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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_exp_729
_audit_block_doi                 10.5517/ccdc.csd.cc2kq33j
_database_code_depnum_ccdc_archive 'CCDC 2374727'
loop_
_audit_author_name
_audit_author_address
'Akio Mishima'
;Fukuoka University
Japan
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_audit_creation_date             2024-07-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30 H22 Fe N6, C6 H Cl2 O4, C3 Cl0.989 O2, H2 O, C3 H Cl O2'
_chemical_formula_sum            'C42 H26 Cl4 Fe N6 O9'
_chemical_formula_weight         956.16
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N10O20Cl2Fe1
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'
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'

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

_cell_length_a                   8.9753(2)
_cell_length_b                   10.8907(2)
_cell_length_c                   20.9485(4)
_cell_angle_alpha                85.702(2)
_cell_angle_beta                 80.124(2)
_cell_angle_gamma                85.417(2)
_cell_volume                     2006.95(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12707
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.4440
_cell_measurement_theta_min      2.0740
_shelx_estimated_absorpt_T_max   0.871
_shelx_estimated_absorpt_T_min   0.676
_exptl_absorpt_coefficient_mu    0.708
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            35122
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_min         2.178
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     85.00 110.00   0.50   28.00    --   20.00  54.00 -90.00   50
  2  ω    -74.00 107.00   0.50   28.00    --   20.00  54.00 150.00  362
  3  ω    -73.00  29.00   0.50   28.00    --   20.00  54.00  30.00  204
  4  ω    -69.00  95.00   0.50   28.00    --   20.00  54.00-150.00  328
  5  ω    -72.00  11.00   0.50   28.00    --   20.00  54.00 -30.00  166
  6  ω     44.00  71.00   0.50   28.00    --   20.00  54.00 -30.00   54
  7  ω    -64.00 -35.00   0.50   28.00    --   20.00  54.00  60.00   58
  8  ω     20.00  67.00   0.50   28.00    --   20.00  54.00  60.00   94
  9  ω    -74.00 -42.00   0.50   28.00    --   20.00  54.00 -60.00   64
 10  ω     -1.00  36.00   0.50   28.00    --   20.00  54.00 -60.00   74
 11  ω    -63.00 -38.00   0.50   28.00    --   20.00  54.00   0.00   50
 12  ω     70.00  97.00   0.50   28.00    --   20.00  54.00   0.00   54
 13  ω    -71.00 -44.00   0.50   28.00    --   20.00  54.00 120.00   54
 14  ω    -17.00  11.00   0.50   28.00    --   20.00  54.00 120.00   56
 15  ω    -43.00 -18.00   0.50   28.00    --   20.00  54.00-180.00   50
 16  ω     31.00  56.00   0.50   28.00    --   20.00  54.00-180.00   50
 17  ω    -74.00  33.00   0.50   28.00    --   20.00  54.00 -90.00  214
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0328982000
_diffrn_orient_matrix_UB_12      0.0602356000
_diffrn_orient_matrix_UB_13      -0.0060659000
_diffrn_orient_matrix_UB_21      -0.0201388000
_diffrn_orient_matrix_UB_22      0.0064043000
_diffrn_orient_matrix_UB_23      0.0338955000
_diffrn_orient_matrix_UB_31      0.0705473000
_diffrn_orient_matrix_UB_32      0.0248258000
_diffrn_orient_matrix_UB_33      0.0003118000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9355
_reflns_number_total             11624
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         11624
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0638P)²+1.2101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1418
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1A-C31 \\sim O1B-C31
 with sigma of 0.02
 C32-Cl1A \\sim C32-Cl1B
 with sigma of 0.02
3. Others
 Fixed Sof: O1A(0.5) H1A(0.5) Cl1A(0.5) O2B(0.5) O2A(0.5) O1B(0.5) H1B(0.5)
 Cl1B(0.5)
4.a Free rotating group:
 O9(H9A,H9B)
4.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C1(H1), C22(H22), C19(H19), C15(H15), C7(H7), C18(H18), C30(H30),
 C8(H8), C17(H17), C23(H23), C24(H24), C9(H9), C12(H12), C27(H27), C29(H29),
 C3(H3), C28(H28), C2(H2), C14(H14), C13(H13)
4.c Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B(H1B)
4.d Idealised tetrahedral OH refined as rotating group:
 O3(H3A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe01 Fe 0.23832(3) 0.79042(3) 0.75136(2) 0.02313(8) Uani 1 1 d . . . . .
Cl3 Cl 0.95201(8) 1.17450(7) 0.47233(3) 0.05077(17) Uani 1 1 d . . . . .
Cl2 Cl 0.38147(10) 1.27185(9) 0.69014(5) 0.0746(3) Uani 1 1 d . . . . .
O5 O 0.9117(2) 1.36248(16) 0.57257(9) 0.0412(4) Uani 1 1 d . . . . .
N2 N 0.2783(2) 0.70613(16) 0.67410(8) 0.0263(3) Uani 1 1 d . . . . .
O8 O -0.2597(2) 0.59758(17) 0.95897(10) 0.0499(5) Uani 1 1 d . . . . .
N4 N 0.1469(2) 0.95162(16) 0.72151(8) 0.0263(3) Uani 1 1 d . . . . .
N3 N 0.4450(2) 0.84333(16) 0.71729(9) 0.0285(4) Uani 1 1 d . . . . .
N5 N 0.2029(2) 0.86890(15) 0.83033(8) 0.0253(3) Uani 1 1 d . . . . .
N1 N 0.0423(2) 0.71356(16) 0.75819(8) 0.0278(3) Uani 1 1 d . . . . .
N6 N 0.3194(2) 0.65596(16) 0.80753(9) 0.0293(4) Uani 1 1 d . . . . .
O9 O 0.8112(2) 0.6059(2) 0.52206(13) 0.0602(6) Uani 1 1 d G . . . .
H9A H 0.845526 0.644190 0.493219 0.090 Uiso 1 1 d G U . . .
H9B H 0.865755 0.551635 0.547478 0.090 Uiso 1 1 d G U . . .
O6 O 0.6512(2) 1.0664(2) 0.49227(10) 0.0578(6) Uani 1 1 d . . . . .
O3 O 0.4141(3) 1.1026(2) 0.58428(12) 0.0676(7) Uani 1 1 d . . . . .
H3A H 0.436780 1.049238 0.558043 0.101 Uiso 1 1 calc R U . . .
O4 O 0.6687(3) 1.3979(2) 0.66549(12) 0.0715(7) Uani 1 1 d . . . . .
O7 O 0.1292(3) 0.2820(2) 0.95777(15) 0.0796(9) Uani 1 1 d . . . . .
C37 C 0.8030(3) 1.2984(2) 0.57336(11) 0.0328(5) Uani 1 1 d . . . . .
C5 C 0.0352(2) 0.63962(19) 0.70909(10) 0.0290(4) Uani 1 1 d . . . . .
C6 C 0.1751(2) 0.6323(2) 0.66080(10) 0.0289(4) Uani 1 1 d . . . . .
C10 C 0.4158(2) 0.7106(2) 0.63603(10) 0.0294(4) Uani 1 1 d . . . . .
C21 C 0.1351(3) 0.98372(19) 0.83297(10) 0.0295(4) Uani 1 1 d . . . . .
C20 C 0.0991(2) 1.03147(19) 0.76939(10) 0.0292(4) Uani 1 1 d . . . . .
C11 C 0.5109(2) 0.7944(2) 0.65993(10) 0.0311(4) Uani 1 1 d . . . . .
C25 C 0.2483(3) 0.8098(2) 0.88344(10) 0.0297(4) Uani 1 1 d . . . . .
C42 C -0.1362(3) 0.5492(2) 0.97722(12) 0.0362(5) Uani 1 1 d . . . . .
C16 C 0.1276(3) 0.9893(2) 0.66089(11) 0.0331(4) Uani 1 1 d . . . . .
H16 H 0.161625 0.936638 0.627681 0.040 Uiso 1 1 calc R U . . .
C1 C -0.0813(3) 0.7275(2) 0.80414(11) 0.0367(5) Uani 1 1 d . . . . .
H1 H -0.078613 0.778041 0.837723 0.044 Uiso 1 1 calc R U . . .
C38 C 0.7961(3) 1.2065(2) 0.53115(11) 0.0350(5) Uani 1 1 d . . . . .
C26 C 0.3205(3) 0.6869(2) 0.86934(11) 0.0313(4) Uani 1 1 d . . . . .
C22 C 0.1108(3) 1.0450(2) 0.89007(12) 0.0387(5) Uani 1 1 d . . . . .
H22 H 0.064479 1.124492 0.891615 0.046 Uiso 1 1 calc R U . . .
C36 C 0.6633(3) 1.3216(2) 0.62706(13) 0.0406(5) Uani 1 1 d . . . . .
C19 C 0.0279(3) 1.1464(2) 0.75731(13) 0.0389(5) Uani 1 1 d . . . . .
H19 H -0.005516 1.198338 0.790899 0.047 Uiso 1 1 calc R U . . .
C41 C -0.0678(3) 0.4367(2) 0.95721(12) 0.0390(5) Uani 1 1 d . . . . .
C15 C 0.5233(3) 0.9227(2) 0.74236(12) 0.0403(5) Uani 1 1 d . . . . .
H15 H 0.479794 0.956604 0.781234 0.048 Uiso 1 1 calc R U . . .
C7 C 0.2071(3) 0.5597(2) 0.60801(12) 0.0387(5) Uani 1 1 d . . . . .
H7 H 0.135834 0.508807 0.599063 0.046 Uiso 1 1 calc R U . . .
C18 C 0.0071(3) 1.1828(2) 0.69463(14) 0.0442(6) Uani 1 1 d . . . . .
H18 H -0.041093 1.259249 0.685451 0.053 Uiso 1 1 calc R U . . .
C30 C 0.3774(3) 0.5426(2) 0.79122(13) 0.0380(5) Uani 1 1 d . . . . .
H30 H 0.374770 0.518946 0.749699 0.046 Uiso 1 1 calc R U . . .
C4 C -0.0922(3) 0.5799(2) 0.70516(13) 0.0406(5) Uani 1 1 d . . . . .
C8 C 0.3473(3) 0.5646(3) 0.56895(12) 0.0440(6) Uani 1 1 d . . . . .
H8 H 0.370648 0.516836 0.533110 0.053 Uiso 1 1 calc R U . . .
C17 C 0.0590(3) 1.1038(2) 0.64590(13) 0.0421(6) Uani 1 1 d . . . . .
H17 H 0.048054 1.127327 0.603261 0.051 Uiso 1 1 calc R U . . .
C23 C 0.1575(3) 0.9848(3) 0.94468(12) 0.0419(6) Uani 1 1 d . . . . .
H23 H 0.143035 1.024207 0.983360 0.050 Uiso 1 1 calc R U . . .
O1A O 0.7160(8) 0.8415(6) 0.9356(3) 0.0496(13) Uani 0.5 1 d D . P A 1
H1A H 0.706799 0.774255 0.955722 0.074 Uiso 0.5 1 calc R U P A 1
C24 C 0.2254(3) 0.8663(2) 0.94190(11) 0.0392(5) Uani 1 1 d . . . . .
H24 H 0.255135 0.825076 0.978645 0.047 Uiso 1 1 calc R U . . .
C9 C 0.4533(3) 0.6399(2) 0.58273(12) 0.0400(5) Uani 1 1 d . . . . .
H9 H 0.547986 0.642956 0.556609 0.048 Uiso 1 1 calc R U . . .
C35 C 0.5336(3) 1.2507(2) 0.62853(13) 0.0432(6) Uani 1 1 d . . . . .
C40 C 0.0655(3) 0.3838(2) 0.97721(14) 0.0422(6) Uani 1 1 d . . . . .
C34 C 0.5325(3) 1.1679(2) 0.58407(13) 0.0431(6) Uani 1 1 d . . . . .
C39 C 0.6669(3) 1.1423(2) 0.53150(12) 0.0390(5) Uani 1 1 d . . . . .
C32 C 0.5698(3) 1.0430(3) 0.93873(12) 0.0421(6) Uani 1 1 d D . . . .
C33 C 0.4679(3) 1.1217(2) 0.97480(15) 0.0466(6) Uani 1 1 d . . . . .
C12 C 0.6533(3) 0.8237(3) 0.62822(13) 0.0434(6) Uani 1 1 d . . . . .
H12 H 0.695980 0.788736 0.589536 0.052 Uiso 1 1 calc R U . . .
C27 C 0.3861(3) 0.6088(3) 0.91390(13) 0.0440(6) Uani 1 1 d . . . B 1
H27 H 0.387874 0.632967 0.955380 0.053 Uiso 1 1 calc R U . B 1
C29 C 0.4411(3) 0.4596(2) 0.83440(15) 0.0477(6) Uani 1 1 d . . . . .
H29 H 0.478221 0.381280 0.821936 0.057 Uiso 1 1 calc R U . . .
C3 C -0.2180(3) 0.5949(3) 0.75351(14) 0.0501(7) Uani 1 1 d . . . . .
H3 H -0.305298 0.555043 0.752318 0.060 Uiso 1 1 calc R U . . .
C28 C 0.4490(3) 0.4933(3) 0.89502(15) 0.0507(7) Uani 1 1 d . . . . .
H28 H 0.495863 0.439845 0.923449 0.061 Uiso 1 1 calc R U . B 1
C2 C -0.2121(3) 0.6693(3) 0.80324(13) 0.0486(7) Uani 1 1 d . . . . .
H2 H -0.295414 0.680350 0.835915 0.058 Uiso 1 1 calc R U . . .
C31 C 0.6049(3) 0.9219(2) 0.96065(16) 0.0513(7) Uani 1 1 d D . . . .
C14 C 0.6655(3) 0.9561(3) 0.71296(15) 0.0522(7) Uani 1 1 d . . . . .
H14 H 0.716157 1.011369 0.731770 0.063 Uiso 1 1 calc R U . . .
C13 C 0.7312(3) 0.9062(3) 0.65523(15) 0.0539(7) Uani 1 1 d . . . . .
H13 H 0.826708 0.927632 0.634648 0.065 Uiso 1 1 calc R U . . .
Cl1A Cl 0.6743(3) 1.07667(17) 0.86265(12) 0.0474(4) Uani 0.5 1 d D . P C 1
Cl4 Cl -0.15279(10) 0.35645(7) 0.90588(4) 0.0591(3) Uani 0.989(3) 1 d . . . D 2
O2B O 0.4305(7) 1.2255(4) 0.9395(2) 0.0472(12) Uani 0.5 1 d . . P E 2
O2A O 0.4423(8) 1.2445(5) 0.9723(3) 0.0711(17) Uani 0.5 1 d . . P E .
O1B O 0.6736(11) 0.8604(7) 0.9121(3) 0.094(3) Uani 0.5 1 d D . P A 2
H1B H 0.675810 0.786320 0.922711 0.141 Uiso 0.5 1 calc R U P A 2
Cl1B Cl 0.6324(4) 1.1223(2) 0.86265(14) 0.0791(8) Uani 0.5 1 d D . P C 2
H4 H -0.089(4) 0.530(3) 0.6710(18) 0.070(11) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 N2 1.8871(17) . ?
Fe01 N4 1.9819(18) . ?
Fe01 N3 1.9839(19) . ?
Fe01 N5 1.8859(16) . ?
Fe01 N1 1.9869(18) . ?
Fe01 N6 1.9808(18) . ?
Cl3 C38 1.730(2) . ?
Cl2 C35 1.724(3) . ?
O5 C37 1.241(3) . ?
N2 C6 1.351(3) . ?
N2 C10 1.351(3) . ?
O8 C42 1.294(3) . ?
N4 C20 1.367(3) . ?
N4 C16 1.340(3) . ?
N3 C11 1.371(3) . ?
N3 C15 1.345(3) . ?
N5 C21 1.347(3) . ?
N5 C25 1.351(3) . ?
N1 C5 1.366(3) . ?
N1 C1 1.345(3) . ?
N6 C26 1.364(3) . ?
N6 C30 1.346(3) . ?
O9 H9A 0.7434 . ?
O9 H9B 0.9320 . ?
O6 C39 1.240(3) . ?
O3 H3A 0.8200 . ?
O3 C34 1.324(3) . ?
O4 C36 1.209(3) . ?
O7 C40 1.269(3) . ?
C37 C38 1.396(3) . ?
C37 C36 1.552(3) . ?
C5 C6 1.472(3) . ?
C5 C4 1.377(3) . ?
C6 C7 1.385(3) . ?
C10 C11 1.467(3) . ?
C10 C9 1.383(3) . ?
C21 C20 1.471(3) . ?
C21 C22 1.390(3) . ?
C20 C19 1.386(3) . ?
C11 C12 1.385(3) . ?
C25 C26 1.468(3) . ?
C25 C24 1.388(3) . ?
C42 C41 1.386(3) . ?
C42 C40 1.494(3) 2_567 ?
C16 H16 0.9300 . ?
C16 C17 1.385(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.381(4) . ?
C38 C39 1.400(3) . ?
C26 C27 1.390(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.387(4) . ?
C36 C35 1.443(3) . ?
C19 H19 0.9300 . ?
C19 C18 1.382(4) . ?
C41 C40 1.401(3) . ?
C41 Cl4 1.741(2) . ?
C15 H15 0.9300 . ?
C15 C14 1.383(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.380(3) . ?
C18 H18 0.9300 . ?
C18 C17 1.380(4) . ?
C30 H30 0.9300 . ?
C30 C29 1.391(4) . ?
C4 C3 1.389(4) . ?
C4 H4 0.93(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.385(4) . ?
C17 H17 0.9300 . ?
C23 H23 0.9300 . ?
C23 C24 1.383(4) . ?
O1A H1A 0.8200 . ?
O1A C31 1.336(6) . ?
C24 H24 0.9300 . ?
C9 H9 0.9300 . ?
C35 C34 1.346(3) . ?
C34 C39 1.511(4) . ?
C32 C33 1.370(4) . ?
C32 C31 1.394(4) . ?
C32 Cl1A 1.734(3) . ?
C32 Cl1B 1.779(4) . ?
C33 C31 1.460(4) 2_677 ?
C33 O2B 1.355(5) . ?
C33 O2A 1.338(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.389(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.393(4) . ?
C29 H29 0.9300 . ?
C29 C28 1.363(4) . ?
C3 H3 0.9300 . ?
C3 C2 1.378(4) . ?
C28 H28 0.9300 . ?
C2 H2 0.9300 . ?
C31 O1B 1.298(7) . ?
C14 H14 0.9300 . ?
C14 C13 1.382(4) . ?
C13 H13 0.9300 . ?
O2B O2A 0.759(7) . ?
O1B H1B 0.8200 . ?

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 Fe01 N4 101.79(7) . . ?
N2 Fe01 N3 80.88(7) . . ?
N2 Fe01 N1 80.81(7) . . ?
N2 Fe01 N6 96.56(8) . . ?
N4 Fe01 N3 90.90(7) . . ?
N4 Fe01 N1 91.16(7) . . ?
N3 Fe01 N1 161.62(7) . . ?
N5 Fe01 N2 177.50(8) . . ?
N5 Fe01 N4 80.69(7) . . ?
N5 Fe01 N3 98.84(7) . . ?
N5 Fe01 N1 99.53(7) . . ?
N5 Fe01 N6 80.96(7) . . ?
N6 Fe01 N4 161.64(7) . . ?
N6 Fe01 N3 91.52(8) . . ?
N6 Fe01 N1 92.26(8) . . ?
C6 N2 Fe01 119.57(14) . . ?
C6 N2 C10 120.57(17) . . ?
C10 N2 Fe01 119.53(14) . . ?
C20 N4 Fe01 114.64(14) . . ?
C16 N4 Fe01 127.47(15) . . ?
C16 N4 C20 117.89(19) . . ?
C11 N3 Fe01 114.27(14) . . ?
C15 N3 Fe01 128.05(16) . . ?
C15 N3 C11 117.6(2) . . ?
C21 N5 Fe01 119.81(14) . . ?
C21 N5 C25 120.74(18) . . ?
C25 N5 Fe01 119.44(14) . . ?
C5 N1 Fe01 114.40(14) . . ?
C1 N1 Fe01 127.84(15) . . ?
C1 N1 C5 117.76(19) . . ?
C26 N6 Fe01 114.19(14) . . ?
C30 N6 Fe01 128.05(17) . . ?
C30 N6 C26 117.7(2) . . ?
H9A O9 H9B 124.7 . . ?
C34 O3 H3A 109.5 . . ?
O5 C37 C38 126.0(2) . . ?
O5 C37 C36 116.7(2) . . ?
C38 C37 C36 117.32(19) . . ?
N1 C5 C6 113.49(18) . . ?
N1 C5 C4 122.7(2) . . ?
C4 C5 C6 123.8(2) . . ?
N2 C6 C5 111.51(17) . . ?
N2 C6 C7 121.0(2) . . ?
C7 C6 C5 127.5(2) . . ?
N2 C10 C11 111.55(18) . . ?
N2 C10 C9 120.7(2) . . ?
C9 C10 C11 127.8(2) . . ?
N5 C21 C20 111.58(17) . . ?
N5 C21 C22 121.1(2) . . ?
C22 C21 C20 127.3(2) . . ?
N4 C20 C21 113.15(18) . . ?
N4 C20 C19 122.1(2) . . ?
C19 C20 C21 124.7(2) . . ?
N3 C11 C10 113.54(19) . . ?
N3 C11 C12 122.2(2) . . ?
C12 C11 C10 124.3(2) . . ?
N5 C25 C26 111.47(18) . . ?
N5 C25 C24 120.5(2) . . ?
C24 C25 C26 128.0(2) . . ?
O8 C42 C41 122.9(2) . . ?
O8 C42 C40 118.71(19) . 2_567 ?
C41 C42 C40 118.4(2) . 2_567 ?
N4 C16 H16 118.8 . . ?
N4 C16 C17 122.4(2) . . ?
C17 C16 H16 118.8 . . ?
N1 C1 H1 118.8 . . ?
N1 C1 C2 122.3(2) . . ?
C2 C1 H1 118.8 . . ?
C37 C38 Cl3 118.67(18) . . ?
C37 C38 C39 123.6(2) . . ?
C39 C38 Cl3 117.61(18) . . ?
N6 C26 C25 113.69(18) . . ?
N6 C26 C27 122.4(2) . . ?
C27 C26 C25 123.9(2) . . ?
C21 C22 H22 120.8 . . ?
C23 C22 C21 118.3(2) . . ?
C23 C22 H22 120.8 . . ?
O4 C36 C37 118.5(2) . . ?
O4 C36 C35 123.3(3) . . ?
C35 C36 C37 118.2(2) . . ?
C20 C19 H19 120.5 . . ?
C18 C19 C20 119.0(2) . . ?
C18 C19 H19 120.5 . . ?
C42 C41 C40 123.0(2) . . ?
C42 C41 Cl4 118.52(19) . . ?
C40 C41 Cl4 118.50(17) . . ?
N3 C15 H15 118.5 . . ?
N3 C15 C14 123.0(2) . . ?
C14 C15 H15 118.5 . . ?
C6 C7 H7 120.8 . . ?
C8 C7 C6 118.5(2) . . ?
C8 C7 H7 120.8 . . ?
C19 C18 H18 120.5 . . ?
C17 C18 C19 118.9(2) . . ?
C17 C18 H18 120.5 . . ?
N6 C30 H30 118.9 . . ?
N6 C30 C29 122.2(2) . . ?
C29 C30 H30 118.9 . . ?
C5 C4 C3 118.5(2) . . ?
C5 C4 H4 118(2) . . ?
C3 C4 H4 123(2) . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.5(2) . . ?
C9 C8 H8 119.7 . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.6(2) . . ?
C18 C17 H17 120.2 . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.8 . . ?
C31 O1A H1A 109.5 . . ?
C25 C24 H24 120.5 . . ?
C23 C24 C25 119.0(2) . . ?
C23 C24 H24 120.5 . . ?
C10 C9 C8 118.8(2) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
C36 C35 Cl2 118.19(19) . . ?
C34 C35 Cl2 120.8(2) . . ?
C34 C35 C36 121.0(2) . . ?
O7 C40 C42 118.7(2) . 2_567 ?
O7 C40 C41 122.7(2) . . ?
C41 C40 C42 118.62(19) . 2_567 ?
O3 C34 C35 121.9(2) . . ?
O3 C34 C39 115.9(2) . . ?
C35 C34 C39 122.2(2) . . ?
O6 C39 C38 126.2(2) . . ?
O6 C39 C34 116.4(2) . . ?
C38 C39 C34 117.4(2) . . ?
C33 C32 C31 122.6(2) . . ?
C33 C32 Cl1A 126.7(2) . . ?
C33 C32 Cl1B 107.5(2) . . ?
C31 C32 Cl1A 110.6(2) . . ?
C31 C32 Cl1B 129.7(2) . . ?
C32 C33 C31 118.9(2) . 2_677 ?
O2B C33 C32 112.1(3) . . ?
O2B C33 C31 128.0(3) . 2_677 ?
O2A C33 C32 133.2(4) . . ?
O2A C33 C31 105.7(4) . 2_677 ?
O2A C33 O2B 32.7(3) . . ?
C11 C12 H12 120.6 . . ?
C11 C12 C13 118.8(2) . . ?
C13 C12 H12 120.6 . . ?
C26 C27 H27 120.7 . . ?
C26 C27 C28 118.5(3) . . ?
C28 C27 H27 120.7 . . ?
C30 C29 H29 120.1 . . ?
C28 C29 C30 119.9(2) . . ?
C28 C29 H29 120.1 . . ?
C4 C3 H3 120.4 . . ?
C2 C3 C4 119.3(2) . . ?
C2 C3 H3 120.4 . . ?
C27 C28 H28 120.4 . . ?
C29 C28 C27 119.2(2) . . ?
C29 C28 H28 120.4 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.4(2) . . ?
C3 C2 H2 120.3 . . ?
O1A C31 C32 129.0(4) . . ?
O1A C31 C33 111.6(4) . 2_677 ?
C32 C31 C33 118.5(2) . 2_677 ?
O1B C31 C32 109.4(4) . . ?
C15 C14 H14 120.5 . . ?
C13 C14 C15 119.0(2) . . ?
C13 C14 H14 120.5 . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.3(2) . . ?
C14 C13 H13 120.3 . . ?
O2A O2B C33 72.4(6) . . ?
O2B O2A C33 74.9(7) . . ?
C31 O1B H1B 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe01 N2 C6 C5 5.3(2) . . . . ?
Fe01 N2 C6 C7 -173.46(18) . . . . ?
Fe01 N2 C10 C11 -5.4(2) . . . . ?
Fe01 N2 C10 C9 173.48(18) . . . . ?
Fe01 N4 C20 C21 3.8(2) . . . . ?
Fe01 N4 C20 C19 -177.72(18) . . . . ?
Fe01 N4 C16 C17 178.64(18) . . . . ?
Fe01 N3 C11 C10 -1.1(2) . . . . ?
Fe01 N3 C11 C12 178.3(2) . . . . ?
Fe01 N3 C15 C14 -177.7(2) . . . . ?
Fe01 N5 C21 C20 -0.5(2) . . . . ?
Fe01 N5 C21 C22 -178.42(18) . . . . ?
Fe01 N5 C25 C26 -0.5(2) . . . . ?
Fe01 N5 C25 C24 179.16(18) . . . . ?
Fe01 N1 C5 C6 -0.2(2) . . . . ?
Fe01 N1 C5 C4 -179.09(19) . . . . ?
Fe01 N1 C1 C2 179.5(2) . . . . ?
Fe01 N6 C26 C25 5.4(2) . . . . ?
Fe01 N6 C26 C27 -173.89(19) . . . . ?
Fe01 N6 C30 C29 175.08(19) . . . . ?
Cl3 C38 C39 O6 -2.3(4) . . . . ?
Cl3 C38 C39 C34 178.4(2) . . . . ?
Cl2 C35 C34 O3 2.3(4) . . . . ?
Cl2 C35 C34 C39 -176.8(2) . . . . ?
O5 C37 C38 Cl3 1.0(3) . . . . ?
O5 C37 C38 C39 -175.7(2) . . . . ?
O5 C37 C36 O4 -1.4(4) . . . . ?
O5 C37 C36 C35 178.6(2) . . . . ?
N2 C6 C7 C8 -0.2(4) . . . . ?
N2 C10 C11 N3 4.0(3) . . . . ?
N2 C10 C11 C12 -175.4(2) . . . . ?
N2 C10 C9 C8 0.1(4) . . . . ?
O8 C42 C41 C40 -179.6(3) . . . . ?
O8 C42 C41 Cl4 -0.6(4) . . . . ?
N4 Fe01 N2 C6 -93.61(17) . . . . ?
N4 Fe01 N2 C10 92.90(17) . . . . ?
N4 Fe01 N5 C21 2.01(16) . . . . ?
N4 Fe01 N5 C25 -176.88(17) . . . . ?
N4 C20 C19 C18 -1.4(4) . . . . ?
N4 C16 C17 C18 -0.4(4) . . . . ?
N3 Fe01 N2 C6 177.38(17) . . . . ?
N3 Fe01 N2 C10 3.89(16) . . . . ?
N3 Fe01 N5 C21 91.47(17) . . . . ?
N3 Fe01 N5 C25 -87.42(17) . . . . ?
N3 C11 C12 C13 -0.5(4) . . . . ?
N3 C15 C14 C13 -0.1(5) . . . . ?
N5 C21 C20 N4 -2.3(3) . . . . ?
N5 C21 C20 C19 179.4(2) . . . . ?
N5 C21 C22 C23 -0.4(4) . . . . ?
N5 C25 C26 N6 -3.3(3) . . . . ?
N5 C25 C26 C27 176.0(2) . . . . ?
N5 C25 C24 C23 -1.1(4) . . . . ?
N1 Fe01 N2 C6 -4.34(16) . . . . ?
N1 Fe01 N2 C10 -177.83(17) . . . . ?
N1 Fe01 N5 C21 -87.61(17) . . . . ?
N1 Fe01 N5 C25 93.50(17) . . . . ?
N1 C5 C6 N2 -3.1(3) . . . . ?
N1 C5 C6 C7 175.6(2) . . . . ?
N1 C5 C4 C3 -0.6(4) . . . . ?
N1 C1 C2 C3 -0.5(4) . . . . ?
N6 Fe01 N2 C6 86.89(17) . . . . ?
N6 Fe01 N2 C10 -86.59(17) . . . . ?
N6 Fe01 N5 C21 -178.40(17) . . . . ?
N6 Fe01 N5 C25 2.72(16) . . . . ?
N6 C26 C27 C28 -1.8(4) . . . . ?
N6 C30 C29 C28 -1.4(4) . . . . ?
O3 C34 C39 O6 2.7(4) . . . . ?
O3 C34 C39 C38 -177.9(3) . . . . ?
O4 C36 C35 Cl2 -2.6(4) . . . . ?
O4 C36 C35 C34 179.1(3) . . . . ?
C37 C38 C39 O6 174.5(3) . . . . ?
C37 C38 C39 C34 -4.9(4) . . . . ?
C37 C36 C35 Cl2 177.39(19) . . . . ?
C37 C36 C35 C34 -0.9(4) . . . . ?
C5 N1 C1 C2 0.5(4) . . . . ?
C5 C6 C7 C8 -178.7(2) . . . . ?
C5 C4 C3 C2 0.6(5) . . . . ?
C6 N2 C10 C11 -178.83(19) . . . . ?
C6 N2 C10 C9 0.1(3) . . . . ?
C6 C5 C4 C3 -179.4(2) . . . . ?
C6 C7 C8 C9 0.4(4) . . . . ?
C10 N2 C6 C5 178.72(19) . . . . ?
C10 N2 C6 C7 0.0(3) . . . . ?
C10 C11 C12 C13 178.8(3) . . . . ?
C21 N5 C25 C26 -179.40(19) . . . . ?
C21 N5 C25 C24 0.3(3) . . . . ?
C21 C20 C19 C18 176.9(2) . . . . ?
C21 C22 C23 C24 -0.4(4) . . . . ?
C20 N4 C16 C17 -1.4(3) . . . . ?
C20 C21 C22 C23 -178.0(2) . . . . ?
C20 C19 C18 C17 -0.5(4) . . . . ?
C11 N3 C15 C14 0.0(4) . . . . ?
C11 C10 C9 C8 178.8(2) . . . . ?
C11 C12 C13 C14 0.4(5) . . . . ?
C25 N5 C21 C20 178.40(19) . . . . ?
C25 N5 C21 C22 0.4(3) . . . . ?
C25 C26 C27 C28 179.0(2) . . . . ?
C42 C41 C40 O7 -178.6(3) . . . . ?
C42 C41 C40 C42 0.8(5) . . . 2_567 ?
C16 N4 C20 C21 -176.13(19) . . . . ?
C16 N4 C20 C19 2.3(3) . . . . ?
C1 N1 C5 C6 179.0(2) . . . . ?
C1 N1 C5 C4 0.0(3) . . . . ?
C38 C37 C36 O4 177.6(3) . . . . ?
C38 C37 C36 C35 -2.4(3) . . . . ?
C26 N6 C30 C29 -1.9(4) . . . . ?
C26 C25 C24 C23 178.6(2) . . . . ?
C26 C27 C28 C29 -1.6(4) . . . . ?
C22 C21 C20 N4 175.5(2) . . . . ?
C22 C21 C20 C19 -2.9(4) . . . . ?
C22 C23 C24 C25 1.1(4) . . . . ?
C36 C37 C38 Cl3 -177.93(18) . . . . ?
C36 C37 C38 C39 5.4(4) . . . . ?
C36 C35 C34 O3 -179.5(3) . . . . ?
C36 C35 C34 C39 1.4(5) . . . . ?
C19 C18 C17 C16 1.4(4) . . . . ?
C15 N3 C11 C10 -179.1(2) . . . . ?
C15 N3 C11 C12 0.3(4) . . . . ?
C15 C14 C13 C12 -0.1(5) . . . . ?
C7 C8 C9 C10 -0.4(4) . . . . ?
C30 N6 C26 C25 -177.2(2) . . . . ?
C30 N6 C26 C27 3.5(3) . . . . ?
C30 C29 C28 C27 3.1(4) . . . . ?
C4 C5 C6 N2 175.8(2) . . . . ?
C4 C5 C6 C7 -5.5(4) . . . . ?
C4 C3 C2 C1 -0.1(5) . . . . ?
C24 C25 C26 N6 177.1(2) . . . . ?
C24 C25 C26 C27 -3.6(4) . . . . ?
C9 C10 C11 N3 -174.8(2) . . . . ?
C9 C10 C11 C12 5.8(4) . . . . ?
C35 C34 C39 O6 -178.1(3) . . . . ?
C35 C34 C39 C38 1.3(4) . . . . ?
C40 C42 C41 C40 -0.8(5) 2_567 . . . ?
C40 C42 C41 Cl4 178.3(2) 2_567 . . . ?
C32 C33 O2B O2A -137.1(8) . . . . ?
C32 C33 O2A O2B 59.8(11) . . . . ?
C33 C32 C31 O1A -169.2(5) . . . . ?
C33 C32 C31 C33 -1.3(5) . . . 2_677 ?
C33 C32 C31 O1B 164.5(6) . . . . ?
C31 C32 C33 C31 1.3(5) . . . 2_677 ?
C31 C32 C33 O2B -168.4(4) . . . . ?
C31 C32 C33 O2A 161.3(5) . . . . ?
C31 C33 O2B O2A 54.4(10) 2_677 . . . ?
C31 C33 O2A O2B -138.3(8) 2_677 . . . ?
Cl1A C32 C33 C31 -177.4(2) . . . 2_677 ?
Cl1A C32 C33 O2A -17.4(7) . . . . ?
Cl1A C32 C31 O1A 9.7(6) . . . . ?
Cl1A C32 C31 C33 177.6(2) . . . 2_677 ?
Cl4 C41 C40 O7 2.4(4) . . . . ?
Cl4 C41 C40 C42 -178.3(2) . . . 2_567 ?
Cl1B C32 C33 C31 178.3(3) . . . 2_677 ?
Cl1B C32 C33 O2B 8.7(4) . . . . ?
Cl1B C32 C33 O2A -21.6(6) . . . . ?
Cl1B C32 C31 C33 -177.6(3) . . . 2_677 ?
Cl1B C32 C31 O1B -11.9(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.679
####################################################################### 
# 
# 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_exp_698
_audit_block_doi                 10.5517/ccdc.csd.cc2kq47p
_database_code_depnum_ccdc_archive 'CCDC 2374762'
loop_
_audit_author_name
_audit_author_address
'Akio Mishima'
;Fukuoka University
Japan
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_audit_creation_date             2024-06-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        
'[Co(C15N3H11)2](C6O4H2Cl2)0.5(C6O4HCl2)(C6O4Cl2)0.5(H2O)'
_chemical_formula_moiety         
'C30 H22 Co N6, C6 H Cl2 O4, C3 H Cl O2, C3 Cl O2, H2 O'
_chemical_formula_sum            'C42 H26 Cl4 Co N6 O9'
_chemical_formula_weight         959.42
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N10O10Co1Cl2
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.9669(2)
_cell_length_b                   10.9875(2)
_cell_length_c                   20.9096(4)
_cell_angle_alpha                85.6270(10)
_cell_angle_beta                 80.052(2)
_cell_angle_gamma                85.213(2)
_cell_volume                     2018.03(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12454
_cell_measurement_temperature    292.6(3)
_cell_measurement_theta_max      30.5710
_cell_measurement_theta_min      2.0080
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             974
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38624
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.530
_diffrn_reflns_theta_min         1.982
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.6(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      9.00  51.00   0.50   25.00    --   20.00  54.00-161.22   84
  2  ω     59.00 110.00   0.50   25.00    --   20.00  54.00-161.22  102
  3  ω    -74.00 -14.00   0.50   25.00    --   20.00  54.00-132.08  120
  4  ω     30.00  56.00   0.50   25.00    --   20.00  54.00-132.08   52
  5  ω    -73.00  64.00   0.50   25.00    --   20.00  54.00 150.00  274
  6  ω     75.00 107.00   0.50   25.00    --   20.00  54.00 150.00   64
  7  ω    -70.00 -27.00   0.50   25.00    --   20.00  54.00 -60.00   86
  8  ω    -16.00  13.00   0.50   25.00    --   20.00  54.00 -60.00   58
  9  ω     19.00  44.00   0.50   25.00    --   20.00  54.00 -60.00   50
 10  ω    -63.00  99.00   0.50   25.00    --   20.00  54.00 -30.00  324
 11  ω    -64.00 -38.00   0.50   25.00    --   20.00  54.00 120.00   52
 12  ω     75.00 107.00   0.50   25.00    --   20.00  54.00 120.00   64
 13  ω    -72.00  85.00   0.50   25.00    --   20.00  54.00  30.00  314
 14  ω    -61.00 -34.00   0.50   25.00    --   20.00  54.00-180.00   54
 15  ω     20.00  45.00   0.50   25.00    --   20.00  54.00-180.00   50
 16  ω    -72.00 -47.00   0.50   25.00    --   20.00  54.00 -90.00   50
 17  ω      1.00  49.00   0.50   25.00    --   20.00  54.00 -90.00   96
 18  ω    -70.00  49.00   0.50   25.00    --   20.00  54.00  90.00  238
 19  ω    -33.00  -8.00   0.50   25.00    --   20.00  54.00-161.22   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0081807000
_diffrn_orient_matrix_UB_12      0.0639001000
_diffrn_orient_matrix_UB_13      -0.0020312000
_diffrn_orient_matrix_UB_21      0.0285836000
_diffrn_orient_matrix_UB_22      -0.0019603000
_diffrn_orient_matrix_UB_23      -0.0337513000
_diffrn_orient_matrix_UB_31      -0.0748261000
_diffrn_orient_matrix_UB_32      0.0112349000
_diffrn_orient_matrix_UB_33      -0.0068967000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9014
_reflns_number_total             11660
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.848
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         11660
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0516
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0614P)²+1.5965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1346
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C22(H22), C16(H16), C12(H12), C24(H24), C7(H7), C15(H15), C23(H23),
 C18(H18), C17(H17), C30(H30), C8(H8), C27(H27), C4(H4), C1(H1), C13(H13),
 C28(H28), C29(H29), C14(H14), C2(H2), C3(H3)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O3(H3A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.76866(3) 0.20675(2) 0.74751(2) 0.02614(8) Uani 1 1 d . . . . .
Cl3 Cl 0.05207(8) -0.17715(7) 1.02796(3) 0.05377(18) Uani 1 1 d . . . . .
Cl1 Cl 0.84357(9) 0.35549(6) 0.40719(4) 0.0576(2) Uani 1 1 d . . . . .
Cl2 Cl 0.62465(10) -0.27111(10) 0.80988(5) 0.0799(3) Uani 1 1 d . . . . .
Cl4 Cl 0.37422(16) 0.87700(10) 0.63839(4) 0.0943(4) Uani 1 1 d . . . . .
O5 O 0.0957(2) -0.36473(16) 0.92808(9) 0.0436(4) Uani 1 1 d . . . . .
N5 N 0.80325(19) 0.12810(15) 0.66801(8) 0.0266(3) Uani 1 1 d . . . . .
N2 N 0.72575(19) 0.29205(16) 0.82580(8) 0.0268(3) Uani 1 1 d . . . . .
O1 O 0.7532(2) 0.60420(17) 0.45145(10) 0.0543(5) Uani 1 1 d . . . . .
H1A H 0.723835 0.665285 0.471586 0.082 Uiso 1 1 calc R U . . .
N4 N 0.8607(2) 0.03762(17) 0.77784(9) 0.0309(4) Uani 1 1 d . . . . .
N1 N 0.9745(2) 0.28625(17) 0.74353(9) 0.0308(4) Uani 1 1 d . . . . .
N6 N 0.6895(2) 0.34619(17) 0.68730(9) 0.0327(4) Uani 1 1 d . . . . .
N3 N 0.5488(2) 0.15489(17) 0.78421(9) 0.0337(4) Uani 1 1 d . . . . .
O6 O 0.3515(2) -0.0684(2) 1.00813(10) 0.0599(6) Uani 1 1 d . . . . .
O2 O 1.1010(3) 0.27026(18) 0.47639(13) 0.0688(7) Uani 1 1 d . . . . .
O3 O 0.5899(3) -0.1033(2) 0.91591(12) 0.0707(7) Uani 1 1 d . . . . .
H3A H 0.571561 -0.058343 0.946296 0.106 Uiso 1 1 calc R U . . .
O4 O 0.3401(3) -0.3985(2) 0.83540(13) 0.0782(8) Uani 1 1 d . . . . .
O7 O 0.5556(3) 0.75738(17) 0.52499(13) 0.0694(7) Uani 1 1 d . . . . .
C37 C 0.2040(3) -0.3000(2) 0.92724(11) 0.0345(5) Uani 1 1 d . . . . .
C21 C 0.8677(2) 0.01212(19) 0.66577(11) 0.0304(4) Uani 1 1 d . . . . .
C11 C 0.9728(2) 0.35935(19) 0.79315(10) 0.0292(4) Uani 1 1 d . . . . .
C10 C 0.8283(2) 0.36582(19) 0.83901(10) 0.0293(4) Uani 1 1 d . . . . .
C20 C 0.9062(2) -0.03805(19) 0.72869(11) 0.0310(4) Uani 1 1 d . . . . .
C25 C 0.7581(2) 0.1872(2) 0.61480(10) 0.0304(4) Uani 1 1 d . . . . .
C6 C 0.5876(2) 0.2881(2) 0.86327(10) 0.0308(4) Uani 1 1 d . . . . .
C5 C 0.4888(2) 0.2043(2) 0.84141(11) 0.0316(4) Uani 1 1 d . . . . .
C40 C 0.5271(3) 0.8716(2) 0.51677(13) 0.0413(6) Uani 1 1 d . . . . .
C26 C 0.6882(3) 0.3112(2) 0.62662(11) 0.0313(4) Uani 1 1 d . . . . .
C19 C 0.9785(3) -0.1526(2) 0.73875(13) 0.0416(5) Uani 1 1 d . . . . .
H19 H 1.010581 -0.202541 0.704310 0.050 Uiso 1 1 calc R U . . .
O8 O 0.3378(3) 1.1397(2) 0.58996(14) 0.0919(9) Uani 1 1 d . . . . .
C22 C 0.8868(3) -0.0493(2) 0.60883(12) 0.0408(5) Uani 1 1 d . . . . .
H22 H 0.929885 -0.129198 0.607475 0.049 Uiso 1 1 calc R U . . .
C38 C 0.2091(3) -0.2085(2) 0.96934(11) 0.0371(5) Uani 1 1 d . . . . .
C31 C 0.8712(3) 0.5524(2) 0.47165(12) 0.0399(5) Uani 1 1 d . . . . .
C16 C 0.8822(3) -0.0027(2) 0.83779(12) 0.0399(5) Uani 1 1 d . . . . .
H16 H 0.849083 0.047973 0.871839 0.048 Uiso 1 1 calc R U . . .
C12 C 1.0971(3) 0.4213(2) 0.79920(12) 0.0402(5) Uani 1 1 d . . . . .
H12 H 1.093817 0.470459 0.833767 0.048 Uiso 1 1 calc R U . . .
C32 C 0.9315(3) 0.4372(2) 0.45633(12) 0.0402(5) Uani 1 1 d . . . . .
C24 C 0.7783(3) 0.1303(2) 0.55664(11) 0.0392(5) Uani 1 1 d . . . . .
H24 H 0.750422 0.171880 0.519598 0.047 Uiso 1 1 calc R U . . .
C33 C 1.0530(3) 0.3764(2) 0.48433(13) 0.0423(6) Uani 1 1 d . . . . .
C9 C 0.7933(3) 0.4395(2) 0.89132(12) 0.0410(5) Uani 1 1 d . . . . .
C7 C 0.5470(3) 0.3601(2) 0.91608(12) 0.0418(6) Uani 1 1 d . . . . .
H7 H 0.451594 0.357455 0.941797 0.050 Uiso 1 1 calc R U . . .
C15 C 1.1009(3) 0.2750(2) 0.69928(12) 0.0407(5) Uani 1 1 d . . . . .
H15 H 1.102696 0.225047 0.665166 0.049 Uiso 1 1 calc R U . . .
C36 C 0.3437(3) -0.3224(2) 0.87402(13) 0.0425(6) Uani 1 1 d . . . . .
C42 C 0.4109(3) 1.0715(2) 0.54974(14) 0.0454(6) Uani 1 1 d . . . . .
C39 C 0.3379(3) -0.1440(2) 0.96888(12) 0.0408(5) Uani 1 1 d . . . . .
C23 C 0.8406(3) 0.0106(2) 0.55445(12) 0.0434(6) Uani 1 1 d . . . . .
H23 H 0.851308 -0.029462 0.516144 0.052 Uiso 1 1 calc R U . . .
C41 C 0.4417(3) 0.9447(2) 0.56242(12) 0.0439(6) Uani 1 1 d . . . . .
C18 C 1.0022(3) -0.1914(3) 0.80113(14) 0.0489(6) Uani 1 1 d . . . . .
H18 H 1.051921 -0.267377 0.809004 0.059 Uiso 1 1 calc R U . . .
C35 C 0.4725(3) -0.2508(3) 0.87184(13) 0.0470(6) Uani 1 1 d . . . . .
C17 C 0.9514(3) -0.1163(3) 0.85110(13) 0.0479(6) Uani 1 1 d . . . . .
H17 H 0.963617 -0.141787 0.893445 0.058 Uiso 1 1 calc R U . . .
C30 C 0.6319(3) 0.4589(2) 0.70210(14) 0.0437(6) Uani 1 1 d . . . . .
H30 H 0.633519 0.483880 0.743455 0.052 Uiso 1 1 calc R U . . .
C8 C 0.6517(3) 0.4359(3) 0.92964(13) 0.0471(6) Uani 1 1 d . . . . .
H8 H 0.626491 0.484911 0.964834 0.057 Uiso 1 1 calc R U . . .
C27 C 0.6235(3) 0.3861(2) 0.58102(13) 0.0452(6) Uani 1 1 d . . . . .
H27 H 0.620832 0.359471 0.540109 0.054 Uiso 1 1 calc R U . . .
C4 C 0.3484(3) 0.1758(3) 0.87549(13) 0.0473(6) Uani 1 1 d . . . . .
H4 H 0.309121 0.210401 0.914668 0.057 Uiso 1 1 calc R U . . .
C1 C 0.4678(3) 0.0777(2) 0.76023(13) 0.0455(6) Uani 1 1 d . . . . .
H1 H 0.507965 0.044499 0.720762 0.055 Uiso 1 1 calc R U . . .
C34 C 0.4730(3) -0.1687(2) 0.91630(13) 0.0447(6) Uani 1 1 d . . . . .
C13 C 1.2268(3) 0.4086(3) 0.75265(14) 0.0502(7) Uani 1 1 d . . . . .
H13 H 1.311630 0.449745 0.755524 0.060 Uiso 1 1 calc R U . . .
C28 C 0.5629(4) 0.5019(3) 0.59773(16) 0.0546(7) Uani 1 1 d . . . . .
H28 H 0.517779 0.553797 0.568175 0.066 Uiso 1 1 calc R U . . .
C29 C 0.5700(3) 0.5393(2) 0.65795(16) 0.0537(7) Uani 1 1 d . . . . .
H29 H 0.533546 0.617957 0.669096 0.064 Uiso 1 1 calc R U . . .
C14 C 1.2292(3) 0.3348(3) 0.70221(14) 0.0500(7) Uani 1 1 d . . . . .
H14 H 1.315449 0.325237 0.670664 0.060 Uiso 1 1 calc R U . . .
C2 C 0.3266(3) 0.0453(3) 0.79185(16) 0.0565(8) Uani 1 1 d . . . . .
H2 H 0.273032 -0.008749 0.774041 0.068 Uiso 1 1 calc R U . . .
C3 C 0.2673(3) 0.0946(3) 0.85000(16) 0.0589(8) Uani 1 1 d . . . . .
H3 H 0.172980 0.073582 0.872258 0.071 Uiso 1 1 calc R U . . .
H9 H 0.865(3) 0.492(3) 0.9015(14) 0.044(7) Uiso 1 1 d . . . . .
O9 O 0.1895(2) 0.3932(2) 0.98108(13) 0.0639(6) Uani 1 1 d G . . . .
H9A H 0.147297 0.453094 0.961055 0.096 Uiso 1 1 d G U . . .
H9B H 0.117040 0.363029 1.007598 0.096 Uiso 1 1 d G 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 N5 1.8979(17) . ?
Co1 N2 1.9137(17) . ?
Co1 N4 2.0692(19) . ?
Co1 N1 2.0932(19) . ?
Co1 N6 2.0663(19) . ?
Co1 N3 2.097(2) . ?
Cl3 C38 1.729(2) . ?
Cl1 C32 1.739(2) . ?
Cl2 C35 1.724(3) . ?
Cl4 C41 1.734(3) . ?
O5 C37 1.248(3) . ?
N5 C21 1.355(3) . ?
N5 C25 1.351(3) . ?
N2 C10 1.351(3) . ?
N2 C6 1.349(3) . ?
O1 H1A 0.8200 . ?
O1 C31 1.280(3) . ?
N4 C20 1.358(3) . ?
N4 C16 1.338(3) . ?
N1 C11 1.357(3) . ?
N1 C15 1.337(3) . ?
N6 C26 1.356(3) . ?
N6 C30 1.339(3) . ?
N3 C5 1.357(3) . ?
N3 C1 1.339(3) . ?
O6 C39 1.238(3) . ?
O2 C33 1.222(3) . ?
O3 H3A 0.8200 . ?
O3 C34 1.318(3) . ?
O4 C36 1.212(3) . ?
O7 C40 1.264(3) . ?
C37 C38 1.394(3) . ?
C37 C36 1.542(3) . ?
C21 C20 1.473(3) . ?
C21 C22 1.391(3) . ?
C11 C10 1.473(3) . ?
C11 C12 1.382(3) . ?
C10 C9 1.387(3) . ?
C20 C19 1.385(3) . ?
C25 C26 1.471(3) . ?
C25 C24 1.387(3) . ?
C6 C5 1.477(3) . ?
C6 C7 1.387(3) . ?
C5 C4 1.383(3) . ?
C40 C42 1.514(4) 2_676 ?
C40 C41 1.380(4) . ?
C26 C27 1.384(3) . ?
C19 H19 0.9300 . ?
C19 C18 1.387(4) . ?
O8 C42 1.234(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.378(4) . ?
C38 C39 1.404(3) . ?
C31 C32 1.372(3) . ?
C31 C33 1.529(3) 2_766 ?
C16 H16 0.9300 . ?
C16 C17 1.378(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.386(3) . ?
C32 C33 1.420(4) . ?
C24 H24 0.9300 . ?
C24 C23 1.386(4) . ?
C9 C8 1.381(3) . ?
C9 H9 0.96(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.383(4) . ?
C15 H15 0.9300 . ?
C15 C14 1.384(4) . ?
C36 C35 1.443(3) . ?
C42 C41 1.411(4) . ?
C39 C34 1.510(4) . ?
C23 H23 0.9300 . ?
C18 H18 0.9300 . ?
C18 C17 1.373(4) . ?
C35 C34 1.345(3) . ?
C17 H17 0.9300 . ?
C30 H30 0.9300 . ?
C30 C29 1.383(4) . ?
C8 H8 0.9300 . ?
C27 H27 0.9300 . ?
C27 C28 1.387(4) . ?
C4 H4 0.9300 . ?
C4 C3 1.387(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.385(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.374(4) . ?
C28 H28 0.9300 . ?
C28 C29 1.367(4) . ?
C29 H29 0.9300 . ?
C14 H14 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.373(4) . ?
C3 H3 0.9300 . ?
O9 H9A 0.8502 . ?
O9 H9B 0.8499 . ?

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 Co1 N2 176.88(7) . . ?
N5 Co1 N4 79.87(7) . . ?
N5 Co1 N1 101.53(7) . . ?
N5 Co1 N6 80.25(7) . . ?
N5 Co1 N3 99.23(7) . . ?
N2 Co1 N4 103.02(7) . . ?
N2 Co1 N1 79.66(7) . . ?
N2 Co1 N6 96.86(7) . . ?
N2 Co1 N3 79.66(7) . . ?
N4 Co1 N1 91.78(7) . . ?
N4 Co1 N3 90.76(7) . . ?
N1 Co1 N3 159.21(7) . . ?
N6 Co1 N4 160.11(7) . . ?
N6 Co1 N1 92.23(7) . . ?
N6 Co1 N3 92.36(8) . . ?
C21 N5 Co1 119.84(14) . . ?
C25 N5 Co1 119.32(14) . . ?
C25 N5 C21 120.79(18) . . ?
C10 N2 Co1 119.34(14) . . ?
C6 N2 Co1 119.50(14) . . ?
C6 N2 C10 120.77(17) . . ?
C31 O1 H1A 109.5 . . ?
C20 N4 Co1 113.35(14) . . ?
C16 N4 Co1 128.36(16) . . ?
C16 N4 C20 118.3(2) . . ?
C11 N1 Co1 112.90(14) . . ?
C15 N1 Co1 128.78(15) . . ?
C15 N1 C11 118.32(19) . . ?
C26 N6 Co1 112.78(14) . . ?
C30 N6 Co1 128.62(17) . . ?
C30 N6 C26 118.4(2) . . ?
C5 N3 Co1 112.90(14) . . ?
C1 N3 Co1 128.59(17) . . ?
C1 N3 C5 118.4(2) . . ?
C34 O3 H3A 109.5 . . ?
O5 C37 C38 125.9(2) . . ?
O5 C37 C36 116.7(2) . . ?
C38 C37 C36 117.3(2) . . ?
N5 C21 C20 113.00(18) . . ?
N5 C21 C22 120.7(2) . . ?
C22 C21 C20 126.3(2) . . ?
N1 C11 C10 114.03(18) . . ?
N1 C11 C12 122.1(2) . . ?
C12 C11 C10 123.90(19) . . ?
N2 C10 C11 113.71(17) . . ?
N2 C10 C9 120.6(2) . . ?
C9 C10 C11 125.7(2) . . ?
N4 C20 C21 113.72(18) . . ?
N4 C20 C19 121.8(2) . . ?
C19 C20 C21 124.4(2) . . ?
N5 C25 C26 113.22(18) . . ?
N5 C25 C24 120.3(2) . . ?
C24 C25 C26 126.4(2) . . ?
N2 C6 C5 113.76(18) . . ?
N2 C6 C7 120.8(2) . . ?
C7 C6 C5 125.4(2) . . ?
N3 C5 C6 113.87(19) . . ?
N3 C5 C4 121.9(2) . . ?
C4 C5 C6 124.2(2) . . ?
O7 C40 C42 115.7(2) . 2_676 ?
O7 C40 C41 125.1(3) . . ?
C41 C40 C42 119.1(2) . 2_676 ?
N6 C26 C25 114.07(19) . . ?
N6 C26 C27 122.0(2) . . ?
C27 C26 C25 123.9(2) . . ?
C20 C19 H19 120.6 . . ?
C20 C19 C18 118.8(2) . . ?
C18 C19 H19 120.6 . . ?
C21 C22 H22 120.6 . . ?
C23 C22 C21 118.7(2) . . ?
C23 C22 H22 120.6 . . ?
C37 C38 Cl3 118.71(18) . . ?
C37 C38 C39 123.5(2) . . ?
C39 C38 Cl3 117.77(18) . . ?
O1 C31 C32 123.6(2) . . ?
O1 C31 C33 117.5(2) . 2_766 ?
C32 C31 C33 118.9(2) . 2_766 ?
N4 C16 H16 118.7 . . ?
N4 C16 C17 122.6(2) . . ?
C17 C16 H16 118.7 . . ?
C11 C12 H12 120.7 . . ?
C11 C12 C13 118.6(2) . . ?
C13 C12 H12 120.7 . . ?
C31 C32 Cl1 118.8(2) . . ?
C31 C32 C33 122.8(2) . . ?
C33 C32 Cl1 117.99(17) . . ?
C25 C24 H24 120.4 . . ?
C25 C24 C23 119.1(2) . . ?
C23 C24 H24 120.4 . . ?
O2 C33 C31 117.2(2) . 2_766 ?
O2 C33 C32 124.8(2) . . ?
C32 C33 C31 118.01(19) . 2_766 ?
C10 C9 H9 121.8(18) . . ?
C8 C9 C10 118.7(2) . . ?
C8 C9 H9 119.5(17) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 C6 118.5(2) . . ?
C8 C7 H7 120.7 . . ?
N1 C15 H15 118.7 . . ?
N1 C15 C14 122.6(2) . . ?
C14 C15 H15 118.7 . . ?
O4 C36 C37 118.6(2) . . ?
O4 C36 C35 122.8(3) . . ?
C35 C36 C37 118.6(2) . . ?
O8 C42 C40 117.6(3) . 2_676 ?
O8 C42 C41 123.9(3) . . ?
C41 C42 C40 118.4(2) . 2_676 ?
O6 C39 C38 125.8(2) . . ?
O6 C39 C34 116.6(2) . . ?
C38 C39 C34 117.6(2) . . ?
C22 C23 C24 120.3(2) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C40 C41 Cl4 118.0(2) . . ?
C40 C41 C42 122.4(2) . . ?
C42 C41 Cl4 119.6(2) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 C19 119.2(2) . . ?
C17 C18 H18 120.4 . . ?
C36 C35 Cl2 118.32(19) . . ?
C34 C35 Cl2 120.7(2) . . ?
C34 C35 C36 121.0(2) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 C16 119.2(2) . . ?
C18 C17 H17 120.4 . . ?
N6 C30 H30 118.9 . . ?
N6 C30 C29 122.2(3) . . ?
C29 C30 H30 118.9 . . ?
C9 C8 C7 120.5(2) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C26 C27 H27 120.8 . . ?
C26 C27 C28 118.5(3) . . ?
C28 C27 H27 120.8 . . ?
C5 C4 H4 120.7 . . ?
C5 C4 C3 118.6(2) . . ?
C3 C4 H4 120.7 . . ?
N3 C1 H1 118.7 . . ?
N3 C1 C2 122.6(2) . . ?
C2 C1 H1 118.7 . . ?
O3 C34 C39 116.0(2) . . ?
O3 C34 C35 122.2(2) . . ?
C35 C34 C39 121.8(2) . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13 120.2 . . ?
C27 C28 H28 120.2 . . ?
C29 C28 C27 119.6(3) . . ?
C29 C28 H28 120.2 . . ?
C30 C29 H29 120.4 . . ?
C28 C29 C30 119.2(2) . . ?
C28 C29 H29 120.4 . . ?
C15 C14 H14 120.6 . . ?
C13 C14 C15 118.7(2) . . ?
C13 C14 H14 120.6 . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.6(2) . . ?
C3 C2 H2 120.7 . . ?
C4 C3 H3 120.1 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
H9A O9 H9B 104.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N5 C21 C20 -1.1(2) . . . . ?
Co1 N5 C21 C22 176.67(18) . . . . ?
Co1 N5 C25 C26 1.3(2) . . . . ?
Co1 N5 C25 C24 -178.19(17) . . . . ?
Co1 N2 C10 C11 -6.9(2) . . . . ?
Co1 N2 C10 C9 172.55(18) . . . . ?
Co1 N2 C6 C5 6.2(3) . . . . ?
Co1 N2 C6 C7 -172.45(18) . . . . ?
Co1 N4 C20 C21 -5.3(2) . . . . ?
Co1 N4 C20 C19 176.25(18) . . . . ?
Co1 N4 C16 C17 -176.97(19) . . . . ?
Co1 N1 C11 C10 0.6(2) . . . . ?
Co1 N1 C11 C12 -179.47(19) . . . . ?
Co1 N1 C15 C14 179.0(2) . . . . ?
Co1 N6 C26 C25 -6.3(2) . . . . ?
Co1 N6 C26 C27 172.57(19) . . . . ?
Co1 N6 C30 C29 -173.8(2) . . . . ?
Co1 N3 C5 C6 3.0(2) . . . . ?
Co1 N3 C5 C4 -176.2(2) . . . . ?
Co1 N3 C1 C2 175.7(2) . . . . ?
Cl3 C38 C39 O6 2.3(4) . . . . ?
Cl3 C38 C39 C34 -178.1(2) . . . . ?
Cl1 C32 C33 O2 0.1(4) . . . . ?
Cl1 C32 C33 C31 -179.11(19) . . . 2_766 ?
Cl2 C35 C34 O3 -2.1(5) . . . . ?
Cl2 C35 C34 C39 176.6(2) . . . . ?
O5 C37 C38 Cl3 -1.2(4) . . . . ?
O5 C37 C38 C39 175.6(2) . . . . ?
O5 C37 C36 O4 1.6(4) . . . . ?
O5 C37 C36 C35 -179.1(2) . . . . ?
N5 C21 C20 N4 4.3(3) . . . . ?
N5 C21 C20 C19 -177.3(2) . . . . ?
N5 C21 C22 C23 0.8(4) . . . . ?
N5 C25 C26 N6 3.5(3) . . . . ?
N5 C25 C26 C27 -175.3(2) . . . . ?
N5 C25 C24 C23 2.2(4) . . . . ?
N2 C10 C9 C8 0.0(4) . . . . ?
N2 C6 C5 N3 -5.8(3) . . . . ?
N2 C6 C5 C4 173.4(2) . . . . ?
N2 C6 C7 C8 -0.2(4) . . . . ?
O1 C31 C32 Cl1 -0.4(4) . . . . ?
O1 C31 C32 C33 -173.5(3) . . . . ?
N4 Co1 N5 C21 -1.35(16) . . . . ?
N4 Co1 N5 C25 176.27(17) . . . . ?
N4 C20 C19 C18 1.2(4) . . . . ?
N4 C16 C17 C18 0.7(4) . . . . ?
N1 Co1 N5 C21 88.41(17) . . . . ?
N1 Co1 N5 C25 -93.97(16) . . . . ?
N1 C11 C10 N2 3.8(3) . . . . ?
N1 C11 C10 C9 -175.7(2) . . . . ?
N1 C11 C12 C13 0.5(4) . . . . ?
N1 C15 C14 C13 0.1(5) . . . . ?
N6 Co1 N5 C21 178.71(17) . . . . ?
N6 Co1 N5 C25 -3.67(16) . . . . ?
N6 C26 C27 C28 2.1(4) . . . . ?
N6 C30 C29 C28 2.0(4) . . . . ?
N3 Co1 N5 C21 -90.46(17) . . . . ?
N3 Co1 N5 C25 87.16(16) . . . . ?
N3 C5 C4 C3 -0.2(4) . . . . ?
N3 C1 C2 C3 0.2(5) . . . . ?
O6 C39 C34 O3 -2.7(4) . . . . ?
O6 C39 C34 C35 178.6(3) . . . . ?
O4 C36 C35 Cl2 2.3(4) . . . . ?
O4 C36 C35 C34 -178.8(3) . . . . ?
O7 C40 C41 Cl4 2.9(4) . . . . ?
O7 C40 C41 C42 -178.5(3) . . . . ?
C37 C38 C39 O6 -174.6(3) . . . . ?
C37 C38 C39 C34 5.1(4) . . . . ?
C37 C36 C35 Cl2 -177.0(2) . . . . ?
C37 C36 C35 C34 1.9(4) . . . . ?
C21 N5 C25 C26 178.91(19) . . . . ?
C21 N5 C25 C24 -0.6(3) . . . . ?
C21 C20 C19 C18 -177.1(2) . . . . ?
C21 C22 C23 C24 0.9(4) . . . . ?
C11 N1 C15 C14 0.0(4) . . . . ?
C11 C10 C9 C8 179.4(2) . . . . ?
C11 C12 C13 C14 -0.4(4) . . . . ?
C10 N2 C6 C5 179.04(19) . . . . ?
C10 N2 C6 C7 0.4(3) . . . . ?
C10 C11 C12 C13 -179.6(2) . . . . ?
C10 C9 C8 C7 0.1(4) . . . . ?
C20 N4 C16 C17 1.5(3) . . . . ?
C20 C21 C22 C23 178.2(2) . . . . ?
C20 C19 C18 C17 1.0(4) . . . . ?
C25 N5 C21 C20 -178.69(18) . . . . ?
C25 N5 C21 C22 -0.9(3) . . . . ?
C25 C26 C27 C28 -179.2(2) . . . . ?
C25 C24 C23 C22 -2.3(4) . . . . ?
C6 N2 C10 C11 -179.74(19) . . . . ?
C6 N2 C10 C9 -0.3(3) . . . . ?
C6 C5 C4 C3 -179.3(3) . . . . ?
C6 C7 C8 C9 0.0(4) . . . . ?
C5 N3 C1 C2 -0.8(4) . . . . ?
C5 C6 C7 C8 -178.7(2) . . . . ?
C5 C4 C3 C2 -0.5(5) . . . . ?
C40 C42 C41 Cl4 179.24(19) 2_676 . . . ?
C40 C42 C41 C40 0.6(4) 2_676 . . . ?
C26 N6 C30 C29 0.8(4) . . . . ?
C26 C25 C24 C23 -177.2(2) . . . . ?
C26 C27 C28 C29 0.7(4) . . . . ?
C19 C18 C17 C16 -1.9(4) . . . . ?
O8 C42 C41 Cl4 0.2(4) . . . . ?
O8 C42 C41 C40 -178.4(3) . . . . ?
C22 C21 C20 N4 -173.3(2) . . . . ?
C22 C21 C20 C19 5.1(4) . . . . ?
C38 C37 C36 O4 -177.5(3) . . . . ?
C38 C37 C36 C35 1.8(4) . . . . ?
C38 C39 C34 O3 177.6(3) . . . . ?
C38 C39 C34 C35 -1.1(4) . . . . ?
C31 C32 C33 O2 173.3(3) . . . . ?
C31 C32 C33 C31 -6.0(4) . . . 2_766 ?
C16 N4 C20 C21 176.0(2) . . . . ?
C16 N4 C20 C19 -2.4(3) . . . . ?
C12 C11 C10 N2 -176.2(2) . . . . ?
C12 C11 C10 C9 4.4(4) . . . . ?
C12 C13 C14 C15 0.1(5) . . . . ?
C24 C25 C26 N6 -177.0(2) . . . . ?
C24 C25 C26 C27 4.2(4) . . . . ?
C33 C31 C32 Cl1 179.10(19) 2_766 . . . ?
C33 C31 C32 C33 6.0(4) 2_766 . . . ?
C7 C6 C5 N3 172.8(2) . . . . ?
C7 C6 C5 C4 -8.0(4) . . . . ?
C15 N1 C11 C10 179.8(2) . . . . ?
C15 N1 C11 C12 -0.3(3) . . . . ?
C36 C37 C38 Cl3 177.86(18) . . . . ?
C36 C37 C38 C39 -5.3(4) . . . . ?
C36 C35 C34 O3 179.1(3) . . . . ?
C36 C35 C34 C39 -2.3(5) . . . . ?
C42 C40 C41 Cl4 -179.27(19) 2_676 . . . ?
C42 C40 C41 C42 -0.6(4) 2_676 . . . ?
C30 N6 C26 C25 178.3(2) . . . . ?
C30 N6 C26 C27 -2.9(3) . . . . ?
C27 C28 C29 C30 -2.7(5) . . . . ?
C1 N3 C5 C6 -180.0(2) . . . . ?
C1 N3 C5 C4 0.8(4) . . . . ?
C1 C2 C3 C4 0.5(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.367
_oxdiff_exptl_absorpt_empirical_full_min 0.873
####################################################################### 
# 
# 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_exp_706
_database_code_depnum_ccdc_archive 'CCDC 2374766'
loop_
_audit_author_name
_audit_author_address
'Akio Mishima'
;Fukuoka University
Japan
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_audit_creation_date             2024-07-31
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 N6 Ni, 2(C3 Cl0.985 O2), 6(H2 O)'
_chemical_formula_sum            'C36 H34 Cl1.99 N6 Ni O10.01'
_chemical_formula_weight         840.11
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H20N10O10Ni1Cl2
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'

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

_cell_length_a                   9.0426(2)
_cell_length_b                   9.0675(3)
_cell_length_c                   22.4477(6)
_cell_angle_alpha                92.511(2)
_cell_angle_beta                 96.200(2)
_cell_angle_gamma                90.655(2)
_cell_volume                     1827.81(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    13533
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.3800
_cell_measurement_theta_min      2.2500
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             868
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35522
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.586
_diffrn_reflns_theta_min         2.249
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 -32.00   0.50   24.00    --   20.00  54.00   0.00   84
  2  ω    -17.00   9.00   0.50   24.00    --   20.00  54.00   0.00   52
  3  ω     28.00  55.00   0.50   24.00    --   20.00  54.00   0.00   54
  4  ω    -71.00 -44.00   0.50   24.00    --   20.00  54.00 150.00   54
  5  ω    -17.00   9.00   0.50   24.00    --   20.00  54.00 150.00   52
  6  ω     44.00  70.00   0.50   24.00    --   20.00  54.00 150.00   52
  7  ω    -74.00  59.00   0.50   24.00    --   20.00  54.00-120.00  266
  8  ω     66.00 108.00   0.50   24.00    --   20.00  54.00-120.00   84
  9  ω    -70.00 -45.00   0.50   24.00    --   20.00  54.00 -60.00   50
 10  ω      3.00  29.00   0.50   24.00    --   20.00  54.00 -60.00   52
 11  ω     59.00  84.00   0.50   24.00    --   20.00  54.00 -60.00   50
 12  ω    -66.00 -23.00   0.50   24.00    --   20.00  54.00-150.00   86
 13  ω    -17.00  27.00   0.50   24.00    --   20.00  54.00-150.00   88
 14  ω    -11.00  22.00   0.50   24.00    --   20.00  54.00  90.00   66
 15  ω    -65.00 100.00   0.50   24.00    --   20.00  54.00  30.00  330
 16  ω    -42.00 -17.00   0.50   24.00    --   20.00  54.00 -30.00   50
 17  ω     -8.00  47.00   0.50   24.00    --   20.00  54.00 -30.00  110
 18  ω    -74.00 -49.00   0.50   24.00    --   20.00  54.00-180.00   50
 19  ω     84.00 109.00   0.50   24.00    --   20.00  54.00 -90.00   50
 20  ω    -73.00  45.00   0.50   24.00    --   20.00  54.00 120.00  236
 21  ω    -68.00  60.00   0.50   24.00    --   20.00  54.00  76.12  256
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0198928000
_diffrn_orient_matrix_UB_12      -0.0297613000
_diffrn_orient_matrix_UB_13      0.0284030000
_diffrn_orient_matrix_UB_21      -0.0102626000
_diffrn_orient_matrix_UB_22      0.0699932000
_diffrn_orient_matrix_UB_23      0.0142059000
_diffrn_orient_matrix_UB_31      -0.0756701000
_diffrn_orient_matrix_UB_32      -0.0186449000
_diffrn_orient_matrix_UB_33      0.0019367000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7688
_reflns_number_total             10601
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         10601
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0546
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0451P)²+0.9411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1185
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B), O5(H5A,H5B), O6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C1(H1), C16(H16), C24(H24), C12(H12), C9(H9), C7(H7), C22(H22),
 C27(H27), C30(H30), C8(H8), C23(H23), C29(H29), C17(H17), C4(H4), C14(H14),
 C19(H19), C28(H28), C2(H2), C13(H13), C18(H18), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni01 Ni 0.71717(3) 0.32373(3) 0.24973(2) 0.03001(8) Uani 1 1 d . . . . .
Cl02 Cl 0.81743(9) -0.20091(9) 0.39779(3) 0.0619(3) Uani 0.985(3) 1 d . . . A 1
O1 O 0.71389(19) -0.0814(2) 0.51281(8) 0.0497(4) Uani 1 1 d . . . . .
O3 O 1.0775(2) 0.2121(2) -0.01250(9) 0.0526(5) Uani 1 1 d . . . . .
O7 O 0.7046(3) 0.6051(2) 0.52116(9) 0.0589(5) Uani 1 1 d G . . . .
H7A H 0.648442 0.578504 0.489558 0.088 Uiso 1 1 d G U . . .
H7B H 0.718227 0.698111 0.522208 0.088 Uiso 1 1 d G U . . .
N2 N 0.7412(2) 0.3200(2) 0.33881(8) 0.0329(4) Uani 1 1 d . . . . .
O8 O 0.5012(2) 0.5517(2) 0.41528(10) 0.0581(5) Uani 1 1 d G . . . .
H8A H 0.472102 0.640560 0.415310 0.087 Uiso 1 1 d G U . . .
H8B H 0.435654 0.505351 0.431913 0.087 Uiso 1 1 d G U . . .
O9 O 0.3888(2) 0.1861(3) -0.02087(9) 0.0582(5) Uani 1 1 d G . . . .
H9A H 0.296915 0.201104 -0.018572 0.087 Uiso 1 1 d G U . . .
H9B H 0.419694 0.149583 0.012367 0.087 Uiso 1 1 d G U . . .
N3 N 0.5131(2) 0.2299(2) 0.26637(8) 0.0343(4) Uani 1 1 d . . . . .
N5 N 0.7022(2) 0.3262(2) 0.16067(8) 0.0341(4) Uani 1 1 d . . . . .
N6 N 0.8041(2) 0.1163(2) 0.22789(8) 0.0360(4) Uani 1 1 d . . . . .
N1 N 0.9312(2) 0.4190(2) 0.27086(8) 0.0358(4) Uani 1 1 d . . . . .
O4 O 1.1069(2) 0.6667(2) 0.09721(9) 0.0614(6) Uani 1 1 d . . . . .
O2 O 1.1278(2) -0.0870(2) 0.40185(9) 0.0598(5) Uani 1 1 d . . . . .
O10 O 0.4659(2) 0.0352(2) 0.08827(10) 0.0629(5) Uani 1 1 d G . . . .
H10A H 0.375967 0.004933 0.085287 0.094 Uiso 1 1 d G U . . .
H10B H 0.516030 -0.023142 0.067984 0.094 Uiso 1 1 d G U . . .
N4 N 0.6209(2) 0.5311(2) 0.23399(8) 0.0353(4) Uani 1 1 d . . . . .
O5 O 0.4517(3) -0.1517(2) 0.42211(12) 0.0730(6) Uani 1 1 d G . . . .
H5A H 0.526827 -0.108671 0.441703 0.110 Uiso 1 1 d G U . . .
H5B H 0.379091 -0.096448 0.428309 0.110 Uiso 1 1 d G U . . .
C10 C 0.6326(3) 0.2579(2) 0.36652(10) 0.0346(5) Uani 1 1 d . . . . .
O6 O 1.1688(3) -0.0183(3) 0.07511(14) 0.0853(8) Uani 1 1 d G . . . .
H6A H 1.131015 0.034355 0.047158 0.128 Uiso 1 1 d G U . . .
H6B H 1.112969 -0.094838 0.072862 0.128 Uiso 1 1 d G U . . .
C26 C 0.8102(3) 0.0905(3) 0.16810(11) 0.0390(5) Uani 1 1 d . . . . .
C36 C 1.0595(3) 0.5857(3) 0.05380(11) 0.0412(5) Uani 1 1 d . . . . .
C33 C 1.0639(3) -0.0490(3) 0.44601(11) 0.0391(5) Uani 1 1 d . . . . .
C11 C 0.4991(3) 0.2119(3) 0.32507(10) 0.0359(5) Uani 1 1 d . . . . .
C31 C 0.8458(3) -0.0479(3) 0.50418(11) 0.0371(5) Uani 1 1 d . . . . .
C25 C 0.7542(3) 0.2119(3) 0.13007(10) 0.0376(5) Uani 1 1 d . . . . .
C21 C 0.6468(3) 0.4458(3) 0.13326(10) 0.0383(5) Uani 1 1 d . . . . .
C34 C 1.0459(3) 0.3458(3) -0.00378(11) 0.0393(5) Uani 1 1 d . . . . .
C5 C 0.9753(3) 0.4335(3) 0.33039(10) 0.0379(5) Uani 1 1 d . . . . .
C32 C 0.9165(3) -0.0903(3) 0.45429(11) 0.0403(5) Uani 1 1 d . . . . .
C6 C 0.8697(3) 0.3698(3) 0.36901(10) 0.0370(5) Uani 1 1 d . . . . .
C35 C 1.0964(3) 0.4352(3) 0.04590(11) 0.0413(5) Uani 1 1 d . . . . .
C15 C 0.3987(3) 0.1888(3) 0.22557(11) 0.0422(6) Uani 1 1 d . . . . .
H15 H 0.408250 0.199898 0.185171 0.051 Uiso 1 1 calc R U . . .
C1 C 1.0205(3) 0.4728(3) 0.23263(11) 0.0426(6) Uani 1 1 d . . . . .
H1 H 0.990866 0.461251 0.191691 0.051 Uiso 1 1 calc R U . . .
C16 C 0.5813(3) 0.6295(3) 0.27517(11) 0.0418(5) Uani 1 1 d . . . . .
H16 H 0.598602 0.608598 0.315495 0.050 Uiso 1 1 calc R U . . .
C24 C 0.7529(3) 0.2143(3) 0.06783(11) 0.0495(7) Uani 1 1 d . . . . .
H24 H 0.789780 0.135802 0.046151 0.059 Uiso 1 1 calc R U . . .
C12 C 0.3703(3) 0.1540(3) 0.34369(12) 0.0484(6) Uani 1 1 d . . . . .
H12 H 0.362587 0.143045 0.384245 0.058 Uiso 1 1 calc R U . . .
C9 C 0.6522(3) 0.2426(3) 0.42813(10) 0.0452(6) Uani 1 1 d . . . . .
H9 H 0.578637 0.198857 0.447664 0.054 Uiso 1 1 calc R U . . .
C7 C 0.8943(3) 0.3574(3) 0.43101(11) 0.0482(6) Uani 1 1 d . . . . .
H7 H 0.982928 0.390981 0.452413 0.058 Uiso 1 1 calc R U . . .
C20 C 0.5972(3) 0.5614(3) 0.17506(10) 0.0388(5) Uani 1 1 d . . . . .
C22 C 0.6419(3) 0.4537(3) 0.07129(11) 0.0503(7) Uani 1 1 d . . . . .
H22 H 0.603657 0.535810 0.051958 0.060 Uiso 1 1 calc R U . . .
C27 C 0.8664(3) -0.0406(3) 0.14652(13) 0.0523(7) Uani 1 1 d . . . . .
H27 H 0.869649 -0.057860 0.105540 0.063 Uiso 1 1 calc R U . . .
C30 C 0.8525(3) 0.0125(3) 0.26599(12) 0.0438(6) Uani 1 1 d . . . . .
H30 H 0.846577 0.029740 0.306800 0.053 Uiso 1 1 calc R U . . .
C8 C 0.7838(3) 0.2939(3) 0.45980(11) 0.0516(7) Uani 1 1 d . . . . .
H8 H 0.798088 0.285582 0.501156 0.062 Uiso 1 1 calc R U . . .
C23 C 0.6955(3) 0.3362(4) 0.03937(11) 0.0551(8) Uani 1 1 d . . . . .
H23 H 0.692798 0.339242 -0.002086 0.066 Uiso 1 1 calc R U . . .
C29 C 0.9108(3) -0.1191(3) 0.24651(14) 0.0563(7) Uani 1 1 d . . . . .
H29 H 0.944812 -0.188736 0.273773 0.068 Uiso 1 1 calc R U . . .
C17 C 0.5151(3) 0.7622(3) 0.25973(13) 0.0543(7) Uani 1 1 d . . . . .
H17 H 0.488238 0.829117 0.289102 0.065 Uiso 1 1 calc R U . . .
C4 C 1.1071(3) 0.5043(4) 0.35200(13) 0.0589(8) Uani 1 1 d . . . . .
H4 H 1.136101 0.513761 0.393037 0.071 Uiso 1 1 calc R U . . .
C14 C 0.2665(3) 0.1304(3) 0.24151(14) 0.0541(7) Uani 1 1 d . . . . .
H14 H 0.188456 0.103827 0.212443 0.065 Uiso 1 1 calc R U . . .
C19 C 0.5315(4) 0.6907(3) 0.15730(13) 0.0580(8) Uani 1 1 d . . . . .
H19 H 0.514822 0.709966 0.116788 0.070 Uiso 1 1 calc R U . . .
C28 C 0.9175(3) -0.1451(3) 0.18614(15) 0.0594(8) Uani 1 1 d . . . . .
H28 H 0.956315 -0.232905 0.172060 0.071 Uiso 1 1 calc R U . . .
C2 C 1.1542(3) 0.5445(4) 0.25128(14) 0.0569(7) Uani 1 1 d . . . . .
H2 H 1.213937 0.580202 0.223735 0.068 Uiso 1 1 calc R U . . .
C13 C 0.2539(3) 0.1129(4) 0.30143(14) 0.0602(8) Uani 1 1 d . . . . .
H13 H 0.166943 0.073365 0.313254 0.072 Uiso 1 1 calc R U . . .
C18 C 0.4904(4) 0.7919(3) 0.20017(15) 0.0683(9) Uani 1 1 d . . . . .
H18 H 0.446156 0.879806 0.188624 0.082 Uiso 1 1 calc R U . . .
C3 C 1.1956(4) 0.5611(4) 0.31168(15) 0.0729(10) Uani 1 1 d . . . . .
H3 H 1.283906 0.610845 0.325709 0.087 Uiso 1 1 calc R U . . .
Cl2 Cl 1.21718(10) 0.36117(9) 0.10222(3) 0.0703(2) 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
Ni01 N2 1.9897(18) . ?
Ni01 N3 2.0999(19) . ?
Ni01 N5 1.9904(18) . ?
Ni01 N6 2.1050(19) . ?
Ni01 N1 2.1081(19) . ?
Ni01 N4 2.1091(19) . ?
Cl02 C32 1.744(3) . ?
O1 C31 1.265(3) . ?
O3 C34 1.260(3) . ?
O7 H7A 0.8504 . ?
O7 H7B 0.8500 . ?
N2 C10 1.349(3) . ?
N2 C6 1.343(3) . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8504 . ?
O9 H9A 0.8499 . ?
O9 H9B 0.8504 . ?
N3 C11 1.354(3) . ?
N3 C15 1.343(3) . ?
N5 C25 1.336(3) . ?
N5 C21 1.345(3) . ?
N6 C26 1.359(3) . ?
N6 C30 1.345(3) . ?
N1 C5 1.353(3) . ?
N1 C1 1.343(3) . ?
O4 C36 1.230(3) . ?
O2 C33 1.239(3) . ?
O10 H10A 0.8501 . ?
O10 H10B 0.8495 . ?
N4 C16 1.336(3) . ?
N4 C20 1.358(3) . ?
O5 H5A 0.8497 . ?
O5 H5B 0.8502 . ?
C10 C11 1.486(3) . ?
C10 C9 1.389(3) . ?
O6 H6A 0.8501 . ?
O6 H6B 0.8500 . ?
C26 C25 1.482(4) . ?
C26 C27 1.387(3) . ?
C36 C34 1.549(3) 2_765 ?
C36 C35 1.416(3) . ?
C33 C31 1.546(3) 2_756 ?
C33 C32 1.414(3) . ?
C11 C12 1.385(3) . ?
C31 C32 1.390(3) . ?
C25 C24 1.397(3) . ?
C21 C20 1.482(3) . ?
C21 C22 1.392(3) . ?
C34 C35 1.383(3) . ?
C5 C6 1.485(3) . ?
C5 C4 1.378(4) . ?
C6 C7 1.395(3) . ?
C35 Cl2 1.742(3) . ?
C15 H15 0.9300 . ?
C15 C14 1.390(4) . ?
C1 H1 0.9300 . ?
C1 C2 1.382(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.391(4) . ?
C24 H24 0.9300 . ?
C24 C23 1.379(4) . ?
C12 H12 0.9300 . ?
C12 C13 1.375(4) . ?
C9 H9 0.9300 . ?
C9 C8 1.383(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.380(4) . ?
C20 C19 1.376(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.379(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.377(4) . ?
C30 H30 0.9300 . ?
C30 C29 1.382(4) . ?
C8 H8 0.9300 . ?
C23 H23 0.9300 . ?
C29 H29 0.9300 . ?
C29 C28 1.373(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.371(4) . ?
C4 H4 0.9300 . ?
C4 C3 1.383(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.378(4) . ?
C19 H19 0.9300 . ?
C19 C18 1.384(4) . ?
C28 H28 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.369(4) . ?
C13 H13 0.9300 . ?
C18 H18 0.9300 . ?
C3 H3 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni01 N3 78.39(8) . . ?
N2 Ni01 N5 177.60(8) . . ?
N2 Ni01 N6 100.11(7) . . ?
N2 Ni01 N1 78.53(8) . . ?
N2 Ni01 N4 102.85(7) . . ?
N3 Ni01 N6 92.37(7) . . ?
N3 Ni01 N1 156.91(7) . . ?
N3 Ni01 N4 92.23(7) . . ?
N5 Ni01 N3 103.63(7) . . ?
N5 Ni01 N6 78.61(8) . . ?
N5 Ni01 N1 99.46(7) . . ?
N5 Ni01 N4 78.45(8) . . ?
N6 Ni01 N1 92.35(7) . . ?
N6 Ni01 N4 157.04(7) . . ?
N1 Ni01 N4 92.18(7) . . ?
H7A O7 H7B 109.4 . . ?
C10 N2 Ni01 118.93(15) . . ?
C6 N2 Ni01 118.78(16) . . ?
C6 N2 C10 122.1(2) . . ?
H8A O8 H8B 104.5 . . ?
H9A O9 H9B 104.5 . . ?
C11 N3 Ni01 114.50(15) . . ?
C15 N3 Ni01 127.00(16) . . ?
C15 N3 C11 118.5(2) . . ?
C25 N5 Ni01 118.93(16) . . ?
C25 N5 C21 121.9(2) . . ?
C21 N5 Ni01 119.09(15) . . ?
C26 N6 Ni01 113.62(16) . . ?
C30 N6 Ni01 127.27(16) . . ?
C30 N6 C26 119.1(2) . . ?
C5 N1 Ni01 113.98(16) . . ?
C1 N1 Ni01 127.37(16) . . ?
C1 N1 C5 118.5(2) . . ?
H10A O10 H10B 109.4 . . ?
C16 N4 Ni01 126.86(16) . . ?
C16 N4 C20 119.3(2) . . ?
C20 N4 Ni01 113.85(16) . . ?
H5A O5 H5B 104.5 . . ?
N2 C10 C11 113.52(19) . . ?
N2 C10 C9 120.0(2) . . ?
C9 C10 C11 126.5(2) . . ?
H6A O6 H6B 104.5 . . ?
N6 C26 C25 114.8(2) . . ?
N6 C26 C27 120.6(2) . . ?
C27 C26 C25 124.5(2) . . ?
O4 C36 C34 117.5(2) . 2_765 ?
O4 C36 C35 124.7(2) . . ?
C35 C36 C34 117.8(2) . 2_765 ?
O2 C33 C31 117.0(2) . 2_756 ?
O2 C33 C32 124.7(2) . . ?
C32 C33 C31 118.3(2) . 2_756 ?
N3 C11 C10 114.4(2) . . ?
N3 C11 C12 121.7(2) . . ?
C12 C11 C10 123.9(2) . . ?
O1 C31 C33 116.6(2) . 2_756 ?
O1 C31 C32 126.1(2) . . ?
C32 C31 C33 117.3(2) . 2_756 ?
N5 C25 C26 113.94(19) . . ?
N5 C25 C24 120.2(2) . . ?
C24 C25 C26 125.9(2) . . ?
N5 C21 C20 113.68(19) . . ?
N5 C21 C22 120.4(2) . . ?
C22 C21 C20 126.0(2) . . ?
O3 C34 C36 116.2(2) . 2_765 ?
O3 C34 C35 126.1(2) . . ?
C35 C34 C36 117.8(2) . 2_765 ?
N1 C5 C6 114.6(2) . . ?
N1 C5 C4 121.4(2) . . ?
C4 C5 C6 124.1(2) . . ?
C33 C32 Cl02 117.47(18) . . ?
C31 C32 Cl02 118.20(19) . . ?
C31 C32 C33 124.3(2) . . ?
N2 C6 C5 113.91(19) . . ?
N2 C6 C7 120.0(2) . . ?
C7 C6 C5 126.1(2) . . ?
C36 C35 Cl2 117.03(18) . . ?
C34 C35 C36 124.4(2) . . ?
C34 C35 Cl2 118.55(19) . . ?
N3 C15 H15 118.8 . . ?
N3 C15 C14 122.4(2) . . ?
C14 C15 H15 118.8 . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.1(2) . . ?
C2 C1 H1 118.5 . . ?
N4 C16 H16 118.9 . . ?
N4 C16 C17 122.2(2) . . ?
C17 C16 H16 118.9 . . ?
C25 C24 H24 120.9 . . ?
C23 C24 C25 118.3(3) . . ?
C23 C24 H24 120.9 . . ?
C11 C12 H12 120.4 . . ?
C13 C12 C11 119.1(2) . . ?
C13 C12 H12 120.4 . . ?
C10 C9 H9 120.8 . . ?
C8 C9 C10 118.5(3) . . ?
C8 C9 H9 120.8 . . ?
C6 C7 H7 120.8 . . ?
C8 C7 C6 118.4(3) . . ?
C8 C7 H7 120.8 . . ?
N4 C20 C21 114.9(2) . . ?
N4 C20 C19 120.9(2) . . ?
C19 C20 C21 124.2(2) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 C21 118.1(3) . . ?
C23 C22 H22 120.9 . . ?
C26 C27 H27 120.2 . . ?
C28 C27 C26 119.6(3) . . ?
C28 C27 H27 120.2 . . ?
N6 C30 H30 118.9 . . ?
N6 C30 C29 122.2(2) . . ?
C29 C30 H30 118.9 . . ?
C9 C8 H8 119.5 . . ?
C7 C8 C9 121.1(2) . . ?
C7 C8 H8 119.5 . . ?
C24 C23 H23 119.4 . . ?
C22 C23 C24 121.2(2) . . ?
C22 C23 H23 119.4 . . ?
C30 C29 H29 120.6 . . ?
C28 C29 C30 118.7(3) . . ?
C28 C29 H29 120.6 . . ?
C16 C17 H17 120.8 . . ?
C18 C17 C16 118.4(3) . . ?
C18 C17 H17 120.8 . . ?
C5 C4 H4 120.5 . . ?
C5 C4 C3 118.9(3) . . ?
C3 C4 H4 120.5 . . ?
C15 C14 H14 120.8 . . ?
C13 C14 C15 118.4(3) . . ?
C13 C14 H14 120.8 . . ?
C20 C19 H19 120.3 . . ?
C20 C19 C18 119.5(3) . . ?
C18 C19 H19 120.3 . . ?
C27 C28 H28 120.1 . . ?
C29 C28 C27 119.7(3) . . ?
C29 C28 H28 120.1 . . ?
C1 C2 H2 121.2 . . ?
C3 C2 C1 117.7(3) . . ?
C3 C2 H2 121.2 . . ?
C12 C13 C14 119.9(3) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C17 C18 C19 119.7(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C4 C3 H3 119.8 . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 H3 119.8 . . ?

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
Ni01 N2 C10 C11 -5.6(2) . . . . ?
Ni01 N2 C10 C9 174.51(16) . . . . ?
Ni01 N2 C6 C5 4.5(3) . . . . ?
Ni01 N2 C6 C7 -174.76(17) . . . . ?
Ni01 N3 C11 C10 -1.7(2) . . . . ?
Ni01 N3 C11 C12 178.83(18) . . . . ?
Ni01 N3 C15 C14 -178.6(2) . . . . ?
Ni01 N5 C25 C26 3.4(3) . . . . ?
Ni01 N5 C25 C24 -176.37(17) . . . . ?
Ni01 N5 C21 C20 -2.3(3) . . . . ?
Ni01 N5 C21 C22 176.79(18) . . . . ?
Ni01 N6 C26 C25 -0.3(2) . . . . ?
Ni01 N6 C26 C27 179.23(19) . . . . ?
Ni01 N6 C30 C29 -178.5(2) . . . . ?
Ni01 N1 C5 C6 4.3(2) . . . . ?
Ni01 N1 C5 C4 -174.8(2) . . . . ?
Ni01 N1 C1 C2 174.4(2) . . . . ?
Ni01 N4 C16 C17 -178.4(2) . . . . ?
Ni01 N4 C20 C21 -1.6(3) . . . . ?
Ni01 N4 C20 C19 178.3(2) . . . . ?
O1 C31 C32 Cl02 -0.4(4) . . . . ?
O1 C31 C32 C33 179.2(2) . . . . ?
O3 C34 C35 C36 179.3(2) . . . . ?
O3 C34 C35 Cl2 1.0(4) . . . . ?
N2 C10 C11 N3 4.6(3) . . . . ?
N2 C10 C11 C12 -175.9(2) . . . . ?
N2 C10 C9 C8 0.8(3) . . . . ?
N2 C6 C7 C8 -0.3(4) . . . . ?
N3 C11 C12 C13 0.4(4) . . . . ?
N3 C15 C14 C13 -0.7(4) . . . . ?
N5 C25 C24 C23 -0.7(4) . . . . ?
N5 C21 C20 N4 2.5(3) . . . . ?
N5 C21 C20 C19 -177.3(2) . . . . ?
N5 C21 C22 C23 -0.1(4) . . . . ?
N6 C26 C25 N5 -1.9(3) . . . . ?
N6 C26 C25 C24 177.9(2) . . . . ?
N6 C26 C27 C28 -0.4(4) . . . . ?
N6 C30 C29 C28 -0.9(4) . . . . ?
N1 C5 C6 N2 -5.7(3) . . . . ?
N1 C5 C6 C7 173.5(2) . . . . ?
N1 C5 C4 C3 -0.1(4) . . . . ?
N1 C1 C2 C3 -0.3(4) . . . . ?
O4 C36 C35 C34 -178.2(3) . . . . ?
O4 C36 C35 Cl2 0.2(4) . . . . ?
O2 C33 C32 Cl02 -0.8(4) . . . . ?
O2 C33 C32 C31 179.6(3) . . . . ?
N4 C16 C17 C18 -0.1(4) . . . . ?
N4 C20 C19 C18 0.7(4) . . . . ?
C10 N2 C6 C5 179.62(19) . . . . ?
C10 N2 C6 C7 0.3(3) . . . . ?
C10 C11 C12 C13 -179.0(2) . . . . ?
C10 C9 C8 C7 -0.8(4) . . . . ?
C26 N6 C30 C29 1.1(4) . . . . ?
C26 C25 C24 C23 179.5(2) . . . . ?
C26 C27 C28 C29 0.7(4) . . . . ?
C36 C34 C35 C36 -0.7(4) 2_765 . . . ?
C36 C34 C35 Cl2 -179.08(17) 2_765 . . . ?
C33 C31 C32 Cl02 179.45(16) 2_756 . . . ?
C33 C31 C32 C33 -0.9(4) 2_756 . . . ?
C11 N3 C15 C14 0.8(4) . . . . ?
C11 C10 C9 C8 -179.1(2) . . . . ?
C11 C12 C13 C14 -0.3(4) . . . . ?
C31 C33 C32 Cl02 -179.44(17) 2_756 . . . ?
C31 C33 C32 C31 0.9(4) 2_756 . . . ?
C25 N5 C21 C20 -179.0(2) . . . . ?
C25 N5 C21 C22 0.1(3) . . . . ?
C25 C26 C27 C28 179.1(2) . . . . ?
C25 C24 C23 C22 0.7(4) . . . . ?
C21 N5 C25 C26 -179.9(2) . . . . ?
C21 N5 C25 C24 0.3(3) . . . . ?
C21 C20 C19 C18 -179.5(3) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
C34 C36 C35 C34 0.7(4) 2_765 . . . ?
C34 C36 C35 Cl2 179.11(17) 2_765 . . . ?
C5 N1 C1 C2 -1.1(4) . . . . ?
C5 C6 C7 C8 -179.5(2) . . . . ?
C5 C4 C3 C2 -1.3(5) . . . . ?
C6 N2 C10 C11 179.30(19) . . . . ?
C6 N2 C10 C9 -0.6(3) . . . . ?
C6 C5 C4 C3 -179.1(3) . . . . ?
C6 C7 C8 C9 0.6(4) . . . . ?
C15 N3 C11 C10 178.9(2) . . . . ?
C15 N3 C11 C12 -0.6(3) . . . . ?
C15 C14 C13 C12 0.5(5) . . . . ?
C1 N1 C5 C6 -179.7(2) . . . . ?
C1 N1 C5 C4 1.3(4) . . . . ?
C1 C2 C3 C4 1.5(5) . . . . ?
C16 N4 C20 C21 179.3(2) . . . . ?
C16 N4 C20 C19 -0.9(4) . . . . ?
C16 C17 C18 C19 -0.1(5) . . . . ?
C9 C10 C11 N3 -175.5(2) . . . . ?
C9 C10 C11 C12 4.0(4) . . . . ?
C20 N4 C16 C17 0.6(4) . . . . ?
C20 C21 C22 C23 178.9(2) . . . . ?
C20 C19 C18 C17 -0.2(5) . . . . ?
C22 C21 C20 N4 -176.6(2) . . . . ?
C22 C21 C20 C19 3.6(4) . . . . ?
C27 C26 C25 N5 178.6(2) . . . . ?
C27 C26 C25 C24 -1.7(4) . . . . ?
C30 N6 C26 C25 -180.0(2) . . . . ?
C30 N6 C26 C27 -0.4(3) . . . . ?
C30 C29 C28 C27 0.0(5) . . . . ?
C4 C5 C6 N2 173.3(2) . . . . ?
C4 C5 C6 C7 -7.5(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.058
_oxdiff_exptl_absorpt_empirical_full_min 0.948
####################################################################### 
# 
# 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_exp_709
_database_code_depnum_ccdc_archive 'CCDC 2374763'
loop_
_audit_author_name
_audit_author_address
'Akio Mishima'
;Fukuoka University
Japan
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_audit_creation_date             2024-06-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C30 H22 N6 Ni, C6 H Cl2 O4, C3 H Cl O2, C3 Cl O2, H2 O'
_chemical_formula_sum            'C42 H26 Cl4 N6 Ni O9'
_chemical_formula_weight         959.20
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N10O10Ni1Cl2
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'

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

_cell_length_a                   8.9581(3)
_cell_length_b                   11.0350(3)
_cell_length_c                   20.9833(5)
_cell_angle_alpha                85.086(2)
_cell_angle_beta                 80.136(2)
_cell_angle_gamma                85.180(2)
_cell_volume                     2030.99(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12079
_cell_measurement_temperature    293
_cell_measurement_theta_max      30.2750
_cell_measurement_theta_min      2.0310
_shelx_estimated_absorpt_T_max   0.855
_shelx_estimated_absorpt_T_min   0.643
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36938
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.549
_diffrn_reflns_theta_min         1.975
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     72.00 109.00   0.50   26.00    --   20.00  54.00 156.45   74
  2  ω    -72.00 -26.00   0.50   26.00    --   20.00  54.00  49.05   92
  3  ω      7.00 109.00   0.50   26.00    --   20.00  54.00  49.05  204
  4  ω    -70.00 -32.00   0.50   26.00    --   20.00  54.00 -90.00   76
  5  ω     28.00  75.00   0.50   26.00    --   20.00  54.00 -90.00   94
  6  ω    -72.00   5.00   0.50   26.00    --   20.00  54.00  -9.64  154
  7  ω     27.00  53.00   0.50   26.00    --   20.00  54.00  -9.64   52
  8  ω    -74.00 -17.00   0.50   26.00    --   20.00  54.00 120.00  114
  9  ω    -12.00  60.00   0.50   26.00    --   20.00  54.00 120.00  144
 10  ω    -73.00  74.00   0.50   26.00    --   20.00  54.00-150.00  294
 11  ω    -70.00 -45.00   0.50   26.00    --   20.00  54.00 -60.00   50
 12  ω    -18.00   7.00   0.50   26.00    --   20.00  54.00 -60.00   50
 13  ω     26.00  51.00   0.50   26.00    --   20.00  54.00 -60.00   50
 14  ω     69.00  94.00   0.50   26.00    --   20.00  54.00 -60.00   50
 15  ω    -63.00 -16.00   0.50   26.00    --   20.00  54.00  60.00   94
 16  ω     21.00  51.00   0.50   26.00    --   20.00  54.00  60.00   60
 17  ω    -65.00 -38.00   0.50   26.00    --   20.00  54.00 -30.00   54
 18  ω     82.00 107.00   0.50   26.00    --   20.00  54.00 -30.00   50
 19  ω    -71.00  49.00   0.50   26.00    --   20.00  54.00-180.00  240
 20  ω     21.00  52.00   0.50   26.00    --   20.00  54.00 156.45   62
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0079681000
_diffrn_orient_matrix_UB_12      0.0051182000
_diffrn_orient_matrix_UB_13      0.0339005000
_diffrn_orient_matrix_UB_21      0.0033677000
_diffrn_orient_matrix_UB_22      0.0641157000
_diffrn_orient_matrix_UB_23      -0.0054492000
_diffrn_orient_matrix_UB_31      -0.0801028000
_diffrn_orient_matrix_UB_32      0.0067823000
_diffrn_orient_matrix_UB_33      0.0021181000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9556
_reflns_number_total             11630
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         11630
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0458P)²+1.4601P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1071
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C16(H16), C19(H19), C24(H24), C23(H23), C4(H4), C7(H7), C18(H18),
 C1(H1), C15(H15), C17(H17), C9(H9), C27(H27), C30(H30), C8(H8), C12(H12),
 C3(H3), C2(H2), C28(H28), C29(H29), C14(H14), C13(H13)
2.c Idealised tetrahedral OH refined as rotating group:
 O3(H3A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni01 Ni 0.22676(3) 0.79303(2) 0.75217(2) 0.02491(6) Uani 1 1 d . . . . .
Cl3 Cl 0.94504(7) 1.17885(6) 0.47161(3) 0.05373(15) Uani 1 1 d . . . . .
Cl1 Cl -0.15527(8) 0.35828(6) 0.90627(3) 0.05692(17) Uani 1 1 d . . . . .
Cl2 Cl 0.37391(9) 1.26789(8) 0.69025(4) 0.0778(3) Uani 1 1 d . . . . .
Cl4 Cl 0.64091(15) 1.10772(10) 0.86018(4) 0.1043(4) Uani 1 1 d . . . . .
O5 O 0.90207(17) 1.36492(14) 0.57104(8) 0.0421(3) Uani 1 1 d . . . . .
N2 N 0.27238(16) 0.70379(13) 0.67163(7) 0.0268(3) Uani 1 1 d . . . . .
N5 N 0.19232(17) 0.87564(13) 0.83464(7) 0.0262(3) Uani 1 1 d . . . . .
N4 N 0.13346(17) 0.96662(14) 0.72321(7) 0.0285(3) Uani 1 1 d . . . . .
O1 O -0.2397(2) 0.60861(15) 0.94753(9) 0.0539(4) Uani 1 1 d . . . . .
N6 N 0.30616(18) 0.65448(14) 0.81682(8) 0.0312(3) Uani 1 1 d . . . . .
N3 N 0.44984(18) 0.84260(14) 0.71325(7) 0.0310(3) Uani 1 1 d . . . . .
N1 N 0.02125(17) 0.71125(14) 0.75447(7) 0.0300(3) Uani 1 1 d . . . . .
O9 O -0.1877(2) 0.60732(18) 0.51913(11) 0.0605(5) Uani 1 1 d G . . . .
H9A H -0.156188 0.543629 0.540050 0.091 Uiso 1 1 d G U . . .
H9B H -0.107855 0.634027 0.496249 0.091 Uiso 1 1 d G U . . .
O2 O 0.0949(2) 0.26895(15) 0.97939(11) 0.0665(6) Uani 1 1 d . . . . .
O6 O 0.6454(2) 1.07007(18) 0.49167(9) 0.0604(5) Uani 1 1 d . . . . .
O4 O 0.6580(2) 1.3965(2) 0.66399(11) 0.0744(6) Uani 1 1 d . . . . .
O3 O 0.4075(2) 1.1019(2) 0.58433(10) 0.0687(6) Uani 1 1 d . . . . .
H3A H 0.420743 1.064501 0.551477 0.103 Uiso 1 1 calc R U . . .
C6 C 0.1701(2) 0.62993(16) 0.65969(8) 0.0287(3) Uani 1 1 d . . . . .
O7 O 0.4523(3) 1.23890(16) 0.96811(11) 0.0735(6) Uani 1 1 d . . . . .
C5 C 0.0242(2) 0.63777(16) 0.70532(8) 0.0288(3) Uani 1 1 d . . . . .
C21 C 0.1297(2) 0.99064(16) 0.83567(9) 0.0289(3) Uani 1 1 d . . . . .
C37 C 0.7937(2) 1.29987(17) 0.57203(9) 0.0333(4) Uani 1 1 d . . . . .
C25 C 0.2378(2) 0.81717(16) 0.88728(8) 0.0285(3) Uani 1 1 d . . . . .
C10 C 0.4109(2) 0.70703(17) 0.63534(9) 0.0298(4) Uani 1 1 d . . . . .
C20 C 0.0901(2) 1.04120(16) 0.77225(9) 0.0292(3) Uani 1 1 d . . . . .
C26 C 0.3077(2) 0.69204(17) 0.87653(9) 0.0302(4) Uani 1 1 d . . . . .
C22 C 0.1120(2) 1.05321(19) 0.89159(10) 0.0390(4) Uani 1 1 d . . . . .
H22 H 0.070186 1.133235 0.892208 0.047 Uiso 1 1 calc R U . . .
C11 C 0.5091(2) 0.79265(17) 0.65671(9) 0.0310(4) Uani 1 1 d . . . . .
O8 O 0.6702(3) 0.8503(2) 0.91664(12) 0.0879(8) Uani 1 1 d . . . . .
C16 C 0.1105(2) 1.00735(19) 0.66348(9) 0.0347(4) Uani 1 1 d . . . . .
H16 H 0.142008 0.956961 0.629658 0.042 Uiso 1 1 calc R U . . .
C19 C 0.0180(2) 1.15572(18) 0.76248(11) 0.0391(4) Uani 1 1 d . . . . .
H19 H -0.013071 1.204881 0.796859 0.047 Uiso 1 1 calc R U . . .
C24 C 0.2197(2) 0.8741(2) 0.94502(9) 0.0374(4) Uani 1 1 d . . . . .
H24 H 0.248280 0.832884 0.982078 0.045 Uiso 1 1 calc R U . . .
C23 C 0.1582(3) 0.9933(2) 0.94615(10) 0.0415(5) Uani 1 1 d . . . . .
H23 H 0.147930 1.033463 0.984019 0.050 Uiso 1 1 calc R U . . .
C36 C 0.6539(3) 1.3212(2) 0.62550(11) 0.0416(5) Uani 1 1 d . . . . .
C31 C -0.1249(3) 0.55460(18) 0.96957(10) 0.0393(4) Uani 1 1 d . . . . .
C33 C 0.0502(3) 0.37570(18) 0.98575(11) 0.0405(5) Uani 1 1 d . . . . .
C4 C -0.1007(2) 0.57619(19) 0.69919(10) 0.0388(4) Uani 1 1 d . . . . .
H4 H -0.096942 0.526892 0.665072 0.047 Uiso 1 1 calc R U . . .
C7 C 0.2057(2) 0.5539(2) 0.60888(10) 0.0400(5) Uani 1 1 d . . . . .
H7 H 0.135626 0.502235 0.600524 0.048 Uiso 1 1 calc R U . . .
C18 C -0.0071(3) 1.1956(2) 0.70044(12) 0.0457(5) Uani 1 1 d . . . . .
H18 H -0.056549 1.271675 0.692805 0.055 Uiso 1 1 calc R U . . .
C1 C -0.1060(2) 0.7230(2) 0.79800(10) 0.0385(4) Uani 1 1 d . . . . .
H1 H -0.108109 0.773112 0.831658 0.046 Uiso 1 1 calc R U . . .
C15 C 0.5306(2) 0.9206(2) 0.73622(11) 0.0414(5) Uani 1 1 d . . . . .
H15 H 0.490447 0.954435 0.775141 0.050 Uiso 1 1 calc R U . . .
C40 C 0.4762(3) 1.12727(18) 0.97962(12) 0.0421(5) Uani 1 1 d . . . . .
C38 C 0.7881(2) 1.20933(19) 0.53027(10) 0.0366(4) Uani 1 1 d . . . . .
C32 C -0.0678(2) 0.43865(18) 0.95585(10) 0.0387(4) Uani 1 1 d . . . . .
C17 C 0.0418(3) 1.1215(2) 0.65013(11) 0.0428(5) Uani 1 1 d . . . . .
H17 H 0.028805 1.147808 0.608007 0.051 Uiso 1 1 calc R U . . .
C9 C 0.4532(2) 0.6336(2) 0.58369(10) 0.0413(5) Uani 1 1 d . . . . .
H9 H 0.548939 0.635771 0.558305 0.050 Uiso 1 1 calc R U . . .
C27 C 0.3724(3) 0.6190(2) 0.92303(11) 0.0429(5) Uani 1 1 d . . . . .
H27 H 0.375637 0.647210 0.963241 0.051 Uiso 1 1 calc R U . . .
C39 C 0.6594(3) 1.1449(2) 0.53077(10) 0.0401(4) Uani 1 1 d . . . . .
C30 C 0.3634(3) 0.54131(18) 0.80408(11) 0.0414(5) Uani 1 1 d . . . . .
H30 H 0.361220 0.514780 0.763377 0.050 Uiso 1 1 calc R U . . .
C8 C 0.3480(3) 0.5570(2) 0.57114(11) 0.0469(5) Uani 1 1 d . . . . .
H8 H 0.373723 0.507042 0.536836 0.056 Uiso 1 1 calc R U . . .
C35 C 0.5252(3) 1.2493(2) 0.62794(11) 0.0454(5) Uani 1 1 d . . . . .
C41 C 0.5635(3) 1.0479(2) 0.93663(11) 0.0448(5) Uani 1 1 d . . . . .
C42 C 0.5914(3) 0.9245(2) 0.95317(12) 0.0456(5) Uani 1 1 d . . . . .
C12 C 0.6496(2) 0.8210(2) 0.62225(11) 0.0451(5) Uani 1 1 d . . . . .
H12 H 0.688749 0.785688 0.583633 0.054 Uiso 1 1 calc R U . . .
C34 C 0.5244(3) 1.1681(2) 0.58351(11) 0.0449(5) Uani 1 1 d . . . . .
C3 C -0.2315(3) 0.5896(2) 0.74507(12) 0.0481(5) Uani 1 1 d . . . . .
H3 H -0.316464 0.548823 0.742083 0.058 Uiso 1 1 calc R U . . .
C2 C -0.2348(3) 0.6637(2) 0.79504(11) 0.0471(5) Uani 1 1 d . . . . .
H2 H -0.321555 0.673703 0.826080 0.056 Uiso 1 1 calc R U . . .
C28 C 0.4322(3) 0.5026(2) 0.90828(13) 0.0519(6) Uani 1 1 d . . . . .
H28 H 0.476773 0.452047 0.938630 0.062 Uiso 1 1 calc R U . . .
C29 C 0.4254(3) 0.4624(2) 0.84893(13) 0.0499(6) Uani 1 1 d . . . . .
H29 H 0.461782 0.383627 0.839024 0.060 Uiso 1 1 calc R U . . .
C14 C 0.6716(3) 0.9528(2) 0.70426(13) 0.0525(6) Uani 1 1 d . . . . .
H14 H 0.725224 1.007085 0.721479 0.063 Uiso 1 1 calc R U . . .
C13 C 0.7309(3) 0.9032(2) 0.64658(13) 0.0545(6) Uani 1 1 d . . . . .
H13 H 0.824840 0.924446 0.624005 0.065 Uiso 1 1 calc R U . . .
H1A H -0.283(9) 0.679(7) 0.966(4) 0.26(3) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni01 N2 1.9935(14) . ?
Ni01 N5 1.9901(14) . ?
Ni01 N4 2.1077(15) . ?
Ni01 N6 2.1157(16) . ?
Ni01 N3 2.1231(16) . ?
Ni01 N1 2.1089(15) . ?
Cl3 C38 1.733(2) . ?
Cl1 C32 1.743(2) . ?
Cl2 C35 1.726(2) . ?
Cl4 C41 1.733(2) . ?
O5 C37 1.251(2) . ?
N2 C6 1.344(2) . ?
N2 C10 1.342(2) . ?
N5 C21 1.344(2) . ?
N5 C25 1.338(2) . ?
N4 C20 1.357(2) . ?
N4 C16 1.338(2) . ?
O1 C31 1.281(3) . ?
O1 H1A 0.93(8) . ?
N6 C26 1.356(2) . ?
N6 C30 1.340(2) . ?
N3 C11 1.357(2) . ?
N3 C15 1.339(2) . ?
N1 C5 1.361(2) . ?
N1 C1 1.337(2) . ?
O9 H9A 0.8502 . ?
O9 H9B 0.8501 . ?
O2 C33 1.223(2) . ?
O6 C39 1.240(2) . ?
O4 C36 1.214(3) . ?
O3 H3A 0.8200 . ?
O3 C34 1.322(3) . ?
C6 C5 1.483(2) . ?
C6 C7 1.391(2) . ?
O7 C40 1.243(3) . ?
C5 C4 1.386(3) . ?
C21 C20 1.486(3) . ?
C21 C22 1.391(2) . ?
C37 C36 1.548(3) . ?
C37 C38 1.394(3) . ?
C25 C26 1.486(2) . ?
C25 C24 1.391(2) . ?
C10 C11 1.488(2) . ?
C10 C9 1.390(2) . ?
C20 C19 1.386(3) . ?
C26 C27 1.385(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.380(3) . ?
C11 C12 1.386(3) . ?
O8 C42 1.258(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.383(3) . ?
C19 H19 0.9300 . ?
C19 C18 1.387(3) . ?
C24 H24 0.9300 . ?
C24 C23 1.383(3) . ?
C23 H23 0.9300 . ?
C36 C35 1.445(3) . ?
C31 C33 1.531(3) 2_567 ?
C31 C32 1.373(3) . ?
C33 C32 1.422(3) . ?
C4 H4 0.9300 . ?
C4 C3 1.390(3) . ?
C7 H7 0.9300 . ?
C7 C8 1.382(3) . ?
C18 H18 0.9300 . ?
C18 C17 1.380(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.387(3) . ?
C15 H15 0.9300 . ?
C15 C14 1.384(3) . ?
C40 C41 1.404(3) . ?
C40 C42 1.520(3) 2_677 ?
C38 C39 1.403(3) . ?
C17 H17 0.9300 . ?
C9 H9 0.9300 . ?
C9 C8 1.389(3) . ?
C27 H27 0.9300 . ?
C27 C28 1.388(3) . ?
C39 C34 1.514(3) . ?
C30 H30 0.9300 . ?
C30 C29 1.382(3) . ?
C8 H8 0.9300 . ?
C35 C34 1.349(3) . ?
C41 C42 1.389(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.390(3) . ?
C3 H3 0.9300 . ?
C3 C2 1.379(3) . ?
C2 H2 0.9300 . ?
C28 H28 0.9300 . ?
C28 C29 1.370(4) . ?
C29 H29 0.9300 . ?
C14 H14 0.9300 . ?
C14 C13 1.376(3) . ?
C13 H13 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni01 N4 105.07(6) . . ?
N2 Ni01 N6 98.34(6) . . ?
N2 Ni01 N3 78.20(6) . . ?
N2 Ni01 N1 78.48(6) . . ?
N5 Ni01 N2 176.29(6) . . ?
N5 Ni01 N4 78.18(6) . . ?
N5 Ni01 N6 78.40(6) . . ?
N5 Ni01 N3 100.08(6) . . ?
N5 Ni01 N1 103.33(6) . . ?
N4 Ni01 N6 156.58(6) . . ?
N4 Ni01 N3 91.24(6) . . ?
N4 Ni01 N1 92.74(6) . . ?
N6 Ni01 N3 92.70(6) . . ?
N1 Ni01 N6 92.76(6) . . ?
N1 Ni01 N3 156.58(6) . . ?
C6 N2 Ni01 118.70(12) . . ?
C10 N2 Ni01 119.18(12) . . ?
C10 N2 C6 121.59(15) . . ?
C21 N5 Ni01 119.42(12) . . ?
C25 N5 Ni01 119.18(12) . . ?
C25 N5 C21 121.34(15) . . ?
C20 N4 Ni01 114.24(12) . . ?
C16 N4 Ni01 127.10(13) . . ?
C16 N4 C20 118.64(16) . . ?
C31 O1 H1A 117(5) . . ?
C26 N6 Ni01 113.39(12) . . ?
C30 N6 Ni01 128.04(14) . . ?
C30 N6 C26 118.37(17) . . ?
C11 N3 Ni01 113.80(12) . . ?
C15 N3 Ni01 127.42(13) . . ?
C15 N3 C11 118.66(17) . . ?
C5 N1 Ni01 113.83(12) . . ?
C1 N1 Ni01 127.66(13) . . ?
C1 N1 C5 118.51(16) . . ?
H9A O9 H9B 104.5 . . ?
C34 O3 H3A 109.5 . . ?
N2 C6 C5 113.90(14) . . ?
N2 C6 C7 120.46(17) . . ?
C7 C6 C5 125.64(17) . . ?
N1 C5 C6 114.63(15) . . ?
N1 C5 C4 121.85(17) . . ?
C4 C5 C6 123.51(16) . . ?
N5 C21 C20 113.50(15) . . ?
N5 C21 C22 120.76(17) . . ?
C22 C21 C20 125.68(17) . . ?
O5 C37 C36 116.57(17) . . ?
O5 C37 C38 126.20(19) . . ?
C38 C37 C36 117.23(17) . . ?
N5 C25 C26 113.72(15) . . ?
N5 C25 C24 120.46(17) . . ?
C24 C25 C26 125.81(17) . . ?
N2 C10 C11 113.78(15) . . ?
N2 C10 C9 120.71(17) . . ?
C9 C10 C11 125.50(17) . . ?
N4 C20 C21 114.43(15) . . ?
N4 C20 C19 121.79(17) . . ?
C19 C20 C21 123.77(17) . . ?
N6 C26 C25 114.91(15) . . ?
N6 C26 C27 121.83(18) . . ?
C27 C26 C25 123.25(17) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 C21 118.19(18) . . ?
C23 C22 H22 120.9 . . ?
N3 C11 C10 114.59(16) . . ?
N3 C11 C12 121.77(17) . . ?
C12 C11 C10 123.64(17) . . ?
N4 C16 H16 118.7 . . ?
N4 C16 C17 122.51(19) . . ?
C17 C16 H16 118.7 . . ?
C20 C19 H19 120.6 . . ?
C20 C19 C18 118.73(19) . . ?
C18 C19 H19 120.6 . . ?
C25 C24 H24 120.7 . . ?
C23 C24 C25 118.57(18) . . ?
C23 C24 H24 120.7 . . ?
C22 C23 C24 120.64(17) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
O4 C36 C37 118.60(19) . . ?
O4 C36 C35 122.9(2) . . ?
C35 C36 C37 118.49(17) . . ?
O1 C31 C33 117.24(17) . 2_567 ?
O1 C31 C32 123.6(2) . . ?
C32 C31 C33 119.14(19) . 2_567 ?
O2 C33 C31 117.3(2) . 2_567 ?
O2 C33 C32 124.8(2) . . ?
C32 C33 C31 117.87(16) . 2_567 ?
C5 C4 H4 120.7 . . ?
C5 C4 C3 118.62(18) . . ?
C3 C4 H4 120.7 . . ?
C6 C7 H7 120.9 . . ?
C8 C7 C6 118.30(18) . . ?
C8 C7 H7 120.9 . . ?
C19 C18 H18 120.3 . . ?
C17 C18 C19 119.5(2) . . ?
C17 C18 H18 120.3 . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.74(18) . . ?
C2 C1 H1 118.6 . . ?
N3 C15 H15 118.7 . . ?
N3 C15 C14 122.52(19) . . ?
C14 C15 H15 118.7 . . ?
O7 C40 C41 125.3(2) . . ?
O7 C40 C42 116.2(2) . 2_677 ?
C41 C40 C42 118.49(18) . 2_677 ?
C37 C38 Cl3 118.64(15) . . ?
C37 C38 C39 123.69(19) . . ?
C39 C38 Cl3 117.59(15) . . ?
C31 C32 Cl1 119.09(17) . . ?
C31 C32 C33 122.76(18) . . ?
C33 C32 Cl1 117.81(14) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 C16 118.82(19) . . ?
C18 C17 H17 120.6 . . ?
C10 C9 H9 121.0 . . ?
C8 C9 C10 117.97(18) . . ?
C8 C9 H9 121.0 . . ?
C26 C27 H27 120.7 . . ?
C26 C27 C28 118.5(2) . . ?
C28 C27 H27 120.7 . . ?
O6 C39 C38 125.9(2) . . ?
O6 C39 C34 116.47(19) . . ?
C38 C39 C34 117.59(17) . . ?
N6 C30 H30 118.6 . . ?
N6 C30 C29 122.7(2) . . ?
C29 C30 H30 118.6 . . ?
C7 C8 C9 120.97(18) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C36 C35 Cl2 118.22(16) . . ?
C34 C35 Cl2 120.81(17) . . ?
C34 C35 C36 121.0(2) . . ?
C40 C41 Cl4 118.23(18) . . ?
C42 C41 Cl4 119.03(18) . . ?
C42 C41 C40 122.7(2) . . ?
O8 C42 C40 116.2(2) . 2_677 ?
O8 C42 C41 125.0(2) . . ?
C41 C42 C40 118.78(18) . 2_677 ?
C11 C12 H12 120.7 . . ?
C11 C12 C13 118.7(2) . . ?
C13 C12 H12 120.7 . . ?
O3 C34 C39 116.02(18) . . ?
O3 C34 C35 122.2(2) . . ?
C35 C34 C39 121.78(19) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 C4 119.72(19) . . ?
C2 C3 H3 120.1 . . ?
C1 C2 H2 120.7 . . ?
C3 C2 C1 118.56(19) . . ?
C3 C2 H2 120.7 . . ?
C27 C28 H28 120.1 . . ?
C29 C28 C27 119.9(2) . . ?
C29 C28 H28 120.1 . . ?
C30 C29 H29 120.7 . . ?
C28 C29 C30 118.6(2) . . ?
C28 C29 H29 120.7 . . ?
C15 C14 H14 120.6 . . ?
C13 C14 C15 118.8(2) . . ?
C13 C14 H14 120.6 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13 120.2 . . ?

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
Ni01 N2 C6 C5 7.7(2) . . . . ?
Ni01 N2 C6 C7 -171.41(15) . . . . ?
Ni01 N2 C10 C11 -7.4(2) . . . . ?
Ni01 N2 C10 C9 171.66(16) . . . . ?
Ni01 N5 C21 C20 1.3(2) . . . . ?
Ni01 N5 C21 C22 -176.36(15) . . . . ?
Ni01 N5 C25 C26 -1.4(2) . . . . ?
Ni01 N5 C25 C24 177.93(15) . . . . ?
Ni01 N4 C20 C21 5.4(2) . . . . ?
Ni01 N4 C20 C19 -175.89(15) . . . . ?
Ni01 N4 C16 C17 176.95(15) . . . . ?
Ni01 N6 C26 C25 6.6(2) . . . . ?
Ni01 N6 C26 C27 -172.30(16) . . . . ?
Ni01 N6 C30 C29 173.53(17) . . . . ?
Ni01 N3 C11 C10 -3.8(2) . . . . ?
Ni01 N3 C11 C12 175.88(17) . . . . ?
Ni01 N3 C15 C14 -175.31(19) . . . . ?
Ni01 N1 C5 C6 -0.3(2) . . . . ?
Ni01 N1 C5 C4 179.82(16) . . . . ?
Ni01 N1 C1 C2 -179.41(18) . . . . ?
Cl3 C38 C39 O6 -2.3(3) . . . . ?
Cl3 C38 C39 C34 177.82(17) . . . . ?
Cl2 C35 C34 O3 1.9(4) . . . . ?
Cl2 C35 C34 C39 -176.36(19) . . . . ?
Cl4 C41 C42 O8 0.1(4) . . . . ?
Cl4 C41 C42 C40 179.76(17) . . . 2_677 ?
O5 C37 C36 O4 -1.7(3) . . . . ?
O5 C37 C36 C35 179.2(2) . . . . ?
O5 C37 C38 Cl3 1.3(3) . . . . ?
O5 C37 C38 C39 -175.4(2) . . . . ?
N2 C6 C5 N1 -4.6(2) . . . . ?
N2 C6 C5 C4 175.28(18) . . . . ?
N2 C6 C7 C8 -0.3(3) . . . . ?
N2 C10 C11 N3 7.2(2) . . . . ?
N2 C10 C11 C12 -172.5(2) . . . . ?
N2 C10 C9 C8 -0.2(3) . . . . ?
N5 C21 C20 N4 -4.4(2) . . . . ?
N5 C21 C20 C19 176.85(18) . . . . ?
N5 C21 C22 C23 -1.1(3) . . . . ?
N5 C25 C26 N6 -3.7(2) . . . . ?
N5 C25 C26 C27 175.18(19) . . . . ?
N5 C25 C24 C23 -2.0(3) . . . . ?
N4 C20 C19 C18 -1.5(3) . . . . ?
N4 C16 C17 C18 -1.0(3) . . . . ?
O1 C31 C32 Cl1 -0.5(3) . . . . ?
O1 C31 C32 C33 -173.6(2) . . . . ?
N6 C26 C27 C28 -2.3(3) . . . . ?
N6 C30 C29 C28 -1.7(4) . . . . ?
N3 C11 C12 C13 -0.2(4) . . . . ?
N3 C15 C14 C13 0.2(4) . . . . ?
N1 C5 C4 C3 -0.6(3) . . . . ?
N1 C1 C2 C3 -0.1(4) . . . . ?
O2 C33 C32 Cl1 -0.2(4) . . . . ?
O2 C33 C32 C31 173.1(3) . . . . ?
O6 C39 C34 O3 3.0(3) . . . . ?
O6 C39 C34 C35 -178.6(2) . . . . ?
O4 C36 C35 Cl2 -2.4(4) . . . . ?
O4 C36 C35 C34 178.8(3) . . . . ?
C6 N2 C10 C11 -178.94(16) . . . . ?
C6 N2 C10 C9 0.2(3) . . . . ?
C6 C5 C4 C3 179.6(2) . . . . ?
C6 C7 C8 C9 0.3(4) . . . . ?
O7 C40 C41 Cl4 -1.9(3) . . . . ?
O7 C40 C41 C42 177.3(2) . . . . ?
C5 N1 C1 C2 -0.1(3) . . . . ?
C5 C6 C7 C8 -179.4(2) . . . . ?
C5 C4 C3 C2 0.4(4) . . . . ?
C21 N5 C25 C26 -178.59(16) . . . . ?
C21 N5 C25 C24 0.7(3) . . . . ?
C21 C20 C19 C18 177.12(19) . . . . ?
C21 C22 C23 C24 -0.3(3) . . . . ?
C37 C36 C35 Cl2 176.63(16) . . . . ?
C37 C36 C35 C34 -2.1(4) . . . . ?
C37 C38 C39 O6 174.5(2) . . . . ?
C37 C38 C39 C34 -5.4(3) . . . . ?
C25 N5 C21 C20 178.49(16) . . . . ?
C25 N5 C21 C22 0.9(3) . . . . ?
C25 C26 C27 C28 178.9(2) . . . . ?
C25 C24 C23 C22 1.8(3) . . . . ?
C10 N2 C6 C5 179.28(16) . . . . ?
C10 N2 C6 C7 0.1(3) . . . . ?
C10 C11 C12 C13 179.4(2) . . . . ?
C10 C9 C8 C7 0.0(4) . . . . ?
C20 N4 C16 C17 -1.3(3) . . . . ?
C20 C21 C22 C23 -178.4(2) . . . . ?
C20 C19 C18 C17 -0.8(3) . . . . ?
C26 N6 C30 C29 -0.9(3) . . . . ?
C26 C25 C24 C23 177.19(19) . . . . ?
C26 C27 C28 C29 -0.4(4) . . . . ?
C22 C21 C20 N4 173.06(19) . . . . ?
C22 C21 C20 C19 -5.7(3) . . . . ?
C11 N3 C15 C14 0.5(3) . . . . ?
C11 C10 C9 C8 178.8(2) . . . . ?
C11 C12 C13 C14 0.9(4) . . . . ?
C16 N4 C20 C21 -176.19(16) . . . . ?
C16 N4 C20 C19 2.6(3) . . . . ?
C19 C18 C17 C16 2.0(3) . . . . ?
C24 C25 C26 N6 177.04(19) . . . . ?
C24 C25 C26 C27 -4.1(3) . . . . ?
C36 C37 C38 Cl3 -177.71(15) . . . . ?
C36 C37 C38 C39 5.5(3) . . . . ?
C36 C35 C34 O3 -179.4(2) . . . . ?
C36 C35 C34 C39 2.3(4) . . . . ?
C31 C33 C32 Cl1 -178.76(16) 2_567 . . . ?
C31 C33 C32 C31 -5.5(4) 2_567 . . . ?
C33 C31 C32 Cl1 178.74(16) 2_567 . . . ?
C33 C31 C32 C33 5.6(4) 2_567 . . . ?
C4 C3 C2 C1 -0.1(4) . . . . ?
C7 C6 C5 N1 174.52(19) . . . . ?
C7 C6 C5 C4 -5.6(3) . . . . ?
C1 N1 C5 C6 -179.72(17) . . . . ?
C1 N1 C5 C4 0.4(3) . . . . ?
C15 N3 C11 C10 179.88(18) . . . . ?
C15 N3 C11 C12 -0.5(3) . . . . ?
C15 C14 C13 C12 -0.9(4) . . . . ?
C40 C41 C42 O8 -179.1(3) . . . . ?
C40 C41 C42 C40 0.5(4) . . . 2_677 ?
C38 C37 C36 O4 177.4(2) . . . . ?
C38 C37 C36 C35 -1.7(3) . . . . ?
C38 C39 C34 O3 -177.1(2) . . . . ?
C38 C39 C34 C35 1.3(4) . . . . ?
C9 C10 C11 N3 -171.9(2) . . . . ?
C9 C10 C11 C12 8.5(3) . . . . ?
C27 C28 C29 C30 2.3(4) . . . . ?
C30 N6 C26 C25 -178.17(18) . . . . ?
C30 N6 C26 C27 2.9(3) . . . . ?
C42 C40 C41 Cl4 -179.76(17) 2_677 . . . ?
C42 C40 C41 C42 -0.5(4) 2_677 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.865
####################################################################### 
# 
# 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_exp_783
_database_code_depnum_ccdc_archive 'CCDC 2374764'
loop_
_audit_author_name
_audit_author_address
'Akio Mishima'
;Fukuoka University
Japan
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_audit_creation_date             2024-06-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 Fe N6, 2(C3 Cl O2), 6(H2 O)'
_chemical_formula_sum            'C36 H34 Cl2 Fe N6 O10'
_chemical_formula_weight         837.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N20O20Cl2Fe1
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'
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'

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

_cell_length_a                   9.0180(2)
_cell_length_b                   9.02320(10)
_cell_length_c                   22.2494(3)
_cell_angle_alpha                91.6850(10)
_cell_angle_beta                 95.6840(10)
_cell_angle_gamma                90.432(2)
_cell_volume                     1800.68(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12428
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.6700
_cell_measurement_theta_min      2.2550
_shelx_estimated_absorpt_T_max   0.883
_shelx_estimated_absorpt_T_min   0.702
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            34721
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.606
_diffrn_reflns_theta_min         2.258
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  20.00   0.50   30.00    --   20.00  54.00  90.00   80
  2  ω    -74.00 -33.00   0.50   30.00    --   20.00  54.00-150.00   82
  3  ω    -23.00   3.00   0.50   30.00    --   20.00  54.00-150.00   52
  4  ω      8.00  34.00   0.50   30.00    --   20.00  54.00-150.00   52
  5  ω     85.00 110.00   0.50   30.00    --   20.00  54.00-150.00   50
  6  ω    -71.00  76.00   0.50   30.00    --   20.00  54.00 -30.00  294
  7  ω    -71.00 -13.00   0.50   30.00    --   20.00  54.00 -90.00  116
  8  ω      3.00  69.00   0.50   30.00    --   20.00  54.00 -90.00  132
  9  ω     85.00 110.00   0.50   30.00    --   20.00  54.00 -90.00   50
 10  ω    -71.00 -38.00   0.50   30.00    --   20.00  54.00  30.00   66
 11  ω    -25.00  79.00   0.50   30.00    --   20.00  54.00  30.00  208
 12  ω    -72.00  26.00   0.50   30.00    --   20.00  54.00 120.00  196
 13  ω     80.00 105.00   0.50   30.00    --   20.00  54.00 120.00   50
 14  ω    -65.00 -39.00   0.50   30.00    --   20.00  54.00-120.00   52
 15  ω     27.00  52.00   0.50   30.00    --   20.00  54.00-120.00   50
 16  ω    -63.00  98.00   0.50   30.00    --   20.00  54.00 150.00  322
 17  ω    -43.00 -18.00   0.50   30.00    --   20.00  54.00 -60.00   50
 18  ω     68.00  93.00   0.50   30.00    --   20.00  54.00 -60.00   50
 19  ω    -66.00  -2.00   0.50   30.00    --   20.00  54.00  60.00  128
 20  ω    -63.00 -38.00   0.50   30.00    --   20.00  54.00  90.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0375796000
_diffrn_orient_matrix_UB_12      -0.0343121000
_diffrn_orient_matrix_UB_13      -0.0263625000
_diffrn_orient_matrix_UB_21      0.0371822000
_diffrn_orient_matrix_UB_22      -0.0673339000
_diffrn_orient_matrix_UB_23      0.0068346000
_diffrn_orient_matrix_UB_31      -0.0587681000
_diffrn_orient_matrix_UB_32      -0.0217730000
_diffrn_orient_matrix_UB_33      0.0169006000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7616
_reflns_number_total             10443
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         10443
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0460
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0388P)²+0.7410P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1025
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B), O10(H10A,H10B), O5(H5A,H5B), O6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C30(H30), C9(H9), C1(H1), C22(H22), C24(H24), C8(H8),
 C7(H7), C12(H12), C27(H27), C23(H23), C29(H29), C17(H17), C28(H28), C4(H4),
 C2(H2), C19(H19), C18(H18), C14(H14), C13(H13), C3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe01 Fe 0.72807(3) 0.81697(3) 0.24970(2) 0.02468(7) Uani 1 1 d . . . . .
Cl2 Cl 1.22786(8) 0.85920(7) 0.09935(3) 0.06100(18) Uani 1 1 d . . . . .
Cl1 Cl 0.82083(7) 0.28989(8) 0.40121(3) 0.05771(18) Uani 1 1 d . . . . .
O1 O 0.71633(16) 0.41457(17) 0.51626(7) 0.0448(4) Uani 1 1 d . . . . .
O3 O 1.08088(18) 0.71150(16) -0.01422(7) 0.0466(4) Uani 1 1 d . . . . .
N3 N 0.53130(17) 0.72909(16) 0.26110(7) 0.0278(3) Uani 1 1 d . . . . .
N2 N 0.74704(17) 0.81130(16) 0.33488(6) 0.0271(3) Uani 1 1 d . . . . .
N5 N 0.71290(17) 0.82091(17) 0.16451(6) 0.0280(3) Uani 1 1 d . . . . .
O7 O 0.7035(2) 1.10220(18) 0.52264(7) 0.0542(4) Uani 1 1 d G . . . .
H7A H 0.710562 1.196288 0.524305 0.081 Uiso 1 1 d G U . . .
H7B H 0.660089 1.081861 0.487688 0.081 Uiso 1 1 d G U . . .
N6 N 0.81152(17) 0.61882(17) 0.23277(7) 0.0288(3) Uani 1 1 d . . . . .
N1 N 0.92946(17) 0.90676(17) 0.26638(7) 0.0293(3) Uani 1 1 d . . . . .
O8 O 0.5009(2) 1.05626(19) 0.41462(8) 0.0551(4) Uani 1 1 d G . . . .
H8A H 0.468895 1.144468 0.416305 0.083 Uiso 1 1 d G U . . .
H8B H 0.439289 1.005638 0.432305 0.083 Uiso 1 1 d G U . . .
O9 O 0.3907(2) 0.6864(2) -0.02238(8) 0.0553(4) Uani 1 1 d G . . . .
H9A H 0.298048 0.698765 -0.020159 0.083 Uiso 1 1 d G U . . .
H9B H 0.422929 0.653550 0.011836 0.083 Uiso 1 1 d G U . . .
O4 O 1.1078(2) 1.16353(18) 0.09748(7) 0.0543(4) Uani 1 1 d . . . . .
N4 N 0.63836(17) 1.01509(17) 0.23856(7) 0.0286(3) Uani 1 1 d . . . . .
O10 O 0.4646(2) 0.5297(2) 0.08919(8) 0.0582(4) Uani 1 1 d G . . . .
H10A H 0.372593 0.506433 0.085013 0.087 Uiso 1 1 d G U . . .
H10B H 0.505563 0.463725 0.068547 0.087 Uiso 1 1 d G U . . .
O2 O 1.12563(19) 0.4152(2) 0.40019(7) 0.0564(5) Uani 1 1 d . . . . .
O5 O 0.4573(2) 0.3551(2) 0.42438(10) 0.0682(5) Uani 1 1 d G . . . .
H5A H 0.380707 0.405799 0.430231 0.102 Uiso 1 1 d G U . . .
H5B H 0.526143 0.392724 0.449166 0.102 Uiso 1 1 d G U . . .
O6 O 1.1657(2) 0.4815(2) 0.07446(11) 0.0742(6) Uani 1 1 d G . . . .
H6A H 1.119405 0.540048 0.050111 0.111 Uiso 1 1 d G U . . .
H6B H 1.118855 0.399488 0.068477 0.111 Uiso 1 1 d G U . . .
C10 C 0.6356(2) 0.7528(2) 0.36325(8) 0.0303(4) Uani 1 1 d . . . . .
C26 C 0.8182(2) 0.5861(2) 0.17257(9) 0.0330(4) Uani 1 1 d . . . . .
C31 C 0.8478(2) 0.4490(2) 0.50617(9) 0.0330(4) Uani 1 1 d . . . . .
C21 C 0.6557(2) 0.9413(2) 0.13624(8) 0.0334(4) Uani 1 1 d . . . . .
C5 C 0.9787(2) 0.9219(2) 0.32649(8) 0.0327(4) Uani 1 1 d . . . . .
C11 C 0.5079(2) 0.7076(2) 0.32026(8) 0.0310(4) Uani 1 1 d . . . . .
C25 C 0.7623(2) 0.7045(2) 0.13284(8) 0.0327(4) Uani 1 1 d . . . . .
C6 C 0.8743(2) 0.8622(2) 0.36654(8) 0.0311(4) Uani 1 1 d . . . . .
C33 C 1.0634(2) 0.4511(2) 0.44526(9) 0.0348(4) Uani 1 1 d . . . . .
C36 C 1.0607(2) 1.0841(2) 0.05374(9) 0.0351(4) Uani 1 1 d . . . . .
C15 C 0.4217(2) 0.6906(2) 0.21830(9) 0.0344(4) Uani 1 1 d . . . . .
H15 H 0.436421 0.705155 0.178100 0.041 Uiso 1 1 calc R U . . .
C16 C 0.6017(2) 1.1112(2) 0.28177(9) 0.0348(4) Uani 1 1 d . . . . .
H16 H 0.620509 1.085625 0.321972 0.042 Uiso 1 1 calc R U . . .
C20 C 0.6106(2) 1.0541(2) 0.17956(8) 0.0334(4) Uani 1 1 d . . . . .
C34 C 1.0482(2) 0.8456(2) -0.00487(9) 0.0344(4) Uani 1 1 d . . . . .
C32 C 0.9178(2) 0.4057(2) 0.45612(9) 0.0346(4) Uani 1 1 d . . . . .
C30 C 0.8613(2) 0.5172(2) 0.27268(9) 0.0354(4) Uani 1 1 d . . . . .
H30 H 0.855402 0.537717 0.313578 0.043 Uiso 1 1 calc R U . . .
C9 C 0.6502(3) 0.7414(2) 0.42577(9) 0.0392(5) Uani 1 1 d . . . . .
H9 H 0.574184 0.700006 0.445378 0.047 Uiso 1 1 calc R U . . .
C1 C 1.0181(2) 0.9577(2) 0.22611(9) 0.0360(4) Uani 1 1 d . . . . .
H1 H 0.986616 0.946419 0.185140 0.043 Uiso 1 1 calc R U . . .
C22 C 0.6465(3) 0.9483(3) 0.07373(9) 0.0435(5) Uani 1 1 d . . . . .
H22 H 0.607480 1.031070 0.054142 0.052 Uiso 1 1 calc R U . . .
C24 C 0.7560(2) 0.7067(3) 0.07025(9) 0.0423(5) Uani 1 1 d . . . . .
H24 H 0.791083 0.627071 0.048432 0.051 Uiso 1 1 calc R U . . .
C8 C 0.7800(3) 0.7927(2) 0.45811(9) 0.0431(5) Uani 1 1 d . . . . .
H8 H 0.791243 0.786175 0.499945 0.052 Uiso 1 1 calc R U . . .
C35 C 1.1010(2) 0.9347(2) 0.04456(9) 0.0352(4) Uani 1 1 d . . . . .
C7 C 0.8936(3) 0.8536(2) 0.42894(9) 0.0409(5) Uani 1 1 d . . . . .
H7 H 0.980971 0.888081 0.450751 0.049 Uiso 1 1 calc R U . . .
C12 C 0.3759(2) 0.6487(2) 0.33599(10) 0.0420(5) Uani 1 1 d . . . . .
H12 H 0.361779 0.635905 0.376367 0.050 Uiso 1 1 calc R U . . .
C27 C 0.8742(3) 0.4530(2) 0.15301(10) 0.0440(5) Uani 1 1 d . . . . .
H27 H 0.876088 0.431981 0.111921 0.053 Uiso 1 1 calc R U . . .
C23 C 0.6973(3) 0.8279(3) 0.04110(9) 0.0466(6) Uani 1 1 d . . . . .
H23 H 0.691320 0.829919 -0.000840 0.056 Uiso 1 1 calc R U . . .
C29 C 0.9208(3) 0.3840(2) 0.25565(11) 0.0456(5) Uani 1 1 d . . . . .
H29 H 0.955998 0.317296 0.284662 0.055 Uiso 1 1 calc R U . . .
C17 C 0.5371(3) 1.2468(2) 0.26894(11) 0.0473(5) Uani 1 1 d . . . . .
H17 H 0.513218 1.310996 0.299923 0.057 Uiso 1 1 calc R U . . .
C28 C 0.9275(3) 0.3507(3) 0.19506(11) 0.0504(6) Uani 1 1 d . . . . .
H28 H 0.967042 0.261368 0.182625 0.061 Uiso 1 1 calc R U . . .
C4 C 1.1137(3) 0.9892(3) 0.34598(10) 0.0488(6) Uani 1 1 d . . . . .
H4 H 1.145351 0.998080 0.387003 0.059 Uiso 1 1 calc R U . . .
C2 C 1.1543(2) 1.0263(3) 0.24330(10) 0.0458(5) Uani 1 1 d . . . . .
H2 H 1.213007 1.060329 0.214397 0.055 Uiso 1 1 calc R U . . .
C19 C 0.5456(3) 1.1873(3) 0.16406(11) 0.0499(6) Uani 1 1 d . . . . .
H19 H 0.526683 1.211415 0.123686 0.060 Uiso 1 1 calc R U . . .
C18 C 0.5088(3) 1.2849(3) 0.20942(12) 0.0570(7) Uani 1 1 d . . . . .
H18 H 0.465396 1.375442 0.199747 0.068 Uiso 1 1 calc R U . . .
C14 C 0.2877(2) 0.6303(3) 0.23134(11) 0.0453(5) Uani 1 1 d . . . . .
H14 H 0.214067 0.604275 0.200482 0.054 Uiso 1 1 calc R U . . .
C13 C 0.2650(3) 0.6093(3) 0.29095(12) 0.0503(6) Uani 1 1 d . . . . .
H13 H 0.175625 0.568838 0.300708 0.060 Uiso 1 1 calc R U . . .
C3 C 1.2010(3) 1.0432(3) 0.30378(12) 0.0575(7) Uani 1 1 d . . . . .
H3 H 1.291069 1.090872 0.316257 0.069 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe01 N3 1.9804(15) . ?
Fe01 N2 1.8882(14) . ?
Fe01 N5 1.8882(14) . ?
Fe01 N6 1.9854(16) . ?
Fe01 N1 1.9796(16) . ?
Fe01 N4 1.9798(16) . ?
Cl2 C35 1.745(2) . ?
Cl1 C32 1.746(2) . ?
O1 C31 1.266(2) . ?
O3 C34 1.263(2) . ?
N3 C11 1.372(2) . ?
N3 C15 1.339(2) . ?
N2 C10 1.351(2) . ?
N2 C6 1.356(2) . ?
N5 C21 1.351(2) . ?
N5 C25 1.351(2) . ?
O7 H7A 0.8503 . ?
O7 H7B 0.8497 . ?
N6 C26 1.370(2) . ?
N6 C30 1.344(2) . ?
N1 C5 1.369(2) . ?
N1 C1 1.347(2) . ?
O8 H8A 0.8498 . ?
O8 H8B 0.8502 . ?
O9 H9A 0.8499 . ?
O9 H9B 0.8501 . ?
O4 C36 1.230(2) . ?
N4 C16 1.343(2) . ?
N4 C20 1.369(2) . ?
O10 H10A 0.8501 . ?
O10 H10B 0.8501 . ?
O2 C33 1.234(2) . ?
O5 H5A 0.8499 . ?
O5 H5B 0.8503 . ?
O6 H6A 0.8497 . ?
O6 H6B 0.8499 . ?
C10 C11 1.469(3) . ?
C10 C9 1.391(2) . ?
C26 C25 1.467(3) . ?
C26 C27 1.382(3) . ?
C31 C33 1.543(3) 2_766 ?
C31 C32 1.382(3) . ?
C21 C20 1.468(3) . ?
C21 C22 1.388(3) . ?
C5 C6 1.469(3) . ?
C5 C4 1.381(3) . ?
C11 C12 1.381(3) . ?
C25 C24 1.389(3) . ?
C6 C7 1.387(3) . ?
C33 C32 1.418(3) . ?
C36 C34 1.546(3) 2_775 ?
C36 C35 1.413(3) . ?
C15 H15 0.9300 . ?
C15 C14 1.382(3) . ?
C16 H16 0.9300 . ?
C16 C17 1.384(3) . ?
C20 C19 1.380(3) . ?
C34 C35 1.386(3) . ?
C30 H30 0.9300 . ?
C30 C29 1.378(3) . ?
C9 H9 0.9300 . ?
C9 C8 1.381(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.385(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.394(3) . ?
C24 H24 0.9300 . ?
C24 C23 1.372(3) . ?
C8 H8 0.9300 . ?
C8 C7 1.384(3) . ?
C7 H7 0.9300 . ?
C12 H12 0.9300 . ?
C12 C13 1.381(3) . ?
C27 H27 0.9300 . ?
C27 C28 1.388(3) . ?
C23 H23 0.9300 . ?
C29 H29 0.9300 . ?
C29 C28 1.380(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.378(3) . ?
C28 H28 0.9300 . ?
C4 H4 0.9300 . ?
C4 C3 1.381(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.373(3) . ?
C19 H19 0.9300 . ?
C19 C18 1.387(4) . ?
C18 H18 0.9300 . ?
C14 H14 0.9300 . ?
C14 C13 1.380(3) . ?
C13 H13 0.9300 . ?
C3 H3 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Fe01 N6 91.65(6) . . ?
N2 Fe01 N3 80.90(6) . . ?
N2 Fe01 N6 98.08(6) . . ?
N2 Fe01 N1 81.07(6) . . ?
N2 Fe01 N4 99.95(6) . . ?
N5 Fe01 N3 99.87(6) . . ?
N5 Fe01 N2 178.85(7) . . ?
N5 Fe01 N6 81.06(7) . . ?
N5 Fe01 N1 98.19(6) . . ?
N5 Fe01 N4 80.91(7) . . ?
N1 Fe01 N3 161.93(6) . . ?
N1 Fe01 N6 91.94(6) . . ?
N1 Fe01 N4 91.05(6) . . ?
N4 Fe01 N3 90.99(6) . . ?
N4 Fe01 N6 161.97(6) . . ?
C11 N3 Fe01 114.49(12) . . ?
C15 N3 Fe01 127.50(13) . . ?
C15 N3 C11 118.01(16) . . ?
C10 N2 Fe01 119.60(13) . . ?
C10 N2 C6 120.99(16) . . ?
C6 N2 Fe01 119.38(12) . . ?
C21 N5 Fe01 119.54(13) . . ?
C25 N5 Fe01 119.41(13) . . ?
C25 N5 C21 121.03(16) . . ?
H7A O7 H7B 104.5 . . ?
C26 N6 Fe01 114.05(13) . . ?
C30 N6 Fe01 127.96(13) . . ?
C30 N6 C26 117.99(17) . . ?
C5 N1 Fe01 114.39(12) . . ?
C1 N1 Fe01 127.65(13) . . ?
C1 N1 C5 117.92(17) . . ?
H8A O8 H8B 104.5 . . ?
H9A O9 H9B 104.5 . . ?
C16 N4 Fe01 127.38(13) . . ?
C16 N4 C20 118.14(17) . . ?
C20 N4 Fe01 114.47(13) . . ?
H10A O10 H10B 104.5 . . ?
H5A O5 H5B 104.5 . . ?
H6A O6 H6B 104.5 . . ?
N2 C10 C11 111.60(15) . . ?
N2 C10 C9 120.48(19) . . ?
C9 C10 C11 127.92(18) . . ?
N6 C26 C25 113.74(17) . . ?
N6 C26 C27 121.46(19) . . ?
C27 C26 C25 124.80(18) . . ?
O1 C31 C33 116.25(17) . 2_766 ?
O1 C31 C32 126.13(19) . . ?
C32 C31 C33 117.62(17) . 2_766 ?
N5 C21 C20 111.54(16) . . ?
N5 C21 C22 120.6(2) . . ?
C22 C21 C20 127.84(19) . . ?
N1 C5 C6 113.61(16) . . ?
N1 C5 C4 121.73(18) . . ?
C4 C5 C6 124.65(18) . . ?
N3 C11 C10 113.35(16) . . ?
N3 C11 C12 121.75(18) . . ?
C12 C11 C10 124.90(18) . . ?
N5 C25 C26 111.72(16) . . ?
N5 C25 C24 120.41(19) . . ?
C24 C25 C26 127.9(2) . . ?
N2 C6 C5 111.47(15) . . ?
N2 C6 C7 120.53(18) . . ?
C7 C6 C5 128.00(19) . . ?
O2 C33 C31 117.26(18) . 2_766 ?
O2 C33 C32 124.93(19) . . ?
C32 C33 C31 117.81(17) . 2_766 ?
O4 C36 C34 117.28(19) . 2_775 ?
O4 C36 C35 124.8(2) . . ?
C35 C36 C34 117.90(17) . 2_775 ?
N3 C15 H15 118.6 . . ?
N3 C15 C14 122.78(19) . . ?
C14 C15 H15 118.6 . . ?
N4 C16 H16 118.6 . . ?
N4 C16 C17 122.72(19) . . ?
C17 C16 H16 118.6 . . ?
N4 C20 C21 113.52(17) . . ?
N4 C20 C19 121.7(2) . . ?
C19 C20 C21 124.80(19) . . ?
O3 C34 C36 116.28(17) . 2_775 ?
O3 C34 C35 126.33(19) . . ?
C35 C34 C36 117.40(18) . 2_775 ?
C31 C32 Cl1 118.48(16) . . ?
C31 C32 C33 124.53(18) . . ?
C33 C32 Cl1 116.98(15) . . ?
N6 C30 H30 118.6 . . ?
N6 C30 C29 122.87(19) . . ?
C29 C30 H30 118.6 . . ?
C10 C9 H9 120.7 . . ?
C8 C9 C10 118.64(19) . . ?
C8 C9 H9 120.7 . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.61(19) . . ?
C2 C1 H1 118.7 . . ?
C21 C22 H22 120.9 . . ?
C21 C22 C23 118.3(2) . . ?
C23 C22 H22 120.9 . . ?
C25 C24 H24 120.5 . . ?
C23 C24 C25 119.0(2) . . ?
C23 C24 H24 120.5 . . ?
C9 C8 H8 119.6 . . ?
C9 C8 C7 120.74(18) . . ?
C7 C8 H8 119.6 . . ?
C36 C35 Cl2 117.07(15) . . ?
C34 C35 Cl2 118.23(16) . . ?
C34 C35 C36 124.69(18) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 C6 118.6(2) . . ?
C8 C7 H7 120.7 . . ?
C11 C12 H12 120.5 . . ?
C13 C12 C11 119.1(2) . . ?
C13 C12 H12 120.5 . . ?
C26 C27 H27 120.2 . . ?
C26 C27 C28 119.6(2) . . ?
C28 C27 H27 120.2 . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.62(19) . . ?
C24 C23 H23 119.7 . . ?
C30 C29 H29 120.4 . . ?
C30 C29 C28 119.2(2) . . ?
C28 C29 H29 120.4 . . ?
C16 C17 H17 120.6 . . ?
C18 C17 C16 118.8(2) . . ?
C18 C17 H17 120.6 . . ?
C27 C28 H28 120.6 . . ?
C29 C28 C27 118.8(2) . . ?
C29 C28 H28 120.6 . . ?
C5 C4 H4 120.4 . . ?
C3 C4 C5 119.2(2) . . ?
C3 C4 H4 120.4 . . ?
C1 C2 H2 120.6 . . ?
C3 C2 C1 118.8(2) . . ?
C3 C2 H2 120.6 . . ?
C20 C19 H19 120.4 . . ?
C20 C19 C18 119.2(2) . . ?
C18 C19 H19 120.4 . . ?
C17 C18 C19 119.5(2) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C15 C14 H14 120.6 . . ?
C13 C14 C15 118.8(2) . . ?
C13 C14 H14 120.6 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13 120.2 . . ?
C4 C3 H3 120.1 . . ?
C2 C3 C4 119.7(2) . . ?
C2 C3 H3 120.1 . . ?

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
Fe01 N3 C11 C10 -0.7(2) . . . . ?
Fe01 N3 C11 C12 179.30(15) . . . . ?
Fe01 N3 C15 C14 -179.74(16) . . . . ?
Fe01 N2 C10 C11 -2.9(2) . . . . ?
Fe01 N2 C10 C9 177.02(14) . . . . ?
Fe01 N2 C6 C5 2.5(2) . . . . ?
Fe01 N2 C6 C7 -177.32(15) . . . . ?
Fe01 N5 C21 C20 -0.9(2) . . . . ?
Fe01 N5 C21 C22 178.52(15) . . . . ?
Fe01 N5 C25 C26 1.9(2) . . . . ?
Fe01 N5 C25 C24 -178.23(14) . . . . ?
Fe01 N6 C26 C25 0.1(2) . . . . ?
Fe01 N6 C26 C27 179.62(15) . . . . ?
Fe01 N6 C30 C29 -178.30(16) . . . . ?
Fe01 N1 C5 C6 2.5(2) . . . . ?
Fe01 N1 C5 C4 -176.72(17) . . . . ?
Fe01 N1 C1 C2 176.26(16) . . . . ?
Fe01 N4 C16 C17 -179.00(16) . . . . ?
Fe01 N4 C20 C21 -1.0(2) . . . . ?
Fe01 N4 C20 C19 178.70(17) . . . . ?
O1 C31 C32 Cl1 -1.2(3) . . . . ?
O1 C31 C32 C33 177.5(2) . . . . ?
O3 C34 C35 Cl2 1.4(3) . . . . ?
O3 C34 C35 C36 -179.3(2) . . . . ?
N3 Fe01 N2 C10 2.05(14) . . . . ?
N3 Fe01 N2 C6 -179.83(15) . . . . ?
N3 Fe01 N5 C21 89.71(14) . . . . ?
N3 Fe01 N5 C25 -91.65(14) . . . . ?
N3 C11 C12 C13 0.6(3) . . . . ?
N3 C15 C14 C13 0.4(3) . . . . ?
N2 C10 C11 N3 2.2(2) . . . . ?
N2 C10 C11 C12 -177.78(18) . . . . ?
N2 C10 C9 C8 0.8(3) . . . . ?
N2 C6 C7 C8 -0.2(3) . . . . ?
N5 C21 C20 N4 1.2(2) . . . . ?
N5 C21 C20 C19 -178.5(2) . . . . ?
N5 C21 C22 C23 0.2(3) . . . . ?
N5 C25 C24 C23 -0.8(3) . . . . ?
N6 Fe01 N2 C10 -88.33(14) . . . . ?
N6 Fe01 N2 C6 89.79(14) . . . . ?
N6 Fe01 N5 C21 179.83(15) . . . . ?
N6 Fe01 N5 C25 -1.52(14) . . . . ?
N6 C26 C25 N5 -1.2(2) . . . . ?
N6 C26 C25 C24 178.96(19) . . . . ?
N6 C26 C27 C28 -1.2(3) . . . . ?
N6 C30 C29 C28 -1.3(3) . . . . ?
N1 Fe01 N2 C10 -179.04(15) . . . . ?
N1 Fe01 N2 C6 -0.92(14) . . . . ?
N1 Fe01 N5 C21 -89.48(14) . . . . ?
N1 Fe01 N5 C25 89.17(14) . . . . ?
N1 C5 C6 N2 -3.2(2) . . . . ?
N1 C5 C6 C7 176.59(19) . . . . ?
N1 C5 C4 C3 0.3(4) . . . . ?
N1 C1 C2 C3 0.0(4) . . . . ?
O4 C36 C35 Cl2 -0.5(3) . . . . ?
O4 C36 C35 C34 -179.7(2) . . . . ?
N4 Fe01 N2 C10 91.46(14) . . . . ?
N4 Fe01 N2 C6 -90.42(14) . . . . ?
N4 Fe01 N5 C21 0.28(14) . . . . ?
N4 Fe01 N5 C25 178.92(14) . . . . ?
N4 C16 C17 C18 0.1(3) . . . . ?
N4 C20 C19 C18 0.7(3) . . . . ?
O2 C33 C32 Cl1 0.1(3) . . . . ?
O2 C33 C32 C31 -178.6(2) . . . . ?
C10 N2 C6 C5 -179.43(16) . . . . ?
C10 N2 C6 C7 0.8(3) . . . . ?
C10 C11 C12 C13 -179.3(2) . . . . ?
C10 C9 C8 C7 -0.3(3) . . . . ?
C26 N6 C30 C29 1.3(3) . . . . ?
C26 C25 C24 C23 179.04(19) . . . . ?
C26 C27 C28 C29 1.1(3) . . . . ?
C31 C33 C32 Cl1 -178.79(14) 2_766 . . . ?
C31 C33 C32 C31 2.5(3) 2_766 . . . ?
C21 N5 C25 C26 -179.45(16) . . . . ?
C21 N5 C25 C24 0.4(3) . . . . ?
C21 C20 C19 C18 -179.7(2) . . . . ?
C21 C22 C23 C24 -0.6(3) . . . . ?
C5 N1 C1 C2 -1.2(3) . . . . ?
C5 C6 C7 C8 180.0(2) . . . . ?
C5 C4 C3 C2 -1.5(4) . . . . ?
C11 N3 C15 C14 -0.2(3) . . . . ?
C11 C10 C9 C8 -179.25(19) . . . . ?
C11 C12 C13 C14 -0.5(4) . . . . ?
C25 N5 C21 C20 -179.48(16) . . . . ?
C25 N5 C21 C22 -0.1(3) . . . . ?
C25 C26 C27 C28 178.3(2) . . . . ?
C25 C24 C23 C22 0.9(3) . . . . ?
C6 N2 C10 C11 178.99(16) . . . . ?
C6 N2 C10 C9 -1.1(3) . . . . ?
C6 C5 C4 C3 -178.9(2) . . . . ?
C33 C31 C32 Cl1 178.81(14) 2_766 . . . ?
C33 C31 C32 C33 -2.5(3) 2_766 . . . ?
C36 C34 C35 Cl2 -178.36(14) 2_775 . . . ?
C36 C34 C35 C36 0.9(3) 2_775 . . . ?
C15 N3 C11 C10 179.70(17) . . . . ?
C15 N3 C11 C12 -0.3(3) . . . . ?
C15 C14 C13 C12 0.0(4) . . . . ?
C16 N4 C20 C21 179.71(16) . . . . ?
C16 N4 C20 C19 -0.6(3) . . . . ?
C16 C17 C18 C19 -0.1(4) . . . . ?
C20 N4 C16 C17 0.2(3) . . . . ?
C20 C21 C22 C23 179.47(19) . . . . ?
C20 C19 C18 C17 -0.3(4) . . . . ?
C34 C36 C35 Cl2 178.36(14) 2_775 . . . ?
C34 C36 C35 C34 -0.9(3) 2_775 . . . ?
C30 N6 C26 C25 -179.55(17) . . . . ?
C30 N6 C26 C27 0.0(3) . . . . ?
C30 C29 C28 C27 0.1(3) . . . . ?
C9 C10 C11 N3 -177.70(18) . . . . ?
C9 C10 C11 C12 2.3(3) . . . . ?
C9 C8 C7 C6 0.0(3) . . . . ?
C1 N1 C5 C6 -179.69(17) . . . . ?
C1 N1 C5 C4 1.0(3) . . . . ?
C1 C2 C3 C4 1.4(4) . . . . ?
C22 C21 C20 N4 -178.16(19) . . . . ?
C22 C21 C20 C19 2.2(3) . . . . ?
C27 C26 C25 N5 179.26(18) . . . . ?
C27 C26 C25 C24 -0.6(3) . . . . ?
C4 C5 C6 N2 176.1(2) . . . . ?
C4 C5 C6 C7 -4.2(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.112
_oxdiff_exptl_absorpt_empirical_full_min 0.931
####################################################################### 
# 
# 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_exp_693
_database_code_depnum_ccdc_archive 'CCDC 2374765'
loop_
_audit_author_name
_audit_author_address
'Akio Mishima'
;Fukuoka University
Japan
;
_audit_update_record             
;
2024-07-31 deposited with the CCDC.	2025-01-15 downloaded from the CCDC.
;
_audit_creation_date             2024-06-27
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H22 Co N6, 2(C3 Cl O2), 6(H2 O)'
_chemical_formula_sum            'C36 H34 Cl2 Co N6 O10'
_chemical_formula_weight         840.52
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N10O20Co1Cl2
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.03554(12)
_cell_length_b                   9.04710(13)
_cell_length_c                   22.3304(3)
_cell_angle_alpha                92.0770(12)
_cell_angle_beta                 95.9851(11)
_cell_angle_gamma                90.5673(11)
_cell_volume                     1814.09(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14361
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.6200
_cell_measurement_theta_min      2.2540
_shelx_estimated_absorpt_T_max   0.934
_shelx_estimated_absorpt_T_min   0.683
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             866
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            35106
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.532
_diffrn_reflns_theta_min         2.253
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 107.00   0.50   25.00    --   20.00  54.00-116.41  362
  2  ω    -74.00   5.00   0.50   25.00    --   20.00  54.00 -60.00  158
  3  ω     15.00  84.00   0.50   25.00    --   20.00  54.00 -60.00  138
  4  ω    -73.00  75.00   0.50   25.00    --   20.00  54.00-180.00  296
  5  ω    -69.00   2.00   0.50   25.00    --   20.00  54.00 -30.00  142
  6  ω     22.00  47.00   0.50   25.00    --   20.00  54.00 -30.00   50
  7  ω     77.00 102.00   0.50   25.00    --   20.00  54.00 -30.00   50
  8  ω    -73.00 -17.00   0.50   25.00    --   20.00  54.00  60.00  112
  9  ω     56.00 109.00   0.50   25.00    --   20.00  54.00  60.00  106
 10  ω      6.00  93.00   0.50   25.00    --   20.00  54.00-150.00  174
 11  ω    -63.00 -37.00   0.50   25.00    --   20.00  54.00 120.00   52
 12  ω      8.00  78.00   0.50   25.00    --   20.00  54.00 120.00  140
 13  ω    -60.00 -34.00   0.50   25.00    --   20.00  54.00   0.00   52
 14  ω      0.00  25.00   0.50   25.00    --   20.00  54.00   0.00   50
 15  ω    -40.00 -15.00   0.50   25.00    --   20.00  54.00-120.00   50
 16  ω     25.00  50.00   0.50   25.00    --   20.00  54.00-120.00   50
 17  ω    -68.00  24.00   0.50   25.00    --   20.00  54.00 107.90  184
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0526315000
_diffrn_orient_matrix_UB_12      0.0408135000
_diffrn_orient_matrix_UB_13      -0.0144114000
_diffrn_orient_matrix_UB_21      -0.0587780000
_diffrn_orient_matrix_UB_22      0.0325705000
_diffrn_orient_matrix_UB_23      -0.0183405000
_diffrn_orient_matrix_UB_31      -0.0025341000
_diffrn_orient_matrix_UB_32      0.0585607000
_diffrn_orient_matrix_UB_33      0.0218496000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8338
_reflns_number_total             10517
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0006(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         10517
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0421
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0369P)²+0.6483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0872
_refine_ls_wR_factor_ref         0.0929
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O10-H10A = O10-H10B
 0.85 with sigma of 0.02
 O9-H9A = O9-H9B
 0.85 with sigma of 0.02
 O7-H7A = O7-H7B
 0.85 with sigma of 0.02
 O8-H8A = O8-H8B
 0.85 with sigma of 0.02
 O5-H5A = O5-H5B
 0.85 with sigma of 0.02
 O6-H6A = O6-H6B
 0.85 with sigma of 0.02
 H10A-H10B
 1.34 with sigma of 0.04
 H9A-H9B
 1.34 with sigma of 0.04
 H7A-H7B
 1.34 with sigma of 0.04
 H8A-H8B
 1.34 with sigma of 0.04
 H5A-H5B
 1.34 with sigma of 0.04
 H6A-H6B
 1.34 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C16(H16), C9(H9), C22(H22), C1(H1), C30(H30), C7(H7),
 C19(H19), C17(H17), C14(H14), C27(H27), C8(H8), C15(H15), C18(H18), C2(H2),
 C13(H13), C29(H29), C3(H3), C12(H12), C4(H4), C28(H28)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.27735(2) 0.17978(2) 0.25053(2) 0.03025(6) Uani 1 1 d . . . . .
Cl5 Cl 0.17984(6) 0.70742(7) 0.10024(2) 0.05999(15) Uani 1 1 d . . . . .
Cl11 Cl -0.22498(7) 0.13818(6) 0.39962(2) 0.06540(16) Uani 1 1 d . . . . .
N6 N 0.37115(15) -0.02601(15) 0.26336(6) 0.0347(3) Uani 1 1 d . . . . .
N3 N 0.48157(15) 0.27209(15) 0.23653(6) 0.0335(3) Uani 1 1 d . . . . .
N1 N 0.06595(15) 0.08573(15) 0.23218(6) 0.0356(3) Uani 1 1 d . . . . .
O1 O 0.28465(14) 0.58270(15) -0.01425(6) 0.0474(3) Uani 1 1 d . . . . .
O4 O -0.11032(17) -0.16670(16) 0.40336(6) 0.0571(4) Uani 1 1 d . . . . .
N4 N 0.19151(15) 0.38558(15) 0.26947(6) 0.0347(3) Uani 1 1 d . . . . .
N2 N 0.25562(15) 0.18434(14) 0.16494(6) 0.0313(3) Uani 1 1 d . . . . .
O10 O 0.53403(17) 0.46614(18) 0.41167(7) 0.0585(4) Uani 1 1 d D . . . .
H10A H 0.6243(19) 0.496(3) 0.4153(12) 0.088 Uiso 1 1 d D U . . .
H10B H 0.490(3) 0.532(3) 0.4313(12) 0.088 Uiso 1 1 d D U . . .
C20 C 0.18537(18) 0.41333(19) 0.32927(7) 0.0359(4) Uani 1 1 d . . . . .
C21 C 0.24113(18) 0.29221(19) 0.36743(7) 0.0360(4) Uani 1 1 d . . . . .
O9 O 0.61007(17) 0.31302(18) 0.52172(7) 0.0564(4) Uani 1 1 d D . . . .
H9A H 0.7042(19) 0.305(3) 0.5202(12) 0.085 Uiso 1 1 d D U . . .
H9B H 0.580(3) 0.342(3) 0.4877(9) 0.085 Uiso 1 1 d D U . . .
O3 O -0.07923(15) 0.28801(14) 0.51312(6) 0.0497(3) Uani 1 1 d . . . . .
N5 N 0.29259(14) 0.17682(15) 0.33591(6) 0.0322(3) Uani 1 1 d . . . . .
C11 C 0.49743(18) 0.29045(17) 0.17749(7) 0.0332(3) Uani 1 1 d . . . . .
C35 C -0.09943(19) 0.06452(19) 0.45490(8) 0.0377(4) Uani 1 1 d . . . . .
O7 O 0.29554(18) -0.10330(17) -0.02206(7) 0.0565(4) Uani 1 1 d D . . . .
H7A H 0.340(3) -0.082(3) 0.0121(9) 0.085 Uiso 1 1 d D U . . .
H7B H 0.293(3) -0.1961(18) -0.0234(12) 0.085 Uiso 1 1 d D U . . .
O2 O -0.12803(16) 0.58933(17) 0.09822(6) 0.0581(4) Uani 1 1 d . . . . .
C36 C -0.06150(19) -0.08538(19) 0.44671(8) 0.0373(4) Uani 1 1 d . . . . .
C34 C -0.04704(18) 0.15396(18) 0.50416(8) 0.0357(3) Uani 1 1 d . . . . .
O8 O 0.49741(18) -0.05315(17) 0.08477(7) 0.0557(4) Uani 1 1 d D . . . .
H8A H 0.531(3) -0.1415(19) 0.0815(12) 0.083 Uiso 1 1 d D U . . .
H8B H 0.559(3) -0.007(3) 0.0673(12) 0.083 Uiso 1 1 d D U . . .
C10 C 0.36526(18) 0.24439(17) 0.13632(7) 0.0328(3) Uani 1 1 d . . . . .
C23 C 0.3035(2) 0.1685(2) 0.45893(8) 0.0504(5) Uani 1 1 d . . . . .
H23 H 0.308335 0.166130 0.500690 0.060 Uiso 1 1 calc R U . . .
C32 C 0.08260(19) 0.59300(19) 0.04484(7) 0.0366(4) Uani 1 1 d . . . . .
C5 C 0.02192(18) 0.07066(19) 0.17225(7) 0.0367(4) Uani 1 1 d . . . . .
C24 C 0.3551(2) 0.0501(2) 0.42648(8) 0.0468(4) Uani 1 1 d . . . . .
H24 H 0.393533 -0.032350 0.446008 0.056 Uiso 1 1 calc R U . . .
C33 C -0.06423(19) 0.55063(18) 0.05401(7) 0.0361(3) Uani 1 1 d . . . . .
C6 C 0.12791(19) 0.13370(18) 0.13371(7) 0.0351(3) Uani 1 1 d . . . . .
C16 C 0.1428(2) 0.4888(2) 0.23118(8) 0.0421(4) Uani 1 1 d . . . . .
H16 H 0.148504 0.470618 0.190229 0.051 Uiso 1 1 calc R U . . .
C9 C 0.3476(2) 0.2573(2) 0.07418(8) 0.0432(4) Uani 1 1 d . . . . .
H9 H 0.422398 0.299699 0.054547 0.052 Uiso 1 1 calc R U . . .
C22 C 0.2452(2) 0.2898(2) 0.42995(8) 0.0464(4) Uani 1 1 d . . . . .
H22 H 0.209204 0.368811 0.451686 0.056 Uiso 1 1 calc R U . . .
O5 O 0.54546(19) 0.64967(19) 0.07665(9) 0.0715(5) Uani 1 1 d D . . . .
H5A H 0.473(3) 0.616(3) 0.0537(13) 0.107 Uiso 1 1 d D U . . .
H5B H 0.620(2) 0.605(3) 0.0702(14) 0.107 Uiso 1 1 d D U . . .
C1 C -0.0236(2) 0.0334(2) 0.27073(8) 0.0430(4) Uani 1 1 d . . . . .
H1 H 0.005479 0.045578 0.311822 0.052 Uiso 1 1 calc R U . . .
C30 C 0.4102(2) -0.1240(2) 0.22175(8) 0.0430(4) Uani 1 1 d . . . . .
H30 H 0.392973 -0.101642 0.181327 0.052 Uiso 1 1 calc R U . . .
C26 C 0.39697(19) -0.05848(19) 0.32239(7) 0.0364(4) Uani 1 1 d . . . . .
C7 C 0.1058(2) 0.1442(2) 0.07155(8) 0.0462(4) Uani 1 1 d . . . . .
H7 H 0.017632 0.110123 0.050036 0.055 Uiso 1 1 calc R U . . .
C31 C 0.15329(18) 0.54892(18) -0.00490(8) 0.0349(3) Uani 1 1 d . . . . .
C19 C 0.1297(2) 0.5450(2) 0.35060(9) 0.0482(5) Uani 1 1 d . . . . .
H19 H 0.127258 0.563062 0.391752 0.058 Uiso 1 1 calc R U . . .
C17 C 0.0844(2) 0.6215(2) 0.24960(10) 0.0529(5) Uani 1 1 d . . . . .
H17 H 0.050432 0.690425 0.221663 0.064 Uiso 1 1 calc R U . . .
C25 C 0.34846(18) 0.05671(19) 0.36408(7) 0.0361(4) Uani 1 1 d . . . . .
C14 C 0.7268(2) 0.3702(2) 0.26205(10) 0.0547(5) Uani 1 1 d . . . . .
H14 H 0.803618 0.396842 0.291598 0.066 Uiso 1 1 calc R U . . .
C27 C 0.4626(3) -0.1890(2) 0.34006(9) 0.0542(5) Uani 1 1 d . . . . .
H27 H 0.480400 -0.209336 0.380685 0.065 Uiso 1 1 calc R U . . .
C8 C 0.2176(2) 0.2064(2) 0.04218(8) 0.0477(5) Uani 1 1 d . . . . .
H8 H 0.204608 0.213804 0.000536 0.057 Uiso 1 1 calc R U . . .
C15 C 0.5950(2) 0.3119(2) 0.27753(8) 0.0419(4) Uani 1 1 d . . . . .
H15 H 0.584581 0.299741 0.318055 0.050 Uiso 1 1 calc R U . . .
C18 C 0.0778(2) 0.6491(2) 0.31014(11) 0.0571(5) Uani 1 1 d . . . . .
H18 H 0.038624 0.737275 0.323771 0.069 Uiso 1 1 calc R U . . .
O6 O -0.1685(2) 0.5180(2) 0.42523(11) 0.0808(6) Uani 1 1 d D . . . .
H6A H -0.119(3) 0.594(2) 0.4314(15) 0.121 Uiso 1 1 d D U . . .
H6B H -0.131(4) 0.456(3) 0.4497(14) 0.121 Uiso 1 1 d D U . . .
C2 C -0.1573(2) -0.0377(2) 0.25236(10) 0.0539(5) Uani 1 1 d . . . . .
H2 H -0.217077 -0.073014 0.280337 0.065 Uiso 1 1 calc R U . . .
C13 C 0.7426(2) 0.3884(3) 0.20207(11) 0.0582(5) Uani 1 1 d . . . . .
H13 H 0.830433 0.427621 0.190653 0.070 Uiso 1 1 calc R U . . .
C29 C 0.4752(2) -0.2571(2) 0.23648(10) 0.0552(5) Uani 1 1 d . . . . .
H29 H 0.500558 -0.323549 0.206597 0.066 Uiso 1 1 calc R U . . .
C3 C -0.1998(2) -0.0549(3) 0.19158(10) 0.0667(7) Uani 1 1 d . . . . .
H3 H -0.288527 -0.103847 0.177876 0.080 Uiso 1 1 calc R U . . .
C12 C 0.6272(2) 0.3479(2) 0.15904(9) 0.0464(4) Uani 1 1 d . . . . .
H12 H 0.636333 0.359014 0.118341 0.056 Uiso 1 1 calc R U . . .
C4 C -0.1105(2) 0.0006(3) 0.15085(9) 0.0564(5) Uani 1 1 d . . . . .
H4 H -0.139100 -0.009126 0.109658 0.068 Uiso 1 1 calc R U . . .
C28 C 0.5016(3) -0.2893(2) 0.29635(11) 0.0665(6) Uani 1 1 d . . . . .
H28 H 0.545437 -0.378139 0.307404 0.080 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N6 2.0702(14) . ?
Co1 N3 2.0757(14) . ?
Co1 N1 2.0784(14) . ?
Co1 N4 2.0706(14) . ?
Co1 N2 1.9028(13) . ?
Co1 N5 1.8985(13) . ?
Cl5 C32 1.7426(17) . ?
Cl11 C35 1.7429(17) . ?
N6 C30 1.338(2) . ?
N6 C26 1.358(2) . ?
N3 C11 1.3569(19) . ?
N3 C15 1.339(2) . ?
N1 C5 1.357(2) . ?
N1 C1 1.337(2) . ?
O1 C31 1.263(2) . ?
O4 C36 1.235(2) . ?
N4 C20 1.357(2) . ?
N4 C16 1.336(2) . ?
N2 C10 1.353(2) . ?
N2 C6 1.351(2) . ?
O10 H10A 0.853(16) . ?
O10 H10B 0.851(16) . ?
C20 C21 1.473(2) . ?
C20 C19 1.386(2) . ?
C21 N5 1.351(2) . ?
C21 C22 1.394(2) . ?
O9 H9A 0.859(16) . ?
O9 H9B 0.832(16) . ?
O3 C34 1.264(2) . ?
N5 C25 1.351(2) . ?
C11 C10 1.476(2) . ?
C11 C12 1.385(2) . ?
C35 C36 1.412(2) . ?
C35 C34 1.381(2) . ?
O7 H7A 0.841(16) . ?
O7 H7B 0.839(16) . ?
O2 C33 1.236(2) . ?
C36 C34 1.545(2) 2_556 ?
O8 H8A 0.862(16) . ?
O8 H8B 0.830(16) . ?
C10 C9 1.389(2) . ?
C23 H23 0.9300 . ?
C23 C24 1.383(3) . ?
C23 C22 1.375(3) . ?
C32 C33 1.415(2) . ?
C32 C31 1.386(2) . ?
C5 C6 1.477(2) . ?
C5 C4 1.380(2) . ?
C24 H24 0.9300 . ?
C24 C25 1.392(2) . ?
C33 C31 1.546(2) 2_565 ?
C6 C7 1.388(2) . ?
C16 H16 0.9300 . ?
C16 C17 1.382(3) . ?
C9 H9 0.9300 . ?
C9 C8 1.376(3) . ?
C22 H22 0.9300 . ?
O5 H5A 0.839(17) . ?
O5 H5B 0.816(17) . ?
C1 H1 0.9300 . ?
C1 C2 1.380(3) . ?
C30 H30 0.9300 . ?
C30 C29 1.380(3) . ?
C26 C25 1.473(2) . ?
C26 C27 1.379(2) . ?
C7 H7 0.9300 . ?
C7 C8 1.386(3) . ?
C19 H19 0.9300 . ?
C19 C18 1.380(3) . ?
C17 H17 0.9300 . ?
C17 C18 1.373(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.379(3) . ?
C14 C13 1.377(3) . ?
C27 H27 0.9300 . ?
C27 C28 1.383(3) . ?
C8 H8 0.9300 . ?
C15 H15 0.9300 . ?
C18 H18 0.9300 . ?
O6 H6A 0.817(17) . ?
O6 H6B 0.849(17) . ?
C2 H2 0.9300 . ?
C2 C3 1.374(3) . ?
C13 H13 0.9300 . ?
C13 C12 1.379(3) . ?
C29 H29 0.9300 . ?
C29 C28 1.375(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.381(3) . ?
C12 H12 0.9300 . ?
C4 H4 0.9300 . ?
C28 H28 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N6 Co1 N3 91.48(5) . . ?
N6 Co1 N1 91.41(5) . . ?
N6 Co1 N4 160.38(5) . . ?
N3 Co1 N1 160.09(5) . . ?
N4 Co1 N3 91.79(5) . . ?
N4 Co1 N1 92.07(5) . . ?
N2 Co1 N6 100.97(5) . . ?
N2 Co1 N3 79.94(6) . . ?
N2 Co1 N1 80.18(6) . . ?
N2 Co1 N4 98.66(5) . . ?
N5 Co1 N6 80.16(6) . . ?
N5 Co1 N3 101.50(5) . . ?
N5 Co1 N1 98.40(5) . . ?
N5 Co1 N4 80.23(6) . . ?
N5 Co1 N2 178.18(6) . . ?
C30 N6 Co1 128.30(12) . . ?
C30 N6 C26 118.70(15) . . ?
C26 N6 Co1 112.99(11) . . ?
C11 N3 Co1 113.24(11) . . ?
C15 N3 Co1 128.37(12) . . ?
C15 N3 C11 118.39(15) . . ?
C5 N1 Co1 112.76(11) . . ?
C1 N1 Co1 128.69(12) . . ?
C1 N1 C5 118.44(15) . . ?
C20 N4 Co1 112.94(11) . . ?
C16 N4 Co1 128.65(12) . . ?
C16 N4 C20 118.41(15) . . ?
C10 N2 Co1 119.62(11) . . ?
C6 N2 Co1 119.48(11) . . ?
C6 N2 C10 120.83(14) . . ?
H10A O10 H10B 103(2) . . ?
N4 C20 C21 114.01(14) . . ?
N4 C20 C19 121.27(17) . . ?
C19 C20 C21 124.72(16) . . ?
N5 C21 C20 113.34(14) . . ?
N5 C21 C22 120.46(17) . . ?
C22 C21 C20 126.19(16) . . ?
H9A O9 H9B 103(2) . . ?
C21 N5 Co1 119.40(11) . . ?
C25 N5 Co1 119.56(11) . . ?
C25 N5 C21 120.97(14) . . ?
N3 C11 C10 113.84(14) . . ?
N3 C11 C12 121.77(16) . . ?
C12 C11 C10 124.39(15) . . ?
C36 C35 Cl11 117.02(13) . . ?
C34 C35 Cl11 118.51(13) . . ?
C34 C35 C36 124.45(15) . . ?
H7A O7 H7B 103(2) . . ?
O4 C36 C35 124.73(17) . . ?
O4 C36 C34 117.35(15) . 2_556 ?
C35 C36 C34 117.91(14) . 2_556 ?
O3 C34 C35 126.15(16) . . ?
O3 C34 C36 116.22(15) . 2_556 ?
C35 C34 C36 117.64(15) . 2_556 ?
H8A O8 H8B 100(2) . . ?
N2 C10 C11 113.23(13) . . ?
N2 C10 C9 120.51(16) . . ?
C9 C10 C11 126.26(16) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C22 C23 C24 120.54(16) . . ?
C33 C32 Cl5 117.29(13) . . ?
C31 C32 Cl5 118.43(13) . . ?
C31 C32 C33 124.28(16) . . ?
N1 C5 C6 114.09(14) . . ?
N1 C5 C4 121.47(17) . . ?
C4 C5 C6 124.44(16) . . ?
C23 C24 H24 120.6 . . ?
C23 C24 C25 118.81(18) . . ?
C25 C24 H24 120.6 . . ?
O2 C33 C32 124.70(17) . . ?
O2 C33 C31 117.20(15) . 2_565 ?
C32 C33 C31 118.09(14) . 2_565 ?
N2 C6 C5 113.29(14) . . ?
N2 C6 C7 120.54(16) . . ?
C7 C6 C5 126.17(16) . . ?
N4 C16 H16 118.5 . . ?
N4 C16 C17 123.03(18) . . ?
C17 C16 H16 118.5 . . ?
C10 C9 H9 120.6 . . ?
C8 C9 C10 118.90(17) . . ?
C8 C9 H9 120.6 . . ?
C21 C22 H22 120.6 . . ?
C23 C22 C21 118.83(18) . . ?
C23 C22 H22 120.6 . . ?
H5A O5 H5B 109(3) . . ?
N1 C1 H1 118.5 . . ?
N1 C1 C2 123.02(17) . . ?
C2 C1 H1 118.5 . . ?
N6 C30 H30 118.7 . . ?
N6 C30 C29 122.56(17) . . ?
C29 C30 H30 118.7 . . ?
N6 C26 C25 113.98(14) . . ?
N6 C26 C27 121.54(17) . . ?
C27 C26 C25 124.48(16) . . ?
C6 C7 H7 120.6 . . ?
C8 C7 C6 118.74(18) . . ?
C8 C7 H7 120.6 . . ?
O1 C31 C32 126.11(16) . . ?
O1 C31 C33 116.28(15) . 2_565 ?
C32 C31 C33 117.61(14) . 2_565 ?
C20 C19 H19 120.3 . . ?
C18 C19 C20 119.30(18) . . ?
C18 C19 H19 120.3 . . ?
C16 C17 H17 120.8 . . ?
C18 C17 C16 118.45(19) . . ?
C18 C17 H17 120.8 . . ?
N5 C25 C24 120.38(17) . . ?
N5 C25 C26 113.26(14) . . ?
C24 C25 C26 126.36(16) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.82(19) . . ?
C26 C27 H27 120.6 . . ?
C26 C27 C28 118.89(18) . . ?
C28 C27 H27 120.6 . . ?
C9 C8 C7 120.48(16) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
N3 C15 C14 122.61(17) . . ?
N3 C15 H15 118.7 . . ?
C14 C15 H15 118.7 . . ?
C19 C18 H18 120.2 . . ?
C17 C18 C19 119.52(18) . . ?
C17 C18 H18 120.2 . . ?
H6A O6 H6B 107(3) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 C1 118.14(19) . . ?
C3 C2 H2 120.9 . . ?
C14 C13 H13 120.2 . . ?
C14 C13 C12 119.57(18) . . ?
C12 C13 H13 120.2 . . ?
C30 C29 H29 120.7 . . ?
C28 C29 C30 118.5(2) . . ?
C28 C29 H29 120.7 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 119.94(19) . . ?
C4 C3 H3 120.0 . . ?
C11 C12 H12 120.6 . . ?
C13 C12 C11 118.84(18) . . ?
C13 C12 H12 120.6 . . ?
C5 C4 C3 118.96(18) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C27 C28 H28 120.1 . . ?
C29 C28 C27 119.79(19) . . ?
C29 C28 H28 120.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N6 C30 C29 178.57(14) . . . . ?
Co1 N6 C26 C25 1.91(17) . . . . ?
Co1 N6 C26 C27 -178.28(15) . . . . ?
Co1 N3 C11 C10 1.40(16) . . . . ?
Co1 N3 C11 C12 -178.78(13) . . . . ?
Co1 N3 C15 C14 178.88(14) . . . . ?
Co1 N1 C5 C6 -4.23(17) . . . . ?
Co1 N1 C5 C4 175.17(15) . . . . ?
Co1 N1 C1 C2 -174.53(15) . . . . ?
Co1 N4 C20 C21 0.20(17) . . . . ?
Co1 N4 C20 C19 -179.34(13) . . . . ?
Co1 N4 C16 C17 178.45(14) . . . . ?
Co1 N2 C10 C11 4.35(17) . . . . ?
Co1 N2 C10 C9 -175.89(12) . . . . ?
Co1 N2 C6 C5 -3.67(18) . . . . ?
Co1 N2 C6 C7 176.04(12) . . . . ?
Co1 N5 C25 C24 -177.49(12) . . . . ?
Co1 N5 C25 C26 2.16(18) . . . . ?
Cl5 C32 C33 O2 0.3(2) . . . . ?
Cl5 C32 C33 C31 179.08(11) . . . 2_565 ?
Cl5 C32 C31 O1 0.7(3) . . . . ?
Cl5 C32 C31 C33 -179.09(11) . . . 2_565 ?
Cl11 C35 C36 O4 0.3(3) . . . . ?
Cl11 C35 C36 C34 -178.73(12) . . . 2_556 ?
Cl11 C35 C34 O3 -1.4(3) . . . . ?
Cl11 C35 C34 C36 178.70(12) . . . 2_556 ?
N6 Co1 N5 C21 -177.93(12) . . . . ?
N6 Co1 N5 C25 -0.90(12) . . . . ?
N6 C30 C29 C28 -0.5(3) . . . . ?
N6 C26 C25 N5 -2.6(2) . . . . ?
N6 C26 C25 C24 177.01(16) . . . . ?
N6 C26 C27 C28 -0.6(3) . . . . ?
N3 Co1 N5 C21 92.56(12) . . . . ?
N3 Co1 N5 C25 -90.41(12) . . . . ?
N3 C11 C10 N2 -3.57(19) . . . . ?
N3 C11 C10 C9 176.68(15) . . . . ?
N3 C11 C12 C13 -0.5(3) . . . . ?
N1 Co1 N5 C21 -87.96(12) . . . . ?
N1 Co1 N5 C25 89.08(12) . . . . ?
N1 C5 C6 N2 5.1(2) . . . . ?
N1 C5 C6 C7 -174.54(16) . . . . ?
N1 C5 C4 C3 0.2(3) . . . . ?
N1 C1 C2 C3 -0.1(3) . . . . ?
N4 Co1 N5 C21 2.71(11) . . . . ?
N4 Co1 N5 C25 179.74(12) . . . . ?
N4 C20 C21 N5 1.9(2) . . . . ?
N4 C20 C21 C22 -178.75(16) . . . . ?
N4 C20 C19 C18 0.8(3) . . . . ?
N4 C16 C17 C18 0.8(3) . . . . ?
N2 C10 C9 C8 -0.8(2) . . . . ?
N2 C6 C7 C8 0.5(3) . . . . ?
C20 N4 C16 C17 -1.0(3) . . . . ?
C20 C21 N5 Co1 -3.34(18) . . . . ?
C20 C21 N5 C25 179.67(14) . . . . ?
C20 C21 C22 C23 -178.86(16) . . . . ?
C20 C19 C18 C17 -1.0(3) . . . . ?
C21 C20 C19 C18 -178.69(17) . . . . ?
C21 N5 C25 C24 -0.5(2) . . . . ?
C21 N5 C25 C26 179.15(14) . . . . ?
N5 C21 C22 C23 0.5(2) . . . . ?
C11 N3 C15 C14 -0.2(3) . . . . ?
C11 C10 C9 C8 178.93(16) . . . . ?
C36 C35 C34 O3 -179.57(17) . . . . ?
C36 C35 C34 C36 0.6(3) . . . 2_556 ?
C34 C35 C36 O4 178.47(18) . . . . ?
C34 C35 C36 C34 -0.6(3) . . . 2_556 ?
C10 N2 C6 C5 179.40(13) . . . . ?
C10 N2 C6 C7 -0.9(2) . . . . ?
C10 C11 C12 C13 179.32(18) . . . . ?
C10 C9 C8 C7 0.4(3) . . . . ?
C23 C24 C25 N5 0.0(3) . . . . ?
C23 C24 C25 C26 -179.58(16) . . . . ?
C5 N1 C1 C2 1.3(3) . . . . ?
C5 C6 C7 C8 -179.82(16) . . . . ?
C24 C23 C22 C21 -1.0(3) . . . . ?
C33 C32 C31 O1 -178.96(17) . . . . ?
C33 C32 C31 C33 1.2(3) . . . 2_565 ?
C6 N2 C10 C11 -178.72(13) . . . . ?
C6 N2 C10 C9 1.0(2) . . . . ?
C6 C5 C4 C3 179.5(2) . . . . ?
C6 C7 C8 C9 -0.3(3) . . . . ?
C16 N4 C20 C21 179.77(15) . . . . ?
C16 N4 C20 C19 0.2(2) . . . . ?
C16 C17 C18 C19 0.3(3) . . . . ?
C22 C21 N5 Co1 177.24(12) . . . . ?
C22 C21 N5 C25 0.3(2) . . . . ?
C22 C23 C24 C25 0.7(3) . . . . ?
C1 N1 C5 C6 179.27(15) . . . . ?
C1 N1 C5 C4 -1.3(3) . . . . ?
C1 C2 C3 C4 -1.1(4) . . . . ?
C30 N6 C26 C25 -179.55(14) . . . . ?
C30 N6 C26 C27 0.3(3) . . . . ?
C30 C29 C28 C27 0.2(4) . . . . ?
C26 N6 C30 C29 0.3(3) . . . . ?
C26 C27 C28 C29 0.4(4) . . . . ?
C31 C32 C33 O2 179.95(18) . . . . ?
C31 C32 C33 C31 -1.2(3) . . . 2_565 ?
C19 C20 C21 N5 -178.62(16) . . . . ?
C19 C20 C21 C22 0.8(3) . . . . ?
C25 C26 C27 C28 179.2(2) . . . . ?
C14 C13 C12 C11 0.3(3) . . . . ?
C27 C26 C25 N5 177.58(17) . . . . ?
C27 C26 C25 C24 -2.8(3) . . . . ?
C15 N3 C11 C10 -179.43(14) . . . . ?
C15 N3 C11 C12 0.4(2) . . . . ?
C15 C14 C13 C12 -0.1(3) . . . . ?
C2 C3 C4 C5 1.1(4) . . . . ?
C13 C14 C15 N3 0.0(3) . . . . ?
C12 C11 C10 N2 176.61(15) . . . . ?
C12 C11 C10 C9 -3.1(3) . . . . ?
C4 C5 C6 N2 -174.24(18) . . . . ?
C4 C5 C6 C7 6.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.091
_oxdiff_exptl_absorpt_empirical_full_min 0.932
