 0.50 1 calc PR A 2
C7' C 1.141(5) 1.261(3) 0.029(3) 0.081(10) Uani 0.50 1 d PU A 2
H7'1 H 1.0603 1.2503 0.0187 0.121 Uiso 0.50 1 calc PR A 2
H7'2 H 1.2121 1.1933 0.0341 0.121 Uiso 0.50 1 calc PR A 2
H7'3 H 1.1584 1.3098 -0.0269 0.121 Uiso 0.50 1 calc PR A 2
C1S C 1.496(3) 1.395(3) 0.162(3) 0.165(13) Uani 1 1 d DU . .
H1S1 H 1.4240 1.3889 0.2062 0.248 Uiso 1 1 calc R . .
H1S2 H 1.5169 1.3443 0.1174 0.248 Uiso 1 1 calc R . .
H1S3 H 1.4725 1.4666 0.1244 0.248 Uiso 1 1 calc R . .
C2S C 1.611(3) 1.3738(19) 0.220(3) 0.164(13) Uani 1 1 d DU . .
H2S1 H 1.6050 1.3350 0.2864 0.196 Uiso 1 1 calc R . .
H2S2 H 1.6933 1.3361 0.1866 0.196 Uiso 1 1 calc R . .
C3S C 1.677(4) 1.536(3) 0.164(2) 0.171(14) Uani 1 1 d DU . .
H3S1 H 1.6340 1.5783 0.1038 0.205 Uiso 1 1 calc R . .
H3S2 H 1.7586 1.4826 0.1456 0.205 Uiso 1 1 calc R . .
C4S C 1.708(2) 1.6067(16) 0.2193(15) 0.090(6) Uani 1 1 d DU . .
H4S1 H 1.6815 1.6783 0.1821 0.135 Uiso 1 1 calc R . .
H4S2 H 1.8013 1.5810 0.2289 0.135 Uiso 1 1 calc R . .
H4S3 H 1.6616 1.6070 0.2828 0.135 Uiso 1 1 calc R . .
C5S C 0.741(2) 1.3159(13) 0.9480(11) 0.072(5) Uani 1 1 d . . .
H5S1 H 0.7307 1.2866 1.0167 0.108 Uiso 1 1 calc R . .
H5S2 H 0.6564 1.3483 0.9188 0.108 Uiso 1 1 calc R . .
H5S3 H 0.7818 1.3692 0.9436 0.108 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
Ho1 O15 2.218(6) 2_776 ?
Ho1 O14 2.231(6) 2_776 ?
Ho1 O3 2.267(6) . ?
Ho1 O7 2.289(6) . ?
Ho1 O2 2.384(6) . ?
Ho1 O4 2.491(6) . ?
Ho1 O5 2.531(6) . ?
Ho1 O1 2.539(5) 2_776 ?
Ho1 N1 2.919(8) . ?
Ho2 O12 2.209(6) . ?
Ho2 O16 2.235(7) . ?
Ho2 O3 2.269(6) . ?
Ho2 O8 2.307(6) . ?
Ho2 O2 2.384(6) . ?
Ho2 O9 2.463(7) . ?
Ho2 O10 2.471(6) . ?
Ho2 O1 2.709(5) . ?
Ho2 N2 2.889(8) . ?
Cu1 O1 1.939(5) . ?
Cu1 O1 1.939(5) 2_776 ?
Cu1 O2 1.976(6) . ?
Cu1 O2 1.976(6) 2_776 ?
Cu1 Ho1 3.1523(10) 2_776 ?
Cu1 Ho2 3.2635(9) 2_776 ?
Cu2 O16 1.903(6) . ?
Cu2 O15 1.912(6) . ?
Cu2 O1 1.930(5) . ?
Cu2 N4 2.001(8) . ?
Cu2 Ho1 3.2635(12) 2_776 ?
Cu3 O14 1.907(6) . ?
Cu3 O12 1.928(6) . ?
Cu3 O1 1.930(5) . ?
Cu3 N3 1.999(8) . ?
Cu3 O13 2.436(8) . ?
Cu3 Ho1 3.2730(14) 2_776 ?
O1 Ho1 2.539(5) 2_776 ?
O2 C1 1.442(10) . ?
O3 C2 1.403(11) . ?
O4 N1 1.275(10) . ?
O5 N1 1.248(11) . ?
O6 N1 1.236(10) . ?
O7 C3 1.240(12) . ?
O8 C3 1.241(13) . ?
O9 N2 1.284(12) . ?
O10 N2 1.253(11) . ?
O11 N2 1.202(11) . ?
O12 C8 1.392(11) . ?
O13 C11 1.439(12) . ?
O13 H13 0.8400 . ?
O14 C13 1.421(11) . ?
O14 Ho1 2.231(6) 2_776 ?
O15 C15 1.406(11) . ?
O15 Ho1 2.218(6) 2_776 ?
O16 C17 1.401(12) . ?
O17 C19 1.446(13) . ?
O17 H17 0.8400 . ?
O1S C3S 1.436(10) . ?
O1S C2S 1.462(10) . ?
O2S C5S 1.405(18) . ?
O2S H2S 0.8400 . ?
N3 C9 1.497(12) . ?
N3 C12 1.498(12) . ?
N3 C10 1.510(14) . ?
N4 C18 1.482(14) . ?
N4 C14 1.493(12) . ?
N4 C16 1.511(12) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.566(12) . ?
C4 C7' 1.41(4) . ?
C4 C5 1.47(3) . ?
C4 C5' 1.52(3) . ?
C4 C6 1.52(3) . ?
C4 C7 1.56(3) . ?
C4 C6' 1.63(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.536(13) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.492(16) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.518(13) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.553(15) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.525(14) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.508(15) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C5' H5'1 0.9800 . ?
C5' H5'2 0.9800 . ?
C5' H5'3 0.9800 . ?
C6' H6'1 0.9800 . ?
C6' H6'2 0.9800 . ?
C6' H6'3 0.9800 . ?
C7' H7'1 0.9800 . ?
C7' H7'2 0.9800 . ?
C7' H7'3 0.9800 . ?
C1S C2S 1.490(10) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?
C3S C4S 1.496(10) . ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
C5S H5S1 0.9800 . ?
C5S H5S2 0.9800 . ?
C5S H5S3 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
O15 Ho1 O14 104.0(2) 2_776 2_776 ?
O15 Ho1 O3 148.6(2) 2_776 . ?
O14 Ho1 O3 87.9(2) 2_776 . ?
O15 Ho1 O7 89.4(3) 2_776 . ?
O14 Ho1 O7 147.4(2) 2_776 . ?
O3 Ho1 O7 95.8(3) . . ?
O15 Ho1 O2 85.5(2) 2_776 . ?
O14 Ho1 O2 131.5(2) 2_776 . ?
O3 Ho1 O2 65.6(2) . . ?
O7 Ho1 O2 78.3(2) . . ?
O15 Ho1 O4 76.1(2) 2_776 . ?
O14 Ho1 O4 78.4(2) 2_776 . ?
O3 Ho1 O4 135.2(2) . . ?
O7 Ho1 O4 76.3(2) . . ?
O2 Ho1 O4 148.5(2) . . ?
O15 Ho1 O5 126.6(2) 2_776 . ?
O14 Ho1 O5 74.4(2) 2_776 . ?
O3 Ho1 O5 84.3(2) . . ?
O7 Ho1 O5 73.8(2) . . ?
O2 Ho1 O5 136.2(2) . . ?
O4 Ho1 O5 50.9(2) . . ?
O15 Ho1 O1 70.82(19) 2_776 2_776 ?
O14 Ho1 O1 70.15(19) 2_776 2_776 ?
O3 Ho1 O1 86.84(19) . 2_776 ?
O7 Ho1 O1 142.3(2) . 2_776 ?
O2 Ho1 O1 68.63(18) . 2_776 ?
O4 Ho1 O1 126.10(19) . 2_776 ?
O5 Ho1 O1 143.72(19) . 2_776 ?
O15 Ho1 N1 101.7(2) 2_776 . ?
O14 Ho1 N1 74.2(2) 2_776 . ?
O3 Ho1 N1 109.5(2) . . ?
O7 Ho1 N1 74.0(2) . . ?
O2 Ho1 N1 151.2(2) . . ?
O4 Ho1 N1 25.7(2) . . ?
O5 Ho1 N1 25.2(2) . . ?
O1 Ho1 N1 140.12(19) 2_776 . ?
O12 Ho2 O16 95.5(2) . . ?
O12 Ho2 O3 146.8(2) . . ?
O16 Ho2 O3 91.8(2) . . ?
O12 Ho2 O8 88.0(2) . . ?
O16 Ho2 O8 151.5(2) . . ?
O3 Ho2 O8 100.5(2) . . ?
O12 Ho2 O2 85.4(2) . . ?
O16 Ho2 O2 130.1(2) . . ?
O3 Ho2 O2 65.5(2) . . ?
O8 Ho2 O2 78.3(2) . . ?
O12 Ho2 O9 131.4(2) . . ?
O16 Ho2 O9 79.4(2) . . ?
O3 Ho2 O9 81.7(2) . . ?
O8 Ho2 O9 77.2(3) . . ?
O2 Ho2 O9 134.2(2) . . ?
O12 Ho2 O10 79.9(2) . . ?
O16 Ho2 O10 76.9(2) . . ?
O3 Ho2 O10 133.3(2) . . ?
O8 Ho2 O10 75.9(2) . . ?
O2 Ho2 O10 150.6(2) . . ?
O9 Ho2 O10 51.8(2) . . ?
O12 Ho2 O1 70.07(19) . . ?
O16 Ho2 O1 68.37(19) . . ?
O3 Ho2 O1 82.89(19) . . ?
O8 Ho2 O1 138.2(2) . . ?
O2 Ho2 O1 65.25(18) . . ?
O9 Ho2 O1 143.6(2) . . ?
O10 Ho2 O1 130.6(2) . . ?
O12 Ho2 N2 105.4(2) . . ?
O16 Ho2 N2 76.1(2) . . ?
O3 Ho2 N2 107.8(2) . . ?
O8 Ho2 N2 75.7(3) . . ?
O2 Ho2 N2 151.4(2) . . ?
O9 Ho2 N2 26.2(3) . . ?
O10 Ho2 N2 25.5(2) . . ?
O1 Ho2 N2 143.3(2) . . ?
O1 Cu1 O1 180.0(2) . 2_776 ?
O1 Cu1 O2 89.6(2) . . ?
O1 Cu1 O2 90.4(2) 2_776 . ?
O1 Cu1 O2 90.4(2) . 2_776 ?
O1 Cu1 O2 89.6(2) 2_776 2_776 ?
O2 Cu1 O2 180.0(3) . 2_776 ?
O1 Cu1 Ho1 53.62(16) . 2_776 ?
O1 Cu1 Ho1 126.38(16) 2_776 2_776 ?
O2 Cu1 Ho1 130.92(17) . 2_776 ?
O2 Cu1 Ho1 49.08(17) 2_776 2_776 ?
O1 Cu1 Ho2 123.96(16) . 2_776 ?
O1 Cu1 Ho2 56.04(16) 2_776 2_776 ?
O2 Cu1 Ho2 133.45(16) . 2_776 ?
O2 Cu1 Ho2 46.55(16) 2_776 2_776 ?
Ho1 Cu1 Ho2 70.35(3) 2_776 2_776 ?
O16 Cu2 O15 172.4(3) . . ?
O16 Cu2 O1 94.1(3) . . ?
O15 Cu2 O1 92.2(2) . . ?
O16 Cu2 N4 86.8(3) . . ?
O15 Cu2 N4 87.1(3) . . ?
O1 Cu2 N4 177.3(3) . . ?
O16 Cu2 Ho1 144.9(2) . 2_776 ?
O15 Cu2 Ho1 41.24(18) . 2_776 ?
O1 Cu2 Ho1 50.99(16) . 2_776 ?
N4 Cu2 Ho1 128.3(2) . 2_776 ?
O14 Cu3 O12 164.3(3) . . ?
O14 Cu3 O1 91.7(2) . . ?
O12 Cu3 O1 95.4(2) . . ?
O14 Cu3 N3 87.6(3) . . ?
O12 Cu3 N3 86.1(3) . . ?
O1 Cu3 N3 176.9(3) . . ?
O14 Cu3 O13 93.5(3) . . ?
O12 Cu3 O13 99.8(3) . . ?
O1 Cu3 O13 94.2(2) . . ?
N3 Cu3 O13 82.8(3) . . ?
O14 Cu3 Ho1 41.35(18) . 2_776 ?
O12 Cu3 Ho1 145.43(18) . 2_776 ?
O1 Cu3 Ho1 50.76(16) . 2_776 ?
N3 Cu3 Ho1 128.1(2) . 2_776 ?
O13 Cu3 Ho1 90.61(17) . 2_776 ?
Cu3 O1 Cu2 107.5(3) . . ?
Cu3 O1 Cu1 128.9(3) . . ?
Cu2 O1 Cu1 123.4(3) . . ?
Cu3 O1 Ho1 93.2(2) . 2_776 ?
Cu2 O1 Ho1 92.8(2) . 2_776 ?
Cu1 O1 Ho1 88.43(19) . 2_776 ?
Cu3 O1 Ho2 88.87(19) . . ?
Cu2 O1 Ho2 89.9(2) . . ?
Cu1 O1 Ho2 87.54(19) . . ?
Ho1 O1 Ho2 175.9(2) 2_776 . ?
C1 O2 Cu1 116.7(5) . . ?
C1 O2 Ho1 122.6(5) . . ?
Cu1 O2 Ho1 92.1(2) . . ?
C1 O2 Ho2 121.0(5) . . ?
Cu1 O2 Ho2 96.5(2) . . ?
Ho1 O2 Ho2 101.7(2) . . ?
C2 O3 Ho1 123.5(5) . . ?
C2 O3 Ho2 123.3(6) . . ?
Ho1 O3 Ho2 109.2(2) . . ?
N1 O4 Ho1 96.2(5) . . ?
N1 O5 Ho1 95.0(5) . . ?
C3 O7 Ho1 139.2(7) . . ?
C3 O8 Ho2 133.2(6) . . ?
N2 O9 Ho2 95.7(5) . . ?
N2 O10 Ho2 96.2(5) . . ?
C8 O12 Cu3 113.7(5) . . ?
C8 O12 Ho2 140.3(5) . . ?
Cu3 O12 Ho2 105.4(3) . . ?
C11 O13 Cu3 95.6(6) . . ?
C11 O13 H13 109.5 . . ?
Cu3 O13 H13 106.1 . . ?
C13 O14 Cu3 112.2(5) . . ?
C13 O14 Ho1 141.5(5) . 2_776 ?
Cu3 O14 Ho1 104.3(2) . 2_776 ?
C15 O15 Cu2 111.8(5) . . ?
C15 O15 Ho1 143.5(5) . 2_776 ?
Cu2 O15 Ho1 104.1(3) . 2_776 ?
C17 O16 Cu2 112.8(6) . . ?
C17 O16 Ho2 140.5(6) . . ?
Cu2 O16 Ho2 106.7(3) . . ?
C19 O17 H17 109.5 . . ?
C3S O1S C2S 124(3) . . ?
C5S O2S H2S 109.5 . . ?
O6 N1 O5 122.0(8) . . ?
O6 N1 O4 120.3(8) . . ?
O5 N1 O4 117.7(7) . . ?
O6 N1 Ho1 176.0(7) . . ?
O5 N1 Ho1 59.8(4) . . ?
O4 N1 Ho1 58.0(4) . . ?
O11 N2 O10 123.5(10) . . ?
O11 N2 O9 120.3(9) . . ?
O10 N2 O9 116.2(7) . . ?
O11 N2 Ho2 176.7(8) . . ?
O10 N2 Ho2 58.2(4) . . ?
O9 N2 Ho2 58.0(4) . . ?
C9 N3 C12 112.6(8) . . ?
C9 N3 C10 113.3(7) . . ?
C12 N3 C10 112.8(8) . . ?
C9 N3 Cu3 104.0(6) . . ?
C12 N3 Cu3 103.0(5) . . ?
C10 N3 Cu3 110.2(6) . . ?
C18 N4 C14 115.1(8) . . ?
C18 N4 C16 113.1(8) . . ?
C14 N4 C16 113.4(8) . . ?
C18 N4 Cu2 110.1(6) . . ?
C14 N4 Cu2 103.8(6) . . ?
C16 N4 Cu2 99.7(6) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C2 H2A 109.5 . . ?
O3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O7 C3 O8 124.7(9) . . ?
O7 C3 C4 116.7(10) . . ?
O8 C3 C4 118.6(9) . . ?
C7' C4 C5 132(2) . . ?
C7' C4 C5' 112(2) . . ?
C5 C4 C5' 44.1(16) . . ?
C7' C4 C6 57(2) . . ?
C5 C4 C6 116.7(19) . . ?
C5' C4 C6 147.4(16) . . ?
C7' C4 C7 50(2) . . ?
C5 C4 C7 109.3(19) . . ?
C5' C4 C7 69(2) . . ?
C6 C4 C7 106(2) . . ?
C7' C4 C3 116.0(18) . . ?
C5 C4 C3 111.7(13) . . ?
C5' C4 C3 106.2(14) . . ?
C6 C4 C3 106.0(12) . . ?
C7 C4 C3 106.2(13) . . ?
C7' C4 C6' 110(3) . . ?
C5 C4 C6' 65(2) . . ?
C5' C4 C6' 109(2) . . ?
C6 C4 C6' 58(2) . . ?
C7 C4 C6' 149.8(19) . . ?
C3 C4 C6' 103.2(15) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
O12 C8 C9 109.5(7) . . ?
O12 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
O12 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.2 . . ?
N3 C9 C8 108.5(7) . . ?
N3 C9 H9A 110.0 . . ?
C8 C9 H9A 110.0 . . ?
N3 C9 H9B 110.0 . . ?
C8 C9 H9B 110.0 . . ?
H9A C9 H9B 108.4 . . ?
C11 C10 N3 115.0(8) . . ?
C11 C10 H10A 108.5 . . ?
N3 C10 H10A 108.5 . . ?
C11 C10 H10B 108.5 . . ?
N3 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
O13 C11 C10 112.3(8) . . ?
O13 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
O13 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
N3 C12 C13 109.0(8) . . ?
N3 C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
N3 C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O14 C13 C12 108.9(8) . . ?
O14 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
O14 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
N4 C14 C15 106.2(8) . . ?
N4 C14 H14A 110.5 . . ?
C15 C14 H14A 110.5 . . ?
N4 C14 H14B 110.5 . . ?
C15 C14 H14B 110.5 . . ?
H14A C14 H14B 108.7 . . ?
O15 C15 C14 108.9(7) . . ?
O15 C15 H15A 109.9 . . ?
C14 C15 H15A 109.9 . . ?
O15 C15 H15B 109.9 . . ?
C14 C15 H15B 109.9 . . ?
H15A C15 H15B 108.3 . . ?
N4 C16 C17 108.8(8) . . ?
N4 C16 H16A 109.9 . . ?
C17 C16 H16A 109.9 . . ?
N4 C16 H16B 109.9 . . ?
C17 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
O16 C17 C16 110.1(8) . . ?
O16 C17 H17A 109.6 . . ?
C16 C17 H17A 109.6 . . ?
O16 C17 H17B 109.6 . . ?
C16 C17 H17B 109.6 . . ?
H17A C17 H17B 108.2 . . ?
N4 C18 C19 116.0(10) . . ?
N4 C18 H18A 108.3 . . ?
C19 C18 H18A 108.3 . . ?
N4 C18 H18B 108.3 . . ?
C19 C18 H18B 108.3 . . ?
H18A C18 H18B 107.4 . . ?
O17 C19 C18 108.2(9) . . ?
O17 C19 H19A 110.1 . . ?
C18 C19 H19A 110.1 . . ?
O17 C19 H19B 110.1 . . ?
C18 C19 H19B 110.1 . . ?
H19A C19 H19B 108.4 . . ?
C4 C5' H5'1 109.5 . . ?
C4 C5' H5'2 109.5 . . ?
H5'1 C5' H5'2 109.5 . . ?
C4 C5' H5'3 109.5 . . ?
H5'1 C5' H5'3 109.5 . . ?
H5'2 C5' H5'3 109.5 . . ?
C4 C6' H6'1 109.5 . . ?
C4 C6' H6'2 109.5 . . ?
H6'1 C6' H6'2 109.5 . . ?
C4 C6' H6'3 109.5 . . ?
H6'1 C6' H6'3 109.5 . . ?
H6'2 C6' H6'3 109.5 . . ?
C4 C7' H7'1 109.5 . . ?
C4 C7' H7'2 109.5 . . ?
H7'1 C7' H7'2 109.5 . . ?
C4 C7' H7'3 109.5 . . ?
H7'1 C7' H7'3 109.5 . . ?
H7'2 C7' H7'3 109.5 . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
O1S C2S C1S 96(2) . . ?
O1S C2S H2S1 112.5 . . ?
C1S C2S H2S1 112.5 . . ?
O1S C2S H2S2 112.5 . . ?
C1S C2S H2S2 112.5 . . ?
H2S1 C2S H2S2 110.0 . . ?
O1S C3S C4S 113(2) . . ?
O1S C3S H3S1 109.0 . . ?
C4S C3S H3S1 109.0 . . ?
O1S C3S H3S2 109.0 . . ?
C4S C3S H3S2 109.0 . . ?
H3S1 C3S H3S2 107.8 . . ?
C3S C4S H4S1 109.5 . . ?
C3S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
C3S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
O2S C5S H5S1 109.5 . . ?
O2S C5S H5S2 109.5 . . ?
H5S1 C5S H5S2 109.5 . . ?
O2S C5S H5S3 109.5 . . ?
H5S1 C5S H5S3 109.5 . . ?
H5S2 C5S H5S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.918
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.918
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.742
_refine_diff_density_rms         0.327


####################################################################### 
# 
# 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_Cu5Tb4final
_audit_block_doi                 10.5517/ccw4vnh
_database_code_depnum_ccdc_archive 'CCDC 809027'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1002/chem.201100218 2011
_audit_update_record             
;
2011-01-20 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
#TrackingRef '2 Cu5Tb4final.cif'

#==========================================================================

_audit_creation_method           SHELXL-97
_audit_creation_date             '9 November 2005'
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C38 H82 Cu5 N8 O34 Tb4, 2(C4 H10 O), 2(C H4 O)
;
_chemical_formula_sum            'C48 H110 Cu5 N8 O38 Tb4'
_chemical_formula_weight         2360.82

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 '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

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

_cell_length_a                   11.0443(4)
_cell_length_b                   13.8090(5)
_cell_length_c                   14.0113(5)
_cell_angle_alpha                78.935(2)
_cell_angle_beta                 83.743(2)
_cell_angle_gamma                69.405(2)
_cell_volume                     1961.12(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9878
_cell_measurement_theta_min      2.12
_cell_measurement_theta_max      28.80

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1163
_exptl_absorpt_coefficient_mu    4.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.742
_exptl_absorpt_correction_T_max  0.780
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'APEX X8 Apex CCD'
_diffrn_measurement_method       'scans in phi and omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            27457
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_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         2.52
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8661
_reflns_number_gt                6995
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex2 V2.0'
_computing_cell_refinement       'Bruker Apex2 V2.0'
_computing_data_reduction        'Bruker Apex2 V2.0'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    X-SEED
_computing_publication_material  'XCIF V6.12 (BrukerAXS, 2001).'

_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 asymmetric unit contains half the cluster which lies upon an
inversion centre as well as solvent MeOH and Et2O molecules. All non
H-atoms are refined anisotropically and H-atoms are placed in
calculated positions. A bond restraint (DFIX) is placed on C3S and C4S of
tthe solvent Et2O molecule, with thermal (ISOR) restraints placed on
C5 C6 C7 and C11.
;

_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)+(0.0000P)²+32.6408P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8661
_refine_ls_number_parameters     477
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1000
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.088
_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
Tb1 Tb 0.16771(3) 0.47475(3) 0.30243(2) 0.01156(9) Uani 1 1 d . . .
Tb2 Tb 0.13931(3) 0.67910(3) 0.45065(2) 0.01226(9) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.5000 0.5000 0.0105(2) Uani 1 2 d S . .
Cu2 Cu 0.09778(9) 0.58271(7) 0.68411(6) 0.01382(19) Uani 1 1 d . . .
Cu3 Cu -0.14120(9) 0.74503(7) 0.57542(6) 0.01290(18) Uani 1 1 d . . .
O1 O -0.0193(5) 0.6039(4) 0.5823(3) 0.0126(10) Uani 1 1 d . . .
O2 O 0.0060(5) 0.6047(4) 0.3836(3) 0.0104(10) Uani 1 1 d . . .
O3 O 0.2356(5) 0.5052(4) 0.4378(4) 0.0150(11) Uani 1 1 d . . .
O4 O 0.2720(5) 0.4168(4) 0.1450(4) 0.0198(12) Uani 1 1 d . . .
O5 O 0.4026(5) 0.4377(4) 0.2366(4) 0.0183(11) Uani 1 1 d . . .
O6 O 0.4765(6) 0.3741(5) 0.1037(4) 0.0283(14) Uani 1 1 d . . .
O7 O 0.1748(6) 0.6286(4) 0.2061(4) 0.0305(15) Uani 1 1 d . . .
O8 O 0.1372(6) 0.7593(5) 0.2874(4) 0.0280(14) Uani 1 1 d . . .
O9 O 0.3660(5) 0.6777(4) 0.4178(4) 0.0241(13) Uani 1 1 d . . .
O10 O 0.2261(5) 0.8226(4) 0.4508(4) 0.0229(12) Uani 1 1 d . . .
O11 O 0.4301(6) 0.8053(5) 0.4329(6) 0.0447(19) Uani 1 1 d . . .
O12 O -0.0459(5) 0.8079(4) 0.4756(4) 0.0170(11) Uani 1 1 d . . .
O13 O -0.0630(6) 0.7745(5) 0.7206(4) 0.0267(13) Uani 1 1 d . . .
H14 H -0.1079 0.7639 0.7693 0.032 Uiso 1 1 calc R . .
O14 O -0.2715(5) 0.6966(4) 0.6482(4) 0.0173(11) Uani 1 1 d . . .
O15 O -0.0012(5) 0.5188(4) 0.7790(4) 0.0186(11) Uani 1 1 d . . .
O16 O 0.2025(5) 0.6520(4) 0.6035(4) 0.0189(11) Uani 1 1 d . . .
O17 O 0.3878(7) 0.3474(5) 0.9321(4) 0.0314(15) Uani 1 1 d . . .
H10 H 0.4235 0.3406 0.9826 0.038 Uiso 1 1 calc R . .
O1S O 0.5912(14) 0.9845(11) 0.2171(11) 0.131(6) Uani 1 1 d . . .
O2S O -0.1859(7) 0.7410(6) 0.8953(5) 0.0381(17) Uani 1 1 d . . .
H2S H -0.2146 0.6925 0.9047 0.046 Uiso 1 1 calc R . .
N1 N 0.3849(6) 0.4096(5) 0.1605(5) 0.0190(14) Uani 1 1 d . . .
N2 N 0.3422(7) 0.7693(5) 0.4334(5) 0.0248(16) Uani 1 1 d . . .
N3 N -0.2652(6) 0.8917(5) 0.5777(4) 0.0154(13) Uani 1 1 d . . .
N4 N 0.2218(6) 0.5543(5) 0.7866(4) 0.0177(14) Uani 1 1 d . . .
C1 C -0.1152(7) 0.6694(6) 0.3435(6) 0.0180(16) Uani 1 1 d . . .
H1A H -0.1395 0.6334 0.3007 0.027 Uiso 1 1 calc R . .
H1B H -0.1076 0.7338 0.3078 0.027 Uiso 1 1 calc R . .
H1C H -0.1802 0.6844 0.3952 0.027 Uiso 1 1 calc R . .
C2 C 0.3541(8) 0.4417(6) 0.4814(6) 0.0225(18) Uani 1 1 d . . .
H2A H 0.3764 0.3712 0.4694 0.034 Uiso 1 1 calc R . .
H2B H 0.3447 0.4419 0.5503 0.034 Uiso 1 1 calc R . .
H2C H 0.4213 0.4691 0.4540 0.034 Uiso 1 1 calc R . .
C3 C 0.1498(7) 0.7229(6) 0.2096(6) 0.0211(17) Uani 1 1 d . . .
C4 C 0.1351(9) 0.7967(6) 0.1130(6) 0.0264(19) Uani 1 1 d . . .
C5 C 0.1156(15) 0.9055(10) 0.1230(10) 0.068(4) Uani 1 1 d U . .
H5A H 0.1889 0.9074 0.1527 0.103 Uiso 1 1 calc R . .
H5B H 0.0388 0.9316 0.1630 0.103 Uiso 1 1 calc R . .
H5C H 0.1063 0.9485 0.0598 0.103 Uiso 1 1 calc R . .
C6 C 0.0208(13) 0.7896(10) 0.0635(9) 0.063(3) Uani 1 1 d U . .
H6A H -0.0590 0.8236 0.0971 0.094 Uiso 1 1 calc R . .
H6B H 0.0308 0.7173 0.0659 0.094 Uiso 1 1 calc R . .
H6C H 0.0197 0.8236 -0.0031 0.094 Uiso 1 1 calc R . .
C7 C 0.2490(15) 0.7538(12) 0.0462(10) 0.083(5) Uani 1 1 d U . .
H7A H 0.2256 0.7811 -0.0201 0.125 Uiso 1 1 calc R . .
H7B H 0.2750 0.6787 0.0567 0.125 Uiso 1 1 calc R . .
H7C H 0.3194 0.7742 0.0592 0.125 Uiso 1 1 calc R . .
C8 C -0.1034(8) 0.9172(6) 0.4495(6) 0.0207(17) Uani 1 1 d . . .
H8A H -0.0918 0.9375 0.3798 0.025 Uiso 1 1 calc R . .
H8B H -0.0627 0.9527 0.4822 0.025 Uiso 1 1 calc R . .
C9 C -0.2471(8) 0.9486(6) 0.4786(6) 0.0219(17) Uani 1 1 d . . .
H9A H -0.2829 1.0236 0.4783 0.026 Uiso 1 1 calc R . .
H9B H -0.2924 0.9315 0.4322 0.026 Uiso 1 1 calc R . .
C10 C -0.2333(9) 0.9364(6) 0.6568(6) 0.0244(18) Uani 1 1 d . . .
H10A H -0.2917 0.9298 0.7126 0.029 Uiso 1 1 calc R . .
H10B H -0.2497 1.0107 0.6345 0.029 Uiso 1 1 calc R . .
C11 C -0.0924(9) 0.8851(6) 0.6903(6) 0.0222(18) Uani 1 1 d U . .
H11A H -0.0330 0.8979 0.6371 0.027 Uiso 1 1 calc R . .
H11B H -0.0820 0.9163 0.7439 0.027 Uiso 1 1 calc R . .
C12 C -0.3933(7) 0.8772(6) 0.5950(6) 0.0229(18) Uani 1 1 d . . .
H12A H -0.4213 0.8686 0.5348 0.028 Uiso 1 1 calc R . .
H12B H -0.4569 0.9387 0.6168 0.028 Uiso 1 1 calc R . .
C13 C -0.3836(8) 0.7814(6) 0.6713(7) 0.0256(19) Uani 1 1 d . . .
H13A H -0.3768 0.7962 0.7351 0.031 Uiso 1 1 calc R . .
H13B H -0.4606 0.7626 0.6726 0.031 Uiso 1 1 calc R . .
C14 C 0.1426(8) 0.5467(8) 0.8803(5) 0.0256(19) Uani 1 1 d . . .
H14A H 0.0884 0.6160 0.8923 0.031 Uiso 1 1 calc R . .
H14B H 0.1986 0.5125 0.9344 0.031 Uiso 1 1 calc R . .
C15 C 0.0587(8) 0.4819(7) 0.8687(5) 0.0214(17) Uani 1 1 d . . .
H15A H 0.1122 0.4087 0.8720 0.026 Uiso 1 1 calc R . .
H15B H -0.0068 0.4871 0.9214 0.026 Uiso 1 1 calc R . .
C16 C 0.2589(8) 0.6501(7) 0.7657(6) 0.0235(18) Uani 1 1 d . . .
H16A H 0.3332 0.6397 0.8024 0.028 Uiso 1 1 calc R . .
H16B H 0.1878 0.7093 0.7845 0.028 Uiso 1 1 calc R . .
C17 C 0.2919(9) 0.6714(7) 0.6564(5) 0.0241(18) Uani 1 1 d . . .
H17A H 0.2881 0.7437 0.6372 0.029 Uiso 1 1 calc R . .
H17B H 0.3792 0.6263 0.6419 0.029 Uiso 1 1 calc R . .
C18 C 0.3340(8) 0.4573(7) 0.7778(6) 0.0248(18) Uani 1 1 d . . .
H18A H 0.3809 0.4697 0.7167 0.030 Uiso 1 1 calc R . .
H18B H 0.3006 0.4021 0.7737 0.030 Uiso 1 1 calc R . .
C19 C 0.4295(8) 0.4170(7) 0.8572(6) 0.0260(19) Uani 1 1 d . . .
H19A H 0.5148 0.3800 0.8310 0.031 Uiso 1 1 calc R . .
H19B H 0.4346 0.4751 0.8840 0.031 Uiso 1 1 calc R . .
C1S C 0.487(2) 0.8811(19) 0.1790(19) 0.167(12) Uani 1 1 d . . .
H1S1 H 0.4219 0.8973 0.2302 0.250 Uiso 1 1 calc R . .
H1S2 H 0.4930 0.8161 0.1607 0.250 Uiso 1 1 calc R . .
H1S3 H 0.4649 0.9361 0.1237 0.250 Uiso 1 1 calc R . .
C2S C 0.5992(19) 0.8728(19) 0.2095(17) 0.132(9) Uani 1 1 d . . .
H2S1 H 0.6688 0.8431 0.1638 0.158 Uiso 1 1 calc R . .
H2S2 H 0.6150 0.8279 0.2725 0.158 Uiso 1 1 calc R . .
C3S C 0.703(2) 0.9988(13) 0.1914(13) 0.112(7) Uani 1 1 d D . .
H3S1 H 0.7176 1.0026 0.1215 0.134 Uiso 1 1 calc R . .
H3S2 H 0.7720 0.9388 0.2220 0.134 Uiso 1 1 calc R . .
C4S C 0.7094(14) 1.0959(10) 0.2191(10) 0.070(4) Uani 1 1 d D . .
H4S1 H 0.6580 1.1562 0.1765 0.106 Uiso 1 1 calc R . .
H4S2 H 0.7977 1.0939 0.2135 0.106 Uiso 1 1 calc R . .
H4S3 H 0.6767 1.1003 0.2850 0.106 Uiso 1 1 calc R . .
C5S C -0.2689(13) 0.8226(10) 0.9402(9) 0.057(3) Uani 1 1 d . . .
H5S1 H -0.2747 0.7988 1.0090 0.086 Uiso 1 1 calc R . .
H5S2 H -0.3532 0.8457 0.9143 0.086 Uiso 1 1 calc R . .
H5S3 H -0.2360 0.8799 0.9284 0.086 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
Tb1 O15 2.236(5) 2_566 ?
Tb1 O14 2.243(5) 2_566 ?
Tb1 O3 2.274(5) . ?
Tb1 O7 2.310(5) . ?
Tb1 O2 2.406(5) . ?
Tb1 O4 2.511(5) . ?
Tb1 O1 2.545(5) 2_566 ?
Tb1 O5 2.563(5) . ?
Tb1 N1 2.940(6) . ?
Tb2 O12 2.235(5) . ?
Tb2 O16 2.247(5) . ?
Tb2 O3 2.293(5) . ?
Tb2 O8 2.340(5) . ?
Tb2 O2 2.417(5) . ?
Tb2 O10 2.487(5) . ?
Tb2 O9 2.490(6) . ?
Tb2 O1 2.719(5) . ?
Tb2 N2 2.891(7) . ?
Cu1 O1 1.949(5) 2_566 ?
Cu1 O1 1.949(5) . ?
Cu1 O2 1.973(5) . ?
Cu1 O2 1.973(5) 2_566 ?
Cu1 Tb1 3.1645(3) 2_566 ?
Cu1 Tb2 3.2788(4) 2_566 ?
Cu2 O16 1.899(5) . ?
Cu2 O15 1.911(5) . ?
Cu2 O1 1.941(5) . ?
Cu2 N4 1.981(6) . ?
Cu2 Tb1 3.2744(9) 2_566 ?
Cu3 O14 1.911(5) . ?
Cu3 O12 1.917(5) . ?
Cu3 O1 1.932(5) . ?
Cu3 N3 2.010(6) . ?
Cu3 Tb1 3.2784(9) 2_566 ?
O1 Tb1 2.545(5) 2_566 ?
O2 C1 1.427(8) . ?
O3 C2 1.420(9) . ?
O4 N1 1.255(8) . ?
O5 N1 1.258(8) . ?
O6 N1 1.234(8) . ?
O7 C3 1.243(10) . ?
O8 C3 1.261(10) . ?
O9 N2 1.255(9) . ?
O10 N2 1.258(9) . ?
O11 N2 1.236(9) . ?
O12 C8 1.407(9) . ?
O13 C11 1.433(9) . ?
O13 H14 0.8200 . ?
O14 C13 1.430(9) . ?
O14 Tb1 2.243(5) 2_566 ?
O15 C15 1.405(9) . ?
O15 Tb1 2.236(5) 2_566 ?
O16 C17 1.421(9) . ?
O17 C19 1.434(10) . ?
O17 H10 0.8200 . ?
O1S C3S 1.32(2) . ?
O1S C2S 1.54(2) . ?
O2S C5S 1.388(12) . ?
O2S H2S 0.8200 . ?
N3 C12 1.486(10) . ?
N3 C9 1.489(10) . ?
N3 C10 1.494(10) . ?
N4 C16 1.486(10) . ?
N4 C18 1.486(10) . ?
N4 C14 1.504(9) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.515(11) . ?
C4 C5 1.474(15) . ?
C4 C7 1.497(16) . ?
C4 C6 1.544(15) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.522(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.549(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.512(11) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.535(11) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.533(10) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.505(11) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C1S C2S 1.31(2) . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
C2S H2S1 0.9700 . ?
C2S H2S2 0.9700 . ?
C3S C4S 1.492(9) . ?
C3S H3S1 0.9700 . ?
C3S H3S2 0.9700 . ?
C4S H4S1 0.9600 . ?
C4S H4S2 0.9600 . ?
C4S H4S3 0.9600 . ?
C5S H5S1 0.9600 . ?
C5S H5S2 0.9600 . ?
C5S H5S3 0.9600 . ?

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
O15 Tb1 O14 104.9(2) 2_566 2_566 ?
O15 Tb1 O3 147.48(18) 2_566 . ?
O14 Tb1 O3 87.64(19) 2_566 . ?
O15 Tb1 O7 90.2(2) 2_566 . ?
O14 Tb1 O7 147.1(2) 2_566 . ?
O3 Tb1 O7 95.1(2) . . ?
O15 Tb1 O2 84.13(18) 2_566 . ?
O14 Tb1 O2 131.40(17) 2_566 . ?
O3 Tb1 O2 65.73(17) . . ?
O7 Tb1 O2 78.35(18) . . ?
O15 Tb1 O4 76.42(18) 2_566 . ?
O14 Tb1 O4 78.59(18) 2_566 . ?
O3 Tb1 O4 136.00(18) . . ?
O7 Tb1 O4 76.77(19) . . ?
O2 Tb1 O4 148.16(17) . . ?
O15 Tb1 O1 70.79(17) 2_566 2_566 ?
O14 Tb1 O1 70.19(17) 2_566 2_566 ?
O3 Tb1 O1 86.24(17) . 2_566 ?
O7 Tb1 O1 142.70(19) . 2_566 ?
O2 Tb1 O1 68.28(15) . 2_566 ?
O4 Tb1 O1 125.95(16) . 2_566 ?
O15 Tb1 O5 126.33(17) 2_566 . ?
O14 Tb1 O5 73.70(17) 2_566 . ?
O3 Tb1 O5 85.78(17) . . ?
O7 Tb1 O5 73.80(19) . . ?
O2 Tb1 O5 137.83(16) . . ?
O4 Tb1 O5 50.28(16) . . ?
O1 Tb1 O5 143.26(17) 2_566 . ?
O15 Tb1 N1 101.42(18) 2_566 . ?
O14 Tb1 N1 73.62(18) 2_566 . ?
O3 Tb1 N1 110.93(18) . . ?
O7 Tb1 N1 74.78(19) . . ?
O2 Tb1 N1 152.53(17) . . ?
O4 Tb1 N1 25.07(17) . . ?
O1 Tb1 N1 139.05(17) 2_566 . ?
O5 Tb1 N1 25.26(17) . . ?
O12 Tb2 O16 94.4(2) . . ?
O12 Tb2 O3 146.19(18) . . ?
O16 Tb2 O3 92.38(19) . . ?
O12 Tb2 O8 87.7(2) . . ?
O16 Tb2 O8 151.31(19) . . ?
O3 Tb2 O8 101.7(2) . . ?
O12 Tb2 O2 85.36(18) . . ?
O16 Tb2 O2 129.90(17) . . ?
O3 Tb2 O2 65.25(17) . . ?
O8 Tb2 O2 78.78(18) . . ?
O12 Tb2 O10 80.59(18) . . ?
O16 Tb2 O10 76.22(19) . . ?
O3 Tb2 O10 133.12(18) . . ?
O8 Tb2 O10 75.92(19) . . ?
O2 Tb2 O10 151.42(17) . . ?
O12 Tb2 O9 131.65(18) . . ?
O16 Tb2 O9 79.62(19) . . ?
O3 Tb2 O9 82.16(18) . . ?
O8 Tb2 O9 77.7(2) . . ?
O2 Tb2 O9 134.47(17) . . ?
O10 Tb2 O9 51.24(18) . . ?
O12 Tb2 O1 69.64(16) . . ?
O16 Tb2 O1 68.24(17) . . ?
O3 Tb2 O1 82.38(16) . . ?
O8 Tb2 O1 137.91(18) . . ?
O2 Tb2 O1 64.86(15) . . ?
O10 Tb2 O1 130.73(16) . . ?
O9 Tb2 O1 143.52(17) . . ?
O12 Tb2 N2 106.24(19) . . ?
O16 Tb2 N2 75.51(19) . . ?
O3 Tb2 N2 107.53(19) . . ?
O8 Tb2 N2 76.4(2) . . ?
O2 Tb2 N2 152.06(18) . . ?
O10 Tb2 N2 25.67(19) . . ?
O9 Tb2 N2 25.62(18) . . ?
O1 Tb2 N2 142.85(18) . . ?
O1 Cu1 O1 180.0(2) 2_566 . ?
O1 Cu1 O2 90.3(2) 2_566 . ?
O1 Cu1 O2 89.7(2) . . ?
O1 Cu1 O2 89.7(2) 2_566 2_566 ?
O1 Cu1 O2 90.3(2) . 2_566 ?
O2 Cu1 O2 180.0(2) . 2_566 ?
O1 Cu1 Tb1 126.50(14) 2_566 2_566 ?
O1 Cu1 Tb1 53.50(14) . 2_566 ?
O2 Cu1 Tb1 130.56(14) . 2_566 ?
O2 Cu1 Tb1 49.44(14) 2_566 2_566 ?
O1 Cu1 Tb2 55.94(14) 2_566 2_566 ?
O1 Cu1 Tb2 124.06(14) . 2_566 ?
O2 Cu1 Tb2 132.85(13) . 2_566 ?
O2 Cu1 Tb2 47.14(13) 2_566 2_566 ?
Tb1 Cu1 Tb2 70.563(9) 2_566 2_566 ?
O16 Cu2 O15 172.5(2) . . ?
O16 Cu2 O1 94.2(2) . . ?
O15 Cu2 O1 92.4(2) . . ?
O16 Cu2 N4 86.2(2) . . ?
O15 Cu2 N4 87.4(2) . . ?
O1 Cu2 N4 177.3(2) . . ?
O16 Cu2 Tb1 144.79(16) . 2_566 ?
O15 Cu2 Tb1 41.48(16) . 2_566 ?
O1 Cu2 Tb1 50.91(15) . 2_566 ?
N4 Cu2 Tb1 128.90(18) . 2_566 ?
O14 Cu3 O12 164.1(2) . . ?
O14 Cu3 O1 91.9(2) . . ?
O12 Cu3 O1 95.8(2) . . ?
O14 Cu3 N3 87.3(2) . . ?
O12 Cu3 N3 85.9(2) . . ?
O1 Cu3 N3 176.0(2) . . ?
O14 Cu3 Tb1 41.60(15) . 2_566 ?
O12 Cu3 Tb1 146.00(15) . 2_566 ?
O1 Cu3 Tb1 50.80(15) . 2_566 ?
N3 Cu3 Tb1 127.89(17) . 2_566 ?
Cu3 O1 Cu2 107.2(2) . . ?
Cu3 O1 Cu1 129.3(3) . . ?
Cu2 O1 Cu1 123.4(3) . . ?
Cu3 O1 Tb1 93.16(19) . 2_566 ?
Cu2 O1 Tb1 92.78(18) . 2_566 ?
Cu1 O1 Tb1 88.50(18) . 2_566 ?
Cu3 O1 Tb2 88.94(18) . . ?
Cu2 O1 Tb2 89.74(19) . . ?
Cu1 O1 Tb2 87.62(17) . . ?
Tb1 O1 Tb2 176.1(2) 2_566 . ?
C1 O2 Cu1 116.5(4) . . ?
C1 O2 Tb1 123.5(4) . . ?
Cu1 O2 Tb1 92.01(18) . . ?
C1 O2 Tb2 121.0(4) . . ?
Cu1 O2 Tb2 96.10(18) . . ?
Tb1 O2 Tb2 101.05(17) . . ?
C2 O3 Tb1 123.6(4) . . ?
C2 O3 Tb2 122.4(4) . . ?
Tb1 O3 Tb2 109.2(2) . . ?
N1 O4 Tb1 97.0(4) . . ?
N1 O5 Tb1 94.4(4) . . ?
C3 O7 Tb1 141.0(5) . . ?
C3 O8 Tb2 131.4(5) . . ?
N2 O9 Tb2 95.3(4) . . ?
N2 O10 Tb2 95.4(4) . . ?
C8 O12 Cu3 114.2(4) . . ?
C8 O12 Tb2 139.9(4) . . ?
Cu3 O12 Tb2 105.3(2) . . ?
C11 O13 H14 109.5 . . ?
C13 O14 Cu3 112.1(4) . . ?
C13 O14 Tb1 141.4(4) . 2_566 ?
Cu3 O14 Tb1 103.9(2) . 2_566 ?
C15 O15 Cu2 111.7(5) . . ?
C15 O15 Tb1 144.1(5) . 2_566 ?
Cu2 O15 Tb1 104.0(2) . 2_566 ?
C17 O16 Cu2 113.0(4) . . ?
C17 O16 Tb2 140.3(4) . . ?
Cu2 O16 Tb2 106.7(2) . . ?
C19 O17 H10 109.5 . . ?
C3S O1S C2S 111.3(13) . . ?
C5S O2S H2S 109.5 . . ?
O6 N1 O4 121.0(6) . . ?
O6 N1 O5 120.8(7) . . ?
O4 N1 O5 118.2(6) . . ?
O6 N1 Tb1 174.8(5) . . ?
O4 N1 Tb1 58.0(3) . . ?
O5 N1 Tb1 60.3(3) . . ?
O11 N2 O9 121.1(7) . . ?
O11 N2 O10 121.1(7) . . ?
O9 N2 O10 117.8(6) . . ?
O11 N2 Tb2 175.6(6) . . ?
O9 N2 Tb2 59.0(4) . . ?
O10 N2 Tb2 58.9(4) . . ?
C12 N3 C9 113.2(6) . . ?
C12 N3 C10 112.8(6) . . ?
C9 N3 C10 113.0(6) . . ?
C12 N3 Cu3 103.2(4) . . ?
C9 N3 Cu3 103.7(4) . . ?
C10 N3 Cu3 110.0(5) . . ?
C16 N4 C18 112.5(7) . . ?
C16 N4 C14 113.1(6) . . ?
C18 N4 C14 113.3(6) . . ?
C16 N4 Cu2 101.9(5) . . ?
C18 N4 Cu2 110.8(5) . . ?
C14 N4 Cu2 104.2(5) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C2 H2A 109.5 . . ?
O3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O7 C3 O8 124.1(8) . . ?
O7 C3 C4 116.6(7) . . ?
O8 C3 C4 119.4(7) . . ?
C5 C4 C7 112.0(10) . . ?
C5 C4 C3 113.2(8) . . ?
C7 C4 C3 109.2(8) . . ?
C5 C4 C6 111.6(9) . . ?
C7 C4 C6 103.3(10) . . ?
C3 C4 C6 107.0(8) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O12 C8 C9 109.0(6) . . ?
O12 C8 H8A 109.9 . . ?
C9 C8 H8A 109.9 . . ?
O12 C8 H8B 109.9 . . ?
C9 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N3 C9 C8 109.5(6) . . ?
N3 C9 H9A 109.8 . . ?
C8 C9 H9A 109.8 . . ?
N3 C9 H9B 109.8 . . ?
C8 C9 H9B 109.8 . . ?
H9A C9 H9B 108.2 . . ?
N3 C10 C11 115.4(6) . . ?
N3 C10 H10A 108.4 . . ?
C11 C10 H10A 108.4 . . ?
N3 C10 H10B 108.4 . . ?
C11 C10 H10B 108.4 . . ?
H10A C10 H10B 107.5 . . ?
O13 C11 C10 110.1(6) . . ?
O13 C11 H11A 109.6 . . ?
C10 C11 H11A 109.6 . . ?
O13 C11 H11B 109.6 . . ?
C10 C11 H11B 109.6 . . ?
H11A C11 H11B 108.2 . . ?
N3 C12 C13 109.7(6) . . ?
N3 C12 H12A 109.7 . . ?
C13 C12 H12A 109.7 . . ?
N3 C12 H12B 109.7 . . ?
C13 C12 H12B 109.7 . . ?
H12A C12 H12B 108.2 . . ?
O14 C13 C12 108.8(6) . . ?
O14 C13 H13A 109.9 . . ?
C12 C13 H13A 109.9 . . ?
O14 C13 H13B 109.9 . . ?
C12 C13 H13B 109.9 . . ?
H13A C13 H13B 108.3 . . ?
N4 C14 C15 106.7(6) . . ?
N4 C14 H14A 110.4 . . ?
C15 C14 H14A 110.4 . . ?
N4 C14 H14B 110.4 . . ?
C15 C14 H14B 110.4 . . ?
H14A C14 H14B 108.6 . . ?
O15 C15 C14 110.1(6) . . ?
O15 C15 H15A 109.6 . . ?
C14 C15 H15A 109.6 . . ?
O15 C15 H15B 109.6 . . ?
C14 C15 H15B 109.6 . . ?
H15A C15 H15B 108.2 . . ?
N4 C16 C17 108.3(6) . . ?
N4 C16 H16A 110.0 . . ?
C17 C16 H16A 110.0 . . ?
N4 C16 H16B 110.0 . . ?
C17 C16 H16B 110.0 . . ?
H16A C16 H16B 108.4 . . ?
O16 C17 C16 109.6(6) . . ?
O16 C17 H17A 109.7 . . ?
C16 C17 H17A 109.7 . . ?
O16 C17 H17B 109.7 . . ?
C16 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
N4 C18 C19 117.7(7) . . ?
N4 C18 H18A 107.9 . . ?
C19 C18 H18A 107.9 . . ?
N4 C18 H18B 107.9 . . ?
C19 C18 H18B 107.9 . . ?
H18A C18 H18B 107.2 . . ?
O17 C19 C18 108.9(7) . . ?
O17 C19 H19A 109.9 . . ?
C18 C19 H19A 109.9 . . ?
O17 C19 H19B 109.9 . . ?
C18 C19 H19B 109.9 . . ?
H19A C19 H19B 108.3 . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
C1S C2S O1S 106(2) . . ?
C1S C2S H2S1 110.5 . . ?
O1S C2S H2S1 110.5 . . ?
C1S C2S H2S2 110.5 . . ?
O1S C2S H2S2 110.5 . . ?
H2S1 C2S H2S2 108.7 . . ?
O1S C3S C4S 113.1(14) . . ?
O1S C3S H3S1 109.0 . . ?
C4S C3S H3S1 109.0 . . ?
O1S C3S H3S2 109.0 . . ?
C4S C3S H3S2 109.0 . . ?
H3S1 C3S H3S2 107.8 . . ?
C3S C4S H4S1 109.5 . . ?
C3S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
C3S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
O2S C5S H5S1 109.5 . . ?
O2S C5S H5S2 109.5 . . ?
H5S1 C5S H5S2 109.5 . . ?
O2S C5S H5S3 109.5 . . ?
H5S1 C5S H5S3 109.5 . . ?
H5S2 C5S H5S3 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         1.539
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.209
