# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1568172'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 B4 Cl6 Dy2 N24 O4'
_chemical_formula_weight         1553.97

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'
B B 0.0013 0.0007 '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'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   13.932(3)
_cell_length_b                   15.014(3)
_cell_length_c                   14.827(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.69(3)
_cell_angle_gamma                90
_cell_volume                     2954.8(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            violet
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_F_000             1524
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.845
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28184
_diffrn_reflns_av_unetI/netI     0.0864
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.757
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7240
_reflns_number_gt                5088
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
; 
 w=1/[σ²(Fo²)+(0.0230P)²+1.0981P] 
 where P=(Fo²+2Fc²)/3 
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7240
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0753
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.91723(2) 0.13112(2) 0.22525(2) 0.00783(6) Uani 1 1 d . . . . .
O1 O 0.9720(2) -0.00233(19) 0.1706(2) 0.0100(7) Uani 1 1 d . . . . .
O2 O 0.9283(2) 0.14261(19) 0.0696(2) 0.0112(7) Uani 1 1 d . . . . .
B1 B 1.1209(4) 0.2728(3) 0.3655(4) 0.0140(12) Uani 1 1 d . . . . .
H1 H 1.1760 0.3112 0.4019 0.017 Uiso 1 1 calc R U . . .
B2 B 0.6803(4) 0.0691(3) 0.2539(4) 0.0118(11) Uani 1 1 d . . . . .
H2 H 0.6164 0.0524 0.2641 0.014 Uiso 1 1 calc R U . . .
C1 C 0.7355(3) 0.0160(3) 0.0359(3) 0.0131(10) Uani 1 1 d . . . . .
H1A H 0.7746 0.0190 -0.0049 0.016 Uiso 1 1 calc R U . . .
C2 C 0.6465(4) -0.0316(3) 0.0174(3) 0.0164(11) Uani 1 1 d . . . . .
H2A H 0.6151 -0.0653 -0.0361 0.020 Uiso 1 1 calc R U . . .
C3 C 0.6148(3) -0.0180(3) 0.0955(3) 0.0142(11) Uani 1 1 d . . . . .
H3 H 0.5570 -0.0419 0.1049 0.017 Uiso 1 1 calc R U . . .
C4 C 0.7588(4) 0.3007(3) 0.2552(3) 0.0131(10) Uani 1 1 d . . . . .
H4 H 0.8024 0.3455 0.2489 0.016 Uiso 1 1 calc R U . . .
C5 C 0.6734(4) 0.3149(3) 0.2821(3) 0.0170(11) Uani 1 1 d . . . . .
H5 H 0.6487 0.3689 0.2963 0.020 Uiso 1 1 calc R U . . .
C6 C 0.6328(4) 0.2313(3) 0.2831(3) 0.0154(11) Uani 1 1 d . . . . .
H6 H 0.5748 0.2185 0.2993 0.018 Uiso 1 1 calc R U . . .
C7 C 0.9179(3) -0.0260(3) 0.3956(3) 0.0141(10) Uani 1 1 d . . . . .
H7 H 0.9860 -0.0386 0.4079 0.017 Uiso 1 1 calc R U . . .
C8 C 0.8597(3) -0.0557(3) 0.4496(3) 0.0137(10) Uani 1 1 d . . . . .
H8 H 0.8799 -0.0911 0.5035 0.016 Uiso 1 1 calc R U . . .
C9 C 0.7651(3) -0.0217(3) 0.4065(3) 0.0114(10) Uani 1 1 d . . . . .
H9 H 0.7088 -0.0298 0.4268 0.014 Uiso 1 1 calc R U . . .
C10 C 1.1652(3) 0.0435(3) 0.3091(3) 0.0147(11) Uani 1 1 d . . . . .
H10 H 1.1448 -0.0131 0.2855 0.018 Uiso 1 1 calc R U . . .
C11 C 1.2644(4) 0.0670(3) 0.3576(3) 0.0163(11) Uani 1 1 d . . . . .
H11 H 1.3213 0.0309 0.3713 0.020 Uiso 1 1 calc R U . . .
C12 C 1.2595(3) 0.1541(3) 0.3802(3) 0.0143(11) Uani 1 1 d . . . . .
H12 H 1.3138 0.1889 0.4140 0.017 Uiso 1 1 calc R U . . .
C13 C 0.9203(3) 0.1971(3) 0.4549(3) 0.0131(10) Uani 1 1 d . . . . .
H13 H 0.8618 0.1650 0.4499 0.016 Uiso 1 1 calc R U . . .
C14 C 0.9723(4) 0.2466(3) 0.5334(3) 0.0144(10) Uani 1 1 d . . . . .
H14 H 0.9564 0.2539 0.5895 0.017 Uiso 1 1 calc R U . . .
C15 C 1.0521(4) 0.2823(3) 0.5106(3) 0.0151(11) Uani 1 1 d . . . . .
H15 H 1.1012 0.3191 0.5493 0.018 Uiso 1 1 calc R U . . .
C16 C 1.0823(4) 0.3990(3) 0.2395(3) 0.0181(11) Uani 1 1 d . . . . .
H16 H 1.1335 0.4380 0.2706 0.022 Uiso 1 1 calc R U . . .
C17 C 1.0117(4) 0.4130(3) 0.1520(3) 0.0191(11) Uani 1 1 d . . . . .
H17 H 1.0047 0.4629 0.1133 0.023 Uiso 1 1 calc R U . . .
C18 C 0.9543(3) 0.3367(3) 0.1352(3) 0.0141(10) Uani 1 1 d . . . . .
H18 H 0.9009 0.3265 0.0807 0.017 Uiso 1 1 calc R U . . .
C19 C 0.9886(3) -0.0060(3) 0.0927(3) 0.0106(10) Uani 1 1 d . . . . .
C20 C 0.9599(3) 0.0789(3) 0.0307(3) 0.0108(10) Uani 1 1 d . . . . .
C21 C 0.9701(3) 0.0781(3) -0.0590(3) 0.0105(10) Uani 1 1 d . . . . .
C22 C 0.6859(6) 0.2716(4) 0.5390(5) 0.071(3) Uani 1 1 d . . . . .
H22A H 0.6129 0.2752 0.5180 0.085 Uiso 1 1 calc R U . . .
H22B H 0.7095 0.2948 0.4884 0.085 Uiso 1 1 calc R U . . .
Cl1 Cl 0.93405(9) 0.17106(7) -0.13141(8) 0.0160(3) Uani 1 1 d . . . . .
Cl2 Cl 0.72030(16) 0.16118(11) 0.55647(15) 0.0652(6) Uani 1 1 d . . . . .
Cl3 Cl 0.73130(16) 0.33890(13) 0.63705(12) 0.0624(6) Uani 1 1 d . . . . .
N1 N 0.7582(3) 0.0569(2) 0.1194(3) 0.0103(8) Uani 1 1 d . . . . .
N2 N 0.6817(3) 0.0357(2) 0.1563(3) 0.0101(8) Uani 1 1 d . . . . .
N3 N 0.8633(3) 0.0235(2) 0.3229(3) 0.0105(8) Uani 1 1 d . . . . .
N4 N 0.7679(3) 0.0252(2) 0.3299(3) 0.0095(8) Uani 1 1 d . . . . .
N5 N 0.7707(3) 0.2142(2) 0.2395(3) 0.0111(8) Uani 1 1 d . . . . .
N6 N 0.6909(3) 0.1717(2) 0.2569(3) 0.0118(8) Uani 1 1 d . . . . .
N7 N 1.1032(3) 0.1134(2) 0.3009(3) 0.0121(8) Uani 1 1 d . . . . .
N8 N 1.1637(3) 0.1820(2) 0.3460(3) 0.0123(8) Uani 1 1 d . . . . .
N9 N 0.9848(3) 0.2793(2) 0.2069(3) 0.0114(8) Uani 1 1 d . . . . .
N10 N 1.0638(3) 0.3187(2) 0.2716(3) 0.0122(9) Uani 1 1 d . . . . .
N11 N 0.9656(3) 0.2015(2) 0.3868(3) 0.0107(8) Uani 1 1 d . . . . .
N12 N 1.0479(3) 0.2552(2) 0.4223(3) 0.0120(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.366(3) . ?
Dy1 O1 2.372(3) . ?
Dy1 N3 2.436(4) . ?
Dy1 N5 2.456(4) . ?
Dy1 N9 2.463(4) . ?
Dy1 N7 2.506(4) . ?
Dy1 N11 2.515(4) . ?
Dy1 N1 2.550(4) . ?
O1 C19 1.248(5) . ?
O2 C20 1.264(5) . ?
B1 N12 1.528(7) . ?
B1 N10 1.540(6) . ?
B1 N8 1.551(6) . ?
B2 N2 1.538(6) . ?
B2 N4 1.536(6) . ?
B2 N6 1.546(6) . ?
C1 N1 1.330(5) . ?
C1 C2 1.385(6) . ?
C2 C3 1.374(7) . ?
C3 N2 1.349(5) . ?
C4 N5 1.339(5) . ?
C4 C5 1.381(6) . ?
C5 C6 1.378(6) . ?
C6 N6 1.342(6) . ?
C7 N3 1.339(5) . ?
C7 C8 1.375(6) . ?
C8 C9 1.376(6) . ?
C9 N4 1.347(5) . ?
C10 N7 1.340(5) . ?
C10 C11 1.395(6) . ?
C11 C12 1.357(6) . ?
C12 N8 1.343(5) . ?
C13 N11 1.344(6) . ?
C13 C14 1.386(6) . ?
C14 C15 1.366(7) . ?
C15 N12 1.355(6) . ?
C16 N10 1.349(6) . ?
C16 C17 1.385(6) . ?
C17 C18 1.376(6) . ?
C18 N9 1.333(5) . ?
C19 C21 1.387(6) 3_755 ?
C19 C20 1.551(6) . ?
C20 C21 1.381(6) . ?
C21 C19 1.387(6) 3_755 ?
C21 Cl1 1.739(4) . ?
C22 Cl2 1.724(6) . ?
C22 Cl3 1.725(6) . ?
N1 N2 1.375(5) . ?
N3 N4 1.364(5) . ?
N5 N6 1.373(5) . ?
N7 N8 1.369(5) . ?
N9 N10 1.356(5) . ?
N11 N12 1.370(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Dy1 O1 66.77(10) . . ?
O2 Dy1 N3 138.72(11) . . ?
O1 Dy1 N3 80.31(12) . . ?
O2 Dy1 N5 110.44(11) . . ?
O1 Dy1 N5 145.13(11) . . ?
N3 Dy1 N5 82.61(12) . . ?
O2 Dy1 N9 71.68(11) . . ?
O1 Dy1 N9 123.50(12) . . ?
N3 Dy1 N9 149.59(12) . . ?
N5 Dy1 N9 84.61(12) . . ?
O2 Dy1 N7 94.55(11) . . ?
O1 Dy1 N7 70.55(11) . . ?
N3 Dy1 N7 97.32(12) . . ?
N5 Dy1 N7 142.10(12) . . ?
N9 Dy1 N7 76.56(12) . . ?
O2 Dy1 N11 145.12(11) . . ?
O1 Dy1 N11 131.23(11) . . ?
N3 Dy1 N11 75.79(12) . . ?
N5 Dy1 N11 72.16(12) . . ?
N9 Dy1 N11 74.05(12) . . ?
N7 Dy1 N11 71.16(12) . . ?
O2 Dy1 N1 74.54(11) . . ?
O1 Dy1 N1 74.34(11) . . ?
N3 Dy1 N1 73.05(12) . . ?
N5 Dy1 N1 71.67(12) . . ?
N9 Dy1 N1 128.06(11) . . ?
N7 Dy1 N1 144.71(11) . . ?
N11 Dy1 N1 134.50(12) . . ?
C19 O1 Dy1 121.6(3) . . ?
C20 O2 Dy1 121.7(3) . . ?
N12 B1 N10 109.2(4) . . ?
N12 B1 N8 108.0(4) . . ?
N10 B1 N8 110.4(4) . . ?
N2 B2 N4 108.4(4) . . ?
N2 B2 N6 108.8(4) . . ?
N4 B2 N6 111.0(4) . . ?
N1 C1 C2 111.6(4) . . ?
C3 C2 C1 104.7(4) . . ?
N2 C3 C2 108.6(4) . . ?
N5 C4 C5 111.2(4) . . ?
C6 C5 C4 104.8(4) . . ?
N6 C6 C5 108.6(4) . . ?
N3 C7 C8 110.9(4) . . ?
C7 C8 C9 105.1(4) . . ?
N4 C9 C8 108.4(4) . . ?
N7 C10 C11 111.0(4) . . ?
C12 C11 C10 104.8(4) . . ?
N8 C12 C11 109.0(4) . . ?
N11 C13 C14 111.1(4) . . ?
C15 C14 C13 105.0(4) . . ?
N12 C15 C14 108.9(4) . . ?
N10 C16 C17 108.0(4) . . ?
C18 C17 C16 104.5(4) . . ?
N9 C18 C17 111.5(4) . . ?
O1 C19 C21 125.6(4) . 3_755 ?
O1 C19 C20 115.1(4) . . ?
C21 C19 C20 119.2(4) 3_755 . ?
O2 C20 C21 126.7(4) . . ?
O2 C20 C19 114.6(4) . . ?
C21 C20 C19 118.7(4) . . ?
C20 C21 C19 121.9(4) . 3_755 ?
C20 C21 Cl1 119.5(3) . . ?
C19 C21 Cl1 118.5(4) 3_755 . ?
Cl2 C22 Cl3 115.0(4) . . ?
C1 N1 N2 105.7(4) . . ?
C1 N1 Dy1 133.7(3) . . ?
N2 N1 Dy1 119.3(3) . . ?
C3 N2 N1 109.5(4) . . ?
C3 N2 B2 128.4(4) . . ?
N1 N2 B2 122.2(3) . . ?
C7 N3 N4 106.1(4) . . ?
C7 N3 Dy1 130.1(3) . . ?
N4 N3 Dy1 121.1(3) . . ?
C9 N4 N3 109.4(3) . . ?
C9 N4 B2 128.5(4) . . ?
N3 N4 B2 121.8(4) . . ?
C4 N5 N6 105.6(4) . . ?
C4 N5 Dy1 131.2(3) . . ?
N6 N5 Dy1 121.4(3) . . ?
C6 N6 N5 109.8(4) . . ?
C6 N6 B2 127.7(4) . . ?
N5 N6 B2 122.3(4) . . ?
C10 N7 N8 105.1(4) . . ?
C10 N7 Dy1 132.4(3) . . ?
N8 N7 Dy1 122.5(3) . . ?
C12 N8 N7 110.1(3) . . ?
C12 N8 B1 126.8(4) . . ?
N7 N8 B1 122.6(4) . . ?
C18 N9 N10 106.0(4) . . ?
C18 N9 Dy1 129.2(3) . . ?
N10 N9 Dy1 124.8(3) . . ?
C16 N10 N9 110.0(4) . . ?
C16 N10 B1 128.1(4) . . ?
N9 N10 B1 122.0(4) . . ?
C13 N11 N12 105.7(4) . . ?
C13 N11 Dy1 130.0(3) . . ?
N12 N11 Dy1 124.3(3) . . ?
C15 N12 N11 109.4(4) . . ?
C15 N12 B1 129.8(4) . . ?
N11 N12 B1 120.7(4) . . ?

_refine_diff_density_max         1.083
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.180

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1568175'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 B4 Cl6 N24 O4 Y2'
_chemical_formula_weight         1406.79

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'
B B 0.0013 0.0007 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.937(3)
_cell_length_b                   15.046(3)
_cell_length_c                   14.786(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.46(3)
_cell_angle_gamma                90
_cell_volume                     2957.8(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    2.287
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25422
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.762
_diffrn_reflns_theta_max         26.414
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6076
_reflns_number_gt                3984
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0511P)²+3.0850P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6076
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.1203
_refine_ls_wR_factor_gt          0.1054
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.41745(3) 0.13066(3) 0.22513(3) 0.01172(12) Uani 1 1 d . . . . .
B1 B 0.6196(4) 0.2728(3) 0.3643(4) 0.0188(12) Uani 1 1 d . . . . .
H1 H 0.6746 0.3113 0.4003 0.023 Uiso 1 1 calc R U . . .
B2 B 0.1804(4) 0.0701(3) 0.2541(4) 0.0188(12) Uani 1 1 d . . . . .
H2 H 0.1165 0.0539 0.2647 0.023 Uiso 1 1 calc R U . . .
O1 O 0.4712(2) -0.00248(18) 0.1711(2) 0.0148(7) Uani 1 1 d . . . . .
O2 O 0.4286(2) 0.14191(18) 0.0695(2) 0.0167(7) Uani 1 1 d . . . . .
N1 N 0.5471(3) 0.2551(2) 0.4224(2) 0.0167(8) Uani 1 1 d . . . . .
N2 N 0.4660(3) 0.2005(2) 0.3875(3) 0.0160(8) Uani 1 1 d . . . . .
N3 N 0.6625(3) 0.1821(2) 0.3448(3) 0.0175(9) Uani 1 1 d . . . . .
N4 N 0.6028(3) 0.1134(2) 0.2994(2) 0.0158(8) Uani 1 1 d . . . . .
N5 N 0.5626(3) 0.3179(2) 0.2706(3) 0.0173(9) Uani 1 1 d . . . . .
N6 N 0.4833(3) 0.2783(2) 0.2056(3) 0.0176(9) Uani 1 1 d . . . . .
N7 N 0.2682(3) 0.0256(2) 0.3301(2) 0.0145(8) Uani 1 1 d . . . . .
N8 N 0.3638(3) 0.0245(2) 0.3228(2) 0.0138(8) Uani 1 1 d . . . . .
N9 N 0.1819(3) 0.0361(2) 0.1566(3) 0.0143(8) Uani 1 1 d . . . . .
N10 N 0.2589(3) 0.0574(2) 0.1201(2) 0.0149(8) Uani 1 1 d . . . . .
N11 N 0.1922(3) 0.1721(2) 0.2572(3) 0.0161(8) Uani 1 1 d . . . . .
N12 N 0.2717(3) 0.2138(2) 0.2391(3) 0.0162(8) Uani 1 1 d . . . . .
C1 C 0.4534(3) 0.3357(3) 0.1343(3) 0.0194(10) Uani 1 1 d . . . . .
H1A H 0.3999 0.3257 0.0799 0.023 Uiso 1 1 calc R U . . .
C2 C 0.5108(4) 0.4112(3) 0.1506(3) 0.0254(11) Uani 1 1 d . . . . .
H2A H 0.5044 0.4605 0.1113 0.030 Uiso 1 1 calc R U . . .
C3 C 0.5801(4) 0.3980(3) 0.2379(4) 0.0255(12) Uani 1 1 d . . . . .
H3 H 0.6304 0.4376 0.2691 0.031 Uiso 1 1 calc R U . . .
C4 C 0.6649(3) 0.0439(3) 0.3072(3) 0.0216(11) Uani 1 1 d . . . . .
H4 H 0.6447 -0.0125 0.2830 0.026 Uiso 1 1 calc R U . . .
C5 C 0.7634(4) 0.0668(3) 0.3560(3) 0.0243(11) Uani 1 1 d . . . . .
H5 H 0.8202 0.0307 0.3704 0.029 Uiso 1 1 calc R U . . .
C6 C 0.7578(3) 0.1545(3) 0.3780(3) 0.0211(11) Uani 1 1 d . . . . .
H6 H 0.8120 0.1896 0.4111 0.025 Uiso 1 1 calc R U . . .
C7 C 0.4209(4) 0.1969(3) 0.4549(3) 0.0192(10) Uani 1 1 d . . . . .
H7 H 0.3623 0.1651 0.4500 0.023 Uiso 1 1 calc R U . . .
C8 C 0.4723(4) 0.2466(3) 0.5331(3) 0.0207(11) Uani 1 1 d . . . . .
H8 H 0.4561 0.2540 0.5893 0.025 Uiso 1 1 calc R U . . .
C9 C 0.5521(4) 0.2824(3) 0.5102(3) 0.0208(11) Uani 1 1 d . . . . .
H9 H 0.6012 0.3192 0.5486 0.025 Uiso 1 1 calc R U . . .
C10 C 0.1340(4) 0.2320(3) 0.2832(3) 0.0202(11) Uani 1 1 d . . . . .
H10 H 0.0758 0.2193 0.2991 0.024 Uiso 1 1 calc R U . . .
C11 C 0.1748(4) 0.3151(3) 0.2825(3) 0.0241(11) Uani 1 1 d . . . . .
H11 H 0.1506 0.3690 0.2974 0.029 Uiso 1 1 calc R U . . .
C12 C 0.2601(4) 0.3007(3) 0.2548(3) 0.0215(11) Uani 1 1 d . . . . .
H12 H 0.3036 0.3452 0.2480 0.026 Uiso 1 1 calc R U . . .
C13 C 0.1149(4) -0.0169(3) 0.0954(3) 0.0212(11) Uani 1 1 d . . . . .
H13 H 0.0567 -0.0403 0.1047 0.025 Uiso 1 1 calc R U . . .
C14 C 0.1468(4) -0.0306(3) 0.0175(3) 0.0242(11) Uani 1 1 d . . . . .
H14 H 0.1154 -0.0645 -0.0358 0.029 Uiso 1 1 calc R U . . .
C15 C 0.2360(3) 0.0168(3) 0.0349(3) 0.0177(10) Uani 1 1 d . . . . .
H15 H 0.2746 0.0202 -0.0065 0.021 Uiso 1 1 calc R U . . .
C16 C 0.2652(4) -0.0216(3) 0.4062(3) 0.0180(10) Uani 1 1 d . . . . .
H16 H 0.2088 -0.0298 0.4266 0.022 Uiso 1 1 calc R U . . .
C17 C 0.3598(3) -0.0560(3) 0.4493(3) 0.0205(11) Uani 1 1 d . . . . .
H17 H 0.3798 -0.0919 0.5029 0.025 Uiso 1 1 calc R U . . .
C18 C 0.4178(4) -0.0252(3) 0.3953(3) 0.0201(10) Uani 1 1 d . . . . .
H18 H 0.4859 -0.0375 0.4077 0.024 Uiso 1 1 calc R U . . .
C19 C 0.5291(3) -0.0782(3) 0.0590(3) 0.0137(9) Uani 1 1 d . . . . .
C20 C 0.4884(3) -0.0055(3) 0.0931(3) 0.0127(9) Uani 1 1 d . . . . .
C21 C 0.4604(3) 0.0788(3) 0.0317(3) 0.0134(9) Uani 1 1 d . . . . .
C22 C 0.6852(7) 0.2293(5) 0.0388(6) 0.102(3) Uani 1 1 d . . . . .
H22A H 0.7079 0.2062 -0.0125 0.122 Uiso 1 1 calc R U . . .
H22B H 0.6124 0.2255 0.0191 0.122 Uiso 1 1 calc R U . . .
Cl1 Cl 0.56492(9) -0.17092(7) 0.13089(8) 0.0224(3) Uani 1 1 d . . . . .
Cl2 Cl 0.73235(19) 0.16261(16) 0.13700(14) 0.0905(7) Uani 1 1 d . . . . .
Cl3 Cl 0.71924(19) 0.33959(14) 0.05566(19) 0.0962(8) Uani 1 1 d . . . . .


_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
Y1 O2 2.358(3) . ?
Y1 O1 2.361(3) . ?
Y1 N8 2.418(4) . ?
Y1 N12 2.446(4) . ?
Y1 N6 2.453(4) . ?
Y1 N4 2.499(4) . ?
Y1 N2 2.520(4) . ?
Y1 N10 2.540(4) . ?
B1 N5 1.533(6) . ?
B1 N1 1.533(6) . ?
B1 N3 1.552(6) . ?
B2 N9 1.536(6) . ?
B2 N7 1.543(6) . ?
B2 N11 1.543(6) . ?
O1 C20 1.246(5) . ?
O2 C21 1.249(5) . ?
N1 C9 1.343(6) . ?
N1 N2 1.366(5) . ?
N2 C7 1.330(6) . ?
N3 C6 1.337(6) . ?
N3 N4 1.369(5) . ?
N4 C4 1.341(5) . ?
N5 C3 1.348(6) . ?
N5 N6 1.365(5) . ?
N6 C1 1.328(5) . ?
N7 C16 1.342(5) . ?
N7 N8 1.370(5) . ?
N8 C18 1.338(5) . ?
N9 C13 1.348(5) . ?
N9 N10 1.376(5) . ?
N10 C15 1.348(5) . ?
N11 C10 1.344(5) . ?
N11 N12 1.368(5) . ?
N12 C12 1.346(5) . ?
C1 C2 1.369(6) . ?
C2 C3 1.375(7) . ?
C4 C5 1.389(7) . ?
C5 C6 1.367(7) . ?
C7 C8 1.383(6) . ?
C8 C9 1.367(7) . ?
C10 C11 1.376(7) . ?
C11 C12 1.385(7) . ?
C13 C14 1.369(7) . ?
C14 C15 1.390(6) . ?
C16 C17 1.381(6) . ?
C17 C18 1.375(6) . ?
C19 C21 1.392(6) 3_655 ?
C19 C20 1.395(6) . ?
C19 Cl1 1.734(4) . ?
C20 C21 1.540(6) . ?
C21 C19 1.392(6) 3_655 ?
C22 Cl3 1.723(7) . ?
C22 Cl2 1.725(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Y1 O1 67.03(10) . . ?
O2 Y1 N8 138.86(11) . . ?
O1 Y1 N8 80.10(11) . . ?
O2 Y1 N12 110.20(11) . . ?
O1 Y1 N12 144.93(11) . . ?
N8 Y1 N12 82.78(12) . . ?
O2 Y1 N6 71.55(11) . . ?
O1 Y1 N6 124.09(11) . . ?
N8 Y1 N6 149.58(12) . . ?
N12 Y1 N6 84.04(12) . . ?
O2 Y1 N4 94.23(11) . . ?
O1 Y1 N4 70.69(11) . . ?
N8 Y1 N4 97.64(12) . . ?
N12 Y1 N4 142.29(11) . . ?
N6 Y1 N4 76.82(11) . . ?
O2 Y1 N2 145.29(11) . . ?
O1 Y1 N2 130.89(11) . . ?
N8 Y1 N2 75.47(12) . . ?
N12 Y1 N2 72.48(12) . . ?
N6 Y1 N2 74.45(12) . . ?
N4 Y1 N2 71.21(12) . . ?
O2 Y1 N10 74.61(11) . . ?
O1 Y1 N10 74.39(11) . . ?
N8 Y1 N10 73.17(11) . . ?
N12 Y1 N10 71.42(11) . . ?
N6 Y1 N10 127.46(12) . . ?
N4 Y1 N10 144.96(11) . . ?
N2 Y1 N10 134.36(12) . . ?
N5 B1 N1 109.4(4) . . ?
N5 B1 N3 110.2(4) . . ?
N1 B1 N3 107.9(4) . . ?
N9 B2 N7 108.0(4) . . ?
N9 B2 N11 109.1(4) . . ?
N7 B2 N11 110.8(4) . . ?
C20 O1 Y1 120.8(3) . . ?
C21 O2 Y1 121.2(3) . . ?
C9 N1 N2 110.2(4) . . ?
C9 N1 B1 129.5(4) . . ?
N2 N1 B1 120.2(3) . . ?
C7 N2 N1 105.4(3) . . ?
C7 N2 Y1 130.2(3) . . ?
N1 N2 Y1 124.4(3) . . ?
C6 N3 N4 109.7(4) . . ?
C6 N3 B1 126.9(4) . . ?
N4 N3 B1 122.9(3) . . ?
C4 N4 N3 105.4(3) . . ?
C4 N4 Y1 132.4(3) . . ?
N3 N4 Y1 122.2(3) . . ?
C3 N5 N6 109.4(4) . . ?
C3 N5 B1 128.3(4) . . ?
N6 N5 B1 122.3(3) . . ?
C1 N6 N5 105.7(3) . . ?
C1 N6 Y1 130.0(3) . . ?
N5 N6 Y1 124.4(3) . . ?
C16 N7 N8 109.6(3) . . ?
C16 N7 B2 128.6(4) . . ?
N8 N7 B2 121.7(4) . . ?
C18 N8 N7 105.7(4) . . ?
C18 N8 Y1 130.4(3) . . ?
N7 N8 Y1 121.4(2) . . ?
C13 N9 N10 109.9(4) . . ?
C13 N9 B2 128.6(4) . . ?
N10 N9 B2 121.5(4) . . ?
C15 N10 N9 105.4(3) . . ?
C15 N10 Y1 133.3(3) . . ?
N9 N10 Y1 120.0(2) . . ?
C10 N11 N12 110.1(4) . . ?
C10 N11 B2 127.4(4) . . ?
N12 N11 B2 122.4(4) . . ?
C12 N12 N11 105.3(4) . . ?
C12 N12 Y1 131.1(3) . . ?
N11 N12 Y1 121.6(2) . . ?
N6 C1 C2 111.9(4) . . ?
C1 C2 C3 104.7(4) . . ?
N5 C3 C2 108.3(4) . . ?
N4 C4 C5 111.3(4) . . ?
C6 C5 C4 104.2(4) . . ?
N3 C6 C5 109.5(4) . . ?
N2 C7 C8 111.2(4) . . ?
C9 C8 C7 105.1(4) . . ?
N1 C9 C8 108.0(4) . . ?
N11 C10 C11 108.7(4) . . ?
C10 C11 C12 104.6(4) . . ?
N12 C12 C11 111.3(4) . . ?
N9 C13 C14 108.6(4) . . ?
C13 C14 C15 105.4(4) . . ?
N10 C15 C14 110.7(4) . . ?
N7 C16 C17 108.7(4) . . ?
C18 C17 C16 104.6(4) . . ?
N8 C18 C17 111.5(4) . . ?
C21 C19 C20 121.7(4) 3_655 . ?
C21 C19 Cl1 119.4(3) 3_655 . ?
C20 C19 Cl1 118.9(3) . . ?
O1 C20 C19 125.1(4) . . ?
O1 C20 C21 115.5(4) . . ?
C19 C20 C21 119.4(4) . . ?
O2 C21 C19 126.2(4) . 3_655 ?
O2 C21 C20 115.1(4) . . ?
C19 C21 C20 118.8(4) 3_655 . ?
Cl3 C22 Cl2 114.8(5) . . ?

_refine_diff_density_max         0.416
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.104

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_b
_database_code_depnum_ccdc_archive 'CCDC 1568174'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 B4 Cl6 Gd2 N24 O4'
_chemical_formula_weight         1543.47

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'
B B 0.0013 0.0007 '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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.150(3)
_cell_length_b                   15.225(3)
_cell_length_c                   14.969(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.75(3)
_cell_angle_gamma                90
_cell_volume                     3071.3(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_F_000             1516
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.463
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_T_max  0.691
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28469
_diffrn_reflns_av_unetI/netI     0.4480
_diffrn_reflns_av_R_equivalents  0.3682
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.734
_diffrn_reflns_theta_max         29.175
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8275
_reflns_number_gt                2723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8275
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2825
_refine_ls_R_factor_gt           0.0933
_refine_ls_wR_factor_ref         0.1463
_refine_ls_wR_factor_gt          0.0989
_refine_ls_goodness_of_fit_ref   0.814
_refine_ls_restrained_S_all      0.814
_refine_ls_shift/su_max          0.000
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.08251(6) 0.13048(5) 0.77538(5) 0.02445(16) Uani 1 1 d . . . . .
B1 B 0.3178(15) 0.0700(11) 0.7461(13) 0.037(5) Uani 1 1 d . . . . .
H1 H 0.3809 0.0542 0.7360 0.044 Uiso 1 1 calc R U . . .
B2 B -0.1210(14) 0.2715(12) 0.6347(12) 0.041(5) Uani 1 1 d . . . . .
H2 H -0.1756 0.3092 0.5990 0.049 Uiso 1 1 calc R U . . .
O1 O 0.0708(7) 0.1414(6) 0.9317(5) 0.037(2) Uani 1 1 d . . . . .
O2 O 0.0291(7) -0.0029(6) 0.8319(6) 0.034(3) Uani 1 1 d . . . . .
N1 N 0.2417(9) 0.0574(7) 0.8789(8) 0.038(3) Uani 1 1 d . . . . .
N2 N 0.3165(9) 0.0359(7) 0.8441(8) 0.033(3) Uani 1 1 d . . . . .
N3 N 0.2281(9) 0.2125(7) 0.7596(7) 0.029(3) Uani 1 1 d . . . . .
N4 N 0.3063(10) 0.1698(8) 0.7438(8) 0.039(3) Uani 1 1 d . . . . .
N5 N 0.1377(8) 0.0256(7) 0.6774(8) 0.029(3) Uani 1 1 d . . . . .
N6 N 0.2314(8) 0.0267(7) 0.6702(8) 0.032(3) Uani 1 1 d . . . . .
N7 N 0.0159(10) 0.2787(7) 0.7935(8) 0.041(3) Uani 1 1 d . . . . .
N8 N -0.0623(10) 0.3168(7) 0.7290(10) 0.043(4) Uani 1 1 d . . . . .
N9 N -0.1028(9) 0.1145(7) 0.7016(7) 0.042(3) Uani 1 1 d . . . . .
N10 N -0.1611(9) 0.1833(8) 0.6561(8) 0.037(3) Uani 1 1 d . . . . .
N11 N 0.0320(9) 0.2021(8) 0.6134(8) 0.039(3) Uani 1 1 d . . . . .
N12 N -0.0484(8) 0.2545(6) 0.5784(7) 0.031(3) Uani 1 1 d . . . . .
C1 C 0.3642(12) 0.2289(10) 0.7169(11) 0.050(4) Uani 1 1 d . . . . .
H1A H 0.4209 0.2154 0.7008 0.060 Uiso 1 1 calc R U . . .
C2 C 0.3262(13) 0.3114(10) 0.7173(10) 0.055(5) Uani 1 1 d . . . . .
H2A H 0.3504 0.3642 0.7021 0.066 Uiso 1 1 calc R U . . .
C3 C 0.2424(11) 0.2973(9) 0.7461(10) 0.041(4) Uani 1 1 d . . . . .
H3 H 0.2013 0.3420 0.7549 0.049 Uiso 1 1 calc R U . . .
C4 C 0.3856(11) -0.0153(9) 0.9023(11) 0.048(4) Uani 1 1 d . . . . .
H4 H 0.4432 -0.0371 0.8928 0.058 Uiso 1 1 calc R U . . .
C5 C 0.3520(12) -0.0289(11) 0.9810(12) 0.059(5) Uani 1 1 d . . . . .
H5 H 0.3818 -0.0624 1.0340 0.071 Uiso 1 1 calc R U . . .
C6 C 0.2667(12) 0.0177(10) 0.9620(11) 0.053(4) Uani 1 1 d . . . . .
H6 H 0.2292 0.0216 1.0032 0.063 Uiso 1 1 calc R U . . .
C7 C 0.2357(11) -0.0218(9) 0.5938(10) 0.041(4) Uani 1 1 d . . . . .
H7 H 0.2910 -0.0305 0.5736 0.049 Uiso 1 1 calc R U . . .
C8 C 0.1421(12) -0.0545(10) 0.5537(12) 0.053(5) Uani 1 1 d . . . . .
H8 H 0.1223 -0.0905 0.5010 0.063 Uiso 1 1 calc R U . . .
C9 C 0.0824(12) -0.0248(9) 0.6050(9) 0.041(4) Uani 1 1 d . . . . .
H9 H 0.0152 -0.0371 0.5923 0.049 Uiso 1 1 calc R U . . .
C10 C -0.2572(12) 0.1581(11) 0.6225(11) 0.051(5) Uani 1 1 d . . . . .
H10 H -0.3098 0.1931 0.5885 0.061 Uiso 1 1 calc R U . . .
C11 C -0.2637(14) 0.0727(12) 0.6469(12) 0.059(6) Uani 1 1 d . . . . .
H11 H -0.3202 0.0379 0.6355 0.070 Uiso 1 1 calc R U . . .
C12 C -0.1656(13) 0.0499(11) 0.6930(11) 0.045(5) Uani 1 1 d . . . . .
H12 H -0.1465 -0.0063 0.7157 0.055 Uiso 1 1 calc R U . . .
C13 C -0.0529(13) 0.2810(10) 0.4906(10) 0.051(5) Uani 1 1 d . . . . .
H13 H -0.1020 0.3166 0.4520 0.061 Uiso 1 1 calc R U . . .
C14 C 0.0249(12) 0.2476(10) 0.4682(10) 0.041(4) Uani 1 1 d . . . . .
H14 H 0.0413 0.2568 0.4133 0.050 Uiso 1 1 calc R U . . .
C15 C 0.0751(12) 0.1970(10) 0.5436(11) 0.045(4) Uani 1 1 d . . . . .
H15 H 0.1311 0.1637 0.5467 0.054 Uiso 1 1 calc R U . . .
C16 C -0.0806(12) 0.3955(10) 0.7599(12) 0.053(5) Uani 1 1 d . . . . .
H16 H -0.1307 0.4338 0.7281 0.064 Uiso 1 1 calc R U . . .
C17 C -0.0126(12) 0.4106(10) 0.8474(14) 0.061(5) Uani 1 1 d . . . . .
H17 H -0.0076 0.4594 0.8859 0.073 Uiso 1 1 calc R U . . .
C18 C 0.0457(11) 0.3367(9) 0.8638(10) 0.040(4) Uani 1 1 d . . . . .
H18 H 0.0995 0.3280 0.9173 0.048 Uiso 1 1 calc R U . . .
C19 C 0.0112(10) -0.0042(9) 0.9065(11) 0.034(4) Uani 1 1 d . . . . .
C20 C 0.0397(10) 0.0787(8) 0.9667(9) 0.025(3) Uani 1 1 d . . . . .
C21 C 0.0267(10) 0.0763(8) 1.0574(9) 0.028(3) Uani 1 1 d . . . . .
C22 C 0.820(3) 0.234(3) 0.951(3) 0.27(3) Uani 1 1 d . . . . .
H22A H 0.8900 0.2346 0.9569 0.325 Uiso 1 1 calc R U . . .
H22B H 0.8136 0.2106 1.0095 0.325 Uiso 1 1 calc R U . . .
Cl1 Cl 0.0623(3) 0.1695(2) 1.1285(3) 0.0531(12) Uani 1 1 d . . . . .
Cl2 Cl 0.7809(9) 0.3380(6) 0.9424(8) 0.250(6) Uani 1 1 d . . . . .
Cl3 Cl 0.7640(10) 0.1686(8) 0.8670(8) 0.248(6) Uani 1 1 d . . . . .


_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 O1 2.402(7) . ?
Gd1 O2 2.409(9) . ?
Gd1 N5 2.452(11) . ?
Gd1 N3 2.480(11) . ?
Gd1 N7 2.492(12) . ?
Gd1 N9 2.528(13) . ?
Gd1 N11 2.554(11) . ?
Gd1 N1 2.565(11) . ?
B1 N4 1.529(17) . ?
B1 N6 1.54(2) . ?
B1 N2 1.56(2) . ?
B2 N10 1.53(2) . ?
B2 N12 1.537(19) . ?
B2 N8 1.56(2) . ?
O1 C20 1.232(14) . ?
O2 C19 1.219(15) . ?
N1 C6 1.331(17) . ?
N1 N2 1.355(15) . ?
N2 C4 1.343(16) . ?
N3 C3 1.332(15) . ?
N3 N4 1.364(16) . ?
N4 C1 1.358(17) . ?
N5 N6 1.362(13) . ?
N5 C9 1.362(15) . ?
N6 C7 1.378(16) . ?
N7 C18 1.340(16) . ?
N7 N8 1.359(16) . ?
N8 C16 1.337(16) . ?
N9 C12 1.304(17) . ?
N9 N10 1.377(14) . ?
N10 C10 1.355(18) . ?
N11 N12 1.357(14) . ?
N11 C15 1.363(17) . ?
N12 C13 1.357(16) . ?
C1 C2 1.366(19) . ?
C2 C3 1.397(19) . ?
C4 C5 1.41(2) . ?
C5 C6 1.353(19) . ?
C7 C8 1.371(19) . ?
C8 C9 1.381(19) . ?
C10 C11 1.36(2) . ?
C11 C12 1.39(2) . ?
C13 C14 1.35(2) . ?
C14 C15 1.373(19) . ?
C16 C17 1.39(2) . ?
C17 C18 1.372(17) . ?
C19 C21 1.401(17) 3_557 ?
C19 C20 1.532(17) . ?
C20 C21 1.424(17) . ?
C21 C19 1.401(17) 3_557 ?
C21 Cl1 1.753(12) . ?
C22 Cl3 1.62(3) . ?
C22 Cl2 1.66(3) . ?

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
O1 Gd1 O2 66.0(3) . . ?
O1 Gd1 N5 139.2(3) . . ?
O2 Gd1 N5 81.5(3) . . ?
O1 Gd1 N3 111.3(3) . . ?
O2 Gd1 N3 144.7(3) . . ?
N5 Gd1 N3 81.1(3) . . ?
O1 Gd1 N7 72.0(4) . . ?
O2 Gd1 N7 123.8(3) . . ?
N5 Gd1 N7 148.8(4) . . ?
N3 Gd1 N7 84.7(4) . . ?
O1 Gd1 N9 93.5(3) . . ?
O2 Gd1 N9 71.2(3) . . ?
N5 Gd1 N9 98.8(4) . . ?
N3 Gd1 N9 142.0(4) . . ?
N7 Gd1 N9 76.0(4) . . ?
O1 Gd1 N11 144.4(4) . . ?
O2 Gd1 N11 131.8(3) . . ?
N5 Gd1 N11 76.0(4) . . ?
N3 Gd1 N11 72.2(4) . . ?
N7 Gd1 N11 73.2(4) . . ?
N9 Gd1 N11 70.9(4) . . ?
O1 Gd1 N1 75.5(4) . . ?
O2 Gd1 N1 74.6(3) . . ?
N5 Gd1 N1 72.4(4) . . ?
N3 Gd1 N1 71.0(4) . . ?
N7 Gd1 N1 128.2(4) . . ?
N9 Gd1 N1 145.6(4) . . ?
N11 Gd1 N1 134.3(4) . . ?
N4 B1 N6 110.7(14) . . ?
N4 B1 N2 108.6(13) . . ?
N6 B1 N2 108.5(13) . . ?
N10 B2 N12 108.6(12) . . ?
N10 B2 N8 109.1(12) . . ?
N12 B2 N8 108.1(13) . . ?
C20 O1 Gd1 120.0(8) . . ?
C19 O2 Gd1 120.7(9) . . ?
C6 N1 N2 103.5(12) . . ?
C6 N1 Gd1 134.1(11) . . ?
N2 N1 Gd1 121.2(8) . . ?
C4 N2 N1 113.1(12) . . ?
C4 N2 B1 125.9(14) . . ?
N1 N2 B1 121.0(12) . . ?
C3 N3 N4 105.4(12) . . ?
C3 N3 Gd1 132.2(10) . . ?
N4 N3 Gd1 121.2(8) . . ?
C1 N4 N3 109.3(13) . . ?
C1 N4 B1 126.6(15) . . ?
N3 N4 B1 123.8(13) . . ?
N6 N5 C9 106.4(11) . . ?
N6 N5 Gd1 122.3(8) . . ?
C9 N5 Gd1 129.2(9) . . ?
N5 N6 C7 110.4(11) . . ?
N5 N6 B1 121.3(11) . . ?
C7 N6 B1 128.0(13) . . ?
C18 N7 N8 105.6(12) . . ?
C18 N7 Gd1 130.1(11) . . ?
N8 N7 Gd1 124.3(9) . . ?
C16 N8 N7 109.8(14) . . ?
C16 N8 B2 127.1(14) . . ?
N7 N8 B2 123.2(11) . . ?
C12 N9 N10 103.8(13) . . ?
C12 N9 Gd1 134.4(11) . . ?
N10 N9 Gd1 121.8(8) . . ?
C10 N10 N9 110.5(12) . . ?
C10 N10 B2 124.4(14) . . ?
N9 N10 B2 124.6(12) . . ?
N12 N11 C15 104.8(11) . . ?
N12 N11 Gd1 125.2(8) . . ?
C15 N11 Gd1 130.0(10) . . ?
N11 N12 C13 109.6(12) . . ?
N11 N12 B2 120.6(11) . . ?
C13 N12 B2 129.7(13) . . ?
N4 C1 C2 109.5(14) . . ?
C1 C2 C3 103.4(13) . . ?
N3 C3 C2 112.2(13) . . ?
N2 C4 C5 105.1(13) . . ?
C6 C5 C4 104.7(15) . . ?
N1 C6 C5 113.6(16) . . ?
C8 C7 N6 106.1(13) . . ?
C7 C8 C9 108.1(14) . . ?
N5 C9 C8 109.0(14) . . ?
N10 C10 C11 108.2(16) . . ?
C10 C11 C12 103.4(16) . . ?
N9 C12 C11 114.0(15) . . ?
C14 C13 N12 109.2(14) . . ?
C13 C14 C15 105.3(13) . . ?
N11 C15 C14 111.0(13) . . ?
N8 C16 C17 108.9(15) . . ?
C18 C17 C16 103.9(14) . . ?
N7 C18 C17 111.8(15) . . ?
O2 C19 C21 125.2(13) . 3_557 ?
O2 C19 C20 115.8(12) . . ?
C21 C19 C20 118.8(12) 3_557 . ?
O1 C20 C21 126.2(11) . . ?
O1 C20 C19 116.9(11) . . ?
C21 C20 C19 116.9(11) . . ?
C19 C21 C20 124.3(12) 3_557 . ?
C19 C21 Cl1 118.2(10) 3_557 . ?
C20 C21 Cl1 117.5(9) . . ?
Cl3 C22 Cl2 117(2) . . ?

_refine_diff_density_max         0.943
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.174

_shelxl_version_number           2013-2

####################################################################### 
# 
# 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_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1568173'
_audit_update_record             
;
2017-08-10 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H44 B4 Cl6 N24 O4 Tb2'
_chemical_formula_weight         1546.81

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'
B B 0.0013 0.0007 '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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.003(3)
_cell_length_b                   15.079(3)
_cell_length_c                   14.825(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.59(3)
_cell_angle_gamma                90
_cell_volume                     2983.9(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    2.683
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_T_max  0.634
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27465
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.754
_diffrn_reflns_theta_max         28.307
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7353
_reflns_number_gt                5471
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0484P)²+8.1775P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7353
_refine_ls_number_parameters     379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.1078
_refine_ls_wR_factor_gt          0.0960
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.41672(2) 0.13120(2) 0.72538(2) 0.01230(8) Uani 1 1 d . . . . .
B1 B 0.1798(4) 0.0703(4) 0.7543(4) 0.0186(12) Uani 1 1 d . . . . .
H1 H 0.1161 0.0542 0.7645 0.022 Uiso 1 1 calc R U . . .
B2 B 0.6201(5) 0.2726(4) 0.8652(4) 0.0215(13) Uani 1 1 d . . . . .
H19 H 0.6749 0.3109 0.9015 0.026 Uiso 1 1 calc R U . . .
Cl1 Cl 0.43563(11) 0.17063(9) 0.36904(9) 0.0244(3) Uani 1 1 d . . . . .
Cl2 Cl 0.2195(3) 0.1599(2) 0.0561(3) 0.1395(16) Uani 1 1 d . . . . .
Cl3 Cl 0.2315(3) 0.3379(3) 0.1360(2) 0.1274(14) Uani 1 1 d . . . . .
O1 O 0.4710(3) -0.0024(2) 0.6708(2) 0.0163(7) Uani 1 1 d . . . . .
O2 O 0.4283(3) 0.1419(2) 0.5689(2) 0.0174(7) Uani 1 1 d . . . . .
N1 N 0.1914(3) 0.1716(3) 0.7578(3) 0.0172(9) Uani 1 1 d . . . . .
N2 N 0.2701(3) 0.2142(3) 0.7402(3) 0.0179(9) Uani 1 1 d . . . . .
N3 N 0.2670(3) 0.0258(3) 0.8308(3) 0.0149(9) Uani 1 1 d . . . . .
N4 N 0.3619(3) 0.0240(3) 0.8232(3) 0.0153(9) Uani 1 1 d . . . . .
N5 N 0.1813(3) 0.0363(3) 0.6566(3) 0.0169(9) Uani 1 1 d . . . . .
N6 N 0.2577(3) 0.0572(3) 0.6203(3) 0.0159(9) Uani 1 1 d . . . . .
N7 N 0.6040(3) 0.1150(3) 0.7996(3) 0.0187(9) Uani 1 1 d . . . . .
N8 N 0.6632(3) 0.1832(3) 0.8459(3) 0.0191(9) Uani 1 1 d . . . . .
N9 N 0.4662(3) 0.2010(3) 0.8877(3) 0.0169(9) Uani 1 1 d . . . . .
N10 N 0.5482(3) 0.2549(3) 0.9233(3) 0.0188(9) Uani 1 1 d . . . . .
N11 N 0.4837(3) 0.2797(3) 0.7074(3) 0.0206(10) Uani 1 1 d . . . . .
N12 N 0.5631(3) 0.3191(3) 0.7716(3) 0.0205(10) Uani 1 1 d . . . . .
C1 C 0.1329(4) 0.2312(4) 0.7835(4) 0.0236(12) Uani 1 1 d . . . . .
H1A H 0.0747 0.2183 0.7988 0.028 Uiso 1 1 calc R U . . .
C2 C 0.1734(4) 0.3143(4) 0.7834(4) 0.0271(13) Uani 1 1 d . . . . .
H2 H 0.1493 0.3679 0.7986 0.032 Uiso 1 1 calc R U . . .
C3 C 0.2581(4) 0.3005(3) 0.7555(4) 0.0215(11) Uani 1 1 d . . . . .
H3 H 0.3010 0.3452 0.7484 0.026 Uiso 1 1 calc R U . . .
C4 C 0.2645(4) -0.0209(3) 0.9071(3) 0.0190(11) Uani 1 1 d . . . . .
H4 H 0.2084 -0.0290 0.9273 0.023 Uiso 1 1 calc R U . . .
C5 C 0.3584(4) -0.0547(4) 0.9504(3) 0.0211(11) Uani 1 1 d . . . . .
H5 H 0.3783 -0.0898 1.0045 0.025 Uiso 1 1 calc R U . . .
C6 C 0.4161(4) -0.0252(3) 0.8963(3) 0.0186(11) Uani 1 1 d . . . . .
H6 H 0.4839 -0.0378 0.9087 0.022 Uiso 1 1 calc R U . . .
C7 C 0.1151(4) -0.0166(4) 0.5956(4) 0.0244(12) Uani 1 1 d . . . . .
H7 H 0.0574 -0.0398 0.6051 0.029 Uiso 1 1 calc R U . . .
C8 C 0.1457(4) -0.0311(4) 0.5178(4) 0.0257(13) Uani 1 1 d . . . . .
H8 H 0.1144 -0.0650 0.4647 0.031 Uiso 1 1 calc R U . . .
C9 C 0.2344(4) 0.0165(4) 0.5363(4) 0.0209(11) Uani 1 1 d . . . . .
H9 H 0.2730 0.0198 0.4952 0.025 Uiso 1 1 calc R U . . .
C10 C 0.7582(4) 0.1555(4) 0.8793(4) 0.0242(12) Uani 1 1 d . . . . .
H10 H 0.8121 0.1901 0.9133 0.029 Uiso 1 1 calc R U . . .
C11 C 0.7639(4) 0.0678(4) 0.8553(4) 0.0267(13) Uani 1 1 d . . . . .
H11 H 0.8205 0.0320 0.8690 0.032 Uiso 1 1 calc R U . . .
C12 C 0.6652(4) 0.0448(4) 0.8058(4) 0.0251(12) Uani 1 1 d . . . . .
H12 H 0.6447 -0.0110 0.7806 0.030 Uiso 1 1 calc R U . . .
C13 C 0.5530(4) 0.2815(4) 1.0114(4) 0.0238(12) Uani 1 1 d . . . . .
H13 H 0.6024 0.3177 1.0501 0.029 Uiso 1 1 calc R U . . .
C14 C 0.4735(4) 0.2467(4) 1.0346(4) 0.0240(12) Uani 1 1 d . . . . .
H14 H 0.4576 0.2544 1.0907 0.029 Uiso 1 1 calc R U . . .
C15 C 0.4215(4) 0.1972(4) 0.9557(3) 0.0209(11) Uani 1 1 d . . . . .
H15 H 0.3631 0.1656 0.9509 0.025 Uiso 1 1 calc R U . . .
C16 C 0.5813(4) 0.3990(4) 0.7395(4) 0.0296(13) Uani 1 1 d . . . . .
H16 H 0.6319 0.4381 0.7707 0.036 Uiso 1 1 calc R U . . .
C17 C 0.5116(5) 0.4125(4) 0.6522(4) 0.0308(14) Uani 1 1 d . . . . .
H17 H 0.5052 0.4619 0.6131 0.037 Uiso 1 1 calc R U . . .
C18 C 0.4536(4) 0.3371(4) 0.6355(4) 0.0238(12) Uani 1 1 d . . . . .
H18 H 0.4003 0.3272 0.5811 0.029 Uiso 1 1 calc R U . . .
C19 C 0.4881(4) -0.0053(3) 0.5924(3) 0.0139(10) Uani 1 1 d . . . . .
C20 C 0.4603(4) 0.0786(3) 0.5314(3) 0.0157(10) Uani 1 1 d . . . . .
C21 C 0.4709(4) 0.0777(3) 0.4410(3) 0.0172(10) Uani 1 1 d . . . . .
C22 C 0.1804(11) 0.2682(8) 0.0431(10) 0.151(7) Uani 1 1 d . . . . .
H22A H 0.1945 0.2921 -0.0123 0.181 Uiso 1 1 calc R U . . .
H22B H 0.1083 0.2688 0.0302 0.181 Uiso 1 1 calc R U . . .


_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 O2 2.379(3) . ?
Tb1 O1 2.380(3) . ?
Tb1 N4 2.445(4) . ?
Tb1 N2 2.471(4) . ?
Tb1 N11 2.474(4) . ?
Tb1 N9 2.524(4) . ?
Tb1 N7 2.530(4) . ?
Tb1 N6 2.556(4) . ?
B1 N1 1.534(8) . ?
B1 N5 1.543(7) . ?
B1 N3 1.546(7) . ?
B2 N10 1.533(7) . ?
B2 N8 1.540(8) . ?
B2 N12 1.544(7) . ?
Cl1 C21 1.739(5) . ?
Cl2 C22 1.713(11) . ?
Cl3 C22 1.709(11) . ?
O1 C19 1.257(6) . ?
O2 C20 1.253(6) . ?
N1 C1 1.347(7) . ?
N1 N2 1.367(6) . ?
N2 C3 1.340(7) . ?
N3 C4 1.342(6) . ?
N3 N4 1.367(6) . ?
N4 C6 1.344(6) . ?
N5 C7 1.344(6) . ?
N5 N6 1.371(6) . ?
N6 C9 1.338(6) . ?
N7 C12 1.347(7) . ?
N7 N8 1.368(6) . ?
N8 C10 1.338(7) . ?
N9 C15 1.339(6) . ?
N9 N10 1.375(6) . ?
N10 C13 1.350(6) . ?
N11 C18 1.338(7) . ?
N11 N12 1.362(6) . ?
N12 C16 1.347(7) . ?
C1 C2 1.376(8) . ?
C2 C3 1.383(8) . ?
C4 C5 1.375(7) . ?
C5 C6 1.374(7) . ?
C7 C8 1.364(8) . ?
C8 C9 1.389(8) . ?
C10 C11 1.377(8) . ?
C11 C12 1.399(8) . ?
C13 C14 1.366(8) . ?
C14 C15 1.394(7) . ?
C16 C17 1.382(8) . ?
C17 C18 1.376(8) . ?
C19 C21 1.391(7) 3_656 ?
C19 C20 1.536(7) . ?
C20 C21 1.393(7) . ?
C21 C19 1.391(7) 3_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Tb1 O1 66.62(11) . . ?
O2 Tb1 N4 138.52(13) . . ?
O1 Tb1 N4 80.31(13) . . ?
O2 Tb1 N2 110.84(13) . . ?
O1 Tb1 N2 144.94(13) . . ?
N4 Tb1 N2 82.16(14) . . ?
O2 Tb1 N11 72.17(13) . . ?
O1 Tb1 N11 124.03(14) . . ?
N4 Tb1 N11 149.29(14) . . ?
N2 Tb1 N11 84.45(15) . . ?
O2 Tb1 N9 145.23(13) . . ?
O1 Tb1 N9 130.80(13) . . ?
N4 Tb1 N9 75.82(14) . . ?
N2 Tb1 N9 72.52(14) . . ?
N11 Tb1 N9 73.82(14) . . ?
O2 Tb1 N7 93.65(13) . . ?
O1 Tb1 N7 70.76(13) . . ?
N4 Tb1 N7 98.52(14) . . ?
N2 Tb1 N7 142.20(14) . . ?
N11 Tb1 N7 75.97(14) . . ?
N9 Tb1 N7 71.11(14) . . ?
O2 Tb1 N6 74.87(13) . . ?
O1 Tb1 N6 74.48(13) . . ?
N4 Tb1 N6 72.59(13) . . ?
N2 Tb1 N6 71.39(14) . . ?
N11 Tb1 N6 128.21(14) . . ?
N9 Tb1 N6 134.45(14) . . ?
N7 Tb1 N6 145.12(13) . . ?
N1 B1 N5 109.3(4) . . ?
N1 B1 N3 110.8(4) . . ?
N5 B1 N3 108.2(4) . . ?
N10 B2 N8 108.2(4) . . ?
N10 B2 N12 109.6(4) . . ?
N8 B2 N12 110.9(4) . . ?
C19 O1 Tb1 120.9(3) . . ?
C20 O2 Tb1 121.3(3) . . ?
C1 N1 N2 109.5(4) . . ?
C1 N1 B1 127.3(5) . . ?
N2 N1 B1 123.1(4) . . ?
C3 N2 N1 106.0(4) . . ?
C3 N2 Tb1 131.1(4) . . ?
N1 N2 Tb1 121.2(3) . . ?
C4 N3 N4 109.4(4) . . ?
C4 N3 B1 129.0(4) . . ?
N4 N3 B1 121.4(4) . . ?
C6 N4 N3 105.7(4) . . ?
C6 N4 Tb1 129.9(3) . . ?
N3 N4 Tb1 121.5(3) . . ?
C7 N5 N6 109.5(4) . . ?
C7 N5 B1 128.8(5) . . ?
N6 N5 B1 121.7(4) . . ?
C9 N6 N5 105.1(4) . . ?
C9 N6 Tb1 133.6(4) . . ?
N5 N6 Tb1 120.0(3) . . ?
C12 N7 N8 106.2(4) . . ?
C12 N7 Tb1 131.3(4) . . ?
N8 N7 Tb1 122.5(3) . . ?
C10 N8 N7 109.6(4) . . ?
C10 N8 B2 127.3(5) . . ?
N7 N8 B2 122.6(4) . . ?
C15 N9 N10 105.2(4) . . ?
C15 N9 Tb1 130.1(3) . . ?
N10 N9 Tb1 124.7(3) . . ?
C13 N10 N9 109.8(4) . . ?
C13 N10 B2 130.0(5) . . ?
N9 N10 B2 120.1(4) . . ?
C18 N11 N12 105.6(4) . . ?
C18 N11 Tb1 129.3(4) . . ?
N12 N11 Tb1 125.1(3) . . ?
C16 N12 N11 110.2(4) . . ?
C16 N12 B2 128.4(5) . . ?
N11 N12 B2 121.4(4) . . ?
N1 C1 C2 108.8(5) . . ?
C1 C2 C3 104.7(5) . . ?
N2 C3 C2 111.1(5) . . ?
N3 C4 C5 108.9(5) . . ?
C6 C5 C4 104.8(4) . . ?
N4 C6 C5 111.1(5) . . ?
N5 C7 C8 109.6(5) . . ?
C7 C8 C9 103.9(5) . . ?
N6 C9 C8 111.8(5) . . ?
N8 C10 C11 109.4(5) . . ?
C10 C11 C12 104.4(5) . . ?
N7 C12 C11 110.4(5) . . ?
N10 C13 C14 108.9(5) . . ?
C13 C14 C15 104.7(5) . . ?
N9 C15 C14 111.4(5) . . ?
N12 C16 C17 107.9(5) . . ?
C18 C17 C16 104.9(5) . . ?
N11 C18 C17 111.4(5) . . ?
O1 C19 C21 124.8(5) . 3_656 ?
O1 C19 C20 115.5(4) . . ?
C21 C19 C20 119.7(4) 3_656 . ?
O2 C20 C21 126.2(5) . . ?
O2 C20 C19 115.3(4) . . ?
C21 C20 C19 118.5(4) . . ?
C19 C21 C20 121.7(5) 3_656 . ?
C19 C21 Cl1 119.0(4) 3_656 . ?
C20 C21 Cl1 119.3(4) . . ?
Cl3 C22 Cl2 117.0(7) . . ?

_refine_diff_density_max         1.530
_refine_diff_density_min         -2.002
_refine_diff_density_rms         0.168

_shelxl_version_number           2013-2

