# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
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data_dy_dbm_no3_sq
_database_code_depnum_ccdc_archive 'CCDC 1847187'
_audit_update_record             
;
2018-06-05 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_audit_creation_date             2018-05-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_email
kelsey.schulte@chem.tamu.edu
dunbar@chem.tamu.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 Dy N2 O10, 1.33(C18 H20 B2 Co1 N12)'
_chemical_formula_sum            'C54 H48.67 B2.67 Co1.33 Dy N18 O10'
_chemical_formula_weight         1379.67
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 -0.0001 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.2163 0.3559 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.6814 1.7355 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0005 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_H-M_alt        'I 2 3'
_space_group_name_Hall           'I 2 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'

_cell_length_a                   20.9059(3)
_cell_length_b                   20.9059(3)
_cell_length_c                   20.9059(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9137.1(4)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    77526
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.972
_shelx_estimated_absorpt_T_min   0.945
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1150 before and 0.0526 after correction. The Ratio of minimum to maximum transmission is 0.9104. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4164
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.071
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_number            7378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         20.110
_diffrn_reflns_theta_min         1.387
_diffrn_ambient_temperature      100
_diffrn_detector                 ' Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS hybrid pixel array detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'huber three-circle diffractometer'
_diffrn_measurement_device_type  Syncrotron
_diffrn_measurement_method       '0.5\ ω and 0.5\ φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'Si 111 and Si 311'
_diffrn_radiation_probe          synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_diffrn_source_type              synchrotron
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6841
_reflns_number_total             7378
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_refine_diff_density_max         1.636
_refine_diff_density_min         -3.500
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         7378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0469
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0495P)²+15.1538P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1217
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.58(3)
 0.42(3)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C4(H4), C2(H2A), C7(H7), C8(H8), C5(H5), C11(H11), C6(H6),
  C13(H13), C9(H9), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.0000 0.0000 0.5000 0.05141(12) Uani 1 4 d S T P . .
Co1 Co 0.24544(2) 0.24544(2) 0.75456(2) 0.02289(12) Uani 1 3 d S T P . .
C12 C 0.33485(18) 0.31476(17) 0.84201(17) 0.0326(6) Uani 1 1 d . . . . .
H12 H 0.3199 0.2959 0.8806 0.039 Uiso 1 1 calc R . . . .
C14 C 0.38904(18) 0.37378(17) 0.7733(2) 0.0362(7) Uani 1 1 d . . . . .
H14 H 0.4182 0.4034 0.7548 0.043 Uiso 1 1 calc R . . . .
N5 N 0.34686(13) 0.33740(13) 0.74066(13) 0.0295(5) Uani 1 1 d . . . . .
N4 N 0.31324(13) 0.30123(13) 0.78345(13) 0.0284(5) Uani 1 1 d . . . . .
O3 O 0.0000 0.0000 0.3007(3) 0.0777(16) Uani 1 2 d S T P . .
C3 C 0.12007(14) 0.18328(14) 0.50399(18) 0.0315(5) Uani 1 1 d . . . . .
O1 O 0.06478(13) 0.08687(13) 0.5088(3) 0.0583(10) Uani 1 1 d . . . . .
N2 N 0.17882(14) 0.19027(13) 0.72457(14) 0.0290(5) Uani 1 1 d . . . . .
N3 N 0.14532(14) 0.15440(14) 0.76755(15) 0.0322(5) Uani 1 1 d . . . . .
C4 C 0.17788(14) 0.14912(16) 0.50358(19) 0.0349(5) Uani 1 1 d . . . . .
H4 H 0.1772 0.1037 0.5040 0.042 Uiso 1 1 calc R . . . .
C2 C 0.0000 0.17768(19) 0.5000 0.0341(7) Uani 1 2 d S T P . .
H2A H 0.0000 0.2231 0.5000 0.041 Uiso 1 2 calc RS T P . .
N1 N 0.0000 0.0000 0.3597(4) 0.0630(16) Uani 1 2 d S T P . .
C7 C 0.18177(18) 0.28134(18) 0.5028(2) 0.0423(7) Uani 1 1 d . . . . .
H7 H 0.1833 0.3268 0.5026 0.051 Uiso 1 1 calc R . . . .
C8 C 0.12254(16) 0.25046(15) 0.50357(18) 0.0362(5) Uani 1 1 d . . . . .
H8 H 0.0841 0.2747 0.5038 0.043 Uiso 1 1 calc R . . . .
C5 C 0.23589(16) 0.1810(2) 0.5026(2) 0.0434(7) Uani 1 1 d . . . . .
H5 H 0.2746 0.1571 0.5020 0.052 Uiso 1 1 calc R . . . .
C1 C 0.05887(14) 0.14657(13) 0.50388(19) 0.0323(5) Uani 1 1 d . . . . .
B1 B 0.3310(2) 0.3310(2) 0.6690(2) 0.0306(11) Uani 1 3 d S T P . .
H1 H 0.3586 0.3586 0.6414 0.037 Uiso 1 3 calc RS T P . .
O2 O -0.04911(19) -0.01352(19) 0.3918(2) 0.0740(12) Uani 1 1 d . . . . .
B2 B 0.1611(2) 0.1611(2) 0.8389(2) 0.0361(13) Uani 1 3 d S T P . .
H2 H 0.1335 0.1335 0.8665 0.043 Uiso 1 3 calc RS T P . .
C11 C 0.10317(18) 0.11792(17) 0.73487(19) 0.0359(7) Uani 1 1 d . . . . .
H11 H 0.0743 0.0880 0.7533 0.043 Uiso 1 1 calc R . . . .
C6 C 0.23819(17) 0.24697(19) 0.5024(2) 0.0456(8) Uani 1 1 d . . . . .
H6 H 0.2782 0.2685 0.5019 0.055 Uiso 1 1 calc R . . . .
C13 C 0.3829(2) 0.36103(18) 0.83774(19) 0.0374(7) Uani 1 1 d . . . . .
H13 H 0.4063 0.3797 0.8719 0.045 Uiso 1 1 calc R . . . .
C9 C 0.15694(18) 0.17650(18) 0.66564(17) 0.0326(6) Uani 1 1 d . . . . .
H9 H 0.1720 0.1949 0.6269 0.039 Uiso 1 1 calc R . . . .
C10 C 0.10865(19) 0.13091(18) 0.67073(19) 0.0370(7) Uani 1 1 d . . . . .
H10 H 0.0845 0.1126 0.6369 0.044 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 O1 2.273(3) 2 ?
Dy1 O1 2.273(3) 3_556 ?
Dy1 O1 2.273(3) 4_556 ?
Dy1 O1 2.273(3) . ?
Dy1 N1 2.933(8) 3_556 ?
Dy1 N1 2.933(8) . ?
Dy1 O2 2.499(5) . ?
Dy1 O2 2.499(5) 4_556 ?
Dy1 O2 2.499(5) 3_556 ?
Dy1 O2 2.499(5) 2 ?
Co1 N4 1.932(3) . ?
Co1 N4 1.932(3) 8_656 ?
Co1 N4 1.932(3) 11_566 ?
Co1 N2 1.914(3) . ?
Co1 N2 1.914(3) 11_566 ?
Co1 N2 1.914(3) 8_656 ?
C12 H12 0.9500 . ?
C12 N4 1.335(4) . ?
C12 C13 1.398(5) . ?
C14 H14 0.9500 . ?
C14 N5 1.349(4) . ?
C14 C13 1.380(6) . ?
N5 N4 1.366(4) . ?
N5 B1 1.540(4) . ?
O3 N1 1.234(9) . ?
C3 C4 1.404(4) . ?
C3 C8 1.406(4) . ?
C3 C1 1.492(4) . ?
O1 C1 1.258(4) . ?
N2 N3 1.364(4) . ?
N2 C9 1.345(5) . ?
N3 B2 1.534(4) . ?
N3 C11 1.351(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(5) . ?
C2 H2A 0.9500 . ?
C2 C1 1.394(3) 3_556 ?
C2 C1 1.394(3) . ?
N1 O2 1.259(6) . ?
N1 O2 1.259(6) 2 ?
C7 H7 0.9500 . ?
C7 C8 1.396(4) . ?
C7 C6 1.381(6) . ?
C8 H8 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.381(6) . ?
B1 N5 1.540(4) 11_566 ?
B1 N5 1.540(4) 8_656 ?
B1 H1 1.0000 . ?
B2 N3 1.534(4) 11_566 ?
B2 N3 1.534(4) 8_656 ?
B2 H2 1.0000 . ?
C11 H11 0.9500 . ?
C11 C10 1.373(6) . ?
C6 H6 0.9500 . ?
C13 H13 0.9500 . ?
C9 H9 0.9500 . ?
C9 C10 1.393(5) . ?
C10 H10 0.9500 . ?

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 Dy1 O1 73.93(14) 2 4_556 ?
O1 Dy1 O1 106.85(14) 2 3_556 ?
O1 Dy1 O1 170.7(3) 4_556 3_556 ?
O1 Dy1 O1 170.7(3) 2 . ?
O1 Dy1 O1 106.85(14) 4_556 . ?
O1 Dy1 O1 73.93(14) 3_556 . ?
O1 Dy1 N1 85.38(14) . 3_556 ?
O1 Dy1 N1 94.63(14) 2 . ?
O1 Dy1 N1 94.62(14) . . ?
O1 Dy1 N1 94.63(14) 4_556 3_556 ?
O1 Dy1 N1 85.37(14) 4_556 . ?
O1 Dy1 N1 85.37(14) 3_556 . ?
O1 Dy1 N1 85.37(14) 2 3_556 ?
O1 Dy1 N1 94.63(14) 3_556 3_556 ?
O1 Dy1 O2 74.80(16) 3_556 4_556 ?
O1 Dy1 O2 114.08(16) . . ?
O1 Dy1 O2 76.86(16) 4_556 2 ?
O1 Dy1 O2 94.67(16) 3_556 2 ?
O1 Dy1 O2 94.67(16) 4_556 . ?
O1 Dy1 O2 74.80(16) . 2 ?
O1 Dy1 O2 74.80(16) 4_556 3_556 ?
O1 Dy1 O2 114.09(16) 4_556 4_556 ?
O1 Dy1 O2 114.09(16) 2 2 ?
O1 Dy1 O2 94.67(16) . 4_556 ?
O1 Dy1 O2 114.09(16) 3_556 3_556 ?
O1 Dy1 O2 94.67(16) 2 3_556 ?
O1 Dy1 O2 74.80(16) 2 . ?
O1 Dy1 O2 76.86(16) 2 4_556 ?
O1 Dy1 O2 76.86(16) 3_556 . ?
O1 Dy1 O2 76.86(16) . 3_556 ?
N1 Dy1 N1 180.0 3_556 . ?
O2 Dy1 N1 154.78(10) 4_556 . ?
O2 Dy1 N1 154.78(10) . 3_556 ?
O2 Dy1 N1 154.78(10) 2 3_556 ?
O2 Dy1 N1 25.22(10) 4_556 3_556 ?
O2 Dy1 N1 25.22(10) . . ?
O2 Dy1 N1 154.78(10) 3_556 . ?
O2 Dy1 N1 25.22(10) 3_556 3_556 ?
O2 Dy1 N1 25.22(10) 2 . ?
O2 Dy1 O2 131.5(2) 4_556 . ?
O2 Dy1 O2 167.02(18) 3_556 . ?
O2 Dy1 O2 131.5(2) 3_556 2 ?
O2 Dy1 O2 50.44(19) 2 . ?
O2 Dy1 O2 50.44(19) 3_556 4_556 ?
O2 Dy1 O2 167.02(18) 4_556 2 ?
N4 Co1 N4 88.59(12) . 11_566 ?
N4 Co1 N4 88.58(12) 11_566 8_656 ?
N4 Co1 N4 88.59(12) . 8_656 ?
N2 Co1 N4 90.97(12) 11_566 . ?
N2 Co1 N4 90.61(12) . 11_566 ?
N2 Co1 N4 90.61(12) 11_566 8_656 ?
N2 Co1 N4 90.97(12) . 8_656 ?
N2 Co1 N4 179.09(14) . . ?
N2 Co1 N4 90.97(12) 8_656 11_566 ?
N2 Co1 N4 90.61(12) 8_656 . ?
N2 Co1 N4 179.09(14) 8_656 8_656 ?
N2 Co1 N4 179.09(14) 11_566 11_566 ?
N2 Co1 N2 89.83(13) . 11_566 ?
N2 Co1 N2 89.83(13) . 8_656 ?
N2 Co1 N2 89.83(13) 11_566 8_656 ?
N4 C12 H12 125.3 . . ?
N4 C12 C13 109.3(3) . . ?
C13 C12 H12 125.3 . . ?
N5 C14 H14 125.6 . . ?
N5 C14 C13 108.9(3) . . ?
C13 C14 H14 125.6 . . ?
C14 N5 N4 108.5(3) . . ?
C14 N5 B1 132.9(4) . . ?
N4 N5 B1 118.6(3) . . ?
C12 N4 Co1 131.5(3) . . ?
C12 N4 N5 108.0(3) . . ?
N5 N4 Co1 120.4(2) . . ?
C4 C3 C8 118.5(3) . . ?
C4 C3 C1 118.5(3) . . ?
C8 C3 C1 123.1(3) . . ?
C1 O1 Dy1 136.7(2) . . ?
N3 N2 Co1 119.3(2) . . ?
C9 N2 Co1 132.6(2) . . ?
C9 N2 N3 108.1(3) . . ?
N2 N3 B2 118.7(4) . . ?
C11 N3 N2 108.2(3) . . ?
C11 N3 B2 133.1(4) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 H4 119.7 . . ?
C1 C2 H2A 117.8 . . ?
C1 C2 H2A 117.8 3_556 . ?
C1 C2 C1 124.4(4) 3_556 . ?
O3 N1 Dy1 180.0 . . ?
O3 N1 O2 122.3(4) . . ?
O3 N1 O2 122.3(4) . 2 ?
O2 N1 Dy1 57.7(4) . . ?
O2 N1 Dy1 57.7(4) 2 . ?
O2 N1 O2 115.5(8) . 2 ?
C8 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C6 C7 C8 121.1(3) . . ?
C3 C8 H8 120.2 . . ?
C7 C8 C3 119.6(3) . . ?
C7 C8 H8 120.2 . . ?
C4 C5 H5 119.6 . . ?
C6 C5 C4 120.8(3) . . ?
C6 C5 H5 119.6 . . ?
O1 C1 C3 115.2(3) . . ?
O1 C1 C2 123.6(3) . . ?
C2 C1 C3 121.1(3) . . ?
N5 B1 N5 106.0(3) 11_566 8_656 ?
N5 B1 N5 106.0(3) . 11_566 ?
N5 B1 N5 106.0(3) . 8_656 ?
N5 B1 H1 112.8 8_656 . ?
N5 B1 H1 112.8 . . ?
N5 B1 H1 112.8 11_566 . ?
N1 O2 Dy1 97.0(4) . . ?
N3 B2 N3 106.2(3) . 11_566 ?
N3 B2 N3 106.2(3) . 8_656 ?
N3 B2 N3 106.2(3) 11_566 8_656 ?
N3 B2 H2 112.6 8_656 . ?
N3 B2 H2 112.6 11_566 . ?
N3 B2 H2 112.6 . . ?
N3 C11 H11 125.4 . . ?
N3 C11 C10 109.1(3) . . ?
C10 C11 H11 125.4 . . ?
C7 C6 H6 120.3 . . ?
C5 C6 C7 119.3(3) . . ?
C5 C6 H6 120.3 . . ?
C12 C13 H13 127.4 . . ?
C14 C13 C12 105.2(3) . . ?
C14 C13 H13 127.4 . . ?
N2 C9 H9 125.6 . . ?
N2 C9 C10 108.8(3) . . ?
C10 C9 H9 125.6 . . ?
C11 C10 C9 105.7(3) . . ?
C11 C10 H10 127.2 . . ?
C9 C10 H10 127.2 . . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 1 1 0.801
0 0 2 1.133

_platon_squeeze_details          
;
TITL data_0m_a.res in I23
CELL   20.9059   20.9059   20.9059     90.00     90.00     90.00
SPGR I23
# Solvent Accessible Volume =    1051.3
# Electrons Found in S.A.V. =     204.9
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 1.000 1.000 0.000 !       1.97 eA-3
C102 0.135 1.000 0.000 !       1.54 eA-3
C103 0.496 0.572 0.343 !       1.28 eA-3
Q104 1.000 0.998 0.484 !       1.20 eA-3
C105 0.961 0.867 0.017 !       1.17 eA-3
C106 0.381 0.510 0.332 !       1.00 eA-3
C107 0.876 0.101-0.001 !       0.97 eA-3
C108 0.376 0.601 0.499 !       0.97 eA-3
C109 0.499 0.374 0.603 !       0.97 eA-3
C110 0.999 0.874 0.103 !       0.97 eA-3
C111 0.624 0.602 0.499 !       0.96 eA-3
C112 0.590 0.507 0.627 !       0.96 eA-3
C113 0.061 0.006 0.162 !       0.72 eA-3
Q114 0.315 0.542 0.485 !       0.69 eA-3
C115 0.989 0.090 0.047 !       0.61 eA-3
C116 0.576 0.424 0.424 !       0.55 eA-3
Q117 0.951 0.499 0.112 !       0.55 eA-3
Q118 0.499 0.552 0.102 !       0.50 eA-3
C119 0.344 0.467 0.445 !       0.50 eA-3
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 514 105 ' '
2 0.500 0.500 0.500 514 105 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.58(3)
2 0.42(3)

# start Validation Reply Form
_vrf_PLAT111_dy_dbm_no3_sq       
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry .        100 %Fit  
RESPONSE: The structure was solved as an inversion twin. The mirror plane
required in the higher symmetry space group does not allow for the torsion 
in the DBM and nitrate ligands which is visible in I23.
;
_vrf_PLAT974_dy_dbm_no3_sq       
;
PROBLEM: Check Calcd Negative Resid. Density on       Dy1      -1.89 eA-3  
RESPONSE: There is some disorder over the center of the Dy moiety. Attempts 
to model this disorder were not successful. Adjustments of the absorption 
correction made no appreciable difference.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_tb_dbm_no3_sq
_database_code_depnum_ccdc_archive 'CCDC 1847190'
_audit_update_record             
;
2018-06-05 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_audit_creation_date             2018-06-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_email
kelsey.schulte@chem.tamu.edu
dunbar@chem.tamu.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 N2 O10 Tb, 1.33(C18 H20 B2 Co1 N12)'
_chemical_formula_sum            'C54 H48.67 B2.67 Co1.33 N18 O10 Tb'
_chemical_formula_weight         1376.09
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0010 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.2360 0.3980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.7221 1.6294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_H-M_alt        'I 2 3'
_space_group_name_Hall           'I 2 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'

_cell_length_a                   20.9135(4)
_cell_length_b                   20.9135(4)
_cell_length_c                   20.9135(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9147.0(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    47411
_cell_measurement_temperature    100
_cell_measurement_theta_max      16.48
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.957
_shelx_estimated_absorpt_T_min   0.707
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.7440
_exptl_absorpt_correction_T_min  0.6636
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1012 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.8919. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4158
_exptl_crystal_size_max          0.94
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.113
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_number            3381
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         15.353
_diffrn_reflns_theta_min         1.387
_diffrn_ambient_temperature      100.0
_diffrn_detector                 ' Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS hybrid pixel array detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'huber three-circle diffractometer'
_diffrn_measurement_device_type  'Pilatus1M(CdTe) pixel array detector'
_diffrn_measurement_method       '0.5\ ω and 0.5\ φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'Si 111 and Si 311'
_diffrn_radiation_probe          synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_diffrn_source_type              synchrotron
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3351
_reflns_number_total             3381
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_refine_diff_density_max         0.403
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3381
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0277P)²+19.2636P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0812
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.49(5)
 0.51(5)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C8(H8), C5(H5), C4(H4), C13(H13), C2(H2A), C10(H10),
 C7(H7), C6(H6), C9(H9), C14(H14)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.5000 0.0000 0.5000 0.05149(16) Uani 1 4 d S T P . .
Co1 Co 0.75478(3) 0.24522(3) 0.75478(3) 0.0239(2) Uani 1 3 d S T P . .
C11 C 0.6654(2) 0.1580(2) 0.6859(2) 0.0326(9) Uani 1 1 d . . . . .
H11 H 0.6802 0.1196 0.7050 0.039 Uiso 1 1 calc R . . . .
N2 N 0.68684(19) 0.21631(19) 0.69920(18) 0.0302(8) Uani 1 1 d . . . . .
N4 N 0.82166(19) 0.2754(2) 0.80991(18) 0.0294(8) Uani 1 1 d . . . . .
N5 N 0.85525(19) 0.2319(2) 0.84581(19) 0.0339(9) Uani 1 1 d . . . . .
N3 N 0.65346(18) 0.25917(18) 0.66293(18) 0.0284(8) Uani 1 1 d . . . . .
O3 O 0.5000 0.1991(4) 0.5000 0.0796(17) Uani 1 2 d S T P . .
C12 C 0.8973(2) 0.2646(2) 0.8818(2) 0.0369(11) Uani 1 1 d . . . . .
H12 H 0.9263 0.2462 0.9116 0.044 Uiso 1 1 calc R . . . .
C3 C 0.38010(18) -0.0045(3) 0.31632(19) 0.0343(8) Uani 1 1 d . . . . .
O1 O 0.43524(16) -0.0090(3) 0.41276(16) 0.0593(12) Uani 1 1 d . . . . .
N1 N 0.5000 0.1401(4) 0.5000 0.0648(18) Uani 1 2 d S T P . .
C8 C 0.3225(2) -0.0041(3) 0.3501(2) 0.0376(9) Uani 1 1 d . . . . .
H8 H 0.3231 -0.0049 0.3955 0.045 Uiso 1 1 calc R . . . .
C5 C 0.3190(2) -0.0034(3) 0.2183(2) 0.0445(10) Uani 1 1 d . . . . .
H5 H 0.3177 -0.0037 0.1729 0.053 Uiso 1 1 calc R . . . .
C4 C 0.3776(2) -0.0040(2) 0.2491(2) 0.0391(9) Uani 1 1 d . . . . .
H4 H 0.4160 -0.0042 0.2249 0.047 Uiso 1 1 calc R . . . .
B1 B 0.8392(3) 0.1608(3) 0.8392(3) 0.039(2) Uani 1 3 d S T P . .
H1 H 0.8668 0.1332 0.8668 0.047 Uiso 1 3 calc RS T P . .
C13 C 0.8919(2) 0.3285(3) 0.8690(2) 0.0365(10) Uani 1 1 d . . . . .
H13 H 0.9162 0.3622 0.8875 0.044 Uiso 1 1 calc R . . . .
C2 C 0.5000 0.0000 0.3221(3) 0.0378(12) Uani 1 2 d S T P . .
H2A H 0.5000 0.0000 0.2767 0.045 Uiso 1 2 calc RS T P . .
C10 C 0.6176(3) 0.1621(3) 0.6393(2) 0.0396(11) Uani 1 1 d . . . . .
H10 H 0.5945 0.1278 0.6204 0.048 Uiso 1 1 calc R . . . .
C7 C 0.2645(2) -0.0024(3) 0.3183(2) 0.0465(10) Uani 1 1 d . . . . .
H7 H 0.2259 -0.0014 0.3421 0.056 Uiso 1 1 calc R . . . .
C6 C 0.2623(2) -0.0024(3) 0.2524(2) 0.0478(11) Uani 1 1 d . . . . .
H6 H 0.2224 -0.0016 0.2308 0.057 Uiso 1 1 calc R . . . .
O2 O 0.5484(2) 0.1083(3) 0.5144(2) 0.0760(14) Uani 1 1 d . . . . .
C1 C 0.4415(2) -0.0038(3) 0.35325(18) 0.0367(9) Uani 1 1 d . . . . .
C9 C 0.6112(2) 0.2263(3) 0.6268(2) 0.0372(11) Uani 1 1 d . . . . .
H9 H 0.5818 0.2446 0.5975 0.045 Uiso 1 1 calc R . . . .
B2 B 0.6694(3) 0.3306(3) 0.6694(3) 0.0321(19) Uani 1 3 d S T P . .
H2 H 0.6418 0.3582 0.6418 0.039 Uiso 1 3 calc RS T P . .
C14 C 0.8436(2) 0.3342(2) 0.8235(3) 0.0328(9) Uani 1 1 d . . . . .
H14 H 0.8287 0.3730 0.8052 0.039 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 O1 2.280(3) . ?
Tb1 O1 2.280(3) 3_656 ?
Tb1 O1 2.280(3) 2_655 ?
Tb1 O1 2.280(3) 4_556 ?
Tb1 N1 2.930(9) . ?
Tb1 N1 2.930(9) 2_655 ?
Tb1 O2 2.498(5) 3_656 ?
Tb1 O2 2.498(5) 4_556 ?
Tb1 O2 2.498(5) 2_655 ?
Tb1 O2 2.498(5) . ?
Co1 N2 1.933(4) 6_566 ?
Co1 N2 1.933(4) . ?
Co1 N2 1.933(4) 12_665 ?
Co1 N4 1.920(4) . ?
Co1 N4 1.920(4) 12_665 ?
Co1 N4 1.920(4) 6_566 ?
C11 H11 0.9500 . ?
C11 N2 1.329(6) . ?
C11 C10 1.397(7) . ?
N2 N3 1.366(5) . ?
N4 N5 1.373(5) . ?
N4 C14 1.343(6) . ?
N5 C12 1.345(6) . ?
N5 B1 1.532(6) . ?
N3 C9 1.350(6) . ?
N3 B2 1.536(5) . ?
O3 N1 1.233(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.368(7) . ?
C3 C8 1.396(6) . ?
C3 C4 1.407(6) . ?
C3 C1 1.498(5) . ?
O1 C1 1.256(5) . ?
N1 O2 1.249(6) 3_656 ?
N1 O2 1.249(6) . ?
C8 H8 0.9500 . ?
C8 C7 1.383(6) . ?
C5 H5 0.9500 . ?
C5 C4 1.384(6) . ?
C5 C6 1.384(6) . ?
C4 H4 0.9500 . ?
B1 N5 1.532(6) 6_566 ?
B1 N5 1.532(6) 12_665 ?
B1 H1 1.0000 . ?
C13 H13 0.9500 . ?
C13 C14 1.394(7) . ?
C2 H2A 0.9500 . ?
C2 C1 1.389(5) 2_655 ?
C2 C1 1.389(5) . ?
C10 H10 0.9500 . ?
C10 C9 1.375(8) . ?
C7 H7 0.9500 . ?
C7 C6 1.378(7) . ?
C6 H6 0.9500 . ?
C9 H9 0.9500 . ?
B2 N3 1.536(5) 12_665 ?
B2 N3 1.536(5) 6_566 ?
B2 H2 1.0000 . ?
C14 H14 0.9500 . ?

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 Tb1 O1 170.5(3) . 3_656 ?
O1 Tb1 O1 73.70(17) . 2_655 ?
O1 Tb1 O1 107.12(17) 3_656 2_655 ?
O1 Tb1 O1 73.70(17) 3_656 4_556 ?
O1 Tb1 O1 107.12(17) . 4_556 ?
O1 Tb1 O1 170.5(3) 4_556 2_655 ?
O1 Tb1 N1 85.26(16) . 2_655 ?
O1 Tb1 N1 85.26(16) 3_656 2_655 ?
O1 Tb1 N1 85.26(16) 4_556 . ?
O1 Tb1 N1 85.26(16) 2_655 . ?
O1 Tb1 N1 94.74(16) . . ?
O1 Tb1 N1 94.74(16) 3_656 . ?
O1 Tb1 N1 94.74(16) 2_655 2_655 ?
O1 Tb1 N1 94.74(16) 4_556 2_655 ?
O1 Tb1 O2 77.36(19) 4_556 3_656 ?
O1 Tb1 O2 114.34(18) 4_556 4_556 ?
O1 Tb1 O2 74.79(19) 2_655 4_556 ?
O1 Tb1 O2 74.78(19) 3_656 . ?
O1 Tb1 O2 114.34(18) 2_655 2_655 ?
O1 Tb1 O2 77.36(19) 2_655 . ?
O1 Tb1 O2 77.36(19) . 2_655 ?
O1 Tb1 O2 114.35(18) . . ?
O1 Tb1 O2 93.96(18) 3_656 2_655 ?
O1 Tb1 O2 93.96(18) 2_655 3_656 ?
O1 Tb1 O2 93.96(18) . 4_556 ?
O1 Tb1 O2 114.34(18) 3_656 3_656 ?
O1 Tb1 O2 74.79(19) 4_556 2_655 ?
O1 Tb1 O2 77.36(19) 3_656 4_556 ?
O1 Tb1 O2 74.78(19) . 3_656 ?
O1 Tb1 O2 93.96(18) 4_556 . ?
N1 Tb1 N1 180.0 2_655 . ?
O2 Tb1 N1 25.01(11) 4_556 2_655 ?
O2 Tb1 N1 154.99(11) 4_556 . ?
O2 Tb1 N1 25.01(11) 3_656 . ?
O2 Tb1 N1 154.99(11) . 2_655 ?
O2 Tb1 N1 25.01(11) . . ?
O2 Tb1 N1 25.01(11) 2_655 2_655 ?
O2 Tb1 N1 154.99(11) 3_656 2_655 ?
O2 Tb1 N1 154.99(11) 2_655 . ?
O2 Tb1 O2 50.0(2) . 3_656 ?
O2 Tb1 O2 166.1(2) 4_556 3_656 ?
O2 Tb1 O2 132.2(2) . 4_556 ?
O2 Tb1 O2 132.2(2) 2_655 3_656 ?
O2 Tb1 O2 50.0(2) 2_655 4_556 ?
O2 Tb1 O2 166.1(2) 2_655 . ?
N2 Co1 N2 88.63(17) 12_665 . ?
N2 Co1 N2 88.64(17) 6_566 12_665 ?
N2 Co1 N2 88.63(17) 6_566 . ?
N4 Co1 N2 90.48(17) 6_566 12_665 ?
N4 Co1 N2 179.0(2) 6_566 6_566 ?
N4 Co1 N2 90.48(17) . 6_566 ?
N4 Co1 N2 90.90(17) 12_665 6_566 ?
N4 Co1 N2 179.0(2) 12_665 12_665 ?
N4 Co1 N2 90.90(17) . 12_665 ?
N4 Co1 N2 90.48(17) 12_665 . ?
N4 Co1 N2 90.90(17) 6_566 . ?
N4 Co1 N2 179.0(2) . . ?
N4 Co1 N4 89.98(17) . 6_566 ?
N4 Co1 N4 89.98(17) . 12_665 ?
N4 Co1 N4 89.98(17) 6_566 12_665 ?
N2 C11 H11 125.3 . . ?
N2 C11 C10 109.4(5) . . ?
C10 C11 H11 125.3 . . ?
C11 N2 Co1 131.4(4) . . ?
C11 N2 N3 108.2(4) . . ?
N3 N2 Co1 120.3(3) . . ?
N5 N4 Co1 118.9(3) . . ?
C14 N4 Co1 132.6(3) . . ?
C14 N4 N5 108.4(4) . . ?
N4 N5 B1 118.9(5) . . ?
C12 N5 N4 107.7(4) . . ?
C12 N5 B1 133.4(5) . . ?
N2 N3 B2 118.5(5) . . ?
C9 N3 N2 108.1(4) . . ?
C9 N3 B2 133.4(5) . . ?
N5 C12 H12 125.3 . . ?
N5 C12 C13 109.4(4) . . ?
C13 C12 H12 125.3 . . ?
C8 C3 C4 118.2(4) . . ?
C8 C3 C1 118.6(4) . . ?
C4 C3 C1 123.2(4) . . ?
C1 O1 Tb1 136.4(3) . . ?
O3 N1 Tb1 180.0 . . ?
O3 N1 O2 122.2(4) . . ?
O3 N1 O2 122.2(4) . 3_656 ?
O2 N1 Tb1 57.8(4) . . ?
O2 N1 Tb1 57.8(4) 3_656 . ?
O2 N1 O2 115.5(9) 3_656 . ?
C3 C8 H8 119.6 . . ?
C7 C8 C3 120.9(4) . . ?
C7 C8 H8 119.6 . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C6 C5 C4 121.1(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 119.9(4) . . ?
C5 C4 H4 120.0 . . ?
N5 B1 N5 106.3(4) 6_566 12_665 ?
N5 B1 N5 106.3(4) 6_566 . ?
N5 B1 N5 106.3(4) 12_665 . ?
N5 B1 H1 112.5 12_665 . ?
N5 B1 H1 112.5 6_566 . ?
N5 B1 H1 112.5 . . ?
C12 C13 H13 127.0 . . ?
C12 C13 C14 106.1(4) . . ?
C14 C13 H13 127.0 . . ?
C1 C2 H2A 118.0 . . ?
C1 C2 H2A 118.0 2_655 . ?
C1 C2 C1 124.0(5) . 2_655 ?
C11 C10 H10 127.4 . . ?
C9 C10 C11 105.1(5) . . ?
C9 C10 H10 127.4 . . ?
C8 C7 H7 119.7 . . ?
C6 C7 C8 120.7(4) . . ?
C6 C7 H7 119.7 . . ?
C5 C6 H6 120.4 . . ?
C7 C6 C5 119.2(4) . . ?
C7 C6 H6 120.4 . . ?
N1 O2 Tb1 97.2(5) . . ?
O1 C1 C3 114.9(4) . . ?
O1 C1 C2 124.1(4) . . ?
C2 C1 C3 120.9(4) . . ?
N3 C9 C10 109.2(5) . . ?
N3 C9 H9 125.4 . . ?
C10 C9 H9 125.4 . . ?
N3 B2 N3 106.2(4) 6_566 12_665 ?
N3 B2 N3 106.2(4) 12_665 . ?
N3 B2 N3 106.2(4) 6_566 . ?
N3 B2 H2 112.6 6_566 . ?
N3 B2 H2 112.6 12_665 . ?
N3 B2 H2 112.6 . . ?
N4 C14 C13 108.3(4) . . ?
N4 C14 H14 125.9 . . ?
C13 C14 H14 125.9 . . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 1 1 0.801

_platon_squeeze_details          
;
TITL data_0m_b.res in I23
CELL   20.9135   20.9135   20.9135     90.00     90.00     90.00
SPGR I23
# Solvent Accessible Volume =    1055.7
# Electrons Found in S.A.V. =     252.9
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.138 0.010 0.008 !       1.57 eA-3
C102 0.012 0.855 0.047 !       1.21 eA-3
C103 0.436 0.507 0.336 !       1.17 eA-3
C104 0.922 0.868 0.987 !       1.14 eA-3
C105 0.422 0.368 0.487 !       1.14 eA-3
C106 0.093 0.120 1.003 !       1.10 eA-3
C107 0.481 0.545 0.422 !       0.73 eA-3
C108 0.484 0.515 0.485 !       0.72 eA-3
C109 0.940 0.049 0.090 !       0.58 eA-3
C110 0.491 0.491 0.491 !       0.55 eA-3
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 515 128 ' '
2 0.500 0.500 0.500 515 128 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.49(5)
2 0.51(5)

# start Validation Reply Form
_vrf_PLAT111_tb_dbm_no3_sq       
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry .        100 %Fit  
RESPONSE: The structure was solved as an inversion twin. The mirror plane
required in the higher symmetry space group does not allow for the torsion 
in the DBM and nitrate ligands which is visible in I23.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_y_dbm_no3_sq
_database_code_depnum_ccdc_archive 'CCDC 1847189'
_audit_update_record             
;
2018-06-05 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_audit_creation_date             2018-05-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_email
kelsey.schulte@chem.tamu.edu
dunbar@chem.tamu.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 N2 O10 Y, 1.33(C18 H20 B2 Co1 N12)'
_chemical_formula_sum            'C54 H48.67 B2.67 Co1.33 N18 O10 Y'
_chemical_formula_weight         1306.08
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 -0.0001 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.2163 0.3559 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0005 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y 0.2083 1.4374 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_H-M_alt        'I 2 3'
_space_group_name_Hall           'I 2 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'

_cell_length_a                   20.9091(4)
_cell_length_b                   20.9091(4)
_cell_length_c                   20.9091(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9141.3(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    40908
_cell_measurement_temperature    100
_cell_measurement_theta_max      18.90
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.966
_shelx_estimated_absorpt_T_min   0.735
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.7094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0797 before and 0.0567 after correction. The Ratio of minimum to maximum transmission is 0.9531. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4002
_exptl_crystal_size_max          0.97
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.102
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_number            5076
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         17.677
_diffrn_reflns_theta_min         1.387
_diffrn_ambient_temperature      100
_diffrn_detector                 ' Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS hybrid pixel array detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'huber three-circle diffractometer'
_diffrn_measurement_device_type  'Pilatus1M(CdTe) pixel array detector'
_diffrn_measurement_method       '0.5\ ω and 0.5\ φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'Si 111 and Si 311'
_diffrn_radiation_probe          synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   synchrotron
_diffrn_source_type              synchrotron
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4858
_reflns_number_total             5076
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008-2013)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008-2013)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2013)'
_refine_diff_density_max         0.373
_refine_diff_density_min         -1.252
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5076
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0432P)²+6.6492P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0901
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.53(2)
 0.47(2)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Ternary CH refined with riding coordinates:
 B2(H2), B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C14(H14), C11(H11), C4(H4), C8(H8), C2(H2A), C7(H7),
 C12(H12), C5(H5), C6(H6), C10(H10)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.5000 1.0000 0.5000 0.05010(14) Uani 1 4 d S T P . .
Co1 Co 0.24507(2) 0.75493(2) 0.24507(2) 0.02383(11) Uani 1 3 d S T P . .
N2 N 0.31242(9) 0.78413(9) 0.30068(9) 0.0279(4) Uani 1 1 d . . . . .
N4 N 0.17800(10) 0.72538(10) 0.18967(9) 0.0285(4) Uani 1 1 d . . . . .
N3 N 0.34603(9) 0.74149(10) 0.33685(9) 0.0290(4) Uani 1 1 d . . . . .
N5 N 0.14458(10) 0.76818(10) 0.15357(10) 0.0310(4) Uani 1 1 d . . . . .
O3 O 0.56495(10) 1.01021(16) 0.58572(10) 0.0557(7) Uani 1 1 d . . . . .
O2 O 0.5000 0.8018(2) 0.5000 0.0737(11) Uani 1 2 d S T P . .
C13 C 0.10823(13) 0.67127(13) 0.12996(12) 0.0365(5) Uani 1 1 d . . . . .
H13 H 0.0846 0.6372 0.1114 0.044 Uiso 1 1 calc R . . . .
C9 C 0.33414(12) 0.84269(12) 0.31443(13) 0.0322(4) Uani 1 1 d . . . . .
H9 H 0.3190 0.8813 0.2958 0.039 Uiso 1 1 calc R . . . .
O1 O 0.45134(13) 0.89305(17) 0.48470(13) 0.0712(8) Uani 1 1 d . . . . .
N1 N 0.5000 0.8615(3) 0.5000 0.0608(11) Uani 1 2 d S T P . .
C3 C 0.62012(11) 1.00493(12) 0.68256(11) 0.0319(4) Uani 1 1 d . . . . .
C14 C 0.10230(12) 0.73578(13) 0.11721(12) 0.0349(5) Uani 1 1 d . . . . .
H14 H 0.0732 0.7543 0.0877 0.042 Uiso 1 1 calc R . . . .
C11 C 0.38839(12) 0.77382(13) 0.37310(12) 0.0347(5) Uani 1 1 d . . . . .
H11 H 0.4176 0.7553 0.4026 0.042 Uiso 1 1 calc R . . . .
C4 C 0.62253(12) 1.00448(12) 0.74971(12) 0.0370(5) Uani 1 1 d . . . . .
H4 H 0.5841 1.0046 0.7739 0.044 Uiso 1 1 calc R . . . .
C8 C 0.67796(12) 1.00456(12) 0.64860(13) 0.0357(5) Uani 1 1 d . . . . .
H8 H 0.6772 1.0050 0.6032 0.043 Uiso 1 1 calc R . . . .
C2 C 0.5000 1.0000 0.67681(16) 0.0350(6) Uani 1 2 d S T P . .
H2A H 0.5000 1.0000 0.7222 0.042 Uiso 1 2 calc RS T P . .
C7 C 0.73616(13) 1.00361(14) 0.68005(15) 0.0440(6) Uani 1 1 d . . . . .
H7 H 0.7748 1.0033 0.6562 0.053 Uiso 1 1 calc R . . . .
C12 C 0.15636(13) 0.66673(12) 0.17590(13) 0.0326(5) Uani 1 1 d . . . . .
H12 H 0.1714 0.6281 0.1945 0.039 Uiso 1 1 calc R . . . .
C1 C 0.55906(11) 1.00484(13) 0.64567(11) 0.0330(4) Uani 1 1 d . . . . .
C5 C 0.68144(14) 1.00390(14) 0.78069(14) 0.0421(5) Uani 1 1 d . . . . .
H5 H 0.6828 1.0040 0.8261 0.050 Uiso 1 1 calc R . . . .
C6 C 0.73801(13) 1.00315(14) 0.74641(15) 0.0463(6) Uani 1 1 d . . . . .
H6 H 0.7779 1.0023 0.7681 0.056 Uiso 1 1 calc R . . . .
C10 C 0.38237(13) 0.83844(13) 0.36026(12) 0.0365(5) Uani 1 1 d . . . . .
H10 H 0.4060 0.8726 0.3787 0.044 Uiso 1 1 calc R . . . .
B2 B 0.16024(13) 0.83976(13) 0.16024(13) 0.0313(9) Uani 1 3 d S T P . .
H2 H 0.1326 0.8674 0.1326 0.038 Uiso 1 3 calc RS T P . .
B1 B 0.33002(13) 0.66998(13) 0.33002(13) 0.0306(9) Uani 1 3 d S T P . .
H1 H 0.3576 0.6424 0.3576 0.037 Uiso 1 3 calc RS T P . .


_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 O3 2.259(2) . ?
Y1 O3 2.259(2) 3_656 ?
Y1 O3 2.259(2) 4_576 ?
Y1 O3 2.259(2) 2_675 ?
Y1 O1 2.477(3) 2_675 ?
Y1 O1 2.477(3) 3_656 ?
Y1 O1 2.478(3) . ?
Y1 O1 2.477(3) 4_576 ?
Y1 N1 2.896(6) . ?
Y1 N1 2.896(6) 2_675 ?
Co1 N2 1.9256(19) . ?
Co1 N2 1.9257(19) 6_566 ?
Co1 N2 1.9257(19) 12_665 ?
Co1 N4 1.921(2) . ?
Co1 N4 1.921(2) 6_566 ?
Co1 N4 1.921(2) 12_665 ?
N2 N3 1.364(3) . ?
N2 C9 1.337(3) . ?
N4 N5 1.363(3) . ?
N4 C12 1.338(3) . ?
N3 C11 1.348(3) . ?
N3 B1 1.539(3) . ?
N5 C14 1.348(3) . ?
N5 B2 1.539(3) . ?
O3 C1 1.265(3) . ?
O2 N1 1.247(6) . ?
C13 H13 0.9500 . ?
C13 C14 1.381(4) . ?
C13 C12 1.394(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.394(4) . ?
O1 N1 1.254(4) . ?
N1 O1 1.254(4) 3_656 ?
C3 C4 1.405(3) . ?
C3 C8 1.402(3) . ?
C3 C1 1.492(3) . ?
C14 H14 0.9500 . ?
C11 H11 0.9500 . ?
C11 C10 1.383(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(4) . ?
C8 H8 0.9500 . ?
C8 C7 1.383(4) . ?
C2 H2A 0.9500 . ?
C2 C1 1.400(3) . ?
C2 C1 1.400(3) 2_675 ?
C7 H7 0.9500 . ?
C7 C6 1.388(4) . ?
C12 H12 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.383(4) . ?
C6 H6 0.9500 . ?
C10 H10 0.9500 . ?
B2 N5 1.539(3) 6_566 ?
B2 N5 1.539(3) 12_665 ?
B2 H2 1.0000 . ?
B1 N3 1.539(3) 6_566 ?
B1 N3 1.539(3) 12_665 ?
B1 H1 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Y1 O3 169.15(17) . 3_656 ?
O3 Y1 O3 74.97(10) 3_656 4_576 ?
O3 Y1 O3 106.09(10) . 4_576 ?
O3 Y1 O3 106.09(10) 3_656 2_675 ?
O3 Y1 O3 74.98(10) . 2_675 ?
O3 Y1 O3 169.15(17) 4_576 2_675 ?
O3 Y1 O1 74.69(10) 2_675 4_576 ?
O3 Y1 O1 115.77(11) . . ?
O3 Y1 O1 115.76(11) 2_675 2_675 ?
O3 Y1 O1 115.76(11) 3_656 3_656 ?
O3 Y1 O1 76.72(10) 4_576 3_656 ?
O3 Y1 O1 93.39(10) 2_675 3_656 ?
O3 Y1 O1 76.72(10) . 2_675 ?
O3 Y1 O1 115.76(11) 4_576 4_576 ?
O3 Y1 O1 93.39(10) 3_656 2_675 ?
O3 Y1 O1 76.72(10) 2_675 . ?
O3 Y1 O1 93.39(10) 4_576 . ?
O3 Y1 O1 74.69(10) 3_656 . ?
O3 Y1 O1 93.39(10) . 4_576 ?
O3 Y1 O1 74.69(10) . 3_656 ?
O3 Y1 O1 76.72(10) 3_656 4_576 ?
O3 Y1 O1 74.69(10) 4_576 2_675 ?
O3 Y1 N1 95.42(8) . . ?
O3 Y1 N1 95.42(8) 4_576 2_675 ?
O3 Y1 N1 84.58(8) 2_675 . ?
O3 Y1 N1 84.58(8) 3_656 2_675 ?
O3 Y1 N1 84.58(8) 4_576 . ?
O3 Y1 N1 95.42(8) 2_675 2_675 ?
O3 Y1 N1 95.42(8) 3_656 . ?
O3 Y1 N1 84.58(8) . 2_675 ?
O1 Y1 O1 165.16(13) 4_576 3_656 ?
O1 Y1 O1 165.16(13) 2_675 . ?
O1 Y1 O1 131.50(13) 4_576 . ?
O1 Y1 O1 51.00(13) 2_675 4_576 ?
O1 Y1 O1 131.50(13) 2_675 3_656 ?
O1 Y1 O1 51.00(13) 3_656 . ?
O1 Y1 N1 154.50(7) . 2_675 ?
O1 Y1 N1 154.50(7) 3_656 2_675 ?
O1 Y1 N1 154.50(7) 4_576 . ?
O1 Y1 N1 25.50(7) 4_576 2_675 ?
O1 Y1 N1 154.50(7) 2_675 . ?
O1 Y1 N1 25.50(7) 2_675 2_675 ?
O1 Y1 N1 25.50(7) 3_656 . ?
O1 Y1 N1 25.50(7) . . ?
N1 Y1 N1 180.0 . 2_675 ?
N2 Co1 N2 88.96(9) 6_566 12_665 ?
N2 Co1 N2 88.96(9) . 12_665 ?
N2 Co1 N2 88.96(9) . 6_566 ?
N4 Co1 N2 90.82(8) . 6_566 ?
N4 Co1 N2 90.88(8) 12_665 6_566 ?
N4 Co1 N2 179.73(10) 6_566 6_566 ?
N4 Co1 N2 90.82(8) 6_566 12_665 ?
N4 Co1 N2 90.88(8) 6_566 . ?
N4 Co1 N2 179.73(10) . . ?
N4 Co1 N2 90.88(8) . 12_665 ?
N4 Co1 N2 179.73(10) 12_665 12_665 ?
N4 Co1 N2 90.82(8) 12_665 . ?
N4 Co1 N4 89.34(9) 6_566 12_665 ?
N4 Co1 N4 89.34(9) . 6_566 ?
N4 Co1 N4 89.34(9) . 12_665 ?
N3 N2 Co1 120.28(15) . . ?
C9 N2 Co1 131.95(18) . . ?
C9 N2 N3 107.7(2) . . ?
N5 N4 Co1 119.79(15) . . ?
C12 N4 Co1 132.16(17) . . ?
C12 N4 N5 108.0(2) . . ?
N2 N3 B1 118.1(2) . . ?
C11 N3 N2 108.8(2) . . ?
C11 N3 B1 133.0(2) . . ?
N4 N5 B2 118.6(2) . . ?
C14 N5 N4 108.6(2) . . ?
C14 N5 B2 132.8(2) . . ?
C1 O3 Y1 136.02(17) . . ?
C14 C13 H13 127.3 . . ?
C14 C13 C12 105.3(2) . . ?
C12 C13 H13 127.3 . . ?
N2 C9 H9 125.2 . . ?
N2 C9 C10 109.6(2) . . ?
C10 C9 H9 125.2 . . ?
N1 O1 Y1 96.2(3) . . ?
O2 N1 Y1 180.0 . . ?
O2 N1 O1 121.7(3) . 3_656 ?
O2 N1 O1 121.7(3) . . ?
O1 N1 Y1 58.3(3) . . ?
O1 N1 Y1 58.3(3) 3_656 . ?
O1 N1 O1 116.5(5) . 3_656 ?
C4 C3 C1 123.2(2) . . ?
C8 C3 C4 118.4(2) . . ?
C8 C3 C1 118.4(2) . . ?
N5 C14 C13 108.8(2) . . ?
N5 C14 H14 125.6 . . ?
C13 C14 H14 125.6 . . ?
N3 C11 H11 125.6 . . ?
N3 C11 C10 108.7(2) . . ?
C10 C11 H11 125.6 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C8 H8 119.4 . . ?
C7 C8 C3 121.2(3) . . ?
C7 C8 H8 119.4 . . ?
C1 C2 H2A 117.7 . . ?
C1 C2 H2A 117.7 2_675 . ?
C1 C2 C1 124.6(3) 2_675 . ?
C8 C7 H7 120.0 . . ?
C8 C7 C6 120.0(3) . . ?
C6 C7 H7 120.0 . . ?
N4 C12 C13 109.3(2) . . ?
N4 C12 H12 125.4 . . ?
C13 C12 H12 125.4 . . ?
O3 C1 C3 115.4(2) . . ?
O3 C1 C2 123.6(2) . . ?
C2 C1 C3 121.0(2) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(3) . . ?
C6 C5 H5 119.5 . . ?
C7 C6 H6 120.2 . . ?
C5 C6 C7 119.6(2) . . ?
C5 C6 H6 120.2 . . ?
C9 C10 H10 127.4 . . ?
C11 C10 C9 105.2(2) . . ?
C11 C10 H10 127.4 . . ?
N5 B2 N5 106.01(19) 6_566 . ?
N5 B2 N5 106.01(19) 6_566 12_665 ?
N5 B2 N5 106.01(19) 12_665 . ?
N5 B2 H2 112.7 . . ?
N5 B2 H2 112.7 6_566 . ?
N5 B2 H2 112.7 12_665 . ?
N3 B1 N3 106.34(19) . 6_566 ?
N3 B1 N3 106.34(19) . 12_665 ?
N3 B1 N3 106.34(19) 6_566 12_665 ?
N3 B1 H1 112.4 . . ?
N3 B1 H1 112.4 6_566 . ?
N3 B1 H1 112.4 12_665 . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 1 1 0.801
0 0 2 1.133

_platon_squeeze_details          
;
TITL data_0m_b.res in I23
CELL   20.9091   20.9091   20.9091     90.00     90.00     90.00
SPGR I23
# Solvent Accessible Volume =    1061.2
# Electrons Found in S.A.V. =     211.8
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.138 1.000 0.000 !       1.86 eA-3
C102 0.847 0.945-0.001 !       1.20 eA-3
C103 0.497 0.612 0.372 !       0.92 eA-3
C104 0.373 0.503 0.588 !       0.91 eA-3
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 517 108 ' '
2 0.500 0.500 0.500 517 108 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.53(2)
2 0.47(2)

# start Validation Reply Form
_vrf_PLAT111_y_dbm_no3_sq        
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry .        100 %Fit  
RESPONSE: The structure was solved as an inversion twin. The mirror plane
required in the higher symmetry space group does not allow for the torsion 
in the DBM and nitrate ligands which is visible in I23.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_er_dbm_no3_sq
_database_code_depnum_ccdc_archive 'CCDC 1847188'
_audit_update_record             
;
2018-06-05 deposited with the CCDC.
2018-08-09 downloaded from the CCDC.
;
_audit_creation_date             2018-06-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
loop_
_audit_author_email
kelsey.schulte@chem.tamu.edu
dunbar@chem.tamu.edu
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 Er N2 O10, 1.33(C18 H20 B2 Co1 N12)'
_chemical_formula_sum            'C54 H48.67 B2.67 Co1.33 Er N18 O10'
_chemical_formula_weight         1384.43
_chemical_absolute_configuration ad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 -0.0001 0.0002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.2163 0.3559 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.6111 1.9638 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0005 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_H-M_alt        'I 2 3'
_space_group_name_Hall           'I 2 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+1/2'

_cell_length_a                   20.9076(4)
_cell_length_b                   20.9076(4)
_cell_length_c                   20.9076(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9139.3(5)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    91606
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.60
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.913
_shelx_estimated_absorpt_T_min   0.897
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.6774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1557 before and 0.0577 after correction. The Ratio of minimum to maximum transmission is 0.9267. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.214
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       2
_diffrn_reflns_number            7435
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         20.178
_diffrn_reflns_theta_min         1.387
_diffrn_ambient_temperature      100
_diffrn_detector                 ' Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS hybrid pixel array detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'huber three-circle diffractometer'
_diffrn_measurement_device_type  'Pilatus1M(CdTe) pixel array detector'
_diffrn_measurement_method       '0.5\ ω and 0.5\ φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'Si 111 and Si 311'
_diffrn_radiation_probe          synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_diffrn_source_type              synchrotron
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7091
_reflns_number_total             7435
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_data_collection       'APEX3(Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.702
_refine_diff_density_min         -3.760
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         7435
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0454
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0579P)²+13.3852P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1208
_refine_special_details          
'Refined as a 2-component inversion twin.,SQUEEZE'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.55(3)
 0.45(3)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
3.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C2(H2A), C12(H12), C5(H5), C4(H4), C6(H6), C11(H11), C7(H7),
  C13(H13), C8(H8), C14(H14)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Er1 Er 0.5000 0.5000 0.0000 0.04983(11) Uani 1 4 d S T P . .
Co1 Co 0.24460(2) 0.24460(2) 0.24460(2) 0.02116(11) Uani 1 3 d S T P . .
N2 N 0.17785(13) 0.27437(12) 0.18909(12) 0.0274(4) Uani 1 1 d . . . . .
C9 C 0.15614(16) 0.33325(16) 0.17520(16) 0.0309(5) Uani 1 1 d . . . . .
H9 H 0.1712 0.3720 0.1936 0.037 Uiso 1 1 calc R . . . .
C10 C 0.10790(17) 0.32831(18) 0.12937(17) 0.0355(6) Uani 1 1 d . . . . .
H10 H 0.0840 0.3623 0.1109 0.043 Uiso 1 1 calc R . . . .
N3 N 0.14422(13) 0.23144(14) 0.15322(12) 0.0300(5) Uani 1 1 d . . . . .
C2 C 0.32382(19) 0.5000 0.0000 0.0327(7) Uani 1 2 d S T P . .
H2A H 0.2784 0.5000 0.0000 0.039 Uiso 1 2 calc RS T P . .
O1 O 0.41469(13) 0.43518(13) -0.0113(2) 0.0544(9) Uani 1 1 d . . . . .
N5 N 0.34549(12) 0.25832(12) 0.33644(12) 0.0275(4) Uani 1 1 d . . . . .
C12 C 0.33366(16) 0.15685(15) 0.31395(16) 0.0307(5) Uani 1 1 d . . . . .
H12 H 0.3186 0.1183 0.2951 0.037 Uiso 1 1 calc R . . . .
C5 C 0.21972(18) 0.31832(18) -0.0037(2) 0.0413(7) Uani 1 1 d . . . . .
H5 H 0.1743 0.3169 -0.0032 0.050 Uiso 1 1 calc R . . . .
C4 C 0.25074(15) 0.37756(16) -0.00489(16) 0.0353(5) Uani 1 1 d . . . . .
H4 H 0.2265 0.4160 -0.0054 0.042 Uiso 1 1 calc R . . . .
C6 C 0.2538(2) 0.26199(16) -0.0032(2) 0.0450(8) Uani 1 1 d . . . . .
H6 H 0.2320 0.2221 -0.0026 0.054 Uiso 1 1 calc R . . . .
C3 C 0.31801(14) 0.38000(14) -0.00531(15) 0.0306(5) Uani 1 1 d . . . . .
O3 O 0.5000 0.5000 0.1974(3) 0.0731(15) Uani 1 2 d S T P . .
C1 C 0.35480(13) 0.44101(13) -0.00523(17) 0.0308(5) Uani 1 1 d . . . . .
C11 C 0.10212(17) 0.26417(17) 0.11649(16) 0.0341(6) Uani 1 1 d . . . . .
H11 H 0.0732 0.2457 0.0866 0.041 Uiso 1 1 calc R . . . .
C7 C 0.3201(2) 0.26393(16) -0.0035(2) 0.0427(7) Uani 1 1 d . . . . .
H7 H 0.3437 0.2251 -0.0030 0.051 Uiso 1 1 calc R . . . .
C13 C 0.38190(18) 0.16104(17) 0.36008(17) 0.0350(6) Uani 1 1 d . . . . .
H13 H 0.4054 0.1269 0.3786 0.042 Uiso 1 1 calc R . . . .
O2 O 0.51669(17) 0.54842(19) 0.1060(3) 0.0687(11) Uani 1 1 d . . . . .
C8 C 0.35215(16) 0.32194(14) -0.00468(17) 0.0342(5) Uani 1 1 d . . . . .
H8 H 0.3976 0.3225 -0.0050 0.041 Uiso 1 1 calc R . . . .
N1 N 0.5000 0.5000 0.1384(4) 0.0595(14) Uani 1 2 d S T P . .
N4 N 0.31194(12) 0.21551(12) 0.30046(12) 0.0267(4) Uani 1 1 d . . . . .
B1 B 0.15983(17) 0.15983(17) 0.15983(17) 0.0331(11) Uani 1 3 d S T P . .
H1 H 0.1322 0.1322 0.1322 0.040 Uiso 1 3 calc RS T P . .
C14 C 0.38795(16) 0.22579(18) 0.37294(15) 0.0333(6) Uani 1 1 d . . . . .
H14 H 0.4171 0.2443 0.4025 0.040 Uiso 1 1 calc R . . . .
B2 B 0.32986(17) 0.32986(17) 0.32986(17) 0.0291(10) Uani 1 3 d S T P . .
H2 H 0.3575 0.3575 0.3575 0.035 Uiso 1 3 calc RS T P . .


_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
Er1 O1 2.253(3) . ?
Er1 O1 2.253(3) 2_665 ?
Er1 O1 2.253(3) 4_565 ?
Er1 O1 2.253(3) 3_655 ?
Er1 O2 2.462(5) 4_565 ?
Er1 O2 2.462(5) 3_655 ?
Er1 O2 2.462(5) 2_665 ?
Er1 O2 2.462(5) . ?
Er1 N1 2.893(8) . ?
Er1 N1 2.893(8) 3_655 ?
Co1 N2 1.919(3) . ?
Co1 N2 1.919(3) 9 ?
Co1 N2 1.919(3) 5 ?
Co1 N4 1.928(3) 5 ?
Co1 N4 1.928(3) . ?
Co1 N4 1.928(3) 9 ?
N2 C9 1.344(4) . ?
N2 N3 1.365(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.373(5) . ?
N3 C11 1.354(4) . ?
N3 B1 1.539(4) . ?
C2 H2A 0.9500 . ?
C2 C1 1.397(3) 4_565 ?
C2 C1 1.397(3) . ?
O1 C1 1.264(4) . ?
N5 N4 1.363(4) . ?
N5 C14 1.354(4) . ?
N5 B2 1.537(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.398(5) . ?
C12 N4 1.338(4) . ?
C5 H5 0.9500 . ?
C5 C4 1.398(5) . ?
C5 C6 1.376(6) . ?
C4 H4 0.9500 . ?
C4 C3 1.407(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.387(6) . ?
C3 C1 1.490(4) . ?
C3 C8 1.408(4) . ?
O3 N1 1.235(9) . ?
C11 H11 0.9500 . ?
C7 H7 0.9500 . ?
C7 C8 1.386(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.386(5) . ?
O2 N1 1.266(6) . ?
C8 H8 0.9500 . ?
N1 O2 1.266(6) 2_665 ?
B1 N3 1.539(4) 9 ?
B1 N3 1.539(4) 5 ?
B1 H1 1.0000 . ?
C14 H14 0.9500 . ?
B2 N5 1.537(3) 9 ?
B2 N5 1.537(3) 5 ?
B2 H2 1.0000 . ?

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 Er1 O1 167.9(2) . 2_665 ?
O1 Er1 O1 106.03(14) 2_665 4_565 ?
O1 Er1 O1 75.29(14) . 4_565 ?
O1 Er1 O1 75.29(14) 2_665 3_655 ?
O1 Er1 O1 106.03(14) . 3_655 ?
O1 Er1 O1 167.9(2) 4_565 3_655 ?
O1 Er1 O2 117.03(15) 3_655 3_655 ?
O1 Er1 O2 117.03(15) . . ?
O1 Er1 O2 74.64(15) 3_655 4_565 ?
O1 Er1 O2 117.03(15) 2_665 2_665 ?
O1 Er1 O2 92.31(14) 4_565 2_665 ?
O1 Er1 O2 76.71(14) 3_655 2_665 ?
O1 Er1 O2 76.70(14) . 4_565 ?
O1 Er1 O2 74.64(15) 4_565 3_655 ?
O1 Er1 O2 92.31(14) 2_665 4_565 ?
O1 Er1 O2 92.32(14) 3_655 . ?
O1 Er1 O2 76.70(14) 4_565 . ?
O1 Er1 O2 74.64(15) 2_665 . ?
O1 Er1 O2 92.31(14) . 3_655 ?
O1 Er1 O2 74.65(15) . 2_665 ?
O1 Er1 O2 76.71(14) 2_665 3_655 ?
O1 Er1 O2 117.03(15) 4_565 4_565 ?
O1 Er1 N1 96.04(12) . . ?
O1 Er1 N1 96.04(12) 4_565 3_655 ?
O1 Er1 N1 83.96(12) 3_655 . ?
O1 Er1 N1 83.96(12) 2_665 3_655 ?
O1 Er1 N1 83.96(12) 4_565 . ?
O1 Er1 N1 96.04(12) 3_655 3_655 ?
O1 Er1 N1 96.04(12) 2_665 . ?
O1 Er1 N1 83.96(12) . 3_655 ?
O2 Er1 O2 163.70(17) 3_655 2_665 ?
O2 Er1 O2 163.71(17) 4_565 . ?
O2 Er1 O2 131.44(19) 3_655 . ?
O2 Er1 O2 51.56(19) 4_565 3_655 ?
O2 Er1 O2 131.44(19) 4_565 2_665 ?
O2 Er1 O2 51.56(19) 2_665 . ?
O2 Er1 N1 154.22(10) . 3_655 ?
O2 Er1 N1 154.22(10) 2_665 3_655 ?
O2 Er1 N1 154.22(10) 3_655 . ?
O2 Er1 N1 25.78(10) 3_655 3_655 ?
O2 Er1 N1 154.22(10) 4_565 . ?
O2 Er1 N1 25.78(10) 4_565 3_655 ?
O2 Er1 N1 25.78(10) 2_665 . ?
O2 Er1 N1 25.78(10) . . ?
N1 Er1 N1 180.0 . 3_655 ?
N2 Co1 N2 89.55(11) 9 5 ?
N2 Co1 N2 89.55(11) . 9 ?
N2 Co1 N2 89.55(11) . 5 ?
N2 Co1 N4 90.91(11) 9 5 ?
N2 Co1 N4 179.46(12) . . ?
N2 Co1 N4 90.74(11) 9 . ?
N2 Co1 N4 90.91(11) 5 . ?
N2 Co1 N4 90.74(11) 5 9 ?
N2 Co1 N4 179.47(12) 9 9 ?
N2 Co1 N4 90.90(11) . 9 ?
N2 Co1 N4 179.47(12) 5 5 ?
N2 Co1 N4 90.74(11) . 5 ?
N4 Co1 N4 88.80(11) . 9 ?
N4 Co1 N4 88.80(11) 5 9 ?
N4 Co1 N4 88.80(11) . 5 ?
C9 N2 Co1 132.3(2) . . ?
C9 N2 N3 108.0(3) . . ?
N3 N2 Co1 119.6(2) . . ?
N2 C9 H9 125.5 . . ?
N2 C9 C10 108.9(3) . . ?
C10 C9 H9 125.5 . . ?
C9 C10 H10 127.1 . . ?
C11 C10 C9 105.7(3) . . ?
C11 C10 H10 127.1 . . ?
N2 N3 B1 118.8(3) . . ?
C11 N3 N2 108.3(3) . . ?
C11 N3 B1 132.9(3) . . ?
C1 C2 H2A 117.6 4_565 . ?
C1 C2 H2A 117.6 . . ?
C1 C2 C1 124.8(4) 4_565 . ?
C1 O1 Er1 135.7(2) . . ?
N4 N5 B2 118.7(3) . . ?
C14 N5 N4 108.6(3) . . ?
C14 N5 B2 132.7(3) . . ?
C13 C12 H12 125.3 . . ?
N4 C12 H12 125.3 . . ?
N4 C12 C13 109.4(3) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C6 C5 C4 121.2(3) . . ?
C5 C4 H4 120.1 . . ?
C5 C4 C3 119.7(3) . . ?
C3 C4 H4 120.1 . . ?
C5 C6 H6 120.3 . . ?
C5 C6 C7 119.5(3) . . ?
C7 C6 H6 120.3 . . ?
C4 C3 C1 123.2(3) . . ?
C4 C3 C8 118.4(3) . . ?
C8 C3 C1 118.4(3) . . ?
C2 C1 C3 121.1(3) . . ?
O1 C1 C2 123.5(3) . . ?
O1 C1 C3 115.4(3) . . ?
C10 C11 H11 125.5 . . ?
N3 C11 C10 109.0(3) . . ?
N3 C11 H11 125.5 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.6(3) . . ?
C8 C7 H7 119.7 . . ?
C12 C13 H13 127.4 . . ?
C14 C13 C12 105.1(3) . . ?
C14 C13 H13 127.4 . . ?
N1 O2 Er1 96.5(4) . . ?
C3 C8 H8 119.7 . . ?
C7 C8 C3 120.6(3) . . ?
C7 C8 H8 119.7 . . ?
O3 N1 Er1 180.0 . . ?
O3 N1 O2 122.3(4) . . ?
O3 N1 O2 122.3(4) . 2_665 ?
O2 N1 Er1 57.7(4) 2_665 . ?
O2 N1 Er1 57.7(4) . . ?
O2 N1 O2 115.5(7) 2_665 . ?
N5 N4 Co1 120.19(19) . . ?
C12 N4 Co1 131.7(2) . . ?
C12 N4 N5 108.1(3) . . ?
N3 B1 N3 105.9(3) . 9 ?
N3 B1 N3 105.9(3) . 5 ?
N3 B1 N3 105.9(3) 9 5 ?
N3 B1 H1 112.8 . . ?
N3 B1 H1 112.8 9 . ?
N3 B1 H1 112.8 5 . ?
N5 C14 C13 108.8(3) . . ?
N5 C14 H14 125.6 . . ?
C13 C14 H14 125.6 . . ?
N5 B2 N5 106.0(3) . 9 ?
N5 B2 N5 106.0(3) . 5 ?
N5 B2 N5 106.0(3) 9 5 ?
N5 B2 H2 112.8 . . ?
N5 B2 H2 112.8 9 . ?
N5 B2 H2 112.8 5 . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 1 1 0.801

_platon_squeeze_details          
;
TITL data_0m_a.res in I23
CELL   20.9076   20.9076   20.9076     90.00     90.00     90.00
SPGR I23
# Solvent Accessible Volume =    1066.8
# Electrons Found in S.A.V. =     244.6
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.509 0.658 0.428 !       1.41 eA-3
C102 0.136 1.000 0.000 !       1.39 eA-3
Q103 0.516 1.000 0.000 !       1.12 eA-3
C104 0.955 0.017 0.134 !       1.12 eA-3
C105 0.657 0.508 0.440 !       1.00 eA-3
C106 0.063 0.153 0.993 !       1.00 eA-3
C107 0.862 0.008 0.088 !       0.96 eA-3
C108 0.507 0.619 0.336 !       0.94 eA-3
C109 0.837 0.030 0.018 !       0.90 eA-3
C110 0.820 0.017 0.038 !       0.80 eA-3
C111 0.883 0.122-0.001 !       0.78 eA-3
C112 0.960 0.826 0.057 !       0.63 eA-3
C113 0.095 0.014 0.051 !       0.61 eA-3
Q114 0.398 0.330 0.434 !       0.61 eA-3
Q115 0.602 0.326 0.559 !       0.61 eA-3
Q116 0.958 0.197 0.083 !       0.60 eA-3
Q117 0.572 0.565 0.298 !       0.57 eA-3
Q118 0.192 0.048 0.078 !       0.57 eA-3
C119 0.655 0.481 0.436 !       0.56 eA-3
C120 0.536 0.363 0.384 !       0.52 eA-3
C121 0.986 0.014 0.014 !       0.51 eA-3
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 520 124 ' '
2 0.500 0.500 0.500 520 124 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.55(3)
2 0.45(3)

# start Validation Reply Form
_vrf_PLAT974_er_dbm_no3_sq       
;
PROBLEM: Check Calcd Negative Resid. Density on       Er1      -2.05 eA-3  
RESPONSE: There is some disorder over the center of the Er moiety. Attempts 
to model this disorder were not successful. Adjustments of the absorption 
correction made no appreciable difference.
;
_vrf_PLAT111_er_dbm_no3_sq       
;
PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry .        100 %Fit  
RESPONSE: The structure was solved as an inversion twin. The mirror plane
required in the higher symmetry space group does not allow for the torsion 
in the DBM and nitrate ligands which is visible in I23.
;
# end Validation Reply Form
