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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c
_database_code_depnum_ccdc_archive 'CCDC 1823164'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'[hexakis(isonicotinoyl)cyclotricatechylene]disilver(I) tetrafluoroborate dimethylformamide hydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C81 H96 Ag2 B2 F8 N14 O22'
_chemical_formula_weight         2007.08

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'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/m

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

_cell_length_a                   11.80360(10)
_cell_length_b                   33.2827(4)
_cell_length_c                   12.53830(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.6160(10)
_cell_angle_gamma                90.00
_cell_volume                     4639.87(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12136
_cell_measurement_theta_min      3.7510
_cell_measurement_theta_max      73.7560

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2064
_exptl_absorpt_coefficient_mu    4.178
_exptl_absorpt_correction_T_min  0.50501
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            20679
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.97
_diffrn_reflns_theta_max         73.88
_reflns_number_total             9253
_reflns_number_gt                8333
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1357P)²+13.0576P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9253
_refine_ls_number_parameters     602
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.2080
_refine_ls_wR_factor_gt          0.2009
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.80568(3) 0.086033(9) 0.18723(3) 0.02739(15) Uani 1 1 d . . .
F1 F 0.1567(3) 0.10947(8) 0.3147(3) 0.0368(6) Uani 1 1 d . . .
F2 F 0.3602(4) 0.1135(2) 0.3751(6) 0.106(2) Uani 1 1 d . . .
F3 F 0.2632(4) 0.11157(19) 0.1970(4) 0.0846(15) Uani 1 1 d . . .
F4 F 0.2694(4) 0.05586(13) 0.3125(7) 0.099(2) Uani 1 1 d . . .
O1 O 0.0611(4) 0.16657(16) 0.7671(3) 0.0530(11) Uani 1 1 d . . .
O2 O -0.1291(3) 0.14965(9) 0.6634(3) 0.0267(6) Uani 1 1 d . . .
O3 O -0.1714(3) 0.07626(11) 0.4998(3) 0.0380(8) Uani 1 1 d . . .
O4 O 0.0098(3) 0.10662(9) 0.5600(3) 0.0248(6) Uani 1 1 d . . .
O5 O 0.2683(5) 0.2003(2) 0.0898(4) 0.093(3) Uani 1 1 d . . .
O6 O 0.3408(3) 0.20863(9) 0.2775(3) 0.0246(6) Uani 1 1 d . . .
O7 O 0.6519(4) 0.04086(12) 0.0466(3) 0.0425(9) Uani 1 1 d . . .
O8 O 0.7422(7) 0.2500 0.7110(6) 0.0652(19) Uani 1 2 d S . .
O9 O 0.5244(6) 0.1523(4) 0.8350(5) 0.130(4) Uani 1 1 d . . .
O10 O 0.3460(9) 0.2500 0.5521(9) 0.085(3) Uani 1 2 d S . .
O11 O 0.5893(4) -0.05167(15) 0.2954(4) 0.0540(11) Uani 1 1 d . . .
N1 N -0.1310(4) 0.11184(13) 1.0423(3) 0.0326(9) Uani 1 1 d . . .
N2 N 0.1078(4) -0.03173(11) 0.7148(3) 0.0289(8) Uani 1 1 d . . .
N3 N 0.6679(3) 0.13187(11) 0.2002(3) 0.0236(7) Uani 1 1 d . . .
N4 N 0.4598(4) 0.05557(15) 0.0348(4) 0.0412(10) Uani 1 1 d . . .
N5 N 0.8868(8) 0.2500 0.8865(7) 0.064(2) Uani 1 2 d S . .
N6 N 0.3966(6) 0.1571(3) 0.6574(5) 0.0694(18) Uani 1 1 d . . .
N7 N 0.2608(8) 0.2500 0.6924(9) 0.065(2) Uani 1 2 d S . .
N8 N 0.4571(5) -0.0491(3) 0.3914(6) 0.079(2) Uani 1 1 d . . .
C1 C -0.2376(5) 0.2500 0.3630(5) 0.0175(10) Uani 1 2 d S . .
H1A H -0.3141 0.2500 0.3792 0.021 Uiso 1 2 calc SR . .
H1B H -0.2572 0.2500 0.2798 0.021 Uiso 1 2 calc SR . .
C2 C -0.1667(3) 0.21223(11) 0.4124(3) 0.0177(7) Uani 1 1 d . . .
C3 C -0.1732(4) 0.19844(12) 0.5153(3) 0.0202(8) Uani 1 1 d . . .
H3 H -0.2196 0.2128 0.5516 0.024 Uiso 1 1 calc R . .
C4 C -0.1128(4) 0.16408(13) 0.5648(4) 0.0225(8) Uani 1 1 d . . .
C5 C -0.0475(4) 0.14245(12) 0.5119(4) 0.0222(8) Uani 1 1 d . . .
C6 C -0.0377(4) 0.15588(12) 0.4113(3) 0.0202(8) Uani 1 1 d . . .
H6 H 0.0093 0.1412 0.3763 0.024 Uiso 1 1 calc R . .
C7 C -0.0966(3) 0.19108(11) 0.3604(3) 0.0173(7) Uani 1 1 d . . .
C8 C -0.0851(4) 0.20358(11) 0.2479(3) 0.0177(7) Uani 1 1 d . . .
H8A H -0.1576 0.2191 0.2045 0.021 Uiso 1 1 calc R . .
H8B H -0.0826 0.1791 0.2038 0.021 Uiso 1 1 calc R . .
C9 C 0.0263(4) 0.22898(12) 0.2596(3) 0.0184(7) Uani 1 1 d . . .
C10 C 0.1328(4) 0.20846(12) 0.2672(3) 0.0205(8) Uani 1 1 d . . .
H10 H 0.1343 0.1799 0.2693 0.025 Uiso 1 1 calc R . .
C11 C 0.2348(4) 0.22932(12) 0.2718(3) 0.0221(8) Uani 1 1 d . . .
C12 C -0.0353(5) 0.15358(15) 0.7616(4) 0.0322(10) Uani 1 1 d . . .
C13 C -0.0708(5) 0.13948(14) 0.8587(4) 0.0312(10) Uani 1 1 d . . .
C14 C -0.1881(5) 0.12895(17) 0.8449(4) 0.0371(11) Uani 1 1 d . . .
H14 H -0.2500 0.1315 0.7735 0.045 Uiso 1 1 calc R . .
C15 C -0.2127(5) 0.11456(18) 0.9392(4) 0.0386(11) Uani 1 1 d . . .
H15 H -0.2926 0.1062 0.9293 0.046 Uiso 1 1 calc R . .
C16 C -0.0188(5) 0.12291(16) 1.0542(4) 0.0354(11) Uani 1 1 d . . .
H16 H 0.0406 0.1212 1.1273 0.042 Uiso 1 1 calc R . .
C17 C 0.0154(5) 0.13673(16) 0.9655(4) 0.0360(11) Uani 1 1 d . . .
H17 H 0.0964 0.1442 0.9775 0.043 Uiso 1 1 calc R . .
C18 C -0.0661(4) 0.07470(13) 0.5497(4) 0.0246(8) Uani 1 1 d . . .
C19 C -0.0010(4) 0.03813(13) 0.6083(4) 0.0251(9) Uani 1 1 d . . .
C20 C -0.0697(4) 0.00469(14) 0.6110(4) 0.0301(10) Uani 1 1 d . . .
H20 H -0.1547 0.0053 0.5767 0.036 Uiso 1 1 calc R . .
C21 C -0.0122(4) -0.02967(14) 0.6648(4) 0.0315(10) Uani 1 1 d . . .
H21 H -0.0593 -0.0527 0.6665 0.038 Uiso 1 1 calc R . .
C22 C 0.1731(4) 0.00107(14) 0.7123(4) 0.0311(10) Uani 1 1 d . . .
H22 H 0.2579 -0.0001 0.7483 0.037 Uiso 1 1 calc R . .
C23 C 0.1224(4) 0.03670(14) 0.6596(4) 0.0296(9) Uani 1 1 d . . .
H23 H 0.1712 0.0593 0.6589 0.036 Uiso 1 1 calc R . .
C24 C 0.3471(5) 0.19569(18) 0.1780(4) 0.0390(12) Uani 1 1 d . . .
C25 C 0.4630(4) 0.17481(15) 0.1904(4) 0.0313(10) Uani 1 1 d . . .
C26 C 0.5399(4) 0.16073(13) 0.2933(4) 0.0259(9) Uani 1 1 d . . .
H26 H 0.5249 0.1660 0.3618 0.031 Uiso 1 1 calc R . .
C27 C 0.6399(4) 0.13864(13) 0.2930(4) 0.0255(9) Uani 1 1 d . . .
H27 H 0.6909 0.1278 0.3627 0.031 Uiso 1 1 calc R . .
C28 C 0.5952(5) 0.14760(19) 0.1027(4) 0.0423(13) Uani 1 1 d . . .
H28 H 0.6160 0.1443 0.0363 0.051 Uiso 1 1 calc R . .
C29 C 0.4918(6) 0.1683(2) 0.0948(5) 0.0509(16) Uani 1 1 d . . .
H29 H 0.4408 0.1779 0.0236 0.061 Uiso 1 1 calc R . .
C30 C 0.5484(5) 0.05105(17) -0.0073(5) 0.0397(12) Uani 1 1 d . . .
H30 H 0.5302 0.0561 -0.0858 0.048 Uiso 1 1 calc R . .
C31 C 0.4778(6) 0.0471(2) 0.1522(6) 0.0505(14) Uani 1 1 d . . .
H31A H 0.4263 0.0246 0.1572 0.076 Uiso 1 1 calc R . .
H31B H 0.4571 0.0709 0.1879 0.076 Uiso 1 1 calc R . .
H31C H 0.5622 0.0400 0.1912 0.076 Uiso 1 1 calc R . .
C32 C 0.3394(6) 0.0668(4) -0.0368(7) 0.079(3) Uani 1 1 d . . .
H32A H 0.3351 0.0668 -0.1162 0.119 Uiso 1 1 calc R . .
H32B H 0.3206 0.0938 -0.0160 0.119 Uiso 1 1 calc R . .
H32C H 0.2812 0.0476 -0.0265 0.119 Uiso 1 1 calc R . .
C33 C 0.4230(10) 0.1514(4) 0.7672(8) 0.096(3) Uani 1 1 d . . .
H33 H 0.3587 0.1462 0.7949 0.115 Uiso 1 1 calc R . .
C34 C 0.2758(7) 0.1533(3) 0.5803(8) 0.079(2) Uani 1 1 d . . .
H34A H 0.2211 0.1489 0.6232 0.119 Uiso 1 1 calc R . .
H34B H 0.2711 0.1304 0.5298 0.119 Uiso 1 1 calc R . .
H34C H 0.2528 0.1779 0.5354 0.119 Uiso 1 1 calc R . .
C35 C 0.4908(8) 0.1619(4) 0.6093(8) 0.088(3) Uani 1 1 d . . .
H35A H 0.5570 0.1774 0.6615 0.132 Uiso 1 1 calc R . .
H35B H 0.4592 0.1761 0.5370 0.132 Uiso 1 1 calc R . .
H35C H 0.5202 0.1354 0.5968 0.132 Uiso 1 1 calc R . .
C36 C 0.3542(10) 0.2500 0.6550(11) 0.069(3) Uani 1 2 d S . .
H36 H 0.4326 0.2500 0.7099 0.083 Uiso 1 2 calc SR . .
C37 C 0.1375(8) 0.2500 0.6159(12) 0.071(3) Uani 1 2 d S . .
H37A H 0.1021 0.2766 0.6159 0.106 Uiso 0.50 1 calc PR . .
H37B H 0.0911 0.2299 0.6410 0.106 Uiso 0.50 1 calc PR . .
H37C H 0.1359 0.2434 0.5393 0.106 Uiso 0.50 1 calc PR . .
C38 C 0.2808(12) 0.2500 0.8141(12) 0.082(4) Uani 1 2 d S . .
H38A H 0.2234 0.2683 0.8302 0.123 Uiso 0.50 1 calc PR . .
H38B H 0.3630 0.2590 0.8552 0.123 Uiso 0.50 1 calc PR . .
H38C H 0.2695 0.2228 0.8384 0.123 Uiso 0.50 1 calc PR . .
C39 C 0.5648(6) -0.0538(3) 0.3811(7) 0.075(3) Uani 1 1 d . . .
H39 H 0.6295 -0.0595 0.4487 0.090 Uiso 1 1 calc R . .
C40 C 0.3529(6) -0.0405(2) 0.2957(7) 0.0599(17) Uani 1 1 d . . .
H40A H 0.3311 -0.0121 0.2974 0.090 Uiso 1 1 calc R . .
H40B H 0.2859 -0.0574 0.2981 0.090 Uiso 1 1 calc R . .
H40C H 0.3702 -0.0459 0.2259 0.090 Uiso 1 1 calc R . .
C41 C 0.4383(9) -0.0488(7) 0.5016(11) 0.198(12) Uani 1 1 d . . .
H41A H 0.5164 -0.0494 0.5625 0.297 Uiso 1 1 calc R . .
H41B H 0.3912 -0.0724 0.5075 0.297 Uiso 1 1 calc R . .
H41C H 0.3949 -0.0243 0.5081 0.297 Uiso 1 1 calc R . .
C42 C 0.8487(9) 0.2500 0.7747(7) 0.0481(19) Uani 1 2 d S . .
H42 H 0.9086 0.2500 0.7395 0.058 Uiso 1 2 calc SR . .
C43 C 0.8007(16) 0.2500 0.9443(12) 0.184(15) Uani 1 2 d S . .
H43A H 0.7937 0.2228 0.9716 0.276 Uiso 0.50 1 calc PR . .
H43B H 0.7223 0.2587 0.8921 0.276 Uiso 0.50 1 calc PR . .
H43C H 0.8271 0.2685 1.0087 0.276 Uiso 0.50 1 calc PR . .
C44 C 1.0133(10) 0.2500 0.9536(9) 0.064(3) Uani 1 2 d S . .
H44A H 1.0223 0.2500 1.0342 0.096 Uiso 1 2 calc SR . .
H44B H 1.0517 0.2740 0.9360 0.096 Uiso 0.50 1 calc PR . .
H44C H 1.0517 0.2260 0.9360 0.096 Uiso 0.50 1 calc PR . .
B1 B 0.2606(6) 0.0958(2) 0.2969(7) 0.0487(16) Uani 1 1 d . . .
O12 O 0.5628(14) 0.2500 0.4986(13) 0.138(5) Uiso 1 2 d S . .
O13 O 0.0000 0.0000 1.0000 0.133(4) Uiso 1 2 d S . .


_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
Ag1 N2 2.231(3) 3_656 ?
Ag1 N3 2.275(3) . ?
Ag1 N1 2.348(4) 1_654 ?
Ag1 O7 2.553(4) . ?
F1 B1 1.395(7) . ?
F2 B1 1.384(10) . ?
F3 B1 1.367(9) . ?
F4 B1 1.343(8) . ?
O1 C12 1.197(6) . ?
O2 C12 1.358(6) . ?
O2 C4 1.398(5) . ?
O3 C18 1.191(6) . ?
O4 C18 1.367(5) . ?
O4 C5 1.403(5) . ?
O5 C24 1.192(7) . ?
O6 C24 1.346(6) . ?
O6 C11 1.408(5) . ?
O7 C30 1.228(7) . ?
O8 C42 1.242(12) . ?
O9 C33 1.214(12) . ?
O10 C36 1.261(16) . ?
O11 C39 1.205(9) . ?
N1 C15 1.331(7) . ?
N1 C16 1.335(7) . ?
N1 Ag1 2.348(4) 1_456 ?
N2 C22 1.343(6) . ?
N2 C21 1.345(6) . ?
N2 Ag1 2.230(3) 3_656 ?
N3 C27 1.331(6) . ?
N3 C28 1.342(6) . ?
N4 C30 1.329(7) . ?
N4 C31 1.443(8) . ?
N4 C32 1.453(9) . ?
N5 C42 1.320(12) . ?
N5 C43 1.433(16) . ?
N5 C44 1.447(14) . ?
N6 C33 1.320(11) . ?
N6 C34 1.434(10) . ?
N6 C35 1.440(11) . ?
N7 C36 1.335(15) . ?
N7 C37 1.449(14) . ?
N7 C38 1.463(17) . ?
N8 C39 1.330(9) . ?
N8 C40 1.430(9) . ?
N8 C41 1.471(13) . ?
C1 C2 1.522(5) . ?
C1 C2 1.522(5) 4_565 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.396(6) . ?
C2 C7 1.402(6) . ?
C3 C4 1.380(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.377(6) . ?
C5 C6 1.379(6) . ?
C6 C7 1.402(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.520(5) . ?
C8 C9 1.529(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C9 1.400(8) 4_565 ?
C9 C10 1.405(6) . ?
C10 C11 1.374(6) . ?
C10 H10 0.9500 . ?
C11 C11 1.376(8) 4_565 ?
C12 C13 1.489(6) . ?
C13 C14 1.382(7) . ?
C13 C17 1.386(7) . ?
C14 C15 1.394(7) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.383(7) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.494(6) . ?
C19 C23 1.381(6) . ?
C19 C20 1.384(6) . ?
C20 C21 1.385(6) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 C23 1.391(6) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C25 1.495(7) . ?
C25 C29 1.369(7) . ?
C25 C26 1.386(7) . ?
C26 C27 1.392(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.375(7) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 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
N2 Ag1 N3 135.23(14) 3_656 . ?
N2 Ag1 N1 121.13(15) 3_656 1_654 ?
N3 Ag1 N1 103.35(14) . 1_654 ?
N2 Ag1 O7 89.49(14) 3_656 . ?
N3 Ag1 O7 94.85(13) . . ?
N1 Ag1 O7 91.02(14) 1_654 . ?
C12 O2 C4 117.2(3) . . ?
C18 O4 C5 114.5(3) . . ?
C24 O6 C11 115.7(3) . . ?
C30 O7 Ag1 124.2(4) . . ?
C15 N1 C16 117.3(4) . . ?
C15 N1 Ag1 117.5(3) . 1_456 ?
C16 N1 Ag1 125.2(3) . 1_456 ?
C22 N2 C21 118.1(4) . . ?
C22 N2 Ag1 120.8(3) . 3_656 ?
C21 N2 Ag1 120.9(3) . 3_656 ?
C27 N3 C28 117.4(4) . . ?
C27 N3 Ag1 124.7(3) . . ?
C28 N3 Ag1 116.8(3) . . ?
C30 N4 C31 121.1(5) . . ?
C30 N4 C32 121.4(6) . . ?
C31 N4 C32 117.4(6) . . ?
C42 N5 C43 119.3(11) . . ?
C42 N5 C44 122.3(9) . . ?
C43 N5 C44 118.3(10) . . ?
C33 N6 C34 121.6(8) . . ?
C33 N6 C35 120.5(8) . . ?
C34 N6 C35 117.4(7) . . ?
C36 N7 C37 122.1(11) . . ?
C36 N7 C38 120.2(11) . . ?
C37 N7 C38 117.7(10) . . ?
C39 N8 C40 121.6(7) . . ?
C39 N8 C41 122.8(7) . . ?
C40 N8 C41 115.4(6) . . ?
C2 C1 C2 111.4(4) . 4_565 ?
C2 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 4_565 . ?
C2 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 4_565 . ?
H1A C1 H1B 108.0 . . ?
C3 C2 C7 119.3(4) . . ?
C3 C2 C1 117.0(4) . . ?
C7 C2 C1 123.7(4) . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 120.3(4) . . ?
C5 C4 O2 120.8(4) . . ?
C3 C4 O2 118.6(4) . . ?
C4 C5 C6 120.2(4) . . ?
C4 C5 O4 120.3(4) . . ?
C6 C5 O4 119.5(4) . . ?
C5 C6 C7 120.4(4) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C2 119.2(4) . . ?
C6 C7 C8 117.8(3) . . ?
C2 C7 C8 123.0(3) . . ?
C7 C8 C9 113.8(3) . . ?
C7 C8 H8A 108.8 . . ?
C9 C8 H8A 108.8 . . ?
C7 C8 H8B 108.8 . . ?
C9 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
C9 C9 C10 119.1(2) 4_565 . ?
C9 C9 C8 123.6(2) 4_565 . ?
C10 C9 C8 117.3(3) . . ?
C11 C10 C9 120.6(4) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C11 120.3(2) . 4_565 ?
C10 C11 O6 120.4(4) . . ?
C11 C11 O6 119.3(2) 4_565 . ?
O1 C12 O2 123.8(4) . . ?
O1 C12 C13 126.1(5) . . ?
O2 C12 C13 110.1(4) . . ?
C14 C13 C17 118.9(5) . . ?
C14 C13 C12 121.5(5) . . ?
C17 C13 C12 119.6(5) . . ?
C13 C14 C15 117.8(5) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
N1 C15 C14 123.9(5) . . ?
N1 C15 H15 118.1 . . ?
C14 C15 H15 118.1 . . ?
N1 C16 C17 123.2(5) . . ?
N1 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C16 C17 C13 118.8(5) . . ?
C16 C17 H17 120.6 . . ?
C13 C17 H17 120.6 . . ?
O3 C18 O4 123.4(4) . . ?
O3 C18 C19 124.6(4) . . ?
O4 C18 C19 112.0(4) . . ?
C23 C19 C20 119.8(4) . . ?
C23 C19 C18 123.0(4) . . ?
C20 C19 C18 117.2(4) . . ?
C21 C20 C19 118.7(4) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
N2 C21 C20 122.5(4) . . ?
N2 C21 H21 118.8 . . ?
C20 C21 H21 118.8 . . ?
N2 C22 C23 123.1(4) . . ?
N2 C22 H22 118.5 . . ?
C23 C22 H22 118.5 . . ?
C19 C23 C22 117.9(4) . . ?
C19 C23 H23 121.0 . . ?
C22 C23 H23 121.0 . . ?
O5 C24 O6 123.4(5) . . ?
O5 C24 C25 123.9(5) . . ?
O6 C24 C25 112.7(4) . . ?
C29 C25 C26 118.9(4) . . ?
C29 C25 C24 118.1(4) . . ?
C26 C25 C24 123.0(4) . . ?
C25 C26 C27 117.9(4) . . ?
C25 C26 H26 121.0 . . ?
C27 C26 H26 121.0 . . ?
N3 C27 C26 123.4(4) . . ?
N3 C27 H27 118.3 . . ?
C26 C27 H27 118.3 . . ?
N3 C28 C29 122.7(5) . . ?
N3 C28 H28 118.6 . . ?
C29 C28 H28 118.6 . . ?
C25 C29 C28 119.5(5) . . ?
C25 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
O7 C30 N4 125.6(5) . . ?
O7 C30 H30 117.2 . . ?
N4 C30 H30 117.2 . . ?
N4 C31 H31A 109.5 . . ?
N4 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N4 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N4 C32 H32A 109.5 . . ?
N4 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N4 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O9 C33 N6 124.0(10) . . ?
O9 C33 H33 118.0 . . ?
N6 C33 H33 118.0 . . ?
N6 C34 H34A 109.5 . . ?
N6 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N6 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N6 C35 H35A 109.5 . . ?
N6 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N6 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
O10 C36 N7 124.8(12) . . ?
O10 C36 H36 117.6 . . ?
N7 C36 H36 117.6 . . ?
N7 C37 H37A 109.5 . . ?
N7 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N7 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N7 C38 H38A 109.5 . . ?
N7 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N7 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O11 C39 N8 127.1(7) . . ?
O11 C39 H39 116.5 . . ?
N8 C39 H39 116.5 . . ?
N8 C40 H40A 109.5 . . ?
N8 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N8 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N8 C41 H41A 109.5 . . ?
N8 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N8 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O8 C42 N5 126.4(9) . . ?
O8 C42 H42 116.8 . . ?
N5 C42 H42 116.8 . . ?
N5 C43 H43A 109.5 . . ?
N5 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N5 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N5 C44 H44A 109.5 . . ?
N5 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N5 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
F4 B1 F3 119.3(8) . . ?
F4 B1 F2 108.2(6) . . ?
F3 B1 F2 102.2(6) . . ?
F4 B1 F1 109.1(5) . . ?
F3 B1 F1 108.2(5) . . ?
F2 B1 F1 109.4(7) . . ?

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
N2 Ag1 O7 C30 150.3(4) 3_656 . . . ?
N3 Ag1 O7 C30 14.9(4) . . . . ?
N1 Ag1 O7 C30 -88.6(4) 1_654 . . . ?
N2 Ag1 N3 C27 19.4(5) 3_656 . . . ?
N1 Ag1 N3 C27 -154.2(4) 1_654 . . . ?
O7 Ag1 N3 C27 113.6(4) . . . . ?
N2 Ag1 N3 C28 -147.9(4) 3_656 . . . ?
N1 Ag1 N3 C28 38.5(4) 1_654 . . . ?
O7 Ag1 N3 C28 -53.7(4) . . . . ?
C2 C1 C2 C3 84.7(5) 4_565 . . . ?
C2 C1 C2 C7 -95.3(5) 4_565 . . . ?
C7 C2 C3 C4 -0.9(6) . . . . ?
C1 C2 C3 C4 179.1(4) . . . . ?
C2 C3 C4 C5 -1.5(6) . . . . ?
C2 C3 C4 O2 -175.2(4) . . . . ?
C12 O2 C4 C5 77.6(5) . . . . ?
C12 O2 C4 C3 -108.7(5) . . . . ?
C3 C4 C5 C6 2.7(6) . . . . ?
O2 C4 C5 C6 176.3(4) . . . . ?
C3 C4 C5 O4 -177.4(4) . . . . ?
O2 C4 C5 O4 -3.8(6) . . . . ?
C18 O4 C5 C4 74.3(5) . . . . ?
C18 O4 C5 C6 -105.7(4) . . . . ?
C4 C5 C6 C7 -1.7(6) . . . . ?
O4 C5 C6 C7 178.4(4) . . . . ?
C5 C6 C7 C2 -0.7(6) . . . . ?
C5 C6 C7 C8 -178.3(4) . . . . ?
C3 C2 C7 C6 1.9(6) . . . . ?
C1 C2 C7 C6 -178.1(4) . . . . ?
C3 C2 C7 C8 179.4(3) . . . . ?
C1 C2 C7 C8 -0.6(6) . . . . ?
C6 C7 C8 C9 -86.5(4) . . . . ?
C2 C7 C8 C9 96.0(4) . . . . ?
C7 C8 C9 C9 -93.8(3) . . . 4_565 ?
C7 C8 C9 C10 88.2(4) . . . . ?
C9 C9 C10 C11 -1.6(5) 4_565 . . . ?
C8 C9 C10 C11 176.5(4) . . . . ?
C9 C10 C11 C11 1.6(5) . . . 4_565 ?
C9 C10 C11 O6 -179.0(4) . . . . ?
C24 O6 C11 C10 82.7(5) . . . . ?
C24 O6 C11 C11 -97.9(4) . . . 4_565 ?
C4 O2 C12 O1 -4.1(7) . . . . ?
C4 O2 C12 C13 175.9(4) . . . . ?
O1 C12 C13 C14 173.1(6) . . . . ?
O2 C12 C13 C14 -7.0(7) . . . . ?
O1 C12 C13 C17 -7.0(8) . . . . ?
O2 C12 C13 C17 173.0(4) . . . . ?
C17 C13 C14 C15 -2.4(8) . . . . ?
C12 C13 C14 C15 177.5(5) . . . . ?
C16 N1 C15 C14 -1.4(8) . . . . ?
Ag1 N1 C15 C14 -179.5(5) 1_456 . . . ?
C13 C14 C15 N1 2.7(9) . . . . ?
C15 N1 C16 C17 -0.1(8) . . . . ?
Ag1 N1 C16 C17 177.8(4) 1_456 . . . ?
N1 C16 C17 C13 0.3(8) . . . . ?
C14 C13 C17 C16 1.1(8) . . . . ?
C12 C13 C17 C16 -178.9(5) . . . . ?
C5 O4 C18 O3 3.3(6) . . . . ?
C5 O4 C18 C19 -176.6(4) . . . . ?
O3 C18 C19 C23 175.9(5) . . . . ?
O4 C18 C19 C23 -4.1(6) . . . . ?
O3 C18 C19 C20 -4.7(7) . . . . ?
O4 C18 C19 C20 175.3(4) . . . . ?
C23 C19 C20 C21 -0.5(7) . . . . ?
C18 C19 C20 C21 -179.9(4) . . . . ?
C22 N2 C21 C20 0.4(8) . . . . ?
Ag1 N2 C21 C20 174.8(4) 3_656 . . . ?
C19 C20 C21 N2 0.2(8) . . . . ?
C21 N2 C22 C23 -0.7(8) . . . . ?
Ag1 N2 C22 C23 -175.1(4) 3_656 . . . ?
C20 C19 C23 C22 0.2(7) . . . . ?
C18 C19 C23 C22 179.6(4) . . . . ?
N2 C22 C23 C19 0.4(8) . . . . ?
C11 O6 C24 O5 -1.4(9) . . . . ?
C11 O6 C24 C25 178.7(4) . . . . ?
O5 C24 C25 C29 14.5(10) . . . . ?
O6 C24 C25 C29 -165.7(6) . . . . ?
O5 C24 C25 C26 -163.3(7) . . . . ?
O6 C24 C25 C26 16.5(8) . . . . ?
C29 C25 C26 C27 -3.4(8) . . . . ?
C24 C25 C26 C27 174.4(5) . . . . ?
C28 N3 C27 C26 0.4(7) . . . . ?
Ag1 N3 C27 C26 -166.8(3) . . . . ?
C25 C26 C27 N3 2.9(7) . . . . ?
C27 N3 C28 C29 -3.4(9) . . . . ?
Ag1 N3 C28 C29 164.9(6) . . . . ?
C26 C25 C29 C28 0.7(10) . . . . ?
C24 C25 C29 C28 -177.2(6) . . . . ?
N3 C28 C29 C25 2.9(11) . . . . ?
Ag1 O7 C30 N4 -73.0(7) . . . . ?
C31 N4 C30 O7 -2.3(9) . . . . ?
C32 N4 C30 O7 -178.5(7) . . . . ?
C34 N6 C33 O9 176.1(12) . . . . ?
C35 N6 C33 O9 5(2) . . . . ?
C37 N7 C36 O10 0.000(6) . . . . ?
C38 N7 C36 O10 180.000(4) . . . . ?
C40 N8 C39 O11 0.1(17) . . . . ?
C41 N8 C39 O11 -174.3(15) . . . . ?
C43 N5 C42 O8 0.000(5) . . . . ?
C44 N5 C42 O8 180.000(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        73.88
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         2.278
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.155
# start Validation Reply Form
_vrf_DIFF019_I                   
;
PROBLEM: _diffrn_standards_number is missing
RESPONSE: not relevant
;
_vrf_DIFF020_I                   
;
PROBLEM: _diffrn_standards_interval_count and
RESPONSE: not relevant
;
_vrf_DIFF022_I                   
;
PROBLEM: _diffrn_standards_decay_% is missing
RESPONSE: not relevant
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cono3sqd
_database_code_depnum_ccdc_archive 'CCDC 1823168'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
hexaaquobis{hexakis(isonicotinoyl)cyclotricatechylene}tricobalt(II)nitrate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C114 H84 Co3 N18 O48'
_chemical_formula_weight         2650.78

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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   34.7067(11)
_cell_length_b                   20.1430(5)
_cell_length_c                   32.4896(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.879(4)
_cell_angle_gamma                90.00
_cell_volume                     22050.3(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7939
_cell_measurement_theta_min      4.010
_cell_measurement_theta_max      51.270

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.798
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5436
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5949
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26709
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0538
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         4.02
_diffrn_reflns_theta_max         51.33
_reflns_number_total             11837
_reflns_number_gt                7782
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1841P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11837
_refine_ls_number_parameters     644
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0841
_refine_ls_wR_factor_ref         0.2882
_refine_ls_wR_factor_gt          0.2736
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.107
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.5000 0.11625(5) 0.2500 0.0580(4) Uani 1 2 d S . .
Co2 Co 0.74867(2) 0.86771(5) 0.24851(3) 0.0615(4) Uani 1 1 d . . .
O1 O 0.43156(10) 0.46880(17) 0.37917(10) 0.0509(9) Uani 1 1 d . . .
O3 O 0.49970(11) 0.39793(16) 0.37888(11) 0.0512(10) Uani 1 1 d . . .
O11 O 0.43549(11) 0.78114(18) 0.38603(11) 0.0604(10) Uani 1 1 d . . .
O9 O 0.50667(12) 0.8468(2) 0.38851(13) 0.0704(12) Uani 1 1 d . . .
O7 O 0.65856(12) 0.6843(2) 0.38496(13) 0.0664(11) Uani 1 1 d . . .
O5 O 0.65746(12) 0.5465(2) 0.38539(13) 0.0704(12) Uani 1 1 d . . .
O2 O 0.42932(13) 0.36868(19) 0.40888(12) 0.0681(12) Uani 1 1 d . . .
O4 O 0.52597(14) 0.32536(18) 0.43072(13) 0.0779(13) Uani 1 1 d . . .
C20 C 0.50532(15) 0.6813(2) 0.46591(14) 0.0393(13) Uani 1 1 d . . .
C6 C 0.53873(15) 0.5223(2) 0.46279(14) 0.0379(12) Uani 1 1 d . . .
N2 N 0.50095(17) 0.1913(2) 0.29721(15) 0.0702(15) Uani 1 1 d . . .
C21 C 0.50250(15) 0.6178(2) 0.48956(14) 0.0357(12) Uani 1 1 d . . .
H21A H 0.4772 0.6175 0.4987 0.043 Uiso 1 1 calc R . .
H21B H 0.5245 0.6161 0.5153 0.043 Uiso 1 1 calc R . .
C1 C 0.50435(15) 0.5568(2) 0.46266(14) 0.0384(12) Uani 1 1 d . . .
O13 O 0.43899(5) 0.11697(10) 0.23334(10) 0.0925(15) Uani 1 1 d . . .
H13A H 0.4227 0.1291 0.2499 0.139 Uiso 1 1 d R . .
H13B H 0.4240 0.1047 0.2079 0.139 Uiso 1 1 d R . .
C15 C 0.54148(5) 0.71483(8) 0.46749(5) 0.0440(13) Uani 1 1 d R . .
N1 N 0.30354(5) 0.38449(8) 0.29415(5) 0.0697(15) Uani 1 1 d R . .
O14 O 0.77227(5) 0.77970(13) 0.23140(5) 0.1032(16) Uani 1 1 d R . .
H14B H 0.7739 0.7426 0.2453 0.155 Uiso 1 1 d R . .
H14A H 0.7820 0.7741 0.2095 0.155 Uiso 1 1 d R . .
C4 C 0.50196(5) 0.44929(9) 0.40765(5) 0.0429(13) Uani 1 1 d R . .
C13 C 0.60267(5) 0.65187(8) 0.46693(5) 0.0454(13) Uani 1 1 d R . .
C5 C 0.53707(5) 0.46819(9) 0.43490(5) 0.0449(14) Uani 1 1 d R . .
H5 H 0.5607 0.4443 0.4349 0.054 Uiso 1 1 calc R . .
C3 C 0.46853(5) 0.48534(9) 0.40816(5) 0.0441(13) Uani 1 1 d R . .
C8 C 0.60234(5) 0.58235(9) 0.46737(5) 0.0464(14) Uani 1 1 d R . .
C14 C 0.58056(5) 0.69321(8) 0.49344(5) 0.0457(13) Uani 1 1 d R . .
H14C H 0.5767 0.6665 0.5177 0.055 Uiso 1 1 calc R . .
H14D H 0.5966 0.7327 0.5048 0.055 Uiso 1 1 calc R . .
O12 O 0.40268(13) 0.7939(3) 0.43650(15) 0.1004(17) Uani 1 1 d . . .
O15 O 0.72364(12) 0.95607(15) 0.26698(13) 0.1104(17) Uani 1 1 d . . .
H15A H 0.7248 0.9680 0.2932 0.166 Uiso 1 1 d R . .
H15B H 0.7111 0.9869 0.2498 0.166 Uiso 1 1 d R . .
N4 N 0.72749(11) 0.81697(15) 0.29670(9) 0.0825(17) Uani 1 1 d R . .
C2 C 0.46843(10) 0.53729(15) 0.43480(11) 0.0391(12) Uani 1 1 d R . .
H2 H 0.4445 0.5602 0.4346 0.047 Uiso 1 1 calc R . .
C7 C 0.57942(14) 0.5407(2) 0.49114(15) 0.0420(13) Uani 1 1 d . . .
H7A H 0.5757 0.5655 0.5162 0.050 Uiso 1 1 calc R . .
H7B H 0.5945 0.4998 0.5012 0.050 Uiso 1 1 calc R . .
C11 C 0.64185(15) 0.6514(3) 0.41483(17) 0.0513(14) Uani 1 1 d . . .
N3 N 0.73114(15) 0.4252(3) 0.29663(16) 0.0722(15) Uani 1 1 d . . .
N5 N 0.49551(19) 1.0420(2) 0.29539(18) 0.0862(18) Uani 1 1 d . . .
N6 N 0.30482(6) 0.84670(10) 0.29930(6) 0.0873(18) Uani 1 1 d . . .
C18 C 0.46993(6) 0.75810(10) 0.41459(6) 0.0490(14) Uani 1 1 d R . .
C10 C 0.64160(6) 0.58519(10) 0.41541(6) 0.0573(15) Uani 1 1 d R . .
O8 O 0.69827(6) 0.74805(10) 0.43467(6) 0.1050(17) Uani 1 1 d R . .
O6 O 0.71776(6) 0.58592(10) 0.41180(6) 0.1119(18) Uani 1 1 d R . .
C17 C 0.50523(6) 0.79184(10) 0.41686(6) 0.0603(16) Uani 1 1 d R . .
C16 C 0.54038(6) 0.77196(10) 0.44240(6) 0.0452(13) Uani 1 1 d R . .
H16 H 0.5639 0.7965 0.4433 0.054 Uiso 1 1 calc R . .
C19 C 0.47011(6) 0.70582(10) 0.43849(6) 0.0445(13) Uani 1 1 d R . .
H19 H 0.4458 0.6835 0.4374 0.053 Uiso 1 1 calc R . .
C23 C 0.37675(17) 0.4036(3) 0.35171(17) 0.0548(15) Uani 1 1 d . . .
C9 C 0.62272(14) 0.5488(3) 0.44037(16) 0.0514(14) Uani 1 1 d . . .
H9 H 0.6232 0.5016 0.4397 0.062 Uiso 1 1 calc R . .
C12 C 0.62285(15) 0.6858(3) 0.44060(16) 0.0554(15) Uani 1 1 d . . .
H12 H 0.6233 0.7330 0.4407 0.066 Uiso 1 1 calc R . .
C41 C 0.70018(17) 0.7602(4) 0.3620(2) 0.0748(19) Uani 1 1 d . . .
C28 C 0.51273(8) 0.33817(12) 0.39319(8) 0.0662(18) Uani 1 1 d . . .
O10 O 0.46470(8) 0.90720(12) 0.41618(8) 0.116(2) Uani 1 1 d R . .
C22 C 0.41520(8) 0.41005(12) 0.38319(8) 0.0555(15) Uani 1 1 d R . .
C29 C 0.50686(8) 0.28734(12) 0.35906(8) 0.0625(17) Uani 1 1 d R . .
C53 C 0.36873(8) 0.81417(12) 0.36290(8) 0.0750(19) Uani 1 1 d R . .
C31 C 0.47802(8) 0.24549(12) 0.29051(8) 0.0743(18) Uani 1 1 d R . .
H31 H 0.4586 0.2503 0.2646 0.089 Uiso 1 1 calc R . .
C25 C 0.32116(14) 0.4436(2) 0.29866(14) 0.0713(18) Uani 1 1 d . . .
H25 H 0.3084 0.4793 0.2816 0.086 Uiso 1 1 calc R . .
C24 C 0.35791(14) 0.4557(2) 0.32755(14) 0.0648(17) Uani 1 1 d R . .
H24 H 0.3694 0.4988 0.3303 0.078 Uiso 1 1 calc R . .
C30 C 0.4824(2) 0.2944(3) 0.32099(18) 0.0704(18) Uani 1 1 d . . .
H30 H 0.4675 0.3342 0.3146 0.084 Uiso 1 1 calc R . .
C35 C 0.70884(19) 0.5068(3) 0.3561(2) 0.0719(18) Uani 1 1 d . . .
C37 C 0.6958(2) 0.4191(4) 0.3052(2) 0.089(2) Uani 1 1 d . . .
H37 H 0.6783 0.3865 0.2900 0.106 Uiso 1 1 calc R . .
C52 C 0.4037(2) 0.7951(4) 0.3998(2) 0.084(2) Uani 1 1 d . . .
C42 C 0.69340(14) 0.7281(2) 0.32436(14) 0.0790(19) Uani 1 1 d . . .
H42 H 0.6787 0.6879 0.3194 0.095 Uiso 1 1 calc R . .
C48 C 0.51810(14) 0.9403(2) 0.33429(14) 0.081(2) Uani 1 1 d R . .
H48 H 0.5357 0.9035 0.3397 0.097 Uiso 1 1 calc R . .
C54 C 0.3749(2) 0.8322(3) 0.3257(2) 0.0737(18) Uani 1 1 d . . .
H54 H 0.4006 0.8326 0.3202 0.088 Uiso 1 1 calc R . .
C49 C 0.5197(2) 0.9896(3) 0.3036(2) 0.092(2) Uani 1 1 d . . .
H49 H 0.5393 0.9850 0.2878 0.110 Uiso 1 1 calc R . .
C47 C 0.4891(2) 0.9505(3) 0.3554(2) 0.084(2) Uani 1 1 d . . .
C55 C 0.3399(2) 0.8511(4) 0.2944(2) 0.093(2) Uani 1 1 d . . .
H55 H 0.3433 0.8682 0.2682 0.111 Uiso 1 1 calc R . .
C32 C 0.52514(16) 0.1833(2) 0.33567(15) 0.091(2) Uani 1 1 d . . .
H32 H 0.5408 0.1441 0.3413 0.109 Uiso 1 1 calc R . .
C36 C 0.68251(16) 0.4574(2) 0.33502(15) 0.087(2) Uani 1 1 d R . .
H36 H 0.6572 0.4506 0.3407 0.104 Uiso 1 1 calc R . .
C40 C 0.6846(2) 0.7289(4) 0.3972(2) 0.087(2) Uani 1 1 d . . .
C34 C 0.6942(2) 0.5490(4) 0.3867(2) 0.093(2) Uani 1 1 d . . .
C27 C 0.3591(2) 0.3414(4) 0.3478(2) 0.100(2) Uani 1 1 d . . .
H27 H 0.3708 0.3050 0.3649 0.120 Uiso 1 1 calc R . .
C33 C 0.5283(2) 0.2301(3) 0.36767(18) 0.079(2) Uani 1 1 d . . .
H33 H 0.5450 0.2224 0.3950 0.094 Uiso 1 1 calc R . .
C45 C 0.71888(15) 0.8207(3) 0.36797(16) 0.100(2) Uani 1 1 d . . .
H45 H 0.7228 0.8436 0.3942 0.119 Uiso 1 1 calc R . .
C43 C 0.71027(15) 0.7594(3) 0.29157(16) 0.099(3) Uani 1 1 d R . .
H43 H 0.7085 0.7365 0.2656 0.119 Uiso 1 1 calc R . .
C44 C 0.7315(2) 0.8460(4) 0.3354(2) 0.100(3) Uani 1 1 d . . .
H44 H 0.7443 0.8879 0.3396 0.120 Uiso 1 1 calc R . .
C39 C 0.7453(2) 0.5174(5) 0.3485(2) 0.112(3) Uani 1 1 d . . .
H39 H 0.7626 0.5517 0.3618 0.134 Uiso 1 1 calc R . .
C26 C 0.3222(2) 0.3348(4) 0.3164(2) 0.103(3) Uani 1 1 d . . .
H26 H 0.3107 0.2918 0.3115 0.123 Uiso 1 1 calc R . .
C46 C 0.4848(3) 0.8994(4) 0.3905(3) 0.104(3) Uani 1 1 d . . .
C38 C 0.75503(19) 0.4713(3) 0.31821(19) 0.111(3) Uani 1 1 d . . .
H38 H 0.7809 0.4744 0.3134 0.134 Uiso 1 1 calc R . .
C50 C 0.46715(19) 1.0480(3) 0.31858(19) 0.128(3) Uani 1 1 d R . .
H50 H 0.4496 1.0849 0.3134 0.154 Uiso 1 1 calc R . .
C56 C 0.3014(2) 0.8286(5) 0.3391(2) 0.112(3) Uani 1 1 d . . .
H56 H 0.2757 0.8293 0.3444 0.134 Uiso 1 1 calc R . .
C57 C 0.3316(3) 0.8101(5) 0.3710(3) 0.121(3) Uani 1 1 d . . .
H57 H 0.3277 0.7951 0.3974 0.145 Uiso 1 1 calc R . .
C51 C 0.4633(3) 1.0023(4) 0.3489(3) 0.126(3) Uani 1 1 d . . .
H51 H 0.4436 1.0069 0.3645 0.151 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O13 2.0559(17) 2_655 ?
Co1 O13 2.0560(17) . ?
Co1 N5 2.133(5) 2_645 ?
Co1 N5 2.133(5) 1_545 ?
Co1 N2 2.149(4) . ?
Co1 N2 2.149(4) 2_655 ?
Co2 O14 2.083(3) . ?
Co2 N3 2.115(5) 4_655 ?
Co2 O15 2.129(3) . ?
Co2 N1 2.141(2) 3 ?
Co2 N4 2.142(3) . ?
Co2 N6 2.158(2) 2_655 ?
O1 C22 1.333(4) . ?
O1 C3 1.437(4) . ?
O3 C28 1.330(4) . ?
O3 C4 1.384(4) . ?
O11 C52 1.318(7) . ?
O11 C18 1.405(4) . ?
O9 C46 1.313(9) . ?
O9 C17 1.448(4) . ?
O7 C40 1.267(8) . ?
O7 C11 1.410(6) . ?
O5 C34 1.269(8) . ?
O5 C10 1.456(4) . ?
O2 C22 1.198(4) . ?
O4 C28 1.223(5) . ?
C20 C15 1.415(5) . ?
C20 C19 1.417(5) . ?
C20 C21 1.507(6) . ?
C6 C1 1.380(6) . ?
C6 C5 1.409(5) . ?
C6 C7 1.535(7) . ?
N2 C31 1.337(5) . ?
N2 C32 1.338(6) . ?
C21 C1 1.519(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C1 C2 1.409(6) . ?
O13 H13A 0.9008 . ?
O13 H13B 0.9005 . ?
C15 C16 1.405(3) . ?
C15 C14 1.4804 . ?
N1 C26 1.312(8) . ?
N1 C25 1.330(5) . ?
N1 Co2 2.1411(19) 3_445 ?
O14 H14B 0.8672 . ?
O14 H14A 0.8671 . ?
C4 C3 1.3722 . ?
C4 C5 1.3770 . ?
C13 C8 1.4005 . ?
C13 C12 1.406(5) . ?
C13 C14 1.5301 . ?
C5 H5 0.9500 . ?
C3 C2 1.358(4) . ?
C8 C9 1.423(5) . ?
C8 C7 1.492(5) . ?
C14 H14C 0.9900 . ?
C14 H14D 0.9900 . ?
O12 C52 1.201(7) . ?
O15 H15A 0.8770 . ?
O15 H15B 0.8778 . ?
N4 C43 1.297(6) . ?
N4 C44 1.362(8) . ?
C2 H2 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C11 C10 1.334(6) . ?
C11 C12 1.372(7) . ?
N3 C37 1.326(8) . ?
N3 C38 1.328(8) . ?
N3 Co2 2.115(5) 4_645 ?
N5 C49 1.335(8) . ?
N5 C50 1.381(7) . ?
N5 Co1 2.133(5) 1_565 ?
N6 C55 1.270(8) . ?
N6 C56 1.376(8) . ?
N6 Co2 2.158(2) 2_655 ?
C18 C19 1.3075 . ?
C18 C17 1.3874 . ?
C10 C9 1.371(5) . ?
O8 C40 1.256(7) . ?
O6 C34 1.252(7) . ?
C17 C16 1.3607 . ?
C16 H16 0.9500 . ?
C19 H19 0.9500 . ?
C23 C24 1.378(7) . ?
C23 C27 1.387(9) . ?
C23 C22 1.480(6) . ?
C9 H9 0.9500 . ?
C12 H12 0.9500 . ?
C41 C42 1.352(7) . ?
C41 C45 1.372(8) . ?
C41 C40 1.517(9) . ?
C28 C29 1.4870 . ?
O10 C46 1.221(8) . ?
C29 C30 1.329(7) . ?
C29 C33 1.364(7) . ?
C53 C54 1.329(6) . ?
C53 C57 1.378(8) . ?
C53 C52 1.536(7) . ?
C31 C30 1.379(6) . ?
C31 H31 0.9500 . ?
C25 C24 1.4118 . ?
C25 H25 0.9500 . ?
C24 H24 0.9500 . ?
C30 H30 0.9500 . ?
C35 C39 1.361(9) . ?
C35 C36 1.411(8) . ?
C35 C34 1.485(9) . ?
C37 C36 1.402(8) . ?
C37 H37 0.9500 . ?
C42 C43 1.475(6) . ?
C42 H42 0.9500 . ?
C48 C47 1.363(8) . ?
C48 C49 1.418(8) . ?
C48 H48 0.9500 . ?
C54 C55 1.434(9) . ?
C54 H54 0.9500 . ?
C49 H49 0.9500 . ?
C47 C51 1.358(9) . ?
C47 C46 1.568(9) . ?
C55 H55 0.9500 . ?
C32 C33 1.388(7) . ?
C32 H32 0.9500 . ?
C36 H36 0.9500 . ?
C27 C26 1.438(9) . ?
C27 H27 0.9500 . ?
C33 H33 0.9500 . ?
C45 C44 1.339(8) . ?
C45 H45 0.9500 . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C39 C38 1.451(9) . ?
C39 H39 0.9500 . ?
C26 H26 0.9500 . ?
C38 H38 0.9500 . ?
C50 C51 1.376(9) . ?
C50 H50 0.9500 . ?
C56 C57 1.337(10) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C51 H51 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O13 Co1 O13 179.19(13) 2_655 . ?
O13 Co1 N5 86.9(2) 2_655 2_645 ?
O13 Co1 N5 93.69(18) . 2_645 ?
O13 Co1 N5 93.68(18) 2_655 1_545 ?
O13 Co1 N5 86.9(2) . 1_545 ?
N5 Co1 N5 90.9(3) 2_645 1_545 ?
O13 Co1 N2 88.20(18) 2_655 . ?
O13 Co1 N2 91.23(16) . . ?
N5 Co1 N2 175.1(2) 2_645 . ?
N5 Co1 N2 89.5(2) 1_545 . ?
O13 Co1 N2 91.24(16) 2_655 2_655 ?
O13 Co1 N2 88.20(18) . 2_655 ?
N5 Co1 N2 89.5(2) 2_645 2_655 ?
N5 Co1 N2 175.1(2) 1_545 2_655 ?
N2 Co1 N2 90.5(2) . 2_655 ?
O14 Co2 N3 93.65(17) . 4_655 ?
O14 Co2 O15 178.40(9) . . ?
N3 Co2 O15 87.91(18) 4_655 . ?
O14 Co2 N1 88.74(8) . 3 ?
N3 Co2 N1 90.37(15) 4_655 3 ?
O15 Co2 N1 91.60(14) . 3 ?
O14 Co2 N4 90.85(10) . . ?
N3 Co2 N4 175.33(18) 4_655 . ?
O15 Co2 N4 87.60(11) . . ?
N1 Co2 N4 88.47(12) 3 . ?
O14 Co2 N6 88.08(8) . 2_655 ?
N3 Co2 N6 88.80(15) 4_655 2_655 ?
O15 Co2 N6 91.61(14) . 2_655 ?
N1 Co2 N6 176.65(10) 3 2_655 ?
N4 Co2 N6 92.62(12) . 2_655 ?
C22 O1 C3 118.4(3) . . ?
C28 O3 C4 118.8(3) . . ?
C52 O11 C18 119.7(4) . . ?
C46 O9 C17 118.5(4) . . ?
C40 O7 C11 119.8(5) . . ?
C34 O5 C10 119.7(5) . . ?
C15 C20 C19 118.7(3) . . ?
C15 C20 C21 123.5(4) . . ?
C19 C20 C21 117.7(4) . . ?
C1 C6 C5 119.0(4) . . ?
C1 C6 C7 123.4(4) . . ?
C5 C6 C7 117.6(4) . . ?
C31 N2 C32 117.8(4) . . ?
C31 N2 Co1 123.5(3) . . ?
C32 N2 Co1 118.7(3) . . ?
C20 C21 C1 112.1(4) . . ?
C20 C21 H21A 109.2 . . ?
C1 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C1 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C6 C1 C2 119.5(4) . . ?
C6 C1 C21 124.2(4) . . ?
C2 C1 C21 116.2(4) . . ?
Co1 O13 H13A 126.7 . . ?
Co1 O13 H13B 125.0 . . ?
H13A O13 H13B 108.3 . . ?
C16 C15 C20 118.0(2) . . ?
C16 C15 C14 117.70(10) . . ?
C20 C15 C14 124.3(2) . . ?
C26 N1 C25 117.9(4) . . ?
C26 N1 Co2 120.1(3) . 3_445 ?
C25 N1 Co2 121.8(2) . 3_445 ?
Co2 O14 H14B 125.1 . . ?
Co2 O14 H14A 125.9 . . ?
H14B O14 H14A 109.0 . . ?
C3 C4 C5 117.8 . . ?
C3 C4 O3 119.52(17) . . ?
C5 C4 O3 122.61(17) . . ?
C8 C13 C12 119.9(3) . . ?
C8 C13 C14 122.1 . . ?
C12 C13 C14 117.9(3) . . ?
C4 C5 C6 121.4(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C2 C3 C4 123.14(16) . . ?
C2 C3 O1 117.3(2) . . ?
C4 C3 O1 119.60(15) . . ?
C13 C8 C9 117.5(2) . . ?
C13 C8 C7 125.00(19) . . ?
C9 C8 C7 117.2(3) . . ?
C15 C14 C13 110.7 . . ?
C15 C14 H14C 109.5 . . ?
C13 C14 H14C 109.5 . . ?
C15 C14 H14D 109.5 . . ?
C13 C14 H14D 109.5 . . ?
H14C C14 H14D 108.1 . . ?
Co2 O15 H15A 125.3 . . ?
Co2 O15 H15B 125.8 . . ?
H15A O15 H15B 108.9 . . ?
C43 N4 C44 116.3(4) . . ?
C43 N4 Co2 124.1(3) . . ?
C44 N4 Co2 119.5(4) . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C8 C7 C6 110.7(3) . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C10 C11 C12 119.4(4) . . ?
C10 C11 O7 119.0(4) . . ?
C12 C11 O7 121.3(5) . . ?
C37 N3 C38 116.5(6) . . ?
C37 N3 Co2 124.8(5) . 4_645 ?
C38 N3 Co2 118.7(4) . 4_645 ?
C49 N5 C50 117.2(5) . . ?
C49 N5 Co1 123.1(5) . 1_565 ?
C50 N5 Co1 119.7(4) . 1_565 ?
C55 N6 C56 115.9(5) . . ?
C55 N6 Co2 125.6(4) . 2_655 ?
C56 N6 Co2 118.4(3) . 2_655 ?
C19 C18 C17 119.0 . . ?
C19 C18 O11 122.72(17) . . ?
C17 C18 O11 118.29(17) . . ?
C11 C10 C9 123.3(3) . . ?
C11 C10 O5 121.4(3) . . ?
C9 C10 O5 114.9(3) . . ?
C16 C17 C18 122.6 . . ?
C16 C17 O9 116.74(18) . . ?
C18 C17 O9 120.35(18) . . ?
C17 C16 C15 119.36(10) . . ?
C17 C16 H16 120.3 . . ?
C15 C16 H16 120.3 . . ?
C18 C19 C20 122.3(2) . . ?
C18 C19 H19 118.9 . . ?
C20 C19 H19 118.9 . . ?
C24 C23 C27 119.8(6) . . ?
C24 C23 C22 123.5(5) . . ?
C27 C23 C22 116.6(5) . . ?
C10 C9 C8 119.3(4) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C11 C12 C13 120.5(5) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C42 C41 C45 121.8(6) . . ?
C42 C41 C40 117.8(6) . . ?
C45 C41 C40 120.3(6) . . ?
O4 C28 O3 123.7(3) . . ?
O4 C28 C29 123.3(2) . . ?
O3 C28 C29 112.85(18) . . ?
O2 C22 O1 125.0(3) . . ?
O2 C22 C23 124.8(4) . . ?
O1 C22 C23 110.2(3) . . ?
C30 C29 C33 118.4(4) . . ?
C30 C29 C28 124.3(3) . . ?
C33 C29 C28 117.3(3) . . ?
C54 C53 C57 123.5(5) . . ?
C54 C53 C52 120.7(5) . . ?
C57 C53 C52 115.8(5) . . ?
N2 C31 C30 120.5(4) . . ?
N2 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
N1 C25 C24 123.1(2) . . ?
N1 C25 H25 118.4 . . ?
C24 C25 H25 118.4 . . ?
C23 C24 C25 118.5(3) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
C29 C30 C31 121.9(5) . . ?
C29 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
C39 C35 C36 122.9(6) . . ?
C39 C35 C34 120.8(7) . . ?
C36 C35 C34 116.3(6) . . ?
N3 C37 C36 124.7(7) . . ?
N3 C37 H37 117.7 . . ?
C36 C37 H37 117.7 . . ?
O12 C52 O11 124.0(6) . . ?
O12 C52 C53 125.1(6) . . ?
O11 C52 C53 110.9(5) . . ?
C41 C42 C43 115.8(5) . . ?
C41 C42 H42 122.1 . . ?
C43 C42 H42 122.1 . . ?
C47 C48 C49 114.1(5) . . ?
C47 C48 H48 123.0 . . ?
C49 C48 H48 123.0 . . ?
C53 C54 C55 115.1(6) . . ?
C53 C54 H54 122.5 . . ?
C55 C54 H54 122.5 . . ?
N5 C49 C48 124.4(6) . . ?
N5 C49 H49 117.8 . . ?
C48 C49 H49 117.8 . . ?
C51 C47 C48 125.1(6) . . ?
C51 C47 C46 116.4(7) . . ?
C48 C47 C46 118.5(6) . . ?
N6 C55 C54 124.5(6) . . ?
N6 C55 H55 117.7 . . ?
C54 C55 H55 117.7 . . ?
N2 C32 C33 122.4(5) . . ?
N2 C32 H32 118.8 . . ?
C33 C32 H32 118.8 . . ?
C37 C36 C35 116.2(5) . . ?
C37 C36 H36 121.9 . . ?
C35 C36 H36 121.9 . . ?
O8 C40 O7 126.7(6) . . ?
O8 C40 C41 118.8(7) . . ?
O7 C40 C41 114.4(6) . . ?
O6 C34 O5 122.6(7) . . ?
O6 C34 C35 120.2(7) . . ?
O5 C34 C35 117.2(6) . . ?
C23 C27 C26 116.5(6) . . ?
C23 C27 H27 121.7 . . ?
C26 C27 H27 121.7 . . ?
C29 C33 C32 118.7(5) . . ?
C29 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
C44 C45 C41 117.3(6) . . ?
C44 C45 H45 121.4 . . ?
C41 C45 H45 121.4 . . ?
N4 C43 C42 122.7(5) . . ?
N4 C43 H43 118.7 . . ?
C42 C43 H43 118.7 . . ?
C45 C44 N4 125.9(6) . . ?
C45 C44 H44 117.1 . . ?
N4 C44 H44 117.1 . . ?
C35 C39 C38 113.6(7) . . ?
C35 C39 H39 123.2 . . ?
C38 C39 H39 123.2 . . ?
N1 C26 C27 123.9(6) . . ?
N1 C26 H26 118.0 . . ?
C27 C26 H26 118.0 . . ?
O10 C46 O9 124.7(7) . . ?
O10 C46 C47 125.5(8) . . ?
O9 C46 C47 109.8(6) . . ?
N3 C38 C39 126.0(6) . . ?
N3 C38 H38 117.0 . . ?
C39 C38 H38 117.0 . . ?
C51 C50 N5 122.4(6) . . ?
C51 C50 H50 118.8 . . ?
N5 C50 H50 118.8 . . ?
C57 C56 N6 125.1(7) . . ?
C57 C56 H56 117.5 . . ?
N6 C56 H56 117.5 . . ?
C56 C57 C53 115.5(7) . . ?
C56 C57 H57 122.2 . . ?
C53 C57 H57 122.2 . . ?
C47 C51 C50 116.9(7) . . ?
C47 C51 H51 121.5 . . ?
C50 C51 H51 121.5 . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        51.33
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.072
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 -0.004 0.373 -0.034 13849 3466 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_DIFF019_I                   
;
PROBLEM: _diffrn_standards_number is missing
RESPONSE: not relevant as not point detector
;
_vrf_DIFF020_I                   
;
PROBLEM: _diffrn_standards_interval_count and
RESPONSE: not relevant
;
_vrf_DIFF022_I                   
;
PROBLEM: _diffrn_standards_decay_% is missing
RESPONSE: not relevant
;
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: anions not located in structure are included in formula
;
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Diffraction weak at high angles due to disorder/voids
;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      51.33 Degree
RESPONSE: Diffraction weak at high angles due to disorder/voids
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1823167'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'hexakis(isonicotinoyl)cyclotricatechylene dimethyl formamide clathrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H43 N7 O13'
_chemical_formula_weight         1070.01

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.6325(4)
_cell_length_b                   14.2524(2)
_cell_length_c                   14.6263(6)
_cell_angle_alpha                81.277(3)
_cell_angle_beta                 67.960(3)
_cell_angle_gamma                79.096(2)
_cell_volume                     2576.42(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    56317
_cell_measurement_theta_min      1.46
_cell_measurement_theta_max      36.20

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9882
_exptl_absorpt_correction_T_max  0.9931
_exptl_absorpt_process_details   
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56317
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0623
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         36.20
_reflns_number_total             23748
_reflns_number_gt                13103
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1130P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         23748
_refine_ls_number_parameters     723
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.2075
_refine_ls_wR_factor_gt          0.1879
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_restrained_S_all      0.969
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.41611(9) 0.75123(7) 0.81416(8) 0.0449(2) Uani 1 1 d . . .
O2 O 0.37056(8) 0.63454(6) 0.75544(7) 0.0388(2) Uani 1 1 d . . .
O3 O 0.19400(9) 0.64756(8) 0.97277(9) 0.0506(3) Uani 1 1 d . . .
O4 O 0.22446(8) 0.52372(7) 0.88246(7) 0.0381(2) Uani 1 1 d . . .
O5 O 0.31570(9) 0.17910(7) 0.83834(8) 0.0442(2) Uani 1 1 d . . .
O6 O 0.38102(8) 0.04929(6) 0.91895(7) 0.03477(19) Uani 1 1 d . . .
O7 O 0.52885(9) 0.01135(7) 0.71696(8) 0.0450(2) Uani 1 1 d . . .
O8 O 0.59755(8) -0.03680(6) 0.83764(6) 0.03352(19) Uani 1 1 d . . .
O9 O 1.05409(8) 0.17837(8) 0.58916(8) 0.0459(2) Uani 1 1 d . . .
O10 O 0.91757(7) 0.24383(6) 0.53588(6) 0.03309(18) Uani 1 1 d . . .
O11 O 0.87137(7) 0.44224(6) 0.51715(6) 0.03347(18) Uani 1 1 d . . .
O12 O 0.73918(10) 0.40328(9) 0.47813(9) 0.0547(3) Uani 1 1 d . . .
O13 O 0.45691(13) 0.38474(10) 0.47364(11) 0.0702(4) Uani 1 1 d . . .
N1 N 0.28455(12) 0.91851(11) 0.54356(11) 0.0561(4) Uani 1 1 d . . .
N2 N -0.14633(11) 0.66943(11) 0.90466(10) 0.0516(3) Uani 1 1 d . . .
N3 N 0.07758(12) -0.06701(10) 0.87966(12) 0.0547(4) Uani 1 1 d . . .
N4 N 0.74595(12) -0.31505(9) 0.63680(11) 0.0514(3) Uani 1 1 d . . .
N5 N 1.11967(10) 0.01305(8) 0.28703(9) 0.0392(2) Uani 1 1 d . . .
N6 N 0.88291(13) 0.67311(9) 0.22579(10) 0.0524(3) Uani 1 1 d . . .
N7 N 0.49553(11) 0.30181(9) 0.60669(10) 0.0484(3) Uani 1 1 d . . .
C1 C 0.54243(10) 0.46702(8) 0.87302(9) 0.0298(2) Uani 1 1 d . . .
C2 C 0.51063(11) 0.54336(8) 0.81312(9) 0.0327(2) Uani 1 1 d . . .
H2 H 0.5613 0.5826 0.7697 0.039 Uiso 1 1 calc R . .
C3 C 0.40525(11) 0.56228(9) 0.81666(10) 0.0348(3) Uani 1 1 d . . .
C4 C 0.33132(11) 0.50478(9) 0.87932(10) 0.0342(3) Uani 1 1 d . . .
C5 C 0.36236(10) 0.42791(9) 0.93664(9) 0.0325(2) Uani 1 1 d . . .
H5 H 0.3116 0.3878 0.9781 0.039 Uiso 1 1 calc R . .
C6 C 0.46778(10) 0.40795(8) 0.93469(9) 0.0300(2) Uani 1 1 d . . .
C7 C 0.49413(10) 0.32294(8) 1.00187(9) 0.0307(2) Uani 1 1 d . . .
H7A H 0.4313 0.3181 1.0638 0.037 Uiso 1 1 calc R . .
H7B H 0.5540 0.3343 1.0196 0.037 Uiso 1 1 calc R . .
C8 C 0.52474(10) 0.22856(8) 0.95510(8) 0.0289(2) Uani 1 1 d . . .
C9 C 0.44229(10) 0.18225(8) 0.95748(9) 0.0318(2) Uani 1 1 d . . .
H9 H 0.3702 0.2099 0.9889 0.038 Uiso 1 1 calc R . .
C10 C 0.46361(10) 0.09657(8) 0.91476(9) 0.0317(2) Uani 1 1 d . . .
C11 C 0.56892(11) 0.05433(8) 0.87244(9) 0.0315(2) Uani 1 1 d . . .
C12 C 0.65187(10) 0.09841(8) 0.87070(9) 0.0299(2) Uani 1 1 d . . .
H12 H 0.7235 0.0680 0.8428 0.036 Uiso 1 1 calc R . .
C13 C 0.63190(10) 0.18672(8) 0.90921(8) 0.0287(2) Uani 1 1 d . . .
C14 C 0.72773(10) 0.23415(8) 0.89579(9) 0.0295(2) Uani 1 1 d . . .
H14A H 0.7088 0.2763 0.9497 0.035 Uiso 1 1 calc R . .
H14B H 0.7874 0.1842 0.9004 0.035 Uiso 1 1 calc R . .
C15 C 0.76372(10) 0.29296(8) 0.79679(9) 0.0283(2) Uani 1 1 d . . .
C16 C 0.82800(10) 0.24389(8) 0.71423(9) 0.0300(2) Uani 1 1 d . . .
H16 H 0.8488 0.1766 0.7222 0.036 Uiso 1 1 calc R . .
C17 C 0.86177(10) 0.29202(8) 0.62097(9) 0.0302(2) Uani 1 1 d . . .
C18 C 0.83327(10) 0.39033(8) 0.60956(9) 0.0307(2) Uani 1 1 d . . .
C19 C 0.77013(10) 0.44015(8) 0.68979(9) 0.0312(2) Uani 1 1 d . . .
H19 H 0.7516 0.5077 0.6809 0.037 Uiso 1 1 calc R . .
C20 C 0.73296(10) 0.39267(8) 0.78407(9) 0.0293(2) Uani 1 1 d . . .
C21 C 0.65840(10) 0.45189(8) 0.86787(9) 0.0300(2) Uani 1 1 d . . .
H21A H 0.6825 0.5151 0.8586 0.036 Uiso 1 1 calc R . .
H21B H 0.6622 0.4192 0.9314 0.036 Uiso 1 1 calc R . .
C22 C 0.38273(11) 0.72712(9) 0.75805(10) 0.0360(3) Uani 1 1 d . . .
C23 C 0.34689(11) 0.79191(9) 0.68338(10) 0.0371(3) Uani 1 1 d . . .
C24 C 0.35513(13) 0.88882(10) 0.67466(12) 0.0456(3) Uani 1 1 d . . .
H24 H 0.3825 0.9134 0.7157 0.055 Uiso 1 1 calc R . .
C25 C 0.32233(15) 0.94855(12) 0.60439(13) 0.0552(4) Uani 1 1 d . . .
H25 H 0.3270 1.0149 0.5991 0.066 Uiso 1 1 calc R . .
C26 C 0.27718(13) 0.82538(12) 0.55361(12) 0.0489(4) Uani 1 1 d . . .
H26 H 0.2499 0.8028 0.5113 0.059 Uiso 1 1 calc R . .
C27 C 0.30693(11) 0.75906(11) 0.62227(10) 0.0415(3) Uani 1 1 d . . .
H27 H 0.2999 0.6933 0.6269 0.050 Uiso 1 1 calc R . .
C28 C 0.16355(11) 0.60128(9) 0.92952(10) 0.0357(3) Uani 1 1 d . . .
C29 C 0.05565(11) 0.62214(9) 0.92075(10) 0.0364(3) Uani 1 1 d . . .
C30 C -0.01233(13) 0.70258(13) 0.95855(16) 0.0610(5) Uani 1 1 d . . .
H30 H 0.0081 0.7434 0.9919 0.073 Uiso 1 1 calc R . .
C31 C -0.11100(14) 0.72376(14) 0.94757(17) 0.0647(5) Uani 1 1 d . . .
H31 H -0.1559 0.7808 0.9724 0.078 Uiso 1 1 calc R . .
C32 C -0.08213(14) 0.58883(13) 0.87282(14) 0.0564(4) Uani 1 1 d . . .
H32 H -0.1069 0.5470 0.8442 0.068 Uiso 1 1 calc R . .
C33 C 0.01898(13) 0.56223(12) 0.87904(13) 0.0490(4) Uani 1 1 d . . .
H33 H 0.0618 0.5041 0.8550 0.059 Uiso 1 1 calc R . .
C34 C 0.31156(11) 0.09829(9) 0.87483(10) 0.0353(3) Uani 1 1 d . . .
C35 C 0.22987(12) 0.03958(9) 0.87931(10) 0.0385(3) Uani 1 1 d . . .
C36 C 0.14985(14) 0.08154(11) 0.84219(13) 0.0489(4) Uani 1 1 d . . .
H36 H 0.1459 0.1468 0.8162 0.059 Uiso 1 1 calc R . .
C37 C 0.07621(15) 0.02558(12) 0.84413(15) 0.0582(4) Uani 1 1 d . . .
H37 H 0.0217 0.0544 0.8189 0.070 Uiso 1 1 calc R . .
C38 C 0.15523(13) -0.10561(11) 0.91502(12) 0.0479(4) Uani 1 1 d . . .
H38 H 0.1572 -0.1710 0.9407 0.057 Uiso 1 1 calc R . .
C39 C 0.23282(13) -0.05615(10) 0.91651(11) 0.0419(3) Uani 1 1 d . . .
H39 H 0.2865 -0.0868 0.9422 0.050 Uiso 1 1 calc R . .
C40 C 0.58129(11) -0.04776(8) 0.75441(9) 0.0340(2) Uani 1 1 d . . .
C41 C 0.63852(11) -0.14161(8) 0.71549(10) 0.0338(2) Uani 1 1 d . . .
C42 C 0.63211(13) -0.16504(10) 0.62961(11) 0.0436(3) Uani 1 1 d . . .
H42 H 0.5915 -0.1225 0.5960 0.052 Uiso 1 1 calc R . .
C43 C 0.68647(15) -0.25231(11) 0.59373(13) 0.0533(4) Uani 1 1 d . . .
H43 H 0.6811 -0.2684 0.5352 0.064 Uiso 1 1 calc R . .
C44 C 0.75249(13) -0.29012(9) 0.71829(11) 0.0425(3) Uani 1 1 d . . .
H44 H 0.7952 -0.3332 0.7494 0.051 Uiso 1 1 calc R . .
C45 C 0.70086(11) -0.20530(9) 0.76035(10) 0.0356(3) Uani 1 1 d . . .
H45 H 0.7080 -0.1910 0.8187 0.043 Uiso 1 1 calc R . .
C46 C 1.01133(10) 0.18502(9) 0.53017(9) 0.0332(2) Uani 1 1 d . . .
C47 C 1.04957(10) 0.12897(8) 0.44205(9) 0.0306(2) Uani 1 1 d . . .
C48 C 1.00716(11) 0.15023(9) 0.36771(10) 0.0354(3) Uani 1 1 d . . .
H48 H 0.9540 0.2043 0.3687 0.042 Uiso 1 1 calc R . .
C49 C 1.04443(12) 0.09035(10) 0.29173(11) 0.0394(3) Uani 1 1 d . . .
H49 H 1.0155 0.1045 0.2405 0.047 Uiso 1 1 calc R . .
C50 C 1.16008(11) -0.00456(9) 0.35894(10) 0.0377(3) Uani 1 1 d . . .
H50 H 1.2138 -0.0586 0.3559 0.045 Uiso 1 1 calc R . .
C51 C 1.12903(10) 0.05043(9) 0.43715(10) 0.0334(2) Uani 1 1 d . . .
H51 H 1.1607 0.0354 0.4864 0.040 Uiso 1 1 calc R . .
C52 C 0.80901(11) 0.45148(10) 0.46096(10) 0.0378(3) Uani 1 1 d . . .
C53 C 0.83896(12) 0.52705(10) 0.37762(10) 0.0389(3) Uani 1 1 d . . .
C54 C 0.92830(15) 0.57023(12) 0.35393(12) 0.0500(4) Uani 1 1 d . . .
H54 H 0.9759 0.5510 0.3892 0.060 Uiso 1 1 calc R . .
C55 C 0.94733(17) 0.64263(13) 0.27721(13) 0.0580(4) Uani 1 1 d . . .
H55 H 1.0095 0.6721 0.2604 0.070 Uiso 1 1 calc R . .
C56 C 0.79675(14) 0.63028(11) 0.24965(12) 0.0475(3) Uani 1 1 d . . .
H56 H 0.7499 0.6517 0.2139 0.057 Uiso 1 1 calc R . .
C57 C 0.77181(13) 0.55632(11) 0.32365(11) 0.0439(3) Uani 1 1 d . . .
H57 H 0.7106 0.5264 0.3372 0.053 Uiso 1 1 calc R . .
C58 C 0.49217(15) 0.37939(12) 0.54224(13) 0.0548(4) Uani 1 1 d . . .
H58 H 0.5184 0.4340 0.5493 0.066 Uiso 1 1 calc R . .
C59 C 0.53766(17) 0.30043(16) 0.68447(14) 0.0636(5) Uani 1 1 d . . .
H59A H 0.5632 0.3615 0.6793 0.095 Uiso 1 1 calc R . .
H59B H 0.5971 0.2478 0.6775 0.095 Uiso 1 1 calc R . .
H59C H 0.4811 0.2910 0.7492 0.095 Uiso 1 1 calc R . .
C60 C 0.45641(15) 0.21741(11) 0.59835(13) 0.0532(4) Uani 1 1 d . . .
H60A H 0.3861 0.2132 0.6502 0.080 Uiso 1 1 calc R . .
H60B H 0.5064 0.1602 0.6060 0.080 Uiso 1 1 calc R . .
H60C H 0.4502 0.2215 0.5332 0.080 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C22 1.1932(15) . ?
O2 C22 1.3685(16) . ?
O2 C3 1.3929(15) . ?
O3 C28 1.1978(16) . ?
O4 C28 1.3564(16) . ?
O4 C4 1.4149(16) . ?
O5 C34 1.1959(15) . ?
O6 C34 1.3684(16) . ?
O6 C10 1.3957(15) . ?
O7 C40 1.2028(16) . ?
O8 C40 1.3523(15) . ?
O8 C11 1.3992(14) . ?
O9 C46 1.1937(15) . ?
O10 C46 1.3708(15) . ?
O10 C17 1.3966(14) . ?
O11 C52 1.3655(16) . ?
O11 C18 1.3998(15) . ?
O12 C52 1.2070(17) . ?
O13 C58 1.252(2) . ?
N1 C26 1.332(2) . ?
N1 C25 1.335(2) . ?
N2 C31 1.319(2) . ?
N2 C32 1.334(2) . ?
N3 C38 1.340(2) . ?
N3 C37 1.342(2) . ?
N4 C44 1.3323(19) . ?
N4 C43 1.339(2) . ?
N5 C50 1.3324(18) . ?
N5 C49 1.3466(18) . ?
N6 C56 1.331(2) . ?
N6 C55 1.333(2) . ?
N7 C58 1.346(2) . ?
N7 C60 1.443(2) . ?
N7 C59 1.450(2) . ?
C1 C2 1.3989(17) . ?
C1 C6 1.4010(18) . ?
C1 C21 1.5292(17) . ?
C2 C3 1.3931(19) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(2) . ?
C4 C5 1.3764(18) . ?
C5 C6 1.4016(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.5171(16) . ?
C7 C8 1.5178(16) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.3944(17) . ?
C8 C13 1.4128(17) . ?
C9 C10 1.3882(17) . ?
C9 H9 0.9500 . ?
C10 C11 1.3877(18) . ?
C11 C12 1.3844(17) . ?
C12 C13 1.3949(16) . ?
C12 H12 0.9500 . ?
C13 C14 1.5178(17) . ?
C14 C15 1.5147(17) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.3947(16) . ?
C15 C20 1.4080(16) . ?
C16 C17 1.3811(18) . ?
C16 H16 0.9500 . ?
C17 C18 1.3833(16) . ?
C18 C19 1.3733(17) . ?
C19 C20 1.3923(18) . ?
C19 H19 0.9500 . ?
C20 C21 1.5172(16) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.4859(18) . ?
C23 C27 1.3798(19) . ?
C23 C24 1.390(2) . ?
C24 C25 1.384(2) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.393(2) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.4944(19) . ?
C29 C30 1.373(2) . ?
C29 C33 1.378(2) . ?
C30 C31 1.386(3) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.392(2) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.4919(19) . ?
C35 C39 1.3891(19) . ?
C35 C36 1.393(2) . ?
C36 C37 1.386(2) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.386(2) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.4916(18) . ?
C41 C42 1.3848(19) . ?
C41 C45 1.3866(18) . ?
C42 C43 1.389(2) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.3835(19) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.4905(17) . ?
C47 C48 1.3835(17) . ?
C47 C51 1.3924(17) . ?
C48 C49 1.3861(18) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.3730(18) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.4857(19) . ?
C53 C54 1.373(2) . ?
C53 C57 1.390(2) . ?
C54 C55 1.387(2) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.383(2) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 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
C22 O2 C3 119.02(9) . . ?
C28 O4 C4 115.88(10) . . ?
C34 O6 C10 116.47(9) . . ?
C40 O8 C11 118.23(9) . . ?
C46 O10 C17 118.43(9) . . ?
C52 O11 C18 115.16(10) . . ?
C26 N1 C25 116.78(13) . . ?
C31 N2 C32 116.27(14) . . ?
C38 N3 C37 116.82(13) . . ?
C44 N4 C43 116.69(13) . . ?
C50 N5 C49 117.31(11) . . ?
C56 N6 C55 117.43(13) . . ?
C58 N7 C60 119.27(15) . . ?
C58 N7 C59 121.84(15) . . ?
C60 N7 C59 118.89(14) . . ?
C2 C1 C6 119.23(11) . . ?
C2 C1 C21 117.94(11) . . ?
C6 C1 C21 122.83(10) . . ?
C3 C2 C1 120.51(12) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 O2 117.15(11) . . ?
C4 C3 C2 119.94(11) . . ?
O2 C3 C2 122.82(12) . . ?
C5 C4 C3 120.06(12) . . ?
C5 C4 O4 120.02(12) . . ?
C3 C4 O4 119.90(11) . . ?
C4 C5 C6 120.93(12) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.29(11) . . ?
C1 C6 C7 123.47(11) . . ?
C5 C6 C7 117.23(11) . . ?
C6 C7 C8 113.21(9) . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C13 119.20(10) . . ?
C9 C8 C7 117.71(11) . . ?
C13 C8 C7 123.09(11) . . ?
C10 C9 C8 121.26(12) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C11 C10 C9 119.27(11) . . ?
C11 C10 O6 119.41(10) . . ?
C9 C10 O6 121.20(12) . . ?
C12 C11 C10 120.31(11) . . ?
C12 C11 O8 116.24(11) . . ?
C10 C11 O8 123.21(11) . . ?
C11 C12 C13 121.05(12) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C8 118.80(11) . . ?
C12 C13 C14 117.49(11) . . ?
C8 C13 C14 123.67(10) . . ?
C15 C14 C13 111.50(9) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C20 119.18(11) . . ?
C16 C15 C14 117.26(10) . . ?
C20 C15 C14 123.53(11) . . ?
C17 C16 C15 120.77(10) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 119.62(11) . . ?
C16 C17 O10 122.06(10) . . ?
C18 C17 O10 118.15(11) . . ?
C19 C18 C17 120.61(11) . . ?
C19 C18 O11 118.16(10) . . ?
C17 C18 O11 121.18(11) . . ?
C18 C19 C20 120.68(10) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C19 C20 C15 119.10(11) . . ?
C19 C20 C21 117.48(10) . . ?
C15 C20 C21 123.40(11) . . ?
C20 C21 C1 112.33(9) . . ?
C20 C21 H21A 109.1 . . ?
C1 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
C1 C21 H21B 109.1 . . ?
H21A C21 H21B 107.9 . . ?
O1 C22 O2 123.80(11) . . ?
O1 C22 C23 125.62(12) . . ?
O2 C22 C23 110.57(11) . . ?
C27 C23 C24 119.22(13) . . ?
C27 C23 C22 122.37(12) . . ?
C24 C23 C22 118.41(12) . . ?
C25 C24 C23 118.03(15) . . ?
C25 C24 H24 121.0 . . ?
C23 C24 H24 121.0 . . ?
N1 C25 C24 123.99(16) . . ?
N1 C25 H25 118.0 . . ?
C24 C25 H25 118.0 . . ?
N1 C26 C27 124.07(15) . . ?
N1 C26 H26 118.0 . . ?
C27 C26 H26 118.0 . . ?
C23 C27 C26 117.90(14) . . ?
C23 C27 H27 121.1 . . ?
C26 C27 H27 121.1 . . ?
O3 C28 O4 123.14(12) . . ?
O3 C28 C29 124.32(12) . . ?
O4 C28 C29 112.54(11) . . ?
C30 C29 C33 117.75(14) . . ?
C30 C29 C28 119.30(13) . . ?
C33 C29 C28 122.91(13) . . ?
C29 C30 C31 119.39(15) . . ?
C29 C30 H30 120.3 . . ?
C31 C30 H30 120.3 . . ?
N2 C31 C30 123.93(16) . . ?
N2 C31 H31 118.0 . . ?
C30 C31 H31 118.0 . . ?
N2 C32 C33 123.96(16) . . ?
N2 C32 H32 118.0 . . ?
C33 C32 H32 118.0 . . ?
C29 C33 C32 118.55(15) . . ?
C29 C33 H33 120.7 . . ?
C32 C33 H33 120.7 . . ?
O5 C34 O6 123.49(12) . . ?
O5 C34 C35 124.47(12) . . ?
O6 C34 C35 112.03(10) . . ?
C39 C35 C36 119.00(13) . . ?
C39 C35 C34 122.21(12) . . ?
C36 C35 C34 118.76(12) . . ?
C37 C36 C35 118.29(13) . . ?
C37 C36 H36 120.9 . . ?
C35 C36 H36 120.9 . . ?
N3 C37 C36 123.71(14) . . ?
N3 C37 H37 118.1 . . ?
C36 C37 H37 118.1 . . ?
N3 C38 C39 124.13(14) . . ?
N3 C38 H38 117.9 . . ?
C39 C38 H38 117.9 . . ?
C38 C39 C35 118.05(13) . . ?
C38 C39 H39 121.0 . . ?
C35 C39 H39 121.0 . . ?
O7 C40 O8 123.97(12) . . ?
O7 C40 C41 125.31(12) . . ?
O8 C40 C41 110.72(10) . . ?
C42 C41 C45 118.51(12) . . ?
C42 C41 C40 118.99(12) . . ?
C45 C41 C40 122.47(11) . . ?
C41 C42 C43 118.40(13) . . ?
C41 C42 H42 120.8 . . ?
C43 C42 H42 120.8 . . ?
N4 C43 C42 123.79(14) . . ?
N4 C43 H43 118.1 . . ?
C42 C43 H43 118.1 . . ?
N4 C44 C45 123.99(13) . . ?
N4 C44 H44 118.0 . . ?
C45 C44 H44 118.0 . . ?
C44 C45 C41 118.59(12) . . ?
C44 C45 H45 120.7 . . ?
C41 C45 H45 120.7 . . ?
O9 C46 O10 124.39(11) . . ?
O9 C46 C47 125.34(12) . . ?
O10 C46 C47 110.25(10) . . ?
C48 C47 C51 119.49(11) . . ?
C48 C47 C46 122.72(11) . . ?
C51 C47 C46 117.76(11) . . ?
C47 C48 C49 118.05(12) . . ?
C47 C48 H48 121.0 . . ?
C49 C48 H48 121.0 . . ?
N5 C49 C48 123.13(12) . . ?
N5 C49 H49 118.4 . . ?
C48 C49 H49 118.4 . . ?
N5 C50 C51 124.11(12) . . ?
N5 C50 H50 117.9 . . ?
C51 C50 H50 117.9 . . ?
C50 C51 C47 117.88(12) . . ?
C50 C51 H51 121.1 . . ?
C47 C51 H51 121.1 . . ?
O12 C52 O11 123.23(12) . . ?
O12 C52 C53 125.44(13) . . ?
O11 C52 C53 111.32(12) . . ?
C54 C53 C57 119.25(13) . . ?
C54 C53 C52 122.56(13) . . ?
C57 C53 C52 118.17(14) . . ?
C53 C54 C55 118.29(15) . . ?
C53 C54 H54 120.9 . . ?
C55 C54 H54 120.9 . . ?
N6 C55 C54 123.46(16) . . ?
N6 C55 H55 118.3 . . ?
C54 C55 H55 118.3 . . ?
N6 C56 C57 123.51(15) . . ?
N6 C56 H56 118.2 . . ?
C57 C56 H56 118.2 . . ?
C56 C57 C53 118.04(15) . . ?
C56 C57 H57 121.0 . . ?
C53 C57 H57 121.0 . . ?
O13 C58 N7 124.70(17) . . ?
O13 C58 H58 117.6 . . ?
N7 C58 H58 117.6 . . ?
N7 C59 H59A 109.5 . . ?
N7 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
N7 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N7 C60 H60A 109.5 . . ?
N7 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
N7 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.874
_diffrn_reflns_theta_full        36.20
_diffrn_measured_fraction_theta_full 0.874
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.063
####################################################################### 
# 
# 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_cobrsqd
_database_code_depnum_ccdc_archive 'CCDC 1823171'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'hexabromobis{hexakis(isonicotinoyl)cyclotricatechylene}tricobalt(II) dimethylformamide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H86 Br6 Co3 N14 O26'
_chemical_formula_weight         2796.28

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   35.9310(11)
_cell_length_b                   20.5186(5)
_cell_length_c                   32.4986(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.330(3)
_cell_angle_gamma                90.00
_cell_volume                     22318.5(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    46183
_cell_measurement_theta_min      1.13
_cell_measurement_theta_max      27.79

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5612
_exptl_absorpt_coefficient_mu    1.337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   
;
CCP4 7.0.040: AIMLESS, version 0.5.32 : 29/03/17
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.68890
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            79562
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0711
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.13
_diffrn_reflns_theta_max         25.17
_reflns_number_total             21159
_reflns_number_gt                12776
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         21159
_refine_ls_number_parameters     735
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0884
_refine_ls_wR_factor_ref         0.3030
_refine_ls_wR_factor_gt          0.2873
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.295895(18) 0.60594(3) 0.72702(2) 0.0943(2) Uani 1 1 d . . .
Br2 Br -0.20981(2) 0.81583(4) 0.77607(3) 0.1050(3) Uani 1 1 d . . .
Br3 Br 0.05814(3) 0.96460(3) 0.72053(3) 0.1056(3) Uani 1 1 d . . .
Co1 Co -0.253106(17) 0.71114(3) 0.750523(19) 0.0659(2) Uani 1 1 d . . .
Co2 Co 0.0000 0.96521(3) 0.7500 0.0717(3) Uani 1 2 d S . .
O1 O -0.07954(7) 0.53680(12) 0.87506(9) 0.0485(6) Uani 1 1 d . . .
O2 O -0.11966(8) 0.49867(16) 0.90966(9) 0.0614(8) Uani 1 1 d . . .
O3 O -0.08070(8) 0.40133(13) 0.87566(9) 0.0503(6) Uani 1 1 d . . .
O4 O -0.08879(10) 0.34595(17) 0.93264(11) 0.0709(8) Uani 1 1 d . . .
O5 O 0.07156(9) 0.24077(13) 0.88486(10) 0.0589(7) Uani 1 1 d . . .
O6 O 0.12627(12) 0.17969(16) 0.91560(13) 0.0844(10) Uani 1 1 d . . .
O7 O 0.13949(9) 0.30412(14) 0.88405(10) 0.0593(7) Uani 1 1 d . . .
O8 O 0.19863(10) 0.29029(19) 0.93935(12) 0.0815(10) Uani 1 1 d . . .
O9 O 0.14819(10) 0.61440(13) 0.88416(11) 0.0647(8) Uani 1 1 d . . .
O10 O 0.16675(13) 0.71204(18) 0.91599(13) 0.0906(12) Uani 1 1 d . . .
O11 O 0.08096(10) 0.68725(12) 0.87928(10) 0.0590(7) Uani 1 1 d . . .
O12 O 0.08676(12) 0.75621(15) 0.93551(12) 0.0806(10) Uani 1 1 d . . .
N1 N -0.20599(10) 0.6547(2) 0.79609(12) 0.0656(10) Uani 1 1 d . . .
N2 N -0.19921(12) 0.2648(2) 0.79719(13) 0.0695(11) Uani 1 1 d . . .
N3 N 0.03085(15) 0.03921(16) 0.79756(15) 0.0711(11) Uani 1 1 d . . .
N4 N 0.22285(11) 0.2305(2) 0.80134(13) 0.0698(11) Uani 1 1 d . . .
N5 N 0.22791(12) 0.69545(19) 0.79956(13) 0.0687(11) Uani 1 1 d . . .
N6 N 0.02960(17) 0.89183(18) 0.79897(15) 0.0830(13) Uani 1 1 d . . .
N7 N -0.1946(3) 0.3551(6) 0.9467(4) 0.1927(18) Uiso 1 1 d D . .
C1 C 0.01930(10) 0.50297(16) 0.95896(11) 0.0370(7) Uani 1 1 d . . .
C2 C -0.01428(10) 0.53530(16) 0.93063(13) 0.0412(8) Uani 1 1 d . . .
H2 H -0.0144 0.5816 0.9296 0.049 Uiso 1 1 calc R . .
C3 C -0.04720(10) 0.50132(17) 0.90412(12) 0.0436(8) Uani 1 1 d . . .
C4 C -0.04723(11) 0.43377(18) 0.90500(12) 0.0453(8) Uani 1 1 d . . .
C5 C -0.01435(11) 0.40113(17) 0.93254(12) 0.0425(8) Uani 1 1 d . . .
H5 H -0.0143 0.3548 0.9328 0.051 Uiso 1 1 calc R . .
C6 C 0.01901(10) 0.43474(16) 0.96005(12) 0.0392(8) Uani 1 1 d . . .
C7 C 0.05431(11) 0.39432(17) 0.99001(12) 0.0412(8) Uani 1 1 d . . .
H7A H 0.0708 0.4212 1.0154 0.049 Uiso 1 1 calc R . .
H7B H 0.0442 0.3564 1.0016 0.049 Uiso 1 1 calc R . .
C8 C 0.07963(11) 0.37093(16) 0.96484(12) 0.0418(8) Uani 1 1 d . . .
C9 C 0.06745(12) 0.31597(17) 0.93889(14) 0.0487(9) Uani 1 1 d . . .
H9 H 0.0445 0.2932 0.9390 0.058 Uiso 1 1 calc R . .
C10 C 0.08752(13) 0.29299(18) 0.91286(14) 0.0520(10) Uani 1 1 d . . .
C11 C 0.12124(12) 0.32517(19) 0.91321(13) 0.0506(9) Uani 1 1 d . . .
C12 C 0.13447(11) 0.38063(19) 0.93922(13) 0.0490(9) Uani 1 1 d . . .
H12 H 0.1576 0.4030 0.9392 0.059 Uiso 1 1 calc R . .
C13 C 0.11375(11) 0.40334(16) 0.96537(12) 0.0423(8) Uani 1 1 d . . .
C14 C 0.12967(11) 0.46534(16) 0.99148(13) 0.0436(8) Uani 1 1 d . . .
H14A H 0.1206 0.4674 1.0168 0.052 Uiso 1 1 calc R . .
H14B H 0.1592 0.4640 1.0034 0.052 Uiso 1 1 calc R . .
C15 C 0.11598(11) 0.52538(17) 0.96380(13) 0.0435(8) Uani 1 1 d . . .
C16 C 0.13764(12) 0.54626(18) 0.93831(14) 0.0501(9) Uani 1 1 d . . .
H16 H 0.1608 0.5227 0.9396 0.060 Uiso 1 1 calc R . .
C17 C 0.12643(13) 0.59970(19) 0.91151(15) 0.0558(10) Uani 1 1 d . . .
C18 C 0.09284(13) 0.63437(18) 0.90875(14) 0.0522(9) Uani 1 1 d . . .
C19 C 0.07090(11) 0.61541(17) 0.93364(13) 0.0459(9) Uani 1 1 d . . .
H19 H 0.0479 0.6398 0.9319 0.055 Uiso 1 1 calc R . .
C20 C 0.08157(10) 0.56157(17) 0.96112(12) 0.0400(8) Uani 1 1 d . . .
C21 C 0.05522(10) 0.54348(16) 0.98638(12) 0.0386(8) Uani 1 1 d . . .
H21A H 0.0457 0.5838 0.9962 0.046 Uiso 1 1 calc R . .
H21B H 0.0711 0.5185 1.0131 0.046 Uiso 1 1 calc R . .
C22 C -0.11503(12) 0.5324(2) 0.88136(15) 0.0529(10) Uani 1 1 d . . .
C23 C -0.14569(11) 0.5746(2) 0.85139(13) 0.0547(10) Uani 1 1 d . . .
C24 C -0.13713(13) 0.6222(2) 0.82489(16) 0.0633(11) Uani 1 1 d . . .
H24 H -0.1108 0.6270 0.8249 0.076 Uiso 1 1 calc R . .
C25 C -0.16756(13) 0.6614(2) 0.79899(16) 0.0684(12) Uani 1 1 d . . .
H25 H -0.1614 0.6948 0.7823 0.082 Uiso 1 1 calc R . .
C26 C -0.21293(13) 0.6082(3) 0.82159(16) 0.0714(13) Uani 1 1 d . . .
H26 H -0.2396 0.6023 0.8200 0.086 Uiso 1 1 calc R . .
C27 C -0.18454(13) 0.5693(2) 0.84916(15) 0.0648(11) Uani 1 1 d . . .
H27 H -0.1913 0.5383 0.8670 0.078 Uiso 1 1 calc R . .
C28 C -0.09911(13) 0.3578(2) 0.89385(17) 0.0622(11) Uani 1 1 d . . .
C29 C -0.13389(14) 0.3268(2) 0.85911(15) 0.0642(12) Uani 1 1 d . . .
C30 C -0.15308(14) 0.3538(3) 0.81753(16) 0.0709(13) Uani 1 1 d . . .
H30 H -0.1441 0.3936 0.8095 0.085 Uiso 1 1 calc R . .
C31 C -0.18497(16) 0.3220(3) 0.78878(17) 0.0797(15) Uani 1 1 d . . .
H31 H -0.1982 0.3413 0.7607 0.096 Uiso 1 1 calc R . .
C32 C -0.18068(16) 0.2406(3) 0.83767(16) 0.0751(14) Uani 1 1 d . . .
H32 H -0.1904 0.2009 0.8450 0.090 Uiso 1 1 calc R . .
C33 C -0.14799(15) 0.2697(3) 0.86987(16) 0.0713(13) Uani 1 1 d . . .
H33 H -0.1359 0.2507 0.8983 0.086 Uiso 1 1 calc R . .
C34 C 0.09323(17) 0.1860(2) 0.88912(17) 0.0681(12) Uani 1 1 d . . .
C35 C 0.07015(15) 0.1354(2) 0.85710(17) 0.0670(12) Uani 1 1 d . . .
C36 C 0.03014(16) 0.1408(2) 0.83331(17) 0.0718(13) Uani 1 1 d . . .
H36 H 0.0155 0.1779 0.8364 0.086 Uiso 1 1 calc R . .
C37 C 0.01135(17) 0.0906(2) 0.80448(18) 0.0741(13) Uani 1 1 d . . .
H37 H -0.0167 0.0931 0.7890 0.089 Uiso 1 1 calc R . .
C38 C 0.06945(19) 0.0356(2) 0.8203(2) 0.0840(16) Uani 1 1 d . . .
H38 H 0.0836 -0.0008 0.8154 0.101 Uiso 1 1 calc R . .
C39 C 0.09048(18) 0.0812(2) 0.85060(19) 0.0846(16) Uani 1 1 d . . .
H39 H 0.1183 0.0759 0.8667 0.101 Uiso 1 1 calc R . .
C40 C 0.17859(14) 0.2884(2) 0.90110(17) 0.0659(12) Uani 1 1 d . . .
C41 C 0.19311(15) 0.2666(2) 0.86584(16) 0.0689(13) Uani 1 1 d . . .
C42 C 0.16768(13) 0.2454(3) 0.82461(16) 0.0689(12) Uani 1 1 d . . .
H42 H 0.1396 0.2436 0.8175 0.083 Uiso 1 1 calc R . .
C43 C 0.18434(15) 0.2271(3) 0.79431(17) 0.0771(14) Uani 1 1 d . . .
H43 H 0.1670 0.2109 0.7666 0.093 Uiso 1 1 calc R . .
C44 C 0.24740(15) 0.2518(3) 0.84132(17) 0.0829(16) Uani 1 1 d . . .
H44 H 0.2752 0.2550 0.8469 0.099 Uiso 1 1 calc R . .
C45 C 0.23356(15) 0.2694(3) 0.87478(18) 0.0817(15) Uani 1 1 d . . .
H45 H 0.2516 0.2829 0.9029 0.098 Uiso 1 1 calc R . .
C46 C 0.16770(17) 0.6722(3) 0.89029(19) 0.0773(14) Uani 1 1 d . . .
C47 C 0.18932(15) 0.6781(2) 0.85886(17) 0.0688(12) Uani 1 1 d . . .
C48 C 0.19491(15) 0.6260(2) 0.83485(17) 0.0692(12) Uani 1 1 d . . .
H48 H 0.1855 0.5838 0.8381 0.083 Uiso 1 1 calc R . .
C49 C 0.21459(15) 0.6368(2) 0.80582(17) 0.0725(13) Uani 1 1 d . . .
H49 H 0.2188 0.6008 0.7896 0.087 Uiso 1 1 calc R . .
C50 C 0.22158(18) 0.7451(3) 0.82285(18) 0.0812(15) Uani 1 1 d . . .
H50 H 0.2306 0.7872 0.8186 0.097 Uiso 1 1 calc R . .
C51 C 0.20283(18) 0.7386(3) 0.85234(19) 0.0842(16) Uani 1 1 d . . .
H51 H 0.1991 0.7754 0.8682 0.101 Uiso 1 1 calc R . .
C52 C 0.07835(17) 0.7461(2) 0.89687(19) 0.0705(13) Uani 1 1 d . . .
C53 C 0.06286(18) 0.7957(2) 0.86217(17) 0.0729(13) Uani 1 1 d . . .
C54 C 0.06207(18) 0.7884(2) 0.81951(17) 0.0762(14) Uani 1 1 d . . .
H54 H 0.0721 0.7499 0.8110 0.091 Uiso 1 1 calc R . .
C55 C 0.04624(18) 0.8387(2) 0.78933(18) 0.0790(15) Uani 1 1 d . . .
H55 H 0.0473 0.8350 0.7607 0.095 Uiso 1 1 calc R . .
C56 C 0.0304(2) 0.8988(2) 0.84020(19) 0.096(2) Uani 1 1 d . . .
H56 H 0.0192 0.9372 0.8473 0.115 Uiso 1 1 calc R . .
C57 C 0.0468(2) 0.8526(2) 0.87320(19) 0.0918(18) Uani 1 1 d . . .
H57 H 0.0471 0.8592 0.9022 0.110 Uiso 1 1 calc R . .
C58 C -0.1858(5) 0.4122(7) 0.9304(4) 0.1927(18) Uiso 1 1 d . . .
H58 H -0.1586 0.4228 0.9362 0.231 Uiso 1 1 calc R . .
C59 C -0.1606(4) 0.3151(6) 0.9752(4) 0.1927(18) Uiso 1 1 d . . .
H59A H -0.1367 0.3253 0.9686 0.289 Uiso 1 1 calc R . .
H59B H -0.1671 0.2688 0.9695 0.289 Uiso 1 1 calc R . .
H59C H -0.1555 0.3248 1.0063 0.289 Uiso 1 1 calc R . .
C60 C -0.2315(4) 0.3484(7) 0.9624(4) 0.1927(18) Uiso 1 1 d D . .
H60A H -0.2565 0.3505 0.9367 0.289 Uiso 1 1 calc R . .
H60B H -0.2308 0.3840 0.9828 0.289 Uiso 1 1 calc R . .
H60C H -0.2300 0.3065 0.9775 0.289 Uiso 1 1 calc R . .
O13 O -0.2127(3) 0.4516(4) 0.9077(3) 0.1927(18) Uiso 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
Br1 Co1 2.5984(10) . ?
Br2 Co1 2.6045(11) . ?
Br3 Co2 2.5955(8) . ?
Co1 N1 2.140(4) . ?
Co1 N2 2.149(4) 4_456 ?
Co1 N5 2.155(3) 2_556 ?
Co1 N4 2.161(4) 3_455 ?
Co2 N3 2.163(4) 2_566 ?
Co2 N3 2.163(4) 1_565 ?
Co2 N6 2.168(4) 2_556 ?
Co2 N6 2.168(4) . ?
Co2 Br3 2.5955(8) 2_556 ?
O1 C22 1.366(5) . ?
O1 C3 1.405(4) . ?
O2 C22 1.210(5) . ?
O3 C28 1.366(5) . ?
O3 C4 1.402(4) . ?
O4 C28 1.203(5) . ?
O5 C34 1.345(5) . ?
O5 C10 1.388(5) . ?
O6 C34 1.193(6) . ?
O7 C40 1.348(5) . ?
O7 C11 1.402(5) . ?
O8 C40 1.189(5) . ?
O9 C46 1.354(6) . ?
O9 C17 1.413(5) . ?
O10 C46 1.178(6) . ?
O11 C52 1.354(6) . ?
O11 C18 1.407(5) . ?
O12 C52 1.198(6) . ?
N1 C26 1.345(6) . ?
N1 C25 1.356(5) . ?
N2 C32 1.335(6) . ?
N2 C31 1.348(6) . ?
N2 Co1 2.149(4) 4_446 ?
N3 C38 1.315(7) . ?
N3 C37 1.329(6) . ?
N3 Co2 2.163(4) 1_545 ?
N4 C43 1.320(6) . ?
N4 C44 1.350(7) . ?
N4 Co1 2.161(4) 3_545 ?
N5 C50 1.337(6) . ?
N5 C49 1.338(6) . ?
N5 Co1 2.155(3) 2_556 ?
N6 C55 1.334(6) . ?
N6 C56 1.338(7) . ?
N7 C58 1.369(15) . ?
N7 C59 1.483(15) . ?
N7 C60 1.594(15) . ?
C1 C2 1.391(5) . ?
C1 C6 1.401(5) . ?
C1 C21 1.521(5) . ?
C2 C3 1.373(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(5) . ?
C4 C5 1.370(5) . ?
C5 C6 1.390(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.532(5) . ?
C7 C8 1.506(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.381(5) . ?
C8 C13 1.389(5) . ?
C9 C10 1.379(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.376(6) . ?
C11 C12 1.394(6) . ?
C12 C13 1.398(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.521(5) . ?
C14 C15 1.499(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.395(5) . ?
C15 C20 1.417(5) . ?
C16 C17 1.367(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.376(6) . ?
C18 C19 1.375(5) . ?
C19 C20 1.384(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.508(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.460(6) . ?
C23 C27 1.376(6) . ?
C23 C24 1.407(6) . ?
C24 C25 1.372(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.347(6) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.488(6) . ?
C29 C33 1.371(6) . ?
C29 C30 1.389(7) . ?
C30 C31 1.354(7) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.392(7) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.490(7) . ?
C35 C36 1.367(7) . ?
C35 C39 1.387(6) . ?
C36 C37 1.391(7) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.369(8) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.490(6) . ?
C41 C45 1.376(7) . ?
C41 C42 1.389(7) . ?
C42 C43 1.378(6) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.398(7) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.496(7) . ?
C47 C51 1.378(7) . ?
C47 C48 1.380(7) . ?
C48 C49 1.387(6) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.364(7) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.470(7) . ?
C53 C54 1.384(7) . ?
C53 C57 1.405(7) . ?
C54 C55 1.395(7) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.393(8) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 O13 1.270(14) . ?
C58 H58 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 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
N1 Co1 N2 177.67(15) . 4_456 ?
N1 Co1 N5 89.88(13) . 2_556 ?
N2 Co1 N5 88.57(14) 4_456 2_556 ?
N1 Co1 N4 90.36(14) . 3_455 ?
N2 Co1 N4 91.25(14) 4_456 3_455 ?
N5 Co1 N4 177.72(17) 2_556 3_455 ?
N1 Co1 Br1 89.33(12) . . ?
N2 Co1 Br1 88.97(13) 4_456 . ?
N5 Co1 Br1 91.16(12) 2_556 . ?
N4 Co1 Br1 91.11(13) 3_455 . ?
N1 Co1 Br2 89.74(12) . . ?
N2 Co1 Br2 91.99(13) 4_456 . ?
N5 Co1 Br2 89.86(12) 2_556 . ?
N4 Co1 Br2 87.88(13) 3_455 . ?
Br1 Co1 Br2 178.62(3) . . ?
N3 Co2 N3 90.8(2) 2_566 1_565 ?
N3 Co2 N6 88.62(17) 2_566 2_556 ?
N3 Co2 N6 177.99(17) 1_565 2_556 ?
N3 Co2 N6 177.99(17) 2_566 . ?
N3 Co2 N6 88.62(17) 1_565 . ?
N6 Co2 N6 92.0(2) 2_556 . ?
N3 Co2 Br3 89.71(13) 2_566 2_556 ?
N3 Co2 Br3 90.68(13) 1_565 2_556 ?
N6 Co2 Br3 91.24(14) 2_556 2_556 ?
N6 Co2 Br3 88.37(14) . 2_556 ?
N3 Co2 Br3 90.68(13) 2_566 . ?
N3 Co2 Br3 89.71(13) 1_565 . ?
N6 Co2 Br3 88.37(14) 2_556 . ?
N6 Co2 Br3 91.25(14) . . ?
Br3 Co2 Br3 179.44(4) 2_556 . ?
C22 O1 C3 117.0(3) . . ?
C28 O3 C4 116.5(3) . . ?
C34 O5 C10 119.5(4) . . ?
C40 O7 C11 118.0(3) . . ?
C46 O9 C17 118.0(3) . . ?
C52 O11 C18 116.8(3) . . ?
C26 N1 C25 116.2(4) . . ?
C26 N1 Co1 122.2(3) . . ?
C25 N1 Co1 121.5(3) . . ?
C32 N2 C31 115.7(4) . . ?
C32 N2 Co1 120.1(3) . 4_446 ?
C31 N2 Co1 124.2(3) . 4_446 ?
C38 N3 C37 117.5(4) . . ?
C38 N3 Co2 121.6(3) . 1_545 ?
C37 N3 Co2 120.8(4) . 1_545 ?
C43 N4 C44 117.4(4) . . ?
C43 N4 Co1 122.9(3) . 3_545 ?
C44 N4 Co1 119.5(3) . 3_545 ?
C50 N5 C49 117.1(4) . . ?
C50 N5 Co1 121.2(3) . 2_556 ?
C49 N5 Co1 121.4(3) . 2_556 ?
C55 N6 C56 118.4(4) . . ?
C55 N6 Co2 122.5(3) . . ?
C56 N6 Co2 119.1(3) . . ?
C58 N7 C59 117.6(12) . . ?
C58 N7 C60 122.3(12) . . ?
C59 N7 C60 110.1(10) . . ?
C2 C1 C6 118.7(3) . . ?
C2 C1 C21 118.3(3) . . ?
C6 C1 C21 122.9(3) . . ?
C3 C2 C1 121.0(3) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 120.1(3) . . ?
C2 C3 O1 118.1(3) . . ?
C4 C3 O1 121.7(3) . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 O3 122.3(3) . . ?
C3 C4 O3 117.9(3) . . ?
C4 C5 C6 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C7 117.5(3) . . ?
C1 C6 C7 123.0(3) . . ?
C8 C7 C6 110.6(3) . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C13 118.7(3) . . ?
C9 C8 C7 118.2(3) . . ?
C13 C8 C7 123.1(3) . . ?
C10 C9 C8 122.3(4) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C11 C10 C9 119.1(4) . . ?
C11 C10 O5 121.9(3) . . ?
C9 C10 O5 118.9(4) . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 O7 118.3(4) . . ?
C12 C11 O7 121.4(4) . . ?
C11 C12 C13 120.1(4) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C8 C13 C12 119.7(3) . . ?
C8 C13 C14 123.9(3) . . ?
C12 C13 C14 116.3(3) . . ?
C15 C14 C13 112.2(3) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 C20 117.7(3) . . ?
C16 C15 C14 118.5(3) . . ?
C20 C15 C14 123.8(3) . . ?
C17 C16 C15 121.8(3) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 120.3(3) . . ?
C16 C17 O9 118.0(4) . . ?
C18 C17 O9 121.4(4) . . ?
C19 C18 C17 119.5(4) . . ?
C19 C18 O11 121.4(4) . . ?
C17 C18 O11 119.0(3) . . ?
C18 C19 C20 121.5(3) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 H19 119.3 . . ?
C19 C20 C15 119.2(3) . . ?
C19 C20 C21 117.8(3) . . ?
C15 C20 C21 123.0(3) . . ?
C20 C21 C1 112.5(3) . . ?
C20 C21 H21A 109.1 . . ?
C1 C21 H21A 109.1 . . ?
C20 C21 H21B 109.1 . . ?
C1 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
O2 C22 O1 123.1(4) . . ?
O2 C22 C23 124.6(4) . . ?
O1 C22 C23 112.3(3) . . ?
C27 C23 C24 117.8(4) . . ?
C27 C23 C22 119.5(4) . . ?
C24 C23 C22 122.7(3) . . ?
C25 C24 C23 118.6(4) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
N1 C25 C24 123.2(4) . . ?
N1 C25 H25 118.4 . . ?
C24 C25 H25 118.4 . . ?
N1 C26 C27 124.4(4) . . ?
N1 C26 H26 117.8 . . ?
C27 C26 H26 117.8 . . ?
C26 C27 C23 119.8(4) . . ?
C26 C27 H27 120.1 . . ?
C23 C27 H27 120.1 . . ?
O4 C28 O3 125.0(4) . . ?
O4 C28 C29 124.2(4) . . ?
O3 C28 C29 110.8(4) . . ?
C33 C29 C30 119.3(4) . . ?
C33 C29 C28 117.3(4) . . ?
C30 C29 C28 123.4(4) . . ?
C31 C30 C29 118.3(4) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
N2 C31 C30 124.7(5) . . ?
N2 C31 H31 117.7 . . ?
C30 C31 H31 117.7 . . ?
N2 C32 C33 124.3(4) . . ?
N2 C32 H32 117.8 . . ?
C33 C32 H32 117.8 . . ?
C29 C33 C32 117.6(5) . . ?
C29 C33 H33 121.2 . . ?
C32 C33 H33 121.2 . . ?
O6 C34 O5 123.5(4) . . ?
O6 C34 C35 125.6(4) . . ?
O5 C34 C35 110.9(4) . . ?
C36 C35 C39 118.9(5) . . ?
C36 C35 C34 122.8(4) . . ?
C39 C35 C34 118.3(5) . . ?
C35 C36 C37 118.3(4) . . ?
C35 C36 H36 120.9 . . ?
C37 C36 H36 120.9 . . ?
N3 C37 C36 123.0(5) . . ?
N3 C37 H37 118.5 . . ?
C36 C37 H37 118.5 . . ?
N3 C38 C39 124.0(4) . . ?
N3 C38 H38 118.0 . . ?
C39 C38 H38 118.0 . . ?
C38 C39 C35 118.3(5) . . ?
C38 C39 H39 120.9 . . ?
C35 C39 H39 120.9 . . ?
O8 C40 O7 124.5(4) . . ?
O8 C40 C41 124.4(4) . . ?
O7 C40 C41 111.1(4) . . ?
C45 C41 C42 119.4(4) . . ?
C45 C41 C40 117.6(5) . . ?
C42 C41 C40 123.0(4) . . ?
C43 C42 C41 118.1(4) . . ?
C43 C42 H42 121.0 . . ?
C41 C42 H42 121.0 . . ?
N4 C43 C42 124.2(5) . . ?
N4 C43 H43 117.9 . . ?
C42 C43 H43 117.9 . . ?
N4 C44 C45 122.6(5) . . ?
N4 C44 H44 118.7 . . ?
C45 C44 H44 118.7 . . ?
C41 C45 C44 118.2(5) . . ?
C41 C45 H45 120.9 . . ?
C44 C45 H45 120.9 . . ?
O10 C46 O9 124.4(4) . . ?
O10 C46 C47 125.7(5) . . ?
O9 C46 C47 109.9(4) . . ?
C51 C47 C48 118.6(4) . . ?
C51 C47 C46 118.5(5) . . ?
C48 C47 C46 122.8(4) . . ?
C47 C48 C49 118.4(4) . . ?
C47 C48 H48 120.8 . . ?
C49 C48 H48 120.8 . . ?
N5 C49 C48 123.1(4) . . ?
N5 C49 H49 118.5 . . ?
C48 C49 H49 118.5 . . ?
N5 C50 C51 123.6(4) . . ?
N5 C50 H50 118.2 . . ?
C51 C50 H50 118.2 . . ?
C50 C51 C47 119.2(5) . . ?
C50 C51 H51 120.4 . . ?
C47 C51 H51 120.4 . . ?
O12 C52 O11 124.6(4) . . ?
O12 C52 C53 124.4(4) . . ?
O11 C52 C53 111.0(4) . . ?
C54 C53 C57 119.0(5) . . ?
C54 C53 C52 123.9(4) . . ?
C57 C53 C52 117.1(5) . . ?
C53 C54 C55 118.6(4) . . ?
C53 C54 H54 120.7 . . ?
C55 C54 H54 120.7 . . ?
N6 C55 C54 122.9(5) . . ?
N6 C55 H55 118.6 . . ?
C54 C55 H55 118.6 . . ?
N6 C56 C57 123.2(5) . . ?
N6 C56 H56 118.4 . . ?
C57 C56 H56 118.4 . . ?
C56 C57 C53 117.9(5) . . ?
C56 C57 H57 121.1 . . ?
C53 C57 H57 121.1 . . ?
O13 C58 N7 122.4(14) . . ?
O13 C58 H58 118.8 . . ?
N7 C58 H58 118.8 . . ?
N7 C59 H59A 109.5 . . ?
N7 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
N7 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
N7 C60 H60A 109.5 . . ?
N7 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
N7 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        25.17
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.120
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 -0.004 0.000 -0.007 12889 3133 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
# start Validation Reply Form
_vrf_DIFF019_I                   
;
PROBLEM: _diffrn_standards_number is missing
RESPONSE: not relevant
;
_vrf_DIFF020_I                   
;
PROBLEM: _diffrn_standards_interval_count and
RESPONSE: not relevant
;
_vrf_DIFF022_I                   
;
PROBLEM: _diffrn_standards_decay_% is missing
RESPONSE: not relevant
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1823170'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'hexachlorobis{hexakis(isonicotinoyl)cyclotricatechylene}tricobalt(II) dimethylformamide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C114 H72 Cl6 Co3 N12 O24'
_chemical_formula_weight         2383.33

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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   35.226(3)
_cell_length_b                   20.1867(12)
_cell_length_c                   33.622(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.454(9)
_cell_angle_gamma                90.00
_cell_volume                     22401(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7383
_cell_measurement_theta_min      4.106
_cell_measurement_theta_max      66.357

_exptl_crystal_description       plate
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4860
_exptl_absorpt_coefficient_mu    2.702
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7739
_exptl_absorpt_correction_T_max  0.9233
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.735
_oxdiff_exptl_absorpt_empirical_full_max 2.052
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'micro-focus sealed X-ray tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean .
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            70212
_diffrn_reflns_av_R_equivalents  0.1669
_diffrn_reflns_av_sigmaI/netI    0.1146
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         55.00
_reflns_number_total             14078
_reflns_number_gt                7635
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14078
_refine_ls_number_parameters     717
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1674
_refine_ls_R_factor_gt           0.1297
_refine_ls_wR_factor_ref         0.3663
_refine_ls_wR_factor_gt          0.3405
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.74764(4) 0.78053(8) 0.24991(4) 0.0824(5) Uani 1 1 d . . .
Co2 Co 0.5000 1.02817(8) 0.2500 0.0944(7) Uani 1 2 d S . .
Cl1 Cl 0.78675(9) 0.68086(17) 0.26935(11) 0.1327(11) Uani 1 1 d . . .
Cl2 Cl 0.70692(8) 0.87856(16) 0.22959(9) 0.1180(9) Uani 1 1 d . . .
Cl3 Cl 0.44422(11) 1.02968(14) 0.27503(11) 0.1379(11) Uani 1 1 d . . .
O1 O 0.64069(15) 0.6863(3) 0.38320(16) 0.0755(14) Uani 1 1 d . . .
O2 O 0.7011(2) 0.6998(4) 0.4342(2) 0.118(2) Uani 1 1 d . . .
O3 O 0.57211(16) 0.7532(3) 0.38427(17) 0.0781(14) Uani 1 1 d . . .
O4 O 0.6278(3) 0.8173(3) 0.4116(3) 0.123(2) Uani 1 1 d . . .
O5 O 0.41780(14) 0.5909(3) 0.37861(15) 0.0672(13) Uani 1 1 d . . .
O6 O 0.40863(19) 0.6502(3) 0.4310(2) 0.0959(18) Uani 1 1 d . . .
O7 O 0.42107(15) 0.4526(3) 0.38009(17) 0.0760(14) Uani 1 1 d . . .
O8 O 0.37861(16) 0.4894(3) 0.41131(18) 0.0879(16) Uani 1 1 d . . .
O9 O 0.5797(2) 0.3040(3) 0.3824(2) 0.0939(18) Uani 1 1 d . . .
O10 O 0.5830(3) 0.2328(3) 0.4337(3) 0.137(3) Uani 1 1 d . . .
O11 O 0.6480(2) 0.3766(3) 0.3859(2) 0.0958(19) Uani 1 1 d . . .
O12 O 0.6660(3) 0.2778(4) 0.4134(3) 0.136(3) Uani 1 1 d . . .
N1 N 0.7230(2) 0.7572(4) 0.2982(3) 0.090(2) Uani 1 1 d . . .
N2 N 0.5285(3) 0.9527(3) 0.2947(3) 0.107(3) Uani 1 1 d . . .
N3 N 0.3000(2) 0.7294(5) 0.2970(2) 0.105(3) Uani 1 1 d . . .
N4 N 0.29455(19) 0.3395(4) 0.2958(2) 0.085(2) Uani 1 1 d . . .
N5 N 0.5301(3) 0.1027(4) 0.2984(4) 0.122(3) Uani 1 1 d . . .
N6 N 0.7254(2) 0.2992(5) 0.2977(2) 0.104(3) Uani 1 1 d . . .
C1 C 0.6158(2) 0.5902(3) 0.4648(2) 0.0590(17) Uani 1 1 d . . .
C2 C 0.6359(2) 0.6136(4) 0.4381(2) 0.0654(19) Uani 1 1 d . . .
H2 H 0.6594 0.5908 0.4376 0.079 Uiso 1 1 calc R . .
C3 C 0.6231(3) 0.6682(4) 0.4127(2) 0.075(2) Uani 1 1 d . . .
C4 C 0.5888(3) 0.7003(4) 0.4123(2) 0.078(2) Uani 1 1 d . . .
C5 C 0.5669(2) 0.6797(3) 0.4379(2) 0.0638(19) Uani 1 1 d . . .
H5 H 0.5432 0.7026 0.4376 0.077 Uiso 1 1 calc R . .
C6 C 0.5811(2) 0.6240(3) 0.4641(2) 0.0567(17) Uani 1 1 d . . .
C7 C 0.5540(2) 0.6008(3) 0.4888(2) 0.0573(17) Uani 1 1 d . . .
H7A H 0.5704 0.5746 0.5138 0.069 Uiso 1 1 calc R . .
H7B H 0.5433 0.6400 0.4992 0.069 Uiso 1 1 calc R . .
C8 C 0.51913(19) 0.5594(3) 0.4614(2) 0.0544(16) Uani 1 1 d . . .
C9 C 0.4846(2) 0.5922(4) 0.4343(2) 0.0611(18) Uani 1 1 d . . .
H9 H 0.4840 0.6392 0.4345 0.073 Uiso 1 1 calc R . .
C10 C 0.4526(3) 0.5595(4) 0.4081(3) 0.070(2) Uani 1 1 d . . .
C11 C 0.4533(2) 0.4912(4) 0.4084(2) 0.0619(19) Uani 1 1 d . . .
C12 C 0.4860(2) 0.4551(3) 0.4349(2) 0.0583(17) Uani 1 1 d . . .
H12 H 0.4852 0.4081 0.4352 0.070 Uiso 1 1 calc R . .
C13 C 0.5201(2) 0.4898(3) 0.4610(2) 0.0551(17) Uani 1 1 d . . .
C14 C 0.55604(18) 0.4486(3) 0.48731(19) 0.0482(15) Uani 1 1 d . . .
H14A H 0.5719 0.4738 0.5131 0.058 Uiso 1 1 calc R . .
H14B H 0.5462 0.4075 0.4965 0.058 Uiso 1 1 calc R . .
C15 C 0.5829(2) 0.4309(3) 0.4631(2) 0.0625(18) Uani 1 1 d . . .
C16 C 0.5716(2) 0.3750(4) 0.4359(2) 0.0691(19) Uani 1 1 d . . .
H16 H 0.5483 0.3499 0.4344 0.083 Uiso 1 1 calc R . .
C17 C 0.5939(2) 0.3574(4) 0.4121(2) 0.0670(19) Uani 1 1 d . . .
C18 C 0.6263(3) 0.3909(4) 0.4127(3) 0.074(2) Uani 1 1 d . . .
C19 C 0.6387(2) 0.4469(4) 0.4400(3) 0.071(2) Uani 1 1 d . . .
H19 H 0.6618 0.4719 0.4407 0.085 Uiso 1 1 calc R . .
C20 C 0.61753(19) 0.4637(4) 0.4647(2) 0.0586(17) Uani 1 1 d . . .
C21 C 0.63151(19) 0.5283(3) 0.4909(2) 0.0576(16) Uani 1 1 d . . .
H21A H 0.6218 0.5277 0.5153 0.069 Uiso 1 1 calc R . .
H21B H 0.6615 0.5296 0.5024 0.069 Uiso 1 1 calc R . .
C22 C 0.6781(4) 0.7035(5) 0.3973(3) 0.096(3) Uani 1 1 d . . .
C23 C 0.6943(3) 0.7229(5) 0.3621(3) 0.095(3) Uani 1 1 d . . .
C24 C 0.6689(3) 0.7457(5) 0.3252(3) 0.099(3) Uani 1 1 d . . .
H24 H 0.6408 0.7498 0.3204 0.119 Uiso 1 1 calc R . .
C25 C 0.6844(3) 0.7631(6) 0.2941(3) 0.108(3) Uani 1 1 d . . .
H25 H 0.6662 0.7804 0.2682 0.129 Uiso 1 1 calc R . .
C26 C 0.7470(3) 0.7343(5) 0.3359(4) 0.105(3) Uani 1 1 d . . .
H26 H 0.7748 0.7275 0.3399 0.126 Uiso 1 1 calc R . .
C27 C 0.7343(3) 0.7198(5) 0.3693(3) 0.096(3) Uani 1 1 d . . .
H27 H 0.7531 0.7082 0.3964 0.115 Uiso 1 1 calc R . .
C28 C 0.5952(4) 0.8080(5) 0.3864(3) 0.094(3) Uani 1 1 d . . .
C29 C 0.5714(3) 0.8592(4) 0.3550(3) 0.091(3) Uani 1 1 d . . .
C30 C 0.5307(4) 0.8530(5) 0.3330(3) 0.108(3) Uani 1 1 d . . .
H30 H 0.5163 0.8159 0.3377 0.130 Uiso 1 1 calc R . .
C31 C 0.5097(4) 0.9031(4) 0.3025(3) 0.101(3) Uani 1 1 d . . .
H31 H 0.4814 0.8989 0.2879 0.121 Uiso 1 1 calc R . .
C32 C 0.5708(4) 0.9581(5) 0.3173(4) 0.114(3) Uani 1 1 d . . .
H32 H 0.5853 0.9944 0.3115 0.137 Uiso 1 1 calc R . .
C33 C 0.5915(3) 0.9113(5) 0.3477(4) 0.111(3) Uani 1 1 d . . .
H33 H 0.6197 0.9164 0.3630 0.133 Uiso 1 1 calc R . .
C34 C 0.4002(3) 0.6347(5) 0.3943(3) 0.089(3) Uani 1 1 d . . .
C35 C 0.3639(3) 0.6677(5) 0.3594(3) 0.090(3) Uani 1 1 d . . .
C36 C 0.3486(3) 0.6370(5) 0.3209(3) 0.100(3) Uani 1 1 d . . .
H36 H 0.3599 0.5972 0.3147 0.120 Uiso 1 1 calc R . .
C37 C 0.3157(3) 0.6681(6) 0.2913(3) 0.115(4) Uani 1 1 d . . .
H37 H 0.3028 0.6459 0.2651 0.138 Uiso 1 1 calc R . .
C38 C 0.3196(3) 0.7582(6) 0.3372(3) 0.119(4) Uani 1 1 d . . .
H38 H 0.3122 0.8015 0.3428 0.143 Uiso 1 1 calc R . .
C39 C 0.3496(3) 0.7241(6) 0.3687(3) 0.101(3) Uani 1 1 d . . .
H39 H 0.3599 0.7412 0.3968 0.121 Uiso 1 1 calc R . .
C40 C 0.3846(3) 0.4586(4) 0.3849(3) 0.076(2) Uani 1 1 d . . .
C41 C 0.3525(2) 0.4152(4) 0.3531(3) 0.073(2) Uani 1 1 d . . .
C42 C 0.3638(2) 0.3691(4) 0.3286(3) 0.085(2) Uani 1 1 d . . .
H42 H 0.3912 0.3646 0.3308 0.102 Uiso 1 1 calc R . .
C43 C 0.3337(3) 0.3298(5) 0.3009(3) 0.095(3) Uani 1 1 d . . .
H43 H 0.3409 0.2957 0.2855 0.113 Uiso 1 1 calc R . .
C44 C 0.2853(3) 0.3859(5) 0.3192(3) 0.092(3) Uani 1 1 d . . .
H44 H 0.2575 0.3926 0.3152 0.110 Uiso 1 1 calc R . .
C45 C 0.3131(2) 0.4240(5) 0.3483(3) 0.089(3) Uani 1 1 d . . .
H45 H 0.3051 0.4558 0.3647 0.107 Uiso 1 1 calc R . .
C46 C 0.5751(4) 0.2453(6) 0.3951(4) 0.115(4) Uani 1 1 d . . .
C47 C 0.5563(4) 0.1960(4) 0.3588(3) 0.104(3) Uani 1 1 d . . .
C48 C 0.5425(5) 0.1392(7) 0.3702(4) 0.154(6) Uani 1 1 d . . .
H48 H 0.5428 0.1312 0.3981 0.185 Uiso 1 1 calc R . .
C49 C 0.5291(6) 0.0972(7) 0.3400(5) 0.165(6) Uani 1 1 d . . .
H49 H 0.5171 0.0582 0.3461 0.198 Uiso 1 1 calc R . .
C50 C 0.5445(4) 0.1542(6) 0.2889(5) 0.135(4) Uani 1 1 d . . .
H50 H 0.5461 0.1596 0.2615 0.162 Uiso 1 1 calc R . .
C51 C 0.5596(4) 0.2089(6) 0.3229(4) 0.124(4) Uani 1 1 d . . .
H51 H 0.5706 0.2495 0.3176 0.149 Uiso 1 1 calc R . .
C52 C 0.6644(4) 0.3218(8) 0.3870(3) 0.126(4) Uani 1 1 d . . .
C53 C 0.6873(3) 0.3120(5) 0.3569(3) 0.099(3) Uani 1 1 d . . .
C54 C 0.6992(4) 0.2511(6) 0.3491(4) 0.130(4) Uani 1 1 d . . .
H54 H 0.6949 0.2141 0.3645 0.156 Uiso 1 1 calc R . .
C55 C 0.7173(4) 0.2418(6) 0.3196(4) 0.125(4) Uani 1 1 d . . .
H55 H 0.7245 0.1986 0.3135 0.150 Uiso 1 1 calc R . .
C56 C 0.7131(2) 0.3561(5) 0.3042(3) 0.089(3) Uani 1 1 d . . .
H56 H 0.7173 0.3930 0.2887 0.107 Uiso 1 1 calc R . .
C57 C 0.6927(3) 0.3666(5) 0.3344(3) 0.098(3) Uani 1 1 d . . .
H57 H 0.6834 0.4093 0.3386 0.118 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N3 2.127(7) 2_655 ?
Co1 N1 2.144(7) . ?
Co1 N6 2.162(6) 4_655 ?
Co1 N4 2.179(7) 3 ?
Co1 Cl1 2.397(4) . ?
Co1 Cl2 2.399(4) . ?
Co2 N2 2.129(7) . ?
Co2 N2 2.129(7) 2_655 ?
Co2 N5 2.197(10) 1_565 ?
Co2 N5 2.197(10) 2_665 ?
Co2 Cl3 2.393(4) 2_655 ?
Co2 Cl3 2.393(4) . ?
O1 C22 1.282(11) . ?
O1 C3 1.389(9) . ?
O2 C22 1.224(11) . ?
O3 C28 1.361(12) . ?
O3 C4 1.409(9) . ?
O4 C28 1.178(11) . ?
O5 C34 1.294(12) . ?
O5 C10 1.429(9) . ?
O6 C34 1.203(11) . ?
O7 C40 1.355(10) . ?
O7 C11 1.430(9) . ?
O8 C40 1.162(9) . ?
O9 C46 1.288(13) . ?
O9 C17 1.435(9) . ?
O10 C46 1.254(12) . ?
O11 C52 1.243(16) . ?
O11 C18 1.401(9) . ?
O12 C52 1.242(13) . ?
N1 C25 1.324(12) . ?
N1 C26 1.336(13) . ?
N2 C31 1.276(12) . ?
N2 C32 1.422(15) . ?
N3 C37 1.394(13) . ?
N3 C38 1.410(14) . ?
N3 Co1 2.127(7) 2_655 ?
N4 C44 1.334(11) . ?
N4 C43 1.344(11) . ?
N4 Co1 2.179(6) 3_445 ?
N5 C50 1.245(14) . ?
N5 C49 1.416(17) . ?
N5 Co2 2.197(10) 1_545 ?
N6 C56 1.273(12) . ?
N6 C55 1.452(15) . ?
N6 Co1 2.163(6) 4_645 ?
C1 C6 1.392(10) . ?
C1 C2 1.407(10) . ?
C1 C21 1.517(10) . ?
C2 C3 1.370(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.367(12) . ?
C4 C5 1.406(11) . ?
C5 C6 1.408(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.542(9) . ?
C7 C8 1.505(9) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.406(9) . ?
C8 C9 1.404(10) . ?
C9 C10 1.336(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(11) . ?
C11 C12 1.390(10) . ?
C12 C13 1.403(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.515(9) . ?
C14 C15 1.492(10) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.372(10) . ?
C15 C16 1.420(10) . ?
C16 C17 1.350(10) . ?
C16 H16 0.9500 . ?
C17 C18 1.322(11) . ?
C18 C19 1.426(11) . ?
C19 C20 1.340(10) . ?
C19 H19 0.9500 . ?
C20 C21 1.554(10) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.532(13) . ?
C23 C24 1.332(13) . ?
C23 C27 1.346(13) . ?
C24 C25 1.385(13) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.378(13) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.506(14) . ?
C29 C33 1.339(12) . ?
C29 C30 1.371(14) . ?
C30 C31 1.444(14) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.396(16) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.552(12) . ?
C35 C39 1.326(13) . ?
C35 C36 1.366(13) . ?
C36 C37 1.387(13) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.390(13) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.531(12) . ?
C41 C45 1.354(11) . ?
C41 C42 1.388(12) . ?
C42 C43 1.388(12) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.355(12) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.536(16) . ?
C47 C51 1.276(14) . ?
C47 C48 1.352(15) . ?
C48 C49 1.280(18) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.546(17) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.512(16) . ?
C53 C54 1.353(14) . ?
C53 C57 1.387(14) . ?
C54 C55 1.371(15) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.449(13) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Co1 N1 91.8(3) 2_655 . ?
N3 Co1 N6 88.5(3) 2_655 4_655 ?
N1 Co1 N6 176.8(4) . 4_655 ?
N3 Co1 N4 175.9(4) 2_655 3 ?
N1 Co1 N4 89.5(3) . 3 ?
N6 Co1 N4 90.5(3) 4_655 3 ?
N3 Co1 Cl1 91.4(3) 2_655 . ?
N1 Co1 Cl1 87.4(3) . . ?
N6 Co1 Cl1 89.4(3) 4_655 . ?
N4 Co1 Cl1 92.5(2) 3 . ?
N3 Co1 Cl2 87.2(3) 2_655 . ?
N1 Co1 Cl2 92.1(3) . . ?
N6 Co1 Cl2 91.1(3) 4_655 . ?
N4 Co1 Cl2 88.9(2) 3 . ?
Cl1 Co1 Cl2 178.49(11) . . ?
N2 Co2 N2 88.6(4) . 2_655 ?
N2 Co2 N5 88.9(3) . 1_565 ?
N2 Co2 N5 177.5(4) 2_655 1_565 ?
N2 Co2 N5 177.5(4) . 2_665 ?
N2 Co2 N5 88.9(3) 2_655 2_665 ?
N5 Co2 N5 93.6(5) 1_565 2_665 ?
N2 Co2 Cl3 90.9(3) . 2_655 ?
N2 Co2 Cl3 90.1(3) 2_655 2_655 ?
N5 Co2 Cl3 90.5(3) 1_565 2_655 ?
N5 Co2 Cl3 88.5(3) 2_665 2_655 ?
N2 Co2 Cl3 90.1(3) . . ?
N2 Co2 Cl3 90.9(3) 2_655 . ?
N5 Co2 Cl3 88.5(3) 1_565 . ?
N5 Co2 Cl3 90.5(3) 2_665 . ?
Cl3 Co2 Cl3 178.55(16) 2_655 . ?
C22 O1 C3 117.7(7) . . ?
C28 O3 C4 118.7(7) . . ?
C34 O5 C10 115.9(6) . . ?
C40 O7 C11 115.9(6) . . ?
C46 O9 C17 120.9(7) . . ?
C52 O11 C18 121.0(8) . . ?
C25 N1 C26 114.6(8) . . ?
C25 N1 Co1 125.1(7) . . ?
C26 N1 Co1 120.3(6) . . ?
C31 N2 C32 118.2(8) . . ?
C31 N2 Co2 123.9(8) . . ?
C32 N2 Co2 118.0(7) . . ?
C37 N3 C38 114.5(7) . . ?
C37 N3 Co1 125.2(7) . 2_655 ?
C38 N3 Co1 120.3(6) . 2_655 ?
C44 N4 C43 118.5(7) . . ?
C44 N4 Co1 121.4(5) . 3_445 ?
C43 N4 Co1 120.2(6) . 3_445 ?
C50 N5 C49 118.1(12) . . ?
C50 N5 Co2 121.1(10) . 1_545 ?
C49 N5 Co2 120.4(9) . 1_545 ?
C56 N6 C55 119.7(7) . . ?
C56 N6 Co1 123.2(7) . 4_645 ?
C55 N6 Co1 116.7(7) . 4_645 ?
C6 C1 C2 117.3(6) . . ?
C6 C1 C21 123.6(6) . . ?
C2 C1 C21 119.0(6) . . ?
C3 C2 C1 122.5(7) . . ?
C3 C2 H2 118.7 . . ?
C1 C2 H2 118.7 . . ?
C2 C3 C4 119.1(7) . . ?
C2 C3 O1 121.5(8) . . ?
C4 C3 O1 118.8(8) . . ?
C3 C4 C5 121.7(7) . . ?
C3 C4 O3 121.8(7) . . ?
C5 C4 O3 116.4(8) . . ?
C6 C5 C4 117.9(7) . . ?
C6 C5 H5 121.1 . . ?
C4 C5 H5 121.1 . . ?
C1 C6 C5 121.4(6) . . ?
C1 C6 C7 123.3(6) . . ?
C5 C6 C7 115.2(6) . . ?
C8 C7 C6 111.5(5) . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C13 C8 C9 118.8(6) . . ?
C13 C8 C7 123.0(6) . . ?
C9 C8 C7 118.2(6) . . ?
C10 C9 C8 122.3(7) . . ?
C10 C9 H9 118.8 . . ?
C8 C9 H9 118.8 . . ?
C9 C10 C11 118.8(7) . . ?
C9 C10 O5 124.1(7) . . ?
C11 C10 O5 117.1(7) . . ?
C10 C11 C12 122.4(7) . . ?
C10 C11 O7 122.2(7) . . ?
C12 C11 O7 115.3(7) . . ?
C11 C12 C13 118.4(6) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.8 . . ?
C8 C13 C12 119.1(6) . . ?
C8 C13 C14 124.1(6) . . ?
C12 C13 C14 116.7(5) . . ?
C15 C14 C13 112.0(5) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C20 C15 C16 117.0(7) . . ?
C20 C15 C14 126.1(6) . . ?
C16 C15 C14 116.9(6) . . ?
C17 C16 C15 120.0(7) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C18 C17 C16 122.4(7) . . ?
C18 C17 O9 118.9(7) . . ?
C16 C17 O9 118.5(7) . . ?
C17 C18 O11 123.3(7) . . ?
C17 C18 C19 118.9(7) . . ?
O11 C18 C19 117.6(7) . . ?
C20 C19 C18 119.2(7) . . ?
C20 C19 H19 120.4 . . ?
C18 C19 H19 120.4 . . ?
C19 C20 C15 122.3(7) . . ?
C19 C20 C21 115.5(6) . . ?
C15 C20 C21 121.8(6) . . ?
C1 C21 C20 112.4(5) . . ?
C1 C21 H21A 109.1 . . ?
C20 C21 H21A 109.1 . . ?
C1 C21 H21B 109.1 . . ?
C20 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
O2 C22 O1 126.1(8) . . ?
O2 C22 C23 120.2(9) . . ?
O1 C22 C23 113.4(9) . . ?
C24 C23 C27 120.2(8) . . ?
C24 C23 C22 119.7(9) . . ?
C27 C23 C22 120.0(10) . . ?
C23 C24 C25 118.6(9) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
N1 C25 C24 124.0(10) . . ?
N1 C25 H25 118.0 . . ?
C24 C25 H25 118.0 . . ?
N1 C26 C27 124.7(9) . . ?
N1 C26 H26 117.7 . . ?
C27 C26 H26 117.7 . . ?
C23 C27 C26 117.5(10) . . ?
C23 C27 H27 121.2 . . ?
C26 C27 H27 121.2 . . ?
O4 C28 O3 125.5(8) . . ?
O4 C28 C29 124.0(9) . . ?
O3 C28 C29 110.1(9) . . ?
C33 C29 C30 119.6(10) . . ?
C33 C29 C28 117.8(10) . . ?
C30 C29 C28 122.6(8) . . ?
C29 C30 C31 119.9(10) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
N2 C31 C30 121.5(11) . . ?
N2 C31 H31 119.2 . . ?
C30 C31 H31 119.2 . . ?
C33 C32 N2 121.4(9) . . ?
C33 C32 H32 119.3 . . ?
N2 C32 H32 119.3 . . ?
C29 C33 C32 119.4(10) . . ?
C29 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
O6 C34 O5 128.0(8) . . ?
O6 C34 C35 120.3(10) . . ?
O5 C34 C35 111.7(8) . . ?
C39 C35 C36 123.8(9) . . ?
C39 C35 C34 118.1(9) . . ?
C36 C35 C34 118.1(9) . . ?
C35 C36 C37 115.4(9) . . ?
C35 C36 H36 122.3 . . ?
C37 C36 H36 122.3 . . ?
C36 C37 N3 125.1(10) . . ?
C36 C37 H37 117.4 . . ?
N3 C37 H37 117.4 . . ?
C39 C38 N3 120.8(10) . . ?
C39 C38 H38 119.6 . . ?
N3 C38 H38 119.6 . . ?
C35 C39 C38 119.7(10) . . ?
C35 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
O8 C40 O7 124.9(8) . . ?
O8 C40 C41 123.6(8) . . ?
O7 C40 C41 111.4(7) . . ?
C45 C41 C42 120.7(8) . . ?
C45 C41 C40 119.0(8) . . ?
C42 C41 C40 120.3(7) . . ?
C41 C42 C43 118.2(7) . . ?
C41 C42 H42 120.9 . . ?
C43 C42 H42 120.9 . . ?
N4 C43 C42 120.7(8) . . ?
N4 C43 H43 119.6 . . ?
C42 C43 H43 119.6 . . ?
N4 C44 C45 124.2(8) . . ?
N4 C44 H44 117.9 . . ?
C45 C44 H44 117.9 . . ?
C41 C45 C44 117.6(8) . . ?
C41 C45 H45 121.2 . . ?
C44 C45 H45 121.2 . . ?
O10 C46 O9 121.4(10) . . ?
O10 C46 C47 124.8(12) . . ?
O9 C46 C47 113.6(9) . . ?
C51 C47 C48 127.0(11) . . ?
C51 C47 C46 117.6(10) . . ?
C48 C47 C46 114.9(10) . . ?
C49 C48 C47 114.0(13) . . ?
C49 C48 H48 123.0 . . ?
C47 C48 H48 123.0 . . ?
C48 C49 N5 127.0(14) . . ?
C48 C49 H49 116.5 . . ?
N5 C49 H49 116.5 . . ?
N5 C50 C51 118.2(13) . . ?
N5 C50 H50 120.9 . . ?
C51 C50 H50 120.9 . . ?
C47 C51 C50 115.5(11) . . ?
C47 C51 H51 122.2 . . ?
C50 C51 H51 122.2 . . ?
O11 C52 O12 124.2(12) . . ?
O11 C52 C53 116.4(10) . . ?
O12 C52 C53 119.1(14) . . ?
C54 C53 C57 120.4(9) . . ?
C54 C53 C52 121.3(11) . . ?
C57 C53 C52 118.0(10) . . ?
C53 C54 C55 121.2(10) . . ?
C53 C54 H54 119.4 . . ?
C55 C54 H54 119.4 . . ?
C54 C55 N6 118.7(10) . . ?
C54 C55 H55 120.7 . . ?
N6 C55 H55 120.7 . . ?
N6 C56 C57 122.2(9) . . ?
N6 C56 H56 118.9 . . ?
C57 C56 H56 118.9 . . ?
C53 C57 C56 117.5(8) . . ?
C53 C57 H57 121.2 . . ?
C56 C57 H57 121.2 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        55.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.754
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.087
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 -0.010 0.275 -0.014 14094 3948 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_DIFF019_I                   
;
PROBLEM: _diffrn_standards_number is missing
RESPONSE: not relevant
;
_vrf_DIFF020_I                   
;
PROBLEM: _diffrn_standards_interval_count and
RESPONSE: not relevant
;
_vrf_DIFF022_I                   
;
PROBLEM: _diffrn_standards_decay_% is missing
RESPONSE: not relevant
;
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Weakly diffracting sample with no high angle data observed
;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      55.00 Degree
RESPONSE: Weakly diffracting sample with no high angle data observed
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1823169'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
hexaaquobis{hexakis(isonicotinoyl)cyclotricatechylene}tricopper(II)nitrate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C114 H84 Cu3 N18 O48'
_chemical_formula_weight         2664.61

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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   34.8581(12)
_cell_length_b                   20.3238(7)
_cell_length_c                   30.9326(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.984(3)
_cell_angle_gamma                90.00
_cell_volume                     21701.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10740
_cell_measurement_theta_min      3.9440
_cell_measurement_theta_max      72.1040

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5460
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76207
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40034
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.89
_diffrn_reflns_theta_max         74.21
_reflns_number_total             19201
_reflns_number_gt                11609
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1990P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         19201
_refine_ls_number_parameters     717
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0957
_refine_ls_wR_factor_ref         0.3043
_refine_ls_wR_factor_gt          0.2812
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.250345(18) 0.61744(4) 0.747232(17) 0.0836(3) Uani 1 1 d . . .
Cu2 Cu 0.5000 0.86838(4) 0.7500 0.0856(4) Uani 1 2 d S . .
O1 O 0.35456(7) 0.28985(14) 0.61710(8) 0.0617(7) Uani 1 1 d . . .
O2 O 0.29634(9) 0.3268(2) 0.58755(11) 0.0911(11) Uani 1 1 d . . .
O3 O 0.35174(7) 0.42625(13) 0.61850(7) 0.0549(6) Uani 1 1 d . . .
O4 O 0.31610(9) 0.48195(18) 0.56365(8) 0.0799(9) Uani 1 1 d . . .
O5 O 0.50810(7) 0.58768(12) 0.62557(7) 0.0535(6) Uani 1 1 d . . .
O6 O 0.54792(9) 0.64922(15) 0.59095(8) 0.0702(8) Uani 1 1 d . . .
O7 O 0.57831(7) 0.52229(13) 0.62777(7) 0.0541(6) Uani 1 1 d . . .
O8 O 0.61403(9) 0.53721(19) 0.57275(8) 0.0820(10) Uani 1 1 d . . .
O9 O 0.58134(8) 0.21037(14) 0.61931(8) 0.0649(7) Uani 1 1 d . . .
O10 O 0.58533(11) 0.11081(19) 0.58954(11) 0.0964(12) Uani 1 1 d . . .
O11 O 0.51318(9) 0.14005(13) 0.61833(8) 0.0631(7) Uani 1 1 d . . .
O12 O 0.49031(12) 0.06997(15) 0.56477(9) 0.0928(11) Uani 1 1 d . . .
O13 O 0.22003(12) 0.5178(2) 0.77157(11) 0.1111(14) Uani 1 1 d . . .
O14 O 0.28206(12) 0.7153(3) 0.72254(13) 0.1197(15) Uani 1 1 d . . .
O15 O 0.5698(2) 0.86824(19) 0.76772(14) 0.1328(19) Uani 1 1 d . . .
N1 N 0.27199(11) 0.1739(3) 0.70809(12) 0.0894(14) Uani 1 1 d . . .
N2 N 0.27369(12) 0.5679(3) 0.70105(11) 0.0907(14) Uani 1 1 d . . .
N3 N 0.50448(14) 0.79803(18) 0.70457(12) 0.0796(11) Uani 1 1 d . . .
N4 N 0.70254(11) 0.5979(2) 0.70731(10) 0.0797(12) Uani 1 1 d . . .
N5 N 0.70154(12) 0.1313(2) 0.70495(12) 0.0851(13) Uani 1 1 d . . .
N6 N 0.50108(15) -0.06160(17) 0.70327(12) 0.0885(13) Uani 1 1 d . . .
C1 C 0.41930(9) 0.32966(16) 0.53667(9) 0.0421(7) Uani 1 1 d . . .
C2 C 0.39645(9) 0.29452(18) 0.56223(10) 0.0478(7) Uani 1 1 d . . .
H2 H 0.3965 0.2478 0.5615 0.057 Uiso 1 1 calc R . .
C3 C 0.37396(10) 0.32664(18) 0.58833(11) 0.0518(8) Uani 1 1 d . . .
C4 C 0.37329(10) 0.39493(19) 0.58987(10) 0.0497(8) Uani 1 1 d . . .
C5 C 0.39534(9) 0.42993(17) 0.56404(9) 0.0451(7) Uani 1 1 d . . .
H5 H 0.3943 0.4766 0.5642 0.054 Uiso 1 1 calc R . .
C6 C 0.41898(8) 0.39866(15) 0.53777(9) 0.0402(7) Uani 1 1 d . . .
C7 C 0.44377(8) 0.44173(15) 0.51307(8) 0.0392(6) Uani 1 1 d . . .
H7A H 0.4290 0.4815 0.5025 0.047 Uiso 1 1 calc R . .
H7B H 0.4505 0.4175 0.4874 0.047 Uiso 1 1 calc R . .
C8 C 0.48074(8) 0.46193(15) 0.54227(8) 0.0396(6) Uani 1 1 d . . .
C9 C 0.47944(9) 0.51489(16) 0.56968(9) 0.0429(7) Uani 1 1 d . . .
H9 H 0.4558 0.5383 0.5696 0.051 Uiso 1 1 calc R . .
C10 C 0.51196(10) 0.53467(17) 0.59745(9) 0.0475(7) Uani 1 1 d . . .
C11 C 0.54639(10) 0.50125(17) 0.59827(9) 0.0485(8) Uani 1 1 d . . .
C12 C 0.54842(9) 0.44824(17) 0.57111(9) 0.0462(7) Uani 1 1 d . . .
H12 H 0.5723 0.4254 0.5717 0.055 Uiso 1 1 calc R . .
C13 C 0.51614(9) 0.42731(16) 0.54264(9) 0.0425(7) Uani 1 1 d . . .
C14 C 0.52071(9) 0.36805(16) 0.51426(9) 0.0431(7) Uani 1 1 d . . .
H14A H 0.5008 0.3696 0.4881 0.052 Uiso 1 1 calc R . .
H14B H 0.5465 0.3695 0.5043 0.052 Uiso 1 1 calc R . .
C15 C 0.51671(9) 0.30473(16) 0.53848(9) 0.0437(7) Uani 1 1 d . . .
C16 C 0.54959(10) 0.28238(18) 0.56575(11) 0.0537(8) Uani 1 1 d . . .
H16 H 0.5732 0.3061 0.5672 0.064 Uiso 1 1 calc R . .
C17 C 0.54796(11) 0.22624(19) 0.59054(10) 0.0569(9) Uani 1 1 d . . .
C18 C 0.51403(11) 0.19262(18) 0.58966(10) 0.0540(8) Uani 1 1 d . . .
C19 C 0.48098(10) 0.21289(17) 0.56221(10) 0.0490(7) Uani 1 1 d . . .
H19 H 0.4577 0.1883 0.5609 0.059 Uiso 1 1 calc R . .
C20 C 0.48216(9) 0.26877(16) 0.53686(9) 0.0428(7) Uani 1 1 d . . .
C21 C 0.44449(9) 0.29019(16) 0.50971(9) 0.0436(7) Uani 1 1 d . . .
H21A H 0.4301 0.2508 0.4977 0.052 Uiso 1 1 calc R . .
H21B H 0.4504 0.3173 0.4849 0.052 Uiso 1 1 calc R . .
C22 C 0.31609(13) 0.2936(3) 0.61355(14) 0.0750(12) Uani 1 1 d . . .
C23 C 0.30124(12) 0.2504(3) 0.64695(13) 0.0781(13) Uani 1 1 d . . .
C24 C 0.32339(13) 0.2001(3) 0.66753(14) 0.0763(12) Uani 1 1 d . . .
H24 H 0.3488 0.1918 0.6611 0.092 Uiso 1 1 calc R . .
C25 C 0.30750(13) 0.1615(3) 0.69818(14) 0.0768(13) Uani 1 1 d . . .
H25 H 0.3221 0.1261 0.7121 0.092 Uiso 1 1 calc R . .
C26 C 0.25067(15) 0.2238(3) 0.68768(17) 0.1014(19) Uani 1 1 d . . .
H26 H 0.2252 0.2311 0.6944 0.122 Uiso 1 1 calc R . .
C27 C 0.26447(15) 0.2638(3) 0.65799(19) 0.0983(17) Uani 1 1 d . . .
H27 H 0.2496 0.2997 0.6452 0.118 Uiso 1 1 calc R . .
C28 C 0.32486(12) 0.4707(2) 0.60136(12) 0.0677(11) Uani 1 1 d . . .
C29 C 0.30649(12) 0.5019(2) 0.63744(12) 0.0696(11) Uani 1 1 d . . .
C30 C 0.30705(12) 0.4751(3) 0.67758(13) 0.0728(12) Uani 1 1 d . . .
H30 H 0.3195 0.4341 0.6842 0.087 Uiso 1 1 calc R . .
C31 C 0.28989(13) 0.5068(3) 0.70834(13) 0.0781(13) Uani 1 1 d . . .
H31 H 0.2891 0.4861 0.7357 0.094 Uiso 1 1 calc R . .
C32 C 0.27286(16) 0.5937(3) 0.66109(14) 0.0915(17) Uani 1 1 d . . .
H32 H 0.2608 0.6352 0.6549 0.110 Uiso 1 1 calc R . .
C33 C 0.28912(16) 0.5615(3) 0.62851(15) 0.0916(16) Uani 1 1 d . . .
H33 H 0.2882 0.5807 0.6004 0.110 Uiso 1 1 calc R . .
C34 C 0.52721(12) 0.64352(19) 0.61871(10) 0.0584(9) Uani 1 1 d . . .
C35 C 0.51803(13) 0.6973(2) 0.64865(11) 0.0641(10) Uani 1 1 d . . .
C36 C 0.48749(14) 0.6941(2) 0.67232(13) 0.0700(11) Uani 1 1 d . . .
H36 H 0.4707 0.6570 0.6696 0.084 Uiso 1 1 calc R . .
C37 C 0.48141(15) 0.7450(2) 0.70006(13) 0.0746(12) Uani 1 1 d . . .
H37 H 0.4603 0.7424 0.7164 0.089 Uiso 1 1 calc R . .
C38 C 0.53387(19) 0.8007(2) 0.68010(14) 0.0937(17) Uani 1 1 d . . .
H38 H 0.5501 0.8385 0.6824 0.112 Uiso 1 1 calc R . .
C39 C 0.54115(18) 0.7516(2) 0.65226(14) 0.0867(15) Uani 1 1 d . . .
H39 H 0.5620 0.7552 0.6357 0.104 Uiso 1 1 calc R . .
C40 C 0.61051(12) 0.5399(2) 0.61136(11) 0.0674(11) Uani 1 1 d . . .
C41 C 0.64211(11) 0.5595(2) 0.64572(11) 0.0651(11) Uani 1 1 d . . .
C42 C 0.63538(13) 0.5855(3) 0.68567(12) 0.0752(13) Uani 1 1 d . . .
H42 H 0.6097 0.5908 0.6922 0.090 Uiso 1 1 calc R . .
C43 C 0.66654(14) 0.6030(3) 0.71529(13) 0.0836(15) Uani 1 1 d . . .
H43 H 0.6620 0.6197 0.7428 0.100 Uiso 1 1 calc R . .
C44 C 0.70945(14) 0.5743(3) 0.66885(13) 0.0910(17) Uani 1 1 d . . .
H44 H 0.7355 0.5696 0.6634 0.109 Uiso 1 1 calc R . .
C45 C 0.67970(13) 0.5566(3) 0.63695(12) 0.0810(14) Uani 1 1 d . . .
H45 H 0.6851 0.5426 0.6091 0.097 Uiso 1 1 calc R . .
C46 C 0.59802(14) 0.1522(2) 0.61513(13) 0.0748(12) Uani 1 1 d . . .
C47 C 0.63462(14) 0.1469(2) 0.64720(13) 0.0763(13) Uani 1 1 d . . .
C48 C 0.65256(13) 0.2004(3) 0.66659(15) 0.0831(14) Uani 1 1 d . . .
H48 H 0.6424 0.2433 0.6605 0.100 Uiso 1 1 calc R . .
C49 C 0.68667(14) 0.1909(3) 0.69607(16) 0.0865(14) Uani 1 1 d . . .
H49 H 0.6994 0.2281 0.7100 0.104 Uiso 1 1 calc R . .
C50 C 0.68272(16) 0.0783(3) 0.68490(16) 0.0938(18) Uani 1 1 d . . .
H50 H 0.6931 0.0356 0.6913 0.113 Uiso 1 1 calc R . .
C51 C 0.64968(16) 0.0844(3) 0.65618(15) 0.0911(16) Uani 1 1 d . . .
H51 H 0.6372 0.0467 0.6426 0.109 Uiso 1 1 calc R . .
C52 C 0.50008(14) 0.0813(2) 0.60215(12) 0.0705(11) Uani 1 1 d . . .
C53 C 0.50053(16) 0.0320(2) 0.63871(13) 0.0775(13) Uani 1 1 d . . .
C54 C 0.52567(17) 0.0377(2) 0.67730(13) 0.0837(15) Uani 1 1 d . . .
H54 H 0.5428 0.0741 0.6824 0.100 Uiso 1 1 calc R . .
C55 C 0.52498(19) -0.0116(2) 0.70850(14) 0.0919(17) Uani 1 1 d . . .
H55 H 0.5427 -0.0089 0.7347 0.110 Uiso 1 1 calc R . .
C56 C 0.4757(2) -0.0648(3) 0.66673(16) 0.0995(18) Uani 1 1 d . . .
H56 H 0.4569 -0.0989 0.6640 0.119 Uiso 1 1 calc R . .
C57 C 0.4756(2) -0.0206(2) 0.63253(16) 0.1002(19) Uani 1 1 d . . .
H57 H 0.4589 -0.0264 0.6058 0.120 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 2.010(4) . ?
Cu1 N5 2.017(3) 3_455 ?
Cu1 N1 2.033(4) 4_556 ?
Cu1 N4 2.047(3) 2_656 ?
Cu2 N3 2.026(4) 2_656 ?
Cu2 N3 2.026(4) . ?
Cu2 N6 2.033(4) 1_565 ?
Cu2 N6 2.033(4) 2_666 ?
O1 C22 1.332(5) . ?
O1 C3 1.406(4) . ?
O2 C22 1.193(5) . ?
O3 C28 1.356(5) . ?
O3 C4 1.392(4) . ?
O4 C28 1.186(4) . ?
O5 C34 1.348(4) . ?
O5 C10 1.403(4) . ?
O6 C34 1.202(5) . ?
O7 C40 1.343(5) . ?
O7 C11 1.404(3) . ?
O8 C40 1.219(5) . ?
O9 C46 1.331(5) . ?
O9 C17 1.401(4) . ?
O10 C46 1.197(6) . ?
O11 C52 1.350(5) . ?
O11 C18 1.391(4) . ?
O12 C52 1.182(5) . ?
N1 C25 1.340(7) . ?
N1 C26 1.360(7) . ?
N1 Cu1 2.033(4) 4_546 ?
N2 C32 1.339(6) . ?
N2 C31 1.370(6) . ?
N3 C37 1.341(6) . ?
N3 C38 1.357(7) . ?
N4 C43 1.316(7) . ?
N4 C44 1.335(6) . ?
N4 Cu1 2.047(3) 2_656 ?
N5 C49 1.331(6) . ?
N5 C50 1.365(7) . ?
N5 Cu1 2.017(3) 3_545 ?
N6 C55 1.309(7) . ?
N6 C56 1.336(6) . ?
N6 Cu2 2.033(4) 1_545 ?
C1 C2 1.395(4) . ?
C1 C6 1.403(5) . ?
C1 C21 1.521(5) . ?
C2 C3 1.367(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(5) . ?
C4 C5 1.381(5) . ?
C5 C6 1.389(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.510(4) . ?
C7 C8 1.524(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.375(5) . ?
C8 C13 1.419(5) . ?
C9 C10 1.384(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.376(5) . ?
C11 C12 1.374(5) . ?
C12 C13 1.396(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.512(5) . ?
C14 C15 1.505(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.404(5) . ?
C15 C16 1.401(4) . ?
C16 C17 1.380(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.363(6) . ?
C18 C19 1.395(5) . ?
C19 C20 1.384(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.521(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.502(6) . ?
C23 C24 1.382(7) . ?
C23 C27 1.399(7) . ?
C24 C25 1.402(6) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.363(7) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.502(6) . ?
C29 C30 1.353(6) . ?
C29 C33 1.365(7) . ?
C30 C31 1.355(6) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.387(7) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.496(6) . ?
C35 C39 1.361(6) . ?
C35 C36 1.375(6) . ?
C36 C37 1.379(6) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.365(7) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.475(5) . ?
C41 C45 1.376(6) . ?
C41 C42 1.394(6) . ?
C42 C43 1.368(5) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.376(5) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.507(5) . ?
C47 C48 1.352(7) . ?
C47 C51 1.387(6) . ?
C48 C49 1.407(6) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.359(6) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.509(6) . ?
C53 C57 1.373(7) . ?
C53 C54 1.384(5) . ?
C54 C55 1.395(6) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.388(7) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 N5 89.86(14) . 3_455 ?
N2 Cu1 N1 175.7(2) . 4_556 ?
N5 Cu1 N1 89.65(14) 3_455 4_556 ?
N2 Cu1 N4 91.46(13) . 2_656 ?
N5 Cu1 N4 175.3(2) 3_455 2_656 ?
N1 Cu1 N4 89.37(14) 4_556 2_656 ?
N3 Cu2 N3 90.2(2) 2_656 . ?
N3 Cu2 N6 176.62(19) 2_656 1_565 ?
N3 Cu2 N6 89.43(14) . 1_565 ?
N3 Cu2 N6 89.43(14) 2_656 2_666 ?
N3 Cu2 N6 176.62(19) . 2_666 ?
N6 Cu2 N6 91.1(2) 1_565 2_666 ?
C22 O1 C3 119.0(3) . . ?
C28 O3 C4 117.4(3) . . ?
C34 O5 C10 117.2(3) . . ?
C40 O7 C11 117.6(2) . . ?
C46 O9 C17 118.6(3) . . ?
C52 O11 C18 118.6(3) . . ?
C25 N1 C26 119.8(4) . . ?
C25 N1 Cu1 120.2(4) . 4_546 ?
C26 N1 Cu1 120.0(3) . 4_546 ?
C32 N2 C31 117.6(4) . . ?
C32 N2 Cu1 120.0(3) . . ?
C31 N2 Cu1 122.4(3) . . ?
C37 N3 C38 117.6(4) . . ?
C37 N3 Cu2 122.5(3) . . ?
C38 N3 Cu2 119.7(3) . . ?
C43 N4 C44 119.4(3) . . ?
C43 N4 Cu1 123.4(3) . 2_656 ?
C44 N4 Cu1 117.1(3) . 2_656 ?
C49 N5 C50 118.4(4) . . ?
C49 N5 Cu1 122.0(4) . 3_545 ?
C50 N5 Cu1 119.5(3) . 3_545 ?
C55 N6 C56 118.5(4) . . ?
C55 N6 Cu2 122.0(3) . 1_545 ?
C56 N6 Cu2 119.5(3) . 1_545 ?
C2 C1 C6 119.4(3) . . ?
C2 C1 C21 117.4(3) . . ?
C6 C1 C21 123.2(3) . . ?
C3 C2 C1 120.7(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C4 120.7(3) . . ?
C2 C3 O1 119.1(3) . . ?
C4 C3 O1 119.9(3) . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 O3 119.5(3) . . ?
C5 C4 O3 121.7(3) . . ?
C4 C5 C6 121.7(3) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 118.6(3) . . ?
C5 C6 C7 117.3(3) . . ?
C1 C6 C7 124.1(3) . . ?
C6 C7 C8 110.7(2) . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C13 119.1(3) . . ?
C9 C8 C7 118.6(3) . . ?
C13 C8 C7 122.3(3) . . ?
C8 C9 C10 121.1(3) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 O5 121.7(3) . . ?
C9 C10 O5 117.9(3) . . ?
C12 C11 C10 119.6(3) . . ?
C12 C11 O7 122.2(3) . . ?
C10 C11 O7 118.2(3) . . ?
C11 C12 C13 121.3(3) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 H12 119.4 . . ?
C12 C13 C8 118.6(3) . . ?
C12 C13 C14 117.9(3) . . ?
C8 C13 C14 123.5(3) . . ?
C15 C14 C13 111.6(2) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C20 C15 C16 118.6(3) . . ?
C20 C15 C14 124.4(3) . . ?
C16 C15 C14 116.9(3) . . ?
C17 C16 C15 120.6(3) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C18 C17 C16 120.4(3) . . ?
C18 C17 O9 122.6(3) . . ?
C16 C17 O9 116.7(3) . . ?
C17 C18 O11 117.9(3) . . ?
C17 C18 C19 120.3(3) . . ?
O11 C18 C19 121.7(3) . . ?
C20 C19 C18 120.0(3) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C20 C15 120.0(3) . . ?
C19 C20 C21 117.2(3) . . ?
C15 C20 C21 122.8(3) . . ?
C20 C21 C1 111.6(2) . . ?
C20 C21 H21A 109.3 . . ?
C1 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C1 C21 H21B 109.3 . . ?
H21A C21 H21B 108.0 . . ?
O2 C22 O1 124.6(4) . . ?
O2 C22 C23 125.0(4) . . ?
O1 C22 C23 110.4(4) . . ?
C24 C23 C27 120.3(4) . . ?
C24 C23 C22 121.7(4) . . ?
C27 C23 C22 118.0(5) . . ?
C23 C24 C25 118.5(4) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
N1 C25 C24 120.9(5) . . ?
N1 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
C27 C26 N1 122.4(5) . . ?
C27 C26 H26 118.8 . . ?
N1 C26 H26 118.8 . . ?
C26 C27 C23 118.0(5) . . ?
C26 C27 H27 121.0 . . ?
C23 C27 H27 121.0 . . ?
O4 C28 O3 125.6(4) . . ?
O4 C28 C29 124.9(4) . . ?
O3 C28 C29 109.5(3) . . ?
C30 C29 C33 119.5(4) . . ?
C30 C29 C28 124.0(4) . . ?
C33 C29 C28 116.6(4) . . ?
C29 C30 C31 120.1(4) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C30 C31 N2 121.8(4) . . ?
C30 C31 H31 119.1 . . ?
N2 C31 H31 119.1 . . ?
N2 C32 C33 121.8(5) . . ?
N2 C32 H32 119.1 . . ?
C33 C32 H32 119.1 . . ?
C29 C33 C32 119.1(4) . . ?
C29 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
O6 C34 O5 123.5(4) . . ?
O6 C34 C35 125.0(3) . . ?
O5 C34 C35 111.4(3) . . ?
C39 C35 C36 119.2(4) . . ?
C39 C35 C34 117.9(4) . . ?
C36 C35 C34 122.9(4) . . ?
C35 C36 C37 119.5(4) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
N3 C37 C36 121.7(5) . . ?
N3 C37 H37 119.1 . . ?
C36 C37 H37 119.1 . . ?
N3 C38 C39 122.9(4) . . ?
N3 C38 H38 118.5 . . ?
C39 C38 H38 118.6 . . ?
C35 C39 C38 119.0(5) . . ?
C35 C39 H39 120.5 . . ?
C38 C39 H39 120.5 . . ?
O8 C40 O7 124.2(3) . . ?
O8 C40 C41 123.4(4) . . ?
O7 C40 C41 112.3(3) . . ?
C45 C41 C42 118.2(3) . . ?
C45 C41 C40 118.9(4) . . ?
C42 C41 C40 122.7(4) . . ?
C43 C42 C41 118.5(4) . . ?
C43 C42 H42 120.8 . . ?
C41 C42 H42 120.8 . . ?
N4 C43 C42 122.9(4) . . ?
N4 C43 H43 118.6 . . ?
C42 C43 H43 118.6 . . ?
N4 C44 C45 121.4(5) . . ?
N4 C44 H44 119.3 . . ?
C45 C44 H44 119.3 . . ?
C44 C45 C41 119.4(4) . . ?
C44 C45 H45 120.3 . . ?
C41 C45 H45 120.3 . . ?
O10 C46 O9 124.2(4) . . ?
O10 C46 C47 125.9(4) . . ?
O9 C46 C47 110.0(4) . . ?
C48 C47 C51 120.5(4) . . ?
C48 C47 C46 122.1(4) . . ?
C51 C47 C46 117.4(4) . . ?
C47 C48 C49 118.3(4) . . ?
C47 C48 H48 120.8 . . ?
C49 C48 H48 120.8 . . ?
N5 C49 C48 121.9(5) . . ?
N5 C49 H49 119.1 . . ?
C48 C49 H49 119.1 . . ?
C51 C50 N5 122.3(5) . . ?
C51 C50 H50 118.9 . . ?
N5 C50 H50 118.9 . . ?
C50 C51 C47 118.5(5) . . ?
C50 C51 H51 120.7 . . ?
C47 C51 H51 120.7 . . ?
O12 C52 O11 124.9(4) . . ?
O12 C52 C53 125.2(4) . . ?
O11 C52 C53 110.0(3) . . ?
C57 C53 C54 119.9(4) . . ?
C57 C53 C52 118.1(4) . . ?
C54 C53 C52 122.0(4) . . ?
C53 C54 C55 117.8(5) . . ?
C53 C54 H54 121.1 . . ?
C55 C54 H54 121.1 . . ?
N6 C55 C54 123.0(4) . . ?
N6 C55 H55 118.5 . . ?
C54 C55 H55 118.5 . . ?
N6 C56 C57 123.0(5) . . ?
N6 C56 H56 118.5 . . ?
C57 C56 H56 118.5 . . ?
C53 C57 C56 117.6(4) . . ?
C53 C57 H57 121.2 . . ?
C56 C57 H57 121.2 . . ?

_diffrn_measured_fraction_theta_max 0.868
_diffrn_reflns_theta_full        74.21
_diffrn_measured_fraction_theta_full 0.868
_refine_diff_density_max         1.695
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.082
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 0.015 0.384 -0.040 13629 4100 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
# start Validation Reply Form
_vrf_CHEMW03_I                   
;
PROBLEM: ALERT: The ratio of given/expected molecular weight as
RESPONSE: anions not located in structure are included in formula
;
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.868 Why?  
RESPONSE: Large cell. obs data:parameter ratio >10
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_c_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1823166'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
trisbromotriscarbonylbis{hexakis(isonicotinoyl)cyclotricatechylene}trirhenium(I) nitromethane clathrate
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C119 H90 Br3 N14 O37 Re3'
_chemical_formula_weight         3106.38

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'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-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+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-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+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'

_cell_length_a                   19.6665(4)
_cell_length_b                   19.6665(4)
_cell_length_c                   31.6873(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     10613.8(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5174
_cell_measurement_theta_min      4.176
_cell_measurement_theta_max      72.578

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4584
_exptl_absorpt_coefficient_mu    6.541
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7896
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         73.56
_reflns_number_total             2571
_reflns_number_gt                2444
_reflns_threshold_expression     >2sigma(I)

_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2571
_refine_ls_number_parameters     128
_refine_ls_number_restraints     113
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.1496
_refine_ls_wR_factor_ref         0.5003
_refine_ls_wR_factor_gt          0.4970
_refine_ls_goodness_of_fit_ref   2.517
_refine_ls_restrained_S_all      2.482
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.8333 0.1667 0.1667 0.0496(7) Uani 1 4 d SU . .
Br1 Br 0.75518(16) 0.24482(16) 0.17651(13) 0.0659(13) Uani 0.50 2 d SPU . .
O1 O 1.1088(12) 0.4057(10) 0.0089(6) 0.104(5) Uani 1 1 d U . .
O2 O 1.1372(15) 0.4991(13) 0.0567(6) 0.138(9) Uani 1 1 d U . .
O4 O 0.975(3) 0.4875(16) 0.2184(16) 0.088(12) Uiso 0.50 2 d SP . .
O5 O 1.1599(16) 0.320(3) 0.079(2) 0.092(15) Uiso 0.50 2 d SP . .
N2 N 1.3333 0.6667 0.0775(19) 0.105(14) Uiso 1 6 d SU . .
C1 C 1.2272(13) 0.6136(7) -0.0911(6) 0.058(4) Uani 1 2 d SU . .
H1A H 1.1726 0.5863 -0.1017 0.070 Uiso 1 2 calc SR . .
H1B H 1.2628 0.6314 -0.1158 0.070 Uiso 1 2 calc SR . .
C2 C 1.2408(9) 0.5568(8) -0.0660(3) 0.055(3) Uani 1 1 d U . .
C3 C 1.1808(14) 0.5031(12) -0.0410(5) 0.099(7) Uani 1 1 d U . .
H3 H 1.1319 0.5017 -0.0414 0.119 Uiso 1 1 calc R . .
C4 C 1.1889(15) 0.4533(10) -0.0163(5) 0.112(7) Uani 1 1 d U . .
C5 C 1.0978(16) 0.4371(15) 0.0439(8) 0.087(5) Uani 1 1 d U . .
C6 C 1.0298(9) 0.3682(7) 0.0702(4) 0.092(5) Uani 1 1 d GU . .
C7 C 1.0028(10) 0.2894(8) 0.0617(4) 0.107(8) Uani 1 1 d GU . .
H7 H 1.0244 0.2752 0.0388 0.129 Uiso 1 1 calc R . .
C8 C 0.9444(9) 0.2316(6) 0.0866(4) 0.086(5) Uani 1 1 d GU . .
H8 H 0.9259 0.1778 0.0808 0.103 Uiso 1 1 calc R . .
N1 N 0.9129(7) 0.2525(6) 0.1201(3) 0.070(3) Uani 1 1 d GU . .
C9 C 0.9398(9) 0.3313(7) 0.1286(4) 0.090(5) Uani 1 1 d GU . .
H9 H 0.9183 0.3456 0.1515 0.108 Uiso 1 1 calc R . .
C10 C 0.9983(9) 0.3891(6) 0.1037(4) 0.089(5) Uani 1 1 d GU . .
H10 H 1.0167 0.4430 0.1095 0.107 Uiso 1 1 calc R . .
C11 C 1.3333 0.6667 0.0340(14) 0.065(9) Uiso 1 6 d SU . .
H11A H 1.3207 0.6147 0.0237 0.098 Uiso 0.17 1 calc PR . .
H11 H 1.3853 0.7061 0.0237 0.098 Uiso 0.17 1 calc PR . .
H11C H 1.2939 0.6793 0.0237 0.098 Uiso 0.17 1 calc PR . .
O3 O 1.384(3) 0.721(3) 0.0971(14) 0.088(12) Uiso 0.33 1 d PU . .


_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
Re1 N1 2.199(9) 25_655 ?
Re1 N1 2.199(18) 12_545 ?
Re1 N1 2.199(19) 24_665 ?
Re1 N1 2.199(9) . ?
Re1 Br1 2.680(6) . ?
Re1 Br1 2.680(6) 25_655 ?
O1 C5 1.34(4) . ?
O1 C4 1.59(3) . ?
O2 C5 1.14(3) . ?
O4 O5 1.15(7) 26_565 ?
O5 O4 1.15(7) 27_545 ?
N2 O3 1.20(5) 22_755 ?
N2 O3 1.20(5) 2_755 ?
N2 O3 1.20(5) 24_775 ?
N2 O3 1.20(5) . ?
N2 O3 1.20(5) 3_775 ?
N2 O3 1.20(5) 23 ?
N2 C11 1.38(7) . ?
C1 C2 1.500(19) . ?
C1 C2 1.500(19) 23 ?
C2 C3 1.37(2) . ?
C2 C2 1.48(4) 22_755 ?
C3 C4 1.32(4) . ?
C4 C4 1.49(6) 22_755 ?
C5 C6 1.58(3) . ?
C6 C7 1.3900 . ?
C6 C10 1.3900 . ?
C7 C8 1.3900 . ?
C8 N1 1.3900 . ?
N1 C9 1.3900 . ?
C9 C10 1.3900 . ?
O3 O3 0.93(9) 22_755 ?
O3 O3 1.13(9) 23 ?
O3 O3 1.79(8) 3_775 ?
O3 O3 1.79(8) 2_755 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Re1 N1 95.4(17) 25_655 12_545 ?
N1 Re1 N1 84.6(17) 25_655 24_665 ?
N1 Re1 N1 180.0(14) 12_545 24_665 ?
N1 Re1 N1 180.0(10) 25_655 . ?
N1 Re1 N1 84.6(9) 12_545 . ?
N1 Re1 N1 95.4(10) 24_665 . ?
N1 Re1 Br1 88.3(12) 25_655 . ?
N1 Re1 Br1 88.3(9) 12_545 . ?
N1 Re1 Br1 91.7(9) 24_665 . ?
N1 Re1 Br1 91.7(4) . . ?
N1 Re1 Br1 91.7(12) 25_655 25_655 ?
N1 Re1 Br1 91.7(9) 12_545 25_655 ?
N1 Re1 Br1 88.3(9) 24_665 25_655 ?
N1 Re1 Br1 88.3(4) . 25_655 ?
Br1 Re1 Br1 180.0 . 25_655 ?
C5 O1 C4 119.1(18) . . ?
O3 N2 O3 56(4) 22_755 2_755 ?
O3 N2 O3 96(4) 22_755 24_775 ?
O3 N2 O3 45(4) 2_755 24_775 ?
O3 N2 O3 45(4) 22_755 . ?
O3 N2 O3 96(4) 2_755 . ?
O3 N2 O3 118(6) 24_775 . ?
O3 N2 O3 118(6) 22_755 3_775 ?
O3 N2 O3 96(4) 2_755 3_775 ?
O3 N2 O3 56(4) 24_775 3_775 ?
O3 N2 O3 96(4) . 3_775 ?
O3 N2 O3 96(4) 22_755 23 ?
O3 N2 O3 118(6) 2_755 23 ?
O3 N2 O3 96(4) 24_775 23 ?
O3 N2 O3 56(4) . 23 ?
O3 N2 O3 45(4) 3_775 23 ?
O3 N2 C11 121(3) 22_755 . ?
O3 N2 C11 121(3) 2_755 . ?
O3 N2 C11 121(3) 24_775 . ?
O3 N2 C11 121(3) . . ?
O3 N2 C11 121(3) 3_775 . ?
O3 N2 C11 121(3) 23 . ?
C2 C1 C2 112.9(15) . 23 ?
C3 C2 C2 118.3(16) . 22_755 ?
C3 C2 C1 118(2) . . ?
C2 C2 C1 123.4(10) 22_755 . ?
C4 C3 C2 122(3) . . ?
C3 C4 C4 119.3(15) . 22_755 ?
C3 C4 O1 106(2) . . ?
C4 C4 O1 134.2(12) 22_755 . ?
O2 C5 O1 127(3) . . ?
O2 C5 C6 124(2) . . ?
O1 C5 C6 107.8(19) . . ?
C7 C6 C10 120.0 . . ?
C7 C6 C5 122.6(14) . . ?
C10 C6 C5 117.4(14) . . ?
C6 C7 C8 120.0 . . ?
N1 C8 C7 120.0 . . ?
C8 N1 C9 120.0 . . ?
C8 N1 Re1 122.4(6) . . ?
C9 N1 Re1 117.0(6) . . ?
C10 C9 N1 120.0 . . ?
C9 C10 C6 120.0 . . ?
O3 O3 O3 120.00(5) 22_755 23 ?
O3 O3 N2 67(2) 22_755 . ?
O3 O3 N2 62(2) 23 . ?
O3 O3 O3 93(2) 22_755 3_775 ?
O3 O3 O3 27(2) 23 3_775 ?
N2 O3 O3 42(2) . 3_775 ?
O3 O3 O3 33(2) 22_755 2_755 ?
O3 O3 O3 87(2) 23 2_755 ?
N2 O3 O3 42(2) . 2_755 ?
O3 O3 O3 59.998(9) 3_775 2_755 ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        73.56
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         2.301
_refine_diff_density_min         -6.193
_refine_diff_density_rms         0.378

# start Validation Reply Form
_vrf_PLAT084_I                   
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.50 Report
RESPONSE: Structure has void spaces likely to contain disordered solvent. Residual electron density could not be meaningfully modelled
;
_vrf_PLAT430_I                   
;
PROBLEM: Short Inter D...A Contact  O4       ..O5               1.16 Ang.  
RESPONSE: two positions of a disordered water which are not at full occupany
;
_vrf_PLAT601_I                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .        427 Ang**3
RESPONSE: Likely to contain disordered solvent. Residual electron
density could not be meaningfully modelled
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_coi2sqd
_database_code_depnum_ccdc_archive 'CCDC 1823172'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'tetraquobis{hexakis(isonicotinoyl)cyclotricatechylene}diiodotricobalt(II) iodide'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C114 H81 Co3 I6 N12 O28.50'
_chemical_formula_weight         3013.10

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'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   35.4694(8)
_cell_length_b                   20.3503(5)
_cell_length_c                   33.3657(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.579(3)
_cell_angle_gamma                90.00
_cell_volume                     22547.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6054
_cell_measurement_theta_min      4.140
_cell_measurement_theta_max      59.277

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.888
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5904
_exptl_absorpt_coefficient_mu    8.506
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83634
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         .
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        .
_diffrn_reflns_number            19206
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         2.83
_diffrn_reflns_theta_max         59.64
_reflns_number_total             13349
_reflns_number_gt                9188
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
not all lattice disordered I- positions were located but are inlcuded in formula. 
Disordered aquo/I ligands and lattice I- refined isotropically. 
Disordered aquo/I ligands modelled as 0.75:0.25 O:I. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13349
_refine_ls_number_parameters     715
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1620
_refine_ls_R_factor_gt           0.1409
_refine_ls_wR_factor_ref         0.4171
_refine_ls_wR_factor_gt          0.3930
_refine_ls_goodness_of_fit_ref   1.559
_refine_ls_restrained_S_all      1.559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co2 Co 0.25077(4) 0.22350(8) 0.24931(4) 0.0562(5) Uani 1 1 d . . .
Co1 Co 0.5000 -0.02853(9) 0.2500 0.0628(6) Uani 1 2 d S . .
O1 O 0.57075(15) 0.2481(3) 0.38249(17) 0.0479(14) Uani 1 1 d . . .
O2 O 0.6252(3) 0.1839(4) 0.4125(2) 0.093(2) Uani 1 1 d . . .
O3 O 0.63899(15) 0.3110(3) 0.38225(16) 0.0522(15) Uani 1 1 d . . .
O4 O 0.6987(2) 0.2970(4) 0.43493(19) 0.080(2) Uani 1 1 d . . .
O5 O 0.64538(16) 0.6235(3) 0.38248(17) 0.0516(14) Uani 1 1 d . . .
O6 O 0.6631(2) 0.7233(4) 0.4125(2) 0.085(2) Uani 1 1 d . . .
O7 O 0.57829(16) 0.6955(3) 0.38068(16) 0.0475(13) Uani 1 1 d . . .
O8 O 0.5840(2) 0.7678(3) 0.4346(2) 0.0737(19) Uani 1 1 d . . .
O9 O 0.41954(12) 0.5469(2) 0.37800(14) 0.0339(11) Uani 1 1 d . . .
O10 O 0.37822(14) 0.5124(3) 0.41218(15) 0.0489(14) Uani 1 1 d . . .
O11 O 0.41663(13) 0.4107(3) 0.37704(14) 0.0374(12) Uani 1 1 d . . .
O12 O 0.40598(17) 0.3562(3) 0.43133(16) 0.0620(18) Uani 1 1 d . . .
O13 O 0.4430(2) -0.0297(3) 0.2721(2) 0.224(2) Uiso 0.75 1 d P . .
N1 N 0.5287(3) 0.0461(4) 0.2956(3) 0.070(2) Uani 1 1 d . . .
N2 N 0.7235(2) 0.2456(5) 0.2988(2) 0.068(2) Uani 1 1 d . . .
N3 N 0.7224(2) 0.7051(4) 0.2960(2) 0.063(2) Uani 1 1 d . . .
N4 N 0.5274(3) 0.8971(4) 0.2987(3) 0.078(2) Uani 1 1 d . . .
N5 N 0.2949(2) 0.6655(4) 0.2963(2) 0.063(2) Uani 1 1 d . . .
N6 N 0.2983(2) 0.2765(4) 0.29723(19) 0.060(2) Uani 1 1 d . . .
C1 C 0.5780(2) 0.3759(4) 0.4622(2) 0.0333(16) Uani 1 1 d . . .
C2 C 0.5652(2) 0.3214(4) 0.4361(2) 0.0396(17) Uani 1 1 d . . .
H2 H 0.5413 0.2993 0.4352 0.048 Uiso 1 1 calc R . .
C3 C 0.5867(2) 0.2980(4) 0.4109(2) 0.0425(19) Uani 1 1 d . . .
C4 C 0.6214(2) 0.3326(4) 0.4118(2) 0.0391(18) Uani 1 1 d . . .
C5 C 0.6344(2) 0.3864(4) 0.4367(2) 0.0413(19) Uani 1 1 d . . .
H5 H 0.6580 0.4086 0.4366 0.050 Uiso 1 1 calc R . .
C6 C 0.61357(19) 0.4100(4) 0.4627(2) 0.0314(16) Uani 1 1 d . . .
C7 C 0.62895(19) 0.4708(4) 0.48864(19) 0.0320(16) Uani 1 1 d . . .
H7A H 0.6588 0.4697 0.5001 0.038 Uiso 1 1 calc R . .
H7B H 0.6194 0.4714 0.5132 0.038 Uiso 1 1 calc R . .
C8 C 0.61488(18) 0.5333(4) 0.4622(2) 0.0314(16) Uani 1 1 d . . .
C9 C 0.6360(2) 0.5536(4) 0.4357(2) 0.0382(17) Uani 1 1 d . . .
H9 H 0.6591 0.5296 0.4359 0.046 Uiso 1 1 calc R . .
C10 C 0.6239(2) 0.6071(4) 0.4098(2) 0.045(2) Uani 1 1 d . . .
C11 C 0.5911(2) 0.6434(4) 0.4086(2) 0.0411(18) Uani 1 1 d . . .
C12 C 0.5693(2) 0.6231(4) 0.4347(2) 0.0375(17) Uani 1 1 d . . .
H12 H 0.5462 0.6472 0.4339 0.045 Uiso 1 1 calc R . .
C13 C 0.58082(18) 0.5691(3) 0.46145(18) 0.0232(14) Uani 1 1 d . . .
C14 C 0.55443(18) 0.5508(3) 0.48598(19) 0.0264(14) Uani 1 1 d . . .
H14A H 0.5448 0.5914 0.4957 0.032 Uiso 1 1 calc R . .
H14B H 0.5704 0.5255 0.5117 0.032 Uiso 1 1 calc R . .
C15 C 0.51819(17) 0.5099(3) 0.45939(19) 0.0213(14) Uani 1 1 d . . .
C16 C 0.48454(18) 0.5430(3) 0.43235(18) 0.0245(14) Uani 1 1 d . . .
H16 H 0.4843 0.5897 0.4322 0.029 Uiso 1 1 calc R . .
C17 C 0.45234(19) 0.5099(4) 0.4064(2) 0.0322(16) Uani 1 1 d . . .
C18 C 0.45163(19) 0.4422(4) 0.40653(19) 0.0328(16) Uani 1 1 d . . .
C19 C 0.48300(18) 0.4081(3) 0.43234(19) 0.0262(14) Uani 1 1 d . . .
H19 H 0.4823 0.3614 0.4324 0.031 Uiso 1 1 calc R . .
C20 C 0.51732(17) 0.4420(3) 0.45957(17) 0.0238(14) Uani 1 1 d . . .
C21 C 0.55277(19) 0.3994(3) 0.4874(2) 0.0290(15) Uani 1 1 d . . .
H21A H 0.5698 0.4255 0.5122 0.035 Uiso 1 1 calc R . .
H21B H 0.5422 0.3611 0.4984 0.035 Uiso 1 1 calc R . .
C22 C 0.5920(3) 0.1924(5) 0.3848(3) 0.063(2) Uani 1 1 d . . .
C23 C 0.5685(3) 0.1414(4) 0.3537(3) 0.060(2) Uani 1 1 d . . .
C24 C 0.5906(3) 0.0880(5) 0.3478(4) 0.082(3) Uani 1 1 d . . .
H24 H 0.6186 0.0836 0.3635 0.099 Uiso 1 1 calc R . .
C25 C 0.5701(4) 0.0430(6) 0.3184(4) 0.095(4) Uani 1 1 d . . .
H25 H 0.5847 0.0071 0.3130 0.114 Uiso 1 1 calc R . .
C26 C 0.5097(3) 0.0994(5) 0.3031(3) 0.075(3) Uani 1 1 d . . .
H26 H 0.4817 0.1043 0.2876 0.090 Uiso 1 1 calc R . .
C27 C 0.5290(3) 0.1472(5) 0.3322(3) 0.072(3) Uani 1 1 d . . .
H27 H 0.5144 0.1837 0.3370 0.087 Uiso 1 1 calc R . .
C28 C 0.6790(3) 0.2984(6) 0.3984(3) 0.080(4) Uani 1 1 d . . .
C29 C 0.6932(3) 0.2773(5) 0.3632(3) 0.062(2) Uani 1 1 d . . .
C30 C 0.7345(3) 0.2813(6) 0.3709(3) 0.081(4) Uani 1 1 d . . .
H30 H 0.7531 0.2949 0.3978 0.097 Uiso 1 1 calc R . .
C31 C 0.7469(3) 0.2648(7) 0.3378(3) 0.089(4) Uani 1 1 d . . .
H31 H 0.7750 0.2672 0.3431 0.107 Uiso 1 1 calc R . .
C32 C 0.6852(3) 0.2397(6) 0.2929(3) 0.071(3) Uani 1 1 d . . .
H32 H 0.6680 0.2215 0.2666 0.085 Uiso 1 1 calc R . .
C33 C 0.6676(3) 0.2591(5) 0.3238(3) 0.064(3) Uani 1 1 d . . .
H33 H 0.6393 0.2591 0.3170 0.077 Uiso 1 1 calc R . .
C34 C 0.6635(3) 0.6844(5) 0.3854(3) 0.060(2) Uani 1 1 d . . .
C35 C 0.6841(3) 0.6896(5) 0.3546(3) 0.059(2) Uani 1 1 d . . .
C36 C 0.6958(4) 0.7495(6) 0.3478(3) 0.085(4) Uani 1 1 d . . .
H36 H 0.6925 0.7863 0.3638 0.102 Uiso 1 1 calc R . .
C37 C 0.7132(3) 0.7563(5) 0.3166(3) 0.070(3) Uani 1 1 d . . .
H37 H 0.7189 0.7994 0.3093 0.084 Uiso 1 1 calc R . .
C38 C 0.7114(3) 0.6440(6) 0.3028(3) 0.069(3) Uani 1 1 d . . .
H38 H 0.7170 0.6077 0.2879 0.083 Uiso 1 1 calc R . .
C39 C 0.6911(3) 0.6340(5) 0.3326(3) 0.070(3) Uani 1 1 d . . .
H39 H 0.6827 0.5914 0.3374 0.083 Uiso 1 1 calc R . .
C40 C 0.5737(3) 0.7571(4) 0.3961(3) 0.062(2) Uani 1 1 d . . .
C41 C 0.5588(3) 0.8039(4) 0.3612(3) 0.057(2) Uani 1 1 d . . .
C42 C 0.5388(4) 0.8613(6) 0.3685(4) 0.095(4) Uani 1 1 d . . .
H42 H 0.5364 0.8680 0.3956 0.115 Uiso 1 1 calc R . .
C43 C 0.5232(5) 0.9062(6) 0.3368(4) 0.107(5) Uani 1 1 d . . .
H43 H 0.5094 0.9437 0.3416 0.128 Uiso 1 1 calc R . .
C44 C 0.5436(4) 0.8459(4) 0.2896(3) 0.085(4) Uani 1 1 d . . .
H44 H 0.5447 0.8411 0.2617 0.102 Uiso 1 1 calc R . .
C45 C 0.5606(3) 0.7944(4) 0.3218(3) 0.069(3) Uani 1 1 d . . .
H45 H 0.5724 0.7559 0.3151 0.083 Uiso 1 1 calc R . .
C46 C 0.3836(2) 0.5459(4) 0.3835(2) 0.0387(18) Uani 1 1 d . . .
C47 C 0.3532(2) 0.5885(5) 0.3530(2) 0.047(2) Uani 1 1 d . . .
C48 C 0.3646(2) 0.6348(5) 0.3300(2) 0.052(2) Uani 1 1 d . . .
H48 H 0.3920 0.6405 0.3326 0.063 Uiso 1 1 calc R . .
C49 C 0.3338(2) 0.6736(5) 0.3023(3) 0.062(3) Uani 1 1 d . . .
H49 H 0.3410 0.7077 0.2869 0.074 Uiso 1 1 calc R . .
C50 C 0.2852(2) 0.6176(6) 0.3194(3) 0.071(3) Uani 1 1 d . . .
H50 H 0.2576 0.6108 0.3154 0.085 Uiso 1 1 calc R . .
C51 C 0.3139(2) 0.5781(6) 0.3488(3) 0.077(4) Uani 1 1 d . . .
H51 H 0.3065 0.5455 0.3650 0.093 Uiso 1 1 calc R . .
C52 C 0.3969(2) 0.3663(4) 0.3935(2) 0.045(2) Uani 1 1 d . . .
C53 C 0.3624(2) 0.3368(5) 0.3589(3) 0.059(3) Uani 1 1 d . . .
C54 C 0.3454(2) 0.3650(5) 0.3191(3) 0.060(3) Uani 1 1 d . . .
H54 H 0.3550 0.4053 0.3120 0.072 Uiso 1 1 calc R . .
C55 C 0.3137(3) 0.3318(5) 0.2900(3) 0.067(3) Uani 1 1 d . . .
H55 H 0.3019 0.3507 0.2623 0.080 Uiso 1 1 calc R . .
C56 C 0.3141(3) 0.2501(5) 0.3369(3) 0.070(3) Uani 1 1 d . . .
H56 H 0.3024 0.2112 0.3431 0.084 Uiso 1 1 calc R . .
C57 C 0.3467(3) 0.2777(5) 0.3688(3) 0.065(3) Uani 1 1 d . . .
H57 H 0.3580 0.2578 0.3962 0.078 Uiso 1 1 calc R . .
I1 I 0.46395(13) 0.7352(2) 0.39936(15) 0.1988(16) Uiso 0.50 1 d P A 1
I2 I 0.73235(10) 0.46460(16) 0.41589(11) 0.1747(12) Uiso 0.50 1 d P B 1
I3 I 0.29030(17) 0.1284(3) 0.27105(18) 0.199(2) Uiso 0.25 1 d P . .
I4 I 0.21132(18) 0.3200(3) 0.22844(17) 0.202(2) Uiso 0.25 1 d P . .
O4A O 0.21132(18) 0.3200(3) 0.22844(17) 0.202(2) Uiso 0.75 1 d P . .
O3A O 0.29030(17) 0.1284(3) 0.27105(18) 0.199(2) Uiso 0.75 1 d P . .
I8 I 0.46871(12) 0.7377(2) 0.42494(15) 0.1055(12) Uiso 0.25 1 d P C 3
I13 I 0.4430(2) -0.0297(3) 0.2721(2) 0.224(2) Uiso 0.25 1 d 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
Co2 N5 2.144(7) 4_545 ?
Co2 N2 2.154(7) 2_655 ?
Co2 N6 2.161(6) . ?
Co2 N3 2.164(6) 3_445 ?
Co2 I3 2.349(6) . ?
Co2 I4 2.370(6) . ?
Co1 N1 2.137(9) . ?
Co1 N1 2.137(9) 2_655 ?
Co1 N4 2.183(8) 2_645 ?
Co1 N4 2.183(8) 1_545 ?
Co1 I13 2.382(7) 2_655 ?
Co1 O13 2.382(7) 2_655 ?
Co1 O13 2.383(7) . ?
O1 C22 1.350(10) . ?
O1 C3 1.368(9) . ?
O2 C22 1.226(11) . ?
O3 C28 1.353(11) . ?
O3 C4 1.408(8) . ?
O4 C28 1.174(10) . ?
O5 C34 1.384(11) . ?
O5 C10 1.419(8) . ?
O6 C34 1.205(11) . ?
O7 C11 1.380(9) . ?
O7 C40 1.385(10) . ?
O8 C40 1.227(10) . ?
O9 C46 1.349(8) . ?
O9 C17 1.429(8) . ?
O10 C46 1.244(9) . ?
O11 C52 1.370(9) . ?
O11 C18 1.435(7) . ?
O12 C52 1.206(9) . ?
N1 C26 1.345(12) . ?
N1 C25 1.399(14) . ?
N2 C32 1.307(13) . ?
N2 C31 1.333(12) . ?
N2 Co2 2.154(7) 2_655 ?
N3 C38 1.346(12) . ?
N3 C37 1.350(13) . ?
N3 Co2 2.164(6) 3 ?
N4 C44 1.276(12) . ?
N4 C43 1.347(13) . ?
N4 Co1 2.183(8) 1_565 ?
N5 C49 1.331(11) . ?
N5 C50 1.362(12) . ?
N5 Co2 2.145(7) 4 ?
N6 C55 1.310(11) . ?
N6 C56 1.355(11) . ?
C1 C2 1.385(10) . ?
C1 C6 1.437(10) . ?
C1 C21 1.503(9) . ?
C2 C3 1.401(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.410(11) . ?
C4 C5 1.355(11) . ?
C5 C6 1.409(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.497(10) . ?
C7 C8 1.528(10) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C13 1.404(9) . ?
C8 C9 1.408(9) . ?
C9 C10 1.362(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.369(11) . ?
C11 C12 1.413(9) . ?
C12 C13 1.382(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.491(8) . ?
C14 C15 1.526(8) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C20 1.383(9) . ?
C15 C16 1.391(9) . ?
C16 C17 1.346(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(10) . ?
C18 C19 1.336(9) . ?
C19 C20 1.416(8) . ?
C19 H19 0.9500 . ?
C20 C21 1.540(9) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.496(13) . ?
C23 C27 1.337(14) . ?
C23 C24 1.394(12) . ?
C24 C25 1.351(14) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.373(14) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 C29 1.494(12) . ?
C29 C33 1.362(12) . ?
C29 C30 1.398(14) . ?
C30 C31 1.366(12) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.435(11) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.458(11) . ?
C35 C36 1.334(13) . ?
C35 C39 1.418(13) . ?
C36 C37 1.392(13) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.430(12) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.451(13) . ?
C41 C45 1.356(12) . ?
C41 C42 1.429(13) . ?
C42 C43 1.358(15) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.470(13) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.476(10) . ?
C47 C48 1.366(11) . ?
C47 C51 1.368(12) . ?
C48 C49 1.401(10) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.393(11) . ?
C50 H50 0.9500 . ?
C51 H51 0.9500 . ?
C52 C53 1.483(10) . ?
C53 C54 1.375(12) . ?
C53 C57 1.413(12) . ?
C54 C55 1.376(11) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C57 1.385(12) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Co2 N2 90.0(3) 4_545 2_655 ?
N5 Co2 N6 176.5(3) 4_545 . ?
N2 Co2 N6 91.3(2) 2_655 . ?
N5 Co2 N3 89.3(2) 4_545 3_445 ?
N2 Co2 N3 176.9(3) 2_655 3_445 ?
N6 Co2 N3 89.6(2) . 3_445 ?
N5 Co2 I3 89.2(3) 4_545 . ?
N2 Co2 I3 92.2(3) 2_655 . ?
N6 Co2 I3 87.5(3) . . ?
N3 Co2 I3 90.7(3) 3_445 . ?
N5 Co2 I4 91.5(3) 4_545 . ?
N2 Co2 I4 88.2(3) 2_655 . ?
N6 Co2 I4 91.7(3) . . ?
N3 Co2 I4 88.8(3) 3_445 . ?
I3 Co2 I4 179.1(2) . . ?
N1 Co1 N1 89.4(4) . 2_655 ?
N1 Co1 N4 176.9(3) . 2_645 ?
N1 Co1 N4 89.3(3) 2_655 2_645 ?
N1 Co1 N4 89.3(3) . 1_545 ?
N1 Co1 N4 176.9(3) 2_655 1_545 ?
N4 Co1 N4 92.2(4) 2_645 1_545 ?
N1 Co1 I13 89.1(3) . 2_655 ?
N1 Co1 I13 91.7(3) 2_655 2_655 ?
N4 Co1 I13 88.2(3) 2_645 2_655 ?
N4 Co1 I13 91.1(3) 1_545 2_655 ?
N1 Co1 O13 89.1(3) . 2_655 ?
N1 Co1 O13 91.7(3) 2_655 2_655 ?
N4 Co1 O13 88.2(3) 2_645 2_655 ?
N4 Co1 O13 91.1(3) 1_545 2_655 ?
I13 Co1 O13 0.0(4) 2_655 2_655 ?
N1 Co1 O13 91.7(3) . . ?
N1 Co1 O13 89.1(3) 2_655 . ?
N4 Co1 O13 91.1(3) 2_645 . ?
N4 Co1 O13 88.2(3) 1_545 . ?
I13 Co1 O13 178.9(3) 2_655 . ?
O13 Co1 O13 178.9(3) 2_655 . ?
C22 O1 C3 119.9(6) . . ?
C28 O3 C4 116.2(6) . . ?
C34 O5 C10 120.4(6) . . ?
C11 O7 C40 120.0(6) . . ?
C46 O9 C17 119.3(5) . . ?
C52 O11 C18 117.4(5) . . ?
C26 N1 C25 115.7(9) . . ?
C26 N1 Co1 124.2(7) . . ?
C25 N1 Co1 120.1(6) . . ?
C32 N2 C31 115.5(8) . . ?
C32 N2 Co2 124.0(6) . 2_655 ?
C31 N2 Co2 120.5(6) . 2_655 ?
C38 N3 C37 119.4(7) . . ?
C38 N3 Co2 121.1(7) . 3 ?
C37 N3 Co2 119.3(6) . 3 ?
C44 N4 C43 123.1(9) . . ?
C44 N4 Co1 120.6(7) . 1_565 ?
C43 N4 Co1 116.0(8) . 1_565 ?
C49 N5 C50 117.3(7) . . ?
C49 N5 Co2 121.6(6) . 4 ?
C50 N5 Co2 121.1(5) . 4 ?
C55 N6 C56 117.7(7) . . ?
C55 N6 Co2 124.0(5) . . ?
C56 N6 Co2 118.2(6) . . ?
C2 C1 C6 119.1(6) . . ?
C2 C1 C21 118.7(6) . . ?
C6 C1 C21 122.1(6) . . ?
C1 C2 C3 121.6(7) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
O1 C3 C2 119.2(7) . . ?
O1 C3 C4 122.0(6) . . ?
C2 C3 C4 118.2(7) . . ?
C5 C4 O3 122.8(7) . . ?
C5 C4 C3 121.6(6) . . ?
O3 C4 C3 115.4(7) . . ?
C4 C5 C6 121.0(7) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 118.5(7) . . ?
C5 C6 C7 118.3(6) . . ?
C1 C6 C7 123.1(5) . . ?
C6 C7 C8 112.0(5) . . ?
C6 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C13 C8 C9 118.8(7) . . ?
C13 C8 C7 123.2(5) . . ?
C9 C8 C7 117.9(6) . . ?
C10 C9 C8 120.9(7) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 121.7(6) . . ?
C9 C10 O5 118.4(6) . . ?
C11 C10 O5 119.8(7) . . ?
C10 C11 O7 120.6(6) . . ?
C10 C11 C12 117.8(7) . . ?
O7 C11 C12 121.4(7) . . ?
C13 C12 C11 121.9(7) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C12 C13 C8 118.8(6) . . ?
C12 C13 C14 116.9(6) . . ?
C8 C13 C14 124.2(6) . . ?
C13 C14 C15 112.3(5) . . ?
C13 C14 H14A 109.1 . . ?
C15 C14 H14A 109.1 . . ?
C13 C14 H14B 109.1 . . ?
C15 C14 H14B 109.1 . . ?
H14A C14 H14B 107.9 . . ?
C20 C15 C16 118.1(5) . . ?
C20 C15 C14 123.9(5) . . ?
C16 C15 C14 117.9(5) . . ?
C17 C16 C15 121.1(6) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C18 120.7(6) . . ?
C16 C17 O9 118.2(6) . . ?
C18 C17 O9 121.2(6) . . ?
C19 C18 C17 120.6(6) . . ?
C19 C18 O11 122.3(6) . . ?
C17 C18 O11 117.1(6) . . ?
C18 C19 C20 119.6(6) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C15 C20 C19 120.0(6) . . ?
C15 C20 C21 123.4(5) . . ?
C19 C20 C21 116.6(6) . . ?
C1 C21 C20 111.3(5) . . ?
C1 C21 H21A 109.4 . . ?
C20 C21 H21A 109.4 . . ?
C1 C21 H21B 109.4 . . ?
C20 C21 H21B 109.4 . . ?
H21A C21 H21B 108.0 . . ?
O2 C22 O1 122.0(8) . . ?
O2 C22 C23 125.4(8) . . ?
O1 C22 C23 112.3(8) . . ?
C27 C23 C24 121.9(9) . . ?
C27 C23 C22 122.4(8) . . ?
C24 C23 C22 115.7(9) . . ?
C25 C24 C23 116.5(10) . . ?
C25 C24 H24 121.8 . . ?
C23 C24 H24 121.8 . . ?
C24 C25 N1 123.9(9) . . ?
C24 C25 H25 118.1 . . ?
N1 C25 H25 118.1 . . ?
N1 C26 C27 123.1(10) . . ?
N1 C26 H26 118.5 . . ?
C27 C26 H26 118.5 . . ?
C23 C27 C26 118.9(9) . . ?
C23 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
O4 C28 O3 125.3(8) . . ?
O4 C28 C29 124.4(8) . . ?
O3 C28 C29 109.8(7) . . ?
C33 C29 C30 119.5(8) . . ?
C33 C29 C28 122.9(8) . . ?
C30 C29 C28 117.5(9) . . ?
C31 C30 C29 116.9(9) . . ?
C31 C30 H30 121.6 . . ?
C29 C30 H30 121.6 . . ?
N2 C31 C30 126.5(9) . . ?
N2 C31 H31 116.8 . . ?
C30 C31 H31 116.8 . . ?
N2 C32 C33 123.9(9) . . ?
N2 C32 H32 118.0 . . ?
C33 C32 H32 118.0 . . ?
C29 C33 C32 117.3(8) . . ?
C29 C33 H33 121.4 . . ?
C32 C33 H33 121.4 . . ?
O6 C34 O5 120.9(7) . . ?
O6 C34 C35 128.5(8) . . ?
O5 C34 C35 110.4(8) . . ?
C36 C35 C39 121.2(8) . . ?
C36 C35 C34 116.7(9) . . ?
C39 C35 C34 122.1(8) . . ?
C35 C36 C37 117.7(11) . . ?
C35 C36 H36 121.2 . . ?
C37 C36 H36 121.2 . . ?
N3 C37 C36 123.7(9) . . ?
N3 C37 H37 118.2 . . ?
C36 C37 H37 118.2 . . ?
N3 C38 C39 119.6(9) . . ?
N3 C38 H38 120.2 . . ?
C39 C38 H38 120.2 . . ?
C35 C39 C38 118.1(8) . . ?
C35 C39 H39 121.0 . . ?
C38 C39 H39 121.0 . . ?
O8 C40 O7 121.2(9) . . ?
O8 C40 C41 127.8(9) . . ?
O7 C40 C41 110.8(7) . . ?
C45 C41 C42 118.5(9) . . ?
C45 C41 C40 123.7(8) . . ?
C42 C41 C40 117.7(8) . . ?
C43 C42 C41 120.6(10) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
N4 C43 C42 119.4(11) . . ?
N4 C43 H43 120.3 . . ?
C42 C43 H43 120.3 . . ?
N4 C44 C45 120.8(8) . . ?
N4 C44 H44 119.6 . . ?
C45 C44 H44 119.6 . . ?
C41 C45 C44 117.4(8) . . ?
C41 C45 H45 121.3 . . ?
C44 C45 H45 121.3 . . ?
O10 C46 O9 121.4(6) . . ?
O10 C46 C47 125.3(6) . . ?
O9 C46 C47 113.2(6) . . ?
C48 C47 C51 122.8(7) . . ?
C48 C47 C46 120.2(7) . . ?
C51 C47 C46 116.9(7) . . ?
C47 C48 C49 116.3(7) . . ?
C47 C48 H48 121.8 . . ?
C49 C48 H48 121.8 . . ?
N5 C49 C48 123.8(8) . . ?
N5 C49 H49 118.1 . . ?
C48 C49 H49 118.1 . . ?
N5 C50 C51 123.0(8) . . ?
N5 C50 H50 118.5 . . ?
C51 C50 H50 118.5 . . ?
C47 C51 C50 116.7(9) . . ?
C47 C51 H51 121.6 . . ?
C50 C51 H51 121.6 . . ?
O12 C52 O11 123.1(6) . . ?
O12 C52 C53 126.2(7) . . ?
O11 C52 C53 110.6(6) . . ?
C54 C53 C57 120.4(8) . . ?
C54 C53 C52 123.1(8) . . ?
C57 C53 C52 116.6(7) . . ?
C53 C54 C55 116.6(8) . . ?
C53 C54 H54 121.7 . . ?
C55 C54 H54 121.7 . . ?
N6 C55 C54 125.6(8) . . ?
N6 C55 H55 117.2 . . ?
C54 C55 H55 117.2 . . ?
N6 C56 C57 122.4(8) . . ?
N6 C56 H56 118.8 . . ?
C57 C56 H56 118.8 . . ?
C56 C57 C53 117.2(8) . . ?
C56 C57 H57 121.4 . . ?
C53 C57 H57 121.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Co1 N1 C26 45.7(7) 2_655 . . . ?
N4 Co1 N1 C26 110(6) 2_645 . . . ?
N4 Co1 N1 C26 -131.5(9) 1_545 . . . ?
I13 Co1 N1 C26 137.4(9) 2_655 . . . ?
O13 Co1 N1 C26 137.4(9) 2_655 . . . ?
O13 Co1 N1 C26 -43.4(9) . . . . ?
N1 Co1 N1 C25 -131.4(10) 2_655 . . . ?
N4 Co1 N1 C25 -67(6) 2_645 . . . ?
N4 Co1 N1 C25 51.5(9) 1_545 . . . ?
I13 Co1 N1 C25 -39.6(9) 2_655 . . . ?
O13 Co1 N1 C25 -39.6(9) 2_655 . . . ?
O13 Co1 N1 C25 139.6(9) . . . . ?
N5 Co2 N6 C55 150(4) 4_545 . . . ?
N2 Co2 N6 C55 39.2(9) 2_655 . . . ?
N3 Co2 N6 C55 -137.8(9) 3_445 . . . ?
I3 Co2 N6 C55 131.4(8) . . . . ?
I4 Co2 N6 C55 -49.0(9) . . . . ?
N5 Co2 N6 C56 -28(5) 4_545 . . . ?
N2 Co2 N6 C56 -138.8(8) 2_655 . . . ?
N3 Co2 N6 C56 44.1(8) 3_445 . . . ?
I3 Co2 N6 C56 -46.6(8) . . . . ?
I4 Co2 N6 C56 132.9(7) . . . . ?
C6 C1 C2 C3 1.4(11) . . . . ?
C21 C1 C2 C3 178.2(6) . . . . ?
C22 O1 C3 C2 -123.5(8) . . . . ?
C22 O1 C3 C4 64.9(10) . . . . ?
C1 C2 C3 O1 -173.6(7) . . . . ?
C1 C2 C3 C4 -1.7(11) . . . . ?
C28 O3 C4 C5 56.8(11) . . . . ?
C28 O3 C4 C3 -129.0(9) . . . . ?
O1 C3 C4 C5 172.7(7) . . . . ?
C2 C3 C4 C5 1.0(11) . . . . ?
O1 C3 C4 O3 -1.6(11) . . . . ?
C2 C3 C4 O3 -173.2(6) . . . . ?
O3 C4 C5 C6 173.7(6) . . . . ?
C3 C4 C5 C6 -0.1(11) . . . . ?
C4 C5 C6 C1 -0.2(10) . . . . ?
C4 C5 C6 C7 -178.5(6) . . . . ?
C2 C1 C6 C5 -0.5(10) . . . . ?
C21 C1 C6 C5 -177.1(6) . . . . ?
C2 C1 C6 C7 177.7(6) . . . . ?
C21 C1 C6 C7 1.1(10) . . . . ?
C5 C6 C7 C8 82.0(7) . . . . ?
C1 C6 C7 C8 -96.2(7) . . . . ?
C6 C7 C8 C13 95.7(7) . . . . ?
C6 C7 C8 C9 -80.9(7) . . . . ?
C13 C8 C9 C10 0.2(11) . . . . ?
C7 C8 C9 C10 176.9(7) . . . . ?
C8 C9 C10 C11 0.3(12) . . . . ?
C8 C9 C10 O5 -177.3(7) . . . . ?
C34 O5 C10 C9 -121.4(9) . . . . ?
C34 O5 C10 C11 60.9(10) . . . . ?
C9 C10 C11 O7 -177.0(7) . . . . ?
O5 C10 C11 O7 0.6(12) . . . . ?
C9 C10 C11 C12 -1.0(12) . . . . ?
O5 C10 C11 C12 176.6(6) . . . . ?
C40 O7 C11 C10 -125.5(9) . . . . ?
C40 O7 C11 C12 58.7(10) . . . . ?
C10 C11 C12 C13 1.1(11) . . . . ?
O7 C11 C12 C13 177.1(6) . . . . ?
C11 C12 C13 C8 -0.6(10) . . . . ?
C11 C12 C13 C14 -177.4(6) . . . . ?
C9 C8 C13 C12 -0.1(9) . . . . ?
C7 C8 C13 C12 -176.6(6) . . . . ?
C9 C8 C13 C14 176.4(6) . . . . ?
C7 C8 C13 C14 -0.1(10) . . . . ?
C12 C13 C14 C15 82.3(7) . . . . ?
C8 C13 C14 C15 -94.3(7) . . . . ?
C13 C14 C15 C20 94.4(7) . . . . ?
C13 C14 C15 C16 -83.4(6) . . . . ?
C20 C15 C16 C17 -1.5(8) . . . . ?
C14 C15 C16 C17 176.5(5) . . . . ?
C15 C16 C17 C18 1.3(9) . . . . ?
C15 C16 C17 O9 -177.2(5) . . . . ?
C46 O9 C17 C16 -114.4(7) . . . . ?
C46 O9 C17 C18 67.2(8) . . . . ?
C16 C17 C18 C19 -0.4(9) . . . . ?
O9 C17 C18 C19 178.0(5) . . . . ?
C16 C17 C18 O11 -178.4(5) . . . . ?
O9 C17 C18 O11 0.0(8) . . . . ?
C52 O11 C18 C19 56.0(8) . . . . ?
C52 O11 C18 C17 -126.0(7) . . . . ?
C17 C18 C19 C20 -0.3(8) . . . . ?
O11 C18 C19 C20 177.6(5) . . . . ?
C16 C15 C20 C19 0.8(8) . . . . ?
C14 C15 C20 C19 -177.1(5) . . . . ?
C16 C15 C20 C21 179.0(5) . . . . ?
C14 C15 C20 C21 1.1(8) . . . . ?
C18 C19 C20 C15 0.1(8) . . . . ?
C18 C19 C20 C21 -178.2(5) . . . . ?
C2 C1 C21 C20 -81.5(8) . . . . ?
C6 C1 C21 C20 95.1(7) . . . . ?
C15 C20 C21 C1 -97.3(7) . . . . ?
C19 C20 C21 C1 81.0(7) . . . . ?
C3 O1 C22 O2 1.9(14) . . . . ?
C3 O1 C22 C23 175.2(7) . . . . ?
O2 C22 C23 C27 161.8(11) . . . . ?
O1 C22 C23 C27 -11.3(14) . . . . ?
O2 C22 C23 C24 -19.6(15) . . . . ?
O1 C22 C23 C24 167.3(9) . . . . ?
C27 C23 C24 C25 1.4(17) . . . . ?
C22 C23 C24 C25 -177.3(11) . . . . ?
C23 C24 C25 N1 -2.4(19) . . . . ?
C26 N1 C25 C24 2.7(18) . . . . ?
Co1 N1 C25 C24 -180.0(10) . . . . ?
C25 N1 C26 C27 -2.0(16) . . . . ?
Co1 N1 C26 C27 -179.1(8) . . . . ?
C24 C23 C27 C26 -0.7(16) . . . . ?
C22 C23 C27 C26 177.8(10) . . . . ?
N1 C26 C27 C23 1.1(17) . . . . ?
C4 O3 C28 O4 8.8(17) . . . . ?
C4 O3 C28 C29 -179.0(8) . . . . ?
O4 C28 C29 C33 158.0(13) . . . . ?
O3 C28 C29 C33 -14.4(15) . . . . ?
O4 C28 C29 C30 -26.6(19) . . . . ?
O3 C28 C29 C30 161.1(10) . . . . ?
C33 C29 C30 C31 -1.5(17) . . . . ?
C28 C29 C30 C31 -177.1(11) . . . . ?
C32 N2 C31 C30 -3.1(19) . . . . ?
Co2 N2 C31 C30 178.8(10) 2_655 . . . ?
C29 C30 C31 N2 0(2) . . . . ?
C31 N2 C32 C33 6.8(16) . . . . ?
Co2 N2 C32 C33 -175.2(8) 2_655 . . . ?
C30 C29 C33 C32 4.8(16) . . . . ?
C28 C29 C33 C32 -179.8(10) . . . . ?
N2 C32 C33 C29 -7.9(16) . . . . ?
C10 O5 C34 O6 3.7(13) . . . . ?
C10 O5 C34 C35 179.3(7) . . . . ?
O6 C34 C35 C36 -17.9(16) . . . . ?
O5 C34 C35 C36 166.9(9) . . . . ?
O6 C34 C35 C39 162.4(11) . . . . ?
O5 C34 C35 C39 -12.7(13) . . . . ?
C39 C35 C36 C37 3.7(17) . . . . ?
C34 C35 C36 C37 -176.0(10) . . . . ?
C38 N3 C37 C36 6.0(15) . . . . ?
Co2 N3 C37 C36 -178.5(9) 3 . . . ?
C35 C36 C37 N3 -6.9(17) . . . . ?
C37 N3 C38 C39 -1.8(14) . . . . ?
Co2 N3 C38 C39 -177.3(7) 3 . . . ?
C36 C35 C39 C38 0.1(15) . . . . ?
C34 C35 C39 C38 179.7(9) . . . . ?
N3 C38 C39 C35 -1.1(14) . . . . ?
C11 O7 C40 O8 6.1(12) . . . . ?
C11 O7 C40 C41 -178.0(7) . . . . ?
O8 C40 C41 C45 157.3(11) . . . . ?
O7 C40 C41 C45 -18.2(14) . . . . ?
O8 C40 C41 C42 -26.8(16) . . . . ?
O7 C40 C41 C42 157.7(9) . . . . ?
C45 C41 C42 C43 -2.2(19) . . . . ?
C40 C41 C42 C43 -178.3(12) . . . . ?
C44 N4 C43 C42 4(2) . . . . ?
Co1 N4 C43 C42 178.8(11) 1_565 . . . ?
C41 C42 C43 N4 -1(2) . . . . ?
C43 N4 C44 C45 -3.0(19) . . . . ?
Co1 N4 C44 C45 -177.4(8) 1_565 . . . ?
C42 C41 C45 C44 3.2(16) . . . . ?
C40 C41 C45 C44 179.0(10) . . . . ?
N4 C44 C45 C41 -0.8(18) . . . . ?
C17 O9 C46 O10 -1.4(10) . . . . ?
C17 O9 C46 C47 177.6(6) . . . . ?
O10 C46 C47 C48 163.9(8) . . . . ?
O9 C46 C47 C48 -15.0(11) . . . . ?
O10 C46 C47 C51 -17.3(13) . . . . ?
O9 C46 C47 C51 163.8(8) . . . . ?
C51 C47 C48 C49 2.2(14) . . . . ?
C46 C47 C48 C49 -179.1(7) . . . . ?
C50 N5 C49 C48 1.7(14) . . . . ?
Co2 N5 C49 C48 -176.5(7) 4 . . . ?
C47 C48 C49 N5 -3.0(14) . . . . ?
C49 N5 C50 C51 0.6(15) . . . . ?
Co2 N5 C50 C51 178.8(8) 4 . . . ?
C48 C47 C51 C50 -0.1(15) . . . . ?
C46 C47 C51 C50 -178.9(8) . . . . ?
N5 C50 C51 C47 -1.3(16) . . . . ?
C18 O11 C52 O12 5.4(11) . . . . ?
C18 O11 C52 C53 -178.3(7) . . . . ?
O12 C52 C53 C54 157.2(10) . . . . ?
O11 C52 C53 C54 -19.0(12) . . . . ?
O12 C52 C53 C57 -21.5(14) . . . . ?
O11 C52 C53 C57 162.2(8) . . . . ?
C57 C53 C54 C55 -1.8(14) . . . . ?
C52 C53 C54 C55 179.5(9) . . . . ?
C56 N6 C55 C54 1.8(16) . . . . ?
Co2 N6 C55 C54 -176.3(8) . . . . ?
C53 C54 C55 N6 0.7(16) . . . . ?
C55 N6 C56 C57 -3.2(16) . . . . ?
Co2 N6 C56 C57 175.0(8) . . . . ?
N6 C56 C57 C53 2.1(16) . . . . ?
C54 C53 C57 C56 0.4(15) . . . . ?
C52 C53 C57 C56 179.3(9) . . . . ?

_diffrn_measured_fraction_theta_max 0.806
_diffrn_reflns_theta_full        59.64
_diffrn_measured_fraction_theta_full 0.806
_refine_diff_density_max         1.337
_refine_diff_density_min         -1.636
_refine_diff_density_rms         0.116
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 -0.005 0.361 -0.013 13176 3761 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

# start Validation Reply Form
_vrf_DIFF019_I                   
;
PROBLEM: _diffrn_standards_number is missing
RESPONSE: not relevant
;
_vrf_DIFF020_I                   
;
PROBLEM: _diffrn_standards_interval_count and
RESPONSE: not relevant
;
_vrf_DIFF022_I                   
;
PROBLEM: _diffrn_standards_decay_% is missing
RESPONSE: not relevant
;
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.806 Why?  
RESPONSE: large cell, obs data:parameter ratio is > 12
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cutfa_sq
_database_code_depnum_ccdc_archive 'CCDC 1823165'
_audit_update_record             
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_audit_creation_date             2017-08-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            
;
[hexakis(isonicotinoyl)cyclotricatechylene]
tris(trifluoroacetate)(isoniconinate)dicopper(II)
;
_chemical_name_systematic        ?
_chemical_formula_moiety         'C69 H40 Cu2 F9 N7 O20'
_chemical_formula_sum            'C69 H40 Cu2 F9 N7 O20'
_chemical_formula_weight         1585.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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                   18.1806(11)
_cell_length_b                   18.4809(11)
_cell_length_c                   19.4599(13)
_cell_angle_alpha                103.319(6)
_cell_angle_beta                 109.243(6)
_cell_angle_gamma                103.091(5)
_cell_volume                     5672.3(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      49.4030
_cell_measurement_theta_min      3.8310
_shelx_estimated_absorpt_T_max   0.970
_shelx_estimated_absorpt_T_min   0.932
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.1295
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27829
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        51.417
_diffrn_reflns_theta_max         51.417
_diffrn_reflns_theta_min         2.978
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     21.00  61.00   1.00    2.00    --    0.00  57.00  30.00   40
  2  ω     31.00 133.00   1.00    8.00    --   59.61  19.00 150.00  102
  3  ω     55.00  80.00   1.00    8.00    --   59.61 -65.00  88.14   25
  4  ω     53.00  87.00   1.00    8.00    --   59.61 -65.00 144.54   34
  5  ω     50.00  87.00   1.00    8.00    --   59.61 -65.00  36.91   37
  6  ω     60.00  87.00   1.00    8.00    --   59.61 -65.00 -66.23   27
  7  ω     53.00  81.00   1.00    8.00    --   59.61 -64.00 -86.31   28
  8  ω     52.00  87.00   1.00    8.00    --   59.61 -64.00-121.27   35
  9  ω     52.00  82.00   1.00    8.00    --   59.61 -65.00-170.05   30
 10  ω     51.00  79.00   1.00    8.00    --   59.61 -65.00-150.86   28
 11  ω     27.00  87.00   1.00    8.00    --   59.61 -65.00  -6.78   60
 12  ω     17.00  77.00   1.00    8.00    --   59.61 -65.00 127.28   60
 13  ω    -17.00  90.00   1.00    8.00    --   59.61 -19.00 -60.00  107
 14  ω     72.00 124.00   1.00    8.00    --   59.61  65.00-177.21   52
 15  ω     32.00  59.00   1.00    8.00    --   59.61  65.00-177.21   27
 16  ω     -7.00  39.00   1.00    8.00    --   59.61 -64.00 -86.31   46
 17  ω     -9.00  29.00   1.00    8.00    --   59.61 -64.00-121.27   38
 18  ω    -59.00 -32.00   1.00    2.00    --    0.00 -57.00-180.00   27
 19  ω    -25.00  18.00   1.00    2.00    --    0.00  57.00  30.00   43
 20  ω    -65.00  24.00   1.00    2.00    --    0.00 -57.00-120.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0409991000
_diffrn_orient_matrix_UB_12      -0.0618341000
_diffrn_orient_matrix_UB_13      -0.0191662000
_diffrn_orient_matrix_UB_21      -0.0701087000
_diffrn_orient_matrix_UB_22      -0.0386218000
_diffrn_orient_matrix_UB_23      -0.0812454000
_diffrn_orient_matrix_UB_31      0.0493770000
_diffrn_orient_matrix_UB_32      0.0539912000
_diffrn_orient_matrix_UB_33      -0.0305289000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6609
_reflns_number_total             11988
_reflns_odcompleteness_completeness 98.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_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         0.916
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         11988
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1792
_refine_ls_R_factor_gt           0.1249
_refine_ls_restrained_S_all      1.055
_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)+(0.1826P)²+38.2928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3474
_refine_ls_wR_factor_ref         0.3868
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C64-C65
 1.45 with sigma of 0.02
 C68-C70
 1.45 with sigma of 0.02
 O15-C68
 1.35 with sigma of 0.02
3. Restrained planarity
 O16, C64, C65, O17
 with sigma of 0.1
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C24(H24), C25(H25),
 C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C37(H37),
  C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C48(H48),
 C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56), C57(H57), C60(H60),
  C61(H61), C62(H62), C63(H63)
;
_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
Cu1 Cu 0.39438(10) 0.72038(9) 0.54849(11) 0.0393(5) Uani 1 1 d . . . . .
Cu2 Cu -0.12549(10) 0.63968(10) 0.68197(11) 0.0436(6) Uani 1 1 d . . . . .
F1 F -0.1774(10) 0.6293(9) 0.4133(9) 0.163(5) Uiso 1 1 d . . . . .
F2 F -0.0525(9) 0.6881(9) 0.4895(8) 0.148(5) Uiso 1 1 d . . . . .
F3 F -0.1073(10) 0.5690(9) 0.4244(9) 0.168(5) Uiso 1 1 d . . . . .
F4 F -0.1768(6) 0.6135(6) 0.8914(6) 0.089(3) Uiso 1 1 d . . . . .
F5 F -0.2028(8) 0.4894(8) 0.8543(8) 0.141(4) Uiso 1 1 d . . . . .
F6 F -0.2962(10) 0.5357(9) 0.8060(9) 0.166(5) Uiso 1 1 d . . . . .
F7 F 0.1435(14) 0.7673(14) 0.5280(14) 0.255(9) Uiso 1 1 d . . . . .
F8 F 0.0871(13) 0.7191(11) 0.4068(12) 0.205(7) Uiso 1 1 d . . . . .
F9 F 0.1120(11) 0.6402(11) 0.4732(10) 0.198(7) Uiso 1 1 d . . . . .
O1 O 0.4153(6) 0.6227(5) 0.8787(5) 0.056(2) Uiso 1 1 d . . . . .
O2 O 0.3157(5) 0.5146(4) 0.7884(4) 0.037(2) Uiso 1 1 d . . . . .
O3 O 0.1927(5) 0.5057(5) 0.8448(5) 0.049(2) Uiso 1 1 d . . . . .
O4 O 0.1219(8) 0.4023(8) 0.7375(7) 0.098(4) Uiso 1 1 d . . . . .
O5 O 0.0362(6) 0.2048(6) 0.9977(6) 0.069(3) Uiso 1 1 d . . . . .
O6 O 0.0408(5) 0.1546(5) 0.8848(5) 0.051(2) Uiso 1 1 d . . . . .
O7 O 0.0760(5) 0.0351(5) 0.9600(5) 0.055(2) Uiso 1 1 d . . . . .
O8 O 0.1174(5) 0.0438(5) 0.8619(5) 0.045(2) Uiso 1 1 d . . . . .
O9 O 0.4264(5) 0.0992(5) 0.7715(5) 0.051(2) Uiso 1 1 d . . . . .
O10 O 0.5634(7) 0.1230(6) 0.8106(6) 0.077(3) Uiso 1 1 d . . . . .
O11 O 0.4873(5) 0.2367(5) 0.7444(5) 0.046(2) Uiso 1 1 d . . . . .
O12 O 0.6171(6) 0.3184(5) 0.8196(6) 0.060(3) Uiso 1 1 d . . . . .
O13 O 0.5099(5) 0.7265(4) 0.5865(4) 0.036(2) Uiso 1 1 d . . . . .
O14 O 0.4596(5) 0.5989(5) 0.5129(5) 0.047(2) Uiso 1 1 d . . . . .
O15 O 0.2702(5) 0.6971(5) 0.5055(5) 0.051(2) Uiso 1 1 d D . . . .
O16 O -0.0934(5) 0.6593(5) 0.6001(5) 0.053(2) Uiso 1 1 d . . . . .
O17 O -0.1816(6) 0.5385(6) 0.5147(6) 0.070(3) Uiso 1 1 d . . . . .
O18 O -0.1550(5) 0.6225(5) 0.7678(5) 0.049(2) Uiso 1 1 d . . . . .
O19 O -0.2120(6) 0.4896(5) 0.7120(5) 0.061(3) Uiso 1 1 d . . . . .
O21 O 0.2503(13) 0.7825(13) 0.4322(12) 0.191(8) Uiso 1 1 d . . . . .
N1 N 0.3828(6) 0.6771(5) 0.6306(5) 0.032(2) Uiso 1 1 d . . . . .
N2 N -0.0403(7) 0.5871(7) 0.7114(7) 0.056(3) Uiso 1 1 d . . . . .
N3 N -0.2525(15) 0.0396(16) 0.8267(16) 0.170(9) Uiso 1 1 d . . . . .
N4 N -0.0553(6) -0.2367(6) 0.7564(6) 0.042(3) Uiso 1 1 d . . . . .
N5 N 0.4312(6) -0.1535(6) 0.6209(6) 0.042(3) Uiso 1 1 d . . . . .
N6 N 0.5953(6) 0.2690(6) 0.5470(6) 0.045(3) Uiso 1 1 d . . . . .
N7 N 0.7630(6) 0.6499(5) 0.6320(5) 0.036(2) Uiso 1 1 d . . . . .
C1 C 0.3828(7) 0.4185(6) 0.9344(7) 0.033(3) Uiso 1 1 d . . . . .
C2 C 0.3811(7) 0.4538(6) 0.8768(7) 0.035(3) Uiso 1 1 d . . . . .
H2 H 0.4248 0.4601 0.8598 0.042 Uiso 1 1 calc R . . . .
C3 C 0.3183(8) 0.4780(7) 0.8466(7) 0.042(3) Uiso 1 1 d . . . . .
C4 C 0.2538(8) 0.4707(7) 0.8711(7) 0.045(3) Uiso 1 1 d . . . . .
C5 C 0.2502(8) 0.4317(7) 0.9222(7) 0.040(3) Uiso 1 1 d . . . . .
H5 H 0.2033 0.4221 0.9346 0.048 Uiso 1 1 calc R . . . .
C6 C 0.3150(8) 0.4061(7) 0.9564(7) 0.042(3) Uiso 1 1 d . . . . .
C7 C 0.3093(8) 0.3684(7) 1.0160(7) 0.041(3) Uiso 1 1 d . . . . .
H7A H 0.2821 0.3945 1.0457 0.049 Uiso 1 1 calc R . . . .
H7B H 0.3657 0.3762 1.0525 0.049 Uiso 1 1 calc R . . . .
C8 C 0.2616(7) 0.2816(6) 0.9801(6) 0.029(3) Uiso 1 1 d . . . . .
C9 C 0.1756(7) 0.2561(7) 0.9491(7) 0.042(3) Uiso 1 1 d . . . . .
H9 H 0.1485 0.2943 0.9516 0.050 Uiso 1 1 calc R . . . .
C10 C 0.1301(7) 0.1807(7) 0.9162(7) 0.037(3) Uiso 1 1 d . . . . .
C11 C 0.1667(8) 0.1274(7) 0.9063(7) 0.046(3) Uiso 1 1 d . . . . .
C12 C 0.2508(7) 0.1430(7) 0.9320(7) 0.041(3) Uiso 1 1 d . . . . .
H12 H 0.2745 0.1025 0.9243 0.049 Uiso 1 1 calc R . . . .
C13 C 0.3001(7) 0.2240(7) 0.9708(7) 0.038(3) Uiso 1 1 d . . . . .
C14 C 0.3933(8) 0.2406(8) 0.9975(7) 0.045(3) Uiso 1 1 d . . . . .
H14A H 0.4229 0.2918 1.0398 0.054 Uiso 1 1 calc R . . . .
H14B H 0.4083 0.1991 1.0178 0.054 Uiso 1 1 calc R . . . .
C15 C 0.4186(7) 0.2425(7) 0.9336(7) 0.041(3) Uiso 1 1 d . . . . .
C16 C 0.4153(7) 0.1716(7) 0.8843(7) 0.040(3) Uiso 1 1 d . . . . .
H16 H 0.3976 0.1236 0.8933 0.048 Uiso 1 1 calc R . . . .
C17 C 0.4376(7) 0.1716(7) 0.8230(7) 0.040(3) Uiso 1 1 d . . . . .
C18 C 0.4688(7) 0.2413(7) 0.8110(7) 0.039(3) Uiso 1 1 d . . . . .
C19 C 0.4732(7) 0.3102(7) 0.8605(7) 0.035(3) Uiso 1 1 d . . . . .
H19 H 0.4956 0.3583 0.8535 0.041 Uiso 1 1 calc R . . . .
C20 C 0.4483(7) 0.3129(7) 0.9166(7) 0.034(3) Uiso 1 1 d . . . . .
C21 C 0.4547(7) 0.3926(6) 0.9676(7) 0.033(3) Uiso 1 1 d . . . . .
H21A H 0.4590 0.3891 1.0188 0.039 Uiso 1 1 calc R . . . .
H21B H 0.5058 0.4328 0.9755 0.039 Uiso 1 1 calc R . . . .
C22 C 0.3733(8) 0.5883(7) 0.8138(7) 0.039(3) Uiso 1 1 d . . . . .
C23 C 0.3728(7) 0.6140(7) 0.7455(7) 0.037(3) Uiso 1 1 d . . . . .
C24 C 0.3190(9) 0.5775(8) 0.6728(8) 0.055(4) Uiso 1 1 d . . . . .
H24 H 0.2780 0.5287 0.6601 0.066 Uiso 1 1 calc R . . . .
C25 C 0.3211(9) 0.6084(8) 0.6158(8) 0.053(4) Uiso 1 1 d . . . . .
H25 H 0.2795 0.5823 0.5651 0.064 Uiso 1 1 calc R . . . .
C26 C 0.4379(8) 0.7128(8) 0.7039(7) 0.049(4) Uiso 1 1 d . . . . .
H26 H 0.4808 0.7601 0.7157 0.058 Uiso 1 1 calc R . . . .
C27 C 0.4352(8) 0.6832(7) 0.7650(8) 0.047(3) Uiso 1 1 d . . . . .
H27 H 0.4746 0.7099 0.8166 0.057 Uiso 1 1 calc R . . . .
C28 C 0.1302(9) 0.4661(9) 0.7746(9) 0.060(4) Uiso 1 1 d . . . . .
C29 C 0.0719(8) 0.5088(8) 0.7523(8) 0.052(4) Uiso 1 1 d . . . . .
C30 C 0.0069(10) 0.4779(10) 0.6905(9) 0.073(5) Uiso 1 1 d . . . . .
H30 H -0.0042 0.4257 0.6593 0.088 Uiso 1 1 calc R . . . .
C31 C -0.0511(10) 0.5182(9) 0.6650(10) 0.073(5) Uiso 1 1 d . . . . .
H31 H -0.0960 0.4953 0.6159 0.088 Uiso 1 1 calc R . . . .
C32 C 0.0247(9) 0.6166(9) 0.7776(9) 0.067(4) Uiso 1 1 d . . . . .
H32 H 0.0316 0.6668 0.8102 0.080 Uiso 1 1 calc R . . . .
C33 C 0.0824(10) 0.5842(9) 0.8046(9) 0.070(4) Uiso 1 1 d . . . . .
H33 H 0.1266 0.6086 0.8541 0.084 Uiso 1 1 calc R . . . .
C34 C 0.0030(9) 0.1636(8) 0.9345(9) 0.058(4) Uiso 1 1 d . . . . .
C35 C -0.0894(11) 0.1169(10) 0.8849(11) 0.083(5) Uiso 1 1 d . . . . .
C36 C -0.1178(13) 0.0635(12) 0.8157(12) 0.105(6) Uiso 1 1 d . . . . .
H36 H -0.0842 0.0549 0.7883 0.127 Uiso 1 1 calc R . . . .
C37 C -0.2082(17) 0.0177(16) 0.7845(16) 0.147(9) Uiso 1 1 d . . . . .
H37 H -0.2341 -0.0251 0.7372 0.177 Uiso 1 1 calc R . . . .
C38 C -0.223(2) 0.094(2) 0.886(2) 0.195(13) Uiso 1 1 d . . . . .
H38 H -0.2593 0.1077 0.9089 0.234 Uiso 1 1 calc R . . . .
C39 C -0.140(2) 0.1377(18) 0.9245(18) 0.166(11) Uiso 1 1 d . . . . .
H39 H -0.1183 0.1783 0.9729 0.199 Uiso 1 1 calc R . . . .
C40 C 0.0761(8) 0.0033(8) 0.8968(8) 0.048(3) Uiso 1 1 d . . . . .
C41 C 0.0312(8) -0.0779(8) 0.8477(8) 0.054(4) Uiso 1 1 d . . . . .
C42 C 0.0296(8) -0.1069(8) 0.7728(8) 0.056(4) Uiso 1 1 d . . . . .
H42 H 0.0567 -0.0732 0.7520 0.067 Uiso 1 1 calc R . . . .
C43 C -0.0122(9) -0.1850(8) 0.7317(9) 0.060(4) Uiso 1 1 d . . . . .
H43 H -0.0112 -0.2049 0.6825 0.072 Uiso 1 1 calc R . . . .
C44 C -0.0490(8) -0.2054(8) 0.8296(8) 0.051(4) Uiso 1 1 d . . . . .
H44 H -0.0739 -0.2404 0.8506 0.061 Uiso 1 1 calc R . . . .
C45 C -0.0105(8) -0.1291(8) 0.8753(8) 0.050(4) Uiso 1 1 d . . . . .
H45 H -0.0119 -0.1111 0.9246 0.060 Uiso 1 1 calc R . . . .
C46 C 0.4940(10) 0.0787(9) 0.7711(9) 0.061(4) Uiso 1 1 d . . . . .
C47 C 0.4710(8) 0.0003(7) 0.7169(7) 0.044(3) Uiso 1 1 d . . . . .
C48 C 0.5328(9) -0.0310(8) 0.7137(8) 0.056(4) Uiso 1 1 d . . . . .
H48 H 0.5893 -0.0019 0.7452 0.067 Uiso 1 1 calc R . . . .
C49 C 0.5081(9) -0.1084(8) 0.6614(8) 0.054(4) Uiso 1 1 d . . . . .
H49 H 0.5501 -0.1286 0.6554 0.065 Uiso 1 1 calc R . . . .
C50 C 0.3741(9) -0.1212(8) 0.6308(8) 0.053(4) Uiso 1 1 d . . . . .
H50 H 0.3177 -0.1528 0.6025 0.064 Uiso 1 1 calc R . . . .
C51 C 0.3907(9) -0.0475(8) 0.6778(8) 0.054(4) Uiso 1 1 d . . . . .
H51 H 0.3473 -0.0295 0.6833 0.065 Uiso 1 1 calc R . . . .
C52 C 0.5662(8) 0.2817(7) 0.7582(8) 0.043(3) Uiso 1 1 d . . . . .
C53 C 0.5744(8) 0.2745(7) 0.6860(7) 0.042(3) Uiso 1 1 d . . . . .
C54 C 0.5181(8) 0.2179(8) 0.6130(7) 0.050(4) Uiso 1 1 d . . . . .
H54 H 0.4710 0.1805 0.6107 0.060 Uiso 1 1 calc R . . . .
C55 C 0.5288(8) 0.2149(7) 0.5457(7) 0.042(3) Uiso 1 1 d . . . . .
H55 H 0.4902 0.1754 0.4985 0.050 Uiso 1 1 calc R . . . .
C56 C 0.6533(8) 0.3262(7) 0.6206(7) 0.045(3) Uiso 1 1 d . . . . .
H56 H 0.7006 0.3639 0.6237 0.055 Uiso 1 1 calc R . . . .
C57 C 0.6402(8) 0.3261(8) 0.6845(8) 0.052(4) Uiso 1 1 d . . . . .
H57 H 0.6795 0.3646 0.7321 0.062 Uiso 1 1 calc R . . . .
C58 C 0.5179(7) 0.6592(7) 0.5550(7) 0.032(3) Uiso 1 1 d . . . . .
C59 C 0.6039(8) 0.6567(7) 0.5817(7) 0.041(3) Uiso 1 1 d . . . . .
C60 C 0.6177(8) 0.5845(7) 0.5662(7) 0.044(3) Uiso 1 1 d . . . . .
H60 H 0.5729 0.5366 0.5376 0.053 Uiso 1 1 calc R . . . .
C61 C 0.6972(7) 0.5846(7) 0.5934(7) 0.042(3) Uiso 1 1 d . . . . .
H61 H 0.7063 0.5354 0.5843 0.050 Uiso 1 1 calc R . . . .
C62 C 0.7497(8) 0.7182(8) 0.6447(8) 0.050(4) Uiso 1 1 d . . . . .
H62 H 0.7961 0.7649 0.6717 0.060 Uiso 1 1 calc R . . . .
C63 C 0.6738(7) 0.7251(7) 0.6213(7) 0.039(3) Uiso 1 1 d . . . . .
H63 H 0.6676 0.7757 0.6314 0.047 Uiso 1 1 calc R . . . .
C64 C -0.1318(9) 0.6058(9) 0.5363(9) 0.068(4) Uiso 1 1 d D . . . .
C65 C -0.115(2) 0.6232(19) 0.4729(16) 0.163(10) Uiso 1 1 d D . . . .
C66 C -0.1904(8) 0.5498(8) 0.7640(8) 0.045(3) Uiso 1 1 d . . . . .
C67 C -0.2032(15) 0.5515(15) 0.8354(14) 0.118(7) Uiso 1 1 d . . . . .
C68 C 0.2281(17) 0.7319(16) 0.4658(15) 0.149(9) Uiso 1 1 d D . . . .
C70 C 0.142(2) 0.705(2) 0.456(2) 0.192(13) Uiso 1 1 d 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 O13 1.949(8) . ?
Cu1 O15 2.033(9) . ?
Cu1 N1 1.992(9) . ?
Cu1 N5 2.241(10) 1_565 ?
Cu1 N6 1.977(10) 2_666 ?
Cu2 O16 1.947(9) . ?
Cu2 O18 1.984(8) . ?
Cu2 N2 2.007(11) . ?
Cu2 N4 2.209(10) 1_565 ?
Cu2 N7 2.013(9) 1_455 ?
F1 C65 1.38(3) . ?
F2 C65 1.34(3) . ?
F3 C65 1.27(3) . ?
F4 C67 1.25(2) . ?
F5 C67 1.28(2) . ?
F6 C67 1.53(2) . ?
F7 C70 1.58(4) . ?
F8 C70 1.25(3) . ?
F9 C70 1.37(3) . ?
O1 C22 1.164(13) . ?
O2 C3 1.442(14) . ?
O2 C22 1.377(14) . ?
O3 C4 1.420(14) . ?
O3 C28 1.353(16) . ?
O4 C28 1.178(16) . ?
O5 C34 1.152(15) . ?
O6 C10 1.448(14) . ?
O6 C34 1.360(16) . ?
O7 C40 1.236(14) . ?
O8 C11 1.477(15) . ?
O8 C40 1.379(14) . ?
O9 C17 1.401(14) . ?
O9 C46 1.368(16) . ?
O10 C46 1.207(16) . ?
O11 C18 1.433(14) . ?
O11 C52 1.387(14) . ?
O12 C52 1.164(14) . ?
O13 C58 1.316(13) . ?
O14 C58 1.229(13) . ?
O15 C68 1.287(16) . ?
O16 C64 1.248(17) . ?
O17 C64 1.241(17) . ?
O18 C66 1.325(14) . ?
O19 C66 1.199(14) . ?
O21 C68 1.32(3) . ?
N1 C25 1.387(15) . ?
N1 C26 1.342(15) . ?
N2 C31 1.308(18) . ?
N2 C32 1.318(17) . ?
N3 C37 1.39(3) . ?
N3 C38 1.21(3) . ?
N4 Cu2 2.209(10) 1_545 ?
N4 C43 1.371(16) . ?
N4 C44 1.364(15) . ?
N5 Cu1 2.241(10) 1_545 ?
N5 C49 1.309(16) . ?
N5 C50 1.354(15) . ?
N6 Cu1 1.977(10) 2_666 ?
N6 C55 1.374(15) . ?
N6 C56 1.442(16) . ?
N7 Cu2 2.013(9) 1_655 ?
N7 C61 1.337(14) . ?
N7 C62 1.320(15) . ?
C1 C2 1.416(15) . ?
C1 C6 1.421(16) . ?
C1 C21 1.493(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.325(15) . ?
C3 C4 1.395(17) . ?
C4 C5 1.366(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.392(16) . ?
C6 C7 1.503(16) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.506(15) . ?
C8 C9 1.395(16) . ?
C8 C13 1.410(15) . ?
C9 H9 0.9500 . ?
C9 C10 1.324(16) . ?
C10 C11 1.322(16) . ?
C11 C12 1.379(16) . ?
C12 H12 0.9500 . ?
C12 C13 1.428(16) . ?
C13 C14 1.532(16) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.466(16) . ?
C15 C16 1.409(16) . ?
C15 C20 1.447(16) . ?
C16 H16 0.9500 . ?
C16 C17 1.382(16) . ?
C17 C18 1.389(16) . ?
C18 C19 1.375(16) . ?
C19 H19 0.9500 . ?
C19 C20 1.308(15) . ?
C20 C21 1.530(15) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.511(17) . ?
C23 C24 1.327(17) . ?
C23 C27 1.379(16) . ?
C24 H24 0.9500 . ?
C24 C25 1.367(17) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C26 C27 1.429(17) . ?
C27 H27 0.9500 . ?
C28 C29 1.473(19) . ?
C29 C30 1.269(19) . ?
C29 C33 1.454(19) . ?
C30 H30 0.9500 . ?
C30 C31 1.45(2) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C32 C33 1.340(19) . ?
C33 H33 0.9500 . ?
C34 C35 1.55(2) . ?
C35 C36 1.32(2) . ?
C35 C39 1.44(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.50(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C38 C39 1.38(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.450(18) . ?
C41 C42 1.420(18) . ?
C41 C45 1.391(18) . ?
C42 H42 0.9500 . ?
C42 C43 1.368(18) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C44 C45 1.354(17) . ?
C45 H45 0.9500 . ?
C46 C47 1.454(18) . ?
C47 C48 1.388(17) . ?
C47 C51 1.365(17) . ?
C48 H48 0.9500 . ?
C48 C49 1.422(18) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C50 C51 1.358(18) . ?
C51 H51 0.9500 . ?
C52 C53 1.441(17) . ?
C53 C54 1.425(17) . ?
C53 C57 1.364(17) . ?
C54 H54 0.9500 . ?
C54 C55 1.376(17) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C56 C57 1.343(17) . ?
C57 H57 0.9500 . ?
C58 C59 1.492(16) . ?
C59 C60 1.396(16) . ?
C59 C63 1.409(16) . ?
C60 H60 0.9500 . ?
C60 C61 1.365(16) . ?
C61 H61 0.9500 . ?
C62 H62 0.9500 . ?
C62 C63 1.350(17) . ?
C63 H63 0.9500 . ?
C64 C65 1.453(17) . ?
C66 C67 1.48(2) . ?
C68 C70 1.464(18) . ?

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
O13 Cu1 O15 171.8(3) . . ?
O13 Cu1 N1 88.9(3) . . ?
O13 Cu1 N5 89.8(3) . 1_565 ?
O13 Cu1 N6 87.1(4) . 2_666 ?
O15 Cu1 N5 97.8(4) . 1_565 ?
N1 Cu1 O15 87.3(4) . . ?
N1 Cu1 N5 94.8(4) . 1_565 ?
N6 Cu1 O15 94.4(4) 2_666 . ?
N6 Cu1 N1 162.9(4) 2_666 . ?
N6 Cu1 N5 101.8(4) 2_666 1_565 ?
O16 Cu2 O18 178.2(4) . . ?
O16 Cu2 N2 90.9(4) . . ?
O16 Cu2 N4 90.4(4) . 1_565 ?
O16 Cu2 N7 92.2(4) . 1_455 ?
O18 Cu2 N2 88.7(4) . . ?
O18 Cu2 N4 87.9(4) . 1_565 ?
O18 Cu2 N7 88.8(4) . 1_455 ?
N2 Cu2 N4 101.6(4) . 1_565 ?
N2 Cu2 N7 158.5(4) . 1_455 ?
N7 Cu2 N4 99.6(4) 1_455 1_565 ?
C22 O2 C3 115.1(9) . . ?
C28 O3 C4 117.7(10) . . ?
C34 O6 C10 118.5(10) . . ?
C40 O8 C11 116.5(9) . . ?
C46 O9 C17 119.2(10) . . ?
C52 O11 C18 115.8(9) . . ?
C58 O13 Cu1 110.9(7) . . ?
C68 O15 Cu1 128.1(15) . . ?
C64 O16 Cu2 114.7(10) . . ?
C66 O18 Cu2 119.4(8) . . ?
C25 N1 Cu1 123.2(8) . . ?
C26 N1 Cu1 120.1(8) . . ?
C26 N1 C25 116.6(11) . . ?
C31 N2 Cu2 119.2(11) . . ?
C31 N2 C32 117.6(14) . . ?
C32 N2 Cu2 123.1(10) . . ?
C38 N3 C37 124(3) . . ?
C43 N4 Cu2 121.1(9) . 1_545 ?
C44 N4 Cu2 124.6(8) . 1_545 ?
C44 N4 C43 114.3(11) . . ?
C49 N5 Cu1 123.3(9) . 1_545 ?
C49 N5 C50 115.4(11) . . ?
C50 N5 Cu1 121.1(9) . 1_545 ?
C55 N6 Cu1 122.2(8) . 2_666 ?
C55 N6 C56 117.8(11) . . ?
C56 N6 Cu1 119.5(8) . 2_666 ?
C61 N7 Cu2 118.9(8) . 1_655 ?
C62 N7 Cu2 122.7(9) . 1_655 ?
C62 N7 C61 117.6(11) . . ?
C2 C1 C6 119.4(10) . . ?
C2 C1 C21 118.4(10) . . ?
C6 C1 C21 122.1(10) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 C1 119.7(11) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 O2 120.6(11) . . ?
C2 C3 C4 121.6(12) . . ?
C4 C3 O2 117.7(10) . . ?
C3 C4 O3 120.4(11) . . ?
C5 C4 O3 119.4(11) . . ?
C5 C4 C3 120.2(12) . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.2(12) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C7 124.2(11) . . ?
C5 C6 C1 118.5(11) . . ?
C5 C6 C7 117.3(11) . . ?
C6 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
C6 C7 C8 111.9(10) . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
C9 C8 C7 119.8(10) . . ?
C9 C8 C13 117.4(11) . . ?
C13 C8 C7 122.6(10) . . ?
C8 C9 H9 118.7 . . ?
C10 C9 C8 122.7(11) . . ?
C10 C9 H9 118.7 . . ?
C9 C10 O6 122.3(11) . . ?
C11 C10 O6 118.3(11) . . ?
C11 C10 C9 119.1(12) . . ?
C10 C11 O8 120.5(11) . . ?
C10 C11 C12 125.1(12) . . ?
C12 C11 O8 114.3(10) . . ?
C11 C12 H12 122.2 . . ?
C11 C12 C13 115.6(11) . . ?
C13 C12 H12 122.2 . . ?
C8 C13 C12 119.7(11) . . ?
C8 C13 C14 125.2(11) . . ?
C12 C13 C14 115.0(10) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 C13 110.8(10) . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
C16 C15 C14 119.2(11) . . ?
C16 C15 C20 115.8(11) . . ?
C20 C15 C14 124.9(11) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(11) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 O9 118.5(10) . . ?
C16 C17 C18 121.4(11) . . ?
C18 C17 O9 120.2(11) . . ?
C17 C18 O11 118.3(10) . . ?
C19 C18 O11 123.9(10) . . ?
C19 C18 C17 117.5(11) . . ?
C18 C19 H19 118.3 . . ?
C20 C19 C18 123.4(11) . . ?
C20 C19 H19 118.3 . . ?
C15 C20 C21 119.3(10) . . ?
C19 C20 C15 121.3(11) . . ?
C19 C20 C21 119.3(10) . . ?
C1 C21 C20 113.1(9) . . ?
C1 C21 H21A 109.0 . . ?
C1 C21 H21B 109.0 . . ?
C20 C21 H21A 109.0 . . ?
C20 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
O1 C22 O2 123.1(11) . . ?
O1 C22 C23 127.4(12) . . ?
O2 C22 C23 109.5(10) . . ?
C24 C23 C22 126.3(12) . . ?
C24 C23 C27 120.4(12) . . ?
C27 C23 C22 113.3(11) . . ?
C23 C24 H24 119.2 . . ?
C23 C24 C25 121.7(14) . . ?
C25 C24 H24 119.2 . . ?
N1 C25 H25 119.4 . . ?
C24 C25 N1 121.3(13) . . ?
C24 C25 H25 119.4 . . ?
N1 C26 H26 118.5 . . ?
N1 C26 C27 123.1(12) . . ?
C27 C26 H26 118.5 . . ?
C23 C27 C26 116.9(12) . . ?
C23 C27 H27 121.6 . . ?
C26 C27 H27 121.6 . . ?
O3 C28 C29 113.1(12) . . ?
O4 C28 O3 122.7(14) . . ?
O4 C28 C29 124.1(15) . . ?
C30 C29 C28 121.3(14) . . ?
C30 C29 C33 117.6(14) . . ?
C33 C29 C28 120.8(13) . . ?
C29 C30 H30 118.3 . . ?
C29 C30 C31 123.4(16) . . ?
C31 C30 H30 118.3 . . ?
N2 C31 C30 118.4(15) . . ?
N2 C31 H31 120.8 . . ?
C30 C31 H31 120.8 . . ?
N2 C32 H32 116.1 . . ?
N2 C32 C33 127.8(15) . . ?
C33 C32 H32 116.1 . . ?
C29 C33 H33 122.6 . . ?
C32 C33 C29 114.8(15) . . ?
C32 C33 H33 122.6 . . ?
O5 C34 O6 123.5(14) . . ?
O5 C34 C35 130.8(15) . . ?
O6 C34 C35 105.2(13) . . ?
C36 C35 C34 124.0(18) . . ?
C36 C35 C39 125(2) . . ?
C39 C35 C34 111.4(19) . . ?
C35 C36 H36 123.1 . . ?
C35 C36 C37 114(2) . . ?
C37 C36 H36 123.1 . . ?
N3 C37 C36 118(3) . . ?
N3 C37 H37 121.0 . . ?
C36 C37 H37 121.0 . . ?
N3 C38 H38 117.8 . . ?
N3 C38 C39 124(4) . . ?
C39 C38 H38 117.8 . . ?
C35 C39 H39 122.5 . . ?
C38 C39 C35 115(3) . . ?
C38 C39 H39 122.5 . . ?
O7 C40 O8 122.7(12) . . ?
O7 C40 C41 126.4(12) . . ?
O8 C40 C41 110.9(11) . . ?
C42 C41 C40 121.9(12) . . ?
C45 C41 C40 118.9(13) . . ?
C45 C41 C42 119.2(13) . . ?
C41 C42 H42 121.1 . . ?
C43 C42 C41 117.7(13) . . ?
C43 C42 H42 121.1 . . ?
N4 C43 H43 117.7 . . ?
C42 C43 N4 124.7(14) . . ?
C42 C43 H43 117.7 . . ?
N4 C44 H44 116.9 . . ?
C45 C44 N4 126.3(13) . . ?
C45 C44 H44 116.9 . . ?
C41 C45 H45 121.2 . . ?
C44 C45 C41 117.7(13) . . ?
C44 C45 H45 121.2 . . ?
O9 C46 C47 111.9(12) . . ?
O10 C46 O9 122.1(14) . . ?
O10 C46 C47 126.0(14) . . ?
C48 C47 C46 118.7(12) . . ?
C51 C47 C46 122.0(12) . . ?
C51 C47 C48 118.7(12) . . ?
C47 C48 H48 121.4 . . ?
C47 C48 C49 117.3(13) . . ?
C49 C48 H48 121.4 . . ?
N5 C49 C48 124.2(13) . . ?
N5 C49 H49 117.9 . . ?
C48 C49 H49 117.9 . . ?
N5 C50 H50 117.3 . . ?
N5 C50 C51 125.3(13) . . ?
C51 C50 H50 117.3 . . ?
C47 C51 H51 120.6 . . ?
C50 C51 C47 118.7(13) . . ?
C50 C51 H51 120.6 . . ?
O11 C52 C53 109.5(11) . . ?
O12 C52 O11 123.9(12) . . ?
O12 C52 C53 126.6(13) . . ?
C54 C53 C52 125.8(12) . . ?
C57 C53 C52 119.1(12) . . ?
C57 C53 C54 115.0(12) . . ?
C53 C54 H54 118.5 . . ?
C55 C54 C53 123.0(13) . . ?
C55 C54 H54 118.5 . . ?
N6 C55 C54 119.9(12) . . ?
N6 C55 H55 120.1 . . ?
C54 C55 H55 120.1 . . ?
N6 C56 H56 120.1 . . ?
C57 C56 N6 119.9(12) . . ?
C57 C56 H56 120.1 . . ?
C53 C57 H57 117.8 . . ?
C56 C57 C53 124.4(13) . . ?
C56 C57 H57 117.8 . . ?
O13 C58 C59 115.4(10) . . ?
O14 C58 O13 124.0(10) . . ?
O14 C58 C59 120.1(10) . . ?
C60 C59 C58 120.0(11) . . ?
C60 C59 C63 117.3(11) . . ?
C63 C59 C58 122.7(11) . . ?
C59 C60 H60 121.0 . . ?
C61 C60 C59 118.1(12) . . ?
C61 C60 H60 121.0 . . ?
N7 C61 C60 124.0(12) . . ?
N7 C61 H61 118.0 . . ?
C60 C61 H61 118.0 . . ?
N7 C62 H62 118.2 . . ?
N7 C62 C63 123.6(13) . . ?
C63 C62 H62 118.2 . . ?
C59 C63 H63 120.3 . . ?
C62 C63 C59 119.4(12) . . ?
C62 C63 H63 120.3 . . ?
O16 C64 C65 115.2(19) . . ?
O17 C64 O16 133.5(15) . . ?
O17 C64 C65 111.3(19) . . ?
F1 C65 C64 119(2) . . ?
F2 C65 F1 102(2) . . ?
F2 C65 C64 118(2) . . ?
F3 C65 F1 89(2) . . ?
F3 C65 F2 106(2) . . ?
F3 C65 C64 119(2) . . ?
O18 C66 C67 109.6(14) . . ?
O19 C66 O18 128.3(12) . . ?
O19 C66 C67 122.0(15) . . ?
F4 C67 F5 114(2) . . ?
F4 C67 F6 101.4(17) . . ?
F4 C67 C66 122(2) . . ?
F5 C67 F6 97.2(17) . . ?
F5 C67 C66 115(2) . . ?
C66 C67 F6 100.5(16) . . ?
O15 C68 O21 130(3) . . ?
O15 C68 C70 111(3) . . ?
O21 C68 C70 119(2) . . ?
F8 C70 F7 95(3) . . ?
F8 C70 F9 113(3) . . ?
F8 C70 C68 121(3) . . ?
F9 C70 F7 96(3) . . ?
F9 C70 C68 120(3) . . ?
C68 C70 F7 102(3) . . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 2.726
0 1 0 2.602
-1 0 1 2.887
0 0 1 2.549
1 -3 2 8.095

_platon_squeeze_details          
;
TITL tbl1cutfa_a.res in P-1
CELL   18.1806   18.4809   19.4599    103.32    109.24    103.09
SPGR P-1
# Solvent Accessible Volume =    2902.7
# Electrons Found in S.A.V. =     929.9
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.327 0.207 0.181 !      11.90 eA-3
C102 0.510 0.565 0.279 !       9.83 eA-3
C103 0.529 0.072 0.144 !       8.14 eA-3
C104 0.265 0.716 0.044 !       7.13 eA-3
C105 0.776 0.280 0.293 !       5.82 eA-3
C106 0.383 0.186 0.159 !       5.41 eA-3
C107 0.379 0.947 0.486 !       4.80 eA-3
C108 0.504 0.495 0.214 !       4.62 eA-3
C109 0.735 0.816 0.420 !       4.06 eA-3
C110 0.560 0.021 0.106 !       3.85 eA-3
C111 0.780 0.748 0.238 !       3.83 eA-3
C112 0.487 0.518 0.345 !       3.58 eA-3
C113 0.821 0.285 0.022 !       3.50 eA-3
C114 0.232 0.146 0.108 !       3.30 eA-3
C115 0.023 0.654 0.203 !       3.21 eA-3
C116 0.393 0.969 0.403 !       3.11 eA-3
C117 0.877 0.824 0.292 !       3.05 eA-3
C118 0.561 0.139 0.074 !       3.02 eA-3
C119 0.012 0.661 0.127 !       2.99 eA-3
C120 0.635 0.248 0.067 !       2.97 eA-3
C121 0.731 0.029 0.140 !       2.90 eA-3
C122 0.801 0.192 0.280 !       2.87 eA-3
C123 0.895 0.097 0.452 !       2.87 eA-3
C124 0.328 0.984 0.425 !       2.84 eA-3
C125 0.863 0.360 0.339 !       2.81 eA-3
C126 0.358 0.919 0.390 !       2.76 eA-3
C127 0.799 1.007 0.265 !       2.75 eA-3
C128 0.867 0.792 0.327 !       2.66 eA-3
C129 0.328 0.299 0.200 !       2.63 eA-3
C130 0.453 0.032 0.112 !       2.62 eA-3
C131 0.126 0.658 0.233 !       2.58 eA-3
C132 0.766 0.059 0.056 !       2.57 eA-3
C133 0.112 0.671 0.019 !       2.57 eA-3
C134 0.596 0.592 0.330 !       2.51 eA-3
C135 0.155 0.103 0.411 !       2.50 eA-3
C136 0.747 0.269 0.207 !       2.48 eA-3
C137 0.329 0.093 0.411 !       2.47 eA-3
C138 0.318 0.958 0.372 !       2.40 eA-3
C139 0.113 0.095 0.372 !       2.34 eA-3
C140 0.666 0.309-0.004 !       2.33 eA-3
C141 0.581 0.952 0.490 !       2.30 eA-3
C142 0.486 0.481 0.280 !       2.29 eA-3
C143 0.807 0.194 0.109 !       2.28 eA-3
C144 0.805 0.750 0.319 !       2.27 eA-3
C145 0.126 0.745 0.214 !       2.26 eA-3
C146 0.965 0.623 0.112 !       2.22 eA-3
C147 0.826 0.084 0.407 !       2.14 eA-3
C148 0.358 0.070 0.436 !       2.09 eA-3
C149 0.170 0.099 0.346 !       2.08 eA-3
C150 0.799 0.820 0.232 !       2.05 eA-3
C151 0.357 0.747 0.027 !       1.96 eA-3
C152 0.277 0.622 0.020 !       1.95 eA-3
C153 0.991 0.451 0.073 !       1.94 eA-3
C154 0.797 0.258 0.060 !       1.92 eA-3
C155 0.926 0.552 0.060 !       1.85 eA-3
C156 0.092 0.112 0.454 !       1.85 eA-3
C157 0.784 0.794 0.315 !       1.84 eA-3
C158 0.292 0.776 0.029 !       1.81 eA-3
C159 0.325 0.939 0.348 !       1.80 eA-3
Q160 0.892 0.622 0.473 !       1.77 eA-3
C161 0.911 0.581 0.033 !       1.74 eA-3
C162 0.715 0.285 0.061 !       1.72 eA-3
C163 0.939 0.531 0.024 !       1.71 eA-3
Q164 0.013 0.689 0.277 !       1.70 eA-3
C165 0.968 0.112 0.419 !       1.69 eA-3
C166 0.960 0.094 0.436 !       1.68 eA-3
Q167 0.952 0.647 0.462 !       1.66 eA-3
C168 0.629 0.606 0.376 !       1.66 eA-3
C169 0.968 0.357 0.035 !       1.66 eA-3
C170 0.892 0.851 0.359 !       1.63 eA-3
C171 0.954 0.116 0.504 !       1.63 eA-3
C172 0.074 0.982 0.343 !       1.61 eA-3
C173 0.824 0.210 0.182 !       1.59 eA-3
C174 0.704 0.036 0.506 !       1.58 eA-3
Q175 0.319 0.880 0.437 !       1.57 eA-3
C176 0.877 0.909 0.303 !       1.55 eA-3
C177 0.757 0.189 0.236 !       1.55 eA-3
C178 0.815 0.048 0.328 !       1.53 eA-3
C179 0.940 0.016 0.445 !       1.52 eA-3
C180 0.921 0.454 0.036 !       1.51 eA-3
C181 0.268 0.912 0.353 !       1.50 eA-3
C182 0.653 0.188-0.001 !       1.50 eA-3
C183 0.962 0.781 0.283 !       1.48 eA-3
C184 0.828 0.076 0.297 !       1.47 eA-3
Q185 0.846 0.579 0.393 !       1.46 eA-3
C186 0.015 0.620 0.077 !       1.46 eA-3
C187 0.448 0.036 0.480 !       1.44 eA-3
C188 0.280 0.929 0.429 !       1.44 eA-3
C189 0.396 0.027 0.442 !       1.43 eA-3
C190 0.283 0.151 0.499 !       1.42 eA-3
Q191 0.896 0.139 0.499 !       1.41 eA-3
C192 0.997 0.587 0.148 !       1.41 eA-3
Q193 0.258 0.901 0.467 !       1.40 eA-3
Q194 0.934 0.652 0.233 !       1.40 eA-3
C195 0.372 0.251 0.237 !       1.39 eA-3
C196 0.487 0.918 0.085 !       1.38 eA-3
C197 0.992 0.529 0.082 !       1.38 eA-3
C198 0.971 0.434 0.011 !       1.38 eA-3
Q199 0.905 0.623 0.256 !       1.37 eA-3
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.074 -0.036 0.366 2857 931 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.257
_oxdiff_exptl_absorpt_empirical_full_min 0.904

# start Validation Reply Form

_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: crystals were weakly diffracting with no high angle data
;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      51.42 Degree
RESPONSE: crystals were weakly diffracting with no high angle data
;
_vrf_PLAT201_I                   
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......        105 Report
RESPONSE: very weak data, insufficient obs data for anisotropic refinement
;
# end Validation Reply Form

