# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
# 
#######################################################################

data_code-sr
_database_code_depnum_ccdc_archive 'CCDC 1408297'
_audit_update_record             
;
2015-06-23 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2014-07-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.20 svn.r2946 for OlexSys, GUI svn.r4855)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C20 H24 Co2 N2 O7'
_chemical_formula_sum            'C20 H24 Co2 N2 O7'
_chemical_formula_weight         522.27
_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 0.0033 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'
Co Co 0.3494 0.9721 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   10.503(2)
_cell_length_b                   17.689(4)
_cell_length_c                   14.495(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.17(3)
_cell_angle_gamma                90.00
_cell_volume                     2632.4(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5490
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.1115
_cell_measurement_theta_min      1.8415
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3311
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.1167
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16484
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.84
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 49.9617
	          2theta: -29.9248
scan:
	Number of images: 140
	           Slice: -120.0000 - 20.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 49.9617
	          2theta: -29.9248
scan:
	Number of images: 70
	           Slice: -120.0000 - -50.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 49.9617
	          2theta: -29.9248
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             6058
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0337
_diffrn_orient_matrix_UB_12      -0.0436
_diffrn_orient_matrix_UB_13      0.0803
_diffrn_orient_matrix_UB_21      -0.0486
_diffrn_orient_matrix_UB_22      -0.0284
_diffrn_orient_matrix_UB_23      0.0050
_diffrn_orient_matrix_UB_31      0.0310
_diffrn_orient_matrix_UB_32      -0.0577
_diffrn_orient_matrix_UB_33      -0.0263
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                3287
_reflns_number_total             4646
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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         1.262
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4646
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0664
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0859P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1768
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 O3, Co2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Rotating group:
 O7(H7a,H7b)
3.b Ternary CH refined with riding coordinates:
 C37(H37)
3.c Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C34(H34a,H34b)
3.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C12(H12), C13(H13), C29(H29), C24(H24), C23(H23), C31(H31), C30(H30)
3.e Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C26(H26a,H26b,H26c), C38(H38a,H38b,H38c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Co1 Co 0.51663(7) 0.65056(4) 0.48483(5) 0.0402(2) Uani 1 d . . . .
Co2 Co 0.50034(8) 0.49279(4) 0.39247(5) 0.0436(3) Uani 1 d . . . U
O3 O 0.6036(4) 0.5413(2) 0.5129(3) 0.0485(9) Uani 1 d . . . U
O4 O 0.4051(3) 0.5876(2) 0.3829(2) 0.0400(8) Uani 1 d . . . .
O1 O 0.6476(4) 0.6770(2) 0.4111(2) 0.0456(9) Uani 1 d . . . .
O2 O 0.5644(4) 0.3876(2) 0.4038(2) 0.0455(9) Uani 1 d . . . .
O6 O 0.3481(4) 0.7287(2) 0.3953(2) 0.0431(9) Uani 1 d . . . .
N1 N 0.3825(4) 0.4567(3) 0.2778(3) 0.0408(11) Uani 1 d . . . .
C8 C 0.3312(5) 0.6184(3) 0.3059(3) 0.0370(12) Uani 1 d . . . .
O9 O 0.8139(4) 0.6807(3) 0.3030(3) 0.0600(12) Uani 1 d . . . .
O7 O 0.6290(6) 0.5385(3) 0.3219(3) 0.0792(15) Uani 1 d . . . .
H7A H 0.6074 0.5279 0.2614 0.119 Uiso 1 d . . GR .
H7B H 0.7081 0.5209 0.3433 0.119 Uiso 1 d . . GR .
C33 C 0.6511(6) 0.7894(3) 0.5637(4) 0.0474(14) Uani 1 d . . . .
H33 H 0.6580 0.8303 0.6049 0.057 Uiso 1 calc . . R .
C12 C 0.3081(5) 0.4964(3) 0.2148(4) 0.0407(13) Uani 1 d . . . .
H12 H 0.2648 0.4721 0.1603 0.049 Uiso 1 calc . . R .
C13 C 0.2040(5) 0.6155(3) 0.1467(3) 0.0441(13) Uani 1 d . . . .
H13 H 0.1699 0.5888 0.0917 0.053 Uiso 1 calc . . R .
C14 C 0.3854(6) 0.3748(3) 0.2669(4) 0.0479(14) Uani 1 d . . . .
H14A H 0.3732 0.3621 0.2005 0.057 Uiso 1 calc . . R .
H14B H 0.3150 0.3521 0.2911 0.057 Uiso 1 calc . . R .
C28 C 0.8211(6) 0.7393(4) 0.3655(4) 0.0504(15) Uani 1 d . . . .
C29 C 0.9051(6) 0.7999(4) 0.3745(5) 0.0628(19) Uani 1 d . . . .
H29 H 0.9639 0.8026 0.3348 0.075 Uiso 1 calc . . R .
N2 N 0.5737(4) 0.7369(3) 0.5748(3) 0.0421(11) Uani 1 d . . . .
C24 C 0.1733(5) 0.6896(3) 0.1515(4) 0.0464(14) Uani 1 d . . . .
H24 H 0.1218 0.7134 0.0996 0.056 Uiso 1 calc . . R .
C22 C 0.2971(5) 0.6943(3) 0.3105(3) 0.0411(13) Uani 1 d . . . .
C27 C 0.7272(5) 0.7341(3) 0.4244(4) 0.0407(13) Uani 1 d . . . .
C25 C 0.2868(5) 0.5771(3) 0.2230(3) 0.0443(14) Uani 1 d . . . .
C23 C 0.2196(5) 0.7306(3) 0.2353(4) 0.0446(13) Uani 1 d . . . .
H23 H 0.1980 0.7813 0.2395 0.054 Uiso 1 calc . . R .
C37 C 0.5134(6) 0.3440(3) 0.3195(4) 0.0461(14) Uani 1 d . . . .
H37 H 0.5761 0.3457 0.2781 0.055 Uiso 1 calc . . R .
C21 C 0.3151(6) 0.8042(3) 0.4095(4) 0.0485(14) Uani 1 d . . . .
H21A H 0.3497 0.8183 0.4739 0.073 Uiso 1 calc . . GR .
H21B H 0.2220 0.8094 0.3961 0.073 Uiso 1 calc . . GR .
H21C H 0.3509 0.8366 0.3683 0.073 Uiso 1 calc . . GR .
C31 C 0.8183(6) 0.8531(4) 0.4975(4) 0.0593(18) Uani 1 d . . . .
H31 H 0.8164 0.8917 0.5408 0.071 Uiso 1 calc . . R .
C32 C 0.7309(6) 0.7919(3) 0.4920(4) 0.0476(14) Uani 1 d . . . .
C30 C 0.9061(6) 0.8564(4) 0.4395(5) 0.0648(19) Uani 1 d . . . .
H30 H 0.9650 0.8962 0.4443 0.078 Uiso 1 calc . . R .
C34 C 0.5007(6) 0.7374(3) 0.6504(4) 0.0530(16) Uani 1 d . . . .
H34A H 0.4154 0.7598 0.6281 0.064 Uiso 1 calc . . R .
H34B H 0.5468 0.7669 0.7035 0.064 Uiso 1 calc . . R .
C26 C 0.9137(6) 0.6767(5) 0.2495(5) 0.079(2) Uani 1 d . . . .
H26A H 0.9036 0.7178 0.2053 0.119 Uiso 1 calc . . GR .
H26B H 0.9068 0.6296 0.2159 0.119 Uiso 1 calc . . GR .
H26C H 0.9975 0.6800 0.2913 0.119 Uiso 1 calc . . GR .
C38 C 0.7460(9) 0.5395(6) 0.5422(8) 0.114(3) Uani 1 d . . . .
H38A H 0.7839 0.5512 0.4892 0.171 Uiso 1 calc . . GR .
H38B H 0.7734 0.4901 0.5655 0.171 Uiso 1 calc . . GR .
H38C H 0.7739 0.5762 0.5911 0.171 Uiso 1 calc . . GR .


_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
Co1 O3 2.139(4) . ?
Co1 O4 2.016(4) . ?
Co1 O1 1.968(3) . ?
Co1 O2 2.089(3) 3_666 ?
Co1 O6 2.399(4) . ?
Co1 N2 2.016(4) . ?
Co2 O3 2.040(4) . ?
Co2 O3 2.017(4) 3_666 ?
Co2 O4 1.942(4) . ?
Co2 O2 1.974(4) . ?
Co2 N1 1.959(4) . ?
Co2 O7 2.027(4) . ?
O3 Co2 2.017(4) 3_666 ?
O3 C38 1.467(10) . ?
O4 C8 1.335(6) . ?
O1 C27 1.300(6) . ?
O2 Co1 2.089(3) 3_666 ?
O2 C37 1.449(6) . ?
O6 C22 1.375(6) . ?
O6 C21 1.407(6) . ?
N1 C12 1.279(7) . ?
N1 C14 1.458(7) . ?
C8 C22 1.394(8) . ?
C8 C25 1.400(7) . ?
O9 C28 1.367(7) . ?
O9 C26 1.431(7) . ?
O7 H7A 0.8790 . ?
O7 H7B 0.8792 . ?
C33 H33 0.9300 . ?
C33 N2 1.267(7) . ?
C33 C32 1.467(8) . ?
C12 H12 0.9300 . ?
C12 C25 1.453(8) . ?
C13 H13 0.9300 . ?
C13 C24 1.354(8) . ?
C13 C25 1.428(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C37 1.501(8) . ?
C28 C29 1.377(9) . ?
C28 C27 1.437(7) . ?
C29 H29 0.9300 . ?
C29 C30 1.373(10) . ?
N2 C34 1.465(6) . ?
C24 H24 0.9300 . ?
C24 C23 1.409(8) . ?
C22 C23 1.375(8) . ?
C27 C32 1.411(8) . ?
C23 H23 0.9300 . ?
C37 H37 0.9800 . ?
C37 C34 1.522(8) 3_666 ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C31 H31 0.9300 . ?
C31 C32 1.411(8) . ?
C31 C30 1.373(9) . ?
C30 H30 0.9300 . ?
C34 C37 1.522(8) 3_666 ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O6 149.26(14) . . ?
O4 Co1 O3 78.38(14) . . ?
O4 Co1 O2 96.82(14) . 3_666 ?
O4 Co1 O6 70.95(14) . . ?
O1 Co1 O3 89.91(15) . . ?
O1 Co1 O4 95.63(14) . . ?
O1 Co1 O2 160.34(16) . 3_666 ?
O1 Co1 O6 95.14(15) . . ?
O1 Co1 N2 91.43(16) . . ?
O2 Co1 O3 77.80(14) 3_666 . ?
O2 Co1 O6 103.27(14) 3_666 . ?
N2 Co1 O3 120.30(17) . . ?
N2 Co1 O4 160.10(17) . . ?
N2 Co1 O2 81.89(16) . 3_666 ?
N2 Co1 O6 89.92(16) . . ?
O3 Co2 O3 79.06(16) 3_666 . ?
O3 Co2 O7 167.5(2) 3_666 . ?
O4 Co2 O3 87.83(15) . 3_666 ?
O4 Co2 O3 82.55(16) . . ?
O4 Co2 O2 168.87(15) . . ?
O4 Co2 N1 89.84(17) . . ?
O4 Co2 O7 90.46(18) . . ?
O2 Co2 O3 102.42(16) . . ?
O2 Co2 O3 83.41(15) . 3_666 ?
O2 Co2 O7 99.57(17) . . ?
N1 Co2 O3 172.02(17) . . ?
N1 Co2 O3 98.30(17) . 3_666 ?
N1 Co2 O2 84.65(17) . . ?
N1 Co2 O7 94.1(2) . . ?
O7 Co2 O3 88.4(2) . . ?
Co2 O3 Co1 97.40(15) 3_666 . ?
Co2 O3 Co1 95.11(17) . . ?
Co2 O3 Co2 100.94(16) 3_666 . ?
C38 O3 Co1 116.3(4) . . ?
C38 O3 Co2 117.5(5) . 3_666 ?
C38 O3 Co2 124.4(5) . . ?
Co2 O4 Co1 102.36(16) . . ?
C8 O4 Co1 122.1(3) . . ?
C8 O4 Co2 127.8(3) . . ?
C27 O1 Co1 127.3(3) . . ?
Co2 O2 Co1 100.46(14) . 3_666 ?
C37 O2 Co1 110.0(3) . 3_666 ?
C37 O2 Co2 111.8(3) . . ?
C22 O6 Co1 109.5(3) . . ?
C22 O6 C21 119.3(4) . . ?
C21 O6 Co1 130.1(3) . . ?
C12 N1 Co2 127.4(4) . . ?
C12 N1 C14 119.5(5) . . ?
C14 N1 Co2 113.1(3) . . ?
O4 C8 C22 117.6(4) . . ?
O4 C8 C25 122.3(5) . . ?
C22 C8 C25 120.1(5) . . ?
C28 O9 C26 116.9(5) . . ?
Co2 O7 H7A 111.0 . . ?
Co2 O7 H7B 111.2 . . ?
H7A O7 H7B 107.5 . . ?
N2 C33 H33 117.0 . . ?
N2 C33 C32 126.1(5) . . ?
C32 C33 H33 117.0 . . ?
N1 C12 H12 117.9 . . ?
N1 C12 C25 124.3(5) . . ?
C25 C12 H12 117.9 . . ?
C24 C13 H13 118.9 . . ?
C24 C13 C25 122.2(5) . . ?
C25 C13 H13 118.9 . . ?
N1 C14 H14A 109.7 . . ?
N1 C14 H14B 109.7 . . ?
N1 C14 C37 110.0(4) . . ?
H14A C14 H14B 108.2 . . ?
C37 C14 H14A 109.7 . . ?
C37 C14 H14B 109.7 . . ?
O9 C28 C29 126.7(5) . . ?
O9 C28 C27 113.3(5) . . ?
C29 C28 C27 120.0(6) . . ?
C28 C29 H29 118.5 . . ?
C30 C29 C28 123.0(6) . . ?
C30 C29 H29 118.5 . . ?
C33 N2 Co1 125.8(4) . . ?
C33 N2 C34 122.8(5) . . ?
C34 N2 Co1 111.0(4) . . ?
C13 C24 H24 120.0 . . ?
C13 C24 C23 120.0(5) . . ?
C23 C24 H24 120.0 . . ?
O6 C22 C8 114.4(4) . . ?
O6 C22 C23 123.8(5) . . ?
C23 C22 C8 121.8(5) . . ?
O1 C27 C28 117.5(5) . . ?
O1 C27 C32 126.1(5) . . ?
C32 C27 C28 116.4(5) . . ?
C8 C25 C12 123.6(5) . . ?
C8 C25 C13 117.0(5) . . ?
C13 C25 C12 119.0(5) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 C24 118.8(6) . . ?
C22 C23 H23 120.6 . . ?
O2 C37 C14 111.6(4) . . ?
O2 C37 H37 108.9 . . ?
O2 C37 C34 107.6(4) . 3_666 ?
C14 C37 H37 108.9 . . ?
C14 C37 C34 111.0(5) . 3_666 ?
C34 C37 H37 108.9 3_666 . ?
O6 C21 H21A 109.5 . . ?
O6 C21 H21B 109.5 . . ?
O6 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C32 C31 H31 119.6 . . ?
C30 C31 H31 119.6 . . ?
C30 C31 C32 120.8(7) . . ?
C27 C32 C33 122.3(5) . . ?
C31 C32 C33 116.4(6) . . ?
C31 C32 C27 121.1(5) . . ?
C29 C30 C31 118.7(6) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
N2 C34 C37 107.8(4) . 3_666 ?
N2 C34 H34A 110.1 . . ?
N2 C34 H34B 110.1 . . ?
C37 C34 H34A 110.1 3_666 . ?
C37 C34 H34B 110.1 3_666 . ?
H34A C34 H34B 108.5 . . ?
O9 C26 H26A 109.5 . . ?
O9 C26 H26B 109.5 . . ?
O9 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O3 C38 H38A 109.5 . . ?
O3 C38 H38B 109.5 . . ?
O3 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O4 C8 C22 -21.4(6) . . . . ?
Co1 O4 C8 C25 159.4(4) . . . . ?
Co1 O1 C27 C28 175.8(4) . . . . ?
Co1 O1 C27 C32 -3.9(8) . . . . ?
Co1 O2 C37 C14 84.5(5) 3_666 . . . ?
Co1 O2 C37 C34 -37.5(5) 3_666 . . 3_666 ?
Co1 O6 C22 C8 14.0(5) . . . . ?
Co1 O6 C22 C23 -165.6(4) . . . . ?
Co1 N2 C34 C37 40.6(5) . . . 3_666 ?
Co2 O4 C8 C22 -165.2(3) . . . . ?
Co2 O4 C8 C25 15.6(7) . . . . ?
Co2 O2 C37 C14 -26.2(5) . . . . ?
Co2 O2 C37 C34 -148.2(3) . . . 3_666 ?
Co2 N1 C12 C25 -7.3(8) . . . . ?
Co2 N1 C14 C37 -24.8(5) . . . . ?
O3 Co1 O4 Co2 -9.77(14) . . . . ?
O3 Co1 O4 C8 -161.2(4) . . . . ?
O3 Co1 O1 C27 -123.5(4) . . . . ?
O3 Co1 O6 C22 -22.4(4) . . . . ?
O3 Co1 O6 C21 170.1(4) . . . . ?
O3 Co1 N2 C33 100.9(5) . . . . ?
O3 Co1 N2 C34 -86.7(4) . . . . ?
O3 Co2 O3 Co1 -98.57(18) 3_666 . . . ?
O3 Co2 O3 Co2 0.0 3_666 . . 3_666 ?
O3 Co2 O3 C38 134.5(6) 3_666 . . . ?
O3 Co2 O4 Co1 10.12(14) . . . . ?
O3 Co2 O4 Co1 89.37(16) 3_666 . . . ?
O3 Co2 O4 C8 159.3(4) . . . . ?
O3 Co2 O4 C8 -121.4(4) 3_666 . . . ?
O3 Co2 O2 Co1 69.63(17) . . . 3_666 ?
O3 Co2 O2 Co1 -7.60(15) 3_666 . . 3_666 ?
O3 Co2 O2 C37 109.0(3) 3_666 . . . ?
O3 Co2 O2 C37 -173.7(3) . . . . ?
O3 Co2 N1 C12 106.6(5) 3_666 . . . ?
O3 Co2 N1 C12 36.6(14) . . . . ?
O3 Co2 N1 C14 -73.8(4) 3_666 . . . ?
O3 Co2 N1 C14 -143.9(11) . . . . ?
O4 Co1 O3 Co2 -92.64(16) . . . 3_666 ?
O4 Co1 O3 Co2 9.12(13) . . . . ?
O4 Co1 O3 C38 141.7(5) . . . . ?
O4 Co1 O1 C27 158.2(4) . . . . ?
O4 Co1 O6 C22 -18.1(3) . . . . ?
O4 Co1 O6 C21 174.4(4) . . . . ?
O4 Co1 N2 C33 -100.8(6) . . . . ?
O4 Co1 N2 C34 71.7(6) . . . . ?
O4 Co2 O3 Co1 -9.35(13) . . . . ?
O4 Co2 O3 Co2 89.22(17) . . . 3_666 ?
O4 Co2 O3 C38 -136.2(5) . . . . ?
O4 Co2 O2 Co1 -45.9(8) . . . 3_666 ?
O4 Co2 O2 C37 70.7(8) . . . . ?
O4 Co2 N1 C12 18.8(5) . . . . ?
O4 Co2 N1 C14 -161.6(3) . . . . ?
O4 C8 C22 O6 1.6(6) . . . . ?
O4 C8 C22 C23 -178.9(5) . . . . ?
O4 C8 C25 C12 4.7(8) . . . . ?
O4 C8 C25 C13 177.4(4) . . . . ?
O1 Co1 O3 Co2 171.60(16) . . . 3_666 ?
O1 Co1 O3 Co2 -86.65(15) . . . . ?
O1 Co1 O3 C38 45.9(5) . . . . ?
O1 Co1 O4 Co2 78.98(17) . . . . ?
O1 Co1 O4 C8 -72.4(4) . . . . ?
O1 Co1 O6 C22 76.1(3) . . . . ?
O1 Co1 O6 C21 -91.4(4) . . . . ?
O1 Co1 N2 C33 10.1(5) . . . . ?
O1 Co1 N2 C34 -177.4(4) . . . . ?
O1 C27 C32 C33 6.7(9) . . . . ?
O1 C27 C32 C31 -177.3(5) . . . . ?
O2 Co1 O3 Co2 7.06(14) 3_666 . . 3_666 ?
O2 Co1 O3 Co2 108.82(16) 3_666 . . . ?
O2 Co1 O3 C38 -118.6(5) 3_666 . . . ?
O2 Co1 O4 Co2 -85.78(17) 3_666 . . . ?
O2 Co1 O4 C8 122.8(3) 3_666 . . . ?
O2 Co1 O1 C27 -72.7(7) 3_666 . . . ?
O2 Co1 O6 C22 -110.8(3) 3_666 . . . ?
O2 Co1 O6 C21 81.7(4) 3_666 . . . ?
O2 Co1 N2 C33 171.6(5) 3_666 . . . ?
O2 Co1 N2 C34 -16.0(4) 3_666 . . . ?
O2 Co2 O3 Co1 -179.23(13) . . . . ?
O2 Co2 O3 Co2 -80.66(18) . . . 3_666 ?
O2 Co2 O3 C38 53.9(5) . . . . ?
O2 Co2 O4 Co1 127.4(7) . . . . ?
O2 Co2 O4 C8 -83.4(8) . . . . ?
O2 Co2 N1 C12 -170.8(5) . . . . ?
O2 Co2 N1 C14 8.7(3) . . . . ?
O6 Co1 O3 Co2 -88.5(3) . . . 3_666 ?
O6 Co1 O3 Co2 13.3(3) . . . . ?
O6 Co1 O3 C38 145.9(5) . . . . ?
O6 Co1 O4 Co2 172.49(18) . . . . ?
O6 Co1 O4 C8 21.1(3) . . . . ?
O6 Co1 O1 C27 86.8(4) . . . . ?
O6 Co1 N2 C33 -85.0(5) . . . . ?
O6 Co1 N2 C34 87.5(4) . . . . ?
O6 C22 C23 C24 179.7(5) . . . . ?
N1 Co2 O3 Co1 -27.2(12) . . . . ?
N1 Co2 O3 Co2 71.3(12) . . . 3_666 ?
N1 Co2 O3 C38 -154.1(12) . . . . ?
N1 Co2 O4 Co1 -172.32(16) . . . . ?
N1 Co2 O4 C8 -23.1(4) . . . . ?
N1 Co2 O2 Co1 -106.61(17) . . . 3_666 ?
N1 Co2 O2 C37 10.0(3) . . . . ?
N1 C12 C25 C8 -9.1(8) . . . . ?
N1 C12 C25 C13 178.3(5) . . . . ?
N1 C14 C37 O2 33.0(6) . . . . ?
N1 C14 C37 C34 153.0(4) . . . 3_666 ?
C8 C22 C23 C24 0.2(8) . . . . ?
O9 C28 C29 C30 -179.8(6) . . . . ?
O9 C28 C27 O1 -1.0(7) . . . . ?
O9 C28 C27 C32 178.6(5) . . . . ?
O7 Co2 O3 Co1 81.31(18) . . . . ?
O7 Co2 O3 Co2 179.9(2) . . . 3_666 ?
O7 Co2 O3 C38 -45.6(5) . . . . ?
O7 Co2 O4 Co1 -78.2(2) . . . . ?
O7 Co2 O4 C8 70.9(4) . . . . ?
O7 Co2 O2 Co1 160.1(2) . . . 3_666 ?
O7 Co2 O2 C37 -83.2(3) . . . . ?
O7 Co2 N1 C12 -71.6(5) . . . . ?
O7 Co2 N1 C14 107.9(4) . . . . ?
C33 N2 C34 C37 -146.7(5) . . . 3_666 ?
C12 N1 C14 C37 154.8(5) . . . . ?
C13 C24 C23 C22 0.9(8) . . . . ?
C14 N1 C12 C25 173.2(5) . . . . ?
C28 C29 C30 C31 -0.8(10) . . . . ?
C28 C27 C32 C33 -173.0(5) . . . . ?
C28 C27 C32 C31 3.0(8) . . . . ?
C29 C28 C27 O1 178.0(5) . . . . ?
C29 C28 C27 C32 -2.3(8) . . . . ?
N2 Co1 O3 Co2 80.0(2) . . . 3_666 ?
N2 Co1 O3 Co2 -178.25(16) . . . . ?
N2 Co1 O3 C38 -45.7(5) . . . . ?
N2 Co1 O4 Co2 -170.8(4) . . . . ?
N2 Co1 O4 C8 37.8(6) . . . . ?
N2 Co1 O1 C27 -3.2(5) . . . . ?
N2 Co1 O6 C22 167.5(3) . . . . ?
N2 Co1 O6 C21 0.0(4) . . . . ?
N2 C33 C32 C27 1.2(9) . . . . ?
N2 C33 C32 C31 -175.0(6) . . . . ?
C24 C13 C25 C8 2.9(8) . . . . ?
C24 C13 C25 C12 175.9(5) . . . . ?
C22 C8 C25 C12 -174.4(5) . . . . ?
C22 C8 C25 C13 -1.7(7) . . . . ?
C27 C28 C29 C30 1.3(9) . . . . ?
C25 C8 C22 O6 -179.3(4) . . . . ?
C25 C8 C22 C23 0.3(8) . . . . ?
C25 C13 C24 C23 -2.5(8) . . . . ?
C21 O6 C22 C8 -177.0(4) . . . . ?
C21 O6 C22 C23 3.5(7) . . . . ?
C32 C33 N2 Co1 -10.5(8) . . . . ?
C32 C33 N2 C34 177.8(5) . . . . ?
C32 C31 C30 C29 1.6(9) . . . . ?
C30 C31 C32 C33 173.5(5) . . . . ?
C30 C31 C32 C27 -2.8(9) . . . . ?
C26 O9 C28 C29 8.2(9) . . . . ?
C26 O9 C28 C27 -172.8(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_details          
;
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.014 0.000 -0.017 447 141 ' '
2 -0.242 0.500 0.255 447 141 ' '

####################################################################### 
# 
# 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_nini
_database_code_depnum_ccdc_archive 'CCDC 1408299'
_audit_update_record             
;
2015-06-23 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H60 Cl6 N4 Ni4 O16'
_chemical_formula_weight         1372.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '

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

_cell_length_a                   9.4859(19)
_cell_length_b                   19.986(4)
_cell_length_c                   14.498(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.14(3)
_cell_angle_gamma                90.00
_cell_volume                     2727.3(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_absorpt_coefficient_mu    1.724
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27922
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         25.01
_reflns_number_total             4819
_reflns_number_gt                3848
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1552P)²+6.7572P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4819
_refine_ls_number_parameters     349
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0857
_refine_ls_wR_factor_ref         0.2506
_refine_ls_wR_factor_gt          0.2325
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.52078(9) 0.12008(4) 0.41729(5) 0.0340(3) Uani 1 1 d . . .
N2 N 0.4272(6) 0.1625(3) 0.3021(4) 0.0388(13) Uani 1 1 d . . .
O1 O 0.7324(6) 0.1832(3) 0.4107(4) 0.0514(13) Uani 1 1 d . . .
O2 O 0.6663(5) 0.0897(2) 0.5198(3) 0.0339(10) Uani 1 1 d . . .
O4 O 0.4603(5) 0.1958(2) 0.4946(3) 0.0429(12) Uani 1 1 d . . .
O7 O 0.4020(4) 0.0511(2) 0.4803(3) 0.0322(10) Uani 1 1 d . . .
C21 C 0.2563(7) 0.0658(4) 0.4905(6) 0.0451(17) Uani 1 1 d . . .
H21A H 0.2073 0.0797 0.4317 0.068 Uiso 1 1 calc R . .
H21B H 0.2528 0.1009 0.5352 0.068 Uiso 1 1 calc R . .
H21C H 0.2115 0.0264 0.5113 0.068 Uiso 1 1 calc R . .
C12 C 0.5200(14) 0.3034(7) 0.6512(8) 0.102(4) Uani 1 1 d . . .
H12A H 0.5858 0.2769 0.6215 0.154 Uiso 1 1 calc R . .
H12B H 0.5431 0.3003 0.7175 0.154 Uiso 1 1 calc R . .
H12C H 0.5258 0.3492 0.6322 0.154 Uiso 1 1 calc R . .
O5 O 0.3835(7) 0.2799(3) 0.6259(4) 0.0577(15) Uani 1 1 d . . .
C13 C 0.3752(8) 0.2449(3) 0.4672(5) 0.0389(16) Uani 1 1 d . . .
C14 C 0.3338(9) 0.2912(4) 0.5349(5) 0.0472(18) Uani 1 1 d . . .
C15 C 0.2443(10) 0.3441(4) 0.5091(6) 0.055(2) Uani 1 1 d . . .
H15 H 0.2216 0.3739 0.5543 0.067 Uiso 1 1 calc R . .
C16 C 0.1874(10) 0.3539(4) 0.4173(7) 0.063(2) Uani 1 1 d . . .
H16 H 0.1239 0.3887 0.4014 0.076 Uiso 1 1 calc R . .
C17 C 0.2255(9) 0.3119(4) 0.3504(6) 0.0509(19) Uani 1 1 d . . .
H17 H 0.1889 0.3193 0.2887 0.061 Uiso 1 1 calc R . .
C18 C 0.3193(8) 0.2572(4) 0.3722(5) 0.0407(16) Uani 1 1 d . . .
C19 C 0.3516(7) 0.2161(4) 0.2954(5) 0.0414(17) Uani 1 1 d . . .
H19 H 0.3144 0.2297 0.2360 0.050 Uiso 1 1 calc R . .
Ni1 Ni 0.55076(8) 0.03190(4) 0.59447(5) 0.0302(3) Uani 1 1 d . . .
N1 N 0.7164(6) 0.0252(3) 0.6927(4) 0.0358(13) Uani 1 1 d . . .
O3 O 0.4617(5) -0.0388(2) 0.6740(3) 0.0352(10) Uani 1 1 d . . .
O6 O 0.4875(5) 0.1231(2) 0.6545(3) 0.0412(11) Uani 1 1 d . . .
C1 C 0.7582(16) 0.2354(7) 0.3499(8) 0.122(6) Uani 1 1 d . . .
H1A H 0.7556 0.2775 0.3815 0.183 Uiso 1 1 calc R . .
H1B H 0.6865 0.2349 0.2969 0.183 Uiso 1 1 calc R . .
H1C H 0.8500 0.2294 0.3297 0.183 Uiso 1 1 calc R . .
C2 C 0.7774(7) 0.1268(3) 0.5526(5) 0.0352(15) Uani 1 1 d . . .
C3 C 0.8191(8) 0.1774(4) 0.4949(5) 0.0408(16) Uani 1 1 d . . .
C4 C 0.9394(8) 0.2157(4) 0.5202(6) 0.0497(19) Uani 1 1 d . . .
H4 H 0.9662 0.2486 0.4805 0.060 Uiso 1 1 calc R . .
C5 C 1.0193(9) 0.2042(4) 0.6057(6) 0.059(2) Uani 1 1 d . . .
H5 H 1.1004 0.2296 0.6231 0.070 Uiso 1 1 calc R . .
C6 C 0.9802(8) 0.1557(4) 0.6651(6) 0.0466(18) Uani 1 1 d . . .
H6 H 1.0345 0.1488 0.7223 0.056 Uiso 1 1 calc R . .
C20 C 0.3864(10) 0.1279(4) 0.7192(6) 0.056(2) Uani 1 1 d . . .
H20A H 0.2921 0.1261 0.6864 0.084 Uiso 1 1 calc R . .
H20B H 0.3993 0.1694 0.7524 0.084 Uiso 1 1 calc R . .
H20C H 0.3996 0.0913 0.7624 0.084 Uiso 1 1 calc R . .
C7 C 0.8578(7) 0.1163(3) 0.6393(5) 0.0349(15) Uani 1 1 d . . .
C8 C 0.8259(7) 0.0643(4) 0.7045(5) 0.0391(16) Uani 1 1 d . . .
H8 H 0.8889 0.0589 0.7585 0.047 Uiso 1 1 calc R . .
C9 C 0.7073(7) -0.0312(4) 0.7556(5) 0.0411(17) Uani 1 1 d . . .
H9A H 0.7508 -0.0191 0.8174 0.049 Uiso 1 1 calc R . .
H9B H 0.7589 -0.0690 0.7346 0.049 Uiso 1 1 calc R . .
C10 C 0.5507(7) -0.0509(4) 0.7588(5) 0.0381(15) Uani 1 1 d . . .
H10 H 0.5142 -0.0252 0.8083 0.046 Uiso 1 1 calc R . .
C11 C 0.5445(9) -0.1263(4) 0.7827(5) 0.0439(17) Uani 1 1 d . . .
H11A H 0.6157 -0.1373 0.8344 0.053 Uiso 1 1 calc R . .
H11B H 0.4516 -0.1380 0.7992 0.053 Uiso 1 1 calc R . .
C22 C 0.9020(11) 0.0485(7) 0.3239(10) 0.104(5) Uani 1 1 d . . .
H22A H 0.9501 0.0852 0.2986 0.157 Uiso 1 1 calc R . .
H22B H 0.9668 0.0118 0.3365 0.157 Uiso 1 1 calc R . .
H22C H 0.8678 0.0623 0.3805 0.157 Uiso 1 1 calc R . .
C23 C 0.1837(16) 0.0520(8) 0.9065(17) 0.157(8) Uani 1 1 d . . .
H23 H 0.1795 0.0390 0.8410 0.188 Uiso 1 1 calc R . .
Cl1 Cl 0.0693(8) -0.0055(6) 0.9842(9) 0.286(5) Uani 1 1 d . . .
Cl2 Cl 0.1212(15) 0.1225(5) 0.9242(7) 0.302(5) Uani 1 1 d . . .
Cl3 Cl 0.3498(7) 0.0368(4) 0.9761(5) 0.219(3) Uani 1 1 d . . .
O8 O 0.7909(7) 0.0290(5) 0.2617(5) 0.094(3) Uani 1 1 d . . .
H8A H 0.7392 0.0040 0.2874 0.142 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 N2 1.982(6) . ?
Ni2 O2 1.993(4) . ?
Ni2 O4 2.009(5) . ?
Ni2 O7 2.064(4) . ?
Ni2 O3 2.114(5) 3_656 ?
Ni2 O1 2.383(5) . ?
N2 C19 1.286(9) . ?
N2 C11 1.479(9) 3_656 ?
O1 C3 1.389(9) . ?
O1 C1 1.406(11) . ?
O2 C2 1.326(8) . ?
O2 Ni1 2.001(4) . ?
O4 C13 1.300(8) . ?
O7 C21 1.439(8) . ?
O7 Ni1 2.060(4) 3_656 ?
O7 Ni1 2.073(4) . ?
C12 O5 1.382(13) . ?
O5 C14 1.364(9) . ?
C13 C18 1.434(10) . ?
C13 C14 1.439(10) . ?
C14 C15 1.378(11) . ?
C15 C16 1.387(12) . ?
C16 C17 1.365(12) . ?
C17 C18 1.420(10) . ?
C18 C19 1.446(10) . ?
Ni1 N1 1.990(6) . ?
Ni1 O7 2.060(4) 3_656 ?
Ni1 O3 2.069(5) . ?
Ni1 O6 2.137(5) . ?
N1 C8 1.293(9) . ?
N1 C9 1.459(9) . ?
O3 C10 1.423(8) . ?
O3 Ni2 2.114(5) 3_656 ?
O6 C20 1.426(9) . ?
C2 C3 1.401(10) . ?
C2 C7 1.403(9) . ?
C3 C4 1.385(10) . ?
C4 C5 1.390(12) . ?
C5 C6 1.377(12) . ?
C6 C7 1.414(10) . ?
C7 C8 1.463(10) . ?
C9 C10 1.543(10) . ?
C10 C11 1.549(10) . ?
C11 N2 1.479(9) 3_656 ?
C22 O8 1.356(13) . ?
C23 Cl2 1.562(15) . ?
C23 Cl3 1.79(2) . ?
C23 Cl1 2.02(2) . ?
Cl1 Cl1 1.461(17) 3_557 ?

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
N2 Ni2 O2 162.7(2) . . ?
N2 Ni2 O4 91.0(2) . . ?
O2 Ni2 O4 91.89(19) . . ?
N2 Ni2 O7 116.5(2) . . ?
O2 Ni2 O7 80.34(17) . . ?
O4 Ni2 O7 92.72(19) . . ?
N2 Ni2 O3 82.1(2) . 3_656 ?
O2 Ni2 O3 97.58(18) . 3_656 ?
O4 Ni2 O3 167.92(19) . 3_656 ?
O7 Ni2 O3 81.55(18) . 3_656 ?
N2 Ni2 O1 91.8(2) . . ?
O2 Ni2 O1 71.48(18) . . ?
O4 Ni2 O1 85.6(2) . . ?
O7 Ni2 O1 151.68(17) . . ?
O3 Ni2 O1 104.46(19) 3_656 . ?
C19 N2 C11 120.1(6) . 3_656 ?
C19 N2 Ni2 127.4(5) . . ?
C11 N2 Ni2 112.5(4) 3_656 . ?
C3 O1 C1 118.9(7) . . ?
C3 O1 Ni2 109.3(4) . . ?
C1 O1 Ni2 129.1(6) . . ?
C2 O2 Ni2 122.9(4) . . ?
C2 O2 Ni1 126.4(4) . . ?
Ni2 O2 Ni1 101.77(19) . . ?
C13 O4 Ni2 127.4(4) . . ?
C21 O7 Ni1 119.5(4) . 3_656 ?
C21 O7 Ni2 119.5(4) . . ?
Ni1 O7 Ni2 97.98(18) 3_656 . ?
C21 O7 Ni1 121.5(4) . . ?
Ni1 O7 Ni1 95.77(18) 3_656 . ?
Ni2 O7 Ni1 97.01(17) . . ?
C14 O5 C12 113.6(8) . . ?
O4 C13 C18 124.3(6) . . ?
O4 C13 C14 119.2(6) . . ?
C18 C13 C14 116.5(6) . . ?
O5 C14 C15 121.1(7) . . ?
O5 C14 C13 117.6(7) . . ?
C15 C14 C13 121.3(7) . . ?
C14 C15 C16 121.5(8) . . ?
C17 C16 C15 119.3(8) . . ?
C16 C17 C18 122.0(8) . . ?
C17 C18 C13 119.5(7) . . ?
C17 C18 C19 116.9(7) . . ?
C13 C18 C19 123.6(6) . . ?
N2 C19 C18 125.8(6) . . ?
N1 Ni1 O2 89.4(2) . . ?
N1 Ni1 O7 96.8(2) . 3_656 ?
O2 Ni1 O7 90.62(18) . 3_656 ?
N1 Ni1 O3 84.0(2) . . ?
O2 Ni1 O3 170.00(19) . . ?
O7 Ni1 O3 82.73(18) 3_656 . ?
N1 Ni1 O7 169.3(2) . . ?
O2 Ni1 O7 79.95(17) . . ?
O7 Ni1 O7 84.23(18) 3_656 . ?
O3 Ni1 O7 106.65(18) . . ?
N1 Ni1 O6 90.2(2) . . ?
O2 Ni1 O6 85.88(18) . . ?
O7 Ni1 O6 172.19(18) 3_656 . ?
O3 Ni1 O6 101.61(18) . . ?
O7 Ni1 O6 88.28(18) . . ?
C8 N1 C9 119.5(6) . . ?
C8 N1 Ni1 127.2(5) . . ?
C9 N1 Ni1 113.3(4) . . ?
C10 O3 Ni1 110.9(4) . . ?
C10 O3 Ni2 109.1(4) . 3_656 ?
Ni1 O3 Ni2 96.14(19) . 3_656 ?
C20 O6 Ni1 124.8(5) . . ?
O2 C2 C3 117.4(6) . . ?
O2 C2 C7 123.9(6) . . ?
C3 C2 C7 118.7(6) . . ?
C4 C3 O1 124.4(7) . . ?
C4 C3 C2 121.7(7) . . ?
O1 C3 C2 113.9(6) . . ?
C3 C4 C5 119.0(7) . . ?
C6 C5 C4 121.0(7) . . ?
C5 C6 C7 120.1(7) . . ?
C2 C7 C6 119.5(7) . . ?
C2 C7 C8 123.5(6) . . ?
C6 C7 C8 117.0(6) . . ?
N1 C8 C7 124.8(6) . . ?
N1 C9 C10 110.4(5) . . ?
O3 C10 C9 113.6(5) . . ?
O3 C10 C11 108.8(5) . . ?
C9 C10 C11 108.6(6) . . ?
N2 C11 C10 105.9(5) 3_656 . ?
Cl2 C23 Cl3 112.8(12) . . ?
Cl2 C23 Cl1 100.4(10) . . ?
Cl3 C23 Cl1 94.8(12) . . ?
Cl1 Cl1 C23 131.1(13) 3_557 . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.973
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.172
####################################################################### 
# 
# 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_P150509F
_database_code_depnum_ccdc_archive 'CCDC 1408300'
_audit_update_record             
;
2015-06-23 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-06-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_formula_moiety         'C42 H48 Br4 Co4 N4 O14, O, 2(C H3 O)'
_chemical_formula_sum            'C44 H54 Br4 Co4 N4 O17'
_chemical_formula_weight         1466.28
_chemical_oxdiff_formula         C1H1O1N1CO1
_chemical_oxdiff_usercomment     C8
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Co 0.35655 0.96576 12.28410 7.34090 4.00340 2.34880 4.27910 0.27840 13.53590
71.16920 1.01180005074
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Br -0.28346 2.55990 17.17890 5.23580 5.63770 3.98510 2.17230 16.57960 0.26090
41.43280 2.95569992065
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/c 1'
_space_group_name_Hall           '-C 2yc (x,y,-x+z)'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z+1/2
6 -x+1/2,y+1/2,-z+1
7 -x+1/2,-y+1/2,-z+1/2
8 x+1/2,-y+1/2,z

_symmetry_Int_Tables_number      15
_cell_length_a                   17.1056(4)
_cell_length_b                   11.7616(2)
_cell_length_c                   27.3199(8)
_cell_angle_alpha                90
_cell_angle_beta                 104.388(2)
_cell_angle_gamma                90
_cell_volume                     5324.1(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5196
_cell_measurement_temperature    125.40(14)
_cell_measurement_theta_max      28.7160
_cell_measurement_theta_min      3.7810
_exptl_absorpt_coefficient_mu    4.298
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.8292
_exptl_crystal_description       prism
_exptl_crystal_F_000             2922.6677
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13100
_diffrn_reflns_theta_full        25.0095
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.89
_diffrn_ambient_temperature      125.40(14)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9983
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -5.00   56.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -99.0000 -120.0000 61

#__ type_ start__ end____ width___ exp.time_
  2 omega   34.00   86.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497   63.0000  -61.0000 52

#__ type_ start__ end____ width___ exp.time_
  3 omega  -28.00   45.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -19.0000  -30.0000 73

#__ type_ start__ end____ width___ exp.time_
  4 omega    1.00   59.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3497  -99.0000  120.0000 58
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0210827000
_diffrn_orient_matrix_UB_12      0.0369335000
_diffrn_orient_matrix_UB_13      0.0127906000
_diffrn_orient_matrix_UB_21      -0.0073067000
_diffrn_orient_matrix_UB_22      -0.0461335000
_diffrn_orient_matrix_UB_23      0.0149748000
_diffrn_orient_matrix_UB_31      0.0365324000
_diffrn_orient_matrix_UB_32      0.0120941000
_diffrn_orient_matrix_UB_33      0.0181708000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                4084
_reflns_number_total             4688
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         0.8117
_refine_diff_density_min         -0.7686
_refine_diff_density_rms         0.1141
_refine_ls_d_res_high            0.8406
_refine_ls_d_res_low             7.0568
_refine_ls_goodness_of_fit_ref   1.0662
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     346
_refine_ls_number_reflns         4688
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0318
_refine_ls_restrained_S_all      1.0660
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0274P)²+22.4461P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0770
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 C21-H7
 1.8832 with sigma of 0.02
3. Others
 Fixed Sof: Br0a(0.5) Br1(0.5)
4.a Ternary CH refined with riding coordinates:
 C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C11(H11a,H11b), C9(H9a,H9b)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C6(H6), C4(H4), C8(H8), C16(H16), C12(H12)
4.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C1(H1a,H1b,H1c), C22(H22a,H22b,H22c), C20(H20a,H20b,
 H20c), C21(H21a,H21b,H21c)
;
_atom_sites_solution_primary     iterative
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br2 Br 0.62319(2) 0.50021(4) 0.485526(15) 0.03054(12) Uani 1.000000 1 . . .
Br0a Br 0.48837(12) 1.1776(3) 0.02034(9) 0.0220(4) Uani 0.500000 1 . . .
Co2 Co 0.29750(3) 0.80452(4) 0.300403(17) 0.01543(12) Uani 1.000000 1 . . .
Co1 Co 0.26079(3) 0.94497(4) 0.199083(17) 0.01717(12) Uani 1.000000 1 . . .
O4 O 0.34382(13) 0.6443(2) 0.31549(9) 0.0176(5) Uani 1.000000 1 . . .
O3 O 0.27505(13) 0.9700(2) 0.27735(9) 0.0176(5) Uani 1.000000 1 . . .
O6 O 0.30838(13) 0.78565(19) 0.22551(9) 0.0158(5) Uani 1.000000 1 . . .
O1 O 0.28759(15) 0.8484(2) 0.04150(9) 0.0232(6) Uani 1.000000 1 . . .
O2 O 0.28377(15) 0.9170(2) 0.13147(9) 0.0221(6) Uani 1.000000 1 . . .
O5 O 0.34962(14) 0.4364(2) 0.34750(9) 0.0233(6) Uani 1.000000 1 . . .
O7 O 0.26646(17) 0.8040(2) 0.37190(9) 0.0267(6) Uani 1.000000 1 D . .
H7 H 0.248(2) 0.7395(18) 0.3772(10) 0.0401(9) Uiso 1.000000 1 DR . .
C15 C 0.5366(2) 0.5490(3) 0.43122(13) 0.0217(8) Uani 1.000000 1 . . .
N2 N 0.41187(17) 0.8640(2) 0.32858(11) 0.0197(7) Uani 1.000000 1 . . .
N1 N 0.33546(18) 1.0816(2) 0.20989(11) 0.0198(7) Uani 1.000000 1 . . .
O9 O 0.0 1.1669(6) 0.25 0.124(3) Uani 1.000000 2 S T P
C5 C 0.4185(2) 1.1010(3) 0.05400(15) 0.0250(8) Uani 1.000000 1 . . .
O8 O 0.1570(3) 1.0968(4) 0.29822(18) 0.0897(16) Uani 1.000000 1 . . .
C14 C 0.5348(2) 0.6577(3) 0.41346(14) 0.0220(8) Uani 1.000000 1 . . .
H14 H 0.5768(2) 0.7074(3) 0.42710(14) 0.0264(10) Uiso 1.000000 1 R . .
C17 C 0.4127(2) 0.5058(3) 0.37167(13) 0.0191(8) Uani 1.000000 1 . . .
C18 C 0.40672(19) 0.6180(3) 0.35276(13) 0.0172(7) Uani 1.000000 1 . . .
C3 C 0.3308(2) 0.9451(3) 0.05866(13) 0.0193(8) Uani 1.000000 1 . . .
C10 C 0.3422(2) 1.0417(3) 0.29756(13) 0.0203(8) Uani 1.000000 1 . . .
H10 H 0.3353(2) 1.0762(3) 0.32889(13) 0.0244(9) Uiso 1.000000 1 R . .
C6 C 0.4142(2) 1.1395(3) 0.09994(14) 0.0228(8) Uani 1.000000 1 . . .
H6 H 0.4417(2) 1.2054(3) 0.11310(14) 0.0274(10) Uiso 1.000000 1 R . .
C2 C 0.3253(2) 0.9796(3) 0.10798(13) 0.0177(7) Uani 1.000000 1 . . .
C4 C 0.3765(2) 1.0041(3) 0.03215(14) 0.0226(8) Uani 1.000000 1 . . .
H4 H 0.3794(2) 0.9799(3) 0.00024(14) 0.0271(10) Uiso 1.000000 1 R . .
C11 C 0.4222(2) 0.9763(3) 0.30901(14) 0.0227(8) Uani 1.000000 1 . . .
H11a H 0.4627(2) 1.0180(3) 0.33364(14) 0.0272(10) Uiso 1.000000 1 R . .
H11b H 0.4409(2) 0.9692(3) 0.27838(14) 0.0272(10) Uiso 1.000000 1 R . .
C8 C 0.3720(2) 1.1234(3) 0.17829(14) 0.0203(8) Uani 1.000000 1 . . .
H8 H 0.4038(2) 1.1874(3) 0.18844(14) 0.0243(9) Uiso 1.000000 1 R . .
C19 C 0.3456(3) 0.3260(3) 0.36833(17) 0.0344(10) Uani 1.000000 1 . . .
H19a H 0.2978(9) 0.2879(10) 0.3497(7) 0.0517(15) Uiso 1.000000 1 GR . .
H19b H 0.3923(9) 0.2829(9) 0.3662(10) 0.0517(15) Uiso 1.000000 1 GR . .
H19c H 0.3440(17) 0.3330(3) 0.4031(3) 0.0517(15) Uiso 1.000000 1 GR . .
C16 C 0.4759(2) 0.4708(3) 0.41068(14) 0.0222(8) Uani 1.000000 1 . . .
H16 H 0.4780(2) 0.3969(3) 0.42303(14) 0.0267(10) Uiso 1.000000 1 R . .
C13 C 0.4693(2) 0.6947(3) 0.37447(13) 0.0192(8) Uani 1.000000 1 . . .
C9 C 0.3444(2) 1.1359(3) 0.25945(13) 0.0218(8) Uani 1.000000 1 . . .
H9a H 0.3952(2) 1.1767(3) 0.26909(13) 0.0262(10) Uiso 1.000000 1 R . .
H9b H 0.3008(2) 1.1895(3) 0.25819(13) 0.0262(10) Uiso 1.000000 1 R . .
C12 C 0.4711(2) 0.8120(3) 0.35738(13) 0.0209(8) Uani 1.000000 1 . . .
H12 H 0.5192(2) 0.8518(3) 0.36837(13) 0.0251(9) Uiso 1.000000 1 R . .
C7 C 0.3680(2) 1.0796(3) 0.12811(14) 0.0194(8) Uani 1.000000 1 . . .
C1 C 0.2872(2) 0.8107(3) -0.00805(14) 0.0271(9) Uani 1.000000 1 . . .
H1a H 0.2698(15) 0.8716(7) -0.03165(19) 0.0407(13) Uiso 1.000000 1 GR . .
H1b H 0.3406(4) 0.787(2) -0.0090(3) 0.0407(13) Uiso 1.000000 1 GR . .
H1c H 0.2509(12) 0.7475(14) -0.0170(4) 0.0407(13) Uiso 1.000000 1 GR . .
C22 C 0.1488(5) 1.0644(6) 0.3475(3) 0.106(3) Uani 1.000000 1 . . .
H22a H 0.185(3) 1.109(4) 0.3728(3) 0.159(4) Uiso 1.000000 1 GR . .
H22b H 0.0942(10) 1.077(5) 0.3495(8) 0.159(4) Uiso 1.000000 1 GR . .
H22c H 0.162(4) 0.9853(14) 0.3531(10) 0.159(4) Uiso 1.000000 1 GR . .
C20 C 0.3824(2) 0.7467(3) 0.21713(14) 0.0244(8) Uani 1.000000 1 . . .
H20a H 0.4239(4) 0.8019(10) 0.2298(8) 0.0366(13) Uiso 1.000000 1 GR . .
H20b H 0.3969(8) 0.6758(11) 0.2344(8) 0.0366(13) Uiso 1.000000 1 GR . .
H20c H 0.3766(5) 0.736(2) 0.18156(16) 0.0366(13) Uiso 1.000000 1 GR . .
C21 C 0.3024(4) 0.8589(5) 0.41726(18) 0.0633(17) Uani 1.000000 1 D . .
H21a H 0.331(2) 0.925(2) 0.4104(2) 0.095(3) Uiso 1.000000 1 GR . .
H21b H 0.2615(4) 0.881(3) 0.4338(8) 0.095(3) Uiso 1.000000 1 GR . .
H21c H 0.3396(18) 0.8080(13) 0.4388(6) 0.095(3) Uiso 1.000000 1 GR . .
Br1 Br 0.47777(19) 1.1808(3) 0.01370(13) 0.0673(10) Uani 0.500000 1 . . .


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
Br2 C15 1.906(3) . ?
Br0a C5 1.906(5) . ?
Br0a Br1 0.226(5) . ?
Co2 O4 2.046(2) . ?
Co2 O3 2.052(2) . ?
Co2 O6 2.112(2) . ?
Co2 O6 2.066(2) 7_565 ?
Co2 O7 2.148(3) . ?
Co2 N2 2.040(3) . ?
Co1 O4 2.027(2) 7_565 ?
Co1 O3 2.112(2) . ?
Co1 O6 2.098(2) . ?
Co1 O2 2.009(2) . ?
Co1 N1 2.029(3) . ?
O4 C18 1.321(4) . ?
O3 C10 1.422(4) . ?
O6 C20 1.418(4) . ?
O1 C3 1.374(4) . ?
O1 C1 1.423(4) . ?
O2 C2 1.298(4) . ?
O5 C17 1.383(4) . ?
O5 C19 1.426(4) . ?
O7 C21 1.397(5) . ?
C15 C14 1.365(5) . ?
C15 C16 1.396(5) . ?
N2 C11 1.452(5) . ?
N2 C12 1.274(4) . ?
N1 C8 1.283(5) . ?
N1 C9 1.470(4) . ?
C5 C6 1.353(5) . ?
C5 C4 1.399(5) . ?
C5 Br1 1.917(5) . ?
O8 C22 1.440(7) . ?
C14 C13 1.409(5) . ?
C17 C18 1.412(5) . ?
C17 C16 1.378(5) . ?
C18 C13 1.412(5) . ?
C3 C2 1.432(5) . ?
C3 C4 1.378(5) . ?
C10 C11 1.533(5) . ?
C10 C9 1.527(5) . ?
C6 C7 1.420(5) . ?
C2 C7 1.422(5) . ?
C8 C7 1.450(5) . ?
C13 C12 1.459(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Br0a C5 89.5(15) . . ?
O3 Co2 O4 165.65(9) . . ?
O6 Co2 O4 81.89(9) 7_565 . ?
O6 Co2 O4 88.59(9) . . ?
O6 Co2 O3 81.78(9) . . ?
O6 Co2 O3 107.48(9) 7_565 . ?
O7 Co2 O4 89.14(10) . . ?
O7 Co2 O3 102.25(10) . . ?
O7 Co2 O6 169.14(9) . . ?
O7 Co2 O6 85.20(9) . 7_565 ?
N2 Co2 O4 87.30(10) . . ?
N2 Co2 O3 83.06(10) . . ?
N2 Co2 O6 95.43(10) . . ?
N2 Co2 O6 169.18(11) . 7_565 ?
N2 Co2 O7 95.08(11) . . ?
O3 Co1 O4 98.34(9) . 7_565 ?
O6 Co1 O4 81.55(9) . 7_565 ?
O6 Co1 O3 80.71(9) . . ?
O2 Co1 O4 95.71(10) . 7_565 ?
O2 Co1 O3 162.59(9) . . ?
O2 Co1 O6 91.28(9) . . ?
N1 Co1 O4 158.78(11) . 7_565 ?
N1 Co1 O3 80.34(10) . . ?
N1 Co1 O6 118.76(10) . . ?
N1 Co1 O2 90.21(11) . . ?
Co1 O4 Co2 99.14(10) 7_565 . ?
C18 O4 Co2 124.9(2) . . ?
C18 O4 Co1 122.7(2) . 7_565 ?
Co1 O3 Co2 98.31(10) . . ?
C10 O3 Co2 111.85(19) . . ?
C10 O3 Co1 110.78(19) . . ?
Co1 O6 Co2 96.87(9) . . ?
Co1 O6 Co2 96.22(9) . 7_565 ?
C20 O6 Co2 119.2(2) . . ?
C20 O6 Co2 121.4(2) . 7_565 ?
C20 O6 Co1 121.2(2) . . ?
C1 O1 C3 117.3(3) . . ?
C2 O2 Co1 128.2(2) . . ?
C19 O5 C17 117.1(3) . . ?
C21 O7 Co2 130.6(3) . . ?
C14 C15 Br2 120.2(3) . . ?
C16 C15 Br2 118.1(3) . . ?
C16 C15 C14 121.7(3) . . ?
C11 N2 Co2 111.5(2) . . ?
C12 N2 Co2 127.5(2) . . ?
C12 N2 C11 120.9(3) . . ?
C8 N1 Co1 126.9(2) . . ?
C9 N1 Co1 113.3(2) . . ?
C9 N1 C8 119.8(3) . . ?
C6 C5 Br0a 118.3(3) . . ?
C4 C5 Br0a 119.8(3) . . ?
C4 C5 C6 121.9(3) . . ?
Br1 C5 Br0a 6.76(14) . . ?
Br1 C5 C6 121.8(3) . . ?
Br1 C5 C4 116.3(3) . . ?
C13 C14 C15 120.1(3) . . ?
C18 C17 O5 113.6(3) . . ?
C16 C17 O5 124.2(3) . . ?
C16 C17 C18 122.2(3) . . ?
C17 C18 O4 118.2(3) . . ?
C13 C18 O4 124.1(3) . . ?
C13 C18 C17 117.7(3) . . ?
C2 C3 O1 113.6(3) . . ?
C4 C3 O1 124.4(3) . . ?
C4 C3 C2 122.0(3) . . ?
C11 C10 O3 112.1(3) . . ?
C9 C10 O3 108.7(3) . . ?
C9 C10 C11 109.3(3) . . ?
C7 C6 C5 120.1(3) . . ?
C3 C2 O2 118.5(3) . . ?
C7 C2 O2 124.7(3) . . ?
C7 C2 C3 116.8(3) . . ?
C3 C4 C5 119.0(3) . . ?
C10 C11 N2 110.3(3) . . ?
C7 C8 N1 125.7(3) . . ?
C17 C16 C15 118.4(3) . . ?
C18 C13 C14 119.8(3) . . ?
C12 C13 C14 117.2(3) . . ?
C12 C13 C18 122.9(3) . . ?
C10 C9 N1 107.3(3) . . ?
C13 C12 N2 125.1(3) . . ?
C2 C7 C6 120.2(3) . . ?
C8 C7 C6 115.8(3) . . ?
C8 C7 C2 124.0(3) . . ?
C5 Br1 Br0a 83.7(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O7 H7 1 0.8500 0.0100 0.0020
C21 H7 1 1.8832 0.0200 0.0050

####################################################################### 
# 
# 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_Znde
_database_code_depnum_ccdc_archive 'CCDC 1408301'
_audit_update_record             
;
2015-06-23 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2014-08-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.20 svn.r2946 for OlexSys, GUI svn.r4855)
;
_chemical_formula_moiety         'C42 H52 N4 O14 Zn4, 4(C H4 O)'
_chemical_formula_sum            'C46 H68 N4 O18 Zn4'
_chemical_formula_weight         1226.65
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Zn 0.31207 1.46666 14.07430 7.03180 5.16520 2.41000 3.26550 0.23330 10.31630
58.70970 1.30410003662
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   12.212(2)
_cell_length_b                   16.600(3)
_cell_length_c                   13.056(3)
_cell_angle_alpha                90
_cell_angle_beta                 90.21(3)
_cell_angle_gamma                90
_cell_volume                     2646.7(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7895
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8984
_cell_measurement_theta_min      1.5597
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7953
_exptl_absorpt_correction_type   Multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.5391
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1275.0807
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22224
_diffrn_reflns_theta_full        25.0070
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.07
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.9938
_diffrn_measured_fraction_theta_max 0.9938
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -110.0000 - 70.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 49.9890
	          2theta: -19.8952
scan:
	Number of images: 150
	           Slice: -110.0000 - 40.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 49.9890
	          2theta: -19.8952
scan:
	Number of images: 80
	           Slice: -110.0000 - -30.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 49.9890
	          2theta: -19.8952
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             11904
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0231
_diffrn_orient_matrix_UB_12      0.0393
_diffrn_orient_matrix_UB_13      -0.0681
_diffrn_orient_matrix_UB_21      -0.0733
_diffrn_orient_matrix_UB_22      -0.0074
_diffrn_orient_matrix_UB_23      0.0209
_diffrn_orient_matrix_UB_31      0.0032
_diffrn_orient_matrix_UB_32      0.0525
_diffrn_orient_matrix_UB_33      0.0293
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4117
_reflns_number_total             4647
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         0.3933
_refine_diff_density_min         -0.4771
_refine_diff_density_rms         0.0896
_refine_ls_d_res_high            0.8406
_refine_ls_d_res_low             9.8368
_refine_ls_goodness_of_fit_ref   1.0333
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4647
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0312
_refine_ls_restrained_S_all      1.0330
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0422P)²+1.1696P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0739
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 Zn1-H6
 2.759927 with sigma of 0.02
 C20-H6
 1.892168 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C11(H11a,H11b)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C16(H16), C6(H6a), C4(H4), C15(H15), C14(H14), C5(H5)
3.d Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C1(H1a,H1b,
 H1c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c)
3.e Idealised tetrahedral OH refined as rotating group:
 O8(H8a), O9(H9)
;
_atom_sites_solution_primary     iterative
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_refinement_flags_posn
Zn1 Zn 0.88294(2) 0.459421(15) 0.498629(19) 0.01206(9) Uani 1.000000 D
Zn2 Zn 1.08236(2) 0.380589(15) 0.61199(2) 0.01305(9) Uani 1.000000 .
O3 O 0.90636(13) 0.39028(9) 0.62736(12) 0.0140(3) Uani 1.000000 .
O2 O 0.87640(13) 0.50637(9) 0.35108(12) 0.0145(3) Uani 1.000000 .
O4 O 1.23379(13) 0.34709(10) 0.56918(13) 0.0191(4) Uani 1.000000 .
O6 O 0.71731(13) 0.50944(10) 0.51804(13) 0.0176(4) Uani 1.000000 D
H6 H 0.7076(16) 0.5561(9) 0.4911(16) 0.0264(6) Uiso 1.000000 DR
O7 O 0.94703(12) 0.56904(9) 0.53009(11) 0.0120(3) Uani 1.000000 .
O1 O 0.83978(14) 0.60964(10) 0.20684(13) 0.0204(4) Uani 1.000000 .
O5 O 1.43719(14) 0.33874(10) 0.51488(14) 0.0244(4) Uani 1.000000 .
N3 N 0.82714(15) 0.35362(11) 0.43745(15) 0.0132(4) Uani 1.000000 .
N4 N 1.04632(15) 0.26524(11) 0.64790(14) 0.0152(4) Uani 1.000000 .
C10 C 0.86022(19) 0.31217(13) 0.61653(18) 0.0152(5) Uani 1.000000 .
H10 H 0.78646(19) 0.31220(13) 0.64586(18) 0.0182(6) Uiso 1.000000 R
C12 C 1.11446(19) 0.20587(14) 0.65021(17) 0.0147(5) Uani 1.000000 .
H12 H 1.08661(19) 0.15602(14) 0.66958(17) 0.0176(6) Uiso 1.000000 R
C2 C 0.80958(18) 0.48293(14) 0.27740(18) 0.0146(5) Uani 1.000000 .
C21 C 0.9177(2) 0.60733(14) 0.62308(18) 0.0165(5) Uani 1.000000 .
H21a H 0.9209(13) 0.5690(3) 0.6781(3) 0.0247(8) Uiso 1.000000 GR
H21b H 0.9676(8) 0.6507(6) 0.6368(6) 0.0247(8) Uiso 1.000000 GR
H21c H 0.8446(5) 0.6282(8) 0.6174(5) 0.0247(8) Uiso 1.000000 GR
C8 C 0.77607(18) 0.34384(14) 0.35253(18) 0.0144(5) Uani 1.000000 .
H8 H 0.74747(18) 0.29299(14) 0.33908(18) 0.0172(6) Uiso 1.000000 R
C18 C 1.28190(19) 0.27827(14) 0.58539(17) 0.0152(5) Uani 1.000000 .
C17 C 1.3939(2) 0.27028(14) 0.55736(18) 0.0168(5) Uani 1.000000 .
C9 C 0.8532(2) 0.28531(14) 0.50374(18) 0.0168(5) Uani 1.000000 .
H9a H 0.7971(2) 0.24432(14) 0.49642(18) 0.0202(6) Uiso 1.000000 R
H9b H 0.9226(2) 0.26202(14) 0.48319(18) 0.0202(6) Uiso 1.000000 R
C11 C 0.93227(19) 0.25228(14) 0.67663(19) 0.0174(5) Uani 1.000000 .
H11a H 0.91069(19) 0.19745(14) 0.66067(19) 0.0209(6) Uiso 1.000000 R
H11b H 0.92337(19) 0.26070(14) 0.74965(19) 0.0209(6) Uiso 1.000000 R
C3 C 0.7886(2) 0.53623(14) 0.19568(18) 0.0171(5) Uani 1.000000 .
C7 C 0.75920(19) 0.40598(14) 0.27531(18) 0.0153(5) Uani 1.000000 .
C16 C 1.4497(2) 0.19900(15) 0.5711(2) 0.0234(6) Uani 1.000000 .
H16 H 1.5227(2) 0.19516(15) 0.5516(2) 0.0281(7) Uiso 1.000000 R
C13 C 1.22899(19) 0.20897(14) 0.62588(17) 0.0153(5) Uani 1.000000 .
C6 C 0.6937(2) 0.38490(15) 0.1899(2) 0.0216(6) Uani 1.000000 .
H6a H 0.6614(2) 0.33420(15) 0.1874(2) 0.0260(7) Uiso 1.000000 R
C4 C 0.7240(2) 0.51412(16) 0.11341(19) 0.0233(6) Uani 1.000000 .
H4 H 0.7119(2) 0.55008(16) 0.05993(19) 0.0280(7) Uiso 1.000000 R
C15 C 1.3970(2) 0.13213(15) 0.6144(2) 0.0263(6) Uani 1.000000 .
H15 H 1.4358(2) 0.08474(15) 0.6256(2) 0.0316(7) Uiso 1.000000 R
C14 C 1.2895(2) 0.13637(15) 0.63993(18) 0.0195(5) Uani 1.000000 .
H14 H 1.2548(2) 0.09128(15) 0.66698(18) 0.0234(7) Uiso 1.000000 R
C5 C 0.6768(2) 0.43770(17) 0.1108(2) 0.0262(6) Uani 1.000000 .
H5 H 0.6338(2) 0.42250(17) 0.0552(2) 0.0314(7) Uiso 1.000000 R
C19 C 1.5471(2) 0.33423(17) 0.4802(2) 0.0337(7) Uani 1.000000 .
H19a H 1.5947(3) 0.3230(12) 0.5371(3) 0.0506(11) Uiso 1.000000 GR
H19b H 1.5535(4) 0.2920(8) 0.4303(11) 0.0506(11) Uiso 1.000000 GR
H19c H 1.5675(6) 0.3846(4) 0.4496(14) 0.0506(11) Uiso 1.000000 GR
C20 C 0.6515(2) 0.50716(18) 0.6080(2) 0.0284(6) Uani 1.000000 D
H20a H 0.6599(12) 0.5567(5) 0.6451(8) 0.0425(10) Uiso 1.000000 GR
H20b H 0.5761(3) 0.5002(11) 0.5890(2) 0.0425(10) Uiso 1.000000 GR
H20c H 0.6743(10) 0.4630(7) 0.6505(7) 0.0425(10) Uiso 1.000000 GR
C1 C 0.8181(3) 0.66901(17) 0.1308(2) 0.0354(7) Uani 1.000000 .
H1a H 0.8541(14) 0.7184(4) 0.1491(8) 0.0531(11) Uiso 1.000000 GR
H1b H 0.8450(14) 0.6507(5) 0.0658(4) 0.0531(11) Uiso 1.000000 GR
H1c H 0.7406(3) 0.6780(9) 0.1260(11) 0.0531(11) Uiso 1.000000 GR
O8 O 0.82457(16) 0.43966(12) 0.80638(14) 0.0316(5) Uani 1.000000 .
H8a H 0.8532(3) 0.429(2) 0.7512(5) 0.0473(7) Uiso 1.000000 GR
O9 O 0.64636(19) 0.33961(14) 0.8419(2) 0.0613(7) Uani 1.000000 .
H9 H 0.6950(5) 0.3721(12) 0.829(3) 0.0920(11) Uiso 1.000000 GR
C22 C 0.9065(3) 0.4460(2) 0.8829(2) 0.0376(8) Uani 1.000000 .
H22a H 0.8739(4) 0.4635(12) 0.9459(5) 0.0563(11) Uiso 1.000000 GR
H22b H 0.9404(12) 0.3944(3) 0.8929(11) 0.0563(11) Uiso 1.000000 GR
H22c H 0.9607(9) 0.4843(9) 0.8618(7) 0.0563(11) Uiso 1.000000 GR
C23 C 0.5447(3) 0.3716(2) 0.8118(3) 0.0565(10) Uani 1.000000 .
H23a H 0.5350(10) 0.4237(7) 0.8424(16) 0.0848(15) Uiso 1.000000 GR
H23b H 0.5425(9) 0.3767(15) 0.7385(3) 0.0848(15) Uiso 1.000000 GR
H23c H 0.4871(3) 0.3363(8) 0.8337(18) 0.0848(15) Uiso 1.000000 GR


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
Zn1 O3 2.0544(16) . ?
Zn1 O2 2.0794(16) . ?
Zn1 O6 2.2020(17) . ?
Zn1 O7 2.1636(16) 3_766 ?
Zn1 O7 2.0225(15) . ?
Zn1 N3 2.0451(19) . ?
Zn2 O3 2.1654(16) . ?
Zn2 O2 2.0013(16) 3_766 ?
Zn2 O4 2.0122(17) . ?
Zn2 O7 2.0650(16) 3_766 ?
Zn2 N4 2.0202(19) . ?
O3 C10 1.421(3) . ?
O2 C2 1.318(3) . ?
O4 C18 1.302(3) . ?
O6 H6 0.859(9) . ?
O6 C20 1.426(3) . ?
O7 C21 1.418(3) . ?
O1 C3 1.377(3) . ?
O1 C1 1.424(3) . ?
O5 C17 1.371(3) . ?
O5 C19 1.421(3) . ?
N3 C8 1.281(3) . ?
N3 C9 1.461(3) . ?
N4 C12 1.290(3) . ?
N4 C11 1.460(3) . ?
C10 H10 0.9800 . ?
C10 C9 1.541(3) . ?
C10 C11 1.540(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.436(3) . ?
C2 C3 1.409(3) . ?
C2 C7 1.418(3) . ?
C21 H21a 0.9600 . ?
C21 H21b 0.9600 . ?
C21 H21c 0.9600 . ?
C8 H8 0.9300 . ?
C8 C7 1.456(3) . ?
C18 C17 1.423(3) . ?
C18 C13 1.422(3) . ?
C17 C16 1.377(3) . ?
C9 H9a 0.9700 . ?
C9 H9b 0.9700 . ?
C11 H11a 0.9700 . ?
C11 H11b 0.9700 . ?
C3 C4 1.380(3) . ?
C7 C6 1.414(3) . ?
C16 H16 0.9300 . ?
C16 C15 1.403(4) . ?
C13 C14 1.425(3) . ?
C6 H6a 0.9300 . ?
C6 C5 1.369(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(4) . ?
C15 H15 0.9300 . ?
C15 C14 1.358(4) . ?
C14 H14 0.9300 . ?
C5 H5 0.9300 . ?
C19 H19a 0.9600 . ?
C19 H19b 0.9600 . ?
C19 H19c 0.9600 . ?
C20 H20a 0.9600 . ?
C20 H20b 0.9600 . ?
C20 H20c 0.9600 . ?
C1 H1a 0.9600 . ?
C1 H1b 0.9600 . ?
C1 H1c 0.9600 . ?
O8 H8a 0.8200 . ?
O8 C22 1.415(3) . ?
O9 H9 0.8200 . ?
O9 C23 1.406(4) . ?
C22 H22a 0.9600 . ?
C22 H22b 0.9600 . ?
C22 H22c 0.9600 . ?
C23 H23a 0.9600 . ?
C23 H23b 0.9600 . ?
C23 H23c 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Zn1 O3 166.44(6) . . ?
O6 Zn1 O3 103.99(6) . . ?
O6 Zn1 O2 86.16(6) . . ?
O7 Zn1 O3 106.49(6) . . ?
O7 Zn1 O3 83.63(6) 3_766 . ?
O7 Zn1 O2 82.21(6) . . ?
O7 Zn1 O2 87.42(6) 3_766 . ?
O7 Zn1 O6 89.56(6) . . ?
O7 Zn1 O6 170.02(6) 3_766 . ?
N3 Zn1 O3 83.39(7) . . ?
N3 Zn1 O2 87.05(7) . . ?
N3 Zn1 O6 93.66(7) . . ?
N3 Zn1 O7 168.55(7) . . ?
N3 Zn1 O7 93.63(7) . 3_766 ?
O2 Zn2 O3 99.03(6) 3_766 . ?
O4 Zn2 O3 163.70(6) . . ?
O4 Zn2 O2 95.47(7) . 3_766 ?
O7 Zn2 O3 83.33(6) 3_766 . ?
O7 Zn2 O2 83.08(6) 3_766 3_766 ?
O7 Zn2 O4 91.10(6) 3_766 . ?
N4 Zn2 O3 80.32(7) . . ?
N4 Zn2 O2 152.57(7) . 3_766 ?
N4 Zn2 O4 90.21(7) . . ?
N4 Zn2 O7 123.70(7) . 3_766 ?
Zn2 O3 Zn1 95.79(6) . . ?
C10 O3 Zn1 112.00(13) . . ?
C10 O3 Zn2 108.45(13) . . ?
Zn2 O2 Zn1 96.86(6) 3_766 . ?
C2 O2 Zn1 125.95(14) . . ?
C2 O2 Zn2 127.39(14) . 3_766 ?
C18 O4 Zn2 127.74(15) . . ?
H6 O6 Zn1 114.8(12) . . ?
C20 O6 Zn1 127.24(15) . . ?
C20 O6 H6 106.5(12) . . ?
Zn2 O7 Zn1 96.66(6) 3_766 . ?
Zn2 O7 Zn1 95.53(6) 3_766 3_766 ?
C21 O7 Zn1 118.58(13) . . ?
C21 O7 Zn1 119.50(13) . 3_766 ?
C21 O7 Zn2 122.97(13) . 3_766 ?
C1 O1 C3 117.10(19) . . ?
C19 O5 C17 116.9(2) . . ?
C8 N3 Zn1 127.42(16) . . ?
C9 N3 Zn1 111.33(14) . . ?
C9 N3 C8 121.3(2) . . ?
C12 N4 Zn2 126.05(16) . . ?
C11 N4 Zn2 114.09(14) . . ?
C11 N4 C12 119.8(2) . . ?
H10 C10 O3 108.99(11) . . ?
C9 C10 O3 112.33(18) . . ?
C9 C10 H10 108.99(13) . . ?
C11 C10 O3 108.23(18) . . ?
C11 C10 H10 108.99(12) . . ?
C11 C10 C9 109.26(19) . . ?
H12 C12 N4 116.71(14) . . ?
C13 C12 N4 126.6(2) . . ?
C13 C12 H12 116.71(13) . . ?
C3 C2 O2 118.5(2) . . ?
C7 C2 O2 123.2(2) . . ?
C7 C2 C3 118.3(2) . . ?
H21a C21 O7 109.5 . . ?
H21b C21 O7 109.5 . . ?
H21b C21 H21a 109.5 . . ?
H21c C21 O7 109.5 . . ?
H21c C21 H21a 109.5 . . ?
H21c C21 H21b 109.5 . . ?
H8 C8 N3 117.39(13) . . ?
C7 C8 N3 125.2(2) . . ?
C7 C8 H8 117.39(13) . . ?
C17 C18 O4 118.3(2) . . ?
C13 C18 O4 124.4(2) . . ?
C13 C18 C17 117.3(2) . . ?
C18 C17 O5 113.5(2) . . ?
C16 C17 O5 125.0(2) . . ?
C16 C17 C18 121.5(2) . . ?
C10 C9 N3 110.66(18) . . ?
H9a C9 N3 109.51(12) . . ?
H9a C9 C10 109.51(12) . . ?
H9b C9 N3 109.51(12) . . ?
H9b C9 C10 109.51(13) . . ?
H9b C9 H9a 108.1 . . ?
C10 C11 N4 108.53(18) . . ?
H11a C11 N4 109.99(12) . . ?
H11a C11 C10 109.99(12) . . ?
H11b C11 N4 109.99(12) . . ?
H11b C11 C10 109.99(13) . . ?
H11b C11 H11a 108.4 . . ?
C2 C3 O1 113.2(2) . . ?
C4 C3 O1 125.2(2) . . ?
C4 C3 C2 121.6(2) . . ?
C8 C7 C2 124.4(2) . . ?
C6 C7 C2 118.8(2) . . ?
C6 C7 C8 116.7(2) . . ?
H16 C16 C17 119.86(15) . . ?
C15 C16 C17 120.3(2) . . ?
C15 C16 H16 119.86(15) . . ?
C18 C13 C12 123.7(2) . . ?
C14 C13 C12 116.5(2) . . ?
C14 C13 C18 119.7(2) . . ?
H6a C6 C7 119.36(14) . . ?
C5 C6 C7 121.3(2) . . ?
C5 C6 H6a 119.36(15) . . ?
H4 C4 C3 120.13(15) . . ?
C5 C4 C3 119.7(2) . . ?
C5 C4 H4 120.13(15) . . ?
H15 C15 C16 119.88(15) . . ?
C14 C15 C16 120.2(2) . . ?
C14 C15 H15 119.88(15) . . ?
C15 C14 C13 120.9(2) . . ?
H14 C14 C13 119.56(14) . . ?
H14 C14 C15 119.56(15) . . ?
C4 C5 C6 120.2(2) . . ?
H5 C5 C6 119.88(15) . . ?
H5 C5 C4 119.88(15) . . ?
H19a C19 O5 109.5 . . ?
H19b C19 O5 109.5 . . ?
H19b C19 H19a 109.5 . . ?
H19c C19 O5 109.5 . . ?
H19c C19 H19a 109.5 . . ?
H19c C19 H19b 109.5 . . ?
H20a C20 O6 109.5 . . ?
H20b C20 O6 109.5 . . ?
H20b C20 H20a 109.5 . . ?
H20c C20 O6 109.5 . . ?
H20c C20 H20a 109.5 . . ?
H20c C20 H20b 109.5 . . ?
H1a C1 O1 109.5 . . ?
H1b C1 O1 109.5 . . ?
H1b C1 H1a 109.5 . . ?
H1c C1 O1 109.5 . . ?
H1c C1 H1a 109.5 . . ?
H1c C1 H1b 109.5 . . ?
C22 O8 H8a 109.5 . . ?
C23 O9 H9 109.5 . . ?
H22a C22 O8 109.5 . . ?
H22b C22 O8 109.5 . . ?
H22b C22 H22a 109.5 . . ?
H22c C22 O8 109.5 . . ?
H22c C22 H22a 109.5 . . ?
H22c C22 H22b 109.5 . . ?
H23a C23 O9 109.5 . . ?
H23b C23 O9 109.5 . . ?
H23b C23 H23a 109.5 . . ?
H23c C23 O9 109.5 . . ?
H23c C23 H23a 109.5 . . ?
H23c C23 H23b 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
Zn1 H6 1 2.7599 0.0200 0.0819
O6 H6 1 0.8500 0.0100 -0.0092
C20 H6 1 1.8922 0.0200 0.0302

####################################################################### 
# 
# 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_nide
_database_code_depnum_ccdc_archive 'CCDC 1409533'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-11-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C19 H21 N5 Ni2 O6, 3(C3 H7 N O)'
_chemical_formula_sum            'C28 H42 N8 Ni2 O9'
_chemical_formula_weight         752.11
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.220(2)
_cell_length_b                   12.342(3)
_cell_length_c                   13.322(3)
_cell_angle_alpha                66.12(3)
_cell_angle_beta                 80.13(3)
_cell_angle_gamma                79.10(3)
_cell_volume                     1647.2(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4666
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8944
_cell_measurement_theta_min      2.3835
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8738
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16738
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.903
_diffrn_reflns_theta_min         1.681
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -110.0000 - 70.0000
	     Image width: 1.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0089
	          2theta: -19.9118
scan:
	Number of images: 150
	           Slice: -110.0000 - 40.0000
	     Image width: 1.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0089
	          2theta: -19.9118
scan:
	Number of images: 100
	           Slice: -110.0000 - -10.0000
	     Image width: 1.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0089
	          2theta: -19.9118
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             7730
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0360
_diffrn_orient_matrix_UB_12      -0.0758
_diffrn_orient_matrix_UB_13      -0.0359
_diffrn_orient_matrix_UB_21      -0.0856
_diffrn_orient_matrix_UB_22      -0.0172
_diffrn_orient_matrix_UB_23      -0.0194
_diffrn_orient_matrix_UB_31      0.0348
_diffrn_orient_matrix_UB_32      0.0524
_diffrn_orient_matrix_UB_33      -0.0535
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5540
_reflns_number_total             7728
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         2.795
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7728
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0576
_refine_ls_restrained_S_all      1.060
_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)+(0.1140P)²+1.4270P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1824
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Rigid bond restraints
 N3, N4, N5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim N5: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Rotating group:
 O6(H6A,H6B)
4.b Ternary CH refined with riding coordinates:
 C10(H10)
4.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B)
4.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C16(H16), C12(H12), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15),
 C19(H19), C23(H23), C25(H25)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C38(H38A,H38B,H38C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C24(H24A,
 H24B,H24C)
;
_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
Ni2 Ni 0.12315(4) 0.00940(4) 0.03232(4) 0.01434(14) Uani 1 1 d . . . . .
Ni1 Ni -0.03654(4) -0.18762(4) 0.19593(4) 0.01618(14) Uani 1 1 d . . . . .
O3 O -0.1309(2) -0.1816(2) 0.0730(2) 0.0185(5) Uani 1 1 d . . . . .
O4 O 0.1270(2) -0.1683(2) 0.1094(2) 0.0178(5) Uani 1 1 d . . . . .
O5 O 0.0791(2) -0.3767(2) 0.2471(2) 0.0204(6) Uani 1 1 d . . . . .
O2 O 0.0253(2) -0.1720(2) 0.3218(2) 0.0208(6) Uani 1 1 d . . . . .
O1 O 0.1351(2) -0.1262(3) 0.4540(2) 0.0253(6) Uani 1 1 d . . . . .
N2 N 0.2991(3) -0.0187(3) -0.0211(3) 0.0167(6) Uani 1 1 d . . . . .
N1 N -0.1837(3) -0.2511(3) 0.2916(3) 0.0205(7) Uani 1 1 d . . . . .
C18 C 0.2216(3) -0.2502(3) 0.1369(3) 0.0170(7) Uani 1 1 d . . . . .
C8 C -0.2216(3) -0.2501(3) 0.3880(3) 0.0221(8) Uani 1 1 d . . . . .
H8 H -0.2976 -0.2746 0.4195 0.026 Uiso 1 1 calc R . . . .
C16 C 0.2958(4) -0.4583(4) 0.2428(4) 0.0286(9) Uani 1 1 d . . . . .
H16 H 0.2803 -0.5343 0.2921 0.034 Uiso 1 1 calc R . . . .
C17 C 0.2015(3) -0.3670(3) 0.2124(3) 0.0199(7) Uani 1 1 d . . . . .
C13 C 0.3437(3) -0.2296(3) 0.0936(3) 0.0200(8) Uani 1 1 d . . . . .
C12 C 0.3745(3) -0.1148(4) 0.0111(3) 0.0206(8) Uani 1 1 d . . . . .
H12 H 0.4550 -0.1111 -0.0205 0.025 Uiso 1 1 calc R . . . .
C3 C 0.0197(4) -0.1570(4) 0.4929(3) 0.0235(8) Uani 1 1 d . . . . .
C4 C -0.0399(4) -0.1625(4) 0.5936(3) 0.0288(9) Uani 1 1 d . . . . .
H4 H -0.0013 -0.1457 0.6410 0.035 Uiso 1 1 calc R . . . .
C5 C -0.1592(4) -0.1935(4) 0.6254(3) 0.0315(10) Uani 1 1 d . . . . .
H5 H -0.1994 -0.1971 0.6936 0.038 Uiso 1 1 calc R . . . .
C11 C -0.3365(3) -0.0865(3) 0.1158(3) 0.0208(8) Uani 1 1 d . . . . .
H11A H -0.4204 -0.0937 0.1130 0.025 Uiso 1 1 calc R . . . .
H11B H -0.3322 -0.0768 0.1837 0.025 Uiso 1 1 calc R . . . .
C6 C -0.2153(4) -0.2179(4) 0.5556(3) 0.0275(9) Uani 1 1 d . . . . .
H6 H -0.2943 -0.2374 0.5769 0.033 Uiso 1 1 calc R . . . .
C7 C -0.1568(4) -0.2144(3) 0.4514(3) 0.0229(8) Uani 1 1 d . . . . .
C9 C -0.2562(3) -0.2920(4) 0.2348(3) 0.0232(8) Uani 1 1 d . . . . .
H9A H -0.3394 -0.2953 0.2698 0.028 Uiso 1 1 calc R . . . .
H9B H -0.2212 -0.3710 0.2372 0.028 Uiso 1 1 calc R . . . .
C10 C -0.2535(3) -0.2010(3) 0.1151(3) 0.0189(7) Uani 1 1 d . . . . .
H10 H -0.2861 -0.2330 0.0705 0.023 Uiso 1 1 calc R . . . .
C1 C 0.2021(4) -0.1144(4) 0.5300(4) 0.0302(9) Uani 1 1 d . . . . .
H1A H 0.2830 -0.0987 0.4960 0.045 Uiso 1 1 calc GR . . . .
H1B H 0.2067 -0.1871 0.5946 0.045 Uiso 1 1 calc GR . . . .
H1C H 0.1617 -0.0494 0.5505 0.045 Uiso 1 1 calc GR . . . .
C14 C 0.4392(4) -0.3252(4) 0.1253(4) 0.0303(9) Uani 1 1 d . . . . .
H14 H 0.5189 -0.3124 0.0954 0.036 Uiso 1 1 calc R . . . .
C2 C -0.0363(3) -0.1815(3) 0.4167(3) 0.0207(8) Uani 1 1 d . . . . .
C38 C 0.0475(4) -0.4881(4) 0.3277(4) 0.0370(11) Uani 1 1 d . . . . .
H38A H 0.0826 -0.5058 0.3943 0.056 Uiso 1 1 calc GR . . . .
H38B H 0.0783 -0.5501 0.3003 0.056 Uiso 1 1 calc GR . . . .
H38C H -0.0397 -0.4835 0.3428 0.056 Uiso 1 1 calc GR . . . .
C15 C 0.4165(4) -0.4362(4) 0.1990(4) 0.0352(11) Uani 1 1 d . . . . .
H15 H 0.4808 -0.4975 0.2205 0.042 Uiso 1 1 calc R . . . .
N3 N -0.0582(2) -0.0008(2) 0.1032(2) 0.0112(5) Uani 1 1 d . U . . .
N4 N -0.1166(4) 0.0715(4) 0.1511(3) 0.0350(8) Uani 1 1 d . U . . .
O7 O 0.3571(3) 0.1220(4) 0.1648(3) 0.0544(11) Uani 1 1 d . . . . .
N6 N 0.5034(3) 0.1215(4) 0.2635(4) 0.0364(9) Uani 1 1 d . . . . .
C19 C 0.4234(4) 0.0693(5) 0.2401(5) 0.0409(12) Uani 1 1 d . . . . .
H19 H 0.4173 -0.0110 0.2828 0.049 Uiso 1 1 calc R . . . .
C20 C 0.5198(6) 0.2422(5) 0.2056(6) 0.0632(18) Uani 1 1 d . . . . .
H20A H 0.6017 0.2475 0.1700 0.095 Uiso 1 1 calc GR . . . .
H20B H 0.5057 0.2819 0.2562 0.095 Uiso 1 1 calc GR . . . .
H20C H 0.4632 0.2797 0.1509 0.095 Uiso 1 1 calc GR . . . .
C21 C 0.5741(6) 0.0487(7) 0.3564(5) 0.0668(19) Uani 1 1 d . . . . .
H21A H 0.5612 0.0863 0.4086 0.100 Uiso 1 1 calc GR . . . .
H21B H 0.6592 0.0412 0.3301 0.100 Uiso 1 1 calc GR . . . .
H21C H 0.5482 -0.0292 0.3915 0.100 Uiso 1 1 calc GR . . . .
N7 N 0.3539(3) -0.3520(3) 0.4763(3) 0.0273(8) Uani 1 1 d . . . . .
C22 C 0.2432(4) -0.4057(4) 0.5002(4) 0.0351(10) Uani 1 1 d . . . . .
H22A H 0.1904 -0.3595 0.4436 0.053 Uiso 1 1 calc GR . . . .
H22B H 0.2026 -0.4076 0.5703 0.053 Uiso 1 1 calc GR . . . .
H22C H 0.2631 -0.4858 0.5024 0.053 Uiso 1 1 calc GR . . . .
C23 C 0.3798(4) -0.2663(4) 0.3787(5) 0.0420(12) Uani 1 1 d . . . . .
H23 H 0.3310 -0.2423 0.3216 0.050 Uiso 1 1 calc R . . . .
O8 O 0.4750(4) -0.2188(4) 0.3678(5) 0.0814(15) Uani 1 1 d . . . . .
N8 N -0.1473(5) -0.5878(4) 0.0700(4) 0.0502(12) Uani 1 1 d . . . . .
O9 O -0.2215(6) -0.5782(4) 0.2346(4) 0.0935(19) Uani 1 1 d . . . . .
C25 C -0.1468(6) -0.6135(5) 0.1772(5) 0.0555(15) Uani 1 1 d . . . . .
H25 H -0.0801 -0.6649 0.2104 0.067 Uiso 1 1 calc R . . . .
C26 C -0.2487(7) -0.5141(7) 0.0129(6) 0.0693(19) Uani 1 1 d . . . . .
H26A H -0.3132 -0.4991 0.0650 0.104 Uiso 1 1 calc GR . . . .
H26B H -0.2773 -0.5541 -0.0251 0.104 Uiso 1 1 calc GR . . . .
H26C H -0.2237 -0.4396 -0.0395 0.104 Uiso 1 1 calc GR . . . .
C27 C -0.0471(6) -0.6429(6) 0.0117(6) 0.0628(18) Uani 1 1 d . . . . .
H27A H -0.0036 -0.5818 -0.0443 0.094 Uiso 1 1 calc GR . . . .
H27B H -0.0800 -0.6848 -0.0220 0.094 Uiso 1 1 calc GR . . . .
H27C H 0.0077 -0.6980 0.0633 0.094 Uiso 1 1 calc GR . . . .
C24 C 0.4277(6) -0.3921(10) 0.5623(6) 0.101(3) Uani 1 1 d . . . . .
H24A H 0.3772 -0.4073 0.6313 0.152 Uiso 1 1 calc GR . . . .
H24B H 0.4776 -0.3321 0.5508 0.152 Uiso 1 1 calc GR . . . .
H24C H 0.4789 -0.4644 0.5640 0.152 Uiso 1 1 calc GR . . . .
O6 O 0.1528(3) 0.0247(3) 0.1770(2) 0.0270(6) Uani 1 1 d . . . . .
H6A H 0.2258 0.0418 0.1714 0.040 Uiso 1 1 d GR . . . .
H6B H 0.1450 -0.0421 0.2332 0.040 Uiso 1 1 d GR . . . .
N5 N -0.1659(7) 0.1253(7) 0.1983(6) 0.0910(18) 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
Ni2 O3 2.026(3) 2 ?
Ni2 O4 2.006(3) . ?
Ni2 N2 1.996(3) . ?
Ni2 N3 2.107(3) 2 ?
Ni2 N3 2.095(3) . ?
Ni2 O6 2.097(3) . ?
Ni1 O3 2.067(3) . ?
Ni1 O4 1.993(3) . ?
Ni1 O5 2.338(3) . ?
Ni1 O2 2.010(3) . ?
Ni1 N1 1.981(3) . ?
Ni1 N3 2.118(3) . ?
O3 Ni2 2.026(3) 2 ?
O3 C10 1.420(4) . ?
O4 C18 1.307(4) . ?
O5 C17 1.383(4) . ?
O5 C38 1.424(5) . ?
O2 C2 1.304(5) . ?
O1 C3 1.373(5) . ?
O1 C1 1.426(4) . ?
N2 C12 1.280(5) . ?
N2 C11 1.467(5) 2 ?
N1 C8 1.287(5) . ?
N1 C9 1.470(5) . ?
C18 C17 1.418(5) . ?
C18 C13 1.420(5) . ?
C8 H8 0.9300 . ?
C8 C7 1.438(6) . ?
C16 H16 0.9300 . ?
C16 C17 1.371(5) . ?
C16 C15 1.409(6) . ?
C13 C12 1.459(5) . ?
C13 C14 1.411(5) . ?
C12 H12 0.9300 . ?
C3 C4 1.373(6) . ?
C3 C2 1.433(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.409(6) . ?
C5 H5 0.9300 . ?
C5 C6 1.360(6) . ?
C11 N2 1.467(5) 2 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C10 1.541(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.418(6) . ?
C7 C2 1.431(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.534(6) . ?
C10 H10 0.9800 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C14 H14 0.9300 . ?
C14 C15 1.364(6) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C15 H15 0.9300 . ?
N3 Ni2 2.107(3) 2 ?
N3 N4 1.315(5) . ?
N4 N5 1.106(7) . ?
O7 C19 1.235(7) . ?
N6 C19 1.341(6) . ?
N6 C20 1.405(7) . ?
N6 C21 1.461(7) . ?
C19 H19 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
N7 C22 1.445(5) . ?
N7 C23 1.329(7) . ?
N7 C24 1.398(7) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23 0.9300 . ?
C23 O8 1.273(6) . ?
N8 C25 1.333(7) . ?
N8 C26 1.430(8) . ?
N8 C27 1.473(7) . ?
O9 C25 1.178(8) . ?
C25 H25 0.9300 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
O6 H6A 0.8670 . ?
O6 H6B 0.8672 . ?

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 Ni2 N3 81.85(11) 2 2 ?
O3 Ni2 N3 106.42(11) 2 . ?
O3 Ni2 O6 98.65(11) 2 . ?
O4 Ni2 O3 168.46(10) . 2 ?
O4 Ni2 N3 79.63(11) . . ?
O4 Ni2 N3 89.08(11) . 2 ?
O4 Ni2 O6 91.61(12) . . ?
N2 Ni2 O3 85.47(12) . 2 ?
N2 Ni2 O4 88.21(12) . . ?
N2 Ni2 N3 167.83(12) . . ?
N2 Ni2 N3 94.75(12) . 2 ?
N2 Ni2 O6 96.09(12) . . ?
N3 Ni2 N3 84.64(12) . 2 ?
N3 Ni2 O6 84.84(11) . . ?
O6 Ni2 N3 169.15(11) . 2 ?
O3 Ni1 O5 103.14(10) . . ?
O3 Ni1 N3 80.63(11) . . ?
O4 Ni1 O3 97.77(10) . . ?
O4 Ni1 O5 72.47(10) . . ?
O4 Ni1 O2 90.78(11) . . ?
O4 Ni1 N3 79.35(11) . . ?
O2 Ni1 O3 168.41(10) . . ?
O2 Ni1 O5 86.85(11) . . ?
O2 Ni1 N3 93.36(11) . . ?
N1 Ni1 O3 82.62(12) . . ?
N1 Ni1 O4 165.19(12) . . ?
N1 Ni1 O5 92.97(11) . . ?
N1 Ni1 O2 91.12(13) . . ?
N1 Ni1 N3 115.19(12) . . ?
N3 Ni1 O5 151.82(10) . . ?
Ni2 O3 Ni1 99.91(11) 2 . ?
C10 O3 Ni2 110.6(2) . 2 ?
C10 O3 Ni1 110.1(2) . . ?
Ni1 O4 Ni2 103.70(12) . . ?
C18 O4 Ni2 128.6(2) . . ?
C18 O4 Ni1 122.4(2) . . ?
C17 O5 Ni1 110.6(2) . . ?
C17 O5 C38 118.0(3) . . ?
C38 O5 Ni1 129.2(2) . . ?
C2 O2 Ni1 126.2(2) . . ?
C3 O1 C1 116.6(3) . . ?
C12 N2 Ni2 128.8(3) . . ?
C12 N2 C11 119.8(3) . 2 ?
C11 N2 Ni2 111.2(2) 2 . ?
C8 N1 Ni1 126.9(3) . . ?
C8 N1 C9 121.3(3) . . ?
C9 N1 Ni1 111.5(2) . . ?
O4 C18 C17 118.5(3) . . ?
O4 C18 C13 123.7(3) . . ?
C17 C18 C13 117.8(3) . . ?
N1 C8 H8 117.2 . . ?
N1 C8 C7 125.6(4) . . ?
C7 C8 H8 117.2 . . ?
C17 C16 H16 120.2 . . ?
C17 C16 C15 119.6(4) . . ?
C15 C16 H16 120.2 . . ?
O5 C17 C18 112.6(3) . . ?
C16 C17 O5 125.6(4) . . ?
C16 C17 C18 121.8(3) . . ?
C18 C13 C12 122.6(3) . . ?
C14 C13 C18 119.4(4) . . ?
C14 C13 C12 117.9(3) . . ?
N2 C12 C13 125.0(3) . . ?
N2 C12 H12 117.5 . . ?
C13 C12 H12 117.5 . . ?
O1 C3 C4 124.7(4) . . ?
O1 C3 C2 113.5(3) . . ?
C4 C3 C2 121.8(4) . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.4(4) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.5(4) . . ?
C6 C5 H5 120.2 . . ?
N2 C11 H11A 109.5 2 . ?
N2 C11 H11B 109.5 2 . ?
N2 C11 C10 110.7(3) 2 . ?
H11A C11 H11B 108.1 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C5 C6 H6 119.0 . . ?
C5 C6 C7 122.0(4) . . ?
C7 C6 H6 119.0 . . ?
C6 C7 C8 117.0(4) . . ?
C6 C7 C2 119.4(4) . . ?
C2 C7 C8 123.5(4) . . ?
N1 C9 H9A 110.4 . . ?
N1 C9 H9B 110.4 . . ?
N1 C9 C10 106.5(3) . . ?
H9A C9 H9B 108.6 . . ?
C10 C9 H9A 110.4 . . ?
C10 C9 H9B 110.4 . . ?
O3 C10 C11 112.9(3) . . ?
O3 C10 C9 109.0(3) . . ?
O3 C10 H10 109.2 . . ?
C11 C10 H10 109.2 . . ?
C9 C10 C11 107.2(3) . . ?
C9 C10 H10 109.2 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C13 C14 H14 119.4 . . ?
C15 C14 C13 121.1(4) . . ?
C15 C14 H14 119.4 . . ?
O2 C2 C3 118.2(3) . . ?
O2 C2 C7 125.0(3) . . ?
C7 C2 C3 116.8(4) . . ?
O5 C38 H38A 109.5 . . ?
O5 C38 H38B 109.5 . . ?
O5 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C16 C15 H15 119.9 . . ?
C14 C15 C16 120.3(4) . . ?
C14 C15 H15 119.9 . . ?
Ni2 N3 Ni2 95.36(12) . 2 ?
Ni2 N3 Ni1 95.72(11) 2 . ?
Ni2 N3 Ni1 96.57(12) . . ?
N4 N3 Ni2 122.4(2) . . ?
N4 N3 Ni2 121.2(2) . 2 ?
N4 N3 Ni1 119.3(3) . . ?
N5 N4 N3 174.9(6) . . ?
C19 N6 C20 123.4(5) . . ?
C19 N6 C21 117.6(5) . . ?
C20 N6 C21 119.0(5) . . ?
O7 C19 N6 123.6(5) . . ?
O7 C19 H19 118.2 . . ?
N6 C19 H19 118.2 . . ?
N6 C20 H20A 109.5 . . ?
N6 C20 H20B 109.5 . . ?
N6 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N6 C21 H21A 109.5 . . ?
N6 C21 H21B 109.5 . . ?
N6 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 N7 C22 120.8(4) . . ?
C23 N7 C24 122.9(5) . . ?
C24 N7 C22 116.3(5) . . ?
N7 C22 H22A 109.5 . . ?
N7 C22 H22B 109.5 . . ?
N7 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N7 C23 H23 121.8 . . ?
O8 C23 N7 116.3(6) . . ?
O8 C23 H23 121.8 . . ?
C25 N8 C26 120.5(5) . . ?
C25 N8 C27 119.8(5) . . ?
C26 N8 C27 119.6(5) . . ?
N8 C25 H25 116.4 . . ?
O9 C25 N8 127.2(7) . . ?
O9 C25 H25 116.4 . . ?
N8 C26 H26A 109.5 . . ?
N8 C26 H26B 109.5 . . ?
N8 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N8 C27 H27A 109.5 . . ?
N8 C27 H27B 109.5 . . ?
N8 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N7 C24 H24A 109.5 . . ?
N7 C24 H24B 109.5 . . ?
N7 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Ni2 O6 H6A 110.5 . . ?
Ni2 O6 H6B 110.3 . . ?
H6A O6 H6B 108.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni2 O3 C10 C11 -26.2(4) 2 . . . ?
Ni2 O3 C10 C9 -145.3(2) 2 . . . ?
Ni2 O4 C18 C17 165.9(2) . . . . ?
Ni2 O4 C18 C13 -15.4(5) . . . . ?
Ni2 N2 C12 C13 3.1(5) . . . . ?
Ni1 O3 C10 C11 83.3(3) . . . . ?
Ni1 O3 C10 C9 -35.8(3) . . . . ?
Ni1 O4 C18 C17 16.2(4) . . . . ?
Ni1 O4 C18 C13 -165.2(3) . . . . ?
Ni1 O5 C17 C18 -12.2(4) . . . . ?
Ni1 O5 C17 C16 169.5(3) . . . . ?
Ni1 O2 C2 C3 -174.5(2) . . . . ?
Ni1 O2 C2 C7 5.3(5) . . . . ?
Ni1 N1 C8 C7 -7.5(6) . . . . ?
Ni1 N1 C9 C10 -39.5(3) . . . . ?
O4 C18 C17 O5 -0.1(5) . . . . ?
O4 C18 C17 C16 178.2(4) . . . . ?
O4 C18 C13 C12 -2.0(6) . . . . ?
O4 C18 C13 C14 -177.5(4) . . . . ?
O1 C3 C4 C5 179.0(4) . . . . ?
O1 C3 C2 O2 -0.2(5) . . . . ?
O1 C3 C2 C7 179.9(3) . . . . ?
N2 C11 C10 O3 34.2(4) 2 . . . ?
N2 C11 C10 C9 154.2(3) 2 . . . ?
N1 C8 C7 C6 179.0(4) . . . . ?
N1 C8 C7 C2 -3.8(6) . . . . ?
N1 C9 C10 O3 49.2(4) . . . . ?
N1 C9 C10 C11 -73.3(3) . . . . ?
C18 C13 C12 N2 8.4(6) . . . . ?
C18 C13 C14 C15 -1.9(6) . . . . ?
C8 N1 C9 C10 135.3(4) . . . . ?
C8 C7 C2 O2 4.9(6) . . . . ?
C8 C7 C2 C3 -175.3(3) . . . . ?
C17 C18 C13 C12 176.7(3) . . . . ?
C17 C18 C13 C14 1.1(5) . . . . ?
C17 C16 C15 C14 -1.2(7) . . . . ?
C13 C18 C17 O5 -178.8(3) . . . . ?
C13 C18 C17 C16 -0.5(6) . . . . ?
C13 C14 C15 C16 1.9(7) . . . . ?
C12 C13 C14 C15 -177.6(4) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
C4 C3 C2 O2 178.6(4) . . . . ?
C4 C3 C2 C7 -1.2(6) . . . . ?
C4 C5 C6 C7 0.6(6) . . . . ?
C5 C6 C7 C8 175.7(4) . . . . ?
C5 C6 C7 C2 -1.6(6) . . . . ?
C11 N2 C12 C13 -171.1(3) 2 . . . ?
C6 C7 C2 O2 -178.0(4) . . . . ?
C6 C7 C2 C3 1.8(5) . . . . ?
C9 N1 C8 C7 178.6(3) . . . . ?
C1 O1 C3 C4 8.4(6) . . . . ?
C1 O1 C3 C2 -172.8(3) . . . . ?
C14 C13 C12 N2 -175.9(4) . . . . ?
C2 C3 C4 C5 0.3(6) . . . . ?
C38 O5 C17 C18 -176.7(4) . . . . ?
C38 O5 C17 C16 5.0(6) . . . . ?
C15 C16 C17 O5 178.6(4) . . . . ?
C15 C16 C17 C18 0.5(6) . . . . ?
C20 N6 C19 O7 0.7(8) . . . . ?
C21 N6 C19 O7 178.8(5) . . . . ?
C22 N7 C23 O8 175.5(4) . . . . ?
C26 N8 C25 O9 -3.0(11) . . . . ?
C27 N8 C25 O9 -178.4(7) . . . . ?
C24 N7 C23 O8 -2.0(8) . . . . ?

_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_p150406a_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1409534'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-11-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H46 Cd3 N4 O14, C H4 O, C H3 O'
_chemical_formula_sum            'C44 H53 Cd3 N4 O16'
_chemical_formula_weight         1231.10
_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 0.0033 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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.9377(5)
_cell_length_b                   15.2966(4)
_cell_length_c                   21.3004(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.035(3)
_cell_angle_gamma                90.00
_cell_volume                     4908.9(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13599
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8490
_cell_measurement_theta_min      3.4350
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2468
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8629
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.99
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       ?
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                7794
_reflns_number_total             8629
_reflns_threshold_expression     >2sigma(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  'ShelXH-1997 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8629
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0326
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0270P)²+9.2077P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0764
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C29(H29), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B), C30(H30A,H30B), C28(H28A,H28B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C4(H4), C5(H5), C15(H15), C16(H16), C12(H12), C23(H23),
 C35(H35), C27(H27), C8(H8A), C31(H31), C33(H33), C24(H24), C25(H25), C34(H34)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C43(H43A,
 H43B,H43C)
2.e Idealised tetrahedral OH refined as rotating group:
 O8(H8), O15(H15A), O3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Cd1 Cd 0.971487(16) 0.487216(17) 0.209348(12) 0.01666(7) Uani 1 d . . .
Cd2 Cd 1.171120(17) 0.404248(17) 0.185085(13) 0.02009(8) Uani 1 d . . .
Cd3 Cd 0.773202(17) 0.549740(18) 0.243272(13) 0.02272(8) Uani 1 d . . .
O2 O 1.12121(16) 0.47856(16) 0.25777(12) 0.0209(5) Uani 1 d . . .
O4 O 1.02264(16) 0.39704(15) 0.14548(12) 0.0200(5) Uani 1 d . . .
O10 O 1.00035(17) 0.33799(16) 0.27849(12) 0.0230(6) Uani 1 d . . .
O1 O 1.04328(16) 0.59098(16) 0.31079(11) 0.0204(5) Uani 1 d . . .
O9 O 0.88907(16) 0.45933(16) 0.27632(12) 0.0204(5) Uani 1 d . . .
O6 O 0.98246(18) 0.59949(16) 0.12494(12) 0.0252(6) Uani 1 d . . .
O5 O 0.85727(17) 0.44233(17) 0.09778(12) 0.0246(6) Uani 1 d . . .
O7 O 0.87038(16) 0.59624(16) 0.19147(12) 0.0205(5) Uani 1 d . . .
N3 N 0.7964(2) 0.5594(2) 0.35508(17) 0.0321(8) Uani 1 d . . .
O12 O 1.2239(2) 0.53144(18) 0.15657(16) 0.0374(7) Uani 1 d . . .
C3 C 1.1210(2) 0.5562(2) 0.35283(17) 0.0180(7) Uani 1 d . . .
N2 N 1.1574(2) 0.2636(2) 0.14748(16) 0.0254(7) Uani 1 d . . .
C1 C 0.9986(3) 0.6531(3) 0.33872(19) 0.0261(9) Uani 1 d . . .
H1A H 0.9456 0.6726 0.3051 0.039 Uiso 1 calc . . GR
H1B H 1.0370 0.7021 0.3556 0.039 Uiso 1 calc . . GR
H1C H 0.9833 0.6262 0.3742 0.039 Uiso 1 calc . . GR
C13 C 0.9983(3) 0.2642(2) 0.07992(17) 0.0212(8) Uani 1 d . . .
O13 O 0.6191(2) 0.5153(2) 0.22933(16) 0.0440(8) Uani 1 d . . .
O11 O 1.2869(2) 0.4194(2) 0.12677(18) 0.0506(9) Uani 1 d . . .
C6 C 1.2800(3) 0.4815(2) 0.42716(18) 0.0255(9) Uani 1 d . . .
H6 H 1.3335 0.4566 0.4526 0.031 Uiso 1 calc . . R
C22 C 0.9388(2) 0.6771(2) 0.12715(17) 0.0221(8) Uani 1 d . . .
O8 O 0.8109(2) 0.7530(2) 0.37205(17) 0.0530(9) Uani 1 d . . .
H8 H 0.8072 0.8019 0.3556 0.080 Uiso 1 calc . . GR
N1 N 1.2777(2) 0.3614(2) 0.27806(17) 0.0309(8) Uani 1 d . . .
C2 C 1.1613(2) 0.4952(2) 0.32055(17) 0.0170(7) Uani 1 d . . .
C7 C 1.2427(2) 0.4569(2) 0.35980(18) 0.0209(8) Uani 1 d . . .
N4 N 0.7436(2) 0.6953(2) 0.23674(17) 0.0301(8) Uani 1 d . . .
O14 O 0.6923(2) 0.4330(2) 0.18070(15) 0.0422(8) Uani 1 d . . .
C21 C 0.8800(2) 0.6717(2) 0.16494(17) 0.0206(8) Uani 1 d . . .
C37 C 0.9285(2) 0.4236(2) 0.33494(17) 0.0202(8) Uani 1 d . . .
C14 C 0.9359(3) 0.2138(2) 0.03143(18) 0.0255(9) Uani 1 d . . .
H14 H 0.9540 0.1608 0.0187 0.031 Uiso 1 calc . . R
C4 C 1.1585(3) 0.5787(2) 0.41846(17) 0.0222(8) Uani 1 d . . .
H4 H 1.1304 0.6186 0.4378 0.027 Uiso 1 calc . . R
C5 C 1.2396(3) 0.5410(3) 0.45608(19) 0.0284(9) Uani 1 d . . .
H5 H 1.2658 0.5563 0.5004 0.034 Uiso 1 calc . . R
C17 C 0.8800(2) 0.3674(2) 0.07151(17) 0.0200(8) Uani 1 d . . .
C36 C 0.9919(3) 0.3565(2) 0.33906(18) 0.0234(8) Uani 1 d . . .
C39 C 1.2812(3) 0.5007(3) 0.13489(19) 0.0295(9) Uani 1 d . . .
C32 C 0.9136(3) 0.4484(3) 0.39491(19) 0.0276(9) Uani 1 d . . .
C15 C 0.8500(3) 0.2394(3) 0.00235(19) 0.0295(9) Uani 1 d . . .
H15 H 0.8108 0.2055 -0.0306 0.035 Uiso 1 calc . . R
C18 C 0.9707(2) 0.3444(2) 0.10047(16) 0.0177(7) Uani 1 d . . .
C16 C 0.8219(3) 0.3180(3) 0.02310(18) 0.0257(8) Uani 1 d . . .
H16 H 0.7635 0.3366 0.0038 0.031 Uiso 1 calc . . R
C12 C 1.0876(3) 0.2285(2) 0.10675(19) 0.0253(9) Uani 1 d . . .
H12 H 1.0951 0.1725 0.0924 0.030 Uiso 1 calc . . R
O15 O 0.6444(2) 0.6896(3) -0.05701(16) 0.0561(10) Uani 1 d . . .
H15A H 0.6566 0.6469 -0.0757 0.084 Uiso 1 calc . . GR
C23 C 0.9503(3) 0.7535(3) 0.09663(19) 0.0293(9) Uani 1 d . . .
H23 H 0.9879 0.7543 0.0711 0.035 Uiso 1 calc . . R
O3 O 1.2345(2) 0.1835(2) 0.2749(2) 0.0562(10) Uani 1 d . . .
H3 H 1.2564 0.1409 0.2978 0.084 Uiso 1 calc . . GR
C35 C 1.0387(3) 0.3172(3) 0.3984(2) 0.0334(10) Uani 1 d . . .
H35 H 1.0799 0.2737 0.3994 0.040 Uiso 1 calc . . R
C27 C 0.7728(3) 0.7554(3) 0.2082(2) 0.0312(10) Uani 1 d . . .
H27 H 0.7517 0.8113 0.2115 0.037 Uiso 1 calc . . R
C8 C 1.2919(2) 0.3916(3) 0.3368(2) 0.0272(9) Uani 1 d . . .
H8A H 1.3409 0.3682 0.3694 0.033 Uiso 1 calc . . R
C26 C 0.8350(2) 0.7489(2) 0.17124(19) 0.0252(9) Uani 1 d . . .
C11 C 1.2394(3) 0.2118(3) 0.1658(2) 0.0346(10) Uani 1 d . . .
H11A H 1.2775 0.2350 0.1423 0.041 Uiso 1 calc . . R
H11B H 1.2245 0.1522 0.1508 0.041 Uiso 1 calc . . R
C41 C 0.6218(3) 0.4509(3) 0.1935(2) 0.0339(10) Uani 1 d . . .
C31 C 0.8509(3) 0.5143(3) 0.4008(2) 0.0301(10) Uani 1 d . . .
H31 H 0.8504 0.5249 0.4436 0.036 Uiso 1 calc . . R
C40 C 1.3470(3) 0.5608(3) 0.1205(2) 0.0334(10) Uani 1 d . . .
H40A H 1.3221 0.6185 0.1115 0.050 Uiso 1 calc . . GR
H40B H 1.3607 0.5398 0.0825 0.050 Uiso 1 calc . . GR
H40C H 1.4002 0.5628 0.1582 0.050 Uiso 1 calc . . GR
C33 C 0.9627(3) 0.4058(3) 0.4544(2) 0.0384(11) Uani 1 d . . .
H33 H 0.9527 0.4215 0.4935 0.046 Uiso 1 calc . . R
C9 C 1.3380(3) 0.2936(3) 0.2688(2) 0.0416(11) Uani 1 d . . .
H9A H 1.3815 0.2800 0.3116 0.050 Uiso 1 calc . . R
H9B H 1.3697 0.3165 0.2404 0.050 Uiso 1 calc . . R
C30 C 0.7359(3) 0.6188(3) 0.3757(2) 0.0428(12) Uani 1 d . . .
H30A H 0.7570 0.6225 0.4238 0.051 Uiso 1 calc . . R
H30B H 0.6775 0.5923 0.3625 0.051 Uiso 1 calc . . R
C38 C 1.0607(3) 0.2688(3) 0.2771(2) 0.0360(10) Uani 1 d . . .
H38A H 1.0589 0.2590 0.2322 0.054 Uiso 1 calc . . GR
H38B H 1.0436 0.2162 0.2944 0.054 Uiso 1 calc . . GR
H38C H 1.1198 0.2848 0.3037 0.054 Uiso 1 calc . . GR
C20 C 1.0205(3) 0.5904(3) 0.0730(2) 0.0435(12) Uani 1 d . . .
H20A H 1.0723 0.6267 0.0825 0.065 Uiso 1 calc . . GR
H20B H 0.9779 0.6079 0.0315 0.065 Uiso 1 calc . . GR
H20C H 1.0368 0.5305 0.0701 0.065 Uiso 1 calc . . GR
C19 C 0.7742(3) 0.4818(3) 0.0621(2) 0.0432(12) Uani 1 d . . .
H19A H 0.7269 0.4420 0.0602 0.065 Uiso 1 calc . . GR
H19B H 0.7730 0.4955 0.0178 0.065 Uiso 1 calc . . GR
H19C H 0.7669 0.5345 0.0842 0.065 Uiso 1 calc . . GR
C28 C 0.6849(3) 0.7221(3) 0.2735(2) 0.0400(11) Uani 1 d . . .
H28A H 0.6308 0.6879 0.2584 0.048 Uiso 1 calc . . R
H28B H 0.6691 0.7830 0.2640 0.048 Uiso 1 calc . . R
C24 C 0.9064(3) 0.8289(3) 0.1037(2) 0.0350(10) Uani 1 d . . .
H24 H 0.9151 0.8806 0.0836 0.042 Uiso 1 calc . . R
C25 C 0.8501(3) 0.8270(3) 0.1405(2) 0.0326(10) Uani 1 d . . .
H25 H 0.8211 0.8780 0.1454 0.039 Uiso 1 calc . . R
C34 C 1.0242(3) 0.3428(3) 0.4568(2) 0.0420(11) Uani 1 d . . .
H34 H 1.0562 0.3171 0.4971 0.050 Uiso 1 calc . . R
C42 C 0.5428(3) 0.3927(3) 0.1677(3) 0.0466(12) Uani 1 d . . .
H42A H 0.5600 0.3395 0.1513 0.070 Uiso 1 calc . . GR
H42B H 0.4981 0.4218 0.1324 0.070 Uiso 1 calc . . GR
H42C H 0.5196 0.3794 0.2029 0.070 Uiso 1 calc . . GR
C29 C 0.7267(3) 0.7106(3) 0.3480(2) 0.0446(12) Uani 1 d . . .
H29 H 0.6880 0.7417 0.3680 0.053 Uiso 1 calc . . R
C10 C 1.2904(3) 0.2103(3) 0.2383(2) 0.0386(11) Uani 1 d . . .
H10 H 1.3361 0.1652 0.2449 0.046 Uiso 1 calc . . R
C44 C 1.0493(4) 0.0217(4) 0.1906(3) 0.0629(16) Uani 1 d . . .
H44A H 1.0406 0.0131 0.1442 0.094 Uiso 1 calc . . GR
H44B H 1.0515 -0.0341 0.2118 0.094 Uiso 1 calc . . GR
H44C H 1.1042 0.0522 0.2108 0.094 Uiso 1 calc . . GR
O16 O 0.9834(4) 0.0679(4) 0.1974(4) 0.144(3) Uani 1 d . . .
C43 C 0.7188(6) 0.7142(4) -0.0038(3) 0.116(4) Uani 1 d . . .
H43A H 0.7001 0.7452 0.0285 0.175 Uiso 1 calc . . GR
H43B H 0.7562 0.7513 -0.0197 0.175 Uiso 1 calc . . GR
H43C H 0.7513 0.6629 0.0162 0.175 Uiso 1 calc . . GR


_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 O2 2.274(2) . ?
Cd1 O4 2.267(2) . ?
Cd1 O1 2.624(2) . ?
Cd1 O9 2.273(2) . ?
Cd1 O6 2.533(2) . ?
Cd1 O5 2.571(2) . ?
Cd1 O7 2.263(2) . ?
Cd2 O2 2.264(2) . ?
Cd2 O4 2.241(2) . ?
Cd2 O12 2.279(3) . ?
Cd2 N2 2.281(3) . ?
Cd2 O11 2.549(3) . ?
Cd2 N1 2.245(3) . ?
Cd3 O9 2.229(2) . ?
Cd3 O7 2.288(2) . ?
Cd3 N3 2.293(3) . ?
Cd3 O13 2.433(3) . ?
Cd3 N4 2.270(3) . ?
Cd3 O14 2.346(3) . ?
Cd3 C41 2.749(4) . ?
O2 C2 1.305(4) . ?
O4 C18 1.317(4) . ?
O10 C36 1.369(4) . ?
O10 C38 1.437(4) . ?
O1 C3 1.377(4) . ?
O1 C1 1.427(4) . ?
O9 C37 1.319(4) . ?
O6 C22 1.385(4) . ?
O6 C20 1.431(5) . ?
O5 C17 1.375(4) . ?
O5 C19 1.428(5) . ?
O7 C21 1.316(4) . ?
N3 C31 1.276(5) . ?
N3 C30 1.491(5) . ?
O12 C39 1.243(5) . ?
C3 C2 1.430(5) . ?
C3 C4 1.373(5) . ?
N2 C12 1.284(5) . ?
N2 C11 1.469(5) . ?
C13 C14 1.408(5) . ?
C13 C18 1.420(5) . ?
C13 C12 1.456(5) . ?
O13 C41 1.256(5) . ?
O11 C39 1.262(5) . ?
C6 C7 1.413(5) . ?
C6 C5 1.371(6) . ?
C22 C21 1.423(5) . ?
C22 C23 1.379(5) . ?
O8 C29 1.427(6) . ?
N1 C8 1.283(5) . ?
N1 C9 1.470(5) . ?
C2 C7 1.420(5) . ?
C7 C8 1.450(5) . ?
N4 C27 1.272(5) . ?
N4 C28 1.461(5) . ?
O14 C41 1.268(5) . ?
C21 C26 1.410(5) . ?
C37 C36 1.424(5) . ?
C37 C32 1.424(5) . ?
C14 C15 1.364(6) . ?
C4 C5 1.403(5) . ?
C17 C18 1.418(5) . ?
C17 C16 1.367(5) . ?
C36 C35 1.378(5) . ?
C39 C40 1.500(5) . ?
C32 C31 1.453(6) . ?
C32 C33 1.412(6) . ?
C15 C16 1.404(5) . ?
O15 C43 1.399(7) . ?
C23 C24 1.383(6) . ?
O3 C10 1.423(5) . ?
C35 C34 1.395(6) . ?
C27 C26 1.456(6) . ?
C26 C25 1.420(6) . ?
C11 C10 1.492(6) . ?
C41 C42 1.493(6) . ?
C33 C34 1.364(6) . ?
C9 C10 1.517(6) . ?
C30 C29 1.513(7) . ?
C28 C29 1.516(7) . ?
C24 C25 1.372(6) . ?
C44 O16 1.312(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cd1 O1 63.28(8) . . ?
O2 Cd1 O6 93.23(9) . . ?
O2 Cd1 O5 136.52(8) . . ?
O4 Cd1 O2 72.98(8) . . ?
O4 Cd1 O1 135.77(8) . . ?
O4 Cd1 O9 131.07(9) . . ?
O4 Cd1 O6 82.24(8) . . ?
O4 Cd1 O5 64.39(8) . . ?
O9 Cd1 O2 116.12(9) . . ?
O9 Cd1 O1 77.45(8) . . ?
O9 Cd1 O6 139.51(8) . . ?
O9 Cd1 O5 98.64(8) . . ?
O6 Cd1 O1 93.55(8) . . ?
O6 Cd1 O5 73.56(9) . . ?
O5 Cd1 O1 155.48(8) . . ?
O7 Cd1 O2 134.71(9) . . ?
O7 Cd1 O4 136.29(9) . . ?
O7 Cd1 O1 77.77(8) . . ?
O7 Cd1 O9 73.64(9) . . ?
O7 Cd1 O6 65.87(8) . . ?
O7 Cd1 O5 77.92(8) . . ?
O2 Cd2 O12 89.78(10) . . ?
O2 Cd2 N2 134.32(10) . . ?
O2 Cd2 O11 139.39(10) . . ?
O4 Cd2 O2 73.66(8) . . ?
O4 Cd2 O12 112.20(10) . . ?
O4 Cd2 N2 81.53(10) . . ?
O4 Cd2 O11 131.64(11) . . ?
O4 Cd2 N1 136.03(11) . . ?
O12 Cd2 N2 135.49(11) . . ?
O12 Cd2 O11 53.38(10) . . ?
N2 Cd2 O11 85.23(10) . . ?
N1 Cd2 O2 82.92(10) . . ?
N1 Cd2 O12 104.21(12) . . ?
N1 Cd2 N2 89.59(12) . . ?
N1 Cd2 O11 89.83(12) . . ?
O9 Cd3 O7 73.97(9) . . ?
O9 Cd3 N3 82.86(11) . . ?
O9 Cd3 O13 127.12(10) . . ?
O9 Cd3 N4 139.63(11) . . ?
O9 Cd3 O14 87.28(10) . . ?
O9 Cd3 C41 108.24(11) . . ?
O7 Cd3 N3 125.13(10) . . ?
O7 Cd3 O13 145.41(10) . . ?
O7 Cd3 O14 107.19(10) . . ?
O7 Cd3 C41 129.16(11) . . ?
N3 Cd3 O13 87.44(11) . . ?
N3 Cd3 O14 120.80(12) . . ?
N3 Cd3 C41 105.09(12) . . ?
O13 Cd3 C41 27.18(12) . . ?
N4 Cd3 O7 79.96(10) . . ?
N4 Cd3 N3 87.72(13) . . ?
N4 Cd3 O13 91.32(11) . . ?
N4 Cd3 O14 130.27(12) . . ?
N4 Cd3 C41 112.12(13) . . ?
O14 Cd3 O13 54.57(11) . . ?
O14 Cd3 C41 27.39(12) . . ?
Cd2 O2 Cd1 105.66(9) . . ?
C2 O2 Cd1 123.0(2) . . ?
C2 O2 Cd2 129.4(2) . . ?
Cd2 O4 Cd1 106.64(10) . . ?
C18 O4 Cd1 123.0(2) . . ?
C18 O4 Cd2 129.8(2) . . ?
C36 O10 C38 116.3(3) . . ?
C3 O1 Cd1 111.1(2) . . ?
C3 O1 C1 116.8(3) . . ?
C1 O1 Cd1 127.1(2) . . ?
Cd3 O9 Cd1 105.91(10) . . ?
C37 O9 Cd1 118.5(2) . . ?
C37 O9 Cd3 130.2(2) . . ?
C22 O6 Cd1 113.9(2) . . ?
C22 O6 C20 117.0(3) . . ?
C20 O6 Cd1 128.9(2) . . ?
C17 O5 Cd1 113.4(2) . . ?
C17 O5 C19 117.2(3) . . ?
C19 O5 Cd1 129.3(2) . . ?
Cd1 O7 Cd3 104.27(10) . . ?
C21 O7 Cd1 122.9(2) . . ?
C21 O7 Cd3 132.2(2) . . ?
C31 N3 Cd3 126.6(3) . . ?
C31 N3 C30 116.7(3) . . ?
C30 N3 Cd3 116.4(3) . . ?
C39 O12 Cd2 99.0(2) . . ?
O1 C3 C2 112.9(3) . . ?
C4 C3 O1 124.5(3) . . ?
C4 C3 C2 122.6(3) . . ?
C12 N2 Cd2 126.5(3) . . ?
C12 N2 C11 117.0(3) . . ?
C11 N2 Cd2 116.1(2) . . ?
C14 C13 C18 118.9(4) . . ?
C14 C13 C12 116.7(3) . . ?
C18 C13 C12 124.4(3) . . ?
C41 O13 Cd3 90.6(3) . . ?
C39 O11 Cd2 85.8(2) . . ?
C5 C6 C7 122.0(4) . . ?
O6 C22 C21 113.7(3) . . ?
C23 C22 O6 124.4(3) . . ?
C23 C22 C21 122.0(4) . . ?
C8 N1 Cd2 126.7(3) . . ?
C8 N1 C9 118.0(3) . . ?
C9 N1 Cd2 115.3(3) . . ?
O2 C2 C3 118.2(3) . . ?
O2 C2 C7 124.8(3) . . ?
C7 C2 C3 117.0(3) . . ?
C6 C7 C2 119.2(3) . . ?
C6 C7 C8 115.6(3) . . ?
C2 C7 C8 125.2(3) . . ?
C27 N4 Cd3 129.6(3) . . ?
C27 N4 C28 116.8(4) . . ?
C28 N4 Cd3 113.5(3) . . ?
C41 O14 Cd3 94.3(3) . . ?
O7 C21 C22 118.9(3) . . ?
O7 C21 C26 124.0(3) . . ?
C26 C21 C22 117.1(3) . . ?
O9 C37 C36 117.8(3) . . ?
O9 C37 C32 124.9(3) . . ?
C36 C37 C32 117.3(3) . . ?
C15 C14 C13 122.7(4) . . ?
C3 C4 C5 119.5(3) . . ?
C6 C5 C4 119.7(4) . . ?
O5 C17 C18 113.4(3) . . ?
C16 C17 O5 124.3(3) . . ?
C16 C17 C18 122.4(3) . . ?
O10 C36 C37 112.1(3) . . ?
O10 C36 C35 125.7(4) . . ?
C35 C36 C37 122.1(4) . . ?
O12 C39 O11 121.2(4) . . ?
O12 C39 C40 119.4(4) . . ?
O11 C39 C40 119.3(4) . . ?
C37 C32 C31 125.6(4) . . ?
C33 C32 C37 118.5(4) . . ?
C33 C32 C31 116.0(4) . . ?
C14 C15 C16 118.6(4) . . ?
O4 C18 C13 124.6(3) . . ?
O4 C18 C17 118.3(3) . . ?
C17 C18 C13 117.0(3) . . ?
C17 C16 C15 120.2(4) . . ?
N2 C12 C13 129.0(3) . . ?
C22 C23 C24 120.4(4) . . ?
C36 C35 C34 119.9(4) . . ?
N4 C27 C26 128.9(4) . . ?
N1 C8 C7 129.4(4) . . ?
C21 C26 C27 124.4(4) . . ?
C21 C26 C25 119.5(4) . . ?
C25 C26 C27 116.0(4) . . ?
N2 C11 C10 114.9(3) . . ?
O13 C41 Cd3 62.2(2) . . ?
O13 C41 O14 120.5(4) . . ?
O13 C41 C42 120.0(4) . . ?
O14 C41 Cd3 58.3(2) . . ?
O14 C41 C42 119.5(4) . . ?
C42 C41 Cd3 176.7(3) . . ?
N3 C31 C32 128.8(4) . . ?
C34 C33 C32 122.8(4) . . ?
N1 C9 C10 113.1(3) . . ?
N3 C30 C29 116.1(4) . . ?
N4 C28 C29 112.9(4) . . ?
C25 C24 C23 119.5(4) . . ?
C24 C25 C26 121.5(4) . . ?
C33 C34 C35 119.4(4) . . ?
O8 C29 C30 108.8(4) . . ?
O8 C29 C28 111.4(4) . . ?
C30 C29 C28 118.0(4) . . ?
O3 C10 C11 110.2(4) . . ?
O3 C10 C9 108.8(4) . . ?
C11 C10 C9 117.3(4) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 19 1 ' '
2 0.000 0.000 0.500 154 19 ' '
3 0.500 0.500 1.000 154 19 ' '
4 0.500 0.500 0.500 19 1 ' '
_platon_squeeze_details          ?
####################################################################### 
# 
# 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_cdde_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1409535'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-11-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C42 H42 Br4 Cd3 N4 O14, C H4 O'
_chemical_formula_sum            'C43 H46 Br4 Cd3 N4 O15'
_chemical_formula_weight         1515.68
_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 0.0033 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'
Br Br -0.2901 2.4595 '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'
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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   16.133(3)
_cell_length_b                   15.107(3)
_cell_length_c                   24.295(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.57(2)
_cell_angle_gamma                90.00
_cell_volume                     5296(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_exptl_absorpt_coefficient_mu    4.277
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            9321
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.85
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                7581
_reflns_number_total             9321
_reflns_threshold_expression     >2sigma(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    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9321
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0348
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0326P)²+5.1856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0805
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: Br7(0.5) Br1(0.5)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C9(H9a,H9b), C11(H11a,H11b), C30(H30a,H30b)
3.c Aromatic/amide H refined with riding coordinates:
 C16(H16), C35(H35), C23(H23), C25(H25), C6(H6), C8(H8a), C27(H27), C4(H4),
 C14(H14), C12(H12), C31(H31), C33(H33)
3.d Idealised Me refined as rotating group:
 C40(H40a,H40b,H40c), C38(H38a,H38b,H38c), C42(H42a,H42b,H42c), C20(H20a,H20b,
 H20c), C19(H19a,H19b,H19c), C1(H1a,H1b,H1c), C43(Ha,Hb,Hc)
3.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O8(H8), O15(H)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Cd1 Cd -0.77050(2) -0.51223(2) -0.795754(14) 0.01523(9) Uani 1 d . . .
Cd2 Cd -0.54040(2) -0.57163(2) -0.770337(16) 0.02050(9) Uani 1 d . . .
Cd3 Cd -0.99977(2) -0.45020(2) -0.817955(16) 0.02279(9) Uani 1 d . . .
Br3 Br -0.85145(4) -0.15876(3) -1.02155(2) 0.03333(14) Uani 1 d . . .
Br2 Br -0.55394(4) -0.32611(4) -0.49259(2) 0.03741(14) Uani 1 d . . .
Br4 Br -0.73722(4) -0.63098(4) -0.48913(2) 0.04174(15) Uani 1 d . . .
Br7 Br -0.8843(5) -0.9624(6) -0.9243(3) 0.0308(10) Uani 0.50 d . . .
O10 O -0.7217(2) -0.6170(2) -0.70017(13) 0.0201(7) Uani 1 d . . .
O2 O -0.6898(2) -0.62003(19) -0.81489(13) 0.0188(7) Uani 1 d . . .
O4 O -0.6182(2) -0.48005(19) -0.73644(13) 0.0189(7) Uani 1 d . . .
O6 O -0.7760(2) -0.4562(2) -0.89628(14) 0.0277(8) Uani 1 d . . .
O7 O -0.8942(2) -0.42661(19) -0.85311(13) 0.0191(7) Uani 1 d . . .
O5 O -0.7338(2) -0.3668(2) -0.73111(14) 0.0219(7) Uani 1 d . . .
O3 O -0.4233(3) -0.7623(2) -0.63849(17) 0.0364(9) Uani 1 d . . .
H3 H -0.4425 -0.8116 -0.6524 0.055 Uiso 1 calc . . GR
O9 O -0.8667(2) -0.5168(2) -0.75080(14) 0.0222(7) Uani 1 d . . .
O1 O -0.8689(2) -0.6227(2) -0.87721(14) 0.0250(8) Uani 1 d . . .
O12 O -0.5301(3) -0.4446(3) -0.82555(18) 0.0474(11) Uani 1 d . . .
O14 O -1.1566(3) -0.4860(3) -0.8915(2) 0.0744(16) Uani 1 d . . .
O11 O -0.4100(4) -0.5358(3) -0.7865(3) 0.0859(18) Uani 1 d . . .
O8 O -0.9800(3) -0.2384(3) -0.7270(3) 0.0735(15) Uani 1 d . . .
H8 H -0.9794 -0.1899 -0.7117 0.110 Uiso 1 calc . . GR
O13 O -1.0643(3) -0.5890(2) -0.8399(2) 0.0579(13) Uani 1 d . . .
N2 N -0.4392(2) -0.5744(2) -0.66774(18) 0.0223(9) Uani 1 d . . .
N3 N -1.0316(3) -0.3047(2) -0.84688(19) 0.0261(9) Uani 1 d . . .
N1 N -0.5176(3) -0.7215(2) -0.76859(17) 0.0225(9) Uani 1 d . . .
N4 N -1.0128(3) -0.4169(3) -0.7323(2) 0.0379(11) Uani 1 d . . .
C40 C -0.3968(8) -0.4119(5) -0.8438(6) 0.165(6) Uani 1 d . . .
H40A H -0.4148 -0.3510 -0.8457 0.248 Uiso 1 calc . . GR
H40B H -0.4083 -0.4316 -0.8842 0.248 Uiso 1 calc . . GR
H40C H -0.3320 -0.4177 -0.8164 0.248 Uiso 1 calc . . GR
C24 C -0.8671(3) -0.2414(3) -0.9683(2) 0.0217(11) Uani 1 d . . .
C21 C -0.8889(3) -0.3659(3) -0.8895(2) 0.0176(10) Uani 1 d . . .
C16 C -0.6476(3) -0.3521(3) -0.6212(2) 0.0208(10) Uani 1 d . . .
H16 H -0.6901 -0.3124 -0.6191 0.025 Uiso 1 calc . . R
C35 C -0.7264(3) -0.6146(3) -0.6022(2) 0.0229(11) Uani 1 d . . .
H35 H -0.6727 -0.6484 -0.5833 0.027 Uiso 1 calc . . R
C10 C -0.3735(3) -0.7259(3) -0.6690(2) 0.0293(12) Uani 1 d . . .
H10 H -0.3128 -0.7549 -0.6515 0.035 Uiso 1 calc . . R
C23 C -0.8157(3) -0.3192(3) -0.9545(2) 0.0234(11) Uani 1 d . . .
H23 H -0.7747 -0.3303 -0.9710 0.028 Uiso 1 calc . . R
C3 C -0.8255(3) -0.7024(3) -0.8705(2) 0.0192(10) Uani 1 d . . .
C15 C -0.5695(3) -0.3773(3) -0.5682(2) 0.0261(11) Uani 1 d . . .
C32 C -0.8856(3) -0.5081(3) -0.6577(2) 0.0222(11) Uani 1 d . . .
C38 C -0.6455(3) -0.6774(3) -0.6747(2) 0.0233(11) Uani 1 d . . .
H38A H -0.6289 -0.6958 -0.7063 0.035 Uiso 1 calc . . GR
H38B H -0.6630 -0.7281 -0.6585 0.035 Uiso 1 calc . . GR
H38C H -0.5935 -0.6487 -0.6423 0.035 Uiso 1 calc . . GR
C42 C -1.2189(4) -0.6307(4) -0.9031(3) 0.0542(18) Uani 1 d . . .
H42A H -1.1955 -0.6858 -0.9102 0.081 Uiso 1 calc . . GR
H42B H -1.2664 -0.6088 -0.9412 0.081 Uiso 1 calc . . GR
H42C H -1.2442 -0.6400 -0.8745 0.081 Uiso 1 calc . . GR
C25 C -0.9279(3) -0.2239(3) -0.9440(2) 0.0235(11) Uani 1 d . . .
H25 H -0.9612 -0.1712 -0.9537 0.028 Uiso 1 calc . . R
C6 C -0.7242(4) -0.8571(3) -0.8501(2) 0.0251(11) Uani 1 d . . .
H6 H -0.6910 -0.9095 -0.8434 0.030 Uiso 1 calc . . R
C26 C -0.9398(3) -0.2855(3) -0.9045(2) 0.0189(10) Uani 1 d . . .
C13 C -0.5184(3) -0.4715(3) -0.6274(2) 0.0202(10) Uani 1 d . . .
C17 C -0.6603(3) -0.3867(3) -0.6762(2) 0.0175(10) Uani 1 d . . .
C2 C -0.7267(3) -0.6976(3) -0.83580(19) 0.0172(10) Uani 1 d . . .
C41 C -1.1417(4) -0.5648(4) -0.8770(3) 0.0373(14) Uani 1 d . . .
C37 C -0.8400(3) -0.5366(3) -0.6927(2) 0.0189(10) Uani 1 d . . .
C20 C -0.7360(4) -0.4912(4) -0.9335(2) 0.0396(14) Uani 1 d . . .
H20A H -0.6872 -0.4528 -0.9313 0.059 Uiso 1 calc . . GR
H20B H -0.7827 -0.4953 -0.9754 0.059 Uiso 1 calc . . GR
H20C H -0.7112 -0.5490 -0.9188 0.059 Uiso 1 calc . . GR
C8 C -0.5770(3) -0.7844(3) -0.7926(2) 0.0237(11) Uani 1 d . . .
H8A H -0.5528 -0.8412 -0.7883 0.028 Uiso 1 calc . . R
C34 C -0.7750(3) -0.5878(3) -0.5696(2) 0.0258(11) Uani 1 d . . .
C27 C -1.0046(3) -0.2603(3) -0.8806(2) 0.0246(11) Uani 1 d . . .
H27 H -1.0299 -0.2039 -0.8914 0.030 Uiso 1 calc . . R
C18 C -0.5980(3) -0.4484(3) -0.6817(2) 0.0160(10) Uani 1 d . . .
C4 C -0.8704(3) -0.7805(3) -0.8948(2) 0.0233(11) Uani 1 d . . .
H4 H -0.9343 -0.7814 -0.9185 0.028 Uiso 1 calc . . R
C36 C -0.7597(3) -0.5900(3) -0.6627(2) 0.0180(10) Uani 1 d . . .
C5 C -0.8194(4) -0.8581(3) -0.8837(2) 0.0261(11) Uani 1 d . . .
C28 C -1.0975(4) -0.2605(3) -0.8292(3) 0.0367(14) Uani 1 d . . .
H28A H -1.1583 -0.2863 -0.8527 0.044 Uiso 1 calc . . R
H28B H -1.1014 -0.1985 -0.8405 0.044 Uiso 1 calc . . R
C14 C -0.5066(3) -0.4350(3) -0.5707(2) 0.0266(11) Uani 1 d . . .
H14 H -0.4551 -0.4507 -0.5346 0.032 Uiso 1 calc . . R
C12 C -0.4452(3) -0.5311(3) -0.6249(2) 0.0239(11) Uani 1 d . . .
H12 H -0.3958 -0.5383 -0.5861 0.029 Uiso 1 calc . . R
C22 C -0.8268(3) -0.3799(3) -0.9156(2) 0.0204(10) Uani 1 d . . .
C29 C -1.0736(4) -0.2663(4) -0.7625(3) 0.0437(15) Uani 1 d . . .
H29 H -1.1133 -0.2240 -0.7548 0.052 Uiso 1 calc . . R
C19 C -0.8023(3) -0.3075(3) -0.7287(2) 0.0325(13) Uani 1 d . . .
H19A H -0.8503 -0.2975 -0.7696 0.049 Uiso 1 calc . . GR
H19B H -0.7735 -0.2521 -0.7110 0.049 Uiso 1 calc . . GR
H19C H -0.8286 -0.3333 -0.7040 0.049 Uiso 1 calc . . GR
C9 C -0.4199(3) -0.7474(3) -0.7371(2) 0.0291(12) Uani 1 d . . .
H9A H -0.3866 -0.7175 -0.7566 0.035 Uiso 1 calc . . R
H9B H -0.4152 -0.8106 -0.7423 0.035 Uiso 1 calc . . R
C7 C -0.6771(3) -0.7772(3) -0.8257(2) 0.0185(10) Uani 1 d . . .
C31 C -0.9647(3) -0.4486(3) -0.6786(2) 0.0285(12) Uani 1 d . . .
H31 H -0.9828 -0.4314 -0.6489 0.034 Uiso 1 calc . . R
C11 C -0.3559(3) -0.6283(3) -0.6515(2) 0.0279(12) Uani 1 d . . .
H11A H -0.3176 -0.6242 -0.6075 0.033 Uiso 1 calc . . R
H11B H -0.3210 -0.6032 -0.6715 0.033 Uiso 1 calc . . R
C39 C -0.4535(6) -0.4688(4) -0.8201(4) 0.072(3) Uani 1 d . . .
C30 C -1.0865(5) -0.3534(4) -0.7396(3) 0.0543(18) Uani 1 d . . .
H30A H -1.0873 -0.3455 -0.7003 0.065 Uiso 1 calc . . R
H30B H -1.1460 -0.3777 -0.7682 0.065 Uiso 1 calc . . R
C33 C -0.8509(3) -0.5367(3) -0.5958(2) 0.0243(11) Uani 1 d . . .
H33 H -0.8814 -0.5197 -0.5728 0.029 Uiso 1 calc . . R
C1 C -0.9601(3) -0.6142(3) -0.9266(2) 0.0374(14) Uani 1 d . . .
H1A H -1.0025 -0.6493 -0.9179 0.056 Uiso 1 calc . . GR
H1B H -0.9603 -0.6342 -0.9641 0.056 Uiso 1 calc . . GR
H1C H -0.9789 -0.5532 -0.9308 0.056 Uiso 1 calc . . GR
O15 O -0.2541(5) -0.5950(5) -0.7833(3) 0.113(2) Uani 1 d . . .
H H -0.3003 -0.5806 -0.7796 0.169 Uiso 1 calc . . GR
C43 C -0.1735(6) -0.5832(5) -0.7258(4) 0.085(3) Uani 1 d . . .
HA H -0.1771 -0.6216 -0.6955 0.127 Uiso 1 calc . . GR
HB H -0.1701 -0.5228 -0.7127 0.127 Uiso 1 calc . . GR
HC H -0.1191 -0.5973 -0.7307 0.127 Uiso 1 calc . . GR
Br1 Br -0.8799(5) -0.9682(6) -0.9140(3) 0.0470(15) Uani 0.50 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
Cd1 O10 2.623(3) . ?
Cd1 O2 2.259(3) . ?
Cd1 O4 2.277(3) . ?
Cd1 O6 2.549(3) . ?
Cd1 O7 2.260(3) . ?
Cd1 O5 2.610(3) . ?
Cd1 O9 2.263(3) . ?
Cd1 O1 2.532(3) . ?
Cd2 O2 2.277(3) . ?
Cd2 O4 2.256(3) . ?
Cd2 O12 2.389(4) . ?
Cd2 O11 2.369(5) . ?
Cd2 N2 2.289(4) . ?
Cd2 N1 2.292(4) . ?
Cd2 C39 2.712(6) . ?
Cd3 O7 2.249(3) . ?
Cd3 O9 2.269(3) . ?
Cd3 O14 2.417(4) . ?
Cd3 O13 2.295(4) . ?
Cd3 N3 2.295(4) . ?
Cd3 N4 2.240(4) . ?
Cd3 C41 2.713(6) . ?
Br3 C24 1.894(4) . ?
Br2 C15 1.903(5) . ?
Br4 C34 1.885(5) . ?
Br7 C5 1.905(10) . ?
O10 C38 1.430(5) . ?
O10 C36 1.368(5) . ?
O2 C2 1.309(5) . ?
O4 C18 1.311(5) . ?
O6 C20 1.426(6) . ?
O6 C22 1.371(5) . ?
O7 C21 1.303(5) . ?
O5 C17 1.364(5) . ?
O5 C19 1.444(5) . ?
O3 H3 0.8200 . ?
O3 C10 1.425(6) . ?
O9 C37 1.312(5) . ?
O1 C3 1.366(5) . ?
O1 C1 1.429(5) . ?
O12 C39 1.238(8) . ?
O14 C41 1.234(7) . ?
O11 C39 1.292(8) . ?
O8 H8 0.8200 . ?
O8 C29 1.427(7) . ?
O13 C41 1.224(7) . ?
N2 C12 1.270(6) . ?
N2 C11 1.467(6) . ?
N3 C27 1.276(6) . ?
N3 C28 1.473(6) . ?
N1 C8 1.289(6) . ?
N1 C9 1.465(6) . ?
N4 C31 1.276(6) . ?
N4 C30 1.474(7) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C40 C39 1.543(9) . ?
C24 C23 1.390(6) . ?
C24 C25 1.377(7) . ?
C21 C26 1.418(6) . ?
C21 C22 1.421(6) . ?
C16 H16 0.9300 . ?
C16 C15 1.393(6) . ?
C16 C17 1.361(6) . ?
C35 H35 0.9300 . ?
C35 C34 1.401(6) . ?
C35 C36 1.371(6) . ?
C10 H10 0.9800 . ?
C10 C9 1.516(7) . ?
C10 C11 1.524(7) . ?
C23 H23 0.9300 . ?
C23 C22 1.384(6) . ?
C3 C2 1.433(6) . ?
C3 C4 1.372(6) . ?
C15 C14 1.359(7) . ?
C32 C37 1.418(6) . ?
C32 C31 1.454(7) . ?
C32 C33 1.416(6) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C42 C41 1.496(7) . ?
C25 H25 0.9300 . ?
C25 C26 1.411(6) . ?
C6 H6 0.9300 . ?
C6 C5 1.379(7) . ?
C6 C7 1.407(6) . ?
C26 C27 1.456(6) . ?
C13 C18 1.413(6) . ?
C13 C14 1.415(7) . ?
C13 C12 1.464(6) . ?
C17 C18 1.420(6) . ?
C2 C7 1.404(6) . ?
C37 C36 1.421(6) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C8 H8A 0.9300 . ?
C8 C7 1.451(6) . ?
C34 C33 1.343(7) . ?
C27 H27 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.389(6) . ?
C5 Br1 1.901(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.490(8) . ?
C14 H14 0.9300 . ?
C12 H12 0.9300 . ?
C29 H29 0.9800 . ?
C29 C30 1.479(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C31 H31 0.9300 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C33 H33 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
O15 H 0.8200 . ?
O15 C43 1.432(9) . ?
C43 HA 0.9600 . ?
C43 HB 0.9600 . ?
C43 HC 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cd1 O10 76.99(10) . . ?
O2 Cd1 O4 74.10(10) . . ?
O2 Cd1 O6 79.55(10) . . ?
O2 Cd1 O7 135.78(11) . . ?
O2 Cd1 O5 137.24(10) . . ?
O2 Cd1 O9 131.29(11) . . ?
O2 Cd1 O1 65.27(10) . . ?
O4 Cd1 O10 75.93(10) . . ?
O4 Cd1 O6 95.77(11) . . ?
O4 Cd1 O5 63.22(10) . . ?
O4 Cd1 O1 139.23(10) . . ?
O6 Cd1 O10 156.45(9) . . ?
O6 Cd1 O5 101.43(10) . . ?
O7 Cd1 O10 136.34(10) . . ?
O7 Cd1 O4 132.33(11) . . ?
O7 Cd1 O6 64.95(10) . . ?
O7 Cd1 O5 77.84(10) . . ?
O7 Cd1 O9 73.02(11) . . ?
O7 Cd1 O1 79.82(10) . . ?
O5 Cd1 O10 94.45(10) . . ?
O9 Cd1 O10 63.47(10) . . ?
O9 Cd1 O4 118.69(11) . . ?
O9 Cd1 O6 137.33(11) . . ?
O9 Cd1 O5 75.82(10) . . ?
O9 Cd1 O1 91.81(11) . . ?
O1 Cd1 O10 97.43(10) . . ?
O1 Cd1 O6 74.28(11) . . ?
O1 Cd1 O5 156.81(10) . . ?
O2 Cd2 O12 108.40(13) . . ?
O2 Cd2 O11 145.52(17) . . ?
O2 Cd2 N2 126.83(12) . . ?
O2 Cd2 N1 79.55(12) . . ?
O2 Cd2 C39 128.4(2) . . ?
O4 Cd2 O2 74.16(10) . . ?
O4 Cd2 O12 84.38(13) . . ?
O4 Cd2 O11 126.93(14) . . ?
O4 Cd2 N2 81.71(12) . . ?
O4 Cd2 N1 135.24(12) . . ?
O4 Cd2 C39 107.10(16) . . ?
O12 Cd2 C39 27.16(17) . . ?
O11 Cd2 O12 55.51(15) . . ?
O11 Cd2 C39 28.46(19) . . ?
N2 Cd2 O12 115.56(14) . . ?
N2 Cd2 O11 86.07(18) . . ?
N2 Cd2 N1 86.06(13) . . ?
N2 Cd2 C39 103.7(2) . . ?
N1 Cd2 O12 138.87(14) . . ?
N1 Cd2 O11 94.67(15) . . ?
N1 Cd2 C39 117.63(17) . . ?
O7 Cd3 O9 73.12(11) . . ?
O7 Cd3 O14 118.33(15) . . ?
O7 Cd3 O13 113.47(14) . . ?
O7 Cd3 N3 80.54(12) . . ?
O7 Cd3 C41 120.24(14) . . ?
O9 Cd3 O14 140.62(13) . . ?
O9 Cd3 O13 86.94(14) . . ?
O9 Cd3 N3 130.91(13) . . ?
O9 Cd3 C41 113.60(16) . . ?
O14 Cd3 C41 27.06(16) . . ?
O13 Cd3 O14 53.69(15) . . ?
O13 Cd3 C41 26.67(15) . . ?
N3 Cd3 O14 88.36(15) . . ?
N3 Cd3 O13 142.00(15) . . ?
N3 Cd3 C41 115.42(17) . . ?
N4 Cd3 O7 135.95(15) . . ?
N4 Cd3 O9 83.31(14) . . ?
N4 Cd3 O14 103.61(18) . . ?
N4 Cd3 O13 101.52(17) . . ?
N4 Cd3 N3 88.18(15) . . ?
N4 Cd3 C41 103.11(17) . . ?
C38 O10 Cd1 128.8(2) . . ?
C36 O10 Cd1 111.3(2) . . ?
C36 O10 C38 117.2(3) . . ?
Cd1 O2 Cd2 104.81(12) . . ?
C2 O2 Cd1 121.4(3) . . ?
C2 O2 Cd2 132.3(3) . . ?
Cd2 O4 Cd1 104.89(12) . . ?
C18 O4 Cd1 115.3(3) . . ?
C18 O4 Cd2 132.0(3) . . ?
C20 O6 Cd1 130.7(3) . . ?
C22 O6 Cd1 111.5(3) . . ?
C22 O6 C20 117.8(4) . . ?
Cd3 O7 Cd1 106.56(12) . . ?
C21 O7 Cd1 120.9(3) . . ?
C21 O7 Cd3 131.3(3) . . ?
C17 O5 Cd1 105.5(2) . . ?
C17 O5 C19 116.3(3) . . ?
C19 O5 Cd1 125.1(3) . . ?
C10 O3 H3 109.5 . . ?
Cd1 O9 Cd3 105.78(12) . . ?
C37 O9 Cd1 124.1(3) . . ?
C37 O9 Cd3 128.6(3) . . ?
C3 O1 Cd1 112.3(2) . . ?
C3 O1 C1 117.4(4) . . ?
C1 O1 Cd1 130.3(3) . . ?
C39 O12 Cd2 91.1(4) . . ?
C41 O14 Cd3 89.9(4) . . ?
C39 O11 Cd2 90.6(4) . . ?
C29 O8 H8 109.5 . . ?
C41 O13 Cd3 96.1(3) . . ?
C12 N2 Cd2 127.2(3) . . ?
C12 N2 C11 117.6(4) . . ?
C11 N2 Cd2 115.1(3) . . ?
C27 N3 Cd3 127.3(3) . . ?
C27 N3 C28 116.6(4) . . ?
C28 N3 Cd3 115.9(3) . . ?
C8 N1 Cd2 129.7(3) . . ?
C8 N1 C9 116.7(4) . . ?
C9 N1 Cd2 113.6(3) . . ?
C31 N4 Cd3 126.8(3) . . ?
C31 N4 C30 117.2(5) . . ?
C30 N4 Cd3 116.1(4) . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
C23 C24 Br3 118.4(4) . . ?
C25 C24 Br3 120.2(3) . . ?
C25 C24 C23 121.3(4) . . ?
O7 C21 C26 124.9(4) . . ?
O7 C21 C22 118.1(4) . . ?
C26 C21 C22 117.0(4) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
C17 C16 C15 118.7(4) . . ?
C34 C35 H35 120.7 . . ?
C36 C35 H35 120.7 . . ?
C36 C35 C34 118.5(4) . . ?
O3 C10 H10 106.7 . . ?
O3 C10 C9 111.6(4) . . ?
O3 C10 C11 107.8(4) . . ?
C9 C10 H10 106.7 . . ?
C9 C10 C11 116.8(4) . . ?
C11 C10 H10 106.7 . . ?
C24 C23 H23 120.7 . . ?
C22 C23 C24 118.7(4) . . ?
C22 C23 H23 120.7 . . ?
O1 C3 C2 113.6(4) . . ?
O1 C3 C4 124.3(4) . . ?
C4 C3 C2 122.1(4) . . ?
C16 C15 Br2 117.1(4) . . ?
C14 C15 Br2 121.7(4) . . ?
C14 C15 C16 121.2(4) . . ?
C37 C32 C31 125.9(4) . . ?
C33 C32 C37 118.7(4) . . ?
C33 C32 C31 115.3(4) . . ?
O10 C38 H38A 109.5 . . ?
O10 C38 H38B 109.5 . . ?
O10 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.3(4) . . ?
C26 C25 H25 119.8 . . ?
C5 C6 H6 119.7 . . ?
C5 C6 C7 120.5(4) . . ?
C7 C6 H6 119.7 . . ?
C21 C26 C27 123.9(4) . . ?
C25 C26 C21 120.0(4) . . ?
C25 C26 C27 116.1(4) . . ?
C18 C13 C14 118.8(4) . . ?
C18 C13 C12 124.8(4) . . ?
C14 C13 C12 116.4(4) . . ?
O5 C17 C18 113.3(4) . . ?
C16 C17 O5 124.0(4) . . ?
C16 C17 C18 122.8(4) . . ?
O2 C2 C3 117.8(4) . . ?
O2 C2 C7 125.0(4) . . ?
C7 C2 C3 117.1(4) . . ?
O14 C41 Cd3 63.0(3) . . ?
O14 C41 C42 120.1(6) . . ?
O13 C41 Cd3 57.3(3) . . ?
O13 C41 O14 120.2(5) . . ?
O13 C41 C42 119.7(5) . . ?
C42 C41 Cd3 174.0(4) . . ?
O9 C37 C32 124.6(4) . . ?
O9 C37 C36 117.8(4) . . ?
C32 C37 C36 117.6(4) . . ?
O6 C20 H20A 109.5 . . ?
O6 C20 H20B 109.5 . . ?
O6 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C8 H8A 116.0 . . ?
N1 C8 C7 127.9(4) . . ?
C7 C8 H8A 116.0 . . ?
C35 C34 Br4 118.9(4) . . ?
C33 C34 Br4 119.6(4) . . ?
C33 C34 C35 121.4(4) . . ?
N3 C27 C26 129.1(4) . . ?
N3 C27 H27 115.5 . . ?
C26 C27 H27 115.5 . . ?
O4 C18 C13 124.5(4) . . ?
O4 C18 C17 118.1(4) . . ?
C13 C18 C17 117.5(4) . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(4) . . ?
C5 C4 H4 120.3 . . ?
O10 C36 C35 123.7(4) . . ?
O10 C36 C37 113.9(4) . . ?
C35 C36 C37 122.4(4) . . ?
C6 C5 Br7 121.7(4) . . ?
C6 C5 C4 120.7(4) . . ?
C6 C5 Br1 118.9(4) . . ?
C4 C5 Br7 117.2(4) . . ?
C4 C5 Br1 120.4(4) . . ?
Br1 C5 Br7 7.3(4) . . ?
N3 C28 H28A 108.5 . . ?
N3 C28 H28B 108.5 . . ?
N3 C28 C29 114.9(4) . . ?
H28A C28 H28B 107.5 . . ?
C29 C28 H28A 108.5 . . ?
C29 C28 H28B 108.5 . . ?
C15 C14 C13 121.1(4) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
N2 C12 C13 129.7(4) . . ?
N2 C12 H12 115.2 . . ?
C13 C12 H12 115.2 . . ?
O6 C22 C21 114.0(4) . . ?
O6 C22 C23 123.3(4) . . ?
C23 C22 C21 122.6(4) . . ?
O8 C29 C28 109.2(5) . . ?
O8 C29 H29 107.2 . . ?
O8 C29 C30 108.9(5) . . ?
C28 C29 H29 107.2 . . ?
C30 C29 C28 116.7(5) . . ?
C30 C29 H29 107.2 . . ?
O5 C19 H19A 109.5 . . ?
O5 C19 H19B 109.5 . . ?
O5 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C9 C10 113.8(4) . . ?
N1 C9 H9A 108.8 . . ?
N1 C9 H9B 108.8 . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C6 C7 C8 115.3(4) . . ?
C2 C7 C6 120.2(4) . . ?
C2 C7 C8 124.5(4) . . ?
N4 C31 C32 128.8(5) . . ?
N4 C31 H31 115.6 . . ?
C32 C31 H31 115.6 . . ?
N2 C11 C10 115.4(4) . . ?
N2 C11 H11A 108.4 . . ?
N2 C11 H11B 108.4 . . ?
C10 C11 H11A 108.4 . . ?
C10 C11 H11B 108.4 . . ?
H11A C11 H11B 107.5 . . ?
O12 C39 Cd2 61.7(3) . . ?
O12 C39 O11 122.3(6) . . ?
O12 C39 C40 121.7(6) . . ?
O11 C39 Cd2 60.9(3) . . ?
O11 C39 C40 115.3(7) . . ?
C40 C39 Cd2 175.5(7) . . ?
N4 C30 C29 112.5(5) . . ?
N4 C30 H30A 109.1 . . ?
N4 C30 H30B 109.1 . . ?
C29 C30 H30A 109.1 . . ?
C29 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C32 C33 H33 119.3 . . ?
C34 C33 C32 121.5(4) . . ?
C34 C33 H33 119.3 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C43 O15 H 109.5 . . ?
O15 C43 HA 109.5 . . ?
O15 C43 HB 109.5 . . ?
O15 C43 HC 109.5 . . ?
HA C43 HB 109.5 . . ?
HA C43 HC 109.5 . . ?
HB C43 HC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O10 C36 C35 -160.2(4) . . . . ?
Cd1 O10 C36 C37 22.3(4) . . . . ?
Cd1 O2 C2 C3 26.2(5) . . . . ?
Cd1 O2 C2 C7 -152.2(3) . . . . ?
Cd1 O4 C18 C13 139.9(4) . . . . ?
Cd1 O4 C18 C17 -40.1(5) . . . . ?
Cd1 O6 C22 C21 -20.2(4) . . . . ?
Cd1 O6 C22 C23 156.6(3) . . . . ?
Cd1 O7 C21 C26 -149.1(3) . . . . ?
Cd1 O7 C21 C22 29.9(5) . . . . ?
Cd1 O5 C17 C16 -145.5(4) . . . . ?
Cd1 O5 C17 C18 33.9(4) . . . . ?
Cd1 O9 C37 C32 154.2(3) . . . . ?
Cd1 O9 C37 C36 -25.6(5) . . . . ?
Cd1 O1 C3 C2 -21.5(4) . . . . ?
Cd1 O1 C3 C4 159.3(4) . . . . ?
Cd2 O2 C2 C3 -170.0(3) . . . . ?
Cd2 O2 C2 C7 11.6(6) . . . . ?
Cd2 O4 C18 C13 -4.0(6) . . . . ?
Cd2 O4 C18 C17 176.0(3) . . . . ?
Cd2 O12 C39 O11 -7.0(8) . . . . ?
Cd2 O12 C39 C40 -176.7(9) . . . . ?
Cd2 O11 C39 O12 7.1(8) . . . . ?
Cd2 O11 C39 C40 177.3(7) . . . . ?
Cd2 N2 C12 C13 3.2(7) . . . . ?
Cd2 N2 C11 C10 -59.1(5) . . . . ?
Cd2 N1 C8 C7 -3.1(7) . . . . ?
Cd2 N1 C9 C10 64.9(5) . . . . ?
Cd3 O7 C21 C26 16.1(6) . . . . ?
Cd3 O7 C21 C22 -164.9(3) . . . . ?
Cd3 O9 C37 C32 -9.3(6) . . . . ?
Cd3 O9 C37 C36 170.9(3) . . . . ?
Cd3 O14 C41 O13 -3.8(6) . . . . ?
Cd3 O14 C41 C42 174.2(5) . . . . ?
Cd3 O13 C41 O14 4.0(6) . . . . ?
Cd3 O13 C41 C42 -174.0(4) . . . . ?
Cd3 N3 C27 C26 -7.0(7) . . . . ?
Cd3 N3 C28 C29 53.4(6) . . . . ?
Cd3 N4 C31 C32 5.3(8) . . . . ?
Cd3 N4 C30 C29 -60.8(6) . . . . ?
Br3 C24 C23 C22 180.0(3) . . . . ?
Br3 C24 C25 C26 179.8(3) . . . . ?
Br2 C15 C14 C13 -179.0(3) . . . . ?
Br4 C34 C33 C32 -175.4(3) . . . . ?
O10 Cd1 O2 Cd2 -89.75(12) . . . . ?
O10 Cd1 O2 C2 77.9(3) . . . . ?
O10 Cd1 O4 Cd2 91.23(12) . . . . ?
O10 Cd1 O4 C18 -61.8(3) . . . . ?
O10 Cd1 O6 C20 2.9(6) . . . . ?
O10 Cd1 O6 C22 -177.4(3) . . . . ?
O10 Cd1 O7 Cd3 -4.6(2) . . . . ?
O10 Cd1 O7 C21 163.8(3) . . . . ?
O10 Cd1 O5 C17 33.1(3) . . . . ?
O10 Cd1 O5 C19 -106.1(3) . . . . ?
O10 Cd1 O9 Cd3 -166.76(16) . . . . ?
O10 Cd1 O9 C37 26.5(3) . . . . ?
O10 Cd1 O1 C3 -47.3(3) . . . . ?
O10 Cd1 O1 C1 131.6(4) . . . . ?
O2 Cd1 O10 C38 24.2(3) . . . . ?
O2 Cd1 O10 C36 -175.3(3) . . . . ?
O2 Cd1 O4 Cd2 11.01(11) . . . . ?
O2 Cd1 O4 C18 -142.0(3) . . . . ?
O2 Cd1 O6 C20 -2.1(4) . . . . ?
O2 Cd1 O6 C22 177.7(3) . . . . ?
O2 Cd1 O7 Cd3 122.95(14) . . . . ?
O2 Cd1 O7 C21 -68.6(3) . . . . ?
O2 Cd1 O5 C17 -42.5(3) . . . . ?
O2 Cd1 O5 C19 178.3(3) . . . . ?
O2 Cd1 O9 Cd3 -127.39(13) . . . . ?
O2 Cd1 O9 C37 65.9(4) . . . . ?
O2 Cd1 O1 C3 24.6(3) . . . . ?
O2 Cd1 O1 C1 -156.4(4) . . . . ?
O2 Cd2 O4 Cd1 -10.92(11) . . . . ?
O2 Cd2 O4 C18 135.6(4) . . . . ?
O2 Cd2 O12 C39 -141.7(4) . . . . ?
O2 Cd2 O11 C39 67.3(5) . . . . ?
O2 Cd2 N2 C12 -65.9(4) . . . . ?
O2 Cd2 N2 C11 118.3(3) . . . . ?
O2 Cd2 N1 C8 6.9(4) . . . . ?
O2 Cd2 N1 C9 -175.7(3) . . . . ?
O2 Cd2 C39 O12 48.6(5) . . . . ?
O2 Cd2 C39 O11 -138.2(4) . . . . ?
O2 Cd2 C39 C40 -170(7) . . . . ?
O2 C2 C7 C6 179.5(4) . . . . ?
O2 C2 C7 C8 -2.8(7) . . . . ?
O4 Cd1 O10 C38 -52.4(3) . . . . ?
O4 Cd1 O10 C36 108.1(3) . . . . ?
O4 Cd1 O2 Cd2 -10.91(11) . . . . ?
O4 Cd1 O2 C2 156.7(3) . . . . ?
O4 Cd1 O6 C20 70.5(4) . . . . ?
O4 Cd1 O6 C22 -109.7(3) . . . . ?
O4 Cd1 O7 Cd3 -123.18(13) . . . . ?
O4 Cd1 O7 C21 45.3(3) . . . . ?
O4 Cd1 O5 C17 -38.7(2) . . . . ?
O4 Cd1 O5 C19 -177.9(4) . . . . ?
O4 Cd1 O9 Cd3 138.89(11) . . . . ?
O4 Cd1 O9 C37 -27.8(4) . . . . ?
O4 Cd1 O1 C3 29.7(3) . . . . ?
O4 Cd1 O1 C1 -151.3(4) . . . . ?
O4 Cd2 O2 Cd1 11.00(11) . . . . ?
O4 Cd2 O2 C2 -154.7(4) . . . . ?
O4 Cd2 O12 C39 147.1(5) . . . . ?
O4 Cd2 O11 C39 -52.1(5) . . . . ?
O4 Cd2 N2 C12 -2.9(4) . . . . ?
O4 Cd2 N2 C11 -178.7(3) . . . . ?
O4 Cd2 N1 C8 61.4(5) . . . . ?
O4 Cd2 N1 C9 -121.2(3) . . . . ?
O4 Cd2 C39 O12 -34.5(5) . . . . ?
O4 Cd2 C39 O11 138.7(4) . . . . ?
O4 Cd2 C39 C40 107(7) . . . . ?
O6 Cd1 O10 C38 19.2(5) . . . . ?
O6 Cd1 O10 C36 179.7(3) . . . . ?
O6 Cd1 O2 Cd2 88.23(13) . . . . ?
O6 Cd1 O2 C2 -104.1(3) . . . . ?
O6 Cd1 O4 Cd2 -66.38(12) . . . . ?
O6 Cd1 O4 C18 140.6(3) . . . . ?
O6 Cd1 O7 Cd3 162.82(16) . . . . ?
O6 Cd1 O7 C21 -28.7(3) . . . . ?
O6 Cd1 O5 C17 -129.4(3) . . . . ?
O6 Cd1 O5 C19 91.4(3) . . . . ?
O6 Cd1 O9 Cd3 -0.8(2) . . . . ?
O6 Cd1 O9 C37 -167.5(3) . . . . ?
O6 Cd1 O1 C3 110.2(3) . . . . ?
O6 Cd1 O1 C1 -70.9(4) . . . . ?
O7 Cd1 O10 C38 169.6(3) . . . . ?
O7 Cd1 O10 C36 -29.8(3) . . . . ?
O7 Cd1 O2 Cd2 124.43(14) . . . . ?
O7 Cd1 O2 C2 -67.9(3) . . . . ?
O7 Cd1 O4 Cd2 -127.46(13) . . . . ?
O7 Cd1 O4 C18 79.5(3) . . . . ?
O7 Cd1 O6 C20 -155.0(5) . . . . ?
O7 Cd1 O6 C22 24.7(3) . . . . ?
O7 Cd1 O5 C17 169.6(3) . . . . ?
O7 Cd1 O5 C19 30.4(3) . . . . ?
O7 Cd1 O9 Cd3 9.43(11) . . . . ?
O7 Cd1 O9 C37 -157.3(3) . . . . ?
O7 Cd1 O1 C3 176.8(3) . . . . ?
O7 Cd1 O1 C1 -4.3(4) . . . . ?
O7 Cd3 O9 Cd1 -9.47(11) . . . . ?
O7 Cd3 O9 C37 156.4(4) . . . . ?
O7 Cd3 O14 C41 101.7(4) . . . . ?
O7 Cd3 O13 C41 -111.0(4) . . . . ?
O7 Cd3 N3 C27 14.1(4) . . . . ?
O7 Cd3 N3 C28 -172.0(4) . . . . ?
O7 Cd3 N4 C31 -69.0(5) . . . . ?
O7 Cd3 N4 C30 112.8(4) . . . . ?
O7 Cd3 C41 O14 -93.8(4) . . . . ?
O7 Cd3 C41 O13 82.3(4) . . . . ?
O7 Cd3 C41 C42 143(4) . . . . ?
O7 C21 C26 C25 179.4(4) . . . . ?
O7 C21 C26 C27 0.4(7) . . . . ?
O7 C21 C22 O6 -2.8(6) . . . . ?
O7 C21 C22 C23 -179.6(4) . . . . ?
O5 Cd1 O10 C38 -113.4(3) . . . . ?
O5 Cd1 O10 C36 47.2(3) . . . . ?
O5 Cd1 O2 Cd2 -7.4(2) . . . . ?
O5 Cd1 O2 C2 160.3(3) . . . . ?
O5 Cd1 O4 Cd2 -166.29(15) . . . . ?
O5 Cd1 O4 C18 40.7(3) . . . . ?
O5 Cd1 O6 C20 134.3(4) . . . . ?
O5 Cd1 O6 C22 -45.9(3) . . . . ?
O5 Cd1 O7 Cd3 -88.24(12) . . . . ?
O5 Cd1 O7 C21 80.2(3) . . . . ?
O5 Cd1 O9 Cd3 90.79(13) . . . . ?
O5 Cd1 O9 C37 -75.9(3) . . . . ?
O5 Cd1 O1 C3 -167.5(3) . . . . ?
O5 Cd1 O1 C1 11.4(5) . . . . ?
O5 C17 C18 O4 -1.6(6) . . . . ?
O5 C17 C18 C13 178.4(4) . . . . ?
O3 C10 C9 N1 54.0(5) . . . . ?
O3 C10 C11 N2 -59.3(5) . . . . ?
O9 Cd1 O10 C38 174.9(4) . . . . ?
O9 Cd1 O10 C36 -24.6(3) . . . . ?
O9 Cd1 O2 Cd2 -125.37(13) . . . . ?
O9 Cd1 O2 C2 42.3(3) . . . . ?
O9 Cd1 O4 Cd2 139.78(11) . . . . ?
O9 Cd1 O4 C18 -13.2(3) . . . . ?
O9 Cd1 O6 C20 -144.2(4) . . . . ?
O9 Cd1 O6 C22 35.5(3) . . . . ?
O9 Cd1 O7 Cd3 -9.55(11) . . . . ?
O9 Cd1 O7 C21 158.9(3) . . . . ?
O9 Cd1 O5 C17 94.3(3) . . . . ?
O9 Cd1 O5 C19 -44.9(3) . . . . ?
O9 Cd1 O1 C3 -110.8(3) . . . . ?
O9 Cd1 O1 C1 68.1(4) . . . . ?
O9 Cd3 O7 Cd1 9.52(11) . . . . ?
O9 Cd3 O7 C21 -157.3(4) . . . . ?
O9 Cd3 O14 C41 3.8(5) . . . . ?
O9 Cd3 O13 C41 178.8(4) . . . . ?
O9 Cd3 N3 C27 71.9(5) . . . . ?
O9 Cd3 N3 C28 -114.3(3) . . . . ?
O9 Cd3 N4 C31 -11.8(5) . . . . ?
O9 Cd3 N4 C30 170.0(4) . . . . ?
O9 Cd3 C41 O14 -177.4(4) . . . . ?
O9 Cd3 C41 O13 -1.3(4) . . . . ?
O9 Cd3 C41 C42 60(4) . . . . ?
O9 C37 C36 O10 -2.2(6) . . . . ?
O9 C37 C36 C35 -179.7(4) . . . . ?
O1 Cd1 O10 C38 86.6(3) . . . . ?
O1 Cd1 O10 C36 -112.9(3) . . . . ?
O1 Cd1 O2 Cd2 165.62(15) . . . . ?
O1 Cd1 O2 C2 -26.8(3) . . . . ?
O1 Cd1 O4 Cd2 6.2(2) . . . . ?
O1 Cd1 O4 C18 -146.8(3) . . . . ?
O1 Cd1 O6 C20 -69.1(4) . . . . ?
O1 Cd1 O6 C22 110.6(3) . . . . ?
O1 Cd1 O7 Cd3 85.52(13) . . . . ?
O1 Cd1 O7 C21 -106.0(3) . . . . ?
O1 Cd1 O5 C17 153.9(3) . . . . ?
O1 Cd1 O5 C19 14.7(5) . . . . ?
O1 Cd1 O9 Cd3 -69.35(13) . . . . ?
O1 Cd1 O9 C37 123.9(3) . . . . ?
O1 C3 C2 O2 0.1(6) . . . . ?
O1 C3 C2 C7 178.7(4) . . . . ?
O1 C3 C4 C5 -178.4(4) . . . . ?
O12 Cd2 O2 Cd1 -67.36(15) . . . . ?
O12 Cd2 O2 C2 127.0(4) . . . . ?
O12 Cd2 O4 Cd1 100.03(14) . . . . ?
O12 Cd2 O4 C18 -113.4(4) . . . . ?
O12 Cd2 O11 C39 -3.8(4) . . . . ?
O12 Cd2 N2 C12 76.8(4) . . . . ?
O12 Cd2 N2 C11 -99.1(3) . . . . ?
O12 Cd2 N1 C8 -99.1(4) . . . . ?
O12 Cd2 N1 C9 78.3(4) . . . . ?
O12 Cd2 C39 O11 173.2(8) . . . . ?
O12 Cd2 C39 C40 141(7) . . . . ?
O14 Cd3 O7 Cd1 -129.42(15) . . . . ?
O14 Cd3 O7 C21 63.8(4) . . . . ?
O14 Cd3 O9 Cd1 104.9(2) . . . . ?
O14 Cd3 O9 C37 -89.3(4) . . . . ?
O14 Cd3 O13 C41 -2.2(4) . . . . ?
O14 Cd3 N3 C27 -105.0(4) . . . . ?
O14 Cd3 N3 C28 68.9(4) . . . . ?
O14 Cd3 N4 C31 128.8(5) . . . . ?
O14 Cd3 N4 C30 -49.5(4) . . . . ?
O14 Cd3 C41 O13 176.1(6) . . . . ?
O14 Cd3 C41 C42 -123(5) . . . . ?
O11 Cd2 O2 Cd1 -122.6(2) . . . . ?
O11 Cd2 O2 C2 71.7(4) . . . . ?
O11 Cd2 O4 Cd1 138.24(19) . . . . ?
O11 Cd2 O4 C18 -75.2(4) . . . . ?
O11 Cd2 O12 C39 3.9(5) . . . . ?
O11 Cd2 N2 C12 125.3(4) . . . . ?
O11 Cd2 N2 C11 -50.5(3) . . . . ?
O11 Cd2 N1 C8 -138.8(4) . . . . ?
O11 Cd2 N1 C9 38.6(3) . . . . ?
O11 Cd2 C39 O12 -173.2(8) . . . . ?
O11 Cd2 C39 C40 -32(7) . . . . ?
O8 C29 C30 N4 -48.2(7) . . . . ?
O13 Cd3 O7 Cd1 -69.38(17) . . . . ?
O13 Cd3 O7 C21 123.8(4) . . . . ?
O13 Cd3 O9 Cd1 106.18(16) . . . . ?
O13 Cd3 O9 C37 -87.9(4) . . . . ?
O13 Cd3 O14 C41 2.2(3) . . . . ?
O13 Cd3 N3 C27 -102.1(5) . . . . ?
O13 Cd3 N3 C28 71.8(4) . . . . ?
O13 Cd3 N4 C31 73.7(5) . . . . ?
O13 Cd3 N4 C30 -104.5(4) . . . . ?
O13 Cd3 C41 O14 -176.1(6) . . . . ?
O13 Cd3 C41 C42 61(4) . . . . ?
N2 Cd2 O2 Cd1 77.44(17) . . . . ?
N2 Cd2 O2 C2 -88.2(4) . . . . ?
N2 Cd2 O4 Cd1 -143.07(14) . . . . ?
N2 Cd2 O4 C18 3.5(3) . . . . ?
N2 Cd2 O12 C39 69.0(5) . . . . ?
N2 Cd2 O11 C39 -128.6(5) . . . . ?
N2 Cd2 N1 C8 135.5(4) . . . . ?
N2 Cd2 N1 C9 -47.1(3) . . . . ?
N2 Cd2 C39 O12 -119.9(4) . . . . ?
N2 Cd2 C39 O11 53.3(5) . . . . ?
N2 Cd2 C39 C40 21(7) . . . . ?
N3 Cd3 O7 Cd1 147.63(15) . . . . ?
N3 Cd3 O7 C21 -19.2(3) . . . . ?
N3 Cd3 O9 Cd1 -70.1(2) . . . . ?
N3 Cd3 O9 C37 95.8(4) . . . . ?
N3 Cd3 O14 C41 -180.0(4) . . . . ?
N3 Cd3 O13 C41 -5.7(5) . . . . ?
N3 Cd3 N4 C31 -143.4(5) . . . . ?
N3 Cd3 N4 C30 38.4(4) . . . . ?
N3 Cd3 C41 O14 0.0(4) . . . . ?
N3 Cd3 C41 O13 176.1(3) . . . . ?
N3 Cd3 C41 C42 -123(4) . . . . ?
N3 C28 C29 O8 51.4(6) . . . . ?
N3 C28 C29 C30 -72.6(6) . . . . ?
N1 Cd2 O2 Cd1 154.41(14) . . . . ?
N1 Cd2 O2 C2 -11.3(4) . . . . ?
N1 Cd2 O4 Cd1 -67.3(2) . . . . ?
N1 Cd2 O4 C18 79.2(4) . . . . ?
N1 Cd2 O12 C39 -46.5(5) . . . . ?
N1 Cd2 O11 C39 145.6(5) . . . . ?
N1 Cd2 N2 C12 -139.7(4) . . . . ?
N1 Cd2 N2 C11 44.4(3) . . . . ?
N1 Cd2 C39 O12 147.4(4) . . . . ?
N1 Cd2 C39 O11 -39.4(5) . . . . ?
N1 Cd2 C39 C40 -71(7) . . . . ?
N1 C8 C7 C6 176.4(4) . . . . ?
N1 C8 C7 C2 -1.5(8) . . . . ?
N4 Cd3 O7 Cd1 70.3(2) . . . . ?
N4 Cd3 O7 C21 -96.5(4) . . . . ?
N4 Cd3 O9 Cd1 -151.83(16) . . . . ?
N4 Cd3 O9 C37 14.1(4) . . . . ?
N4 Cd3 O14 C41 -92.3(4) . . . . ?
N4 Cd3 O13 C41 96.3(4) . . . . ?
N4 Cd3 N3 C27 151.4(4) . . . . ?
N4 Cd3 N3 C28 -34.7(4) . . . . ?
N4 Cd3 C41 O14 94.3(4) . . . . ?
N4 Cd3 C41 O13 -89.6(4) . . . . ?
N4 Cd3 C41 C42 -29(4) . . . . ?
C24 C23 C22 O6 -176.3(4) . . . . ?
C24 C23 C22 C21 0.2(7) . . . . ?
C24 C25 C26 C21 0.1(6) . . . . ?
C24 C25 C26 C27 179.2(4) . . . . ?
C21 C26 C27 N3 -4.8(8) . . . . ?
C16 C15 C14 C13 0.0(7) . . . . ?
C16 C17 C18 O4 177.8(4) . . . . ?
C16 C17 C18 C13 -2.2(6) . . . . ?
C35 C34 C33 C32 0.4(7) . . . . ?
C23 C24 C25 C26 -0.4(7) . . . . ?
C3 C2 C7 C6 1.1(6) . . . . ?
C3 C2 C7 C8 178.8(4) . . . . ?
C3 C4 C5 Br7 -175.0(4) . . . . ?
C3 C4 C5 C6 -1.8(7) . . . . ?
C3 C4 C5 Br1 177.5(4) . . . . ?
C15 C16 C17 O5 -179.8(4) . . . . ?
C15 C16 C17 C18 0.9(7) . . . . ?
C32 C37 C36 O10 178.0(4) . . . . ?
C32 C37 C36 C35 0.5(6) . . . . ?
C38 O10 C36 C35 2.8(6) . . . . ?
C38 O10 C36 C37 -174.7(4) . . . . ?
C25 C24 C23 C22 0.2(7) . . . . ?
C25 C26 C27 N3 176.2(5) . . . . ?
C26 C21 C22 O6 176.3(4) . . . . ?
C26 C21 C22 C23 -0.5(6) . . . . ?
C17 C16 C15 Br2 179.3(3) . . . . ?
C17 C16 C15 C14 0.2(7) . . . . ?
C2 C3 C4 C5 2.6(7) . . . . ?
C41 Cd3 O7 Cd1 -98.38(19) . . . . ?
C41 Cd3 O7 C21 94.8(4) . . . . ?
C41 Cd3 O9 Cd1 106.75(16) . . . . ?
C41 Cd3 O9 C37 -87.4(4) . . . . ?
C41 Cd3 N3 C27 -105.0(4) . . . . ?
C41 Cd3 N3 C28 68.9(4) . . . . ?
C41 Cd3 N4 C31 100.9(5) . . . . ?
C41 Cd3 N4 C30 -77.3(4) . . . . ?
C37 C32 C31 N4 6.4(8) . . . . ?
C37 C32 C33 C34 1.8(7) . . . . ?
C20 O6 C22 C21 159.6(4) . . . . ?
C20 O6 C22 C23 -23.6(6) . . . . ?
C8 N1 C9 C10 -117.3(5) . . . . ?
C34 C35 C36 O10 -175.6(4) . . . . ?
C34 C35 C36 C37 1.7(7) . . . . ?
C27 N3 C28 C29 -132.1(5) . . . . ?
C18 C13 C14 C15 -1.4(7) . . . . ?
C18 C13 C12 N2 -2.4(8) . . . . ?
C4 C3 C2 O2 179.3(4) . . . . ?
C4 C3 C2 C7 -2.2(7) . . . . ?
C36 C35 C34 Br4 173.7(3) . . . . ?
C36 C35 C34 C33 -2.1(7) . . . . ?
C5 C6 C7 C2 -0.5(7) . . . . ?
C5 C6 C7 C8 -178.4(4) . . . . ?
C28 N3 C27 C26 179.2(5) . . . . ?
C28 C29 C30 N4 76.0(7) . . . . ?
C14 C13 C18 O4 -177.6(4) . . . . ?
C14 C13 C18 C17 2.4(6) . . . . ?
C14 C13 C12 N2 177.8(5) . . . . ?
C12 N2 C11 C10 124.6(5) . . . . ?
C12 C13 C18 O4 2.5(7) . . . . ?
C12 C13 C18 C17 -177.5(4) . . . . ?
C12 C13 C14 C15 178.5(4) . . . . ?
C22 C21 C26 C25 0.3(6) . . . . ?
C22 C21 C26 C27 -178.6(4) . . . . ?
C19 O5 C17 C16 -2.1(6) . . . . ?
C19 O5 C17 C18 177.3(4) . . . . ?
C9 N1 C8 C7 179.6(4) . . . . ?
C9 C10 C11 N2 67.2(6) . . . . ?
C7 C6 C5 Br7 173.7(4) . . . . ?
C7 C6 C5 C4 0.8(7) . . . . ?
C7 C6 C5 Br1 -178.5(4) . . . . ?
C31 N4 C30 C29 120.8(6) . . . . ?
C31 C32 C37 O9 -4.1(7) . . . . ?
C31 C32 C37 C36 175.7(4) . . . . ?
C31 C32 C33 C34 -176.3(4) . . . . ?
C11 N2 C12 C13 178.9(4) . . . . ?
C11 C10 C9 N1 -70.6(6) . . . . ?
C39 Cd2 O2 Cd1 -88.5(2) . . . . ?
C39 Cd2 O2 C2 105.8(4) . . . . ?
C39 Cd2 O4 Cd1 115.1(2) . . . . ?
C39 Cd2 O4 C18 -98.4(4) . . . . ?
C39 Cd2 N2 C12 102.8(4) . . . . ?
C39 Cd2 N2 C11 -73.0(3) . . . . ?
C39 Cd2 N1 C8 -121.1(4) . . . . ?
C39 Cd2 N1 C9 56.3(4) . . . . ?
C30 N4 C31 C32 -176.5(5) . . . . ?
C33 C32 C37 O9 178.0(4) . . . . ?
C33 C32 C37 C36 -2.2(6) . . . . ?
C33 C32 C31 N4 -175.7(5) . . . . ?
C1 O1 C3 C2 159.4(4) . . . . ?
C1 O1 C3 C4 -19.7(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_details          ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 336 45 ' '
2 0.500 0.500 0.000 336 45 ' '

####################################################################### 
# 
# 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_cd
_database_code_depnum_ccdc_archive 'CCDC 1409536'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-09-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38 H40 Cd3 Cl2 N4 O10'
_chemical_formula_sum            'C38 H40 Cd3 Cl2 N4 O10'
_chemical_formula_weight         1120.84
_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 0.0033 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'
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'

_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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   15.432(3)
_cell_length_b                   19.782(4)
_cell_length_c                   15.142(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4622.5(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12784
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8864
_cell_measurement_theta_min      1.6753
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8165
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10653
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.897
_diffrn_reflns_theta_min         1.674
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.1391
	          2theta: -29.8951
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.1391
	          2theta: -29.8951
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.1391
	          2theta: -29.8951
;
_diffrn_measurement_device       
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details 
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       dtprofit.ref
_diffrn_number_total             21928
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0570
_diffrn_orient_matrix_UB_12      0.0333
_diffrn_orient_matrix_UB_13      0.0011
_diffrn_orient_matrix_UB_21      0.0224
_diffrn_orient_matrix_UB_22      0.0399
_diffrn_orient_matrix_UB_23      -0.0459
_diffrn_orient_matrix_UB_31      -0.0185
_diffrn_orient_matrix_UB_32      -0.0307
_diffrn_orient_matrix_UB_33      -0.0356
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_diffrn_special_details          
;
 ?
;
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4963
_reflns_number_total             5520
_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
????
;
_refine_diff_density_max         0.737
_refine_diff_density_min         -2.095
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         5520
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.187
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1519
_refine_ls_wR_factor_ref         0.1569
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C36(H36)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C41(H41A,H41B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C16(H16), C18(H18), C20(H20), C29(H29), C32(H32), C34(H34)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C)
2.e Idealised tetrahedral OH refined as rotating group:
 O21(H21)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Cd1 Cd 0.16621(2) 0.17430(2) 0.58072(2) 0.02416(13) Uani 1 1 d . . . . .
Cd2 Cd 0.0000 0.17130(2) 0.7500 0.01722(13) Uani 1 2 d S T P . .
Cl1 Cl 0.30431(6) 0.11263(5) 0.58751(8) 0.0424(3) Uani 1 1 d . . . . .
O5 O 0.06185(15) 0.26179(12) 0.85729(16) 0.0245(5) Uani 1 1 d . . . . .
O7 O 0.09512(15) 0.07670(11) 0.80256(15) 0.0225(5) Uani 1 1 d . . . . .
O8 O 0.03772(15) 0.12786(11) 0.61538(15) 0.0212(5) Uani 1 1 d . . . . .
O9 O 0.12298(15) 0.22780(11) 0.70414(17) 0.0236(5) Uani 1 1 d . . . . .
C11 C 0.1568(2) 0.03294(16) 0.9395(2) 0.0212(6) Uani 1 1 d . . . . .
H11 H 0.2040 0.0144 0.9099 0.025 Uiso 1 1 calc R . . . .
C12 C 0.1673(2) 0.0482(2) 0.7556(2) 0.0286(8) Uani 1 1 d . . . . .
H12A H 0.1577 0.0524 0.6932 0.043 Uiso 1 1 calc GR . . . .
H12B H 0.1731 0.0013 0.7708 0.043 Uiso 1 1 calc GR . . . .
H12C H 0.2193 0.0718 0.7715 0.043 Uiso 1 1 calc GR . . . .
C13 C 0.0940(2) 0.06709(15) 0.8936(2) 0.0200(6) Uani 1 1 d . . . . .
C14 C -0.0799(2) 0.05521(18) 0.4258(2) 0.0266(7) Uani 1 1 d . . . . .
H14 H -0.0756 0.0515 0.3647 0.032 Uiso 1 1 calc R . . . .
C15 C -0.0202(2) 0.09694(15) 0.5653(2) 0.0185(6) Uani 1 1 d . . . . .
C16 C 0.1991(3) 0.33319(19) 0.5798(3) 0.0333(9) Uani 1 1 d . . . . .
H16 H 0.2208 0.3717 0.5524 0.040 Uiso 1 1 calc R . . . .
N17 N 0.20397(18) 0.27812(15) 0.5337(2) 0.0293(7) Uani 1 1 d . . . . .
C18 C 0.1496(2) 0.02604(17) 1.0317(2) 0.0236(7) Uani 1 1 d . . . . .
H18 H 0.1912 0.0022 1.0635 0.028 Uiso 1 1 calc R . . . .
C20 C 0.0527(3) 0.11959(19) 0.4163(2) 0.0295(8) Uani 1 1 d . . . . .
H20 H 0.0464 0.1133 0.3558 0.035 Uiso 1 1 calc R . . . .
O21 O 0.1055(2) 0.28475(15) 0.3698(2) 0.0429(7) Uani 1 1 d . . . . .
H21 H 0.0704 0.2593 0.3464 0.064 Uiso 1 1 calc GR . . . .
C22 C 0.0289(2) 0.2790(2) 0.9432(3) 0.0310(8) Uani 1 1 d . . . . .
H22A H -0.0194 0.3092 0.9371 0.047 Uiso 1 1 calc GR . . . .
H22B H 0.0737 0.3006 0.9770 0.047 Uiso 1 1 calc GR . . . .
H22C H 0.0106 0.2386 0.9731 0.047 Uiso 1 1 calc GR . . . .
C24 C -0.0151(2) 0.09051(16) 0.4725(2) 0.0220(6) Uani 1 1 d . . . . .
N26 N 0.1195(2) 0.15260(16) 0.4412(2) 0.0305(7) Uani 1 1 d . . . . .
C27 C 0.1287(2) 0.29302(17) 0.7236(2) 0.0243(7) Uani 1 1 d . . . . .
C28 C 0.1644(2) 0.3437(2) 0.6686(3) 0.0303(8) Uani 1 1 d . . . . .
C29 C 0.1662(3) 0.4110(2) 0.6987(3) 0.0372(9) Uani 1 1 d . . . . .
H29 H 0.1898 0.4440 0.6621 0.045 Uiso 1 1 calc R . . . .
C31 C 0.0958(2) 0.31436(17) 0.8075(3) 0.0264(7) Uani 1 1 d . . . . .
C32 C 0.1347(3) 0.42988(19) 0.7789(3) 0.0372(9) Uani 1 1 d . . . . .
H32 H 0.1374 0.4749 0.7966 0.045 Uiso 1 1 calc R . . . .
C33 C 0.2432(3) 0.2841(2) 0.4454(3) 0.0387(9) Uani 1 1 d . . . . .
H33A H 0.2992 0.2619 0.4459 0.046 Uiso 1 1 calc R . . . .
H33B H 0.2528 0.3316 0.4327 0.046 Uiso 1 1 calc R . . . .
C34 C 0.0985(2) 0.38110(18) 0.8346(3) 0.0328(8) Uani 1 1 d . . . . .
H34 H 0.0763 0.3934 0.8894 0.039 Uiso 1 1 calc R . . . .
C36 C 0.1878(3) 0.2535(2) 0.3715(3) 0.0382(9) Uani 1 1 d . . . . .
H36 H 0.2164 0.2656 0.3158 0.046 Uiso 1 1 calc R . . . .
C41 C 0.1778(3) 0.1766(2) 0.3706(4) 0.0403(11) Uani 1 1 d . . . . .
H41A H 0.1549 0.1626 0.3138 0.048 Uiso 1 1 calc R . . . .
H41B H 0.2343 0.1558 0.3780 0.048 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 Cl1 2.4576(10) . ?
Cd1 O8 2.248(2) . ?
Cd1 O9 2.249(3) . ?
Cd1 N17 2.250(3) . ?
Cd1 N26 2.273(3) . ?
Cd2 O5 2.599(2) . ?
Cd2 O5 2.599(2) 4_556 ?
Cd2 O7 2.508(2) 4_556 ?
Cd2 O7 2.508(2) . ?
Cd2 O8 2.287(2) 4_556 ?
Cd2 O8 2.287(2) . ?
Cd2 O9 2.309(2) 4_556 ?
Cd2 O9 2.309(2) . ?
O5 C22 1.438(5) . ?
O5 C31 1.387(4) . ?
O7 C12 1.437(4) . ?
O7 C13 1.391(4) . ?
O8 C15 1.322(4) . ?
O9 C27 1.326(4) . ?
C11 C13 1.371(5) . ?
C11 C18 1.407(5) . ?
C13 C15 1.427(4) 4_556 ?
C14 C18 1.380(5) 4_556 ?
C14 C24 1.411(5) . ?
C15 C13 1.427(4) 4_556 ?
C15 C24 1.413(5) . ?
C16 N17 1.296(5) . ?
C16 C28 1.461(6) . ?
N17 C33 1.472(5) . ?
C18 C14 1.380(5) 4_556 ?
C20 C24 1.466(5) . ?
C20 N26 1.277(5) . ?
O21 C36 1.412(5) . ?
N26 C41 1.475(5) . ?
C27 C28 1.414(5) . ?
C27 C31 1.433(6) . ?
C28 C29 1.408(6) . ?
C29 C32 1.360(7) . ?
C31 C34 1.383(5) . ?
C32 C34 1.399(6) . ?
C33 C36 1.533(6) . ?
C36 C41 1.530(6) . ?

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
O8 Cd1 Cl1 123.53(6) . . ?
O8 Cd1 O9 74.72(8) . . ?
O8 Cd1 N17 132.48(9) . . ?
O8 Cd1 N26 81.97(10) . . ?
O9 Cd1 Cl1 117.13(7) . . ?
O9 Cd1 N17 84.84(10) . . ?
O9 Cd1 N26 140.10(10) . . ?
N17 Cd1 Cl1 103.99(8) . . ?
N17 Cd1 N26 87.74(12) . . ?
N26 Cd1 Cl1 102.71(9) . . ?
O5 Cd2 O5 92.94(11) 4_556 . ?
O7 Cd2 O5 158.00(8) 4_556 . ?
O7 Cd2 O5 95.77(8) 4_556 4_556 ?
O7 Cd2 O5 95.77(8) . . ?
O7 Cd2 O5 158.01(8) . 4_556 ?
O7 Cd2 O7 83.48(11) . 4_556 ?
O8 Cd2 O5 78.18(8) . 4_556 ?
O8 Cd2 O5 78.18(8) 4_556 . ?
O8 Cd2 O5 136.25(8) 4_556 4_556 ?
O8 Cd2 O5 136.25(8) . . ?
O8 Cd2 O7 65.54(8) . 4_556 ?
O8 Cd2 O7 65.53(8) 4_556 . ?
O8 Cd2 O7 81.57(8) . . ?
O8 Cd2 O7 81.57(8) 4_556 4_556 ?
O8 Cd2 O8 135.86(11) 4_556 . ?
O8 Cd2 O9 72.83(8) 4_556 4_556 ?
O8 Cd2 O9 72.83(8) . . ?
O8 Cd2 O9 131.22(9) . 4_556 ?
O8 Cd2 O9 131.22(9) 4_556 . ?
O9 Cd2 O5 77.32(8) 4_556 . ?
O9 Cd2 O5 63.44(8) 4_556 4_556 ?
O9 Cd2 O5 63.44(8) . . ?
O9 Cd2 O5 77.32(8) . 4_556 ?
O9 Cd2 O7 88.60(8) . . ?
O9 Cd2 O7 138.30(8) 4_556 . ?
O9 Cd2 O7 138.31(8) . 4_556 ?
O9 Cd2 O7 88.60(8) 4_556 4_556 ?
O9 Cd2 O9 122.11(12) 4_556 . ?
C22 O5 Cd2 126.8(2) . . ?
C31 O5 Cd2 108.4(2) . . ?
C31 O5 C22 116.6(3) . . ?
C12 O7 Cd2 126.2(2) . . ?
C13 O7 Cd2 114.16(18) . . ?
C13 O7 C12 116.4(3) . . ?
Cd1 O8 Cd2 106.20(9) . . ?
C15 O8 Cd1 130.7(2) . . ?
C15 O8 Cd2 120.9(2) . . ?
Cd1 O9 Cd2 105.42(9) . . ?
C27 O9 Cd1 128.5(2) . . ?
C27 O9 Cd2 117.3(2) . . ?
C13 C11 C18 119.7(3) . . ?
O7 C13 C15 112.6(3) . 4_556 ?
C11 C13 O7 124.2(3) . . ?
C11 C13 C15 123.2(3) . 4_556 ?
C18 C14 C24 121.7(3) 4_556 . ?
O8 C15 C13 118.8(3) . 4_556 ?
O8 C15 C24 125.0(3) . . ?
C24 C15 C13 116.2(3) . 4_556 ?
N17 C16 C28 129.5(3) . . ?
C16 N17 Cd1 125.6(3) . . ?
C16 N17 C33 116.4(3) . . ?
C33 N17 Cd1 117.9(2) . . ?
C14 C18 C11 119.0(3) 4_556 . ?
N26 C20 C24 127.2(3) . . ?
C14 C24 C15 120.3(3) . . ?
C14 C24 C20 114.1(3) . . ?
C15 C24 C20 125.6(3) . . ?
C20 N26 Cd1 128.8(3) . . ?
C20 N26 C41 116.3(4) . . ?
C41 N26 Cd1 114.8(3) . . ?
O9 C27 C28 125.8(4) . . ?
O9 C27 C31 117.4(3) . . ?
C28 C27 C31 116.9(3) . . ?
C27 C28 C16 125.7(4) . . ?
C29 C28 C16 115.1(4) . . ?
C29 C28 C27 119.2(4) . . ?
C32 C29 C28 122.8(4) . . ?
O5 C31 C27 113.3(3) . . ?
C34 C31 O5 124.5(4) . . ?
C34 C31 C27 122.3(4) . . ?
C29 C32 C34 119.5(4) . . ?
N17 C33 C36 113.8(3) . . ?
C31 C34 C32 119.4(4) . . ?
O21 C36 C33 110.0(3) . . ?
O21 C36 C41 110.1(3) . . ?
C41 C36 C33 117.1(4) . . ?
N26 C41 C36 112.1(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.008 0.000 0.500 422 149 ' '
2 -0.010 0.500 1.000 421 149 ' '
_platon_squeeze_details          ?
####################################################################### 
# 
# 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_ni
_database_code_depnum_ccdc_archive 'CCDC 1443674'
_audit_update_record             
;
2015-12-21 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-09-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C42 H46 Br4 N4 Ni4 O14, 2(C H3 O), O'
_chemical_formula_sum            'C44 H54 Br4 N4 Ni4 O17'
_chemical_formula_weight         1465.39
_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 0.0033 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'
Br Br -0.2901 2.4595 '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'
Ni Ni 0.3393 1.1124 '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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   27.937(10)
_cell_length_b                   11.757(4)
_cell_length_c                   16.933(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.483(4)
_cell_angle_gamma                90.00
_cell_volume                     5175(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4527
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_exptl_absorpt_coefficient_mu    4.595
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2936
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ?
;
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20917
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         3.13
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
scan:
	Number of images: 360
	           Slice: -120.0000 - 60.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 49.8438
	          2theta: -30.1104
scan:
	Number of images: 300
	           Slice: -120.0000 - 30.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 49.8438
	          2theta: -30.1104
scan:
	Number of images: 200
	           Slice: -120.0000 - -20.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 49.8438
	          2theta: -30.1104
;
_diffrn_measurement_device       
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.023323
_diffrn_orient_matrix_UB_12      0.018805
_diffrn_orient_matrix_UB_13      0.024128
_diffrn_orient_matrix_UB_21      0.025974
_diffrn_orient_matrix_UB_22      0.049771
_diffrn_orient_matrix_UB_23      -0.063898
_diffrn_orient_matrix_UB_31      -0.029270
_diffrn_orient_matrix_UB_32      0.049572
_diffrn_orient_matrix_UB_33      0.026714
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_special_details          
;
 ?
;
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4957
_reflns_number_total             5947
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5947
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0542
_refine_ls_restrained_S_all      1.271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1757
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Br4(0.5) Br1(0.5)
3.a Ternary CH refined with riding coordinates:
 C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b), C29(H29a,H29b)
3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C24(H24), C26(H26), C28(H28), C32(H32), C34(H34)
3.d Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C17(H17a,H17b,H17c), C23(H23a,H23b,H23c), C33(H33a,H33b,
 H33c), C46(H46a,H46b,H46c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Br0A Br 0.26304(2) 0.75281(5) 0.63673(4) 0.02777(18) Uani 1 d . . 1 . . .
Ni2 Ni 0.44987(3) 0.44760(5) 0.49748(4) 0.01548(18) Uani 1 d . . 1 . . .
Ni3 Ni 0.54973(3) 0.30530(5) 0.55983(4) 0.01755(18) Uani 1 d . . 1 . . .
Br4 Br 0.72837(13) 0.0761(4) 0.9669(3) 0.0259(6) Uani 0.50 d . . 1 . . .
O5 O 0.52429(14) 0.4611(3) 0.5819(2) 0.0154(7) Uani 1 d . . 1 . . .
O6 O 0.61974(16) 0.3322(3) 0.6460(2) 0.0229(8) Uani 1 d . . 1 . . .
N7 N 0.53914(17) 0.1731(4) 0.6238(3) 0.0199(9) Uani 1 d . . 1 . . .
O8 O 0.40552(15) 0.8152(3) 0.5055(3) 0.0226(8) Uani 1 d . . 1 . . .
O9 O 0.47192(15) 0.2825(3) 0.4917(2) 0.0185(7) Uani 1 d . . 1 . . .
O10 O 0.71072(16) 0.4046(3) 0.7438(2) 0.0250(8) Uani 1 d . . 1 . . .
O11 O 0.43518(14) 0.6055(3) 0.5274(2) 0.0193(7) Uani 1 d . . 1 . . .
N12 N 0.42054(18) 0.3872(4) 0.5804(3) 0.0206(9) Uani 1 d . . 1 . . .
C13 C 0.5451(3) -0.1541(5) 0.6464(4) 0.0327(14) Uani 1 d . . 1 . . .
H13A H 0.5361 -0.2021 0.5973 0.049 Uiso 1 calc . . 1 GR . .
H13B H 0.5464 -0.0764 0.6300 0.049 Uiso 1 calc . . 1 GR . .
H13C H 0.5197 -0.1618 0.6720 0.049 Uiso 1 calc . . 1 GR . .
O14 O 0.37854(17) 0.4476(4) 0.3959(3) 0.0322(10) Uani 1 d . . 1 . . .
C15 C 0.4511(2) 0.2102(4) 0.5373(3) 0.0200(11) Uani 1 d . . 1 . . .
H15 H 0.4195 0.1755 0.4979 0.024 Uiso 1 calc . . 1 R . .
C16 C 0.4387(2) 0.2742(4) 0.6083(3) 0.0210(11) Uani 1 d . . 1 . . .
H16A H 0.4125 0.2328 0.6216 0.025 Uiso 1 calc . . 1 R . .
H16B H 0.4693 0.2783 0.6593 0.025 Uiso 1 calc . . 1 R . .
C17 C 0.5335(2) 0.4991(5) 0.6661(3) 0.0237(11) Uani 1 d . . 1 . . .
H17A H 0.5163 0.5703 0.6641 0.035 Uiso 1 calc . . 1 GR . .
H17B H 0.5698 0.5088 0.6959 0.035 Uiso 1 calc . . 1 GR . .
H17C H 0.5206 0.4437 0.6950 0.035 Uiso 1 calc . . 1 GR . .
C18 C 0.3792(2) 0.7467(4) 0.5423(3) 0.0206(11) Uani 1 d . . 1 . . .
C19 C 0.6976(3) 0.1525(5) 0.8634(3) 0.0267(13) Uani 1 d . . 1 . . .
C20 C 0.3350(2) 0.5938(5) 0.6196(3) 0.0216(11) Uani 1 d . . 1 . . .
H20 H 0.3210 0.5440 0.6480 0.026 Uiso 1 calc . . 1 R . .
C21 C 0.3177(2) 0.7023(5) 0.6046(3) 0.0214(11) Uani 1 d . . 1 . . .
C22 C 0.6220(2) 0.1738(4) 0.7385(3) 0.0218(11) Uani 1 d . . 1 . . .
C23 C 0.7601(2) 0.4428(5) 0.7935(4) 0.0270(12) Uani 1 d . . 1 . . .
H23A H 0.7714 0.4975 0.7620 0.041 Uiso 1 calc . . 1 GR . .
H23B H 0.7834 0.3796 0.8083 0.041 Uiso 1 calc . . 1 GR . .
H23C H 0.7592 0.4777 0.8442 0.041 Uiso 1 calc . . 1 GR . .
C24 C 0.3903(2) 0.4381(4) 0.6091(3) 0.0188(10) Uani 1 d . . 1 . . .
H24 H 0.3772 0.3970 0.6436 0.023 Uiso 1 calc . . 1 R . .
C25 C 0.6431(2) 0.2726(4) 0.7143(3) 0.0196(11) Uani 1 d . . 1 . . .
C26 C 0.7194(2) 0.2499(4) 0.8439(4) 0.0248(12) Uani 1 d . . 1 . . .
H26 H 0.7515 0.2755 0.8801 0.030 Uiso 1 calc . . 1 R . .
C27 C 0.6928(2) 0.3076(4) 0.7701(3) 0.0208(11) Uani 1 d . . 1 . . .
C28 C 0.3402(2) 0.7815(5) 0.5658(3) 0.0207(11) Uani 1 d . . 1 . . .
H28 H 0.3284 0.8562 0.5567 0.025 Uiso 1 calc . . 1 R . .
C29 C 0.4902(2) 0.1159(5) 0.5796(4) 0.0252(12) Uani 1 d . . 1 . . .
H29A H 0.4795 0.0732 0.6193 0.030 Uiso 1 calc . . 1 R . .
H29B H 0.4932 0.0640 0.5371 0.030 Uiso 1 calc . . 1 R . .
C30 C 0.3972(2) 0.6312(4) 0.5532(3) 0.0187(10) Uani 1 d . . 1 . . .
C31 C 0.3746(2) 0.5556(4) 0.5918(3) 0.0200(10) Uani 1 d . . 1 . . .
C32 C 0.5722(2) 0.1288(4) 0.6920(3) 0.0224(11) Uani 1 d . . 1 . . .
H32 H 0.5628 0.0623 0.7123 0.027 Uiso 1 calc . . 1 R . .
C33 C 0.3828(3) 0.9236(5) 0.4768(4) 0.0332(14) Uani 1 d . . 1 . . .
H33A H 0.3481 0.9133 0.4377 0.050 Uiso 1 calc . . 1 GR . .
H33B H 0.4023 0.9627 0.4488 0.050 Uiso 1 calc . . 1 GR . .
H33C H 0.3827 0.9677 0.5244 0.050 Uiso 1 calc . . 1 GR . .
C34 C 0.6507(2) 0.1140(5) 0.8133(3) 0.0255(12) Uani 1 d . . 1 . . .
H34 H 0.6373 0.0484 0.8280 0.031 Uiso 1 calc . . 1 R . .
C46 C 0.3361(3) 0.3812(8) 0.3774(6) 0.068(3) Uani 1 d . . 1 . . .
H46A H 0.3456 0.3089 0.4050 0.102 Uiso 1 calc . . 1 GR . .
H46B H 0.3209 0.3701 0.3171 0.102 Uiso 1 calc . . 1 GR . .
H46C H 0.3117 0.4177 0.3969 0.102 Uiso 1 calc . . 1 GR . .
Br1 Br 0.74294(15) 0.0705(4) 0.9631(3) 0.0455(10) Uani 0.50 d . . 1 . . .
O0AA O 0.5000 -0.0722(9) 0.7500 0.165(9) Uani 1 d . . 2 S T P
O1 O 0.5935(6) -0.1864(12) 0.7052(10) 0.206(8) Uani 1 d . . 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
Br0A C21 1.894(5) . ?
Ni2 O5 2.047(3) 5_666 ?
Ni2 O5 2.053(4) . ?
Ni2 O9 2.050(4) . ?
Ni2 O11 2.006(4) . ?
Ni2 N12 1.997(5) . ?
Ni2 O14 2.102(4) . ?
Ni3 O5 2.048(3) . ?
Ni3 O6 1.991(4) . ?
Ni3 N7 1.978(4) . ?
Ni3 O8 2.410(4) 5_666 ?
Ni3 O9 2.071(4) . ?
Ni3 O11 1.979(4) 5_666 ?
Br4 C19 1.874(7) . ?
O5 Ni2 2.047(3) 5_666 ?
O5 C17 1.424(6) . ?
O6 C25 1.304(6) . ?
N7 C29 1.460(7) . ?
N7 C32 1.295(7) . ?
O8 Ni3 2.410(4) 5_666 ?
O8 C18 1.383(6) . ?
O8 C33 1.428(6) . ?
O9 C15 1.409(6) . ?
O10 C23 1.401(7) . ?
O10 C27 1.383(7) . ?
O11 Ni3 1.979(4) 5_666 ?
O11 C30 1.321(6) . ?
N12 C16 1.439(7) . ?
N12 C24 1.269(7) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13 O1 1.407(15) . ?
O14 C46 1.357(9) . ?
C15 H15 0.9800 . ?
C15 C16 1.561(7) . ?
C15 C29 1.536(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 C28 1.354(8) . ?
C18 C30 1.437(7) . ?
C19 C26 1.393(8) . ?
C19 C34 1.351(9) . ?
C19 Br1 1.954(7) . ?
C20 H20 0.9300 . ?
C20 C21 1.355(8) . ?
C20 C31 1.424(7) . ?
C21 C28 1.413(8) . ?
C22 C25 1.428(7) . ?
C22 C32 1.426(8) . ?
C22 C34 1.413(7) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24 0.9300 . ?
C24 C31 1.446(7) . ?
C25 C27 1.424(8) . ?
C26 H26 0.9300 . ?
C26 C27 1.377(8) . ?
C28 H28 0.9300 . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.385(7) . ?
C32 H32 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34 0.9300 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Ni2 O5 84.60(14) 5_666 . ?
O5 Ni2 O9 106.30(14) 5_666 . ?
O5 Ni2 O14 85.37(16) 5_666 . ?
O5 Ni2 O14 169.93(16) . . ?
O9 Ni2 O5 82.02(14) . . ?
O9 Ni2 O14 99.92(16) . . ?
O11 Ni2 O5 90.06(15) . . ?
O11 Ni2 O5 80.49(14) . 5_666 ?
O11 Ni2 O9 168.92(15) . . ?
O11 Ni2 O14 89.23(17) . . ?
N12 Ni2 O5 96.29(16) . . ?
N12 Ni2 O5 169.11(16) . 5_666 ?
N12 Ni2 O9 84.55(16) . . ?
N12 Ni2 O11 88.66(16) . . ?
N12 Ni2 O14 93.74(19) . . ?
O5 Ni3 O8 151.94(13) . 5_666 ?
O5 Ni3 O9 81.60(14) . . ?
O6 Ni3 O5 92.15(15) . . ?
O6 Ni3 O8 83.95(15) . 5_666 ?
O6 Ni3 O9 167.81(15) . . ?
N7 Ni3 O5 118.12(16) . . ?
N7 Ni3 O6 91.54(17) . . ?
N7 Ni3 O8 89.81(15) . 5_666 ?
N7 Ni3 O9 82.33(17) . . ?
N7 Ni3 O11 160.20(17) . 5_666 ?
O9 Ni3 O8 106.46(14) . 5_666 ?
O11 Ni3 O5 81.10(14) 5_666 . ?
O11 Ni3 O6 92.44(15) 5_666 . ?
O11 Ni3 O8 71.36(14) 5_666 5_666 ?
O11 Ni3 O9 96.88(15) 5_666 . ?
Ni2 O5 Ni2 95.40(14) 5_666 . ?
Ni2 O5 Ni3 96.88(14) 5_666 . ?
Ni3 O5 Ni2 97.71(15) . . ?
C17 O5 Ni2 121.0(3) . 5_666 ?
C17 O5 Ni2 119.1(3) . . ?
C17 O5 Ni3 121.0(3) . . ?
C25 O6 Ni3 127.1(4) . . ?
C29 N7 Ni3 112.3(3) . . ?
C32 N7 Ni3 127.1(4) . . ?
C32 N7 C29 120.1(5) . . ?
C18 O8 Ni3 108.4(3) . 5_666 ?
C18 O8 C33 115.4(4) . . ?
C33 O8 Ni3 127.5(4) . 5_666 ?
Ni2 O9 Ni3 97.08(15) . . ?
C15 O9 Ni2 110.7(3) . . ?
C15 O9 Ni3 109.4(3) . . ?
C27 O10 C23 117.6(4) . . ?
Ni3 O11 Ni2 100.52(16) 5_666 . ?
C30 O11 Ni2 124.0(3) . . ?
C30 O11 Ni3 122.8(3) . 5_666 ?
C16 N12 Ni2 111.9(3) . . ?
C24 N12 Ni2 127.2(4) . . ?
C24 N12 C16 120.9(4) . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O1 C13 H13A 109.5 . . ?
O1 C13 H13B 109.5 . . ?
O1 C13 H13C 109.5 . . ?
C46 O14 Ni2 132.5(4) . . ?
O9 C15 H15 109.0 . . ?
O9 C15 C16 112.6(4) . . ?
O9 C15 C29 109.0(4) . . ?
C16 C15 H15 109.0 . . ?
C29 C15 H15 109.0 . . ?
C29 C15 C16 108.1(4) . . ?
N12 C16 C15 110.1(4) . . ?
N12 C16 H16A 109.6 . . ?
N12 C16 H16B 109.6 . . ?
C15 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
H16A C16 H16B 108.2 . . ?
O5 C17 H17A 109.5 . . ?
O5 C17 H17B 109.5 . . ?
O5 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O8 C18 C30 112.8(5) . . ?
C28 C18 O8 125.1(5) . . ?
C28 C18 C30 122.0(5) . . ?
Br4 C19 Br1 12.97(15) . . ?
C26 C19 Br4 121.6(5) . . ?
C26 C19 Br1 114.1(5) . . ?
C34 C19 Br4 115.7(5) . . ?
C34 C19 C26 122.3(5) . . ?
C34 C19 Br1 123.4(5) . . ?
C21 C20 H20 119.9 . . ?
C21 C20 C31 120.2(5) . . ?
C31 C20 H20 119.9 . . ?
C20 C21 Br0A 120.8(4) . . ?
C20 C21 C28 121.2(5) . . ?
C28 C21 Br0A 117.9(4) . . ?
C32 C22 C25 124.4(5) . . ?
C34 C22 C25 120.3(5) . . ?
C34 C22 C32 115.3(5) . . ?
O10 C23 H23A 109.5 . . ?
O10 C23 H23B 109.5 . . ?
O10 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N12 C24 H24 117.7 . . ?
N12 C24 C31 124.6(5) . . ?
C31 C24 H24 117.7 . . ?
O6 C25 C22 124.5(5) . . ?
O6 C25 C27 118.9(5) . . ?
C27 C25 C22 116.7(5) . . ?
C19 C26 H26 120.6 . . ?
C27 C26 C19 118.8(6) . . ?
C27 C26 H26 120.6 . . ?
O10 C27 C25 113.9(5) . . ?
C26 C27 O10 124.0(5) . . ?
C26 C27 C25 122.1(5) . . ?
C18 C28 C21 118.7(5) . . ?
C18 C28 H28 120.6 . . ?
C21 C28 H28 120.6 . . ?
N7 C29 C15 106.2(4) . . ?
N7 C29 H29A 110.5 . . ?
N7 C29 H29B 110.5 . . ?
C15 C29 H29A 110.5 . . ?
C15 C29 H29B 110.5 . . ?
H29A C29 H29B 108.7 . . ?
O11 C30 C18 117.4(5) . . ?
O11 C30 C31 124.6(5) . . ?
C31 C30 C18 117.9(5) . . ?
C20 C31 C24 116.6(5) . . ?
C30 C31 C20 119.8(5) . . ?
C30 C31 C24 123.5(5) . . ?
N7 C32 C22 125.2(5) . . ?
N7 C32 H32 117.4 . . ?
C22 C32 H32 117.4 . . ?
O8 C33 H33A 109.5 . . ?
O8 C33 H33B 109.5 . . ?
O8 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C19 C34 C22 119.8(5) . . ?
C19 C34 H34 120.1 . . ?
C22 C34 H34 120.1 . . ?
O14 C46 H46A 109.5 . . ?
O14 C46 H46B 109.5 . . ?
O14 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Br0A C21 C28 C18 -179.8(4) . . . . ?
Ni2 O9 C15 C16 -24.7(5) . . . . ?
Ni2 O9 C15 C29 -144.6(3) . . . . ?
Ni2 O11 C30 C18 -157.4(4) . . . . ?
Ni2 O11 C30 C31 24.4(7) . . . . ?
Ni2 N12 C16 C15 -28.9(5) . . . . ?
Ni2 N12 C24 C31 -5.7(8) . . . . ?
Ni3 O6 C25 C22 1.3(7) . . . . ?
Ni3 O6 C25 C27 -177.9(3) . . . . ?
Ni3 N7 C29 C15 -37.5(5) . . . . ?
Ni3 N7 C32 C22 5.7(8) . . . . ?
Ni3 O8 C18 C28 -162.5(5) 5_666 . . . ?
Ni3 O8 C18 C30 17.1(5) 5_666 . . . ?
Ni3 O9 C15 C16 81.1(5) . . . . ?
Ni3 O9 C15 C29 -38.8(4) . . . . ?
Ni3 O11 C30 C18 -23.3(6) 5_666 . . . ?
Ni3 O11 C30 C31 158.5(4) 5_666 . . . ?
Br4 C19 C26 C27 -174.5(4) . . . . ?
Br4 C19 C34 C22 173.1(4) . . . . ?
O5 Ni2 O5 Ni2 0.0 5_666 . . 5_666 ?
O5 Ni2 O5 Ni3 -97.71(16) 5_666 . . . ?
O5 Ni2 O5 C17 130.2(4) 5_666 . . . ?
O5 Ni2 O9 Ni3 -9.50(14) . . . . ?
O5 Ni2 O9 Ni3 72.45(17) 5_666 . . . ?
O5 Ni2 O9 C15 104.4(3) . . . . ?
O5 Ni2 O9 C15 -173.7(3) 5_666 . . . ?
O5 Ni2 O11 Ni3 92.35(16) . . . 5_666 ?
O5 Ni2 O11 Ni3 7.83(15) 5_666 . . 5_666 ?
O5 Ni2 O11 C30 149.9(4) 5_666 . . . ?
O5 Ni2 O11 C30 -125.6(4) . . . . ?
O5 Ni2 N12 C16 -162.3(8) 5_666 . . . ?
O5 Ni2 N12 C16 -68.2(4) . . . . ?
O5 Ni2 N12 C24 16.4(12) 5_666 . . . ?
O5 Ni2 N12 C24 110.5(5) . . . . ?
O5 Ni2 O14 C46 155.0(10) . . . . ?
O5 Ni2 O14 C46 160.5(8) 5_666 . . . ?
O5 Ni3 O6 C25 119.3(4) . . . . ?
O5 Ni3 N7 C29 90.3(4) . . . . ?
O5 Ni3 N7 C32 -97.7(5) . . . . ?
O5 Ni3 O9 Ni2 9.53(14) . . . . ?
O5 Ni3 O9 C15 -105.4(3) . . . . ?
O6 Ni3 O5 Ni2 84.56(16) . . . 5_666 ?
O6 Ni3 O5 Ni2 -179.01(14) . . . . ?
O6 Ni3 O5 C17 -48.1(4) . . . . ?
O6 Ni3 N7 C29 -176.5(4) . . . . ?
O6 Ni3 N7 C32 -4.5(5) . . . . ?
O6 Ni3 O9 Ni2 69.2(7) . . . . ?
O6 Ni3 O9 C15 -45.7(8) . . . . ?
O6 C25 C27 O10 0.1(7) . . . . ?
O6 C25 C27 C26 179.0(5) . . . . ?
N7 Ni3 O5 Ni2 -86.1(2) . . . . ?
N7 Ni3 O5 Ni2 177.45(17) . . . 5_666 ?
N7 Ni3 O5 C17 44.8(4) . . . . ?
N7 Ni3 O6 C25 1.1(4) . . . . ?
N7 Ni3 O9 Ni2 129.58(18) . . . . ?
N7 Ni3 O9 C15 14.7(3) . . . . ?
O8 Ni3 O5 Ni2 99.8(3) 5_666 . . . ?
O8 Ni3 O5 Ni2 3.4(4) 5_666 . . 5_666 ?
O8 Ni3 O5 C17 -129.3(4) 5_666 . . . ?
O8 Ni3 O6 C25 -88.5(4) 5_666 . . . ?
O8 Ni3 N7 C29 -92.5(4) 5_666 . . . ?
O8 Ni3 N7 C32 79.5(5) 5_666 . . . ?
O8 Ni3 O9 Ni2 -142.91(13) 5_666 . . . ?
O8 Ni3 O9 C15 102.2(3) 5_666 . . . ?
O8 C18 C28 C21 -178.5(5) . . . . ?
O8 C18 C30 O11 -0.3(7) . . . . ?
O8 C18 C30 C31 178.1(5) . . . . ?
O9 Ni2 O5 Ni2 107.33(15) . . . 5_666 ?
O9 Ni2 O5 Ni3 9.62(14) . . . . ?
O9 Ni2 O5 C17 -122.5(4) . . . . ?
O9 Ni2 O11 Ni3 136.5(7) . . . 5_666 ?
O9 Ni2 O11 C30 -81.4(9) . . . . ?
O9 Ni2 N12 C16 13.1(4) . . . . ?
O9 Ni2 N12 C24 -168.2(5) . . . . ?
O9 Ni2 O14 C46 54.7(8) . . . . ?
O9 Ni3 O5 Ni2 -105.96(16) . . . 5_666 ?
O9 Ni3 O5 Ni2 -9.53(14) . . . . ?
O9 Ni3 O5 C17 121.4(4) . . . . ?
O9 Ni3 O6 C25 60.6(9) . . . . ?
O9 Ni3 N7 C29 14.1(4) . . . . ?
O9 Ni3 N7 C32 -173.9(5) . . . . ?
O9 C15 C16 N12 35.8(6) . . . . ?
O9 C15 C29 N7 50.0(5) . . . . ?
O11 Ni2 O5 Ni2 -80.44(15) . . . 5_666 ?
O11 Ni2 O5 Ni3 -178.15(14) . . . . ?
O11 Ni2 O5 C17 49.7(4) . . . . ?
O11 Ni2 O9 Ni3 -54.2(8) . . . . ?
O11 Ni2 O9 C15 59.6(9) . . . . ?
O11 Ni2 N12 C16 -158.1(4) . . . . ?
O11 Ni2 N12 C24 20.6(5) . . . . ?
O11 Ni2 O14 C46 -119.0(8) . . . . ?
O11 Ni3 O5 Ni2 88.85(16) 5_666 . . . ?
O11 Ni3 O5 Ni2 -7.58(15) 5_666 . . 5_666 ?
O11 Ni3 O5 C17 -140.2(4) 5_666 . . . ?
O11 Ni3 O6 C25 -159.5(4) 5_666 . . . ?
O11 Ni3 N7 C29 -74.9(6) 5_666 . . . ?
O11 Ni3 N7 C32 97.1(7) 5_666 . . . ?
O11 Ni3 O9 Ni2 -70.37(16) 5_666 . . . ?
O11 Ni3 O9 C15 174.7(3) 5_666 . . . ?
O11 C30 C31 C20 178.0(5) . . . . ?
O11 C30 C31 C24 0.2(9) . . . . ?
N12 Ni2 O5 Ni2 -169.09(16) . . . 5_666 ?
N12 Ni2 O5 Ni3 93.20(17) . . . . ?
N12 Ni2 O5 C17 -38.9(4) . . . . ?
N12 Ni2 O9 Ni3 -106.66(18) . . . . ?
N12 Ni2 O9 C15 7.2(3) . . . . ?
N12 Ni2 O11 Ni3 -171.36(19) . . . 5_666 ?
N12 Ni2 O11 C30 -29.3(4) . . . . ?
N12 Ni2 O14 C46 -30.4(8) . . . . ?
N12 C24 C31 C20 171.5(5) . . . . ?
N12 C24 C31 C30 -10.7(9) . . . . ?
O14 Ni2 O5 Ni2 5.5(10) . . . 5_666 ?
O14 Ni2 O5 Ni3 -92.2(9) . . . . ?
O14 Ni2 O5 C17 135.7(9) . . . . ?
O14 Ni2 O9 Ni3 160.49(17) . . . . ?
O14 Ni2 O9 C15 -85.6(3) . . . . ?
O14 Ni2 O11 Ni3 -77.60(19) . . . 5_666 ?
O14 Ni2 O11 C30 64.5(4) . . . . ?
O14 Ni2 N12 C16 112.8(4) . . . . ?
O14 Ni2 N12 C24 -68.5(5) . . . . ?
C16 N12 C24 C31 172.9(5) . . . . ?
C16 C15 C29 N7 -72.6(5) . . . . ?
C18 C30 C31 C20 -0.2(8) . . . . ?
C18 C30 C31 C24 -178.0(5) . . . . ?
C19 C26 C27 O10 -179.5(5) . . . . ?
C19 C26 C27 C25 1.7(8) . . . . ?
C20 C21 C28 C18 1.1(8) . . . . ?
C21 C20 C31 C24 -179.0(5) . . . . ?
C21 C20 C31 C30 3.1(8) . . . . ?
C22 C25 C27 O10 -179.1(4) . . . . ?
C22 C25 C27 C26 -0.2(8) . . . . ?
C23 O10 C27 C25 -177.9(4) . . . . ?
C23 O10 C27 C26 3.2(7) . . . . ?
C24 N12 C16 C15 152.3(5) . . . . ?
C25 C22 C32 N7 -2.3(9) . . . . ?
C25 C22 C34 C19 2.0(8) . . . . ?
C26 C19 C34 C22 -0.5(9) . . . . ?
C28 C18 C30 O11 179.4(5) . . . . ?
C28 C18 C30 C31 -2.3(8) . . . . ?
C29 N7 C32 C22 177.1(5) . . . . ?
C29 C15 C16 N12 156.3(4) . . . . ?
C30 C18 C28 C21 1.9(8) . . . . ?
C31 C20 C21 Br0A 177.3(4) . . . . ?
C31 C20 C21 C28 -3.6(8) . . . . ?
C32 N7 C29 C15 149.9(5) . . . . ?
C32 C22 C25 O6 -1.4(8) . . . . ?
C32 C22 C25 C27 177.9(5) . . . . ?
C32 C22 C34 C19 -177.5(5) . . . . ?
C33 O8 C18 C28 -12.2(8) . . . . ?
C33 O8 C18 C30 167.4(5) . . . . ?
C34 C19 C26 C27 -1.3(9) . . . . ?
C34 C22 C25 O6 179.2(5) . . . . ?
C34 C22 C25 C27 -1.6(7) . . . . ?
C34 C22 C32 N7 177.2(5) . . . . ?
Br1 C19 C26 C27 173.5(4) . . . . ?
Br1 C19 C34 C22 -174.8(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
