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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_CoChrys-1
_database_code_depnum_ccdc_archive 'CCDC 1044027'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2016-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        
"dodeca(acetato)-hexa(chrysazinato)-hexa(N,N-dimethylformamide)-dodeca-cobalt(II) hexa(N,N'-dimethylformamide) solvate"
_chemical_formula_moiety         'C126 H114 Co12 N6 O54'
_chemical_formula_sum            'C144 H156 Co12 N12 O60'
_chemical_formula_weight         3721.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Co12 C141 H149 N11 O59'
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   28.6873(9)
_cell_length_b                   28.6873(9)
_cell_length_c                   15.9087(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11338.2(10)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      24.6250
_cell_measurement_theta_min      2.0780
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.377
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             5724
_exptl_crystal_size_max          0.1896
_exptl_crystal_size_mid          0.1651
_exptl_crystal_size_min          0.1012
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17691
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.166
_diffrn_reflns_theta_min         2.080
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9028
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0228332000
_diffrn_orient_matrix_UB_12      0.0176141000
_diffrn_orient_matrix_UB_13      -0.0243408000
_diffrn_orient_matrix_UB_21      0.0161368000
_diffrn_orient_matrix_UB_22      -0.0072435000
_diffrn_orient_matrix_UB_23      0.0242296000
_diffrn_orient_matrix_UB_31      -0.0057589000
_diffrn_orient_matrix_UB_32      -0.0212763000
_diffrn_orient_matrix_UB_33      -0.0284412000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3063
_reflns_number_total             5582
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5582
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0538
_refine_ls_restrained_S_all      0.901
_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)+(0.0619P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1331
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim C1: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.001
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C19(H19)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.68000(2) 0.12675(2) 0.33979(4) 0.03107(18) Uani 1 1 d . . . . .
Co2 Co 0.77841(2) 0.23797(2) 0.35867(4) 0.03153(18) Uani 1 1 d . . . . .
O1 O 0.71247(11) 0.18589(11) 0.43026(18) 0.0338(6) Uani 1 1 d . U . . .
O2 O 0.61005(11) 0.10841(11) 0.40355(19) 0.0302(7) Uani 1 1 d . . . . .
O3 O 0.50359(11) 0.07990(11) 0.3780(2) 0.0333(7) Uani 1 1 d . . . . .
O4 O 0.57542(16) 0.08183(15) 0.7334(2) 0.0731(12) Uani 1 1 d . . . . .
O5 O 0.65233(11) 0.17243(11) 0.26886(18) 0.0315(7) Uani 1 1 d . . . . .
O6 O 0.72657(11) 0.25293(11) 0.28332(19) 0.0348(7) Uani 1 1 d . . . . .
O7 O 0.63998(11) 0.06530(11) 0.25945(19) 0.0350(7) Uani 1 1 d . . . . .
O8 O 0.56424(11) 0.06636(11) 0.22947(19) 0.0354(7) Uani 1 1 d . . . . .
O9 O 0.69557(12) 0.07730(11) 0.4178(2) 0.0387(8) Uani 1 1 d . . . . .
N1 N 0.74662(15) 0.08094(15) 0.5294(3) 0.0421(10) Uani 1 1 d . . . . .
C1 C 0.69995(17) 0.17544(17) 0.5095(3) 0.0349(8) Uani 1 1 d . U . . .
C2 C 0.74061(19) 0.2015(2) 0.5710(3) 0.0488(13) Uani 1 1 d . . . . .
H2 H 0.7753 0.2267 0.5541 0.059 Uiso 1 1 calc R U . . .
C3 C 0.7300(2) 0.1905(3) 0.6547(4) 0.0636(16) Uani 1 1 d . . . . .
H3 H 0.7577 0.2082 0.6933 0.076 Uiso 1 1 calc R U . . .
C4 C 0.6789(2) 0.1536(2) 0.6836(3) 0.0554(14) Uani 1 1 d . . . . .
H4 H 0.6729 0.1456 0.7405 0.066 Uiso 1 1 calc R U . . .
C5 C 0.6372(2) 0.12893(19) 0.6266(3) 0.0444(12) Uani 1 1 d . . . . .
C6 C 0.5828(2) 0.09289(19) 0.6578(3) 0.0494(14) Uani 1 1 d . . . . .
C7 C 0.5377(2) 0.07248(18) 0.5995(3) 0.0415(12) Uani 1 1 d . . . . .
C8 C 0.4859(2) 0.04105(18) 0.6302(3) 0.0481(14) Uani 1 1 d . . . . .
H8 H 0.4807 0.0328 0.6872 0.058 Uiso 1 1 calc R U . . .
C9 C 0.4415(2) 0.02161(18) 0.5765(3) 0.0458(13) Uani 1 1 d . . . . .
H9 H 0.4069 -0.0001 0.5973 0.055 Uiso 1 1 calc R U . . .
C10 C 0.44942(18) 0.03477(17) 0.4933(3) 0.0390(12) Uani 1 1 d . . . . .
H10 H 0.4196 0.0217 0.4582 0.047 Uiso 1 1 calc R U . . .
C11 C 0.50098(17) 0.06737(16) 0.4582(3) 0.0336(11) Uani 1 1 d . . . . .
C12 C 0.54606(18) 0.08472(15) 0.5116(3) 0.0328(11) Uani 1 1 d . . . . .
C13 C 0.60142(17) 0.11071(16) 0.4806(3) 0.0313(10) Uani 1 1 d . . . . .
C14 C 0.64701(18) 0.13808(17) 0.5388(3) 0.0354(11) Uani 1 1 d . . . . .
C15 C 0.67935(17) 0.22412(17) 0.2598(3) 0.0328(10) Uani 1 1 d . . . . .
C16 C 0.65114(19) 0.25008(18) 0.2169(3) 0.0480(13) Uani 1 1 d . . . . .
H16A H 0.6369 0.2638 0.2586 0.072 Uiso 1 1 calc R U . . .
H16B H 0.6222 0.2238 0.1829 0.072 Uiso 1 1 calc R U . . .
H16C H 0.6763 0.2791 0.1820 0.072 Uiso 1 1 calc R U . . .
C17 C 0.59812(18) 0.05128(17) 0.2167(3) 0.0330(11) Uani 1 1 d . . . . .
C18 C 0.5866(2) 0.0120(2) 0.1458(3) 0.0543(14) Uani 1 1 d . . . . .
H18A H 0.6200 0.0177 0.1226 0.081 Uiso 1 1 calc R U . . .
H18B H 0.5663 0.0175 0.1030 0.081 Uiso 1 1 calc R U . . .
H18C H 0.5663 -0.0241 0.1669 0.081 Uiso 1 1 calc R U . . .
C19 C 0.73964(19) 0.09674(18) 0.4557(3) 0.0388(11) Uani 1 1 d . . . . .
H19 H 0.7697 0.1245 0.4295 0.047 Uiso 1 1 calc R U . . .
C20 C 0.79932(19) 0.1073(2) 0.5698(3) 0.0556(15) Uani 1 1 d . . . . .
H20A H 0.8252 0.1346 0.5331 0.083 Uiso 1 1 calc R U . . .
H20B H 0.8101 0.0812 0.5814 0.083 Uiso 1 1 calc R U . . .
H20C H 0.7974 0.1236 0.6215 0.083 Uiso 1 1 calc R U . . .
C21 C 0.7028(2) 0.0414(2) 0.5788(4) 0.0661(17) Uani 1 1 d . . . . .
H21A H 0.6972 0.0585 0.6265 0.099 Uiso 1 1 calc R U . . .
H21B H 0.7111 0.0146 0.5977 0.099 Uiso 1 1 calc R U . . .
H21C H 0.6707 0.0246 0.5452 0.099 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.058(3) . ?
Co1 O2 2.068(3) . ?
Co1 O3 2.084(3) 18_545 ?
Co1 O5 2.159(3) . ?
Co1 O7 2.009(3) . ?
Co1 O9 2.095(3) . ?
Co2 O1 2.069(3) . ?
Co2 O2 2.092(3) 18_545 ?
Co2 O3 2.048(3) 18_545 ?
Co2 O5 2.113(3) 18_545 ?
Co2 O6 2.115(3) . ?
Co2 O8 2.050(3) 18_545 ?
O1 C1 1.304(5) . ?
O2 Co2 2.092(3) 17 ?
O2 C13 1.258(5) . ?
O3 Co1 2.084(3) 17 ?
O3 Co2 2.048(3) 17 ?
O3 C11 1.319(5) . ?
O4 C6 1.234(6) . ?
O5 Co2 2.114(3) 17 ?
O5 C15 1.293(5) . ?
O6 C15 1.241(5) . ?
O7 C17 1.258(5) . ?
O8 Co2 2.050(3) 17 ?
O8 C17 1.263(5) . ?
O9 C19 1.252(5) . ?
N1 C19 1.308(6) . ?
N1 C20 1.459(6) . ?
N1 C21 1.435(6) . ?
C1 C2 1.416(6) . ?
C1 C14 1.430(6) . ?
C2 H2 0.9300 . ?
C2 C3 1.367(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.388(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.380(7) . ?
C5 C6 1.462(7) . ?
C5 C14 1.423(6) . ?
C6 C7 1.457(7) . ?
C7 C8 1.384(6) . ?
C7 C12 1.431(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.397(7) . ?
C9 H9 0.9300 . ?
C9 C10 1.364(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.411(6) . ?
C11 C12 1.414(6) . ?
C12 C13 1.462(6) . ?
C13 C14 1.469(6) . ?
C15 C16 1.509(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.509(6) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
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 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O2 81.28(11) . . ?
O1 Co1 O3 82.62(11) . 18_545 ?
O1 Co1 O5 91.00(11) . . ?
O1 Co1 O9 88.96(12) . . ?
O2 Co1 O3 161.27(11) . 18_545 ?
O2 Co1 O5 78.83(11) . . ?
O2 Co1 O9 92.60(12) . . ?
O3 Co1 O5 91.96(11) 18_545 . ?
O3 Co1 O9 96.63(12) 18_545 . ?
O7 Co1 O1 173.08(12) . . ?
O7 Co1 O2 91.88(11) . . ?
O7 Co1 O3 104.30(12) . 18_545 ?
O7 Co1 O5 88.74(11) . . ?
O7 Co1 O9 90.26(12) . . ?
O9 Co1 O5 171.33(11) . . ?
O1 Co2 O2 165.91(12) . 18_545 ?
O1 Co2 O5 113.00(11) . 18_545 ?
O1 Co2 O6 88.67(11) . . ?
O2 Co2 O5 79.34(11) 18_545 18_545 ?
O2 Co2 O6 85.27(11) 18_545 . ?
O3 Co2 O1 83.23(11) 18_545 . ?
O3 Co2 O2 83.92(11) 18_545 18_545 ?
O3 Co2 O5 162.88(12) 18_545 18_545 ?
O3 Co2 O6 88.68(11) 18_545 . ?
O3 Co2 O8 97.07(11) 18_545 18_545 ?
O5 Co2 O6 86.41(11) 18_545 . ?
O8 Co2 O1 92.70(11) 18_545 . ?
O8 Co2 O2 94.60(11) 18_545 18_545 ?
O8 Co2 O5 87.87(11) 18_545 18_545 ?
O8 Co2 O6 174.20(11) 18_545 . ?
Co1 O1 Co2 94.81(12) . . ?
C1 O1 Co1 121.8(3) . . ?
C1 O1 Co2 138.2(3) . . ?
Co1 O2 Co2 98.51(12) . 17 ?
C13 O2 Co1 131.0(3) . . ?
C13 O2 Co2 123.5(3) . 17 ?
Co2 O3 Co1 94.66(12) 17 17 ?
C11 O3 Co1 122.5(3) . 17 ?
C11 O3 Co2 127.5(3) . 17 ?
Co2 O5 Co1 95.06(11) 17 . ?
C15 O5 Co1 124.3(3) . . ?
C15 O5 Co2 126.4(3) . 17 ?
C15 O6 Co2 132.9(3) . . ?
C17 O7 Co1 131.3(3) . . ?
C17 O8 Co2 127.9(3) . 17 ?
C19 O9 Co1 119.6(3) . . ?
C19 N1 C20 120.9(4) . . ?
C19 N1 C21 122.6(4) . . ?
C21 N1 C20 116.2(4) . . ?
O1 C1 C2 119.2(4) . . ?
O1 C1 C14 123.7(4) . . ?
C2 C1 C14 117.1(4) . . ?
C1 C2 H2 119.3 . . ?
C3 C2 C1 121.4(5) . . ?
C3 C2 H2 119.3 . . ?
C2 C3 H3 119.1 . . ?
C2 C3 C4 121.8(5) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.2(5) . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 119.0(5) . . ?
C4 C5 C14 120.6(5) . . ?
C14 C5 C6 120.4(5) . . ?
O4 C6 C5 119.8(5) . . ?
O4 C6 C7 120.9(5) . . ?
C7 C6 C5 119.2(5) . . ?
C8 C7 C6 119.0(5) . . ?
C8 C7 C12 119.9(5) . . ?
C12 C7 C6 121.1(4) . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.7(5) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.4(5) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 118.6 . . ?
C9 C10 C11 122.7(5) . . ?
C11 C10 H10 118.6 . . ?
O3 C11 C10 117.4(4) . . ?
O3 C11 C12 124.7(4) . . ?
C10 C11 C12 117.9(4) . . ?
C7 C12 C13 117.5(4) . . ?
C11 C12 C7 119.2(4) . . ?
C11 C12 C13 123.1(4) . . ?
O2 C13 C12 119.6(4) . . ?
O2 C13 C14 119.8(4) . . ?
C12 C13 C14 120.6(4) . . ?
C1 C14 C13 121.5(4) . . ?
C5 C14 C1 119.7(4) . . ?
C5 C14 C13 118.6(4) . . ?
O5 C15 C16 117.1(4) . . ?
O6 C15 O5 124.0(4) . . ?
O6 C15 C16 119.0(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O7 C17 O8 125.4(4) . . ?
O7 C17 C18 117.4(4) . . ?
O8 C17 C18 117.2(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O9 C19 N1 124.9(5) . . ?
O9 C19 H19 117.5 . . ?
N1 C19 H19 117.5 . . ?
N1 C20 H20A 109.5 . . ?
N1 C20 H20B 109.5 . . ?
N1 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N1 C21 H21A 109.5 . . ?
N1 C21 H21B 109.5 . . ?
N1 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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 O1 C1 C2 140.9(4) . . . . ?
Co1 O1 C1 C14 -38.2(5) . . . . ?
Co1 O2 C13 C12 -167.1(3) . . . . ?
Co1 O2 C13 C14 11.2(6) . . . . ?
Co1 O3 C11 C10 52.1(4) 17 . . . ?
Co1 O3 C11 C12 -127.2(4) 17 . . . ?
Co1 O5 C15 O6 7.8(6) . . . . ?
Co1 O5 C15 C16 -172.9(3) . . . . ?
Co1 O7 C17 O8 -17.4(7) . . . . ?
Co1 O7 C17 C18 164.4(3) . . . . ?
Co1 O9 C19 N1 148.0(4) . . . . ?
Co2 O1 C1 C2 -6.5(7) . . . . ?
Co2 O1 C1 C14 174.4(3) . . . . ?
Co2 O2 C13 C12 48.8(5) 17 . . . ?
Co2 O2 C13 C14 -133.0(3) 17 . . . ?
Co2 O3 C11 C10 179.8(3) 17 . . . ?
Co2 O3 C11 C12 0.5(6) 17 . . . ?
Co2 O5 C15 O6 137.2(4) 17 . . . ?
Co2 O5 C15 C16 -43.5(5) 17 . . . ?
Co2 O6 C15 O5 -10.3(7) . . . . ?
Co2 O6 C15 C16 170.3(3) . . . . ?
Co2 O8 C17 O7 10.9(7) 17 . . . ?
Co2 O8 C17 C18 -170.8(3) 17 . . . ?
O1 C1 C2 C3 -177.6(5) . . . . ?
O1 C1 C14 C5 179.5(4) . . . . ?
O1 C1 C14 C13 -3.8(6) . . . . ?
O2 C13 C14 C1 18.7(6) . . . . ?
O2 C13 C14 C5 -164.5(4) . . . . ?
O3 C11 C12 C7 174.3(4) . . . . ?
O3 C11 C12 C13 -11.3(6) . . . . ?
O4 C6 C7 C8 1.1(7) . . . . ?
O4 C6 C7 C12 -179.3(4) . . . . ?
C1 C2 C3 C4 -0.4(9) . . . . ?
C2 C1 C14 C5 0.4(6) . . . . ?
C2 C1 C14 C13 177.2(4) . . . . ?
C2 C3 C4 C5 -2.7(9) . . . . ?
C3 C4 C5 C6 -175.9(5) . . . . ?
C3 C4 C5 C14 4.6(8) . . . . ?
C4 C5 C6 O4 -5.4(7) . . . . ?
C4 C5 C6 C7 171.8(5) . . . . ?
C4 C5 C14 C1 -3.5(7) . . . . ?
C4 C5 C14 C13 179.7(4) . . . . ?
C5 C6 C7 C8 -176.1(4) . . . . ?
C5 C6 C7 C12 3.5(7) . . . . ?
C6 C5 C14 C1 177.0(4) . . . . ?
C6 C5 C14 C13 0.1(6) . . . . ?
C6 C7 C8 C9 178.7(5) . . . . ?
C6 C7 C12 C11 -175.4(4) . . . . ?
C6 C7 C12 C13 9.8(6) . . . . ?
C7 C8 C9 C10 -1.4(7) . . . . ?
C7 C12 C13 O2 159.6(4) . . . . ?
C7 C12 C13 C14 -18.6(6) . . . . ?
C8 C7 C12 C11 4.1(6) . . . . ?
C8 C7 C12 C13 -170.6(4) . . . . ?
C8 C9 C10 C11 0.2(7) . . . . ?
C9 C10 C11 O3 -176.4(4) . . . . ?
C9 C10 C11 C12 3.0(6) . . . . ?
C10 C11 C12 C7 -5.1(6) . . . . ?
C10 C11 C12 C13 169.3(4) . . . . ?
C11 C12 C13 O2 -14.9(6) . . . . ?
C11 C12 C13 C14 166.9(4) . . . . ?
C12 C7 C8 C9 -0.8(7) . . . . ?
C12 C13 C14 C1 -163.1(4) . . . . ?
C12 C13 C14 C5 13.7(6) . . . . ?
C14 C1 C2 C3 1.5(7) . . . . ?
C14 C5 C6 O4 174.1(5) . . . . ?
C14 C5 C6 C7 -8.6(7) . . . . ?
C20 N1 C19 O9 -177.9(4) . . . . ?
C21 N1 C19 O9 -4.9(7) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-23 37 9 0.0960 -22.9993 36.9671 9.0203 -0.0936 -0.4203 -0.9106
-18 21 19 0.0551 -17.9571 21.4557 19.0049 -0.4947 0.0153 -0.8936
22 3 16 0.0674 22.0197 3.0285 15.9781 0.1672 0.7205 -0.6457
16 -9 -21 0.0371 15.9386 -9.4496 -20.9979 0.7086 -0.1831 0.7065
-15 17 20 0.0559 -14.9523 17.4581 20.0011 -0.5207 0.1169 -0.8542
6 -25 17 0.0557 6.0716 -24.5232 16.9758 -0.7065 0.6869 0.0040
-1 22 -18 0.0427 -1.0754 21.5326 -17.9790 0.7923 -0.6089 0.0594
17 -3 20 0.0492 17.0429 -2.9901 19.9758 -0.1498 0.7807 -0.6027
-23 -9 13 0.0854 -22.9312 -9.0676 13.0003 -0.9997 0.0106 -0.0448
-25 0 -16 0.0459 -25.0206 -0.0327 -15.9753 -0.1830 -0.7906 0.5991
30 -37 -5 0.0594 30.0036 -36.9574 -5.0269 0.1565 0.6301 0.7565

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.500 859 186 'DMF, about 5 molecules'
2 0.333 0.667 1.167 855 185 'DMF, about 5 molecules'
3 0.667 0.333 0.833 855 185 'DMF, about 5 molecules'
_platon_squeeze_details          
;
;

_vrf_CHEMW03_CoChrys-1           
;
RESPONSE:
Due to the inclusion of disordered solvent removed by SQUEEZE.
;
####################################################################### 
# 
# 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_CoChrys-2
_database_code_depnum_ccdc_archive 'CCDC 1044028'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2014-09-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2013-4
_chemical_name_systematic        
'di(acetato)-di(chrysazinato)-pyridine-tri(N,N-dimethylformamide)-dodeca-cobalt(II) hexa(N,N-dimethylformamide) solvate'
_chemical_name_common            ?
_chemical_formula_moiety         'C46 H44 Co3 N4 O15'
_chemical_formula_sum            'C46 H44 Co3 N4 O15'
_chemical_formula_weight         1069.64
_chemical_melting_point          ?
_exptl_crystal_description       block
_diffrn_ambient_temperature      121(1)
_chemical_oxdiff_formula         'Co3 C44 H44 O15 N4'
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'
Co Co 0.3494 0.9721 '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                   12.3354(5)
_cell_length_b                   12.8534(7)
_cell_length_c                   14.3146(5)
_cell_angle_alpha                91.265(4)
_cell_angle_beta                 97.978(3)
_cell_angle_gamma                94.724(4)
_cell_volume                     2238.72(18)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7211
_cell_measurement_temperature    121(1)
_cell_measurement_theta_max      27.7860
_cell_measurement_theta_min      2.0370
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1098
_exptl_crystal_size_max          0.3417
_exptl_crystal_size_mid          0.2835
_exptl_crystal_size_min          0.0707
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17016
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.591
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.9995
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0004975000
_diffrn_orient_matrix_UB_12      -0.0552111000
_diffrn_orient_matrix_UB_13      -0.0026400000
_diffrn_orient_matrix_UB_21      -0.0552640000
_diffrn_orient_matrix_UB_22      -0.0046117000
_diffrn_orient_matrix_UB_23      0.0090329000
_diffrn_orient_matrix_UB_31      -0.0184997000
_diffrn_orient_matrix_UB_32      0.0002021000
_diffrn_orient_matrix_UB_33      -0.0491717000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          ?
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7460
_reflns_number_total             8806
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_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       
;
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    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         8806
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0298
_refine_ls_restrained_S_all      1.020
_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)+(0.0300P)²+1.1385P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0722
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C17(H17), C27(H27), C29(H29), C44(H44), C18(H18), C6(H6), C2(H2),
 C14(H14), C13(H13), C16(H16), C28(H28), C12(H12), C41(H41), C25(H25), C1(H1),
 C38(H38), C39(H39), C37(H37), C40(H40)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C30(H30A,H30B,
 H30C), C36(H36A,H36B,H36C), C33(H33A,H33B,H33C), C43(H43A,H43B,H43C), C32(H32A,
 H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.87481(2) 0.22455(2) 0.25120(2) 0.01402(7) Uani 1 1 d . . . . .
Co2 Co 0.75670(2) 0.42333(2) 0.28014(2) 0.01547(7) Uani 1 1 d . . . . .
Co3 Co 0.79265(2) 0.00637(2) 0.16804(2) 0.01434(7) Uani 1 1 d . . . . .
O1 O 0.75887(11) 0.32072(11) 0.16264(9) 0.0154(3) Uani 1 1 d . . . . .
O2 O 0.86463(11) 0.14728(11) 0.12992(9) 0.0153(3) Uani 1 1 d . . . . .
O3 O 0.66414(13) 0.35905(12) -0.21213(10) 0.0249(4) Uani 1 1 d . . . . .
O4 O 0.69054(13) 0.52068(11) 0.18903(10) 0.0209(3) Uani 1 1 d . . . . .
O5 O 0.80760(12) 0.29354(11) 0.35044(9) 0.0160(3) Uani 1 1 d . . . . .
O6 O 0.75083(11) 0.09630(11) 0.27875(9) 0.0156(3) Uani 1 1 d . . . . .
O7 O 0.70973(12) -0.11223(11) 0.21755(10) 0.0191(3) Uani 1 1 d . . . . .
O8 O 0.65245(11) 0.05003(11) 0.07482(10) 0.0185(3) Uani 1 1 d . . . . .
O9 O 0.77536(12) 0.53714(11) 0.39127(10) 0.0206(3) Uani 1 1 d . . . . .
O10 O 0.91543(12) 0.48121(11) 0.26174(11) 0.0221(3) Uani 1 1 d . . . . .
O11 O 0.99618(12) 0.33654(11) 0.23244(10) 0.0195(3) Uani 1 1 d . . . . .
O12 O 0.94107(12) -0.01986(11) 0.24962(10) 0.0189(3) Uani 1 1 d . . . . .
O13 O 0.98561(12) 0.13671(11) 0.32483(10) 0.0211(3) Uani 1 1 d . . . . .
O14 O 0.82312(12) -0.09367(11) 0.05843(10) 0.0194(3) Uani 1 1 d . . . . .
O15 O 0.60571(14) -0.01054(13) 0.60652(11) 0.0285(4) Uani 1 1 d . . . . .
N1 N 0.57592(14) 0.08199(13) -0.07472(12) 0.0183(4) Uani 1 1 d . . . . .
N2 N 0.88386(16) 0.68400(14) 0.44247(13) 0.0241(4) Uani 1 1 d . . . . .
N3 N 0.59197(15) 0.37293(14) 0.30568(12) 0.0200(4) Uani 1 1 d . . . . .
N4 N 0.86479(15) -0.25165(14) 0.00864(13) 0.0228(4) Uani 1 1 d . . . . .
C1 C 0.72519(19) 0.29603(18) 0.58248(15) 0.0233(5) Uani 1 1 d . . . . .
H1 H 0.7244 0.3449 0.6312 0.028 Uiso 1 1 calc R U . . .
C2 C 0.76710(18) 0.32540(17) 0.50190(15) 0.0206(5) Uani 1 1 d . . . . .
H2 H 0.7956 0.3941 0.4975 0.025 Uiso 1 1 calc R U . . .
C3 C 0.76804(17) 0.25428(16) 0.42582(14) 0.0164(4) Uani 1 1 d . . . . .
C4 C 0.72647(16) 0.14845(16) 0.43329(14) 0.0150(4) Uani 1 1 d . . . . .
C5 C 0.68534(17) 0.12094(17) 0.51866(14) 0.0178(4) Uani 1 1 d . . . . .
C6 C 0.68415(18) 0.19359(17) 0.59106(15) 0.0213(5) Uani 1 1 d . . . . .
H6 H 0.6558 0.1737 0.6455 0.026 Uiso 1 1 calc R U . . .
C7 C 0.64046(17) 0.01283(18) 0.53259(15) 0.0204(5) Uani 1 1 d . . . . .
C8 C 0.63896(17) -0.06600(17) 0.45570(15) 0.0184(4) Uani 1 1 d . . . . .
C9 C 0.68080(16) -0.03962(16) 0.36992(14) 0.0161(4) Uani 1 1 d . . . . .
C10 C 0.72133(16) 0.06852(16) 0.35669(14) 0.0147(4) Uani 1 1 d . . . . .
C11 C 0.67575(16) -0.12123(16) 0.29865(14) 0.0164(4) Uani 1 1 d . . . . .
C12 C 0.62723(18) -0.22229(17) 0.31752(16) 0.0219(5) Uani 1 1 d . . . . .
H12 H 0.6227 -0.2756 0.2718 0.026 Uiso 1 1 calc R U . . .
C13 C 0.5875(2) -0.24336(18) 0.39982(17) 0.0267(5) Uani 1 1 d . . . . .
H13 H 0.5559 -0.3099 0.4092 0.032 Uiso 1 1 calc R U . . .
C14 C 0.59405(19) -0.16511(18) 0.47017(16) 0.0243(5) Uani 1 1 d . . . . .
H14 H 0.5681 -0.1799 0.5268 0.029 Uiso 1 1 calc R U . . .
C15 C 0.85025(16) 0.17985(15) 0.04146(14) 0.0140(4) Uani 1 1 d . . . . .
C16 C 0.89557(17) 0.12118(16) -0.02501(14) 0.0171(4) Uani 1 1 d . . . . .
H16 H 0.9373 0.0670 -0.0041 0.021 Uiso 1 1 calc R U . . .
C17 C 0.88078(17) 0.14067(16) -0.11968(14) 0.0179(4) Uani 1 1 d . . . . .
H17 H 0.9134 0.1014 -0.1616 0.021 Uiso 1 1 calc R U . . .
C18 C 0.81632(17) 0.21993(16) -0.15213(14) 0.0178(4) Uani 1 1 d . . . . .
H18 H 0.8028 0.2318 -0.2164 0.021 Uiso 1 1 calc R U . . .
C19 C 0.77246(16) 0.28100(15) -0.08864(14) 0.0146(4) Uani 1 1 d . . . . .
C20 C 0.79134(16) 0.26640(15) 0.01051(14) 0.0132(4) Uani 1 1 d . . . . .
C21 C 0.74851(16) 0.33900(15) 0.07540(14) 0.0134(4) Uani 1 1 d . . . . .
C22 C 0.69799(16) 0.43122(15) 0.03845(14) 0.0142(4) Uani 1 1 d . . . . .
C23 C 0.67192(17) 0.44045(16) -0.06134(14) 0.0165(4) Uani 1 1 d . . . . .
C24 C 0.69968(17) 0.36029(16) -0.12761(14) 0.0175(4) Uani 1 1 d . . . . .
C25 C 0.62126(18) 0.52402(17) -0.10072(15) 0.0203(5) Uani 1 1 d . . . . .
H25 H 0.6036 0.5267 -0.1659 0.024 Uiso 1 1 calc R U . . .
C26 C 0.67196(17) 0.51423(16) 0.09840(14) 0.0166(4) Uani 1 1 d . . . . .
C27 C 0.62174(18) 0.60030(17) 0.05343(15) 0.0201(5) Uani 1 1 d . . . . .
H27 H 0.6057 0.6553 0.0910 0.024 Uiso 1 1 calc R U . . .
C28 C 0.59658(18) 0.60482(17) -0.04219(16) 0.0228(5) Uani 1 1 d . . . . .
H28 H 0.5630 0.6616 -0.0685 0.027 Uiso 1 1 calc R U . . .
C29 C 0.64083(17) 0.03323(16) -0.01202(15) 0.0168(4) Uani 1 1 d . . . . .
H29 H 0.6809 -0.0176 -0.0346 0.020 Uiso 1 1 calc R U . . .
C30 C 0.51133(18) 0.16380(17) -0.04594(17) 0.0237(5) Uani 1 1 d . . . . .
H30A H 0.5168 0.1671 0.0216 0.036 Uiso 1 1 calc R U . . .
H30B H 0.4358 0.1486 -0.0729 0.036 Uiso 1 1 calc R U . . .
H30C H 0.5388 0.2297 -0.0675 0.036 Uiso 1 1 calc R U . . .
C31 C 0.5644(2) 0.0547(2) -0.17506(16) 0.0277(5) Uani 1 1 d . . . . .
H31A H 0.6216 0.0120 -0.1868 0.042 Uiso 1 1 calc R U . . .
H31B H 0.5697 0.1173 -0.2101 0.042 Uiso 1 1 calc R U . . .
H31C H 0.4941 0.0169 -0.1944 0.042 Uiso 1 1 calc R U . . .
C32 C 0.9010(3) 0.6527(2) 0.54047(17) 0.0423(7) Uani 1 1 d . . . . .
H32A H 0.8483 0.5958 0.5491 0.063 Uiso 1 1 calc R U . . .
H32B H 0.8921 0.7107 0.5813 0.063 Uiso 1 1 calc R U . . .
H32C H 0.9739 0.6311 0.5555 0.063 Uiso 1 1 calc R U . . .
C33 C 0.9380(2) 0.78378(19) 0.42068(19) 0.0365(6) Uani 1 1 d . . . . .
H33A H 1.0160 0.7833 0.4381 0.055 Uiso 1 1 calc R U . . .
H33B H 0.9118 0.8390 0.4553 0.055 Uiso 1 1 calc R U . . .
H33C H 0.9220 0.7948 0.3543 0.055 Uiso 1 1 calc R U . . .
C34 C 0.82502(18) 0.62343(16) 0.37627(15) 0.0195(5) Uani 1 1 d . . . . .
H34 H 0.8196 0.6454 0.3145 0.023 Uiso 1 1 calc R U . . .
C35 C 0.99473(18) 0.43400(17) 0.24110(14) 0.0190(5) Uani 1 1 d . . . . .
C36 C 1.0972(2) 0.50034(19) 0.22555(19) 0.0315(6) Uani 1 1 d . . . . .
H36A H 1.1604 0.4626 0.2434 0.047 Uiso 1 1 calc R U . . .
H36B H 1.1034 0.5638 0.2633 0.047 Uiso 1 1 calc R U . . .
H36C H 1.0928 0.5167 0.1601 0.047 Uiso 1 1 calc R U . . .
C37 C 0.5324(2) 0.4363(2) 0.34823(17) 0.0297(5) Uani 1 1 d . . . . .
H37 H 0.5656 0.5011 0.3713 0.036 Uiso 1 1 calc R U . . .
C38 C 0.4239(2) 0.4111(2) 0.36001(18) 0.0362(6) Uani 1 1 d . . . . .
H38 H 0.3855 0.4577 0.3905 0.043 Uiso 1 1 calc R U . . .
C39 C 0.3741(2) 0.3157(2) 0.32555(19) 0.0370(6) Uani 1 1 d . . . . .
H39 H 0.3010 0.2969 0.3314 0.044 Uiso 1 1 calc R U . . .
C40 C 0.4334(2) 0.2493(2) 0.28288(19) 0.0358(6) Uani 1 1 d . . . . .
H40 H 0.4018 0.1839 0.2600 0.043 Uiso 1 1 calc R U . . .
C41 C 0.5419(2) 0.28028(19) 0.27375(17) 0.0284(5) Uani 1 1 d . . . . .
H41 H 0.5815 0.2343 0.2440 0.034 Uiso 1 1 calc R U . . .
C42 C 1.00184(18) 0.04302(17) 0.30745(15) 0.0190(5) Uani 1 1 d . . . . .
C43 C 1.1035(2) 0.0043(2) 0.36128(19) 0.0341(6) Uani 1 1 d . . . . .
H43A H 1.0962 0.0021 0.4271 0.051 Uiso 1 1 calc R U . . .
H43B H 1.1664 0.0506 0.3531 0.051 Uiso 1 1 calc R U . . .
H43C H 1.1129 -0.0646 0.3380 0.051 Uiso 1 1 calc R U . . .
C44 C 0.85158(17) -0.18258(17) 0.07483(15) 0.0188(4) Uani 1 1 d . . . . .
H44 H 0.8643 -0.2017 0.1374 0.023 Uiso 1 1 calc R U . . .
C45 C 0.8469(2) -0.2266(2) -0.09068(17) 0.0324(6) Uani 1 1 d . . . . .
H45A H 0.7840 -0.2689 -0.1221 0.049 Uiso 1 1 calc R U . . .
H45B H 0.9105 -0.2404 -0.1192 0.049 Uiso 1 1 calc R U . . .
H45C H 0.8343 -0.1542 -0.0963 0.049 Uiso 1 1 calc R U . . .
C46 C 0.9056(2) -0.35209(18) 0.0325(2) 0.0333(6) Uani 1 1 d . . . . .
H46A H 0.9781 -0.3541 0.0159 0.050 Uiso 1 1 calc R U . . .
H46B H 0.8576 -0.4069 -0.0015 0.050 Uiso 1 1 calc R U . . .
H46C H 0.9079 -0.3615 0.0991 0.050 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.2445(14) . ?
Co1 O2 1.9643(14) . ?
Co1 O5 1.9710(14) . ?
Co1 O6 2.2344(14) . ?
Co1 O11 2.0394(15) . ?
Co1 O13 2.0397(14) . ?
Co2 O1 2.1189(14) . ?
Co2 O4 1.9691(14) . ?
Co2 O5 2.0643(14) . ?
Co2 O9 2.1127(14) . ?
Co2 O10 2.0900(15) . ?
Co2 N3 2.1639(18) . ?
Co3 O2 2.0687(14) . ?
Co3 O6 2.0877(14) . ?
Co3 O7 1.9658(15) . ?
Co3 O8 2.1537(14) . ?
Co3 O12 2.0869(14) . ?
Co3 O14 2.1002(14) . ?
O1 C21 1.267(2) . ?
O2 C15 1.335(2) . ?
O3 C24 1.228(2) . ?
O4 C26 1.285(2) . ?
O5 C3 1.337(2) . ?
O6 C10 1.270(2) . ?
O7 C11 1.292(2) . ?
O8 C29 1.243(2) . ?
O9 C34 1.260(3) . ?
O10 C35 1.258(3) . ?
O11 C35 1.258(3) . ?
O12 C42 1.264(3) . ?
O13 C42 1.262(3) . ?
O14 C44 1.241(2) . ?
O15 C7 1.230(2) . ?
N1 C29 1.322(3) . ?
N1 C30 1.456(3) . ?
N1 C31 1.456(3) . ?
N2 C32 1.460(3) . ?
N2 C33 1.457(3) . ?
N2 C34 1.309(3) . ?
N3 C37 1.332(3) . ?
N3 C41 1.336(3) . ?
N4 C44 1.320(3) . ?
N4 C45 1.455(3) . ?
N4 C46 1.454(3) . ?
C1 C2 1.376(3) . ?
C1 C6 1.386(3) . ?
C2 C3 1.408(3) . ?
C3 C4 1.425(3) . ?
C4 C5 1.427(3) . ?
C4 C10 1.477(3) . ?
C5 C6 1.382(3) . ?
C5 C7 1.481(3) . ?
C7 C8 1.477(3) . ?
C8 C9 1.433(3) . ?
C8 C14 1.378(3) . ?
C9 C10 1.463(3) . ?
C9 C11 1.438(3) . ?
C11 C12 1.432(3) . ?
C12 C13 1.362(3) . ?
C13 C14 1.397(3) . ?
C15 C16 1.404(3) . ?
C15 C20 1.424(3) . ?
C16 C17 1.373(3) . ?
C17 C18 1.392(3) . ?
C18 C19 1.382(3) . ?
C19 C20 1.425(3) . ?
C19 C24 1.481(3) . ?
C20 C21 1.481(3) . ?
C21 C22 1.460(3) . ?
C22 C23 1.430(3) . ?
C22 C26 1.439(3) . ?
C23 C24 1.478(3) . ?
C23 C25 1.379(3) . ?
C25 C28 1.399(3) . ?
C26 C27 1.434(3) . ?
C27 C28 1.365(3) . ?
C35 C36 1.511(3) . ?
C37 C38 1.386(3) . ?
C38 C39 1.375(4) . ?
C39 C40 1.356(4) . ?
C40 C41 1.389(3) . ?
C42 C43 1.506(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O1 80.84(5) . . ?
O2 Co1 O5 151.78(6) . . ?
O2 Co1 O6 82.33(5) . . ?
O2 Co1 O11 98.74(6) . . ?
O2 Co1 O13 96.49(6) . . ?
O5 Co1 O1 79.68(5) . . ?
O5 Co1 O6 80.11(5) . . ?
O5 Co1 O11 100.36(6) . . ?
O5 Co1 O13 103.63(6) . . ?
O6 Co1 O1 97.29(5) . . ?
O11 Co1 O1 86.82(6) . . ?
O11 Co1 O6 175.87(6) . . ?
O11 Co1 O13 91.28(6) . . ?
O13 Co1 O1 176.44(6) . . ?
O13 Co1 O6 84.63(6) . . ?
O1 Co2 N3 96.55(6) . . ?
O4 Co2 O1 86.53(6) . . ?
O4 Co2 O5 165.61(6) . . ?
O4 Co2 O9 91.89(6) . . ?
O4 Co2 O10 91.70(6) . . ?
O4 Co2 N3 87.56(7) . . ?
O5 Co2 O1 80.71(5) . . ?
O5 Co2 O9 101.69(6) . . ?
O5 Co2 O10 94.29(6) . . ?
O5 Co2 N3 87.34(6) . . ?
O9 Co2 O1 171.60(6) . . ?
O9 Co2 N3 91.61(6) . . ?
O10 Co2 O1 87.37(6) . . ?
O10 Co2 O9 84.43(6) . . ?
O10 Co2 N3 175.95(6) . . ?
O2 Co3 O6 83.63(5) . . ?
O2 Co3 O8 83.31(5) . . ?
O2 Co3 O12 89.03(6) . . ?
O2 Co3 O14 101.04(6) . . ?
O6 Co3 O8 91.10(5) . . ?
O6 Co3 O14 174.93(6) . . ?
O7 Co3 O2 169.87(6) . . ?
O7 Co3 O6 86.75(6) . . ?
O7 Co3 O8 93.72(6) . . ?
O7 Co3 O12 94.18(6) . . ?
O7 Co3 O14 88.47(6) . . ?
O12 Co3 O6 90.12(6) . . ?
O12 Co3 O8 172.06(6) . . ?
O12 Co3 O14 91.92(6) . . ?
O14 Co3 O8 87.52(5) . . ?
Co2 O1 Co1 90.18(5) . . ?
C21 O1 Co1 131.06(12) . . ?
C21 O1 Co2 129.85(12) . . ?
Co1 O2 Co3 98.63(6) . . ?
C15 O2 Co1 130.92(12) . . ?
C15 O2 Co3 122.53(12) . . ?
C26 O4 Co2 130.34(13) . . ?
Co1 O5 Co2 99.98(6) . . ?
C3 O5 Co1 130.36(12) . . ?
C3 O5 Co2 125.58(12) . . ?
Co3 O6 Co1 90.04(5) . . ?
C10 O6 Co1 129.14(13) . . ?
C10 O6 Co3 130.05(13) . . ?
C11 O7 Co3 129.40(13) . . ?
C29 O8 Co3 122.67(13) . . ?
C34 O9 Co2 116.00(13) . . ?
C35 O10 Co2 130.20(14) . . ?
C35 O11 Co1 127.67(14) . . ?
C42 O12 Co3 127.85(13) . . ?
C42 O13 Co1 127.44(14) . . ?
C44 O14 Co3 120.87(14) . . ?
C29 N1 C30 121.28(18) . . ?
C29 N1 C31 121.44(18) . . ?
C31 N1 C30 117.28(17) . . ?
C33 N2 C32 117.3(2) . . ?
C34 N2 C32 121.4(2) . . ?
C34 N2 C33 121.3(2) . . ?
C37 N3 Co2 121.26(16) . . ?
C37 N3 C41 116.5(2) . . ?
C41 N3 Co2 122.03(15) . . ?
C44 N4 C45 120.92(19) . . ?
C44 N4 C46 121.3(2) . . ?
C46 N4 C45 117.66(19) . . ?
C2 C1 C6 120.0(2) . . ?
C1 C2 C3 121.8(2) . . ?
O5 C3 C2 115.87(19) . . ?
O5 C3 C4 125.04(18) . . ?
C2 C3 C4 119.08(19) . . ?
C3 C4 C5 117.27(18) . . ?
C3 C4 C10 123.26(18) . . ?
C5 C4 C10 119.45(18) . . ?
C4 C5 C7 121.00(19) . . ?
C6 C5 C4 121.8(2) . . ?
C6 C5 C7 117.16(19) . . ?
C5 C6 C1 120.0(2) . . ?
O15 C7 C5 120.7(2) . . ?
O15 C7 C8 121.0(2) . . ?
C8 C7 C5 118.31(18) . . ?
C9 C8 C7 121.26(19) . . ?
C14 C8 C7 116.70(19) . . ?
C14 C8 C9 122.0(2) . . ?
C8 C9 C10 119.31(19) . . ?
C8 C9 C11 117.53(19) . . ?
C11 C9 C10 123.10(18) . . ?
O6 C10 C4 118.49(18) . . ?
O6 C10 C9 120.95(18) . . ?
C9 C10 C4 120.55(18) . . ?
O7 C11 C9 126.23(19) . . ?
O7 C11 C12 115.97(19) . . ?
C12 C11 C9 117.79(19) . . ?
C13 C12 C11 122.6(2) . . ?
C12 C13 C14 120.0(2) . . ?
C8 C14 C13 120.1(2) . . ?
O2 C15 C16 116.01(18) . . ?
O2 C15 C20 125.11(17) . . ?
C16 C15 C20 118.87(18) . . ?
C17 C16 C15 122.62(19) . . ?
C16 C17 C18 119.22(19) . . ?
C19 C18 C17 119.85(19) . . ?
C18 C19 C20 122.20(19) . . ?
C18 C19 C24 117.44(18) . . ?
C20 C19 C24 120.30(18) . . ?
C15 C20 C19 116.92(17) . . ?
C15 C20 C21 123.45(18) . . ?
C19 C20 C21 119.62(17) . . ?
O1 C21 C20 118.93(17) . . ?
O1 C21 C22 121.32(18) . . ?
C22 C21 C20 119.73(17) . . ?
C23 C22 C21 119.44(18) . . ?
C23 C22 C26 117.77(18) . . ?
C26 C22 C21 122.80(18) . . ?
C22 C23 C24 120.98(18) . . ?
C25 C23 C22 122.33(19) . . ?
C25 C23 C24 116.69(19) . . ?
O3 C24 C19 120.78(19) . . ?
O3 C24 C23 121.54(19) . . ?
C23 C24 C19 117.68(18) . . ?
C23 C25 C28 119.7(2) . . ?
O4 C26 C22 126.83(18) . . ?
O4 C26 C27 115.74(18) . . ?
C27 C26 C22 117.42(18) . . ?
C28 C27 C26 122.7(2) . . ?
C27 C28 C25 120.0(2) . . ?
O8 C29 N1 125.1(2) . . ?
O9 C34 N2 123.9(2) . . ?
O10 C35 O11 125.7(2) . . ?
O10 C35 C36 117.03(19) . . ?
O11 C35 C36 117.25(19) . . ?
N3 C37 C38 123.7(2) . . ?
C39 C38 C37 118.4(3) . . ?
C40 C39 C38 119.0(2) . . ?
C39 C40 C41 119.2(3) . . ?
N3 C41 C40 123.2(2) . . ?
O12 C42 C43 118.00(19) . . ?
O13 C42 O12 126.04(19) . . ?
O13 C42 C43 116.0(2) . . ?
O14 C44 N4 123.8(2) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-17 0 -1 0.0338 -17.0000 -0.0004 -1.0001 0.0111 0.9305 0.3637
-3 2 -19 0.1084 -3.0000 2.0000 -19.0000 -0.0588 -0.0151 0.9902
15 -10 -2 0.1170 15.0000 -9.9996 -2.0000 0.5499 -0.8009 -0.1812
17 2 -4 0.0396 17.0000 2.0004 -4.0000 -0.1083 -0.9848 -0.1174
-2 14 -13 0.1392 -2.0000 14.0000 -13.0000 -0.7376 -0.0715 0.6791
3 7 17 0.1591 3.0000 6.9999 17.0001 -0.4328 -0.0445 -0.8900
-17 1 6 0.0360 -17.0000 0.9996 6.0000 -0.0626 0.9891 0.0197
2 18 -1 0.1510 2.0000 18.0000 -1.0000 -0.9922 -0.2026 0.0158
-2 -18 1 0.1673 -2.0000 -18.0000 1.0000 0.9922 0.2026 -0.0158
-15 0 -7 0.0676 -15.0000 -0.0003 -7.0001 0.0260 0.7657 0.6217
15 1 -13 0.0965 15.0000 1.0004 -13.0000 -0.0284 -0.9510 0.3619
-15 -1 13 0.0965 -15.0000 -1.0004 13.0000 0.0284 0.9510 -0.3619
12 0 12 0.0941 12.0000 0.0002 12.0001 -0.0377 -0.5548 -0.8121
-3 0 -19 0.1197 -3.0000 0.0000 -19.0001 0.0517 -0.0058 0.9898
17 0 1 0.0368 17.0000 0.0004 1.0001 -0.0111 -0.9305 -0.3637

####################################################################### 
# 
# 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_CoChrys-3
_database_code_depnum_ccdc_archive 'CCDC 1044029'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2016-04-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        
'di[tetra(chrysazinato)-tetra(N,N-dimethylformamide)-tetra-cobalt(II)] di(N,N-dimethylformamide) solvate hemihydrate'
_chemical_formula_moiety         
'2(C68 H52 Co4 N4 O20), 2.35(C3 H7 N O), 0.5(O)'
_chemical_formula_sum            'C143.05 H120.45 Co8 N10.35 O42.85'
_chemical_formula_weight         3141.48
_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'

_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                   15.6278(16)
_cell_length_b                   15.6996(15)
_cell_length_c                   29.048(3)
_cell_angle_alpha                90.9201(10)
_cell_angle_beta                 104.1390(16)
_cell_angle_gamma                90.2340(13)
_cell_volume                     6909.8(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    19366
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'Dark Red'
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3220
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            119113
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.602
_diffrn_reflns_theta_min         2.256
_diffrn_ambient_temperature      100
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_measurement_specimen_support MiTeGen
_diffrn_detector                 CCD
_diffrn_measurement_details      
;
scan:
	Number of images: 330
	           Slice: -95.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 18.0000
	             Phi: -180.0000
	             XTD: 50.0076
	          2theta: -20.0488
scan:
	Number of images: 180
	           Slice: -69.0000 - 21.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: -90.0000
	             XTD: 50.0076
	          2theta: -20.0488
scan:
	Number of images: 204
	           Slice: -32.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: -150.0000
	             XTD: 50.0076
	          2theta: -20.0488
scan:
	Number of images: 178
	           Slice: -69.0000 - 20.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: 90.0000
	             XTD: 50.0076
	          2theta: -20.0488
scan:
	Number of images: 52
	           Slice: -34.0000 - -8.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 54.0000
	             Phi: 60.0000
	             XTD: 50.0076
	          2theta: -20.0488
scan:
	Number of images: 330
	           Slice: -95.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 18.0000
	             Phi: 30.0000
	             XTD: 50.0076
	          2theta: -20.0488
scan:
	Number of images: 182
	           Slice: -70.0000 - 21.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: 120.0000
	             XTD: 50.0076
	          2theta: -20.0488
scan:
	Number of images: 204
	           Slice: -32.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 72.0000
	             Phi: 60.0000
	             XTD: 50.0076
	          2theta: -20.0488
scan:
	Number of images: 22
	           Slice: -69.0000 - -58.0000
	     Image width: 0.5000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: -60.0000
	             XTD: 50.0076
	          2theta: -20.0488

;
_diffrn_orient_matrix_UB_11      0.055508
_diffrn_orient_matrix_UB_12      0.013734
_diffrn_orient_matrix_UB_13      -0.032938
_diffrn_orient_matrix_UB_21      0.003197
_diffrn_orient_matrix_UB_22      -0.060149
_diffrn_orient_matrix_UB_23      -0.020746
_diffrn_orient_matrix_UB_31      -0.011235
_diffrn_orient_matrix_UB_32      0.009851
_diffrn_orient_matrix_UB_33      -0.032210
_diffrn_orient_matrix_type       d*Trek
_diffrn_reflns_transf_matrix_11  0.055508
_diffrn_reflns_transf_matrix_12  0.013734
_diffrn_reflns_transf_matrix_13  -0.032938
_diffrn_reflns_transf_matrix_21  0.003197
_diffrn_reflns_transf_matrix_22  -0.060149
_diffrn_reflns_transf_matrix_23  -0.020746
_diffrn_reflns_transf_matrix_31  -0.011235
_diffrn_reflns_transf_matrix_32  0.009851
_diffrn_reflns_transf_matrix_33  -0.032210

_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                27773
_reflns_number_total             31716
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         1.698
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2078
_refine_ls_number_reflns         31716
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0627
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0886P)²+16.1538P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1829
_refine_special_details          ?
# SQUEEZE RESULTS (APPEND TO CIF)
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 0.039 0.518 0.046 10.6 0.3 ' '
2 0.500 1.000 1.000 327.9 27.5 'unidentified solvent (most likely DMF)'
3 0.276 0.157 0.413 14.5 -0.4 ' '
4 0.301 0.309 0.547 21.4 0.2 ' '
5 0.699 0.691 0.453 21.5 -0.4 ' '
6 0.724 0.843 0.587 14.5 -0.3 ' '
7 0.961 0.482 0.954 10.4 0.8 ' '
_platon_squeeze_details          
;
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O40-C162 = O40-C161
 1.21 with sigma of 0.01
 C172-N10 = C171-N10
 1.44 with sigma of 0.01
 C171-O42
 2.78 with sigma of 0.01
 C170-N10
 1.3 with sigma of 0.01
 O42-C170
 1.21 with sigma of 0.01
 C162-N8B = C161-N8A
 1.3 with sigma of 0.01
 O41-C167
 1.21 with sigma of 0.01
 C168-O41
 2.78 with sigma of 0.01
 C167-N9
 1.3 with sigma of 0.01
 C168-N9 = C169-N9
 1.44 with sigma of 0.01
 N8A-C163 = N8A-C165 = N8B-C166 = N8B-C164
 1.44 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N4 \\sim C67 \\sim C68: within 1.7A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C137) \\sim Ueq, Uanis(C136) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.005
Uanis(C175) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C174) \\sim Ueq, Uanis(C173)
\\sim Ueq, Uanis(O43) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.05
Uanis(C170) \\sim Ueq, Uanis(C171) \\sim Ueq, Uanis(C172) \\sim Ueq, Uanis(N10)
\\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.005
Uanis(C167) \\sim Ueq, Uanis(C168) \\sim Ueq, Uanis(C169) \\sim Ueq, Uanis(N9)
\\sim Ueq, Uanis(O41) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.005
Uanis(C108) = Uanis(C109)
Uanis(C110) = Uanis(C111)
Uanis(C99) = Uanis(C117)
Uanis(C118) = Uanis(C119)
Uanis(C106) = Uanis(C107)
Uanis(C96) = Uanis(C97)
Uanis(C98) = Uanis(C99)
Uanis(C145) = Uanis(C144)
Uanis(O36A) = Uanis(O36B)
Uanis(C125) = Uanis(C4)
Uanis(C137) = Uanis(C136)
Uanis(C145) = Uanis(C144)
Uanis(C127) = Uanis(C126)
Uanis(C135) = Uanis(C134)
Uanis(C139) = Uanis(C138)
Uanis(C147) = Uanis(C146)
Uanis(C96) = Uanis(C97)
Uanis(C106) = Uanis(C107)
Uanis(C108) = Uanis(C109)
Uanis(C110) = Uanis(C111)
Uanis(C116) = Uanis(C117)
Uanis(C118) = Uanis(C119)
Uanis(C120) = Uanis(C121)
Uanis(C122) = Uanis(C123)
Uanis(C112) = Uanis(C113)
Uanis(C114) = Uanis(C115)
Uanis(C104) = Uanis(C105)
Uanis(C102) = Uanis(C103)
Uanis(C100) = Uanis(C101)
Uanis(C98) = Uanis(C99)
Uanis(C96) = Uanis(C97)
Uanis(C144) = Uanis(C145)
Uanis(C146) = Uanis(C147)
Uanis(C148) = Uanis(C149)
Uanis(C150) = Uanis(C151)
Uanis(C140) = Uanis(C141)
Uanis(C138) = Uanis(C139)
Uanis(C142) = Uanis(C143)
Uanis(O36A) = Uanis(O36B)
Uanis(C136) = Uanis(C137)
Uanis(C134) = Uanis(C135)
Uanis(C132) = Uanis(C133)
Uanis(C4) = Uanis(C125)
Uanis(C126) = Uanis(C127)
Uanis(C128) = Uanis(C129)
Uanis(C130) = Uanis(C131)
Uanis(C132) = Uanis(C133)
4. Others
 Sof(C125)=Sof(C127)=Sof(H127)=Sof(C129)=Sof(H129)=Sof(C131)=Sof(H131)=
 Sof(C133)=Sof(C135)=Sof(C137)=Sof(C139)=Sof(C141)=Sof(C143)=Sof(C145)=
 Sof(C147)=Sof(H147)=Sof(C149)=Sof(H149)=Sof(C151)=Sof(H151)=Sof(O36B)=1-FVAR(1)
 Sof(C4)=Sof(C126)=Sof(H126)=Sof(C128)=Sof(H128)=Sof(C130)=Sof(H130)=Sof(C132)=
 Sof(C134)=Sof(C136)=Sof(C138)=Sof(C140)=Sof(C142)=Sof(C144)=Sof(C146)=
 Sof(H146)=Sof(C148)=Sof(H148)=Sof(C150)=Sof(H150)=Sof(O36A)=FVAR(1)
 Fixed Sof: O41(0.5) O42(0.5) N9(0.5) N10(0.5) C96(0.5) C97(0.5) C98(0.5)
 H98(0.5) C99(0.5) H99(0.5) C100(0.5) H100(0.5) C101(0.5) H101(0.5) C102(0.5)
 H102(0.5) C103(0.5) H103(0.5) C104(0.5) C105(0.5) C106(0.5) C107(0.5)
 C108(0.5) C109(0.5) C110(0.5) C111(0.5) C112(0.5) C113(0.5) C114(0.5)
 C115(0.5) C116(0.5) C117(0.5) C118(0.5) H118(0.5) C119(0.5) H119(0.5)
 C120(0.5) H120(0.5) C121(0.5) H121(0.5) C122(0.5) H122(0.5) C123(0.5)
 H123(0.5) C161(0.5) H161(0.5) C162(0.5) H162(0.5) C163(0.5) H16D(0.5)
 H16E(0.5) H16F(0.5) C164(0.5) H16G(0.5) H16H(0.5) H16I(0.5) C165(0.5)
 H16J(0.5) H16K(0.5) H16L(0.5) C166(0.5) H16M(0.5) H16N(0.5) H16O(0.5)
 C167(0.5) H167(0.5) C168(0.5) H16P(0.5) H16Q(0.5) H16R(0.5) C169(0.5)
 H16S(0.5) H16T(0.5) H16U(0.5) C170(0.5) H170(0.5) C171(0.5) H17A(0.5)
 H17B(0.5) H17C(0.5) C172(0.5) H17D(0.5) H17E(0.5) H17F(0.5) O32A(0.5) N8A(0.5)
 C40A(0.5) H40A(0.5) C41A(0.5) H41A(0.5) C42A(0.5) H42A(0.5) C54A(0.5)
 H54A(0.5) C55A(0.5) H55A(0.5) C56A(0.5) H56A(0.5) O32B(0.5) N8B(0.5) C40B(0.5)
 H40B(0.5) C41B(0.5) H41B(0.5) C42B(0.5) H42B(0.5) C54B(0.5) H54B(0.5)
 C55B(0.5) H55B(0.5) C56B(0.5) H56B(0.5) O1W(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C10(H10), C13(H13), C14(H14), C18(H18), C26(H26), C27(H27),
 C32(H32), C44(H44), C45(H45), C46(H46), C57(H57), C60(H60), C66(H66), C70(H70),
  C71(H71), C72(H72), C80(H80), C81(H81), C82(H82), C84(H84), C85(H85),
 C86(H86), C93(H93), C94(H94), C95(H95), C98(H98), C99(H99), C100(H100),
 C101(H101), C102(H102), C103(H103), C118(H118), C119(H119), C120(H120),
 C121(H121), C122(H122), C123(H123), C126(H126), C127(H127), C128(H128),
 C129(H129), C130(H130), C131(H131), C146(H146), C147(H147), C148(H148),
 C149(H149), C150(H150), C151(H151), C152(H152), C155(H155), C158(H158),
 C161(H161), C162(H162), C167(H167), C170(H170), C173(H173), C1A(H1A),
 C40A(H40A), C41A(H41A), C42A(H42A), C54A(H54A), C55A(H55A), C56A(H56A),
 C40B(H40B), C41B(H41B), C42B(H42B), C54B(H54B), C55B(H55B), C56B(H56B),
 C1G(H1G), C1N(H1N), C1O(H1O), C1Q(H1Q), C1T(H1T), C1V(H1V)
5.b Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C62(H62A,H62B,
 H62C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C), C153(H15A,H15B,H15C), C154(H15D,H15E,H15F), C156(H15G,H15H,H15I),
 C157(H15J,H15K,H15L), C159(H15M,H15N,H15O), C160(H16A,H16B,H16C), C163(H16D,
 H16E,H16F), C164(H16G,H16H,H16I), C165(H16J,H16K,H16L), C166(H16M,H16N,H16O),
 C168(H16P,H16Q,H16R), C169(H16S,H16T,H16U), C171(H17A,H17B,H17C), C172(H17D,
 H17E,H17F), C174(H17G,H17H,H17I), C175(H17J,H17K,H17L)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.60889(3) 0.26838(3) 0.26109(2) 0.02118(10) Uani 1 1 d . . . . .
Co2 Co 0.61538(3) 0.47531(3) 0.25340(2) 0.01973(10) Uani 1 1 d . . . . .
Co3 Co 0.40879(3) 0.48450(3) 0.25659(2) 0.02010(10) Uani 1 1 d . . . . .
Co4 Co 0.39425(3) 0.27746(3) 0.24126(2) 0.02069(10) Uani 1 1 d . . . . .
Co5 Co -0.08712(3) 0.99070(3) 0.24816(2) 0.02602(11) Uani 1 1 d . . . . .
Co6 Co -0.11802(3) 0.78425(3) 0.23700(2) 0.02345(10) Uani 1 1 d . . . . .
Co7 Co 0.09576(3) 0.76039(3) 0.25511(2) 0.02247(10) Uani 1 1 d . . . . .
Co8 Co 0.11813(3) 0.96602(3) 0.24560(2) 0.02822(11) Uani 1 1 d . . . . .
O1 O 0.29496(16) 0.24435(15) 0.18810(8) 0.0275(5) Uani 1 1 d . . . . .
O2 O 0.39736(14) 0.38753(13) 0.20265(7) 0.0204(4) Uani 1 1 d . . . . .
O3 O 0.49151(14) 0.52968(13) 0.21791(8) 0.0212(4) Uani 1 1 d . . . . .
O4 O 0.2788(2) 0.4636(2) 0.01805(9) 0.0432(7) Uani 1 1 d . . . . .
O5 O 0.49733(15) 0.22477(13) 0.21373(8) 0.0230(4) Uani 1 1 d . . . . .
O6 O 0.58448(15) 0.36729(13) 0.21006(7) 0.0206(4) Uani 1 1 d . . . . .
O7 O 0.68473(15) 0.50766(15) 0.20864(8) 0.0266(5) Uani 1 1 d . . . . .
O8 O 0.5404(2) 0.32534(19) 0.02119(9) 0.0434(7) Uani 1 1 d . . . . .
O9 O 0.39515(17) 0.56771(16) 0.30555(9) 0.0325(6) Uani 1 1 d . . . . .
O10 O 0.53331(14) 0.46656(13) 0.30150(8) 0.0207(4) Uani 1 1 d . . . . .
O11 O 0.67540(15) 0.38002(14) 0.29612(8) 0.0227(4) Uani 1 1 d . . . . .
O12 O 0.6572(2) 0.5036(2) 0.49094(9) 0.0458(7) Uani 1 1 d . . . . .
O13 O 0.36275(15) 0.37262(14) 0.28369(8) 0.0230(4) Uani 1 1 d . . . . .
O14 O 0.51108(15) 0.28567(13) 0.29806(8) 0.0216(4) Uani 1 1 d . . . . .
O15 O 0.65416(19) 0.18403(17) 0.31057(9) 0.0377(6) Uani 1 1 d . . . . .
O16 O 0.5106(2) 0.2481(2) 0.48192(9) 0.0419(7) Uani 1 1 d . . . . .
O17 O 0.36915(17) 0.17502(14) 0.28089(9) 0.0279(5) Uani 1 1 d . . . . .
O18 O 0.28752(15) 0.52195(15) 0.21317(8) 0.0262(5) Uani 1 1 d . . . . .
O19 O 0.69597(16) 0.22840(15) 0.22145(8) 0.0264(5) Uani 1 1 d . . . . .
O20 O 0.66385(17) 0.58177(15) 0.29617(9) 0.0294(5) Uani 1 1 d . . . . .
O21 O -0.00138(16) 1.02750(14) 0.20835(9) 0.0279(5) Uani 1 1 d . . . . .
O22 O -0.10287(15) 0.88944(14) 0.19690(8) 0.0225(4) Uani 1 1 d . . . . .
O23 O -0.22792(16) 0.76627(17) 0.18690(9) 0.0327(6) Uani 1 1 d . . . . .
O24 O -0.1840(3) 0.9262(2) 0.00762(10) 0.0601(10) Uani 1 1 d . . . . .
O25 O 0.19481(17) 0.98501(16) 0.20227(11) 0.0364(6) Uani 1 1 d . . . . .
O26 O 0.07773(15) 0.85780(14) 0.20355(8) 0.0235(4) Uani 1 1 d . . . . .
O27 O -0.02021(15) 0.72239(14) 0.20802(8) 0.0232(4) Uani 1 1 d . . . . .
O28 O 0.0483(2) 0.7991(2) 0.01751(10) 0.0475(7) Uani 1 1 d . . . . .
O29 O -0.09264(19) 1.08067(19) 0.29481(10) 0.0431(7) Uani 1 1 d . . . . .
O30 O 0.03553(16) 0.96698(15) 0.29324(9) 0.0287(5) Uani 1 1 d . . . . .
O31 O 0.17104(16) 0.86865(15) 0.28994(9) 0.0300(5) Uani 1 1 d . . . . .
O33 O 0.13478(16) 0.67239(16) 0.30346(9) 0.0299(5) Uani 1 1 d . . . . .
O34 O 0.00151(15) 0.78636(15) 0.29219(8) 0.0246(5) Uani 1 1 d . . . . .
O35 O -0.13835(16) 0.88464(16) 0.27913(8) 0.0294(5) Uani 1 1 d . . . . .
O37 O -0.14527(18) 0.68205(18) 0.27652(9) 0.0352(6) Uani 1 1 d . . . . .
O38 O 0.18688(16) 0.71866(15) 0.21787(9) 0.0281(5) Uani 1 1 d . . . . .
O39 O 0.16883(18) 1.07651(17) 0.28477(11) 0.0405(7) Uani 1 1 d . . . . .
O40 O -0.20897(16) 1.02595(16) 0.20410(9) 0.0326(5) Uani 1 1 d D . . . .
O41 O 0.5796(6) 0.9394(5) 0.3705(3) 0.075(2) Uani 0.5 1 d D U P . .
O42 O 0.0208(7) 0.3691(6) 0.3791(3) 0.092(3) Uani 0.5 1 d D U P . .
O43 O 0.9142(3) 0.4016(3) 0.14901(16) 0.0745(11) Uani 1 1 d . U . . .
N1 N 0.3794(2) 0.03463(18) 0.29780(12) 0.0313(6) Uani 1 1 d . . . . .
N2 N 0.13993(19) 0.51779(18) 0.20405(11) 0.0288(6) Uani 1 1 d . . . . .
N3 N 0.8312(2) 0.2287(2) 0.20679(12) 0.0328(7) Uani 1 1 d . . . . .
N4 N 0.6576(4) 0.7262(3) 0.2968(2) 0.0716(10) Uani 1 1 d . U . . .
N5 N -0.1252(3) 0.5398(2) 0.29235(14) 0.0463(9) Uani 1 1 d . . . . .
N6 N 0.3291(2) 0.7298(2) 0.21500(16) 0.0484(9) Uani 1 1 d . . . . .
N7 N 0.1547(2) 1.2195(2) 0.27923(14) 0.0394(8) Uani 1 1 d . . . . .
N9 N 0.5868(5) 0.8817(5) 0.4409(3) 0.058(2) Uani 0.5 1 d D U P . .
N10 N 0.1013(5) 0.3614(4) 0.4583(3) 0.0438(17) Uani 0.5 1 d D U P . .
N11 N 0.9159(4) 0.3790(3) 0.07192(18) 0.0715(14) Uani 1 1 d . U . . .
C1 C 0.4635(2) 0.53723(19) 0.17138(11) 0.0215(6) Uani 1 1 d . . . . .
C2 C 0.4972(2) 0.6064(2) 0.15031(12) 0.0251(6) Uani 1 1 d . . . . .
H2 H 0.5396 0.6420 0.1693 0.030 Uiso 1 1 calc R U . . .
C3 C 0.4688(2) 0.6223(2) 0.10262(12) 0.0304(7) Uani 1 1 d . . . . .
H3 H 0.4923 0.6682 0.0898 0.036 Uiso 1 1 calc R U . . .
C4 C 0.1343(14) 0.6818(13) 0.3475(9) 0.0229(15) Uani 0.351(3) 1 d . . P A 2
C6 C 0.1280(2) 0.8910(2) 0.13586(13) 0.0280(7) Uani 1 1 d . . . . .
C7 C 0.4010(2) 0.48152(19) 0.14121(11) 0.0212(6) Uani 1 1 d . . . . .
C10 C 0.4055(2) 0.5704(2) 0.07349(12) 0.0307(7) Uani 1 1 d . . . . .
H10 H 0.3852 0.5825 0.0414 0.037 Uiso 1 1 calc R U . . .
C11 C 0.2741(2) 0.2707(2) 0.14474(12) 0.0248(6) Uani 1 1 d . . . . .
C13 C 0.4211(3) 0.6216(3) 0.42885(16) 0.0511(12) Uani 1 1 d . . . . .
H13 H 0.3902 0.6521 0.4472 0.061 Uiso 1 1 calc R U . . .
C14 C 0.6328(3) 0.4689(2) 0.06357(13) 0.0357(8) Uani 1 1 d . . . . .
H14 H 0.6202 0.4630 0.0307 0.043 Uiso 1 1 calc R U . . .
C15 C 0.3080(2) 0.4441(2) 0.05934(12) 0.0293(7) Uani 1 1 d . . . . .
C18 C 0.4684(2) 0.2035(2) 0.06791(12) 0.0283(7) Uani 1 1 d . . . . .
H18 H 0.4613 0.1975 0.0353 0.034 Uiso 1 1 calc R U . . .
C20 C 0.5292(2) 0.28230(19) 0.14220(11) 0.0207(6) Uani 1 1 d . . . . .
C22 C 0.6167(2) 0.4181(2) 0.14041(11) 0.0234(6) Uani 1 1 d . . . . .
C23 C 0.6017(2) 0.4093(2) 0.09004(12) 0.0281(7) Uani 1 1 d . . . . .
C24 C 0.5521(2) 0.3349(2) 0.06439(12) 0.0289(7) Uani 1 1 d . . . . .
C25 C 0.6677(2) 0.4896(2) 0.16354(12) 0.0248(6) Uani 1 1 d . . . . .
C26 C 0.7016(2) 0.5470(2) 0.13453(13) 0.0306(7) Uani 1 1 d . . . . .
H26 H 0.7373 0.5921 0.1491 0.037 Uiso 1 1 calc R U . . .
C27 C 0.6834(3) 0.5380(2) 0.08621(14) 0.0360(8) Uani 1 1 d . . . . .
H27 H 0.7047 0.5780 0.0684 0.043 Uiso 1 1 calc R U . . .
C29 C 0.4335(2) 0.5699(2) 0.35046(12) 0.0285(7) Uani 1 1 d . . . . .
C32 C 0.4980(3) 0.5781(3) 0.45083(13) 0.0366(8) Uani 1 1 d . . . . .
H32 H 0.5181 0.5793 0.4837 0.044 Uiso 1 1 calc R U . . .
C33 C 0.5438(2) 0.5336(2) 0.42345(12) 0.0268(7) Uani 1 1 d . . . . .
C34 C 0.5132(2) 0.52700(19) 0.37315(11) 0.0225(6) Uani 1 1 d . . . . .
C35 C 0.5622(2) 0.47736(19) 0.34586(11) 0.0208(6) Uani 1 1 d . . . . .
C36 C 0.6461(2) 0.4379(2) 0.36915(11) 0.0247(6) Uani 1 1 d . . . . .
C37 C 0.6767(3) 0.4441(3) 0.41904(12) 0.0360(9) Uani 1 1 d . . . . .
C38 C 0.6276(3) 0.4939(2) 0.44792(12) 0.0325(8) Uani 1 1 d . . . . .
C39 C 0.6966(2) 0.3899(2) 0.34309(11) 0.0274(7) Uani 1 1 d . . . . .
C43 C 0.3726(2) 0.3630(2) 0.33009(11) 0.0232(6) Uani 1 1 d . . . . .
C44 C 0.3119(2) 0.4045(2) 0.35145(13) 0.0306(7) Uani 1 1 d . . . . .
H44 H 0.2682 0.4378 0.3328 0.037 Uiso 1 1 calc R U . . .
C45 C 0.3152(3) 0.3973(3) 0.39915(13) 0.0352(8) Uani 1 1 d . . . . .
H45 H 0.2746 0.4260 0.4122 0.042 Uiso 1 1 calc R U . . .
C46 C 0.3791(3) 0.3472(2) 0.42757(12) 0.0318(7) Uani 1 1 d . . . . .
H46 H 0.3805 0.3409 0.4595 0.038 Uiso 1 1 calc R U . . .
C47 C 0.4409(2) 0.3064(2) 0.40802(12) 0.0257(6) Uani 1 1 d . . . . .
C48 C 0.4399(2) 0.31351(19) 0.35926(11) 0.0228(6) Uani 1 1 d . . . . .
C49 C 0.5104(2) 0.27430(18) 0.34090(11) 0.0217(6) Uani 1 1 d . . . . .
C50 C 0.5773(3) 0.2237(2) 0.37123(13) 0.0339(8) Uani 1 1 d . . . . .
C51 C 0.5762(3) 0.2141(3) 0.41951(14) 0.0480(12) Uani 1 1 d . . . . .
C52 C 0.5098(3) 0.2559(2) 0.43998(12) 0.0304(7) Uani 1 1 d . . . . .
C53 C 0.6425(4) 0.1804(3) 0.35311(16) 0.0532(14) Uani 1 1 d . . . . .
C57 C 0.3756(2) 0.0994(2) 0.26883(13) 0.0284(7) Uani 1 1 d . . . . .
H57 H 0.3778 0.0878 0.2377 0.034 Uiso 1 1 calc R U . . .
C58 C 0.3754(3) 0.0484(3) 0.34698(15) 0.0450(10) Uani 1 1 d . . . . .
H58A H 0.3235 0.0211 0.3521 0.068 Uiso 1 1 calc R U . . .
H58B H 0.3731 0.1084 0.3534 0.068 Uiso 1 1 calc R U . . .
H58C H 0.4268 0.0249 0.3678 0.068 Uiso 1 1 calc R U . . .
C59 C 0.3830(3) -0.0525(2) 0.28063(18) 0.0441(10) Uani 1 1 d . . . . .
H59A H 0.4324 -0.0809 0.3005 0.066 Uiso 1 1 calc R U . . .
H59B H 0.3894 -0.0520 0.2486 0.066 Uiso 1 1 calc R U . . .
H59C H 0.3295 -0.0820 0.2815 0.066 Uiso 1 1 calc R U . . .
C60 C 0.2215(2) 0.5211(2) 0.22982(13) 0.0282(7) Uani 1 1 d . . . . .
H60 H 0.2305 0.5228 0.2627 0.034 Uiso 1 1 calc R U . . .
C61 C 0.1217(3) 0.5233(4) 0.15276(15) 0.0547(13) Uani 1 1 d . . . . .
H61A H 0.0702 0.4898 0.1386 0.082 Uiso 1 1 calc R U . . .
H61B H 0.1712 0.5020 0.1421 0.082 Uiso 1 1 calc R U . . .
H61C H 0.1117 0.5816 0.1437 0.082 Uiso 1 1 calc R U . . .
C62 C 0.0653(2) 0.5197(2) 0.22647(15) 0.0355(8) Uani 1 1 d . . . . .
H62A H 0.0368 0.5740 0.2213 0.053 Uiso 1 1 calc R U . . .
H62B H 0.0864 0.5111 0.2600 0.053 Uiso 1 1 calc R U . . .
H62C H 0.0239 0.4754 0.2128 0.053 Uiso 1 1 calc R U . . .
C64 C 0.7982(3) 0.2118(3) 0.15645(15) 0.0457(10) Uani 1 1 d . . . . .
H64A H 0.8210 0.2539 0.1389 0.069 Uiso 1 1 calc R U . . .
H64B H 0.7349 0.2139 0.1483 0.069 Uiso 1 1 calc R U . . .
H64C H 0.8167 0.1563 0.1487 0.069 Uiso 1 1 calc R U . . .
C65 C 0.9264(3) 0.2354(3) 0.2257(2) 0.0488(11) Uani 1 1 d . . . . .
H65A H 0.9392 0.2455 0.2594 0.073 Uiso 1 1 calc R U . . .
H65B H 0.9490 0.2819 0.2110 0.073 Uiso 1 1 calc R U . . .
H65C H 0.9536 0.1834 0.2192 0.073 Uiso 1 1 calc R U . . .
C66 C 0.6585(3) 0.6519(2) 0.27664(17) 0.0427(10) Uani 1 1 d . . . . .
H66 H 0.6547 0.6512 0.2442 0.051 Uiso 1 1 calc R U . . .
C67 C 0.6557(5) 0.7298(4) 0.3438(3) 0.0830(13) Uani 1 1 d . U . . .
H67A H 0.7131 0.7454 0.3628 0.125 Uiso 1 1 calc R U . . .
H67B H 0.6391 0.6750 0.3532 0.125 Uiso 1 1 calc R U . . .
H67C H 0.6135 0.7715 0.3482 0.125 Uiso 1 1 calc R U . . .
C68 C 0.6546(4) 0.8061(3) 0.2711(3) 0.0721(12) Uani 1 1 d . U . . .
H68A H 0.6061 0.8397 0.2757 0.108 Uiso 1 1 calc R U . . .
H68B H 0.6470 0.7939 0.2379 0.108 Uiso 1 1 calc R U . . .
H68C H 0.7088 0.8372 0.2830 0.108 Uiso 1 1 calc R U . . .
C69 C -0.0218(2) 1.0269(2) 0.16157(13) 0.0274(7) Uani 1 1 d . . . . .
C70 C 0.0204(2) 1.0865(2) 0.13802(15) 0.0365(8) Uani 1 1 d . . . . .
H70 H 0.0596 1.1258 0.1562 0.044 Uiso 1 1 calc R U . . .
C71 C 0.0055(3) 1.0882(3) 0.08980(16) 0.0420(9) Uani 1 1 d . . . . .
H71 H 0.0358 1.1273 0.0759 0.050 Uiso 1 1 calc R U . . .
C72 C -0.0548(3) 1.0320(3) 0.06115(15) 0.0388(9) Uani 1 1 d . . . . .
H72 H -0.0641 1.0326 0.0283 0.047 Uiso 1 1 calc R U . . .
C73 C -0.1002(2) 0.9754(2) 0.08237(13) 0.0304(7) Uani 1 1 d . . . . .
C74 C -0.0843(2) 0.9697(2) 0.13217(12) 0.0248(6) Uani 1 1 d . . . . .
C75 C -0.1271(2) 0.90143(19) 0.15296(11) 0.0219(6) Uani 1 1 d . . . . .
C76 C -0.1968(2) 0.8499(2) 0.12319(11) 0.0239(6) Uani 1 1 d . . . . .
C77 C -0.2208(2) 0.8622(2) 0.07310(12) 0.0285(7) Uani 1 1 d . . . . .
C78 C -0.1692(3) 0.9207(2) 0.05071(13) 0.0342(8) Uani 1 1 d . . . . .
C79 C -0.2466(2) 0.7904(2) 0.14313(12) 0.0284(7) Uani 1 1 d . . . . .
C80 C -0.3238(3) 0.7557(2) 0.11197(14) 0.0368(9) Uani 1 1 d . . . . .
H80 H -0.3614 0.7223 0.1247 0.044 Uiso 1 1 calc R U . . .
C81 C -0.3455(3) 0.7693(3) 0.06410(14) 0.0416(9) Uani 1 1 d . . . . .
H81 H -0.3957 0.7436 0.0449 0.050 Uiso 1 1 calc R U . . .
C82 C -0.2925(3) 0.8214(2) 0.04426(13) 0.0369(8) Uani 1 1 d . . . . .
H82 H -0.3054 0.8286 0.0116 0.044 Uiso 1 1 calc R U . . .
C83 C 0.1882(2) 0.9560(2) 0.15969(15) 0.0330(8) Uani 1 1 d . . . . .
C84 C 0.2453(3) 0.9926(3) 0.13372(17) 0.0441(10) Uani 1 1 d . . . . .
H84 H 0.2872 1.0327 0.1489 0.053 Uiso 1 1 calc R U . . .
C85 C 0.2410(3) 0.9714(3) 0.08753(18) 0.0505(11) Uani 1 1 d . . . . .
H85 H 0.2793 0.9972 0.0719 0.061 Uiso 1 1 calc R U . . .
C86 C 0.1793(3) 0.9109(3) 0.06337(16) 0.0419(9) Uani 1 1 d . . . . .
H86 H 0.1757 0.8973 0.0317 0.050 Uiso 1 1 calc R U . . .
C87 C 0.1236(2) 0.8714(2) 0.08715(13) 0.0316(7) Uani 1 1 d . . . . .
C88 C 0.0756(2) 0.84154(19) 0.16048(12) 0.0223(6) Uani 1 1 d . . . . .
C89 C 0.0206(2) 0.77049(19) 0.13670(12) 0.0228(6) Uani 1 1 d . . . . .
C90 C 0.0102(2) 0.7563(2) 0.08752(12) 0.0264(7) Uani 1 1 d . . . . .
C91 C 0.0592(3) 0.8086(2) 0.06048(13) 0.0321(7) Uani 1 1 d . . . . .
C92 C -0.0269(2) 0.71693(19) 0.16187(12) 0.0224(6) Uani 1 1 d . . . . .
C93 C -0.0828(2) 0.6534(2) 0.13515(12) 0.0276(7) Uani 1 1 d . . . . .
H93 H -0.1139 0.6178 0.1507 0.033 Uiso 1 1 calc R U . . .
C94 C -0.0929(2) 0.6421(2) 0.08671(13) 0.0309(7) Uani 1 1 d . . . . .
H94 H -0.1310 0.6003 0.0702 0.037 Uiso 1 1 calc R U . . .
C95 C -0.0457(2) 0.6938(2) 0.06287(13) 0.0304(7) Uani 1 1 d . . . . .
H95 H -0.0519 0.6861 0.0304 0.036 Uiso 1 1 calc R U . . .
C96 C -0.0445(8) 1.0971(7) 0.3347(4) 0.0287(17) Uani 0.5 1 d . . P B 2
C97 C -0.0624(8) 1.0739(7) 0.3439(4) 0.0287(17) Uani 0.5 1 d . . P B 1
C98 C -0.0706(5) 1.1659(5) 0.3625(3) 0.0332(12) Uani 0.5 1 d . . P B 2
H98 H -0.1148 1.2024 0.3471 0.040 Uiso 0.5 1 calc R U P B 2
C99 C -0.1020(5) 1.1292(5) 0.3719(3) 0.0332(12) Uani 0.5 1 d . . P B 1
H99 H -0.1485 1.1637 0.3570 0.040 Uiso 0.5 1 calc R U P B 1
C100 C -0.0348(6) 1.1800(5) 0.4090(3) 0.0398(13) Uani 0.5 1 d . . P B 2
H100 H -0.0570 1.2225 0.4253 0.048 Uiso 0.5 1 calc R U P B 2
C101 C -0.0732(6) 1.1324(5) 0.4201(3) 0.0398(13) Uani 0.5 1 d . . P B 1
H101 H -0.1004 1.1686 0.4377 0.048 Uiso 0.5 1 calc R U P B 1
C102 C 0.0364(6) 1.1302(5) 0.4327(3) 0.0375(12) Uani 0.5 1 d . . P B 2
H102 H 0.0618 1.1397 0.4648 0.045 Uiso 0.5 1 calc R U P B 2
C103 C -0.0030(6) 1.0816(5) 0.4434(3) 0.0375(12) Uani 0.5 1 d . . P B 1
H103 H 0.0143 1.0821 0.4764 0.045 Uiso 0.5 1 calc R U P B 1
C104 C 0.0685(5) 1.0664(4) 0.4077(2) 0.0264(10) Uani 0.5 1 d . . P B 2
C105 C 0.0402(5) 1.0313(4) 0.4177(2) 0.0264(10) Uani 0.5 1 d . . P B 1
C106 C 0.0300(6) 1.0500(5) 0.3592(3) 0.0225(12) Uani 0.5 1 d . . P B 2
C107 C 0.0123(6) 1.0242(5) 0.3676(3) 0.0225(12) Uani 0.5 1 d . . P B 1
C108 C 0.0681(14) 0.9891(10) 0.3332(6) 0.021(2) Uani 0.5 1 d . . P B 2
C109 C 0.0618(14) 0.9699(10) 0.3418(6) 0.021(2) Uani 0.5 1 d . . P B 1
C110 C 0.1514(9) 0.9445(7) 0.3577(5) 0.0219(16) Uani 0.5 1 d . . P B 2
C111 C 0.1375(9) 0.9231(7) 0.3658(5) 0.0219(16) Uani 0.5 1 d . . P B 1
C112 C 0.1862(5) 0.9559(5) 0.4070(3) 0.0270(11) Uani 0.5 1 d . . P B 2
C113 C 0.1618(5) 0.9240(5) 0.4155(3) 0.0270(11) Uani 0.5 1 d . . P B 1
C114 C 0.1431(5) 1.0157(5) 0.4343(3) 0.0299(11) Uani 0.5 1 d . . P B 2
C115 C 0.1161(5) 0.9824(5) 0.4439(3) 0.0299(11) Uani 0.5 1 d . . P B 1
C116 C 0.1944(13) 0.8833(12) 0.3335(6) 0.0332(12) Uani 0.5 1 d . . P B 2
C117 C 0.1874(13) 0.8737(12) 0.3399(6) 0.0332(12) Uani 0.5 1 d . . P B 1
C118 C 0.2703(9) 0.8428(7) 0.3592(5) 0.0282(18) Uani 0.5 1 d . . P B 2
H118 H 0.3007 0.8067 0.3431 0.034 Uiso 0.5 1 calc R U P B 2
C119 C 0.2536(9) 0.8207(8) 0.3675(5) 0.0282(18) Uani 0.5 1 d . . P B 1
H119 H 0.2849 0.7851 0.3518 0.034 Uiso 0.5 1 calc R U P B 1
C120 C 0.3013(5) 0.8548(5) 0.4073(3) 0.0315(12) Uani 0.5 1 d . . P B 2
H120 H 0.3503 0.8250 0.4237 0.038 Uiso 0.5 1 calc R U P B 2
C121 C 0.2735(5) 0.8195(5) 0.4163(3) 0.0315(12) Uani 0.5 1 d . . P B 1
H121 H 0.3178 0.7841 0.4328 0.038 Uiso 0.5 1 calc R U P B 1
C122 C 0.2588(5) 0.9120(5) 0.4315(3) 0.0308(11) Uani 0.5 1 d . . P B 2
H122 H 0.2795 0.9204 0.4641 0.037 Uiso 0.5 1 calc R U P B 2
C123 C 0.2272(5) 0.8715(5) 0.4411(3) 0.0308(11) Uani 0.5 1 d . . P B 1
H123 H 0.2398 0.8709 0.4741 0.037 Uiso 0.5 1 calc R U P B 1
C125 C 0.1160(6) 0.6621(6) 0.3445(4) 0.0229(15) Uani 0.649(3) 1 d . . P A 1
C126 C 0.1875(10) 0.6259(9) 0.3785(5) 0.0309(14) Uani 0.351(3) 1 d . . P A 2
H126 H 0.2216 0.5873 0.3663 0.037 Uiso 0.351(3) 1 calc R U P A 2
C127 C 0.1627(5) 0.5966(4) 0.3745(3) 0.0309(14) Uani 0.649(3) 1 d . . P A 1
H127 H 0.1974 0.5590 0.3621 0.037 Uiso 0.649(3) 1 calc R U P A 1
C128 C 0.1917(9) 0.6254(9) 0.4259(5) 0.0388(15) Uani 0.351(3) 1 d . . P A 2
H128 H 0.2283 0.5871 0.4454 0.047 Uiso 0.351(3) 1 calc R U P A 2
C129 C 0.1579(5) 0.5874(5) 0.4209(2) 0.0388(15) Uani 0.649(3) 1 d . . P A 1
H129 H 0.1895 0.5446 0.4392 0.047 Uiso 0.649(3) 1 calc R U P A 1
C130 C 0.1404(8) 0.6831(8) 0.4455(4) 0.0353(13) Uani 0.351(3) 1 d . . P A 2
H130 H 0.1448 0.6848 0.4780 0.042 Uiso 0.351(3) 1 calc R U P A 2
C131 C 0.1056(4) 0.6423(4) 0.4406(2) 0.0353(13) Uani 0.649(3) 1 d . . P A 1
H131 H 0.1040 0.6374 0.4723 0.042 Uiso 0.649(3) 1 calc R U P A 1
C132 C 0.0834(8) 0.7370(8) 0.4154(4) 0.0280(12) Uani 0.351(3) 1 d . . P A 2
C133 C 0.0566(4) 0.7034(4) 0.4129(2) 0.0280(12) Uani 0.649(3) 1 d . . P A 1
C134 C 0.0781(11) 0.7371(10) 0.3665(7) 0.0226(13) Uani 0.351(3) 1 d . . P A 2
C135 C 0.0587(5) 0.7135(5) 0.3644(3) 0.0226(13) Uani 0.649(3) 1 d . . P A 1
C136 C 0.0128(14) 0.7913(12) 0.3367(9) 0.0208(14) Uani 0.351(3) 1 d . U P A 2
C137 C -0.0015(7) 0.7719(5) 0.3349(4) 0.0208(14) Uani 0.649(3) 1 d . U P A 1
C138 C -0.0493(12) 0.8445(9) 0.3569(6) 0.0234(13) Uani 0.351(3) 1 d . . P A 2
C139 C -0.0661(5) 0.8180(4) 0.3540(3) 0.0234(13) Uani 0.649(3) 1 d . . P A 1
C140 C -0.0374(8) 0.8489(8) 0.4054(4) 0.0272(11) Uani 0.351(3) 1 d . . P A 2
C141 C -0.0630(4) 0.8152(4) 0.4038(2) 0.0272(11) Uani 0.649(3) 1 d . . P A 1
C142 C 0.0288(8) 0.7935(8) 0.4373(4) 0.0286(11) Uani 0.351(3) 1 d . . P A 2
C143 C 0.0015(4) 0.7590(4) 0.4352(2) 0.0286(11) Uani 0.649(3) 1 d . . P A 1
C144 C -0.1144(13) 0.8967(9) 0.3284(7) 0.0229(13) Uani 0.351(3) 1 d . . P A 2
C145 C -0.1296(6) 0.8717(4) 0.3249(3) 0.0229(13) Uani 0.649(3) 1 d . . P A 1
C146 C -0.1638(12) 0.9491(11) 0.3495(7) 0.0324(17) Uani 0.351(3) 1 d . . P A 2
H146 H -0.2073 0.9824 0.3306 0.039 Uiso 0.351(3) 1 calc R U P A 2
C147 C -0.1847(6) 0.9209(5) 0.3477(3) 0.0324(17) Uani 0.649(3) 1 d . . P A 1
H147 H -0.2259 0.9571 0.3295 0.039 Uiso 0.649(3) 1 calc R U P A 1
C148 C -0.1509(10) 0.9537(10) 0.3980(5) 0.0405(17) Uani 0.351(3) 1 d . . P A 2
H148 H -0.1847 0.9902 0.4117 0.049 Uiso 0.351(3) 1 calc R U P A 2
C149 C -0.1789(5) 0.9168(5) 0.3956(3) 0.0405(17) Uani 0.649(3) 1 d . . P A 1
H149 H -0.2158 0.9499 0.4092 0.049 Uiso 0.649(3) 1 calc R U P A 1
C150 C -0.0866(9) 0.9031(8) 0.4265(4) 0.0355(13) Uani 0.351(3) 1 d . . P A 2
H150 H -0.0769 0.9058 0.4594 0.043 Uiso 0.351(3) 1 calc R U P A 2
C151 C -0.1182(5) 0.8632(4) 0.4240(2) 0.0355(13) Uani 0.649(3) 1 d . . P A 1
H151 H -0.1149 0.8598 0.4563 0.043 Uiso 0.649(3) 1 calc R U P A 1
C152 C -0.1377(3) 0.6044(3) 0.26304(17) 0.0423(9) Uani 1 1 d . . . . .
H152 H -0.1413 0.5934 0.2311 0.051 Uiso 1 1 calc R U . . .
C153 C -0.1166(4) 0.5544(4) 0.34197(18) 0.0610(13) Uani 1 1 d . . . . .
H15A H -0.1641 0.5263 0.3514 0.091 Uiso 1 1 calc R U . . .
H15B H -0.1186 0.6145 0.3483 0.091 Uiso 1 1 calc R U . . .
H15C H -0.0613 0.5322 0.3596 0.091 Uiso 1 1 calc R U . . .
C154 C -0.1238(3) 0.4525(3) 0.2731(2) 0.0623(15) Uani 1 1 d . . . . .
H15D H -0.0703 0.4250 0.2891 0.093 Uiso 1 1 calc R U . . .
H15E H -0.1268 0.4547 0.2397 0.093 Uiso 1 1 calc R U . . .
H15F H -0.1736 0.4209 0.2779 0.093 Uiso 1 1 calc R U . . .
C155 C 0.2668(3) 0.7239(2) 0.23743(17) 0.0389(9) Uani 1 1 d . . . . .
H155 H 0.2832 0.7237 0.2704 0.047 Uiso 1 1 calc R U . . .
C156 C 0.3064(4) 0.7285(5) 0.1643(2) 0.087(2) Uani 1 1 d . . . . .
H15G H 0.3390 0.7722 0.1531 0.131 Uiso 1 1 calc R U . . .
H15H H 0.2443 0.7385 0.1529 0.131 Uiso 1 1 calc R U . . .
H15I H 0.3205 0.6740 0.1529 0.131 Uiso 1 1 calc R U . . .
C157 C 0.4227(3) 0.7310(3) 0.2414(2) 0.0650(16) Uani 1 1 d . . . . .
H15J H 0.4265 0.7366 0.2748 0.098 Uiso 1 1 calc R U . . .
H15K H 0.4523 0.7784 0.2314 0.098 Uiso 1 1 calc R U . . .
H15L H 0.4502 0.6789 0.2352 0.098 Uiso 1 1 calc R U . . .
C158 C 0.1656(2) 1.1434(2) 0.26205(16) 0.0376(9) Uani 1 1 d . . . . .
H158 H 0.1711 1.1393 0.2309 0.045 Uiso 1 1 calc R U . . .
C159 C 0.1459(4) 1.2301(3) 0.3277(2) 0.0655(15) Uani 1 1 d . . . . .
H15M H 0.0993 1.2694 0.3283 0.098 Uiso 1 1 calc R U . . .
H15N H 0.2003 1.2518 0.3475 0.098 Uiso 1 1 calc R U . . .
H15O H 0.1323 1.1760 0.3393 0.098 Uiso 1 1 calc R U . . .
C160 C 0.1541(3) 1.2956(3) 0.25132(19) 0.0498(11) Uani 1 1 d . . . . .
H16A H 0.1599 1.2798 0.2202 0.075 Uiso 1 1 calc R U . . .
H16B H 0.2025 1.3322 0.2666 0.075 Uiso 1 1 calc R U . . .
H16C H 0.0996 1.3252 0.2488 0.075 Uiso 1 1 calc R U . . .
C161 C -0.2798(4) 0.9987(5) 0.2046(3) 0.0321(17) Uani 0.5 1 d D . P C 1
H161 H -0.2866 0.9810 0.2339 0.039 Uiso 0.5 1 calc R U P C 1
C162 C -0.2714(4) 1.0263(5) 0.2251(3) 0.0257(15) Uani 0.5 1 d D . P C 2
H162 H -0.2571 1.0362 0.2578 0.031 Uiso 0.5 1 calc R U P C 2
C163 C -0.3480(6) 1.0164(6) 0.1216(3) 0.046(2) Uani 0.5 1 d D . P C 1
H16D H -0.3839 1.0660 0.1134 0.070 Uiso 0.5 1 calc R U P C 1
H16E H -0.3709 0.9709 0.0995 0.070 Uiso 0.5 1 calc R U P C 1
H16F H -0.2885 1.0293 0.1203 0.070 Uiso 0.5 1 calc R U P C 1
C164 C -0.3785(9) 0.9982(12) 0.1529(4) 0.066(4) Uani 0.5 1 d D . P C 2
H16G H -0.3265 0.9839 0.1425 0.100 Uiso 0.5 1 calc R U P C 2
H16H H -0.4043 1.0487 0.1372 0.100 Uiso 0.5 1 calc R U P C 2
H16I H -0.4202 0.9520 0.1453 0.100 Uiso 0.5 1 calc R U P C 2
C165 C -0.4287(5) 0.9505(6) 0.1747(3) 0.046(2) Uani 0.5 1 d D . P C 1
H16J H -0.4323 0.8935 0.1619 0.069 Uiso 0.5 1 calc R U P C 1
H16K H -0.4788 0.9823 0.1581 0.069 Uiso 0.5 1 calc R U P C 1
H16L H -0.4281 0.9488 0.2078 0.069 Uiso 0.5 1 calc R U P C 1
C166 C -0.4254(5) 1.0203(5) 0.2281(3) 0.0356(17) Uani 0.5 1 d D . P C 2
H16M H -0.4004 1.0328 0.2611 0.053 Uiso 0.5 1 calc R U P C 2
H16N H -0.4576 0.9675 0.2249 0.053 Uiso 0.5 1 calc R U P C 2
H16O H -0.4645 1.0652 0.2146 0.053 Uiso 0.5 1 calc R U P C 2
C167 C 0.6102(8) 0.9343(7) 0.4123(3) 0.069(3) Uani 0.5 1 d D U P D 2
H167 H 0.6557 0.9722 0.4257 0.082 Uiso 0.5 1 calc R U P D 2
C168 C 0.5177(11) 0.8204(10) 0.4217(5) 0.120(6) Uani 0.5 1 d D U P D 2
H16P H 0.4700 0.8282 0.4368 0.180 Uiso 0.5 1 calc R U P D 2
H16Q H 0.5405 0.7638 0.4274 0.180 Uiso 0.5 1 calc R U P D 2
H16R H 0.4966 0.8284 0.3882 0.180 Uiso 0.5 1 calc R U P D 2
C169 C 0.6199(11) 0.8957(11) 0.4893(4) 0.102(5) Uani 0.5 1 d D U P D .
H16S H 0.6823 0.9059 0.4959 0.153 Uiso 0.5 1 calc R U P . .
H16T H 0.6085 0.8465 0.5062 0.153 Uiso 0.5 1 calc R U P . .
H16U H 0.5916 0.9444 0.4993 0.153 Uiso 0.5 1 calc R U P . .
C170 C 0.0519(12) 0.3845(11) 0.4191(4) 0.124(6) Uani 0.5 1 d D U P . .
H170 H 0.0308 0.4379 0.4250 0.149 Uiso 0.5 1 calc R U P . .
C171 C 0.1343(9) 0.2804(7) 0.4510(4) 0.094(4) Uani 0.5 1 d D U P . .
H17A H 0.1822 0.2670 0.4775 0.140 Uiso 0.5 1 calc R U P . .
H17B H 0.1551 0.2804 0.4225 0.140 Uiso 0.5 1 calc R U P . .
H17C H 0.0883 0.2385 0.4479 0.140 Uiso 0.5 1 calc R U P . .
C172 C 0.1113(11) 0.4057(9) 0.5008(4) 0.094(4) Uani 0.5 1 d D U P . .
H17D H 0.1166 0.3661 0.5262 0.140 Uiso 0.5 1 calc R U P . .
H17E H 0.0607 0.4409 0.4994 0.140 Uiso 0.5 1 calc R U P . .
H17F H 0.1634 0.4407 0.5064 0.140 Uiso 0.5 1 calc R U P . .
C173 C 0.8822(4) 0.4085(3) 0.1072(2) 0.0593(13) Uani 1 1 d . U . . .
H173 H 0.8288 0.4371 0.0985 0.071 Uiso 1 1 calc R U . . .
C174 C 0.9996(5) 0.3335(5) 0.0819(3) 0.097(3) Uani 1 1 d . U . . .
H17G H 0.9911 0.2787 0.0663 0.146 Uiso 1 1 calc R U . . .
H17H H 1.0203 0.3261 0.1156 0.146 Uiso 1 1 calc R U . . .
H17I H 1.0424 0.3657 0.0706 0.146 Uiso 1 1 calc R U . . .
C175 C 0.8763(7) 0.3959(6) 0.0221(3) 0.136(4) Uani 1 1 d . U . . .
H17J H 0.8271 0.4334 0.0197 0.204 Uiso 1 1 calc R U . . .
H17K H 0.8564 0.3433 0.0056 0.204 Uiso 1 1 calc R U . . .
H17L H 0.9193 0.4222 0.0082 0.204 Uiso 1 1 calc R U . . .
O32A O 0.1703(5) 1.0227(5) 0.4778(2) 0.0387(15) Uani 0.5 1 d . . P B 2
O36A O 0.0333(7) 0.7913(6) 0.4801(4) 0.0356(10) Uani 0.351(3) 1 d . . P A 2
N8A N -0.3489(5) 0.9908(6) 0.1692(3) 0.038(2) Uani 0.5 1 d D . P C 1
C1A C 0.2136(2) 0.2201(2) 0.11080(13) 0.0319(7) Uani 1 1 d . . . . .
H1A H 0.1895 0.1719 0.1211 0.038 Uiso 1 1 calc R U . . .
C40A C 0.7667(12) 0.3394(9) 0.3681(7) 0.024(3) Uani 0.5 1 d . . P E 1
H40A H 0.7967 0.3041 0.3514 0.029 Uiso 0.5 1 calc R U P E 1
C41A C 0.7909(8) 0.3421(7) 0.4170(4) 0.033(2) Uani 0.5 1 d . . P E 1
H41A H 0.8401 0.3123 0.4331 0.040 Uiso 0.5 1 calc R U P E 1
C42A C 0.7415(10) 0.3899(9) 0.4425(6) 0.036(3) Uani 0.5 1 d . . P E 1
H42A H 0.7524 0.3849 0.4752 0.043 Uiso 0.5 1 calc R U P E 1
C54A C 0.6812(6) 0.1098(5) 0.3798(3) 0.0308(15) Uani 0.5 1 d . . P F 1
H54A H 0.7112 0.0698 0.3659 0.037 Uiso 0.5 1 calc R U P F 1
C55A C 0.6755(6) 0.0990(5) 0.4255(3) 0.0390(19) Uani 0.5 1 d . . P F 1
H55A H 0.7102 0.0583 0.4441 0.047 Uiso 0.5 1 calc R U P F 1
C56A C 0.6184(6) 0.1483(6) 0.4445(3) 0.0305(15) Uani 0.5 1 d . . P F 1
H56A H 0.6093 0.1360 0.4741 0.037 Uiso 0.5 1 calc R U P F 1
O32B O 0.1435(5) 0.9889(6) 0.4873(3) 0.0448(17) Uani 0.5 1 d . . P B 1
O36B O 0.0057(3) 0.7571(3) 0.47774(17) 0.0356(10) Uani 0.649(3) 1 d . . P A 1
N8B N -0.3552(3) 1.0133(4) 0.2035(2) 0.0292(12) Uani 0.5 1 d D . P C 2
C40B C 0.7823(12) 0.3643(9) 0.3689(7) 0.027(3) Uani 0.5 1 d . . P E 2
H40B H 0.8192 0.3392 0.3519 0.033 Uiso 0.5 1 calc R U P E 2
C41B C 0.8132(8) 0.3745(7) 0.4168(4) 0.036(2) Uani 0.5 1 d . . P E 2
H41B H 0.8677 0.3524 0.4320 0.043 Uiso 0.5 1 calc R U P E 2
C42B C 0.7626(9) 0.4181(8) 0.4431(5) 0.031(3) Uani 0.5 1 d . . P E 2
H42B H 0.7847 0.4298 0.4753 0.037 Uiso 0.5 1 calc R U P E 2
C54B C 0.7241(6) 0.1491(6) 0.3909(3) 0.0346(16) Uani 0.5 1 d . . P F 2
H54B H 0.7729 0.1299 0.3808 0.042 Uiso 0.5 1 calc R U P F 2
C55B C 0.7271(6) 0.1485(6) 0.4386(3) 0.0411(19) Uani 0.5 1 d . . P F 2
H55B H 0.7748 0.1245 0.4599 0.049 Uiso 0.5 1 calc R U P F 2
C56B C 0.6576(6) 0.1844(6) 0.4548(3) 0.0345(17) Uani 0.5 1 d . . P F 2
H56B H 0.6618 0.1898 0.4872 0.041 Uiso 0.5 1 calc R U P F 2
C1G C 0.3915(3) 0.6192(3) 0.38054(15) 0.0453(11) Uani 1 1 d . . . . .
H1G H 0.3420 0.6509 0.3666 0.054 Uiso 1 1 calc R U . . .
C1I C 0.3727(2) 0.5004(2) 0.09239(12) 0.0257(6) Uani 1 1 d . . . . .
C1N C 0.2217(2) 0.3124(2) 0.04717(12) 0.0309(7) Uani 1 1 d . . . . .
H1N H 0.2050 0.3255 0.0151 0.037 Uiso 1 1 calc R U . . .
C1O C 0.7772(2) 0.2342(2) 0.23487(13) 0.0291(7) Uani 1 1 d . . . . .
H1O H 0.8017 0.2430 0.2671 0.035 Uiso 1 1 calc R U . . .
C1P C 0.4908(2) 0.22134(19) 0.16730(11) 0.0230(6) Uani 1 1 d . . . . .
C1Q C 0.1890(3) 0.2388(2) 0.06353(13) 0.0354(8) Uani 1 1 d . . . . .
H1Q H 0.1505 0.2027 0.0424 0.042 Uiso 1 1 calc R U . . .
C1S C 0.2785(2) 0.3651(2) 0.07853(12) 0.0256(6) Uani 1 1 d . . . . .
C1T C 0.4312(3) 0.1441(2) 0.09254(13) 0.0337(8) Uani 1 1 d . . . . .
H1T H 0.3989 0.0981 0.0764 0.040 Uiso 1 1 calc R U . . .
C1U C 0.3688(2) 0.40362(18) 0.15916(11) 0.0199(6) Uani 1 1 d . . . . .
C1V C 0.4422(3) 0.1537(2) 0.14086(13) 0.0302(7) Uani 1 1 d . . . . .
H1V H 0.4163 0.1138 0.1567 0.036 Uiso 1 1 calc R U . . .
O1W O 0.6071(5) 0.0150(4) 0.2879(2) 0.0565(17) Uani 0.5 1 d . . P G 1
C1W C 0.5777(2) 0.35656(19) 0.16612(11) 0.0205(6) Uani 1 1 d . . . . .
C1X C 0.3076(2) 0.34633(19) 0.12779(11) 0.0205(6) Uani 1 1 d . . . . .
C1Y C 0.5163(2) 0.2717(2) 0.09255(11) 0.0243(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O5 2.047(2) . ?
Co1 O6 2.135(2) . ?
Co1 O11 2.144(2) . ?
Co1 O14 2.088(2) . ?
Co1 O15 1.973(2) . ?
Co1 O19 2.079(2) . ?
Co2 O3 2.146(2) . ?
Co2 O6 2.079(2) . ?
Co2 O7 1.957(2) . ?
Co2 O10 2.121(2) . ?
Co2 O11 2.040(2) . ?
Co2 O20 2.091(2) . ?
Co3 O2 2.142(2) . ?
Co3 O3 2.041(2) . ?
Co3 O9 1.966(2) . ?
Co3 O10 2.084(2) . ?
Co3 O13 2.129(2) . ?
Co3 O18 2.096(2) . ?
Co4 O1 1.965(2) . ?
Co4 O2 2.082(2) . ?
Co4 O5 2.130(2) . ?
Co4 O13 2.058(2) . ?
Co4 O14 2.143(2) . ?
Co4 O17 2.083(2) . ?
Co5 O21 2.059(3) . ?
Co5 O22 2.132(2) . ?
Co5 O29 1.958(3) . ?
Co5 O30 2.079(2) . ?
Co5 O35 2.148(3) . ?
Co5 O40 2.100(2) . ?
Co6 O22 2.082(2) . ?
Co6 O23 1.977(2) . ?
Co6 O27 2.145(2) . ?
Co6 O34 2.144(2) . ?
Co6 O35 2.053(3) . ?
Co6 O37 2.089(3) . ?
Co7 O26 2.129(2) . ?
Co7 O27 2.065(2) . ?
Co7 O31 2.155(2) . ?
Co7 O33 1.976(2) . ?
Co7 O34 2.064(2) . ?
Co7 O38 2.089(2) . ?
Co8 O21 2.157(2) . ?
Co8 O25 1.963(3) . ?
Co8 O26 2.080(2) . ?
Co8 O30 2.110(3) . ?
Co8 O31 2.057(3) . ?
Co8 O39 2.102(2) . ?
O1 C11 1.296(4) . ?
O2 C1U 1.263(4) . ?
O3 C1 1.322(4) . ?
O4 C15 1.219(4) . ?
O5 C1P 1.328(4) . ?
O6 C1W 1.263(4) . ?
O7 C25 1.298(4) . ?
O8 C24 1.230(4) . ?
O9 C29 1.295(4) . ?
O10 C35 1.265(4) . ?
O11 C39 1.329(4) . ?
O12 C38 1.229(4) . ?
O13 C43 1.330(4) . ?
O14 C49 1.262(4) . ?
O15 C53 1.294(5) . ?
O16 C52 1.223(4) . ?
O17 C57 1.243(4) . ?
O18 C60 1.242(4) . ?
O19 C1O 1.236(4) . ?
O20 C66 1.241(5) . ?
O21 C69 1.318(4) . ?
O22 C75 1.257(4) . ?
O23 C79 1.296(4) . ?
O24 C78 1.221(5) . ?
O25 C83 1.291(5) . ?
O26 C88 1.265(4) . ?
O27 C92 1.320(4) . ?
O28 C91 1.224(5) . ?
O29 C96 1.240(13) . ?
O29 C97 1.395(11) . ?
O30 C108 1.19(2) . ?
O30 C109 1.369(18) . ?
O31 C116 1.246(18) . ?
O31 C117 1.413(17) . ?
O33 C4 1.29(3) . ?
O33 C125 1.308(12) . ?
O34 C136 1.26(3) . ?
O34 C137 1.277(12) . ?
O35 C144 1.397(19) . ?
O35 C145 1.322(10) . ?
O37 C152 1.289(5) . ?
O38 C155 1.241(5) . ?
O39 C158 1.244(5) . ?
O40 C161 1.188(7) . ?
O40 C162 1.270(7) . ?
O41 C167 1.196(8) . ?
O42 C170 1.167(9) . ?
O43 C173 1.202(7) . ?
N1 C57 1.323(4) . ?
N1 C58 1.458(5) . ?
N1 C59 1.454(5) . ?
N2 C60 1.312(4) . ?
N2 C61 1.451(5) . ?
N2 C62 1.468(5) . ?
N3 C64 1.447(5) . ?
N3 C65 1.457(5) . ?
N3 C1O 1.311(5) . ?
N4 C66 1.297(6) . ?
N4 C67 1.373(8) . ?
N4 C68 1.465(7) . ?
N5 C152 1.319(5) . ?
N5 C153 1.429(6) . ?
N5 C154 1.475(6) . ?
N6 C155 1.302(5) . ?
N6 C156 1.427(8) . ?
N6 C157 1.476(6) . ?
N7 C158 1.315(5) . ?
N7 C159 1.455(6) . ?
N7 C160 1.453(6) . ?
N9 C167 1.294(8) . ?
N9 C168 1.443(9) . ?
N9 C169 1.387(9) . ?
N10 C170 1.269(9) . ?
N10 C171 1.406(9) . ?
N10 C172 1.382(9) . ?
N11 C173 1.338(7) . ?
N11 C174 1.461(8) . ?
N11 C175 1.458(9) . ?
C1 C2 1.415(4) . ?
C1 C7 1.428(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.375(5) . ?
C3 H3 0.9300 . ?
C3 C10 1.386(5) . ?
C4 C126 1.39(3) . ?
C4 C134 1.43(3) . ?
C6 C83 1.434(5) . ?
C6 C87 1.428(5) . ?
C6 C88 1.443(4) . ?
C7 C1I 1.415(4) . ?
C7 C1U 1.471(4) . ?
C10 H10 0.9300 . ?
C10 C1I 1.388(5) . ?
C11 C1A 1.418(5) . ?
C11 C1X 1.437(4) . ?
C13 H13 0.9300 . ?
C13 C32 1.402(6) . ?
C13 C1G 1.366(6) . ?
C14 H14 0.9300 . ?
C14 C23 1.379(5) . ?
C14 C27 1.397(5) . ?
C15 C1I 1.489(5) . ?
C15 C1S 1.484(5) . ?
C18 H18 0.9300 . ?
C18 C1T 1.393(5) . ?
C18 C1Y 1.388(5) . ?
C20 C1P 1.427(4) . ?
C20 C1W 1.458(4) . ?
C20 C1Y 1.414(4) . ?
C22 C23 1.429(4) . ?
C22 C25 1.433(4) . ?
C22 C1W 1.451(4) . ?
C23 C24 1.485(5) . ?
C24 C1Y 1.487(4) . ?
C25 C26 1.428(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.367(5) . ?
C27 H27 0.9300 . ?
C29 C34 1.435(4) . ?
C29 C1G 1.434(5) . ?
C32 H32 0.9300 . ?
C32 C33 1.376(5) . ?
C33 C34 1.424(4) . ?
C33 C38 1.475(5) . ?
C34 C35 1.450(4) . ?
C35 C36 1.465(4) . ?
C36 C37 1.412(5) . ?
C36 C39 1.429(5) . ?
C37 C38 1.485(5) . ?
C37 C42A 1.378(17) . ?
C37 C42B 1.418(14) . ?
C39 C40A 1.41(2) . ?
C39 C40B 1.428(19) . ?
C43 C44 1.410(5) . ?
C43 C48 1.422(5) . ?
C44 H44 0.9300 . ?
C44 C45 1.380(5) . ?
C45 H45 0.9300 . ?
C45 C46 1.386(5) . ?
C46 H46 0.9300 . ?
C46 C47 1.388(5) . ?
C47 C48 1.419(4) . ?
C47 C52 1.481(5) . ?
C48 C49 1.469(4) . ?
C49 C50 1.442(5) . ?
C50 C51 1.417(5) . ?
C50 C53 1.425(5) . ?
C51 C52 1.469(5) . ?
C51 C56A 1.350(8) . ?
C51 C56B 1.506(9) . ?
C53 C54A 1.414(8) . ?
C53 C54B 1.553(9) . ?
C57 H57 0.9300 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C59 H59A 0.9600 . ?
C59 H59B 0.9600 . ?
C59 H59C 0.9600 . ?
C60 H60 0.9300 . ?
C61 H61A 0.9600 . ?
C61 H61B 0.9600 . ?
C61 H61C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 H66 0.9300 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 C70 1.419(5) . ?
C69 C74 1.431(5) . ?
C70 H70 0.9300 . ?
C70 C71 1.364(6) . ?
C71 H71 0.9300 . ?
C71 C72 1.394(6) . ?
C72 H72 0.9300 . ?
C72 C73 1.379(5) . ?
C73 C74 1.411(5) . ?
C73 C78 1.492(5) . ?
C74 C75 1.475(4) . ?
C75 C76 1.449(4) . ?
C76 C77 1.427(5) . ?
C76 C79 1.429(4) . ?
C77 C78 1.479(5) . ?
C77 C82 1.372(5) . ?
C79 C80 1.421(5) . ?
C80 H80 0.9300 . ?
C80 C81 1.369(5) . ?
C81 H81 0.9300 . ?
C81 C82 1.390(6) . ?
C82 H82 0.9300 . ?
C83 C84 1.426(5) . ?
C84 H84 0.9300 . ?
C84 C85 1.363(7) . ?
C85 H85 0.9300 . ?
C85 C86 1.402(6) . ?
C86 H86 0.9300 . ?
C86 C87 1.385(5) . ?
C87 C91 1.475(5) . ?
C88 C89 1.462(4) . ?
C89 C90 1.412(5) . ?
C89 C92 1.440(4) . ?
C90 C91 1.478(5) . ?
C90 C95 1.381(5) . ?
C92 C93 1.413(4) . ?
C93 H93 0.9300 . ?
C93 C94 1.385(5) . ?
C94 H94 0.9300 . ?
C94 C95 1.394(5) . ?
C95 H95 0.9300 . ?
C96 C98 1.456(14) . ?
C96 C106 1.425(15) . ?
C97 C99 1.424(14) . ?
C97 C107 1.440(15) . ?
C98 H98 0.9300 . ?
C98 C100 1.343(11) . ?
C99 H99 0.9300 . ?
C99 C101 1.363(11) . ?
C100 H100 0.9300 . ?
C100 C102 1.405(11) . ?
C101 H101 0.9300 . ?
C101 C103 1.399(11) . ?
C102 H102 0.9300 . ?
C102 C104 1.392(10) . ?
C103 H103 0.9300 . ?
C103 C105 1.367(10) . ?
C104 C106 1.411(11) . ?
C104 C114 1.476(10) . ?
C105 C107 1.416(11) . ?
C105 C115 1.471(10) . ?
C106 C108 1.43(2) . ?
C107 C109 1.47(2) . ?
C108 C110 1.50(2) . ?
C109 C111 1.43(2) . ?
C110 C112 1.411(16) . ?
C110 C116 1.44(2) . ?
C111 C113 1.401(15) . ?
C111 C117 1.43(2) . ?
C112 C114 1.484(11) . ?
C112 C122 1.377(10) . ?
C113 C115 1.515(11) . ?
C113 C123 1.390(10) . ?
C114 O32A 1.234(10) . ?
C115 O32B 1.232(10) . ?
C116 C118 1.40(2) . ?
C117 C119 1.42(2) . ?
C118 H118 0.9300 . ?
C118 C120 1.373(16) . ?
C119 H119 0.9300 . ?
C119 C121 1.374(16) . ?
C120 H120 0.9300 . ?
C120 C122 1.399(11) . ?
C121 H121 0.9300 . ?
C121 C123 1.396(11) . ?
C122 H122 0.9300 . ?
C123 H123 0.9300 . ?
C125 C127 1.439(14) . ?
C125 C135 1.425(15) . ?
C126 H126 0.9300 . ?
C126 C128 1.36(2) . ?
C127 H127 0.9300 . ?
C127 C129 1.379(10) . ?
C128 H128 0.9300 . ?
C128 C130 1.413(17) . ?
C129 H129 0.9300 . ?
C129 C131 1.398(9) . ?
C130 H130 0.9300 . ?
C130 C132 1.387(16) . ?
C131 H131 0.9300 . ?
C131 C133 1.373(8) . ?
C132 C134 1.40(2) . ?
C132 C142 1.473(17) . ?
C133 C135 1.430(11) . ?
C133 C143 1.478(8) . ?
C134 C136 1.45(3) . ?
C135 C137 1.448(15) . ?
C136 C138 1.50(3) . ?
C137 C139 1.454(15) . ?
C138 C140 1.38(2) . ?
C138 C144 1.42(3) . ?
C139 C141 1.437(10) . ?
C139 C145 1.425(12) . ?
C140 C142 1.500(16) . ?
C140 C150 1.382(17) . ?
C141 C143 1.487(8) . ?
C141 C151 1.376(8) . ?
C142 O36A 1.229(15) . ?
C143 O36B 1.221(8) . ?
C144 C146 1.37(3) . ?
C145 C147 1.429(13) . ?
C146 H146 0.9300 . ?
C146 C148 1.37(3) . ?
C147 H147 0.9300 . ?
C147 C149 1.376(12) . ?
C148 H148 0.9300 . ?
C148 C150 1.396(19) . ?
C149 H149 0.9300 . ?
C149 C151 1.390(9) . ?
C150 H150 0.9300 . ?
C151 H151 0.9300 . ?
C152 H152 0.9300 . ?
C153 H15A 0.9600 . ?
C153 H15B 0.9600 . ?
C153 H15C 0.9600 . ?
C154 H15D 0.9600 . ?
C154 H15E 0.9600 . ?
C154 H15F 0.9600 . ?
C155 H155 0.9300 . ?
C156 H15G 0.9600 . ?
C156 H15H 0.9600 . ?
C156 H15I 0.9600 . ?
C157 H15J 0.9600 . ?
C157 H15K 0.9600 . ?
C157 H15L 0.9600 . ?
C158 H158 0.9300 . ?
C159 H15M 0.9600 . ?
C159 H15N 0.9600 . ?
C159 H15O 0.9600 . ?
C160 H16A 0.9600 . ?
C160 H16B 0.9600 . ?
C160 H16C 0.9600 . ?
C161 H161 0.9300 . ?
C161 N8A 1.301(8) . ?
C162 H162 0.9300 . ?
C162 N8B 1.321(7) . ?
C163 H16D 0.9600 . ?
C163 H16E 0.9600 . ?
C163 H16F 0.9600 . ?
C163 N8A 1.451(8) . ?
C164 H16G 0.9600 . ?
C164 H16H 0.9600 . ?
C164 H16I 0.9600 . ?
C164 N8B 1.441(8) . ?
C165 H16J 0.9600 . ?
C165 H16K 0.9600 . ?
C165 H16L 0.9600 . ?
C165 N8A 1.439(8) . ?
C166 H16M 0.9600 . ?
C166 H16N 0.9600 . ?
C166 H16O 0.9600 . ?
C166 N8B 1.452(7) . ?
C167 H167 0.9300 . ?
C168 H16P 0.9600 . ?
C168 H16Q 0.9600 . ?
C168 H16R 0.9600 . ?
C169 H16S 0.9600 . ?
C169 H16T 0.9600 . ?
C169 H16U 0.9600 . ?
C170 H170 0.9300 . ?
C171 H17A 0.9600 . ?
C171 H17B 0.9600 . ?
C171 H17C 0.9600 . ?
C172 H17D 0.9600 . ?
C172 H17E 0.9600 . ?
C172 H17F 0.9600 . ?
C173 H173 0.9300 . ?
C174 H17G 0.9600 . ?
C174 H17H 0.9600 . ?
C174 H17I 0.9600 . ?
C175 H17J 0.9600 . ?
C175 H17K 0.9600 . ?
C175 H17L 0.9600 . ?
C1A H1A 0.9300 . ?
C1A C1Q 1.370(5) . ?
C40A H40A 0.9300 . ?
C40A C41A 1.38(2) . ?
C41A H41A 0.9300 . ?
C41A C42A 1.41(2) . ?
C42A H42A 0.9300 . ?
C54A H54A 0.9300 . ?
C54A C55A 1.365(10) . ?
C55A H55A 0.9300 . ?
C55A C56A 1.390(11) . ?
C56A H56A 0.9300 . ?
C40B H40B 0.9300 . ?
C40B C41B 1.36(2) . ?
C41B H41B 0.9300 . ?
C41B C42B 1.399(19) . ?
C42B H42B 0.9300 . ?
C54B H54B 0.9300 . ?
C54B C55B 1.376(11) . ?
C55B H55B 0.9300 . ?
C55B C56B 1.401(12) . ?
C56B H56B 0.9300 . ?
C1G H1G 0.9300 . ?
C1N H1N 0.9300 . ?
C1N C1Q 1.397(5) . ?
C1N C1S 1.371(5) . ?
C1O H1O 0.9300 . ?
C1P C1V 1.406(5) . ?
C1Q H1Q 0.9300 . ?
C1S C1X 1.428(4) . ?
C1T H1T 0.9300 . ?
C1T C1V 1.377(5) . ?
C1U C1X 1.448(4) . ?
C1V H1V 0.9300 . ?

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 Co1 O6 77.99(9) . . ?
O5 Co1 O11 144.29(8) . . ?
O5 Co1 O14 77.01(9) . . ?
O5 Co1 O19 95.65(9) . . ?
O6 Co1 O11 73.49(8) . . ?
O14 Co1 O6 103.64(8) . . ?
O14 Co1 O11 89.21(9) . . ?
O15 Co1 O5 111.43(11) . . ?
O15 Co1 O6 169.49(11) . . ?
O15 Co1 O11 99.28(11) . . ?
O15 Co1 O14 83.57(10) . . ?
O15 Co1 O19 91.96(10) . . ?
O19 Co1 O6 82.19(9) . . ?
O19 Co1 O11 101.22(9) . . ?
O19 Co1 O14 169.22(9) . . ?
O6 Co2 O3 89.42(8) . . ?
O6 Co2 O10 104.59(8) . . ?
O6 Co2 O20 172.30(10) . . ?
O7 Co2 O3 98.76(9) . . ?
O7 Co2 O6 84.14(9) . . ?
O7 Co2 O10 168.45(9) . . ?
O7 Co2 O11 110.90(10) . . ?
O7 Co2 O20 90.26(10) . . ?
O10 Co2 O3 74.13(8) . . ?
O11 Co2 O3 145.46(9) . . ?
O11 Co2 O6 76.86(9) . . ?
O11 Co2 O10 78.88(8) . . ?
O11 Co2 O20 100.37(9) . . ?
O20 Co2 O3 96.67(9) . . ?
O20 Co2 O10 81.70(9) . . ?
O3 Co3 O2 78.19(8) . . ?
O3 Co3 O10 77.12(9) . . ?
O3 Co3 O13 144.46(9) . . ?
O3 Co3 O18 99.55(9) . . ?
O9 Co3 O2 168.79(10) . . ?
O9 Co3 O3 111.24(11) . . ?
O9 Co3 O10 83.93(9) . . ?
O9 Co3 O13 99.69(10) . . ?
O9 Co3 O18 90.08(10) . . ?
O10 Co3 O2 104.59(8) . . ?
O10 Co3 O13 89.61(9) . . ?
O10 Co3 O18 171.47(9) . . ?
O13 Co3 O2 73.47(8) . . ?
O18 Co3 O2 82.16(9) . . ?
O18 Co3 O13 97.39(9) . . ?
O1 Co4 O2 84.44(9) . . ?
O1 Co4 O5 97.67(10) . . ?
O1 Co4 O13 112.98(10) . . ?
O1 Co4 O14 167.63(9) . . ?
O1 Co4 O17 91.20(10) . . ?
O2 Co4 O5 90.09(8) . . ?
O2 Co4 O14 104.47(8) . . ?
O2 Co4 O17 169.75(10) . . ?
O5 Co4 O14 74.09(9) . . ?
O13 Co4 O2 76.21(9) . . ?
O13 Co4 O5 144.55(9) . . ?
O13 Co4 O14 77.92(9) . . ?
O13 Co4 O17 97.12(9) . . ?
O17 Co4 O5 99.70(9) . . ?
O17 Co4 O14 81.34(9) . . ?
O21 Co5 O22 78.37(9) . . ?
O21 Co5 O30 77.45(10) . . ?
O21 Co5 O35 145.05(9) . . ?
O21 Co5 O40 101.30(10) . . ?
O22 Co5 O35 74.24(9) . . ?
O29 Co5 O21 109.23(12) . . ?
O29 Co5 O22 170.84(11) . . ?
O29 Co5 O30 83.75(10) . . ?
O29 Co5 O35 100.42(12) . . ?
O29 Co5 O40 92.18(11) . . ?
O30 Co5 O22 103.26(9) . . ?
O30 Co5 O35 88.07(10) . . ?
O30 Co5 O40 175.02(10) . . ?
O40 Co5 O22 81.09(9) . . ?
O40 Co5 O35 95.52(10) . . ?
O22 Co6 O27 87.21(9) . . ?
O22 Co6 O34 102.77(9) . . ?
O22 Co6 O37 174.73(10) . . ?
O23 Co6 O22 83.54(9) . . ?
O23 Co6 O27 103.18(10) . . ?
O23 Co6 O34 172.66(10) . . ?
O23 Co6 O35 107.59(11) . . ?
O23 Co6 O37 92.78(10) . . ?
O34 Co6 O27 73.69(9) . . ?
O35 Co6 O22 77.32(9) . . ?
O35 Co6 O27 143.47(9) . . ?
O35 Co6 O34 77.76(9) . . ?
O35 Co6 O37 100.33(11) . . ?
O37 Co6 O27 97.31(10) . . ?
O37 Co6 O34 81.17(10) . . ?
O26 Co7 O31 74.02(9) . . ?
O27 Co7 O26 77.92(9) . . ?
O27 Co7 O31 144.57(9) . . ?
O27 Co7 O38 99.87(9) . . ?
O33 Co7 O26 169.92(10) . . ?
O33 Co7 O27 110.10(10) . . ?
O33 Co7 O31 100.52(10) . . ?
O33 Co7 O34 84.35(10) . . ?
O33 Co7 O38 91.01(10) . . ?
O34 Co7 O26 103.77(9) . . ?
O34 Co7 O27 77.04(9) . . ?
O34 Co7 O31 89.02(9) . . ?
O34 Co7 O38 173.08(9) . . ?
O38 Co7 O26 81.40(9) . . ?
O38 Co7 O31 96.89(9) . . ?
O25 Co8 O21 101.22(11) . . ?
O25 Co8 O26 84.12(10) . . ?
O25 Co8 O30 170.85(10) . . ?
O25 Co8 O31 107.87(11) . . ?
O25 Co8 O39 90.48(12) . . ?
O26 Co8 O21 88.52(9) . . ?
O26 Co8 O30 103.76(9) . . ?
O26 Co8 O39 174.50(11) . . ?
O30 Co8 O21 74.68(9) . . ?
O31 Co8 O21 145.77(10) . . ?
O31 Co8 O26 77.12(9) . . ?
O31 Co8 O30 78.79(10) . . ?
O31 Co8 O39 103.63(11) . . ?
O39 Co8 O21 93.61(10) . . ?
O39 Co8 O30 81.71(11) . . ?
C11 O1 Co4 130.0(2) . . ?
Co4 O2 Co3 101.57(9) . . ?
C1U O2 Co3 121.71(18) . . ?
C1U O2 Co4 132.24(19) . . ?
Co3 O3 Co2 102.07(9) . . ?
C1 O3 Co2 124.7(2) . . ?
C1 O3 Co3 120.33(19) . . ?
Co1 O5 Co4 102.85(9) . . ?
C1P O5 Co1 122.1(2) . . ?
C1P O5 Co4 120.9(2) . . ?
Co2 O6 Co1 101.49(9) . . ?
C1W O6 Co1 124.88(19) . . ?
C1W O6 Co2 130.96(19) . . ?
C25 O7 Co2 127.3(2) . . ?
C29 O9 Co3 128.9(2) . . ?
Co3 O10 Co2 101.50(9) . . ?
C35 O10 Co2 122.7(2) . . ?
C35 O10 Co3 131.8(2) . . ?
Co2 O11 Co1 102.46(9) . . ?
C39 O11 Co1 122.5(2) . . ?
C39 O11 Co2 120.8(2) . . ?
Co4 O13 Co3 102.81(10) . . ?
C43 O13 Co3 121.09(19) . . ?
C43 O13 Co4 121.88(19) . . ?
Co1 O14 Co4 101.05(9) . . ?
C49 O14 Co1 132.1(2) . . ?
C49 O14 Co4 122.8(2) . . ?
C53 O15 Co1 128.8(2) . . ?
C57 O17 Co4 123.1(2) . . ?
C60 O18 Co3 118.4(2) . . ?
C1O O19 Co1 124.6(2) . . ?
C66 O20 Co2 117.4(3) . . ?
Co5 O21 Co8 100.91(11) . . ?
C69 O21 Co5 123.7(2) . . ?
C69 O21 Co8 119.0(2) . . ?
Co6 O22 Co5 101.96(10) . . ?
C75 O22 Co5 122.7(2) . . ?
C75 O22 Co6 130.9(2) . . ?
C79 O23 Co6 129.0(2) . . ?
C83 O25 Co8 129.9(2) . . ?
Co8 O26 Co7 101.93(10) . . ?
C88 O26 Co7 121.79(19) . . ?
C88 O26 Co8 131.4(2) . . ?
Co7 O27 Co6 102.17(10) . . ?
C92 O27 Co6 122.18(19) . . ?
C92 O27 Co7 121.65(19) . . ?
C96 O29 Co5 131.5(6) . . ?
C97 O29 Co5 125.4(5) . . ?
Co5 O30 Co8 101.80(11) . . ?
C108 O30 Co5 131.9(10) . . ?
C108 O30 Co8 117.0(9) . . ?
C109 O30 Co5 130.1(9) . . ?
C109 O30 Co8 126.7(9) . . ?
Co8 O31 Co7 101.78(10) . . ?
C116 O31 Co7 126.7(8) . . ?
C116 O31 Co8 118.8(9) . . ?
C117 O31 Co7 117.0(7) . . ?
C117 O31 Co8 123.9(8) . . ?
C4 O33 Co7 124.0(11) . . ?
C125 O33 Co7 130.3(5) . . ?
Co7 O34 Co6 102.26(10) . . ?
C136 O34 Co6 130.1(10) . . ?
C136 O34 Co7 127.1(11) . . ?
C137 O34 Co6 119.6(4) . . ?
C137 O34 Co7 132.1(5) . . ?
Co6 O35 Co5 102.40(10) . . ?
C144 O35 Co5 107.6(6) . . ?
C144 O35 Co6 131.2(8) . . ?
C145 O35 Co5 126.6(3) . . ?
C145 O35 Co6 118.5(4) . . ?
C152 O37 Co6 121.2(3) . . ?
C155 O38 Co7 118.9(2) . . ?
C158 O39 Co8 116.6(3) . . ?
C161 O40 Co5 127.1(4) . . ?
C162 O40 Co5 113.3(3) . . ?
C57 N1 C58 120.9(3) . . ?
C57 N1 C59 120.7(3) . . ?
C59 N1 C58 118.4(3) . . ?
C60 N2 C61 120.2(3) . . ?
C60 N2 C62 120.9(3) . . ?
C61 N2 C62 118.5(3) . . ?
C64 N3 C65 118.1(4) . . ?
C1O N3 C64 120.9(3) . . ?
C1O N3 C65 120.9(4) . . ?
C66 N4 C67 118.4(5) . . ?
C66 N4 C68 123.0(5) . . ?
C67 N4 C68 118.5(5) . . ?
C152 N5 C153 120.1(4) . . ?
C152 N5 C154 119.3(4) . . ?
C153 N5 C154 120.6(4) . . ?
C155 N6 C156 119.2(4) . . ?
C155 N6 C157 120.5(5) . . ?
C156 N6 C157 120.1(4) . . ?
C158 N7 C159 120.5(4) . . ?
C158 N7 C160 121.5(4) . . ?
C160 N7 C159 117.9(4) . . ?
C167 N9 C168 118.7(10) . . ?
C167 N9 C169 117.7(10) . . ?
C169 N9 C168 122.9(10) . . ?
C170 N10 C171 107.7(12) . . ?
C170 N10 C172 124.3(12) . . ?
C172 N10 C171 127.7(10) . . ?
C173 N11 C174 121.0(5) . . ?
C173 N11 C175 122.8(6) . . ?
C175 N11 C174 116.1(6) . . ?
O3 C1 C2 117.4(3) . . ?
O3 C1 C7 124.6(3) . . ?
C2 C1 C7 118.0(3) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.8(3) . . ?
C3 C2 H2 119.1 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C10 120.4(3) . . ?
C10 C3 H3 119.8 . . ?
O33 C4 C126 116(2) . . ?
O33 C4 C134 126(2) . . ?
C126 C4 C134 118(2) . . ?
C83 C6 C88 121.8(3) . . ?
C87 C6 C83 119.0(3) . . ?
C87 C6 C88 119.1(3) . . ?
C1 C7 C1U 121.7(3) . . ?
C1I C7 C1 118.6(3) . . ?
C1I C7 C1U 119.6(3) . . ?
C3 C10 H10 120.2 . . ?
C3 C10 C1I 119.6(3) . . ?
C1I C10 H10 120.2 . . ?
O1 C11 C1A 117.3(3) . . ?
O1 C11 C1X 125.8(3) . . ?
C1A C11 C1X 116.9(3) . . ?
C32 C13 H13 120.0 . . ?
C1G C13 H13 120.0 . . ?
C1G C13 C32 120.0(4) . . ?
C23 C14 H14 120.0 . . ?
C23 C14 C27 119.9(3) . . ?
C27 C14 H14 120.0 . . ?
O4 C15 C1I 120.7(3) . . ?
O4 C15 C1S 121.3(3) . . ?
C1S C15 C1I 118.0(3) . . ?
C1T C18 H18 120.3 . . ?
C1Y C18 H18 120.3 . . ?
C1Y C18 C1T 119.3(3) . . ?
C1P C20 C1W 121.7(3) . . ?
C1Y C20 C1P 118.7(3) . . ?
C1Y C20 C1W 119.6(3) . . ?
C23 C22 C25 118.3(3) . . ?
C23 C22 C1W 119.3(3) . . ?
C25 C22 C1W 122.3(3) . . ?
C14 C23 C22 121.7(3) . . ?
C14 C23 C24 117.7(3) . . ?
C22 C23 C24 120.7(3) . . ?
O8 C24 C23 121.5(3) . . ?
O8 C24 C1Y 120.6(3) . . ?
C23 C24 C1Y 118.0(3) . . ?
O7 C25 C22 125.6(3) . . ?
O7 C25 C26 116.9(3) . . ?
C26 C25 C22 117.5(3) . . ?
C25 C26 H26 118.8 . . ?
C27 C26 C25 122.5(3) . . ?
C27 C26 H26 118.8 . . ?
C14 C27 H27 120.0 . . ?
C26 C27 C14 120.0(3) . . ?
C26 C27 H27 120.0 . . ?
O9 C29 C34 126.5(3) . . ?
O9 C29 C1G 116.7(3) . . ?
C1G C29 C34 116.8(3) . . ?
C13 C32 H32 120.2 . . ?
C33 C32 C13 119.6(4) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 C34 121.9(3) . . ?
C32 C33 C38 117.7(3) . . ?
C34 C33 C38 120.4(3) . . ?
C29 C34 C35 121.3(3) . . ?
C33 C34 C29 118.8(3) . . ?
C33 C34 C35 120.0(3) . . ?
O10 C35 C34 120.9(3) . . ?
O10 C35 C36 118.4(3) . . ?
C34 C35 C36 120.7(3) . . ?
C37 C36 C35 119.5(3) . . ?
C37 C36 C39 118.5(3) . . ?
C39 C36 C35 122.0(3) . . ?
C36 C37 C38 120.9(3) . . ?
C36 C37 C42B 122.2(6) . . ?
C42A C37 C36 119.9(7) . . ?
C42A C37 C38 117.8(8) . . ?
C42B C37 C38 115.8(6) . . ?
O12 C38 C33 120.9(3) . . ?
O12 C38 C37 120.7(3) . . ?
C33 C38 C37 118.3(3) . . ?
O11 C39 C36 124.3(3) . . ?
O11 C39 C40A 116.0(8) . . ?
O11 C39 C40B 118.4(8) . . ?
C40A C39 C36 119.1(8) . . ?
C40B C39 C36 116.4(8) . . ?
O13 C43 C44 117.6(3) . . ?
O13 C43 C48 124.2(3) . . ?
C44 C43 C48 118.2(3) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 C43 122.2(3) . . ?
C45 C44 H44 118.9 . . ?
C44 C45 H45 120.0 . . ?
C44 C45 C46 120.0(3) . . ?
C46 C45 H45 120.0 . . ?
C45 C46 H46 120.2 . . ?
C45 C46 C47 119.6(3) . . ?
C47 C46 H46 120.2 . . ?
C46 C47 C48 121.8(3) . . ?
C46 C47 C52 117.8(3) . . ?
C48 C47 C52 120.4(3) . . ?
C43 C48 C49 121.9(3) . . ?
C47 C48 C43 118.2(3) . . ?
C47 C48 C49 119.8(3) . . ?
O14 C49 C48 118.6(3) . . ?
O14 C49 C50 120.8(3) . . ?
C50 C49 C48 120.6(3) . . ?
C51 C50 C49 119.4(3) . . ?
C51 C50 C53 119.4(3) . . ?
C53 C50 C49 121.2(3) . . ?
C50 C51 C52 121.8(3) . . ?
C50 C51 C56B 120.0(5) . . ?
C52 C51 C56B 115.6(4) . . ?
C56A C51 C50 120.2(4) . . ?
C56A C51 C52 115.3(4) . . ?
O16 C52 C47 121.1(3) . . ?
O16 C52 C51 121.0(3) . . ?
C51 C52 C47 117.9(3) . . ?
O15 C53 C50 127.2(3) . . ?
O15 C53 C54A 115.3(4) . . ?
O15 C53 C54B 114.3(4) . . ?
C50 C53 C54B 115.7(4) . . ?
C54A C53 C50 115.0(4) . . ?
O17 C57 N1 123.8(3) . . ?
O17 C57 H57 118.1 . . ?
N1 C57 H57 118.1 . . ?
N1 C58 H58A 109.5 . . ?
N1 C58 H58B 109.5 . . ?
N1 C58 H58C 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
N1 C59 H59A 109.5 . . ?
N1 C59 H59B 109.5 . . ?
N1 C59 H59C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
O18 C60 N2 124.2(3) . . ?
O18 C60 H60 117.9 . . ?
N2 C60 H60 117.9 . . ?
N2 C61 H61A 109.5 . . ?
N2 C61 H61B 109.5 . . ?
N2 C61 H61C 109.5 . . ?
H61A C61 H61B 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N2 C62 H62A 109.5 . . ?
N2 C62 H62B 109.5 . . ?
N2 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N3 C64 H64A 109.5 . . ?
N3 C64 H64B 109.5 . . ?
N3 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
N3 C65 H65A 109.5 . . ?
N3 C65 H65B 109.5 . . ?
N3 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
O20 C66 N4 126.8(5) . . ?
O20 C66 H66 116.6 . . ?
N4 C66 H66 116.6 . . ?
N4 C67 H67A 109.5 . . ?
N4 C67 H67B 109.5 . . ?
N4 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N4 C68 H68A 109.5 . . ?
N4 C68 H68B 109.5 . . ?
N4 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
O21 C69 C70 118.7(3) . . ?
O21 C69 C74 124.6(3) . . ?
C70 C69 C74 116.8(3) . . ?
C69 C70 H70 118.8 . . ?
C71 C70 C69 122.5(4) . . ?
C71 C70 H70 118.8 . . ?
C70 C71 H71 119.6 . . ?
C70 C71 C72 120.7(3) . . ?
C72 C71 H71 119.6 . . ?
C71 C72 H72 120.6 . . ?
C73 C72 C71 118.9(4) . . ?
C73 C72 H72 120.6 . . ?
C72 C73 C74 122.0(3) . . ?
C72 C73 C78 117.6(3) . . ?
C74 C73 C78 120.4(3) . . ?
C69 C74 C75 121.1(3) . . ?
C73 C74 C69 119.1(3) . . ?
C73 C74 C75 119.6(3) . . ?
O22 C75 C74 118.9(3) . . ?
O22 C75 C76 120.7(3) . . ?
C76 C75 C74 120.3(3) . . ?
C77 C76 C75 119.8(3) . . ?
C77 C76 C79 118.7(3) . . ?
C79 C76 C75 121.4(3) . . ?
C76 C77 C78 120.5(3) . . ?
C82 C77 C76 121.7(3) . . ?
C82 C77 C78 117.8(3) . . ?
O24 C78 C73 120.6(3) . . ?
O24 C78 C77 121.3(4) . . ?
C77 C78 C73 118.1(3) . . ?
O23 C79 C76 125.9(3) . . ?
O23 C79 C80 117.6(3) . . ?
C80 C79 C76 116.5(3) . . ?
C79 C80 H80 118.5 . . ?
C81 C80 C79 123.0(3) . . ?
C81 C80 H80 118.5 . . ?
C80 C81 H81 120.0 . . ?
C80 C81 C82 119.9(3) . . ?
C82 C81 H81 120.0 . . ?
C77 C82 C81 119.7(3) . . ?
C77 C82 H82 120.1 . . ?
C81 C82 H82 120.1 . . ?
O25 C83 C6 126.0(3) . . ?
O25 C83 C84 117.0(3) . . ?
C84 C83 C6 116.9(4) . . ?
C83 C84 H84 118.7 . . ?
C85 C84 C83 122.7(4) . . ?
C85 C84 H84 118.7 . . ?
C84 C85 H85 119.7 . . ?
C84 C85 C86 120.5(4) . . ?
C86 C85 H85 119.7 . . ?
C85 C86 H86 120.3 . . ?
C87 C86 C85 119.4(4) . . ?
C87 C86 H86 120.3 . . ?
C6 C87 C91 120.8(3) . . ?
C86 C87 C6 121.3(4) . . ?
C86 C87 C91 117.8(4) . . ?
O26 C88 C6 120.5(3) . . ?
O26 C88 C89 118.5(3) . . ?
C6 C88 C89 121.0(3) . . ?
C90 C89 C88 119.5(3) . . ?
C90 C89 C92 119.0(3) . . ?
C92 C89 C88 121.4(3) . . ?
C89 C90 C91 120.8(3) . . ?
C95 C90 C89 121.6(3) . . ?
C95 C90 C91 117.5(3) . . ?
O28 C91 C87 120.8(3) . . ?
O28 C91 C90 121.4(3) . . ?
C87 C91 C90 117.8(3) . . ?
O27 C92 C89 124.3(3) . . ?
O27 C92 C93 118.5(3) . . ?
C93 C92 C89 117.2(3) . . ?
C92 C93 H93 118.8 . . ?
C94 C93 C92 122.5(3) . . ?
C94 C93 H93 118.8 . . ?
C93 C94 H94 120.1 . . ?
C93 C94 C95 119.8(3) . . ?
C95 C94 H94 120.1 . . ?
C90 C95 C94 119.9(3) . . ?
C90 C95 H95 120.0 . . ?
C94 C95 H95 120.0 . . ?
O29 C96 C98 118.1(9) . . ?
O29 C96 C106 126.9(10) . . ?
C106 C96 C98 114.7(9) . . ?
O29 C97 C99 116.2(9) . . ?
O29 C97 C107 124.9(9) . . ?
C99 C97 C107 118.4(9) . . ?
C96 C98 H98 118.0 . . ?
C100 C98 C96 124.1(8) . . ?
C100 C98 H98 118.0 . . ?
C97 C99 H99 119.4 . . ?
C101 C99 C97 121.1(8) . . ?
C101 C99 H99 119.4 . . ?
C98 C100 H100 120.1 . . ?
C98 C100 C102 119.8(7) . . ?
C102 C100 H100 120.1 . . ?
C99 C101 H101 119.7 . . ?
C99 C101 C103 120.6(7) . . ?
C103 C101 H101 119.7 . . ?
C100 C102 H102 120.3 . . ?
C104 C102 C100 119.4(7) . . ?
C104 C102 H102 120.3 . . ?
C101 C103 H103 120.0 . . ?
C105 C103 C101 120.0(7) . . ?
C105 C103 H103 120.0 . . ?
C102 C104 C106 121.3(7) . . ?
C102 C104 C114 117.4(6) . . ?
C106 C104 C114 121.3(6) . . ?
C103 C105 C107 121.9(7) . . ?
C103 C105 C115 117.8(7) . . ?
C107 C105 C115 120.4(7) . . ?
C96 C106 C108 118.9(11) . . ?
C104 C106 C96 120.5(8) . . ?
C104 C106 C108 120.5(10) . . ?
C97 C107 C109 122.7(10) . . ?
C105 C107 C97 117.8(8) . . ?
C105 C107 C109 119.4(10) . . ?
O30 C108 C106 124.2(16) . . ?
O30 C108 C110 116.3(16) . . ?
C106 C108 C110 119.4(15) . . ?
O30 C109 C107 118.2(13) . . ?
O30 C109 C111 119.8(16) . . ?
C111 C109 C107 122.0(14) . . ?
C112 C110 C108 120.1(13) . . ?
C112 C110 C116 117.1(12) . . ?
C116 C110 C108 122.5(15) . . ?
C113 C111 C109 119.3(13) . . ?
C113 C111 C117 119.4(13) . . ?
C117 C111 C109 121.3(14) . . ?
C110 C112 C114 119.8(8) . . ?
C122 C112 C110 122.2(8) . . ?
C122 C112 C114 118.0(7) . . ?
C111 C113 C115 120.7(8) . . ?
C123 C113 C111 122.3(8) . . ?
C123 C113 C115 117.0(7) . . ?
C104 C114 C112 118.1(6) . . ?
O32A C114 C104 121.7(7) . . ?
O32A C114 C112 120.2(7) . . ?
C105 C115 C113 117.8(6) . . ?
O32B C115 C105 122.0(7) . . ?
O32B C115 C113 120.2(7) . . ?
O31 C116 C110 123.3(16) . . ?
O31 C116 C118 117.5(16) . . ?
C118 C116 C110 119.0(15) . . ?
O31 C117 C111 125.1(15) . . ?
O31 C117 C119 118.6(15) . . ?
C119 C117 C111 116.0(14) . . ?
C116 C118 H118 119.0 . . ?
C120 C118 C116 121.9(13) . . ?
C120 C118 H118 119.0 . . ?
C117 C119 H119 118.4 . . ?
C121 C119 C117 123.3(13) . . ?
C121 C119 H119 118.4 . . ?
C118 C120 H120 120.2 . . ?
C118 C120 C122 119.7(8) . . ?
C122 C120 H120 120.2 . . ?
C119 C121 H121 120.1 . . ?
C119 C121 C123 119.8(8) . . ?
C123 C121 H121 120.1 . . ?
C112 C122 C120 119.9(7) . . ?
C112 C122 H122 120.0 . . ?
C120 C122 H122 120.0 . . ?
C113 C123 C121 118.7(7) . . ?
C113 C123 H123 120.6 . . ?
C121 C123 H123 120.6 . . ?
O33 C125 C127 117.3(9) . . ?
O33 C125 C135 126.5(9) . . ?
C135 C125 C127 116.0(9) . . ?
C4 C126 H126 118.6 . . ?
C128 C126 C4 122.7(16) . . ?
C128 C126 H126 118.6 . . ?
C125 C127 H127 118.7 . . ?
C129 C127 C125 122.6(7) . . ?
C129 C127 H127 118.7 . . ?
C126 C128 H128 120.0 . . ?
C126 C128 C130 120.1(12) . . ?
C130 C128 H128 120.0 . . ?
C127 C129 H129 119.9 . . ?
C127 C129 C131 120.2(6) . . ?
C131 C129 H129 119.9 . . ?
C128 C130 H130 120.5 . . ?
C132 C130 C128 119.0(11) . . ?
C132 C130 H130 120.5 . . ?
C129 C131 H131 120.2 . . ?
C133 C131 C129 119.5(6) . . ?
C133 C131 H131 120.2 . . ?
C130 C132 C134 121.1(13) . . ?
C130 C132 C142 116.9(11) . . ?
C134 C132 C142 122.0(12) . . ?
C131 C133 C135 121.6(6) . . ?
C131 C133 C143 117.4(5) . . ?
C135 C133 C143 121.0(6) . . ?
C4 C134 C136 122(2) . . ?
C132 C134 C4 119.3(18) . . ?
C132 C134 C136 118.2(18) . . ?
C125 C135 C133 119.8(8) . . ?
C125 C135 C137 120.4(9) . . ?
C133 C135 C137 119.7(8) . . ?
O34 C136 C134 119(2) . . ?
O34 C136 C138 118.8(19) . . ?
C134 C136 C138 122(2) . . ?
O34 C137 C135 121.7(10) . . ?
O34 C137 C139 117.9(9) . . ?
C135 C137 C139 120.4(10) . . ?
C140 C138 C136 118.7(17) . . ?
C140 C138 C144 118.4(16) . . ?
C144 C138 C136 122.6(18) . . ?
C141 C139 C137 120.3(8) . . ?
C145 C139 C137 121.4(8) . . ?
C145 C139 C141 118.1(7) . . ?
C138 C140 C142 120.9(12) . . ?
C138 C140 C150 121.7(12) . . ?
C150 C140 C142 117.4(10) . . ?
C139 C141 C143 119.8(6) . . ?
C151 C141 C139 122.2(6) . . ?
C151 C141 C143 118.0(5) . . ?
C132 C142 C140 118.1(10) . . ?
O36A C142 C132 120.9(11) . . ?
O36A C142 C140 120.8(11) . . ?
C133 C143 C141 117.8(5) . . ?
O36B C143 C133 121.7(5) . . ?
O36B C143 C141 120.4(5) . . ?
O35 C144 C138 120.1(15) . . ?
C146 C144 O35 119.4(17) . . ?
C146 C144 C138 119.6(18) . . ?
O35 C145 C139 125.7(8) . . ?
O35 C145 C147 116.7(8) . . ?
C139 C145 C147 117.4(8) . . ?
C144 C146 H146 119.2 . . ?
C144 C146 C148 121.5(18) . . ?
C148 C146 H146 119.2 . . ?
C145 C147 H147 118.8 . . ?
C149 C147 C145 122.5(8) . . ?
C149 C147 H147 118.8 . . ?
C146 C148 H148 120.2 . . ?
C146 C148 C150 119.5(14) . . ?
C150 C148 H148 120.2 . . ?
C147 C149 H149 119.8 . . ?
C147 C149 C151 120.3(7) . . ?
C151 C149 H149 119.8 . . ?
C140 C150 C148 119.3(11) . . ?
C140 C150 H150 120.4 . . ?
C148 C150 H150 120.4 . . ?
C141 C151 C149 119.4(6) . . ?
C141 C151 H151 120.3 . . ?
C149 C151 H151 120.3 . . ?
O37 C152 N5 123.3(4) . . ?
O37 C152 H152 118.4 . . ?
N5 C152 H152 118.4 . . ?
N5 C153 H15A 109.5 . . ?
N5 C153 H15B 109.5 . . ?
N5 C153 H15C 109.5 . . ?
H15A C153 H15B 109.5 . . ?
H15A C153 H15C 109.5 . . ?
H15B C153 H15C 109.5 . . ?
N5 C154 H15D 109.5 . . ?
N5 C154 H15E 109.5 . . ?
N5 C154 H15F 109.5 . . ?
H15D C154 H15E 109.5 . . ?
H15D C154 H15F 109.5 . . ?
H15E C154 H15F 109.5 . . ?
O38 C155 N6 124.6(4) . . ?
O38 C155 H155 117.7 . . ?
N6 C155 H155 117.7 . . ?
N6 C156 H15G 109.5 . . ?
N6 C156 H15H 109.5 . . ?
N6 C156 H15I 109.5 . . ?
H15G C156 H15H 109.5 . . ?
H15G C156 H15I 109.5 . . ?
H15H C156 H15I 109.5 . . ?
N6 C157 H15J 109.5 . . ?
N6 C157 H15K 109.5 . . ?
N6 C157 H15L 109.5 . . ?
H15J C157 H15K 109.5 . . ?
H15J C157 H15L 109.5 . . ?
H15K C157 H15L 109.5 . . ?
O39 C158 N7 124.2(4) . . ?
O39 C158 H158 117.9 . . ?
N7 C158 H158 117.9 . . ?
N7 C159 H15M 109.5 . . ?
N7 C159 H15N 109.5 . . ?
N7 C159 H15O 109.5 . . ?
H15M C159 H15N 109.5 . . ?
H15M C159 H15O 109.5 . . ?
H15N C159 H15O 109.5 . . ?
N7 C160 H16A 109.5 . . ?
N7 C160 H16B 109.5 . . ?
N7 C160 H16C 109.5 . . ?
H16A C160 H16B 109.5 . . ?
H16A C160 H16C 109.5 . . ?
H16B C160 H16C 109.5 . . ?
O40 C161 H161 116.0 . . ?
O40 C161 N8A 128.0(8) . . ?
N8A C161 H161 116.0 . . ?
O40 C162 H162 117.9 . . ?
O40 C162 N8B 124.1(7) . . ?
N8B C162 H162 117.9 . . ?
H16D C163 H16E 109.5 . . ?
H16D C163 H16F 109.5 . . ?
H16E C163 H16F 109.5 . . ?
N8A C163 H16D 109.5 . . ?
N8A C163 H16E 109.5 . . ?
N8A C163 H16F 109.5 . . ?
H16G C164 H16H 109.5 . . ?
H16G C164 H16I 109.5 . . ?
H16H C164 H16I 109.5 . . ?
N8B C164 H16G 109.5 . . ?
N8B C164 H16H 109.5 . . ?
N8B C164 H16I 109.5 . . ?
H16J C165 H16K 109.5 . . ?
H16J C165 H16L 109.5 . . ?
H16K C165 H16L 109.5 . . ?
N8A C165 H16J 109.5 . . ?
N8A C165 H16K 109.5 . . ?
N8A C165 H16L 109.5 . . ?
H16M C166 H16N 109.5 . . ?
H16M C166 H16O 109.5 . . ?
H16N C166 H16O 109.5 . . ?
N8B C166 H16M 109.5 . . ?
N8B C166 H16N 109.5 . . ?
N8B C166 H16O 109.5 . . ?
O41 C167 N9 127.0(11) . . ?
O41 C167 H167 116.5 . . ?
N9 C167 H167 116.5 . . ?
N9 C168 H16P 109.5 . . ?
N9 C168 H16Q 109.5 . . ?
N9 C168 H16R 109.5 . . ?
H16P C168 H16Q 109.5 . . ?
H16P C168 H16R 109.5 . . ?
H16Q C168 H16R 109.5 . . ?
N9 C169 H16S 109.5 . . ?
N9 C169 H16T 109.5 . . ?
N9 C169 H16U 109.5 . . ?
H16S C169 H16T 109.5 . . ?
H16S C169 H16U 109.5 . . ?
H16T C169 H16U 109.5 . . ?
O42 C170 N10 148.2(19) . . ?
O42 C170 H170 105.9 . . ?
N10 C170 H170 105.9 . . ?
N10 C171 H17A 109.5 . . ?
N10 C171 H17B 109.5 . . ?
N10 C171 H17C 109.5 . . ?
H17A C171 H17B 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
N10 C172 H17D 109.5 . . ?
N10 C172 H17E 109.5 . . ?
N10 C172 H17F 109.5 . . ?
H17D C172 H17E 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
O43 C173 N11 126.4(6) . . ?
O43 C173 H173 116.8 . . ?
N11 C173 H173 116.8 . . ?
N11 C174 H17G 109.5 . . ?
N11 C174 H17H 109.5 . . ?
N11 C174 H17I 109.5 . . ?
H17G C174 H17H 109.5 . . ?
H17G C174 H17I 109.5 . . ?
H17H C174 H17I 109.5 . . ?
N11 C175 H17J 109.5 . . ?
N11 C175 H17K 109.5 . . ?
N11 C175 H17L 109.5 . . ?
H17J C175 H17K 109.5 . . ?
H17J C175 H17L 109.5 . . ?
H17K C175 H17L 109.5 . . ?
C161 N8A C163 122.0(7) . . ?
C161 N8A C165 121.5(7) . . ?
C165 N8A C163 116.4(7) . . ?
C11 C1A H1A 118.4 . . ?
C1Q C1A C11 123.2(3) . . ?
C1Q C1A H1A 118.4 . . ?
C39 C40A H40A 119.8 . . ?
C41A C40A C39 120.3(15) . . ?
C41A C40A H40A 119.8 . . ?
C40A C41A H41A 119.9 . . ?
C40A C41A C42A 120.2(14) . . ?
C42A C41A H41A 119.9 . . ?
C37 C42A C41A 120.2(13) . . ?
C37 C42A H42A 119.9 . . ?
C41A C42A H42A 119.9 . . ?
C53 C54A H54A 119.3 . . ?
C55A C54A C53 121.5(6) . . ?
C55A C54A H54A 119.3 . . ?
C54A C55A H55A 119.7 . . ?
C54A C55A C56A 120.6(6) . . ?
C56A C55A H55A 119.7 . . ?
C51 C56A C55A 119.5(6) . . ?
C51 C56A H56A 120.2 . . ?
C55A C56A H56A 120.2 . . ?
C162 N8B C164 118.7(8) . . ?
C162 N8B C166 122.5(6) . . ?
C164 N8B C166 118.7(8) . . ?
C39 C40B H40B 118.0 . . ?
C41B C40B C39 123.9(15) . . ?
C41B C40B H40B 118.0 . . ?
C40B C41B H41B 120.1 . . ?
C40B C41B C42B 119.9(13) . . ?
C42B C41B H41B 120.1 . . ?
C37 C42B H42B 121.0 . . ?
C41B C42B C37 118.0(11) . . ?
C41B C42B H42B 121.0 . . ?
C53 C54B H54B 118.7 . . ?
C55B C54B C53 122.7(7) . . ?
C55B C54B H54B 118.7 . . ?
C54B C55B H55B 120.4 . . ?
C54B C55B C56B 119.3(7) . . ?
C56B C55B H55B 120.4 . . ?
C51 C56B H56B 120.1 . . ?
C55B C56B C51 119.8(6) . . ?
C55B C56B H56B 120.1 . . ?
C13 C1G C29 122.7(3) . . ?
C13 C1G H1G 118.7 . . ?
C29 C1G H1G 118.7 . . ?
C7 C1I C15 120.7(3) . . ?
C10 C1I C7 121.5(3) . . ?
C10 C1I C15 117.8(3) . . ?
C1Q C1N H1N 120.1 . . ?
C1S C1N H1N 120.1 . . ?
C1S C1N C1Q 119.8(3) . . ?
O19 C1O N3 124.6(3) . . ?
O19 C1O H1O 117.7 . . ?
N3 C1O H1O 117.7 . . ?
O5 C1P C20 124.4(3) . . ?
O5 C1P C1V 118.0(3) . . ?
C1V C1P C20 117.6(3) . . ?
C1A C1Q C1N 119.8(3) . . ?
C1A C1Q H1Q 120.1 . . ?
C1N C1Q H1Q 120.1 . . ?
C1N C1S C15 117.2(3) . . ?
C1N C1S C1X 121.9(3) . . ?
C1X C1S C15 120.9(3) . . ?
C18 C1T H1T 120.1 . . ?
C1V C1T C18 119.8(3) . . ?
C1V C1T H1T 120.1 . . ?
O2 C1U C7 117.9(3) . . ?
O2 C1U C1X 121.0(3) . . ?
C1X C1U C7 121.1(3) . . ?
C1P C1V H1V 118.6 . . ?
C1T C1V C1P 122.8(3) . . ?
C1T C1V H1V 118.6 . . ?
O6 C1W C20 118.6(3) . . ?
O6 C1W C22 119.9(3) . . ?
C22 C1W C20 121.4(3) . . ?
C11 C1X C1U 122.0(3) . . ?
C1S C1X C11 118.4(3) . . ?
C1S C1X C1U 119.6(3) . . ?
C18 C1Y C20 121.8(3) . . ?
C18 C1Y C24 117.2(3) . . ?
C20 C1Y C24 120.9(3) . . ?

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 O5 C1P C20 -35.5(4) . . . . ?
Co1 O5 C1P C1V 145.2(3) . . . . ?
Co1 O6 C1W C20 41.0(4) . . . . ?
Co1 O6 C1W C22 -139.8(2) . . . . ?
Co1 O11 C39 C36 -98.5(4) . . . . ?
Co1 O11 C39 C40A 72.4(6) . . . . ?
Co1 O11 C39 C40B 93.0(6) . . . . ?
Co1 O14 C49 C48 163.8(2) . . . . ?
Co1 O14 C49 C50 -16.4(5) . . . . ?
Co1 O15 C53 C50 16.6(8) . . . . ?
Co1 O15 C53 C54A 177.8(5) . . . . ?
Co1 O15 C53 C54B -143.4(5) . . . . ?
Co1 O19 C1O N3 -162.8(3) . . . . ?
Co2 O3 C1 C2 -80.2(3) . . . . ?
Co2 O3 C1 C7 100.9(3) . . . . ?
Co2 O6 C1W C20 -161.1(2) . . . . ?
Co2 O6 C1W C22 18.1(4) . . . . ?
Co2 O7 C25 C22 -25.4(5) . . . . ?
Co2 O7 C25 C26 153.4(3) . . . . ?
Co2 O10 C35 C34 137.1(2) . . . . ?
Co2 O10 C35 C36 -43.4(4) . . . . ?
Co2 O11 C39 C36 34.3(5) . . . . ?
Co2 O11 C39 C40A -154.9(6) . . . . ?
Co2 O11 C39 C40B -134.3(6) . . . . ?
Co2 O20 C66 N4 156.6(4) . . . . ?
Co3 O2 C1U C7 43.5(4) . . . . ?
Co3 O2 C1U C1X -137.6(2) . . . . ?
Co3 O3 C1 C2 145.4(2) . . . . ?
Co3 O3 C1 C7 -33.5(4) . . . . ?
Co3 O9 C29 C34 19.4(6) . . . . ?
Co3 O9 C29 C1G -159.8(3) . . . . ?
Co3 O10 C35 C34 -15.8(4) . . . . ?
Co3 O10 C35 C36 163.7(2) . . . . ?
Co3 O13 C43 C44 80.1(3) . . . . ?
Co3 O13 C43 C48 -100.3(3) . . . . ?
Co3 O18 C60 N2 -158.8(3) . . . . ?
Co4 O1 C11 C1A 163.3(2) . . . . ?
Co4 O1 C11 C1X -16.1(5) . . . . ?
Co4 O2 C1U C7 -165.0(2) . . . . ?
Co4 O2 C1U C1X 13.9(4) . . . . ?
Co4 O5 C1P C20 97.4(3) . . . . ?
Co4 O5 C1P C1V -81.9(3) . . . . ?
Co4 O13 C43 C44 -147.1(2) . . . . ?
Co4 O13 C43 C48 32.6(4) . . . . ?
Co4 O14 C49 C48 -43.5(4) . . . . ?
Co4 O14 C49 C50 136.3(3) . . . . ?
Co4 O17 C57 N1 164.3(3) . . . . ?
Co5 O21 C69 C70 151.0(3) . . . . ?
Co5 O21 C69 C74 -29.1(4) . . . . ?
Co5 O22 C75 C74 47.3(4) . . . . ?
Co5 O22 C75 C76 -131.9(3) . . . . ?
Co5 O29 C96 C98 -175.4(5) . . . . ?
Co5 O29 C96 C106 -2.7(12) . . . . ?
Co5 O29 C97 C99 -155.6(6) . . . . ?
Co5 O29 C97 C107 32.9(12) . . . . ?
Co5 O30 C108 C106 -8.1(15) . . . . ?
Co5 O30 C108 C110 167.8(6) . . . . ?
Co5 O30 C109 C107 -24.7(15) . . . . ?
Co5 O30 C109 C111 157.5(8) . . . . ?
Co5 O35 C144 C138 -108.8(12) . . . . ?
Co5 O35 C144 C146 82.0(13) . . . . ?
Co5 O35 C145 C139 -98.3(5) . . . . ?
Co5 O35 C145 C147 76.8(7) . . . . ?
Co5 O40 C161 N8A -149.6(8) . . . . ?
Co5 O40 C162 N8B -152.6(5) . . . . ?
Co6 O22 C75 C74 -160.7(2) . . . . ?
Co6 O22 C75 C76 20.1(4) . . . . ?
Co6 O23 C79 C76 -12.3(5) . . . . ?
Co6 O23 C79 C80 168.4(3) . . . . ?
Co6 O27 C92 C89 101.5(3) . . . . ?
Co6 O27 C92 C93 -79.9(3) . . . . ?
Co6 O34 C136 C134 137.0(12) . . . . ?
Co6 O34 C136 C138 -35.3(17) . . . . ?
Co6 O34 C137 C135 132.9(5) . . . . ?
Co6 O34 C137 C139 -48.9(6) . . . . ?
Co6 O35 C144 C138 16.4(18) . . . . ?
Co6 O35 C144 C146 -152.8(9) . . . . ?
Co6 O35 C145 C139 36.8(7) . . . . ?
Co6 O35 C145 C147 -148.1(4) . . . . ?
Co6 O37 C152 N5 156.9(3) . . . . ?
Co7 O26 C88 C6 -131.4(3) . . . . ?
Co7 O26 C88 C89 47.2(4) . . . . ?
Co7 O27 C92 C89 -31.4(4) . . . . ?
Co7 O27 C92 C93 147.2(2) . . . . ?
Co7 O31 C116 C110 -102.8(14) . . . . ?
Co7 O31 C116 C118 82.3(15) . . . . ?
Co7 O31 C117 C111 -97.7(14) . . . . ?
Co7 O31 C117 C119 76.7(14) . . . . ?
Co7 O33 C4 C126 -161.3(9) . . . . ?
Co7 O33 C4 C134 25.9(18) . . . . ?
Co7 O33 C125 C127 -173.3(4) . . . . ?
Co7 O33 C125 C135 1.5(8) . . . . ?
Co7 O34 C136 C134 -33.2(17) . . . . ?
Co7 O34 C136 C138 154.6(9) . . . . ?
Co7 O34 C137 C135 -14.4(7) . . . . ?
Co7 O34 C137 C139 163.8(4) . . . . ?
Co7 O38 C155 N6 -154.5(3) . . . . ?
Co8 O21 C69 C70 -80.1(3) . . . . ?
Co8 O21 C69 C74 99.8(3) . . . . ?
Co8 O25 C83 C6 -9.9(6) . . . . ?
Co8 O25 C83 C84 169.2(3) . . . . ?
Co8 O26 C88 C6 19.1(4) . . . . ?
Co8 O26 C88 C89 -162.3(2) . . . . ?
Co8 O30 C108 C106 131.8(11) . . . . ?
Co8 O30 C108 C110 -52.3(10) . . . . ?
Co8 O30 C109 C107 139.2(9) . . . . ?
Co8 O30 C109 C111 -38.6(14) . . . . ?
Co8 O31 C116 C110 31.7(17) . . . . ?
Co8 O31 C116 C118 -143.1(10) . . . . ?
Co8 O31 C117 C111 30.6(18) . . . . ?
Co8 O31 C117 C119 -155.1(9) . . . . ?
Co8 O39 C158 N7 147.5(3) . . . . ?
O1 C11 C1A C1Q -177.2(4) . . . . ?
O1 C11 C1X C1S 179.0(3) . . . . ?
O1 C11 C1X C1U -1.4(5) . . . . ?
O2 C1U C1X C11 2.2(5) . . . . ?
O2 C1U C1X C1S -178.2(3) . . . . ?
O3 C1 C2 C3 -176.6(3) . . . . ?
O3 C1 C7 C1I 175.9(3) . . . . ?
O3 C1 C7 C1U -6.9(5) . . . . ?
O4 C15 C1I C7 174.6(4) . . . . ?
O4 C15 C1I C10 -6.9(5) . . . . ?
O4 C15 C1S C1N 4.2(6) . . . . ?
O4 C15 C1S C1X -174.8(4) . . . . ?
O5 C1P C1V C1T 179.9(3) . . . . ?
O7 C25 C26 C27 -175.7(4) . . . . ?
O8 C24 C1Y C18 -1.2(5) . . . . ?
O8 C24 C1Y C20 -179.8(3) . . . . ?
O9 C29 C34 C33 -177.3(3) . . . . ?
O9 C29 C34 C35 2.5(6) . . . . ?
O9 C29 C1G C13 174.9(5) . . . . ?
O10 C35 C36 C37 -175.7(3) . . . . ?
O10 C35 C36 C39 1.6(5) . . . . ?
O11 C39 C40A C41A -177.0(8) . . . . ?
O11 C39 C40B C41B 177.1(9) . . . . ?
O13 C43 C44 C45 178.7(3) . . . . ?
O13 C43 C48 C47 -177.8(3) . . . . ?
O13 C43 C48 C49 5.7(5) . . . . ?
O14 C49 C50 C51 178.2(4) . . . . ?
O14 C49 C50 C53 -4.2(6) . . . . ?
O15 C53 C54A C55A 178.7(8) . . . . ?
O15 C53 C54B C55B 173.9(8) . . . . ?
O21 C69 C70 C71 177.6(4) . . . . ?
O21 C69 C74 C73 -179.8(3) . . . . ?
O21 C69 C74 C75 -4.3(5) . . . . ?
O22 C75 C76 C77 -177.4(3) . . . . ?
O22 C75 C76 C79 6.9(5) . . . . ?
O23 C79 C80 C81 -173.0(4) . . . . ?
O25 C83 C84 C85 -175.7(4) . . . . ?
O26 C88 C89 C90 173.7(3) . . . . ?
O26 C88 C89 C92 -3.2(5) . . . . ?
O27 C92 C93 C94 -179.0(3) . . . . ?
O29 C96 C98 C100 166.8(8) . . . . ?
O29 C96 C106 C104 -167.8(8) . . . . ?
O29 C96 C106 C108 15.5(14) . . . . ?
O29 C97 C99 C101 -175.2(8) . . . . ?
O29 C97 C107 C105 173.4(8) . . . . ?
O29 C97 C107 C109 -4.3(15) . . . . ?
O30 C108 C110 C112 -169.3(9) . . . . ?
O30 C108 C110 C116 4.9(16) . . . . ?
O30 C109 C111 C113 -177.6(9) . . . . ?
O30 C109 C111 C117 0.7(18) . . . . ?
O31 C116 C118 C120 -179.9(10) . . . . ?
O31 C117 C119 C121 -178.7(10) . . . . ?
O33 C4 C126 C128 -177.4(12) . . . . ?
O33 C4 C134 C132 177.2(12) . . . . ?
O33 C4 C134 C136 0(2) . . . . ?
O33 C125 C127 C129 170.8(6) . . . . ?
O33 C125 C135 C133 -169.1(5) . . . . ?
O33 C125 C135 C137 14.9(9) . . . . ?
O34 C136 C138 C140 179.3(12) . . . . ?
O34 C136 C138 C144 -7(2) . . . . ?
O34 C137 C139 C141 -169.7(5) . . . . ?
O34 C137 C139 C145 5.8(8) . . . . ?
O35 C144 C146 C148 170.5(13) . . . . ?
O35 C145 C147 C149 -176.6(6) . . . . ?
O40 C161 N8A C163 -0.4(16) . . . . ?
O40 C161 N8A C165 175.2(9) . . . . ?
O40 C162 N8B C164 -0.3(12) . . . . ?
O40 C162 N8B C166 -175.4(6) . . . . ?
C1 C2 C3 C10 0.1(6) . . . . ?
C1 C7 C1I C10 1.2(5) . . . . ?
C1 C7 C1I C15 179.6(3) . . . . ?
C1 C7 C1U O2 0.9(4) . . . . ?
C1 C7 C1U C1X -178.0(3) . . . . ?
C2 C1 C7 C1I -3.0(5) . . . . ?
C2 C1 C7 C1U 174.2(3) . . . . ?
C2 C3 C10 C1I -2.0(6) . . . . ?
C3 C10 C1I C7 1.3(6) . . . . ?
C3 C10 C1I C15 -177.1(3) . . . . ?
C4 C126 C128 C130 0(2) . . . . ?
C4 C134 C136 O34 4(2) . . . . ?
C4 C134 C136 C138 176.1(13) . . . . ?
C6 C83 C84 C85 3.5(6) . . . . ?
C6 C87 C91 O28 171.3(4) . . . . ?
C6 C87 C91 C90 -10.1(5) . . . . ?
C6 C88 C89 C90 -7.7(5) . . . . ?
C6 C88 C89 C92 175.5(3) . . . . ?
C7 C1 C2 C3 2.4(5) . . . . ?
C7 C1U C1X C11 -178.9(3) . . . . ?
C7 C1U C1X C1S 0.7(4) . . . . ?
C11 C1A C1Q C1N -2.2(6) . . . . ?
C13 C32 C33 C34 -2.9(6) . . . . ?
C13 C32 C33 C38 175.8(4) . . . . ?
C14 C23 C24 O8 1.4(6) . . . . ?
C14 C23 C24 C1Y -178.4(3) . . . . ?
C15 C1S C1X C11 177.5(3) . . . . ?
C15 C1S C1X C1U -2.1(5) . . . . ?
C18 C1T C1V C1P -0.6(6) . . . . ?
C20 C1P C1V C1T 0.6(5) . . . . ?
C22 C23 C24 O8 -178.2(4) . . . . ?
C22 C23 C24 C1Y 1.9(5) . . . . ?
C22 C25 C26 C27 3.2(5) . . . . ?
C23 C14 C27 C26 -0.4(6) . . . . ?
C23 C22 C25 O7 177.8(3) . . . . ?
C23 C22 C25 C26 -0.9(5) . . . . ?
C23 C22 C1W O6 -174.4(3) . . . . ?
C23 C22 C1W C20 4.8(5) . . . . ?
C23 C24 C1Y C18 178.6(3) . . . . ?
C23 C24 C1Y C20 0.0(5) . . . . ?
C25 C22 C23 C14 -1.9(5) . . . . ?
C25 C22 C23 C24 177.8(3) . . . . ?
C25 C22 C1W O6 3.5(5) . . . . ?
C25 C22 C1W C20 -177.3(3) . . . . ?
C25 C26 C27 C14 -2.5(6) . . . . ?
C27 C14 C23 C22 2.6(6) . . . . ?
C27 C14 C23 C24 -177.0(4) . . . . ?
C29 C34 C35 O10 -4.0(5) . . . . ?
C29 C34 C35 C36 176.5(3) . . . . ?
C32 C13 C1G C29 3.3(8) . . . . ?
C32 C33 C34 C29 1.6(5) . . . . ?
C32 C33 C34 C35 -178.2(3) . . . . ?
C32 C33 C38 O12 -3.1(6) . . . . ?
C32 C33 C38 C37 178.6(4) . . . . ?
C33 C34 C35 O10 175.8(3) . . . . ?
C33 C34 C35 C36 -3.7(5) . . . . ?
C34 C29 C1G C13 -4.4(7) . . . . ?
C34 C33 C38 O12 175.6(4) . . . . ?
C34 C33 C38 C37 -2.6(5) . . . . ?
C34 C35 C36 C37 3.8(5) . . . . ?
C34 C35 C36 C39 -178.9(3) . . . . ?
C35 C36 C37 C38 -3.4(6) . . . . ?
C35 C36 C37 C42A 162.8(7) . . . . ?
C35 C36 C37 C42B -170.8(7) . . . . ?
C35 C36 C39 O11 3.4(6) . . . . ?
C35 C36 C39 C40A -167.2(6) . . . . ?
C35 C36 C39 C40B 172.1(6) . . . . ?
C36 C37 C38 O12 -175.5(4) . . . . ?
C36 C37 C38 C33 2.8(6) . . . . ?
C36 C37 C42A C41A 14.3(13) . . . . ?
C36 C37 C42B C41B -9.0(14) . . . . ?
C36 C39 C40A C41A -5.6(13) . . . . ?
C36 C39 C40B C41B 7.7(14) . . . . ?
C37 C36 C39 O11 -179.3(4) . . . . ?
C37 C36 C39 C40A 10.1(7) . . . . ?
C37 C36 C39 C40B -10.6(8) . . . . ?
C38 C33 C34 C29 -177.1(3) . . . . ?
C38 C33 C34 C35 3.1(5) . . . . ?
C38 C37 C42A C41A -179.0(8) . . . . ?
C38 C37 C42B C41B -177.0(9) . . . . ?
C39 C36 C37 C38 179.2(4) . . . . ?
C39 C36 C37 C42A -14.6(8) . . . . ?
C39 C36 C37 C42B 11.8(8) . . . . ?
C39 C40A C41A C42A 5.2(16) . . . . ?
C39 C40B C41B C42B -5.2(18) . . . . ?
C43 C44 C45 C46 -0.8(6) . . . . ?
C43 C48 C49 O14 0.4(5) . . . . ?
C43 C48 C49 C50 -179.4(3) . . . . ?
C44 C43 C48 C47 1.8(5) . . . . ?
C44 C43 C48 C49 -174.6(3) . . . . ?
C44 C45 C46 C47 1.7(6) . . . . ?
C45 C46 C47 C48 -0.8(5) . . . . ?
C45 C46 C47 C52 177.9(3) . . . . ?
C46 C47 C48 C43 -1.0(5) . . . . ?
C46 C47 C48 C49 175.6(3) . . . . ?
C46 C47 C52 O16 2.3(5) . . . . ?
C46 C47 C52 C51 -178.8(4) . . . . ?
C47 C48 C49 O14 -175.9(3) . . . . ?
C47 C48 C49 C50 4.2(5) . . . . ?
C48 C43 C44 C45 -1.0(5) . . . . ?
C48 C47 C52 O16 -178.9(3) . . . . ?
C48 C47 C52 C51 0.0(5) . . . . ?
C48 C49 C50 C51 -2.0(6) . . . . ?
C48 C49 C50 C53 175.6(4) . . . . ?
C49 C50 C51 C52 -1.3(7) . . . . ?
C49 C50 C51 C56A 159.3(6) . . . . ?
C49 C50 C51 C56B -162.2(5) . . . . ?
C49 C50 C53 O15 4.4(8) . . . . ?
C49 C50 C53 C54A -156.9(6) . . . . ?
C49 C50 C53 C54B 164.2(5) . . . . ?
C50 C51 C52 O16 -178.8(4) . . . . ?
C50 C51 C52 C47 2.3(7) . . . . ?
C50 C51 C56A C55A 11.4(13) . . . . ?
C50 C51 C56B C55B -14.1(11) . . . . ?
C50 C53 C54A C55A -17.7(12) . . . . ?
C50 C53 C54B C55B 11.5(11) . . . . ?
C51 C50 C53 O15 -178.0(5) . . . . ?
C51 C50 C53 C54A 20.7(8) . . . . ?
C51 C50 C53 C54B -18.2(8) . . . . ?
C52 C47 C48 C43 -179.7(3) . . . . ?
C52 C47 C48 C49 -3.2(5) . . . . ?
C52 C51 C56A C55A 173.2(8) . . . . ?
C52 C51 C56B C55B -176.1(7) . . . . ?
C53 C50 C51 C52 -179.0(5) . . . . ?
C53 C50 C51 C56A -18.4(9) . . . . ?
C53 C50 C51 C56B 20.2(8) . . . . ?
C53 C54A C55A C56A 11.7(15) . . . . ?
C53 C54B C55B C56B -5.9(15) . . . . ?
C58 N1 C57 O17 0.6(6) . . . . ?
C59 N1 C57 O17 177.3(4) . . . . ?
C61 N2 C60 O18 -6.0(6) . . . . ?
C62 N2 C60 O18 -178.0(3) . . . . ?
C64 N3 C1O O19 -2.3(6) . . . . ?
C65 N3 C1O O19 -179.5(3) . . . . ?
C67 N4 C66 O20 -5.3(9) . . . . ?
C68 N4 C66 O20 177.5(5) . . . . ?
C69 C70 C71 C72 1.8(6) . . . . ?
C69 C74 C75 O22 -5.7(5) . . . . ?
C69 C74 C75 C76 173.6(3) . . . . ?
C70 C69 C74 C73 0.1(5) . . . . ?
C70 C69 C74 C75 175.6(3) . . . . ?
C70 C71 C72 C73 1.1(6) . . . . ?
C71 C72 C73 C74 -3.3(6) . . . . ?
C71 C72 C73 C78 175.4(4) . . . . ?
C72 C73 C74 C69 2.8(5) . . . . ?
C72 C73 C74 C75 -172.9(3) . . . . ?
C72 C73 C78 O24 0.3(6) . . . . ?
C72 C73 C78 C77 -177.6(4) . . . . ?
C73 C74 C75 O22 169.9(3) . . . . ?
C73 C74 C75 C76 -10.9(5) . . . . ?
C74 C69 C70 C71 -2.3(5) . . . . ?
C74 C73 C78 O24 179.0(4) . . . . ?
C74 C73 C78 C77 1.1(5) . . . . ?
C74 C75 C76 C77 3.4(5) . . . . ?
C74 C75 C76 C79 -172.3(3) . . . . ?
C75 C76 C77 C78 6.4(5) . . . . ?
C75 C76 C77 C82 -172.9(3) . . . . ?
C75 C76 C79 O23 -11.3(6) . . . . ?
C75 C76 C79 C80 168.0(3) . . . . ?
C76 C77 C78 O24 173.4(4) . . . . ?
C76 C77 C78 C73 -8.7(5) . . . . ?
C76 C77 C82 C81 2.6(6) . . . . ?
C76 C79 C80 C81 7.6(6) . . . . ?
C77 C76 C79 O23 173.0(3) . . . . ?
C77 C76 C79 C80 -7.7(5) . . . . ?
C78 C73 C74 C69 -175.9(3) . . . . ?
C78 C73 C74 C75 8.5(5) . . . . ?
C78 C77 C82 C81 -176.7(4) . . . . ?
C79 C76 C77 C78 -177.8(3) . . . . ?
C79 C76 C77 C82 2.9(5) . . . . ?
C79 C80 C81 C82 -2.3(7) . . . . ?
C80 C81 C82 C77 -3.0(7) . . . . ?
C82 C77 C78 O24 -7.3(6) . . . . ?
C82 C77 C78 C73 170.6(4) . . . . ?
C83 C6 C87 C86 3.2(5) . . . . ?
C83 C6 C87 C91 -176.5(3) . . . . ?
C83 C6 C88 O26 4.2(5) . . . . ?
C83 C6 C88 C89 -174.4(3) . . . . ?
C83 C84 C85 C86 -0.5(7) . . . . ?
C84 C85 C86 C87 -1.3(7) . . . . ?
C85 C86 C87 C6 -0.2(6) . . . . ?
C85 C86 C87 C91 179.6(4) . . . . ?
C86 C87 C91 O28 -8.5(6) . . . . ?
C86 C87 C91 C90 170.1(3) . . . . ?
C87 C6 C83 O25 174.4(3) . . . . ?
C87 C6 C83 C84 -4.7(5) . . . . ?
C87 C6 C88 O26 -179.5(3) . . . . ?
C87 C6 C88 C89 1.9(5) . . . . ?
C88 C6 C83 O25 -9.3(6) . . . . ?
C88 C6 C83 C84 171.6(3) . . . . ?
C88 C6 C87 C86 -173.2(3) . . . . ?
C88 C6 C87 C91 7.1(5) . . . . ?
C88 C89 C90 C91 4.4(5) . . . . ?
C88 C89 C90 C95 -175.5(3) . . . . ?
C88 C89 C92 O27 -5.4(5) . . . . ?
C88 C89 C92 C93 176.0(3) . . . . ?
C89 C90 C91 O28 -177.2(4) . . . . ?
C89 C90 C91 C87 4.2(5) . . . . ?
C89 C90 C95 C94 -0.7(5) . . . . ?
C89 C92 C93 C94 -0.3(5) . . . . ?
C90 C89 C92 O27 177.7(3) . . . . ?
C90 C89 C92 C93 -0.9(5) . . . . ?
C91 C90 C95 C94 179.4(3) . . . . ?
C92 C89 C90 C91 -178.7(3) . . . . ?
C92 C89 C90 C95 1.4(5) . . . . ?
C92 C93 C94 C95 1.1(6) . . . . ?
C93 C94 C95 C90 -0.6(6) . . . . ?
C95 C90 C91 O28 2.7(5) . . . . ?
C95 C90 C91 C87 -175.9(3) . . . . ?
C96 C98 C100 C102 4.5(15) . . . . ?
C96 C106 C108 O30 -9.5(16) . . . . ?
C96 C106 C108 C110 174.7(8) . . . . ?
C97 C99 C101 C103 0.5(15) . . . . ?
C97 C107 C109 O30 0.3(16) . . . . ?
C97 C107 C109 C111 178.0(10) . . . . ?
C98 C96 C106 C104 5.1(12) . . . . ?
C98 C96 C106 C108 -171.5(9) . . . . ?
C98 C100 C102 C104 -0.3(14) . . . . ?
C99 C97 C107 C105 2.1(12) . . . . ?
C99 C97 C107 C109 -175.6(10) . . . . ?
C99 C101 C103 C105 3.2(14) . . . . ?
C100 C102 C104 C106 -1.0(13) . . . . ?
C100 C102 C104 C114 -179.8(8) . . . . ?
C101 C103 C105 C107 -4.4(13) . . . . ?
C101 C103 C105 C115 177.2(8) . . . . ?
C102 C104 C106 C96 -1.6(12) . . . . ?
C102 C104 C106 C108 175.0(9) . . . . ?
C102 C104 C114 C112 -171.6(7) . . . . ?
C102 C104 C114 O32A 7.6(12) . . . . ?
C103 C105 C107 C97 1.7(12) . . . . ?
C103 C105 C107 C109 179.4(9) . . . . ?
C103 C105 C115 C113 177.7(8) . . . . ?
C103 C105 C115 O32B -3.5(13) . . . . ?
C104 C106 C108 O30 173.8(9) . . . . ?
C104 C106 C108 C110 -2.0(14) . . . . ?
C105 C107 C109 O30 -177.4(9) . . . . ?
C105 C107 C109 C111 0.3(16) . . . . ?
C106 C96 C98 C100 -6.8(13) . . . . ?
C106 C104 C114 C112 9.6(11) . . . . ?
C106 C104 C114 O32A -171.2(8) . . . . ?
C106 C108 C110 C112 6.8(15) . . . . ?
C106 C108 C110 C116 -179.0(11) . . . . ?
C107 C97 C99 C101 -3.2(14) . . . . ?
C107 C105 C115 C113 -0.8(11) . . . . ?
C107 C105 C115 O32B 178.0(9) . . . . ?
C107 C109 C111 C113 4.7(17) . . . . ?
C107 C109 C111 C117 -177.0(12) . . . . ?
C108 C110 C112 C114 -3.3(13) . . . . ?
C108 C110 C112 C122 175.4(9) . . . . ?
C108 C110 C116 O31 7(2) . . . . ?
C108 C110 C116 C118 -178.1(11) . . . . ?
C109 C111 C113 C115 -7.8(14) . . . . ?
C109 C111 C113 C123 171.4(10) . . . . ?
C109 C111 C117 O31 3(2) . . . . ?
C109 C111 C117 C119 -171.5(12) . . . . ?
C110 C112 C114 C104 -4.6(12) . . . . ?
C110 C112 C114 O32A 176.2(8) . . . . ?
C110 C112 C122 C120 1.0(13) . . . . ?
C110 C116 C118 C120 5.0(18) . . . . ?
C111 C113 C115 C105 5.9(12) . . . . ?
C111 C113 C115 O32B -172.9(9) . . . . ?
C111 C113 C123 C121 3.6(13) . . . . ?
C111 C117 C119 C121 -4(2) . . . . ?
C112 C110 C116 O31 -178.6(11) . . . . ?
C112 C110 C116 C118 -3.8(17) . . . . ?
C113 C111 C117 O31 -178.7(11) . . . . ?
C113 C111 C117 C119 6.8(18) . . . . ?
C114 C104 C106 C96 177.1(8) . . . . ?
C114 C104 C106 C108 -6.2(12) . . . . ?
C114 C112 C122 C120 179.7(8) . . . . ?
C115 C105 C107 C97 -179.9(8) . . . . ?
C115 C105 C107 C109 -2.1(12) . . . . ?
C115 C113 C123 C121 -177.2(7) . . . . ?
C116 C110 C112 C114 -177.8(10) . . . . ?
C116 C110 C112 C122 0.9(14) . . . . ?
C116 C118 C120 C122 -3.0(15) . . . . ?
C117 C111 C113 C115 173.9(10) . . . . ?
C117 C111 C113 C123 -7.0(15) . . . . ?
C117 C119 C121 C123 0.7(16) . . . . ?
C118 C120 C122 C112 0.0(13) . . . . ?
C119 C121 C123 C113 -0.4(13) . . . . ?
C122 C112 C114 C104 176.6(7) . . . . ?
C122 C112 C114 O32A -2.6(12) . . . . ?
C123 C113 C115 C105 -173.3(7) . . . . ?
C123 C113 C115 O32B 7.9(13) . . . . ?
C125 C127 C129 C131 0.6(11) . . . . ?
C125 C135 C137 O34 -8.0(8) . . . . ?
C125 C135 C137 C139 173.8(5) . . . . ?
C126 C4 C134 C132 4.5(19) . . . . ?
C126 C4 C134 C136 -173.1(13) . . . . ?
C126 C128 C130 C132 3(2) . . . . ?
C127 C125 C135 C133 5.8(8) . . . . ?
C127 C125 C135 C137 -170.2(5) . . . . ?
C127 C129 C131 C133 2.3(11) . . . . ?
C128 C130 C132 C134 -2(2) . . . . ?
C128 C130 C132 C142 177.6(12) . . . . ?
C129 C131 C133 C135 -1.0(11) . . . . ?
C129 C131 C133 C143 179.2(6) . . . . ?
C130 C132 C134 C4 -1.6(19) . . . . ?
C130 C132 C134 C136 176.1(13) . . . . ?
C130 C132 C142 C140 -176.4(11) . . . . ?
C130 C132 C142 O36A -1.1(18) . . . . ?
C131 C133 C135 C125 -3.2(9) . . . . ?
C131 C133 C135 C137 172.8(6) . . . . ?
C131 C133 C143 C141 -169.8(6) . . . . ?
C131 C133 C143 O36B 7.3(10) . . . . ?
C132 C134 C136 O34 -173.6(12) . . . . ?
C132 C134 C136 C138 -2(2) . . . . ?
C133 C135 C137 O34 176.0(5) . . . . ?
C133 C135 C137 C139 -2.1(8) . . . . ?
C134 C4 C126 C128 -4(2) . . . . ?
C134 C132 C142 C140 3.2(18) . . . . ?
C134 C132 C142 O36A 178.6(12) . . . . ?
C134 C136 C138 C140 7(2) . . . . ?
C134 C136 C138 C144 -178.9(13) . . . . ?
C135 C125 C127 C129 -4.6(9) . . . . ?
C135 C133 C143 C141 10.4(9) . . . . ?
C135 C133 C143 O36B -172.5(6) . . . . ?
C135 C137 C139 C141 8.5(8) . . . . ?
C135 C137 C139 C145 -176.0(5) . . . . ?
C136 C138 C140 C142 -7.6(18) . . . . ?
C136 C138 C140 C150 173.6(13) . . . . ?
C136 C138 C144 O35 16(2) . . . . ?
C136 C138 C144 C146 -174.5(13) . . . . ?
C137 C139 C141 C143 -5.2(9) . . . . ?
C137 C139 C141 C151 174.7(6) . . . . ?
C137 C139 C145 O35 1.0(9) . . . . ?
C137 C139 C145 C147 -174.0(5) . . . . ?
C138 C140 C142 C132 2.7(18) . . . . ?
C138 C140 C142 O36A -172.7(12) . . . . ?
C138 C140 C150 C148 1(2) . . . . ?
C138 C144 C146 C148 1(2) . . . . ?
C139 C141 C143 C133 -4.0(9) . . . . ?
C139 C141 C143 O36B 178.8(6) . . . . ?
C139 C141 C151 C149 -0.3(11) . . . . ?
C139 C145 C147 C149 -1.1(10) . . . . ?
C140 C138 C144 O35 -169.8(11) . . . . ?
C140 C138 C144 C146 -1(2) . . . . ?
C141 C139 C145 O35 176.6(5) . . . . ?
C141 C139 C145 C147 1.6(8) . . . . ?
C142 C132 C134 C4 178.7(12) . . . . ?
C142 C132 C134 C136 -3.6(19) . . . . ?
C142 C140 C150 C148 -177.9(12) . . . . ?
C143 C133 C135 C125 176.6(5) . . . . ?
C143 C133 C135 C137 -7.4(9) . . . . ?
C143 C141 C151 C149 179.6(7) . . . . ?
C144 C138 C140 C142 178.3(12) . . . . ?
C144 C138 C140 C150 -0.5(19) . . . . ?
C144 C146 C148 C150 -1(2) . . . . ?
C145 C139 C141 C143 179.1(5) . . . . ?
C145 C139 C141 C151 -1.0(9) . . . . ?
C145 C147 C149 C151 -0.2(11) . . . . ?
C146 C148 C150 C140 0(2) . . . . ?
C147 C149 C151 C141 0.9(12) . . . . ?
C150 C140 C142 C132 -178.4(12) . . . . ?
C150 C140 C142 O36A 6.2(18) . . . . ?
C151 C141 C143 C133 176.1(6) . . . . ?
C151 C141 C143 O36B -1.1(10) . . . . ?
C153 N5 C152 O37 -2.0(7) . . . . ?
C154 N5 C152 O37 175.6(4) . . . . ?
C156 N6 C155 O38 -1.2(7) . . . . ?
C157 N6 C155 O38 -176.6(4) . . . . ?
C159 N7 C158 O39 0.2(6) . . . . ?
C160 N7 C158 O39 178.1(4) . . . . ?
C168 N9 C167 O41 1(2) . . . . ?
C169 N9 C167 O41 -169.1(14) . . . . ?
C171 N10 C170 O42 0(4) . . . . ?
C172 N10 C170 O42 -174(3) . . . . ?
C174 N11 C173 O43 -0.1(10) . . . . ?
C175 N11 C173 O43 -175.0(7) . . . . ?
C1A C11 C1X C1S -0.4(5) . . . . ?
C1A C11 C1X C1U 179.2(3) . . . . ?
C40A C41A C42A C37 -9.6(16) . . . . ?
C42A C37 C38 O12 18.1(8) . . . . ?
C42A C37 C38 C33 -163.7(6) . . . . ?
C54A C55A C56A C51 -8.0(15) . . . . ?
C56A C51 C52 O16 19.7(8) . . . . ?
C56A C51 C52 C47 -159.1(6) . . . . ?
C40B C41B C42B C37 5.4(17) . . . . ?
C42B C37 C38 O12 -7.2(8) . . . . ?
C42B C37 C38 C33 171.0(6) . . . . ?
C54B C55B C56B C51 6.8(14) . . . . ?
C56B C51 C52 O16 -17.1(7) . . . . ?
C56B C51 C52 C47 164.0(5) . . . . ?
C1G C13 C32 C33 0.5(7) . . . . ?
C1G C29 C34 C33 1.9(5) . . . . ?
C1G C29 C34 C35 -178.3(3) . . . . ?
C1I C7 C1U O2 178.1(3) . . . . ?
C1I C7 C1U C1X -0.9(5) . . . . ?
C1I C15 C1S C1N -177.5(3) . . . . ?
C1I C15 C1S C1X 3.5(5) . . . . ?
C1N C1S C1X C11 -1.4(5) . . . . ?
C1N C1S C1X C1U 179.0(3) . . . . ?
C1P C20 C1W O6 -1.0(4) . . . . ?
C1P C20 C1W C22 179.8(3) . . . . ?
C1P C20 C1Y C18 -0.7(5) . . . . ?
C1P C20 C1Y C24 177.8(3) . . . . ?
C1Q C1N C1S C15 -177.5(3) . . . . ?
C1Q C1N C1S C1X 1.6(6) . . . . ?
C1S C15 C1I C7 -3.7(5) . . . . ?
C1S C15 C1I C10 174.8(3) . . . . ?
C1S C1N C1Q C1A 0.2(6) . . . . ?
C1T C18 C1Y C20 0.7(5) . . . . ?
C1T C18 C1Y C24 -177.9(3) . . . . ?
C1U C7 C1I C10 -176.0(3) . . . . ?
C1U C7 C1I C15 2.4(5) . . . . ?
C1W C20 C1P O5 -1.9(5) . . . . ?
C1W C20 C1P C1V 177.4(3) . . . . ?
C1W C20 C1Y C18 -178.1(3) . . . . ?
C1W C20 C1Y C24 0.5(5) . . . . ?
C1W C22 C23 C14 176.1(3) . . . . ?
C1W C22 C23 C24 -4.3(5) . . . . ?
C1W C22 C25 O7 -0.1(5) . . . . ?
C1W C22 C25 C26 -178.8(3) . . . . ?
C1X C11 C1A C1Q 2.2(5) . . . . ?
C1Y C18 C1T C1V 0.0(6) . . . . ?
C1Y C20 C1P O5 -179.2(3) . . . . ?
C1Y C20 C1P C1V 0.1(5) . . . . ?
C1Y C20 C1W O6 176.3(3) . . . . ?
C1Y C20 C1W C22 -2.9(4) . . . . ?


_vrf_PLAT430_CoChrys-3           
;
RESPONSE:
Caused by split model of the disorder.
;

####################################################################### 
# 
# 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_CuChrys-1
_database_code_depnum_ccdc_archive 'CCDC 1044030'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2014-09-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2013-4
_chemical_name_systematic        di(chrysazinato)-di-copper(II)
_chemical_name_common            ?
_chemical_formula_moiety         'C28 H12 Cu2 O8'
_chemical_formula_sum            'C28 H12 Cu2 O8'
_chemical_formula_weight         603.46
_chemical_melting_point          ?
_diffrn_ambient_temperature      120.0
_chemical_oxdiff_formula         'Cu2 C28 O8 H8'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   13.5308(3)
_cell_length_b                   7.7288(2)
_cell_length_c                   19.6854(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.380(2)
_cell_angle_gamma                90
_cell_volume                     2031.10(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5267
_cell_measurement_temperature    120
_cell_measurement_theta_max      71.1060
_cell_measurement_theta_min      6.1540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.131
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.1319
_exptl_crystal_size_mid          0.1101
_exptl_crystal_size_min          0.0245
_exptl_crystal_description       plate
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.200
_diffrn_reflns_theta_min         3.311
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9454
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   37.00   63.00   1.0000   10.2300
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -25.00   29.00   1.0000   10.2300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -60.0000 54

#__ type_ start__ end____ width___ exp.time_
  3 omega  -16.00   17.00   1.0000   10.2300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  150.0000 33

#__ type_ start__ end____ width___ exp.time_
  4 omega   77.00  124.00   1.0000   32.4000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  -90.0000 47

#__ type_ start__ end____ width___ exp.time_
  5 omega    2.00   58.00   1.0000   32.4000
omega____ theta____ kappa____ phi______ frames
    -       54.7500 -125.0000  -30.0000 56

#__ type_ start__ end____ width___ exp.time_
  6 omega -111.00  -13.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000 -180.0000 98

#__ type_ start__ end____ width___ exp.time_
  7 omega -124.00  -44.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  -63.0000   30.0000 80

#__ type_ start__ end____ width___ exp.time_
  8 omega   38.00   67.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000    0.0000 29

#__ type_ start__ end____ width___ exp.time_
  9 omega   43.00  113.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -63.0000 -150.0000 70

#__ type_ start__ end____ width___ exp.time_
 10 omega   43.00   70.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
 11 omega   39.00   66.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 12 omega   41.00   66.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 13 omega   46.00   72.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 14 omega  110.00  136.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 15 omega   73.00  140.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  -30.0000 67

#__ type_ start__ end____ width___ exp.time_
 16 omega   41.00   67.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   44.00   71.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 18 omega   39.00   65.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega   41.00   66.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000  -90.0000 25

#__ type_ start__ end____ width___ exp.time_
 20 omega   41.00   67.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000  -30.0000 26

#__ type_ start__ end____ width___ exp.time_
 21 omega  138.00  171.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
 22 omega   42.00   70.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000   60.0000 28

#__ type_ start__ end____ width___ exp.time_
 23 omega   74.00  176.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000   12.0000  150.0000 102

#__ type_ start__ end____ width___ exp.time_
 24 omega   38.00   68.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -37.0000  150.0000 30

#__ type_ start__ end____ width___ exp.time_
 25 omega   88.00  113.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 26 omega   39.00   64.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 27 omega  118.00  154.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000   86.0000  134.0000 36

#__ type_ start__ end____ width___ exp.time_
 28 omega   40.00   67.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -91.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 29 omega   80.00  113.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
 30 omega   82.00  107.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000   30.0000 25

#__ type_ start__ end____ width___ exp.time_
 31 omega   42.00   79.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000 -150.0000 37

#__ type_ start__ end____ width___ exp.time_
 32 omega   39.00   64.00   1.0000   27.1100
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0637731000
_diffrn_orient_matrix_UB_12      0.0445412000
_diffrn_orient_matrix_UB_13      0.0699813000
_diffrn_orient_matrix_UB_21      -0.0572158000
_diffrn_orient_matrix_UB_22      0.1720077000
_diffrn_orient_matrix_UB_23      0.0014754000
_diffrn_orient_matrix_UB_31      -0.0772843000
_diffrn_orient_matrix_UB_32      -0.0903004000
_diffrn_orient_matrix_UB_33      0.0373474000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          ?
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3468
_reflns_number_total             3926
_reflns_odcompleteness_completeness 94.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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       
;
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    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3926
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0314
_refine_ls_restrained_S_all      1.066
_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)+(0.0438P)²+2.1374P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0921
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C28(H28), C27(H27), C21(H21), C23(H23), C15(H15), C9(H9), C8(H8),
 C7(H7), C1(H1), C22(H22), C14(H14)
;
_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
Cu1 Cu 0.74759(3) 0.38131(5) 0.09715(2) 0.03123(12) Uani 1 1 d . . . . .
Cu2 Cu 0.64958(3) 0.43989(5) -0.04524(2) 0.02933(12) Uani 1 1 d . . . . .
O1 O 0.86527(13) 0.4626(3) 0.14892(9) 0.0392(5) Uani 1 1 d . . . . .
O2 O 0.77486(12) 0.4943(2) 0.01405(8) 0.0281(4) Uani 1 1 d . . . . .
O3 O 0.68273(14) 0.5706(3) -0.11638(9) 0.0419(5) Uani 1 1 d . . . . .
O4 O 1.09836(18) 0.8519(4) -0.03748(13) 0.0718(8) Uani 1 1 d . . . . .
O5 O 0.70612(15) 0.2724(3) 0.17153(9) 0.0442(5) Uani 1 1 d . . . . .
O6 O 0.62250(12) 0.3251(2) 0.03736(8) 0.0264(3) Uani 1 1 d . . . . .
O7 O 0.52010(13) 0.4041(2) -0.09121(9) 0.0322(4) Uani 1 1 d . . . . .
O8 O 0.31826(14) -0.0966(3) 0.07548(10) 0.0444(5) Uani 1 1 d . . . . .
C1 C 1.0176(2) 0.5976(4) 0.17818(14) 0.0395(6) Uani 1 1 d . . . . .
H1 H 1.0189 0.5570 0.2239 0.047 Uiso 1 1 calc R U . . .
C2 C 0.93360(18) 0.5560(4) 0.12726(13) 0.0316(5) Uani 1 1 d . . . . .
C3 C 0.93136(18) 0.6216(3) 0.05889(13) 0.0283(5) Uani 1 1 d . . . . .
C4 C 0.84996(17) 0.5926(3) 0.00347(12) 0.0260(5) Uani 1 1 d . . . . .
C5 C 0.84776(18) 0.6705(3) -0.06348(12) 0.0275(5) Uani 1 1 d . . . . .
C6 C 0.76509(18) 0.6558(4) -0.11804(13) 0.0308(5) Uani 1 1 d . . . . .
C7 C 0.7694(2) 0.7444(4) -0.18098(14) 0.0376(6) Uani 1 1 d . . . . .
H7 H 0.7134 0.7385 -0.2169 0.045 Uiso 1 1 calc R U . . .
C8 C 0.8511(2) 0.8372(4) -0.19128(14) 0.0417(7) Uani 1 1 d . . . . .
H8 H 0.8516 0.8953 -0.2338 0.050 Uiso 1 1 calc R U . . .
C9 C 0.9339(2) 0.8466(4) -0.13934(15) 0.0413(7) Uani 1 1 d . . . . .
H9 H 0.9919 0.9079 -0.1471 0.050 Uiso 1 1 calc R U . . .
C10 C 0.93255(19) 0.7679(3) -0.07691(14) 0.0326(6) Uani 1 1 d . . . . .
C11 C 1.0219(2) 0.7854(4) -0.02398(16) 0.0416(7) Uani 1 1 d . . . . .
C12 C 1.01683(18) 0.7196(3) 0.04584(14) 0.0323(5) Uani 1 1 d . . . . .
C13 C 1.0963(2) 0.7534(4) 0.09676(15) 0.0389(6) Uani 1 1 d . . . . .
H13 H 1.1518 0.8179 0.0865 0.047 Uiso 1 1 calc R U . . .
C14 C 1.0960(2) 0.6933(4) 0.16383(15) 0.0414(7) Uani 1 1 d . . . . .
H14 H 1.1504 0.7194 0.1993 0.050 Uiso 1 1 calc R U . . .
C15 C 0.6133(2) 0.1106(4) 0.23630(13) 0.0329(6) Uani 1 1 d . . . . .
H15 H 0.6658 0.1249 0.2743 0.040 Uiso 1 1 calc R U . . .
C16 C 0.62347(19) 0.1878(3) 0.17228(13) 0.0297(5) Uani 1 1 d . . . . .
C17 C 0.54333(17) 0.1649(3) 0.11570(12) 0.0252(5) Uani 1 1 d . . . . .
C18 C 0.54388(17) 0.2393(3) 0.04893(12) 0.0241(5) Uani 1 1 d . . . . .
C19 C 0.45904(17) 0.2218(3) -0.00598(12) 0.0240(5) Uani 1 1 d . . . . .
C20 C 0.45303(17) 0.3048(3) -0.07159(12) 0.0259(5) Uani 1 1 d . . . . .
C21 C 0.36471(18) 0.2798(3) -0.12137(13) 0.0302(5) Uani 1 1 d . . . . .
H21 H 0.3595 0.3363 -0.1647 0.036 Uiso 1 1 calc R U . . .
C22 C 0.28765(18) 0.1775(4) -0.10875(13) 0.0319(5) Uani 1 1 d . . . . .
H22 H 0.2302 0.1631 -0.1431 0.038 Uiso 1 1 calc R U . . .
C23 C 0.29328(18) 0.0932(3) -0.04494(14) 0.0312(5) Uani 1 1 d . . . . .
H23 H 0.2397 0.0215 -0.0361 0.037 Uiso 1 1 calc R U . . .
C24 C 0.37609(17) 0.1147(3) 0.00434(12) 0.0257(5) Uani 1 1 d . . . . .
C25 C 0.37936(18) 0.0184(4) 0.06978(13) 0.0303(5) Uani 1 1 d . . . . .
C26 C 0.46002(18) 0.0605(3) 0.12683(12) 0.0275(5) Uani 1 1 d . . . . .
C27 C 0.4542(2) -0.0098(4) 0.19024(14) 0.0348(6) Uani 1 1 d . . . . .
H27 H 0.3974 -0.0766 0.1964 0.042 Uiso 1 1 calc R U . . .
C28 C 0.5311(2) 0.0167(4) 0.24527(13) 0.0355(6) Uani 1 1 d . . . . .
H28 H 0.5264 -0.0306 0.2892 0.043 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu2 2.9342(5) . ?
Cu1 O1 1.8546(18) . ?
Cu1 O2 1.9420(16) . ?
Cu1 O5 1.8535(18) . ?
Cu1 O6 1.9467(16) . ?
Cu2 O2 1.9409(16) . ?
Cu2 O3 1.8407(18) . ?
Cu2 O6 1.9389(16) . ?
Cu2 O7 1.8569(17) . ?
O1 C2 1.298(3) . ?
O2 C4 1.313(3) . ?
O3 C6 1.299(3) . ?
O4 C11 1.222(3) . ?
O5 C16 1.297(3) . ?
O6 C18 1.305(3) . ?
O7 C20 1.294(3) . ?
O8 C25 1.231(3) . ?
C1 C2 1.424(3) . ?
C1 C14 1.360(4) . ?
C2 C3 1.434(4) . ?
C3 C4 1.436(3) . ?
C3 C12 1.440(3) . ?
C4 C5 1.444(3) . ?
C5 C6 1.423(3) . ?
C5 C10 1.433(3) . ?
C6 C7 1.425(4) . ?
C7 C8 1.360(4) . ?
C8 C9 1.390(4) . ?
C9 C10 1.374(4) . ?
C10 C11 1.468(4) . ?
C11 C12 1.478(4) . ?
C12 C13 1.370(4) . ?
C13 C14 1.400(4) . ?
C15 C16 1.421(3) . ?
C15 C28 1.363(4) . ?
C16 C17 1.433(3) . ?
C17 C18 1.436(3) . ?
C17 C26 1.432(3) . ?
C18 C19 1.449(3) . ?
C19 C20 1.433(3) . ?
C19 C24 1.436(3) . ?
C20 C21 1.430(3) . ?
C21 C22 1.363(4) . ?
C22 C23 1.406(4) . ?
C23 C24 1.367(3) . ?
C24 C25 1.482(3) . ?
C25 C26 1.469(3) . ?
C26 C27 1.375(4) . ?
C27 C28 1.390(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 Cu2 133.36(6) . . ?
O1 Cu1 O2 92.67(8) . . ?
O1 Cu1 O6 172.67(9) . . ?
O2 Cu1 Cu2 40.90(5) . . ?
O2 Cu1 O6 81.76(7) . . ?
O5 Cu1 Cu2 132.60(6) . . ?
O5 Cu1 O1 93.62(8) . . ?
O5 Cu1 O2 173.32(7) . . ?
O5 Cu1 O6 91.78(7) . . ?
O6 Cu1 Cu2 40.86(5) . . ?
O2 Cu2 Cu1 40.93(5) . . ?
O3 Cu2 Cu1 133.10(6) . . ?
O3 Cu2 O2 92.38(8) . . ?
O3 Cu2 O6 172.74(8) . . ?
O3 Cu2 O7 92.21(8) . . ?
O6 Cu2 Cu1 41.06(5) . . ?
O6 Cu2 O2 81.99(7) . . ?
O7 Cu2 Cu1 133.33(5) . . ?
O7 Cu2 O2 170.92(8) . . ?
O7 Cu2 O6 92.76(7) . . ?
C2 O1 Cu1 126.97(16) . . ?
Cu2 O2 Cu1 98.17(7) . . ?
C4 O2 Cu1 130.71(15) . . ?
C4 O2 Cu2 130.75(15) . . ?
C6 O3 Cu2 127.85(17) . . ?
C16 O5 Cu1 127.61(16) . . ?
Cu2 O6 Cu1 98.08(7) . . ?
C18 O6 Cu1 131.38(15) . . ?
C18 O6 Cu2 130.53(14) . . ?
C20 O7 Cu2 126.48(15) . . ?
C14 C1 C2 122.4(3) . . ?
O1 C2 C1 115.1(2) . . ?
O1 C2 C3 126.7(2) . . ?
C1 C2 C3 118.2(2) . . ?
C2 C3 C4 123.7(2) . . ?
C2 C3 C12 117.3(2) . . ?
C4 C3 C12 119.0(2) . . ?
O2 C4 C3 119.2(2) . . ?
O2 C4 C5 119.0(2) . . ?
C3 C4 C5 121.8(2) . . ?
C6 C5 C4 123.5(2) . . ?
C6 C5 C10 117.2(2) . . ?
C10 C5 C4 119.3(2) . . ?
O3 C6 C5 126.4(2) . . ?
O3 C6 C7 115.0(2) . . ?
C5 C6 C7 118.6(2) . . ?
C8 C7 C6 122.2(3) . . ?
C7 C8 C9 119.7(3) . . ?
C10 C9 C8 120.5(3) . . ?
C5 C10 C11 120.6(2) . . ?
C9 C10 C5 121.7(2) . . ?
C9 C10 C11 117.7(2) . . ?
O4 C11 C10 120.8(3) . . ?
O4 C11 C12 121.1(3) . . ?
C10 C11 C12 118.1(2) . . ?
C3 C12 C11 120.5(2) . . ?
C13 C12 C3 121.8(3) . . ?
C13 C12 C11 117.7(2) . . ?
C12 C13 C14 120.3(3) . . ?
C1 C14 C13 119.9(2) . . ?
C28 C15 C16 122.5(2) . . ?
O5 C16 C15 115.5(2) . . ?
O5 C16 C17 126.7(2) . . ?
C15 C16 C17 117.8(2) . . ?
C16 C17 C18 123.1(2) . . ?
C26 C17 C16 117.8(2) . . ?
C26 C17 C18 119.2(2) . . ?
O6 C18 C17 119.3(2) . . ?
O6 C18 C19 119.1(2) . . ?
C17 C18 C19 121.6(2) . . ?
C20 C19 C18 123.5(2) . . ?
C20 C19 C24 117.1(2) . . ?
C24 C19 C18 119.4(2) . . ?
O7 C20 C19 126.5(2) . . ?
O7 C20 C21 115.1(2) . . ?
C21 C20 C19 118.4(2) . . ?
C22 C21 C20 122.2(2) . . ?
C21 C22 C23 120.0(2) . . ?
C24 C23 C22 119.8(2) . . ?
C19 C24 C25 120.0(2) . . ?
C23 C24 C19 122.6(2) . . ?
C23 C24 C25 117.4(2) . . ?
O8 C25 C24 121.1(2) . . ?
O8 C25 C26 121.1(2) . . ?
C26 C25 C24 117.8(2) . . ?
C17 C26 C25 120.9(2) . . ?
C27 C26 C17 121.6(2) . . ?
C27 C26 C25 117.4(2) . . ?
C26 C27 C28 120.2(2) . . ?
C15 C28 C27 120.0(2) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-9 0 0 0.0049 -8.9994 0.0005 0.0006 -0.5739 0.5150 0.6955
8 0 2 0.0131 7.9995 -0.0004 1.9994 0.6501 -0.4548 -0.5435
7 2 -7 0.0354 6.9998 1.9992 -7.0000 0.0456 -0.0670 -0.9829
-7 0 9 0.0449 -6.9996 0.0006 8.9998 0.1835 0.4139 0.8770
7 -1 -9 0.0407 6.9995 -1.0004 -8.9997 -0.2280 -0.5858 -0.7867
3 5 -3 0.0531 3.0003 4.9991 -3.0003 0.2040 0.6838 -0.7953
-3 4 5 0.0539 -2.9995 3.9997 4.9996 0.3367 0.8670 0.0574
-5 -4 6 0.0608 -5.0001 -3.9990 6.0001 -0.0771 -0.3929 0.9716
1 -5 -5 0.0502 0.9995 -4.9995 -4.9994 -0.5088 -0.9245 0.1875
-3 2 -10 0.0460 -2.9996 1.9997 -9.9992 -0.8020 0.5008 -0.3222

####################################################################### 
# 
# 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_CuChrys-2
_database_code_depnum_ccdc_archive 'CCDC 1044031'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-11-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2014/6
_chemical_name_systematic        
"di(chrysazinato)di-copper(II) N,N'-dimethylformamide solvate"
_chemical_name_common            ?
_chemical_formula_moiety         'C28 H12 Cu2 O8'
_chemical_formula_sum            'C29.33 H15.11 Cu2 N0.44 O8.44'
_chemical_formula_weight         635.77
_chemical_melting_point          ?
_exptl_crystal_description       needle
_exptl_crystal_colour            black
_diffrn_ambient_temperature      100(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3480 1.2190 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   40.04(3)
_cell_length_b                   40.04(3)
_cell_length_c                   3.674(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5101(9)
_cell_formula_units_Z            9
_cell_measurement_reflns_used    4306
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      1.7
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.801
_exptl_absorpt_coefficient_mu    1.939
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
;
CrystalClear-SM Expert 3.1 b26 (Rigaku, 20112)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2877
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            16552
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.603
_diffrn_reflns_theta_min         1.708
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_details      
;
scan:
	Number of images: 175
	           Slice: -60.0000 - 115.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 59.8393
	          2theta: 30.1018
scan:
	Number of images: 120
	           Slice: -60.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -50.0000
	             Phi: 0.0000
	             XTD: 59.8393
	          2theta: 30.1018
scan:
	Number of images: 120
	           Slice: -60.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -50.0000
	             Phi: 120.0000
	             XTD: 59.8393
	          2theta: 30.1018
scan:
	Number of images: 120
	           Slice: -60.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -50.0000
	             Phi: 240.0000
	             XTD: 59.8393
	          2theta: 30.1018
;
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.028544
_diffrn_orient_matrix_UB_12      -0.003106
_diffrn_orient_matrix_UB_13      -0.002664
_diffrn_orient_matrix_UB_21      0.017754
_diffrn_orient_matrix_UB_22      0.019917
_diffrn_orient_matrix_UB_23      0.010936
_diffrn_orient_matrix_UB_31      0.007218
_diffrn_orient_matrix_UB_32      -0.135882
_diffrn_orient_matrix_UB_33      0.235753
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_probe          ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_source                   synchrotron
_diffrn_source_type              'DLS beamline I19'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2481
_reflns_number_total             2587
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.517
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0503
_refine_ls_restrained_S_all      1.145
_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)+(0.0686P)²+23.2644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1317
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2(0.02) H3(0.021) H4(0.02) H8(0.024) H9(0.024) H10(0.021)
 Fixed X: H2(0.371301) H3(0.371901) H4(0.4278) H8(0.558801) H9(0.611301)
 H10(0.6104)
 Fixed Y: H2(0.3574) H3(0.3029) H4(0.3075) H8(0.3814) H9(0.4403) H10(0.4963)
 Fixed Z: H2(-0.148299) H3(0.0297) H4(0.2787) H8(0.721301) H9(0.910399)
 H10(0.8328)
;
_atom_sites_solution_hydrogens   difmap
_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
Cu1 Cu 0.46008(2) 0.47767(2) -0.14895(10) 0.01608(16) Uani 1 1 d . . . . .
O1 O 0.42271(6) 0.42556(6) -0.1349(6) 0.0178(5) Uani 1 1 d . . . . .
O2 O 0.49598(6) 0.46919(6) 0.1456(6) 0.0164(4) Uani 1 1 d . . . . .
O3 O 0.56206(7) 0.50880(6) 0.5353(6) 0.0192(5) Uani 1 1 d . . . . .
O4 O 0.49598(7) 0.33601(7) 0.4489(7) 0.0246(5) Uani 1 1 d . . . . .
C1 C 0.42680(9) 0.39735(9) -0.0076(8) 0.0146(6) Uani 1 1 d . . . . .
C2 C 0.39364(9) 0.35966(9) -0.0475(9) 0.0166(6) Uani 1 1 d . . . . .
H2 H 0.3713 0.3574 -0.1483 0.020 Uiso 1 1 d . U . . .
C3 C 0.39391(9) 0.32690(9) 0.0582(8) 0.0173(6) Uani 1 1 d . . . . .
H3 H 0.3719 0.3029 0.0297 0.021 Uiso 1 1 d . U . . .
C4 C 0.42754(9) 0.32973(9) 0.2101(8) 0.0166(6) Uani 1 1 d . . . . .
H4 H 0.4278 0.3075 0.2787 0.020 Uiso 1 1 d . U . . .
C5 C 0.46002(9) 0.36518(9) 0.2576(8) 0.0153(6) Uani 1 1 d . . . . .
C6 C 0.49471(9) 0.36607(9) 0.4071(8) 0.0174(6) Uani 1 1 d . . . . .
C7 C 0.52785(9) 0.40402(9) 0.5077(8) 0.0174(6) Uani 1 1 d . . . . .
C8 C 0.55876(10) 0.40435(10) 0.6816(9) 0.0201(6) Uani 1 1 d . . . . .
H8 H 0.5588 0.3814 0.7213 0.024 Uiso 1 1 d . U . . .
C9 C 0.59029(10) 0.43986(10) 0.7980(9) 0.0198(6) Uani 1 1 d . . . . .
H9 H 0.6113 0.4403 0.9104 0.024 Uiso 1 1 d . U . . .
C10 C 0.58993(9) 0.47341(9) 0.7458(8) 0.0178(6) Uani 1 1 d . . . . .
H10 H 0.6104 0.4963 0.8328 0.021 Uiso 1 1 d . U . . .
C11 C 0.55920(9) 0.47435(9) 0.5626(8) 0.0158(6) Uani 1 1 d . . . . .
C12 C 0.52721(9) 0.43894(9) 0.4376(8) 0.0151(6) Uani 1 1 d . . . . .
C13 C 0.49468(9) 0.43679(8) 0.2432(8) 0.0140(6) Uani 1 1 d . . . . .
C14 C 0.46084(9) 0.40044(9) 0.1620(8) 0.0148(6) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu1 2.983(2) 10_665 ?
Cu1 O1 1.863(3) . ?
Cu1 O2 1.970(3) 10_665 ?
Cu1 O2 1.960(3) . ?
Cu1 O3 1.891(3) 10_665 ?
O1 C1 1.306(4) . ?
O2 Cu1 1.970(3) 10_665 ?
O2 C13 1.322(4) . ?
O3 Cu1 1.891(3) 10_665 ?
O3 C11 1.329(4) . ?
O4 C6 1.239(4) . ?
C1 C2 1.435(4) . ?
C1 C14 1.447(4) . ?
C2 C3 1.373(5) . ?
C3 C4 1.409(5) . ?
C4 C5 1.375(5) . ?
C5 C6 1.477(5) . ?
C5 C14 1.439(4) . ?
C6 C7 1.480(5) . ?
C7 C8 1.387(5) . ?
C7 C12 1.434(4) . ?
C8 C9 1.415(5) . ?
C9 C10 1.364(5) . ?
C10 C11 1.419(4) . ?
C11 C12 1.430(4) . ?
C12 C13 1.450(4) . ?
C13 C14 1.439(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 Cu1 132.92(7) . 10_665 ?
O1 Cu1 O2 173.12(9) . 10_665 ?
O1 Cu1 O2 92.22(9) . . ?
O1 Cu1 O3 96.48(10) . 10_665 ?
O2 Cu1 Cu1 40.73(6) . 10_665 ?
O2 Cu1 Cu1 40.48(7) 10_665 10_665 ?
O2 Cu1 O2 81.21(10) . 10_665 ?
O3 Cu1 Cu1 128.24(7) 10_665 10_665 ?
O3 Cu1 O2 89.34(9) 10_665 10_665 ?
O3 Cu1 O2 162.52(10) 10_665 . ?
C1 O1 Cu1 126.9(2) . . ?
Cu1 O2 Cu1 98.78(10) . 10_665 ?
C13 O2 Cu1 130.3(2) . . ?
C13 O2 Cu1 129.37(19) . 10_665 ?
C11 O3 Cu1 123.0(2) . 10_665 ?
O1 C1 C2 115.0(3) . . ?
O1 C1 C14 126.9(3) . . ?
C2 C1 C14 118.1(3) . . ?
C3 C2 C1 122.1(3) . . ?
C2 C3 C4 119.9(3) . . ?
C5 C4 C3 120.4(3) . . ?
C4 C5 C6 117.7(3) . . ?
C4 C5 C14 121.9(3) . . ?
C14 C5 C6 120.5(3) . . ?
O4 C6 C5 121.2(3) . . ?
O4 C6 C7 121.0(3) . . ?
C5 C6 C7 117.8(3) . . ?
C8 C7 C6 117.5(3) . . ?
C8 C7 C12 121.6(3) . . ?
C12 C7 C6 120.8(3) . . ?
C7 C8 C9 119.5(3) . . ?
C10 C9 C8 120.2(3) . . ?
C9 C10 C11 121.9(3) . . ?
O3 C11 C10 115.9(3) . . ?
O3 C11 C12 125.0(3) . . ?
C10 C11 C12 119.0(3) . . ?
C7 C12 C13 119.0(3) . . ?
C11 C12 C7 117.7(3) . . ?
C11 C12 C13 123.3(3) . . ?
O2 C13 C12 118.8(3) . . ?
O2 C13 C14 119.5(3) . . ?
C14 C13 C12 121.7(3) . . ?
C5 C14 C1 117.6(3) . . ?
C13 C14 C1 123.1(3) . . ?
C13 C14 C5 119.3(3) . . ?

_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 -0.021 284 53 'Most likely DMF'
2 0.333 0.667 0.743 284 53 'Most likely DMF'
3 0.667 0.333 0.409 284 53 'Most likely DMF'

_platon_squeeze_void_probe_radius 1.20
_symmetry_cell_setting           ?
_symmetry_space_group_name_h-m   ?
_symmetry_int_tables_number      ?
_chemical_absolute_configuration ?

_vrf_CHEMW03_CuChrys-2           
;
RESPONSE:
Due to the inclusion of disordered solvent removed by SQUEEZE.
;
####################################################################### 
# 
# 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_CuChrys-3
_database_code_depnum_ccdc_archive 'CCDC 1044032'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-08-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        
di(chrysazinato)-bis(dimethylsulfoxide)-di-copper(II)
_chemical_formula_moiety         'C32 H24 Cu2 O10 S2'
_chemical_formula_sum            'C32 H24 Cu2 O10 S2'
_chemical_formula_weight         759.71
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Cu2 C32 H24 O10 S2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z'

_cell_length_a                   7.90242(16)
_cell_length_b                   19.4909(4)
_cell_length_c                   18.5266(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2853.56(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7029
_cell_measurement_temperature    119.95(10)
_cell_measurement_theta_max      67.7770
_cell_measurement_theta_min      2.2630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.758
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.2214
_exptl_crystal_size_mid          0.1789
_exptl_crystal_size_min          0.0371
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12638
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.909
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.846
_diffrn_reflns_theta_min         2.267
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0591
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.8954
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0148906000
_diffrn_orient_matrix_UB_12      0.0026522000
_diffrn_orient_matrix_UB_13      -0.0828709000
_diffrn_orient_matrix_UB_21      0.1152213000
_diffrn_orient_matrix_UB_22      -0.0637528000
_diffrn_orient_matrix_UB_23      0.0015480000
_diffrn_orient_matrix_UB_31      -0.1564135000
_diffrn_orient_matrix_UB_32      -0.0467131000
_diffrn_orient_matrix_UB_33      -0.0067340000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.817
_reflns_Friedel_fraction_max     0.813
_reflns_number_gt                4499
_reflns_number_total             4714
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 
;
 Flack x determined using 1859 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         4714
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0378
_refine_ls_restrained_S_all      1.105
_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)+(0.0629P)²+1.6956P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1019
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Restrained distances
 S1B-O9 \\sim S1A-O9
 with sigma of 0.02
 S1B-C30 \\sim S1B-C29 \\sim S1A-C30 \\sim S1A-C29
 with sigma of 0.02
 S2B-O10 \\sim S2A-O10
 with sigma of 0.02
 S2B-C32 \\sim S2A-C32 \\sim S2A-C31 \\sim S2B-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(S1B) = Uanis(S1A)
Uanis(S2B) = Uanis(S2A)
4. Others
 Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(S1B)=1-FVAR(1)
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(S1A)=FVAR(1)
 Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(S2B)=1-FVAR(2)
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(S2A)=FVAR(2)
5.a Me refined with riding coordinates:
 C29(H29A,H29B,H29C), C29(H29D,H29E,H29F), C30(H30A,H30B,H30C), C30(H30D,H30E,
 H30F), C31(H31A,H31B,H31C), C31(H31D,H31E,H31F), C32(H32A,H32B,H32C), C32(H32D,
 H32E,H32F)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18),
 C26(H26), C27(H27), C28(H28)
;
_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
Cu1 Cu 0.98533(10) 0.23042(4) 0.37522(5) 0.0289(2) Uani 1 1 d . . . . .
Cu2 Cu 0.85783(9) 0.25157(4) 0.22634(5) 0.02867(19) Uani 1 1 d . . . . .
O1 O 1.0893(6) 0.1549(2) 0.4187(2) 0.0365(9) Uani 1 1 d . . . . .
O2 O 0.9346(5) 0.1761(2) 0.2880(2) 0.0307(8) Uani 1 1 d . . . . .
O3 O 0.7802(6) 0.1901(2) 0.1565(2) 0.0354(9) Uani 1 1 d . . . . .
O4 O 0.8923(7) -0.1001(2) 0.2542(3) 0.0477(11) Uani 1 1 d . . . . .
O5 O 1.0790(6) 0.2933(2) 0.4405(2) 0.0374(10) Uani 1 1 d . . . . .
O6 O 0.9123(5) 0.3055(2) 0.3120(2) 0.0319(8) Uani 1 1 d . . . . .
O7 O 0.7262(5) 0.3231(2) 0.1893(2) 0.0334(9) Uani 1 1 d . . . . .
O8 O 0.8953(6) 0.5812(2) 0.3522(3) 0.0409(10) Uani 1 1 d . . . . .
O9 O 0.7187(7) 0.2178(3) 0.4112(3) 0.0595(15) Uani 1 1 d D . . . .
O10 O 1.0998(7) 0.2841(4) 0.1731(4) 0.0642(16) Uani 1 1 d D . . . .
C1 C 1.0761(7) 0.0914(3) 0.3998(3) 0.0293(11) Uani 1 1 d . . . . .
C2 C 1.1501(7) 0.0427(3) 0.4470(3) 0.0326(12) Uani 1 1 d . . . . .
H2 H 1.199(9) 0.055(4) 0.492(4) 0.039 Uiso 1 1 d . U . . .
C3 C 1.1437(7) -0.0266(3) 0.4341(3) 0.0343(13) Uani 1 1 d . . . . .
H3 H 1.1932 -0.0569 0.4667 0.041 Uiso 1 1 calc R U . . .
C4 C 1.0638(7) -0.0519(3) 0.3728(3) 0.0319(11) Uani 1 1 d . . . . .
H4 H 1.0612 -0.0989 0.3641 0.038 Uiso 1 1 calc R U . . .
C5 C 0.9893(7) -0.0076(3) 0.3253(3) 0.0271(11) Uani 1 1 d . . . . .
C6 C 0.9948(6) 0.0661(3) 0.3350(3) 0.0258(11) Uani 1 1 d . . . . .
C7 C 0.9241(7) 0.1095(3) 0.2807(3) 0.0259(10) Uani 1 1 d . . . . .
C8 C 0.8378(6) 0.0824(3) 0.2176(3) 0.0253(11) Uani 1 1 d . . . . .
C9 C 0.8173(7) 0.0091(3) 0.2110(3) 0.0281(12) Uani 1 1 d . . . . .
C10 C 0.9004(7) -0.0374(3) 0.2629(3) 0.0310(12) Uani 1 1 d . . . . .
C11 C 0.7657(7) 0.1239(3) 0.1620(3) 0.0308(11) Uani 1 1 d . . . . .
C12 C 0.6685(7) 0.0912(3) 0.1067(3) 0.0317(12) Uani 1 1 d . . . . .
H12 H 0.6182 0.1182 0.0712 0.038 Uiso 1 1 calc R U . . .
C13 C 0.6473(7) 0.0219(3) 0.1043(3) 0.0333(13) Uani 1 1 d . . . . .
H13 H 0.5811 0.0022 0.0683 0.040 Uiso 1 1 calc R U . . .
C14 C 0.7254(7) -0.0194(3) 0.1560(3) 0.0301(12) Uani 1 1 d . . . . .
H14 H 0.7149 -0.0668 0.1531 0.036 Uiso 1 1 calc R U . . .
C15 C 1.0667(7) 0.3593(3) 0.4404(3) 0.0310(12) Uani 1 1 d . . . . .
C16 C 1.1478(8) 0.3942(3) 0.4984(3) 0.0372(13) Uani 1 1 d . . . . .
H16 H 1.2067 0.3685 0.5324 0.045 Uiso 1 1 calc R U . . .
C17 C 1.1424(7) 0.4639(3) 0.5059(3) 0.0357(13) Uani 1 1 d . . . . .
H17 H 1.1961 0.4849 0.5448 0.043 Uiso 1 1 calc R U . . .
C18 C 1.0568(8) 0.5032(3) 0.4555(4) 0.0370(13) Uani 1 1 d . . . . .
H18 H 1.0527 0.5506 0.4610 0.044 Uiso 1 1 calc R U . . .
C19 C 0.9780(7) 0.4733(3) 0.3976(3) 0.0280(12) Uani 1 1 d . . . . .
C20 C 0.9790(7) 0.4001(3) 0.3876(3) 0.0282(12) Uani 1 1 d . . . . .
C21 C 0.9019(7) 0.3714(3) 0.3229(3) 0.0272(11) Uani 1 1 d . . . . .
C22 C 0.8121(7) 0.4136(3) 0.2719(3) 0.0279(11) Uani 1 1 d . . . . .
C23 C 0.8047(7) 0.4870(3) 0.2830(3) 0.0284(11) Uani 1 1 d . . . . .
C24 C 0.8923(7) 0.5187(3) 0.3454(3) 0.0308(12) Uani 1 1 d . . . . .
C25 C 0.7296(7) 0.3871(3) 0.2090(3) 0.0281(11) Uani 1 1 d . . . . .
C26 C 0.6379(7) 0.4330(3) 0.1638(3) 0.0299(11) Uani 1 1 d . . . . .
H26 H 0.5800 0.4154 0.1242 0.036 Uiso 1 1 calc R U . . .
C27 C 0.6324(7) 0.5016(3) 0.1766(3) 0.0305(12) Uani 1 1 d . . . . .
H27 H 0.5730 0.5304 0.1456 0.037 Uiso 1 1 calc R U . . .
C28 C 0.7170(7) 0.5288(3) 0.2369(3) 0.0316(12) Uani 1 1 d . . . . .
H28 H 0.7133 0.5758 0.2456 0.038 Uiso 1 1 calc R U . . .
C29 C 0.6489(12) 0.3106(4) 0.5127(5) 0.067(3) Uani 1 1 d D . . . .
H29A H 0.6207 0.3131 0.5631 0.101 Uiso 0.836(4) 1 calc R U P A 1
H29B H 0.7522 0.3353 0.5042 0.101 Uiso 0.836(4) 1 calc R U P A 1
H29C H 0.5594 0.3306 0.4847 0.101 Uiso 0.836(4) 1 calc R U P A 1
H29D H 0.5494 0.3360 0.5258 0.101 Uiso 0.164(4) 1 calc R U P A 2
H29E H 0.6847 0.2831 0.5529 0.101 Uiso 0.164(4) 1 calc R U P A 2
H29F H 0.7376 0.3420 0.4999 0.101 Uiso 0.164(4) 1 calc R U P A 2
C30 C 0.4710(11) 0.1954(5) 0.5003(6) 0.082(4) Uani 1 1 d D . . . .
H30A H 0.4407 0.1996 0.5502 0.122 Uiso 0.836(4) 1 calc R U P A 1
H30B H 0.3945 0.2220 0.4714 0.122 Uiso 0.836(4) 1 calc R U P A 1
H30C H 0.4644 0.1481 0.4861 0.122 Uiso 0.836(4) 1 calc R U P A 1
H30D H 0.3821 0.2205 0.5236 0.122 Uiso 0.164(4) 1 calc R U P A 2
H30E H 0.4227 0.1599 0.4708 0.122 Uiso 0.164(4) 1 calc R U P A 2
H30F H 0.5432 0.1751 0.5361 0.122 Uiso 0.164(4) 1 calc R U P A 2
C31 C 1.3511(8) 0.2660(3) 0.2668(4) 0.0394(14) Uani 1 1 d D . . . .
H31A H 1.4711 0.2718 0.2723 0.059 Uiso 0.886(4) 1 calc R U P B 1
H31B H 1.2932 0.2927 0.3026 0.059 Uiso 0.886(4) 1 calc R U P B 1
H31C H 1.3225 0.2185 0.2725 0.059 Uiso 0.886(4) 1 calc R U P B 1
H31D H 1.4370 0.2341 0.2813 0.059 Uiso 0.114(4) 1 calc R U P B 2
H31E H 1.4033 0.3082 0.2519 0.059 Uiso 0.114(4) 1 calc R U P B 2
H31F H 1.2765 0.2747 0.3066 0.059 Uiso 0.114(4) 1 calc R U P B 2
C32 C 1.3893(9) 0.2303(3) 0.1274(4) 0.0432(15) Uani 1 1 d D . . . .
H32A H 1.5096 0.2364 0.1301 0.065 Uiso 0.886(4) 1 calc R U P B 1
H32B H 1.3598 0.1861 0.1465 0.065 Uiso 0.886(4) 1 calc R U P B 1
H32C H 1.3536 0.2331 0.0780 0.065 Uiso 0.886(4) 1 calc R U P B 1
H32D H 1.4767 0.1982 0.1399 0.065 Uiso 0.114(4) 1 calc R U P B 2
H32E H 1.3373 0.2165 0.0829 0.065 Uiso 0.114(4) 1 calc R U P B 2
H32F H 1.4375 0.2751 0.1219 0.065 Uiso 0.114(4) 1 calc R U P B 2
S1A S 0.6753(3) 0.22483(10) 0.48775(11) 0.0432(5) Uani 0.836(4) 1 d D . P A 1
S2A S 1.2883(2) 0.29453(9) 0.17792(10) 0.0362(4) Uani 0.886(4) 1 d D . P B 1
S1B S 0.6038(14) 0.2578(5) 0.4395(5) 0.0432(5) Uani 0.164(4) 1 d D . P A 2
S2B S 1.2371(16) 0.2320(6) 0.1956(6) 0.0362(4) Uani 0.114(4) 1 d D . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Cu2 2.9652(12) . ?
Cu1 O1 1.868(4) . ?
Cu1 O2 1.972(4) . ?
Cu1 O5 1.874(4) . ?
Cu1 O6 1.962(4) . ?
Cu1 O9 2.223(5) . ?
Cu2 O2 1.958(4) . ?
Cu2 O3 1.867(4) . ?
Cu2 O6 1.952(4) . ?
Cu2 O7 1.870(4) . ?
Cu2 O10 2.243(5) . ?
O1 C1 1.291(7) . ?
O2 C7 1.309(6) . ?
O3 C11 1.300(7) . ?
O4 C10 1.233(7) . ?
O5 C15 1.291(7) . ?
O6 C21 1.302(7) . ?
O7 C25 1.301(7) . ?
O8 C24 1.226(7) . ?
O9 S1A 1.465(6) . ?
O9 S1B 1.307(11) . ?
O10 S2A 1.506(5) . ?
O10 S2B 1.543(13) . ?
C1 C2 1.415(8) . ?
C1 C6 1.449(8) . ?
C2 C3 1.373(8) . ?
C3 C4 1.390(9) . ?
C4 C5 1.366(8) . ?
C5 C6 1.447(7) . ?
C5 C10 1.472(8) . ?
C6 C7 1.429(8) . ?
C7 C8 1.453(8) . ?
C8 C9 1.442(7) . ?
C8 C11 1.427(8) . ?
C9 C10 1.477(8) . ?
C9 C14 1.369(8) . ?
C11 C12 1.431(8) . ?
C12 C13 1.362(9) . ?
C13 C14 1.396(8) . ?
C15 C16 1.423(8) . ?
C15 C20 1.439(8) . ?
C16 C17 1.367(9) . ?
C17 C18 1.385(9) . ?
C18 C19 1.371(8) . ?
C19 C20 1.439(8) . ?
C19 C24 1.475(8) . ?
C20 C21 1.456(8) . ?
C21 C22 1.441(8) . ?
C22 C23 1.445(8) . ?
C22 C25 1.432(8) . ?
C23 C24 1.482(8) . ?
C23 C28 1.370(8) . ?
C25 C26 1.423(8) . ?
C26 C27 1.360(9) . ?
C27 C28 1.406(9) . ?
C29 S1A 1.748(8) . ?
C29 S1B 1.740(11) . ?
C30 S1A 1.729(7) . ?
C30 S1B 1.961(12) . ?
C31 S2A 1.807(7) . ?
C31 S2B 1.729(13) . ?
C32 S2A 1.756(6) . ?
C32 S2B 1.745(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 Cu2 131.30(13) . . ?
O1 Cu1 O2 91.15(17) . . ?
O1 Cu1 O5 93.60(18) . . ?
O1 Cu1 O6 167.1(2) . . ?
O1 Cu1 O9 101.5(2) . . ?
O2 Cu1 Cu2 40.85(12) . . ?
O2 Cu1 O9 89.65(18) . . ?
O5 Cu1 Cu2 130.09(13) . . ?
O5 Cu1 O2 163.7(2) . . ?
O5 Cu1 O6 90.80(17) . . ?
O5 Cu1 O9 104.6(2) . . ?
O6 Cu1 Cu2 40.62(12) . . ?
O6 Cu1 O2 81.45(17) . . ?
O6 Cu1 O9 89.0(2) . . ?
O9 Cu1 Cu2 88.43(17) . . ?
O2 Cu2 Cu1 41.21(12) . . ?
O2 Cu2 O10 101.8(2) . . ?
O3 Cu2 Cu1 131.83(13) . . ?
O3 Cu2 O2 91.39(17) . . ?
O3 Cu2 O6 169.0(2) . . ?
O3 Cu2 O7 92.36(18) . . ?
O3 Cu2 O10 99.0(2) . . ?
O6 Cu2 Cu1 40.87(12) . . ?
O6 Cu2 O2 82.07(17) . . ?
O6 Cu2 O10 91.0(2) . . ?
O7 Cu2 Cu1 129.36(13) . . ?
O7 Cu2 O2 161.14(19) . . ?
O7 Cu2 O6 91.11(17) . . ?
O7 Cu2 O10 95.9(2) . . ?
O10 Cu2 Cu1 99.13(16) . . ?
C1 O1 Cu1 127.1(4) . . ?
Cu2 O2 Cu1 97.94(17) . . ?
C7 O2 Cu1 129.1(4) . . ?
C7 O2 Cu2 131.7(4) . . ?
C11 O3 Cu2 127.7(4) . . ?
C15 O5 Cu1 128.4(4) . . ?
Cu2 O6 Cu1 98.51(17) . . ?
C21 O6 Cu1 131.4(4) . . ?
C21 O6 Cu2 130.1(4) . . ?
C25 O7 Cu2 126.9(4) . . ?
S1A O9 Cu1 120.1(3) . . ?
S1B O9 Cu1 135.5(6) . . ?
S2A O10 Cu2 148.8(4) . . ?
S2B O10 Cu2 107.1(6) . . ?
O1 C1 C2 116.2(5) . . ?
O1 C1 C6 125.9(5) . . ?
C2 C1 C6 117.8(5) . . ?
C3 C2 C1 122.5(5) . . ?
C2 C3 C4 120.5(5) . . ?
C5 C4 C3 119.9(5) . . ?
C4 C5 C6 122.3(5) . . ?
C4 C5 C10 117.5(5) . . ?
C6 C5 C10 120.3(5) . . ?
C5 C6 C1 117.0(5) . . ?
C7 C6 C1 123.8(5) . . ?
C7 C6 C5 119.2(5) . . ?
O2 C7 C6 119.4(5) . . ?
O2 C7 C8 118.3(5) . . ?
C6 C7 C8 122.4(5) . . ?
C9 C8 C7 118.7(5) . . ?
C11 C8 C7 124.2(5) . . ?
C11 C8 C9 117.1(5) . . ?
C8 C9 C10 120.3(5) . . ?
C14 C9 C8 121.6(5) . . ?
C14 C9 C10 118.1(5) . . ?
O4 C10 C5 121.3(6) . . ?
O4 C10 C9 120.0(5) . . ?
C5 C10 C9 118.7(5) . . ?
O3 C11 C8 125.8(5) . . ?
O3 C11 C12 115.6(5) . . ?
C8 C11 C12 118.7(5) . . ?
C13 C12 C11 122.0(6) . . ?
C12 C13 C14 119.7(5) . . ?
C9 C14 C13 120.7(5) . . ?
O5 C15 C16 116.2(6) . . ?
O5 C15 C20 126.0(5) . . ?
C16 C15 C20 117.8(5) . . ?
C17 C16 C15 122.6(6) . . ?
C16 C17 C18 119.7(6) . . ?
C19 C18 C17 121.0(6) . . ?
C18 C19 C20 121.3(6) . . ?
C18 C19 C24 117.8(5) . . ?
C20 C19 C24 120.9(5) . . ?
C15 C20 C21 123.3(5) . . ?
C19 C20 C15 117.6(5) . . ?
C19 C20 C21 119.0(5) . . ?
O6 C21 C20 118.7(5) . . ?
O6 C21 C22 119.5(5) . . ?
C22 C21 C20 121.8(5) . . ?
C21 C22 C23 119.4(5) . . ?
C25 C22 C21 123.5(5) . . ?
C25 C22 C23 117.0(5) . . ?
C22 C23 C24 120.4(5) . . ?
C28 C23 C22 121.4(5) . . ?
C28 C23 C24 118.3(5) . . ?
O8 C24 C19 121.3(6) . . ?
O8 C24 C23 120.3(6) . . ?
C19 C24 C23 118.3(5) . . ?
O7 C25 C22 125.7(5) . . ?
O7 C25 C26 115.3(5) . . ?
C26 C25 C22 119.0(5) . . ?
C27 C26 C25 122.1(5) . . ?
C26 C27 C28 119.6(5) . . ?
C23 C28 C27 120.8(5) . . ?
O9 S1A C29 111.9(4) . . ?
O9 S1A C30 108.5(4) . . ?
C30 S1A C29 99.8(4) . . ?
O10 S2A C31 106.5(3) . . ?
O10 S2A C32 108.7(4) . . ?
C32 S2A C31 98.1(3) . . ?
O9 S1B C29 121.5(9) . . ?
O9 S1B C30 103.4(6) . . ?
C29 S1B C30 91.7(6) . . ?
O10 S2B C31 108.7(7) . . ?
O10 S2B C32 107.5(7) . . ?
C31 S2B C32 101.5(7) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -1 12 0.0361 0.0158 -1.0166 11.9956 -0.9965 0.0852 -0.0358
5 4 1 0.1011 5.0051 3.9897 0.9841 0.0036 0.3239 -0.9759
0 13 0 0.0988 0.0036 12.9817 0.0336 0.0317 -0.8272 -0.6072
0 -13 0 0.0988 -0.0036 -12.9817 -0.0336 -0.0317 0.8272 0.6072
-5 3 -2 0.0418 -5.0045 3.0019 -1.9658 0.0964 -0.7711 0.6558
0 1 -12 0.0010 -0.0158 1.0166 -11.9956 0.9965 -0.0852 0.0358
-4 -7 -2 0.0921 -4.0068 -6.9846 -1.9969 0.0873 -0.0195 0.9664
5 -6 0 0.1305 5.0010 -5.9947 -0.0416 0.0620 0.9583 -0.5019

####################################################################### 
# 
# 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_FeChrys-1
_database_code_depnum_ccdc_archive 'CCDC 1044033'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2016-01-18
_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         'C34 H28 Fe N2 O10'
_chemical_formula_sum            'C34 H28 Fe N2 O10'
_chemical_formula_weight         680.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Fe2 C34 N2 O10 H26'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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      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_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.0131(4)
_cell_length_b                   8.4169(4)
_cell_length_c                   18.1414(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.448(4)
_cell_angle_gamma                90
_cell_volume                     1503.60(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2527
_cell_measurement_temperature    269.95(10)
_cell_measurement_theta_max      67.4910
_cell_measurement_theta_min      4.7180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.584
_exptl_absorpt_correction_T_max  0.488
_exptl_absorpt_correction_T_min  0.097
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.4481
_exptl_crystal_size_mid          0.2249
_exptl_crystal_size_min          0.1057
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5822
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.438
_diffrn_reflns_theta_max         67.438
_diffrn_reflns_theta_min         4.719
_diffrn_ambient_temperature      269.95(10)
_diffrn_detector_area_resol_mean 16.1183
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -25.00    2.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -      -26.1037  -99.0000  -60.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -96.00  -68.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -      -26.1037 -178.0000   60.0000 28

#__ type_ start__ end____ width___ exp.time_
  3 omega  -13.00   27.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -      -26.1037  -99.0000  -30.0000 40

#__ type_ start__ end____ width___ exp.time_
  4 omega   -8.00   43.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -       26.1037   57.0000  150.0000 51

#__ type_ start__ end____ width___ exp.time_
  5 omega   47.00   93.00   1.0000    1.0900
omega____ theta____ kappa____ phi______ frames
    -       26.1037   57.0000  150.0000 46

#__ type_ start__ end____ width___ exp.time_
  6 omega -154.00 -127.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      -67.8019  -94.0000   30.0000 27

#__ type_ start__ end____ width___ exp.time_
  7 omega  -95.00  -47.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      -67.8019  -61.0000  -60.0000 48

#__ type_ start__ end____ width___ exp.time_
  8 omega -143.00 -102.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      -67.8019  -61.0000  -60.0000 41

#__ type_ start__ end____ width___ exp.time_
  9 omega   88.00  133.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019  111.0000  -60.0000 45

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  136.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019   61.0000  120.0000 97

#__ type_ start__ end____ width___ exp.time_
 11 omega   13.00   81.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019  -94.0000 -120.0000 68

#__ type_ start__ end____ width___ exp.time_
 12 omega  -19.00    7.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019  -94.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 13 omega  -16.00   50.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -       67.8019  -30.0000 -150.0000 66

#__ type_ start__ end____ width___ exp.time_
 14 omega   31.00   56.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   21.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
 15 omega  105.00  131.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000    0.0000 26

#__ type_ start__ end____ width___ exp.time_
 16 omega   31.00   71.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -43.0000  150.0000 40

#__ type_ start__ end____ width___ exp.time_
 17 omega   90.00  119.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
 18 omega  110.00  178.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  104.0000 -180.0000 68

#__ type_ start__ end____ width___ exp.time_
 19 omega   32.00   60.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -43.0000   30.0000 28

#__ type_ start__ end____ width___ exp.time_
 20 omega   74.00  122.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000  -60.0000 48

#__ type_ start__ end____ width___ exp.time_
 21 omega  123.00  150.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -21.0000   90.0000 27

#__ type_ start__ end____ width___ exp.time_
 22 omega   30.00   73.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -43.0000   90.0000 43

#__ type_ start__ end____ width___ exp.time_
 23 omega   36.00   75.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -43.0000 -150.0000 39

#__ type_ start__ end____ width___ exp.time_
 24 omega  125.00  177.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -21.0000  150.0000 52

#__ type_ start__ end____ width___ exp.time_
 25 omega   58.00  152.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -77.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
 26 omega  126.00  167.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000  -30.0000 41

#__ type_ start__ end____ width___ exp.time_
 27 omega  140.00  168.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -32.0000  -90.0000 28

#__ type_ start__ end____ width___ exp.time_
 28 omega  151.00  178.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   65.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
 29 omega   52.00   78.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -104.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 30 omega  121.00  154.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000   21.0000    0.0000 33

#__ type_ start__ end____ width___ exp.time_
 31 omega   48.00   73.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -65.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
 32 omega  144.00  172.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -32.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
 33 omega  116.00  145.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -21.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
 34 omega  133.00  174.00   1.0000    4.3500
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -32.0000   60.0000 41
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1300217000
_diffrn_orient_matrix_UB_12      0.0399622000
_diffrn_orient_matrix_UB_13      -0.0304284000
_diffrn_orient_matrix_UB_21      -0.0696005000
_diffrn_orient_matrix_UB_22      0.1488298000
_diffrn_orient_matrix_UB_23      -0.0387647000
_diffrn_orient_matrix_UB_31      0.0523363000
_diffrn_orient_matrix_UB_32      0.0985416000
_diffrn_orient_matrix_UB_33      0.0709530000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2349
_reflns_number_total             2679
_reflns_odcompleteness_completeness 93.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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       
;
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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2679
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0385
_refine_ls_restrained_S_all      1.039
_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)+(0.0725P)²+0.1511P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1113
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_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
Fe1 Fe 0.5000 0.5000 0.5000 0.04123(18) Uani 1 2 d S T P . .
O1 O 0.45978(14) 0.58276(18) 0.59613(8) 0.0472(4) Uani 1 1 d . . . . .
O2 O 0.30011(13) 0.43370(19) 0.47768(7) 0.0428(3) Uani 1 1 d . . . . .
O3 O 0.16337(18) 0.2729(2) 0.37171(9) 0.0589(4) Uani 1 1 d . . . . .
H3 H 0.232(3) 0.338(4) 0.3971(18) 0.088 Uiso 1 1 d R . . . .
O4 O -0.07364(17) 0.3253(2) 0.65152(9) 0.0630(5) Uani 1 1 d . . . . .
O5 O 0.46745(17) 0.73420(19) 0.44806(9) 0.0539(4) Uani 1 1 d . . . . .
N1 N 0.37694(18) 0.9011(2) 0.35503(10) 0.0469(4) Uani 1 1 d . . . . .
C1 C 0.3659(2) 0.6141(3) 0.70344(11) 0.0476(5) Uani 1 1 d . . . . .
H1 H 0.4426 0.6705 0.7255 0.057 Uiso 1 1 calc R . . . .
C2 C 0.3592(2) 0.5540(3) 0.62944(11) 0.0404(4) Uani 1 1 d . . . . .
C3 C 0.2391(2) 0.4661(2) 0.59740(11) 0.0369(4) Uani 1 1 d . . . . .
C4 C 0.21766(18) 0.4064(2) 0.52187(10) 0.0359(4) Uani 1 1 d . . . . .
C5 C 0.09677(19) 0.3123(2) 0.49228(11) 0.0377(4) Uani 1 1 d . . . . .
C6 C 0.0763(2) 0.2476(3) 0.41919(12) 0.0438(5) Uani 1 1 d . . . . .
C7 C -0.0376(2) 0.1556(3) 0.39298(13) 0.0534(5) Uani 1 1 d . . . . .
H7 H -0.0497 0.1130 0.3449 0.064 Uiso 1 1 calc R . . . .
C8 C -0.1321(2) 0.1271(3) 0.43720(14) 0.0559(6) Uani 1 1 d . . . . .
H8 H -0.2079 0.0654 0.4189 0.067 Uiso 1 1 calc R . . . .
C9 C -0.1160(2) 0.1891(3) 0.50889(13) 0.0498(5) Uani 1 1 d . . . . .
H9 H -0.1808 0.1695 0.5385 0.060 Uiso 1 1 calc R . . . .
C10 C -0.00266(19) 0.2809(2) 0.53637(11) 0.0400(4) Uani 1 1 d . . . . .
C11 C 0.0127(2) 0.3485(3) 0.61290(11) 0.0440(5) Uani 1 1 d . . . . .
C12 C 0.1364(2) 0.4424(3) 0.64154(11) 0.0396(4) Uani 1 1 d . . . . .
C13 C 0.1482(3) 0.5056(3) 0.71242(13) 0.0484(5) Uani 1 1 d . . . . .
H13 H 0.0793 0.4907 0.7399 0.058 Uiso 1 1 calc R . . . .
C14 C 0.2641(2) 0.5920(3) 0.74296(12) 0.0517(5) Uani 1 1 d . . . . .
H14 H 0.2718 0.6348 0.7908 0.062 Uiso 1 1 calc R . . . .
C15 C 0.3943(2) 0.7596(3) 0.38661(12) 0.0477(5) Uani 1 1 d . . . . .
H15 H 0.3488 0.6739 0.3611 0.057 Uiso 1 1 calc R . . . .
C16 C 0.4464(3) 1.0375(3) 0.39242(18) 0.0725(8) Uani 1 1 d . . . . .
H16A H 0.3956 1.0782 0.4284 0.109 Uiso 1 1 calc GR . . . .
H16B H 0.4543 1.1183 0.3561 0.109 Uiso 1 1 calc GR . . . .
H16C H 0.5353 1.0066 0.4176 0.109 Uiso 1 1 calc GR . . . .
C17 C 0.2791(3) 0.9274(4) 0.28627(13) 0.0619(6) Uani 1 1 d . . . . .
H17A H 0.3233 0.9789 0.2500 0.093 Uiso 1 1 calc GR . . . .
H17B H 0.2067 0.9935 0.2968 0.093 Uiso 1 1 calc GR . . . .
H17C H 0.2429 0.8273 0.2667 0.093 Uiso 1 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
Fe1 O1 1.9857(14) . ?
Fe1 O1 1.9858(15) 3_666 ?
Fe1 O2 2.0464(13) . ?
Fe1 O2 2.0464(13) 3_666 ?
Fe1 O5 2.1837(16) . ?
Fe1 O5 2.1837(16) 3_666 ?
O1 C2 1.288(2) . ?
O2 C4 1.272(2) . ?
O3 H3 0.93(3) . ?
O3 C6 1.349(3) . ?
O4 C11 1.223(2) . ?
O5 C15 1.237(3) . ?
N1 C15 1.319(3) . ?
N1 C16 1.446(3) . ?
N1 C17 1.457(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.425(3) . ?
C1 C14 1.362(3) . ?
C2 C3 1.441(3) . ?
C3 C4 1.439(3) . ?
C3 C12 1.428(3) . ?
C4 C5 1.464(3) . ?
C5 C6 1.414(3) . ?
C5 C10 1.411(3) . ?
C6 C7 1.389(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.368(3) . ?
C8 H8 0.9300 . ?
C8 C9 1.384(3) . ?
C9 H9 0.9300 . ?
C9 C10 1.388(3) . ?
C10 C11 1.482(3) . ?
C11 C12 1.482(3) . ?
C12 C13 1.377(3) . ?
C13 H13 0.9300 . ?
C13 C14 1.396(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 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
O1 Fe1 O1 180.0 . 3_666 ?
O1 Fe1 O2 85.56(6) 3_666 3_666 ?
O1 Fe1 O2 85.56(6) . . ?
O1 Fe1 O2 94.44(6) 3_666 . ?
O1 Fe1 O2 94.44(6) . 3_666 ?
O1 Fe1 O5 88.62(6) 3_666 . ?
O1 Fe1 O5 88.62(6) . 3_666 ?
O1 Fe1 O5 91.38(6) . . ?
O1 Fe1 O5 91.38(6) 3_666 3_666 ?
O2 Fe1 O2 180.0 . 3_666 ?
O2 Fe1 O5 95.55(6) . . ?
O2 Fe1 O5 84.45(6) . 3_666 ?
O2 Fe1 O5 84.45(6) 3_666 . ?
O2 Fe1 O5 95.55(6) 3_666 3_666 ?
O5 Fe1 O5 180.0 . 3_666 ?
C2 O1 Fe1 130.27(14) . . ?
C4 O2 Fe1 130.39(12) . . ?
C6 O3 H3 106(2) . . ?
C15 O5 Fe1 124.26(15) . . ?
C15 N1 C16 119.9(2) . . ?
C15 N1 C17 121.6(2) . . ?
C16 N1 C17 118.2(2) . . ?
C2 C1 H1 118.8 . . ?
C14 C1 H1 118.8 . . ?
C14 C1 C2 122.4(2) . . ?
O1 C2 C1 117.89(19) . . ?
O1 C2 C3 124.99(19) . . ?
C1 C2 C3 117.12(18) . . ?
C4 C3 C2 122.22(18) . . ?
C12 C3 C2 118.61(18) . . ?
C12 C3 C4 119.14(18) . . ?
O2 C4 C3 122.37(18) . . ?
O2 C4 C5 117.04(17) . . ?
C3 C4 C5 120.59(17) . . ?
C6 C5 C4 121.46(18) . . ?
C10 C5 C4 120.99(18) . . ?
C10 C5 C6 117.54(18) . . ?
O3 C6 C5 122.51(19) . . ?
O3 C6 C7 117.1(2) . . ?
C7 C6 C5 120.4(2) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.6(2) . . ?
C8 C7 H7 119.7 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.7(2) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 120.1 . . ?
C8 C9 C10 119.7(2) . . ?
C10 C9 H9 120.1 . . ?
C5 C10 C11 119.68(18) . . ?
C9 C10 C5 121.0(2) . . ?
C9 C10 C11 119.27(19) . . ?
O4 C11 C10 120.7(2) . . ?
O4 C11 C12 121.1(2) . . ?
C12 C11 C10 118.11(17) . . ?
C3 C12 C11 121.31(18) . . ?
C13 C12 C3 121.40(19) . . ?
C13 C12 C11 117.29(19) . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.8(2) . . ?
C14 C13 H13 120.1 . . ?
C1 C14 C13 120.7(2) . . ?
C1 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
O5 C15 N1 123.9(2) . . ?
O5 C15 H15 118.1 . . ?
N1 C15 H15 118.1 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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
Fe1 O1 C2 C1 171.63(14) . . . . ?
Fe1 O1 C2 C3 -8.8(3) . . . . ?
Fe1 O2 C4 C3 20.5(3) . . . . ?
Fe1 O2 C4 C5 -160.43(13) . . . . ?
Fe1 O5 C15 N1 -178.82(15) . . . . ?
O1 C2 C3 C4 -2.7(3) . . . . ?
O1 C2 C3 C12 179.37(19) . . . . ?
O2 C4 C5 C6 3.3(3) . . . . ?
O2 C4 C5 C10 -177.74(17) . . . . ?
O3 C6 C7 C8 -178.7(2) . . . . ?
O4 C11 C12 C3 178.3(2) . . . . ?
O4 C11 C12 C13 -1.7(3) . . . . ?
C1 C2 C3 C4 176.85(18) . . . . ?
C1 C2 C3 C12 -1.1(3) . . . . ?
C2 C1 C14 C13 1.2(4) . . . . ?
C2 C3 C4 O2 -3.3(3) . . . . ?
C2 C3 C4 C5 177.63(18) . . . . ?
C2 C3 C12 C11 -177.93(18) . . . . ?
C2 C3 C12 C13 2.0(3) . . . . ?
C3 C4 C5 C6 -177.60(18) . . . . ?
C3 C4 C5 C10 1.4(3) . . . . ?
C3 C12 C13 C14 -1.4(3) . . . . ?
C4 C3 C12 C11 4.1(3) . . . . ?
C4 C3 C12 C13 -175.94(18) . . . . ?
C4 C5 C6 O3 -2.4(3) . . . . ?
C4 C5 C6 C7 178.48(19) . . . . ?
C4 C5 C10 C9 -178.74(19) . . . . ?
C4 C5 C10 C11 2.1(3) . . . . ?
C5 C6 C7 C8 0.4(3) . . . . ?
C5 C10 C11 O4 178.6(2) . . . . ?
C5 C10 C11 C12 -2.5(3) . . . . ?
C6 C5 C10 C9 0.3(3) . . . . ?
C6 C5 C10 C11 -178.86(17) . . . . ?
C6 C7 C8 C9 -0.1(4) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C8 C9 C10 C5 0.1(3) . . . . ?
C8 C9 C10 C11 179.2(2) . . . . ?
C9 C10 C11 O4 -0.5(3) . . . . ?
C9 C10 C11 C12 178.40(19) . . . . ?
C10 C5 C6 O3 178.57(19) . . . . ?
C10 C5 C6 C7 -0.5(3) . . . . ?
C10 C11 C12 C3 -0.7(3) . . . . ?
C10 C11 C12 C13 179.37(18) . . . . ?
C11 C12 C13 C14 178.5(2) . . . . ?
C12 C3 C4 O2 174.58(18) . . . . ?
C12 C3 C4 C5 -4.5(3) . . . . ?
C12 C13 C14 C1 -0.2(3) . . . . ?
C14 C1 C2 O1 179.1(2) . . . . ?
C14 C1 C2 C3 -0.5(3) . . . . ?
C16 N1 C15 O5 0.4(3) . . . . ?
C17 N1 C15 O5 -173.7(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6 0 -5 0.0639 5.9968 -0.0030 -4.9794 0.9311 -0.2248 -0.0398
-6 0 5 0.0639 -5.9968 0.0030 4.9794 -0.9311 0.2248 0.0398
-6 0 6 0.0529 -5.9974 0.0026 5.9790 -0.9616 0.1860 0.1106
6 0 -6 0.0529 5.9974 -0.0026 -5.9790 0.9616 -0.1860 -0.1106
-1 5 -5 0.1824 -0.9979 5.0015 -5.0042 0.2224 1.0078 0.0856
1 -5 5 0.1824 0.9979 -5.0015 5.0042 -0.2224 -1.0078 -0.0856
2 0 11 0.0928 1.9909 -0.0060 11.0019 -0.0762 -0.5659 0.8842
0 5 5 0.2135 -0.0054 4.9967 4.9950 0.0470 0.5504 0.8465
0 -5 -5 0.2084 0.0054 -4.9967 -4.9950 -0.0470 -0.5504 -0.8465
-2 0 -10 0.1355 -1.9915 0.0056 -10.0023 0.0456 0.5272 -0.8134
6 1 -2 0.0716 5.9944 0.9955 -1.9812 0.8795 -0.1923 0.2713
-5 0 -5 0.0865 -4.9915 0.0061 -5.0136 -0.4962 0.5427 -0.6164
5 0 6 0.0662 4.9909 -0.0065 6.0132 0.4657 -0.5814 0.6872



####################################################################### 
# 
# 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_FeChrys-2
_database_code_depnum_ccdc_archive 'CCDC 1044034'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-08-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2014/6
_chemical_name_systematic        
'tri(chrysazinato)-di-iron(III) N,N-dimethylformamide solvate hemihydrate'
_chemical_formula_moiety         'C42 H18 Fe2 O12, C3 H7 N O, 0.5(H2 O)'
_chemical_formula_sum            'C45 H26 Fe2 N O13.50'
_chemical_formula_weight         908.37
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Fe2 C44 O13 H27 N1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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                   8.2927(4)
_cell_length_b                   15.5166(7)
_cell_length_c                   15.8042(6)
_cell_angle_alpha                118.226(4)
_cell_angle_beta                 92.344(4)
_cell_angle_gamma                92.239(4)
_cell_volume                     1786.33(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5616
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.6870
_cell_measurement_theta_min      3.2540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.204
_exptl_absorpt_correction_T_max  0.771
_exptl_absorpt_correction_T_min  0.263
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.3238
_exptl_crystal_size_mid          0.0487
_exptl_crystal_size_min          0.0427
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14065
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.700
_diffrn_reflns_theta_min         3.181
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0591
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9882
_diffrn_measured_fraction_theta_max 0.9851
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1784130000
_diffrn_orient_matrix_UB_12      -0.0101395000
_diffrn_orient_matrix_UB_13      0.0229301000
_diffrn_orient_matrix_UB_21      -0.0299355000
_diffrn_orient_matrix_UB_22      -0.1124197000
_diffrn_orient_matrix_UB_23      -0.0519776000
_diffrn_orient_matrix_UB_31      0.0446684000
_diffrn_orient_matrix_UB_32      -0.0035848000
_diffrn_orient_matrix_UB_33      -0.0952276000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5430
_reflns_number_total             6352
_reflns_odcompleteness_completeness 98.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         1.775
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         6352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0516
_refine_ls_restrained_S_all      1.022
_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)+(0.0740P)²+3.5751P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1440
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C41(H41),
  C42(H42), C43(H43), C1S(H1S)
3.c Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
;
_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
Fe1 Fe 1.07274(7) 0.32467(4) 0.66867(4) 0.02485(16) Uani 1 1 d . . . . .
Fe2 Fe 0.69155(7) 0.31564(4) 0.65434(4) 0.02501(16) Uani 1 1 d . . . . .
O1 O 1.1763(3) 0.3821(2) 0.60050(19) 0.0304(6) Uani 1 1 d . . . . .
O2 O 0.8856(3) 0.41224(19) 0.66325(18) 0.0284(6) Uani 1 1 d . . . . .
O3 O 0.5937(3) 0.4358(2) 0.72446(18) 0.0315(6) Uani 1 1 d . . . . .
O4 O 0.9050(4) 0.7630(2) 0.6716(3) 0.0498(8) Uani 1 1 d . . . . .
O5 O 1.1791(3) 0.3943(2) 0.79309(18) 0.0300(6) Uani 1 1 d . . . . .
O6 O 0.8802(3) 0.3145(2) 0.74851(18) 0.0288(6) Uani 1 1 d . . . . .
O7 O 0.5803(3) 0.24046(19) 0.70196(18) 0.0286(6) Uani 1 1 d . . . . .
O8 O 0.8467(4) 0.3467(2) 1.10201(19) 0.0392(7) Uani 1 1 d . . . . .
O9 O 1.1688(3) 0.20290(19) 0.62010(18) 0.0292(6) Uani 1 1 d . . . . .
O10 O 0.8786(3) 0.23324(19) 0.57297(17) 0.0275(6) Uani 1 1 d . . . . .
O11 O 0.5829(3) 0.2651(2) 0.53115(18) 0.0300(6) Uani 1 1 d . . . . .
O12 O 0.8928(4) -0.0749(2) 0.2183(2) 0.0417(7) Uani 1 1 d . . . . .
C1 C 0.4937(5) 0.5887(3) 0.7709(3) 0.0357(9) Uani 1 1 d . . . . .
H1 H 0.4040 0.5696 0.7929 0.043 Uiso 1 1 calc R U . . .
C2 C 0.5067(6) 0.6802(3) 0.7794(3) 0.0401(10) Uani 1 1 d . . . . .
H2 H 0.4260 0.7229 0.8076 0.048 Uiso 1 1 calc R U . . .
C3 C 0.6395(6) 0.7112(3) 0.7463(3) 0.0400(10) Uani 1 1 d . . . . .
H3 H 0.6460 0.7738 0.7522 0.048 Uiso 1 1 calc R U . . .
C4 C 0.7603(5) 0.6492(3) 0.7052(3) 0.0321(9) Uani 1 1 d . . . . .
C5 C 0.7531(5) 0.5543(3) 0.6974(2) 0.0272(8) Uani 1 1 d . . . . .
C6 C 0.6152(5) 0.5223(3) 0.7288(2) 0.0297(8) Uani 1 1 d . . . . .
C7 C 0.8898(4) 0.4951(3) 0.6651(2) 0.0256(8) Uani 1 1 d . . . . .
C8 C 0.8999(5) 0.6830(3) 0.6700(3) 0.0356(9) Uani 1 1 d . . . . .
C9 C 1.0350(5) 0.6176(3) 0.6333(3) 0.0313(8) Uani 1 1 d . . . . .
C10 C 1.0317(5) 0.5266(3) 0.6348(2) 0.0264(8) Uani 1 1 d . . . . .
C11 C 1.1629(5) 0.4654(3) 0.5997(3) 0.0278(8) Uani 1 1 d . . . . .
C12 C 1.2886(5) 0.4960(3) 0.5596(3) 0.0338(9) Uani 1 1 d . . . . .
H12 H 1.3726 0.4555 0.5331 0.041 Uiso 1 1 calc R U . . .
C13 C 1.2884(5) 0.5841(3) 0.5594(3) 0.0377(10) Uani 1 1 d . . . . .
H13 H 1.3733 0.6031 0.5339 0.045 Uiso 1 1 calc R U . . .
C14 C 1.1628(5) 0.6458(3) 0.5967(3) 0.0375(9) Uani 1 1 d . . . . .
H14 H 1.1652 0.7059 0.5969 0.045 Uiso 1 1 calc R U . . .
C15 C 1.2805(5) -0.0181(3) 0.4199(3) 0.0368(9) Uani 1 1 d . . . . .
H15 H 1.3653 -0.0592 0.4053 0.044 Uiso 1 1 calc R U . . .
C16 C 1.2826(5) 0.0633(3) 0.5088(3) 0.0330(9) Uani 1 1 d . . . . .
H16 H 1.3697 0.0770 0.5532 0.040 Uiso 1 1 calc R U . . .
C17 C 1.1518(5) -0.0401(3) 0.3508(3) 0.0335(9) Uani 1 1 d . . . . .
H17 H 1.1531 -0.0944 0.2903 0.040 Uiso 1 1 calc R U . . .
C18 C 1.0236(5) 0.0191(3) 0.3730(3) 0.0278(8) Uani 1 1 d . . . . .
C19 C 1.0220(4) 0.1031(3) 0.4652(3) 0.0245(7) Uani 1 1 d . . . . .
C20 C 1.1544(4) 0.1265(3) 0.5337(3) 0.0271(8) Uani 1 1 d . . . . .
C21 C 0.8797(4) 0.1589(3) 0.4893(2) 0.0235(7) Uani 1 1 d . . . . .
C22 C 0.7394(4) 0.1325(3) 0.4232(2) 0.0226(7) Uani 1 1 d . . . . .
C23 C 0.7433(5) 0.0530(3) 0.3287(3) 0.0271(8) Uani 1 1 d . . . . .
C24 C 0.8868(5) -0.0062(3) 0.2996(3) 0.0303(8) Uani 1 1 d . . . . .
C25 C 0.6154(5) 0.0301(3) 0.2616(3) 0.0324(9) Uani 1 1 d . . . . .
H25 H 0.6211 -0.0208 0.1994 0.039 Uiso 1 1 calc R U . . .
C26 C 0.4773(5) 0.0831(3) 0.2867(3) 0.0346(9) Uani 1 1 d . . . . .
H26 H 0.3901 0.0663 0.2417 0.042 Uiso 1 1 calc R U . . .
C27 C 0.4697(5) 0.1601(3) 0.3778(3) 0.0307(8) Uani 1 1 d . . . . .
H27 H 0.3767 0.1945 0.3935 0.037 Uiso 1 1 calc R U . . .
C28 C 0.5993(5) 0.1880(3) 0.4479(3) 0.0261(8) Uani 1 1 d . . . . .
C29 C 1.1567(4) 0.3981(3) 0.8764(3) 0.0259(7) Uani 1 1 d . . . . .
C30 C 1.2837(5) 0.4432(3) 0.9489(3) 0.0296(8) Uani 1 1 d . . . . .
H30 H 1.3772 0.4682 0.9355 0.035 Uiso 1 1 calc R U . . .
C31 C 1.2725(5) 0.4509(3) 1.0384(3) 0.0321(9) Uani 1 1 d . . . . .
H31 H 1.3585 0.4802 1.0845 0.039 Uiso 1 1 calc R U . . .
C32 C 1.1319(5) 0.4148(3) 1.0613(3) 0.0315(8) Uani 1 1 d . . . . .
H32 H 1.1250 0.4203 1.1222 0.038 Uiso 1 1 calc R U . . .
C33 C 1.0044(5) 0.3714(3) 0.9931(3) 0.0273(8) Uani 1 1 d . . . . .
C34 C 1.0135(4) 0.3617(3) 0.8997(2) 0.0242(7) Uani 1 1 d . . . . .
C35 C 0.8728(4) 0.3216(3) 0.8321(2) 0.0239(7) Uani 1 1 d . . . . .
C36 C 0.8544(5) 0.3387(3) 1.0216(3) 0.0294(8) Uani 1 1 d . . . . .
C37 C 0.7143(5) 0.2968(3) 0.9492(3) 0.0253(7) Uani 1 1 d . . . . .
C38 C 0.7247(4) 0.2908(3) 0.8567(2) 0.0227(7) Uani 1 1 d . . . . .
C39 C 0.5864(4) 0.2511(3) 0.7895(3) 0.0247(7) Uani 1 1 d . . . . .
C41 C 0.4461(5) 0.2188(3) 0.8171(3) 0.0276(8) Uani 1 1 d . . . . .
H41 H 0.3554 0.1929 0.7741 0.033 Uiso 1 1 calc R U . . .
C42 C 0.5758(5) 0.2637(3) 0.9725(3) 0.0316(8) Uani 1 1 d . . . . .
H42 H 0.5714 0.2671 1.0327 0.038 Uiso 1 1 calc R U . . .
C43 C 0.4418(5) 0.2251(3) 0.9066(3) 0.0316(8) Uani 1 1 d . . . . .
H43 H 0.3484 0.2033 0.9234 0.038 Uiso 1 1 calc R U . . .
O1S O 0.7090(7) 0.0232(5) 0.9219(3) 0.129(3) Uani 1 1 d . . . . .
N1S N 0.9238(6) 0.1132(4) 1.0279(3) 0.0644(13) Uani 1 1 d . . . . .
C1S C 0.8391(9) 0.0699(5) 0.9414(4) 0.0729(18) Uani 1 1 d . . . . .
H1S H 0.8848 0.0765 0.8918 0.088 Uiso 1 1 calc R U . . .
C2S C 0.8582(8) 0.1286(5) 1.1154(4) 0.0700(17) Uani 1 1 d . . . . .
H2SA H 0.8467 0.1974 1.1554 0.105 Uiso 1 1 calc R U . . .
H2SB H 0.9294 0.1053 1.1484 0.105 Uiso 1 1 calc R U . . .
H2SC H 0.7542 0.0937 1.1015 0.105 Uiso 1 1 calc R U . . .
C3S C 1.0907(7) 0.1547(4) 1.0366(5) 0.0635(15) Uani 1 1 d . . . . .
H3SA H 1.1619 0.1273 1.0657 0.095 Uiso 1 1 calc R U . . .
H3SB H 1.0944 0.2246 1.0760 0.095 Uiso 1 1 calc R U . . .
H3SC H 1.1242 0.1392 0.9738 0.095 Uiso 1 1 calc R U . . .
O1W O 0.4693(13) 0.0841(8) 1.0116(9) 0.090(3) Uani 0.5 1 d G . P . .
H1WA H 0.5574 0.0593 1.0147 0.135 Uiso 0.5 1 d G U P . .
H1WB H 0.3919 0.0548 1.0235 0.135 Uiso 0.5 1 d G U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.902(3) . ?
Fe1 O2 2.128(3) . ?
Fe1 O5 1.894(3) . ?
Fe1 O6 2.121(3) . ?
Fe1 O9 1.895(3) . ?
Fe1 O10 2.118(3) . ?
Fe2 O2 2.109(3) . ?
Fe2 O3 1.898(3) . ?
Fe2 O6 2.121(3) . ?
Fe2 O7 1.892(3) . ?
Fe2 O10 2.111(3) . ?
Fe2 O11 1.891(3) . ?
O1 C11 1.308(5) . ?
O2 C7 1.272(5) . ?
O3 C6 1.316(5) . ?
O4 C8 1.230(5) . ?
O5 C29 1.312(4) . ?
O6 C35 1.277(4) . ?
O7 C39 1.311(4) . ?
O8 C36 1.221(5) . ?
O9 C20 1.314(5) . ?
O10 C21 1.280(4) . ?
O11 C28 1.311(5) . ?
O12 C24 1.226(5) . ?
C1 C2 1.360(6) . ?
C1 C6 1.417(5) . ?
C2 C3 1.400(7) . ?
C3 C4 1.374(6) . ?
C4 C5 1.417(6) . ?
C4 C8 1.486(6) . ?
C5 C6 1.427(5) . ?
C5 C7 1.440(5) . ?
C7 C10 1.440(5) . ?
C8 C9 1.485(6) . ?
C9 C10 1.422(5) . ?
C9 C14 1.380(6) . ?
C10 C11 1.423(5) . ?
C11 C12 1.418(5) . ?
C12 C13 1.370(6) . ?
C13 C14 1.393(6) . ?
C15 C16 1.374(6) . ?
C15 C17 1.404(6) . ?
C16 C20 1.414(5) . ?
C17 C18 1.378(5) . ?
C18 C19 1.425(5) . ?
C18 C24 1.488(5) . ?
C19 C20 1.418(5) . ?
C19 C21 1.446(5) . ?
C21 C22 1.440(5) . ?
C22 C23 1.421(5) . ?
C22 C28 1.428(5) . ?
C23 C24 1.484(6) . ?
C23 C25 1.377(5) . ?
C25 C26 1.396(6) . ?
C26 C27 1.375(6) . ?
C27 C28 1.408(5) . ?
C29 C30 1.413(5) . ?
C29 C34 1.429(5) . ?
C30 C31 1.370(6) . ?
C31 C32 1.406(6) . ?
C32 C33 1.378(5) . ?
C33 C34 1.416(5) . ?
C33 C36 1.491(5) . ?
C34 C35 1.449(5) . ?
C35 C38 1.434(5) . ?
C36 C37 1.487(5) . ?
C37 C38 1.426(5) . ?
C37 C42 1.373(5) . ?
C38 C39 1.432(5) . ?
C39 C41 1.414(5) . ?
C41 C43 1.372(5) . ?
C42 C43 1.394(6) . ?
O1S C1S 1.218(8) . ?
N1S C1S 1.353(8) . ?
N1S C2S 1.423(7) . ?
N1S C3S 1.476(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
O1 Fe1 O2 80.88(11) . . ?
O1 Fe1 O6 151.26(11) . . ?
O1 Fe1 O10 104.63(11) . . ?
O5 Fe1 O1 102.38(12) . . ?
O5 Fe1 O2 106.47(11) . . ?
O5 Fe1 O6 82.01(10) . . ?
O5 Fe1 O9 101.32(11) . . ?
O5 Fe1 O10 151.80(11) . . ?
O6 Fe1 O2 70.74(10) . . ?
O9 Fe1 O1 101.42(12) . . ?
O9 Fe1 O2 150.96(11) . . ?
O9 Fe1 O6 105.55(11) . . ?
O9 Fe1 O10 81.17(10) . . ?
O10 Fe1 O2 70.37(10) . . ?
O10 Fe1 O6 70.41(10) . . ?
O2 Fe2 O6 71.10(10) . . ?
O2 Fe2 O10 70.86(10) . . ?
O3 Fe2 O2 81.41(11) . . ?
O3 Fe2 O6 105.74(11) . . ?
O3 Fe2 O10 151.79(12) . . ?
O7 Fe2 O2 151.24(11) . . ?
O7 Fe2 O3 98.78(12) . . ?
O7 Fe2 O6 81.34(10) . . ?
O7 Fe2 O10 107.97(11) . . ?
O10 Fe2 O6 70.55(10) . . ?
O11 Fe2 O2 107.99(11) . . ?
O11 Fe2 O3 101.96(12) . . ?
O11 Fe2 O6 151.70(11) . . ?
O11 Fe2 O7 100.14(12) . . ?
O11 Fe2 O10 82.32(10) . . ?
C11 O1 Fe1 132.8(2) . . ?
Fe2 O2 Fe1 96.17(11) . . ?
C7 O2 Fe1 131.8(2) . . ?
C7 O2 Fe2 132.1(2) . . ?
C6 O3 Fe2 132.7(2) . . ?
C29 O5 Fe1 134.3(2) . . ?
Fe2 O6 Fe1 96.01(10) . . ?
C35 O6 Fe1 133.8(2) . . ?
C35 O6 Fe2 129.3(2) . . ?
C39 O7 Fe2 129.1(2) . . ?
C20 O9 Fe1 130.3(2) . . ?
Fe2 O10 Fe1 96.41(10) . . ?
C21 O10 Fe1 130.2(2) . . ?
C21 O10 Fe2 133.0(2) . . ?
C28 O11 Fe2 133.7(2) . . ?
C2 C1 C6 120.8(4) . . ?
C1 C2 C3 121.1(4) . . ?
C4 C3 C2 120.0(4) . . ?
C3 C4 C5 120.5(4) . . ?
C3 C4 C8 119.4(4) . . ?
C5 C4 C8 120.1(4) . . ?
C4 C5 C6 119.1(4) . . ?
C4 C5 C7 119.5(4) . . ?
C6 C5 C7 121.3(3) . . ?
O3 C6 C1 116.7(4) . . ?
O3 C6 C5 124.8(3) . . ?
C1 C6 C5 118.5(4) . . ?
O2 C7 C5 119.0(3) . . ?
O2 C7 C10 118.7(3) . . ?
C5 C7 C10 122.3(3) . . ?
O4 C8 C4 121.3(4) . . ?
O4 C8 C9 120.5(4) . . ?
C9 C8 C4 118.2(4) . . ?
C10 C9 C8 120.5(4) . . ?
C14 C9 C8 119.1(4) . . ?
C14 C9 C10 120.5(4) . . ?
C9 C10 C7 119.0(3) . . ?
C9 C10 C11 119.4(4) . . ?
C11 C10 C7 121.4(3) . . ?
O1 C11 C10 125.0(3) . . ?
O1 C11 C12 117.0(4) . . ?
C12 C11 C10 118.0(4) . . ?
C13 C12 C11 121.1(4) . . ?
C12 C13 C14 121.0(4) . . ?
C9 C14 C13 119.9(4) . . ?
C16 C15 C17 120.9(4) . . ?
C15 C16 C20 121.0(4) . . ?
C18 C17 C15 119.8(4) . . ?
C17 C18 C19 120.3(4) . . ?
C17 C18 C24 119.1(4) . . ?
C19 C18 C24 120.5(3) . . ?
C18 C19 C21 119.0(3) . . ?
C20 C19 C18 119.6(3) . . ?
C20 C19 C21 121.2(3) . . ?
O9 C20 C16 116.3(3) . . ?
O9 C20 C19 125.4(3) . . ?
C16 C20 C19 118.4(4) . . ?
O10 C21 C19 118.5(3) . . ?
O10 C21 C22 119.3(3) . . ?
C22 C21 C19 122.2(3) . . ?
C23 C22 C21 119.4(3) . . ?
C23 C22 C28 118.7(3) . . ?
C28 C22 C21 121.7(3) . . ?
C22 C23 C24 120.6(3) . . ?
C25 C23 C22 120.9(4) . . ?
C25 C23 C24 118.5(3) . . ?
O12 C24 C18 120.5(4) . . ?
O12 C24 C23 121.6(4) . . ?
C23 C24 C18 117.9(3) . . ?
C23 C25 C26 120.2(4) . . ?
C27 C26 C25 120.3(4) . . ?
C26 C27 C28 121.6(4) . . ?
O11 C28 C22 124.8(3) . . ?
O11 C28 C27 116.8(3) . . ?
C27 C28 C22 118.3(3) . . ?
O5 C29 C30 116.9(3) . . ?
O5 C29 C34 125.1(3) . . ?
C30 C29 C34 117.9(3) . . ?
C31 C30 C29 121.6(4) . . ?
C30 C31 C32 120.6(4) . . ?
C33 C32 C31 119.7(4) . . ?
C32 C33 C34 120.9(4) . . ?
C32 C33 C36 118.1(3) . . ?
C34 C33 C36 121.0(3) . . ?
C29 C34 C35 121.4(3) . . ?
C33 C34 C29 119.3(3) . . ?
C33 C34 C35 119.1(3) . . ?
O6 C35 C34 119.1(3) . . ?
O6 C35 C38 118.9(3) . . ?
C38 C35 C34 122.0(3) . . ?
O8 C36 C33 121.0(4) . . ?
O8 C36 C37 121.2(4) . . ?
C37 C36 C33 117.7(3) . . ?
C38 C37 C36 120.2(3) . . ?
C42 C37 C36 119.1(3) . . ?
C42 C37 C38 120.7(4) . . ?
C37 C38 C35 119.9(3) . . ?
C37 C38 C39 118.4(3) . . ?
C39 C38 C35 121.7(3) . . ?
O7 C39 C38 124.6(3) . . ?
O7 C39 C41 116.6(3) . . ?
C41 C39 C38 118.7(3) . . ?
C43 C41 C39 120.9(4) . . ?
C37 C42 C43 120.5(4) . . ?
C41 C43 C42 120.7(4) . . ?
C1S N1S C2S 123.9(6) . . ?
C1S N1S C3S 119.9(5) . . ?
C2S N1S C3S 116.0(5) . . ?
O1S C1S N1S 126.5(6) . . ?


loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 5 -10 0.0244 -0.0010 4.9950 -9.9974 -0.2801 -0.0419 0.9341
0 -5 10 0.0244 0.0010 -4.9950 9.9974 0.2801 0.0419 -0.9341
-5 1 0 0.1488 -4.9997 0.9969 0.0037 -0.9020 0.0374 -0.2273
5 0 0 0.1691 4.9989 0.0028 -0.0036 0.8918 -0.1498 0.2236
0 10 -2 0.0160 -0.0074 9.9964 -1.9985 -0.1485 -1.0197 0.1541
0 -9 0 0.0246 0.0072 -8.9974 -0.0010 0.0925 1.0113 0.0327
0 2 8 0.0187 -0.0040 2.0023 7.9986 0.1624 -0.6407 -0.7690

_vrf_PLAT415_FeChrys-2           
;
RESPONSE:
Half-occupied hydrogen on water close to hydrogen (modelled without disorder) on DMF, whilst hydrogen-bonding to oxygen on DMF.
;

####################################################################### 
# 
# 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_NiChrys-1
_database_code_depnum_ccdc_archive 'CCDC 1044035'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2016-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        
'dodeca(acetato)-hexa(chrysazinato)-hexa(N,N-dimethylformamide)-tetra-cobalt(II) N,N-dimethylformamide solvate'
_chemical_formula_moiety         'C126 H114 N6 Ni12 O54'
_chemical_formula_sum            'C144 H156 N12 Ni12 O60'
_chemical_formula_weight         3719.32
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni12 C141 H149 N11 O59'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   28.6809(7)
_cell_length_b                   28.6809(7)
_cell_length_c                   15.8967(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     11324.6(6)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    13246
_cell_measurement_temperature    120.10(14)
_cell_measurement_theta_max      70.8420
_cell_measurement_theta_min      4.5080
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.397
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             5760
_exptl_crystal_size_max          0.1868
_exptl_crystal_size_mid          0.1394
_exptl_crystal_size_min          0.0789
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29190
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.154
_diffrn_reflns_theta_min         3.301
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.10(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9941
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0300452000
_diffrn_orient_matrix_UB_12      -0.0619515000
_diffrn_orient_matrix_UB_13      0.0039501000
_diffrn_orient_matrix_UB_21      0.0396946000
_diffrn_orient_matrix_UB_22      -0.0008731000
_diffrn_orient_matrix_UB_23      -0.0644751000
_diffrn_orient_matrix_UB_31      0.0369773000
_diffrn_orient_matrix_UB_32      0.0026244000
_diffrn_orient_matrix_UB_33      0.0723068000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4425
_reflns_number_total             4851
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4851
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0291
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0482P)²+13.7597P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0847
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C19(H19)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.68003(2) 0.13040(2) 0.33965(2) 0.02772(9) Uani 1 1 d . . . . .
Ni2 Ni 0.77796(2) 0.23921(2) 0.35523(2) 0.02740(9) Uani 1 1 d . . . . .
O1 O 0.71311(5) 0.18962(5) 0.42734(7) 0.0293(3) Uani 1 1 d . . . . .
O2 O 0.61096(5) 0.11004(4) 0.40221(7) 0.0283(2) Uani 1 1 d . . . . .
O3 O 0.50474(5) 0.08161(5) 0.37768(8) 0.0305(3) Uani 1 1 d . . . . .
O4 O 0.57924(8) 0.08016(8) 0.73199(10) 0.0740(6) Uani 1 1 d . . . . .
O5 O 0.65273(4) 0.17383(4) 0.27005(7) 0.0276(2) Uani 1 1 d . . . . .
O6 O 0.72732(5) 0.25434(5) 0.28133(8) 0.0301(3) Uani 1 1 d . . . . .
O7 O 0.64289(5) 0.06983(5) 0.25773(8) 0.0330(3) Uani 1 1 d . . . . .
O8 O 0.56483(5) 0.06819(5) 0.23476(8) 0.0314(3) Uani 1 1 d . . . . .
O9 O 0.69460(5) 0.08097(5) 0.41603(8) 0.0362(3) Uani 1 1 d . . . . .
N1 N 0.74517(7) 0.08197(7) 0.52640(11) 0.0391(4) Uani 1 1 d . . . . .
C1 C 0.70157(7) 0.17883(7) 0.50749(11) 0.0321(4) Uani 1 1 d . . . . .
C2 C 0.74207(8) 0.20626(9) 0.56867(13) 0.0444(5) Uani 1 1 d . . . . .
H2 H 0.7761 0.2328 0.5514 0.053 Uiso 1 1 calc R U . . .
C3 C 0.73246(9) 0.19471(11) 0.65311(14) 0.0547(6) Uani 1 1 d . . . . .
H3 H 0.7602 0.2130 0.6915 0.066 Uiso 1 1 calc R U . . .
C4 C 0.68202(10) 0.15628(10) 0.68161(13) 0.0520(5) Uani 1 1 d . . . . .
H4 H 0.6763 0.1478 0.7385 0.062 Uiso 1 1 calc R U . . .
C5 C 0.64050(9) 0.13071(8) 0.62496(12) 0.0411(4) Uani 1 1 d . . . . .
C6 C 0.64899(8) 0.14048(7) 0.53677(11) 0.0329(4) Uani 1 1 d . . . . .
C7 C 0.60310(7) 0.11260(6) 0.48022(11) 0.0305(4) Uani 1 1 d . . . . .
C8 C 0.54834(8) 0.08627(7) 0.51143(11) 0.0326(4) Uani 1 1 d . . . . .
C9 C 0.53967(9) 0.07279(7) 0.59867(12) 0.0399(4) Uani 1 1 d . . . . .
C10 C 0.58589(10) 0.09264(8) 0.65720(13) 0.0471(5) Uani 1 1 d . . . . .
C11 C 0.48864(9) 0.04082(8) 0.63028(13) 0.0462(5) Uani 1 1 d . . . . .
H11 H 0.4838 0.0319 0.6871 0.055 Uiso 1 1 calc R U . . .
C12 C 0.44420(9) 0.02177(7) 0.57713(13) 0.0430(5) Uani 1 1 d . . . . .
H12 H 0.4098 -0.0002 0.5984 0.052 Uiso 1 1 calc R U . . .
C13 C 0.45110(8) 0.03532(7) 0.49361(13) 0.0379(4) Uani 1 1 d . . . . .
H13 H 0.4209 0.0222 0.4592 0.046 Uiso 1 1 calc R U . . .
C14 C 0.50266(7) 0.06867(7) 0.45788(12) 0.0321(4) Uani 1 1 d . . . . .
C15 C 0.67952(7) 0.22512(7) 0.25962(10) 0.0280(3) Uani 1 1 d . . . . .
C16 C 0.65116(8) 0.25093(8) 0.21751(14) 0.0413(4) Uani 1 1 d . . . . .
H16A H 0.6325 0.2597 0.2591 0.062 Uiso 1 1 calc R U . . .
H16B H 0.6258 0.2264 0.1773 0.062 Uiso 1 1 calc R U . . .
H16C H 0.6771 0.2832 0.1893 0.062 Uiso 1 1 calc R U . . .
C17 C 0.59933(7) 0.05431(7) 0.21928(11) 0.0313(4) Uani 1 1 d . . . . .
C18 C 0.58669(9) 0.01488(10) 0.14808(14) 0.0479(5) Uani 1 1 d . . . . .
H18A H 0.6197 0.0201 0.1239 0.072 Uiso 1 1 calc R U . . .
H18B H 0.5662 0.0207 0.1058 0.072 Uiso 1 1 calc R U . . .
H18C H 0.5662 -0.0212 0.1692 0.072 Uiso 1 1 calc R U . . .
C19 C 0.73868(8) 0.09952(7) 0.45318(11) 0.0338(4) Uani 1 1 d . . . . .
H19 H 0.7689 0.1275 0.4276 0.041 Uiso 1 1 calc R U . . .
C20 C 0.79760(8) 0.10635(10) 0.56714(13) 0.0477(5) Uani 1 1 d . . . . .
H20A H 0.8244 0.1324 0.5301 0.072 Uiso 1 1 calc R U . . .
H20B H 0.8064 0.0789 0.5801 0.072 Uiso 1 1 calc R U . . .
H20C H 0.7966 0.1238 0.6181 0.072 Uiso 1 1 calc R U . . .
C21 C 0.70031(10) 0.04045(10) 0.57355(17) 0.0626(7) Uani 1 1 d . . . . .
H21A H 0.6922 0.0565 0.6201 0.094 Uiso 1 1 calc R U . . .
H21B H 0.7097 0.0147 0.5942 0.094 Uiso 1 1 calc R U . . .
H21C H 0.6694 0.0226 0.5376 0.094 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 Ni2 2.9874(4) . ?
Ni1 O1 2.0289(12) . ?
Ni1 O2 2.0243(12) . ?
Ni1 O3 2.0638(12) 18_545 ?
Ni1 O5 2.0890(11) . ?
Ni1 O7 1.9996(12) . ?
Ni1 O9 2.0619(12) . ?
Ni2 O1 2.0375(12) . ?
Ni2 O2 2.0308(12) 18_545 ?
Ni2 O3 2.0181(12) 18_545 ?
Ni2 O5 2.1040(11) 18_545 ?
Ni2 O6 2.0755(12) . ?
Ni2 O8 2.0226(12) 18_545 ?
O1 C1 1.314(2) . ?
O2 Ni2 2.0306(12) 17 ?
O2 C7 1.269(2) . ?
O3 Ni1 2.0637(12) 17 ?
O3 Ni2 2.0181(12) 17 ?
O3 C14 1.321(2) . ?
O4 C10 1.229(3) . ?
O5 Ni2 2.1039(11) 17 ?
O5 C15 1.285(2) . ?
O6 C15 1.246(2) . ?
O7 C17 1.255(2) . ?
O8 Ni2 2.0222(12) 17 ?
O8 C17 1.262(2) . ?
O9 C19 1.248(2) . ?
N1 C19 1.318(2) . ?
N1 C20 1.455(2) . ?
N1 C21 1.450(3) . ?
C1 C2 1.414(3) . ?
C1 C6 1.429(3) . ?
C2 C3 1.377(3) . ?
C3 C4 1.385(3) . ?
C4 C5 1.376(3) . ?
C5 C6 1.427(3) . ?
C5 C10 1.483(3) . ?
C6 C7 1.459(3) . ?
C7 C8 1.448(3) . ?
C8 C9 1.428(3) . ?
C8 C14 1.426(3) . ?
C9 C10 1.481(3) . ?
C9 C11 1.376(3) . ?
C11 C12 1.393(3) . ?
C12 C13 1.370(3) . ?
C13 C14 1.418(2) . ?
C15 C16 1.503(2) . ?
C17 C18 1.510(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 Ni2 42.83(3) . . ?
O1 Ni1 O3 82.66(5) . 18_545 ?
O1 Ni1 O5 91.30(5) . . ?
O1 Ni1 O9 90.01(5) . . ?
O2 Ni1 Ni2 122.28(3) . . ?
O2 Ni1 O1 83.37(5) . . ?
O2 Ni1 O3 164.49(5) . 18_545 ?
O2 Ni1 O5 80.08(5) . . ?
O2 Ni1 O9 91.03(5) . . ?
O3 Ni1 Ni2 42.36(3) 18_545 . ?
O3 Ni1 O5 93.53(5) 18_545 . ?
O5 Ni1 Ni2 81.84(3) . . ?
O7 Ni1 Ni2 140.88(4) . . ?
O7 Ni1 O1 176.18(5) . . ?
O7 Ni1 O2 92.87(5) . . ?
O7 Ni1 O3 101.16(5) . 18_545 ?
O7 Ni1 O5 88.71(5) . . ?
O7 Ni1 O9 89.38(5) . . ?
O9 Ni1 Ni2 105.16(4) . . ?
O9 Ni1 O3 95.67(5) . 18_545 ?
O9 Ni1 O5 170.79(5) . . ?
O1 Ni2 Ni1 42.61(3) . . ?
O1 Ni2 O5 110.59(5) . 18_545 ?
O1 Ni2 O6 88.54(5) . . ?
O2 Ni2 Ni1 125.80(3) 18_545 . ?
O2 Ni2 O1 168.28(5) 18_545 . ?
O2 Ni2 O5 79.58(5) 18_545 18_545 ?
O2 Ni2 O6 86.21(5) 18_545 . ?
O3 Ni2 Ni1 43.56(3) 18_545 . ?
O3 Ni2 O1 83.59(5) 18_545 . ?
O3 Ni2 O2 85.93(5) 18_545 18_545 ?
O3 Ni2 O5 165.28(5) 18_545 18_545 ?
O3 Ni2 O6 89.86(5) 18_545 . ?
O3 Ni2 O8 95.49(5) 18_545 18_545 ?
O5 Ni2 Ni1 148.11(3) 18_545 . ?
O6 Ni2 Ni1 77.34(3) . . ?
O6 Ni2 O5 86.66(4) . 18_545 ?
O8 Ni2 Ni1 107.17(4) 18_545 . ?
O8 Ni2 O1 92.88(5) 18_545 . ?
O8 Ni2 O2 93.31(5) 18_545 18_545 ?
O8 Ni2 O5 87.95(5) 18_545 18_545 ?
O8 Ni2 O6 174.59(5) 18_545 . ?
Ni1 O1 Ni2 94.56(5) . . ?
C1 O1 Ni1 120.78(11) . . ?
C1 O1 Ni2 138.13(11) . . ?
Ni1 O2 Ni2 98.87(5) . 17 ?
C7 O2 Ni1 129.78(11) . . ?
C7 O2 Ni2 123.05(11) . 17 ?
Ni2 O3 Ni1 94.08(5) 17 17 ?
C14 O3 Ni1 123.94(11) . 17 ?
C14 O3 Ni2 125.58(11) . 17 ?
Ni1 O5 Ni2 94.56(5) . 17 ?
C15 O5 Ni1 124.27(10) . . ?
C15 O5 Ni2 126.69(10) . 17 ?
C15 O6 Ni2 131.75(11) . . ?
C17 O7 Ni1 128.93(11) . . ?
C17 O8 Ni2 127.86(11) . 17 ?
C19 O9 Ni1 119.73(12) . . ?
C19 N1 C20 121.25(17) . . ?
C19 N1 C21 122.25(17) . . ?
C21 N1 C20 116.34(17) . . ?
O1 C1 C2 119.71(17) . . ?
O1 C1 C6 122.81(16) . . ?
C2 C1 C6 117.48(17) . . ?
C3 C2 C1 121.8(2) . . ?
C2 C3 C4 120.9(2) . . ?
C5 C4 C3 119.4(2) . . ?
C4 C5 C6 121.4(2) . . ?
C4 C5 C10 118.71(19) . . ?
C6 C5 C10 119.88(18) . . ?
C1 C6 C7 122.48(16) . . ?
C5 C6 C1 118.83(17) . . ?
C5 C6 C7 118.64(17) . . ?
O2 C7 C6 119.75(16) . . ?
O2 C7 C8 118.84(16) . . ?
C8 C7 C6 121.39(16) . . ?
C9 C8 C7 118.08(17) . . ?
C14 C8 C7 123.02(16) . . ?
C14 C8 C9 118.62(17) . . ?
C8 C9 C10 120.34(18) . . ?
C11 C9 C8 121.2(2) . . ?
C11 C9 C10 118.43(18) . . ?
O4 C10 C5 120.1(2) . . ?
O4 C10 C9 121.2(2) . . ?
C9 C10 C5 118.62(17) . . ?
C9 C11 C12 119.97(19) . . ?
C13 C12 C11 120.18(18) . . ?
C12 C13 C14 122.3(2) . . ?
O3 C14 C8 124.90(15) . . ?
O3 C14 C13 117.49(17) . . ?
C13 C14 C8 117.61(17) . . ?
O5 C15 C16 117.40(15) . . ?
O6 C15 O5 124.13(15) . . ?
O6 C15 C16 118.47(15) . . ?
O7 C17 O8 126.27(16) . . ?
O7 C17 C18 117.00(16) . . ?
O8 C17 C18 116.73(16) . . ?
O9 C19 N1 124.16(18) . . ?

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
Ni1 O1 C1 C2 142.85(15) . . . . ?
Ni1 O1 C1 C6 -37.9(2) . . . . ?
Ni1 O2 C7 C6 9.7(2) . . . . ?
Ni1 O2 C7 C8 -168.59(11) . . . . ?
Ni1 O3 C14 C8 -124.76(15) 17 . . . ?
Ni1 O3 C14 C13 54.43(19) 17 . . . ?
Ni1 O5 C15 O6 8.7(2) . . . . ?
Ni1 O5 C15 C16 -172.11(12) . . . . ?
Ni1 O7 C17 O8 -12.7(3) . . . . ?
Ni1 O7 C17 C18 167.79(14) . . . . ?
Ni1 O9 C19 N1 149.66(15) . . . . ?
Ni2 O1 C1 C2 -0.6(3) . . . . ?
Ni2 O1 C1 C6 178.67(12) . . . . ?
Ni2 O2 C7 C6 -131.66(13) 17 . . . ?
Ni2 O2 C7 C8 50.03(19) 17 . . . ?
Ni2 O3 C14 C8 1.2(2) 17 . . . ?
Ni2 O3 C14 C13 -179.62(11) 17 . . . ?
Ni2 O5 C15 O6 137.58(14) 17 . . . ?
Ni2 O5 C15 C16 -43.2(2) 17 . . . ?
Ni2 O6 C15 O5 -11.2(3) . . . . ?
Ni2 O6 C15 C16 169.61(13) . . . . ?
Ni2 O8 C17 O7 11.0(3) 17 . . . ?
Ni2 O8 C17 C18 -169.54(13) 17 . . . ?
O1 C1 C2 C3 -177.25(19) . . . . ?
O1 C1 C6 C5 178.87(16) . . . . ?
O1 C1 C6 C7 -3.8(3) . . . . ?
O2 C7 C8 C9 158.36(15) . . . . ?
O2 C7 C8 C14 -15.4(2) . . . . ?
C1 C2 C3 C4 -1.4(4) . . . . ?
C1 C6 C7 O2 19.6(2) . . . . ?
C1 C6 C7 C8 -162.11(16) . . . . ?
C2 C1 C6 C5 -1.9(3) . . . . ?
C2 C1 C6 C7 175.43(17) . . . . ?
C2 C3 C4 C5 -2.4(4) . . . . ?
C3 C4 C5 C6 3.9(3) . . . . ?
C3 C4 C5 C10 -175.6(2) . . . . ?
C4 C5 C6 C1 -1.8(3) . . . . ?
C4 C5 C6 C7 -179.17(19) . . . . ?
C4 C5 C10 O4 -7.4(3) . . . . ?
C4 C5 C10 C9 169.1(2) . . . . ?
C5 C6 C7 O2 -163.07(16) . . . . ?
C5 C6 C7 C8 15.2(2) . . . . ?
C6 C1 C2 C3 3.5(3) . . . . ?
C6 C5 C10 O4 173.1(2) . . . . ?
C6 C5 C10 C9 -10.4(3) . . . . ?
C6 C7 C8 C9 -19.9(2) . . . . ?
C6 C7 C8 C14 166.30(16) . . . . ?
C7 C8 C9 C10 9.1(3) . . . . ?
C7 C8 C9 C11 -170.23(17) . . . . ?
C7 C8 C14 O3 -11.5(3) . . . . ?
C7 C8 C14 C13 169.28(15) . . . . ?
C8 C9 C10 O4 -177.9(2) . . . . ?
C8 C9 C10 C5 5.6(3) . . . . ?
C8 C9 C11 C12 -1.1(3) . . . . ?
C9 C8 C14 O3 174.72(16) . . . . ?
C9 C8 C14 C13 -4.5(2) . . . . ?
C9 C11 C12 C13 -0.8(3) . . . . ?
C10 C5 C6 C1 177.71(17) . . . . ?
C10 C5 C6 C7 0.3(3) . . . . ?
C10 C9 C11 C12 179.50(19) . . . . ?
C11 C9 C10 O4 1.5(3) . . . . ?
C11 C9 C10 C5 -175.01(19) . . . . ?
C11 C12 C13 C14 0.0(3) . . . . ?
C12 C13 C14 O3 -176.57(16) . . . . ?
C12 C13 C14 C8 2.7(3) . . . . ?
C14 C8 C9 C10 -176.83(17) . . . . ?
C14 C8 C9 C11 3.8(3) . . . . ?
C20 N1 C19 O9 -178.52(18) . . . . ?
C21 N1 C19 O9 -3.2(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4 -9 9 0.0395 4.0086 -8.9942 8.9978 0.4723 -0.4132 0.7752
-9 16 5 0.0723 -8.9891 15.9985 4.9939 -0.7013 -0.6928 0.0707
9 -10 -9 0.0435 8.9847 -10.0022 -8.9934 0.3142 0.9452 -0.3443
8 -18 1 0.0670 7.9967 -17.9951 1.0037 0.8785 0.2684 0.3210
-14 5 -7 0.0644 -14.0021 4.9989 -6.9980 0.0834 -0.1090 -1.0106
-7 18 -1 0.0757 -6.9971 17.9948 -1.0037 -0.9085 -0.2287 -0.2841
14 -4 6 0.0807 14.0009 -3.9997 5.9983 -0.1492 0.1725 0.9409
2 9 -8 0.0425 1.9900 8.9931 -7.9982 -0.6485 0.5868 -0.4811
-6 4 -10 0.0359 -6.0092 3.9961 -9.9963 -0.1065 0.4025 -0.9345
6 -3 10 0.0594 6.0093 -2.9965 9.9961 0.0446 -0.4033 0.9371
-9 -3 -8 0.0550 -9.0059 -2.9998 -7.9957 0.4248 0.1607 -0.9190
-15 3 -6 0.0674 -15.0006 3.0003 -5.9981 0.2411 -0.2113 -0.9805
-4 9 -9 0.0395 -4.0086 8.9942 -8.9978 -0.4723 0.4132 -0.7752
4 6 9 0.0702 4.0095 6.0004 8.9945 -0.4567 -0.4260 0.8144
-10 4 9 0.0545 -9.9846 4.0046 8.9947 0.0874 -0.9798 0.2917
1 -10 8 0.0338 1.0086 -9.9935 7.9985 0.6204 -0.4669 0.5894
-5 -8 7 0.0384 -4.9899 -7.9931 6.9984 0.6727 -0.6423 0.3005

_platon_squeeze_details          
;
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.500 867 202 'DMF, about 5 molecules'
2 0.333 0.667 1.167 864 202 'DMF, about 5 molecules'
3 0.667 0.333 0.833 864 202 'DMF, about 5 molecules'

_vrf_CHEMW03_NiChrys-1           
;
RESPONSE:
Due to the inclusion of disordered solvent removed by SQUEEZE.
;

####################################################################### 
# 
# 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_NiChrys-2
_database_code_depnum_ccdc_archive 'CCDC 1044036'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2015-08-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_shelxl_version_number           2014/6
_chemical_name_systematic        
'tetra(acetato)-tetra(chrysazinato)-tetra(N,N-dimethylformamide)-hexa-nickel(II) bis(N,N-dimethylformamide) solvate'
_chemical_formula_moiety         'C76 H64 N4 Ni6 O28, 4(C3 H7 N O)'
_chemical_formula_sum            'C88 H92 N8 Ni6 O32'
_chemical_formula_weight         2125.95
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ni6 C88 H92 O32 N8'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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                   9.7302(6)
_cell_length_b                   13.4388(5)
_cell_length_c                   17.0848(7)
_cell_angle_alpha                95.504(3)
_cell_angle_beta                 97.873(4)
_cell_angle_gamma                95.172(4)
_cell_volume                     2190.66(18)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    5065
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      70.9260
_cell_measurement_theta_min      4.6070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.175
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.2686
_exptl_crystal_size_mid          0.1263
_exptl_crystal_size_min          0.0446
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.854
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12949
_diffrn_reflns_point_group_measured_fraction_full 0.854
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.309
_diffrn_reflns_theta_min         3.322
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.8595
_diffrn_measured_fraction_theta_max 0.8311
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0645062000
_diffrn_orient_matrix_UB_12      0.0358257000
_diffrn_orient_matrix_UB_13      0.0866883000
_diffrn_orient_matrix_UB_21      0.0535171000
_diffrn_orient_matrix_UB_22      0.1016696000
_diffrn_orient_matrix_UB_23      -0.0253853000
_diffrn_orient_matrix_UB_31      -0.1371323000
_diffrn_orient_matrix_UB_32      0.0423122000
_diffrn_orient_matrix_UB_33      0.0151042000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5763
_reflns_number_total             7058
_reflns_odcompleteness_completeness 85.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    ?
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         7058
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0598
_refine_ls_restrained_S_all      1.026
_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)+(0.1034P)²+3.2535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1810
_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
2. Restrained distances
 C42-O16 = C42-O17
 1.25 with sigma of 0.01
3. Others
 Fixed Sof: O16(0.5) O17(0.5) H42A(0.5) H42(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C26(H26), C27(H27), C28(H28), C33(H33), C36(H36), C39(H39),
 C42(H42A), C42(H42)
4.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.66510(7) -0.00616(4) 0.01944(4) 0.0285(2) Uani 1 1 d . . . . .
Ni2 Ni 0.54106(7) 0.13693(4) 0.12161(4) 0.0279(2) Uani 1 1 d . . . . .
Ni3 Ni 0.38721(7) 0.26560(5) 0.22572(4) 0.0319(2) Uani 1 1 d . . . . .
O1 O 0.7859(3) -0.1084(2) 0.04931(17) 0.0325(6) Uani 1 1 d . . . . .
O2 O 0.6339(3) 0.01324(18) 0.13521(15) 0.0288(6) Uani 1 1 d . . . . .
O3 O 0.5373(3) 0.1612(2) 0.23586(16) 0.0325(6) Uani 1 1 d . . . . .
O4 O 0.7285(6) -0.2037(3) 0.3791(3) 0.0904(17) Uani 1 1 d . . . . .
O5 O 0.5201(3) 0.10696(18) 0.00372(16) 0.0262(6) Uani 1 1 d . . . . .
O6 O 0.4450(3) 0.26047(19) 0.11238(16) 0.0300(6) Uani 1 1 d . . . . .
O7 O 0.2616(3) 0.3637(2) 0.18906(18) 0.0362(7) Uani 1 1 d . . . . .
O8 O 0.3695(4) 0.4889(2) -0.1272(2) 0.0542(9) Uani 1 1 d . . . . .
O9 O 0.8172(3) 0.1067(2) 0.03748(17) 0.0343(6) Uani 1 1 d . . . . .
O10 O 0.7340(3) 0.2133(2) 0.12536(18) 0.0349(6) Uani 1 1 d . . . . .
O11 O 0.3413(3) 0.05333(18) 0.09966(16) 0.0291(6) Uani 1 1 d . . . . .
O12 O 0.2415(3) 0.1468(2) 0.18699(18) 0.0361(7) Uani 1 1 d . . . . .
O13 O 0.5354(3) 0.3759(2) 0.27884(18) 0.0406(7) Uani 1 1 d . . . . .
O14 O 0.3011(3) 0.2714(2) 0.33059(18) 0.0408(7) Uani 1 1 d . . . . .
O15 O 0.9138(9) 0.4297(13) 0.5682(8) 0.290(9) Uani 1 1 d . . . . .
O16 O 0.8651(19) 0.2101(11) 0.5580(13) 0.194(8) Uani 0.5 1 d D . P A 1
O17 O 0.9796(15) 0.0728(13) 0.5314(10) 0.159(6) Uani 0.5 1 d D . P A 2
N1 N 0.7530(4) 0.4547(3) 0.2901(2) 0.0448(9) Uani 1 1 d . . . . .
N2 N 0.0950(5) 0.2697(3) 0.3803(2) 0.0520(10) Uani 1 1 d . . . . .
N3 N 0.6804(8) 0.4057(5) 0.5755(4) 0.098(2) Uani 1 1 d . . . . .
N4 N 0.8374(6) 0.0773(4) 0.6238(3) 0.0734(14) Uani 1 1 d . . . . .
C1 C 0.8114(4) -0.1435(3) 0.1169(3) 0.0335(9) Uani 1 1 d . . . . .
C2 C 0.9020(5) -0.2210(3) 0.1201(3) 0.0400(10) Uani 1 1 d . . . . .
H2 H 0.9401 -0.2408 0.0747 0.048 Uiso 1 1 calc R U . . .
C3 C 0.9357(5) -0.2678(3) 0.1868(3) 0.0451(11) Uani 1 1 d . . . . .
H3 H 0.9968 -0.3172 0.1864 0.054 Uiso 1 1 calc R U . . .
C4 C 0.8786(6) -0.2417(4) 0.2552(3) 0.0481(12) Uani 1 1 d . . . . .
H4 H 0.8990 -0.2749 0.3000 0.058 Uiso 1 1 calc R U . . .
C5 C 0.7919(5) -0.1667(3) 0.2563(3) 0.0418(10) Uani 1 1 d . . . . .
C6 C 0.7571(4) -0.1125(3) 0.1893(3) 0.0341(9) Uani 1 1 d . . . . .
C7 C 0.6740(4) -0.0295(3) 0.1969(3) 0.0318(9) Uani 1 1 d . . . . .
C8 C 0.6370(4) 0.0087(3) 0.2741(3) 0.0347(9) Uani 1 1 d . . . . .
C9 C 0.6669(6) -0.0485(4) 0.3399(3) 0.0472(12) Uani 1 1 d . . . . .
C10 C 0.7286(6) -0.1448(4) 0.3285(3) 0.0548(13) Uani 1 1 d . . . . .
C11 C 0.5736(4) 0.0998(3) 0.2892(3) 0.0338(9) Uani 1 1 d . . . . .
C12 C 0.5500(5) 0.1283(4) 0.3672(3) 0.0473(12) Uani 1 1 d . . . . .
H12 H 0.5095 0.1874 0.3773 0.057 Uiso 1 1 calc R U . . .
C13 C 0.5839(7) 0.0730(4) 0.4286(3) 0.0605(15) Uani 1 1 d . . . . .
H13 H 0.5694 0.0958 0.4797 0.073 Uiso 1 1 calc R U . . .
C14 C 0.6400(7) -0.0176(4) 0.4148(3) 0.0626(16) Uani 1 1 d . . . . .
H14 H 0.6592 -0.0571 0.4560 0.075 Uiso 1 1 calc R U . . .
C15 C 0.5269(4) 0.1867(3) -0.0402(2) 0.0288(8) Uani 1 1 d . . . . .
C16 C 0.5938(4) 0.1760(3) -0.1075(2) 0.0345(9) Uani 1 1 d . . . . .
H16 H 0.6409 0.1197 -0.1163 0.041 Uiso 1 1 calc R U . . .
C17 C 0.5922(5) 0.2458(3) -0.1607(3) 0.0405(10) Uani 1 1 d . . . . .
H17 H 0.6393 0.2372 -0.2043 0.049 Uiso 1 1 calc R U . . .
C18 C 0.5199(5) 0.3295(3) -0.1496(3) 0.0401(10) Uani 1 1 d . . . . .
H18 H 0.5139 0.3753 -0.1872 0.048 Uiso 1 1 calc R U . . .
C19 C 0.4574(4) 0.3440(3) -0.0823(3) 0.0339(9) Uani 1 1 d . . . . .
C20 C 0.4644(4) 0.2766(3) -0.0230(2) 0.0311(9) Uani 1 1 d . . . . .
C21 C 0.4094(4) 0.3058(3) 0.0519(2) 0.0288(8) Uani 1 1 d . . . . .
C22 C 0.3232(4) 0.3865(3) 0.0579(3) 0.0318(9) Uani 1 1 d . . . . .
C23 C 0.3033(5) 0.4478(3) -0.0060(3) 0.0362(9) Uani 1 1 d . . . . .
C24 C 0.3773(5) 0.4325(3) -0.0752(3) 0.0385(10) Uani 1 1 d . . . . .
C25 C 0.2558(4) 0.4090(3) 0.1270(3) 0.0327(9) Uani 1 1 d . . . . .
C26 C 0.1696(5) 0.4907(3) 0.1241(3) 0.0405(10) Uani 1 1 d . . . . .
H26 H 0.1229 0.5059 0.1670 0.049 Uiso 1 1 calc R U . . .
C27 C 0.1530(5) 0.5465(3) 0.0619(3) 0.0453(11) Uani 1 1 d . . . . .
H27 H 0.0955 0.5982 0.0630 0.054 Uiso 1 1 calc R U . . .
C28 C 0.2220(5) 0.5265(3) -0.0036(3) 0.0438(11) Uani 1 1 d . . . . .
H28 H 0.2130 0.5662 -0.0453 0.053 Uiso 1 1 calc R U . . .
C29 C 0.8257(4) 0.1862(3) 0.0842(3) 0.0323(9) Uani 1 1 d . . . . .
C30 C 0.9594(4) 0.2551(3) 0.0911(3) 0.0403(10) Uani 1 1 d . . . . .
H30A H 0.9938 0.2758 0.1462 0.060 Uiso 1 1 calc R U . . .
H30B H 0.9417 0.3132 0.0642 0.060 Uiso 1 1 calc R U . . .
H30C H 1.0277 0.2201 0.0674 0.060 Uiso 1 1 calc R U . . .
C31 C 0.2370(4) 0.0736(3) 0.1355(2) 0.0316(9) Uani 1 1 d . . . . .
C32 C 0.1046(5) 0.0057(3) 0.1147(3) 0.0442(11) Uani 1 1 d . . . . .
H32A H 0.0499 0.0127 0.1572 0.066 Uiso 1 1 calc R U . . .
H32B H 0.1256 -0.0627 0.1066 0.066 Uiso 1 1 calc R U . . .
H32C H 0.0530 0.0232 0.0669 0.066 Uiso 1 1 calc R U . . .
C33 C 0.6515(5) 0.3863(3) 0.2572(3) 0.0382(10) Uani 1 1 d . . . . .
H33 H 0.6681 0.3425 0.2148 0.046 Uiso 1 1 calc R U . . .
C34 C 0.8808(6) 0.4678(4) 0.2555(4) 0.0612(15) Uani 1 1 d . . . . .
H34A H 0.8816 0.5274 0.2286 0.092 Uiso 1 1 calc R U . . .
H34B H 0.8857 0.4105 0.2182 0.092 Uiso 1 1 calc R U . . .
H34C H 0.9596 0.4743 0.2968 0.092 Uiso 1 1 calc R U . . .
C35 C 0.7305(7) 0.5310(5) 0.3515(4) 0.091(2) Uani 1 1 d . . . . .
H35A H 0.8166 0.5517 0.3862 0.136 Uiso 1 1 calc R U . . .
H35B H 0.6622 0.5040 0.3815 0.136 Uiso 1 1 calc R U . . .
H35C H 0.6978 0.5878 0.3274 0.136 Uiso 1 1 calc R U . . .
C36 C 0.1714(5) 0.2619(3) 0.3222(3) 0.0416(11) Uani 1 1 d . . . . .
H36 H 0.1242 0.2481 0.2706 0.050 Uiso 1 1 calc R U . . .
C37 C -0.0558(6) 0.2521(6) 0.3652(4) 0.0740(18) Uani 1 1 d . . . . .
H37A H -0.0864 0.1969 0.3924 0.111 Uiso 1 1 calc R U . . .
H37B H -0.0859 0.2364 0.3091 0.111 Uiso 1 1 calc R U . . .
H37C H -0.0950 0.3113 0.3839 0.111 Uiso 1 1 calc R U . . .
C38 C 0.1611(8) 0.2947(8) 0.4616(4) 0.111(3) Uani 1 1 d . . . . .
H38A H 0.1612 0.2349 0.4882 0.166 Uiso 1 1 calc R U . . .
H38B H 0.1107 0.3424 0.4882 0.166 Uiso 1 1 calc R U . . .
H38C H 0.2554 0.3232 0.4624 0.166 Uiso 1 1 calc R U . . .
C39 C 0.7967(16) 0.3985(13) 0.5394(8) 0.185(7) Uani 1 1 d . . . . .
H39 H 0.7838 0.3665 0.4878 0.222 Uiso 1 1 calc R U . . .
C40 C 0.5489(12) 0.3612(11) 0.5311(7) 0.195(7) Uani 1 1 d . . . . .
H40A H 0.5048 0.3149 0.5618 0.293 Uiso 1 1 calc R U . . .
H40B H 0.5647 0.3261 0.4820 0.293 Uiso 1 1 calc R U . . .
H40C H 0.4897 0.4131 0.5200 0.293 Uiso 1 1 calc R U . . .
C41 C 0.6883(12) 0.4517(8) 0.6547(5) 0.136(4) Uani 1 1 d . . . . .
H41A H 0.7481 0.4172 0.6899 0.203 Uiso 1 1 calc R U . . .
H41B H 0.5967 0.4480 0.6698 0.203 Uiso 1 1 calc R U . . .
H41C H 0.7254 0.5208 0.6577 0.203 Uiso 1 1 calc R U . . .
C42 C 0.8983(10) 0.1219(7) 0.5687(5) 0.099(3) Uani 1 1 d D . . . .
H42A H 0.8817 0.1867 0.5581 0.119 Uiso 0.5 1 calc R U P A 2
H42 H 0.9604 0.0909 0.5402 0.119 Uiso 0.5 1 calc R U P A 1
C43 C 0.7517(10) 0.1283(8) 0.6718(6) 0.131(4) Uani 1 1 d . . . . .
H43A H 0.7464 0.1954 0.6575 0.197 Uiso 1 1 calc R U . . .
H43B H 0.7910 0.1311 0.7267 0.197 Uiso 1 1 calc R U . . .
H43C H 0.6598 0.0929 0.6635 0.197 Uiso 1 1 calc R U . . .
C44 C 0.8708(12) -0.0222(6) 0.6371(6) 0.132(4) Uani 1 1 d . . . . .
H44A H 0.9192 -0.0483 0.5956 0.197 Uiso 1 1 calc R U . . .
H44B H 0.7863 -0.0651 0.6372 0.197 Uiso 1 1 calc R U . . .
H44C H 0.9291 -0.0199 0.6875 0.197 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 Ni2 2.9245(9) . ?
Ni1 O1 1.947(3) . ?
Ni1 O2 2.038(3) . ?
Ni1 O5 2.122(2) 2_655 ?
Ni1 O5 2.176(3) . ?
Ni1 O9 1.991(3) . ?
Ni1 O11 2.063(3) 2_655 ?
Ni2 O2 1.980(3) . ?
Ni2 O3 1.954(3) . ?
Ni2 O5 1.994(3) . ?
Ni2 O6 1.986(3) . ?
Ni2 O10 2.047(3) . ?
Ni2 O11 2.123(3) . ?
Ni3 O3 2.117(3) . ?
Ni3 O6 2.086(3) . ?
Ni3 O7 1.965(3) . ?
Ni3 O12 2.032(3) . ?
Ni3 O13 2.025(3) . ?
Ni3 O14 2.077(3) . ?
O1 C1 1.291(5) . ?
O2 C7 1.279(5) . ?
O3 C11 1.320(5) . ?
O4 C10 1.226(6) . ?
O5 Ni1 2.122(2) 2_655 ?
O5 C15 1.368(4) . ?
O6 C21 1.272(5) . ?
O7 C25 1.270(5) . ?
O8 C24 1.222(5) . ?
O9 C29 1.260(5) . ?
O10 C29 1.267(5) . ?
O11 Ni1 2.063(3) 2_655 ?
O11 C31 1.291(5) . ?
O12 C31 1.249(5) . ?
O13 C33 1.236(5) . ?
O14 C36 1.244(6) . ?
O15 C39 1.198(16) . ?
O16 C42 1.280(9) . ?
O17 C42 1.272(9) . ?
N1 C33 1.312(6) . ?
N1 C34 1.452(6) . ?
N1 C35 1.447(7) . ?
N2 C36 1.321(6) . ?
N2 C37 1.448(7) . ?
N2 C38 1.443(8) . ?
N3 C39 1.366(13) . ?
N3 C40 1.441(11) . ?
N3 C41 1.422(10) . ?
N4 C42 1.338(9) . ?
N4 C43 1.421(9) . ?
N4 C44 1.437(9) . ?
C1 C2 1.425(6) . ?
C1 C6 1.450(6) . ?
C2 C3 1.369(7) . ?
C3 C4 1.390(7) . ?
C4 C5 1.372(6) . ?
C5 C6 1.431(6) . ?
C5 C10 1.470(7) . ?
C6 C7 1.442(5) . ?
C7 C8 1.472(6) . ?
C8 C9 1.435(6) . ?
C8 C11 1.437(6) . ?
C9 C10 1.483(6) . ?
C9 C14 1.373(7) . ?
C11 C12 1.405(6) . ?
C12 C13 1.365(7) . ?
C13 C14 1.392(7) . ?
C15 C16 1.400(5) . ?
C15 C20 1.424(5) . ?
C16 C17 1.366(6) . ?
C17 C18 1.391(6) . ?
C18 C19 1.378(6) . ?
C19 C20 1.422(6) . ?
C19 C24 1.483(5) . ?
C20 C21 1.487(5) . ?
C21 C22 1.434(5) . ?
C22 C23 1.432(6) . ?
C22 C25 1.447(6) . ?
C23 C24 1.473(6) . ?
C23 C28 1.378(6) . ?
C25 C26 1.440(6) . ?
C26 C27 1.358(7) . ?
C27 C28 1.399(7) . ?
C29 C30 1.512(5) . ?
C31 C32 1.489(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
O1 Ni1 Ni2 129.01(9) . . ?
O1 Ni1 O2 87.40(11) . . ?
O1 Ni1 O5 94.64(11) . 2_655 ?
O1 Ni1 O5 171.28(11) . . ?
O1 Ni1 O9 95.21(12) . . ?
O1 Ni1 O11 91.22(11) . 2_655 ?
O2 Ni1 Ni2 42.52(7) . . ?
O2 Ni1 O5 84.08(10) . . ?
O2 Ni1 O5 87.94(11) . 2_655 ?
O2 Ni1 O11 166.25(11) . 2_655 ?
O5 Ni1 Ni2 92.68(7) 2_655 . ?
O5 Ni1 Ni2 42.99(7) . . ?
O5 Ni1 O5 83.23(10) 2_655 . ?
O9 Ni1 Ni2 80.47(8) . . ?
O9 Ni1 O2 91.71(11) . . ?
O9 Ni1 O5 170.12(11) . 2_655 ?
O9 Ni1 O5 86.91(10) . . ?
O9 Ni1 O11 102.05(11) . 2_655 ?
O11 Ni1 Ni2 139.59(8) 2_655 . ?
O11 Ni1 O5 96.61(10) 2_655 . ?
O11 Ni1 O5 78.52(10) 2_655 2_655 ?
O2 Ni2 Ni1 44.07(8) . . ?
O2 Ni2 O5 90.54(11) . . ?
O2 Ni2 O6 177.56(11) . . ?
O2 Ni2 O10 88.28(11) . . ?
O2 Ni2 O11 91.39(11) . . ?
O3 Ni2 Ni1 134.94(8) . . ?
O3 Ni2 O2 91.32(11) . . ?
O3 Ni2 O5 173.03(11) . . ?
O3 Ni2 O6 86.41(11) . . ?
O3 Ni2 O10 95.11(12) . . ?
O3 Ni2 O11 93.23(11) . . ?
O5 Ni2 Ni1 48.07(7) . . ?
O5 Ni2 O10 91.66(11) . . ?
O5 Ni2 O11 80.01(10) . . ?
O6 Ni2 Ni1 138.29(8) . . ?
O6 Ni2 O5 91.61(11) . . ?
O6 Ni2 O10 92.82(11) . . ?
O6 Ni2 O11 87.84(11) . . ?
O10 Ni2 Ni1 80.24(8) . . ?
O10 Ni2 O11 171.66(11) . . ?
O11 Ni2 Ni1 93.75(7) . . ?
O6 Ni3 O3 79.85(11) . . ?
O7 Ni3 O3 165.30(12) . . ?
O7 Ni3 O6 85.46(11) . . ?
O7 Ni3 O12 93.00(12) . . ?
O7 Ni3 O13 91.93(13) . . ?
O7 Ni3 O14 88.32(12) . . ?
O12 Ni3 O3 87.47(11) . . ?
O12 Ni3 O6 89.46(11) . . ?
O12 Ni3 O14 85.68(12) . . ?
O13 Ni3 O3 89.32(12) . . ?
O13 Ni3 O6 97.08(12) . . ?
O13 Ni3 O12 172.10(13) . . ?
O13 Ni3 O14 88.30(13) . . ?
O14 Ni3 O3 106.36(12) . . ?
O14 Ni3 O6 171.90(12) . . ?
C1 O1 Ni1 129.0(3) . . ?
Ni2 O2 Ni1 93.41(11) . . ?
C7 O2 Ni1 134.0(2) . . ?
C7 O2 Ni2 132.0(2) . . ?
Ni2 O3 Ni3 94.88(12) . . ?
C11 O3 Ni2 126.1(2) . . ?
C11 O3 Ni3 133.6(3) . . ?
Ni1 O5 Ni1 96.77(10) 2_655 . ?
Ni2 O5 Ni1 101.37(11) . 2_655 ?
Ni2 O5 Ni1 88.95(10) . . ?
C15 O5 Ni1 128.7(2) . . ?
C15 O5 Ni1 117.3(2) . 2_655 ?
C15 O5 Ni2 117.6(2) . . ?
Ni2 O6 Ni3 94.89(11) . . ?
C21 O6 Ni2 130.3(2) . . ?
C21 O6 Ni3 133.4(2) . . ?
C25 O7 Ni3 129.8(3) . . ?
C29 O9 Ni1 127.4(3) . . ?
C29 O10 Ni2 124.8(3) . . ?
Ni1 O11 Ni2 99.08(11) 2_655 . ?
C31 O11 Ni1 126.9(3) . 2_655 ?
C31 O11 Ni2 124.9(2) . . ?
C31 O12 Ni3 132.4(3) . . ?
C33 O13 Ni3 121.4(3) . . ?
C36 O14 Ni3 115.4(3) . . ?
C33 N1 C34 120.5(4) . . ?
C33 N1 C35 120.7(4) . . ?
C35 N1 C34 117.7(4) . . ?
C36 N2 C37 121.7(5) . . ?
C36 N2 C38 120.2(5) . . ?
C38 N2 C37 118.1(5) . . ?
C39 N3 C40 117.4(10) . . ?
C39 N3 C41 121.7(10) . . ?
C41 N3 C40 120.8(9) . . ?
C42 N4 C43 121.9(8) . . ?
C42 N4 C44 117.3(7) . . ?
C43 N4 C44 120.6(7) . . ?
O1 C1 C2 116.1(4) . . ?
O1 C1 C6 126.8(4) . . ?
C2 C1 C6 117.1(4) . . ?
C3 C2 C1 123.0(4) . . ?
C2 C3 C4 120.1(4) . . ?
C5 C4 C3 119.7(4) . . ?
C4 C5 C6 122.7(4) . . ?
C4 C5 C10 117.8(4) . . ?
C6 C5 C10 119.4(4) . . ?
C5 C6 C1 117.3(4) . . ?
C5 C6 C7 119.5(4) . . ?
C7 C6 C1 123.2(4) . . ?
O2 C7 C6 119.1(4) . . ?
O2 C7 C8 119.2(4) . . ?
C6 C7 C8 121.6(4) . . ?
C9 C8 C7 118.0(4) . . ?
C9 C8 C11 116.9(4) . . ?
C11 C8 C7 125.1(4) . . ?
C8 C9 C10 120.1(4) . . ?
C14 C9 C8 122.3(4) . . ?
C14 C9 C10 117.6(4) . . ?
O4 C10 C5 121.2(4) . . ?
O4 C10 C9 120.4(5) . . ?
C5 C10 C9 118.4(4) . . ?
O3 C11 C8 125.4(4) . . ?
O3 C11 C12 116.4(4) . . ?
C12 C11 C8 118.2(4) . . ?
C13 C12 C11 122.9(4) . . ?
C12 C13 C14 119.9(5) . . ?
C9 C14 C13 119.6(5) . . ?
O5 C15 C16 117.2(3) . . ?
O5 C15 C20 123.6(3) . . ?
C16 C15 C20 119.1(4) . . ?
C17 C16 C15 122.1(4) . . ?
C16 C17 C18 119.9(4) . . ?
C19 C18 C17 119.4(4) . . ?
C18 C19 C20 122.4(4) . . ?
C18 C19 C24 116.9(4) . . ?
C20 C19 C24 120.7(4) . . ?
C15 C20 C21 125.3(4) . . ?
C19 C20 C15 116.6(4) . . ?
C19 C20 C21 118.1(3) . . ?
O6 C21 C20 118.7(3) . . ?
O6 C21 C22 120.1(4) . . ?
C22 C21 C20 121.2(4) . . ?
C21 C22 C25 122.2(4) . . ?
C23 C22 C21 119.4(4) . . ?
C23 C22 C25 118.4(4) . . ?
C22 C23 C24 120.5(4) . . ?
C28 C23 C22 122.0(4) . . ?
C28 C23 C24 117.3(4) . . ?
O8 C24 C19 120.2(4) . . ?
O8 C24 C23 121.2(4) . . ?
C23 C24 C19 118.5(4) . . ?
O7 C25 C22 127.4(4) . . ?
O7 C25 C26 116.4(4) . . ?
C26 C25 C22 116.2(4) . . ?
C27 C26 C25 123.4(4) . . ?
C26 C27 C28 120.2(4) . . ?
C23 C28 C27 119.7(4) . . ?
O9 C29 O10 126.5(4) . . ?
O9 C29 C30 115.9(4) . . ?
O10 C29 C30 117.5(4) . . ?
O11 C31 C32 118.2(3) . . ?
O12 C31 O11 123.4(4) . . ?
O12 C31 C32 118.3(4) . . ?
O13 C33 N1 124.5(4) . . ?
O14 C36 N2 125.6(5) . . ?
O15 C39 N3 126.0(14) . . ?
O16 C42 N4 115.5(12) . . ?
O17 C42 N4 117.9(12) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 9 -3 0.0498 -0.0053 8.9967 -2.9690 0.0646 0.9898 0.3365
0 0 11 0.0445 -0.0009 0.0054 10.9964 0.9534 -0.2786 0.1664
0 -9 3 0.0766 0.0053 -8.9967 2.9690 -0.0646 -0.9898 -0.3365
6 0 -4 0.1114 5.9931 -0.0152 -4.0050 0.0389 0.4209 -0.8830
0 -1 -11 0.0068 0.0015 -1.0052 -10.9998 -0.9895 0.1771 -0.2089
1 4 8 0.0232 0.9957 4.0009 8.0097 0.9019 0.2567 0.1537
3 -7 4 0.1276 3.0003 -7.0032 3.9722 0.2870 -0.6523 -0.6478
-6 -1 -3 0.1090 -5.9919 -0.9881 -2.9960 -0.6816 -0.3451 0.7346
-1 -2 11 0.0434 -0.9985 -1.9920 10.9908 0.8170 -0.5350 0.2186
-1 1 11 0.0405 -1.0003 1.0074 11.0008 0.9252 -0.2304 0.3460

# start Validation Reply Form
_vrf_PLAT029_NiChrys-2           
;
RESPONSE:
This crystal was picked out of a batch of crystals that was predominantly another phase (NiChrys-1).
Unfortunately we've been unable to make NiChrys-2 again to obtain more complete data, so we submit this as is.
;
####################################################################### 
# 
# 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_NiNOChrys-1
_database_code_depnum_ccdc_archive 'CCDC 1044037'
_audit_update_record             
;
2016-04-20 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_audit_creation_date             2016-01-18
_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         'C40 H36 N8 Ni2 O20'
_chemical_formula_sum            'C40 H36 N8 Ni2 O20'
_chemical_formula_weight         1066.19
_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      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_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.5780(7)
_cell_length_b                   11.0933(8)
_cell_length_c                   20.1508(14)
_cell_angle_alpha                90
_cell_angle_beta                 99.517(6)
_cell_angle_gamma                90
_cell_volume                     2111.6(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13941
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. A51 (1995) 33-38'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.117
_diffrn_reflns_av_unetI/netI     0.063
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15440
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.453
_diffrn_reflns_theta_min         2.752
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
scan:

	Number of images: 108

	           Slice: -35.0000 - 73.0000

	     Image width: 1.0000

	        Exp time: 90.0000

	   Rotation axis: Omega

	           Omega: 0.0000

	           Kappa: 72.0000

	             Phi: 150.0000

	             XTD: 45.1653

	          2theta: -16.9738

scan:

	Number of images: 91

	           Slice: -69.0000 - 22.0000

	     Image width: 1.0000

	        Exp time: 90.0000

	   Rotation axis: Omega

	           Omega: 0.0000

	           Kappa: -72.0000

	             Phi: 30.0000

	             XTD: 45.1653

	          2theta: -16.9738

scan:

	Number of images: 90

	           Slice: -68.0000 - 22.0000

	     Image width: 1.0000

	        Exp time: 90.0000

	   Rotation axis: Omega

	           Omega: 0.0000

	           Kappa: -72.0000

	             Phi: -150.0000

	             XTD: 45.1653

	          2theta: -16.9738

scan:

	Number of images: 64

	           Slice: -56.0000 - 8.0000

	     Image width: 1.0000

	        Exp time: 90.0000

	   Rotation axis: Omega

	           Omega: 0.0000

	           Kappa: 0.0000

	             Phi: -180.0000

	             XTD: 45.1653

	          2theta: -16.9738

scan:

	Number of images: 20

	           Slice: -2.0000 - 18.0000

	     Image width: 1.0000

	        Exp time: 90.0000

	   Rotation axis: Omega

	           Omega: 0.0000

	           Kappa: -36.0000

	             Phi: -150.0000

	             XTD: 45.1653

	          2theta: -16.9738

scan:

	Number of images: 95

	           Slice: -63.0000 - 32.0000

	     Image width: 1.0000

	        Exp time: 90.0000

	   Rotation axis: Omega

	           Omega: 0.0000

	           Kappa: 18.0000

	             Phi: -90.0000

	             XTD: 45.1653

	          2theta: -16.9738
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2879
_reflns_number_total             4722
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4722
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0765
_refine_ls_restrained_S_all      1.137
_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)+(0.0486P)²+6.9532P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1696
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O2) \\sim
Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of
0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C12(H12), C13(H13), C15(H15), C18(H18)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.11210(8) 0.51300(6) 0.56302(4) 0.01371(19) Uani 1 1 d . . . . .
O1 O 0.1798(5) 0.6617(3) 0.6127(2) 0.0171(9) Uani 1 1 d . . . . .
O2 O -0.0122(4) 0.6257(3) 0.4953(2) 0.0153(8) Uani 1 1 d . U . . .
O3 O -0.2262(4) 0.6164(3) 0.3867(2) 0.0186(9) Uani 1 1 d . . . . .
O4 O 0.2329(5) 0.9652(4) 0.3844(2) 0.0252(10) Uani 1 1 d . . . . .
O5 O 0.4325(5) 1.1409(4) 0.5270(3) 0.0386(12) Uani 1 1 d . U . . .
O6 O 0.2209(5) 1.1597(4) 0.4683(2) 0.0278(11) Uani 1 1 d . . . . .
O7 O 0.0163(6) 1.1264(4) 0.3379(2) 0.0302(11) Uani 1 1 d . . . . .
O8 O -0.0078(5) 1.0499(4) 0.2370(2) 0.0313(11) Uani 1 1 d . . . . .
O9 O -0.0326(4) 0.4894(3) 0.62852(19) 0.0190(8) Uani 1 1 d . . . . .
O10 O 0.2599(4) 0.5395(3) 0.50223(19) 0.0166(9) Uani 1 1 d . . . . .
N1 N 0.3122(6) 1.1027(4) 0.5064(3) 0.0243(12) Uani 1 1 d . . . . .
N2 N -0.0125(5) 1.0418(4) 0.2972(2) 0.0193(11) Uani 1 1 d . . . . .
N3 N -0.1078(6) 0.5517(4) 0.7242(3) 0.0213(12) Uani 1 1 d . . . . .
N4 N 0.3909(5) 0.4785(4) 0.4245(2) 0.0178(10) Uani 1 1 d . . . . .
C1 C 0.1996(6) 0.7624(5) 0.5838(3) 0.0170(12) Uani 1 1 d . . . . .
C2 C 0.2959(7) 0.8466(5) 0.6231(3) 0.0207(13) Uani 1 1 d . . . . .
H2 H 0.3356 0.8264 0.6681 0.025 Uiso 1 1 calc R . . . .
C3 C 0.3309(6) 0.9540(5) 0.5970(3) 0.0203(13) Uani 1 1 d . U . . .
H3 H 0.3934 1.0080 0.6238 0.024 Uiso 1 1 calc R . . . .
C4 C 0.2738(6) 0.9842(5) 0.5303(3) 0.0187(12) Uani 1 1 d . U . . .
C5 C 0.1814(6) 0.9092(5) 0.4905(3) 0.0159(12) Uani 1 1 d . . . . .
C6 C 0.1370(6) 0.7977(5) 0.5164(3) 0.0134(11) Uani 1 1 d . U . . .
C7 C 0.0271(6) 0.7271(5) 0.4738(3) 0.0150(12) Uani 1 1 d . . . . .
C8 C -0.0470(6) 0.7730(5) 0.4093(3) 0.0157(12) Uani 1 1 d . . . . .
C9 C 0.0049(7) 0.8806(5) 0.3826(3) 0.0188(13) Uani 1 1 d . . . . .
C10 C 0.1450(6) 0.9261(5) 0.4162(3) 0.0163(12) Uani 1 1 d . . . . .
C11 C -0.1700(6) 0.7157(5) 0.3702(3) 0.0170(12) Uani 1 1 d . . . . .
C12 C -0.2317(7) 0.7718(5) 0.3082(3) 0.0203(13) Uani 1 1 d . . . . .
H12 H -0.3136 0.7360 0.2827 0.024 Uiso 1 1 calc R . . . .
C13 C -0.1792(7) 0.8730(5) 0.2841(3) 0.0203(13) Uani 1 1 d . . . . .
H13 H -0.2219 0.9066 0.2423 0.024 Uiso 1 1 calc R . . . .
C14 C -0.0606(7) 0.9267(5) 0.3224(3) 0.0169(12) Uani 1 1 d . . . . .
C15 C -0.0602(6) 0.5703(5) 0.6673(3) 0.0201(13) Uani 1 1 d . . . . .
H15 H -0.0460 0.6515 0.6549 0.024 Uiso 1 1 calc R . . . .
C16 C -0.1420(8) 0.6527(5) 0.7668(3) 0.0281(16) Uani 1 1 d . . . . .
H16A H -0.0810 0.6486 0.8108 0.042 Uiso 1 1 calc GR . . . .
H16B H -0.2413 0.6471 0.7726 0.042 Uiso 1 1 calc GR . . . .
H16C H -0.1263 0.7294 0.7450 0.042 Uiso 1 1 calc GR . . . .
C17 C -0.1304(8) 0.4296(5) 0.7481(3) 0.0254(14) Uani 1 1 d . . . . .
H17A H -0.2316 0.4169 0.7482 0.038 Uiso 1 1 calc GR . . . .
H17B H -0.0781 0.4196 0.7939 0.038 Uiso 1 1 calc GR . . . .
H17C H -0.0965 0.3706 0.7183 0.038 Uiso 1 1 calc GR . . . .
C18 C 0.3100(6) 0.4579(5) 0.4702(3) 0.0178(12) Uani 1 1 d . . . . .
H18 H 0.2885 0.3766 0.4794 0.021 Uiso 1 1 calc R . . . .
C19 C 0.4231(7) 0.6030(5) 0.4074(3) 0.0210(13) Uani 1 1 d . . . . .
H19A H 0.3539 0.6301 0.3690 0.032 Uiso 1 1 calc GR . . . .
H19B H 0.5184 0.6066 0.3959 0.032 Uiso 1 1 calc GR . . . .
H19C H 0.4183 0.6555 0.4462 0.032 Uiso 1 1 calc GR . . . .
C20 C 0.4475(7) 0.3798(5) 0.3884(3) 0.0231(14) Uani 1 1 d . . . . .
H20A H 0.5511 0.3846 0.3956 0.035 Uiso 1 1 calc GR . . . .
H20B H 0.4106 0.3864 0.3402 0.035 Uiso 1 1 calc GR . . . .
H20C H 0.4186 0.3024 0.4052 0.035 Uiso 1 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
Ni1 O1 1.982(4) . ?
Ni1 O2 2.075(4) . ?
Ni1 O2 2.072(4) 3_566 ?
Ni1 O3 1.979(4) 3_566 ?
Ni1 O9 2.083(4) . ?
Ni1 O10 2.041(4) . ?
O1 C1 1.289(7) . ?
O2 Ni1 2.072(4) 3_566 ?
O2 C7 1.284(6) . ?
O3 Ni1 1.979(4) 3_566 ?
O3 C11 1.293(7) . ?
O4 C10 1.220(7) . ?
O5 N1 1.234(7) . ?
O6 N1 1.239(7) . ?
O7 N2 1.247(6) . ?
O8 N2 1.224(6) . ?
O9 C15 1.247(7) . ?
O10 C18 1.252(6) . ?
N1 C4 1.467(7) . ?
N2 C14 1.475(7) . ?
N3 C15 1.319(7) . ?
N3 C16 1.480(7) . ?
N3 C17 1.465(7) . ?
N4 C18 1.319(7) . ?
N4 C19 1.468(7) . ?
N4 C20 1.468(7) . ?
C1 C2 1.452(8) . ?
C1 C6 1.444(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.366(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.406(8) . ?
C4 C5 1.373(8) . ?
C5 C6 1.435(7) . ?
C5 C10 1.491(8) . ?
C6 C7 1.469(8) . ?
C7 C8 1.465(8) . ?
C8 C9 1.433(8) . ?
C8 C11 1.451(8) . ?
C9 C10 1.488(9) . ?
C9 C14 1.370(8) . ?
C11 C12 1.434(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.353(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.397(9) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O2 170.52(18) . 3_566 ?
O1 Ni1 O2 86.28(17) . . ?
O1 Ni1 O9 88.90(15) . . ?
O1 Ni1 O10 88.97(16) . . ?
O2 Ni1 O2 85.03(14) 3_566 . ?
O2 Ni1 O9 97.07(16) . . ?
O2 Ni1 O9 88.43(15) 3_566 . ?
O3 Ni1 O1 103.77(17) 3_566 . ?
O3 Ni1 O2 169.16(16) 3_566 . ?
O3 Ni1 O2 85.18(16) 3_566 3_566 ?
O3 Ni1 O9 87.31(16) 3_566 . ?
O3 Ni1 O10 91.89(16) 3_566 . ?
O10 Ni1 O2 84.13(16) . . ?
O10 Ni1 O2 93.89(15) . 3_566 ?
O10 Ni1 O9 177.48(16) . . ?
C1 O1 Ni1 123.6(4) . . ?
Ni1 O2 Ni1 94.97(14) 3_566 . ?
C7 O2 Ni1 125.6(4) . . ?
C7 O2 Ni1 126.4(4) . 3_566 ?
C11 O3 Ni1 122.1(4) . 3_566 ?
C15 O9 Ni1 122.6(4) . . ?
C18 O10 Ni1 124.6(3) . . ?
O5 N1 O6 123.9(5) . . ?
O5 N1 C4 118.0(5) . . ?
O6 N1 C4 118.1(5) . . ?
O7 N2 C14 118.2(5) . . ?
O8 N2 O7 123.8(5) . . ?
O8 N2 C14 118.0(5) . . ?
C15 N3 C16 121.7(5) . . ?
C15 N3 C17 121.5(5) . . ?
C17 N3 C16 116.8(5) . . ?
C18 N4 C19 119.8(5) . . ?
C18 N4 C20 121.7(5) . . ?
C19 N4 C20 118.5(4) . . ?
O1 C1 C2 116.0(5) . . ?
O1 C1 C6 126.2(5) . . ?
C6 C1 C2 117.8(5) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 C1 121.7(6) . . ?
C3 C2 H2 119.2 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.6(5) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 N1 116.6(5) . . ?
C5 C4 N1 121.6(5) . . ?
C5 C4 C3 121.8(5) . . ?
C4 C5 C6 120.7(5) . . ?
C4 C5 C10 122.2(5) . . ?
C6 C5 C10 116.1(5) . . ?
C1 C6 C7 123.4(5) . . ?
C5 C6 C1 118.3(5) . . ?
C5 C6 C7 118.3(5) . . ?
O2 C7 C6 119.4(5) . . ?
O2 C7 C8 118.5(5) . . ?
C8 C7 C6 121.9(5) . . ?
C9 C8 C7 118.4(5) . . ?
C9 C8 C11 117.5(5) . . ?
C11 C8 C7 124.1(5) . . ?
C8 C9 C10 117.0(5) . . ?
C14 C9 C8 120.5(6) . . ?
C14 C9 C10 121.6(5) . . ?
O4 C10 C5 120.3(6) . . ?
O4 C10 C9 122.0(5) . . ?
C9 C10 C5 117.3(5) . . ?
O3 C11 C8 124.7(5) . . ?
O3 C11 C12 117.7(5) . . ?
C12 C11 C8 117.7(5) . . ?
C11 C12 H12 118.3 . . ?
C13 C12 C11 123.3(6) . . ?
C13 C12 H12 118.3 . . ?
C12 C13 H13 120.9 . . ?
C12 C13 C14 118.2(6) . . ?
C14 C13 H13 120.9 . . ?
C9 C14 N2 120.3(5) . . ?
C9 C14 C13 122.8(5) . . ?
C13 C14 N2 116.8(5) . . ?
O9 C15 N3 124.8(5) . . ?
O9 C15 H15 117.6 . . ?
N3 C15 H15 117.6 . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 H17A 109.5 . . ?
N3 C17 H17B 109.5 . . ?
N3 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O10 C18 N4 123.7(5) . . ?
O10 C18 H18 118.2 . . ?
N4 C18 H18 118.2 . . ?
N4 C19 H19A 109.5 . . ?
N4 C19 H19B 109.5 . . ?
N4 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 H20A 109.5 . . ?
N4 C20 H20B 109.5 . . ?
N4 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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
Ni1 O1 C1 C2 -157.8(4) . . . . ?
Ni1 O1 C1 C6 21.2(8) . . . . ?
Ni1 O2 C7 C6 -159.0(4) 3_566 . . . ?
Ni1 O2 C7 C6 -27.8(7) . . . . ?
Ni1 O2 C7 C8 25.4(7) 3_566 . . . ?
Ni1 O2 C7 C8 156.6(4) . . . . ?
Ni1 O3 C11 C8 -31.7(7) 3_566 . . . ?
Ni1 O3 C11 C12 146.8(4) 3_566 . . . ?
Ni1 O9 C15 N3 -154.7(5) . . . . ?
Ni1 O10 C18 N4 170.7(4) . . . . ?
O1 C1 C2 C3 176.9(5) . . . . ?
O1 C1 C6 C5 -174.4(5) . . . . ?
O1 C1 C6 C7 7.5(9) . . . . ?
O2 C7 C8 C9 -174.6(5) . . . . ?
O2 C7 C8 C11 5.1(8) . . . . ?
O3 C11 C12 C13 -177.2(5) . . . . ?
O5 N1 C4 C3 35.4(8) . . . . ?
O5 N1 C4 C5 -147.6(6) . . . . ?
O6 N1 C4 C3 -142.7(6) . . . . ?
O6 N1 C4 C5 34.3(8) . . . . ?
O7 N2 C14 C9 -42.6(8) . . . . ?
O7 N2 C14 C13 133.6(6) . . . . ?
O8 N2 C14 C9 139.7(6) . . . . ?
O8 N2 C14 C13 -44.0(7) . . . . ?
N1 C4 C5 C6 -175.3(5) . . . . ?
N1 C4 C5 C10 16.9(8) . . . . ?
C1 C2 C3 C4 -0.6(9) . . . . ?
C1 C6 C7 O2 -3.5(8) . . . . ?
C1 C6 C7 C8 171.9(5) . . . . ?
C2 C1 C6 C5 4.6(8) . . . . ?
C2 C1 C6 C7 -173.5(5) . . . . ?
C2 C3 C4 N1 178.0(5) . . . . ?
C2 C3 C4 C5 1.0(9) . . . . ?
C3 C4 C5 C6 1.5(9) . . . . ?
C3 C4 C5 C10 -166.3(5) . . . . ?
C4 C5 C6 C1 -4.4(8) . . . . ?
C4 C5 C6 C7 173.8(5) . . . . ?
C4 C5 C10 O4 33.3(8) . . . . ?
C4 C5 C10 C9 -153.5(5) . . . . ?
C5 C6 C7 O2 178.4(5) . . . . ?
C5 C6 C7 C8 -6.1(8) . . . . ?
C6 C1 C2 C3 -2.2(8) . . . . ?
C6 C5 C10 O4 -135.0(5) . . . . ?
C6 C5 C10 C9 38.2(7) . . . . ?
C6 C7 C8 C9 10.0(8) . . . . ?
C6 C7 C8 C11 -170.4(5) . . . . ?
C7 C8 C9 C10 10.5(7) . . . . ?
C7 C8 C9 C14 179.8(5) . . . . ?
C7 C8 C11 O3 -1.9(9) . . . . ?
C7 C8 C11 C12 179.6(5) . . . . ?
C8 C9 C10 O4 138.5(5) . . . . ?
C8 C9 C10 C5 -34.5(7) . . . . ?
C8 C9 C14 N2 176.0(5) . . . . ?
C8 C9 C14 C13 0.0(9) . . . . ?
C8 C11 C12 C13 1.4(9) . . . . ?
C9 C8 C11 O3 177.8(5) . . . . ?
C9 C8 C11 C12 -0.8(8) . . . . ?
C10 C5 C6 C1 164.2(5) . . . . ?
C10 C5 C6 C7 -17.7(7) . . . . ?
C10 C9 C14 N2 -15.2(8) . . . . ?
C10 C9 C14 C13 168.8(5) . . . . ?
C11 C8 C9 C10 -169.2(5) . . . . ?
C11 C8 C9 C14 0.1(8) . . . . ?
C11 C12 C13 C14 -1.3(9) . . . . ?
C12 C13 C14 N2 -175.6(5) . . . . ?
C12 C13 C14 C9 0.6(9) . . . . ?
C14 C9 C10 O4 -30.7(8) . . . . ?
C14 C9 C10 C5 156.3(5) . . . . ?
C16 N3 C15 O9 -178.3(6) . . . . ?
C17 N3 C15 O9 1.2(10) . . . . ?
C19 N4 C18 O10 -1.8(9) . . . . ?
C20 N4 C18 O10 179.8(6) . . . . ?



_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
