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

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

data_1b
_database_code_depnum_ccdc_archive 'CCDC 1907068'
loop_
_audit_author_name
_audit_author_address
'Ivan Nemec'
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H18 Co N10 O8'
_chemical_formula_weight         537.33

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        i_1_2/c_1
_space_group_name_Hall           -i_2yc

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

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

_cell_length_a                   15.2228(6)
_cell_length_b                   10.2158(4)
_cell_length_c                   14.4221(5)
_cell_angle_alpha                90
_cell_angle_beta                 110.266(4)
_cell_angle_gamma                90
_cell_volume                     2103.98(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2532
_cell_measurement_theta_min      2.844
_cell_measurement_theta_max      28.222

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.886
_shelx_estimated_absorpt_T_min   0.789
_shelx_estimated_absorpt_T_max   0.843
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5177
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.853
_diffrn_reflns_theta_max         27.500
_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             2413
_reflns_number_gt                2175
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  Bruker
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0294P)²+2.3782P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2413
_refine_ls_number_parameters     165
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0777
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.049
_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 0.5000 0.43356(3) 0.2500 0.00995(11) Uani 1 2 d S T P . .
O7 O 0.28172(8) 0.11161(14) 0.36750(9) 0.0181(3) Uani 1 1 d . . . . .
O8 O 0.42889(9) 0.07145(14) 0.39784(10) 0.0182(3) Uani 1 1 d . . . . .
O6 O 0.32548(9) 0.01066(14) 0.25805(9) 0.0191(3) Uani 1 1 d . . . . .
N4 N 0.54907(10) 0.57814(15) 0.35979(10) 0.0129(3) Uani 1 1 d . . . . .
N5 N 0.56849(10) 0.73021(15) 0.47012(11) 0.0130(3) Uani 1 1 d . . . . .
H5 H 0.5671 0.8076 0.4964 0.016 Uiso 1 1 calc R U . . .
O1 O 0.61755(9) 0.40604(17) 0.21678(10) 0.0238(3) Uani 1 1 d D . . . .
N1 N 0.60519(10) 0.62078(15) 0.52235(11) 0.0134(3) Uani 1 1 d . . . . .
N8 N 0.34509(10) 0.06445(15) 0.34003(11) 0.0131(3) Uani 1 1 d . . . . .
N9 N 0.58088(10) 0.32044(15) 0.38384(10) 0.0110(3) Uani 1 1 d . . . . .
C1 C 0.48545(14) 0.80277(19) 0.29609(13) 0.0202(4) Uani 1 1 d . . . . .
H1C H 0.4972 0.8910 0.3263 0.024 Uiso 1 1 calc R U . . .
H1D H 0.4172 0.7863 0.2749 0.024 Uiso 1 1 calc R U . . .
C2 C 0.66306(13) 0.13453(19) 0.47363(14) 0.0173(4) Uani 1 1 d . . . . .
H2 H 0.6783 0.0443 0.4738 0.021 Uiso 1 1 calc R U . . .
C3 C 0.67626(12) 0.34094(19) 0.55582(13) 0.0154(4) Uani 1 1 d . . . . .
H3 H 0.7003 0.3944 0.6130 0.018 Uiso 1 1 calc R U . . .
C6 C 0.60465(12) 0.19397(18) 0.38802(13) 0.0137(4) Uani 1 1 d . . . . .
H6 H 0.5804 0.1426 0.3298 0.016 Uiso 1 1 calc R U . . .
C10 C 0.53455(12) 0.70446(18) 0.37309(13) 0.0131(4) Uani 1 1 d . . . . .
C11 C 0.59193(11) 0.53109(18) 0.45272(12) 0.0110(3) Uani 1 1 d . . . . .
C12 C 0.69875(12) 0.2088(2) 0.55875(14) 0.0175(4) Uani 1 1 d . . . . .
H12 H 0.7382 0.1698 0.6185 0.021 Uiso 1 1 calc R U . . .
C13 C 0.61763(11) 0.39248(18) 0.46688(12) 0.0115(3) Uani 1 1 d . . . . .
H1A H 0.6704(9) 0.399(2) 0.2609(11) 0.017 Uiso 1 1 d D U . . .
H1B H 0.6209(13) 0.395(2) 0.1608(8) 0.017 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.0259(13) 2_655 ?
Co1 O1 2.0260(13) . ?
Co1 N4 2.1041(15) 2_655 ?
Co1 N4 2.1041(15) . ?
Co1 N9 2.2205(15) 2_655 ?
Co1 N9 2.2206(14) . ?
O7 N8 1.2587(19) . ?
O8 N8 1.2612(19) . ?
O6 N8 1.2427(19) . ?
N4 C10 1.334(2) . ?
N4 C11 1.359(2) . ?
N5 C10 1.339(2) . ?
N5 N1 1.356(2) . ?
N1 C11 1.322(2) . ?
N9 C6 1.337(2) . ?
N9 C13 1.351(2) . ?
C1 C10 1.492(3) . ?
C1 C1 1.540(4) 2_655 ?
C2 C12 1.384(3) . ?
C2 C6 1.387(3) . ?
C3 C13 1.388(2) . ?
C3 C12 1.390(3) . ?
C11 C13 1.464(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O1 164.05(10) 2_655 . ?
O1 Co1 N4 99.38(6) 2_655 2_655 ?
O1 Co1 N4 91.82(6) . 2_655 ?
O1 Co1 N4 91.83(6) 2_655 . ?
O1 Co1 N4 99.38(6) . . ?
N4 Co1 N4 90.83(8) 2_655 . ?
O1 Co1 N9 82.19(5) 2_655 2_655 ?
O1 Co1 N9 89.51(5) . 2_655 ?
N4 Co1 N9 76.45(6) 2_655 2_655 ?
N4 Co1 N9 164.77(6) . 2_655 ?
O1 Co1 N9 89.51(5) 2_655 . ?
O1 Co1 N9 82.19(5) . . ?
N4 Co1 N9 164.77(6) 2_655 . ?
N4 Co1 N9 76.45(6) . . ?
N9 Co1 N9 117.28(8) 2_655 . ?
C10 N4 C11 104.31(14) . . ?
C10 N4 Co1 138.92(12) . . ?
C11 N4 Co1 114.70(12) . . ?
C10 N5 N1 110.74(15) . . ?
C11 N1 N5 102.97(14) . . ?
O6 N8 O7 120.73(14) . . ?
O6 N8 O8 120.58(14) . . ?
O7 N8 O8 118.69(14) . . ?
C6 N9 C13 117.64(15) . . ?
C6 N9 Co1 127.00(12) . . ?
C13 N9 Co1 114.95(12) . . ?
C10 C1 C1 115.01(16) . 2_655 ?
C12 C2 C6 118.91(18) . . ?
C13 C3 C12 118.00(17) . . ?
N9 C6 C2 122.90(17) . . ?
N4 C10 N5 108.49(16) . . ?
N4 C10 C1 127.54(16) . . ?
N5 C10 C1 123.92(16) . . ?
N1 C11 N4 113.49(16) . . ?
N1 C11 C13 126.94(16) . . ?
N4 C11 C13 119.56(15) . . ?
C2 C12 C3 119.23(17) . . ?
N9 C13 C3 123.29(17) . . ?
N9 C13 C11 113.24(15) . . ?
C3 C13 C11 123.44(16) . . ?

_refine_diff_density_max         0.400
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.067

####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1907070'
loop_
_audit_author_name
_audit_author_address
'Ivan Nemec'
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H44 Co2 N18 O13'
_chemical_formula_weight         1030.73

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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   12.1261(8)
_cell_length_b                   31.410(2)
_cell_length_c                   13.6475(10)
_cell_angle_alpha                90
_cell_angle_beta                 109.6370(10)
_cell_angle_gamma                90
_cell_volume                     4895.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9925
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      30.12

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_F_000             2424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.753
_shelx_estimated_absorpt_T_min   0.790
_shelx_estimated_absorpt_T_max   0.941
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39663
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.297
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_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             8617
_reflns_number_gt                7194
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0537P)²+13.7875P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8617
_refine_ls_number_parameters     645
_refine_ls_number_restraints     53
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1392
_refine_ls_wR_factor_gt          0.1309
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 1.52485(4) 0.13749(2) 0.91228(3) 0.01715(13) Uani 1 1 d . . . . .
Co2 Co 0.93584(4) 0.13820(2) 0.52882(3) 0.01849(13) Uani 1 1 d . . . . .
O1W O 1.5851(2) 0.15781(8) 1.06645(19) 0.0238(5) Uani 1 1 d D . . . .
O2W O 1.6751(2) 0.09983(9) 0.9385(2) 0.0302(6) Uani 1 1 d D . . . .
O3W O 0.8756(2) 0.15626(8) 0.3734(2) 0.0253(5) Uani 1 1 d D . . . .
O4W O 0.7813(2) 0.10123(9) 0.5063(2) 0.0306(6) Uani 1 1 d D . . . .
N1 N 1.6095(2) 0.19273(9) 0.8707(2) 0.0208(6) Uani 1 1 d . . . . .
N2 N 1.3894(2) 0.18486(9) 0.8725(2) 0.0196(6) Uani 1 1 d . . . . .
N3 N 1.3495(3) 0.25458(10) 0.8401(2) 0.0268(7) Uani 1 1 d . . . . .
N4 N 1.2548(3) 0.23336(10) 0.8484(2) 0.0272(7) Uani 1 1 d . . . . .
H4 H 1.1869 0.2452 0.8419 0.033 Uiso 1 1 calc R U . . .
N5 N 1.0040(3) 0.10547(10) 0.6756(2) 0.0266(7) Uani 1 1 d . . . . .
N6 N 1.0444(4) 0.06721(15) 0.8153(3) 0.0532(11) Uani 1 1 d . . . . .
H6 H 1.0513 0.0596 0.8792 0.064 Uiso 1 1 calc R U . . .
N7 N 1.0742(3) 0.04254(13) 0.7479(3) 0.0526(11) Uani 1 1 d . . . . .
N8 N 1.0259(3) 0.08529(10) 0.4902(2) 0.0261(7) Uani 1 1 d . . . . .
N9 N 1.4403(3) 0.08424(9) 0.9580(2) 0.0228(6) Uani 1 1 d . . . . .
N10 N 1.4568(2) 0.10125(9) 0.7690(2) 0.0199(6) Uani 1 1 d . . . . .
N11 N 1.4015(3) 0.03463(10) 0.7096(3) 0.0315(8) Uani 1 1 d . . . . .
N12 N 1.4249(3) 0.05884(10) 0.6361(2) 0.0308(7) Uani 1 1 d . . . . .
H12 H 1.4193 0.0498 0.5736 0.037 Uiso 1 1 calc R U . . .
N13 N 1.0740(2) 0.18432(9) 0.5646(2) 0.0197(6) Uani 1 1 d . . . . .
N14 N 1.2138(3) 0.23077(9) 0.5925(2) 0.0218(6) Uani 1 1 d . . . . .
H14 H 1.2831 0.2417 0.6006 0.026 Uiso 1 1 calc R U . . .
N15 N 1.1210(3) 0.25318(9) 0.6003(2) 0.0218(6) Uani 1 1 d . . . . .
N16 N 0.8556(2) 0.19404(9) 0.5680(2) 0.0210(6) Uani 1 1 d . . . . .
C1 C 1.7203(3) 0.19448(12) 0.8719(3) 0.0260(8) Uani 1 1 d . . . . .
H1 H 1.7651 0.1690 0.8838 0.031 Uiso 1 1 calc R U . . .
C2 C 1.7721(4) 0.23201(13) 0.8564(3) 0.0313(9) Uani 1 1 d . . . . .
H2 H 1.8514 0.2322 0.8591 0.038 Uiso 1 1 calc R U . . .
C3 C 1.7072(4) 0.26915(13) 0.8370(3) 0.0317(9) Uani 1 1 d . . . . .
H3 H 1.7409 0.2951 0.8253 0.038 Uiso 1 1 calc R U . . .
C4 C 1.5922(3) 0.26798(12) 0.8348(3) 0.0268(8) Uani 1 1 d . . . . .
H4A H 1.5452 0.2930 0.8213 0.032 Uiso 1 1 calc R U . . .
C5 C 1.5475(3) 0.22911(11) 0.8530(3) 0.0208(7) Uani 1 1 d . . . . .
C6 C 1.4286(3) 0.22404(11) 0.8549(3) 0.0206(7) Uani 1 1 d . . . . .
C7 C 1.2791(3) 0.19222(12) 0.8677(3) 0.0236(8) Uani 1 1 d . . . . .
C8 C 1.1958(3) 0.15998(13) 0.8808(3) 0.0297(9) Uani 1 1 d . . . . .
H8A H 1.2185 0.1523 0.9553 0.036 Uiso 1 1 calc R U . . .
H8B H 1.2016 0.1340 0.8419 0.036 Uiso 1 1 calc R U . . .
C9 C 1.0687(3) 0.17542(16) 0.8428(3) 0.0391(11) Uani 1 1 d . . . . .
H9A H 1.0592 0.1972 0.8919 0.047 Uiso 1 1 calc R U . . .
H9B H 1.0520 0.1893 0.7742 0.047 Uiso 1 1 calc R U . . .
C10 C 0.9792(4) 0.13996(18) 0.8328(3) 0.0492(13) Uani 1 1 d . . . . .
H10A H 0.9838 0.1299 0.9028 0.059 Uiso 1 1 calc R U . . .
H10B H 0.8992 0.1510 0.7972 0.059 Uiso 1 1 calc R U . . .
C11 C 1.0032(3) 0.10466(15) 0.7733(3) 0.0372(10) Uani 1 1 d . . . . .
C12 C 1.0491(3) 0.06685(12) 0.6636(3) 0.0308(9) Uani 1 1 d . . . . .
C13 C 1.0690(3) 0.05633(12) 0.5677(3) 0.0312(9) Uani 1 1 d . . . . .
C14 C 1.1298(4) 0.02045(13) 0.5579(4) 0.0424(11) Uani 1 1 d . . . . .
H14A H 1.1579 0.0008 0.6137 0.051 Uiso 1 1 calc R U . . .
C15 C 1.1486(4) 0.01395(14) 0.4660(5) 0.0543(15) Uani 1 1 d . . . . .
H15 H 1.1907 -0.0104 0.4572 0.065 Uiso 1 1 calc R U . . .
C16 C 1.1064(4) 0.04275(16) 0.3858(5) 0.0533(14) Uani 1 1 d . . . . .
H16 H 1.1193 0.0384 0.3216 0.064 Uiso 1 1 calc R U . . .
C17 C 1.0443(4) 0.07860(14) 0.3999(4) 0.0371(10) Uani 1 1 d . . . . .
H17 H 1.0149 0.0984 0.3447 0.044 Uiso 1 1 calc R U . . .
C18 C 1.4264(3) 0.07865(13) 1.0506(3) 0.0311(9) Uani 1 1 d . . . . .
H18 H 1.4503 0.1007 1.1009 0.037 Uiso 1 1 calc R U . . .
C19 C 1.3786(4) 0.04196(15) 1.0757(4) 0.0404(11) Uani 1 1 d . . . . .
H19 H 1.3706 0.0389 1.1422 0.048 Uiso 1 1 calc R U . . .
C20 C 1.3429(4) 0.01000(14) 1.0030(4) 0.0428(11) Uani 1 1 d . . . . .
H20 H 1.3094 -0.0153 1.0186 0.051 Uiso 1 1 calc R U . . .
C21 C 1.3562(4) 0.01506(13) 0.9072(4) 0.0363(10) Uani 1 1 d . . . . .
H21 H 1.3322 -0.0066 0.8559 0.044 Uiso 1 1 calc R U . . .
C22 C 1.4053(3) 0.05251(11) 0.8876(3) 0.0244(8) Uani 1 1 d . . . . .
C23 C 1.4217(3) 0.06186(11) 0.7883(3) 0.0232(8) Uani 1 1 d . . . . .
C24 C 1.4576(3) 0.09806(12) 0.6716(3) 0.0240(8) Uani 1 1 d . . . . .
C25 C 1.4797(3) 0.13294(13) 0.6063(3) 0.0282(8) Uani 1 1 d . . . . .
H25A H 1.4700 0.1218 0.5360 0.034 Uiso 1 1 calc R U . . .
H25B H 1.5612 0.1432 0.6377 0.034 Uiso 1 1 calc R U . . .
C26 C 1.3952(3) 0.16989(12) 0.5974(3) 0.0251(8) Uani 1 1 d . . . . .
H26A H 1.4082 0.1915 0.5497 0.030 Uiso 1 1 calc R U . . .
H26B H 1.4128 0.1833 0.6666 0.030 Uiso 1 1 calc R U . . .
C27 C 1.2663(3) 0.15644(12) 0.5575(3) 0.0249(8) Uani 1 1 d . . . . .
H27A H 1.2439 0.1492 0.4828 0.030 Uiso 1 1 calc R U . . .
H27B H 1.2569 0.1305 0.5951 0.030 Uiso 1 1 calc R U . . .
C28 C 1.1855(3) 0.19009(11) 0.5708(3) 0.0192(7) Uani 1 1 d . . . . .
C29 C 1.0394(3) 0.22360(10) 0.5839(3) 0.0195(7) Uani 1 1 d . . . . .
C30 C 0.9201(3) 0.23017(11) 0.5869(3) 0.0206(7) Uani 1 1 d . . . . .
C31 C 0.8783(3) 0.26914(12) 0.6066(3) 0.0239(8) Uani 1 1 d . . . . .
H31 H 0.9270 0.2937 0.6207 0.029 Uiso 1 1 calc R U . . .
C32 C 0.7641(4) 0.27141(13) 0.6053(3) 0.0296(9) Uani 1 1 d . . . . .
H32 H 0.7328 0.2977 0.6183 0.036 Uiso 1 1 calc R U . . .
C33 C 0.6954(3) 0.23490(14) 0.5847(3) 0.0325(9) Uani 1 1 d . . . . .
H33 H 0.6166 0.2359 0.5831 0.039 Uiso 1 1 calc R U . . .
C34 C 0.7437(3) 0.19703(13) 0.5666(3) 0.0294(9) Uani 1 1 d . . . . .
H34 H 0.6964 0.1722 0.5525 0.035 Uiso 1 1 calc R U . . .
O5W O 0.6249(3) 0.05526(10) 0.3396(3) 0.0607(10) Uani 1 1 d D . . . .
O1S O 1.4983(4) 0.32400(15) 0.5762(4) 0.0882(15) Uani 1 1 d . . . . .
O2S O 1.3454(3) 0.31916(14) 0.6256(3) 0.0679(11) Uani 1 1 d . . . . .
O3S O 1.4285(3) 0.26408(11) 0.6008(3) 0.0477(8) Uani 1 1 d . . . . .
N1S N 1.4246(3) 0.30510(13) 0.6004(3) 0.0439(9) Uani 1 1 d . . . . .
N3S N 0.7897(2) 0.55741(12) -0.2186(3) 0.0422(9) Uani 1 1 d D . . . .
O7S O 0.7615(6) 0.5939(2) -0.2588(6) 0.0520(8) Uani 0.539(9) 1 d D . P A 7
O8S O 0.8183(7) 0.5306(2) -0.2729(6) 0.0520(8) Uani 0.539(9) 1 d D . P A 7
O9S O 0.7864(7) 0.5506(3) -0.1316(5) 0.0520(8) Uani 0.539(9) 1 d D . P A 7
O7SA O 0.8055(9) 0.5429(3) -0.2942(6) 0.0520(8) Uani 0.461(9) 1 d D . P A 8
O8SA O 0.8101(8) 0.5376(3) -0.1326(6) 0.0520(8) Uani 0.461(9) 1 d D . P A 8
O9SA O 0.7559(7) 0.5958(2) -0.2171(7) 0.0520(8) Uani 0.461(9) 1 d D . P A 8
O14W O 0.7224(4) 0.10668(10) 0.2240(3) 0.0602(11) Uani 1 1 d D . . . .
O15W O 1.4115(6) 0.0272(3) 0.4498(6) 0.0407(14) Uani 0.545(8) 1 d . . P B 1
O16W O 1.4152(8) 0.0470(3) 0.4229(7) 0.0407(14) Uani 0.455(8) 1 d . . P B 2
H5WA H 0.617(3) 0.0293(5) 0.321(4) 0.049 Uiso 1 1 d D U . . .
H5WB H 0.5561(17) 0.0643(12) 0.331(4) 0.049 Uiso 1 1 d D U . . .
H1WA H 1.625(4) 0.1418(10) 1.115(2) 0.049 Uiso 1 1 d D U . . .
H2WB H 1.738(2) 0.1011(15) 0.990(2) 0.049 Uiso 1 1 d D U . . .
H1WB H 1.609(4) 0.1829(5) 1.084(3) 0.049 Uiso 1 1 d D U . . .
H2WA H 1.696(3) 0.0896(15) 0.890(2) 0.049 Uiso 1 1 d D U . . .
H3WA H 0.822(3) 0.1421(11) 0.330(3) 0.049 Uiso 1 1 d D U . . .
H4WA H 0.761(4) 0.0905(13) 0.554(2) 0.049 Uiso 1 1 d D U . . .
H3WB H 0.856(4) 0.1821(4) 0.365(3) 0.049 Uiso 1 1 d D U . . .
H4WB H 0.742(3) 0.0886(13) 0.4508(16) 0.049 Uiso 1 1 d D U . . .
H14D H 0.678(4) 0.1215(11) 0.248(4) 0.049 Uiso 1 1 d D U . . .
H14C H 0.703(4) 0.0815(5) 0.234(4) 0.049 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1W 2.082(2) . ?
Co1 O2W 2.100(3) . ?
Co1 N2 2.146(3) . ?
Co1 N9 2.160(3) . ?
Co1 N10 2.171(3) . ?
Co1 N1 2.186(3) . ?
Co2 O3W 2.076(3) . ?
Co2 O4W 2.137(3) . ?
Co2 N13 2.143(3) . ?
Co2 N8 2.149(3) . ?
Co2 N5 2.153(3) . ?
Co2 N16 2.159(3) . ?
O1W H1WA 0.847(10) . ?
O1W H1WB 0.846(10) . ?
O2W H2WB 0.850(10) . ?
O2W H2WA 0.851(10) . ?
O3W H3WA 0.847(10) . ?
O3W H3WB 0.843(10) . ?
O4W H4WA 0.846(7) . ?
O4W H4WB 0.847(7) . ?
N1 C1 1.339(5) . ?
N1 C5 1.344(5) . ?
N2 C7 1.337(5) . ?
N2 C6 1.369(4) . ?
N3 C6 1.323(5) . ?
N3 N4 1.365(5) . ?
N4 C7 1.332(5) . ?
N4 H4 0.8800 . ?
N5 C11 1.338(5) . ?
N5 C12 1.362(5) . ?
N6 C11 1.330(6) . ?
N6 N7 1.342(6) . ?
N6 H6 0.8800 . ?
N7 C12 1.328(5) . ?
N8 C17 1.340(5) . ?
N8 C13 1.360(5) . ?
N9 C18 1.342(5) . ?
N9 C22 1.350(5) . ?
N10 C24 1.337(5) . ?
N10 C23 1.362(5) . ?
N11 C23 1.330(5) . ?
N11 N12 1.362(5) . ?
N12 C24 1.334(5) . ?
N12 H12 0.8800 . ?
N13 C28 1.339(4) . ?
N13 C29 1.357(4) . ?
N14 C28 1.330(4) . ?
N14 N15 1.362(4) . ?
N14 H14 0.8800 . ?
N15 C29 1.320(4) . ?
N16 C30 1.353(5) . ?
N16 C34 1.354(5) . ?
C1 C2 1.385(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.382(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.460(5) . ?
C7 C8 1.483(5) . ?
C8 C9 1.530(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.529(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.460(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C12 C13 1.447(6) . ?
C13 C14 1.378(6) . ?
C14 C15 1.364(8) . ?
C14 H14A 0.9500 . ?
C15 C16 1.379(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.403(6) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.384(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.375(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.379(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.384(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.464(5) . ?
C24 C25 1.493(5) . ?
C25 C26 1.526(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.531(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.493(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C29 C30 1.475(5) . ?
C30 C31 1.385(5) . ?
C31 C32 1.381(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(6) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
O5W H5WA 0.850(10) . ?
O5W H5WB 0.850(10) . ?
O1S N1S 1.207(5) . ?
O2S N1S 1.207(5) . ?
O3S N1S 1.289(5) . ?
N3S O7SA 1.201(7) . ?
N3S O9S 1.220(7) . ?
N3S O8S 1.246(7) . ?
N3S O7S 1.266(7) . ?
N3S O9SA 1.277(7) . ?
N3S O8SA 1.277(8) . ?
O14W H14D 0.853(10) . ?
O14W H14C 0.853(10) . ?

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
O1W Co1 O2W 90.62(11) . . ?
O1W Co1 N2 91.24(10) . . ?
O2W Co1 N2 168.54(11) . . ?
O1W Co1 N9 89.14(11) . . ?
O2W Co1 N9 89.05(11) . . ?
N2 Co1 N9 102.28(11) . . ?
O1W Co1 N10 165.63(10) . . ?
O2W Co1 N10 84.48(11) . . ?
N2 Co1 N10 96.24(10) . . ?
N9 Co1 N10 77.30(11) . . ?
O1W Co1 N1 89.03(10) . . ?
O2W Co1 N1 92.01(11) . . ?
N2 Co1 N1 76.72(11) . . ?
N9 Co1 N1 177.90(11) . . ?
N10 Co1 N1 104.60(11) . . ?
O3W Co2 O4W 90.64(10) . . ?
O3W Co2 N13 91.57(11) . . ?
O4W Co2 N13 168.65(11) . . ?
O3W Co2 N8 89.65(11) . . ?
O4W Co2 N8 92.17(11) . . ?
N13 Co2 N8 98.97(11) . . ?
O3W Co2 N5 166.78(11) . . ?
O4W Co2 N5 85.32(11) . . ?
N13 Co2 N5 94.86(11) . . ?
N8 Co2 N5 77.96(12) . . ?
O3W Co2 N16 89.87(11) . . ?
O4W Co2 N16 91.75(11) . . ?
N13 Co2 N16 77.13(11) . . ?
N8 Co2 N16 176.05(11) . . ?
N5 Co2 N16 102.81(12) . . ?
Co1 O1W H1WA 122(3) . . ?
Co1 O1W H1WB 123(3) . . ?
H1WA O1W H1WB 106(2) . . ?
Co1 O2W H2WB 127(3) . . ?
Co1 O2W H2WA 123(3) . . ?
H2WB O2W H2WA 104(2) . . ?
Co2 O3W H3WA 120(3) . . ?
Co2 O3W H3WB 113(3) . . ?
H3WA O3W H3WB 107(2) . . ?
Co2 O4W H4WA 125(3) . . ?
Co2 O4W H4WB 126(3) . . ?
H4WA O4W H4WB 106.3(18) . . ?
C1 N1 C5 117.7(3) . . ?
C1 N1 Co1 125.9(2) . . ?
C5 N1 Co1 116.0(2) . . ?
C7 N2 C6 103.6(3) . . ?
C7 N2 Co1 143.2(3) . . ?
C6 N2 Co1 112.7(2) . . ?
C6 N3 N4 102.7(3) . . ?
C7 N4 N3 110.7(3) . . ?
C7 N4 H4 124.7 . . ?
N3 N4 H4 124.7 . . ?
C11 N5 C12 103.9(4) . . ?
C11 N5 Co2 143.8(3) . . ?
C12 N5 Co2 111.0(3) . . ?
C11 N6 N7 111.3(4) . . ?
C11 N6 H6 124.3 . . ?
N7 N6 H6 124.3 . . ?
C12 N7 N6 103.0(4) . . ?
C17 N8 C13 118.1(3) . . ?
C17 N8 Co2 127.0(3) . . ?
C13 N8 Co2 114.8(3) . . ?
C18 N9 C22 117.7(3) . . ?
C18 N9 Co1 126.5(3) . . ?
C22 N9 Co1 115.7(2) . . ?
C24 N10 C23 103.4(3) . . ?
C24 N10 Co1 143.8(2) . . ?
C23 N10 Co1 110.6(2) . . ?
C23 N11 N12 102.0(3) . . ?
C24 N12 N11 111.0(3) . . ?
C24 N12 H12 124.5 . . ?
N11 N12 H12 124.5 . . ?
C28 N13 C29 103.7(3) . . ?
C28 N13 Co2 143.3(2) . . ?
C29 N13 Co2 112.9(2) . . ?
C28 N14 N15 110.9(3) . . ?
C28 N14 H14 124.6 . . ?
N15 N14 H14 124.6 . . ?
C29 N15 N14 102.4(3) . . ?
C30 N16 C34 117.2(3) . . ?
C30 N16 Co2 116.7(2) . . ?
C34 N16 Co2 125.9(3) . . ?
N1 C1 C2 122.5(4) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 118.0(4) . . ?
C3 C4 H4A 121.0 . . ?
C5 C4 H4A 121.0 . . ?
N1 C5 C4 123.4(3) . . ?
N1 C5 C6 113.6(3) . . ?
C4 C5 C6 123.0(3) . . ?
N3 C6 N2 113.7(3) . . ?
N3 C6 C5 126.0(3) . . ?
N2 C6 C5 120.3(3) . . ?
N4 C7 N2 109.3(3) . . ?
N4 C7 C8 124.8(3) . . ?
N2 C7 C8 125.9(3) . . ?
C7 C8 C9 113.1(4) . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 113.8(4) . . ?
C10 C9 H9A 108.8 . . ?
C8 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
C8 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C11 C10 C9 109.6(3) . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10B 109.8 . . ?
C9 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
N6 C11 N5 108.6(4) . . ?
N6 C11 C10 123.2(4) . . ?
N5 C11 C10 127.6(4) . . ?
N7 C12 N5 113.2(4) . . ?
N7 C12 C13 126.3(4) . . ?
N5 C12 C13 120.5(3) . . ?
N8 C13 C14 123.3(4) . . ?
N8 C13 C12 114.5(3) . . ?
C14 C13 C12 122.2(4) . . ?
C15 C14 C13 118.2(5) . . ?
C15 C14 H14A 120.9 . . ?
C13 C14 H14A 120.9 . . ?
C14 C15 C16 120.0(4) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 119.4(5) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
N8 C17 C16 121.0(5) . . ?
N8 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
N9 C18 C19 122.5(4) . . ?
N9 C18 H18 118.7 . . ?
C19 C18 H18 118.7 . . ?
C20 C19 C18 119.1(4) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 H19 120.5 . . ?
C19 C20 C21 119.4(4) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C20 C21 C22 118.4(4) . . ?
C20 C21 H21 120.8 . . ?
C22 C21 H21 120.8 . . ?
N9 C22 C21 122.9(4) . . ?
N9 C22 C23 113.7(3) . . ?
C21 C22 C23 123.4(4) . . ?
N11 C23 N10 114.4(3) . . ?
N11 C23 C22 125.0(3) . . ?
N10 C23 C22 120.6(3) . . ?
N12 C24 N10 109.3(3) . . ?
N12 C24 C25 123.5(3) . . ?
N10 C24 C25 127.0(3) . . ?
C24 C25 C26 110.8(3) . . ?
C24 C25 H25A 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C26 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
C25 C26 C27 113.3(3) . . ?
C25 C26 H26A 108.9 . . ?
C27 C26 H26A 108.9 . . ?
C25 C26 H26B 108.9 . . ?
C27 C26 H26B 108.9 . . ?
H26A C26 H26B 107.7 . . ?
C28 C27 C26 113.2(3) . . ?
C28 C27 H27A 108.9 . . ?
C26 C27 H27A 108.9 . . ?
C28 C27 H27B 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
N14 C28 N13 108.8(3) . . ?
N14 C28 C27 125.2(3) . . ?
N13 C28 C27 125.9(3) . . ?
N15 C29 N13 114.2(3) . . ?
N15 C29 C30 125.6(3) . . ?
N13 C29 C30 120.2(3) . . ?
N16 C30 C31 123.5(3) . . ?
N16 C30 C29 112.8(3) . . ?
C31 C30 C29 123.7(3) . . ?
C32 C31 C30 118.3(4) . . ?
C32 C31 H31 120.9 . . ?
C30 C31 H31 120.9 . . ?
C31 C32 C33 119.4(3) . . ?
C31 C32 H32 120.3 . . ?
C33 C32 H32 120.3 . . ?
C34 C33 C32 119.0(4) . . ?
C34 C33 H33 120.5 . . ?
C32 C33 H33 120.5 . . ?
N16 C34 C33 122.6(4) . . ?
N16 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
H5WA O5W H5WB 106(2) . . ?
O1S N1S O2S 129.1(5) . . ?
O1S N1S O3S 117.6(4) . . ?
O2S N1S O3S 113.3(4) . . ?
O9S N3S O8S 124.6(5) . . ?
O9S N3S O7S 119.2(5) . . ?
O8S N3S O7S 116.2(5) . . ?
O7SA N3S O9SA 121.1(5) . . ?
O7SA N3S O8SA 124.5(6) . . ?
O9SA N3S O8SA 114.2(5) . . ?
H14D O14W H14C 101(2) . . ?

_refine_diff_density_max         1.076
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.085



# start Validation Reply Form
_vrf_PLAT417_2b                  
;
RESPONSE: The hydrogen atoms on coordinated and lattice 
molecules of water were placed to positions as found from the Fourier maps
and they were constrained by DFIX instructions. However, the so obtained results
 might be affected by heavy disorder of anions and lattice solvent molecules 
followed by SQUEEZE procedure. 
;
_vrf_PLAT420_2b                  
;
RESPONSE: This is due to the removement of the disorder lattice water
molecules and two nitrate anions.
;
_vrf_PLAT230_2b                  
;
RESPONSE: The crystal structure of 2b is heavily disordered
 which resulted also to use of SQUEEZE procedure.
It was not possible to model these atoms in better way.  
;



####################################################################### 
# 
# 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_1a
_database_code_depnum_ccdc_archive 'CCDC 1907069'
loop_
_audit_author_name
_audit_author_address
I.Nemec
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-05-09 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H22 N10 Ni O10'
_chemical_formula_weight         573.14

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

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

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

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

_cell_length_a                   8.1311(6)
_cell_length_b                   27.5357(19)
_cell_length_c                   10.5281(7)
_cell_angle_alpha                90
_cell_angle_beta                 102.1120(10)
_cell_angle_gamma                90
_cell_volume                     2304.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3013
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      25.09

_exptl_crystal_description       cubic
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_F_000             1184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.918
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.914
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.9138
_exptl_absorpt_correction_T_max  0.9138
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18005
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.479
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5035
_reflns_number_gt                3670
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0446P)²+1.4716P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5035
_refine_ls_number_parameters     356
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1071
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.046
_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 0.41184(4) 0.63439(2) 0.04873(3) 0.01565(11) Uani 1 1 d . . . . .
N1 N 0.5983(3) 0.68053(8) -0.0098(2) 0.0188(5) Uani 1 1 d . . . . .
N2 N 0.6215(3) 0.61748(8) 0.1860(2) 0.0196(5) Uani 1 1 d . . . . .
N3 N 0.8311(3) 0.60093(9) 0.3420(3) 0.0254(6) Uani 1 1 d . . . . .
H3 H 0.8910 0.5869 0.4117 0.031 Uiso 1 1 calc R U . . .
N4 N 0.8882(3) 0.63765(9) 0.2768(3) 0.0260(6) Uani 1 1 d . . . . .
N5 N 0.2635(3) 0.59114(8) 0.1345(2) 0.0185(5) Uani 1 1 d . . . . .
N6 N 0.0181(3) 0.55142(9) 0.1099(3) 0.0238(6) Uani 1 1 d . . . . .
N7 N 0.1237(3) 0.53916(9) 0.2234(3) 0.0245(6) Uani 1 1 d . . . . .
H7 H 0.0992 0.5182 0.2797 0.029 Uiso 1 1 calc R U . . .
N8 N 0.1762(3) 0.63958(8) -0.0902(2) 0.0187(5) Uani 1 1 d . . . . .
O1 O 0.3472(3) 0.69315(8) 0.1498(2) 0.0318(6) Uani 1 1 d D . . . .
O2 O 0.4578(2) 0.57728(7) -0.0684(2) 0.0199(4) Uani 1 1 d D . . . .
C1 C 0.5837(4) 0.70943(11) -0.1137(3) 0.0251(7) Uani 1 1 d . . . . .
H1 H 0.4798 0.7097 -0.1750 0.030 Uiso 1 1 calc R U . . .
C2 C 0.7115(4) 0.73876(11) -0.1361(3) 0.0306(8) Uani 1 1 d . . . . .
H2 H 0.6951 0.7591 -0.2106 0.037 Uiso 1 1 calc R U . . .
C3 C 0.8637(4) 0.73829(11) -0.0487(3) 0.0311(8) Uani 1 1 d . . . . .
H3A H 0.9539 0.7581 -0.0625 0.037 Uiso 1 1 calc R U . . .
C4 C 0.8832(4) 0.70857(11) 0.0593(3) 0.0264(7) Uani 1 1 d . . . . .
H4 H 0.9868 0.7075 0.1209 0.032 Uiso 1 1 calc R U . . .
C5 C 0.7480(4) 0.68034(10) 0.0754(3) 0.0188(6) Uani 1 1 d . . . . .
C6 C 0.7565(4) 0.64625(10) 0.1830(3) 0.0198(6) Uani 1 1 d . . . . .
C7 C 0.6722(4) 0.58858(10) 0.2874(3) 0.0213(6) Uani 1 1 d . . . . .
C8 C 0.5803(4) 0.54679(11) 0.3299(3) 0.0262(7) Uani 1 1 d . . . . .
H8A H 0.6503 0.5331 0.4103 0.031 Uiso 1 1 calc R U . . .
H8B H 0.5671 0.5213 0.2622 0.031 Uiso 1 1 calc R U . . .
C9 C 0.4062(4) 0.55879(11) 0.3559(3) 0.0256(7) Uani 1 1 d . . . . .
H9A H 0.3750 0.5332 0.4125 0.031 Uiso 1 1 calc R U . . .
H9B H 0.4139 0.5898 0.4043 0.031 Uiso 1 1 calc R U . . .
C10 C 0.2694(4) 0.56305(10) 0.2383(3) 0.0215(7) Uani 1 1 d . . . . .
C11 C 0.1086(4) 0.58315(10) 0.0602(3) 0.0186(6) Uani 1 1 d . . . . .
C12 C 0.0573(3) 0.60902(10) -0.0634(3) 0.0193(6) Uani 1 1 d . . . . .
C13 C -0.0981(4) 0.60299(11) -0.1450(3) 0.0256(7) Uani 1 1 d . . . . .
H13 H -0.1782 0.5813 -0.1225 0.031 Uiso 1 1 calc R U . . .
C14 C -0.1357(4) 0.62895(11) -0.2599(3) 0.0274(7) Uani 1 1 d . . . . .
H14 H -0.2417 0.6254 -0.3178 0.033 Uiso 1 1 calc R U . . .
C15 C -0.0158(4) 0.66005(11) -0.2884(3) 0.0275(7) Uani 1 1 d . . . . .
H15 H -0.0377 0.6782 -0.3669 0.033 Uiso 1 1 calc R U . . .
C16 C 0.1371(4) 0.66455(10) -0.2016(3) 0.0234(7) Uani 1 1 d . . . . .
H16 H 0.2181 0.6864 -0.2221 0.028 Uiso 1 1 calc R U . . .
N1S N 0.0559(3) 0.54400(9) 0.6132(2) 0.0212(5) Uani 1 1 d . . . . .
O1S O 0.1119(3) 0.57274(7) 0.5393(2) 0.0267(5) Uani 1 1 d . . . . .
O2S O -0.0963(2) 0.53168(8) 0.5834(2) 0.0259(5) Uani 1 1 d . . . . .
O3S O 0.1476(3) 0.52854(8) 0.7139(2) 0.0311(5) Uani 1 1 d . . . . .
N2S N 0.3516(4) 0.70324(10) 0.4768(3) 0.0399(8) Uani 1 1 d D . . . .
O4S O 0.4142(7) 0.67383(18) 0.4059(5) 0.0467(6) Uani 0.685(7) 1 d D . P A 1
O5S O 0.2633(6) 0.73706(16) 0.4261(5) 0.0467(6) Uani 0.685(7) 1 d D . P A 1
O6S O 0.4000(7) 0.70028(16) 0.5979(4) 0.0467(6) Uani 0.685(7) 1 d D . P A 1
O4SA O 0.4408(16) 0.6718(4) 0.4491(10) 0.0467(6) Uani 0.315(7) 1 d D . P A 2
O6SA O 0.3241(16) 0.7124(4) 0.5866(9) 0.0467(6) Uani 0.315(7) 1 d D . P A 2
O5SA O 0.2531(14) 0.7263(4) 0.3798(10) 0.0467(6) Uani 0.315(7) 1 d D . P A 2
O1W O -0.3022(3) 0.51258(8) 0.0102(2) 0.0272(5) Uani 1 1 d D . . . .
O2W O 0.4407(3) 0.60082(9) 0.6797(2) 0.0340(6) Uani 1 1 d D . . . .
H1WA H -0.210(4) 0.5207(12) 0.043(4) 0.051 Uiso 1 1 d D U . . .
H1WB H -0.327(4) 0.4862(8) 0.044(3) 0.051 Uiso 1 1 d D U . . .
H2WA H 0.442(4) 0.6307(5) 0.656(4) 0.051 Uiso 1 1 d D U . . .
H2WB H 0.344(2) 0.5908(11) 0.642(3) 0.051 Uiso 1 1 d D U . . .
H2A H 0.548(3) 0.5618(12) -0.042(3) 0.051 Uiso 1 1 d D U . . .
H1B H 0.334(5) 0.7222(6) 0.123(3) 0.051 Uiso 1 1 d D U . . .
H2B H 0.456(4) 0.5873(13) -0.1449(17) 0.051 Uiso 1 1 d D U . . .
H1A H 0.357(5) 0.6935(12) 0.2308(11) 0.051 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N5 2.036(2) . ?
Ni1 N2 2.044(2) . ?
Ni1 O1 2.064(2) . ?
Ni1 O2 2.080(2) . ?
Ni1 N8 2.157(2) . ?
Ni1 N1 2.164(2) . ?
N1 C1 1.337(4) . ?
N1 C5 1.352(4) . ?
N2 C7 1.326(4) . ?
N2 C6 1.359(4) . ?
N3 C7 1.343(4) . ?
N3 N4 1.358(3) . ?
N4 C6 1.316(4) . ?
N5 C10 1.331(4) . ?
N5 C11 1.354(4) . ?
N6 C11 1.319(4) . ?
N6 N7 1.360(4) . ?
N7 C10 1.335(4) . ?
N8 C16 1.339(4) . ?
N8 C12 1.356(4) . ?
C1 C2 1.375(4) . ?
C2 C3 1.378(5) . ?
C3 C4 1.382(4) . ?
C4 C5 1.386(4) . ?
C5 C6 1.462(4) . ?
C7 C8 1.491(4) . ?
C8 C9 1.533(4) . ?
C9 C10 1.485(4) . ?
C11 C12 1.466(4) . ?
C12 C13 1.381(4) . ?
C13 C14 1.383(4) . ?
C14 C15 1.378(4) . ?
C15 C16 1.385(4) . ?
N1S O3S 1.236(3) . ?
N1S O2S 1.258(3) . ?
N1S O1S 1.260(3) . ?
N2S O4SA 1.204(10) . ?
N2S O5S 1.228(5) . ?
N2S O6SA 1.249(8) . ?
N2S O6S 1.256(5) . ?
N2S O4S 1.277(5) . ?
N2S O5SA 1.320(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ni1 N2 92.13(9) . . ?
N5 Ni1 O1 89.50(9) . . ?
N2 Ni1 O1 94.54(10) . . ?
N5 Ni1 O2 91.02(8) . . ?
N2 Ni1 O2 91.14(9) . . ?
O1 Ni1 O2 174.28(9) . . ?
N5 Ni1 N8 79.35(9) . . ?
N2 Ni1 N8 169.99(9) . . ?
O1 Ni1 N8 90.65(10) . . ?
O2 Ni1 N8 83.84(8) . . ?
N5 Ni1 N1 170.12(10) . . ?
N2 Ni1 N1 78.75(9) . . ?
O1 Ni1 N1 87.48(9) . . ?
O2 Ni1 N1 92.93(8) . . ?
N8 Ni1 N1 110.08(9) . . ?
C1 N1 C5 117.3(2) . . ?
C1 N1 Ni1 129.4(2) . . ?
C5 N1 Ni1 113.29(18) . . ?
C7 N2 C6 104.6(2) . . ?
C7 N2 Ni1 141.1(2) . . ?
C6 N2 Ni1 114.14(19) . . ?
C7 N3 N4 111.8(2) . . ?
C6 N4 N3 101.7(2) . . ?
C10 N5 C11 104.4(2) . . ?
C10 N5 Ni1 141.4(2) . . ?
C11 N5 Ni1 113.87(18) . . ?
C11 N6 N7 102.2(2) . . ?
C10 N7 N6 111.3(2) . . ?
C16 N8 C12 116.9(3) . . ?
C16 N8 Ni1 129.9(2) . . ?
C12 N8 Ni1 112.87(19) . . ?
N1 C1 C2 123.3(3) . . ?
C1 C2 C3 119.0(3) . . ?
C2 C3 C4 119.1(3) . . ?
C3 C4 C5 118.4(3) . . ?
N1 C5 C4 122.9(3) . . ?
N1 C5 C6 114.0(2) . . ?
C4 C5 C6 123.1(3) . . ?
N4 C6 N2 114.3(3) . . ?
N4 C6 C5 126.6(3) . . ?
N2 C6 C5 119.0(3) . . ?
N2 C7 N3 107.5(3) . . ?
N2 C7 C8 127.9(3) . . ?
N3 C7 C8 124.4(3) . . ?
C7 C8 C9 115.3(3) . . ?
C10 C9 C8 115.3(2) . . ?
N5 C10 N7 108.1(3) . . ?
N5 C10 C9 128.4(3) . . ?
N7 C10 C9 123.4(3) . . ?
N6 C11 N5 114.1(3) . . ?
N6 C11 C12 126.5(3) . . ?
N5 C11 C12 119.4(2) . . ?
N8 C12 C13 123.0(3) . . ?
N8 C12 C11 113.8(2) . . ?
C13 C12 C11 123.2(3) . . ?
C12 C13 C14 119.2(3) . . ?
C15 C14 C13 118.4(3) . . ?
C14 C15 C16 119.3(3) . . ?
N8 C16 C15 123.2(3) . . ?
O3S N1S O2S 120.4(2) . . ?
O3S N1S O1S 121.0(2) . . ?
O2S N1S O1S 118.6(2) . . ?
O4SA N2S O6SA 127.1(6) . . ?
O5S N2S O6S 121.3(3) . . ?
O5S N2S O4S 119.7(3) . . ?
O6S N2S O4S 118.3(4) . . ?
O4SA N2S O5SA 117.2(6) . . ?
O6SA N2S O5SA 114.9(6) . . ?

_refine_diff_density_max         0.776
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.084

####################################################################### 
# 
# 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_5c
_database_code_depnum_ccdc_archive 'CCDC 1907076'
loop_
_audit_author_name
_audit_author_address
I.Nemec
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-05-09 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 B2 F8 Fe2 N16 O10'
_chemical_formula_weight         1254.36

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.527(5)
_cell_length_b                   12.915(5)
_cell_length_c                   18.114(4)
_cell_angle_alpha                90
_cell_angle_beta                 125.778(18)
_cell_angle_gamma                90
_cell_volume                     2757.1(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9688
_cell_measurement_theta_min      3.002
_cell_measurement_theta_max      26.972

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_F_000             1292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.623
_shelx_estimated_absorpt_T_min   0.845
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_T_min  0.90226
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24841
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.155
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_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             4846
_reflns_number_gt                3826
_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       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+0.5573P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4846
_refine_ls_number_parameters     397
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0898
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.068
_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
Fe1 Fe 0.59243(2) 0.67988(2) 0.48360(2) 0.01874(11) Uani 1 1 d . . . . .
O1 O 0.45519(11) 0.57208(10) 0.40339(9) 0.0214(3) Uani 1 1 d . . . . .
O2 O 0.61934(11) 0.57075(11) 0.58191(9) 0.0224(3) Uani 1 1 d . . . . .
N1 N 0.70215(14) 0.60270(13) 0.45559(11) 0.0215(4) Uani 1 1 d . . . . .
N2 N 0.80742(15) 0.52392(14) 0.42554(13) 0.0294(4) Uani 1 1 d . . . . .
H1N2 H 0.8572 0.4801 0.4305 0.035 Uiso 1 1 calc R U . . .
N3 N 0.74950(15) 0.59358(14) 0.35740(12) 0.0288(4) Uani 1 1 d . . . . .
N4 N 0.55422(13) 0.75989(13) 0.36308(11) 0.0196(4) Uani 1 1 d . . . . .
N5 N 0.50052(14) 0.78540(13) 0.51236(11) 0.0212(4) Uani 1 1 d . . . . .
N6 N 0.41103(15) 0.89011(14) 0.54326(12) 0.0278(4) Uani 1 1 d . . . . .
H1N6 H 0.3559 0.9175 0.5437 0.033 Uiso 1 1 calc R U . . .
N7 N 0.51790(15) 0.92914(14) 0.58944(12) 0.0274(4) Uani 1 1 d . . . . .
N8 N 0.72125(14) 0.79410(13) 0.57211(11) 0.0204(4) Uani 1 1 d . . . . .
C1 C 0.83555(19) 0.46986(17) 0.57072(15) 0.0294(5) Uani 1 1 d . . . . .
H1A H 0.7860 0.4725 0.5916 0.035 Uiso 1 1 calc R U . . .
H1B H 0.9079 0.5043 0.6176 0.035 Uiso 1 1 calc R U . . .
C2 C 0.78042(17) 0.52931(16) 0.48445(14) 0.0232(5) Uani 1 1 d . . . . .
C3 C 0.68702(17) 0.63989(16) 0.37858(14) 0.0216(5) Uani 1 1 d . . . . .
C4 C 0.61057(17) 0.72661(16) 0.32907(14) 0.0212(5) Uani 1 1 d . . . . .
C5 C 0.60023(18) 0.77424(18) 0.25647(15) 0.0282(5) Uani 1 1 d . . . . .
H5 H 0.6398 0.7484 0.2332 0.034 Uiso 1 1 calc R U . . .
C6 C 0.5314(2) 0.85999(19) 0.21837(15) 0.0334(6) Uani 1 1 d . . . . .
H6 H 0.5239 0.8950 0.1690 0.040 Uiso 1 1 calc R U . . .
C7 C 0.4736(2) 0.89452(18) 0.25231(15) 0.0323(5) Uani 1 1 d . . . . .
H7 H 0.4257 0.9535 0.2268 0.039 Uiso 1 1 calc R U . . .
C8 C 0.48627(18) 0.84212(16) 0.32392(15) 0.0257(5) Uani 1 1 d . . . . .
H8 H 0.4450 0.8654 0.3465 0.031 Uiso 1 1 calc R U . . .
C9 C 0.82851(17) 0.79770(17) 0.59766(14) 0.0247(5) Uani 1 1 d . . . . .
H9 H 0.8539 0.7443 0.5775 0.030 Uiso 1 1 calc R U . . .
C10 C 0.90301(19) 0.87466(17) 0.65136(15) 0.0294(5) Uani 1 1 d . . . . .
H10 H 0.9782 0.8747 0.6676 0.035 Uiso 1 1 calc R U . . .
C11 C 0.86718(19) 0.95214(18) 0.68146(15) 0.0312(5) Uani 1 1 d . . . . .
H11 H 0.9174 1.0063 0.7189 0.037 Uiso 1 1 calc R U . . .
C12 C 0.75744(19) 0.94988(17) 0.65643(15) 0.0287(5) Uani 1 1 d . . . . .
H12 H 0.7310 1.0019 0.6769 0.034 Uiso 1 1 calc R U . . .
C13 C 0.68714(17) 0.87080(16) 0.60130(13) 0.0213(5) Uani 1 1 d . . . . .
C14 C 0.56823(17) 0.86358(16) 0.56861(13) 0.0208(4) Uani 1 1 d . . . . .
C15 C 0.40049(18) 0.80523(16) 0.49739(14) 0.0239(5) Uani 1 1 d . . . . .
C16 C 0.29450(18) 0.74395(18) 0.44089(15) 0.0299(5) Uani 1 1 d . . . . .
H16A H 0.3100 0.6815 0.4181 0.036 Uiso 1 1 calc R U . . .
H16B H 0.2371 0.7858 0.3875 0.036 Uiso 1 1 calc R U . . .
C17 C 0.2456(2) 0.71036(18) 0.49268(16) 0.0312(5) Uani 1 1 d . . . . .
H17A H 0.3042 0.6713 0.5476 0.037 Uiso 1 1 calc R U . . .
H17B H 0.2266 0.7728 0.5130 0.037 Uiso 1 1 calc R U . . .
C18 C 0.13992(19) 0.64337(18) 0.43590(16) 0.0317(5) Uani 1 1 d . . . . .
H18A H 0.0910 0.6726 0.3737 0.038 Uiso 1 1 calc R U . . .
H18B H 0.0969 0.6465 0.4627 0.038 Uiso 1 1 calc R U . . .
C20 C 0.45245(17) 0.50029(15) 0.44847(13) 0.0176(4) Uani 1 1 d . . . . .
F1A F 0.0521(2) 0.8833(2) 0.0848(2) 0.0473(6) Uani 0.947(9) 1 d . . P A 1
F2A F 0.2229(2) 0.8615(2) 0.2187(2) 0.0490(7) Uani 0.947(9) 1 d . . P A 1
F3A F 0.0612(3) 0.8339(2) 0.2083(2) 0.0495(7) Uani 0.947(9) 1 d . . P A 1
F4A F 0.1135(3) 0.72238(15) 0.1431(2) 0.0498(7) Uani 0.947(9) 1 d D . P A 1
B1 B 0.1136(2) 0.8248(2) 0.16508(19) 0.0306(6) Uani 1 1 d . . . . .
O1S O 0.04634(16) 0.58859(16) 0.91156(13) 0.0549(5) Uani 1 1 d . . . . .
C1S C -0.0435(2) 0.62959(19) 0.88057(16) 0.0334(5) Uani 1 1 d . . . . .
C2S C -0.0831(2) 0.6542(2) 0.93786(18) 0.0476(7) Uani 1 1 d . . . . .
H2S1 H -0.0352 0.6181 0.9963 0.071 Uiso 1 1 calc R U . . .
H2S2 H -0.1620 0.6316 0.9067 0.071 Uiso 1 1 calc R U . . .
H2S3 H -0.0781 0.7290 0.9485 0.071 Uiso 1 1 calc R U . . .
C3S C -0.1180(2) 0.6631(3) 0.78420(18) 0.0525(8) Uani 1 1 d . . . . .
H3S1 H -0.0757 0.6604 0.7575 0.079 Uiso 1 1 calc R U . . .
H3S2 H -0.1439 0.7341 0.7810 0.079 Uiso 1 1 calc R U . . .
H3S3 H -0.1839 0.6169 0.7503 0.079 Uiso 1 1 calc R U . . .
O2S O 0.25946(14) 0.98434(14) 0.55942(11) 0.0366(4) Uani 1 1 d D . . . .
O3S O 0.2737(2) 0.5676(2) 0.21133(14) 0.0855(9) Uani 1 1 d D . . . .
F1B F 0.075(4) 0.916(4) 0.115(3) 0.0473(6) Uani 0.053(9) 1 d . . P A 2
F3B F 0.071(6) 0.804(5) 0.206(5) 0.0495(7) Uani 0.053(9) 1 d . . P A 2
F4B F 0.062(5) 0.738(3) 0.103(4) 0.0498(7) Uani 0.053(9) 1 d . . P A 2
F2B F 0.231(5) 0.837(5) 0.242(4) 0.0490(7) Uani 0.053(9) 1 d . . P A 2
H2SA H 0.267(2) 0.969(2) 0.6083(12) 0.059 Uiso 1 1 d D U . . .
H2SB H 0.1920(11) 0.969(2) 0.5185(14) 0.059 Uiso 1 1 d D U . . .
H3SB H 0.3259(17) 0.565(2) 0.2676(8) 0.059 Uiso 1 1 d D U . . .
H3SA H 0.2261(19) 0.6195(16) 0.1946(18) 0.059 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O2 2.1204(14) . ?
Fe1 O1 2.1534(15) . ?
Fe1 N5 2.1736(17) . ?
Fe1 N4 2.1737(17) . ?
Fe1 N1 2.1764(17) . ?
Fe1 N8 2.1772(18) . ?
O1 C20 1.251(2) . ?
O2 C20 1.249(2) 3_666 ?
N1 C2 1.330(3) . ?
N1 C3 1.366(3) . ?
N2 C2 1.337(3) . ?
N2 N3 1.351(3) . ?
N2 H1N2 0.8800 . ?
N3 C3 1.318(3) . ?
N4 C8 1.337(3) . ?
N4 C4 1.351(3) . ?
N5 C15 1.338(3) . ?
N5 C14 1.361(3) . ?
N6 C15 1.329(3) . ?
N6 N7 1.359(3) . ?
N6 H1N6 0.8800 . ?
N7 C14 1.310(3) . ?
N8 C9 1.342(3) . ?
N8 C13 1.346(3) . ?
C1 C2 1.486(3) . ?
C1 C18 1.526(3) 3_666 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C3 C4 1.459(3) . ?
C4 C5 1.378(3) . ?
C5 C6 1.377(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.373(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.376(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.369(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.379(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.380(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.375(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.465(3) . ?
C15 C16 1.484(3) . ?
C16 C17 1.534(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.522(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C1 1.526(3) 3_666 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 O2 1.249(2) 3_666 ?
C20 C20 1.542(4) 3_666 ?
F1A B1 1.401(3) . ?
F2A B1 1.372(4) . ?
F3A B1 1.379(4) . ?
F4A B1 1.382(3) . ?
B1 F3B 1.23(7) . ?
B1 F1B 1.38(4) . ?
B1 F4B 1.45(4) . ?
B1 F2B 1.45(6) . ?
O1S C1S 1.201(3) . ?
C1S C3S 1.482(4) . ?
C1S C2S 1.485(3) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?
O2S H2SA 0.847(10) . ?
O2S H2SB 0.837(10) . ?
O3S H3SB 0.843(10) . ?
O3S H3SA 0.880(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Fe1 O1 77.31(6) . . ?
O2 Fe1 N5 93.03(6) . . ?
O1 Fe1 N5 96.37(6) . . ?
O2 Fe1 N4 166.62(6) . . ?
O1 Fe1 N4 92.16(6) . . ?
N5 Fe1 N4 96.35(7) . . ?
O2 Fe1 N1 95.21(6) . . ?
O1 Fe1 N1 93.55(6) . . ?
N5 Fe1 N1 168.29(6) . . ?
N4 Fe1 N1 77.02(6) . . ?
O2 Fe1 N8 100.07(6) . . ?
O1 Fe1 N8 173.23(6) . . ?
N5 Fe1 N8 77.45(7) . . ?
N4 Fe1 N8 91.28(7) . . ?
N1 Fe1 N8 92.90(7) . . ?
C20 O1 Fe1 114.13(12) . . ?
C20 O2 Fe1 114.94(12) 3_666 . ?
C2 N1 C3 104.01(17) . . ?
C2 N1 Fe1 143.99(14) . . ?
C3 N1 Fe1 111.99(13) . . ?
C2 N2 N3 112.21(17) . . ?
C2 N2 H1N2 123.9 . . ?
N3 N2 H1N2 123.9 . . ?
C3 N3 N2 101.72(17) . . ?
C8 N4 C4 117.86(17) . . ?
C8 N4 Fe1 125.90(13) . . ?
C4 N4 Fe1 116.09(13) . . ?
C15 N5 C14 103.50(17) . . ?
C15 N5 Fe1 144.89(15) . . ?
C14 N5 Fe1 111.60(13) . . ?
C15 N6 N7 111.31(17) . . ?
C15 N6 H1N6 124.3 . . ?
N7 N6 H1N6 124.3 . . ?
C14 N7 N6 102.25(17) . . ?
C9 N8 C13 117.31(18) . . ?
C9 N8 Fe1 127.03(14) . . ?
C13 N8 Fe1 115.62(13) . . ?
C2 C1 C18 114.79(19) . 3_666 ?
C2 C1 H1A 108.6 . . ?
C18 C1 H1A 108.6 3_666 . ?
C2 C1 H1B 108.6 . . ?
C18 C1 H1B 108.6 3_666 . ?
H1A C1 H1B 107.5 . . ?
N1 C2 N2 107.80(19) . . ?
N1 C2 C1 126.34(19) . . ?
N2 C2 C1 125.67(19) . . ?
N3 C3 N1 114.25(19) . . ?
N3 C3 C4 125.18(19) . . ?
N1 C3 C4 120.52(17) . . ?
N4 C4 C5 122.4(2) . . ?
N4 C4 C3 114.25(17) . . ?
C5 C4 C3 123.26(19) . . ?
C6 C5 C4 118.6(2) . . ?
C6 C5 H5 120.7 . . ?
C4 C5 H5 120.7 . . ?
C7 C6 C5 119.5(2) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 118.8(2) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
N4 C8 C7 122.8(2) . . ?
N4 C8 H8 118.6 . . ?
C7 C8 H8 118.6 . . ?
N8 C9 C10 123.1(2) . . ?
N8 C9 H9 118.4 . . ?
C10 C9 H9 118.4 . . ?
C9 C10 C11 118.9(2) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C10 C11 C12 119.1(2) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C13 C12 C11 118.6(2) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N8 C13 C12 123.0(2) . . ?
N8 C13 C14 114.34(18) . . ?
C12 C13 C14 122.69(19) . . ?
N7 C14 N5 114.47(18) . . ?
N7 C14 C13 124.55(19) . . ?
N5 C14 C13 120.98(18) . . ?
N6 C15 N5 108.46(18) . . ?
N6 C15 C16 124.39(19) . . ?
N5 C15 C16 127.14(19) . . ?
C15 C16 C17 113.20(19) . . ?
C15 C16 H16A 108.9 . . ?
C17 C16 H16A 108.9 . . ?
C15 C16 H16B 108.9 . . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 C16 113.09(19) . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
C16 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 C1 114.10(19) . 3_666 ?
C17 C18 H18A 108.7 . . ?
C1 C18 H18A 108.7 3_666 . ?
C17 C18 H18B 108.7 . . ?
C1 C18 H18B 108.7 3_666 . ?
H18A C18 H18B 107.6 . . ?
O2 C20 O1 126.40(18) 3_666 . ?
O2 C20 C20 117.1(2) 3_666 3_666 ?
O1 C20 C20 116.5(2) . 3_666 ?
F2A B1 F3A 111.3(3) . . ?
F2A B1 F4A 109.9(2) . . ?
F3A B1 F4A 109.7(2) . . ?
F3B B1 F1B 115(3) . . ?
F2A B1 F1A 108.7(2) . . ?
F3A B1 F1A 108.4(2) . . ?
F4A B1 F1A 108.9(2) . . ?
F3B B1 F4B 94(3) . . ?
F1B B1 F4B 109(2) . . ?
F3B B1 F2B 100(4) . . ?
F1B B1 F2B 110(3) . . ?
F4B B1 F2B 128(3) . . ?
O1S C1S C3S 121.7(2) . . ?
O1S C1S C2S 121.8(2) . . ?
C3S C1S C2S 116.5(2) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C1S C3S H3S1 109.5 . . ?
C1S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
C1S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
H2SA O2S H2SB 104(3) . . ?
H3SB O3S H3SA 114(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 N3 C3 -0.2(2) . . . . ?
C15 N6 N7 C14 -0.1(2) . . . . ?
C3 N1 C2 N2 -0.9(2) . . . . ?
Fe1 N1 C2 N2 177.68(17) . . . . ?
C3 N1 C2 C1 174.3(2) . . . . ?
Fe1 N1 C2 C1 -7.1(4) . . . . ?
N3 N2 C2 N1 0.7(2) . . . . ?
N3 N2 C2 C1 -174.54(19) . . . . ?
C18 C1 C2 N1 143.6(2) 3_666 . . . ?
C18 C1 C2 N2 -42.0(3) 3_666 . . . ?
N2 N3 C3 N1 -0.4(2) . . . . ?
N2 N3 C3 C4 177.05(19) . . . . ?
C2 N1 C3 N3 0.8(2) . . . . ?
Fe1 N1 C3 N3 -178.27(14) . . . . ?
C2 N1 C3 C4 -176.74(18) . . . . ?
Fe1 N1 C3 C4 4.2(2) . . . . ?
C8 N4 C4 C5 0.0(3) . . . . ?
Fe1 N4 C4 C5 -175.84(16) . . . . ?
C8 N4 C4 C3 177.09(18) . . . . ?
Fe1 N4 C4 C3 1.2(2) . . . . ?
N3 C3 C4 N4 179.02(19) . . . . ?
N1 C3 C4 N4 -3.7(3) . . . . ?
N3 C3 C4 C5 -4.0(3) . . . . ?
N1 C3 C4 C5 173.31(19) . . . . ?
N4 C4 C5 C6 1.2(3) . . . . ?
C3 C4 C5 C6 -175.6(2) . . . . ?
C4 C5 C6 C7 -1.2(3) . . . . ?
C5 C6 C7 C8 0.0(3) . . . . ?
C4 N4 C8 C7 -1.3(3) . . . . ?
Fe1 N4 C8 C7 174.17(16) . . . . ?
C6 C7 C8 N4 1.2(3) . . . . ?
C13 N8 C9 C10 0.2(3) . . . . ?
Fe1 N8 C9 C10 177.76(16) . . . . ?
N8 C9 C10 C11 0.4(3) . . . . ?
C9 C10 C11 C12 -0.1(3) . . . . ?
C10 C11 C12 C13 -0.8(3) . . . . ?
C9 N8 C13 C12 -1.2(3) . . . . ?
Fe1 N8 C13 C12 -179.00(16) . . . . ?
C9 N8 C13 C14 178.27(17) . . . . ?
Fe1 N8 C13 C14 0.4(2) . . . . ?
C11 C12 C13 N8 1.5(3) . . . . ?
C11 C12 C13 C14 -177.9(2) . . . . ?
N6 N7 C14 N5 -0.1(2) . . . . ?
N6 N7 C14 C13 179.78(19) . . . . ?
C15 N5 C14 N7 0.3(2) . . . . ?
Fe1 N5 C14 N7 -179.16(14) . . . . ?
C15 N5 C14 C13 -179.60(18) . . . . ?
Fe1 N5 C14 C13 1.0(2) . . . . ?
N8 C13 C14 N7 179.19(19) . . . . ?
C12 C13 C14 N7 -1.4(3) . . . . ?
N8 C13 C14 N5 -1.0(3) . . . . ?
C12 C13 C14 N5 178.45(19) . . . . ?
N7 N6 C15 N5 0.3(2) . . . . ?
N7 N6 C15 C16 179.46(19) . . . . ?
C14 N5 C15 N6 -0.3(2) . . . . ?
Fe1 N5 C15 N6 178.74(17) . . . . ?
C14 N5 C15 C16 -179.5(2) . . . . ?
Fe1 N5 C15 C16 -0.4(4) . . . . ?
N6 C15 C16 C17 -53.9(3) . . . . ?
N5 C15 C16 C17 125.0(2) . . . . ?
C15 C16 C17 C18 -177.36(19) . . . . ?
C16 C17 C18 C1 79.7(3) . . . 3_666 ?
Fe1 O1 C20 O2 178.93(15) . . . 3_666 ?
Fe1 O1 C20 C20 -1.3(2) . . . 3_666 ?

_refine_diff_density_max         0.674
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.060

####################################################################### 
# 
# 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_4c
_database_code_depnum_ccdc_archive 'CCDC 1907075'
loop_
_audit_author_name
_audit_author_address
I.Nemec
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-05-09 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H32 B2 F8 Fe2 N16 O4'
_chemical_formula_weight         1038.09

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.445(5)
_cell_length_b                   15.122(5)
_cell_length_c                   16.263(5)
_cell_angle_alpha                90
_cell_angle_beta                 128.124(19)
_cell_angle_gamma                90
_cell_volume                     2407.7(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    12096
_cell_measurement_theta_min      3.1209
_cell_measurement_theta_max      33.2578

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_F_000             1052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.688
_shelx_estimated_absorpt_T_min   0.820
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_T_min  0.95754
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22230
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.130
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_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             4239
_reflns_number_gt                3174
_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       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0903P)²+3.0298P] 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         4239
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1631
_refine_ls_wR_factor_gt          0.1562
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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
C1 C 0.4675(4) 0.3458(2) 0.7829(3) 0.0262(8) Uani 1 1 d . . . . .
H1 H 0.5615 0.3613 0.8275 0.031 Uiso 1 1 calc R U . . .
C2 C 0.4246(4) 0.2762(3) 0.8110(3) 0.0325(10) Uani 1 1 d . . . . .
H2 H 0.4883 0.2439 0.8734 0.039 Uiso 1 1 calc R U . . .
C3 C 0.2878(5) 0.2543(3) 0.7470(3) 0.0381(10) Uani 1 1 d . . . . .
H3 H 0.2560 0.2067 0.7650 0.046 Uiso 1 1 calc R U . . .
C4 C 0.1980(4) 0.3021(3) 0.6570(3) 0.0336(10) Uani 1 1 d . . . . .
H4 H 0.1032 0.2885 0.6121 0.040 Uiso 1 1 calc R U . . .
C5 C 0.2492(4) 0.3707(2) 0.6335(3) 0.0240(8) Uani 1 1 d . . . . .
C6 C 0.1631(4) 0.4220(3) 0.5353(3) 0.0245(8) Uani 1 1 d . . . . .
C7 C 0.1200(4) 0.5109(2) 0.4181(3) 0.0219(8) Uani 1 1 d . . . . .
C8 C 0.1308(4) 0.5703(2) 0.3500(3) 0.0238(8) Uani 1 1 d . . . . .
H8A H 0.2062 0.6131 0.3935 0.029 Uiso 1 1 calc R U . . .
H8B H 0.0448 0.6038 0.3021 0.029 Uiso 1 1 calc R U . . .
C9 C 0.3039(4) 0.6402(2) 0.6939(3) 0.0264(8) Uani 1 1 d . . . . .
H9 H 0.2230 0.6288 0.6252 0.032 Uiso 1 1 calc R U . . .
C10 C 0.2958(4) 0.6971(3) 0.7559(3) 0.0340(10) Uani 1 1 d . . . . .
H10 H 0.2114 0.7235 0.7310 0.041 Uiso 1 1 calc R U . . .
C11 C 0.4142(4) 0.7148(3) 0.8556(3) 0.0376(10) Uani 1 1 d . . . . .
H11 H 0.4122 0.7533 0.9008 0.045 Uiso 1 1 calc R U . . .
C12 C 0.5351(4) 0.6756(3) 0.8884(3) 0.0326(10) Uani 1 1 d . . . . .
H12 H 0.6177 0.6880 0.9558 0.039 Uiso 1 1 calc R U . . .
C13 C 0.5344(4) 0.6184(2) 0.8222(3) 0.0228(8) Uani 1 1 d . . . . .
C14 C 0.6544(3) 0.5719(2) 0.8471(3) 0.0230(8) Uani 1 1 d . . . . .
C15 C 0.7740(4) 0.4883(2) 0.8274(3) 0.0237(8) Uani 1 1 d . . . . .
C16 C 0.8176(4) 0.4305(3) 0.7792(3) 0.0236(8) Uani 1 1 d . . . . .
H16A H 0.7463 0.3857 0.7345 0.028 Uiso 1 1 calc R U . . .
H16B H 0.9029 0.3993 0.8346 0.028 Uiso 1 1 calc R U . . .
C17 C 0.1583(4) 0.5134(2) 0.2871(3) 0.0232(8) Uani 1 1 d . . . . .
H17A H 0.0794 0.4737 0.2405 0.028 Uiso 1 1 calc R U . . .
H17B H 0.2396 0.4761 0.3357 0.028 Uiso 1 1 calc R U . . .
C18 C 0.4952(3) 0.5516(2) 0.4969(2) 0.0190(7) Uani 1 1 d . . . . .
B1 B -0.1490(7) 0.3183(4) 0.0357(4) 0.0595(18) Uani 1 1 d . . . . .
F1 F -0.2329(4) 0.3926(3) 0.0050(3) 0.0896(12) Uani 1 1 d . . . A 1
F2 F -0.2215(6) 0.2471(3) 0.0161(5) 0.165(3) Uani 1 1 d . . . B 1
F3 F -0.1066(5) 0.3123(3) -0.0285(3) 0.1077(15) Uani 1 1 d . . . C 1
F4 F -0.0339(4) 0.3297(3) 0.1324(2) 0.0985(14) Uani 1 1 d . . . D 1
Fe1 Fe 0.43820(5) 0.50056(3) 0.63622(4) 0.01979(19) Uani 1 1 d . . . . .
N1 N 0.3813(3) 0.39257(19) 0.6947(2) 0.0210(7) Uani 1 1 d . . . . .
N2 N 0.2216(3) 0.48497(18) 0.5144(2) 0.0198(7) Uani 1 1 d . . . . .
N3 N 0.0328(3) 0.4083(3) 0.4593(3) 0.0431(10) Uani 1 1 d . . . . .
N4 N 0.0084(3) 0.4667(3) 0.3854(2) 0.0378(9) Uani 1 1 d . . . . .
H4A H -0.0716 0.4740 0.3239 0.045 Uiso 1 1 calc R U . . .
N5 N 0.4185(3) 0.60020(19) 0.7249(2) 0.0209(7) Uani 1 1 d . . . . .
N6 N 0.6443(3) 0.5154(2) 0.7795(2) 0.0222(7) Uani 1 1 d . . . . .
N7 N 0.7824(3) 0.5792(2) 0.9332(2) 0.0352(8) Uani 1 1 d . . . . .
H7 H 0.8122 0.6123 0.9881 0.042 Uiso 1 1 calc R U . . .
N8 N 0.8588(4) 0.5256(2) 0.9202(2) 0.0335(8) Uani 1 1 d . . . . .
O1 O 0.4684(2) 0.58890(15) 0.55129(18) 0.0206(5) Uani 1 1 d . . . . .
O8 O 0.5144(2) 0.58831(15) 0.43816(18) 0.0217(5) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.344(4) . ?
C1 C2 1.379(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.380(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.376(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(5) . ?
C4 H4 0.9500 . ?
C5 N1 1.335(5) . ?
C5 C6 1.479(5) . ?
C6 N3 1.314(5) . ?
C6 N2 1.362(5) . ?
C7 N4 1.322(5) . ?
C7 N2 1.328(5) . ?
C7 C8 1.495(5) . ?
C8 C17 1.528(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 N5 1.330(5) . ?
C9 C10 1.374(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.387(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(5) . ?
C12 H12 0.9500 . ?
C13 N5 1.357(5) . ?
C13 C14 1.464(5) . ?
C14 N7 1.326(5) . ?
C14 N6 1.336(5) . ?
C15 N8 1.321(5) . ?
C15 N6 1.351(5) . ?
C15 C16 1.483(5) . ?
C16 C17 1.540(5) 3_666 ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C16 1.540(5) 3_666 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 O1 1.255(4) . ?
C18 O8 1.250(4) . ?
C18 C18 1.563(7) 3_666 ?
B1 F2 1.311(7) . ?
B1 F4 1.332(7) . ?
B1 F1 1.400(8) . ?
B1 F3 1.433(8) . ?
Fe1 O1 2.115(2) . ?
Fe1 O8 2.121(2) 3_666 ?
Fe1 N2 2.157(3) . ?
Fe1 N6 2.163(3) . ?
Fe1 N5 2.201(3) . ?
Fe1 N1 2.215(3) . ?
N3 N4 1.365(5) . ?
N4 H4A 0.8800 . ?
N7 N8 1.362(5) . ?
N7 H7 0.8800 . ?
O8 Fe1 2.121(2) 3_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 122.5(4) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C1 C2 C3 118.9(4) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C4 C3 C2 119.3(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C3 C4 C5 118.4(4) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
N1 C5 C4 122.9(3) . . ?
N1 C5 C6 114.4(3) . . ?
C4 C5 C6 122.6(3) . . ?
N3 C6 N2 114.5(3) . . ?
N3 C6 C5 125.7(3) . . ?
N2 C6 C5 119.6(3) . . ?
N4 C7 N2 108.9(3) . . ?
N4 C7 C8 124.0(3) . . ?
N2 C7 C8 126.6(3) . . ?
C7 C8 C17 108.5(3) . . ?
C7 C8 H8A 110.0 . . ?
C17 C8 H8A 110.0 . . ?
C7 C8 H8B 110.0 . . ?
C17 C8 H8B 110.0 . . ?
H8A C8 H8B 108.4 . . ?
N5 C9 C10 123.6(3) . . ?
N5 C9 H9 118.2 . . ?
C10 C9 H9 118.2 . . ?
C9 C10 C11 118.2(4) . . ?
C9 C10 H10 120.9 . . ?
C11 C10 H10 120.9 . . ?
C12 C11 C10 119.0(4) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C11 C12 C13 119.2(4) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
N5 C13 C12 121.9(3) . . ?
N5 C13 C14 113.1(3) . . ?
C12 C13 C14 124.9(3) . . ?
N7 C14 N6 111.4(3) . . ?
N7 C14 C13 127.4(3) . . ?
N6 C14 C13 121.2(3) . . ?
N8 C15 N6 110.9(3) . . ?
N8 C15 C16 124.1(3) . . ?
N6 C15 C16 124.8(3) . . ?
C15 C16 C17 109.8(3) . 3_666 ?
C15 C16 H16A 109.7 . . ?
C17 C16 H16A 109.7 3_666 . ?
C15 C16 H16B 109.7 . . ?
C17 C16 H16B 109.7 3_666 . ?
H16A C16 H16B 108.2 . . ?
C8 C17 C16 112.3(3) . 3_666 ?
C8 C17 H17A 109.1 . . ?
C16 C17 H17A 109.1 3_666 . ?
C8 C17 H17B 109.1 . . ?
C16 C17 H17B 109.1 3_666 . ?
H17A C17 H17B 107.9 . . ?
O1 C18 O8 126.8(3) . . ?
O1 C18 C18 116.6(4) . 3_666 ?
O8 C18 C18 116.7(4) . 3_666 ?
F2 B1 F4 118.1(5) . . ?
F2 B1 F1 108.9(6) . . ?
F4 B1 F1 109.8(5) . . ?
F2 B1 F3 106.2(6) . . ?
F4 B1 F3 104.8(6) . . ?
F1 B1 F3 108.6(4) . . ?
O1 Fe1 O8 78.69(9) . 3_666 ?
O1 Fe1 N2 95.42(10) . . ?
O8 Fe1 N2 92.12(10) 3_666 . ?
O1 Fe1 N6 93.87(10) . . ?
O8 Fe1 N6 96.77(11) 3_666 . ?
N2 Fe1 N6 168.24(11) . . ?
O1 Fe1 N5 97.57(10) . . ?
O8 Fe1 N5 171.86(10) 3_666 . ?
N2 Fe1 N5 95.44(11) . . ?
N6 Fe1 N5 76.16(11) . . ?
O1 Fe1 N1 168.23(10) . . ?
O8 Fe1 N1 93.05(10) 3_666 . ?
N2 Fe1 N1 76.36(11) . . ?
N6 Fe1 N1 95.42(11) . . ?
N5 Fe1 N1 91.65(11) . . ?
C5 N1 C1 118.0(3) . . ?
C5 N1 Fe1 115.8(2) . . ?
C1 N1 Fe1 126.2(2) . . ?
C7 N2 C6 103.6(3) . . ?
C7 N2 Fe1 142.3(2) . . ?
C6 N2 Fe1 113.9(2) . . ?
C6 N3 N4 101.6(3) . . ?
C7 N4 N3 111.5(3) . . ?
C7 N4 H4A 124.3 . . ?
N3 N4 H4A 124.3 . . ?
C9 N5 C13 117.9(3) . . ?
C9 N5 Fe1 126.2(2) . . ?
C13 N5 Fe1 115.8(2) . . ?
C14 N6 C15 104.3(3) . . ?
C14 N6 Fe1 113.5(2) . . ?
C15 N6 Fe1 142.1(3) . . ?
C14 N7 N8 106.6(3) . . ?
C14 N7 H7 126.7 . . ?
N8 N7 H7 126.7 . . ?
C15 N8 N7 106.8(3) . . ?
C18 O1 Fe1 114.0(2) . . ?
C18 O8 Fe1 114.0(2) . 3_666 ?

_refine_diff_density_max         1.090
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.088



####################################################################### 
# 
# 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_5b
_database_code_depnum_ccdc_archive 'CCDC 1907073'
loop_
_audit_author_name
_audit_author_address
I.Nemec
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-05-09 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 B2 Co2 F8 N16 O10'
_chemical_formula_weight         1260.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   14.538(5)
_cell_length_b                   12.883(5)
_cell_length_c                   18.054(4)
_cell_angle_alpha                90
_cell_angle_beta                 125.500(18)
_cell_angle_gamma                90
_cell_volume                     2752.8(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9633
_cell_measurement_theta_min      2.962
_cell_measurement_theta_max      26.684

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_F_000             1296
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    0.699
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.91224
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16883
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.163
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4835
_reflns_number_gt                4106
_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       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0453P)²+0.6342P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4835
_refine_ls_number_parameters     397
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0746
_refine_ls_wR_factor_gt          0.0730
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.59065(2) 0.67872(2) 0.48245(2) 0.01585(8) Uani 1 1 d . . . . .
O1 O 0.45753(10) 0.57086(9) 0.40264(8) 0.0192(3) Uani 1 1 d . . . . .
O2 O 0.61741(9) 0.57260(9) 0.58241(8) 0.0194(3) Uani 1 1 d . . . . .
N1 N 0.69852(12) 0.60166(11) 0.45544(10) 0.0189(3) Uani 1 1 d . . . . .
N2 N 0.80716(13) 0.52506(12) 0.42723(11) 0.0258(3) Uani 1 1 d . . . . .
H1N2 H 0.8578 0.4821 0.4327 0.031 Uiso 1 1 calc R U . . .
N3 N 0.74840(13) 0.59462(12) 0.35833(10) 0.0256(3) Uani 1 1 d . . . . .
N4 N 0.55168(11) 0.75897(11) 0.36423(9) 0.0179(3) Uani 1 1 d . . . . .
N5 N 0.49953(12) 0.78092(11) 0.51169(9) 0.0189(3) Uani 1 1 d . . . . .
N6 N 0.40951(12) 0.88694(12) 0.54190(11) 0.0253(3) Uani 1 1 d . . . . .
H1N6 H 0.3542 0.9147 0.5418 0.030 Uiso 1 1 calc R U . . .
N7 N 0.51616(13) 0.92596(12) 0.58841(10) 0.0252(3) Uani 1 1 d . . . . .
N8 N 0.71859(12) 0.78964(11) 0.57009(9) 0.0181(3) Uani 1 1 d . . . . .
C1 C 0.83537(15) 0.47146(14) 0.57305(13) 0.0260(4) Uani 1 1 d . . . . .
H1A H 0.7858 0.4730 0.5941 0.031 Uiso 1 1 calc R U . . .
H1B H 0.9064 0.5077 0.6193 0.031 Uiso 1 1 calc R U . . .
C2 C 0.77888(14) 0.52960(13) 0.48570(12) 0.0209(4) Uani 1 1 d . . . . .
C3 C 0.68446(14) 0.63964(13) 0.37877(12) 0.0186(4) Uani 1 1 d . . . . .
C4 C 0.60740(14) 0.72653(13) 0.32921(11) 0.0190(4) Uani 1 1 d . . . . .
C5 C 0.59630(15) 0.77489(15) 0.25629(12) 0.0258(4) Uani 1 1 d . . . . .
H5 H 0.6354 0.7495 0.2323 0.031 Uiso 1 1 calc R U . . .
C6 C 0.52716(17) 0.86090(16) 0.21877(13) 0.0306(4) Uani 1 1 d . . . . .
H6 H 0.5193 0.8965 0.1693 0.037 Uiso 1 1 calc R U . . .
C7 C 0.46982(17) 0.89452(15) 0.25377(13) 0.0302(4) Uani 1 1 d . . . . .
H7 H 0.4216 0.9533 0.2287 0.036 Uiso 1 1 calc R U . . .
C8 C 0.48359(15) 0.84137(14) 0.32588(12) 0.0238(4) Uani 1 1 d . . . . .
H8 H 0.4430 0.8642 0.3493 0.029 Uiso 1 1 calc R U . . .
C9 C 0.82554(15) 0.79287(14) 0.59501(12) 0.0225(4) Uani 1 1 d . . . . .
H9 H 0.8507 0.7392 0.5747 0.027 Uiso 1 1 calc R U . . .
C10 C 0.90013(16) 0.87047(15) 0.64860(13) 0.0272(4) Uani 1 1 d . . . . .
H10 H 0.9747 0.8706 0.6641 0.033 Uiso 1 1 calc R U . . .
C11 C 0.86501(16) 0.94815(15) 0.67953(13) 0.0285(4) Uani 1 1 d . . . . .
H11 H 0.9152 1.0023 0.7168 0.034 Uiso 1 1 calc R U . . .
C12 C 0.75581(16) 0.94598(14) 0.65548(13) 0.0262(4) Uani 1 1 d . . . . .
H12 H 0.7299 0.9980 0.6765 0.031 Uiso 1 1 calc R U . . .
C13 C 0.68545(14) 0.86688(13) 0.60039(11) 0.0196(4) Uani 1 1 d . . . . .
C14 C 0.56676(14) 0.85973(13) 0.56779(11) 0.0187(4) Uani 1 1 d . . . . .
C15 C 0.39956(15) 0.80105(14) 0.49633(12) 0.0212(4) Uani 1 1 d . . . . .
C16 C 0.29350(15) 0.74025(15) 0.43916(13) 0.0276(4) Uani 1 1 d . . . . .
H16A H 0.3096 0.6763 0.4182 0.033 Uiso 1 1 calc R U . . .
H16B H 0.2381 0.7816 0.3847 0.033 Uiso 1 1 calc R U . . .
C17 C 0.24088(16) 0.71022(14) 0.48919(13) 0.0268(4) Uani 1 1 d . . . . .
H17A H 0.2980 0.6730 0.5459 0.032 Uiso 1 1 calc R U . . .
H17B H 0.2198 0.7742 0.5064 0.032 Uiso 1 1 calc R U . . .
C18 C 0.13688(15) 0.64189(14) 0.43227(14) 0.0281(4) Uani 1 1 d . . . . .
H18A H 0.0885 0.6706 0.3699 0.034 Uiso 1 1 calc R U . . .
H18B H 0.0931 0.6441 0.4585 0.034 Uiso 1 1 calc R U . . .
C20 C 0.45356(14) 0.49916(12) 0.44804(11) 0.0156(3) Uani 1 1 d . . . . .
F1A F 0.05209(13) 0.88559(17) 0.08406(14) 0.0438(5) Uani 0.957(6) 1 d . . P A 1
F2A F 0.22204(19) 0.86500(18) 0.21880(16) 0.0450(5) Uani 0.957(6) 1 d . . P A 1
F3A F 0.0597(2) 0.83611(17) 0.20771(17) 0.0450(5) Uani 0.957(6) 1 d . . P A 1
F4A F 0.11397(19) 0.72413(11) 0.14358(15) 0.0460(5) Uani 0.957(6) 1 d D . P A 1
B1 B 0.11297(18) 0.82722(17) 0.16466(16) 0.0274(5) Uani 1 1 d . . . . .
O1S O 0.04307(13) 0.58477(13) 0.91069(11) 0.0501(4) Uani 1 1 d . . . . .
C1S C -0.04564(16) 0.62796(15) 0.88031(14) 0.0299(4) Uani 1 1 d . . . . .
C2S C -0.08381(19) 0.65548(19) 0.93847(15) 0.0421(5) Uani 1 1 d . . . . .
H2S1 H -0.0362 0.6199 0.9972 0.063 Uiso 1 1 calc R U . . .
H2S2 H -0.1626 0.6339 0.9082 0.063 Uiso 1 1 calc R U . . .
H2S3 H -0.0778 0.7307 0.9483 0.063 Uiso 1 1 calc R U . . .
C3S C -0.1201(2) 0.6611(2) 0.78348(15) 0.0482(6) Uani 1 1 d . . . . .
H3S1 H -0.0784 0.6563 0.7562 0.072 Uiso 1 1 calc R U . . .
H3S2 H -0.1443 0.7329 0.7802 0.072 Uiso 1 1 calc R U . . .
H3S3 H -0.1865 0.6158 0.7503 0.072 Uiso 1 1 calc R U . . .
O2S O 0.25905(12) 0.98416(12) 0.55825(10) 0.0353(3) Uani 1 1 d D . . . .
O3S O 0.27530(19) 0.56780(18) 0.21108(12) 0.0804(7) Uani 1 1 d D . . . .
F1B F 0.069(3) 0.923(4) 0.112(3) 0.0438(5) Uani 0.043(6) 1 d . . P A 2
F3B F 0.074(6) 0.810(5) 0.203(5) 0.0450(5) Uani 0.043(6) 1 d . . P A 2
F4B F 0.060(4) 0.742(3) 0.101(4) 0.0460(5) Uani 0.043(6) 1 d . . P A 2
F2B F 0.223(5) 0.843(5) 0.239(4) 0.0450(5) Uani 0.043(6) 1 d . . P A 2
H2SA H 0.269(2) 0.965(2) 0.6072(11) 0.054 Uiso 1 1 d D U . . .
H2SB H 0.1918(11) 0.9669(19) 0.5186(13) 0.054 Uiso 1 1 d D U . . .
H3SB H 0.3291(15) 0.570(2) 0.2673(8) 0.054 Uiso 1 1 d D U . . .
H3SA H 0.2296(16) 0.6210(14) 0.1977(15) 0.054 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.1123(12) . ?
Co1 O1 2.1245(13) . ?
Co1 N4 2.1309(15) . ?
Co1 N1 2.1380(15) . ?
Co1 N5 2.1399(15) . ?
Co1 N8 2.1418(15) . ?
O1 C20 1.258(2) . ?
O2 C20 1.250(2) 3_666 ?
N1 C2 1.336(2) . ?
N1 C3 1.367(2) . ?
N2 C2 1.338(2) . ?
N2 N3 1.359(2) . ?
N2 H1N2 0.8800 . ?
N3 C3 1.317(2) . ?
N4 C8 1.338(2) . ?
N4 C4 1.351(2) . ?
N5 C15 1.337(2) . ?
N5 C14 1.365(2) . ?
N6 C15 1.336(2) . ?
N6 N7 1.360(2) . ?
N6 H1N6 0.8800 . ?
N7 C14 1.314(2) . ?
N8 C9 1.345(2) . ?
N8 C13 1.352(2) . ?
C1 C2 1.489(3) . ?
C1 C18 1.533(3) 3_666 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C3 C4 1.465(3) . ?
C4 C5 1.378(3) . ?
C5 C6 1.381(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.376(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.379(3) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.376(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.382(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.376(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.467(2) . ?
C15 C16 1.486(3) . ?
C16 C17 1.534(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.521(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C1 1.533(3) 3_666 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 O2 1.250(2) 3_666 ?
C20 C20 1.550(3) 3_666 ?
F1A B1 1.404(3) . ?
F2A B1 1.381(3) . ?
F3A B1 1.384(3) . ?
F4A B1 1.384(3) . ?
B1 F3B 1.15(6) . ?
B1 F2B 1.38(6) . ?
B1 F4B 1.45(4) . ?
B1 F1B 1.45(4) . ?
O1S C1S 1.205(2) . ?
C1S C3S 1.487(3) . ?
C1S C2S 1.487(3) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?
O2S H2SA 0.846(10) . ?
O2S H2SB 0.839(10) . ?
O3S H3SB 0.848(10) . ?
O3S H3SA 0.885(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O1 78.43(5) . . ?
O2 Co1 N4 168.43(5) . . ?
O1 Co1 N4 91.74(5) . . ?
O2 Co1 N1 95.67(5) . . ?
O1 Co1 N1 92.38(6) . . ?
N4 Co1 N1 78.49(6) . . ?
O2 Co1 N5 91.19(5) . . ?
O1 Co1 N5 96.85(6) . . ?
N4 Co1 N5 96.08(6) . . ?
N1 Co1 N5 169.46(5) . . ?
O2 Co1 N8 98.66(5) . . ?
O1 Co1 N8 174.68(5) . . ?
N4 Co1 N8 91.60(6) . . ?
N1 Co1 N8 92.35(6) . . ?
N5 Co1 N8 78.68(6) . . ?
C20 O1 Co1 114.00(10) . . ?
C20 O2 Co1 114.04(10) 3_666 . ?
C2 N1 C3 104.12(14) . . ?
C2 N1 Co1 144.36(12) . . ?
C3 N1 Co1 111.51(11) . . ?
C2 N2 N3 112.06(15) . . ?
C2 N2 H1N2 124.0 . . ?
N3 N2 H1N2 124.0 . . ?
C3 N3 N2 101.81(14) . . ?
C8 N4 C4 117.87(15) . . ?
C8 N4 Co1 126.15(12) . . ?
C4 N4 Co1 115.84(11) . . ?
C15 N5 C14 103.49(14) . . ?
C15 N5 Co1 145.29(12) . . ?
C14 N5 Co1 111.21(11) . . ?
C15 N6 N7 111.32(14) . . ?
C15 N6 H1N6 124.3 . . ?
N7 N6 H1N6 124.3 . . ?
C14 N7 N6 102.12(14) . . ?
C9 N8 C13 117.15(15) . . ?
C9 N8 Co1 127.37(12) . . ?
C13 N8 Co1 115.43(11) . . ?
C2 C1 C18 114.60(16) . 3_666 ?
C2 C1 H1A 108.6 . . ?
C18 C1 H1A 108.6 3_666 . ?
C2 C1 H1B 108.6 . . ?
C18 C1 H1B 108.6 3_666 . ?
H1A C1 H1B 107.6 . . ?
N1 C2 N2 107.71(16) . . ?
N1 C2 C1 126.60(16) . . ?
N2 C2 C1 125.46(16) . . ?
N3 C3 N1 114.29(15) . . ?
N3 C3 C4 125.40(15) . . ?
N1 C3 C4 120.25(15) . . ?
N4 C4 C5 122.52(16) . . ?
N4 C4 C3 113.84(15) . . ?
C5 C4 C3 123.56(16) . . ?
C4 C5 C6 118.65(17) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C7 C6 C5 119.33(17) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 118.86(18) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 H7 120.6 . . ?
N4 C8 C7 122.75(17) . . ?
N4 C8 H8 118.6 . . ?
C7 C8 H8 118.6 . . ?
N8 C9 C10 122.93(17) . . ?
N8 C9 H9 118.5 . . ?
C10 C9 H9 118.5 . . ?
C9 C10 C11 119.06(17) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C10 C11 C12 119.05(17) . . ?
C10 C11 H11 120.5 . . ?
C12 C11 H11 120.5 . . ?
C13 C12 C11 118.58(17) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.7 . . ?
N8 C13 C12 123.21(16) . . ?
N8 C13 C14 113.82(15) . . ?
C12 C13 C14 122.96(16) . . ?
N7 C14 N5 114.58(15) . . ?
N7 C14 C13 124.55(16) . . ?
N5 C14 C13 120.86(15) . . ?
N6 C15 N5 108.48(16) . . ?
N6 C15 C16 124.20(16) . . ?
N5 C15 C16 127.32(16) . . ?
C15 C16 C17 113.27(16) . . ?
C15 C16 H16A 108.9 . . ?
C17 C16 H16A 108.9 . . ?
C15 C16 H16B 108.9 . . ?
C17 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
C18 C17 C16 112.84(16) . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17B 109.0 . . ?
C16 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C17 C18 C1 113.53(15) . 3_666 ?
C17 C18 H18A 108.9 . . ?
C1 C18 H18A 108.9 3_666 . ?
C17 C18 H18B 108.9 . . ?
C1 C18 H18B 108.9 3_666 . ?
H18A C18 H18B 107.7 . . ?
O2 C20 O1 126.50(15) 3_666 . ?
O2 C20 C20 117.34(17) 3_666 3_666 ?
O1 C20 C20 116.16(18) . 3_666 ?
F3B B1 F2B 98(4) . . ?
F2A B1 F3A 111.1(2) . . ?
F2A B1 F4A 109.98(19) . . ?
F3A B1 F4A 109.42(19) . . ?
F2A B1 F1A 108.58(17) . . ?
F3A B1 F1A 108.44(19) . . ?
F4A B1 F1A 109.26(18) . . ?
F3B B1 F4B 97(3) . . ?
F2B B1 F4B 132(3) . . ?
F3B B1 F1B 112(4) . . ?
F2B B1 F1B 109(3) . . ?
F4B B1 F1B 107(2) . . ?
O1S C1S C3S 121.5(2) . . ?
O1S C1S C2S 121.9(2) . . ?
C3S C1S C2S 116.51(19) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C1S C3S H3S1 109.5 . . ?
C1S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
C1S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
H2SA O2S H2SB 103(2) . . ?
H3SB O3S H3SA 109(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 N3 C3 -0.22(19) . . . . ?
C15 N6 N7 C14 0.13(19) . . . . ?
C3 N1 C2 N2 -1.51(18) . . . . ?
Co1 N1 C2 N2 -179.72(14) . . . . ?
C3 N1 C2 C1 173.15(17) . . . . ?
Co1 N1 C2 C1 -5.1(3) . . . . ?
N3 N2 C2 N1 1.1(2) . . . . ?
N3 N2 C2 C1 -173.59(16) . . . . ?
C18 C1 C2 N1 143.65(17) 3_666 . . . ?
C18 C1 C2 N2 -42.6(2) 3_666 . . . ?
N2 N3 C3 N1 -0.80(19) . . . . ?
N2 N3 C3 C4 176.29(16) . . . . ?
C2 N1 C3 N3 1.5(2) . . . . ?
Co1 N1 C3 N3 -179.63(12) . . . . ?
C2 N1 C3 C4 -175.76(15) . . . . ?
Co1 N1 C3 C4 3.12(19) . . . . ?
C8 N4 C4 C5 -0.1(2) . . . . ?
Co1 N4 C4 C5 -175.97(13) . . . . ?
C8 N4 C4 C3 176.79(15) . . . . ?
Co1 N4 C4 C3 0.91(18) . . . . ?
N3 C3 C4 N4 -179.70(16) . . . . ?
N1 C3 C4 N4 -2.8(2) . . . . ?
N3 C3 C4 C5 -2.9(3) . . . . ?
N1 C3 C4 C5 174.06(16) . . . . ?
N4 C4 C5 C6 1.2(3) . . . . ?
C3 C4 C5 C6 -175.35(17) . . . . ?
C4 C5 C6 C7 -1.3(3) . . . . ?
C5 C6 C7 C8 0.3(3) . . . . ?
C4 N4 C8 C7 -1.0(3) . . . . ?
Co1 N4 C8 C7 174.43(14) . . . . ?
C6 C7 C8 N4 0.9(3) . . . . ?
C13 N8 C9 C10 -0.3(3) . . . . ?
Co1 N8 C9 C10 176.93(13) . . . . ?
N8 C9 C10 C11 0.9(3) . . . . ?
C9 C10 C11 C12 -0.3(3) . . . . ?
C10 C11 C12 C13 -0.8(3) . . . . ?
C9 N8 C13 C12 -0.9(2) . . . . ?
Co1 N8 C13 C12 -178.47(14) . . . . ?
C9 N8 C13 C14 178.05(15) . . . . ?
Co1 N8 C13 C14 0.50(18) . . . . ?
C11 C12 C13 N8 1.5(3) . . . . ?
C11 C12 C13 C14 -177.39(17) . . . . ?
N6 N7 C14 N5 -0.34(19) . . . . ?
N6 N7 C14 C13 179.39(16) . . . . ?
C15 N5 C14 N7 0.4(2) . . . . ?
Co1 N5 C14 N7 179.73(12) . . . . ?
C15 N5 C14 C13 -179.32(16) . . . . ?
Co1 N5 C14 C13 -0.01(19) . . . . ?
N8 C13 C14 N7 179.95(16) . . . . ?
C12 C13 C14 N7 -1.1(3) . . . . ?
N8 C13 C14 N5 -0.3(2) . . . . ?
C12 C13 C14 N5 178.64(16) . . . . ?
N7 N6 C15 N5 0.1(2) . . . . ?
N7 N6 C15 C16 179.92(16) . . . . ?
C14 N5 C15 N6 -0.31(19) . . . . ?
Co1 N5 C15 N6 -179.18(15) . . . . ?
C14 N5 C15 C16 179.91(17) . . . . ?
Co1 N5 C15 C16 1.0(3) . . . . ?
N6 C15 C16 C17 -52.4(2) . . . . ?
N5 C15 C16 C17 127.32(19) . . . . ?
C15 C16 C17 C18 -176.11(15) . . . . ?
C16 C17 C18 C1 76.9(2) . . . 3_666 ?
Co1 O1 C20 O2 178.74(13) . . . 3_666 ?
Co1 O1 C20 C20 -1.3(2) . . . 3_666 ?

_refine_diff_density_max         0.713
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.049

####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1907077'
loop_
_audit_author_name
_audit_author_address
I.Nemec
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-05-09 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H32 Cl2 N16 Ni2 O12'
_chemical_formula_weight         1069.09

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   12.3683(3)
_cell_length_b                   15.2467(3)
_cell_length_c                   16.1543(4)
_cell_angle_alpha                90
_cell_angle_beta                 128.416(2)
_cell_angle_gamma                90
_cell_volume                     2386.84(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4330
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      26.24

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_F_000             1092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.975
_shelx_estimated_absorpt_T_min   0.708
_shelx_estimated_absorpt_T_max   0.814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.5 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19738
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.119
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             4180
_reflns_number_gt                3241
_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       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0902P)²+3.8740P] 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         4180
_refine_ls_number_parameters     303
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1555
_refine_ls_wR_factor_gt          0.1502
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.101
_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
C1 C 0.7017(4) 0.6341(2) 0.3200(3) 0.0277(8) Uani 1 1 d . . . . .
H1 H 0.7826 0.6224 0.3898 0.033 Uiso 1 1 calc R U . . .
C2 C 0.7100(4) 0.6921(3) 0.2596(3) 0.0349(10) Uani 1 1 d . . . . .
H2 H 0.7956 0.7189 0.2869 0.042 Uiso 1 1 calc R U . . .
C3 C 0.5932(4) 0.7116(3) 0.1589(3) 0.0387(10) Uani 1 1 d . . . . .
H3 H 0.5968 0.7516 0.1155 0.046 Uiso 1 1 calc R U . . .
C4 C 0.4708(4) 0.6714(3) 0.1228(3) 0.0365(10) Uani 1 1 d . . . . .
H4 H 0.3880 0.6841 0.0543 0.044 Uiso 1 1 calc R U . . .
C5 C 0.4703(4) 0.6134(2) 0.1865(3) 0.0274(8) Uani 1 1 d . . . . .
C6 C 0.3478(4) 0.5668(2) 0.1584(3) 0.0270(8) Uani 1 1 d . . . . .
C7 C 0.2274(4) 0.4820(2) 0.1759(3) 0.0254(8) Uani 1 1 d . . . . .
C8 C 0.1822(4) 0.4249(2) 0.2229(3) 0.0274(8) Uani 1 1 d . . . . .
H8A H 0.2543 0.3806 0.2691 0.033 Uiso 1 1 calc R U . . .
H8B H 0.0966 0.3936 0.1664 0.033 Uiso 1 1 calc R U . . .
C9 C 0.1559(4) 0.4808(2) 0.2874(3) 0.0267(8) Uani 1 1 d . . . . .
H9A H 0.2361 0.5199 0.3344 0.032 Uiso 1 1 calc R U . . .
H9B H 0.0742 0.5183 0.2385 0.032 Uiso 1 1 calc R U . . .
C10 C 0.5149(4) 0.3470(3) 0.2136(3) 0.0310(9) Uani 1 1 d . . . . .
H10 H 0.4200 0.3625 0.1703 0.037 Uiso 1 1 calc R U . . .
C11 C 0.5547(5) 0.2794(3) 0.1823(4) 0.0381(10) Uani 1 1 d . . . . .
H11 H 0.4884 0.2492 0.1181 0.046 Uiso 1 1 calc R U . . .
C12 C 0.6920(5) 0.2553(3) 0.2446(4) 0.0419(11) Uani 1 1 d . . . . .
H12 H 0.7213 0.2081 0.2245 0.050 Uiso 1 1 calc R U . . .
C13 C 0.7857(4) 0.3012(3) 0.3368(4) 0.0359(10) Uani 1 1 d . . . . .
H13 H 0.8810 0.2866 0.3810 0.043 Uiso 1 1 calc R U . . .
C14 C 0.7379(4) 0.3690(2) 0.3633(3) 0.0267(8) Uani 1 1 d . . . . .
C15 C 0.8269(4) 0.4198(2) 0.4609(3) 0.0251(8) Uani 1 1 d . . . . .
C16 C 0.8751(4) 0.5116(2) 0.5784(3) 0.0246(8) Uani 1 1 d . . . . .
C17 C 0.8682(4) 0.5727(2) 0.6456(3) 0.0272(8) Uani 1 1 d . . . . .
H17A H 0.7917 0.6149 0.6011 0.033 Uiso 1 1 calc R U . . .
H17B H 0.9555 0.6061 0.6917 0.033 Uiso 1 1 calc R U . . .
C18 C 0.5041(3) 0.5511(2) 0.5015(3) 0.0198(8) Uani 1 1 d . . . . .
Cl1 Cl 0.85860(15) 0.82674(9) 0.56012(12) 0.0663(4) Uani 1 1 d D . . . .
N1 N 0.3575(3) 0.51025(19) 0.2264(2) 0.0239(7) Uani 1 1 d . . . . .
N2 N 0.5846(3) 0.59304(19) 0.2850(2) 0.0229(7) Uani 1 1 d . . . . .
N3 N 0.1426(4) 0.5202(3) 0.0817(3) 0.0384(9) Uani 1 1 d . . . . .
N4 N 0.2202(3) 0.5742(2) 0.0703(3) 0.0395(9) Uani 1 1 d . . . . .
H1N4 H 0.1911 0.6073 0.0154 0.047 Uiso 1 1 calc R U . . .
N5 N 0.7698(3) 0.48191(19) 0.4837(2) 0.0230(7) Uani 1 1 d . . . . .
N6 N 0.6044(3) 0.3924(2) 0.3031(2) 0.0245(7) Uani 1 1 d . . . . .
N7 N 0.9882(3) 0.4686(2) 0.6090(3) 0.0318(8) Uani 1 1 d . . . . .
H1N7 H 1.0706 0.4775 0.6694 0.038 Uiso 1 1 calc R U . . .
N8 N 0.9603(3) 0.4090(2) 0.5351(3) 0.0337(8) Uani 1 1 d . . . . .
Ni1 Ni 0.55883(4) 0.49623(3) 0.36484(3) 0.02044(18) Uani 1 1 d . . . . .
O1 O 0.5300(2) 0.58633(15) 0.44564(19) 0.0219(5) Uani 1 1 d . . . . .
O2 O 0.4848(2) 0.58925(15) 0.55959(19) 0.0232(5) Uani 1 1 d . . . . .
O3A O 0.7731(9) 0.9040(5) 0.5241(8) 0.0960(12) Uani 0.624(5) 1 d D . P A 1
O4A O 0.9864(9) 0.8150(5) 0.6602(7) 0.0960(12) Uani 0.624(5) 1 d D . P A 1
O5A O 0.7662(9) 0.7601(5) 0.5329(7) 0.0960(12) Uani 0.624(5) 1 d D . P A 1
O6A O 0.8896(9) 0.8167(5) 0.4832(7) 0.0960(12) Uani 0.624(5) 1 d D . P A 1
O5B O 0.8121(15) 0.7892(8) 0.6171(11) 0.0960(12) Uani 0.376(5) 1 d D . P A 2
O6B O 0.8165(15) 0.7628(8) 0.4866(10) 0.0960(12) Uani 0.376(5) 1 d D . P A 2
O4B O 0.9966(12) 0.8500(9) 0.6298(11) 0.0960(12) Uani 0.376(5) 1 d D . P A 2
O3B O 0.8255(16) 0.9177(7) 0.5517(14) 0.0960(12) Uani 0.376(5) 1 d D . P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.339(5) . ?
C1 C2 1.366(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.379(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.360(6) . ?
C4 H4 0.9500 . ?
C5 N2 1.354(5) . ?
C5 C6 1.467(5) . ?
C6 N4 1.319(5) . ?
C6 N1 1.342(5) . ?
C7 N3 1.331(5) . ?
C7 N1 1.345(5) . ?
C7 C8 1.475(5) . ?
C8 C9 1.530(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C17 1.526(5) 3_666 ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 N6 1.344(5) . ?
C10 C11 1.367(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.379(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(5) . ?
C13 H13 0.9500 . ?
C14 N6 1.343(5) . ?
C14 C15 1.464(5) . ?
C15 N8 1.315(5) . ?
C15 N5 1.362(5) . ?
C16 N5 1.329(5) . ?
C16 N7 1.330(5) . ?
C16 C17 1.474(5) . ?
C17 C9 1.526(5) 3_666 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 O2 1.246(4) . ?
C18 O1 1.251(4) . ?
C18 C18 1.561(7) 3_666 ?
Cl1 O6B 1.365(10) . ?
Cl1 O5A 1.381(7) . ?
Cl1 O4B 1.385(11) . ?
Cl1 O4A 1.403(8) . ?
Cl1 O3B 1.428(11) . ?
Cl1 O3A 1.442(8) . ?
Cl1 O5B 1.470(11) . ?
Cl1 O6A 1.519(7) . ?
N1 Ni1 2.080(3) . ?
N2 Ni1 2.110(3) . ?
N3 N4 1.361(5) . ?
N4 H1N4 0.8800 . ?
N5 Ni1 2.077(3) . ?
N6 Ni1 2.126(3) . ?
N7 N8 1.363(5) . ?
N7 H1N7 0.8800 . ?
Ni1 O1 2.073(2) . ?
Ni1 O2 2.074(2) 3_666 ?
O2 Ni1 2.074(2) 3_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 122.9(4) . . ?
N2 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C3 119.6(4) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C2 C3 C4 118.1(4) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C5 C4 C3 119.2(4) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
N2 C5 C4 123.1(4) . . ?
N2 C5 C6 112.1(3) . . ?
C4 C5 C6 124.8(3) . . ?
N4 C6 N1 112.2(3) . . ?
N4 C6 C5 127.3(4) . . ?
N1 C6 C5 120.6(3) . . ?
N3 C7 N1 110.5(3) . . ?
N3 C7 C8 124.5(3) . . ?
N1 C7 C8 124.7(3) . . ?
C7 C8 C9 109.3(3) . . ?
C7 C8 H8A 109.8 . . ?
C9 C8 H8A 109.8 . . ?
C7 C8 H8B 109.8 . . ?
C9 C8 H8B 109.8 . . ?
H8A C8 H8B 108.3 . . ?
C17 C9 C8 113.8(3) 3_666 . ?
C17 C9 H9A 108.8 3_666 . ?
C8 C9 H9A 108.8 . . ?
C17 C9 H9B 108.8 3_666 . ?
C8 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
N6 C10 C11 122.7(4) . . ?
N6 C10 H10 118.6 . . ?
C11 C10 H10 118.6 . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C13 C12 C11 118.7(4) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C14 118.6(4) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
N6 C14 C13 123.0(4) . . ?
N6 C14 C15 113.7(3) . . ?
C13 C14 C15 123.3(3) . . ?
N8 C15 N5 114.1(3) . . ?
N8 C15 C14 126.4(3) . . ?
N5 C15 C14 119.4(3) . . ?
N5 C16 N7 108.2(3) . . ?
N5 C16 C17 126.8(3) . . ?
N7 C16 C17 124.6(3) . . ?
C16 C17 C9 108.1(3) . 3_666 ?
C16 C17 H17A 110.1 . . ?
C9 C17 H17A 110.1 3_666 . ?
C16 C17 H17B 110.1 . . ?
C9 C17 H17B 110.1 3_666 . ?
H17A C17 H17B 108.4 . . ?
O2 C18 O1 126.7(3) . . ?
O2 C18 C18 116.8(4) . 3_666 ?
O1 C18 C18 116.5(4) . 3_666 ?
O6B Cl1 O4B 120.1(9) . . ?
O5A Cl1 O4A 112.9(5) . . ?
O6B Cl1 O3B 132.8(9) . . ?
O4B Cl1 O3B 88.0(9) . . ?
O5A Cl1 O3A 102.6(5) . . ?
O4A Cl1 O3A 126.0(5) . . ?
O6B Cl1 O5B 100.4(8) . . ?
O4B Cl1 O5B 110.8(9) . . ?
O3B Cl1 O5B 103.7(9) . . ?
O5A Cl1 O6A 104.2(5) . . ?
O4A Cl1 O6A 104.7(5) . . ?
O3A Cl1 O6A 104.3(6) . . ?
C6 N1 C7 104.1(3) . . ?
C6 N1 Ni1 112.6(2) . . ?
C7 N1 Ni1 143.3(3) . . ?
C1 N2 C5 117.0(3) . . ?
C1 N2 Ni1 127.2(2) . . ?
C5 N2 Ni1 115.8(2) . . ?
C7 N3 N4 107.4(3) . . ?
C6 N4 N3 105.9(3) . . ?
C6 N4 H1N4 127.1 . . ?
N3 N4 H1N4 127.1 . . ?
C16 N5 C15 104.2(3) . . ?
C16 N5 Ni1 143.0(3) . . ?
C15 N5 Ni1 112.8(2) . . ?
C14 N6 C10 117.5(3) . . ?
C14 N6 Ni1 115.1(2) . . ?
C10 N6 Ni1 127.4(3) . . ?
C16 N7 N8 111.6(3) . . ?
C16 N7 H1N7 124.2 . . ?
N8 N7 H1N7 124.2 . . ?
C15 N8 N7 101.9(3) . . ?
O1 Ni1 O2 80.58(9) . 3_666 ?
O1 Ni1 N5 95.53(11) . . ?
O2 Ni1 N5 91.54(11) 3_666 . ?
O1 Ni1 N1 92.82(10) . . ?
O2 Ni1 N1 96.98(11) 3_666 . ?
N5 Ni1 N1 168.94(12) . . ?
O1 Ni1 N2 94.09(11) . . ?
O2 Ni1 N2 173.10(10) 3_666 . ?
N5 Ni1 N2 93.34(11) . . ?
N1 Ni1 N2 78.82(12) . . ?
O1 Ni1 N6 171.36(10) . . ?
O2 Ni1 N6 92.86(11) 3_666 . ?
N5 Ni1 N6 78.94(12) . . ?
N1 Ni1 N6 93.55(11) . . ?
N2 Ni1 N6 92.86(12) . . ?
C18 O1 Ni1 113.0(2) . . ?
C18 O2 Ni1 113.1(2) . 3_666 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 C3 1.4(6) . . . . ?
C1 C2 C3 C4 0.3(6) . . . . ?
C2 C3 C4 C5 -1.1(7) . . . . ?
C3 C4 C5 N2 0.4(6) . . . . ?
C3 C4 C5 C6 179.5(4) . . . . ?
N2 C5 C6 N4 177.5(4) . . . . ?
C4 C5 C6 N4 -1.7(7) . . . . ?
N2 C5 C6 N1 -1.2(5) . . . . ?
C4 C5 C6 N1 179.6(4) . . . . ?
N3 C7 C8 C9 -89.8(4) . . . . ?
N1 C7 C8 C9 82.5(4) . . . . ?
C7 C8 C9 C17 -170.4(3) . . . 3_666 ?
N6 C10 C11 C12 0.6(6) . . . . ?
C10 C11 C12 C13 -0.7(7) . . . . ?
C11 C12 C13 C14 0.6(6) . . . . ?
C12 C13 C14 N6 -0.3(6) . . . . ?
C12 C13 C14 C15 177.5(4) . . . . ?
N6 C14 C15 N8 178.0(4) . . . . ?
C13 C14 C15 N8 0.0(6) . . . . ?
N6 C14 C15 N5 1.9(5) . . . . ?
C13 C14 C15 N5 -176.1(3) . . . . ?
N5 C16 C17 C9 87.3(4) . . . 3_666 ?
N7 C16 C17 C9 -84.1(4) . . . 3_666 ?
N4 C6 N1 C7 0.0(4) . . . . ?
C5 C6 N1 C7 178.9(3) . . . . ?
N4 C6 N1 Ni1 179.0(3) . . . . ?
C5 C6 N1 Ni1 -2.1(4) . . . . ?
N3 C7 N1 C6 -0.4(4) . . . . ?
C8 C7 N1 C6 -173.7(3) . . . . ?
N3 C7 N1 Ni1 -178.9(3) . . . . ?
C8 C7 N1 Ni1 7.9(6) . . . . ?
C2 C1 N2 C5 -2.1(5) . . . . ?
C2 C1 N2 Ni1 175.7(3) . . . . ?
C4 C5 N2 C1 1.2(5) . . . . ?
C6 C5 N2 C1 -178.0(3) . . . . ?
C4 C5 N2 Ni1 -176.9(3) . . . . ?
C6 C5 N2 Ni1 3.9(4) . . . . ?
N1 C7 N3 N4 0.7(5) . . . . ?
C8 C7 N3 N4 174.0(3) . . . . ?
N1 C6 N4 N3 0.4(5) . . . . ?
C5 C6 N4 N3 -178.4(4) . . . . ?
C7 N3 N4 C6 -0.6(4) . . . . ?
N7 C16 N5 C15 0.1(4) . . . . ?
C17 C16 N5 C15 -172.5(4) . . . . ?
N7 C16 N5 Ni1 179.6(3) . . . . ?
C17 C16 N5 Ni1 7.0(7) . . . . ?
N8 C15 N5 C16 0.0(4) . . . . ?
C14 C15 N5 C16 176.6(3) . . . . ?
N8 C15 N5 Ni1 -179.7(3) . . . . ?
C14 C15 N5 Ni1 -3.1(4) . . . . ?
C13 C14 N6 C10 0.2(5) . . . . ?
C15 C14 N6 C10 -177.8(3) . . . . ?
C13 C14 N6 Ni1 178.3(3) . . . . ?
C15 C14 N6 Ni1 0.3(4) . . . . ?
C11 C10 N6 C14 -0.3(6) . . . . ?
C11 C10 N6 Ni1 -178.2(3) . . . . ?
N5 C16 N7 N8 -0.1(4) . . . . ?
C17 C16 N7 N8 172.7(3) . . . . ?
N5 C15 N8 N7 0.0(4) . . . . ?
C14 C15 N8 N7 -176.4(4) . . . . ?
C16 N7 N8 C15 0.1(4) . . . . ?
O2 C18 O1 Ni1 178.6(3) . . . . ?
C18 C18 O1 Ni1 -1.0(4) 3_666 . . . ?
O1 C18 O2 Ni1 178.9(3) . . . 3_666 ?
C18 C18 O2 Ni1 -1.5(4) 3_666 . . 3_666 ?

_refine_diff_density_max         0.711
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.098



####################################################################### 
# 
# 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_5a
_database_code_depnum_ccdc_archive 'CCDC 1907072'
loop_
_audit_author_name
_audit_author_address
'Ivan Nemec'
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-06-04 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H56 Cl2 N16 Ni2 O18'
_chemical_formula_weight         1285.36

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   14.649(5)
_cell_length_b                   12.745(5)
_cell_length_c                   17.960(4)
_cell_angle_alpha                90
_cell_angle_beta                 125.061(18)
_cell_angle_gamma                90
_cell_volume                     2744.7(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11860
_cell_measurement_theta_min      2.962
_cell_measurement_theta_max      26.824

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             1332
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.870
_shelx_estimated_absorpt_T_min   0.805
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_T_min  0.92334
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10822
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.173
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measured_fraction_theta_full 0.906
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_Laue_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_point_group_measured_fraction_full 0.906
_reflns_number_total             4380
_reflns_number_gt                3236
_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       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2014)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  ' enCIFer (Allen et al., 2004)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0946P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4380
_refine_ls_number_parameters     384
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1321
_refine_ls_wR_factor_gt          0.1225
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_restrained_S_all      0.948
_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
Ni1 Ni 0.58799(4) 0.67760(3) 0.48149(3) 0.01843(17) Uani 1 1 d . . . . .
O1 O 0.4585(2) 0.57128(17) 0.40290(14) 0.0211(6) Uani 1 1 d D . . . .
O2 O 0.6158(2) 0.57337(17) 0.58191(14) 0.0206(6) Uani 1 1 d . . . . .
N1 N 0.6926(3) 0.6010(2) 0.45547(18) 0.0232(7) Uani 1 1 d . . . . .
N2 N 0.8053(3) 0.5282(2) 0.43031(19) 0.0291(8) Uani 1 1 d . . . . .
H1N2 H 0.8575 0.4865 0.4371 0.035 Uiso 1 1 calc R U . . .
N3 N 0.7465(3) 0.5972(2) 0.3609(2) 0.0308(8) Uani 1 1 d . . . . .
N4 N 0.5496(3) 0.7595(2) 0.36615(17) 0.0215(7) Uani 1 1 d . . . . .
N5 N 0.4989(3) 0.7781(2) 0.50974(17) 0.0213(7) Uani 1 1 d . . . . .
N6 N 0.4098(3) 0.8848(2) 0.5397(2) 0.0290(8) Uani 1 1 d . . . . .
H1N6 H 0.3547 0.9131 0.5392 0.035 Uiso 1 1 calc R U . . .
N7 N 0.5141(3) 0.9235(2) 0.5868(2) 0.0278(8) Uani 1 1 d . . . . .
N8 N 0.7143(3) 0.7860(2) 0.56811(18) 0.0205(7) Uani 1 1 d . . . . .
C1 C 0.8308(4) 0.4738(3) 0.5755(2) 0.0324(10) Uani 1 1 d . . . . .
H1A H 0.7815 0.4747 0.5966 0.039 Uiso 1 1 calc R U . . .
H1B H 0.9000 0.5120 0.6212 0.039 Uiso 1 1 calc R U . . .
C2 C 0.7742(3) 0.5314(3) 0.4871(2) 0.0247(9) Uani 1 1 d . . . . .
C3 C 0.6807(3) 0.6409(3) 0.3795(2) 0.0216(8) Uani 1 1 d . . . . .
C4 C 0.6044(3) 0.7273(3) 0.3304(2) 0.0216(8) Uani 1 1 d . . . . .
C5 C 0.5929(4) 0.7762(3) 0.2572(2) 0.0301(9) Uani 1 1 d . . . . .
H5 H 0.6320 0.7514 0.2330 0.036 Uiso 1 1 calc R U . . .
C6 C 0.5231(4) 0.8623(3) 0.2196(2) 0.0348(10) Uani 1 1 d . . . . .
H6 H 0.5140 0.8979 0.1693 0.042 Uiso 1 1 calc R U . . .
C7 C 0.4675(4) 0.8957(3) 0.2553(2) 0.0337(10) Uani 1 1 d . . . . .
H7 H 0.4191 0.9547 0.2303 0.040 Uiso 1 1 calc R U . . .
C8 C 0.4829(3) 0.8422(3) 0.3286(2) 0.0257(9) Uani 1 1 d . . . . .
H8 H 0.4439 0.8656 0.3533 0.031 Uiso 1 1 calc R U . . .
C9 C 0.8187(4) 0.7894(3) 0.5918(2) 0.0268(10) Uani 1 1 d . . . . .
H9 H 0.8429 0.7356 0.5703 0.032 Uiso 1 1 calc R U . . .
C10 C 0.8933(4) 0.8668(3) 0.6459(2) 0.0317(9) Uani 1 1 d . . . . .
H10 H 0.9669 0.8668 0.6609 0.038 Uiso 1 1 calc R U . . .
C11 C 0.8590(4) 0.9441(3) 0.6778(3) 0.0345(11) Uani 1 1 d . . . . .
H11 H 0.9089 0.9984 0.7154 0.041 Uiso 1 1 calc R U . . .
C12 C 0.7519(4) 0.9423(3) 0.6550(2) 0.0307(10) Uani 1 1 d . . . . .
H12 H 0.7274 0.9945 0.6775 0.037 Uiso 1 1 calc R U . . .
C13 C 0.6805(3) 0.8634(3) 0.5988(2) 0.0231(9) Uani 1 1 d . . . . .
C14 C 0.5650(3) 0.8570(3) 0.5667(2) 0.0220(9) Uani 1 1 d . . . . .
C15 C 0.3999(4) 0.7982(3) 0.4936(2) 0.0253(9) Uani 1 1 d . . . . .
C16 C 0.2944(4) 0.7376(3) 0.4357(3) 0.0327(10) Uani 1 1 d . . . . .
H16A H 0.3101 0.6724 0.4149 0.039 Uiso 1 1 calc R U . . .
H16B H 0.2407 0.7796 0.3811 0.039 Uiso 1 1 calc R U . . .
C17 C 0.2412(4) 0.7089(3) 0.4853(3) 0.0348(10) Uani 1 1 d . . . . .
H17A H 0.2968 0.6719 0.5425 0.042 Uiso 1 1 calc R U . . .
H17B H 0.2194 0.7740 0.5014 0.042 Uiso 1 1 calc R U . . .
C18 C 0.1392(4) 0.6396(3) 0.4282(3) 0.0350(10) Uani 1 1 d . . . . .
H18A H 0.0922 0.6680 0.3656 0.042 Uiso 1 1 calc R U . . .
H18B H 0.0949 0.6415 0.4539 0.042 Uiso 1 1 calc R U . . .
C20 C 0.4544(3) 0.4991(2) 0.4481(2) 0.0168(8) Uani 1 1 d . . . . .
O3 O 0.0480(3) 0.8895(3) 0.0803(2) 0.0556(9) Uani 1 1 d . . . . .
O4 O 0.2230(3) 0.8610(3) 0.2145(2) 0.0530(9) Uani 1 1 d . . . . .
O5 O 0.0608(3) 0.8337(2) 0.2083(2) 0.0483(9) Uani 1 1 d . . . . .
O6 O 0.1083(3) 0.7189(2) 0.1364(3) 0.0652(11) Uani 1 1 d . . . . .
Cl1 Cl 0.11039(9) 0.82583(7) 0.15968(6) 0.0327(3) Uani 1 1 d . . . . .
O1S O 0.0429(3) 0.5843(3) 0.9096(2) 0.0619(10) Uani 1 1 d . . . . .
C1S C -0.0457(4) 0.6241(3) 0.8777(3) 0.0403(11) Uani 1 1 d . . . . .
C2S C -0.0897(5) 0.6503(5) 0.9332(3) 0.0639(16) Uani 1 1 d . . . . .
H2S1 H -0.0468 0.6120 0.9910 0.096 Uiso 1 1 calc R U . . .
H2S2 H -0.1684 0.6300 0.8995 0.096 Uiso 1 1 calc R U . . .
H2S3 H -0.0826 0.7259 0.9453 0.096 Uiso 1 1 calc R U . . .
C3S C -0.1197(5) 0.6575(5) 0.7816(3) 0.0723(18) Uani 1 1 d . . . . .
H3S1 H -0.0777 0.6578 0.7544 0.109 Uiso 1 1 calc R U . . .
H3S2 H -0.1479 0.7282 0.7784 0.109 Uiso 1 1 calc R U . . .
H3S3 H -0.1825 0.6086 0.7481 0.109 Uiso 1 1 calc R U . . .
O2S O 0.2600(3) 0.9825(2) 0.55601(18) 0.0397(7) Uani 1 1 d D . . . .
O3S O 0.2884(5) 0.5763(4) 0.2122(2) 0.116(2) Uani 1 1 d D . . . .
H2SA H 0.266(5) 0.966(6) 0.605(2) 0.139 Uiso 1 1 d D U . . .
H2SB H 0.192(2) 0.972(6) 0.513(3) 0.139 Uiso 1 1 d D U . . .
H3SB H 0.344(3) 0.585(5) 0.2674(14) 0.139 Uiso 1 1 d D U . . .
H3SA H 0.237(4) 0.615(5) 0.205(4) 0.139 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 2.083(3) . ?
Ni1 O2 2.083(2) . ?
Ni1 O1 2.085(2) . ?
Ni1 N4 2.088(3) . ?
Ni1 N5 2.088(3) . ?
Ni1 N8 2.108(3) . ?
O1 C20 1.251(4) . ?
O2 C20 1.251(4) 3_666 ?
N1 C2 1.327(5) . ?
N1 C3 1.371(4) . ?
N2 C2 1.335(5) . ?
N2 N3 1.354(4) . ?
N2 H1N2 0.8800 . ?
N3 C3 1.310(5) . ?
N4 C8 1.328(4) . ?
N4 C4 1.349(5) . ?
N5 C15 1.330(5) . ?
N5 C14 1.363(4) . ?
N6 C15 1.337(5) . ?
N6 N7 1.344(5) . ?
N6 H1N6 0.8800 . ?
N7 C14 1.310(5) . ?
N8 C9 1.332(5) . ?
N8 C13 1.355(5) . ?
C1 C2 1.495(5) . ?
C1 C18 1.524(5) 3_666 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C3 C4 1.452(5) . ?
C4 C5 1.375(5) . ?
C5 C6 1.383(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.362(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.382(5) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.376(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.371(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.442(6) . ?
C15 C16 1.491(6) . ?
C16 C17 1.527(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.517(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C1 1.524(5) 3_666 ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 O2 1.251(4) 3_666 ?
C20 C20 1.548(6) 3_666 ?
O3 Cl1 1.425(3) . ?
O4 Cl1 1.424(3) . ?
O5 Cl1 1.425(3) . ?
O6 Cl1 1.421(3) . ?
O1S C1S 1.189(5) . ?
C1S C3S 1.479(6) . ?
C1S C2S 1.503(7) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?
O2S H2SA 0.854(10) . ?
O2S H2SB 0.853(10) . ?
O3S H3SB 0.853(10) . ?
O3S H3SA 0.851(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 O2 95.30(10) . . ?
N1 Ni1 O1 92.51(11) . . ?
O2 Ni1 O1 79.70(9) . . ?
N1 Ni1 N4 79.94(11) . . ?
O2 Ni1 N4 170.12(9) . . ?
O1 Ni1 N4 91.79(10) . . ?
N1 Ni1 N5 169.88(12) . . ?
O2 Ni1 N5 91.10(10) . . ?
O1 Ni1 N5 96.35(11) . . ?
N4 Ni1 N5 94.86(11) . . ?
N1 Ni1 N8 91.48(12) . . ?
O2 Ni1 N8 97.28(10) . . ?
O1 Ni1 N8 175.20(9) . . ?
N4 Ni1 N8 91.53(11) . . ?
N5 Ni1 N8 79.91(12) . . ?
C20 O1 Ni1 113.7(2) . . ?
C20 O2 Ni1 113.22(19) 3_666 . ?
C2 N1 C3 104.0(3) . . ?
C2 N1 Ni1 144.6(2) . . ?
C3 N1 Ni1 111.2(2) . . ?
C2 N2 N3 111.5(3) . . ?
C2 N2 H1N2 124.2 . . ?
N3 N2 H1N2 124.2 . . ?
C3 N3 N2 102.4(3) . . ?
C8 N4 C4 117.7(3) . . ?
C8 N4 Ni1 126.9(2) . . ?
C4 N4 Ni1 115.2(2) . . ?
C15 N5 C14 103.7(3) . . ?
C15 N5 Ni1 145.1(2) . . ?
C14 N5 Ni1 111.2(3) . . ?
C15 N6 N7 111.9(3) . . ?
C15 N6 H1N6 124.1 . . ?
N7 N6 H1N6 124.1 . . ?
C14 N7 N6 102.1(3) . . ?
C9 N8 C13 117.8(3) . . ?
C9 N8 Ni1 128.1(2) . . ?
C13 N8 Ni1 114.0(3) . . ?
C2 C1 C18 114.6(3) . 3_666 ?
C2 C1 H1A 108.6 . . ?
C18 C1 H1A 108.6 3_666 . ?
C2 C1 H1B 108.6 . . ?
C18 C1 H1B 108.6 3_666 . ?
H1A C1 H1B 107.6 . . ?
N1 C2 N2 108.2(3) . . ?
N1 C2 C1 126.6(3) . . ?
N2 C2 C1 124.9(4) . . ?
N3 C3 N1 113.9(3) . . ?
N3 C3 C4 126.2(3) . . ?
N1 C3 C4 119.9(3) . . ?
N4 C4 C5 122.5(3) . . ?
N4 C4 C3 113.8(3) . . ?
C5 C4 C3 123.6(3) . . ?
C4 C5 C6 118.5(4) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C7 C6 C5 119.5(3) . . ?
C7 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C6 C7 C8 118.7(4) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 H7 120.7 . . ?
N4 C8 C7 123.1(3) . . ?
N4 C8 H8 118.5 . . ?
C7 C8 H8 118.5 . . ?
N8 C9 C10 123.3(4) . . ?
N8 C9 H9 118.3 . . ?
C10 C9 H9 118.3 . . ?
C11 C10 C9 118.5(4) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
C11 C12 C13 119.0(4) . . ?
C11 C12 H12 120.5 . . ?
C13 C12 H12 120.5 . . ?
N8 C13 C12 121.8(4) . . ?
N8 C13 C14 114.5(3) . . ?
C12 C13 C14 123.7(3) . . ?
N7 C14 N5 114.4(4) . . ?
N7 C14 C13 125.2(3) . . ?
N5 C14 C13 120.4(3) . . ?
N5 C15 N6 107.9(4) . . ?
N5 C15 C16 128.0(3) . . ?
N6 C15 C16 124.1(4) . . ?
C15 C16 C17 112.9(3) . . ?
C15 C16 H16A 109.0 . . ?
C17 C16 H16A 109.0 . . ?
C15 C16 H16B 109.0 . . ?
C17 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C18 C17 C16 112.3(3) . . ?
C18 C17 H17A 109.1 . . ?
C16 C17 H17A 109.1 . . ?
C18 C17 H17B 109.1 . . ?
C16 C17 H17B 109.1 . . ?
H17A C17 H17B 107.9 . . ?
C17 C18 C1 112.7(4) . 3_666 ?
C17 C18 H18A 109.1 . . ?
C1 C18 H18A 109.1 3_666 . ?
C17 C18 H18B 109.1 . . ?
C1 C18 H18B 109.1 3_666 . ?
H18A C18 H18B 107.8 . . ?
O2 C20 O1 126.7(3) 3_666 . ?
O2 C20 C20 117.2(3) 3_666 3_666 ?
O1 C20 C20 116.1(4) . 3_666 ?
O6 Cl1 O4 109.0(2) . . ?
O6 Cl1 O5 108.4(2) . . ?
O4 Cl1 O5 110.5(2) . . ?
O6 Cl1 O3 111.0(2) . . ?
O4 Cl1 O3 109.6(2) . . ?
O5 Cl1 O3 108.3(2) . . ?
O1S C1S C3S 123.4(5) . . ?
O1S C1S C2S 122.7(4) . . ?
C3S C1S C2S 113.9(5) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C1S C3S H3S1 109.5 . . ?
C1S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
C1S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
H2SA O2S H2SB 105(2) . . ?
H3SB O3S H3SA 105(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N2 N3 C3 0.3(4) . . . . ?
C15 N6 N7 C14 0.1(4) . . . . ?
C3 N1 C2 N2 -2.2(4) . . . . ?
Ni1 N1 C2 N2 -175.7(3) . . . . ?
C3 N1 C2 C1 171.9(4) . . . . ?
Ni1 N1 C2 C1 -1.6(7) . . . . ?
N3 N2 C2 N1 1.2(4) . . . . ?
N3 N2 C2 C1 -173.0(3) . . . . ?
C18 C1 C2 N1 142.6(4) 3_666 . . . ?
C18 C1 C2 N2 -44.3(5) 3_666 . . . ?
N2 N3 C3 N1 -1.8(4) . . . . ?
N2 N3 C3 C4 175.2(3) . . . . ?
C2 N1 C3 N3 2.5(4) . . . . ?
Ni1 N1 C3 N3 178.5(2) . . . . ?
C2 N1 C3 C4 -174.6(3) . . . . ?
Ni1 N1 C3 C4 1.4(4) . . . . ?
C8 N4 C4 C5 -0.4(5) . . . . ?
Ni1 N4 C4 C5 -176.7(3) . . . . ?
C8 N4 C4 C3 176.2(3) . . . . ?
Ni1 N4 C4 C3 -0.1(4) . . . . ?
N3 C3 C4 N4 -177.7(4) . . . . ?
N1 C3 C4 N4 -0.9(5) . . . . ?
N3 C3 C4 C5 -1.1(6) . . . . ?
N1 C3 C4 C5 175.6(3) . . . . ?
N4 C4 C5 C6 0.6(6) . . . . ?
C3 C4 C5 C6 -175.6(4) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C5 C6 C7 C8 0.1(6) . . . . ?
C4 N4 C8 C7 0.1(5) . . . . ?
Ni1 N4 C8 C7 175.8(3) . . . . ?
C6 C7 C8 N4 0.1(6) . . . . ?
C13 N8 C9 C10 0.4(5) . . . . ?
Ni1 N8 C9 C10 177.0(3) . . . . ?
N8 C9 C10 C11 0.5(5) . . . . ?
C9 C10 C11 C12 -0.1(5) . . . . ?
C10 C11 C12 C13 -1.2(5) . . . . ?
C9 N8 C13 C12 -1.8(5) . . . . ?
Ni1 N8 C13 C12 -178.8(3) . . . . ?
C9 N8 C13 C14 177.2(3) . . . . ?
Ni1 N8 C13 C14 0.1(3) . . . . ?
C11 C12 C13 N8 2.2(5) . . . . ?
C11 C12 C13 C14 -176.7(3) . . . . ?
N6 N7 C14 N5 -0.2(4) . . . . ?
N6 N7 C14 C13 178.8(3) . . . . ?
C15 N5 C14 N7 0.2(4) . . . . ?
Ni1 N5 C14 N7 179.5(2) . . . . ?
C15 N5 C14 C13 -178.8(3) . . . . ?
Ni1 N5 C14 C13 0.5(4) . . . . ?
N8 C13 C14 N7 -179.4(3) . . . . ?
C12 C13 C14 N7 -0.5(5) . . . . ?
N8 C13 C14 N5 -0.4(4) . . . . ?
C12 C13 C14 N5 178.5(3) . . . . ?
C14 N5 C15 N6 -0.1(4) . . . . ?
Ni1 N5 C15 N6 -179.0(3) . . . . ?
C14 N5 C15 C16 -179.7(3) . . . . ?
Ni1 N5 C15 C16 1.4(6) . . . . ?
N7 N6 C15 N5 0.0(4) . . . . ?
N7 N6 C15 C16 179.6(3) . . . . ?
N5 C15 C16 C17 127.8(4) . . . . ?
N6 C15 C16 C17 -51.8(5) . . . . ?
C15 C16 C17 C18 -175.3(3) . . . . ?
C16 C17 C18 C1 76.3(4) . . . 3_666 ?
Ni1 O1 C20 O2 178.7(3) . . . 3_666 ?
Ni1 O1 C20 C20 -1.0(4) . . . 3_666 ?

_refine_diff_density_max         0.647
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.114

####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1907071'
loop_
_audit_author_name
_audit_author_address
I.Nemec
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-05-09 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H48 N20 Ni2 O18'
_chemical_formula_weight         1166.36

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

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

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

_cell_length_a                   12.203(2)
_cell_length_b                   29.025(6)
_cell_length_c                   15.894(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.88(3)
_cell_angle_gamma                90
_cell_volume                     5358(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    7362
_cell_measurement_theta_min      1.403
_cell_measurement_theta_max      26.822

_exptl_crystal_description       prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_F_000             2416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.121
_exptl_absorpt_coefficient_mu    0.788
_shelx_estimated_absorpt_T_min   0.784
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44020
_diffrn_reflns_av_unetI/netI     0.0966
_diffrn_reflns_av_R_equivalents  0.1165
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.403
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_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             9439
_reflns_number_gt                6088
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0844P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9439
_refine_ls_number_parameters     697
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1689
_refine_ls_wR_factor_gt          0.1530
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.018
_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
Ni1 Ni 0.77095(5) 0.38741(2) 0.89309(4) 0.02687(18) Uani 1 1 d . . . . .
Ni2 Ni 0.21021(5) 0.34199(2) 0.49300(4) 0.02747(18) Uani 1 1 d . . . . .
O1W O 0.9464(3) 0.39529(12) 0.9114(2) 0.0329(8) Uani 1 1 d . . . . .
H1WB H 0.9740 0.4142 0.8824 0.039 Uiso 1 1 d R U . . .
H1WA H 0.9890 0.3715 0.9231 0.039 Uiso 1 1 d R U . . .
O2W O 0.8198(3) 0.38184(14) 1.0292(2) 0.0472(10) Uani 1 1 d . . . . .
H2WB H 0.8834 0.3931 1.0609 0.057 Uiso 1 1 d R U . . .
H2WA H 0.7661 0.3857 1.0522 0.057 Uiso 1 1 d R U . . .
O3W O 0.0671(3) 0.38162(13) 0.4201(2) 0.0422(9) Uani 1 1 d . . . . .
H3WB H 0.0012 0.3853 0.4396 0.051 Uiso 1 1 d R U . . .
H3WA H 0.0465 0.3714 0.3630 0.051 Uiso 1 1 d R U . . .
O4W O 0.1478(3) 0.29165(12) 0.3962(2) 0.0390(9) Uani 1 1 d . . . . .
H4WA H 0.1727 0.2641 0.4036 0.047 Uiso 1 1 d R U . . .
H4WB H 0.1631 0.3044 0.3530 0.047 Uiso 1 1 d R U . . .
N1 N 0.3602(3) 0.30137(13) 0.5427(2) 0.0249(9) Uani 1 1 d . . . . .
N2 N 0.5035(3) 0.25136(14) 0.5739(3) 0.0317(10) Uani 1 1 d . . . . .
N3 N 0.5258(4) 0.28087(14) 0.5124(3) 0.0310(10) Uani 1 1 d . . . . .
N4 N 0.3118(4) 0.37025(14) 0.4197(2) 0.0332(10) Uani 1 1 d . . . . .
N5 N 0.5962(3) 0.39086(14) 0.8876(2) 0.0264(9) Uani 1 1 d . . . . .
N6 N 0.4225(3) 0.39383(14) 0.8977(2) 0.0289(9) Uani 1 1 d . . . . .
H6N H 0.3571 0.3855 0.9007 0.014(11) Uiso 1 1 d R . . . .
N7 N 0.4575(3) 0.43956(15) 0.9054(2) 0.0296(9) Uani 1 1 d . . . . .
N8 N 0.7499(3) 0.46039(15) 0.9031(2) 0.0308(10) Uani 1 1 d . . . . .
C1 C 0.3602(4) 0.23844(16) 0.6562(3) 0.0262(11) Uani 1 1 d . . . . .
H1A H 0.3649 0.2048 0.6473 0.031 Uiso 1 1 calc R U . . .
H1B H 0.2781 0.2465 0.6445 0.031 Uiso 1 1 calc R U . . .
C2 C 0.4269(4) 0.25032(17) 0.7533(3) 0.0278(11) Uani 1 1 d . . . . .
H2A H 0.3876 0.2357 0.7925 0.033 Uiso 1 1 calc R U . . .
H2B H 0.5053 0.2371 0.7681 0.033 Uiso 1 1 calc R U . . .
C3 C 0.4366(4) 0.30259(17) 0.7720(3) 0.0289(11) Uani 1 1 d . . . . .
H3A H 0.4857 0.3165 0.7395 0.035 Uiso 1 1 calc R U . . .
H3B H 0.3591 0.3166 0.7493 0.035 Uiso 1 1 calc R U . . .
C4 C 0.4876(4) 0.31410(18) 0.8709(3) 0.0281(11) Uani 1 1 d . . . . .
H4A H 0.4354 0.3023 0.9029 0.034 Uiso 1 1 calc R U . . .
H4B H 0.5626 0.2983 0.8949 0.034 Uiso 1 1 calc R U . . .
C5 C 0.4063(4) 0.26346(16) 0.5911(3) 0.0233(10) Uani 1 1 d . . . . .
C6 C 0.4364(4) 0.30972(16) 0.4958(3) 0.0271(11) Uani 1 1 d . . . . .
C7 C 0.4139(5) 0.34827(17) 0.4305(3) 0.0326(12) Uani 1 1 d . . . . .
C8 C 0.4893(5) 0.3603(2) 0.3828(4) 0.0435(14) Uani 1 1 d . . . . .
H8A H 0.5610 0.3450 0.3931 0.052 Uiso 1 1 calc R U . . .
C9 C 0.4557(6) 0.3955(2) 0.3193(4) 0.0515(17) Uani 1 1 d . . . . .
H9A H 0.5037 0.4034 0.2844 0.062 Uiso 1 1 calc R U . . .
C10 C 0.3531(6) 0.4184(2) 0.3077(4) 0.0525(17) Uani 1 1 d . . . . .
H10A H 0.3305 0.4427 0.2659 0.063 Uiso 1 1 calc R U . . .
C11 C 0.2827(5) 0.40511(19) 0.3586(3) 0.0439(14) Uani 1 1 d . . . . .
H11A H 0.2120 0.4209 0.3504 0.053 Uiso 1 1 calc R U . . .
C12 C 0.5043(4) 0.36495(17) 0.8868(3) 0.0254(11) Uani 1 1 d . . . . .
C13 C 0.5633(4) 0.43582(17) 0.8994(3) 0.0273(11) Uani 1 1 d . . . . .
C14 C 0.6457(4) 0.47464(17) 0.9071(3) 0.0279(11) Uani 1 1 d . . . . .
C15 C 0.8312(4) 0.49414(19) 0.9118(3) 0.0367(13) Uani 1 1 d . . . . .
H15A H 0.9048 0.4852 0.9088 0.044 Uiso 1 1 calc R U . . .
C16 C 0.8134(5) 0.54128(19) 0.9249(3) 0.0409(13) Uani 1 1 d . . . . .
H16A H 0.8734 0.5632 0.9322 0.049 Uiso 1 1 calc R U . . .
C17 C 0.7040(4) 0.55461(19) 0.9267(3) 0.0357(12) Uani 1 1 d . . . . .
H17A H 0.6874 0.5861 0.9332 0.043 Uiso 1 1 calc R U . . .
C18 C 0.6201(4) 0.52124(18) 0.9190(3) 0.0340(12) Uani 1 1 d . . . . .
H18A H 0.5460 0.5296 0.9217 0.041 Uiso 1 1 calc R U . . .
N1A N 0.7455(3) 0.38041(14) 0.7558(2) 0.0275(9) Uani 1 1 d . . . . .
N2A N 0.7556(4) 0.37416(16) 0.6220(3) 0.0402(11) Uani 1 1 d . . . . .
H2NA H 0.7510 0.3797 0.5685 0.048 Uiso 1 1 d R U . . .
N3A N 0.7675(4) 0.32931(15) 0.6528(3) 0.0385(11) Uani 1 1 d . . . . .
N4A N 0.7767(3) 0.31382(15) 0.8810(3) 0.0319(10) Uani 1 1 d . . . . .
N5A N 0.2465(3) 0.39284(13) 0.5943(2) 0.0260(9) Uani 1 1 d . . . . .
N6A N 0.2720(4) 0.44746(14) 0.6937(3) 0.0336(10) Uani 1 1 d . . . . .
H6NA H 0.2900 0.4738 0.7173 0.040 Uiso 1 1 d R U . . .
N7A N 0.1988(4) 0.41631(14) 0.7150(3) 0.0326(10) Uani 1 1 d . . . . .
N8A N 0.1166(3) 0.31447(14) 0.5733(2) 0.0287(9) Uani 1 1 d . . . . .
C1A C 0.7211(5) 0.45556(18) 0.6645(4) 0.0402(13) Uani 1 1 d D . . . .
H1AC H 0.7735 0.4735 0.7102 0.048 Uiso 0.121(7) 1 d R U P A 2
H1AD H 0.7297 0.4640 0.6085 0.048 Uiso 0.121(7) 1 d R U P A 2
H1AA H 0.7315 0.4715 0.7194 0.048 Uiso 0.879(7) 1 d R U P A 1
H1AB H 0.7753 0.4677 0.6375 0.048 Uiso 0.879(7) 1 d R U P A 1
C2A C 0.5974(5) 0.4638(2) 0.6034(4) 0.0319(14) Uani 0.879(7) 1 d D . P A 1
H2AA H 0.5853 0.4972 0.5915 0.038 Uiso 0.879(7) 1 calc R U P A 1
H2AB H 0.5869 0.4480 0.5462 0.038 Uiso 0.879(7) 1 calc R U P A 1
C3A C 0.5092(5) 0.4461(2) 0.6448(4) 0.0327(15) Uani 0.879(7) 1 d D . P A 1
H3AA H 0.5241 0.4598 0.7043 0.039 Uiso 0.879(7) 1 calc R U P A 1
H3AB H 0.5166 0.4122 0.6516 0.039 Uiso 0.879(7) 1 calc R U P A 1
C2A' C 0.5914(18) 0.4624(15) 0.664(2) 0.0319(14) Uani 0.121(7) 1 d D . P A 2
H2AC H 0.5787 0.4437 0.7128 0.038 Uiso 0.121(7) 1 calc R U P A 2
H2AD H 0.5796 0.4951 0.6768 0.038 Uiso 0.121(7) 1 calc R U P A 2
C3A' C 0.5027(19) 0.4487(15) 0.577(2) 0.0327(15) Uani 0.121(7) 1 d D . P A 2
H3AC H 0.5103 0.4155 0.5654 0.039 Uiso 0.121(7) 1 calc R U P A 2
H3AD H 0.5144 0.4668 0.5281 0.039 Uiso 0.121(7) 1 calc R U P A 2
C4A C 0.3835(4) 0.45851(18) 0.5865(4) 0.0369(13) Uani 1 1 d D . . . .
H4AC H 0.3372 0.4660 0.5274 0.044 Uiso 0.121(7) 1 d R U P A 2
H4AD H 0.3952 0.4872 0.6180 0.044 Uiso 0.121(7) 1 d R U P A 2
H4AA H 0.3722 0.4497 0.5262 0.044 Uiso 0.879(7) 1 d R U P A 1
H4AB H 0.3719 0.4911 0.5885 0.044 Uiso 0.879(7) 1 d R U P A 1
C5A C 0.7434(4) 0.40465(18) 0.6827(3) 0.0319(12) Uani 1 1 d . . . . .
C6A C 0.7611(4) 0.33537(17) 0.7342(3) 0.0273(11) Uani 1 1 d . . . . .
C7A C 0.7704(4) 0.29730(17) 0.7999(3) 0.0276(11) Uani 1 1 d . . . . .
C8A C 0.7708(4) 0.25012(18) 0.7794(4) 0.0354(12) Uani 1 1 d . . . . .
H8AA H 0.7664 0.2402 0.7215 0.042 Uiso 1 1 calc R U . . .
C9A C 0.7779(5) 0.2183(2) 0.8471(4) 0.0440(14) Uani 1 1 d . . . . .
H9AA H 0.7794 0.1862 0.8358 0.053 Uiso 1 1 calc R U . . .
C10A C 0.7828(4) 0.2338(2) 0.9306(4) 0.0425(14) Uani 1 1 d . . . . .
H10B H 0.7865 0.2126 0.9771 0.051 Uiso 1 1 calc R U . . .
C11A C 0.7821(4) 0.2816(2) 0.9449(3) 0.0372(13) Uani 1 1 d . . . . .
H11B H 0.7857 0.2921 1.0023 0.045 Uiso 1 1 calc R U . . .
C12A C 0.3000(4) 0.43366(17) 0.6220(3) 0.0274(11) Uani 1 1 d . . . . .
C13A C 0.1880(4) 0.38413(17) 0.6533(3) 0.0291(11) Uani 1 1 d . . . . .
C14A C 0.1194(4) 0.34078(17) 0.6457(3) 0.0258(11) Uani 1 1 d . . . . .
C15A C 0.0696(4) 0.32564(19) 0.7091(3) 0.0336(12) Uani 1 1 d . . . . .
H15B H 0.0717 0.3443 0.7586 0.040 Uiso 1 1 calc R U . . .
C16A C 0.0161(4) 0.2819(2) 0.6980(3) 0.0404(13) Uani 1 1 d . . . . .
H16B H -0.0159 0.2704 0.7412 0.049 Uiso 1 1 calc R U . . .
C17A C 0.0108(4) 0.2563(2) 0.6241(4) 0.0430(14) Uani 1 1 d . . . . .
H17B H -0.0259 0.2271 0.6154 0.052 Uiso 1 1 calc R U . . .
C18A C 0.0600(4) 0.27375(18) 0.5619(3) 0.0330(12) Uani 1 1 d . . . . .
H18B H 0.0535 0.2564 0.5099 0.040 Uiso 1 1 calc R U . . .
O5W O 0.3526(3) 0.53314(13) 0.7566(2) 0.0444(10) Uani 1 1 d . . . . .
H5WB H 0.3019 0.5536 0.7238 0.053 Uiso 1 1 d R U . . .
H5WA H 0.3409 0.5488 0.8020 0.053 Uiso 1 1 d R U . . .
N1N N 0.1787(3) 0.17373(15) 0.4264(2) 0.0304(10) Uani 1 1 d . . . . .
N2N N 0.1971(4) 0.59758(16) 0.5722(3) 0.0388(11) Uani 1 1 d . . . . .
H2N H 0.5368 0.2261 0.5948 0.047 Uiso 1 1 d R U . . .
N4N N 0.6035(4) 0.13783(16) 0.6180(3) 0.0338(10) Uani 1 1 d . . . . .
O1N O 0.2540(3) 0.20525(13) 0.4328(3) 0.0435(9) Uani 1 1 d . . . . .
O2N O 0.0787(3) 0.18501(12) 0.4258(2) 0.0358(8) Uani 1 1 d . . . . .
O3N O 0.2040(3) 0.13171(12) 0.4188(2) 0.0343(8) Uani 1 1 d . . . . .
O4N O 0.2757(4) 0.5785(2) 0.5514(3) 0.0764(16) Uani 1 1 d . . . . .
O5N O 0.1913(4) 0.59393(15) 0.6497(2) 0.0564(12) Uani 1 1 d . . . . .
O6N O 0.1221(4) 0.62136(14) 0.5158(2) 0.0549(12) Uani 1 1 d . . . . .
O10N O 0.5174(4) 0.14000(15) 0.6431(3) 0.0610(13) Uani 1 1 d . . . . .
O11N O 0.6505(3) 0.17539(13) 0.6020(2) 0.0419(9) Uani 1 1 d . . . . .
O12N O 0.6455(3) 0.09911(12) 0.6056(2) 0.0360(9) Uani 1 1 d . . . . .
N3N N 0.0691(5) 0.3499(2) 0.1973(3) 0.0627(15) Uani 1 1 d D . . . .
O7N O 0.0077(8) 0.3709(4) 0.2376(5) 0.0550(10) Uani 0.543(11) 1 d D . P B 1
O8N O 0.0598(12) 0.3574(5) 0.1148(6) 0.0550(10) Uani 0.543(11) 1 d D . P B 1
O9N O 0.1582(13) 0.3270(8) 0.2424(8) 0.0550(10) Uani 0.543(11) 1 d D . P B 1
O7N' O -0.0158(8) 0.3448(5) 0.2374(6) 0.0550(10) Uani 0.457(11) 1 d D . P B 2
O9N' O 0.1625(16) 0.3262(9) 0.2289(9) 0.0550(10) Uani 0.457(11) 1 d D . P B 2
O8N' O 0.0414(15) 0.3656(6) 0.1181(8) 0.0550(10) Uani 0.457(11) 1 d D . P B 2
O13N O 1.0108(5) 0.44635(19) 0.7876(4) 0.0820(17) Uani 1 1 d D . . . .
H13B H 1.019(6) 0.4758(5) 0.782(6) 0.098 Uiso 1 1 d D U . . .
H13A H 1.065(5) 0.4351(17) 0.770(5) 0.098 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2W 2.066(3) . ?
Ni1 O1W 2.083(3) . ?
Ni1 N5 2.110(4) . ?
Ni1 N1A 2.117(4) . ?
Ni1 N8 2.146(4) . ?
Ni1 N4A 2.148(4) . ?
Ni2 O4W 2.088(3) . ?
Ni2 N4 2.110(4) . ?
Ni2 N8A 2.113(4) . ?
Ni2 O3W 2.115(4) . ?
Ni2 N1 2.115(4) . ?
Ni2 N5A 2.128(4) . ?
O1W H1WB 0.8501 . ?
O1W H1WA 0.8498 . ?
O2W H2WB 0.8501 . ?
O2W H2WA 0.8500 . ?
O3W H3WB 0.9522 . ?
O3W H3WA 0.9128 . ?
O4W H4WA 0.8503 . ?
O4W H4WB 0.8499 . ?
N1 C5 1.362(6) . ?
N1 C6 1.381(6) . ?
N2 C5 1.342(6) . ?
N2 N3 1.388(5) . ?
N2 H2N 0.8545 . ?
N3 C6 1.336(6) . ?
N4 C7 1.364(7) . ?
N4 C11 1.372(6) . ?
N5 C12 1.346(6) . ?
N5 C13 1.394(6) . ?
N6 C12 1.355(6) . ?
N6 N7 1.388(6) . ?
N6 H6N 0.8501 . ?
N7 C13 1.328(6) . ?
N8 C14 1.357(6) . ?
N8 C15 1.371(7) . ?
C1 C5 1.507(6) . ?
C1 C2 1.546(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.543(7) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.539(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C12 1.501(7) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C6 C7 1.493(7) . ?
C7 C8 1.403(7) . ?
C8 C9 1.406(8) . ?
C8 H8A 0.9500 . ?
C9 C10 1.380(9) . ?
C9 H9A 0.9500 . ?
C10 C11 1.403(8) . ?
C10 H10A 0.9500 . ?
C11 H11A 0.9500 . ?
C13 C14 1.490(7) . ?
C14 C18 1.414(7) . ?
C15 C16 1.411(7) . ?
C15 H15A 0.9500 . ?
C16 C17 1.398(7) . ?
C16 H16A 0.9500 . ?
C17 C18 1.387(7) . ?
C17 H17A 0.9500 . ?
C18 H18A 0.9500 . ?
N1A C5A 1.352(6) . ?
N1A C6A 1.380(6) . ?
N2A C5A 1.350(6) . ?
N2A N3A 1.383(6) . ?
N2A H2NA 0.8500 . ?
N3A C6A 1.330(6) . ?
N4A C7A 1.355(6) . ?
N4A C11A 1.368(6) . ?
N5A C12A 1.360(6) . ?
N5A C13A 1.365(6) . ?
N6A C12A 1.346(6) . ?
N6A N7A 1.385(6) . ?
N6A H6NA 0.8498 . ?
N7A C13A 1.331(6) . ?
N8A C18A 1.353(6) . ?
N8A C14A 1.373(6) . ?
C1A C5A 1.514(7) . ?
C1A C2A 1.543(7) . ?
C1A C2A' 1.59(2) . ?
C1A H1AC 0.9601 . ?
C1A H1AD 0.9601 . ?
C1A H1AA 0.9602 . ?
C1A H1AB 0.9600 . ?
C2A C3A 1.514(7) . ?
C2A H2AA 0.9900 . ?
C2A H2AB 0.9900 . ?
C3A C4A 1.571(7) . ?
C3A H3AA 0.9900 . ?
C3A H3AB 0.9900 . ?
C2A' C3A' 1.52(2) . ?
C2A' H2AC 0.9900 . ?
C2A' H2AD 0.9900 . ?
C3A' C4A 1.532(19) . ?
C3A' H3AC 0.9900 . ?
C3A' H3AD 0.9900 . ?
C4A C12A 1.494(7) . ?
C4A H4AC 0.9600 . ?
C4A H4AD 0.9601 . ?
C4A H4AA 0.9600 . ?
C4A H4AB 0.9601 . ?
C6A C7A 1.500(7) . ?
C7A C8A 1.408(7) . ?
C8A C9A 1.401(7) . ?
C8A H8AA 0.9500 . ?
C9A C10A 1.385(8) . ?
C9A H9AA 0.9500 . ?
C10A C11A 1.406(8) . ?
C10A H10B 0.9500 . ?
C11A H11B 0.9500 . ?
C13A C14A 1.495(7) . ?
C14A C15A 1.398(7) . ?
C15A C16A 1.413(8) . ?
C15A H15B 0.9500 . ?
C16A C17A 1.374(8) . ?
C16A H16B 0.9500 . ?
C17A C18A 1.401(7) . ?
C17A H17B 0.9500 . ?
C18A H18B 0.9500 . ?
O5W H5WB 0.9002 . ?
O5W H5WA 0.9000 . ?
N1N O2N 1.261(5) . ?
N1N O3N 1.273(5) . ?
N1N O1N 1.278(5) . ?
N2N O4N 1.238(6) . ?
N2N O5N 1.260(5) . ?
N2N O6N 1.270(6) . ?
N4N O10N 1.234(5) . ?
N4N O12N 1.275(5) . ?
N4N O11N 1.294(5) . ?
N3N O7N 1.279(8) . ?
N3N O8N' 1.282(11) . ?
N3N O9N 1.288(10) . ?
N3N O9N' 1.294(12) . ?
N3N O8N 1.299(10) . ?
N3N O7N' 1.381(10) . ?
O13N H13B 0.868(10) . ?
O13N H13A 0.855(9) . ?

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
O2W Ni1 O1W 84.78(14) . . ?
O2W Ni1 N5 90.56(14) . . ?
O1W Ni1 N5 169.48(14) . . ?
O2W Ni1 N1A 167.25(16) . . ?
O1W Ni1 N1A 88.46(14) . . ?
N5 Ni1 N1A 97.80(14) . . ?
O2W Ni1 N8 90.14(15) . . ?
O1W Ni1 N8 91.31(14) . . ?
N5 Ni1 N8 79.26(15) . . ?
N1A Ni1 N8 100.84(15) . . ?
O2W Ni1 N4A 90.53(15) . . ?
O1W Ni1 N4A 93.52(14) . . ?
N5 Ni1 N4A 95.95(16) . . ?
N1A Ni1 N4A 79.09(15) . . ?
N8 Ni1 N4A 175.17(15) . . ?
O4W Ni2 N4 90.50(15) . . ?
O4W Ni2 N8A 92.14(15) . . ?
N4 Ni2 N8A 176.62(15) . . ?
O4W Ni2 O3W 85.63(14) . . ?
N4 Ni2 O3W 90.71(15) . . ?
N8A Ni2 O3W 91.59(15) . . ?
O4W Ni2 N1 87.88(14) . . ?
N4 Ni2 N1 80.53(15) . . ?
N8A Ni2 N1 97.46(14) . . ?
O3W Ni2 N1 169.05(14) . . ?
O4W Ni2 N5A 170.57(14) . . ?
N4 Ni2 N5A 97.30(15) . . ?
N8A Ni2 N5A 80.26(15) . . ?
O3W Ni2 N5A 88.98(14) . . ?
N1 Ni2 N5A 98.58(14) . . ?
Ni1 O1W H1WB 123.8 . . ?
Ni1 O1W H1WA 118.3 . . ?
H1WB O1W H1WA 109.1 . . ?
Ni1 O2W H2WB 120.5 . . ?
Ni1 O2W H2WA 115.3 . . ?
H2WB O2W H2WA 112.2 . . ?
Ni2 O3W H3WB 121.4 . . ?
Ni2 O3W H3WA 107.3 . . ?
H3WB O3W H3WA 111.0 . . ?
Ni2 O4W H4WA 121.5 . . ?
Ni2 O4W H4WB 99.8 . . ?
H4WA O4W H4WB 111.2 . . ?
C5 N1 C6 102.5(4) . . ?
C5 N1 Ni2 145.3(3) . . ?
C6 N1 Ni2 110.5(3) . . ?
C5 N2 N3 111.0(4) . . ?
C5 N2 H2N 119.3 . . ?
N3 N2 H2N 129.0 . . ?
C6 N3 N2 101.6(4) . . ?
C7 N4 C11 117.5(4) . . ?
C7 N4 Ni2 114.7(3) . . ?
C11 N4 Ni2 127.6(4) . . ?
C12 N5 C13 104.5(4) . . ?
C12 N5 Ni1 143.3(3) . . ?
C13 N5 Ni1 111.6(3) . . ?
C12 N6 N7 112.6(4) . . ?
C12 N6 H6N 124.9 . . ?
N7 N6 H6N 122.5 . . ?
C13 N7 N6 101.2(4) . . ?
C14 N8 C15 115.9(4) . . ?
C14 N8 Ni1 116.1(3) . . ?
C15 N8 Ni1 127.8(3) . . ?
C5 C1 C2 112.6(4) . . ?
C5 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
C5 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C1 113.4(4) . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
C4 C3 C2 113.2(4) . . ?
C4 C3 H3A 108.9 . . ?
C2 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.8 . . ?
C12 C4 C3 112.1(4) . . ?
C12 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
C12 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N2 C5 N1 109.5(4) . . ?
N2 C5 C1 123.6(4) . . ?
N1 C5 C1 126.9(4) . . ?
N3 C6 N1 115.3(4) . . ?
N3 C6 C7 124.9(4) . . ?
N1 C6 C7 119.7(4) . . ?
N4 C7 C8 122.8(5) . . ?
N4 C7 C6 113.8(4) . . ?
C8 C7 C6 123.4(5) . . ?
C7 C8 C9 118.3(6) . . ?
C7 C8 H8A 120.9 . . ?
C9 C8 H8A 120.9 . . ?
C10 C9 C8 119.9(5) . . ?
C10 C9 H9A 120.0 . . ?
C8 C9 H9A 120.0 . . ?
C9 C10 C11 118.8(5) . . ?
C9 C10 H10A 120.6 . . ?
C11 C10 H10A 120.6 . . ?
N4 C11 C10 122.7(6) . . ?
N4 C11 H11A 118.7 . . ?
C10 C11 H11A 118.7 . . ?
N5 C12 N6 107.3(4) . . ?
N5 C12 C4 128.4(4) . . ?
N6 C12 C4 124.2(4) . . ?
N7 C13 N5 114.4(4) . . ?
N7 C13 C14 125.4(4) . . ?
N5 C13 C14 120.3(4) . . ?
N8 C14 C18 123.1(5) . . ?
N8 C14 C13 112.6(4) . . ?
C18 C14 C13 124.3(4) . . ?
N8 C15 C16 124.6(5) . . ?
N8 C15 H15A 117.7 . . ?
C16 C15 H15A 117.7 . . ?
C17 C16 C15 117.6(5) . . ?
C17 C16 H16A 121.2 . . ?
C15 C16 H16A 121.2 . . ?
C18 C17 C16 119.2(5) . . ?
C18 C17 H17A 120.4 . . ?
C16 C17 H17A 120.4 . . ?
C17 C18 C14 119.5(5) . . ?
C17 C18 H18A 120.2 . . ?
C14 C18 H18A 120.2 . . ?
C5A N1A C6A 104.3(4) . . ?
C5A N1A Ni1 142.6(3) . . ?
C6A N1A Ni1 111.1(3) . . ?
C5A N2A N3A 112.7(4) . . ?
C5A N2A H2NA 127.1 . . ?
N3A N2A H2NA 120.0 . . ?
C6A N3A N2A 100.9(4) . . ?
C7A N4A C11A 116.1(5) . . ?
C7A N4A Ni1 116.3(3) . . ?
C11A N4A Ni1 127.6(4) . . ?
C12A N5A C13A 103.8(4) . . ?
C12A N5A Ni2 144.8(3) . . ?
C13A N5A Ni2 111.1(3) . . ?
C12A N6A N7A 111.3(4) . . ?
C12A N6A H6NA 122.9 . . ?
N7A N6A H6NA 125.3 . . ?
C13A N7A N6A 101.7(4) . . ?
C18A N8A C14A 118.6(4) . . ?
C18A N8A Ni2 126.7(3) . . ?
C14A N8A Ni2 114.6(3) . . ?
C5A C1A C2A 110.8(4) . . ?
C5A C1A C2A' 104.0(16) . . ?
C5A C1A H1AC 110.3 . . ?
C2A' C1A H1AC 111.3 . . ?
C5A C1A H1AD 111.3 . . ?
C2A' C1A H1AD 111.0 . . ?
H1AC C1A H1AD 109.0 . . ?
C5A C1A H1AA 109.3 . . ?
C2A C1A H1AA 109.2 . . ?
C5A C1A H1AB 109.6 . . ?
C2A C1A H1AB 109.6 . . ?
H1AA C1A H1AB 108.2 . . ?
C3A C2A C1A 111.2(4) . . ?
C3A C2A H2AA 109.4 . . ?
C1A C2A H2AA 109.4 . . ?
C3A C2A H2AB 109.4 . . ?
C1A C2A H2AB 109.4 . . ?
H2AA C2A H2AB 108.0 . . ?
C2A C3A C4A 111.1(4) . . ?
C2A C3A H3AA 109.4 . . ?
C4A C3A H3AA 109.4 . . ?
C2A C3A H3AB 109.4 . . ?
C4A C3A H3AB 109.4 . . ?
H3AA C3A H3AB 108.0 . . ?
C3A' C2A' C1A 113.3(19) . . ?
C3A' C2A' H2AC 108.9 . . ?
C1A C2A' H2AC 108.9 . . ?
C3A' C2A' H2AD 108.9 . . ?
C1A C2A' H2AD 108.9 . . ?
H2AC C2A' H2AD 107.7 . . ?
C2A' C3A' C4A 107.2(17) . . ?
C2A' C3A' H3AC 110.3 . . ?
C4A C3A' H3AC 110.3 . . ?
C2A' C3A' H3AD 110.3 . . ?
C4A C3A' H3AD 110.3 . . ?
H3AC C3A' H3AD 108.5 . . ?
C12A C4A C3A' 136.3(17) . . ?
C12A C4A C3A 108.8(4) . . ?
C12A C4A H4AC 102.3 . . ?
C3A' C4A H4AC 104.0 . . ?
C12A C4A H4AD 103.3 . . ?
C3A' C4A H4AD 102.6 . . ?
H4AC C4A H4AD 105.3 . . ?
C12A C4A H4AA 110.0 . . ?
C3A C4A H4AA 110.1 . . ?
C12A C4A H4AB 109.8 . . ?
C3A C4A H4AB 109.6 . . ?
H4AA C4A H4AB 108.7 . . ?
N2A C5A N1A 107.2(4) . . ?
N2A C5A C1A 123.8(4) . . ?
N1A C5A C1A 128.8(5) . . ?
N3A C6A N1A 114.9(4) . . ?
N3A C6A C7A 124.4(4) . . ?
N1A C6A C7A 120.7(4) . . ?
N4A C7A C8A 124.1(4) . . ?
N4A C7A C6A 111.8(4) . . ?
C8A C7A C6A 124.1(4) . . ?
C9A C8A C7A 117.9(5) . . ?
C9A C8A H8AA 121.0 . . ?
C7A C8A H8AA 121.0 . . ?
C10A C9A C8A 119.7(5) . . ?
C10A C9A H9AA 120.1 . . ?
C8A C9A H9AA 120.1 . . ?
C9A C10A C11A 118.3(5) . . ?
C9A C10A H10B 120.8 . . ?
C11A C10A H10B 120.8 . . ?
N4A C11A C10A 123.8(5) . . ?
N4A C11A H11B 118.1 . . ?
C10A C11A H11B 118.1 . . ?
N6A C12A N5A 108.2(4) . . ?
N6A C12A C4A 123.8(4) . . ?
N5A C12A C4A 127.9(4) . . ?
N7A C13A N5A 115.0(5) . . ?
N7A C13A C14A 125.2(4) . . ?
N5A C13A C14A 119.8(4) . . ?
N8A C14A C15A 121.6(5) . . ?
N8A C14A C13A 113.9(4) . . ?
C15A C14A C13A 124.2(4) . . ?
C14A C15A C16A 118.6(5) . . ?
C14A C15A H15B 120.7 . . ?
C16A C15A H15B 120.7 . . ?
C17A C16A C15A 119.4(5) . . ?
C17A C16A H16B 120.3 . . ?
C15A C16A H16B 120.3 . . ?
C16A C17A C18A 119.3(5) . . ?
C16A C17A H17B 120.3 . . ?
C18A C17A H17B 120.3 . . ?
N8A C18A C17A 122.2(5) . . ?
N8A C18A H18B 118.9 . . ?
C17A C18A H18B 118.9 . . ?
H5WB O5W H5WA 83.2 . . ?
O2N N1N O3N 120.7(4) . . ?
O2N N1N O1N 119.0(4) . . ?
O3N N1N O1N 120.3(4) . . ?
O4N N2N O5N 120.3(5) . . ?
O4N N2N O6N 120.3(4) . . ?
O5N N2N O6N 119.4(4) . . ?
O10N N4N O12N 121.1(4) . . ?
O10N N4N O11N 119.6(4) . . ?
O12N N4N O11N 119.3(4) . . ?
O7N N3N O9N 119.3(7) . . ?
O8N' N3N O9N' 120.4(9) . . ?
O7N N3N O8N 122.8(7) . . ?
O9N N3N O8N 116.5(7) . . ?
O8N' N3N O7N' 118.8(9) . . ?
O9N' N3N O7N' 117.4(10) . . ?
H13B O13N H13A 102(2) . . ?

_refine_diff_density_max         1.227
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.086




# start Validation Reply Form
_vrf_PLAT420_3a                  
;
RESPONSE: Hydrogen bond is missing due to removement of
 electron density of  disordered solvent by SQUEEZE procedure. 
;
####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 1907074'
loop_
_audit_author_name
_audit_author_address
I.Nemec
;Central European Institute of Technology
Czech Republic
;
_audit_update_record             
;
2019-05-09 deposited with the CCDC.	2019-06-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H114 Co4 N40 O45'
_chemical_formula_weight         2495.75

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'

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

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

_cell_length_a                   16.1207(19)
_cell_length_b                   42.286(5)
_cell_length_c                   15.3893(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10491(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    15224
_cell_measurement_theta_min      0.961
_cell_measurement_theta_max      28.931

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_F_000             5176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    0.732
_shelx_estimated_absorpt_T_min   0.844
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'SADABS v2004/1, Sheldrick, G.M., (2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            84325
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -54
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         0.963
_diffrn_reflns_theta_max         26.999
_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             11468
_reflns_number_gt                8656
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0566P)²+40.2605P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11468
_refine_ls_number_parameters     790
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0707
_refine_ls_wR_factor_ref         0.1707
_refine_ls_wR_factor_gt          0.1636
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.147
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.16957(4) 0.25004(2) -0.03330(4) 0.01326(14) Uani 1 1 d . . . . .
O1 O 0.2257(2) 0.22392(8) -0.1302(2) 0.0217(7) Uani 1 1 d D . . . .
O2 O 0.1175(2) 0.27927(8) -0.1297(2) 0.0208(7) Uani 1 1 d D . . . .
N11 N 0.0875(2) 0.26972(8) 0.0616(2) 0.0141(8) Uani 1 1 d . . . . .
N14 N 0.2435(2) 0.22757(9) 0.0658(2) 0.0154(8) Uani 1 1 d . . . . .
N18 N 0.0682(2) 0.21585(9) -0.0307(2) 0.0155(8) Uani 1 1 d . . . . .
N26 N 0.0029(2) 0.29169(9) 0.1527(2) 0.0173(8) Uani 1 1 d . . . . .
H26 H -0.0293 0.3054 0.1832 0.021 Uiso 1 1 d R U . . .
N27 N 0.2735(2) 0.28267(9) -0.0212(2) 0.0145(8) Uani 1 1 d . . . . .
N33 N 0.3239(2) 0.20331(9) 0.1565(2) 0.0186(8) Uani 1 1 d . . . . .
H33 H 0.3417 0.1869 0.1840 0.022 Uiso 1 1 d R U . . .
N35 N 0.3666(3) 0.23017(9) 0.1369(2) 0.0203(8) Uani 1 1 d . . . . .
N51 N -0.0340(2) 0.26382(9) 0.1314(2) 0.0168(8) Uani 1 1 d . . . . .
C28P C 0.0098(3) 0.22097(10) 0.0314(3) 0.0145(8) Uani 1 1 d . . . . .
C34P C 0.1906(3) 0.17566(10) 0.1281(3) 0.0166(9) Uani 1 1 d . . . . .
H34A H 0.2206 0.1554 0.1338 0.020 Uiso 1 1 calc R U . . .
H34B H 0.1541 0.1741 0.0765 0.020 Uiso 1 1 calc R U . . .
C38P C 0.1366(3) 0.18075(11) 0.2094(3) 0.0159(9) Uani 1 1 d . . . . .
H38A H 0.1057 0.2009 0.2030 0.019 Uiso 1 1 calc R U . . .
H38B H 0.0954 0.1634 0.2132 0.019 Uiso 1 1 calc R U . . .
C44P C 0.2521(3) 0.20170(11) 0.1142(3) 0.0173(9) Uani 1 1 d . . . . .
C45P C 0.3304(3) 0.27444(11) 0.0394(3) 0.0169(9) Uani 1 1 d . . . . .
C46P C 0.1863(3) 0.18183(11) 0.2943(3) 0.0183(10) Uani 1 1 d . . . . .
H46A H 0.2157 0.2024 0.2980 0.022 Uiso 1 1 calc R U . . .
H46B H 0.2287 0.1649 0.2932 0.022 Uiso 1 1 calc R U . . .
C47P C 0.1322(3) 0.17773(10) 0.3754(3) 0.0166(9) Uani 1 1 d . . . . .
H47A H 0.0992 0.1581 0.3696 0.020 Uiso 1 1 calc R U . . .
H47B H 0.1684 0.1754 0.4270 0.020 Uiso 1 1 calc R U . . .
C48P C 0.3155(2) 0.24415(10) 0.0824(3) 0.0131(9) Uani 1 1 d . . . . .
C52P C 0.0753(3) 0.29524(10) 0.1111(3) 0.0159(9) Uani 1 1 d . . . . .
C53P C 0.0042(3) 0.16567(11) -0.0582(3) 0.0205(10) Uani 1 1 d . . . . .
H53P H 0.0035 0.1465 -0.0902 0.025 Uiso 1 1 calc R U . . .
C54P C -0.0517(3) 0.19957(11) 0.0512(3) 0.0206(10) Uani 1 1 d . . . . .
H54P H -0.0916 0.2041 0.0948 0.025 Uiso 1 1 calc R U . . .
C58P C -0.0540(3) 0.17116(11) 0.0060(3) 0.0237(11) Uani 1 1 d . . . . .
H58P H -0.0949 0.1557 0.0190 0.028 Uiso 1 1 calc R U . . .
C62P C 0.0637(3) 0.18861(10) -0.0752(3) 0.0176(9) Uani 1 1 d . . . . .
H62P H 0.1028 0.1849 -0.1203 0.021 Uiso 1 1 calc R U . . .
C68P C 0.2854(3) 0.31017(11) -0.0631(3) 0.0200(10) Uani 1 1 d . . . . .
H68P H 0.2468 0.3161 -0.1069 0.024 Uiso 1 1 calc R U . . .
C69P C 0.0191(3) 0.25130(10) 0.0756(3) 0.0154(9) Uani 1 1 d . . . . .
C71P C 0.3507(3) 0.33033(11) -0.0459(3) 0.0203(10) Uani 1 1 d . . . . .
H71P H 0.3562 0.3497 -0.0766 0.024 Uiso 1 1 calc R U . . .
C72P C 0.3981(3) 0.29335(11) 0.0592(3) 0.0197(10) Uani 1 1 d . . . . .
H72P H 0.4374 0.2868 0.1016 0.024 Uiso 1 1 calc R U . . .
C79P C 0.4079(3) 0.32184(11) 0.0165(3) 0.0227(10) Uani 1 1 d . . . . .
H79P H 0.4532 0.3354 0.0300 0.027 Uiso 1 1 calc R U . . .
Co2 Co 0.51448(4) -0.00482(2) 0.73018(3) 0.01228(14) Uani 1 1 d . . . . .
O3 O 0.61498(19) 0.01613(8) 0.66673(19) 0.0164(7) Uani 1 1 d D . . . .
O4 O 0.59949(19) -0.02697(7) 0.8114(2) 0.0170(7) Uani 1 1 d D . . . .
N1P N 0.4215(2) 0.00867(8) 0.6405(2) 0.0147(8) Uani 1 1 d . . . . .
N6P N 0.4274(2) -0.02062(9) 0.8257(2) 0.0146(8) Uani 1 1 d . . . . .
N17 N 0.5082(2) 0.03547(8) 0.8162(2) 0.0150(8) Uani 1 1 d . . . . .
N21 N 0.3332(2) 0.02648(9) 0.5459(2) 0.0156(8) Uani 1 1 d . . . . .
H21 H 0.2970 0.0401 0.5208 0.019 Uiso 1 1 d R U . . .
N25 N 0.3482(2) -0.03863(9) 0.9289(2) 0.0176(8) Uani 1 1 d . . . . .
H25 H 0.3176 -0.0513 0.9636 0.021 Uiso 1 1 d R U . . .
N32 N 0.3727(3) -0.00921(9) 0.9561(2) 0.0203(8) Uani 1 1 d . . . . .
N36 N 0.3639(2) -0.00055(9) 0.5096(2) 0.0152(8) Uani 1 1 d . . . . .
N39 N 0.5197(2) -0.04295(8) 0.6330(2) 0.0141(7) Uani 1 1 d . . . . .
C1P C 0.5048(3) 0.08065(12) 0.9465(3) 0.0250(11) Uani 1 1 d . . . . .
H1P H 0.5042 0.0960 0.9916 0.030 Uiso 1 1 calc R U . . .
C30P C 0.3420(3) 0.05815(10) 0.6819(3) 0.0147(9) Uani 1 1 d . . . . .
H30A H 0.3415 0.0781 0.6484 0.018 Uiso 1 1 calc R U . . .
H30B H 0.3824 0.0604 0.7300 0.018 Uiso 1 1 calc R U . . .
C37P C 0.4681(3) -0.03928(10) 0.5638(3) 0.0127(8) Uani 1 1 d . . . . .
C40P C 0.2238(3) 0.07916(10) 0.7747(3) 0.0157(9) Uani 1 1 d . . . . .
H40A H 0.2296 0.0991 0.7416 0.019 Uiso 1 1 calc R U . . .
H40B H 0.2588 0.0809 0.8274 0.019 Uiso 1 1 calc R U . . .
C42P C 0.5174(3) -0.08666(10) 0.4966(3) 0.0181(9) Uani 1 1 d . . . . .
H42P H 0.5161 -0.1018 0.4510 0.022 Uiso 1 1 calc R U . . .
C49P C 0.3675(3) 0.03155(10) 0.6241(3) 0.0123(8) Uani 1 1 d . . . . .
C55P C 0.2555(3) 0.05178(11) 0.7190(3) 0.0175(9) Uani 1 1 d . . . . .
H55A H 0.2573 0.0323 0.7547 0.021 Uiso 1 1 calc R U . . .
H55B H 0.2163 0.0481 0.6705 0.021 Uiso 1 1 calc R U . . .
C56P C 0.3816(3) -0.04544(10) 0.8509(3) 0.0138(9) Uani 1 1 d . . . . .
C59P C 0.4652(3) -0.06052(10) 0.4951(3) 0.0160(9) Uani 1 1 d . . . . .
H59P H 0.4281 -0.0572 0.4479 0.019 Uiso 1 1 calc R U . . .
C60P C 0.4168(3) -0.01088(10) 0.5687(3) 0.0134(9) Uani 1 1 d . . . . .
C61P C 0.4203(3) 0.00046(11) 0.8922(3) 0.0167(9) Uani 1 1 d . . . . .
C63P C 0.5716(3) -0.09017(11) 0.5663(3) 0.0179(9) Uani 1 1 d . . . . .
H63P H 0.6087 -0.1076 0.5687 0.021 Uiso 1 1 calc R U . . .
C65P C 0.1328(3) 0.07519(10) 0.8024(3) 0.0144(9) Uani 1 1 d . . . . .
H65A H 0.1166 0.0933 0.8393 0.017 Uiso 1 1 calc R U . . .
H65B H 0.0972 0.0754 0.7500 0.017 Uiso 1 1 calc R U . . .
C66P C 0.5494(3) 0.06272(11) 0.8075(3) 0.0163(9) Uani 1 1 d . . . . .
H66P H 0.5793 0.0664 0.7553 0.020 Uiso 1 1 calc R U . . .
C70P C 0.5708(3) -0.06786(10) 0.6321(3) 0.0168(9) Uani 1 1 d . . . . .
H70P H 0.6084 -0.0704 0.6791 0.020 Uiso 1 1 calc R U . . .
C73P C 0.4638(3) 0.03087(10) 0.8891(3) 0.0145(9) Uani 1 1 d . . . . .
C76P C 0.5503(3) 0.08584(11) 0.8718(3) 0.0220(10) Uani 1 1 d . . . . .
H76P H 0.5814 0.1047 0.8645 0.026 Uiso 1 1 calc R U . . .
C78P C 0.4602(3) 0.05295(12) 0.9551(3) 0.0223(10) Uani 1 1 d . . . . .
H78P H 0.4277 0.0492 1.0054 0.027 Uiso 1 1 calc R U . . .
O1S O 0.3128(2) 0.11716(8) 0.0566(2) 0.0214(7) Uani 1 1 d . . . . .
O2S O 0.2640(2) 0.06991(8) 0.0377(2) 0.0261(8) Uani 1 1 d . . . . .
O3S O 0.1995(2) 0.11043(8) -0.0179(2) 0.0241(8) Uani 1 1 d . . . . .
N1S N 0.2588(2) 0.09909(9) 0.0252(2) 0.0184(8) Uani 1 1 d . . . . .
O4S O 0.3790(2) 0.14810(8) 0.2393(2) 0.0239(7) Uani 1 1 d . . . . .
O5S O 0.4788(2) 0.18060(7) 0.2688(2) 0.0235(7) Uani 1 1 d . . . . .
O6S O 0.5009(2) 0.12994(8) 0.2708(2) 0.0234(7) Uani 1 1 d . . . . .
N2S N 0.4538(3) 0.15314(9) 0.2602(2) 0.0184(8) Uani 1 1 d . . . . .
O7S O 0.4111(2) 0.17164(8) 0.7586(2) 0.0287(8) Uani 1 1 d . . . . .
O8S O 0.4707(2) 0.13193(9) 0.6949(2) 0.0276(8) Uani 1 1 d . . . . .
O9S O 0.3805(2) 0.12397(9) 0.7970(3) 0.0374(10) Uani 1 1 d . . . . .
N3S N 0.4206(2) 0.14210(10) 0.7499(3) 0.0220(9) Uani 1 1 d . . . . .
O10S O 0.2371(2) 0.06571(8) 0.4447(2) 0.0247(8) Uani 1 1 d . . . . .
O11S O 0.2173(3) 0.09760(10) 0.5537(2) 0.0394(10) Uani 1 1 d . . . . .
O12S O 0.2006(3) 0.11414(10) 0.4234(3) 0.0520(13) Uani 1 1 d . . . . .
N4S N 0.2188(3) 0.09251(10) 0.4742(3) 0.0243(9) Uani 1 1 d . . . . .
O1W O 0.5126(3) 0.2500 0.2500 0.0169(9) Uani 1 2 d DS T P . .
O2W O 0.3334(3) 0.2500 0.7500 0.0208(10) Uani 1 2 d DS T P . .
O3W O 0.7579(3) 0.16262(9) 0.1167(3) 0.0357(10) Uani 1 1 d D . . . .
O4W O 0.1061(2) 0.15455(8) 0.5946(2) 0.0305(9) Uani 1 1 d D . . . .
O5W O 0.4395(2) 0.08627(8) 0.1444(2) 0.0203(7) Uani 1 1 d D . . . .
O6W O 0.2500 0.0000 0.0887(3) 0.0169(9) Uani 1 2 d DS T P . .
O7W O 0.2375(2) 0.03774(8) 0.2309(2) 0.0179(7) Uani 1 1 d D . . . .
O8W O 0.2377(2) 0.10174(9) 0.2478(2) 0.0301(8) Uani 1 1 d D . . . .
H1A H 0.239(4) 0.2046(5) -0.126(4) 0.045 Uiso 1 1 d D U . . .
H1B H 0.256(3) 0.2313(11) -0.171(3) 0.045 Uiso 1 1 d D U . . .
H2A H 0.106(4) 0.2988(4) -0.125(4) 0.045 Uiso 1 1 d D U . . .
H2B H 0.083(3) 0.2717(11) -0.165(3) 0.045 Uiso 1 1 d D U . . .
H3A H 0.658(2) 0.0218(14) 0.695(3) 0.045 Uiso 1 1 d D U . . .
H3B H 0.632(3) 0.0117(14) 0.6161(16) 0.045 Uiso 1 1 d D U . . .
H4A H 0.586(3) -0.0458(5) 0.825(4) 0.045 Uiso 1 1 d D U . . .
H4B H 0.6488(16) -0.0283(12) 0.792(4) 0.045 Uiso 1 1 d D U . . .
H1W H 0.488(4) 0.2346(10) 0.226(4) 0.045 Uiso 1 1 d D U . . .
H2W H 0.363(3) 0.2420(14) 0.711(3) 0.045 Uiso 1 1 d D U . . .
H3WA H 0.740(3) 0.1483(9) 0.083(3) 0.045 Uiso 1 1 d D U . . .
H3WB H 0.793(3) 0.1534(11) 0.149(3) 0.045 Uiso 1 1 d D U . . .
H4WA H 0.131(4) 0.1393(9) 0.570(3) 0.045 Uiso 1 1 d D U . . .
H4WB H 0.088(4) 0.1469(11) 0.642(2) 0.045 Uiso 1 1 d D U . . .
H5WA H 0.399(3) 0.0943(12) 0.117(3) 0.045 Uiso 1 1 d D U . . .
H5WB H 0.455(3) 0.1000(10) 0.181(3) 0.045 Uiso 1 1 d D U . . .
H6W H 0.288(3) 0.0026(16) 0.051(3) 0.045 Uiso 1 1 d D U . . .
H7WA H 0.236(4) 0.0578(3) 0.229(3) 0.045 Uiso 1 1 d D U . . .
H7WB H 0.231(4) 0.0313(11) 0.1791(14) 0.045 Uiso 1 1 d D U . . .
H8WA H 0.226(3) 0.1050(14) 0.3008(13) 0.045 Uiso 1 1 d D U . . .
H8WB H 0.283(2) 0.1112(14) 0.239(3) 0.045 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O1 2.064(3) . ?
Co1 O2 2.105(3) . ?
Co1 N11 2.139(4) . ?
Co1 N14 2.156(4) . ?
Co1 N27 2.178(4) . ?
Co1 N18 2.182(4) . ?
O1 H1A 0.849(10) . ?
O1 H1B 0.850(10) . ?
O2 H2A 0.849(10) . ?
O2 H2B 0.847(10) . ?
N11 C52P 1.335(6) . ?
N11 C69P 1.367(6) . ?
N14 C44P 1.331(6) . ?
N14 C48P 1.379(6) . ?
N18 C62P 1.342(6) . ?
N18 C28P 1.359(5) . ?
N26 C52P 1.339(6) . ?
N26 N51 1.360(5) . ?
N26 H26 0.9077 . ?
N27 C68P 1.343(6) . ?
N27 C45P 1.354(6) . ?
N33 C44P 1.329(6) . ?
N33 N35 1.362(5) . ?
N33 H33 0.8613 . ?
N35 C48P 1.316(6) . ?
N51 C69P 1.323(6) . ?
C28P C54P 1.377(6) . ?
C28P C69P 1.460(6) . ?
C34P C44P 1.498(6) . ?
C34P C38P 1.540(6) . ?
C34P H34A 0.9900 . ?
C34P H34B 0.9900 . ?
C38P C46P 1.534(6) . ?
C38P H38A 0.9900 . ?
C38P H38B 0.9900 . ?
C45P C72P 1.387(6) . ?
C45P C48P 1.462(6) . ?
C46P C47P 1.532(6) . ?
C46P H46A 0.9900 . ?
C46P H46B 0.9900 . ?
C47P C52P 1.481(6) 3 ?
C47P H47A 0.9900 . ?
C47P H47B 0.9900 . ?
C52P C47P 1.481(6) 3 ?
C53P C58P 1.381(7) . ?
C53P C62P 1.389(6) . ?
C53P H53P 0.9500 . ?
C54P C58P 1.388(7) . ?
C54P H54P 0.9500 . ?
C58P H58P 0.9500 . ?
C62P H62P 0.9500 . ?
C68P C71P 1.381(7) . ?
C68P H68P 0.9500 . ?
C71P C79P 1.378(7) . ?
C71P H71P 0.9500 . ?
C72P C79P 1.381(7) . ?
C72P H72P 0.9500 . ?
C79P H79P 0.9500 . ?
Co2 O4 2.078(3) . ?
Co2 O3 2.089(3) . ?
Co2 N1P 2.116(4) . ?
Co2 N6P 2.140(4) . ?
Co2 N17 2.160(4) . ?
Co2 N39 2.201(4) . ?
O3 H3A 0.848(10) . ?
O3 H3B 0.848(10) . ?
O4 H4A 0.850(10) . ?
O4 H4B 0.850(10) . ?
N1P C49P 1.326(6) . ?
N1P C60P 1.382(5) . ?
N6P C56P 1.340(6) . ?
N6P C61P 1.362(5) . ?
N17 C66P 1.337(6) . ?
N17 C73P 1.344(6) . ?
N21 C49P 1.342(6) . ?
N21 N36 1.365(5) . ?
N21 H21 0.9066 . ?
N25 C56P 1.346(5) . ?
N25 N32 1.371(5) . ?
N25 H25 0.9026 . ?
N32 C61P 1.313(6) . ?
N36 C60P 1.321(6) . ?
N39 C70P 1.337(6) . ?
N39 C37P 1.361(6) . ?
C1P C76P 1.382(7) . ?
C1P C78P 1.380(7) . ?
C1P H1P 0.9500 . ?
C30P C49P 1.491(6) . ?
C30P C55P 1.530(6) . ?
C30P H30A 0.9900 . ?
C30P H30B 0.9900 . ?
C37P C59P 1.388(6) . ?
C37P C60P 1.460(6) . ?
C40P C55P 1.529(6) . ?
C40P C65P 1.537(6) . ?
C40P H40A 0.9900 . ?
C40P H40B 0.9900 . ?
C42P C59P 1.390(6) . ?
C42P C63P 1.393(6) . ?
C42P H42P 0.9500 . ?
C55P H55A 0.9900 . ?
C55P H55B 0.9900 . ?
C56P C65P 1.482(6) 2 ?
C59P H59P 0.9500 . ?
C61P C73P 1.465(6) . ?
C63P C70P 1.383(6) . ?
C63P H63P 0.9500 . ?
C65P C56P 1.482(6) 2 ?
C65P H65A 0.9900 . ?
C65P H65B 0.9900 . ?
C66P C76P 1.391(6) . ?
C66P H66P 0.9500 . ?
C70P H70P 0.9500 . ?
C73P C78P 1.381(6) . ?
C76P H76P 0.9500 . ?
C78P H78P 0.9500 . ?
O1S N1S 1.254(5) . ?
O2S N1S 1.251(5) . ?
O3S N1S 1.259(5) . ?
O4S N2S 1.266(5) . ?
O5S N2S 1.236(5) . ?
O6S N2S 1.251(5) . ?
O7S N3S 1.265(5) . ?
O8S N3S 1.247(5) . ?
O9S N3S 1.237(5) . ?
O10S N4S 1.256(5) . ?
O11S N4S 1.244(5) . ?
O12S N4S 1.238(5) . ?
O1W H1W 0.84(2) . ?
O2W H2W 0.84(2) . ?
O3W H3WA 0.850(10) . ?
O3W H3WB 0.849(10) . ?
O4W H4WA 0.849(10) . ?
O4W H4WB 0.850(10) . ?
O5W H5WA 0.849(10) . ?
O5W H5WB 0.848(10) . ?
O6W H6W 0.851(10) . ?
O7W H7WA 0.849(10) . ?
O7W H7WB 0.848(10) . ?
O8W H8WA 0.848(10) . ?
O8W H8WB 0.849(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Co1 O2 88.84(13) . . ?
O1 Co1 N11 166.48(14) . . ?
O2 Co1 N11 90.38(14) . . ?
O1 Co1 N14 91.88(14) . . ?
O2 Co1 N14 167.78(14) . . ?
N11 Co1 N14 91.73(14) . . ?
O1 Co1 N27 93.65(14) . . ?
O2 Co1 N27 89.70(13) . . ?
N11 Co1 N27 99.83(14) . . ?
N14 Co1 N27 78.08(14) . . ?
O1 Co1 N18 89.23(14) . . ?
O2 Co1 N18 95.94(13) . . ?
N11 Co1 N18 77.43(14) . . ?
N14 Co1 N18 96.27(14) . . ?
N27 Co1 N18 173.73(14) . . ?
Co1 O1 H1A 124(4) . . ?
Co1 O1 H1B 126(4) . . ?
H1A O1 H1B 106(2) . . ?
Co1 O2 H2A 126(4) . . ?
Co1 O2 H2B 120(4) . . ?
H2A O2 H2B 106(2) . . ?
C52P N11 C69P 104.6(4) . . ?
C52P N11 Co1 142.7(3) . . ?
C69P N11 Co1 112.6(3) . . ?
C44P N14 C48P 103.1(4) . . ?
C44P N14 Co1 144.7(3) . . ?
C48P N14 Co1 111.9(3) . . ?
C62P N18 C28P 117.3(4) . . ?
C62P N18 Co1 126.9(3) . . ?
C28P N18 Co1 115.2(3) . . ?
C52P N26 N51 111.2(4) . . ?
C52P N26 H26 132.4 . . ?
N51 N26 H26 115.2 . . ?
C68P N27 C45P 117.2(4) . . ?
C68P N27 Co1 128.1(3) . . ?
C45P N27 Co1 114.7(3) . . ?
C44P N33 N35 112.0(4) . . ?
C44P N33 H33 119.3 . . ?
N35 N33 H33 127.7 . . ?
C48P N35 N33 101.5(4) . . ?
C69P N51 N26 102.7(4) . . ?
N18 C28P C54P 123.3(4) . . ?
N18 C28P C69P 113.4(4) . . ?
C54P C28P C69P 123.3(4) . . ?
C44P C34P C38P 112.8(4) . . ?
C44P C34P H34A 109.0 . . ?
C38P C34P H34A 109.0 . . ?
C44P C34P H34B 109.0 . . ?
C38P C34P H34B 109.0 . . ?
H34A C34P H34B 107.8 . . ?
C46P C38P C34P 113.6(4) . . ?
C46P C38P H38A 108.8 . . ?
C34P C38P H38A 108.8 . . ?
C46P C38P H38B 108.8 . . ?
C34P C38P H38B 108.8 . . ?
H38A C38P H38B 107.7 . . ?
N33 C44P N14 108.8(4) . . ?
N33 C44P C34P 123.0(4) . . ?
N14 C44P C34P 128.0(4) . . ?
N27 C45P C72P 122.5(4) . . ?
N27 C45P C48P 115.2(4) . . ?
C72P C45P C48P 122.3(4) . . ?
C38P C46P C47P 113.1(4) . . ?
C38P C46P H46A 109.0 . . ?
C47P C46P H46A 109.0 . . ?
C38P C46P H46B 109.0 . . ?
C47P C46P H46B 109.0 . . ?
H46A C46P H46B 107.8 . . ?
C52P C47P C46P 112.3(4) 3 . ?
C52P C47P H47A 109.1 3 . ?
C46P C47P H47A 109.1 . . ?
C52P C47P H47B 109.1 3 . ?
C46P C47P H47B 109.1 . . ?
H47A C47P H47B 107.9 . . ?
N35 C48P N14 114.6(4) . . ?
N35 C48P C45P 125.4(4) . . ?
N14 C48P C45P 120.0(4) . . ?
N11 C52P N26 108.1(4) . . ?
N11 C52P C47P 127.8(4) . 3 ?
N26 C52P C47P 124.0(4) . 3 ?
C58P C53P C62P 119.1(4) . . ?
C58P C53P H53P 120.4 . . ?
C62P C53P H53P 120.4 . . ?
C28P C54P C58P 118.5(4) . . ?
C28P C54P H54P 120.8 . . ?
C58P C54P H54P 120.8 . . ?
C53P C58P C54P 119.0(4) . . ?
C53P C58P H58P 120.5 . . ?
C54P C58P H58P 120.5 . . ?
N18 C62P C53P 122.7(4) . . ?
N18 C62P H62P 118.7 . . ?
C53P C62P H62P 118.7 . . ?
N27 C68P C71P 123.4(4) . . ?
N27 C68P H68P 118.3 . . ?
C71P C68P H68P 118.3 . . ?
N51 C69P N11 113.3(4) . . ?
N51 C69P C28P 126.0(4) . . ?
N11 C69P C28P 120.7(4) . . ?
C79P C71P C68P 118.9(4) . . ?
C79P C71P H71P 120.6 . . ?
C68P C71P H71P 120.6 . . ?
C79P C72P C45P 119.2(4) . . ?
C79P C72P H72P 120.4 . . ?
C45P C72P H72P 120.4 . . ?
C72P C79P C71P 118.9(4) . . ?
C72P C79P H79P 120.6 . . ?
C71P C79P H79P 120.6 . . ?
O4 Co2 O3 87.74(13) . . ?
O4 Co2 N1P 168.84(13) . . ?
O3 Co2 N1P 97.49(13) . . ?
O4 Co2 N6P 83.02(13) . . ?
O3 Co2 N6P 164.24(13) . . ?
N1P Co2 N6P 93.89(14) . . ?
O4 Co2 N17 91.04(13) . . ?
O3 Co2 N17 89.34(13) . . ?
N1P Co2 N17 98.84(14) . . ?
N6P Co2 N17 78.13(14) . . ?
O4 Co2 N39 93.04(13) . . ?
O3 Co2 N39 87.90(13) . . ?
N1P Co2 N39 77.38(14) . . ?
N6P Co2 N39 105.27(14) . . ?
N17 Co2 N39 174.98(13) . . ?
Co2 O3 H3A 120(4) . . ?
Co2 O3 H3B 126(4) . . ?
H3A O3 H3B 106(2) . . ?
Co2 O4 H4A 114(4) . . ?
Co2 O4 H4B 116(4) . . ?
H4A O4 H4B 105(2) . . ?
C49P N1P C60P 104.4(4) . . ?
C49P N1P Co2 141.8(3) . . ?
C60P N1P Co2 113.5(3) . . ?
C56P N6P C61P 104.4(4) . . ?
C56P N6P Co2 143.6(3) . . ?
C61P N6P Co2 111.5(3) . . ?
C66P N17 C73P 118.2(4) . . ?
C66P N17 Co2 126.5(3) . . ?
C73P N17 Co2 115.0(3) . . ?
C49P N21 N36 110.6(4) . . ?
C49P N21 H21 123.1 . . ?
N36 N21 H21 126.2 . . ?
C56P N25 N32 110.5(4) . . ?
C56P N25 H25 128.3 . . ?
N32 N25 H25 121.0 . . ?
C61P N32 N25 102.8(4) . . ?
C60P N36 N21 103.2(3) . . ?
C70P N39 C37P 117.3(4) . . ?
C70P N39 Co2 127.5(3) . . ?
C37P N39 Co2 115.1(3) . . ?
C76P C1P C78P 119.4(4) . . ?
C76P C1P H1P 120.3 . . ?
C78P C1P H1P 120.3 . . ?
C49P C30P C55P 109.9(4) . . ?
C49P C30P H30A 109.7 . . ?
C55P C30P H30A 109.7 . . ?
C49P C30P H30B 109.7 . . ?
C55P C30P H30B 109.7 . . ?
H30A C30P H30B 108.2 . . ?
N39 C37P C59P 122.9(4) . . ?
N39 C37P C60P 113.6(4) . . ?
C59P C37P C60P 123.6(4) . . ?
C55P C40P C65P 113.1(4) . . ?
C55P C40P H40A 109.0 . . ?
C65P C40P H40A 109.0 . . ?
C55P C40P H40B 109.0 . . ?
C65P C40P H40B 109.0 . . ?
H40A C40P H40B 107.8 . . ?
C59P C42P C63P 118.5(4) . . ?
C59P C42P H42P 120.7 . . ?
C63P C42P H42P 120.7 . . ?
N1P C49P N21 108.9(4) . . ?
N1P C49P C30P 128.2(4) . . ?
N21 C49P C30P 122.8(4) . . ?
C30P C55P C40P 112.4(4) . . ?
C30P C55P H55A 109.1 . . ?
C40P C55P H55A 109.1 . . ?
C30P C55P H55B 109.1 . . ?
C40P C55P H55B 109.1 . . ?
H55A C55P H55B 107.9 . . ?
N6P C56P N25 108.1(4) . . ?
N6P C56P C65P 127.3(4) . 2 ?
N25 C56P C65P 124.6(4) . 2 ?
C37P C59P C42P 118.8(4) . . ?
C37P C59P H59P 120.6 . . ?
C42P C59P H59P 120.6 . . ?
N36 C60P N1P 112.8(4) . . ?
N36 C60P C37P 127.0(4) . . ?
N1P C60P C37P 120.2(4) . . ?
N32 C61P N6P 114.1(4) . . ?
N32 C61P C73P 125.3(4) . . ?
N6P C61P C73P 120.6(4) . . ?
C70P C63P C42P 119.0(4) . . ?
C70P C63P H63P 120.5 . . ?
C42P C63P H63P 120.5 . . ?
C56P C65P C40P 112.5(4) 2 . ?
C56P C65P H65A 109.1 2 . ?
C40P C65P H65A 109.1 . . ?
C56P C65P H65B 109.1 2 . ?
C40P C65P H65B 109.1 . . ?
H65A C65P H65B 107.8 . . ?
N17 C66P C76P 122.7(4) . . ?
N17 C66P H66P 118.7 . . ?
C76P C66P H66P 118.7 . . ?
N39 C70P C63P 123.4(4) . . ?
N39 C70P H70P 118.3 . . ?
C63P C70P H70P 118.3 . . ?
N17 C73P C78P 122.5(4) . . ?
N17 C73P C61P 114.2(4) . . ?
C78P C73P C61P 123.3(4) . . ?
C1P C76P C66P 118.4(4) . . ?
C1P C76P H76P 120.8 . . ?
C66P C76P H76P 120.8 . . ?
C73P C78P C1P 118.8(4) . . ?
C73P C78P H78P 120.6 . . ?
C1P C78P H78P 120.6 . . ?
O1S N1S O2S 119.7(4) . . ?
O1S N1S O3S 119.8(4) . . ?
O2S N1S O3S 120.5(4) . . ?
O5S N2S O6S 121.7(4) . . ?
O5S N2S O4S 119.7(4) . . ?
O6S N2S O4S 118.7(4) . . ?
O9S N3S O8S 121.5(4) . . ?
O9S N3S O7S 119.1(4) . . ?
O8S N3S O7S 119.4(4) . . ?
O12S N4S O11S 119.3(4) . . ?
O12S N4S O10S 119.6(4) . . ?
O11S N4S O10S 121.1(4) . . ?
H3WA O3W H3WB 105(2) . . ?
H4WA O4W H4WB 104(2) . . ?
H5WA O5W H5WB 106(2) . . ?
H7WA O7W H7WB 106(2) . . ?
H8WA O8W H8WB 106(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C44P N33 N35 C48P 0.9(5) . . . . ?
C52P N26 N51 C69P -0.3(5) . . . . ?
C62P N18 C28P C54P 1.2(6) . . . . ?
Co1 N18 C28P C54P -170.2(4) . . . . ?
C62P N18 C28P C69P -179.4(4) . . . . ?
Co1 N18 C28P C69P 9.3(5) . . . . ?
C44P C34P C38P C46P -61.6(5) . . . . ?
N35 N33 C44P N14 -0.9(5) . . . . ?
N35 N33 C44P C34P -176.0(4) . . . . ?
C48P N14 C44P N33 0.5(5) . . . . ?
Co1 N14 C44P N33 171.7(4) . . . . ?
C48P N14 C44P C34P 175.2(4) . . . . ?
Co1 N14 C44P C34P -13.5(8) . . . . ?
C38P C34P C44P N33 80.7(5) . . . . ?
C38P C34P C44P N14 -93.3(5) . . . . ?
C68P N27 C45P C72P 0.7(6) . . . . ?
Co1 N27 C45P C72P -176.3(3) . . . . ?
C68P N27 C45P C48P -179.2(4) . . . . ?
Co1 N27 C45P C48P 3.8(5) . . . . ?
C34P C38P C46P C47P -164.2(4) . . . . ?
C38P C46P C47P C52P -67.2(5) . . . 3 ?
N33 N35 C48P N14 -0.6(5) . . . . ?
N33 N35 C48P C45P -179.5(4) . . . . ?
C44P N14 C48P N35 0.1(5) . . . . ?
Co1 N14 C48P N35 -174.4(3) . . . . ?
C44P N14 C48P C45P 179.1(4) . . . . ?
Co1 N14 C48P C45P 4.5(5) . . . . ?
N27 C45P C48P N35 173.1(4) . . . . ?
C72P C45P C48P N35 -6.8(7) . . . . ?
N27 C45P C48P N14 -5.7(6) . . . . ?
C72P C45P C48P N14 174.4(4) . . . . ?
C69P N11 C52P N26 0.5(5) . . . . ?
Co1 N11 C52P N26 175.2(4) . . . . ?
C69P N11 C52P C47P 176.5(4) . . . 3 ?
Co1 N11 C52P C47P -8.7(8) . . . 3 ?
N51 N26 C52P N11 -0.1(5) . . . . ?
N51 N26 C52P C47P -176.4(4) . . . 3 ?
N18 C28P C54P C58P 0.5(7) . . . . ?
C69P C28P C54P C58P -178.9(4) . . . . ?
C62P C53P C58P C54P 0.5(7) . . . . ?
C28P C54P C58P C53P -1.3(7) . . . . ?
C28P N18 C62P C53P -2.1(6) . . . . ?
Co1 N18 C62P C53P 168.2(3) . . . . ?
C58P C53P C62P N18 1.3(7) . . . . ?
C45P N27 C68P C71P -1.6(7) . . . . ?
Co1 N27 C68P C71P 175.0(3) . . . . ?
N26 N51 C69P N11 0.6(5) . . . . ?
N26 N51 C69P C28P -179.7(4) . . . . ?
C52P N11 C69P N51 -0.7(5) . . . . ?
Co1 N11 C69P N51 -177.2(3) . . . . ?
C52P N11 C69P C28P 179.6(4) . . . . ?
Co1 N11 C69P C28P 3.0(5) . . . . ?
N18 C28P C69P N51 171.9(4) . . . . ?
C54P C28P C69P N51 -8.6(7) . . . . ?
N18 C28P C69P N11 -8.3(6) . . . . ?
C54P C28P C69P N11 171.1(4) . . . . ?
N27 C68P C71P C79P 1.0(7) . . . . ?
N27 C45P C72P C79P 0.8(7) . . . . ?
C48P C45P C72P C79P -179.4(4) . . . . ?
C45P C72P C79P C71P -1.3(7) . . . . ?
C68P C71P C79P C72P 0.5(7) . . . . ?
C56P N25 N32 C61P 0.1(5) . . . . ?
C49P N21 N36 C60P -0.2(5) . . . . ?
C70P N39 C37P C59P 1.8(6) . . . . ?
Co2 N39 C37P C59P 177.9(3) . . . . ?
C70P N39 C37P C60P -177.8(4) . . . . ?
Co2 N39 C37P C60P -1.7(4) . . . . ?
C60P N1P C49P N21 -1.1(5) . . . . ?
Co2 N1P C49P N21 171.8(3) . . . . ?
C60P N1P C49P C30P 175.3(4) . . . . ?
Co2 N1P C49P C30P -11.7(8) . . . . ?
N36 N21 C49P N1P 0.9(5) . . . . ?
N36 N21 C49P C30P -175.8(4) . . . . ?
C55P C30P C49P N1P -104.7(5) . . . . ?
C55P C30P C49P N21 71.3(5) . . . . ?
C49P C30P C55P C40P -176.7(4) . . . . ?
C65P C40P C55P C30P 172.3(4) . . . . ?
C61P N6P C56P N25 0.9(5) . . . . ?
Co2 N6P C56P N25 171.4(4) . . . . ?
C61P N6P C56P C65P 179.5(4) . . . 2 ?
Co2 N6P C56P C65P -10.0(8) . . . 2 ?
N32 N25 C56P N6P -0.7(5) . . . . ?
N32 N25 C56P C65P -179.3(4) . . . 2 ?
N39 C37P C59P C42P -0.3(6) . . . . ?
C60P C37P C59P C42P 179.3(4) . . . . ?
C63P C42P C59P C37P -1.1(6) . . . . ?
N21 N36 C60P N1P -0.6(5) . . . . ?
N21 N36 C60P C37P -179.8(4) . . . . ?
C49P N1P C60P N36 1.1(5) . . . . ?
Co2 N1P C60P N36 -174.1(3) . . . . ?
C49P N1P C60P C37P -179.6(4) . . . . ?
Co2 N1P C60P C37P 5.2(5) . . . . ?
N39 C37P C60P N36 176.9(4) . . . . ?
C59P C37P C60P N36 -2.7(7) . . . . ?
N39 C37P C60P N1P -2.3(6) . . . . ?
C59P C37P C60P N1P 178.1(4) . . . . ?
N25 N32 C61P N6P 0.5(5) . . . . ?
N25 N32 C61P C73P -179.3(4) . . . . ?
C56P N6P C61P N32 -0.9(5) . . . . ?
Co2 N6P C61P N32 -174.8(3) . . . . ?
C56P N6P C61P C73P 178.9(4) . . . . ?
Co2 N6P C61P C73P 4.9(5) . . . . ?
C59P C42P C63P C70P 0.9(7) . . . . ?
C55P C40P C65P C56P 57.4(5) . . . 2 ?
C73P N17 C66P C76P 2.2(7) . . . . ?
Co2 N17 C66P C76P -171.2(3) . . . . ?
C37P N39 C70P C63P -2.0(6) . . . . ?
Co2 N39 C70P C63P -177.6(3) . . . . ?
C42P C63P C70P N39 0.6(7) . . . . ?
C66P N17 C73P C78P -0.8(6) . . . . ?
Co2 N17 C73P C78P 173.4(4) . . . . ?
C66P N17 C73P C61P 179.5(4) . . . . ?
Co2 N17 C73P C61P -6.4(5) . . . . ?
N32 C61P C73P N17 -179.3(4) . . . . ?
N6P C61P C73P N17 1.0(6) . . . . ?
N32 C61P C73P C78P 0.9(7) . . . . ?
N6P C61P C73P C78P -178.8(4) . . . . ?
C78P C1P C76P C66P 0.0(8) . . . . ?
N17 C66P C76P C1P -1.8(7) . . . . ?
N17 C73P C78P C1P -1.0(7) . . . . ?
C61P C73P C78P C1P 178.8(4) . . . . ?
C76P C1P C78P C73P 1.3(8) . . . . ?

_refine_diff_density_max         0.805
_refine_diff_density_min         -1.077
_refine_diff_density_rms         0.105

