# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_sm358xsr
_database_code_depnum_ccdc_archive 'CCDC 2403817'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        2-fur-Zn7
_chemical_name_common            2-fur-Zn7.3H2O

_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C65 H88 N8 O29 Zn7'
_chemical_formula_weight         1903.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

_cell_length_a                   14.064(2)
_cell_length_b                   14.064(2)
_cell_length_c                   23.056(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3949.3(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    2236
_cell_measurement_theta_min      3.0225
_cell_measurement_theta_max      29.1587

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_F_000             1792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    2.162
_shelx_estimated_absorpt_T_min   0.846
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69269
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            7622
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.029
_diffrn_reflns_theta_max         25.341
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2416
_reflns_number_gt                1718
_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, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_cell_refinement       
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_data_reduction        
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_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          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)+(0.0901P)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         2416
_refine_ls_number_parameters     153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0582
_refine_ls_wR_factor_ref         0.1656
_refine_ls_wR_factor_gt          0.1528
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_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 0.000000 0.000000 0.000000 0.0211(4) Uani 1 6 d S T P . .
O1 O -0.0046(3) -0.1333(3) 0.04520(15) 0.0222(8) Uani 1 1 d . . . . .
N1 N 0.1806(4) -0.2004(4) -0.0736(2) 0.0335(13) Uani 1 1 d . . . . .
C1 C 0.0102(8) -0.1344(8) 0.1095(4) 0.089(3) Uani 1 1 d . . . . .
H1A H -0.051400 -0.134364 0.129311 0.133 Uiso 1 1 calc R U . . .
H1B H 0.079036 -0.069125 0.120933 0.133 Uiso 1 1 calc R U . . .
H1C H 0.012738 -0.200515 0.120336 0.133 Uiso 1 1 calc R U . . .
Zn2 Zn -0.14744(6) -0.25467(5) 0.01144(3) 0.0250(3) Uani 1 1 d . . . . .
O2 O -0.0372(3) -0.2813(3) -0.03431(16) 0.0256(9) Uani 1 1 d . . . . .
N2 N -0.333333 -0.666667 -0.2955(4) 0.042(2) Uani 1 3 d S T P . .
C2 C -0.3540(5) -0.4949(5) -0.0468(3) 0.0462(18) Uani 1 1 d . . . . .
H2A H -0.399947 -0.505357 -0.080859 0.069 Uiso 1 1 calc R U . . .
H2B H -0.387557 -0.482675 -0.012494 0.069 Uiso 1 1 calc R U . . .
H2C H -0.347591 -0.560524 -0.040972 0.069 Uiso 1 1 calc R U . . .
O3 O -0.2469(3) -0.4015(3) -0.05581(19) 0.0350(11) Uani 1 1 d . . . . .
C3 C -0.1760(5) -0.4122(5) -0.0943(3) 0.0284(14) Uani 1 1 d . . . . .
O4 O -0.2377(4) -0.6498(4) -0.2958(2) 0.0667(16) Uani 1 1 d . . . . .
C4 C -0.2102(5) -0.4784(5) -0.1426(3) 0.0388(16) Uani 1 1 d . . . . .
H4 H -0.286199 -0.521963 -0.151323 0.047 Uiso 1 1 calc R U . . .
C5 C -0.1315(5) -0.4805(5) -0.1788(3) 0.0369(16) Uani 1 1 d . . . . .
H5 H -0.154376 -0.527144 -0.211841 0.044 Uiso 1 1 calc R U . . .
C6 C -0.0223(5) -0.4166(5) -0.1673(2) 0.0347(15) Uani 1 1 d . . . . .
H6 H 0.029895 -0.419699 -0.192169 0.042 Uiso 1 1 calc R U . . .
C7 C 0.0146(5) -0.3452(5) -0.1184(2) 0.0289(14) Uani 1 1 d . . . . .
C8 C -0.0633(5) -0.3432(4) -0.0808(2) 0.0243(13) Uani 1 1 d . . . . .
C9 C 0.1303(5) -0.2752(5) -0.1116(2) 0.0314(14) Uani 1 1 d . . . . .
H9 H 0.175339 -0.285510 -0.138667 0.038 Uiso 1 1 calc R U . . .
C10 C 0.3016(5) -0.1366(6) -0.0763(4) 0.060(2) Uani 1 1 d . . . . .
H10A H 0.332241 -0.147789 -0.040465 0.089 Uiso 1 1 calc R U . . .
H10B H 0.325656 -0.058406 -0.080590 0.089 Uiso 1 1 calc R U . . .
H10C H 0.327110 -0.161117 -0.109509 0.089 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 2.117(3) . ?
Zn1 O1 2.117(3) 2 ?
Zn1 O1 2.117(3) 8 ?
Zn1 O1 2.117(3) 7 ?
Zn1 O1 2.117(3) 3 ?
Zn1 O1 2.117(3) 9 ?
O1 C1 1.498(10) . ?
O1 Zn2 2.032(4) . ?
O1 Zn2 2.129(4) 9 ?
N1 C9 1.278(7) . ?
N1 C10 1.476(8) . ?
N1 Zn2 2.106(5) 9 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Zn2 O2 2.031(4) 8 ?
Zn2 O2 2.058(4) . ?
Zn2 O3 2.395(4) . ?
Zn2 Zn2 3.1589(8) 9 ?
Zn2 Zn2 3.1589(8) 8 ?
O2 C8 1.313(6) . ?
N2 O4 1.243(5) . ?
N2 O4 1.243(5) 3_545 ?
N2 O4 1.243(5) 2_445 ?
C2 O3 1.435(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
O3 C3 1.398(7) . ?
C3 C4 1.375(8) . ?
C3 C8 1.419(8) . ?
C4 C5 1.399(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.362(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.423(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.408(8) . ?
C7 C9 1.428(8) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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 97.85(12) . 2 ?
O1 Zn1 O1 82.15(12) . 8 ?
O1 Zn1 O1 180.0(4) 2 8 ?
O1 Zn1 O1 180.00(16) . 7 ?
O1 Zn1 O1 82.15(12) 2 7 ?
O1 Zn1 O1 97.85(12) 8 7 ?
O1 Zn1 O1 97.85(12) . 3 ?
O1 Zn1 O1 97.85(12) 2 3 ?
O1 Zn1 O1 82.15(12) 8 3 ?
O1 Zn1 O1 82.15(12) 7 3 ?
O1 Zn1 O1 82.15(12) . 9 ?
O1 Zn1 O1 82.15(12) 2 9 ?
O1 Zn1 O1 97.85(12) 8 9 ?
O1 Zn1 O1 97.85(12) 7 9 ?
O1 Zn1 O1 180.0(2) 3 9 ?
C1 O1 Zn2 117.0(4) . . ?
C1 O1 Zn1 123.6(4) . . ?
Zn2 O1 Zn1 97.75(15) . . ?
C1 O1 Zn2 119.5(4) . 9 ?
Zn2 O1 Zn2 98.78(14) . 9 ?
Zn1 O1 Zn2 94.81(14) . 9 ?
C9 N1 C10 117.8(5) . . ?
C9 N1 Zn2 126.2(4) . 9 ?
C10 N1 Zn2 115.7(4) . 9 ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Zn2 O1 113.73(15) 8 . ?
O2 Zn2 O2 163.03(9) 8 . ?
O1 Zn2 O2 80.28(14) . . ?
O2 Zn2 N1 86.30(17) 8 8 ?
O1 Zn2 N1 103.41(18) . 8 ?
O2 Zn2 N1 100.13(17) . 8 ?
O2 Zn2 O1 78.62(14) 8 8 ?
O1 Zn2 O1 83.92(19) . 8 ?
O2 Zn2 O1 94.10(14) . 8 ?
N1 Zn2 O1 164.88(16) 8 8 ?
O2 Zn2 O3 93.92(15) 8 . ?
O1 Zn2 O3 151.45(14) . . ?
O2 Zn2 O3 71.29(14) . . ?
N1 Zn2 O3 84.58(18) 8 . ?
O1 Zn2 O3 95.26(15) 8 . ?
O2 Zn2 Zn2 151.60(11) 8 9 ?
O1 Zn2 Zn2 41.75(10) . 9 ?
O2 Zn2 Zn2 39.12(10) . 9 ?
N1 Zn2 Zn2 110.76(14) 8 9 ?
O1 Zn2 Zn2 83.59(9) 8 9 ?
O3 Zn2 Zn2 109.71(10) . 9 ?
O2 Zn2 Zn2 39.73(10) 8 8 ?
O1 Zn2 Zn2 96.23(10) . 8 ?
O2 Zn2 Zn2 133.16(11) . 8 ?
N1 Zn2 Zn2 125.69(14) 8 8 ?
O1 Zn2 Zn2 39.46(9) 8 8 ?
O3 Zn2 Zn2 101.15(11) . 8 ?
Zn2 Zn2 Zn2 117.270(13) 9 8 ?
C8 O2 Zn2 130.2(4) . 9 ?
C8 O2 Zn2 123.6(4) . . ?
Zn2 O2 Zn2 101.15(16) 9 . ?
O4 N2 O4 120.000(11) . 3_545 ?
O4 N2 O4 119.996(11) . 2_445 ?
O4 N2 O4 119.998(12) 3_545 2_445 ?
O3 C2 H2A 109.5 . . ?
O3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
O3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 O3 C2 118.1(4) . . ?
C3 O3 Zn2 111.3(3) . . ?
C2 O3 Zn2 126.1(4) . . ?
C4 C3 O3 124.1(5) . . ?
C4 C3 C8 122.3(6) . . ?
O3 C3 C8 113.5(5) . . ?
C3 C4 C5 119.0(6) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 120.8(6) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 120.9(6) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 119.2(6) . . ?
C8 C7 C9 123.3(5) . . ?
C6 C7 C9 117.5(5) . . ?
O2 C8 C7 123.6(5) . . ?
O2 C8 C3 118.6(5) . . ?
C7 C8 C3 117.7(5) . . ?
N1 C9 C7 127.8(6) . . ?
N1 C9 H9 116.1 . . ?
C7 C9 H9 116.1 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_refine_diff_density_max         1.176
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.144


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.250 403 85 ' '
2 0.000 0.000 0.750 403 85 ' '
3 0.333 0.667 0.438 15 2 ' '
4 0.333 0.666 0.938 15 2 ' '
5 0.666 0.333 0.062 15 2 ' '
6 0.666 0.333 0.562 15 2 ' '
_platon_squeeze_details          
;
;

_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_sm200sq
_database_code_depnum_ccdc_archive 'CCDC 2403822'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        2-Fur-Co7
_chemical_name_common            '[2-Fur-Co7].3H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C59 H76 Co7 N8 O29'
_chemical_formula_weight         1773.81

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

_cell_length_a                   14.100(2)
_cell_length_b                   14.100(2)
_cell_length_c                   22.702(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3908.7(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    149.9(1)
_cell_measurement_reflns_used    3532
_cell_measurement_theta_min      2.8834
_cell_measurement_theta_max      29.1934

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_F_000             1654
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.518
_shelx_estimated_absorpt_T_min   0.895
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      149.9(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            2388
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.889
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2388
_reflns_number_gt                1894
_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, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_cell_refinement       
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_data_reduction        
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_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          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)+(0.1187P)²+24.3244P] 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         2388
_refine_ls_number_parameters     143
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0777
_refine_ls_wR_factor_ref         0.2313
_refine_ls_wR_factor_gt          0.2159
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_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
Co1 Co 0.000000 0.000000 0.000000 0.0255(5) Uani 1 6 d S T P . .
O1 O -0.0048(4) -0.1312(3) 0.0460(2) 0.0320(10) Uani 1 1 d . . . . .
H1 H 0.007528 -0.125803 0.089580 0.038 Uiso 1 1 calc R U . . .
N1 N -0.1934(5) -0.3772(5) 0.0763(3) 0.0427(15) Uani 1 1 d . . . . .
C1 C -0.1277(8) -0.4316(8) 0.0796(4) 0.062(3) Uani 1 1 d . . . . .
H1A H -0.158339 -0.488987 0.109773 0.093 Uiso 1 1 calc R U . . .
H1B H -0.051983 -0.377691 0.089935 0.093 Uiso 1 1 calc R U . . .
H1C H -0.128914 -0.464375 0.041355 0.093 Uiso 1 1 calc R U . . .
Co2 Co -0.14484(7) -0.25498(7) 0.01217(4) 0.0324(4) Uani 1 1 d . . . . .
O2 O -0.2762(3) -0.2441(4) 0.03378(19) 0.0307(10) Uani 1 1 d . . . . .
N2 N -0.666667 -0.333333 0.2938(6) 0.054(3) Uani 1 3 d S T P . .
C2 C -0.2719(6) -0.4096(6) 0.1122(3) 0.0446(18) Uani 1 1 d . . . . .
H2 H -0.284961 -0.468312 0.137715 0.053 Uiso 1 1 calc R U . . .
O3 O -0.4002(4) -0.1612(4) 0.0530(2) 0.0399(12) Uani 1 1 d . . . . .
C3 C -0.3447(6) -0.3636(6) 0.1175(3) 0.0359(15) Uani 1 1 d . . . . .
O4 O -0.6562(8) -0.4146(8) 0.2909(4) 0.104(3) Uani 1 1 d . . . . .
C4 C -0.4212(6) -0.4036(7) 0.1662(3) 0.0421(17) Uani 1 1 d . . . . .
H4 H -0.426161 -0.459823 0.191219 0.051 Uiso 1 1 calc R U . . .
C5 C -0.4860(6) -0.3587(7) 0.1752(3) 0.0476(19) Uani 1 1 d . . . . .
H5 H -0.534817 -0.383534 0.207733 0.057 Uiso 1 1 calc R U . . .
C6 C -0.4840(6) -0.2787(7) 0.1392(3) 0.0428(17) Uani 1 1 d . . . . .
H6 H -0.530451 -0.249284 0.146614 0.051 Uiso 1 1 calc R U . . .
C7 C -0.4127(5) -0.2430(6) 0.0922(3) 0.0349(16) Uani 1 1 d . . . . .
C8 C -0.3414(5) -0.2842(5) 0.0802(3) 0.0271(13) Uani 1 1 d . . . . .
C9 C -0.4935(6) -0.1474(6) 0.0437(4) 0.051(2) Uani 1 1 d . . . . .
H9A H -0.559197 -0.219223 0.038529 0.077 Uiso 1 1 calc R U . . .
H9B H -0.481731 -0.102846 0.008405 0.077 Uiso 1 1 calc R U . . .
H9C H -0.503027 -0.110581 0.077939 0.077 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.096(4) 7 ?
Co1 O1 2.096(4) . ?
Co1 O1 2.096(4) 8 ?
Co1 O1 2.096(4) 2 ?
Co1 O1 2.096(4) 9 ?
Co1 O1 2.096(4) 3 ?
O1 Co2 2.023(4) . ?
O1 Co2 2.173(4) 9 ?
O1 H1 1.0000 . ?
N1 C2 1.262(9) . ?
N1 C1 1.471(10) . ?
N1 Co2 2.093(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Co2 O2 1.995(4) . ?
Co2 O2 2.045(4) 9 ?
Co2 O3 2.329(5) 9 ?
O2 C8 1.324(7) . ?
N2 O4 1.229(9) 3_445 ?
N2 O4 1.229(9) 2_455 ?
N2 O4 1.229(9) . ?
C2 C3 1.468(10) . ?
C2 H2 0.9500 . ?
O3 C7 1.397(9) . ?
O3 C9 1.438(8) . ?
C3 C8 1.386(9) . ?
C3 C4 1.446(10) . ?
C4 C5 1.362(11) . ?
C4 H4 0.9500 . ?
C5 C6 1.381(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(10) . ?
C6 H6 0.9500 . ?
C7 C8 1.417(9) . ?
C9 H9A 0.9800 . ?
C9 H9B 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 Co1 O1 180.0 7 . ?
O1 Co1 O1 97.30(16) 7 8 ?
O1 Co1 O1 82.70(16) . 8 ?
O1 Co1 O1 82.70(16) 7 2 ?
O1 Co1 O1 97.30(16) . 2 ?
O1 Co1 O1 180.0(5) 8 2 ?
O1 Co1 O1 97.29(16) 7 9 ?
O1 Co1 O1 82.71(16) . 9 ?
O1 Co1 O1 97.29(16) 8 9 ?
O1 Co1 O1 82.71(16) 2 9 ?
O1 Co1 O1 82.71(16) 7 3 ?
O1 Co1 O1 97.29(16) . 3 ?
O1 Co1 O1 82.71(16) 8 3 ?
O1 Co1 O1 97.29(16) 2 3 ?
O1 Co1 O1 180.0(3) 9 3 ?
Co2 O1 Co1 99.15(19) . . ?
Co2 O1 Co2 98.15(18) . 9 ?
Co1 O1 Co2 94.52(18) . 9 ?
Co2 O1 H1 119.9 . . ?
Co1 O1 H1 119.9 . . ?
Co2 O1 H1 119.9 9 . ?
C2 N1 C1 116.5(6) . . ?
C2 N1 Co2 127.8(5) . . ?
C1 N1 Co2 115.7(5) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Co2 O1 112.55(18) . . ?
O2 Co2 O2 163.05(10) . 9 ?
O1 Co2 O2 79.93(17) . 9 ?
O2 Co2 N1 87.6(2) . . ?
O1 Co2 N1 102.9(2) . . ?
O2 Co2 N1 101.1(2) 9 . ?
O2 Co2 O1 77.52(17) . 8 ?
O1 Co2 O1 82.5(2) . 8 ?
O2 Co2 O1 93.48(18) 9 8 ?
N1 Co2 O1 165.1(2) . 8 ?
O2 Co2 O3 94.63(18) . 9 ?
O1 Co2 O3 151.84(17) . 9 ?
O2 Co2 O3 71.97(17) 9 9 ?
N1 Co2 O3 84.8(2) . 9 ?
O1 Co2 O3 96.98(18) 8 9 ?
C8 O2 Co2 129.5(4) . . ?
C8 O2 Co2 123.4(4) . 8 ?
Co2 O2 Co2 103.47(19) . 8 ?
O4 N2 O4 119.73(16) 3_445 2_455 ?
O4 N2 O4 119.73(16) 3_445 . ?
O4 N2 O4 119.73(16) 2_455 . ?
N1 C2 C3 125.1(7) . . ?
N1 C2 H2 117.5 . . ?
C3 C2 H2 117.5 . . ?
C7 O3 C9 117.3(6) . . ?
C7 O3 Co2 112.8(4) . 8 ?
C9 O3 Co2 126.0(5) . 8 ?
C8 C3 C4 120.0(6) . . ?
C8 C3 C2 123.8(6) . . ?
C4 C3 C2 116.1(6) . . ?
C5 C4 C3 118.4(7) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C6 123.1(7) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C7 C6 C5 118.0(7) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
C6 C7 O3 124.3(7) . . ?
C6 C7 C8 122.5(7) . . ?
O3 C7 C8 113.2(6) . . ?
O2 C8 C3 124.6(6) . . ?
O2 C8 C7 117.5(6) . . ?
C3 C8 C7 117.9(6) . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_refine_diff_density_max         2.231
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.146


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.250 477 83 ' '
2 0.000 0.000 0.750 477 83 ' '
3 0.333 0.667 0.429 16 3 ' '
4 0.333 0.666 0.929 16 3 ' '
5 0.666 0.333 0.071 16 3 ' '
6 0.666 0.333 0.571 16 3 ' '
_platon_squeeze_details          
;
;


_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_lfjoh1sq
_database_code_depnum_ccdc_archive 'CCDC 2403821'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        Coumarin-Ni7
_chemical_name_common            '[Cou-Ni7].3H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C63 H78 N8 Ni7 O29'
_chemical_formula_weight         1822.19

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

_cell_length_a                   13.82410(10)
_cell_length_b                   13.82410(10)
_cell_length_c                   23.4073(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3873.96(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    29716
_cell_measurement_theta_min      2.4130
_cell_measurement_theta_max      30.0400

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_F_000             1668
_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    1.734
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
crysalispro 1.171.40.84a (rigaku oxford diffraction, 2020)
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(2)
_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 10.0000
_diffrn_reflns_number            74054
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.434
_diffrn_reflns_theta_max         25.347
_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             2379
_reflns_number_gt                2200
_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 1.171.40.84a (rigaku od, 2020)'
_computing_cell_refinement       'crysalispro 1.171.40.84a (rigaku od, 2020)'
_computing_data_reduction        'crysalispro 1.171.40.84a (rigaku od, 2020)'
_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          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)+(0.1256P)²+6.6319P] 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         2379
_refine_ls_number_parameters     143
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0575
_refine_ls_wR_factor_ref         0.1923
_refine_ls_wR_factor_gt          0.1884
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_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
Ni1 Ni 0.000000 0.000000 0.000000 0.0345(4) Uani 1 6 d S T P . .
O1 O 0.1358(2) 0.1247(2) 0.04378(14) 0.0400(7) Uani 1 1 d . . . . .
H1 H 0.132769 0.129654 0.085443 0.048 Uiso 1 1 calc R U . . .
N1 N 0.2032(4) 0.3827(3) -0.06726(18) 0.0483(10) Uani 1 1 d . . . . .
C1 C 0.1442(6) 0.4462(6) -0.0679(3) 0.081(2) Uani 1 1 d . . . . .
H1B H 0.168538 0.495707 -0.100184 0.121 Uiso 1 1 calc R U . . .
H1A H 0.160091 0.488853 -0.033368 0.121 Uiso 1 1 calc R U . . .
H1C H 0.065203 0.395466 -0.070703 0.121 Uiso 1 1 calc R U . . .
Ni2 Ni 0.25692(4) 0.10240(5) 0.00699(2) 0.0391(3) Uani 1 1 d . . . . .
O2 O 0.2797(2) 0.2391(3) -0.03390(14) 0.0401(7) Uani 1 1 d . . . . .
N2 N 0.333333 0.666667 -0.2022(3) 0.0532(17) Uani 1 3 d S T P . .
C2 C 0.2769(5) 0.4087(4) -0.1061(2) 0.0551(12) Uani 1 1 d . . . . .
H2 H 0.288710 0.466824 -0.130420 0.066 Uiso 1 1 calc R U . . .
O3 O 0.3951(3) 0.1417(3) -0.05876(16) 0.0502(8) Uani 1 1 d . . . . .
C3 C 0.3433(4) 0.3572(4) -0.1159(2) 0.0486(11) Uani 1 1 d . . . . .
O4 O 0.2339(5) 0.5907(5) -0.2008(3) 0.0962(16) Uani 1 1 d . . . . .
C4 C 0.4144(5) 0.3916(5) -0.1659(2) 0.0586(14) Uani 1 1 d . . . . .
H4 H 0.417224 0.446629 -0.189885 0.070 Uiso 1 1 calc R U . . .
C5 C 0.4763(5) 0.3440(6) -0.1777(2) 0.0616(14) Uani 1 1 d . . . . .
H5 H 0.522839 0.367968 -0.209524 0.074 Uiso 1 1 calc R U . . .
C6 C 0.4728(5) 0.2601(5) -0.1437(2) 0.0586(13) Uani 1 1 d . . . . .
H6 H 0.514782 0.226772 -0.153229 0.070 Uiso 1 1 calc R U . . .
C7 C 0.4070(4) 0.2270(4) -0.0961(2) 0.0483(12) Uani 1 1 d . . . . .
C8 C 0.3398(3) 0.2751(4) -0.08108(19) 0.0393(10) Uani 1 1 d . . . . .
C9 C 0.4957(5) 0.1384(6) -0.0484(3) 0.0734(18) Uani 1 1 d . . . . .
H9A H 0.517680 0.116353 -0.082648 0.110 Uiso 1 1 calc R U . . .
H9B H 0.482831 0.085520 -0.018577 0.110 Uiso 1 1 calc R U . . .
H9C H 0.554004 0.211105 -0.036885 0.110 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.076(3) . ?
Ni1 O1 2.076(3) 7 ?
Ni1 O1 2.076(3) 9 ?
Ni1 O1 2.076(3) 3 ?
Ni1 O1 2.076(3) 2 ?
Ni1 O1 2.076(3) 8 ?
O1 Ni2 2.039(3) . ?
O1 Ni2 2.085(3) 9 ?
N1 C2 1.275(7) . ?
N1 C1 1.467(7) . ?
N1 Ni2 2.072(4) 9 ?
Ni2 O2 1.969(3) 8 ?
Ni2 O2 1.998(3) . ?
Ni2 O3 2.297(3) . ?
O2 C8 1.321(5) . ?
N2 O4 1.245(6) 3_565 ?
N2 O4 1.245(6) . ?
N2 O4 1.245(6) 2_665 ?
C2 C3 1.434(7) . ?
O3 C7 1.410(6) . ?
O3 C9 1.435(6) . ?
C3 C8 1.378(7) . ?
C3 C4 1.449(7) . ?
C4 C5 1.344(8) . ?
C5 C6 1.388(8) . ?
C6 C7 1.365(7) . ?
C7 C8 1.430(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.00(15) . 7 ?
O1 Ni1 O1 82.28(11) . 9 ?
O1 Ni1 O1 97.73(11) 7 9 ?
O1 Ni1 O1 97.72(11) . 3 ?
O1 Ni1 O1 82.27(11) 7 3 ?
O1 Ni1 O1 180.0(2) 9 3 ?
O1 Ni1 O1 97.73(11) . 2 ?
O1 Ni1 O1 82.27(11) 7 2 ?
O1 Ni1 O1 82.27(11) 9 2 ?
O1 Ni1 O1 97.73(11) 3 2 ?
O1 Ni1 O1 82.27(11) . 8 ?
O1 Ni1 O1 97.73(11) 7 8 ?
O1 Ni1 O1 97.73(11) 9 8 ?
O1 Ni1 O1 82.27(11) 3 8 ?
O1 Ni1 O1 180.0(2) 2 8 ?
Ni2 O1 Ni1 97.81(13) . . ?
Ni2 O1 Ni2 98.06(12) . 9 ?
Ni1 O1 Ni2 96.38(13) . 9 ?
C2 N1 C1 115.3(4) . . ?
C2 N1 Ni2 126.9(4) . 9 ?
C1 N1 Ni2 117.7(3) . 9 ?
O2 Ni2 O2 169.80(7) 8 . ?
O2 Ni2 O1 108.46(13) 8 . ?
O2 Ni2 O1 79.16(12) . . ?
O2 Ni2 N1 87.15(15) 8 8 ?
O2 Ni2 N1 98.33(15) . 8 ?
O1 Ni2 N1 100.14(15) . 8 ?
O2 Ni2 O1 78.73(12) 8 8 ?
O2 Ni2 O1 95.89(13) . 8 ?
O1 Ni2 O1 82.93(16) . 8 ?
N1 Ni2 O1 165.78(15) 8 8 ?
O2 Ni2 O3 97.11(13) 8 . ?
O2 Ni2 O3 74.71(12) . . ?
O1 Ni2 O3 153.64(12) . . ?
N1 Ni2 O3 87.13(16) 8 . ?
O1 Ni2 O3 96.23(13) 8 . ?
C8 O2 Ni2 130.3(3) . 9 ?
C8 O2 Ni2 121.9(3) . . ?
Ni2 O2 Ni2 103.45(13) 9 . ?
O4 N2 O4 119.94(4) 3_565 . ?
O4 N2 O4 119.94(4) 3_565 2_665 ?
O4 N2 O4 119.94(4) . 2_665 ?
N1 C2 C3 126.3(5) . . ?
C7 O3 C9 115.0(4) . . ?
C7 O3 Ni2 110.4(3) . . ?
C9 O3 Ni2 125.7(4) . . ?
C8 C3 C2 123.2(5) . . ?
C8 C3 C4 119.1(5) . . ?
C2 C3 C4 117.6(5) . . ?
C5 C4 C3 119.9(5) . . ?
C4 C5 C6 121.8(5) . . ?
C7 C6 C5 119.1(5) . . ?
C6 C7 O3 124.4(5) . . ?
C6 C7 C8 121.6(5) . . ?
O3 C7 C8 113.9(4) . . ?
O2 C8 C3 124.1(5) . . ?
O2 C8 C7 117.6(4) . . ?
C3 C8 C7 118.3(4) . . ?

_refine_diff_density_max         2.598
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.118



# 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 0.000 0.250 497 108 ' '
2 0.000 0.000 0.750 497 108 ' '
3 0.333 0.667 0.458 8 0 ' '
4 0.333 0.667 0.958 8 0 ' '
5 0.667 0.333 0.042 8 0 ' '
6 0.667 0.333 0.542 8 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_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_sm353sq
_database_code_depnum_ccdc_archive 'CCDC 2403823'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        3-Fur-Ni7
_chemical_name_common            '[3-fur-Ni7].3H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C59 H76 N8 Ni7 O29'
_chemical_formula_weight         1772.13

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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

_cell_length_a                   13.8183(5)
_cell_length_b                   13.8183(5)
_cell_length_c                   23.1848(14)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3833.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.1(1)
_cell_measurement_reflns_used    2651
_cell_measurement_theta_min      3.0703
_cell_measurement_theta_max      29.1647

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_F_000             1668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.752
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.75185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.1(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            7199
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.076
_diffrn_reflns_theta_max         25.336
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2344
_reflns_number_gt                1771
_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, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_cell_refinement       
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_data_reduction        
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_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          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)+(0.1187P)²+15.9166P] 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         2344
_refine_ls_number_parameters     143
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0793
_refine_ls_wR_factor_ref         0.2398
_refine_ls_wR_factor_gt          0.2261
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_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
Ni1 Ni 0.000000 0.000000 0.000000 0.0373(6) Uani 1 6 d S T P . .
O1 O -0.0116(4) -0.1352(4) -0.0440(2) 0.0396(11) Uani 1 1 d . . . . .
H1 H -0.004848 -0.132500 -0.086993 0.048 Uiso 1 1 calc R U . . .
N1 N -0.2028(7) -0.3824(5) -0.0681(3) 0.0577(18) Uani 1 1 d . . . . .
C1 C -0.1373(13) -0.4427(11) -0.0710(6) 0.113(5) Uani 1 1 d . . . . .
H1A H -0.167115 -0.498229 -0.102072 0.169 Uiso 1 1 calc R U . . .
H1B H -0.143760 -0.480303 -0.034210 0.169 Uiso 1 1 calc R U . . .
H1C H -0.058590 -0.388789 -0.078723 0.169 Uiso 1 1 calc R U . . .
Ni2 Ni -0.15281(8) -0.25708(7) -0.00603(4) 0.0456(4) Uani 1 1 d . . . . .
O2 O -0.2797(4) -0.2414(4) -0.0334(2) 0.0414(11) Uani 1 1 d . . . . .
N2 N -0.666667 -0.333333 -0.2947(9) 0.087(5) Uani 1 3 d S T P . .
C2 C -0.2730(8) -0.4086(8) -0.1068(4) 0.068(2) Uani 1 1 d . . . . .
H2 H -0.282003 -0.465789 -0.132759 0.082 Uiso 1 1 calc R U . . .
O3 O -0.3957(5) -0.1456(5) -0.0576(3) 0.0614(16) Uani 1 1 d . . . . .
C3 C -0.3397(7) -0.3607(7) -0.1155(4) 0.059(2) Uani 1 1 d . . . . .
O4 O -0.6514(9) -0.4143(10) -0.2935(5) 0.138(4) Uani 1 1 d . . . . .
C4 C -0.4154(8) -0.3974(9) -0.1667(4) 0.068(3) Uani 1 1 d . . . . .
H4 H -0.422215 -0.455815 -0.191011 0.081 Uiso 1 1 calc R U . . .
C5 C -0.4735(8) -0.3452(9) -0.1772(4) 0.068(2) Uani 1 1 d . . . . .
H5 H -0.516776 -0.364515 -0.211483 0.082 Uiso 1 1 calc R U . . .
C6 C -0.4750(8) -0.2677(9) -0.1427(4) 0.072(3) Uani 1 1 d . . . . .
H6 H -0.521748 -0.237183 -0.150902 0.086 Uiso 1 1 calc R U . . .
C7 C -0.4088(7) -0.2353(7) -0.0968(4) 0.061(2) Uani 1 1 d . . . . .
C8 C -0.3384(6) -0.2793(6) -0.0804(3) 0.0425(17) Uani 1 1 d . . . . .
C9 C -0.4929(11) -0.1370(14) -0.0490(6) 0.118(5) Uani 1 1 d . . . . .
H9A H -0.558563 -0.205038 -0.063076 0.177 Uiso 1 1 calc R U . . .
H9B H -0.485476 -0.072229 -0.070112 0.177 Uiso 1 1 calc R U . . .
H9C H -0.501821 -0.127925 -0.007734 0.177 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.063(4) 9 ?
Ni1 O1 2.063(4) 3 ?
Ni1 O1 2.063(4) . ?
Ni1 O1 2.063(4) 2 ?
Ni1 O1 2.063(4) 8 ?
Ni1 O1 2.063(4) 7 ?
O1 Ni2 2.033(5) . ?
O1 Ni2 2.088(5) 9 ?
O1 H1 1.0000 . ?
N1 C2 1.236(11) . ?
N1 C1 1.508(13) . ?
N1 Ni2 2.085(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Ni2 O2 1.976(5) . ?
Ni2 O2 1.984(5) 9 ?
Ni2 O3 2.254(6) 9 ?
O2 C8 1.300(8) . ?
N2 O4 1.238(12) 3_445 ?
N2 O4 1.238(12) 2_455 ?
N2 O4 1.238(12) . ?
C2 C3 1.392(13) . ?
C2 H2 0.9500 . ?
O3 C9 1.420(11) . ?
O3 C7 1.474(11) . ?
C3 C8 1.382(11) . ?
C3 C4 1.493(13) . ?
C4 C5 1.343(13) . ?
C4 H4 0.9500 . ?
C5 C6 1.345(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.326(12) . ?
C6 H6 0.9500 . ?
C7 C8 1.433(12) . ?
C9 H9A 0.9800 . ?
C9 H9B 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 Ni1 O1 180.0(3) 9 3 ?
O1 Ni1 O1 82.34(17) 9 . ?
O1 Ni1 O1 97.66(17) 3 . ?
O1 Ni1 O1 82.34(17) 9 2 ?
O1 Ni1 O1 97.66(17) 3 2 ?
O1 Ni1 O1 97.66(17) . 2 ?
O1 Ni1 O1 97.66(17) 9 8 ?
O1 Ni1 O1 82.34(17) 3 8 ?
O1 Ni1 O1 82.34(17) . 8 ?
O1 Ni1 O1 180.0(5) 2 8 ?
O1 Ni1 O1 97.66(17) 9 7 ?
O1 Ni1 O1 82.34(17) 3 7 ?
O1 Ni1 O1 180.0 . 7 ?
O1 Ni1 O1 82.34(17) 2 7 ?
O1 Ni1 O1 97.66(17) 8 7 ?
Ni2 O1 Ni1 98.3(2) . . ?
Ni2 O1 Ni2 97.88(19) . 9 ?
Ni1 O1 Ni2 96.5(2) . 9 ?
Ni2 O1 H1 119.7 . . ?
Ni1 O1 H1 119.7 . . ?
Ni2 O1 H1 119.7 9 . ?
C2 N1 C1 113.8(8) . . ?
C2 N1 Ni2 129.1(7) . . ?
C1 N1 Ni2 116.7(6) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Ni2 O2 170.83(12) . 9 ?
O2 Ni2 O1 107.9(2) . . ?
O2 Ni2 O1 79.58(18) 9 . ?
O2 Ni2 N1 85.7(3) . . ?
O2 Ni2 N1 98.4(3) 9 . ?
O1 Ni2 N1 99.9(2) . . ?
O2 Ni2 O1 78.44(19) . 8 ?
O2 Ni2 O1 97.7(2) 9 8 ?
O1 Ni2 O1 82.5(2) . 8 ?
N1 Ni2 O1 163.9(2) . 8 ?
O2 Ni2 O3 96.8(2) . 9 ?
O2 Ni2 O3 75.4(2) 9 9 ?
O1 Ni2 O3 154.9(2) . 9 ?
N1 Ni2 O3 86.4(3) . 9 ?
O1 Ni2 O3 98.2(2) 8 9 ?
C8 O2 Ni2 129.3(5) . . ?
C8 O2 Ni2 122.6(5) . 8 ?
Ni2 O2 Ni2 103.4(2) . 8 ?
O4 N2 O4 119.95(9) 3_445 2_455 ?
O4 N2 O4 119.96(9) 3_445 . ?
O4 N2 O4 119.95(9) 2_455 . ?
N1 C2 C3 125.0(9) . . ?
N1 C2 H2 117.5 . . ?
C3 C2 H2 117.5 . . ?
C9 O3 C7 115.7(8) . . ?
C9 O3 Ni2 127.3(7) . 8 ?
C7 O3 Ni2 110.3(4) . 8 ?
C8 C3 C2 124.1(9) . . ?
C8 C3 C4 117.8(8) . . ?
C2 C3 C4 118.1(8) . . ?
C5 C4 C3 117.9(9) . . ?
C5 C4 H4 121.1 . . ?
C3 C4 H4 121.1 . . ?
C4 C5 C6 124.9(9) . . ?
C4 C5 H5 117.6 . . ?
C6 C5 H5 117.6 . . ?
C7 C6 C5 117.5(10) . . ?
C7 C6 H6 121.3 . . ?
C5 C6 H6 121.3 . . ?
C6 C7 C8 124.9(9) . . ?
C6 C7 O3 123.4(9) . . ?
C8 C7 O3 111.7(7) . . ?
O2 C8 C3 124.9(7) . . ?
O2 C8 C7 118.1(7) . . ?
C3 C8 C7 116.9(8) . . ?
O3 C9 H9A 109.5 . . ?
O3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_refine_diff_density_max         1.545
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.130


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.250 481 82 ' '
2 0.000 0.000 0.750 481 82 ' '
3 0.333 0.666 0.067 11 1 ' '
4 0.333 0.666 0.567 11 1 ' '
5 0.666 0.333 0.433 11 1 ' '
6 0.666 0.333 0.933 11 1 ' '
_platon_squeeze_details          
;
;




_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_sm353asq
_database_code_depnum_ccdc_archive 'CCDC 2403824'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        3-Fur-Co7
_chemical_name_common            '[3-fur-Co7].4.5H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C59 H79 Co7 N8 O30.5'
_chemical_formula_weight         1800.83

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

_cell_length_a                   14.098(2)
_cell_length_b                   14.098(2)
_cell_length_c                   22.706(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3908.5(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    2502
_cell_measurement_theta_min      3.0197
_cell_measurement_theta_max      29.0946

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_F_000             1654
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.518
_shelx_estimated_absorpt_T_min   0.888
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.45939
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'xcalibur, sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1048
_diffrn_reflns_number            7890
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.026
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2388
_reflns_number_gt                1561
_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, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_cell_refinement       
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_computing_data_reduction        
; 
crysalispro, oxford diffraction ltd., 
version 1.171.34.36 (release 02-08-2010 crysalis171 .net) 
(compiled aug  2 2010,13:00:58) 
;
_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          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)+(0.1391P)²+11.4781P] 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         2388
_refine_ls_number_parameters     143
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1275
_refine_ls_R_factor_gt           0.0936
_refine_ls_wR_factor_ref         0.2778
_refine_ls_wR_factor_gt          0.2519
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
Co1 Co 0.000000 0.000000 0.000000 0.0309(7) Uani 1 6 d S T P . .
O1 O -0.1265(4) 0.0042(4) -0.0465(2) 0.0369(14) Uani 1 1 d . . . . .
H1 H -0.133565 -0.008090 -0.089987 0.044 Uiso 1 1 calc R U . . .
N1 N -0.1837(6) 0.1942(7) -0.0759(3) 0.0464(19) Uani 1 1 d . . . . .
C1 C 0.3460(8) 0.4912(8) -0.0453(5) 0.060(3) Uani 1 1 d . . . . .
H1A H 0.393256 0.494011 -0.077747 0.090 Uiso 1 1 calc R U . . .
H1B H 0.376198 0.483818 -0.007874 0.090 Uiso 1 1 calc R U . . .
H1C H 0.342221 0.558748 -0.044974 0.090 Uiso 1 1 calc R U . . .
Co2 Co -0.11025(10) 0.14407(10) -0.01214(5) 0.0385(5) Uani 1 1 d . . . . .
O2 O 0.0320(4) 0.2752(5) -0.0346(2) 0.0362(13) Uani 1 1 d . . . . .
N2 N 0.333333 0.666667 -0.2927(7) 0.057(4) Uani 1 3 d S T P . .
C2 C 0.1690(7) 0.4117(7) -0.0921(4) 0.039(2) Uani 1 1 d . . . . .
O3 O 0.2379(5) 0.3988(5) -0.0533(3) 0.0466(16) Uani 1 1 d . . . . .
C3 C 0.2049(9) 0.4844(9) -0.1382(4) 0.055(3) Uani 1 1 d . . . . .
H3 H 0.280942 0.532457 -0.144607 0.066 Uiso 1 1 calc R U . . .
O4 O 0.2404(8) 0.6537(8) -0.2917(4) 0.099(3) Uani 1 1 d . . . . .
C4 C 0.1257(9) 0.4857(8) -0.1758(4) 0.054(3) Uani 1 1 d . . . . .
H4 H 0.149308 0.533783 -0.208743 0.065 Uiso 1 1 calc R U . . .
C5 C 0.0181(8) 0.4209(8) -0.1663(4) 0.044(2) Uani 1 1 d . . . . .
H5 H -0.033205 0.425558 -0.191503 0.053 Uiso 1 1 calc R U . . .
C6 C -0.0204(8) 0.3441(7) -0.1180(4) 0.046(2) Uani 1 1 d . . . . .
C7 C 0.0564(7) 0.3415(6) -0.0798(3) 0.0298(17) Uani 1 1 d . . . . .
C8 C -0.1390(8) 0.2721(8) -0.1119(4) 0.046(2) Uani 1 1 d . . . . .
H8 H -0.185280 0.285091 -0.136950 0.055 Uiso 1 1 calc R U . . .
C9 C -0.3075(8) 0.1251(10) -0.0799(5) 0.070(3) Uani 1 1 d . . . . .
H9A H -0.334812 0.158806 -0.107857 0.106 Uiso 1 1 calc R U . . .
H9B H -0.339636 0.120495 -0.041045 0.106 Uiso 1 1 calc R U . . .
H9C H -0.327853 0.051307 -0.093525 0.106 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.099(5) . ?
Co1 O1 2.099(5) 8 ?
Co1 O1 2.099(5) 2 ?
Co1 O1 2.099(5) 7 ?
Co1 O1 2.099(5) 9 ?
Co1 O1 2.099(5) 3 ?
O1 Co2 2.023(6) . ?
O1 Co2 2.171(6) 9 ?
O1 H1 1.0000 . ?
N1 C8 1.258(11) . ?
N1 C9 1.518(12) . ?
N1 Co2 2.096(7) . ?
C1 O3 1.438(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Co2 O2 1.998(5) . ?
Co2 O2 2.043(6) 9 ?
Co2 O3 2.327(6) 9 ?
O2 C7 1.314(9) . ?
N2 O4 1.229(10) . ?
N2 O4 1.229(10) 3_565 ?
N2 O4 1.229(10) 2_665 ?
C2 C3 1.372(13) . ?
C2 O3 1.388(11) . ?
C2 C7 1.417(12) . ?
C3 C4 1.415(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.340(14) . ?
C4 H4 0.9500 . ?
C5 C6 1.442(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.402(12) . ?
C6 C8 1.466(13) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 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 Co1 O1 83.0(2) . 8 ?
O1 Co1 O1 97.0(2) . 2 ?
O1 Co1 O1 180.0(4) 8 2 ?
O1 Co1 O1 180.0 . 7 ?
O1 Co1 O1 97.0(2) 8 7 ?
O1 Co1 O1 83.0(2) 2 7 ?
O1 Co1 O1 83.0(2) . 9 ?
O1 Co1 O1 97.0(2) 8 9 ?
O1 Co1 O1 83.0(2) 2 9 ?
O1 Co1 O1 97.0(2) 7 9 ?
O1 Co1 O1 97.0(2) . 3 ?
O1 Co1 O1 83.0(2) 8 3 ?
O1 Co1 O1 97.0(2) 2 3 ?
O1 Co1 O1 83.0(2) 7 3 ?
O1 Co1 O1 180.0(6) 9 3 ?
Co2 O1 Co1 98.6(2) . . ?
Co2 O1 Co2 97.8(2) . 9 ?
Co1 O1 Co2 94.1(2) . 9 ?
Co2 O1 H1 120.2 . . ?
Co1 O1 H1 120.2 . . ?
Co2 O1 H1 120.2 9 . ?
C8 N1 C9 115.7(8) . . ?
C8 N1 Co2 128.9(7) . . ?
C9 N1 Co2 115.4(6) . . ?
O3 C1 H1A 109.5 . . ?
O3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Co2 O1 112.1(2) . . ?
O2 Co2 O2 163.02(13) . 9 ?
O1 Co2 O2 80.4(2) . 9 ?
O2 Co2 N1 87.1(3) . . ?
O1 Co2 N1 103.2(3) . . ?
O2 Co2 N1 101.7(3) 9 . ?
O2 Co2 O1 77.9(2) . 8 ?
O1 Co2 O1 83.1(3) . 8 ?
O2 Co2 O1 92.8(2) 9 8 ?
N1 Co2 O1 164.9(3) . 8 ?
O2 Co2 O3 95.1(2) . 9 ?
O1 Co2 O3 151.9(2) . 9 ?
O2 Co2 O3 71.6(2) 9 9 ?
N1 Co2 O3 84.6(3) . 9 ?
O1 Co2 O3 96.3(2) 8 9 ?
C7 O2 Co2 130.0(5) . . ?
C7 O2 Co2 124.2(5) . 8 ?
Co2 O2 Co2 103.0(2) . 8 ?
O4 N2 O4 119.97(7) . 3_565 ?
O4 N2 O4 119.97(7) . 2_665 ?
O4 N2 O4 119.97(7) 3_565 2_665 ?
C3 C2 O3 124.1(8) . . ?
C3 C2 C7 122.6(9) . . ?
O3 C2 C7 113.4(7) . . ?
C2 O3 C1 117.1(7) . . ?
C2 O3 Co2 113.0(5) . 8 ?
C1 O3 Co2 126.4(6) . 8 ?
C2 C3 C4 118.2(10) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 121.7(9) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 120.5(9) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 119.0(9) . . ?
C7 C6 C8 123.5(9) . . ?
C5 C6 C8 117.5(8) . . ?
O2 C7 C6 124.9(8) . . ?
O2 C7 C2 117.0(7) . . ?
C6 C7 C2 118.1(8) . . ?
N1 C8 C6 124.5(9) . . ?
N1 C8 H8 117.8 . . ?
C6 C8 H8 117.8 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_refine_diff_density_max         1.577
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.150


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.250 479 98 ' '
2 0.000 0.000 0.750 479 98 ' '
3 0.333 0.667 0.561 21 4 ' '
4 0.333 0.667 0.061 21 4 ' '
5 0.667 0.333 0.939 21 4 ' '
6 0.667 0.333 0.439 21 4 ' '
_platon_squeeze_details          ?
_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_bzal-zn7sq
_database_code_depnum_ccdc_archive 'CCDC 2403825'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2025-05-09 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            Bzal-Zn7.5H2O
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C67 H82 N8 O30 Zn7'
_chemical_formula_weight         1937.05

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      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

_cell_length_a                   14.010
_cell_length_b                   14.010
_cell_length_c                   23.002
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3909.9
_cell_formula_units_Z            2
_cell_measurement_temperature    173.0(2)
_cell_measurement_reflns_used    6611
_cell_measurement_theta_min      1.627
_cell_measurement_theta_max      36.064

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             1792
_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    2.184
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_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      173.0(2)
_diffrn_radiation_wavelength     0.6889
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'Dectris, PILATUS 2M'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            82320
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.627
_diffrn_reflns_theta_max         36.064
_diffrn_reflns_theta_full        24.415
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6611
_reflns_number_gt                6212
_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       'gda 8.44; generic data acquisition software'
_computing_cell_refinement       
'xia2 0.4.0.438-g4431aaa, winter, g. (2010) j. appl. cryst. 43'
_computing_data_reduction        
'xia2 0.4.0.438-g4431aaa, winter, g. (2010) j. appl. cryst. 43'
_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          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)+(0.0820P)²+3.4688P] 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         6611
_refine_ls_number_parameters     153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1373
_refine_ls_wR_factor_gt          0.1360
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
Zn1 Zn 0.000000 0.000000 0.500000 0.01694(8) Uani 1 6 d S T P . .
O1 O 0.00212(10) -0.13031(9) 0.54533(5) 0.01955(18) Uani 1 1 d . . . . .
N1 N 0.19716(13) -0.18286(11) 0.57432(7) 0.0248(2) Uani 1 1 d . . . . .
C1 C 0.49629(14) 0.35240(14) 0.54681(10) 0.0292(3) Uani 1 1 d . . . . .
H1A H 0.507609 0.397269 0.581579 0.044 Uiso 1 1 calc R U . . .
H1B H 0.483844 0.387715 0.513160 0.044 Uiso 1 1 calc R U . . .
H1C H 0.561722 0.345659 0.539985 0.044 Uiso 1 1 calc R U . . .
Zn2 Zn 0.14594(2) -0.10930(2) 0.51196(2) 0.01865(6) Uani 1 1 d . . . . .
O2 O 0.28125(9) 0.03563(9) 0.53393(5) 0.01969(18) Uani 1 1 d . . . . .
N2 N 0.666667 0.333333 0.79558(13) 0.0339(6) Uani 1 3 d S T P . .
C2 C 0.41311(12) 0.17537(13) 0.59361(7) 0.0212(2) Uani 1 1 d . . . . .
O3 O 0.40214(10) 0.24487(10) 0.55514(6) 0.0243(2) Uani 1 1 d . . . . .
C3 C 0.48162(14) 0.20983(14) 0.64175(8) 0.0264(3) Uani 1 1 d . . . . .
H3 H 0.526791 0.286225 0.649736 0.032 Uiso 1 1 calc R U . . .
O4 O 0.64882(18) 0.23645(16) 0.79575(9) 0.0481(4) Uani 1 1 d . . . . .
C4 C 0.48397(15) 0.13161(15) 0.67853(8) 0.0280(3) Uani 1 1 d . . . . .
H4 H 0.531333 0.154870 0.711417 0.034 Uiso 1 1 calc R U . . .
C5 C 0.41767(14) 0.02076(14) 0.66716(7) 0.0250(3) Uani 1 1 d . . . . .
H5 H 0.420337 -0.031813 0.692172 0.030 Uiso 1 1 calc R U . . .
C6 C 0.34574(12) -0.01578(12) 0.61877(7) 0.0203(2) Uani 1 1 d . . . . .
C7 C 0.34358(11) 0.06187(12) 0.58066(6) 0.0180(2) Uani 1 1 d . . . . .
C8 C 0.27439(14) -0.13428(13) 0.61210(7) 0.0240(3) Uani 1 1 d . . . . .
H8 H 0.286021 -0.180095 0.638167 0.029 Uiso 1 1 calc R U . . .
C9 C 0.1334(2) -0.30337(16) 0.57724(11) 0.0404(5) Uani 1 1 d . . . . .
H9A H 0.167338 -0.329684 0.605535 0.061 Uiso 1 1 calc R U . . .
H9B H 0.132537 -0.334236 0.538886 0.061 Uiso 1 1 calc R U . . .
H9C H 0.057733 -0.326820 0.589269 0.061 Uiso 1 1 calc R U . . .
C10 C -0.0126(3) -0.1440(2) 0.60755(11) 0.0461(5) Uani 1 1 d . . . . .
H10A H -0.013461 -0.211703 0.619275 0.069 Uiso 1 1 calc R U . . .
H10B H -0.082500 -0.148899 0.618437 0.069 Uiso 1 1 calc R U . . .
H10C H 0.048330 -0.080713 0.627127 0.069 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 2.1154(11) . ?
Zn1 O1 2.1154(11) 8_556 ?
Zn1 O1 2.1154(11) 2 ?
Zn1 O1 2.1154(11) 7_556 ?
Zn1 O1 2.1154(11) 9_556 ?
Zn1 O1 2.1154(11) 3 ?
Zn1 Zn2 3.11947(17) 8_556 ?
Zn1 Zn2 3.11947(17) 2 ?
Zn1 Zn2 3.11947(17) 9_556 ?
Zn1 Zn2 3.11947(17) 3 ?
Zn1 Zn2 3.11946(17) 7_556 ?
Zn1 Zn2 3.11947(17) . ?
O1 C10 1.445(3) . ?
O1 Zn2 2.0353(11) . ?
O1 Zn2 2.1223(11) 8_556 ?
N1 C8 1.286(2) . ?
N1 C9 1.464(2) . ?
N1 Zn2 2.0915(14) . ?
C1 O3 1.435(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Zn2 O2 2.0304(11) . ?
Zn2 O2 2.0492(11) 8_556 ?
Zn2 O3 2.3847(12) 8_556 ?
Zn2 Zn2 3.15564(17) 9_556 ?
Zn2 Zn2 3.15571(18) 8_556 ?
O2 C7 1.3160(17) . ?
N2 O4 1.251(2) . ?
N2 O4 1.251(2) 2_655 ?
N2 O4 1.251(2) 3_665 ?
C2 O3 1.380(2) . ?
C2 C3 1.385(2) . ?
C2 C7 1.420(2) . ?
C3 C4 1.398(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.378(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.414(2) . ?
C5 H5 0.9500 . ?
C6 C7 1.409(2) . ?
C6 C8 1.456(2) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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 82.21(4) . 8_556 ?
O1 Zn1 O1 97.79(4) . 2 ?
O1 Zn1 O1 180.0 8_556 2 ?
O1 Zn1 O1 180.0 . 7_556 ?
O1 Zn1 O1 97.79(4) 8_556 7_556 ?
O1 Zn1 O1 82.21(4) 2 7_556 ?
O1 Zn1 O1 82.21(4) . 9_556 ?
O1 Zn1 O1 97.79(4) 8_556 9_556 ?
O1 Zn1 O1 82.21(4) 2 9_556 ?
O1 Zn1 O1 97.79(4) 7_556 9_556 ?
O1 Zn1 O1 97.79(4) . 3 ?
O1 Zn1 O1 82.21(4) 8_556 3 ?
O1 Zn1 O1 97.79(4) 2 3 ?
O1 Zn1 O1 82.21(4) 7_556 3 ?
O1 Zn1 O1 180.0 9_556 3 ?
O1 Zn1 Zn2 42.68(3) . 8_556 ?
O1 Zn1 Zn2 40.31(3) 8_556 8_556 ?
O1 Zn1 Zn2 139.69(3) 2 8_556 ?
O1 Zn1 Zn2 137.32(3) 7_556 8_556 ?
O1 Zn1 Zn2 84.09(3) 9_556 8_556 ?
O1 Zn1 Zn2 95.91(3) 3 8_556 ?
O1 Zn1 Zn2 137.32(3) . 2 ?
O1 Zn1 Zn2 139.69(3) 8_556 2 ?
O1 Zn1 Zn2 40.31(3) 2 2 ?
O1 Zn1 Zn2 42.68(3) 7_556 2 ?
O1 Zn1 Zn2 95.91(3) 9_556 2 ?
O1 Zn1 Zn2 84.09(3) 3 2 ?
Zn2 Zn1 Zn2 180.0 8_556 2 ?
O1 Zn1 Zn2 95.91(3) . 9_556 ?
O1 Zn1 Zn2 137.32(3) 8_556 9_556 ?
O1 Zn1 Zn2 42.68(3) 2 9_556 ?
O1 Zn1 Zn2 84.09(3) 7_556 9_556 ?
O1 Zn1 Zn2 40.31(3) 9_556 9_556 ?
O1 Zn1 Zn2 139.69(3) 3 9_556 ?
Zn2 Zn1 Zn2 119.231(1) 8_556 9_556 ?
Zn2 Zn1 Zn2 60.769(1) 2 9_556 ?
O1 Zn1 Zn2 84.09(3) . 3 ?
O1 Zn1 Zn2 42.68(3) 8_556 3 ?
O1 Zn1 Zn2 137.32(3) 2 3 ?
O1 Zn1 Zn2 95.91(3) 7_556 3 ?
O1 Zn1 Zn2 139.69(3) 9_556 3 ?
O1 Zn1 Zn2 40.31(3) 3 3 ?
Zn2 Zn1 Zn2 60.769(1) 8_556 3 ?
Zn2 Zn1 Zn2 119.231(1) 2 3 ?
Zn2 Zn1 Zn2 180.0 9_556 3 ?
O1 Zn1 Zn2 139.69(3) . 7_556 ?
O1 Zn1 Zn2 84.09(3) 8_556 7_556 ?
O1 Zn1 Zn2 95.91(3) 2 7_556 ?
O1 Zn1 Zn2 40.31(3) 7_556 7_556 ?
O1 Zn1 Zn2 137.32(3) 9_556 7_556 ?
O1 Zn1 Zn2 42.68(3) 3 7_556 ?
Zn2 Zn1 Zn2 119.231(1) 8_556 7_556 ?
Zn2 Zn1 Zn2 60.769(1) 2 7_556 ?
Zn2 Zn1 Zn2 119.231(1) 9_556 7_556 ?
Zn2 Zn1 Zn2 60.769(1) 3 7_556 ?
O1 Zn1 Zn2 40.31(3) . . ?
O1 Zn1 Zn2 95.91(3) 8_556 . ?
O1 Zn1 Zn2 84.09(3) 2 . ?
O1 Zn1 Zn2 139.69(3) 7_556 . ?
O1 Zn1 Zn2 42.68(3) 9_556 . ?
O1 Zn1 Zn2 137.32(3) 3 . ?
Zn2 Zn1 Zn2 60.770(1) 8_556 . ?
Zn2 Zn1 Zn2 119.230(1) 2 . ?
Zn2 Zn1 Zn2 60.769(1) 9_556 . ?
Zn2 Zn1 Zn2 119.231(1) 3 . ?
Zn2 Zn1 Zn2 180.0 7_556 . ?
C10 O1 Zn2 117.23(14) . . ?
C10 O1 Zn1 122.71(13) . . ?
Zn2 O1 Zn1 97.43(5) . . ?
C10 O1 Zn2 120.55(13) . 8_556 ?
Zn2 O1 Zn2 98.73(4) . 8_556 ?
Zn1 O1 Zn2 94.80(4) . 8_556 ?
C8 N1 C9 116.48(14) . . ?
C8 N1 Zn2 127.45(11) . . ?
C9 N1 Zn2 115.97(11) . . ?
O3 C1 H1A 109.5 . . ?
O3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Zn2 O1 114.37(5) . . ?
O2 Zn2 O2 162.22(3) . 8_556 ?
O1 Zn2 O2 80.14(4) . 8_556 ?
O2 Zn2 N1 86.75(5) . . ?
O1 Zn2 N1 103.23(6) . . ?
O2 Zn2 N1 100.30(5) 8_556 . ?
O2 Zn2 O1 78.53(4) . 9_556 ?
O1 Zn2 O1 83.95(6) . 9_556 ?
O2 Zn2 O1 93.58(4) 8_556 9_556 ?
N1 Zn2 O1 165.25(5) . 9_556 ?
O2 Zn2 O3 93.40(5) . 8_556 ?
O1 Zn2 O3 151.18(4) . 8_556 ?
O2 Zn2 O3 71.19(4) 8_556 8_556 ?
N1 Zn2 O3 85.07(6) . 8_556 ?
O1 Zn2 O3 94.79(5) 9_556 8_556 ?
O2 Zn2 Zn1 92.55(3) . . ?
O1 Zn2 Zn1 42.25(3) . . ?
O2 Zn2 Zn1 92.18(3) 8_556 . ?
N1 Zn2 Zn1 140.62(5) . . ?
O1 Zn2 Zn1 42.51(3) 9_556 . ?
O3 Zn2 Zn1 134.20(3) 8_556 . ?
O2 Zn2 Zn2 39.54(3) . 9_556 ?
O1 Zn2 Zn2 96.55(3) . 9_556 ?
O2 Zn2 Zn2 132.75(3) 8_556 9_556 ?
N1 Zn2 Zn2 125.90(4) . 9_556 ?
O1 Zn2 Zn2 39.60(3) 9_556 9_556 ?
O3 Zn2 Zn2 100.68(4) 8_556 9_556 ?
Zn1 Zn2 Zn2 59.616(1) . 9_556 ?
O2 Zn2 Zn2 151.67(3) . 8_556 ?
O1 Zn2 Zn2 41.66(3) . 8_556 ?
O2 Zn2 Zn2 39.11(3) 8_556 8_556 ?
N1 Zn2 Zn2 110.93(4) . 8_556 ?
O1 Zn2 Zn2 83.07(3) 9_556 8_556 ?
O3 Zn2 Zn2 109.54(3) 8_556 8_556 ?
Zn1 Zn2 Zn2 59.615(1) . 8_556 ?
Zn2 Zn2 Zn2 117.024(4) 9_556 8_556 ?
C7 O2 Zn2 129.79(9) . . ?
C7 O2 Zn2 123.61(10) . 9_556 ?
Zn2 O2 Zn2 101.34(5) . 9_556 ?
O4 N2 O4 119.999(4) . 2_655 ?
O4 N2 O4 119.999(4) . 3_665 ?
O4 N2 O4 119.999(4) 2_655 3_665 ?
O3 C2 C3 124.69(14) . . ?
O3 C2 C7 113.55(13) . . ?
C3 C2 C7 121.72(14) . . ?
C2 O3 C1 117.27(13) . . ?
C2 O3 Zn2 111.91(9) . 9_556 ?
C1 O3 Zn2 126.65(11) . 9_556 ?
C2 C3 C4 119.65(15) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.10(15) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.93(15) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C7 C6 C5 119.77(14) . . ?
C7 C6 C8 123.18(13) . . ?
C5 C6 C8 117.03(14) . . ?
O2 C7 C6 124.05(13) . . ?
O2 C7 C2 118.15(13) . . ?
C6 C7 C2 117.81(13) . . ?
N1 C8 C6 126.24(14) . . ?
N1 C8 H8 116.9 . . ?
C6 C8 H8 116.9 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C10 H10A 109.5 . . ?
O1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_refine_diff_density_max         2.122
_refine_diff_density_min         -1.451
_refine_diff_density_rms         0.133



# 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 0.000 0.250 402 114 ' '
2 0.000 0.000 0.750 402 114 ' '
3 0.333 0.667 0.062 15 0 ' '
4 0.333 0.667 0.562 15 0 ' '
5 0.666 0.333 0.438 15 0 ' '
6 0.666 0.333 0.938 15 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: MeOH'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# 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_apco7s
_database_code_depnum_ccdc_archive 'CCDC 2403820'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        AP-Co7
_chemical_name_common            '[Ap-Co7].7H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H100 Co7 N8 O32'
_chemical_formula_weight         1954.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

_cell_length_a                   14.14340(10)
_cell_length_b                   14.14340(10)
_cell_length_c                   22.9392(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3973.90(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    22887
_cell_measurement_theta_min      3.6200
_cell_measurement_theta_max      70.2660

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_F_000             1750
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.497
_shelx_estimated_absorpt_T_min   0.715
_shelx_estimated_absorpt_T_max   0.877
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.140
_exptl_absorpt_correction_T_max  0.711
_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     0.71073
_diffrn_radiation_type           MoK\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            45790
_diffrn_reflns_av_unetI/netI     0.0126
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.663
_diffrn_reflns_theta_max         25.348
_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             2439
_reflns_number_gt                2331
_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 1.171.39.46b (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 - 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          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)+(0.0913P)²+17.1269P] 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         2439
_refine_ls_number_parameters     153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0719
_refine_ls_wR_factor_ref         0.2042
_refine_ls_wR_factor_gt          0.2024
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_restrained_S_all      1.220
_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
Co1 Co 0.000000 0.000000 0.000000 0.0311(4) Uani 1 6 d S T P . .
Co2 Co 0.25386(6) 0.10967(7) -0.01165(4) 0.0378(3) Uani 1 1 d . . . . .
O1 O 0.1274(3) -0.0038(3) 0.04606(14) 0.0276(8) Uani 1 1 d . . . . .
O2 O 0.2421(3) -0.0320(3) -0.03446(15) 0.0302(8) Uani 1 1 d . . . . .
O3 O 0.1600(3) -0.2382(3) -0.05290(18) 0.0366(9) Uani 1 1 d . . . . .
O4 O 0.4136(7) -0.2374(7) -0.2930(3) 0.112(3) Uani 1 1 d . . . . .
N1 N 0.3758(4) 0.1835(4) -0.0756(2) 0.0371(11) Uani 1 1 d . . . . .
N2 N 0.333333 -0.333333 -0.2936(5) 0.058(3) Uani 1 3 d S T P . .
C1 C 0.1464(6) -0.3451(5) -0.0431(3) 0.0509(16) Uani 1 1 d . . . . .
H1A H 0.106828 -0.392973 -0.075901 0.076 Uiso 1 1 calc R U . . .
H1B H 0.105001 -0.375886 -0.007033 0.076 Uiso 1 1 calc R U . . .
H1C H 0.218304 -0.339137 -0.039534 0.076 Uiso 1 1 calc R U . . .
C2 C 0.2424(5) -0.1693(5) -0.0914(3) 0.0356(12) Uani 1 1 d . . . . .
C3 C 0.2785(5) -0.2046(5) -0.1375(3) 0.0426(13) Uani 1 1 d . . . . .
H3 H 0.249671 -0.280294 -0.144632 0.051 Uiso 1 1 calc R U . . .
C4 C 0.3583(6) -0.1267(6) -0.1735(3) 0.0480(15) Uani 1 1 d . . . . .
H4 H 0.383371 -0.150185 -0.205828 0.058 Uiso 1 1 calc R U . . .
C5 C 0.4018(5) -0.0181(5) -0.1641(2) 0.0419(14) Uani 1 1 d . . . . .
H5 H 0.458081 0.033186 -0.188758 0.050 Uiso 1 1 calc R U . . .
C6 C 0.3621(5) 0.0190(5) -0.1166(3) 0.0370(12) Uani 1 1 d . . . . .
C7 C 0.2831(4) -0.0572(5) -0.0801(2) 0.0295(11) Uani 1 1 d . . . . .
C8 C 0.4065(5) 0.1367(5) -0.1113(3) 0.0400(13) Uani 1 1 d . . . . .
H8 H 0.463854 0.182101 -0.137240 0.048 Uiso 1 1 calc R U . . .
C9 C 0.4311(6) 0.3041(5) -0.0793(3) 0.0589(19) Uani 1 1 d . . . . .
H9A H 0.479258 0.329132 -0.113423 0.088 Uiso 1 1 calc R U . . .
H9B H 0.474292 0.336244 -0.043960 0.088 Uiso 1 1 calc R U . . .
H9C H 0.376241 0.326823 -0.083072 0.088 Uiso 1 1 calc R U . . .
C10 C 0.1454(7) 0.0126(7) 0.1070(3) 0.067(2) Uani 1 1 d . . . . .
H10A H 0.087929 -0.050373 0.127865 0.101 Uiso 1 1 calc R U . . .
H10B H 0.144033 0.078711 0.118418 0.101 Uiso 1 1 calc R U . . .
H10C H 0.216649 0.020994 0.116710 0.101 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.113(3) . ?
Co1 O1 2.113(3) 8 ?
Co1 O1 2.113(3) 7 ?
Co1 O1 2.113(3) 2 ?
Co1 O1 2.113(3) 9 ?
Co1 O1 2.113(3) 3 ?
Co2 O2 1.996(4) . ?
Co2 O1 2.032(4) 9 ?
Co2 O2 2.042(4) 9 ?
Co2 N1 2.101(5) . ?
Co2 O1 2.158(3) . ?
Co2 O3 2.327(4) 9 ?
O1 C10 1.419(8) . ?
O2 C7 1.329(6) . ?
O3 C2 1.397(7) . ?
O3 C1 1.444(7) . ?
O4 N2 1.261(9) . ?
N1 C8 1.261(8) . ?
N1 C9 1.481(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.373(8) . ?
C2 C7 1.413(8) . ?
C3 C4 1.388(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.356(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.440(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.381(8) . ?
C6 C8 1.461(8) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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 Co1 O1 82.82(11) . 8 ?
O1 Co1 O1 180.00(19) . 7 ?
O1 Co1 O1 97.18(11) 8 7 ?
O1 Co1 O1 97.18(11) . 2 ?
O1 Co1 O1 180.0(2) 8 2 ?
O1 Co1 O1 82.82(11) 7 2 ?
O1 Co1 O1 82.82(11) . 9 ?
O1 Co1 O1 97.18(11) 8 9 ?
O1 Co1 O1 97.18(11) 7 9 ?
O1 Co1 O1 82.82(11) 2 9 ?
O1 Co1 O1 97.18(11) . 3 ?
O1 Co1 O1 82.82(11) 8 3 ?
O1 Co1 O1 82.82(11) 7 3 ?
O1 Co1 O1 97.18(11) 2 3 ?
O1 Co1 O1 180.0(4) 9 3 ?
O2 Co2 O1 111.97(15) . 9 ?
O2 Co2 O2 163.63(9) . 9 ?
O1 Co2 O2 79.91(14) 9 9 ?
O2 Co2 N1 87.26(17) . . ?
O1 Co2 N1 101.90(17) 9 . ?
O2 Co2 N1 101.64(17) 9 . ?
O2 Co2 O1 77.98(13) . . ?
O1 Co2 O1 83.64(18) 9 . ?
O2 Co2 O1 92.77(14) 9 . ?
N1 Co2 O1 165.23(16) . . ?
O2 Co2 O3 95.40(15) . 9 ?
O1 Co2 O3 151.87(14) 9 9 ?
O2 Co2 O3 71.99(14) 9 9 ?
N1 Co2 O3 85.17(17) . 9 ?
O1 Co2 O3 96.38(14) . 9 ?
C10 O1 Co2 117.9(4) . 8 ?
C10 O1 Co1 125.0(4) . . ?
Co2 O1 Co1 98.08(14) 8 . ?
C10 O1 Co2 117.9(4) . . ?
Co2 O1 Co2 98.06(13) 8 . ?
Co1 O1 Co2 94.27(13) . . ?
C7 O2 Co2 130.4(3) . . ?
C7 O2 Co2 123.6(3) . 8 ?
Co2 O2 Co2 103.19(16) . 8 ?
C2 O3 C1 117.2(4) . . ?
C2 O3 Co2 113.0(3) . 8 ?
C1 O3 Co2 125.5(4) . 8 ?
C8 N1 C9 116.4(5) . . ?
C8 N1 Co2 127.3(4) . . ?
C9 N1 Co2 116.3(4) . . ?
O4 N2 O4 119.99(3) 3_655 . ?
O4 N2 O4 119.99(3) 3_655 2_545 ?
O4 N2 O4 119.99(3) . 2_545 ?
O3 C1 H1A 109.5 . . ?
O3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 O3 124.4(5) . . ?
C3 C2 C7 122.1(6) . . ?
O3 C2 C7 113.4(5) . . ?
C2 C3 C4 118.2(6) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 122.2(6) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C4 C5 C6 119.7(6) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C7 C6 C5 119.0(5) . . ?
C7 C6 C8 124.0(5) . . ?
C5 C6 C8 117.0(5) . . ?
O2 C7 C6 124.0(5) . . ?
O2 C7 C2 117.2(5) . . ?
C6 C7 C2 118.8(5) . . ?
N1 C8 C6 126.0(5) . . ?
N1 C8 H8 117.0 . . ?
C6 C8 H8 117.0 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C10 H10A 109.5 . . ?
O1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_refine_diff_density_max         2.396
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.130


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.250 418 135 ' '
2 0.000 0.000 0.750 418 135 ' '
3 0.333 0.667 0.572 16 1 ' '
4 0.333 0.667 0.072 16 1 ' '
5 0.666 0.333 0.928 16 1 ' '
6 0.666 0.333 0.428 16 1 ' '
_platon_squeeze_details          ?


_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_afco7s
_database_code_depnum_ccdc_archive 'CCDC 2403819'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        AF-Co7
_chemical_name_common            '[2-AF-Co7].7H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H98 Co7 N8 O33'
_chemical_formula_weight         1944.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'

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

_cell_length_a                   14.05280(10)
_cell_length_b                   14.05280(10)
_cell_length_c                   23.0080(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3934.91(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    22287
_cell_measurement_theta_min      3.6130
_cell_measurement_theta_max      69.9070

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_F_000             1750
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_absorpt_coefficient_mu    1.512
_shelx_estimated_absorpt_T_min   0.792
_shelx_estimated_absorpt_T_max   0.864
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.219
_exptl_absorpt_correction_T_max  0.413
_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     0.71073
_diffrn_radiation_type           MoK\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            45488
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.673
_diffrn_reflns_theta_max         25.350
_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             2417
_reflns_number_gt                2370
_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 1.171.39.46b (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 - 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          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)+(0.0792P)²+17.4340P] 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         2417
_refine_ls_number_parameters     153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0635
_refine_ls_wR_factor_ref         0.1790
_refine_ls_wR_factor_gt          0.1781
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_restrained_S_all      1.186
_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 1.000000 0.000000 0.000000 0.0278(4) Uani 1 6 d S T P . .
O1 O 1.1275(2) 0.1329(2) 0.04579(13) 0.0237(7) Uani 1 1 d . . . . .
N1 N 1.1827(3) 0.3778(3) 0.07527(18) 0.0320(9) Uani 1 1 d . . . . .
C1 C 0.6500(4) 0.1439(5) 0.0439(3) 0.0430(13) Uani 1 1 d . . . . .
H1A H 0.604169 0.110132 0.078334 0.064 Uiso 1 1 calc R U . . .
H1B H 0.615768 0.096748 0.010047 0.064 Uiso 1 1 calc R U . . .
H1C H 0.657006 0.216021 0.037092 0.064 Uiso 1 1 calc R U . . .
Co2 Co 1.10819(6) 0.25515(6) 0.01139(3) 0.0328(3) Uani 1 1 d . . . . .
O2 O 0.7575(3) 0.1571(3) 0.05330(15) 0.0306(8) Uani 1 1 d . . . . .
N2 N 0.666667 0.333333 0.2946(4) 0.0425(19) Uani 1 3 d S T P . .
C2 C 0.8268(4) 0.2389(4) 0.0926(2) 0.0300(10) Uani 1 1 d . . . . .
O3 O 0.9653(3) 0.2424(3) 0.03449(13) 0.0245(7) Uani 1 1 d . . . . .
C3 C 0.7913(4) 0.2729(4) 0.1395(2) 0.0358(11) Uani 1 1 d . . . . .
H3 H 0.715000 0.242733 0.146769 0.043 Uiso 1 1 calc R U . . .
O4 O 0.7632(5) 0.4123(5) 0.2945(2) 0.0729(15) Uani 1 1 d . . . . .
C4 C 0.8688(5) 0.3521(5) 0.1760(2) 0.0383(12) Uani 1 1 d . . . . .
H4 H 0.844918 0.375751 0.208771 0.046 Uiso 1 1 calc R U . . .
C5 C 0.9786(4) 0.3970(5) 0.1659(2) 0.0346(11) Uani 1 1 d . . . . .
H5 H 1.030161 0.452591 0.190964 0.041 Uiso 1 1 calc R U . . .
C6 C 1.0167(4) 0.3609(4) 0.1177(2) 0.0306(10) Uani 1 1 d . . . . .
C7 C 0.9393(4) 0.2812(4) 0.08050(19) 0.0237(9) Uani 1 1 d . . . . .
C8 C 1.1348(4) 0.4072(4) 0.1117(2) 0.0337(11) Uani 1 1 d . . . . .
H8 H 1.180335 0.464853 0.137621 0.040 Uiso 1 1 calc R U . . .
C9 C 1.3034(5) 0.4342(6) 0.0783(3) 0.0516(16) Uani 1 1 d . . . . .
H9A H 1.329068 0.486455 0.110732 0.077 Uiso 1 1 calc R U . . .
H9B H 1.334635 0.473632 0.041896 0.077 Uiso 1 1 calc R U . . .
H9C H 1.326747 0.379873 0.084455 0.077 Uiso 1 1 calc R U . . .
C10 C 1.1441(6) 0.1343(6) 0.1073(3) 0.0607(18) Uani 1 1 d . . . . .
H10A H 1.213691 0.199665 0.117766 0.091 Uiso 1 1 calc R U . . .
H10B H 1.146251 0.068195 0.118745 0.091 Uiso 1 1 calc R U . . .
H10C H 1.083522 0.135864 0.127598 0.091 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.113(3) . ?
Co1 O1 2.113(3) 7_755 ?
Co1 O1 2.113(3) 9_545 ?
Co1 O1 2.113(3) 2_645 ?
Co1 O1 2.113(3) 8_665 ?
Co1 O1 2.113(3) 3_765 ?
O1 C10 1.434(7) . ?
O1 Co2 2.030(3) . ?
O1 Co2 2.152(3) 8_665 ?
N1 C8 1.266(7) . ?
N1 C9 1.472(7) . ?
N1 Co2 2.103(4) . ?
C1 O2 1.443(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Co2 O3 1.996(3) . ?
Co2 O3 2.046(3) 8_665 ?
Co2 O2 2.327(3) 8_665 ?
O2 C2 1.402(6) . ?
N2 O4 1.251(6) 3_665 ?
N2 O4 1.251(6) 2_655 ?
N2 O4 1.252(6) . ?
C2 C3 1.372(7) . ?
C2 C7 1.410(7) . ?
O3 C7 1.323(5) . ?
C3 C4 1.385(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.365(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.429(7) . ?
C5 H5 0.9500 . ?
C6 C7 1.397(7) . ?
C6 C8 1.456(7) . ?
C8 H8 0.9500 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 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 Co1 O1 180.00(14) . 7_755 ?
O1 Co1 O1 82.71(10) . 9_545 ?
O1 Co1 O1 97.29(10) 7_755 9_545 ?
O1 Co1 O1 97.29(10) . 2_645 ?
O1 Co1 O1 82.71(10) 7_755 2_645 ?
O1 Co1 O1 82.71(10) 9_545 2_645 ?
O1 Co1 O1 82.71(10) . 8_665 ?
O1 Co1 O1 97.29(10) 7_755 8_665 ?
O1 Co1 O1 97.29(10) 9_545 8_665 ?
O1 Co1 O1 180.00(17) 2_645 8_665 ?
O1 Co1 O1 97.29(10) . 3_765 ?
O1 Co1 O1 82.71(10) 7_755 3_765 ?
O1 Co1 O1 180.0(2) 9_545 3_765 ?
O1 Co1 O1 97.29(10) 2_645 3_765 ?
O1 Co1 O1 82.71(10) 8_665 3_765 ?
C10 O1 Co2 117.6(4) . . ?
C10 O1 Co1 124.4(3) . . ?
Co2 O1 Co1 98.07(12) . . ?
C10 O1 Co2 118.7(4) . 8_665 ?
Co2 O1 Co2 98.17(12) . 8_665 ?
Co1 O1 Co2 94.36(12) . 8_665 ?
C8 N1 C9 116.7(4) . . ?
C8 N1 Co2 127.0(4) . . ?
C9 N1 Co2 116.2(3) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 Co2 O1 111.99(13) . . ?
O3 Co2 O3 163.93(7) . 8_665 ?
O1 Co2 O3 79.93(12) . 8_665 ?
O3 Co2 N1 87.33(15) . . ?
O1 Co2 N1 101.48(15) . . ?
O3 Co2 N1 101.18(15) 8_665 . ?
O3 Co2 O1 78.14(12) . 9_545 ?
O1 Co2 O1 83.70(16) . 9_545 ?
O3 Co2 O1 93.08(12) 8_665 9_545 ?
N1 Co2 O1 165.46(15) . 9_545 ?
O3 Co2 O2 95.38(12) . 8_665 ?
O1 Co2 O2 151.88(12) . 8_665 ?
O3 Co2 O2 71.98(12) 8_665 8_665 ?
N1 Co2 O2 85.57(15) . 8_665 ?
O1 Co2 O2 96.24(12) 9_545 8_665 ?
C2 O2 C1 117.1(4) . . ?
C2 O2 Co2 112.7(3) . 9_545 ?
C1 O2 Co2 126.0(3) . 9_545 ?
O4 N2 O4 120.000(7) 3_665 2_655 ?
O4 N2 O4 120.000(6) 3_665 . ?
O4 N2 O4 120.000(6) 2_655 . ?
C3 C2 O2 124.6(5) . . ?
C3 C2 C7 122.3(5) . . ?
O2 C2 C7 113.1(4) . . ?
C7 O3 Co2 130.4(3) . . ?
C7 O3 Co2 123.2(3) . 9_545 ?
Co2 O3 Co2 102.89(14) . 9_545 ?
C2 C3 C4 118.7(5) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 121.4(5) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 120.4(5) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C7 C6 C5 118.7(5) . . ?
C7 C6 C8 123.8(4) . . ?
C5 C6 C8 117.4(4) . . ?
O3 C7 C6 123.8(4) . . ?
O3 C7 C2 117.7(4) . . ?
C6 C7 C2 118.4(4) . . ?
N1 C8 C6 126.2(5) . . ?
N1 C8 H8 116.9 . . ?
C6 C8 H8 116.9 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C10 H10A 109.5 . . ?
O1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
O1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

_refine_diff_density_max         1.575
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.121


# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.250 406 128 ' '
2 0.000 0.000 0.750 406 128 ' '
3 0.333 0.666 0.067 14 1 ' '
4 0.333 0.666 0.567 14 1 ' '
5 0.666 0.333 0.433 14 1 ' '
6 0.666 0.333 0.933 14 1 ' '
_platon_squeeze_details          ?

_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_afni7s
_database_code_depnum_ccdc_archive 'CCDC 2403818'
loop_
_audit_author_name
_audit_author_address
'Leigh Jones'
;University of Wolverhampton 
United Kingdom
;
_audit_update_record             
;
2024-11-19 deposited with the CCDC.	2025-05-13 downloaded from the CCDC.
;
_audit_creation_date             2022-06-09
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_chemical_formula_moiety         'C60 H78 N6 Ni7 O18, 2(N1 O3)'
_chemical_formula_sum            'C60 H78 N8 Ni7 O24'
_chemical_formula_weight         1706.181
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Ni 0.35663 1.12491 12.83760 7.29200 4.44380 2.38000 3.87850 0.25650 12.17630
66.34210 1.03410005569
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 x-y,-y,-z+1/2
5 -x,-x+y,-z+1/2
6 y,x,-z+1/2
7 -x,-y,-z
8 y,-x+y,-z
9 x-y,x,-z
10 -x+y,y,z-1/2
11 x,x-y,z-1/2
12 -y,-x,z-1/2

_symmetry_Int_Tables_number      165
_cell_length_a                   13.8113(1)
_cell_length_b                   13.8113(1)
_cell_length_c                   23.2351(1)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3838.35(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_exptl_absorpt_coefficient_mu    1.754
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_F_000             1769.984
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.12
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_Laue_measured_fraction_full 0.9996
_diffrn_reflns_Laue_measured_fraction_max 0.9996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            66489
_diffrn_reflns_point_group_measured_fraction_full 0.9996
_diffrn_reflns_point_group_measured_fraction_max 0.9996
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.70
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.9996
_diffrn_measured_fraction_theta_max 0.9996
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              -27
_reflns_number_gt                2312
_reflns_number_total             2358
_reflns_threshold_expression     I>=2u(I)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.2946
_refine_diff_density_min         -0.7430
_refine_diff_density_rms         0.1517
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             11.9609
_refine_ls_goodness_of_fit_ref   1.0266
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    20
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2358
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0747
_refine_ls_restrained_S_all      1.0266
_refine_ls_shift/su_max          0.0354
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1364P)²+20.3177P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2246
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8)
2.b Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c)
;
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.0 0.0 0.0 0.0372(5) Uani 1.000020 6 S T P
O1 O -0.1359(2) -0.1241(3) 0.04423(13) 0.0248(7) Uani 1.000000 1 . . .
N1 N -0.2035(4) -0.3807(4) -0.06894(19) 0.0354(10) Uani 1.000000 1 . . .
C1 C -0.4959(6) -0.1360(6) -0.0478(4) 0.0595(19) Uani 1.000000 1 . . .
H1a H -0.507(3) -0.096(4) -0.0794(13) 0.089(3) Uiso 1.000000 1 GR . .
H1b H -0.5600(9) -0.2121(6) -0.046(2) 0.089(3) Uiso 1.000000 1 GR . .
H1c H -0.489(2) -0.097(4) -0.0115(13) 0.089(3) Uiso 1.000000 1 GR . .
Ni2 Ni -0.25633(6) -0.10092(7) 0.00695(3) 0.0445(4) Uani 1.000000 1 . . .
O2 O -0.2807(3) -0.2378(3) -0.03420(14) 0.0276(7) Uani 1.000000 1 . . .
N2 N -0.666666666667 -0.333333333333 -0.2981(3) 0.0407(18) Uani 1.000000 3 S T
P
C2 C -0.4069(4) -0.2245(5) -0.0967(2) 0.0358(12) Uani 1.000000 1 . . .
O3 O -0.3961(3) -0.1408(3) -0.05814(16) 0.0370(9) Uani 1.000000 1 . . .
C3 C -0.4724(5) -0.2564(5) -0.1453(2) 0.0445(14) Uani 1.000000 1 . . .
H3 H -0.5161(5) -0.2231(5) -0.1547(2) 0.0534(16) Uiso 1.000000 1 R . .
O4 O -0.6447(5) -0.4100(5) -0.2986(2) 0.0670(14) Uani 1.000000 1 . . .
C4 C -0.4734(5) -0.3372(6) -0.1799(3) 0.0459(14) Uani 1.000000 1 . . .
H4 H -0.5189(5) -0.3594(6) -0.2134(3) 0.0551(16) Uiso 1.000000 1 R . .
C5 C -0.4122(5) -0.3870(5) -0.1683(2) 0.0413(13) Uani 1.000000 1 . . .
H5 H -0.4157(5) -0.4434(5) -0.1931(2) 0.0496(15) Uiso 1.000000 1 R . .
C6 C -0.3418(4) -0.3536(4) -0.1180(2) 0.0350(11) Uani 1.000000 1 . . .
C7 C -0.3399(4) -0.2729(4) -0.0820(2) 0.0268(10) Uani 1.000000 1 . . .
C8 C -0.2750(5) -0.4043(5) -0.1088(2) 0.0384(12) Uani 1.000000 1 . . .
H8 H -0.2848(5) -0.4613(5) -0.1351(2) 0.0461(14) Uiso 1.000000 1 R . .
C9 C -0.1426(7) -0.4430(7) -0.0696(4) 0.065(2) Uani 1.000000 1 . . .
H9a H -0.164(4) -0.491(4) -0.1038(15) 0.098(3) Uiso 1.000000 1 GR . .
H9b H -0.0619(7) -0.3901(7) -0.070(3) 0.098(3) Uiso 1.000000 1 GR . .
H9c H -0.161(4) -0.489(4) -0.0350(14) 0.098(3) Uiso 1.000000 1 GR . .
C10 C -0.1367(12) -0.1328(12) 0.1045(6) 0.122(4) Uiso 1.000000 1 . . .
H10a H -0.136(10) -0.068(5) 0.1218(6) 0.184(7) Uiso 1.000000 1 GR . .
H10b H -0.204(5) -0.201(5) 0.1167(7) 0.184(7) Uiso 1.000000 1 GR . .
H10c H -0.070(5) -0.136(10) 0.1171(7) 0.184(7) Uiso 1.000000 1 GR . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.074(3) 3 ?
Ni1 O1 2.074(3) 8 ?
Ni1 O1 2.074(3) 7 ?
Ni1 O1 2.074(3) . ?
Ni1 O1 2.074(3) 2 ?
Ni1 O1 2.074(3) 9 ?
O1 Ni2 2.038(3) . ?
O1 Ni2 2.080(3) 9 ?
O1 C10 1.405(14) . ?
N1 Ni2 2.080(4) 9 ?
N1 C8 1.272(7) . ?
N1 C9 1.474(8) . ?
C1 H1a 0.9800 . ?
C1 H1b 0.9800 . ?
C1 H1c 0.9800 . ?
C1 O3 1.433(7) . ?
Ni2 O2 1.991(3) . ?
Ni2 O2 1.976(3) 8 ?
Ni2 O3 2.292(4) . ?
O2 C7 1.319(6) . ?
N2 O4 1.238(5) 2_455 ?
N2 O4 1.238(5) 3_445 ?
N2 O4 1.238(5) . ?
C2 O3 1.410(7) . ?
C2 C3 1.375(8) . ?
C2 C7 1.427(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.370(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.357(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.440(8) . ?
C6 C7 1.384(7) . ?
C6 C8 1.426(8) . ?
C8 H8 0.9500 . ?
C9 H9a 0.9800 . ?
C9 H9b 0.9800 . ?
C9 H9c 0.9800 . ?
C10 H10a 0.9800 . ?
C10 H10b 0.9800 . ?
C10 H10c 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 97.56(12) . 3 ?
O1 Ni1 O1 180.0 8 2 ?
O1 Ni1 O1 97.56(11) 9 7 ?
O1 Ni1 O1 97.56(11) 2 3 ?
O1 Ni1 O1 82.44(11) 9 . ?
O1 Ni1 O1 97.56(12) 2 . ?
O1 Ni1 O1 82.44(12) 8 . ?
O1 Ni1 O1 82.44(12) 7 3 ?
O1 Ni1 O1 180.0 9 3 ?
O1 Ni1 O1 180.0 7 . ?
O1 Ni1 O1 82.44(12) 9 2 ?
O1 Ni1 O1 82.44(11) 7 2 ?
O1 Ni1 O1 97.56(12) 9 8 ?
O1 Ni1 O1 82.44(11) 8 3 ?
O1 Ni1 O1 97.56(12) 8 7 ?
Ni2 O1 Ni1 97.57(13) . 2 ?
Ni2 O1 Ni1 96.26(13) 9 2 ?
C10 O1 Ni1 122.0(6) . 2 ?
C10 O1 Ni2 117.7(6) . . ?
C10 O1 Ni2 120.2(6) . 9 ?
C8 N1 Ni2 127.1(4) . 9 ?
C9 N1 Ni2 116.7(4) . 9 ?
C9 N1 C8 116.1(5) . . ?
H1b C1 H1a 109.5 . . ?
H1c C1 H1a 109.5 . . ?
H1c C1 H1b 109.5 . . ?
O3 C1 H1a 109.5 . . ?
O3 C1 H1b 109.5 . . ?
O3 C1 H1c 109.5 . . ?
N1 Ni2 O1 99.12(16) 8 . ?
N1 Ni2 O1 165.57(16) 8 8 ?
O2 Ni2 O1 79.55(13) . . ?
O2 Ni2 O1 108.44(14) 8 . ?
O2 Ni2 O1 95.98(13) . 8 ?
O2 Ni2 O1 78.87(13) 8 8 ?
O2 Ni2 N1 86.93(16) 8 8 ?
O2 Ni2 N1 98.45(16) . 8 ?
O3 Ni2 O1 96.96(14) . 8 ?
O3 Ni2 O1 153.92(13) . . ?
O3 Ni2 N1 87.26(17) . 8 ?
O3 Ni2 O2 74.49(13) . . ?
O3 Ni2 O2 97.09(14) . 8 ?
C7 O2 Ni2 122.2(3) . . ?
C7 O2 Ni2 130.1(3) . 9 ?
O4 N2 O4 119.99(4) 2_455 . ?
O4 N2 O4 119.99(5) 3_445 . ?
O4 N2 O4 119.99(4) 3_445 2_455 ?
C3 C2 O3 124.5(5) . . ?
C7 C2 O3 113.9(4) . . ?
C7 C2 C3 121.6(5) . . ?
Ni2 O3 C1 126.3(4) . . ?
C2 O3 C1 115.7(4) . . ?
C2 O3 Ni2 110.3(3) . . ?
H3 C3 C2 120.7(4) . . ?
C4 C3 C2 118.6(6) . . ?
C4 C3 H3 120.7(4) . . ?
H4 C4 C3 118.6(4) . . ?
C5 C4 C3 122.8(6) . . ?
C5 C4 H4 118.6(3) . . ?
H5 C5 C4 120.3(3) . . ?
C6 C5 C4 119.4(5) . . ?
C6 C5 H5 120.3(3) . . ?
C7 C6 C5 119.1(5) . . ?
C8 C6 C5 117.6(5) . . ?
C8 C6 C7 123.4(5) . . ?
C2 C7 O2 117.2(4) . . ?
C6 C7 O2 124.3(5) . . ?
C6 C7 C2 118.5(5) . . ?
C6 C8 N1 126.3(5) . . ?
H8 C8 N1 116.8(3) . . ?
H8 C8 C6 116.8(3) . . ?
H9a C9 N1 109.5 . . ?
H9b C9 N1 109.5 . . ?
H9b C9 H9a 109.5 . . ?
H9c C9 N1 109.5 . . ?
H9c C9 H9a 109.5 . . ?
H9c C9 H9b 109.5 . . ?
H10a C10 O1 109.5 . . ?
H10b C10 O1 109.5 . . ?
H10b C10 H10a 109.5 . . ?
H10c C10 O1 109.5 . . ?
H10c C10 H10a 109.5 . . ?
H10c C10 H10b 109.5 . . ?


_olex2_submission_special_instructions 'No special instructions were received'

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.250 388 86 ' '
2 0.000 0.000 0.750 388 86 ' '
3 0.333 0.666 0.050 9 1 ' '
4 0.333 0.666 0.550 9 1 ' '
5 0.666 0.333 0.450 9 1 ' '
6 0.666 0.333 0.950 9 1 ' '
_platon_squeeze_details          ?
_chemical_name_systematic        AF-Ni7
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_refine_special_details          SQUEEZE
