# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_co7sq
_database_code_depnum_ccdc_archive 'CCDC 1907525'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;Bangor University 
United Kingdom
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Co7].3.5H2O.14MeOH'
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H94 N12 O40 Co7, C14 H63 O17.5, N1 O3'
_chemical_formula_sum            'C98 H157 Co7 N13 O60.5'
_chemical_formula_weight         2897.88

_smtbx_masks_special_details     
;
A solvent mask was calculated and 639 electrons were 
found in a volume of 2105Å^3 in 1 void. This is consistent with the presence of 
1[NO3], 3.5[H2O] and 14[CH4O] per formula unit.
;
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   17.7308(7)
_cell_length_b                   19.4055(4)
_cell_length_c                   19.8470(4)
_cell_angle_alpha                103.669(2)
_cell_angle_beta                 101.741(3)
_cell_angle_gamma                96.955(3)
_cell_volume                     6393.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    24583
_cell_measurement_theta_min      2.6410
_cell_measurement_theta_max      67.6540

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_F_000             2382
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.122
_exptl_crystal_size_mid          0.113
_exptl_crystal_size_min          0.071
_exptl_absorpt_coefficient_mu    7.560
_shelx_estimated_absorpt_T_min   0.583
_shelx_estimated_absorpt_T_max   0.834
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.533
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_process_details   
; 
crysalispro 1.171.39.46b (rigaku oxford diffraction, 2018) 
numerical absorption correction based on gaussian integration over 
   a multifaceted crystal model 
empirical absorption correction using spherical harmonics, 
 implemented in scale3 abspack scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'rotating-anode x-ray tube'
_diffrn_measurement_device_type  'xtalab afc11 (rcd3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            96789
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_av_R_equivalents  0.1040
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.586
_diffrn_reflns_theta_max         58.928
_diffrn_reflns_theta_full        58.928
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             18366
_reflns_number_gt                12488
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'crysalispro 1.171.39.46b (rigaku od, 2018)'
_computing_cell_refinement       'crysalispro 1.171.39.46b (rigaku od, 2018)'
_computing_data_reduction        'crysalispro 1.171.39.46b (rigaku od, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1007P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18366
_refine_ls_number_parameters     1302
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.1871
_refine_ls_wR_factor_gt          0.1752
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.35009(5) 0.55276(5) 0.34560(5) 0.0677(2) Uani 1 1 d . . . . .
O1 O 0.33614(19) 0.65132(19) 0.31679(18) 0.0670(9) Uani 1 1 d . . . . .
N1 N 0.2650(3) 0.6393(3) 0.2692(3) 0.0746(13) Uani 1 1 d . . . . .
H1H H 0.245189 0.675689 0.257970 0.090 Uiso 1 1 calc R U . . .
C1 C 0.2264(3) 0.5727(4) 0.2405(3) 0.0808(18) Uani 1 1 d . . . . .
Co2 Co 0.42316(4) 0.67957(4) 0.27407(4) 0.0589(2) Uani 1 1 d . . . . .
O2 O 0.2535(2) 0.5216(2) 0.2613(2) 0.0795(11) Uani 1 1 d . . . . .
N2 N 0.4800(2) 0.6491(2) 0.1470(2) 0.0590(10) Uani 1 1 d . . . . .
H2H H 0.507480 0.652583 0.115321 0.071 Uiso 1 1 calc R U . . .
C2 C 0.1508(3) 0.5571(5) 0.1844(3) 0.0882(19) Uani 1 1 d . . . . .
Co3 Co 0.57558(4) 0.62309(4) 0.26375(4) 0.0538(2) Uani 1 1 d . . . . .
O3 O 0.1498(3) 0.6797(3) 0.1894(3) 0.1041(14) Uani 1 1 d . . . . .
N3 N 0.4489(2) 0.5452(2) 0.2955(2) 0.0603(11) Uani 1 1 d . . . . .
C3 C 0.1174(4) 0.4842(5) 0.1559(4) 0.108(2) Uani 1 1 d . . . . .
H3 H 0.142901 0.448248 0.171171 0.130 Uiso 1 1 calc R U . . .
Co4 Co 0.53032(5) 0.66454(4) 0.43211(4) 0.0619(2) Uani 1 1 d . . . . .
O4 O 0.3436(2) 0.4549(2) 0.3694(2) 0.0900(12) Uani 1 1 d . . . . .
H4H H 0.315042 0.452458 0.404735 0.108 Uiso 1 1 calc R U . . .
N4 N 0.6980(2) 0.7374(2) 0.2806(2) 0.0646(11) Uani 1 1 d . . . . .
C4 C 0.0455(5) 0.4645(6) 0.1041(4) 0.123(3) Uani 1 1 d . . . . .
H4 H 0.024240 0.414958 0.082488 0.148 Uiso 1 1 calc R U . . .
Co5 Co 0.60151(4) 0.79690(4) 0.38235(4) 0.0613(2) Uani 1 1 d . . . . .
O5 O 0.2804(2) 0.5722(3) 0.4247(2) 0.0866(12) Uani 1 1 d . . . . .
N5 N 0.6797(2) 0.5297(2) 0.2917(2) 0.0619(11) Uani 1 1 d . . . . .
H5H H 0.656918 0.485371 0.267810 0.074 Uiso 1 1 calc R U . . .
C5 C 0.0070(5) 0.5144(7) 0.0851(5) 0.130(3) Uani 1 1 d . . . . .
H5 H -0.043687 0.500169 0.053759 0.156 Uiso 1 1 calc R U . . .
Co6 Co 0.71656(4) 0.66964(4) 0.39265(4) 0.0621(2) Uani 1 1 d . . . . .
O6 O 0.42590(19) 0.6181(2) 0.43249(18) 0.0704(10) Uani 1 1 d . . . . .
N6 N 0.8696(3) 0.7484(2) 0.4403(3) 0.0722(12) Uani 1 1 d . . . . .
H6H H 0.890038 0.735450 0.478698 0.087 Uiso 1 1 calc R U . . .
C6 C 0.0406(4) 0.5881(6) 0.1109(4) 0.116(3) Uani 1 1 d . . . . .
H6 H 0.014787 0.623098 0.094091 0.140 Uiso 1 1 calc R U . . .
Co7 Co 0.78605(5) 0.82161(5) 0.35291(5) 0.0675(2) Uani 1 1 d . . . . .
O7 O 0.3685(4) 0.7528(3) 0.5918(2) 0.1048(15) Uani 1 1 d . . . . .
N7 N 0.7344(3) 0.9084(2) 0.4625(2) 0.0692(12) Uani 1 1 d . . . . .
H7H H 0.705945 0.920752 0.493363 0.083 Uiso 1 1 calc R U . . .
C7 C 0.1130(4) 0.6093(5) 0.1619(4) 0.0915(19) Uani 1 1 d . . . . .
O8 O 0.51817(19) 0.53274(17) 0.20846(17) 0.0580(8) Uani 1 1 d . . . . .
N8 N 0.6718(3) 0.7574(2) 0.5174(2) 0.0701(12) Uani 1 1 d . . . . .
H8H H 0.721969 0.776075 0.533406 0.084 Uiso 1 1 calc R U . . .
C8 C 0.1085(4) 0.7353(5) 0.1729(5) 0.127(3) Uani 1 1 d . . . . .
H8A H 0.092502 0.726882 0.120938 0.190 Uiso 1 1 calc R U . . .
H8B H 0.142893 0.782309 0.194009 0.190 Uiso 1 1 calc R U . . .
H8C H 0.062064 0.734554 0.192482 0.190 Uiso 1 1 calc R U . . .
O9 O 0.5329(2) 0.39501(19) 0.2503(2) 0.0755(10) Uani 1 1 d . . . . .
N9 N 0.4516(2) 0.7896(2) 0.4142(2) 0.0623(11) Uani 1 1 d . . . . .
H9H H 0.400634 0.780306 0.408935 0.075 Uiso 1 1 calc R U . . .
C9 C 0.3725(5) 0.3880(4) 0.3449(4) 0.104(2) Uani 1 1 d . . . . .
H9A H 0.335836 0.357829 0.300985 0.156 Uiso 1 1 calc R U . . .
H9B H 0.376882 0.362038 0.381862 0.156 Uiso 1 1 calc R U . . .
H9C H 0.423966 0.399525 0.335374 0.156 Uiso 1 1 calc R U . . .
O10 O 0.49996(18) 0.61589(16) 0.32009(16) 0.0572(8) Uani 1 1 d . . . . .
N10 N 0.3928(3) 0.6432(3) 0.4882(2) 0.0748(13) Uani 1 1 d . . . . .
H10H H 0.420239 0.675955 0.526964 0.090 Uiso 1 1 calc R U . . .
C10 C 0.4065(3) 0.6131(3) 0.1273(3) 0.0593(13) Uani 1 1 d . . . . .
O11 O 0.51110(18) 0.68038(17) 0.21849(17) 0.0597(8) Uani 1 1 d . . . . .
N11 N 0.3494(4) 0.8134(4) 0.2575(3) 0.0929(16) Uani 1 1 d . . . . .
C11 C 0.3727(3) 0.5731(3) 0.0520(3) 0.0566(12) Uani 1 1 d . . . . .
O12 O 0.36702(19) 0.61361(18) 0.17335(19) 0.0639(9) Uani 1 1 d . . . . .
N12 N 0.7843(4) 0.6261(4) 0.5294(5) 0.123(2) Uani 1 1 d . . . . .
C12 C 0.2947(3) 0.5383(3) 0.0354(3) 0.0667(14) Uani 1 1 d . . . . .
H12 H 0.266640 0.544199 0.071788 0.080 Uiso 1 1 calc R U . . .
O13 O 0.4893(2) 0.59640(19) 0.01578(18) 0.0679(9) Uani 1 1 d . . . . .
C13 C 0.2569(4) 0.4953(3) -0.0327(3) 0.0786(17) Uani 1 1 d . . . . .
H13 H 0.203787 0.472416 -0.043191 0.094 Uiso 1 1 calc R U . . .
O14 O 0.3990(2) 0.77249(19) 0.2436(2) 0.0774(10) Uani 1 1 d . . . . .
C14 C 0.2989(4) 0.4869(3) -0.0846(3) 0.0752(16) Uani 1 1 d . . . . .
H14 H 0.274084 0.457556 -0.131439 0.090 Uiso 1 1 calc R U . . .
O15 O 0.2878(3) 0.7884(3) 0.2685(3) 0.1130(16) Uani 1 1 d . . . . .
C15 C 0.3751(4) 0.5196(3) -0.0704(3) 0.0715(15) Uani 1 1 d . . . . .
H15 H 0.402490 0.512453 -0.107239 0.086 Uiso 1 1 calc R U . . .
O16 O 0.3688(3) 0.8778(3) 0.2592(3) 0.1292(19) Uani 1 1 d . . . . .
C16 C 0.4134(3) 0.5633(3) -0.0027(3) 0.0620(13) Uani 1 1 d . . . . .
O17 O 0.5502(2) 0.83902(18) 0.30031(19) 0.0708(10) Uani 1 1 d . . . . .
H17 H 0.499386 0.850119 0.300099 0.085 Uiso 1 1 calc R U . . .
C17 C 0.5328(4) 0.5869(3) -0.0386(3) 0.0796(16) Uani 1 1 d . . . . .
H17A H 0.525506 0.535568 -0.063076 0.119 Uiso 1 1 calc R U . . .
H17B H 0.588561 0.605387 -0.016478 0.119 Uiso 1 1 calc R U . . .
H17C H 0.514084 0.613369 -0.073171 0.119 Uiso 1 1 calc R U . . .
O18 O 0.64323(18) 0.71290(17) 0.31948(17) 0.0604(8) Uani 1 1 d . . . . .
C18 C 0.4641(3) 0.5097(3) 0.2375(3) 0.0563(12) Uani 1 1 d . . . . .
O19 O 0.64161(19) 0.62785(18) 0.20106(18) 0.0619(9) Uani 1 1 d . . . . .
C19 C 0.4198(3) 0.4352(3) 0.2022(3) 0.0594(13) Uani 1 1 d . . . . .
O20 O 0.6366(2) 0.7352(2) 0.1050(2) 0.0828(11) Uani 1 1 d . . . . .
C20 C 0.3439(3) 0.4218(3) 0.1617(3) 0.0675(14) Uani 1 1 d . . . . .
H20 H 0.318151 0.461037 0.156451 0.081 Uiso 1 1 calc R U . . .
O21 O 0.7914(3) 0.8853(3) 0.2832(3) 0.1139(16) Uani 1 1 d . . . . .
H21H H 0.756660 0.918847 0.283361 0.137 Uiso 1 1 calc R U . . .
C21 C 0.3041(3) 0.3511(3) 0.1282(3) 0.0768(16) Uani 1 1 d . . . . .
H21 H 0.251684 0.342291 0.100562 0.092 Uiso 1 1 calc R U . . .
O22 O 0.8860(2) 0.7813(2) 0.3429(2) 0.0700(10) Uani 1 1 d . . . . .
C22 C 0.3426(4) 0.2942(3) 0.1362(3) 0.0828(17) Uani 1 1 d . . . . .
H22 H 0.315882 0.246067 0.114561 0.099 Uiso 1 1 calc R U . . .
O23 O 0.9985(3) 0.7329(3) 0.5223(3) 0.1177(16) Uani 1 1 d . . . . .
C23 C 0.4194(4) 0.3069(3) 0.1754(3) 0.0797(17) Uani 1 1 d . . . . .
H23 H 0.445386 0.267593 0.179826 0.096 Uiso 1 1 calc R U . . .
O24 O 0.79413(18) 0.76236(18) 0.42820(18) 0.0656(9) Uani 1 1 d . . . . .
C24 C 0.4585(3) 0.3772(3) 0.2084(3) 0.0693(14) Uani 1 1 d . . . . .
O25 O 0.7483(4) 0.6203(3) 0.4723(3) 0.143(3) Uani 1 1 d . . . . .
C25 C 0.5641(4) 0.3418(3) 0.2823(4) 0.0922(19) Uani 1 1 d . . . . .
H25A H 0.531158 0.328373 0.312869 0.138 Uiso 1 1 calc R U . . .
H25B H 0.617512 0.361920 0.311080 0.138 Uiso 1 1 calc R U . . .
H25C H 0.564838 0.299086 0.244636 0.138 Uiso 1 1 calc R U . . .
O26 O 0.8451(5) 0.6788(5) 0.5486(4) 0.182(3) Uani 1 1 d . . . . .
C26 C 0.7550(3) 0.5537(3) 0.2975(3) 0.0677(15) Uani 1 1 d . . . . .
O27 O 0.7601(7) 0.6047(6) 0.5726(6) 0.266(6) Uani 1 1 d . . . . .
C27 C 0.7998(3) 0.5045(3) 0.2591(3) 0.0659(14) Uani 1 1 d . . . . .
O28 O 0.8501(2) 0.9111(2) 0.4352(2) 0.0883(12) Uani 1 1 d . . . . .
C28 C 0.8787(4) 0.5324(3) 0.2706(4) 0.0859(18) Uani 1 1 d . . . . .
H28 H 0.899607 0.579268 0.301497 0.103 Uiso 1 1 calc R U . . .
O29 O 0.7008(2) 0.86307(18) 0.39469(19) 0.0688(9) Uani 1 1 d . . . . .
C29 C 0.9284(4) 0.4916(4) 0.2366(4) 0.105(2) Uani 1 1 d . . . . .
H29 H 0.982338 0.510710 0.244566 0.126 Uiso 1 1 calc R U . . .
O30 O 0.7394(3) 0.9746(3) 0.5986(2) 0.1023(14) Uani 1 1 d . . . . .
C30 C 0.8978(4) 0.4251(4) 0.1928(4) 0.108(2) Uani 1 1 d . . . . .
H30 H 0.930567 0.397731 0.169538 0.129 Uiso 1 1 calc R U . . .
O31 O 0.48996(18) 0.74225(17) 0.37489(17) 0.0622(9) Uani 1 1 d . . . . .
C31 C 0.8210(4) 0.3966(3) 0.1814(3) 0.0855(18) Uani 1 1 d . . . . .
H31 H 0.801047 0.349598 0.150466 0.103 Uiso 1 1 calc R U . . .
O32 O 0.5668(2) 0.86323(18) 0.46458(18) 0.0652(9) Uani 1 1 d . . . . .
C32 C 0.7712(3) 0.4352(3) 0.2142(3) 0.0699(15) Uani 1 1 d . . . . .
O33 O 0.3285(2) 0.8313(2) 0.4454(2) 0.0827(11) Uani 1 1 d . . . . .
C33 C 0.6601(3) 0.3424(3) 0.1484(3) 0.0793(16) Uani 1 1 d . . . . .
H33A H 0.674440 0.344914 0.103772 0.119 Uiso 1 1 calc R U . . .
H33B H 0.602921 0.333962 0.140314 0.119 Uiso 1 1 calc R U . . .
H33C H 0.680589 0.302803 0.164410 0.119 Uiso 1 1 calc R U . . .
O34 O 0.5844(2) 0.58583(19) 0.46805(19) 0.0724(10) Uani 1 1 d . . . . .
H34 H 0.628689 0.601439 0.507545 0.087 Uiso 1 1 calc R U . . .
C34 C 0.6907(3) 0.6878(3) 0.2214(3) 0.0612(13) Uani 1 1 d . . . . .
O35 O 0.63997(19) 0.72374(18) 0.44538(17) 0.0637(9) Uani 1 1 d . . . . .
C35 C 0.7427(3) 0.7012(3) 0.1728(3) 0.0651(14) Uani 1 1 d . . . . .
O36 O 0.5537(3) 0.7303(2) 0.53842(19) 0.0745(10) Uani 1 1 d . . . . .
C36 C 0.8167(3) 0.6859(3) 0.1854(3) 0.0836(18) Uani 1 1 d . . . . .
H36 H 0.836341 0.670022 0.226288 0.100 Uiso 1 1 calc R U . . .
O37 O 0.7896(3) 0.8177(3) 0.6216(3) 0.1272(19) Uani 1 1 d . . . . .
C37 C 0.8629(4) 0.6937(4) 0.1383(4) 0.102(2) Uani 1 1 d . . . . .
H37 H 0.914039 0.682246 0.146035 0.122 Uiso 1 1 calc R U . . .
O38 O 0.7866(2) 0.6158(2) 0.3333(2) 0.0714(10) Uani 1 1 d . . . . .
C38 C 0.8342(5) 0.7181(4) 0.0802(4) 0.106(2) Uani 1 1 d . . . . .
H38 H 0.866322 0.724526 0.048432 0.127 Uiso 1 1 calc R U . . .
O39 O 0.63907(18) 0.57845(17) 0.32550(17) 0.0618(9) Uani 1 1 d . . . . .
C39 C 0.7600(4) 0.7331(4) 0.0674(4) 0.095(2) Uani 1 1 d . . . . .
H39 H 0.741038 0.750059 0.027107 0.114 Uiso 1 1 calc R U . . .
O40 O 0.6930(2) 0.40975(18) 0.20258(18) 0.0678(9) Uani 1 1 d . . . . .
C40 C 0.7125(4) 0.7238(3) 0.1130(3) 0.0786(16) Uani 1 1 d . . . . .
C41 C 0.6093(5) 0.7734(4) 0.0550(4) 0.119(3) Uani 1 1 d . . . . .
H41A H 0.644988 0.819368 0.065564 0.178 Uiso 1 1 calc R U . . .
H41B H 0.556819 0.782582 0.058111 0.178 Uiso 1 1 calc R U . . .
H41C H 0.607278 0.744689 0.006637 0.178 Uiso 1 1 calc R U . . .
C42 C 0.9100(3) 0.7551(3) 0.3926(3) 0.0698(15) Uani 1 1 d . . . . .
C43 C 0.9849(3) 0.7257(3) 0.3991(3) 0.0750(16) Uani 1 1 d . . . . .
C44 C 1.0139(3) 0.7127(3) 0.3404(4) 0.0837(18) Uani 1 1 d . . . . .
H44 H 0.989798 0.727482 0.300182 0.100 Uiso 1 1 calc R U . . .
C45 C 1.0791(3) 0.6776(4) 0.3368(4) 0.093(2) Uani 1 1 d . . . . .
H45 H 1.097811 0.667347 0.294564 0.112 Uiso 1 1 calc R U . . .
C46 C 1.1134(4) 0.6594(4) 0.3951(5) 0.102(2) Uani 1 1 d . . . . .
H46 H 1.154156 0.631994 0.392622 0.123 Uiso 1 1 calc R U . . .
C47 C 1.0909(4) 0.6795(4) 0.4597(5) 0.113(3) Uani 1 1 d . . . . .
H47 H 1.120172 0.670871 0.501736 0.136 Uiso 1 1 calc R U . . .
C48 C 1.0255(4) 0.7123(4) 0.4619(4) 0.096(2) Uani 1 1 d . . . . .
C49 C 1.0383(5) 0.7178(7) 0.5873(5) 0.156(4) Uani 1 1 d . . . . .
H49A H 1.042349 0.666676 0.577469 0.234 Uiso 1 1 calc R U . . .
H49B H 1.008550 0.729467 0.623804 0.234 Uiso 1 1 calc R U . . .
H49C H 1.090860 0.747224 0.604584 0.234 Uiso 1 1 calc R U . . .
C50 C 0.8105(4) 0.9324(3) 0.4790(3) 0.0753(16) Uani 1 1 d . . . . .
C51 C 0.8494(4) 0.9854(3) 0.5487(4) 0.094(2) Uani 1 1 d . . . . .
C52 C 0.8153(4) 1.0078(3) 0.6053(4) 0.101(2) Uani 1 1 d . . . . .
C53 C 0.8562(5) 1.0591(5) 0.6672(5) 0.133(3) Uani 1 1 d . . . . .
H53 H 0.831978 1.072918 0.705644 0.160 Uiso 1 1 calc R U . . .
C54 C 0.9330(6) 1.0905(6) 0.6731(7) 0.172(5) Uani 1 1 d . . . . .
H54 H 0.961689 1.125504 0.715505 0.206 Uiso 1 1 calc R U . . .
C55 C 0.9670(6) 1.0698(6) 0.6160(7) 0.176(5) Uani 1 1 d . . . . .
H55 H 1.018640 1.091734 0.618294 0.211 Uiso 1 1 calc R U . . .
C56 C 0.9249(5) 1.0173(5) 0.5564(6) 0.150(4) Uani 1 1 d . . . . .
H56 H 0.949522 1.002407 0.518403 0.180 Uiso 1 1 calc R U . . .
C57 C 0.7052(5) 0.9924(5) 0.6588(4) 0.129(3) Uani 1 1 d . . . . .
H57A H 0.741280 0.988239 0.701544 0.193 Uiso 1 1 calc R U . . .
H57B H 0.655759 0.959271 0.649624 0.193 Uiso 1 1 calc R U . . .
H57C H 0.695389 1.041974 0.666177 0.193 Uiso 1 1 calc R U . . .
C58 C 0.6256(4) 0.7605(3) 0.5602(3) 0.0749(16) Uani 1 1 d . . . . .
C59 C 0.6589(5) 0.7983(3) 0.6375(3) 0.092(2) Uani 1 1 d . . . . .
C60 C 0.6068(5) 0.8060(3) 0.6814(4) 0.103(2) Uani 1 1 d . . . . .
H60 H 0.552485 0.788052 0.662024 0.124 Uiso 1 1 calc R U . . .
C61 C 0.6351(8) 0.8405(4) 0.7543(5) 0.136(4) Uani 1 1 d . . . . .
H61 H 0.599896 0.846914 0.784535 0.163 Uiso 1 1 calc R U . . .
C62 C 0.7132(9) 0.8649(6) 0.7815(5) 0.157(5) Uani 1 1 d . . . . .
H62 H 0.731454 0.888146 0.831138 0.188 Uiso 1 1 calc R U . . .
C63 C 0.7659(7) 0.8572(5) 0.7408(5) 0.149(4) Uani 1 1 d . . . . .
H63 H 0.820046 0.874096 0.762433 0.179 Uiso 1 1 calc R U . . .
C64 C 0.7415(6) 0.8247(5) 0.6671(4) 0.116(3) Uani 1 1 d . . . . .
C65 C 0.8724(5) 0.8444(5) 0.6517(5) 0.150(4) Uani 1 1 d . . . . .
H65A H 0.879941 0.891927 0.685508 0.225 Uiso 1 1 calc R U . . .
H65B H 0.898390 0.848397 0.613279 0.225 Uiso 1 1 calc R U . . .
H65C H 0.895096 0.810983 0.676605 0.225 Uiso 1 1 calc R U . . .
C66 C 0.4950(3) 0.8492(3) 0.4596(3) 0.0603(13) Uani 1 1 d . . . . .
C67 C 0.4548(3) 0.8964(3) 0.5068(3) 0.0616(13) Uani 1 1 d . . . . .
C68 C 0.5023(3) 0.9529(3) 0.5589(3) 0.0824(18) Uani 1 1 d . . . . .
H68 H 0.557023 0.960419 0.562033 0.099 Uiso 1 1 calc R U . . .
C69 C 0.4728(4) 0.9999(3) 0.6078(3) 0.0854(18) Uani 1 1 d . . . . .
H69 H 0.506940 1.036679 0.645924 0.103 Uiso 1 1 calc R U . . .
C70 C 0.3934(4) 0.9915(3) 0.5992(3) 0.0787(17) Uani 1 1 d . . . . .
H70 H 0.372236 1.024185 0.630847 0.094 Uiso 1 1 calc R U . . .
C71 C 0.3434(3) 0.9367(3) 0.5458(3) 0.0756(16) Uani 1 1 d . . . . .
H71 H 0.288393 0.931936 0.540510 0.091 Uiso 1 1 calc R U . . .
C72 C 0.3744(3) 0.8880(3) 0.4993(3) 0.0689(15) Uani 1 1 d . . . . .
C73 C 0.2454(4) 0.8188(4) 0.4380(5) 0.134(3) Uani 1 1 d . . . . .
H73A H 0.234039 0.807382 0.480792 0.201 Uiso 1 1 calc R U . . .
H73B H 0.220709 0.778298 0.396039 0.201 Uiso 1 1 calc R U . . .
H73C H 0.224751 0.862114 0.431902 0.201 Uiso 1 1 calc R U . . .
C74 C 0.3199(4) 0.6173(4) 0.4823(4) 0.0798(17) Uani 1 1 d . . . . .
C75 C 0.2848(4) 0.6377(5) 0.5435(4) 0.090(2) Uani 1 1 d . . . . .
C76 C 0.2265(4) 0.5844(5) 0.5482(4) 0.111(3) Uani 1 1 d . . . . .
H76 H 0.210619 0.540244 0.511824 0.133 Uiso 1 1 calc R U . . .
C77 C 0.1912(6) 0.5962(8) 0.6071(6) 0.147(5) Uani 1 1 d . . . . .
H77 H 0.153603 0.559698 0.612083 0.176 Uiso 1 1 calc R U . . .
C78 C 0.2129(7) 0.6612(9) 0.6559(6) 0.151(5) Uani 1 1 d . . . . .
H78 H 0.188430 0.669438 0.694764 0.181 Uiso 1 1 calc R U . . .
C79 C 0.2691(6) 0.7172(6) 0.6531(4) 0.132(4) Uani 1 1 d . . . . .
H79 H 0.280355 0.762544 0.687659 0.159 Uiso 1 1 calc R U . . .
C80 C 0.3091(5) 0.7044(5) 0.5970(4) 0.103(3) Uani 1 1 d . . . . .
C81 C 0.3948(6) 0.8204(4) 0.6474(4) 0.135(3) Uani 1 1 d . . . . .
H81A H 0.351043 0.846517 0.650022 0.202 Uiso 1 1 calc R U . . .
H81B H 0.437100 0.849842 0.636263 0.202 Uiso 1 1 calc R U . . .
H81C H 0.414060 0.810550 0.693491 0.202 Uiso 1 1 calc R U . . .
C82 C 0.5593(3) 0.5099(3) 0.4372(3) 0.0767(16) Uani 1 1 d . . . . .
H82A H 0.501951 0.498475 0.425520 0.115 Uiso 1 1 calc R U . . .
H82B H 0.580860 0.484013 0.471337 0.115 Uiso 1 1 calc R U . . .
H82C H 0.577722 0.495178 0.393525 0.115 Uiso 1 1 calc R U . . .
C83 C 0.5843(4) 0.8527(3) 0.2444(3) 0.0871(18) Uani 1 1 d . . . . .
H83A H 0.639555 0.874816 0.264325 0.131 Uiso 1 1 calc R U . . .
H83B H 0.556565 0.885485 0.222240 0.131 Uiso 1 1 calc R U . . .
H83C H 0.580211 0.807233 0.208424 0.131 Uiso 1 1 calc R U . . .
C84 C 0.8391(5) 0.8848(4) 0.2367(5) 0.131(3) Uani 1 1 d . . . . .
H84A H 0.887560 0.919669 0.260327 0.197 Uiso 1 1 calc R U . . .
H84B H 0.812210 0.898010 0.194541 0.197 Uiso 1 1 calc R U . . .
H84C H 0.851631 0.836543 0.221949 0.197 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O6 2.000(4) . ?
Co1 O2 2.050(4) . ?
Co1 O4 2.059(4) . ?
Co1 O1 2.149(4) . ?
Co1 O5 2.180(4) . ?
Co1 N3 2.187(4) . ?
O1 N1 1.370(5) . ?
O1 Co2 1.987(4) . ?
N1 C1 1.320(8) . ?
N1 H1H 0.8800 . ?
C1 O2 1.271(7) . ?
C1 C2 1.504(9) . ?
Co2 O12 2.073(3) . ?
Co2 O11 2.086(3) . ?
Co2 O14 2.097(4) . ?
Co2 O31 2.103(3) . ?
Co2 O10 2.157(3) . ?
N2 C10 1.336(6) . ?
N2 O11 1.370(5) . ?
N2 H2H 0.8800 . ?
C2 C7 1.389(9) . ?
C2 C3 1.399(10) . ?
Co3 O8 1.876(3) . ?
Co3 O19 1.884(3) . ?
Co3 O39 1.923(3) . ?
Co3 O10 1.925(3) . ?
Co3 O11 1.927(3) . ?
Co3 O18 1.934(3) . ?
O3 C7 1.370(8) . ?
O3 C8 1.438(8) . ?
N3 C18 1.292(6) . ?
N3 O10 1.463(5) . ?
C3 C4 1.411(10) . ?
C3 H3 0.9500 . ?
Co4 O6 1.961(4) . ?
Co4 O35 2.068(4) . ?
Co4 O34 2.086(3) . ?
Co4 O36 2.120(4) . ?
Co4 O10 2.126(3) . ?
Co4 O31 2.195(3) . ?
O4 C9 1.465(7) . ?
O4 H4H 0.9500 . ?
N4 C34 1.302(6) . ?
N4 O18 1.461(5) . ?
N4 Co7 2.128(4) . ?
C4 C5 1.332(12) . ?
C4 H4 0.9500 . ?
Co5 O29 1.984(4) . ?
Co5 O32 2.075(3) . ?
Co5 O17 2.087(4) . ?
Co5 O31 2.087(3) . ?
Co5 O18 2.114(3) . ?
Co5 O35 2.185(3) . ?
O5 C74 1.272(7) . ?
N5 C26 1.332(7) . ?
N5 O39 1.387(5) . ?
N5 H5H 0.8800 . ?
C5 C6 1.408(12) . ?
C5 H5 0.9500 . ?
Co6 O24 2.008(4) . ?
Co6 O25 2.054(5) . ?
Co6 O39 2.085(3) . ?
Co6 O38 2.086(4) . ?
Co6 O35 2.109(3) . ?
Co6 O18 2.139(3) . ?
O6 N10 1.372(5) . ?
N6 C42 1.318(7) . ?
N6 O24 1.382(5) . ?
N6 H6H 0.8800 . ?
C6 C7 1.410(10) . ?
C6 H6 0.9500 . ?
Co7 O29 2.027(3) . ?
Co7 O22 2.048(3) . ?
Co7 O21 2.070(5) . ?
Co7 O24 2.083(4) . ?
Co7 O28 2.098(4) . ?
O7 C80 1.362(10) . ?
O7 C81 1.455(9) . ?
N7 C50 1.318(7) . ?
N7 O29 1.388(5) . ?
N7 H7H 0.8800 . ?
O8 C18 1.302(6) . ?
N8 C58 1.291(7) . ?
N8 O35 1.390(5) . ?
N8 H8H 0.8800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
O9 C24 1.364(6) . ?
O9 C25 1.441(6) . ?
N9 C66 1.324(6) . ?
N9 O31 1.394(5) . ?
N9 H9H 0.8800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
N10 C74 1.300(8) . ?
N10 H10H 0.8800 . ?
C10 O12 1.257(6) . ?
C10 C11 1.474(7) . ?
N11 O15 1.223(7) . ?
N11 O16 1.245(7) . ?
N11 O14 1.282(6) . ?
C11 C12 1.400(7) . ?
C11 C16 1.411(7) . ?
N12 O25 1.154(8) . ?
N12 O27 1.169(9) . ?
N12 O26 1.317(9) . ?
C12 C13 1.391(7) . ?
C12 H12 0.9500 . ?
O13 C16 1.356(6) . ?
O13 C17 1.440(6) . ?
C13 C14 1.380(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.365(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.390(7) . ?
C15 H15 0.9500 . ?
O17 C83 1.428(7) . ?
O17 H17 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.489(7) . ?
O19 C34 1.290(6) . ?
C19 C20 1.380(7) . ?
C19 C24 1.403(7) . ?
O20 C40 1.374(7) . ?
O20 C41 1.416(7) . ?
C20 C21 1.401(8) . ?
C20 H20 0.9500 . ?
O21 C84 1.371(9) . ?
O21 H21H 0.9500 . ?
C21 C22 1.390(8) . ?
C21 H21 0.9500 . ?
O22 C42 1.238(7) . ?
C22 C23 1.385(8) . ?
C22 H22 0.9500 . ?
O23 C48 1.370(8) . ?
O23 C49 1.451(9) . ?
C23 C24 1.391(8) . ?
C23 H23 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 O38 1.241(6) . ?
C26 C27 1.487(7) . ?
C27 C28 1.389(8) . ?
C27 C32 1.395(7) . ?
O28 C50 1.253(7) . ?
C28 C29 1.421(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.350(9) . ?
C29 H29 0.9500 . ?
O30 C52 1.385(8) . ?
O30 C57 1.436(8) . ?
C30 C31 1.357(9) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(7) . ?
C31 H31 0.9500 . ?
O32 C66 1.248(6) . ?
C32 O40 1.368(6) . ?
O33 C72 1.375(6) . ?
O33 C73 1.434(7) . ?
C33 O40 1.449(6) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
O34 C82 1.432(6) . ?
O34 H34 0.9500 . ?
C34 C35 1.507(7) . ?
C35 C36 1.366(8) . ?
C35 C40 1.390(8) . ?
O36 C58 1.278(7) . ?
C36 C37 1.385(9) . ?
C36 H36 0.9500 . ?
O37 C64 1.359(10) . ?
O37 C65 1.447(9) . ?
C37 C38 1.375(10) . ?
C37 H37 0.9500 . ?
C38 C39 1.369(10) . ?
C38 H38 0.9500 . ?
C39 C40 1.383(8) . ?
C39 H39 0.9500 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.502(8) . ?
C43 C44 1.350(8) . ?
C43 C48 1.405(9) . ?
C44 C45 1.416(8) . ?
C44 H44 0.9500 . ?
C45 C46 1.339(9) . ?
C45 H45 0.9500 . ?
C46 C47 1.402(10) . ?
C46 H46 0.9500 . ?
C47 C48 1.393(9) . ?
C47 H47 0.9500 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.488(9) . ?
C51 C56 1.369(10) . ?
C51 C52 1.388(10) . ?
C52 C53 1.383(10) . ?
C53 C54 1.392(12) . ?
C53 H53 0.9500 . ?
C54 C55 1.388(14) . ?
C54 H54 0.9500 . ?
C55 C56 1.372(12) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C59 1.494(8) . ?
C59 C60 1.390(10) . ?
C59 C64 1.442(11) . ?
C60 C61 1.399(11) . ?
C60 H60 0.9500 . ?
C61 C62 1.359(15) . ?
C61 H61 0.9500 . ?
C62 C63 1.354(15) . ?
C62 H62 0.9500 . ?
C63 C64 1.402(11) . ?
C63 H63 0.9500 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 C67 1.499(7) . ?
C67 C68 1.366(7) . ?
C67 C72 1.388(7) . ?
C68 C69 1.396(8) . ?
C68 H68 0.9500 . ?
C69 C70 1.369(8) . ?
C69 H69 0.9500 . ?
C70 C71 1.377(8) . ?
C70 H70 0.9500 . ?
C71 C72 1.403(7) . ?
C71 H71 0.9500 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 C75 1.470(8) . ?
C75 C76 1.404(10) . ?
C75 C80 1.421(11) . ?
C76 C77 1.420(11) . ?
C76 H76 0.9500 . ?
C77 C78 1.352(16) . ?
C77 H77 0.9500 . ?
C78 C79 1.403(15) . ?
C78 H78 0.9500 . ?
C79 C80 1.425(10) . ?
C79 H79 0.9500 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 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
O6 Co1 O2 157.50(16) . . ?
O6 Co1 O4 102.30(17) . . ?
O2 Co1 O4 95.48(18) . . ?
O6 Co1 O1 83.76(14) . . ?
O2 Co1 O1 77.00(15) . . ?
O4 Co1 O1 170.53(15) . . ?
O6 Co1 O5 76.32(16) . . ?
O2 Co1 O5 93.22(16) . . ?
O4 Co1 O5 80.91(17) . . ?
O1 Co1 O5 93.64(15) . . ?
O6 Co1 N3 87.04(14) . . ?
O2 Co1 N3 104.22(15) . . ?
O4 Co1 N3 97.84(16) . . ?
O1 Co1 N3 89.67(14) . . ?
O5 Co1 N3 162.55(17) . . ?
N1 O1 Co2 111.4(3) . . ?
N1 O1 Co1 107.6(3) . . ?
Co2 O1 Co1 109.21(14) . . ?
C1 N1 O1 119.4(5) . . ?
C1 N1 H1H 120.3 . . ?
O1 N1 H1H 120.3 . . ?
O2 C1 N1 119.1(5) . . ?
O2 C1 C2 120.1(7) . . ?
N1 C1 C2 120.8(7) . . ?
O1 Co2 O12 93.07(14) . . ?
O1 Co2 O11 165.09(14) . . ?
O12 Co2 O11 77.16(13) . . ?
O1 Co2 O14 105.14(15) . . ?
O12 Co2 O14 91.96(14) . . ?
O11 Co2 O14 86.64(14) . . ?
O1 Co2 O31 90.72(14) . . ?
O12 Co2 O31 174.39(13) . . ?
O11 Co2 O31 98.29(13) . . ?
O14 Co2 O31 91.03(14) . . ?
O1 Co2 O10 94.98(13) . . ?
O12 Co2 O10 104.32(12) . . ?
O11 Co2 O10 76.92(12) . . ?
O14 Co2 O10 153.42(14) . . ?
O31 Co2 O10 71.20(12) . . ?
C1 O2 Co1 115.2(4) . . ?
C10 N2 O11 117.5(4) . . ?
C10 N2 H2H 121.3 . . ?
O11 N2 H2H 121.3 . . ?
C7 C2 C3 120.0(7) . . ?
C7 C2 C1 124.7(7) . . ?
C3 C2 C1 115.3(7) . . ?
O8 Co3 O19 93.51(15) . . ?
O8 Co3 O39 90.82(14) . . ?
O19 Co3 O39 97.38(14) . . ?
O8 Co3 O10 83.00(14) . . ?
O19 Co3 O10 174.63(14) . . ?
O39 Co3 O10 86.77(13) . . ?
O8 Co3 O11 96.84(13) . . ?
O19 Co3 O11 89.87(14) . . ?
O39 Co3 O11 169.12(13) . . ?
O10 Co3 O11 86.51(14) . . ?
O8 Co3 O18 174.83(13) . . ?
O19 Co3 O18 82.80(14) . . ?
O39 Co3 O18 86.09(14) . . ?
O10 Co3 O18 100.94(14) . . ?
O11 Co3 O18 86.79(14) . . ?
C7 O3 C8 118.7(6) . . ?
C18 N3 O10 108.3(4) . . ?
C18 N3 Co1 138.9(4) . . ?
O10 N3 Co1 107.7(2) . . ?
C2 C3 C4 119.3(8) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
O6 Co4 O35 171.73(14) . . ?
O6 Co4 O34 92.92(15) . . ?
O35 Co4 O34 88.79(14) . . ?
O6 Co4 O36 94.53(16) . . ?
O35 Co4 O36 77.36(15) . . ?
O34 Co4 O36 90.56(14) . . ?
O6 Co4 O10 86.54(14) . . ?
O35 Co4 O10 101.13(13) . . ?
O34 Co4 O10 100.14(13) . . ?
O36 Co4 O10 169.18(13) . . ?
O6 Co4 O31 96.07(14) . . ?
O35 Co4 O31 83.82(13) . . ?
O34 Co4 O31 166.18(14) . . ?
O36 Co4 O31 99.15(13) . . ?
O10 Co4 O31 70.04(12) . . ?
C9 O4 Co1 135.2(4) . . ?
C9 O4 H4H 112.4 . . ?
Co1 O4 H4H 112.4 . . ?
C34 N4 O18 108.8(4) . . ?
C34 N4 Co7 138.1(4) . . ?
O18 N4 Co7 108.8(3) . . ?
C5 C4 C3 121.0(10) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
O29 Co5 O32 94.63(14) . . ?
O29 Co5 O17 88.75(15) . . ?
O32 Co5 O17 97.49(13) . . ?
O29 Co5 O31 170.83(13) . . ?
O32 Co5 O31 77.59(13) . . ?
O17 Co5 O31 87.48(14) . . ?
O29 Co5 O18 89.73(13) . . ?
O32 Co5 O18 164.17(14) . . ?
O17 Co5 O18 97.81(13) . . ?
O31 Co5 O18 99.06(12) . . ?
O29 Co5 O35 101.97(14) . . ?
O32 Co5 O35 94.05(13) . . ?
O17 Co5 O35 163.58(13) . . ?
O31 Co5 O35 83.61(13) . . ?
O18 Co5 O35 70.15(13) . . ?
C74 O5 Co1 111.0(4) . . ?
C26 N5 O39 116.4(4) . . ?
C26 N5 H5H 121.8 . . ?
O39 N5 H5H 121.8 . . ?
C4 C5 C6 120.8(9) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
O24 Co6 O25 101.7(2) . . ?
O24 Co6 O39 162.27(15) . . ?
O25 Co6 O39 93.6(2) . . ?
O24 Co6 O38 93.73(14) . . ?
O25 Co6 O38 91.22(18) . . ?
O39 Co6 O38 76.84(13) . . ?
O24 Co6 O35 87.80(13) . . ?
O25 Co6 O35 92.40(18) . . ?
O39 Co6 O35 100.62(13) . . ?
O38 Co6 O35 175.71(14) . . ?
O24 Co6 O18 91.18(13) . . ?
O25 Co6 O18 158.8(2) . . ?
O39 Co6 O18 77.10(13) . . ?
O38 Co6 O18 104.81(14) . . ?
O35 Co6 O18 71.13(13) . . ?
N10 O6 Co4 120.2(3) . . ?
N10 O6 Co1 114.1(3) . . ?
Co4 O6 Co1 123.69(17) . . ?
C42 N6 O24 117.9(4) . . ?
C42 N6 H6H 121.1 . . ?
O24 N6 H6H 121.1 . . ?
C5 C6 C7 119.2(9) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
O29 Co7 O22 162.36(16) . . ?
O29 Co7 O21 96.89(17) . . ?
O22 Co7 O21 96.38(18) . . ?
O29 Co7 O24 86.61(14) . . ?
O22 Co7 O24 79.12(15) . . ?
O21 Co7 O24 173.45(17) . . ?
O29 Co7 O28 77.78(15) . . ?
O22 Co7 O28 91.23(15) . . ?
O21 Co7 O28 87.6(2) . . ?
O24 Co7 O28 87.72(15) . . ?
O29 Co7 N4 88.36(15) . . ?
O22 Co7 N4 101.77(15) . . ?
O21 Co7 N4 95.9(2) . . ?
O24 Co7 N4 89.70(15) . . ?
O28 Co7 N4 166.02(16) . . ?
C80 O7 C81 118.7(6) . . ?
C50 N7 O29 117.8(5) . . ?
C50 N7 H7H 121.1 . . ?
O29 N7 H7H 121.1 . . ?
O3 C7 C2 117.6(6) . . ?
O3 C7 C6 122.9(8) . . ?
C2 C7 C6 119.5(8) . . ?
C18 O8 Co3 111.6(3) . . ?
C58 N8 O35 117.9(5) . . ?
C58 N8 H8H 121.0 . . ?
O35 N8 H8H 121.0 . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C24 O9 C25 118.3(4) . . ?
C66 N9 O31 117.3(4) . . ?
C66 N9 H9H 121.3 . . ?
O31 N9 H9H 121.3 . . ?
O4 C9 H9A 109.5 . . ?
O4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 O10 Co3 111.7(2) . . ?
N3 O10 Co4 116.3(3) . . ?
Co3 O10 Co4 120.91(16) . . ?
N3 O10 Co2 100.3(2) . . ?
Co3 O10 Co2 97.10(14) . . ?
Co4 O10 Co2 105.83(12) . . ?
C74 N10 O6 118.3(5) . . ?
C74 N10 H10H 120.8 . . ?
O6 N10 H10H 120.8 . . ?
O12 C10 N2 119.6(5) . . ?
O12 C10 C11 120.8(5) . . ?
N2 C10 C11 119.6(5) . . ?
N2 O11 Co3 113.0(2) . . ?
N2 O11 Co2 110.2(3) . . ?
Co3 O11 Co2 99.47(15) . . ?
O15 N11 O16 124.3(6) . . ?
O15 N11 O14 119.8(6) . . ?
O16 N11 O14 115.9(7) . . ?
C12 C11 C16 118.1(5) . . ?
C12 C11 C10 116.1(5) . . ?
C16 C11 C10 125.7(5) . . ?
C10 O12 Co2 114.2(3) . . ?
O25 N12 O27 124.5(10) . . ?
O25 N12 O26 111.6(9) . . ?
O27 N12 O26 120.3(11) . . ?
C13 C12 C11 122.1(5) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C16 O13 C17 117.9(4) . . ?
C14 C13 C12 118.0(6) . . ?
C14 C13 H13 121.0 . . ?
C12 C13 H13 121.0 . . ?
N11 O14 Co2 131.6(4) . . ?
C15 C14 C13 121.6(5) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 121.0(6) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
O13 C16 C15 124.3(5) . . ?
O13 C16 C11 116.4(4) . . ?
C15 C16 C11 119.2(5) . . ?
C83 O17 Co5 126.0(3) . . ?
C83 O17 H17 117.0 . . ?
Co5 O17 H17 117.0 . . ?
O13 C17 H17A 109.5 . . ?
O13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 O18 Co3 111.4(2) . . ?
N4 O18 Co5 114.1(2) . . ?
Co3 O18 Co5 122.14(16) . . ?
N4 O18 Co6 101.7(2) . . ?
Co3 O18 Co6 97.28(14) . . ?
Co5 O18 Co6 106.36(14) . . ?
N3 C18 O8 124.9(5) . . ?
N3 C18 C19 118.6(5) . . ?
O8 C18 C19 116.4(4) . . ?
C34 O19 Co3 111.9(3) . . ?
C20 C19 C24 119.4(5) . . ?
C20 C19 C18 122.3(5) . . ?
C24 C19 C18 118.3(4) . . ?
C40 O20 C41 117.6(5) . . ?
C19 C20 C21 121.1(5) . . ?
C19 C20 H20 119.4 . . ?
C21 C20 H20 119.4 . . ?
C84 O21 Co7 127.9(5) . . ?
C84 O21 H21H 116.0 . . ?
Co7 O21 H21H 116.0 . . ?
C22 C21 C20 118.8(5) . . ?
C22 C21 H21 120.6 . . ?
C20 C21 H21 120.6 . . ?
C42 O22 Co7 111.4(4) . . ?
C23 C22 C21 120.8(6) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C48 O23 C49 118.7(6) . . ?
C22 C23 C24 120.0(6) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
N6 O24 Co6 110.2(3) . . ?
N6 O24 Co7 106.2(3) . . ?
Co6 O24 Co7 111.60(15) . . ?
O9 C24 C23 124.2(5) . . ?
O9 C24 C19 115.8(5) . . ?
C23 C24 C19 120.0(5) . . ?
N12 O25 Co6 147.0(7) . . ?
O9 C25 H25A 109.5 . . ?
O9 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
O9 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O38 C26 N5 120.8(5) . . ?
O38 C26 C27 120.9(5) . . ?
N5 C26 C27 118.3(5) . . ?
C28 C27 C32 118.2(5) . . ?
C28 C27 C26 114.6(5) . . ?
C32 C27 C26 127.2(5) . . ?
C50 O28 Co7 111.1(4) . . ?
C27 C28 C29 120.6(6) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
N7 O29 Co5 117.2(3) . . ?
N7 O29 Co7 108.9(3) . . ?
Co5 O29 Co7 117.89(17) . . ?
C30 C29 C28 118.9(6) . . ?
C30 C29 H29 120.5 . . ?
C28 C29 H29 120.5 . . ?
C52 O30 C57 118.4(5) . . ?
C29 C30 C31 121.3(6) . . ?
C29 C30 H30 119.3 . . ?
C31 C30 H30 119.3 . . ?
N9 O31 Co5 108.2(3) . . ?
N9 O31 Co2 115.7(2) . . ?
Co5 O31 Co2 118.59(16) . . ?
N9 O31 Co4 111.4(3) . . ?
Co5 O31 Co4 95.73(13) . . ?
Co2 O31 Co4 105.30(14) . . ?
C30 C31 C32 120.9(6) . . ?
C30 C31 H31 119.5 . . ?
C32 C31 H31 119.5 . . ?
C66 O32 Co5 112.6(3) . . ?
O40 C32 C31 123.1(5) . . ?
O40 C32 C27 116.9(4) . . ?
C31 C32 C27 119.9(5) . . ?
C72 O33 C73 119.1(4) . . ?
O40 C33 H33A 109.5 . . ?
O40 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
O40 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C82 O34 Co4 124.4(3) . . ?
C82 O34 H34 117.8 . . ?
Co4 O34 H34 117.8 . . ?
O19 C34 N4 124.6(5) . . ?
O19 C34 C35 117.4(4) . . ?
N4 C34 C35 118.1(5) . . ?
N8 O35 Co4 109.7(3) . . ?
N8 O35 Co6 114.4(3) . . ?
Co4 O35 Co6 115.94(15) . . ?
N8 O35 Co5 114.0(3) . . ?
Co4 O35 Co5 96.60(13) . . ?
Co6 O35 Co5 104.93(15) . . ?
C36 C35 C40 121.2(6) . . ?
C36 C35 C34 119.4(5) . . ?
C40 C35 C34 119.1(5) . . ?
C58 O36 Co4 110.7(4) . . ?
C35 C36 C37 119.6(7) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C64 O37 C65 117.6(7) . . ?
C38 C37 C36 119.5(7) . . ?
C38 C37 H37 120.3 . . ?
C36 C37 H37 120.3 . . ?
C26 O38 Co6 113.8(3) . . ?
C39 C38 C37 120.9(7) . . ?
C39 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
N5 O39 Co3 114.9(3) . . ?
N5 O39 Co6 110.3(3) . . ?
Co3 O39 Co6 99.51(15) . . ?
C38 C39 C40 120.2(7) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C32 O40 C33 117.6(4) . . ?
O20 C40 C39 125.6(6) . . ?
O20 C40 C35 115.9(5) . . ?
C39 C40 C35 118.5(6) . . ?
O20 C41 H41A 109.5 . . ?
O20 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
O20 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O22 C42 N6 122.0(5) . . ?
O22 C42 C43 121.2(6) . . ?
N6 C42 C43 116.7(6) . . ?
C44 C43 C48 119.6(6) . . ?
C44 C43 C42 116.6(6) . . ?
C48 C43 C42 123.9(6) . . ?
C43 C44 C45 122.2(7) . . ?
C43 C44 H44 118.9 . . ?
C45 C44 H44 118.9 . . ?
C46 C45 C44 117.5(7) . . ?
C46 C45 H45 121.2 . . ?
C44 C45 H45 121.2 . . ?
C45 C46 C47 122.0(6) . . ?
C45 C46 H46 119.0 . . ?
C47 C46 H46 119.0 . . ?
C48 C47 C46 119.5(7) . . ?
C48 C47 H47 120.2 . . ?
C46 C47 H47 120.2 . . ?
O23 C48 C47 123.7(7) . . ?
O23 C48 C43 117.8(5) . . ?
C47 C48 C43 118.5(7) . . ?
O23 C49 H49A 109.5 . . ?
O23 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
O23 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O28 C50 N7 119.7(6) . . ?
O28 C50 C51 119.7(6) . . ?
N7 C50 C51 120.6(6) . . ?
C56 C51 C52 117.0(7) . . ?
C56 C51 C50 116.7(7) . . ?
C52 C51 C50 126.2(6) . . ?
C53 C52 O30 121.0(7) . . ?
C53 C52 C51 121.5(7) . . ?
O30 C52 C51 117.4(6) . . ?
C52 C53 C54 119.8(9) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C55 C54 C53 119.1(9) . . ?
C55 C54 H54 120.4 . . ?
C53 C54 H54 120.4 . . ?
C56 C55 C54 119.1(9) . . ?
C56 C55 H55 120.4 . . ?
C54 C55 H55 120.4 . . ?
C51 C56 C55 123.4(9) . . ?
C51 C56 H56 118.3 . . ?
C55 C56 H56 118.3 . . ?
O30 C57 H57A 109.5 . . ?
O30 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O30 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O36 C58 N8 121.6(5) . . ?
O36 C58 C59 120.0(6) . . ?
N8 C58 C59 118.3(6) . . ?
C60 C59 C64 120.2(7) . . ?
C60 C59 C58 117.2(7) . . ?
C64 C59 C58 122.6(7) . . ?
C59 C60 C61 119.5(9) . . ?
C59 C60 H60 120.3 . . ?
C61 C60 H60 120.3 . . ?
C62 C61 C60 119.7(10) . . ?
C62 C61 H61 120.1 . . ?
C60 C61 H61 120.1 . . ?
C63 C62 C61 122.6(10) . . ?
C63 C62 H62 118.7 . . ?
C61 C62 H62 118.7 . . ?
C62 C63 C64 120.7(11) . . ?
C62 C63 H63 119.6 . . ?
C64 C63 H63 119.6 . . ?
O37 C64 C63 124.9(9) . . ?
O37 C64 C59 117.9(6) . . ?
C63 C64 C59 117.3(10) . . ?
O37 C65 H65A 109.5 . . ?
O37 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
O37 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
O32 C66 N9 120.8(4) . . ?
O32 C66 C67 122.1(5) . . ?
N9 C66 C67 117.1(5) . . ?
C68 C67 C72 119.1(5) . . ?
C68 C67 C66 116.0(5) . . ?
C72 C67 C66 124.9(5) . . ?
C67 C68 C69 121.9(5) . . ?
C67 C68 H68 119.0 . . ?
C69 C68 H68 119.0 . . ?
C70 C69 C68 118.2(6) . . ?
C70 C69 H69 120.9 . . ?
C68 C69 H69 120.9 . . ?
C69 C70 C71 121.5(5) . . ?
C69 C70 H70 119.2 . . ?
C71 C70 H70 119.2 . . ?
C70 C71 C72 119.4(5) . . ?
C70 C71 H71 120.3 . . ?
C72 C71 H71 120.3 . . ?
O33 C72 C67 117.4(4) . . ?
O33 C72 C71 122.8(5) . . ?
C67 C72 C71 119.7(5) . . ?
O33 C73 H73A 109.5 . . ?
O33 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
O33 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
O5 C74 N10 119.8(5) . . ?
O5 C74 C75 120.4(6) . . ?
N10 C74 C75 119.7(7) . . ?
C76 C75 C80 120.7(7) . . ?
C76 C75 C74 115.1(8) . . ?
C80 C75 C74 124.1(7) . . ?
C75 C76 C77 120.4(10) . . ?
C75 C76 H76 119.8 . . ?
C77 C76 H76 119.8 . . ?
C78 C77 C76 117.8(12) . . ?
C78 C77 H77 121.1 . . ?
C76 C77 H77 121.1 . . ?
C77 C78 C79 124.4(11) . . ?
C77 C78 H78 117.8 . . ?
C79 C78 H78 117.8 . . ?
C78 C79 C80 118.4(10) . . ?
C78 C79 H79 120.8 . . ?
C80 C79 H79 120.8 . . ?
O7 C80 C75 118.4(6) . . ?
O7 C80 C79 123.6(9) . . ?
C75 C80 C79 118.0(10) . . ?
O7 C81 H81A 109.5 . . ?
O7 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
O7 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
O34 C82 H82A 109.5 . . ?
O34 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
O34 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O17 C83 H83A 109.5 . . ?
O17 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
O17 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
O21 C84 H84A 109.5 . . ?
O21 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
O21 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?

_refine_diff_density_max         0.695
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.064



# SQUEEZE RESULTS (Version = 241018)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.008 -0.002 -0.002 2105 639 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_bfm67a
_database_code_depnum_ccdc_archive 'CCDC 1907529'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;Bangor University 
United Kingdom
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Fe2]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H32 N4 O12 Cl2 Fe2 (C4 H6 N2)'
_chemical_formula_sum            'C36 H38 Cl2 Fe2 N6 O12'
_chemical_formula_weight         929.32

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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0272(3)
_cell_length_b                   10.6948(3)
_cell_length_c                   10.8905(4)
_cell_angle_alpha                76.760(3)
_cell_angle_beta                 65.622(3)
_cell_angle_gamma                69.977(3)
_cell_volume                     994.20(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    9026
_cell_measurement_theta_min      5.0320
_cell_measurement_theta_max      70.3150

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_F_000             478
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.934
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
crysalispro 1.171.39.9g (rigaku oxford diffraction, 2015)
empirical absorption correction using spherical harmonics,
 implemented in scale3 abspack scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xtalab afc11 (rcd3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12861
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.037
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             3554
_reflns_number_gt                3289
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_cell_refinement       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_data_reduction        'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+8.2520P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3554
_refine_ls_number_parameters     265
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1719
_refine_ls_wR_factor_gt          0.1406
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_restrained_S_all      1.170
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.15880(9) 0.40452(8) 0.52800(8) 0.0199(2) Uani 1 1 d . . . . .
Cl1 Cl 0.22075(14) 0.42246(12) 0.70393(12) 0.0163(3) Uani 1 1 d . . . . .
O1 O 0.2806(4) 0.5185(4) 0.3790(3) 0.0152(7) Uani 1 1 d . . . . .
N1 N 0.1463(5) 0.5055(4) 0.2651(4) 0.0153(9) Uani 1 1 d . . . . .
H1 H 0.132622 0.511532 0.188932 0.018 Uiso 1 1 calc R U . . .
C1 C 0.2580(6) 0.5421(5) 0.2686(5) 0.0154(10) Uani 1 1 d . . . . .
O2 O 0.0527(4) 0.4575(3) 0.3872(3) 0.0139(7) Uani 1 1 d . . . . .
N2 N 0.2686(5) 0.1353(4) 0.4893(4) 0.0156(9) Uani 1 1 d . . . . .
H2 H 0.329972 0.057956 0.460259 0.019 Uiso 1 1 calc R U . . .
C2 C 0.3538(6) 0.6085(5) 0.1462(5) 0.0151(10) Uani 1 1 d . . . . .
O3 O 0.1940(4) 0.6340(4) 0.0260(4) 0.0215(8) Uani 1 1 d . . . . .
N3 N 0.5477(6) -0.0210(5) 0.2837(5) 0.0319(12) Uani 1 1 d . . . . .
C3 C 0.3207(6) 0.6549(5) 0.0266(5) 0.0162(10) Uani 1 1 d . . . . .
O4 O 0.3148(4) 0.2485(3) 0.4442(4) 0.0165(8) Uani 1 1 d . . . . .
C4 C 0.4142(6) 0.7204(6) -0.0831(5) 0.0215(12) Uani 1 1 d . . . . .
H4 H 0.392046 0.751951 -0.163440 0.026 Uiso 1 1 calc R U . . .
O5 O 0.0489(4) 0.2611(3) 0.6185(3) 0.0151(7) Uani 1 1 d . . . . .
C5 C 0.5409(6) 0.7392(6) -0.0742(6) 0.0243(12) Uani 1 1 d . . . . .
H5 H 0.604877 0.783654 -0.149137 0.029 Uiso 1 1 calc R U . . .
O6 O 0.2954(4) -0.1232(4) 0.5270(4) 0.0198(8) Uani 1 1 d . . . . .
C6 C 0.5748(6) 0.6939(6) 0.0424(6) 0.0238(12) Uani 1 1 d . . . . .
H6 H 0.661069 0.707363 0.047580 0.029 Uiso 1 1 calc R U . . .
C7 C 0.4812(6) 0.6286(5) 0.1513(5) 0.0179(11) Uani 1 1 d . . . . .
H7 H 0.504585 0.597074 0.231069 0.022 Uiso 1 1 calc R U . . .
C8 C 0.1609(7) 0.6772(7) -0.0950(6) 0.0277(13) Uani 1 1 d . . . . .
H8A H 0.143108 0.774366 -0.114779 0.042 Uiso 1 1 calc R U . . .
H8B H 0.069492 0.653846 -0.082770 0.042 Uiso 1 1 calc R U . . .
H8C H 0.247306 0.633015 -0.170562 0.042 Uiso 1 1 calc R U . . .
C9 C 0.1283(6) 0.1452(5) 0.5782(5) 0.0141(10) Uani 1 1 d . . . . .
C10 C 0.0607(6) 0.0323(5) 0.6286(5) 0.0143(10) Uani 1 1 d . . . . .
C11 C 0.1430(6) -0.0996(5) 0.5980(5) 0.0157(10) Uani 1 1 d . . . . .
C12 C 0.0670(6) -0.1990(5) 0.6427(5) 0.0172(11) Uani 1 1 d . . . . .
H12 H 0.121753 -0.288365 0.621975 0.021 Uiso 1 1 calc R U . . .
C13 C -0.0878(6) -0.1670(5) 0.7172(5) 0.0195(11) Uani 1 1 d . . . . .
H13 H -0.139179 -0.234604 0.746377 0.023 Uiso 1 1 calc R U . . .
C14 C -0.1698(6) -0.0367(6) 0.7500(5) 0.0204(11) Uani 1 1 d . . . . .
H14 H -0.276001 -0.015667 0.802093 0.024 Uiso 1 1 calc R U . . .
C15 C -0.0949(6) 0.0616(5) 0.7059(5) 0.0193(11) Uani 1 1 d . . . . .
H15 H -0.150247 0.150288 0.728621 0.023 Uiso 1 1 calc R U . . .
C16 C 0.3808(6) -0.2572(5) 0.4909(6) 0.0226(12) Uani 1 1 d . . . . .
H16A H 0.374781 -0.319132 0.573407 0.034 Uiso 1 1 calc R U . . .
H16B H 0.487685 -0.260008 0.436940 0.034 Uiso 1 1 calc R U . . .
H16C H 0.338036 -0.283437 0.437682 0.034 Uiso 1 1 calc R U . . .
C17 C 0.6688(7) -0.0560(6) 0.2083(6) 0.0231(12) Uani 1 1 d . . . . .
C18 C 0.8238(7) -0.0994(7) 0.1134(6) 0.0326(14) Uani 1 1 d . . . . .
H18A H 0.885380 -0.048643 0.119560 0.049 Uiso 1 1 calc R U . . .
H18B H 0.823908 -0.083926 0.021141 0.049 Uiso 1 1 calc R U . . .
H18C H 0.867039 -0.195001 0.135367 0.049 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O4 1.949(4) . ?
Fe1 O1 2.022(3) . ?
Fe1 O5 2.026(3) . ?
Fe1 O2 2.084(4) . ?
Fe1 O2 2.095(3) 2_566 ?
Fe1 Cl1 2.3078(14) . ?
O1 C1 1.268(6) . ?
N1 C1 1.323(7) . ?
N1 O2 1.379(5) . ?
N1 H1 0.8800 . ?
C1 C2 1.477(7) . ?
N2 C9 1.322(6) . ?
N2 O4 1.358(5) . ?
N2 H2 0.8800 . ?
C2 C7 1.391(7) . ?
C2 C3 1.414(7) . ?
O3 C3 1.366(6) . ?
O3 C8 1.427(7) . ?
N3 C17 1.138(8) . ?
C3 C4 1.393(7) . ?
C4 C5 1.396(8) . ?
C4 H4 0.9500 . ?
O5 C9 1.283(6) . ?
C5 C6 1.387(8) . ?
C5 H5 0.9500 . ?
O6 C11 1.359(6) . ?
O6 C16 1.443(6) . ?
C6 C7 1.388(7) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.472(7) . ?
C10 C15 1.394(7) . ?
C10 C11 1.405(7) . ?
C11 C12 1.400(7) . ?
C12 C13 1.381(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.396(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.382(8) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.449(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 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
O4 Fe1 O1 87.52(14) . . ?
O4 Fe1 O5 79.19(14) . . ?
O1 Fe1 O5 159.42(14) . . ?
O4 Fe1 O2 95.96(15) . . ?
O1 Fe1 O2 76.65(13) . . ?
O5 Fe1 O2 89.08(14) . . ?
O4 Fe1 O2 162.17(14) . 2_566 ?
O1 Fe1 O2 103.14(14) . 2_566 ?
O5 Fe1 O2 86.42(14) . 2_566 ?
O2 Fe1 O2 73.16(15) . 2_566 ?
O4 Fe1 Cl1 104.40(12) . . ?
O1 Fe1 Cl1 99.41(11) . . ?
O5 Fe1 Cl1 99.08(11) . . ?
O2 Fe1 Cl1 159.13(10) . . ?
O2 Fe1 Cl1 88.12(10) 2_566 . ?
C1 O1 Fe1 115.6(3) . . ?
C1 N1 O2 116.4(4) . . ?
C1 N1 H1 121.8 . . ?
O2 N1 H1 121.8 . . ?
O1 C1 N1 118.5(4) . . ?
O1 C1 C2 121.1(5) . . ?
N1 C1 C2 120.4(5) . . ?
N1 O2 Fe1 109.6(3) . . ?
N1 O2 Fe1 114.1(3) . 2_566 ?
Fe1 O2 Fe1 106.84(15) . 2_566 ?
C9 N2 O4 117.9(4) . . ?
C9 N2 H2 121.1 . . ?
O4 N2 H2 121.1 . . ?
C7 C2 C3 118.9(5) . . ?
C7 C2 C1 117.5(5) . . ?
C3 C2 C1 123.6(5) . . ?
C3 O3 C8 117.8(4) . . ?
O3 C3 C4 122.9(5) . . ?
O3 C3 C2 117.1(4) . . ?
C4 C3 C2 120.1(5) . . ?
N2 O4 Fe1 112.6(3) . . ?
C3 C4 C5 119.5(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C9 O5 Fe1 113.6(3) . . ?
C6 C5 C4 121.0(5) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C11 O6 C16 117.5(4) . . ?
C5 C6 C7 119.3(5) . . ?
C5 C6 H6 120.4 . . ?
C7 C6 H6 120.4 . . ?
C6 C7 C2 121.3(5) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 H7 119.3 . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O5 C9 N2 116.6(4) . . ?
O5 C9 C10 120.0(4) . . ?
N2 C9 C10 123.4(5) . . ?
C15 C10 C11 119.4(5) . . ?
C15 C10 C9 117.0(4) . . ?
C11 C10 C9 123.5(4) . . ?
O6 C11 C12 123.6(5) . . ?
O6 C11 C10 116.8(4) . . ?
C12 C11 C10 119.6(5) . . ?
C13 C12 C11 119.9(5) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 120.8(5) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C13 119.4(5) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C10 120.9(5) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
O6 C16 H16A 109.5 . . ?
O6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C17 C18 179.0(7) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?

_refine_diff_density_max         1.150
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.165


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeCN'
_chemical_properties_physical    Hygroscopic
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_lfjbfm24sq
_database_code_depnum_ccdc_archive 'CCDC 1907528'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;Bangor University 
United Kingdom
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_DENSD01_lfjbfm24sq          
;
PROBLEM: The ratio of the submitted crystal density and that
RESPONSE: SQUEEZE info given in the cif. 
;
_vrf_PLAT046_lfjbfm24sq          
;
PROBLEM: Reported Z, MW and D(calc) are Inconsistent ....      1.660 Check
RESPONSE: As to be expected due to extent of SQUEEZE 
;
# Added during the CSD deposition process: Tuesday 04 June 2019 10:11 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Cu5].3H2O.4MeOH'
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H64 N10 O24 Cu5 (C4 H22 O7)'
_chemical_formula_sum            'C66 H86 Cu5 N10 O31'
_chemical_formula_weight         1833.17

_smtbx_masks_special_details     
;
A solvent mask was calculated and 639 electrons were 
found in a volume of 299 A^3 in 1 void. This is consistent with the presence of
3[H2O] and 4[CH4O] per formula unit.
;
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.464(2)
_cell_length_b                   12.740(3)
_cell_length_c                   14.419(3)
_cell_angle_alpha                109.97(3)
_cell_angle_beta                 97.74(3)
_cell_angle_gamma                106.55(3)
_cell_volume                     1833.3(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    16866
_cell_measurement_theta_min      2.1010
_cell_measurement_theta_max      27.5040

_exptl_crystal_description       Plate
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_F_000             841
_exptl_transmission_factor_min   0.840
_exptl_transmission_factor_max   0.970
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.507
_shelx_estimated_absorpt_T_min   0.840
_shelx_estimated_absorpt_T_max   0.970
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6705
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.819
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6705
_reflns_number_gt                5848
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.

 Structure factors included contributions from the .fab file.

 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1231P)²+16.1089P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6705
_refine_ls_number_parameters     449
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0775
_refine_ls_wR_factor_ref         0.2263
_refine_ls_wR_factor_gt          0.2141
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.500000 0.500000 0.500000 0.0186(3) Uani 1 2 d S . P . .
O1 O 0.2502(4) 0.6141(4) 0.3258(3) 0.0209(9) Uani 1 1 d . . . . .
N1 N 0.3736(5) 0.8508(4) 0.6124(4) 0.0191(10) Uani 1 1 d . . . . .
H1H H 0.423586 0.927114 0.672694 0.023 Uiso 1 1 calc R U . . .
C1 C 0.3148(6) 0.6881(6) 0.4085(4) 0.0205(13) Uani 1 1 d . . . . .
Cu2 Cu 0.47508(7) 0.74495(6) 0.60537(5) 0.0174(2) Uani 1 1 d . . . . .
O2 O 0.3674(4) 0.5447(4) 0.4454(3) 0.0237(10) Uani 1 1 d . . . . .
N2 N 0.3814(5) 0.6615(4) 0.4741(4) 0.0214(11) Uani 1 1 d . . . . .
C2 C 0.3185(6) 0.8092(5) 0.4295(4) 0.0196(12) Uani 1 1 d . . . . .
Cu3 Cu 0.28563(7) 0.46825(6) 0.31116(5) 0.0189(2) Uani 1 1 d . . . . .
O3 O 0.3180(4) 0.6134(4) 0.6605(3) 0.0246(10) Uani 1 1 d . . . . .
H3H H 0.344259 0.562698 0.672072 0.030 Uiso 1 1 calc R U . . .
N3 N 0.3606(5) 0.3496(4) 0.3146(4) 0.0176(10) Uani 1 1 d . . . . .
C3 C 0.2929(7) 0.8487(6) 0.3500(5) 0.0255(14) Uani 1 1 d . . . . .
H3 H 0.269409 0.790820 0.281816 0.031 Uiso 1 1 calc R U . . .
O4 O 0.3541(5) 0.5634(4) 0.8289(4) 0.0328(11) Uani 1 1 d . . . . .
N4 N 0.1881(5) 0.3838(5) 0.1739(4) 0.0283(12) Uiso 1 1 d D . . . .
C4 C 0.2988(7) 0.9619(6) 0.3624(5) 0.0284(15) Uani 1 1 d . . . . .
H4 H 0.281552 0.983134 0.306400 0.034 Uiso 1 1 calc R U . . .
O5 O 0.4279(4) 0.1976(4) 0.2617(3) 0.0206(9) Uani 1 1 d . . . . .
N5 N 0.4590(11) 0.6651(7) 0.2091(7) 0.061(3) Uani 1 1 d . . . . .
C5 C 0.3297(7) 1.0370(6) 0.4559(5) 0.0284(15) Uani 1 1 d . . . . .
H5 H 0.335083 1.117145 0.471177 0.034 Uiso 1 1 calc R U . . .
O6 O 0.4186(4) 0.3495(4) 0.4071(3) 0.0184(9) Uani 1 1 d . . . . .
C6 C 0.3557(6) 0.9994(6) 0.5364(5) 0.0240(13) Uani 1 1 d . . . . .
H6 H 0.378727 1.057721 0.604313 0.029 Uiso 1 1 calc R U . . .
C7 C 0.3504(6) 0.8867(5) 0.5244(5) 0.0194(12) Uani 1 1 d . . . . .
C8 C 0.2514(6) 0.8008(6) 0.6390(5) 0.0232(13) Uani 1 1 d . . . . .
H8A H 0.197329 0.725255 0.581064 0.028 Uiso 1 1 calc R U . . .
H8B H 0.206442 0.857966 0.647500 0.028 Uiso 1 1 calc R U . . .
O9 O 0.3902(11) 0.6932(7) 0.1529(6) 0.087(3) Uani 1 1 d . . . . .
C9 C 0.2690(6) 0.7768(6) 0.7356(5) 0.0231(13) Uani 1 1 d . . . . .
O10 O 0.4374(7) 0.5628(5) 0.2084(5) 0.0545(18) Uani 1 1 d . . . . .
C10 C 0.2522(6) 0.8479(6) 0.8188(5) 0.0242(13) Uani 1 1 d . . . . .
H10 H 0.229595 0.914320 0.819643 0.029 Uiso 1 1 calc R U . . .
O11 O 0.5512(11) 0.7407(7) 0.2671(8) 0.098(3) Uani 1 1 d . . . . .
C11 C 0.2685(6) 0.8237(6) 0.9072(5) 0.0258(14) Uani 1 1 d . . . . .
H11 H 0.255988 0.876496 0.966693 0.031 Uiso 1 1 calc R U . . .
C12 C 0.3015(7) 0.7283(6) 0.9148(5) 0.0265(14) Uani 1 1 d . . . . .
H12 H 0.310529 0.716114 0.976351 0.032 Uiso 1 1 calc R U . . .
C13 C 0.3189(6) 0.6578(6) 0.8326(5) 0.0257(14) Uani 1 1 d . . . . .
C14 C 0.3005(6) 0.6815(5) 0.7432(5) 0.0209(13) Uani 1 1 d . . . . .
C15 C 0.3849(9) 0.5403(7) 0.9185(6) 0.0404(19) Uani 1 1 d . . . . .
H15A H 0.448984 0.612349 0.972416 0.061 Uiso 1 1 calc R U . . .
H15B H 0.417658 0.474803 0.901752 0.061 Uiso 1 1 calc R U . . .
H15C H 0.309137 0.518062 0.942384 0.061 Uiso 1 1 calc R U . . .
C16 C 0.3698(6) 0.2668(5) 0.2437(4) 0.0195(12) Uani 1 1 d . . . . .
C17 C 0.3212(6) 0.2573(5) 0.1402(5) 0.0238(13) Uani 1 1 d . . . . .
C18 C 0.3619(7) 0.1885(6) 0.0692(5) 0.0281(14) Uani 1 1 d . . . . .
H18 H 0.412052 0.146625 0.086456 0.034 Uiso 1 1 calc R U . . .
C19 C 0.3298(8) 0.1793(7) -0.0291(5) 0.0386(18) Uani 1 1 d . . . . .
H19 H 0.358322 0.129524 -0.079368 0.046 Uiso 1 1 calc R U . . .
C20 C 0.2574(9) 0.2394(7) -0.0595(5) 0.044(2) Uani 1 1 d . . . . .
H20 H 0.239665 0.232640 -0.128025 0.053 Uiso 1 1 calc R U . . .
C21 C 0.2143(9) 0.3054(7) 0.0095(6) 0.0411(19) Uani 1 1 d . . . . .
H21 H 0.162684 0.345335 -0.009128 0.049 Uiso 1 1 calc R U . . .
C22 C 0.2448(7) 0.3160(6) 0.1080(5) 0.0276(15) Uani 1 1 d . . . . .
O32 O 0.3870(7) 0.4334(5) 0.6298(6) 0.0569(18) Uani 1 1 d D . . . .
H32 H 0.413910 0.490218 0.698557 0.068 Uiso 1 1 calc R U . . .
C46 C 0.2911(14) 0.3231(11) 0.6090(14) 0.149(9) Uani 1 1 d D . . . .
H46A H 0.223099 0.338582 0.639558 0.223 Uiso 1 1 calc R U . . .
H46B H 0.326271 0.276236 0.638203 0.223 Uiso 1 1 calc R U . . .
H46C H 0.257675 0.278523 0.535005 0.223 Uiso 1 1 calc R U . . .
O7A O 0.0407(10) 0.2154(10) 0.4560(8) 0.038(2) Uiso 0.5 1 d . . P A 1
O8A O 0.0848(12) 0.3685(10) 0.3567(9) 0.024(3) Uiso 0.5 1 d . . P A 1
H8A1 H 0.124845 0.406633 0.326655 0.037 Uiso 0.5 1 calc R U P A 1
C23A C 0.0626(13) 0.3188(13) 0.1587(12) 0.020(3) Uiso 0.5 1 d D . P A 1
H23B H 0.021254 0.278060 0.084593 0.024 Uiso 0.5 1 calc R U P A 1
H23A H 0.019476 0.373451 0.190671 0.024 Uiso 0.5 1 calc R U P A 1
C24A C 0.0507(13) 0.2258(14) 0.2052(14) 0.026(4) Uiso 0.5 1 d . . P A 1
C25A C 0.0295(12) 0.1123(14) 0.1536(14) 0.030(4) Uiso 0.5 1 d . . P A 1
H25A H 0.024975 0.083879 0.082670 0.036 Uiso 0.5 1 calc R U P A 1
C26A C 0.0130(14) 0.0293(17) 0.2035(15) 0.038(4) Uiso 0.5 1 d . . P A 1
H26A H -0.002098 -0.051745 0.161897 0.046 Uiso 0.5 1 calc R U P A 1
C27A C 0.0172(17) 0.0567(15) 0.3054(15) 0.038(4) Uiso 0.5 1 d . . P A 1
H27A H 0.006398 -0.000443 0.335050 0.046 Uiso 0.5 1 calc R U P A 1
C28A C 0.0379(15) 0.1709(13) 0.3573(12) 0.030(3) Uiso 0.5 1 d . . P A 1
C29A C 0.0590(14) 0.2548(13) 0.3067(13) 0.022(3) Uiso 0.5 1 d . . P A 1
C30A C 0.0068(18) 0.1363(17) 0.5122(14) 0.046(4) Uiso 0.5 1 d . . P A 1
H30A H -0.075050 0.072847 0.474323 0.069 Uiso 0.5 1 calc R U P A 1
H30B H 0.002036 0.183690 0.580291 0.069 Uiso 0.5 1 calc R U P A 1
H30C H 0.071160 0.100716 0.518619 0.069 Uiso 0.5 1 calc R U P A 1
O7B O 0.1350(13) 0.2295(12) 0.4881(10) 0.054(3) Uiso 0.5 1 d . . P A 2
O8B O 0.1150(13) 0.3699(11) 0.3786(11) 0.034(3) Uiso 0.5 1 d . . P A 2
H8B1 H 0.103889 0.389543 0.437695 0.051 Uiso 0.5 1 calc R U P A 2
C23B C 0.0505(15) 0.3006(15) 0.1797(13) 0.029(4) Uiso 0.5 1 d D . P A 2
H23C H 0.008659 0.354503 0.215369 0.034 Uiso 0.5 1 calc R U P A 2
H23D H -0.003059 0.252011 0.109182 0.034 Uiso 0.5 1 calc R U P A 2
C24B C 0.0560(13) 0.2173(13) 0.2329(14) 0.023(4) Uiso 0.5 1 d . . P A 2
C25B C 0.0264(11) 0.0997(13) 0.1846(13) 0.024(3) Uiso 0.5 1 d . . P A 2
H25B H 0.003648 0.064125 0.112035 0.029 Uiso 0.5 1 calc R U P A 2
C26B C 0.0285(13) 0.0267(14) 0.2406(15) 0.030(3) Uiso 0.5 1 d . . P A 2
H26B H 0.005274 -0.056668 0.202431 0.036 Uiso 0.5 1 calc R U P A 2
C27B C 0.0611(19) 0.0670(17) 0.3441(16) 0.046(4) Uiso 0.5 1 d . . P A 2
H27B H 0.061579 0.016316 0.379413 0.055 Uiso 0.5 1 calc R U P A 2
C28B C 0.0909(19) 0.1800(17) 0.3891(15) 0.048(4) Uiso 0.5 1 d . . P A 2
C29B C 0.0831(17) 0.2548(15) 0.3358(15) 0.034(4) Uiso 0.5 1 d . . P A 2
C30B C 0.088(3) 0.159(3) 0.548(2) 0.084(7) Uiso 0.5 1 d . . P A 2
H30D H 0.025734 0.080986 0.501346 0.125 Uiso 0.5 1 calc R U P A 2
H30E H 0.049672 0.201972 0.597122 0.125 Uiso 0.5 1 calc R U P A 2
H30F H 0.159020 0.147362 0.584301 0.125 Uiso 0.5 1 calc R U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O6 1.797(4) . ?
Cu1 O6 1.797(4) 2_666 ?
Cu1 O2 1.932(4) . ?
Cu1 O2 1.932(4) 2_666 ?
Cu1 O32 2.647(6) . ?
O1 C1 1.206(7) . ?
O1 Cu3 1.962(4) . ?
N1 C7 1.506(8) . ?
N1 C8 1.522(8) . ?
N1 Cu2 2.004(5) . ?
N1 H1H 1.0000 . ?
C1 N2 1.328(8) . ?
C1 C2 1.454(9) . ?
Cu2 N2 1.815(5) . ?
Cu2 O5 1.857(4) 2_666 ?
Cu2 O6 1.927(4) 2_666 ?
O2 N2 1.355(7) . ?
O2 Cu3 1.811(4) . ?
C2 C7 1.310(9) . ?
C2 C3 1.429(9) . ?
Cu3 N4 1.894(6) . ?
Cu3 N3 1.951(5) . ?
O3 C14 1.294(7) . ?
O3 H3H 0.8400 . ?
N3 C16 1.235(8) . ?
N3 O6 1.408(6) . ?
C3 C4 1.371(9) . ?
C3 H3 0.9500 . ?
O4 C13 1.360(8) . ?
O4 C15 1.442(8) . ?
N4 C23A 1.384(16) . ?
N4 C22 1.414(9) . ?
N4 C23B 1.661(19) . ?
C4 C5 1.286(10) . ?
C4 H4 0.9500 . ?
O5 C16 1.316(8) . ?
N5 O11 1.173(13) . ?
N5 O10 1.252(10) . ?
N5 O9 1.262(12) . ?
C5 C6 1.426(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.368(9) . ?
C6 H6 0.9500 . ?
C8 C9 1.524(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.310(9) . ?
C9 C14 1.396(9) . ?
C10 C11 1.411(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.405(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.301(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.423(9) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.472(9) . ?
C17 C18 1.336(9) . ?
C17 C22 1.429(10) . ?
C18 C19 1.372(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.400(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.318(12) . ?
C20 H20 0.9500 . ?
C21 C22 1.366(10) . ?
C21 H21 0.9500 . ?
O32 C46 1.420(10) . ?
O32 H32 0.9500 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
O7A C28A 1.331(19) . ?
O7A C30A 1.50(2) . ?
O8A C29A 1.300(18) . ?
O8A H8A1 0.8400 . ?
C23A C24A 1.53(2) . ?
C23A H23B 0.9900 . ?
C23A H23A 0.9900 . ?
C24A C25A 1.31(2) . ?
C24A C29A 1.36(2) . ?
C25A C26A 1.45(3) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.38(3) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.32(2) . ?
C27A H27A 0.9500 . ?
C28A C29A 1.47(2) . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
O7B C28B 1.30(2) . ?
O7B C30B 1.49(3) . ?
O8B C29B 1.30(2) . ?
O8B H8B1 0.8400 . ?
C23B C24B 1.52(2) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C24B C25B 1.33(2) . ?
C24B C29B 1.35(3) . ?
C25B C26B 1.43(2) . ?
C25B H25B 0.9500 . ?
C26B C27B 1.36(3) . ?
C26B H26B 0.9500 . ?
C27B C28B 1.28(3) . ?
C27B H27B 0.9500 . ?
C28B C29B 1.43(3) . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 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
O6 Cu1 O6 180.0(3) . 2_666 ?
O6 Cu1 O2 88.77(18) . . ?
O6 Cu1 O2 91.23(18) 2_666 . ?
O6 Cu1 O2 91.23(18) . 2_666 ?
O6 Cu1 O2 88.77(18) 2_666 2_666 ?
O2 Cu1 O2 180.0(2) . 2_666 ?
O6 Cu1 O32 87.2(2) . . ?
O6 Cu1 O32 92.8(2) 2_666 . ?
O2 Cu1 O32 95.5(2) . . ?
O2 Cu1 O32 84.5(2) 2_666 . ?
C1 O1 Cu3 105.6(4) . . ?
C7 N1 C8 111.3(5) . . ?
C7 N1 Cu2 118.2(4) . . ?
C8 N1 Cu2 110.4(4) . . ?
C7 N1 H1H 105.3 . . ?
C8 N1 H1H 105.3 . . ?
Cu2 N1 H1H 105.3 . . ?
O1 C1 N2 122.4(6) . . ?
O1 C1 C2 115.2(6) . . ?
N2 C1 C2 122.4(5) . . ?
N2 Cu2 O5 169.1(2) . 2_666 ?
N2 Cu2 O6 94.0(2) . 2_666 ?
O5 Cu2 O6 77.04(17) 2_666 2_666 ?
N2 Cu2 N1 85.1(2) . . ?
O5 Cu2 N1 104.31(19) 2_666 . ?
O6 Cu2 N1 175.1(2) 2_666 . ?
N2 O2 Cu3 107.6(4) . . ?
N2 O2 Cu1 120.2(4) . . ?
Cu3 O2 Cu1 119.9(2) . . ?
C1 N2 O2 116.2(5) . . ?
C1 N2 Cu2 133.7(4) . . ?
O2 N2 Cu2 109.5(4) . . ?
C7 C2 C3 118.2(6) . . ?
C7 C2 C1 119.4(6) . . ?
C3 C2 C1 122.3(5) . . ?
O2 Cu3 N4 175.4(2) . . ?
O2 Cu3 N3 84.35(19) . . ?
N4 Cu3 N3 96.5(2) . . ?
O2 Cu3 O1 86.20(18) . . ?
N4 Cu3 O1 93.7(2) . . ?
N3 Cu3 O1 166.5(2) . . ?
C14 O3 H3H 109.5 . . ?
C16 N3 O6 108.1(5) . . ?
C16 N3 Cu3 129.9(4) . . ?
O6 N3 Cu3 122.0(3) . . ?
C4 C3 C2 126.4(6) . . ?
C4 C3 H3 116.8 . . ?
C2 C3 H3 116.8 . . ?
C13 O4 C15 122.1(5) . . ?
C23A N4 C22 111.3(8) . . ?
C22 N4 C23B 112.8(7) . . ?
C23A N4 Cu3 116.6(8) . . ?
C22 N4 Cu3 114.3(4) . . ?
C23B N4 Cu3 105.2(7) . . ?
C5 C4 C3 114.8(6) . . ?
C5 C4 H4 122.6 . . ?
C3 C4 H4 122.6 . . ?
C16 O5 Cu2 115.1(4) . 2_666 ?
O11 N5 O10 116.7(11) . . ?
O11 N5 O9 117.8(9) . . ?
O10 N5 O9 125.5(11) . . ?
C4 C5 C6 119.8(6) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
N3 O6 Cu1 110.4(3) . . ?
N3 O6 Cu2 115.0(3) . 2_666 ?
Cu1 O6 Cu2 111.8(2) . 2_666 ?
C7 C6 C5 125.7(6) . . ?
C7 C6 H6 117.1 . . ?
C5 C6 H6 117.1 . . ?
C2 C7 C6 115.2(6) . . ?
C2 C7 N1 121.4(5) . . ?
C6 C7 N1 123.4(5) . . ?
N1 C8 C9 114.3(5) . . ?
N1 C8 H8A 108.7 . . ?
C9 C8 H8A 108.7 . . ?
N1 C8 H8B 108.7 . . ?
C9 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10 C9 C14 115.5(6) . . ?
C10 C9 C8 119.5(6) . . ?
C14 C9 C8 124.9(6) . . ?
C9 C10 C11 118.6(6) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C12 C11 C10 125.6(6) . . ?
C12 C11 H11 117.2 . . ?
C10 C11 H11 117.2 . . ?
C13 C12 C11 116.1(6) . . ?
C13 C12 H12 121.9 . . ?
C11 C12 H12 121.9 . . ?
C12 C13 O4 122.8(6) . . ?
C12 C13 C14 118.0(6) . . ?
O4 C13 C14 119.1(6) . . ?
O3 C14 C9 114.4(6) . . ?
O3 C14 C13 119.5(6) . . ?
C9 C14 C13 126.1(6) . . ?
O4 C15 H15A 109.5 . . ?
O4 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O4 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 O5 120.9(6) . . ?
N3 C16 C17 115.9(6) . . ?
O5 C16 C17 123.0(5) . . ?
C18 C17 C22 117.3(6) . . ?
C18 C17 C16 113.3(6) . . ?
C22 C17 C16 129.3(6) . . ?
C17 C18 C19 118.6(7) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C18 C19 C20 123.6(7) . . ?
C18 C19 H19 118.2 . . ?
C20 C19 H19 118.2 . . ?
C21 C20 C19 118.2(7) . . ?
C21 C20 H20 120.9 . . ?
C19 C20 H20 120.9 . . ?
C20 C21 C22 119.3(7) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
C21 C22 N4 114.3(6) . . ?
C21 C22 C17 122.9(7) . . ?
N4 C22 C17 122.7(6) . . ?
C46 O32 Cu1 127.9(9) . . ?
C46 O32 H32 116.1 . . ?
Cu1 O32 H32 116.1 . . ?
O32 C46 H46A 109.5 . . ?
O32 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
O32 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C28A O7A C30A 121.6(12) . . ?
C29A O8A H8A1 109.5 . . ?
N4 C23A C24A 110.4(11) . . ?
N4 C23A H23B 109.6 . . ?
C24A C23A H23B 109.6 . . ?
N4 C23A H23A 109.6 . . ?
C24A C23A H23A 109.6 . . ?
H23B C23A H23A 108.1 . . ?
C25A C24A C29A 113.2(18) . . ?
C25A C24A C23A 124.9(17) . . ?
C29A C24A C23A 121.9(14) . . ?
C24A C25A C26A 121.0(18) . . ?
C24A C25A H25A 119.5 . . ?
C26A C25A H25A 119.5 . . ?
C27A C26A C25A 126.4(17) . . ?
C27A C26A H26A 116.8 . . ?
C25A C26A H26A 116.8 . . ?
C28A C27A C26A 112.7(16) . . ?
C28A C27A H27A 123.6 . . ?
C26A C27A H27A 123.6 . . ?
C27A C28A O7A 122.5(15) . . ?
C27A C28A C29A 120.3(15) . . ?
O7A C28A C29A 117.2(13) . . ?
O8A C29A C24A 112.0(14) . . ?
O8A C29A C28A 121.7(15) . . ?
C24A C29A C28A 126.2(15) . . ?
O7A C30A H30A 109.5 . . ?
O7A C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
O7A C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C28B O7B C30B 118.1(17) . . ?
C29B O8B H8B1 109.5 . . ?
C24B C23B N4 116.0(11) . . ?
C24B C23B H23C 108.3 . . ?
N4 C23B H23C 108.3 . . ?
C24B C23B H23D 108.3 . . ?
N4 C23B H23D 108.3 . . ?
H23C C23B H23D 107.4 . . ?
C25B C24B C29B 113.0(17) . . ?
C25B C24B C23B 124.3(17) . . ?
C29B C24B C23B 122.5(15) . . ?
C24B C25B C26B 120.8(16) . . ?
C24B C25B H25B 119.6 . . ?
C26B C25B H25B 119.6 . . ?
C27B C26B C25B 125.2(16) . . ?
C27B C26B H26B 117.4 . . ?
C25B C26B H26B 117.4 . . ?
C28B C27B C26B 113.1(19) . . ?
C28B C27B H27B 123.4 . . ?
C26B C27B H27B 123.4 . . ?
C27B C28B O7B 118.1(19) . . ?
C27B C28B C29B 123(2) . . ?
O7B C28B C29B 118.6(17) . . ?
O8B C29B C24B 110.3(17) . . ?
O8B C29B C28B 124.9(18) . . ?
C24B C29B C28B 124.4(16) . . ?
O7B C30B H30D 109.5 . . ?
O7B C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
O7B C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?

_refine_diff_density_max         7.229
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.261



# SQUEEZE RESULTS (Version = 241018)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 1.000 299 103 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_bfm82c
_database_code_depnum_ccdc_archive 'CCDC 1907531'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;Bangor University 
United Kingdom
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H11 Cu N3 O7 (H2 O)'
_chemical_formula_sum            'C8 H13 Cu N3 O8'
_chemical_formula_weight         342.75

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   12.2451(4)
_cell_length_b                   10.0658(2)
_cell_length_c                   10.9339(3)
_cell_angle_alpha                90
_cell_angle_beta                 114.906(4)
_cell_angle_gamma                90
_cell_volume                     1222.34(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293.0(2)
_cell_measurement_reflns_used    13558
_cell_measurement_theta_min      2.7050
_cell_measurement_theta_max      31.9300

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_F_000             700
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.832
_shelx_estimated_absorpt_T_min   0.838
_shelx_estimated_absorpt_T_max   0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68995
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
crysalispro 1.171.39.30d (rigaku oxford diffraction, 2017) 
empirical absorption correction using spherical harmonics, 
 implemented in scale3 abspack scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xtalab afc12 (rcd3): kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27186
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.834
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2801
_reflns_number_gt                2674
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'crysalispro 1.171.39.30d (rigaku od, 2017)'
_computing_cell_refinement       'crysalispro 1.171.39.30d (rigaku od, 2017)'
_computing_data_reduction        'crysalispro 1.171.39.30d (rigaku od, 2017)'
_computing_structure_solution    
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0256P)²+1.1862P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2801
_refine_ls_number_parameters     206
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0555
_refine_ls_wR_factor_gt          0.0547
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.65079(2) 0.17027(2) 0.09475(2) 0.00974(6) Uani 1 1 d . . . . .
O1 O 0.81913(9) 0.13058(11) 0.19232(11) 0.0129(2) Uani 1 1 d . . . . .
N1 N 0.74337(11) -0.04375(12) 0.25566(12) 0.0109(2) Uani 1 1 d . . . . .
H1 H 0.752156 -0.119296 0.299322 0.013 Uiso 1 1 calc R U . . .
C1 C 0.83663(13) 0.02044(14) 0.25551(14) 0.0095(3) Uani 1 1 d . . . . .
O2 O 0.63076(9) 0.01173(11) 0.18467(11) 0.0126(2) Uani 1 1 d . . . . .
N2 N 1.32128(11) -0.16198(13) 0.49132(13) 0.0117(2) Uani 1 1 d D . . . .
C2 C 0.96059(12) -0.03148(14) 0.32196(14) 0.0092(3) Uani 1 1 d . . . . .
O3 O 0.90759(9) -0.20666(11) 0.42869(11) 0.0129(2) Uani 1 1 d . . . . .
N3 N 0.62086(12) 0.42824(14) 0.27737(14) 0.0167(3) Uani 1 1 d . . . . .
C3 C 1.04814(13) 0.03603(14) 0.29608(15) 0.0113(3) Uani 1 1 d . . . . .
H3 H 1.025187 0.111264 0.238266 0.014 Uiso 1 1 calc R U . . .
O4 O 0.47895(10) 0.18622(12) -0.02507(12) 0.0145(2) Uani 1 1 d D . . . .
C4 C 1.16741(13) -0.00352(15) 0.35224(15) 0.0123(3) Uani 1 1 d . . . . .
H4 H 1.225600 0.043407 0.332899 0.015 Uiso 1 1 calc R U . . .
O5 O 0.60957(11) 0.30407(12) 0.25680(12) 0.0199(2) Uani 1 1 d . . . . .
C5 C 1.20049(13) -0.11270(14) 0.43713(14) 0.0106(3) Uani 1 1 d . . . . .
O6 O 0.67351(13) 0.46964(13) 0.39576(13) 0.0283(3) Uani 1 1 d . . . . .
C6 C 1.11580(13) -0.18173(14) 0.46666(14) 0.0105(3) Uani 1 1 d . . . . .
H6 H 1.139932 -0.255342 0.526573 0.013 Uiso 1 1 calc R U . . .
O7 O 0.57936(11) 0.50626(13) 0.18076(13) 0.0249(3) Uani 1 1 d . . . . .
C7 C 0.99617(13) -0.14237(14) 0.40811(14) 0.0094(3) Uani 1 1 d . . . . .
O8 O 0.35662(12) 0.25297(13) 0.13138(15) 0.0243(3) Uani 1 1 d . . . . .
C8 C 0.94162(15) -0.31323(15) 0.52476(17) 0.0165(3) Uani 1 1 d . . . . .
H8A H 0.974611 -0.386675 0.491951 0.025 Uiso 1 1 calc R U . . .
H8B H 0.870777 -0.344110 0.536589 0.025 Uiso 1 1 calc R U . . .
H8C H 1.002727 -0.281698 0.611359 0.025 Uiso 1 1 calc R U . . .
H2A H 1.3705(18) -0.101(2) 0.488(2) 0.017(5) Uiso 1 1 d D . . . .
H4A H 0.437(2) 0.214(2) 0.009(2) 0.031(6) Uiso 1 1 d D . . . .
H2B H 1.3425(18) -0.188(2) 0.572(2) 0.015(5) Uiso 1 1 d D . . . .
H4B H 0.447(2) 0.119(2) -0.070(2) 0.032(6) Uiso 1 1 d D . . . .
H8E H 0.418(3) 0.270(3) 0.190(3) 0.050(9) Uiso 1 1 d . . . . .
H8D H 0.347(3) 0.166(3) 0.157(3) 0.055(9) 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
Cu1 O1 1.9221(10) . ?
Cu1 O2 1.9433(11) . ?
Cu1 O4 1.9617(11) . ?
Cu1 N2 2.0311(13) 2_755 ?
Cu1 O5 2.4416(12) . ?
O1 C1 1.2757(18) . ?
N1 C1 1.3127(19) . ?
N1 O2 1.3836(15) . ?
N1 H1 0.8800 . ?
C1 C2 1.4751(19) . ?
N2 C5 1.4306(18) . ?
N2 H2A 0.87(2) . ?
N2 H2B 0.85(2) . ?
C2 C3 1.395(2) . ?
C2 C7 1.406(2) . ?
O3 C7 1.3606(17) . ?
O3 C8 1.4350(18) . ?
N3 O7 1.2405(18) . ?
N3 O6 1.2498(19) . ?
N3 O5 1.2671(18) . ?
C3 C4 1.383(2) . ?
C3 H3 0.9500 . ?
O4 H4A 0.80(2) . ?
O4 H4B 0.84(2) . ?
C4 C5 1.384(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.395(2) . ?
C6 C7 1.387(2) . ?
C6 H6 0.9500 . ?
O8 H8E 0.77(3) . ?
O8 H8D 0.94(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O2 83.27(4) . . ?
O1 Cu1 O4 170.30(5) . . ?
O2 Cu1 O4 94.40(5) . . ?
O1 Cu1 N2 94.56(5) . 2_755 ?
O2 Cu1 N2 177.33(5) . 2_755 ?
O4 Cu1 N2 88.00(5) . 2_755 ?
O1 Cu1 O5 102.30(5) . . ?
O2 Cu1 O5 88.69(4) . . ?
O4 Cu1 O5 87.02(5) . . ?
N2 Cu1 O5 90.25(5) 2_755 . ?
C1 O1 Cu1 112.18(9) . . ?
C1 N1 O2 117.56(12) . . ?
C1 N1 H1 121.2 . . ?
O2 N1 H1 121.2 . . ?
O1 C1 N1 118.72(13) . . ?
O1 C1 C2 118.55(13) . . ?
N1 C1 C2 122.70(13) . . ?
N1 O2 Cu1 107.88(8) . . ?
C5 N2 Cu1 116.29(9) . 2_745 ?
C5 N2 H2A 110.6(13) . . ?
Cu1 N2 H2A 108.3(13) 2_745 . ?
C5 N2 H2B 110.5(14) . . ?
Cu1 N2 H2B 100.6(14) 2_745 . ?
H2A N2 H2B 110.1(18) . . ?
C3 C2 C7 118.34(13) . . ?
C3 C2 C1 116.53(13) . . ?
C7 C2 C1 125.13(13) . . ?
C7 O3 C8 118.07(12) . . ?
O7 N3 O6 121.24(14) . . ?
O7 N3 O5 119.89(14) . . ?
O6 N3 O5 118.87(14) . . ?
C4 C3 C2 121.85(14) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
Cu1 O4 H4A 115.6(17) . . ?
Cu1 O4 H4B 115.8(16) . . ?
H4A O4 H4B 109(2) . . ?
C3 C4 C5 118.83(13) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N3 O5 Cu1 129.23(10) . . ?
C4 C5 C6 120.97(13) . . ?
C4 C5 N2 120.83(13) . . ?
C6 C5 N2 118.12(13) . . ?
C7 C6 C5 119.66(13) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
O3 C7 C6 123.27(13) . . ?
O3 C7 C2 116.40(12) . . ?
C6 C7 C2 120.34(13) . . ?
H8E O8 H8D 99(3) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

_refine_diff_density_max         0.445
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.061


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
####################################################################### 
# 
# 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_bfm93a
_database_code_depnum_ccdc_archive 'CCDC 1907530'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;Bangor University 
United Kingdom
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT971_bfm93a              
;
PROBLEM: Check Calcd Resid. Dens.  1.00A   From O2              3.19 eA-3
RESPONSE: Comment from NCS crystallographer: ?This structure is commensurate/modulated, so this peak is not going to go away so easily. What you can say is that the structure is 5-fold modulated along b, and possibly 2-fold along a as well, and that you see the average structure over many cells??But sorting out the modulation is going to be very time-consuming.?
;
# Added during the CSD deposition process: Monday 20 May 2019 04:56 PM
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Zn1]n'
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H18 N4 O4 Zn1 (C2 H8 O2)'
_chemical_formula_sum            'C18 H26 N4 O6 Zn'
_chemical_formula_weight         459.80
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           27
_space_group_name_H-M_alt        'P c c 2'
_space_group_name_Hall           'P 2 -2c'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z+1/2'
'-x, y, z+1/2'
_cell_length_a                   14.3459(4)
_cell_length_b                   10.8600(3)
_cell_length_c                   6.3652(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     991.68(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    9998
_cell_measurement_theta_min      2.3250
_cell_measurement_theta_max      31.6110
_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_F_000             480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    1.282
_shelx_estimated_absorpt_T_min   0.883
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.57837
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
crysalispro 1.171.39.30d (rigaku oxford diffraction, 2017)
empirical absorption correction using spherical harmonics,
 implemented in scale3 abspack scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xtalab afc12 (rcd3): kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17587
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.875
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             1787
_reflns_number_gt                1758
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.791
_reflns_Friedel_fraction_max     0.974
_reflns_Friedel_fraction_full    0.974
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'crysalispro 1.171.39.30d (rigaku od, 2017)'
_computing_cell_refinement       'crysalispro 1.171.39.30d (rigaku od, 2017)'
_computing_data_reduction        'crysalispro 1.171.39.30d (rigaku od, 2017)'
_computing_structure_solution    
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1064P)²+0.1036P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 754 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         1787
_refine_ls_number_parameters     135
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0457
_refine_ls_wR_factor_ref         0.1165
_refine_ls_wR_factor_gt          0.1160
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.500000 0.500000 0.4452(3) 0.0078(3) Uani 1 2 d S T P . .
O1 O 0.49162(17) 0.3731(3) 0.6990(13) 0.0094(6) Uani 1 1 d . . . . .
N1 N 0.4070(2) 0.3108(3) 0.6772(6) 0.0105(7) Uani 1 1 d . . . . .
H1 H 0.397467 0.241517 0.745514 0.013 Uiso 1 1 calc R U . . .
C1 C 0.3414(3) 0.3558(3) 0.5544(6) 0.0097(7) Uani 1 1 d . . . . .
O2 O 0.35654(19) 0.4526(3) 0.4487(5) 0.0115(6) Uani 1 1 d . . . . .
N2 N 0.2085(2) 0.3701(4) 0.2066(7) 0.0182(8) Uani 1 1 d . . . . .
H2 H 0.265793 0.397228 0.188479 0.022 Uiso 1 1 calc R U . . .
C2 C 0.2525(3) 0.2848(4) 0.5481(7) 0.0137(8) Uani 1 1 d . . . . .
O3 O 0.4155(2) 0.1700(3) 0.0432(5) 0.0234(8) Uani 1 1 d . . . . .
H3 H 0.437879 0.230813 0.107278 0.035 Uiso 1 1 calc R U . . .
C3 C 0.1894(3) 0.2986(4) 0.3765(7) 0.0143(8) Uani 1 1 d . . . . .
C4 C 0.1053(3) 0.2304(4) 0.3848(8) 0.0169(10) Uani 1 1 d . . . . .
H4 H 0.060056 0.241419 0.277480 0.020 Uiso 1 1 calc R U . . .
C5 C 0.0880(3) 0.1491(4) 0.5439(9) 0.0208(10) Uani 1 1 d . . . . .
H5 H 0.032029 0.102268 0.541457 0.025 Uiso 1 1 calc R U . . .
C6 C 0.1500(3) 0.1332(4) 0.7089(9) 0.0225(10) Uani 1 1 d . . . . .
H6 H 0.137428 0.075891 0.818110 0.027 Uiso 1 1 calc R U . . .
C7 C 0.2310(3) 0.2033(4) 0.7101(8) 0.0177(9) Uani 1 1 d . . . . .
H7 H 0.272952 0.195501 0.824794 0.021 Uiso 1 1 calc R U . . .
C8 C 0.1380(3) 0.4030(4) 0.0549(8) 0.0218(10) Uani 1 1 d . . . . .
H8C H 0.165612 0.455089 -0.054277 0.033 Uiso 1 1 calc R U . . .
H8B H 0.087744 0.448109 0.125362 0.033 Uiso 1 1 calc R U . . .
H8A H 0.112666 0.328094 -0.009279 0.033 Uiso 1 1 calc R U . . .
C9 C 0.3808(4) 0.0830(4) 0.1914(9) 0.0273(10) Uani 1 1 d . . . . .
H9B H 0.383438 0.000185 0.130477 0.041 Uiso 1 1 calc R U . . .
H9A H 0.316131 0.103279 0.226712 0.041 Uiso 1 1 calc R U . . .
H9C H 0.419055 0.085658 0.318895 0.041 Uiso 1 1 calc R U . . .
_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.091(6) 4_654 ?
Zn1 O1 2.091(6) 3_564 ?
Zn1 O2 2.122(3) . ?
Zn1 O2 2.122(3) 2_665 ?
Zn1 O1 2.127(6) 2_665 ?
Zn1 O1 2.127(6) . ?
O1 N1 1.396(4) . ?
N1 C1 1.317(6) . ?
N1 H1 0.8800 . ?
C1 O2 1.266(5) . ?
C1 C2 1.491(5) . ?
N2 C3 1.360(6) . ?
N2 C8 1.444(6) . ?
N2 H2 0.8800 . ?
C2 C7 1.393(7) . ?
C2 C3 1.426(6) . ?
O3 C9 1.425(6) . ?
O3 H3 0.8400 . ?
C3 C4 1.416(6) . ?
C4 C5 1.367(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8C 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9C 0.9800 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 82.9(3) 4_654 3_564 ?
O1 Zn1 O2 84.47(13) 4_654 . ?
O1 Zn1 O2 96.46(11) 3_564 . ?
O1 Zn1 O2 96.46(11) 4_654 2_665 ?
O1 Zn1 O2 84.47(13) 3_564 2_665 ?
O2 Zn1 O2 178.8(2) . 2_665 ?
O1 Zn1 O1 173.41(13) 4_654 2_665 ?
O1 Zn1 O1 98.35(13) 3_564 2_665 ?
O2 Zn1 O1 101.77(11) . 2_665 ?
O2 Zn1 O1 77.27(13) 2_665 2_665 ?
O1 Zn1 O1 98.35(13) 4_654 . ?
O1 Zn1 O1 173.41(13) 3_564 . ?
O2 Zn1 O1 77.27(13) . . ?
O2 Zn1 O1 101.77(11) 2_665 . ?
O1 Zn1 O1 81.2(3) 2_665 . ?
N1 O1 Zn1 116.3(4) . 3_565 ?
N1 O1 Zn1 106.7(4) . . ?
Zn1 O1 Zn1 97.97(13) 3_565 . ?
C1 N1 O1 120.0(4) . . ?
C1 N1 H1 120.0 . . ?
O1 N1 H1 120.0 . . ?
O2 C1 N1 120.0(3) . . ?
O2 C1 C2 124.2(4) . . ?
N1 C1 C2 115.8(4) . . ?
C1 O2 Zn1 112.0(2) . . ?
C3 N2 C8 122.1(4) . . ?
C3 N2 H2 118.9 . . ?
C8 N2 H2 118.9 . . ?
C7 C2 C3 119.5(4) . . ?
C7 C2 C1 119.9(4) . . ?
C3 C2 C1 120.6(4) . . ?
C9 O3 H3 109.5 . . ?
N2 C3 C4 120.0(4) . . ?
N2 C3 C2 122.7(4) . . ?
C4 C3 C2 117.2(4) . . ?
C5 C4 C3 121.4(4) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 121.6(4) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
C5 C6 C7 118.2(5) . . ?
C5 C6 H6 120.9 . . ?
C7 C6 H6 120.9 . . ?
C6 C7 C2 121.9(5) . . ?
C6 C7 H7 119.0 . . ?
C2 C7 H7 119.0 . . ?
N2 C8 H8C 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8C C8 H8B 109.5 . . ?
N2 C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
O3 C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
_refine_diff_density_max         3.252
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.119
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_chemical_properties_physical    Hygroscopic
_exptl_crystal_preparation       Luminescent
####################################################################### 
# 
# 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_bfm56d
_database_code_depnum_ccdc_archive 'CCDC 1907527'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;Bangor University 
United Kingdom
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Cu5].3H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'c32 H32 N10 O14 Cu5 (H6 O3)'
_chemical_formula_sum            'C32 H38 Cu5 N10 O17'
_chemical_formula_weight         1152.37

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3704(6)
_cell_length_b                   13.3009(7)
_cell_length_c                   14.8558(8)
_cell_angle_alpha                91.179(4)
_cell_angle_beta                 106.814(5)
_cell_angle_gamma                108.726(5)
_cell_volume                     2020.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    9598
_cell_measurement_theta_min      2.0930
_cell_measurement_theta_max      30.5300

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_F_000             1150
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    2.676
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
crysalispro 1.171.39.46 (rigaku oxford diffraction, 2018) 
empirical absorption correction using spherical harmonics, 
 implemented in scale3 abspack scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'rotating-anode x-ray tube'
_diffrn_measurement_device_type  'xtalab afc12 (rcd3): kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33372
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.991
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7391
_reflns_number_gt                6159
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'crysalispro 1.171.39.46 (rigaku od, 2018)'
_computing_cell_refinement       'crysalispro 1.171.39.46 (rigaku od, 2018)'
_computing_data_reduction        'crysalispro 1.171.39.46 (rigaku od, 2018)'
_computing_structure_solution    
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0584P)²+7.0773P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7391
_refine_ls_number_parameters     569
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1287
_refine_ls_wR_factor_gt          0.1211
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.500000 0.500000 0.000000 0.0122(2) Uani 1 2 d S . P . .
O1 O 0.6603(3) 0.5940(3) 0.0861(2) 0.0146(7) Uani 1 1 d . . . . .
N1 N 0.6921(4) 0.5707(3) 0.1796(3) 0.0147(9) Uani 1 1 d . . . . .
C1 C 0.7403(5) 0.6565(4) 0.2414(4) 0.0160(11) Uani 1 1 d . . . . .
Cu2 Cu 0.67350(6) 0.74104(5) 0.07951(4) 0.01447(16) Uani 1 1 d . . . . .
O2 O 0.7530(3) 0.7509(3) 0.2165(3) 0.0165(8) Uani 1 1 d . . . . .
N2 N 0.7746(4) 0.4535(4) 0.3152(3) 0.0172(10) Uani 1 1 d . . . . .
H2 H 0.756830 0.391979 0.350626 0.021 Uiso 1 1 calc R U . . .
C2 C 0.7819(5) 0.6419(4) 0.3432(4) 0.0151(11) Uani 1 1 d . . . . .
Cu3 Cu 0.37773(6) 0.57697(5) -0.19753(4) 0.01451(16) Uani 1 1 d . . . . .
O3 O 0.4629(3) 0.7277(3) -0.1983(2) 0.0170(8) Uani 1 1 d . . . . .
N3 N 0.6694(4) 0.8889(4) 0.0762(3) 0.0198(10) Uani 1 1 d . . . . .
H3A H 0.742209 0.933453 0.130154 0.024 Uiso 1 1 calc R U . . .
C3 C 0.8015(5) 0.7279(4) 0.4084(4) 0.0178(11) Uani 1 1 d . . . . .
H3 H 0.791986 0.790677 0.386429 0.021 Uiso 1 1 calc R U . . .
Cu4 Cu -0.12760(6) -0.25828(5) -0.04038(4) 0.01327(16) Uani 1 1 d . . . . .
O4 O 0.5307(3) 0.5978(3) -0.0918(2) 0.0141(7) Uani 1 1 d . . . . .
N4 N 0.5965(4) 0.7071(3) -0.0582(3) 0.0139(9) Uani 1 1 d . . . . .
C4 C 0.8346(5) 0.7213(5) 0.5046(4) 0.0214(12) Uani 1 1 d . . . . .
H4 H 0.846507 0.779038 0.546785 0.026 Uiso 1 1 calc R U . . .
Cu5 Cu 0.05754(6) -0.00945(5) 0.22791(4) 0.01329(16) Uani 1 1 d . . . . .
O5 O 0.4073(4) 0.6167(4) 0.0621(3) 0.0390(12) Uani 1 1 d . . . . .
N5 N 0.2979(5) 0.6166(4) 0.0080(4) 0.0294(12) Uani 1 1 d . . . . .
C5 C 0.8499(5) 0.6291(5) 0.5379(4) 0.0223(12) Uani 1 1 d . . . . .
H5 H 0.872492 0.624339 0.602650 0.027 Uiso 1 1 calc R U . . .
Cu6 Cu 0.000000 0.000000 0.000000 0.0125(2) Uani 1 2 d S . P . .
O6 O 0.2002(4) 0.5869(4) 0.0355(4) 0.0394(12) Uani 1 1 d . . . . .
N6 N 0.1828(4) 0.3895(3) 0.1306(3) 0.0159(9) Uani 1 1 d . . . . .
H6A H 0.215426 0.451465 0.098881 0.019 Uiso 1 1 calc R U . . .
C6 C 0.8314(5) 0.5432(4) 0.4745(4) 0.0198(12) Uani 1 1 d . . . . .
H6 H 0.842781 0.481245 0.497358 0.024 Uiso 1 1 calc R U . . .
O7 O 0.2883(4) 0.6481(4) -0.0732(3) 0.0348(11) Uani 1 1 d . . . . .
N7 N 0.1329(4) 0.1759(3) 0.1454(3) 0.0148(9) Uani 1 1 d . . . . .
C7 C 0.7964(5) 0.5482(4) 0.3778(4) 0.0178(11) Uani 1 1 d . . . . .
O8 O 0.0495(4) 0.0688(3) 0.1226(2) 0.0172(8) Uani 1 1 d . . . . .
N8 N 0.0385(4) -0.1059(3) 0.3280(3) 0.0162(9) Uani 1 1 d . . . . .
H8 H -0.055493 -0.145919 0.309962 0.019 Uiso 1 1 calc R U . . .
C8 C 0.8890(6) 0.4589(6) 0.2867(5) 0.0326(15) Uani 1 1 d . . . . .
H8A H 0.901035 0.511362 0.243731 0.049 Uiso 1 1 calc R U . . .
H8B H 0.875950 0.390209 0.255914 0.049 Uiso 1 1 calc R U . . .
H8C H 0.965018 0.478490 0.341730 0.049 Uiso 1 1 calc R U . . .
O9 O 0.1732(3) 0.1300(3) 0.2953(2) 0.0153(8) Uani 1 1 d . . . . .
N9 N -0.0192(4) -0.1381(3) 0.1382(3) 0.0130(9) Uani 1 1 d . . . . .
C9 C 0.6808(5) 0.9411(4) -0.0071(4) 0.0178(11) Uani 1 1 d . . . . .
O10 O -0.0871(3) -0.1308(3) 0.0438(2) 0.0139(7) Uani 1 1 d . . . . .
N10 N -0.1425(5) 0.0952(4) 0.2817(4) 0.0309(12) Uani 1 1 d . . . . .
C10 C 0.7452(5) 1.0510(5) 0.0047(4) 0.0218(12) Uani 1 1 d . . . . .
H10 H 0.783871 1.088213 0.065416 0.026 Uiso 1 1 calc R U . . .
O11 O -0.0540(3) -0.3077(3) 0.0772(2) 0.0150(8) Uani 1 1 d . . . . .
C11 C 0.7524(5) 1.1056(5) -0.0729(4) 0.0239(13) Uani 1 1 d . . . . .
H11 H 0.797095 1.178975 -0.064162 0.029 Uiso 1 1 calc R U . . .
O12 O -0.1373(4) 0.0079(3) 0.2506(3) 0.0239(9) Uani 1 1 d . . . . .
C12 C 0.6927(5) 1.0507(5) -0.1637(4) 0.0225(12) Uani 1 1 d . . . . .
H12 H 0.696283 1.087110 -0.216154 0.027 Uiso 1 1 calc R U . . .
O13 O -0.1263(8) 0.1711(5) 0.2360(5) 0.080(2) Uani 1 1 d . . . . .
C13 C 0.6281(5) 0.9416(5) -0.1757(4) 0.0200(12) Uani 1 1 d . . . . .
H13 H 0.587969 0.905366 -0.236795 0.024 Uiso 1 1 calc R U . . .
O14 O -0.1512(6) 0.1088(4) 0.3597(3) 0.0561(16) Uani 1 1 d . . . . .
C14 C 0.6215(5) 0.8844(4) -0.0989(4) 0.0176(11) Uani 1 1 d . . . . .
C15 C 0.5548(5) 0.7675(4) -0.1189(4) 0.0149(11) Uani 1 1 d . . . . .
C16 C 0.5467(6) 0.8866(6) 0.0948(5) 0.0328(15) Uani 1 1 d . . . . .
H16A H 0.543953 0.957927 0.098855 0.049 Uiso 1 1 calc R U . . .
H16B H 0.544350 0.858365 0.153457 0.049 Uiso 1 1 calc R U . . .
H16C H 0.472643 0.842102 0.044081 0.049 Uiso 1 1 calc R U . . .
O17 O 0.6947(5) 0.2363(4) 0.3629(4) 0.0459(12) Uiso 1 1 d . . . . .
C17 C 0.1901(5) 0.1994(4) 0.2364(4) 0.0138(11) Uani 1 1 d . . . . .
O18 O 0.589(2) 0.9025(17) 0.3931(16) 0.293(10) Uiso 1 1 d . . . . .
C18 C 0.2833(5) 0.3097(4) 0.2703(4) 0.0143(11) Uani 1 1 d . . . . .
O19 O 0.501(2) 0.9376(17) -0.4235(16) 0.303(10) Uiso 1 1 d . . . . .
C19 C 0.3797(5) 0.3246(4) 0.3575(4) 0.0187(12) Uani 1 1 d . . . . .
H19 H 0.379791 0.266808 0.391622 0.022 Uiso 1 1 calc R U . . .
C20 C 0.4741(5) 0.4225(5) 0.3939(4) 0.0214(12) Uani 1 1 d . . . . .
H20 H 0.537288 0.431097 0.452332 0.026 Uiso 1 1 calc R U . . .
C21 C 0.4742(5) 0.5083(5) 0.3428(4) 0.0236(13) Uani 1 1 d . . . . .
H21 H 0.537944 0.574981 0.367027 0.028 Uiso 1 1 calc R U . . .
C22 C 0.3802(5) 0.4955(4) 0.2560(4) 0.0195(12) Uani 1 1 d . . . . .
H22 H 0.381985 0.553318 0.221657 0.023 Uiso 1 1 calc R U . . .
C23 C 0.2833(5) 0.3970(4) 0.2198(4) 0.0153(11) Uani 1 1 d . . . . .
C24 C 0.0596(6) 0.3909(5) 0.1443(4) 0.0270(13) Uani 1 1 d . . . . .
H24A H 0.022068 0.327663 0.170605 0.040 Uiso 1 1 calc R U . . .
H24B H -0.000528 0.392875 0.084380 0.040 Uiso 1 1 calc R U . . .
H24C H 0.077356 0.453057 0.186863 0.040 Uiso 1 1 calc R U . . .
C25 C -0.0083(5) -0.2332(4) 0.1467(3) 0.0100(10) Uani 1 1 d . . . . .
C26 C 0.0715(5) -0.2489(4) 0.2409(4) 0.0139(11) Uani 1 1 d . . . . .
C27 C 0.1299(6) -0.3258(5) 0.2404(4) 0.0239(13) Uani 1 1 d . . . . .
H27 H 0.111350 -0.368054 0.184007 0.029 Uiso 1 1 calc R U . . .
C28 C 0.2148(6) -0.3408(5) 0.3219(4) 0.0311(15) Uani 1 1 d . . . . .
H28 H 0.254705 -0.391450 0.319863 0.037 Uiso 1 1 calc R U . . .
C29 C 0.2406(6) -0.2807(5) 0.4063(4) 0.0278(14) Uani 1 1 d . . . . .
H29 H 0.296868 -0.291360 0.461633 0.033 Uiso 1 1 calc R U . . .
C30 C 0.1819(6) -0.2041(4) 0.4082(4) 0.0217(12) Uani 1 1 d . . . . .
H30 H 0.199318 -0.163474 0.465301 0.026 Uiso 1 1 calc R U . . .
C31 C 0.0979(5) -0.1873(4) 0.3264(4) 0.0170(11) Uani 1 1 d . . . . .
C32 C 0.0698(6) -0.0464(4) 0.4218(4) 0.0210(12) Uani 1 1 d . . . . .
H32A H 0.053435 -0.096036 0.466469 0.031 Uiso 1 1 calc R U . . .
H32B H 0.016039 -0.002646 0.417115 0.031 Uiso 1 1 calc R U . . .
H32C H 0.160198 -0.001730 0.442822 0.031 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.909(3) . ?
Cu1 O1 1.909(3) 2_665 ?
Cu1 O4 1.931(3) 2_665 ?
Cu1 O4 1.931(3) . ?
Cu1 O5 2.435(4) . ?
Cu1 O5 2.435(5) 2_665 ?
O1 N1 1.399(5) . ?
O1 Cu2 1.919(4) . ?
N1 C1 1.307(7) . ?
N1 Cu3 1.924(4) 2_665 ?
C1 O2 1.291(6) . ?
C1 C2 1.486(7) . ?
Cu2 O2 1.955(4) . ?
Cu2 N4 1.957(4) . ?
Cu2 N3 1.984(5) . ?
N2 C7 1.459(7) . ?
N2 C8 1.462(7) . ?
N2 Cu3 1.997(4) 2_665 ?
N2 H2 0.9800 . ?
C2 C7 1.398(8) . ?
C2 C3 1.400(7) . ?
Cu3 O4 1.914(3) . ?
Cu3 O3 1.929(4) . ?
O3 C15 1.291(6) . ?
N3 C9 1.449(7) . ?
N3 C16 1.490(7) . ?
N3 H3A 0.9800 . ?
C3 C4 1.382(8) . ?
C3 H3 0.9300 . ?
Cu4 N7 1.923(4) 2 ?
Cu4 O10 1.932(3) . ?
Cu4 O11 1.933(4) . ?
Cu4 N6 1.987(4) 2 ?
O4 N4 1.406(5) . ?
N4 C15 1.308(7) . ?
C4 C5 1.375(8) . ?
C4 H4 0.9300 . ?
Cu5 O8 1.893(4) . ?
Cu5 N9 1.934(4) . ?
Cu5 O9 1.941(3) . ?
Cu5 N8 1.997(4) . ?
Cu5 O12 2.415(4) . ?
O5 N5 1.271(7) . ?
N5 O6 1.242(7) . ?
N5 O7 1.272(7) . ?
C5 C6 1.387(8) . ?
C5 H5 0.9300 . ?
Cu6 O8 1.866(3) . ?
Cu6 O8 1.866(3) 2 ?
Cu6 O10 1.935(3) 2 ?
Cu6 O10 1.935(3) . ?
N6 C23 1.455(7) . ?
N6 C24 1.478(7) . ?
N6 H6A 0.9800 . ?
C6 C7 1.385(8) . ?
C6 H6 0.9300 . ?
N7 C17 1.300(7) . ?
N7 O8 1.404(5) . ?
N8 C31 1.452(7) . ?
N8 C32 1.478(7) . ?
N8 H8 0.9800 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
O9 C17 1.293(6) . ?
N9 C25 1.315(6) . ?
N9 O10 1.413(5) . ?
C9 C10 1.389(8) . ?
C9 C14 1.408(8) . ?
N10 O14 1.206(7) . ?
N10 O13 1.222(7) . ?
N10 O12 1.266(6) . ?
C10 C11 1.383(8) . ?
C10 H10 0.9300 . ?
O11 C25 1.277(6) . ?
C11 C12 1.388(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.380(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.391(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.475(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.480(7) . ?
C18 C23 1.395(7) . ?
C18 C19 1.395(7) . ?
C19 C20 1.370(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.384(9) . ?
C20 H20 0.9300 . ?
C21 C22 1.383(8) . ?
C21 H21 0.9300 . ?
C22 C23 1.385(7) . ?
C22 H22 0.9300 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.492(7) . ?
C26 C27 1.387(7) . ?
C26 C31 1.398(7) . ?
C27 C28 1.375(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.375(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.390(8) . ?
C29 H29 0.9300 . ?
C30 C31 1.384(8) . ?
C30 H30 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.0 . 2_665 ?
O1 Cu1 O4 93.25(14) . 2_665 ?
O1 Cu1 O4 86.75(14) 2_665 2_665 ?
O1 Cu1 O4 86.75(14) . . ?
O1 Cu1 O4 93.25(14) 2_665 . ?
O4 Cu1 O4 180.0 2_665 . ?
O1 Cu1 O5 83.17(16) . . ?
O1 Cu1 O5 96.83(16) 2_665 . ?
O4 Cu1 O5 92.06(15) 2_665 . ?
O4 Cu1 O5 87.94(15) . . ?
O1 Cu1 O5 96.83(16) . 2_665 ?
O1 Cu1 O5 83.17(15) 2_665 2_665 ?
O4 Cu1 O5 87.94(15) 2_665 2_665 ?
O4 Cu1 O5 92.06(15) . 2_665 ?
O5 Cu1 O5 180.0 . 2_665 ?
N1 O1 Cu1 116.5(3) . . ?
N1 O1 Cu2 112.0(3) . . ?
Cu1 O1 Cu2 111.39(17) . . ?
C1 N1 O1 112.5(4) . . ?
C1 N1 Cu3 129.4(4) . 2_665 ?
O1 N1 Cu3 116.2(3) . 2_665 ?
O2 C1 N1 122.3(5) . . ?
O2 C1 C2 120.4(5) . . ?
N1 C1 C2 117.3(5) . . ?
O1 Cu2 O2 81.95(14) . . ?
O1 Cu2 N4 88.50(16) . . ?
O2 Cu2 N4 170.28(17) . . ?
O1 Cu2 N3 173.85(17) . . ?
O2 Cu2 N3 97.34(17) . . ?
N4 Cu2 N3 92.34(18) . . ?
C1 O2 Cu2 110.1(3) . . ?
C7 N2 C8 112.7(4) . . ?
C7 N2 Cu3 114.1(3) . 2_665 ?
C8 N2 Cu3 107.7(4) . 2_665 ?
C7 N2 H2 107.4 . . ?
C8 N2 H2 107.4 . . ?
Cu3 N2 H2 107.4 2_665 . ?
C7 C2 C3 118.3(5) . . ?
C7 C2 C1 125.1(5) . . ?
C3 C2 C1 116.5(5) . . ?
O4 Cu3 N1 90.79(16) . 2_665 ?
O4 Cu3 O3 81.93(15) . . ?
N1 Cu3 O3 172.32(17) 2_665 . ?
O4 Cu3 N2 174.02(17) . 2_665 ?
N1 Cu3 N2 87.41(18) 2_665 2_665 ?
O3 Cu3 N2 100.08(17) . 2_665 ?
C15 O3 Cu3 109.9(3) . . ?
C9 N3 C16 110.2(4) . . ?
C9 N3 Cu2 118.8(3) . . ?
C16 N3 Cu2 106.6(4) . . ?
C9 N3 H3A 106.9 . . ?
C16 N3 H3A 106.9 . . ?
Cu2 N3 H3A 106.9 . . ?
C4 C3 C2 121.4(5) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
N7 Cu4 O10 89.93(16) 2 . ?
N7 Cu4 O11 158.36(17) 2 . ?
O10 Cu4 O11 82.02(14) . . ?
N7 Cu4 N6 88.91(18) 2 2 ?
O10 Cu4 N6 175.74(16) . 2 ?
O11 Cu4 N6 100.47(16) . 2 ?
N4 O4 Cu3 111.1(3) . . ?
N4 O4 Cu1 117.9(3) . . ?
Cu3 O4 Cu1 112.90(17) . . ?
C15 N4 O4 111.5(4) . . ?
C15 N4 Cu2 127.8(4) . . ?
O4 N4 Cu2 115.4(3) . . ?
C5 C4 C3 119.8(5) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
O8 Cu5 N9 87.36(16) . . ?
O8 Cu5 O9 81.88(14) . . ?
N9 Cu5 O9 161.88(17) . . ?
O8 Cu5 N8 171.33(17) . . ?
N9 Cu5 N8 86.54(17) . . ?
O9 Cu5 N8 105.54(16) . . ?
O8 Cu5 O12 94.12(15) . . ?
N9 Cu5 O12 100.05(15) . . ?
O9 Cu5 O12 95.25(14) . . ?
N8 Cu5 O12 80.91(16) . . ?
N5 O5 Cu1 114.9(4) . . ?
O6 N5 O5 119.5(5) . . ?
O6 N5 O7 120.0(5) . . ?
O5 N5 O7 120.5(5) . . ?
C4 C5 C6 119.7(5) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
O8 Cu6 O8 180.0 . 2 ?
O8 Cu6 O10 91.78(14) . 2 ?
O8 Cu6 O10 88.22(14) 2 2 ?
O8 Cu6 O10 88.23(14) . . ?
O8 Cu6 O10 91.77(14) 2 . ?
O10 Cu6 O10 180.0 2 . ?
C23 N6 C24 112.5(4) . . ?
C23 N6 Cu4 116.1(3) . 2 ?
C24 N6 Cu4 103.9(3) . 2 ?
C23 N6 H6A 108.0 . . ?
C24 N6 H6A 108.0 . . ?
Cu4 N6 H6A 108.0 2 . ?
C7 C6 C5 121.1(5) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C17 N7 O8 110.9(4) . . ?
C17 N7 Cu4 133.8(4) . 2 ?
O8 N7 Cu4 115.0(3) . 2 ?
C6 C7 C2 119.7(5) . . ?
C6 C7 N2 118.0(5) . . ?
C2 C7 N2 122.3(5) . . ?
N7 O8 Cu6 119.8(3) . . ?
N7 O8 Cu5 113.7(3) . . ?
Cu6 O8 Cu5 120.95(18) . . ?
C31 N8 C32 115.9(4) . . ?
C31 N8 Cu5 113.4(3) . . ?
C32 N8 Cu5 112.5(3) . . ?
C31 N8 H8 104.5 . . ?
C32 N8 H8 104.5 . . ?
Cu5 N8 H8 104.5 . . ?
N2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C17 O9 Cu5 110.4(3) . . ?
C25 N9 O10 111.2(4) . . ?
C25 N9 Cu5 130.5(3) . . ?
O10 N9 Cu5 117.9(3) . . ?
C10 C9 C14 119.9(5) . . ?
C10 C9 N3 118.5(5) . . ?
C14 C9 N3 121.5(5) . . ?
N9 O10 Cu4 112.0(3) . . ?
N9 O10 Cu6 112.0(3) . . ?
Cu4 O10 Cu6 113.68(17) . . ?
O14 N10 O13 118.5(6) . . ?
O14 N10 O12 121.4(5) . . ?
O13 N10 O12 119.8(5) . . ?
C11 C10 C9 120.8(5) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C25 O11 Cu4 111.3(3) . . ?
C10 C11 C12 119.8(6) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
N10 O12 Cu5 123.2(4) . . ?
C13 C12 C11 119.6(5) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 121.8(5) . . ?
C12 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C13 C14 C9 118.2(5) . . ?
C13 C14 C15 117.7(5) . . ?
C9 C14 C15 124.1(5) . . ?
O3 C15 N4 122.1(5) . . ?
O3 C15 C14 119.1(5) . . ?
N4 C15 C14 118.7(5) . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O9 C17 N7 122.8(5) . . ?
O9 C17 C18 120.5(4) . . ?
N7 C17 C18 116.6(5) . . ?
C23 C18 C19 118.9(5) . . ?
C23 C18 C17 124.6(5) . . ?
C19 C18 C17 116.6(5) . . ?
C20 C19 C18 121.5(5) . . ?
C20 C19 H19 119.2 . . ?
C18 C19 H19 119.2 . . ?
C19 C20 C21 119.2(5) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C22 C21 C20 120.4(5) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 120.4(5) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C18 119.6(5) . . ?
C22 C23 N6 118.1(5) . . ?
C18 C23 N6 122.3(4) . . ?
N6 C24 H24A 109.5 . . ?
N6 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N6 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O11 C25 N9 123.1(4) . . ?
O11 C25 C26 119.9(4) . . ?
N9 C25 C26 116.8(4) . . ?
C27 C26 C31 119.0(5) . . ?
C27 C26 C25 116.2(5) . . ?
C31 C26 C25 124.7(5) . . ?
C28 C27 C26 121.3(5) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C29 C28 C27 120.0(5) . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C28 C29 C30 119.6(5) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C31 C30 C29 120.9(5) . . ?
C31 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C30 C31 C26 119.3(5) . . ?
C30 C31 N8 121.0(5) . . ?
C26 C31 N8 119.7(5) . . ?
N8 C32 H32A 109.5 . . ?
N8 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N8 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_refine_diff_density_max         1.298
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.134


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_lfjre37a
_database_code_depnum_ccdc_archive 'CCDC 1907526'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;Bangor University 
United Kingdom
;
_audit_update_record             
;
2019-05-20 deposited with the CCDC.	2019-06-04 downloaded from the CCDC.
;
_audit_creation_date             2019-05-01
_audit_creation_method           
;
Olex2 1.3-dev
(compiled 2019.03.18 svn.r3573 for OlexSys, GUI svn.r5585)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            '[Cu1]'
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H16 Cu N2 O6'
_chemical_formula_sum            'C16 H16 Cu N2 O6'
_chemical_formula_weight         395.85
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   3.69870(10)
_cell_length_b                   12.6213(4)
_cell_length_c                   15.7971(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.451(3)
_cell_angle_gamma                90
_cell_volume                     736.11(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.5410
_cell_measurement_theta_min      2.2380
_shelx_estimated_absorpt_T_max   0.942
_shelx_estimated_absorpt_T_min   0.702
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Light-Green
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Rod
_exptl_crystal_F_000             406
_exptl_crystal_preparation       'Magnetic properties,Magnetic properties'
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Methanol'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1342
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.342
_diffrn_reflns_theta_min         2.067
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1315
_reflns_number_total             1342
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1342
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0254
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0509P)²+0.5369P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0859
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9187(11)
 0.0813(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.500000 0.500000 0.500000 0.01322(17) Uani 1 2 d S T P . .
O1 O 0.5425(4) 0.65120(12) 0.47967(9) 0.0144(3) Uani 1 1 d . . . . .
N1 N 0.1987(5) 0.59961(14) 0.36698(11) 0.0134(4) Uani 1 1 d . . . . .
C1 C 0.3848(6) 0.67388(16) 0.40796(12) 0.0125(4) Uani 1 1 d . . . . .
H1 H 0.098(7) 0.611(2) 0.3192(16) 0.013(6) Uiso 1 1 d . . . . .
O2 O 0.1704(5) 0.50140(10) 0.40250(11) 0.0157(4) Uani 1 1 d . . . . .
C2 C 0.4132(5) 0.78117(16) 0.37205(12) 0.0122(4) Uani 1 1 d . . . . .
O3 O 0.1388(4) 0.73169(12) 0.23839(9) 0.0143(3) Uani 1 1 d . . . . .
C3 C 0.5744(6) 0.85869(17) 0.42451(13) 0.0139(4) Uani 1 1 d . . . . .
H3 H 0.660744 0.840109 0.480399 0.017 Uiso 1 1 calc R . . . .
C4 C 0.6120(6) 0.96176(17) 0.39735(13) 0.0153(4) Uani 1 1 d . . . . .
H4 H 0.720643 1.013719 0.434217 0.018 Uiso 1 1 calc R . . . .
C5 C 0.4892(6) 0.98839(17) 0.31566(15) 0.0148(5) Uani 1 1 d . . . . .
H5 H 0.513276 1.059311 0.296659 0.018 Uiso 1 1 calc R . . . .
C6 C 0.3313(6) 0.91321(17) 0.26105(13) 0.0138(4) Uani 1 1 d . . . . .
H6 H 0.251168 0.932329 0.204854 0.017 Uiso 1 1 calc R . . . .
C7 C 0.2914(5) 0.81009(16) 0.28899(13) 0.0121(4) Uani 1 1 d . . . . .
C8 C 0.0146(6) 0.75892(17) 0.15285(12) 0.0153(4) Uani 1 1 d . . . . .
H8A H -0.156679 0.818055 0.154037 0.023 Uiso 1 1 calc GR . . . .
H8B H -0.105732 0.697529 0.125631 0.023 Uiso 1 1 calc GR . . . .
H8C H 0.221974 0.779670 0.120765 0.023 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.9431(15) . ?
Cu1 O1 1.9431(15) 3_666 ?
Cu1 O2 1.9059(17) 3_666 ?
Cu1 O2 1.9058(17) . ?
O1 C1 1.275(3) . ?
N1 C1 1.311(3) . ?
N1 H1 0.83(3) . ?
N1 O2 1.367(2) . ?
C1 C2 1.474(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.409(3) . ?
O3 C7 1.372(2) . ?
O3 C8 1.442(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.379(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.387(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.385(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O1 180.00(9) 3_666 . ?
O2 Cu1 O1 84.92(6) . . ?
O2 Cu1 O1 95.08(6) . 3_666 ?
O2 Cu1 O1 84.92(6) 3_666 3_666 ?
O2 Cu1 O1 95.08(6) 3_666 . ?
O2 Cu1 O2 180.0 . 3_666 ?
C1 O1 Cu1 109.28(13) . . ?
C1 N1 H1 121.2(17) . . ?
C1 N1 O2 119.77(17) . . ?
O2 N1 H1 119.0(17) . . ?
O1 C1 N1 118.48(19) . . ?
O1 C1 C2 120.57(18) . . ?
N1 C1 C2 120.95(18) . . ?
N1 O2 Cu1 106.21(11) . . ?
C3 C2 C1 117.01(18) . . ?
C3 C2 C7 118.24(19) . . ?
C7 C2 C1 124.74(18) . . ?
C7 O3 C8 118.07(16) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.67(19) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 H4 120.5 . . ?
C3 C4 C5 119.1(2) . . ?
C5 C4 H4 120.5 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.1(2) . . ?
C6 C5 H5 119.5 . . ?
C5 C6 H6 120.2 . . ?
C7 C6 C5 119.57(19) . . ?
C7 C6 H6 120.2 . . ?
O3 C7 C2 116.92(18) . . ?
O3 C7 C6 122.69(18) . . ?
C6 C7 C2 120.39(19) . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C1 N1 7.1(2) . . . . ?
Cu1 O1 C1 C2 -172.66(14) . . . . ?
O1 C1 C2 C3 -8.6(3) . . . . ?
O1 C1 C2 C7 171.00(19) . . . . ?
N1 C1 C2 C3 171.65(19) . . . . ?
N1 C1 C2 C7 -8.7(3) . . . . ?
C1 N1 O2 Cu1 -9.4(2) . . . . ?
C1 C2 C3 C4 -179.52(19) . . . . ?
C1 C2 C7 O3 -0.6(3) . . . . ?
C1 C2 C7 C6 -179.83(19) . . . . ?
O2 N1 C1 O1 1.6(3) . . . . ?
O2 N1 C1 C2 -178.64(17) . . . . ?
C2 C3 C4 C5 -0.6(3) . . . . ?
C3 C2 C7 O3 179.03(18) . . . . ?
C3 C2 C7 C6 -0.2(3) . . . . ?
C3 C4 C5 C6 -0.3(3) . . . . ?
C4 C5 C6 C7 0.9(3) . . . . ?
C5 C6 C7 C2 -0.6(3) . . . . ?
C5 C6 C7 O3 -179.82(19) . . . . ?
C7 C2 C3 C4 0.8(3) . . . . ?
C8 O3 C7 C2 -179.49(17) . . . . ?
C8 O3 C7 C6 -0.3(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9187(11)
2 0.0813(11)

