# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_PMBB-2-fsc-1
_database_code_depnum_ccdc_archive 'CCDC 1482197'
_audit_update_record             
;
2016-09-30 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H35 Cd2 Cl5 Cr3 N7 O16'
_chemical_formula_weight         1415.80

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'
Cd Cd -0.8075 1.2024 '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'
Cr Cr 0.3209 0.6236 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_H-M_alt        'C c c a'
_space_group_name_Hall           '-C 2b 2bc'

_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, -y+1/2, z'
'x, -y+1/2, -z+1/2'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z'
'x+1/2, -y+1, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y-1/2, z-1/2'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z'
'-x+1/2, y, z-1/2'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   23.751(3)
_cell_length_b                   30.607(4)
_cell_length_c                   23.764(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17275(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9864
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      22.25

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_F_000             5560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.047
_shelx_estimated_absorpt_T_min   0.979
_shelx_estimated_absorpt_T_max   0.979
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Venture Photon CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            107969
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_av_R_equivalents  0.1450
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.662
_diffrn_reflns_theta_max         20.813
_diffrn_reflns_theta_full        20.813
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4531
_reflns_number_gt                2357
_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.
 
 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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1443P)²+413.7282P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4531
_refine_ls_number_parameters     348
_refine_ls_number_restraints     282
_refine_ls_R_factor_all          0.1758
_refine_ls_R_factor_gt           0.0939
_refine_ls_wR_factor_ref         0.3387
_refine_ls_wR_factor_gt          0.2555
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.062
_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
Cd1 Cd 0.6305(3) 0.2500 0.7500 0.340(4) Uani 1 2 d S TU P . .
Cd2 Cd 0.5000 0.5000 1.0000 0.0855(8) Uani 1 2 d S U P . .
Cr1 Cr 0.71754(11) 0.54779(11) 0.78013(10) 0.0879(11) Uani 1 1 d . U . . .
Cr2 Cr 0.7500 0.5000 0.66102(14) 0.0897(15) Uani 1 2 d S T P . .
C1 C 0.7144(9) 0.4106(8) 0.6884(10) 0.111(5) Uani 1 1 d . U . . .
C2 C 0.6741(7) 0.3780(6) 0.6719(9) 0.146(7) Uani 1 1 d G U . . .
C3 C 0.6406(9) 0.3822(6) 0.6243(8) 0.189(11) Uani 1 1 d G U . . .
H3 H 0.6443 0.4071 0.6007 0.227 Uiso 1 1 calc R U . . .
C4 C 0.6015(10) 0.3500(8) 0.6111(10) 0.31(2) Uani 1 1 d G U . . .
H4 H 0.5785 0.3529 0.5785 0.373 Uiso 1 1 calc R U . . .
C5 C 0.5959(11) 0.3135(7) 0.6455(13) 0.30(2) Uani 1 1 d G U . . .
H5 H 0.5692 0.2915 0.6365 0.363 Uiso 1 1 calc R U . . .
N1 N 0.6295(11) 0.3093(6) 0.6931(12) 0.304(9) Uani 1 1 d G U . . .
C6 C 0.6686(9) 0.3415(8) 0.7063(8) 0.205(11) Uani 1 1 d G U . . .
H6 H 0.6915 0.3386 0.7388 0.246 Uiso 1 1 calc R U . . .
C7 C 0.6785(8) 0.4728(8) 0.8431(6) 0.090(4) Uani 1 1 d . U . . .
C8 C 0.6335(8) 0.4501(8) 0.8787(8) 0.113(5) Uani 1 1 d . U . . .
C9 C 0.6284(11) 0.4019(9) 0.8795(11) 0.166(10) Uani 1 1 d . U . . .
H9 H 0.6526 0.3841 0.8575 0.199 Uiso 1 1 calc R U . . .
C10 C 0.5877(14) 0.3838(10) 0.9131(15) 0.222(17) Uani 1 1 d . U . . .
H10 H 0.5812 0.3532 0.9145 0.266 Uiso 1 1 calc R U . . .
C11 C 0.5574(11) 0.4125(9) 0.9441(11) 0.154(9) Uani 1 1 d . U . . .
H11 H 0.5312 0.3996 0.9694 0.185 Uiso 1 1 calc R U . . .
N2 N 0.5584(7) 0.4570(6) 0.9450(6) 0.113(5) Uani 1 1 d . U . . .
C12 C 0.5989(7) 0.4771(7) 0.9124(7) 0.102(5) Uani 1 1 d . U . . .
H12 H 0.6035 0.5079 0.9127 0.122 Uiso 1 1 calc R U . . .
C13 C 0.6392(7) 0.5423(7) 0.6841(7) 0.096(6) Uani 1 1 d . . . . .
C14 C 0.5850(6) 0.5534(7) 0.6590(6) 0.089(6) Uani 1 1 d . . . . .
C15 C 0.5502(8) 0.5837(8) 0.6830(7) 0.123(8) Uani 1 1 d . . . . .
H15 H 0.5605 0.5974 0.7174 0.148 Uiso 1 1 calc R U . . .
C16 C 0.4990(8) 0.5945(8) 0.6567(8) 0.121(8) Uani 1 1 d . . . . .
H16 H 0.4735 0.6154 0.6718 0.145 Uiso 1 1 calc R U . . .
C17 C 0.4886(8) 0.5725(9) 0.6074(8) 0.128(9) Uani 1 1 d . . . . .
H17 H 0.4541 0.5786 0.5888 0.153 Uiso 1 1 calc R U . . .
N3 N 0.5234(6) 0.5426(6) 0.5827(6) 0.102(5) Uani 1 1 d . . . . .
C18 C 0.5713(7) 0.5337(7) 0.6087(7) 0.097(6) Uani 1 1 d . . . . .
H18 H 0.5967 0.5134 0.5924 0.117 Uiso 1 1 calc R U . . .
O1 O 0.7500 0.5000 0.7426(5) 0.064(4) Uani 1 2 d S T P . .
O2 O 0.7178(6) 0.4433(5) 0.6559(5) 0.118(4) Uani 1 1 d . U . . .
O3 O 0.7410(5) 0.4081(5) 0.7350(6) 0.112(4) Uani 1 1 d . U . . .
O5 O 0.6719(5) 0.5111(5) 0.8314(4) 0.097(3) Uani 1 1 d . U . . .
O6 O 0.6495(4) 0.5539(4) 0.7335(4) 0.093(4) Uani 1 1 d . . . . .
O7 O 0.6750(5) 0.5235(5) 0.6531(4) 0.113(5) Uani 1 1 d . . . . .
O8 O 0.7500 0.5000 0.5769(5) 0.101(6) Uani 1 2 d DS TU P . .
O9 O 0.6847(5) 0.6021(5) 0.8233(5) 0.127(5) Uani 1 1 d . . . . .
O10 O 0.7191(5) 0.4474(4) 0.8338(5) 0.103(4) Uani 1 1 d . U . . .
N4 N 0.7411(9) 0.4646(8) 0.4945(7) 0.121(9) Uani 0.5 1 d D U P A -1
C19 C 0.7242(17) 0.4267(11) 0.4631(11) 0.167(17) Uani 0.5 1 d D U P A -1
H19A H 0.6959 0.4362 0.4357 0.250 Uiso 0.5 1 d R U P A -1
H19B H 0.7561 0.4135 0.4432 0.250 Uiso 0.5 1 d R U P A -1
H19C H 0.7075 0.4051 0.4886 0.250 Uiso 0.5 1 d R U P A -1
C20 C 0.767(2) 0.5006(11) 0.4643(10) 0.22(4) Uani 0.5 1 d D U P A -1
H20A H 0.8002 0.4898 0.4445 0.327 Uiso 0.5 1 d R U P A -1
H20B H 0.7399 0.5126 0.4370 0.327 Uiso 0.5 1 d R U P A -1
H20C H 0.7778 0.5236 0.4909 0.327 Uiso 0.5 1 d R U P A -1
C21 C 0.7339(11) 0.4675(6) 0.5497(7) 0.123(11) Uani 0.5 1 d D U P A -1
H21 H 0.7161 0.4442 0.5691 0.148 Uiso 0.5 1 calc R U P A -1
Cl1 Cl 0.7314(14) 0.2345(11) 0.7137(16) 0.431(15) Uani 0.5 1 d D U P . .
Cl2 Cl 0.5543(16) 0.2174(11) 0.6991(17) 0.453(15) Uani 0.5 1 d D U P . .
Cl3 Cl 0.6246(15) 0.2940(9) 0.8326(15) 0.399(12) Uani 0.5 1 d D U P . .
Cl4 Cl 0.41608(19) 0.4494(2) 0.98358(18) 0.117(2) Uani 1 1 d . 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
Cd1 N1 2.263(17) . ?
Cd1 N1 2.263(17) 3_556 ?
Cd1 Cl3 2.39(3) . ?
Cd1 Cl3 2.39(3) 3_556 ?
Cd1 Cl2 2.39(4) . ?
Cd1 Cl2 2.39(4) 3_556 ?
Cd1 Cl1 2.59(3) . ?
Cd1 Cl1 2.59(3) 3_556 ?
Cd2 N2 2.316(16) . ?
Cd2 N2 2.316(15) 9_667 ?
Cd2 N3 2.423(15) 12_566 ?
Cd2 N3 2.423(15) 4_656 ?
Cd2 Cl4 2.554(5) . ?
Cd2 Cl4 2.554(5) 9_667 ?
Cr1 O1 1.878(6) . ?
Cr1 O6 1.968(10) . ?
Cr1 O10 1.977(11) 6_655 ?
Cr1 O5 1.978(13) . ?
Cr1 O3 1.984(14) 6_655 ?
Cr1 O9 2.102(14) . ?
Cr2 O2 1.900(15) 6_655 ?
Cr2 O2 1.900(15) . ?
Cr2 O7 1.931(11) 6_655 ?
Cr2 O7 1.931(11) . ?
Cr2 O1 1.939(11) . ?
Cr2 O8 2.000(12) . ?
C1 O2 1.27(2) . ?
C1 O3 1.28(2) . ?
C1 C2 1.44(3) . ?
C2 C3 1.3900 . ?
C2 C6 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 N1 1.3900 . ?
C5 H5 0.9500 . ?
N1 C6 1.3900 . ?
C6 H6 0.9500 . ?
C7 O5 1.22(2) . ?
C7 O10 1.26(2) . ?
C7 C8 1.53(3) . ?
C8 C12 1.41(2) . ?
C8 C9 1.48(3) . ?
C9 C10 1.37(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.36(3) . ?
C10 H10 0.9500 . ?
C11 N2 1.36(3) . ?
C11 H11 0.9500 . ?
N2 C12 1.38(2) . ?
C12 H12 0.9500 . ?
C13 O6 1.251(18) . ?
C13 O7 1.263(19) . ?
C13 C14 1.46(2) . ?
C14 C15 1.37(2) . ?
C14 C18 1.38(2) . ?
C15 C16 1.41(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.37(3) . ?
C16 H16 0.9500 . ?
C17 N3 1.37(2) . ?
C17 H17 0.9500 . ?
N3 C18 1.32(2) . ?
N3 Cd2 2.423(15) 4_656 ?
C18 H18 0.9500 . ?
O1 Cr1 1.878(6) 6_655 ?
O3 Cr1 1.984(14) 6_655 ?
O8 C21 1.244(10) . ?
O10 Cr1 1.977(11) 6_655 ?
N4 C21 1.327(9) . ?
N4 C19 1.437(9) . ?
N4 C20 1.450(9) . ?
C19 H19A 0.9801 . ?
C19 H19B 0.9794 . ?
C19 H19C 0.9799 . ?
C20 H20A 0.9806 . ?
C20 H20B 0.9803 . ?
C20 H20C 0.9811 . ?
C21 H21 0.9500 . ?
Cl1 Cl1 1.97(7) 3_556 ?
Cl2 Cl3 1.86(5) 3_556 ?
Cl3 Cl2 1.86(5) 3_556 ?

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
N1 Cd1 N1 179(3) . 3_556 ?
N1 Cd1 Cl3 92.2(10) . . ?
N1 Cd1 Cl3 88(2) 3_556 . ?
N1 Cd1 Cl3 87.7(10) . 3_556 ?
N1 Cd1 Cl3 92(2) 3_556 3_556 ?
Cl3 Cd1 Cl3 173.2(17) . 3_556 ?
N1 Cd1 Cl2 91.4(12) . . ?
N1 Cd1 Cl2 88(2) 3_556 . ?
Cl3 Cd1 Cl2 127.3(13) . . ?
Cl3 Cd1 Cl2 45.9(12) 3_556 . ?
N1 Cd1 Cl2 87.7(11) . 3_556 ?
N1 Cd1 Cl2 91(3) 3_556 3_556 ?
Cl3 Cd1 Cl2 45.9(12) . 3_556 ?
Cl3 Cd1 Cl2 127.3(13) 3_556 3_556 ?
Cl2 Cd1 Cl2 81.8(18) . 3_556 ?
N1 Cd1 Cl1 87.6(11) . . ?
N1 Cd1 Cl1 94(2) 3_556 . ?
Cl3 Cd1 Cl1 115.6(11) . . ?
Cl3 Cd1 Cl1 71.1(12) 3_556 . ?
Cl2 Cd1 Cl1 117.0(11) . . ?
Cl2 Cd1 Cl1 160.7(13) 3_556 . ?
N1 Cd1 Cl1 93.5(11) . 3_556 ?
N1 Cd1 Cl1 88(2) 3_556 3_556 ?
Cl3 Cd1 Cl1 71.1(12) . 3_556 ?
Cl3 Cd1 Cl1 115.6(11) 3_556 3_556 ?
Cl2 Cd1 Cl1 160.7(13) . 3_556 ?
Cl2 Cd1 Cl1 117.0(11) 3_556 3_556 ?
Cl1 Cd1 Cl1 44.7(16) . 3_556 ?
N2 Cd2 N2 180.0 . 9_667 ?
N2 Cd2 N3 90.8(5) . 12_566 ?
N2 Cd2 N3 89.2(5) 9_667 12_566 ?
N2 Cd2 N3 89.2(5) . 4_656 ?
N2 Cd2 N3 90.8(5) 9_667 4_656 ?
N3 Cd2 N3 180.0(4) 12_566 4_656 ?
N2 Cd2 Cl4 92.1(5) . . ?
N2 Cd2 Cl4 87.9(5) 9_667 . ?
N3 Cd2 Cl4 88.7(4) 12_566 . ?
N3 Cd2 Cl4 91.3(4) 4_656 . ?
N2 Cd2 Cl4 87.9(5) . 9_667 ?
N2 Cd2 Cl4 92.1(5) 9_667 9_667 ?
N3 Cd2 Cl4 91.3(4) 12_566 9_667 ?
N3 Cd2 Cl4 88.7(4) 4_656 9_667 ?
Cl4 Cd2 Cl4 180.0(2) . 9_667 ?
O1 Cr1 O6 98.3(4) . . ?
O1 Cr1 O10 93.0(4) . 6_655 ?
O6 Cr1 O10 168.7(5) . 6_655 ?
O1 Cr1 O5 94.3(4) . . ?
O6 Cr1 O5 87.2(5) . . ?
O10 Cr1 O5 93.6(5) 6_655 . ?
O1 Cr1 O3 94.0(5) . 6_655 ?
O6 Cr1 O3 92.2(5) . 6_655 ?
O10 Cr1 O3 85.4(5) 6_655 6_655 ?
O5 Cr1 O3 171.7(6) . 6_655 ?
O1 Cr1 O9 177.5(4) . . ?
O6 Cr1 O9 84.0(5) . . ?
O10 Cr1 O9 84.8(5) 6_655 . ?
O5 Cr1 O9 86.9(6) . . ?
O3 Cr1 O9 84.8(6) 6_655 . ?
O2 Cr2 O2 172.6(8) 6_655 . ?
O2 Cr2 O7 87.9(6) 6_655 6_655 ?
O2 Cr2 O7 91.4(6) . 6_655 ?
O2 Cr2 O7 91.4(6) 6_655 . ?
O2 Cr2 O7 87.9(6) . . ?
O7 Cr2 O7 168.8(7) 6_655 . ?
O2 Cr2 O1 93.7(4) 6_655 . ?
O2 Cr2 O1 93.7(4) . . ?
O7 Cr2 O1 95.6(3) 6_655 . ?
O7 Cr2 O1 95.6(3) . . ?
O2 Cr2 O8 86.3(4) 6_655 . ?
O2 Cr2 O8 86.3(4) . . ?
O7 Cr2 O8 84.4(3) 6_655 . ?
O7 Cr2 O8 84.4(3) . . ?
O1 Cr2 O8 180.0 . . ?
O2 C1 O3 123(2) . . ?
O2 C1 C2 115(2) . . ?
O3 C1 C2 122(2) . . ?
C3 C2 C6 120.0 . . ?
C3 C2 C1 123(2) . . ?
C6 C2 C1 117(2) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
N1 C5 C4 120.0 . . ?
N1 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 N1 C5 120.0 . . ?
C6 N1 Cd1 115.3(15) . . ?
C5 N1 Cd1 124.6(15) . . ?
N1 C6 C2 120.0 . . ?
N1 C6 H6 120.0 . . ?
C2 C6 H6 120.0 . . ?
O5 C7 O10 130.8(19) . . ?
O5 C7 C8 118.5(18) . . ?
O10 C7 C8 110.6(19) . . ?
C12 C8 C9 121.7(19) . . ?
C12 C8 C7 117(2) . . ?
C9 C8 C7 121.2(18) . . ?
C10 C9 C8 118(2) . . ?
C10 C9 H9 121.0 . . ?
C8 C9 H9 121.0 . . ?
C11 C10 C9 115(3) . . ?
C11 C10 H10 122.3 . . ?
C9 C10 H10 122.3 . . ?
C10 C11 N2 130(2) . . ?
C10 C11 H11 114.8 . . ?
N2 C11 H11 114.8 . . ?
C11 N2 C12 116.6(18) . . ?
C11 N2 Cd2 124.5(14) . . ?
C12 N2 Cd2 118.8(15) . . ?
N2 C12 C8 118(2) . . ?
N2 C12 H12 121.2 . . ?
C8 C12 H12 121.2 . . ?
O6 C13 O7 123.0(15) . . ?
O6 C13 C14 119.4(16) . . ?
O7 C13 C14 117.5(15) . . ?
C15 C14 C18 121.0(16) . . ?
C15 C14 C13 121.4(16) . . ?
C18 C14 C13 117.5(17) . . ?
C14 C15 C16 119.8(17) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C16 C15 114.7(19) . . ?
C17 C16 H16 122.6 . . ?
C15 C16 H16 122.6 . . ?
N3 C17 C16 125.9(17) . . ?
N3 C17 H17 117.0 . . ?
C16 C17 H17 117.0 . . ?
C18 N3 C17 117.2(16) . . ?
C18 N3 Cd2 117.8(13) . 4_656 ?
C17 N3 Cd2 124.7(11) . 4_656 ?
N3 C18 C14 121.3(18) . . ?
N3 C18 H18 119.4 . . ?
C14 C18 H18 119.4 . . ?
Cr1 O1 Cr1 123.4(6) 6_655 . ?
Cr1 O1 Cr2 118.3(3) 6_655 . ?
Cr1 O1 Cr2 118.3(3) . . ?
C1 O2 Cr2 135.1(15) . . ?
C1 O3 Cr1 132.4(16) . 6_655 ?
C7 O5 Cr1 128.2(12) . . ?
C13 O6 Cr1 131.5(11) . . ?
C13 O7 Cr2 137.2(10) . . ?
C21 O8 Cr2 121.2(10) . . ?
C7 O10 Cr1 130.6(13) . 6_655 ?
C21 N4 C19 122.3(9) . . ?
C21 N4 C20 119.4(8) . . ?
C19 N4 C20 118.4(8) . . ?
N4 C19 H19A 107.2 . . ?
N4 C19 H19B 111.5 . . ?
H19A C19 H19B 109.5 . . ?
N4 C19 H19C 109.6 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 H20A 108.8 . . ?
N4 C20 H20B 109.7 . . ?
H20A C20 H20B 109.4 . . ?
N4 C20 H20C 109.9 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.4 . . ?
O8 C21 N4 121.9(12) . . ?
O8 C21 H21 119.0 . . ?
N4 C21 H21 119.0 . . ?
Cl1 Cl1 Cd1 67.7(8) 3_556 . ?
Cl3 Cl2 Cd1 66.8(12) 3_556 . ?
Cl2 Cl3 Cd1 67.3(17) 3_556 . ?

_refine_diff_density_max         1.121
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.117



# start Validation Reply Form
_vrf_THETM01_PMBB-2-fsc-1        
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Crystal didn't diffract past aproximately 0.95-1A 
resolution. 
;
# 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_PMBB-2-acs-1
_database_code_depnum_ccdc_archive 'CCDC 1482198'
_audit_update_record             
;
2016-09-30 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H54 Cr3 Cu3 N13 O49'
_chemical_formula_weight         1799.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

_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, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -z-1/2'

_cell_length_a                   20.772(9)
_cell_length_b                   20.772(9)
_cell_length_c                   21.0530(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7867(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1497
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      42.52

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.760
_exptl_crystal_F_000             1824
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.468
_shelx_estimated_absorpt_T_min   0.866
_shelx_estimated_absorpt_T_max   0.908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8710
_exptl_absorpt_correction_T_max  0.9113
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19289
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.098
_diffrn_reflns_theta_max         42.515
_diffrn_reflns_theta_full        42.515
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             1933
_reflns_number_gt                1576
_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.
 
 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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1589P)²+6.9950P] 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         1933
_refine_ls_number_parameters     121
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0726
_refine_ls_wR_factor_ref         0.2411
_refine_ls_wR_factor_gt          0.2137
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.093
_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
Cr1 Cr 0.75976(12) 0.42354(12) 0.2500 0.0887(9) Uani 1 2 d S T P . .
O1 O 0.6667 0.3333 0.2500 0.070(3) Uani 1 6 d S T P . .
Cu1 Cu 0.5000 0.5000 0.5000 0.1632(14) Uani 1 2 d S . P . .
O2 O 0.8609(6) 0.5209(6) 0.2500 0.131(3) Uani 1 2 d S T P . .
O3 O 0.4729(7) 0.5140(7) 0.4043(6) 0.217(5) Uani 1 1 d . . . . .
O10 O 0.7318(5) 0.4696(4) 0.3181(3) 0.114(2) Uani 1 1 d D . . . .
O11 O 0.6077(5) 0.4109(5) 0.3164(3) 0.105(2) Uani 1 1 d D . . . .
C10 C 0.6688(6) 0.4553(6) 0.3384(5) 0.104(3) Uani 1 1 d D . . . .
C11 C 0.6731(8) 0.5015(7) 0.3939(5) 0.128(4) Uani 1 1 d D . . . .
C12 C 0.6058(7) 0.4872(7) 0.4219(6) 0.126(4) Uani 1 1 d D . . . .
H12 H 0.5608 0.4496 0.4036 0.151 Uiso 1 1 calc R U . . .
N10 N 0.6012(8) 0.5235(8) 0.4729(6) 0.146(4) Uani 1 1 d D . . . .
C13 C 0.6665(12) 0.5748(11) 0.4993(8) 0.196(8) Uani 1 1 d D . . . .
H13 H 0.6642 0.6025 0.5342 0.235 Uiso 1 1 calc R U . . .
C14 C 0.7365(12) 0.5899(12) 0.4795(10) 0.211(9) Uani 1 1 d D . . . .
H14 H 0.7802 0.6228 0.5023 0.253 Uiso 1 1 calc R U . . .
C15 C 0.7394(8) 0.5542(9) 0.4241(8) 0.178(6) Uani 1 1 d D . . . .
H15 H 0.7861 0.5655 0.4068 0.214 Uiso 1 1 calc R U . . .
O21 O 0.5485(7) 0.6298(7) 0.5174(6) 0.207(5) 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
Cr1 O1 1.904(2) . ?
Cr1 O11 1.942(8) 4_665 ?
Cr1 O11 1.942(8) 11_666 ?
Cr1 O10 1.966(8) 8_556 ?
Cr1 O10 1.966(8) . ?
Cr1 O2 2.063(10) . ?
O1 Cr1 1.904(2) 4_665 ?
O1 Cr1 1.905(2) 3_655 ?
Cu1 N10 1.989(13) . ?
Cu1 N10 1.989(13) 7_666 ?
Cu1 O3 2.150(13) 7_666 ?
Cu1 O3 2.150(13) . ?
Cu1 O21 2.389(12) . ?
Cu1 O21 2.389(12) 7_666 ?
O10 C10 1.264(8) . ?
O11 C10 1.227(8) . ?
O11 Cr1 1.942(8) 3_655 ?
C10 C11 1.486(9) . ?
C11 C12 1.406(9) . ?
C11 C15 1.412(9) . ?
C12 N10 1.341(9) . ?
C12 H12 0.9500 . ?
N10 C13 1.357(9) . ?
C13 C14 1.389(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.398(9) . ?
C14 H14 0.9500 . ?
C15 H15 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 Cr1 O11 94.8(2) . 4_665 ?
O1 Cr1 O11 94.8(2) . 11_666 ?
O11 Cr1 O11 92.0(4) 4_665 11_666 ?
O1 Cr1 O10 94.4(2) . 8_556 ?
O11 Cr1 O10 170.7(3) 4_665 8_556 ?
O11 Cr1 O10 86.4(3) 11_666 8_556 ?
O1 Cr1 O10 94.4(2) . . ?
O11 Cr1 O10 86.4(3) 4_665 . ?
O11 Cr1 O10 170.7(3) 11_666 . ?
O10 Cr1 O10 93.7(5) 8_556 . ?
O1 Cr1 O2 179.7(4) . . ?
O11 Cr1 O2 84.9(3) 4_665 . ?
O11 Cr1 O2 84.9(3) 11_666 . ?
O10 Cr1 O2 85.8(3) 8_556 . ?
O10 Cr1 O2 85.8(3) . . ?
Cr1 O1 Cr1 120.0 4_665 . ?
Cr1 O1 Cr1 120.0 4_665 3_655 ?
Cr1 O1 Cr1 120.0 . 3_655 ?
N10 Cu1 N10 180.0 . 7_666 ?
N10 Cu1 O3 89.2(5) . 7_666 ?
N10 Cu1 O3 90.8(5) 7_666 7_666 ?
N10 Cu1 O3 90.8(5) . . ?
N10 Cu1 O3 89.2(5) 7_666 . ?
O3 Cu1 O3 180.0 7_666 . ?
N10 Cu1 O21 88.3(5) . . ?
N10 Cu1 O21 91.7(5) 7_666 . ?
O3 Cu1 O21 91.0(5) 7_666 . ?
O3 Cu1 O21 89.0(5) . . ?
N10 Cu1 O21 91.7(5) . 7_666 ?
N10 Cu1 O21 88.3(5) 7_666 7_666 ?
O3 Cu1 O21 89.0(5) 7_666 7_666 ?
O3 Cu1 O21 91.0(5) . 7_666 ?
O21 Cu1 O21 180.0 . 7_666 ?
C10 O10 Cr1 131.0(6) . . ?
C10 O11 Cr1 132.8(6) . 3_655 ?
O11 C10 O10 127.6(9) . . ?
O11 C10 C11 119.3(10) . . ?
O10 C10 C11 113.1(10) . . ?
C12 C11 C15 117.2(10) . . ?
C12 C11 C10 117.4(12) . . ?
C15 C11 C10 125.2(13) . . ?
N10 C12 C11 124.0(11) . . ?
N10 C12 H12 118.0 . . ?
C11 C12 H12 118.0 . . ?
C12 N10 C13 116.4(12) . . ?
C12 N10 Cu1 117.1(12) . . ?
C13 N10 Cu1 126.5(12) . . ?
N10 C13 C14 125.3(14) . . ?
N10 C13 H13 117.4 . . ?
C14 C13 H13 117.4 . . ?
C13 C14 C15 116.6(15) . . ?
C13 C14 H14 121.7 . . ?
C15 C14 H14 121.7 . . ?
C14 C15 C11 120.2(13) . . ?
C14 C15 H15 119.9 . . ?
C11 C15 H15 119.9 . . ?

_refine_diff_density_max         0.342
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.058



_vrf_CHEMW03_PMBB-2-acs-1        
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The formula includes havily disordered nitrate anion
that could not be reliably modeled.
;

# 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_PMBB-2-rtl-1
_database_code_depnum_ccdc_archive 'CCDC 1482199'
_audit_update_record             
;
2016-09-30 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H70 Cd2 Cr3 N11 O41'
_chemical_formula_weight         1813.93

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 0.0000 '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'
Cd Cd -1.1370 2.9560 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.1620 0.2220 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_H-M_alt        'P -4 21 c'
_space_group_name_Hall           'P -4 2n'

_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, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y, x, -z'
'y, -x, -z'

_cell_length_a                   20.608(2)
_cell_length_b                   20.608(2)
_cell_length_c                   22.350(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9491.7(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9449
_cell_measurement_theta_min      0.78
_cell_measurement_theta_max      14.98

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_F_000             3676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.660
_shelx_estimated_absorpt_T_min   0.937
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9374
_exptl_absorpt_correction_T_max  0.9870
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.41328
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            73700
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.265
_diffrn_reflns_theta_max         14.984
_diffrn_reflns_theta_full        14.357
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             9447
_reflns_number_gt                7662
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.823
_reflns_Friedel_fraction_max     0.957
_reflns_Friedel_fraction_full    0.982

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1031P)²+5.5754P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2997 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9447
_refine_ls_number_parameters     543
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0562
_refine_ls_wR_factor_ref         0.1716
_refine_ls_wR_factor_gt          0.1568
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Cd1 Cd 0.71886(4) 1.20871(3) 0.11437(3) 0.0646(3) Uani 1 1 d . . . . .
Cr1 Cr 0.5000 1.0000 0.44649(7) 0.0336(3) Uani 1 2 d S T P . .
Cr2 Cr 0.57764(5) 0.98055(5) 0.31920(5) 0.0373(3) Uani 1 1 d . . . . .
O31 O 0.5000 1.0000 0.3615(3) 0.0346(13) Uani 1 2 d S T P B .
O63 O 0.6966(4) 1.3241(3) 0.1185(5) 0.093(2) Uani 1 1 d D U . . .
O35 O 0.6042(2) 0.9104(2) 0.3742(2) 0.0430(12) Uani 1 1 d . . . . .
O33 O 0.5363(2) 0.9121(2) 0.4530(2) 0.0427(11) Uani 1 1 d . . . . .
N40 N 0.6847(4) 0.7399(4) 0.4287(4) 0.066(2) Uani 1 1 d . . . . .
C41 C 0.6571(4) 0.7953(4) 0.4111(4) 0.0510(19) Uani 1 1 d . . . . .
H41 H 0.6739 0.8168 0.3768 0.061 Uiso 1 1 calc R U . . .
C39 C 0.6573(7) 0.7084(6) 0.4758(5) 0.087(4) Uani 1 1 d . . . . .
H39 H 0.6748 0.6676 0.4873 0.105 Uiso 1 1 calc R U . . .
C38 C 0.6067(6) 0.7320(5) 0.5071(5) 0.083(3) Uani 1 1 d . . . . .
H38 H 0.5911 0.7092 0.5411 0.100 Uiso 1 1 calc R U . . .
C36 C 0.6046(4) 0.8228(4) 0.4410(4) 0.0517(19) Uani 1 1 d . . . . .
C34 C 0.5796(4) 0.8864(4) 0.4210(4) 0.0428(16) Uani 1 1 d . . . . .
C37 C 0.5771(6) 0.7897(5) 0.4900(5) 0.072(3) Uani 1 1 d . . . . .
H37 H 0.5400 0.8060 0.5103 0.086 Uiso 1 1 calc R U . . .
O11 O 0.3704(2) 0.9545(2) 0.3617(2) 0.0426(11) Uani 1 1 d . . . . .
O12 O 0.4137(2) 0.9588(2) 0.4540(2) 0.0397(11) Uani 1 1 d . . . . .
N11 N 0.2813(4) 0.8237(5) 0.5166(4) 0.071(2) Uani 1 1 d . . . . .
C11 C 0.3250(4) 0.8671(5) 0.4944(4) 0.058(2) Uani 1 1 d . . . . .
H11 H 0.3596 0.8807 0.5196 0.070 Uiso 1 1 calc R U . . .
C12 C 0.2338(5) 0.8063(6) 0.4803(5) 0.082(3) Uani 1 1 d . . . . .
H12 H 0.2032 0.7753 0.4943 0.098 Uiso 1 1 calc R U . . .
C13 C 0.3220(4) 0.8922(4) 0.4373(4) 0.052(2) Uani 1 1 d . . . . .
C14 C 0.2259(6) 0.8307(7) 0.4226(5) 0.087(4) Uani 1 1 d . . . . .
H14 H 0.1894 0.8185 0.3992 0.104 Uiso 1 1 calc R U . . .
C15 C 0.2725(4) 0.8732(5) 0.3998(4) 0.067(3) Uani 1 1 d . . . . .
H15 H 0.2702 0.8885 0.3598 0.080 Uiso 1 1 calc R U . . .
C16 C 0.3731(3) 0.9390(4) 0.4162(4) 0.0424(16) Uani 1 1 d . . . . .
O21 O 0.4632(2) 1.0874(2) 0.2703(2) 0.0418(11) Uani 1 1 d . . . . .
O22 O 0.5632(2) 1.0481(2) 0.2573(3) 0.0417(11) Uani 1 1 d . . . . .
N21 N 0.6134(4) 1.1986(4) 0.1497(4) 0.0610(19) Uani 1 1 d . . . . .
C21 C 0.5203(4) 1.0881(3) 0.2480(3) 0.0427(16) Uani 1 1 d . . . . .
C22 C 0.5979(4) 1.1508(4) 0.1862(4) 0.0510(18) Uani 1 1 d . . . . .
H22 H 0.6304 1.1207 0.1980 0.061 Uiso 1 1 calc R U . . .
C23 C 0.4880(5) 1.1871(4) 0.1913(5) 0.068(3) Uani 1 1 d . . . . .
H23 H 0.4449 1.1835 0.2061 0.082 Uiso 1 1 calc R U . . .
C24 C 0.5051(6) 1.2379(6) 0.1518(7) 0.094(4) Uani 1 1 d . . . . .
H24 H 0.4737 1.2688 0.1391 0.112 Uiso 1 1 calc R U . . .
C25 C 0.5346(4) 1.1434(4) 0.2077(4) 0.053(2) Uani 1 1 d . . . . .
C26 C 0.5669(5) 1.2416(5) 0.1324(6) 0.083(3) Uani 1 1 d . . . . .
H26 H 0.5784 1.2755 0.1057 0.099 Uiso 1 1 calc R U . . .
O51 O 0.6599(2) 0.9576(3) 0.2735(3) 0.0499(13) Uani 1 1 d D U . . .
O56 O 0.7697(6) 1.2460(5) 0.2056(4) 0.103(3) Uani 1 1 d . U . . .
O54 O 0.7470(6) 1.1484(6) 0.2127(6) 0.128(3) Uani 1 1 d . U . . .
N55 N 0.7745(6) 1.1936(6) 0.2354(5) 0.103(3) Uani 1 1 d . U . . .
O57 O 0.8020(7) 1.1876(7) 0.2831(4) 0.140(4) Uani 1 1 d . U . . .
N61 N 0.4910(9) 1.1207(9) 0.6281(9) 0.074(5) Uani 0.5 1 d . . P A 1
O58 O 0.4472(10) 1.0864(13) 0.6435(11) 0.098(6) Uani 0.5 1 d . . P A 1
O60 O 0.5300(8) 1.1055(9) 0.5873(7) 0.084(4) Uani 0.5 1 d . . P A 1
O59 O 0.4987(9) 1.1756(8) 0.6574(9) 0.096(5) Uani 0.5 1 d . . P A 1
O61 O 0.5000 1.0000 0.5364(4) 0.0481(17) Uani 1 2 d DS T P B 2
C61 C 0.5206(8) 1.0527(8) 0.5737(8) 0.056(4) Uani 0.5 1 d D . P B 2
H61A H 0.5630 1.0418 0.5920 0.067 Uiso 0.5 1 d R U P B 2
H61B H 0.5254 1.0917 0.5482 0.067 Uiso 0.5 1 d R U P B 2
C62 C 0.4749(15) 1.0681(13) 0.6202(10) 0.101(10) Uani 0.5 1 d D . P B 2
H62A H 0.4328 1.0795 0.6027 0.151 Uiso 0.5 1 d R U P B 2
H62B H 0.4699 1.0301 0.6460 0.151 Uiso 0.5 1 d R U P B 2
H62C H 0.4911 1.1048 0.6439 0.151 Uiso 0.5 1 d R U P B 2
N71 N 0.7462(10) 1.0604(8) 0.1000(7) 0.061(4) Uani 0.5 1 d . U P C 3
O71 O 0.7900(13) 1.1003(9) 0.0948(14) 0.141(9) Uani 0.5 1 d . U P C 3
O72 O 0.6979(11) 1.0877(9) 0.1010(7) 0.089(4) Uani 0.5 1 d . U P C 3
O73 O 0.7531(9) 1.0079(6) 0.1009(6) 0.076(4) Uani 0.5 1 d . U P C 3
O74 O 0.7373(9) 1.0955(12) 0.0835(14) 0.133(10) Uani 0.5 1 d . . P C 4
O48 O 0.6752(5) 0.8448(6) 0.2221(5) 0.111(3) Uani 1 1 d D . . . .
O42 O 0.0885(6) 0.7873(9) 0.5298(9) 0.109(6) Uani 0.5 1 d D U P . .
O45 O 0.4391(12) 0.7861(10) 0.3585(10) 0.122(7) Uani 0.5 1 d D U P D 1
C43 C 0.0470(11) 0.7362(12) 0.5239(15) 0.118(9) Uani 0.5 1 d D U P . .
H43A H 0.0028 0.7525 0.5154 0.141 Uiso 0.5 1 calc R U P . .
H43B H 0.0455 0.7115 0.5618 0.141 Uiso 0.5 1 calc R U P . .
C46 C 0.3890(19) 0.7596(17) 0.3266(18) 0.142(13) Uani 0.5 1 d D U P D 1
H46A H 0.3971 0.7638 0.2836 0.213 Uiso 0.5 1 d R U P D 1
H46B H 0.3847 0.7136 0.3370 0.213 Uiso 0.5 1 d R U P D 1
H46C H 0.3489 0.7825 0.3370 0.213 Uiso 0.5 1 d R U P D 1
C44 C 0.068(2) 0.6930(19) 0.4747(18) 0.167(13) Uani 0.5 1 d D U P . .
H44A H 0.0745 0.7159 0.4367 0.250 Uiso 0.5 1 d R U P . .
H44B H 0.1102 0.6767 0.4890 0.250 Uiso 0.5 1 d R U P . .
H44C H 0.0385 0.6565 0.4688 0.250 Uiso 0.5 1 d R U P . .
C52B C 0.7095(9) 1.0022(9) 0.2565(10) 0.047(5) Uiso 0.35 1 d D U P E 1
H52A H 0.7160 1.0335 0.2895 0.057 Uiso 0.35 1 calc R U P E 1
H52B H 0.6946 1.0268 0.2211 0.057 Uiso 0.35 1 calc R U P E 1
C49 C 0.7131(13) 0.8490(13) 0.1652(8) 0.198(12) Uani 1 1 d D . . . .
H49A H 0.6975 0.8159 0.1372 0.297 Uiso 1 1 calc R U . . .
H49B H 0.7592 0.8417 0.1737 0.297 Uiso 1 1 calc DR U . . .
H49C H 0.7074 0.8921 0.1475 0.297 Uiso 1 1 calc DR U . . .
C64 C 0.6790(17) 1.3566(15) 0.1715(13) 0.122(10) Uani 0.5 1 d D U P . .
H64A H 0.6645 1.3998 0.1591 0.183 Uiso 0.5 1 d R U P . .
H64B H 0.6450 1.3358 0.1955 0.183 Uiso 0.5 1 d R U P . .
H64C H 0.7186 1.3605 0.1955 0.183 Uiso 0.5 1 d R U P . .
O1 O 0.031(2) 0.866(2) 0.449(2) 0.117(12) Uiso 0.25 1 d . . P . .
O81 O 0.413(3) 0.742(2) 0.402(2) 0.131(15) Uiso 0.25 1 d . . P F 2
O3 O 0.600(3) 0.580(3) 0.579(3) 0.159(19) Uiso 0.25 1 d . . P . .
O4 O 0.938(3) 1.168(3) 0.199(3) 0.16(2) Uiso 0.25 1 d . . P . .
O5 O 0.394(3) 0.685(3) 0.325(3) 0.150(18) Uiso 0.25 1 d . . P G 2
O6 O 0.890(5) 1.006(5) 0.121(5) 0.27(4) Uiso 0.25 1 d . . P . .
C65 C 0.7717(15) 0.972(3) 0.242(3) 0.22(3) Uiso 0.35 1 d D U P E 1
H65A H 0.7885 0.9538 0.2798 0.328 Uiso 0.35 1 d R U P E 1
H65B H 0.7737 0.9394 0.2108 0.328 Uiso 0.35 1 d DR U P E 1
H65C H 0.7981 1.0098 0.2310 0.328 Uiso 0.35 1 d R U P E 1
C66 C 0.771(3) 1.002(5) 0.267(5) 0.11(3) Uiso 0.15 1 d D U P E 2
H66A H 0.7695 1.0104 0.2233 0.168 Uiso 0.15 1 d R U P E 2
H66B H 0.7468 1.0366 0.2874 0.168 Uiso 0.15 1 d R U P E 2
H66C H 0.8157 1.0017 0.2803 0.168 Uiso 0.15 1 d R U P E 2
C52A C 0.7256(15) 0.958(3) 0.294(3) 0.065(13) Uiso 0.15 1 d D U P E 2
H52C H 0.7430 0.9132 0.2880 0.078 Uiso 0.15 1 calc R U P E 2
H52D H 0.7252 0.9661 0.3372 0.078 Uiso 0.15 1 calc R U P E 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 N40 2.301(8) 4_655 ?
Cd1 N21 2.322(8) . ?
Cd1 N11 2.363(8) 6_664 ?
Cd1 O56 2.418(9) . ?
Cd1 O63 2.424(8) . ?
Cd1 O74 2.46(2) . ?
Cd1 O72 2.549(19) . ?
Cd1 O54 2.590(12) . ?
Cr1 O31 1.898(8) . ?
Cr1 O33 1.965(5) 2_675 ?
Cr1 O33 1.965(5) . ?
Cr1 O12 1.978(5) 2_675 ?
Cr1 O12 1.978(5) . ?
Cr1 O61 2.009(8) . ?
Cr2 O31 1.902(4) . ?
Cr2 O11 1.960(5) 2_675 ?
Cr2 O21 1.965(5) 2_675 ?
Cr2 O35 1.975(5) . ?
Cr2 O22 1.985(5) . ?
Cr2 O51 2.034(5) . ?
O31 Cr2 1.902(4) 2_675 ?
O63 C64 1.41(2) . ?
O35 C34 1.263(10) . ?
O33 C34 1.261(10) . ?
N40 C41 1.336(11) . ?
N40 C39 1.359(14) . ?
N40 Cd1 2.301(8) 4_645 ?
C41 C36 1.393(11) . ?
C41 H41 0.9500 . ?
C39 C38 1.347(16) . ?
C39 H39 0.9500 . ?
C38 C37 1.390(14) . ?
C38 H38 0.9500 . ?
C36 C37 1.409(13) . ?
C36 C34 1.477(11) . ?
C37 H37 0.9500 . ?
O11 C16 1.260(10) . ?
O11 Cr2 1.960(5) 2_675 ?
O12 C16 1.258(9) . ?
N11 C12 1.323(13) . ?
N11 C11 1.363(11) . ?
N11 Cd1 2.363(8) 6_665 ?
C11 C13 1.378(13) . ?
C11 H11 0.9500 . ?
C12 C14 1.392(16) . ?
C12 H12 0.9500 . ?
C13 C15 1.377(12) . ?
C13 C16 1.504(11) . ?
C14 C15 1.398(14) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
O21 C21 1.279(9) . ?
O21 Cr2 1.965(5) 2_675 ?
O22 C21 1.227(8) . ?
N21 C22 1.319(11) . ?
N21 C26 1.361(13) . ?
C21 C25 1.481(11) . ?
C22 C25 1.399(12) . ?
C22 H22 0.9500 . ?
C23 C25 1.367(12) . ?
C23 C24 1.414(14) . ?
C23 H23 0.9500 . ?
C24 C26 1.346(17) . ?
C24 H24 0.9500 . ?
C26 H26 0.9500 . ?
O51 C52B 1.427(15) . ?
O51 C52A 1.43(3) . ?
O56 N55 1.273(15) . ?
O54 N55 1.203(14) . ?
N55 O57 1.213(15) . ?
N61 O58 1.20(3) . ?
N61 O60 1.25(2) . ?
N61 O59 1.32(2) . ?
O61 C61 1.433(11) . ?
O61 C61 1.433(11) 2_675 ?
C61 C62 1.439(13) . ?
C61 H61A 0.9903 . ?
C61 H61B 0.9902 . ?
C62 H62A 0.9801 . ?
C62 H62B 0.9797 . ?
C62 H62C 0.9803 . ?
N71 O73 1.09(2) . ?
N71 O72 1.14(3) . ?
N71 O71 1.22(3) . ?
O48 C49 1.493(19) . ?
O42 C43 1.36(2) . ?
O45 C46 1.37(2) . ?
C43 C44 1.48(3) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C46 H46A 0.9796 . ?
C46 H46B 0.9797 . ?
C46 H46C 0.9799 . ?
C44 H44A 0.9796 . ?
C44 H44B 0.9802 . ?
C44 H44C 0.9801 . ?
C52B C65 1.46(3) . ?
C52B H52A 0.9900 . ?
C52B H52B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C64 H64A 0.9799 . ?
C64 H64B 0.9802 . ?
C64 H64C 0.9801 . ?
C65 H65A 0.9801 . ?
C65 H65B 0.9797 . ?
C65 H65C 0.9803 . ?
C66 C52A 1.44(3) . ?
C66 H66A 0.9801 . ?
C66 H66B 0.9799 . ?
C66 H66C 0.9798 . ?
C52A H52C 0.9900 . ?
C52A H52D 0.9900 . ?

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
N40 Cd1 N21 167.5(3) 4_655 . ?
N40 Cd1 N11 84.8(3) 4_655 6_664 ?
N21 Cd1 N11 88.5(3) . 6_664 ?
N40 Cd1 O56 83.7(3) 4_655 . ?
N21 Cd1 O56 98.5(3) . . ?
N11 Cd1 O56 155.9(3) 6_664 . ?
N40 Cd1 O63 84.6(3) 4_655 . ?
N21 Cd1 O63 84.1(3) . . ?
N11 Cd1 O63 83.1(3) 6_664 . ?
O56 Cd1 O63 74.8(4) . . ?
N40 Cd1 O74 90.8(5) 4_655 . ?
N21 Cd1 O74 98.9(4) . . ?
N11 Cd1 O74 83.2(8) 6_664 . ?
O56 Cd1 O74 118.1(8) . . ?
O63 Cd1 O74 165.8(8) . . ?
N40 Cd1 O72 111.8(5) 4_655 . ?
N21 Cd1 O72 78.1(5) . . ?
N11 Cd1 O72 85.0(4) 6_664 . ?
O56 Cd1 O72 118.9(4) . . ?
O63 Cd1 O72 158.8(5) . . ?
N40 Cd1 O54 107.2(3) 4_655 . ?
N21 Cd1 O54 83.0(3) . . ?
N11 Cd1 O54 155.4(3) 6_664 . ?
O56 Cd1 O54 48.7(3) . . ?
O63 Cd1 O54 118.7(4) . . ?
O74 Cd1 O54 75.4(8) . . ?
O72 Cd1 O54 70.6(5) . . ?
O31 Cr1 O33 94.23(16) . 2_675 ?
O31 Cr1 O33 94.23(16) . . ?
O33 Cr1 O33 171.5(3) 2_675 . ?
O31 Cr1 O12 94.89(16) . 2_675 ?
O33 Cr1 O12 86.6(2) 2_675 2_675 ?
O33 Cr1 O12 92.7(2) . 2_675 ?
O31 Cr1 O12 94.89(16) . . ?
O33 Cr1 O12 92.7(2) 2_675 . ?
O33 Cr1 O12 86.6(2) . . ?
O12 Cr1 O12 170.2(3) 2_675 . ?
O31 Cr1 O61 180.0 . . ?
O33 Cr1 O61 85.77(16) 2_675 . ?
O33 Cr1 O61 85.77(16) . . ?
O12 Cr1 O61 85.11(16) 2_675 . ?
O12 Cr1 O61 85.11(16) . . ?
O31 Cr2 O11 94.27(19) . 2_675 ?
O31 Cr2 O21 93.82(19) . 2_675 ?
O11 Cr2 O21 171.9(2) 2_675 2_675 ?
O31 Cr2 O35 94.5(2) . . ?
O11 Cr2 O35 92.7(2) 2_675 . ?
O21 Cr2 O35 86.7(2) 2_675 . ?
O31 Cr2 O22 94.2(2) . . ?
O11 Cr2 O22 86.6(2) 2_675 . ?
O21 Cr2 O22 92.8(2) 2_675 . ?
O35 Cr2 O22 171.3(2) . . ?
O31 Cr2 O51 178.63(18) . . ?
O11 Cr2 O51 87.0(2) 2_675 . ?
O21 Cr2 O51 84.9(2) 2_675 . ?
O35 Cr2 O51 84.9(2) . . ?
O22 Cr2 O51 86.4(2) . . ?
Cr1 O31 Cr2 119.8(2) . . ?
Cr1 O31 Cr2 119.8(2) . 2_675 ?
Cr2 O31 Cr2 120.3(4) . 2_675 ?
C64 O63 Cd1 123.1(15) . . ?
C34 O35 Cr2 133.7(5) . . ?
C34 O33 Cr1 128.0(5) . . ?
C41 N40 C39 117.5(8) . . ?
C41 N40 Cd1 118.9(6) . 4_645 ?
C39 N40 Cd1 123.3(6) . 4_645 ?
N40 C41 C36 122.4(8) . . ?
N40 C41 H41 118.8 . . ?
C36 C41 H41 118.8 . . ?
C38 C39 N40 123.4(9) . . ?
C38 C39 H39 118.3 . . ?
N40 C39 H39 118.3 . . ?
C39 C38 C37 120.5(9) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C41 C36 C37 119.3(8) . . ?
C41 C36 C34 119.0(8) . . ?
C37 C36 C34 121.6(8) . . ?
O33 C34 O35 126.1(7) . . ?
O33 C34 C36 116.6(7) . . ?
O35 C34 C36 117.3(7) . . ?
C38 C37 C36 116.8(9) . . ?
C38 C37 H37 121.6 . . ?
C36 C37 H37 121.6 . . ?
C16 O11 Cr2 128.2(5) . 2_675 ?
C16 O12 Cr1 132.9(5) . . ?
C12 N11 C11 116.4(9) . . ?
C12 N11 Cd1 122.1(7) . 6_665 ?
C11 N11 Cd1 121.5(6) . 6_665 ?
N11 C11 C13 123.6(8) . . ?
N11 C11 H11 118.2 . . ?
C13 C11 H11 118.2 . . ?
N11 C12 C14 123.8(9) . . ?
N11 C12 H12 118.1 . . ?
C14 C12 H12 118.1 . . ?
C15 C13 C11 119.4(8) . . ?
C15 C13 C16 120.6(8) . . ?
C11 C13 C16 120.0(7) . . ?
C12 C14 C15 119.0(9) . . ?
C12 C14 H14 120.5 . . ?
C15 C14 H14 120.5 . . ?
C13 C15 C14 117.7(9) . . ?
C13 C15 H15 121.2 . . ?
C14 C15 H15 121.2 . . ?
O12 C16 O11 126.6(7) . . ?
O12 C16 C13 117.6(7) . . ?
O11 C16 C13 115.8(7) . . ?
C21 O21 Cr2 128.3(5) . 2_675 ?
C21 O22 Cr2 134.3(5) . . ?
C22 N21 C26 119.4(9) . . ?
C22 N21 Cd1 120.3(6) . . ?
C26 N21 Cd1 120.3(6) . . ?
O22 C21 O21 126.1(7) . . ?
O22 C21 C25 118.5(7) . . ?
O21 C21 C25 115.4(7) . . ?
N21 C22 C25 121.3(8) . . ?
N21 C22 H22 119.4 . . ?
C25 C22 H22 119.4 . . ?
C25 C23 C24 118.7(9) . . ?
C25 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C26 C24 C23 118.6(10) . . ?
C26 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C23 C25 C22 119.4(8) . . ?
C23 C25 C21 122.0(8) . . ?
C22 C25 C21 118.5(7) . . ?
C24 C26 N21 122.6(9) . . ?
C24 C26 H26 118.7 . . ?
N21 C26 H26 118.7 . . ?
C52B O51 Cr2 125.5(9) . . ?
C52A O51 Cr2 129(3) . . ?
N55 O56 Cd1 101.9(8) . . ?
N55 O54 Cd1 95.3(9) . . ?
O54 N55 O57 120.8(13) . . ?
O54 N55 O56 113.6(12) . . ?
O57 N55 O56 125.7(12) . . ?
O58 N61 O60 123(2) . . ?
O58 N61 O59 117(2) . . ?
O60 N61 O59 119.8(19) . . ?
C61 O61 C61 108.9(16) . 2_675 ?
C61 O61 Cr1 125.6(8) . . ?
C61 O61 Cr1 125.6(8) 2_675 . ?
O61 C61 C62 113.2(15) . . ?
O61 C61 H61A 109.2 . . ?
C62 C61 H61A 109.3 . . ?
O61 C61 H61B 108.1 . . ?
C62 C61 H61B 107.5 . . ?
H61A C61 H61B 109.5 . . ?
C61 C62 H62A 110.2 . . ?
C61 C62 H62B 108.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.8 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O73 N71 O72 127(2) . . ?
O73 N71 O71 125(2) . . ?
O72 N71 O71 108(2) . . ?
N71 O72 Cd1 109.5(17) . . ?
O42 C43 C44 111(3) . . ?
O42 C43 H43A 109.5 . . ?
C44 C43 H43A 109.5 . . ?
O42 C43 H43B 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
O45 C46 H46A 110.4 . . ?
O45 C46 H46B 109.4 . . ?
H46A C46 H46B 109.5 . . ?
O45 C46 H46C 108.6 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C43 C44 H44A 113.2 . . ?
C43 C44 H44B 103.0 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 112.0 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.4 . . ?
O51 C52B C65 115(3) . . ?
O51 C52B H52A 108.6 . . ?
C65 C52B H52A 108.6 . . ?
O51 C52B H52B 108.6 . . ?
C65 C52B H52B 108.6 . . ?
H52A C52B H52B 107.6 . . ?
O48 C49 H49A 109.5 . . ?
O48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
O48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O63 C64 H64A 105.8 . . ?
O63 C64 H64B 115.9 . . ?
H64A C64 H64B 109.5 . . ?
O63 C64 H64C 106.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C52B C65 H65A 106.8 . . ?
C52B C65 H65B 119.1 . . ?
H65A C65 H65B 109.5 . . ?
C52B C65 H65C 102.0 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C52A C66 H66A 120.6 . . ?
C52A C66 H66B 86.6 . . ?
H66A C66 H66B 109.5 . . ?
C52A C66 H66C 118.1 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O51 C52A C66 118(4) . . ?
O51 C52A H52C 107.7 . . ?
C66 C52A H52C 107.7 . . ?
O51 C52A H52D 107.7 . . ?
C66 C52A H52D 107.7 . . ?
H52C C52A H52D 107.1 . . ?

_refine_diff_density_max         0.731
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.108



# start Validation Reply Form
_vrf_CHEMW03_PMBB-2-rtl-1        
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: The formula includes havily disordered nitrate anion
that could not be reliably modeled.
;
# 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_PMBB-2-pcu-1
_database_code_depnum_ccdc_archive 'CCDC 1482200'
_audit_update_record             
;
2016-08-30 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;
_audit_creation_date             2016-08-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'0.17(C612 H708 Cl84 Cr36 Cu36 N132 O216), 5(C3 H7 N O), 1(O)'
_chemical_formula_sum            'C117 H155 Cl14 Cr6 Cu6 N27 O42'
_chemical_formula_weight         3801.21
_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 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      trigonal
_space_group_IT_number           167
_space_group_name_H-M_alt        'R -3 c'
_space_group_name_Hall           '-R 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   21.6177(6)
_cell_length_b                   21.6177(6)
_cell_length_c                   61.464(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     24875(2)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    3748
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.509
_cell_measurement_theta_min      2.764
_shelx_estimated_absorpt_T_max   0.349
_shelx_estimated_absorpt_T_min   0.349
_exptl_absorpt_coefficient_mu    6.658
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             11628
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0689
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -65
_diffrn_reflns_number            29562
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        62.509
_diffrn_reflns_theta_max         62.509
_diffrn_reflns_theta_min         2.764
_diffrn_ambient_temperature      100.11
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture Photon CMOS'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3748
_reflns_number_total             4375
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    ?
_refine_diff_density_max         0.885
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         4375
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0634
_refine_ls_restrained_S_all      1.099
_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)+(0.0745P)²+341.5594P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1631
_refine_ls_wR_factor_ref         0.1695
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N33-C32
 1.32 with sigma of 0.02
 O31-C32
 1.23 with sigma of 0.02
 O49-C50
 1.23 with sigma of 0.02
 N51-C50
 1.32 with sigma of 0.02
 N51-C53 = N51-C52
 1.45 with sigma of 0.02
 N45-C46 = N45-C47
 1.45 with sigma of 0.02
 N45-C44
 1.32 with sigma of 0.02
 O43-C44
 1.23 with sigma of 0.02
 O31-C36
 1.23 with sigma of 0.02
 N37-C36
 1.32 with sigma of 0.02
 N33-C34 = N33-C35
 1.45 with sigma of 0.02
 O31-C39
 1.23 with sigma of 0.02
 N40-C39
 1.32 with sigma of 0.02
 N40-C41 = N40-C42
 1.45 with sigma of 0.02
 N37-C37 = N37-C38
 1.45 with sigma of 0.02
 N56-C55
 1.32 with sigma of 0.02
 O54-C55
 1.23 with sigma of 0.02
 N56-C57 = N56-C58
 1.45 with sigma of 0.02
 O31-N33
 2.26 with sigma of 0.04
 C32-C35
 2.41 with sigma of 0.04
 O49-N51
 2.26 with sigma of 0.04
 C50-C52
 2.41 with sigma of 0.04
 C50-C53
 2.41 with sigma of 0.04
 C53-C52
 2.47 with sigma of 0.04
 O43-N45
 2.26 with sigma of 0.04
 C44-C47
 2.41 with sigma of 0.04
 C46-C44
 2.41 with sigma of 0.04
 C46-C47
 2.47 with sigma of 0.04
 N37-O31
 2.26 with sigma of 0.04
 C38-C36
 2.41 with sigma of 0.04
 C34-C32
 2.41 with sigma of 0.04
 C34-C35
 2.47 with sigma of 0.04
 N40-O31
 2.26 with sigma of 0.04
 C39-C41
 2.41 with sigma of 0.04
 C39-C42
 2.41 with sigma of 0.04
 C42-C41
 2.47 with sigma of 0.04
 C36-C37
 2.41 with sigma of 0.04
 C38-C37
 2.47 with sigma of 0.04
 O54-N56
 2.26 with sigma of 0.04
 C55-C58
 2.41 with sigma of 0.04
 C57-C55
 2.41 with sigma of 0.04
 C57-C58
 2.47 with sigma of 0.04
3. Restrained planarity
 O49, C50, N51, C52, C53
 with sigma of 0.1
 O43, C44, N45, C46, C47
 with sigma of 0.1
 C32, N33, C34, C35
 with sigma of 0.1
 O31, C39, N40, C41, C42
 with sigma of 0.1
 C36, C37, N37, C38
 with sigma of 0.1
 O54, C55, N56, C57, C58
 with sigma of 0.1
4. Rigid bond restraints
 O31, C32, N33, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O25, C26, N27, C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O49 \\sim C50 \\sim N51 \\sim C52 \\sim C53: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O31 \\sim C39 \\sim N40 \\sim C41 \\sim C42: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O31 \\sim C36 \\sim C37 \\sim C38: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O54 \\sim C55 \\sim N56 \\sim C57 \\sim C58: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O25 \\sim Cl55: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uiso(C42) = Uiso(C35)
6. Rigid body (RIGU) restrains
 O31, C32, N33, C34, C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O25, C26, N27, C28, C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(Cl24)=1-FVAR(1)
 Sof(Cl23)=FVAR(1)
 Fixed Sof: O25(0.66667) C26(0.66667) H26(0.66667) N27(0.66667) C28(0.66667)
 H28A(0.66667) H28B(0.66667) H28C(0.66667) C29(0.66667) H29A(0.66667)
 H29B(0.66667) H29C(0.66667) Cl55(0.33333) C32(0.625) H32(0.625) N33(0.625)
 C34(0.625) H34A(0.625) H34B(0.625) H34C(0.625) C35(0.625) H35A(0.625)
 H35B(0.625) H35C(0.625) C36(0.25) H36(0.25) C37(0.25) H37A(0.25) H37B(0.25)
 H37C(0.25) N37(0.25) C38(0.25) H38A(0.25) H38B(0.25) H38C(0.25) C39(0.125)
 H39(0.125) N40(0.125) C41(0.125) H41A(0.125) H41B(0.125) H41C(0.125)
 C42(0.125) H42A(0.125) H42B(0.125) H42C(0.125) O49(0.33333) C50(0.33333)
 H50(0.33333) N51(0.33333) C52(0.33333) H52A(0.33333) H52B(0.33333)
 H52C(0.33333) C53(0.33333) H53A(0.33333) H53B(0.33333) H53C(0.33333)
 O54(0.16666) C55(0.16667) H55(0.16667) N56(0.16667) C57(0.16667) H57A(0.16667)
 H57B(0.16667) H57C(0.16667) C58(0.16667) H58A(0.16667) H58B(0.16667)
 H58C(0.16667) O43(0.33333) C44(0.33333) H44(0.33333) N45(0.33333) C46(0.33333)
 H46A(0.33333) H46B(0.33333) H46C(0.33333) C47(0.33333) H47A(0.33333)
 H47B(0.33333) H47C(0.33333) O48(0.16667)
8.a Riding coordinates:
 C37(H37A,H37B,H37C), C42(H42A,H42B,H42C)
8.b Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
8.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C11(H11), C12(H12), C17(H17), C19(H19), C20(H20), C21(H21),
 C26(H26), C32(H32), C36(H36), C39(H39), C50(H50), C55(H55), C44(H44)
8.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C38(H38A,H38B,
 H38C), C41(H41A,H41B,H41C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Cr1 Cr 1.41651(4) 0.65784(4) 0.28604(2) 0.0127(2) Uani 1 1 d . . . . .
Cu2 Cu 1.49286(5) 0.97595(4) 0.37503(2) 0.0328(3) Uani 1 1 d . . . . .
O3 O 1.3333 0.6667 0.28598(8) 0.0103(11) Uani 1 3 d S T P . .
O4 O 1.38625(18) 0.59514(18) 0.26028(5) 0.0199(7) Uani 1 1 d . . . . .
C5 C 1.3243(3) 0.5467(3) 0.25543(8) 0.0180(10) Uani 1 1 d . . . . .
O6 O 1.26789(18) 0.52960(17) 0.26615(5) 0.0195(7) Uani 1 1 d . . . . .
C7 C 1.3165(3) 0.5036(3) 0.23567(8) 0.0270(12) Uani 1 1 d . . . . .
C8 C 1.2524(3) 0.4411(3) 0.23176(8) 0.0266(12) Uani 1 1 d . . . . .
H8 H 1.2142 0.4268 0.2418 0.032 Uiso 1 1 calc R . . . .
N9 N 1.2426(3) 0.4004(3) 0.21413(7) 0.0339(12) Uani 1 1 d . . . . .
C10 C 1.2962(4) 0.4229(4) 0.19985(11) 0.053(2) Uani 1 1 d . . . . .
H10 H 1.2894 0.3948 0.1872 0.064 Uiso 1 1 calc R . . . .
C11 C 1.3608(4) 0.4849(5) 0.20246(13) 0.076(3) Uani 1 1 d . . . . .
H11 H 1.3970 0.4995 0.1917 0.091 Uiso 1 1 calc R . . . .
C12 C 1.3722(4) 0.5257(4) 0.22109(11) 0.056(2) Uani 1 1 d . . . . .
H12 H 1.4169 0.5675 0.2237 0.067 Uiso 1 1 calc R . . . .
O13 O 1.45471(18) 0.71705(18) 0.31233(5) 0.0205(8) Uani 1 1 d . . . . .
C14 C 1.4500(3) 0.7709(3) 0.31781(8) 0.0198(11) Uani 1 1 d . . . . .
O15 O 1.42412(18) 0.80091(17) 0.30651(5) 0.0192(8) Uani 1 1 d . . . . .
C16 C 1.4769(3) 0.8003(3) 0.33999(9) 0.0284(12) Uani 1 1 d . . . . .
C17 C 1.4742(3) 0.8592(3) 0.34735(8) 0.0295(13) Uani 1 1 d . . . . .
H17 H 1.4560 0.8811 0.3379 0.035 Uiso 1 1 calc R . . . .
N18 N 1.4961(3) 0.8868(3) 0.36727(8) 0.0376(13) Uani 1 1 d . . . . .
C19 C 1.5209(5) 0.8545(4) 0.38039(11) 0.060(2) Uani 1 1 d . . . . .
H19 H 1.5356 0.8727 0.3947 0.072 Uiso 1 1 calc R . . . .
C20 C 1.5259(6) 0.7963(5) 0.37407(12) 0.081(3) Uani 1 1 d . . . . .
H20 H 1.5449 0.7757 0.3837 0.097 Uiso 1 1 calc R . . . .
C21 C 1.5030(5) 0.7679(4) 0.35360(11) 0.057(2) Uani 1 1 d . . . . .
H21 H 1.5051 0.7271 0.3490 0.069 Uiso 1 1 calc R . . . .
Cl22 Cl 1.56333(12) 1.03060(10) 0.34515(3) 0.0587(5) Uani 1 1 d . . . . .
Cl23 Cl 1.516(2) 0.9624(10) 0.41184(9) 0.087(8) Uani 0.49(5) 1 d . . . A 1
Cl24 Cl 1.4678(17) 0.9467(5) 0.40992(19) 0.073(5) Uani 0.51(5) 1 d . . . A 2
O25 O 1.3797(10) 0.9282(10) 0.3607(3) 0.055(5) Uani 0.6667 1 d . U . A 1
C26 C 1.3271(6) 0.9200(6) 0.3711(2) 0.055(3) Uani 0.6667 1 d . U . A 1
H26 H 1.3270 0.9134 0.3864 0.066 Uiso 0.6667 1 calc R . . A 1
N27 N 1.2711(6) 0.9196(6) 0.3625(2) 0.077(3) Uani 0.6667 1 d . U . A 1
C28 C 1.2679(8) 0.9289(9) 0.3382(3) 0.093(5) Uani 0.6667 1 d . U . A 1
H28A H 1.2787 0.8957 0.3305 0.140 Uiso 0.6667 1 calc GR . . A 1
H28B H 1.3029 0.9781 0.3341 0.140 Uiso 0.6667 1 calc GR . . A 1
H28C H 1.2199 0.9190 0.3342 0.140 Uiso 0.6667 1 calc GR . . A 1
C29 C 1.2114(9) 0.9140(12) 0.3748(3) 0.108(6) Uani 0.6667 1 d . U . A 1
H29A H 1.2164 0.9045 0.3901 0.163 Uiso 0.6667 1 calc GR . . A 1
H29B H 1.1667 0.8748 0.3690 0.163 Uiso 0.6667 1 calc GR . . A 1
H29C H 1.2107 0.9588 0.3737 0.163 Uiso 0.6667 1 calc GR . . A 1
Cl55 Cl 1.3700(7) 0.9076(8) 0.3668(3) 0.075(5) Uani 0.3333 1 d . U . A 2
O31 O 1.5057(2) 0.6520(2) 0.28666(6) 0.0308(9) Uani 1 1 d D U . . .
C32 C 1.5173(7) 0.6049(7) 0.2870(2) 0.064(3) Uiso 0.625 1 d D U . B 1
H32 H 1.4774 0.5579 0.2861 0.077 Uiso 0.625 1 calc R . . B 1
N33 N 1.5816(6) 0.6112(6) 0.2886(2) 0.062(4) Uiso 0.625 1 d D U . B 1
C34 C 1.5875(13) 0.5483(11) 0.2935(4) 0.146(9) Uiso 0.625 1 d D U . B 1
H34A H 1.6380 0.5618 0.2941 0.219 Uiso 0.625 1 calc R . . B 1
H34B H 1.5652 0.5287 0.3076 0.219 Uiso 0.625 1 calc R . . B 1
H34C H 1.5633 0.5122 0.2822 0.219 Uiso 0.625 1 calc R . . B 1
C35 C 1.6440(9) 0.6781(8) 0.2838(3) 0.098(6) Uiso 0.625 1 d D U . B 1
H35A H 1.6775 0.6698 0.2753 0.147 Uiso 0.625 1 calc GR . . B 1
H35B H 1.6668 0.7023 0.2974 0.147 Uiso 0.625 1 calc GR . . B 1
H35C H 1.6304 0.7081 0.2754 0.147 Uiso 0.625 1 calc GR . . B 1
C36 C 1.5500(12) 0.6489(14) 0.2762(4) 0.048(6) Uiso 0.25 1 d D U . B 2
H36 H 1.5597 0.6729 0.2626 0.057 Uiso 0.25 1 calc R . . B 2
C37 C 1.641(2) 0.621(3) 0.2654(6) 0.13(2) Uiso 0.25 1 d D U . B 2
H37A H 1.6169 0.5966 0.2519 0.201 Uiso 0.25 1 d R . . B 2
H37B H 1.6766 0.6705 0.2623 0.201 Uiso 0.25 1 d R . . B 2
H37C H 1.6640 0.5965 0.2720 0.201 Uiso 0.25 1 d R . . B 2
N37 N 1.5880(10) 0.6181(10) 0.2802(4) 0.038(6) Uiso 0.25 1 d D . . B 2
C38 C 1.577(2) 0.584(2) 0.3021(5) 0.085(12) Uiso 0.25 1 d D U . B 2
H38A H 1.5912 0.6208 0.3134 0.128 Uiso 0.25 1 calc GR . . B 2
H38B H 1.6070 0.5618 0.3033 0.128 Uiso 0.25 1 calc GR . . B 2
H38C H 1.5270 0.5479 0.3039 0.128 Uiso 0.25 1 calc GR . . B 2
C39 C 1.5284(16) 0.6268(18) 0.2999(5) 0.034(10) Uiso 0.125 1 d D U . B 3
H39 H 1.5009 0.6061 0.3127 0.041 Uiso 0.125 1 calc R . . B 3
N40 N 1.5884(15) 0.6261(18) 0.2978(6) 0.030(9) Uiso 0.125 1 d D U . B 3
C41 C 1.613(3) 0.593(4) 0.3136(10) 0.10(3) Uiso 0.125 1 d D U . B 3
H41A H 1.5770 0.5710 0.3252 0.148 Uiso 0.125 1 calc GR . . B 3
H41B H 1.6582 0.6293 0.3199 0.148 Uiso 0.125 1 calc GR . . B 3
H41C H 1.6193 0.5562 0.3064 0.148 Uiso 0.125 1 calc GR . . B 3
C42 C 1.631(4) 0.653(5) 0.2780(10) 0.098(6) Uiso 0.125 1 d D U . B 3
H42A H 1.6021 0.6249 0.2655 0.147 Uiso 0.125 1 d R . . B 3
H42B H 1.6452 0.7033 0.2758 0.147 Uiso 0.125 1 d R . . B 3
H42C H 1.6732 0.6481 0.2793 0.147 Uiso 0.125 1 d R . . B 3
O49 O 1.325(3) 0.6496(15) 0.2167(2) 0.095(8) Uiso 0.3333 1 d D U . C -1
C50 C 1.3088(15) 0.6099(14) 0.2003(4) 0.116(12) Uiso 0.3333 1 d D U . C -1
H50 H 1.2604 0.5730 0.1989 0.139 Uiso 0.3333 1 calc R . . C -1
N51 N 1.3543(11) 0.6153(11) 0.1847(3) 0.073(6) Uiso 0.3333 1 d D U . C -1
C52 C 1.4306(13) 0.6679(16) 0.1853(6) 0.110(12) Uiso 0.3333 1 d D U . C -1
H52A H 1.4404 0.7081 0.1757 0.165 Uiso 0.3333 1 calc GR . . C -1
H52B H 1.4580 0.6457 0.1803 0.165 Uiso 0.3333 1 calc GR . . C -1
H52C H 1.4446 0.6853 0.2002 0.165 Uiso 0.3333 1 calc GR . . C -1
C53 C 1.332(2) 0.5672(18) 0.1658(5) 0.116(13) Uiso 0.3333 1 d D U . C -1
H53A H 1.2801 0.5356 0.1661 0.175 Uiso 0.3333 1 calc GR . . C -1
H53B H 1.3556 0.5385 0.1663 0.175 Uiso 0.3333 1 calc GR . . C -1
H53C H 1.3456 0.5955 0.1524 0.175 Uiso 0.3333 1 calc GR . . C -1
O54 O 1.330(6) 0.667(7) 0.3624(7) 0.175(17) Uiso 0.1667 1 d D U . D -1
C55 C 1.293(4) 0.621(4) 0.3760(10) 0.18(3) Uiso 0.1667 1 d D U . D -1
H55 H 1.2725 0.5723 0.3719 0.221 Uiso 0.1667 1 calc R . . D -1
N56 N 1.281(3) 0.635(3) 0.3958(8) 0.19(3) Uiso 0.1667 1 d D U . D -1
C57 C 1.238(4) 0.579(4) 0.4110(12) 0.13(3) Uiso 0.1667 1 d D U . D -1
H57A H 1.2344 0.5998 0.4248 0.202 Uiso 0.1667 1 calc R . . D -1
H57B H 1.1897 0.5491 0.4050 0.202 Uiso 0.1667 1 calc R . . D -1
H57C H 1.2597 0.5494 0.4135 0.202 Uiso 0.1667 1 calc R . . D -1
C58 C 1.312(4) 0.710(3) 0.4023(10) 0.12(3) Uiso 0.1667 1 d D U . D -1
H58A H 1.2983 0.7120 0.4173 0.183 Uiso 0.1667 1 calc R . . D -1
H58B H 1.3641 0.7330 0.4013 0.183 Uiso 0.1667 1 calc R . . D -1
H58C H 1.2947 0.7338 0.3927 0.183 Uiso 0.1667 1 calc R . . D -1
O43 O 1.4696(11) 0.4811(12) 0.2552(4) 0.105(8) Uiso 0.3333 1 d D . . E -3
C44 C 1.4244(11) 0.4651(12) 0.2687(4) 0.085(9) Uiso 0.3333 1 d D . . E -3
H44 H 1.4362 0.4981 0.2804 0.102 Uiso 0.3333 1 calc R . . E -3
N45 N 1.3621(11) 0.4095(11) 0.2697(3) 0.096(8) Uiso 0.3333 1 d D . . E -3
C46 C 1.3150(17) 0.4023(19) 0.2871(5) 0.110(13) Uiso 0.3333 1 d D . . E -3
H46A H 1.2686 0.3591 0.2849 0.165 Uiso 0.3333 1 calc GR . . E -3
H46B H 1.3086 0.4441 0.2874 0.165 Uiso 0.3333 1 calc GR . . E -3
H46C H 1.3355 0.3987 0.3010 0.165 Uiso 0.3333 1 calc GR . . E -3
C47 C 1.3421(12) 0.3558(11) 0.2530(4) 0.063(7) Uiso 0.3333 1 d D . . E -3
H47A H 1.3466 0.3776 0.2387 0.095 Uiso 0.3333 1 calc GR . . E -3
H47B H 1.2925 0.3180 0.2553 0.095 Uiso 0.3333 1 calc GR . . E -3
H47C H 1.3735 0.3354 0.2537 0.095 Uiso 0.3333 1 calc GR . . E -3
O48 O 1.405(3) 0.405(3) 0.2500 0.19(2) Uiso 0.3333 2 d S T P F 4


_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
Cr1 O3 1.9007(8) . ?
Cr1 O4 1.972(3) . ?
Cr1 O6 1.962(3) 2_755 ?
Cr1 O13 1.968(3) . ?
Cr1 O15 1.984(3) 3_775 ?
Cr1 O31 1.995(4) . ?
Cu2 N9 2.020(5) 35_755 ?
Cu2 N18 2.021(5) . ?
Cu2 Cl22 2.2996(18) . ?
Cu2 Cl23 2.367(11) . ?
Cu2 Cl24 2.225(7) . ?
Cu2 O25 2.30(2) . ?
Cu2 Cl55 2.359(16) . ?
O3 Cr1 1.9007(8) 2_755 ?
O3 Cr1 1.9007(8) 3_775 ?
O4 C5 1.255(6) . ?
C5 O6 1.268(6) . ?
C5 C7 1.488(7) . ?
O6 Cr1 1.962(3) 3_775 ?
C7 C8 1.390(8) . ?
C7 C12 1.380(8) . ?
C8 H8 0.9500 . ?
C8 N9 1.345(7) . ?
N9 Cu2 2.020(5) 29_645 ?
N9 C10 1.335(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.379(10) . ?
C11 H11 0.9500 . ?
C11 C12 1.391(9) . ?
C12 H12 0.9500 . ?
O13 C14 1.264(6) . ?
C14 O15 1.257(6) . ?
C14 C16 1.494(7) . ?
O15 Cr1 1.984(3) 2_755 ?
C16 C17 1.380(8) . ?
C16 C21 1.379(9) . ?
C17 H17 0.9500 . ?
C17 N18 1.341(7) . ?
N18 C19 1.340(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.372(10) . ?
C20 H20 0.9500 . ?
C20 C21 1.379(9) . ?
C21 H21 0.9500 . ?
O25 C26 1.24(2) . ?
C26 H26 0.9500 . ?
C26 N27 1.318(16) . ?
N27 C28 1.513(18) . ?
N27 C29 1.450(17) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
O31 C32 1.163(12) . ?
O31 C36 1.181(16) . ?
O31 C39 1.213(19) . ?
C32 H32 0.9500 . ?
C32 N33 1.331(13) . ?
N33 C34 1.460(15) . ?
N33 C35 1.431(14) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36 0.9500 . ?
C36 N37 1.314(17) . ?
C37 C37 2.04(9) 4_645 ?
C37 H37A 0.9794 . ?
C37 H37B 0.9797 . ?
C37 H37C 0.9803 . ?
C37 N37 1.433(18) . ?
N37 C38 1.494(18) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 0.9500 . ?
C39 N40 1.311(18) . ?
N40 C41 1.450(19) . ?
N40 C42 1.460(19) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9794 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9799 . ?
O49 C50 1.256(18) . ?
C50 H50 0.9500 . ?
C50 N51 1.337(17) . ?
N51 C52 1.463(18) . ?
N51 C53 1.469(17) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
O54 C55 1.23(2) . ?
C55 H55 0.9500 . ?
C55 N56 1.316(19) . ?
N56 C57 1.447(19) . ?
N56 C58 1.451(19) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
O43 C44 1.198(17) . ?
C44 H44 0.9500 . ?
C44 N45 1.281(17) . ?
N45 C46 1.433(17) . ?
N45 C47 1.443(17) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cr1 O4 93.55(16) . . ?
O3 Cr1 O6 94.70(14) . 2_755 ?
O3 Cr1 O13 92.69(16) . . ?
O3 Cr1 O15 94.72(14) . 3_775 ?
O3 Cr1 O31 177.94(15) . . ?
O4 Cr1 O15 92.78(14) . 3_775 ?
O4 Cr1 O31 88.30(15) . . ?
O6 Cr1 O4 87.39(14) 2_755 . ?
O6 Cr1 O13 93.73(14) 2_755 . ?
O6 Cr1 O15 170.55(14) 2_755 3_775 ?
O6 Cr1 O31 84.47(16) 2_755 . ?
O13 Cr1 O4 173.55(15) . . ?
O13 Cr1 O15 85.06(14) . 3_775 ?
O13 Cr1 O31 85.48(15) . . ?
O15 Cr1 O31 86.09(15) 3_775 . ?
N9 Cu2 N18 176.4(2) 35_755 . ?
N9 Cu2 Cl22 88.27(15) 35_755 . ?
N9 Cu2 Cl23 93.5(3) 35_755 . ?
N9 Cu2 Cl24 89.3(3) 35_755 . ?
N9 Cu2 O25 88.3(5) 35_755 . ?
N9 Cu2 Cl55 94.8(4) 35_755 . ?
N18 Cu2 Cl22 88.37(16) . . ?
N18 Cu2 Cl23 89.8(3) . . ?
N18 Cu2 Cl24 94.4(3) . . ?
N18 Cu2 O25 91.0(5) . . ?
N18 Cu2 Cl55 85.3(4) . . ?
Cl22 Cu2 Cl23 134.4(11) . . ?
Cl22 Cu2 O25 102.0(4) . . ?
Cl22 Cu2 Cl55 113.6(4) . . ?
Cl24 Cu2 Cl22 157.0(9) . . ?
Cl24 Cu2 Cl55 89.4(10) . . ?
O25 Cu2 Cl23 123.6(12) . . ?
Cr1 O3 Cr1 120.001(3) 2_755 . ?
Cr1 O3 Cr1 119.998(3) 3_775 . ?
Cr1 O3 Cr1 120.000(3) 2_755 3_775 ?
C5 O4 Cr1 127.8(3) . . ?
O4 C5 O6 126.1(4) . . ?
O4 C5 C7 117.1(4) . . ?
O6 C5 C7 116.8(4) . . ?
C5 O6 Cr1 132.5(3) . 3_775 ?
C8 C7 C5 119.7(5) . . ?
C12 C7 C5 120.4(5) . . ?
C12 C7 C8 119.9(5) . . ?
C7 C8 H8 119.0 . . ?
N9 C8 C7 121.9(5) . . ?
N9 C8 H8 119.0 . . ?
C8 N9 Cu2 122.2(4) . 29_645 ?
C10 N9 Cu2 119.9(4) . 29_645 ?
C10 N9 C8 117.8(5) . . ?
N9 C10 H10 118.3 . . ?
N9 C10 C11 123.4(6) . . ?
C11 C10 H10 118.3 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119.0(6) . . ?
C12 C11 H11 120.5 . . ?
C7 C12 C11 117.9(6) . . ?
C7 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C14 O13 Cr1 128.1(3) . . ?
O13 C14 C16 116.2(4) . . ?
O15 C14 O13 126.1(4) . . ?
O15 C14 C16 117.7(5) . . ?
C14 O15 Cr1 129.7(3) . 2_755 ?
C17 C16 C14 120.3(5) . . ?
C21 C16 C14 120.6(5) . . ?
C21 C16 C17 119.1(5) . . ?
C16 C17 H17 118.6 . . ?
N18 C17 C16 122.7(5) . . ?
N18 C17 H17 118.6 . . ?
C17 N18 Cu2 117.8(4) . . ?
C19 N18 Cu2 124.6(4) . . ?
C19 N18 C17 117.6(5) . . ?
N18 C19 H19 118.6 . . ?
N18 C19 C20 122.8(6) . . ?
C20 C19 H19 118.6 . . ?
C19 C20 H20 120.3 . . ?
C19 C20 C21 119.4(7) . . ?
C21 C20 H20 120.3 . . ?
C16 C21 H21 120.8 . . ?
C20 C21 C16 118.3(6) . . ?
C20 C21 H21 120.8 . . ?
C26 O25 Cu2 124.2(16) . . ?
O25 C26 H26 117.6 . . ?
O25 C26 N27 124.7(16) . . ?
N27 C26 H26 117.6 . . ?
C26 N27 C28 120.0(11) . . ?
C26 N27 C29 124.5(13) . . ?
C29 N27 C28 115.5(12) . . ?
N27 C28 H28A 109.5 . . ?
N27 C28 H28B 109.5 . . ?
N27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N27 C29 H29A 109.5 . . ?
N27 C29 H29B 109.5 . . ?
N27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C32 O31 Cr1 133.9(7) . . ?
C36 O31 Cr1 146.0(12) . . ?
C39 O31 Cr1 131.5(16) . . ?
O31 C32 H32 117.2 . . ?
O31 C32 N33 125.6(12) . . ?
N33 C32 H32 117.2 . . ?
C32 N33 C34 119.6(14) . . ?
C32 N33 C35 119.8(12) . . ?
C35 N33 C34 120.4(14) . . ?
N33 C34 H34A 109.5 . . ?
N33 C34 H34B 109.5 . . ?
N33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N33 C35 H35A 109.5 . . ?
N33 C35 H35B 109.5 . . ?
N33 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O31 C36 H36 114.4 . . ?
O31 C36 N37 131(2) . . ?
N37 C36 H36 114.4 . . ?
C37 C37 H37A 38.2 4_645 . ?
C37 C37 H37B 73.7 4_645 . ?
C37 C37 H37C 135.6 4_645 . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.4 . . ?
N37 C37 C37 111(3) . 4_645 ?
N37 C37 H37A 108.7 . . ?
N37 C37 H37B 110.4 . . ?
N37 C37 H37C 109.3 . . ?
C36 N37 C37 123(2) . . ?
C36 N37 C38 116(2) . . ?
C37 N37 C38 121(2) . . ?
N37 C38 H38A 109.5 . . ?
N37 C38 H38B 109.5 . . ?
N37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O31 C39 H39 117.8 . . ?
O31 C39 N40 124(3) . . ?
N40 C39 H39 117.8 . . ?
C39 N40 C41 123(3) . . ?
C39 N40 C42 120(3) . . ?
C41 N40 C42 116(3) . . ?
N40 C41 H41A 109.5 . . ?
N40 C41 H41B 109.5 . . ?
N40 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N40 C42 H42A 109.4 . . ?
N40 C42 H42B 110.2 . . ?
N40 C42 H42C 108.8 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O49 C50 H50 117.5 . . ?
O49 C50 N51 125(3) . . ?
N51 C50 H50 117.5 . . ?
C50 N51 C52 123(2) . . ?
C50 N51 C53 123(2) . . ?
C52 N51 C53 114(2) . . ?
N51 C52 H52A 109.5 . . ?
N51 C52 H52B 109.5 . . ?
N51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N51 C53 H53A 109.5 . . ?
N51 C53 H53B 109.5 . . ?
N51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
O54 C55 H55 117.8 . . ?
O54 C55 N56 124(4) . . ?
N56 C55 H55 117.8 . . ?
C55 N56 C57 121(3) . . ?
C55 N56 C58 119(3) . . ?
C57 N56 C58 120(3) . . ?
N56 C57 H57A 109.5 . . ?
N56 C57 H57B 109.5 . . ?
N56 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N56 C58 H58A 109.5 . . ?
N56 C58 H58B 109.5 . . ?
N56 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O43 C44 H44 115.7 . . ?
O43 C44 N45 129(2) . . ?
N45 C44 H44 115.7 . . ?
C44 N45 C46 119(2) . . ?
C44 N45 C47 118.4(18) . . ?
C46 N45 C47 122(2) . . ?
N45 C46 H46A 109.5 . . ?
N45 C46 H46B 109.5 . . ?
N45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N45 C47 H47A 109.5 . . ?
N45 C47 H47B 109.5 . . ?
N45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?

_shelx_SHELXL_version_number     2014/7

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_PMBB-2-stp-1
_database_code_depnum_ccdc_archive 'CCDC 1482201'
_audit_update_record             
;
2016-09-30 deposited with the CCDC.
2016-10-04 downloaded from the CCDC.
;
_audit_creation_date             2016-08-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.08.23 svn.r3337 for OlexSys, GUI svn.r5217)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C156 H96 Cl12 Cr12 Mn6 N24 O64), 6(O)'
_chemical_formula_sum            'C78 H84 Cl6 Cr6 Mn3 N14 O44'
_chemical_formula_weight         2611.11
_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 0.0000 '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'
Cl Cl 0.0550 0.0530 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.1620 0.2220 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.1800 0.2620 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0000 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0020 0.0020 '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      hexagonal
_space_group_IT_number           193
_space_group_name_H-M_alt        'P 63/m c m'
_space_group_name_Hall           '-P 6c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z'
'x, x-y, -z'
'-x+y, y, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'y, x, z'
'-x, -x+y, z'
'x-y, -y, z'

_cell_length_a                   22.045(2)
_cell_length_b                   22.045(2)
_cell_length_c                   21.768(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9161.6(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1978
_cell_measurement_theta_min      1.2
_cell_measurement_theta_max      14.1
_shelx_estimated_absorpt_T_max   0.997
_shelx_estimated_absorpt_T_min   0.993
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9935
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    0.947
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2646
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0835
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31739
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        14.096
_diffrn_reflns_theta_max         14.096
_diffrn_reflns_theta_min         1.204
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_wavelength     0.41328
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         synchrotron
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'phi scans'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1835
_reflns_number_total             2824
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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    ?
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0601
_refine_ls_restrained_S_all      1.080
_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)+(0.1311P)²+12.3736P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2415
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O21-C22 = O21-C21
 1.4 with sigma of 0.02
3. Others
 Fixed Sof: C21(0.25) C22(0.25) O22(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_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
Mn1 Mn 0.5000 0.0000 0.0000 0.0641(5) Uani 1 4 d S T P . .
Cl1 Cl 0.55939(12) 0.0000 0.09714(8) 0.0809(7) Uani 1 2 d S T P . .
Cr1 Cr 0.66517(6) 0.24606(6) 0.2500 0.0510(4) Uani 1 2 d S T P A .
O1 O 0.6667 0.3333 0.2500 0.0476(17) Uani 1 6 d S T P . .
O10 O 0.59406(18) 0.20389(17) 0.18512(14) 0.0581(9) Uani 1 1 d . . . . .
O11 O 0.53641(19) 0.2637(2) 0.1858(2) 0.0772(12) Uani 1 1 d . . . . .
C10 C 0.5486(3) 0.2171(3) 0.1662(2) 0.0576(12) Uani 1 1 d . . . . .
C11 C 0.5036(3) 0.1736(3) 0.1139(2) 0.0638(13) Uani 1 1 d . . . . .
C12 C 0.5172(3) 0.1260(3) 0.0857(2) 0.0597(13) Uani 1 1 d . . . . .
H12 H 0.5557 0.1219 0.0999 0.072 Uiso 1 1 calc R . . . .
N10 N 0.4783(3) 0.0846(2) 0.03870(19) 0.0681(12) Uani 1 1 d . . . . .
C13 C 0.4229(4) 0.0907(4) 0.0212(3) 0.093(2) Uani 1 1 d . . . . .
H13 H 0.3939 0.0611 -0.0108 0.112 Uiso 1 1 calc R . . . .
C14 C 0.4058(4) 0.1371(4) 0.0467(4) 0.112(3) Uani 1 1 d . . . . .
H14 H 0.3667 0.1399 0.0319 0.134 Uiso 1 1 calc R . . . .
C15 C 0.4465(4) 0.1799(3) 0.0945(3) 0.090(2) Uani 1 1 d . . . . .
H15 H 0.4358 0.2123 0.1134 0.108 Uiso 1 1 calc R . . . .
O21 O 0.6669(3) 0.1550(3) 0.2500 0.0730(15) Uani 1 2 d DS T P . .
C21 C 0.6084(11) 0.0866(10) 0.2500 0.124(8) Uiso 0.5 2 d DS T P A 1
C22 C 0.6560(12) 0.1060(11) 0.2932(10) 0.075(6) Uiso 0.25 1 d D . . A 2
O22 O 0.7045(7) 0.1084(7) 0.3506(6) 0.137(4) Uiso 0.5 1 d . . . B 1


_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
Mn1 Cl1 2.4871(17) . ?
Mn1 Cl1 2.4870(17) 13_655 ?
Mn1 N10 2.305(5) 13_655 ?
Mn1 N10 2.305(5) 12_655 ?
Mn1 N10 2.305(5) . ?
Mn1 N10 2.305(5) 24 ?
Cr1 O1 1.9076(11) . ?
Cr1 O10 1.964(3) 14_556 ?
Cr1 O10 1.964(3) . ?
Cr1 O11 1.958(4) 3_655 ?
Cr1 O11 1.958(4) 18_656 ?
Cr1 O21 2.027(5) . ?
O1 Cr1 1.9076(11) 3_655 ?
O1 Cr1 1.9077(11) 4_665 ?
O10 C10 1.245(6) . ?
O11 Cr1 1.958(4) 4_665 ?
O11 C10 1.258(6) . ?
C10 C11 1.500(7) . ?
C11 C12 1.372(7) . ?
C11 C15 1.398(8) . ?
C12 H12 0.9500 . ?
C12 N10 1.354(6) . ?
N10 C13 1.350(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.371(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.391(9) . ?
C15 H15 0.9500 . ?
O21 C21 1.412(16) . ?
O21 C22 1.359(16) . ?
O21 C22 1.359(16) 14_556 ?
C22 C22 1.88(4) 14_556 ?

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
Cl1 Mn1 Cl1 180.0 13_655 . ?
N10 Mn1 Cl1 89.34(11) 12_655 . ?
N10 Mn1 Cl1 89.34(11) 24 13_655 ?
N10 Mn1 Cl1 90.66(11) 12_655 13_655 ?
N10 Mn1 Cl1 89.34(11) 13_655 . ?
N10 Mn1 Cl1 90.66(11) . . ?
N10 Mn1 Cl1 89.34(11) . 13_655 ?
N10 Mn1 Cl1 90.66(11) 24 . ?
N10 Mn1 Cl1 90.66(11) 13_655 13_655 ?
N10 Mn1 N10 89.0(2) 12_655 13_655 ?
N10 Mn1 N10 91.0(2) 24 13_655 ?
N10 Mn1 N10 180.0 13_655 . ?
N10 Mn1 N10 89.0(2) 24 . ?
N10 Mn1 N10 91.0(2) 12_655 . ?
N10 Mn1 N10 180.0(4) 24 12_655 ?
O1 Cr1 O10 94.85(10) . . ?
O1 Cr1 O10 94.85(10) . 14_556 ?
O1 Cr1 O11 95.15(12) . 3_655 ?
O1 Cr1 O11 95.15(12) . 18_656 ?
O1 Cr1 O21 178.19(17) . . ?
O10 Cr1 O10 91.9(2) 14_556 . ?
O10 Cr1 O21 86.40(15) 14_556 . ?
O10 Cr1 O21 86.40(15) . . ?
O11 Cr1 O10 169.99(16) 18_656 . ?
O11 Cr1 O10 169.99(16) 3_655 14_556 ?
O11 Cr1 O10 87.67(17) 18_656 14_556 ?
O11 Cr1 O10 87.67(17) 3_655 . ?
O11 Cr1 O11 91.0(3) 18_656 3_655 ?
O11 Cr1 O21 83.59(16) 3_655 . ?
O11 Cr1 O21 83.59(16) 18_656 . ?
Cr1 O1 Cr1 120.0 . 4_665 ?
Cr1 O1 Cr1 120.0 3_655 4_665 ?
Cr1 O1 Cr1 120.0 . 3_655 ?
C10 O10 Cr1 132.2(3) . . ?
C10 O11 Cr1 132.0(3) . 4_665 ?
O10 C10 O11 127.1(4) . . ?
O10 C10 C11 117.0(5) . . ?
O11 C10 C11 115.8(5) . . ?
C12 C11 C10 120.0(5) . . ?
C12 C11 C15 119.5(5) . . ?
C15 C11 C10 120.5(5) . . ?
C11 C12 H12 118.4 . . ?
N10 C12 C11 123.2(5) . . ?
N10 C12 H12 118.4 . . ?
C12 N10 Mn1 120.3(4) . . ?
C13 N10 Mn1 122.8(4) . . ?
C13 N10 C12 116.5(5) . . ?
N10 C13 H13 118.0 . . ?
N10 C13 C14 124.0(6) . . ?
C14 C13 H13 118.0 . . ?
C13 C14 H14 120.5 . . ?
C13 C14 C15 119.0(6) . . ?
C15 C14 H14 120.5 . . ?
C11 C15 H15 121.1 . . ?
C14 C15 C11 117.8(6) . . ?
C14 C15 H15 121.1 . . ?
C21 O21 Cr1 126.8(12) . . ?
C22 O21 Cr1 134.7(11) 14_556 . ?
C22 O21 Cr1 134.7(11) . . ?
C22 O21 C22 87(2) . 14_556 ?
O21 C22 C22 46.3(11) . 14_556 ?

_shelx_SHELXL_version_number     2014/7

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_CHEMW03_PMBB-2-stp-1        
;
PROBLEM: WARNING: The ratio of given/expected molecular weight as
RESPONSE: The formula includes NO3 counterions. Those could not be 
reliably modeled due to disorder and are assumed 
to balance the charge of framework. 
;

# end Validation Reply Form
