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

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

data_2016ncs0311
_database_code_depnum_ccdc_archive 'CCDC 1874840'
_audit_update_record             
;
2018-12-12 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;
_audit_creation_date             2016-05-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H28 N2 Ni O4'
_chemical_formula_sum            'C30 H28 N2 Ni O4'
_chemical_formula_weight         539.25
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C15 H20 N2 O Ni'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   6.7178(3)
_cell_length_b                   9.3940(4)
_cell_length_c                   10.1699(4)
_cell_angle_alpha                69.232(4)
_cell_angle_beta                 87.650(4)
_cell_angle_gamma                89.471(4)
_cell_volume                     599.58(5)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    6995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4810
_cell_measurement_theta_min      2.3460
_shelx_estimated_absorpt_T_max   0.967
_shelx_estimated_absorpt_T_min   0.890
_exptl_absorpt_coefficient_mu    0.851
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             282
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.888
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8112
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.681
_diffrn_reflns_theta_min         2.143
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -106.00  74.00   1.00    5.00    --  -16.00   0.00 114.00  180
  2  ω    -70.00  23.00   1.00    5.00    --  -16.00 -72.00-115.00   93
  3  ω    -61.00  23.00   1.00    5.00    --  -16.00 -72.00  81.00   84
  4  ω    -30.00  -2.00   1.00    5.00    --  -16.00  72.00  16.00   28
  5  ω    -63.00 -48.00   1.00    5.00    --  -16.00 -72.00-148.00   15
  6  ω   -106.00  23.00   1.00    5.00    --  -16.00 -72.00  49.00  129
  7  ω    -49.00 -26.00   1.00    5.00    --  -16.00   0.00-148.00   23
;
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_detector_area_resol_mean 28.5714

_diffrn_measurement_device       'four-circle κ diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'

_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_radiation_wavelength     0.71075

_diffrn_source                   'Rotating Anode'
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_diffrn_source_current           55.0
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'

_diffrn_ambient_temperature      100(2)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2929
_reflns_number_total             3018
_reflns_odcompleteness_completeness 88.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.62
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3018
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0293
_refine_ls_restrained_S_all      1.185
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0491P)²+0.2447P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0890
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Ni1 Ni 0.5000 0.5000 0.5000 0.01065(9) Uani 1 2 d S T P . .
O1 O 0.63504(16) 0.39369(12) 0.65862(11) 0.0140(2) Uani 1 1 d . . . . .
O2 O 0.79012(16) 0.27588(12) 0.92028(11) 0.0146(2) Uani 1 1 d . . . . .
N1 N 0.67249(18) 0.42840(14) 0.38205(12) 0.0122(2) Uani 1 1 d . . . . .
C1 C 0.4999(2) 0.17102(17) 0.31785(15) 0.0171(3) Uani 1 1 d . . . . .
H1 H 0.6163 0.1408 0.3706 0.020 Uiso 1 1 calc R . . . .
C2 C 0.3625(3) 0.06244(18) 0.31768(16) 0.0203(3) Uani 1 1 d . . . . .
H2 H 0.3843 -0.0418 0.3713 0.024 Uiso 1 1 calc R . . . .
C3 C 0.1936(3) 0.1044(2) 0.24013(18) 0.0215(3) Uani 1 1 d . . . . .
H3 H 0.0990 0.0296 0.2408 0.026 Uiso 1 1 calc R . . . .
C4 C 0.1632(2) 0.25663(19) 0.16135(17) 0.0197(3) Uani 1 1 d . . . . .
H4 H 0.0487 0.2860 0.1063 0.024 Uiso 1 1 calc R . . . .
C5 C 0.2995(2) 0.36607(18) 0.16272(16) 0.0166(3) Uani 1 1 d . . . . .
H5 H 0.2768 0.4703 0.1095 0.020 Uiso 1 1 calc R . . . .
C6 C 0.4687(2) 0.32483(17) 0.24107(15) 0.0136(3) Uani 1 1 d . . . . .
C7 C 0.6184(2) 0.44446(17) 0.23831(14) 0.0135(3) Uani 1 1 d . . . . .
H7A H 0.7396 0.4350 0.1833 0.016 Uiso 1 1 calc R . . . .
H7B H 0.5617 0.5468 0.1913 0.016 Uiso 1 1 calc R . . . .
C8 C 0.8430(2) 0.36601(16) 0.41759(15) 0.0131(3) Uani 1 1 d . . . . .
H8 H 0.9231 0.3486 0.3456 0.016 Uiso 1 1 calc R . . . .
C9 C 0.9246(2) 0.32021(16) 0.55412(15) 0.0131(3) Uani 1 1 d . . . . .
C10 C 1.1154(2) 0.25534(17) 0.57165(16) 0.0148(3) Uani 1 1 d . . . . .
H10 H 1.1890 0.2478 0.4927 0.018 Uiso 1 1 calc R . . . .
C11 C 1.1964(2) 0.20271(17) 0.70199(16) 0.0166(3) Uani 1 1 d . . . . .
H11 H 1.3268 0.1613 0.7132 0.020 Uiso 1 1 calc R . . . .
C12 C 1.0844(2) 0.21094(16) 0.81761(16) 0.0148(3) Uani 1 1 d . . . . .
H12 H 1.1392 0.1739 0.9081 0.018 Uiso 1 1 calc R . . . .
C13 C 0.8963(2) 0.27167(16) 0.80280(15) 0.0127(3) Uani 1 1 d . . . . .
C14 C 0.8111(2) 0.33264(16) 0.66895(15) 0.0120(3) Uani 1 1 d . . . . .
C15 C 0.6329(2) 0.16565(18) 0.96393(16) 0.0178(3) Uani 1 1 d . . . . .
H15A H 0.5479 0.1783 0.8846 0.027 Uiso 1 1 calc GR . . . .
H15B H 0.5534 0.1800 1.0412 0.027 Uiso 1 1 calc GR . . . .
H15C H 0.6897 0.0631 0.9959 0.027 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.8394(10) . ?
Ni1 O1 1.8394(10) 2_666 ?
Ni1 N1 1.9178(12) . ?
Ni1 N1 1.9178(12) 2_666 ?
O1 C14 1.3013(17) . ?
O2 C13 1.3788(17) . ?
O2 C15 1.4282(19) . ?
N1 C7 1.4757(17) . ?
N1 C8 1.2877(19) . ?
C1 H1 0.9500 . ?
C1 C2 1.382(2) . ?
C1 C6 1.396(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.382(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.387(2) . ?
C6 C7 1.507(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8 0.9500 . ?
C8 C9 1.4309(19) . ?
C9 C10 1.405(2) . ?
C9 C14 1.407(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.374(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.395(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.373(2) . ?
C13 C14 1.4191(19) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.0 . 2_666 ?
O1 Ni1 N1 87.46(5) 2_666 . ?
O1 Ni1 N1 92.54(5) 2_666 2_666 ?
O1 Ni1 N1 92.54(5) . . ?
O1 Ni1 N1 87.46(5) . 2_666 ?
N1 Ni1 N1 180.00(6) . 2_666 ?
C14 O1 Ni1 129.30(10) . . ?
C13 O2 C15 112.45(11) . . ?
C7 N1 Ni1 121.23(9) . . ?
C8 N1 Ni1 124.50(10) . . ?
C8 N1 C7 114.26(12) . . ?
C2 C1 H1 119.8 . . ?
C2 C1 C6 120.46(15) . . ?
C6 C1 H1 119.8 . . ?
C1 C2 H2 119.8 . . ?
C3 C2 C1 120.46(15) . . ?
C3 C2 H2 119.8 . . ?
C2 C3 H3 120.2 . . ?
C2 C3 C4 119.51(15) . . ?
C4 C3 H3 120.2 . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.16(15) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.63(14) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C7 121.17(13) . . ?
C5 C6 C1 118.76(14) . . ?
C5 C6 C7 120.03(13) . . ?
N1 C7 C6 111.11(11) . . ?
N1 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
N1 C8 H8 116.6 . . ?
N1 C8 C9 126.80(14) . . ?
C9 C8 H8 116.6 . . ?
C10 C9 C8 118.32(13) . . ?
C10 C9 C14 121.19(13) . . ?
C14 C9 C8 120.40(13) . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.59(14) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119.07(14) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.11(14) . . ?
C13 C12 H12 119.4 . . ?
O2 C13 C14 119.52(13) . . ?
C12 C13 O2 119.13(13) . . ?
C12 C13 C14 121.34(14) . . ?
O1 C14 C9 123.86(13) . . ?
O1 C14 C13 119.51(13) . . ?
C9 C14 C13 116.62(13) . . ?
O2 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
O2 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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
Ni1 O1 C14 C9 -8.9(2) . . . . ?
Ni1 O1 C14 C13 172.23(10) . . . . ?
Ni1 N1 C7 C6 -78.33(14) . . . . ?
Ni1 N1 C8 C9 8.8(2) . . . . ?
O2 C13 C14 O1 1.0(2) . . . . ?
O2 C13 C14 C9 -177.97(12) . . . . ?
N1 Ni1 O1 C14 16.23(13) . . . . ?
N1 Ni1 O1 C14 -163.77(13) 2_666 . . . ?
N1 C8 C9 C10 -179.25(14) . . . . ?
N1 C8 C9 C14 4.1(2) . . . . ?
C1 C2 C3 C4 0.4(2) . . . . ?
C1 C6 C7 N1 -50.41(18) . . . . ?
C2 C1 C6 C5 -1.2(2) . . . . ?
C2 C1 C6 C7 -179.07(13) . . . . ?
C2 C3 C4 C5 -1.3(2) . . . . ?
C3 C4 C5 C6 0.8(2) . . . . ?
C4 C5 C6 C1 0.4(2) . . . . ?
C4 C5 C6 C7 178.28(13) . . . . ?
C5 C6 C7 N1 131.76(14) . . . . ?
C6 C1 C2 C3 0.8(2) . . . . ?
C7 N1 C8 C9 -172.42(14) . . . . ?
C8 N1 C7 C6 102.81(14) . . . . ?
C8 C9 C10 C11 -176.81(14) . . . . ?
C8 C9 C14 O1 -4.6(2) . . . . ?
C8 C9 C14 C13 174.33(13) . . . . ?
C9 C10 C11 C12 1.6(2) . . . . ?
C10 C9 C14 O1 178.92(13) . . . . ?
C10 C9 C14 C13 -2.2(2) . . . . ?
C10 C11 C12 C13 -0.5(2) . . . . ?
C11 C12 C13 O2 179.25(13) . . . . ?
C11 C12 C13 C14 -2.0(2) . . . . ?
C12 C13 C14 O1 -177.76(13) . . . . ?
C12 C13 C14 C9 3.3(2) . . . . ?
C14 C9 C10 C11 -0.2(2) . . . . ?
C15 O2 C13 C12 -106.41(15) . . . . ?
C15 O2 C13 C14 74.82(16) . . . . ?

_shelx_SHELXL_version_number     2014/7
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.357
_oxdiff_exptl_absorpt_empirical_full_min 0.637
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_chemical_properties_physical    Moisture-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_co1s
_database_code_depnum_ccdc_archive 'CCDC 1874842'
_audit_update_record             
;
2018-12-18 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H42 N3 O6 Co1, (C1 H6 O2)'
_chemical_formula_sum            'C46 H48 Co N3 O8'
_chemical_formula_weight         829.82

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

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

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

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

_cell_length_a                   10.3690(2)
_cell_length_b                   10.7727(3)
_cell_length_c                   20.5457(7)
_cell_angle_alpha                85.474(2)
_cell_angle_beta                 84.339(2)
_cell_angle_gamma                63.261(3)
_cell_volume                     2038.05(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    23563
_cell_measurement_theta_min      2.8450
_cell_measurement_theta_max      30.3820

_exptl_crystal_description       Block
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    0.472
_shelx_estimated_absorpt_T_min   0.954
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79861
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
crysalispro 1.171.39.9g (rigaku oxford diffraction, 2015)
empirical absorption correction using spherical harmonics,
 implemented in scale3 abspack scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xtalab afc12 (rcd3): kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            41114
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.205
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7465
_reflns_number_gt                7294
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

 Structure factors included contributions from the .fab file.

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

_computing_data_collection       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_cell_refinement       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_data_reduction        'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0129P)²+3.1620P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7465
_refine_ls_number_parameters     499
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.0929
_refine_ls_wR_factor_gt          0.0924
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_restrained_S_all      1.201
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.20716(3) 0.90292(3) 0.24609(2) 0.00997(8) Uani 1 1 d . . . . .
O1 O 0.30681(17) 0.86749(17) 0.32402(8) 0.0155(3) Uani 1 1 d . . . . .
N1 N 0.0319(2) 1.05408(19) 0.28389(9) 0.0122(4) Uani 1 1 d . . . . .
C1 C 0.5999(3) 0.7436(3) 0.45864(14) 0.0303(7) Uani 1 1 d . . . . .
H1A H 0.613764 0.823569 0.469433 0.046 Uiso 1 1 calc R U . . .
H1B H 0.691361 0.672074 0.439764 0.046 Uiso 1 1 calc R U . . .
H1C H 0.568495 0.705352 0.498482 0.046 Uiso 1 1 calc R U . . .
O2 O 0.49214(18) 0.78690(18) 0.41236(8) 0.0214(4) Uani 1 1 d . . . . .
N2 N 0.1262(2) 0.77430(19) 0.27197(9) 0.0129(4) Uani 1 1 d . . . . .
C2 C 0.3580(3) 0.8915(2) 0.42934(12) 0.0167(5) Uani 1 1 d . . . . .
O3 O 0.37302(17) 0.74225(16) 0.21653(8) 0.0150(3) Uani 1 1 d . . . . .
N3 N 0.3001(2) 1.0196(2) 0.21093(9) 0.0136(4) Uani 1 1 d . . . . .
C3 C 0.3159(3) 0.9513(3) 0.48930(12) 0.0216(6) Uani 1 1 d . . . . .
H3 H 0.382818 0.921818 0.522316 0.026 Uiso 1 1 calc R U . . .
O4 O 0.49441(19) 0.50380(18) 0.16134(9) 0.0228(4) Uani 1 1 d . . . . .
C4 C 0.1746(3) 1.0558(3) 0.50192(12) 0.0216(6) Uani 1 1 d . . . . .
H4 H 0.144981 1.095134 0.543803 0.026 Uiso 1 1 calc R U . . .
O5 O 0.13146(17) 0.93561(16) 0.16349(7) 0.0131(3) Uani 1 1 d . . . . .
C5 C 0.0796(3) 1.1009(3) 0.45378(12) 0.0185(5) Uani 1 1 d . . . . .
H5 H -0.015658 1.172466 0.462326 0.022 Uiso 1 1 calc R U . . .
O6 O 0.16054(18) 0.96222(18) 0.03570(8) 0.0185(4) Uani 1 1 d . . . . .
C6 C 0.1215(3) 1.0423(2) 0.39148(11) 0.0145(5) Uani 1 1 d . . . . .
C7 C 0.2605(3) 0.9336(2) 0.37850(11) 0.0136(5) Uani 1 1 d . . . . .
C8 C 0.0161(2) 1.0955(2) 0.34292(11) 0.0142(5) Uani 1 1 d . . . . .
H8 H -0.075152 1.169315 0.355644 0.017 Uiso 1 1 calc R U . . .
C9 C -0.1002(2) 1.1246(2) 0.24634(12) 0.0152(5) Uani 1 1 d . . . . .
H9A H -0.070831 1.126334 0.199078 0.018 Uiso 1 1 calc R U . . .
H9B H -0.155621 1.222062 0.259797 0.018 Uiso 1 1 calc R U . . .
C10 C -0.1964(2) 1.0517(2) 0.25754(11) 0.0140(5) Uani 1 1 d . . . . .
C11 C -0.2819(3) 1.0650(3) 0.31608(12) 0.0201(5) Uani 1 1 d . . . . .
H11 H -0.282011 1.122425 0.348910 0.024 Uiso 1 1 calc R U . . .
C12 C -0.3665(3) 0.9951(3) 0.32639(13) 0.0230(6) Uani 1 1 d . . . . .
H12 H -0.425235 1.005838 0.366084 0.028 Uiso 1 1 calc R U . . .
C13 C -0.3665(3) 0.9093(3) 0.27942(13) 0.0228(6) Uani 1 1 d . . . . .
H13 H -0.423059 0.859848 0.287204 0.027 Uiso 1 1 calc R U . . .
C14 C -0.2834(3) 0.8968(3) 0.22117(13) 0.0215(5) Uani 1 1 d . . . . .
H14 H -0.283537 0.839287 0.188440 0.026 Uiso 1 1 calc R U . . .
C15 C -0.1998(3) 0.9681(3) 0.21046(12) 0.0176(5) Uani 1 1 d . . . . .
H15 H -0.143754 0.959368 0.170081 0.021 Uiso 1 1 calc R U . . .
C16 C 0.5601(3) 0.3710(3) 0.13297(15) 0.0341(7) Uani 1 1 d . . . . .
H16A H 0.518573 0.377573 0.091255 0.051 Uiso 1 1 calc R U . . .
H16B H 0.542214 0.303892 0.162772 0.051 Uiso 1 1 calc R U . . .
H16C H 0.664587 0.340203 0.125343 0.051 Uiso 1 1 calc R U . . .
C17 C 0.5064(3) 0.6110(3) 0.12593(12) 0.0169(5) Uani 1 1 d . . . . .
C18 C 0.5754(3) 0.6028(3) 0.06429(12) 0.0224(6) Uani 1 1 d . . . . .
H18 H 0.614932 0.518131 0.041985 0.027 Uiso 1 1 calc R U . . .
C19 C 0.5872(3) 0.7196(3) 0.03451(12) 0.0246(6) Uani 1 1 d . . . . .
H19 H 0.635654 0.713385 -0.007727 0.029 Uiso 1 1 calc R U . . .
C20 C 0.5291(3) 0.8424(3) 0.06620(12) 0.0216(5) Uani 1 1 d . . . . .
H20 H 0.540753 0.919952 0.046533 0.026 Uiso 1 1 calc R U . . .
C21 C 0.4522(2) 0.8545(3) 0.12791(12) 0.0163(5) Uani 1 1 d . . . . .
C22 C 0.4392(2) 0.7398(3) 0.15841(11) 0.0150(5) Uani 1 1 d . . . . .
C23 C 0.3938(3) 0.9841(3) 0.16124(12) 0.0166(5) Uani 1 1 d . . . . .
H23 H 0.427873 1.049769 0.144851 0.020 Uiso 1 1 calc R U . . .
C24 C 0.2616(3) 1.1555(2) 0.23807(12) 0.0152(5) Uani 1 1 d . . . . .
H24A H 0.341570 1.181192 0.226370 0.018 Uiso 1 1 calc R U . . .
H24B H 0.250364 1.147244 0.286406 0.018 Uiso 1 1 calc R U . . .
C25 C 0.1226(3) 1.2702(2) 0.21327(12) 0.0153(5) Uani 1 1 d . . . . .
C26 C 0.0845(3) 1.2750(3) 0.14985(12) 0.0197(5) Uani 1 1 d . . . . .
H26 H 0.144430 1.203650 0.120788 0.024 Uiso 1 1 calc R U . . .
C27 C -0.0422(3) 1.3849(3) 0.12912(14) 0.0267(6) Uani 1 1 d . . . . .
H27 H -0.067669 1.388537 0.085596 0.032 Uiso 1 1 calc R U . . .
C28 C -0.1315(3) 1.4888(3) 0.17096(15) 0.0278(6) Uani 1 1 d . . . . .
H28 H -0.217793 1.563104 0.156304 0.033 Uiso 1 1 calc R U . . .
C29 C -0.0944(3) 1.4840(3) 0.23425(14) 0.0252(6) Uani 1 1 d . . . . .
H29 H -0.155490 1.554656 0.263391 0.030 Uiso 1 1 calc R U . . .
C30 C 0.0325(3) 1.3753(2) 0.25509(12) 0.0182(5) Uani 1 1 d . . . . .
H30 H 0.058020 1.372744 0.298497 0.022 Uiso 1 1 calc R U . . .
C31 C 0.1996(3) 0.9669(3) -0.03252(12) 0.0228(6) Uani 1 1 d . . . . .
H31A H 0.296471 0.891594 -0.042327 0.034 Uiso 1 1 calc R U . . .
H31B H 0.199671 1.056633 -0.044947 0.034 Uiso 1 1 calc R U . . .
H31C H 0.129587 0.955830 -0.057260 0.034 Uiso 1 1 calc R U . . .
C32 C 0.1545(2) 0.8424(2) 0.06081(11) 0.0147(5) Uani 1 1 d . . . . .
C33 C 0.1582(3) 0.7393(3) 0.02394(12) 0.0195(5) Uani 1 1 d . . . . .
H33 H 0.167039 0.747674 -0.022472 0.023 Uiso 1 1 calc R U . . .
C34 C 0.1490(3) 0.6219(3) 0.05440(12) 0.0204(5) Uani 1 1 d . . . . .
H34 H 0.152599 0.550791 0.028687 0.025 Uiso 1 1 calc R U . . .
C35 C 0.1350(3) 0.6103(3) 0.12127(12) 0.0180(5) Uani 1 1 d . . . . .
H35 H 0.127488 0.531412 0.141838 0.022 Uiso 1 1 calc R U . . .
C36 C 0.1315(2) 0.7142(2) 0.15971(11) 0.0147(5) Uani 1 1 d . . . . .
C37 C 0.1405(2) 0.8326(2) 0.13030(11) 0.0123(5) Uani 1 1 d . . . . .
C38 C 0.1101(2) 0.7015(2) 0.22979(12) 0.0156(5) Uani 1 1 d . . . . .
H38 H 0.081116 0.632410 0.246453 0.019 Uiso 1 1 calc R U . . .
C39 C 0.0843(3) 0.7516(2) 0.34136(11) 0.0173(5) Uani 1 1 d . . . . .
H39A H -0.022656 0.797040 0.347991 0.021 Uiso 1 1 calc R U . . .
H39B H 0.121327 0.797086 0.369522 0.021 Uiso 1 1 calc R U . . .
C40 C 0.1405(3) 0.5999(3) 0.36287(11) 0.0167(5) Uani 1 1 d . . . . .
C41 C 0.2796(3) 0.5032(3) 0.34358(15) 0.0297(7) Uani 1 1 d . . . . .
H41 H 0.341198 0.532755 0.316545 0.036 Uiso 1 1 calc R U . . .
C42 C 0.3299(3) 0.3646(3) 0.36315(16) 0.0331(7) Uani 1 1 d . . . . .
H42 H 0.425262 0.299590 0.349250 0.040 Uiso 1 1 calc R U . . .
C43 C 0.2420(3) 0.3203(3) 0.40281(13) 0.0288(7) Uani 1 1 d . . . . .
H43 H 0.276016 0.224935 0.415998 0.035 Uiso 1 1 calc R U . . .
C44 C 0.1051(4) 0.4157(3) 0.42296(13) 0.0338(7) Uani 1 1 d . . . . .
H44 H 0.044562 0.386245 0.450870 0.041 Uiso 1 1 calc R U . . .
C45 C 0.0540(3) 0.5551(3) 0.40289(13) 0.0275(6) Uani 1 1 d . . . . .
H45 H -0.041359 0.619852 0.416919 0.033 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 O5 1.8816(15) . ?
Co1 O3 1.8983(16) . ?
Co1 O1 1.9110(16) . ?
Co1 N2 1.9364(19) . ?
Co1 N1 1.9532(19) . ?
Co1 N3 1.9602(19) . ?
O1 C7 1.305(3) . ?
N1 C8 1.295(3) . ?
N1 C9 1.493(3) . ?
C1 O2 1.429(3) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
O2 C2 1.372(3) . ?
N2 C38 1.283(3) . ?
N2 C39 1.483(3) . ?
C2 C3 1.374(4) . ?
C2 C7 1.428(3) . ?
O3 C22 1.313(3) . ?
N3 C23 1.290(3) . ?
N3 C24 1.473(3) . ?
C3 C4 1.403(4) . ?
C3 H3 0.9500 . ?
O4 C17 1.362(3) . ?
O4 C16 1.423(3) . ?
C4 C5 1.368(4) . ?
C4 H4 0.9500 . ?
O5 C37 1.311(3) . ?
C5 C6 1.413(3) . ?
C5 H5 0.9500 . ?
O6 C32 1.377(3) . ?
O6 C31 1.424(3) . ?
C6 C7 1.405(3) . ?
C6 C8 1.442(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.515(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C15 1.386(3) . ?
C10 C11 1.399(3) . ?
C11 C12 1.384(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(3) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.381(4) . ?
C17 C22 1.429(3) . ?
C18 C19 1.405(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.371(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.412(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.396(3) . ?
C21 C23 1.447(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.519(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.389(3) . ?
C25 C30 1.391(3) . ?
C26 C27 1.393(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.382(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.383(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.389(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.378(3) . ?
C32 C37 1.421(3) . ?
C33 C34 1.404(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.369(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.406(3) . ?
C35 H35 0.9500 . ?
C36 C37 1.405(3) . ?
C36 C38 1.440(3) . ?
C38 H38 0.9500 . ?
C39 C40 1.512(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 C45 1.376(3) . ?
C40 C41 1.386(4) . ?
C41 C42 1.382(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.380(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.372(4) . ?
C43 H43 0.9500 . ?
C44 C45 1.391(4) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Co1 O3 91.14(7) . . ?
O5 Co1 O1 172.59(7) . . ?
O3 Co1 O1 84.07(7) . . ?
O5 Co1 N2 91.19(7) . . ?
O3 Co1 N2 84.58(7) . . ?
O1 Co1 N2 93.98(8) . . ?
O5 Co1 N1 92.08(7) . . ?
O3 Co1 N1 173.44(7) . . ?
O1 Co1 N1 93.25(7) . . ?
N2 Co1 N1 89.64(8) . . ?
O5 Co1 N3 84.92(7) . . ?
O3 Co1 N3 89.99(8) . . ?
O1 Co1 N3 89.42(7) . . ?
N2 Co1 N3 173.26(8) . . ?
N1 Co1 N3 95.98(8) . . ?
C7 O1 Co1 127.91(15) . . ?
C8 N1 C9 114.72(19) . . ?
C8 N1 Co1 124.57(16) . . ?
C9 N1 Co1 120.58(15) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 O2 C1 117.7(2) . . ?
C38 N2 C39 116.78(19) . . ?
C38 N2 Co1 121.29(16) . . ?
C39 N2 Co1 121.90(15) . . ?
O2 C2 C3 125.0(2) . . ?
O2 C2 C7 113.6(2) . . ?
C3 C2 C7 121.4(2) . . ?
C22 O3 Co1 121.89(15) . . ?
C23 N3 C24 116.6(2) . . ?
C23 N3 Co1 121.74(17) . . ?
C24 N3 Co1 121.60(15) . . ?
C2 C3 C4 120.3(2) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C17 O4 C16 117.5(2) . . ?
C5 C4 C3 119.8(2) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C37 O5 Co1 120.89(14) . . ?
C4 C5 C6 120.8(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C32 O6 C31 116.56(19) . . ?
C7 C6 C5 120.4(2) . . ?
C7 C6 C8 121.8(2) . . ?
C5 C6 C8 117.8(2) . . ?
O1 C7 C6 125.2(2) . . ?
O1 C7 C2 117.6(2) . . ?
C6 C7 C2 117.2(2) . . ?
N1 C8 C6 127.3(2) . . ?
N1 C8 H8 116.4 . . ?
C6 C8 H8 116.4 . . ?
N1 C9 C10 111.84(18) . . ?
N1 C9 H9A 109.2 . . ?
C10 C9 H9A 109.2 . . ?
N1 C9 H9B 109.2 . . ?
C10 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C15 C10 C11 118.3(2) . . ?
C15 C10 C9 120.8(2) . . ?
C11 C10 C9 120.9(2) . . ?
C12 C11 C10 120.3(2) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 120.7(2) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 H12 119.6 . . ?
C14 C13 C12 119.3(2) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 120.1(2) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 C14 121.3(2) . . ?
C10 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 C18 125.7(2) . . ?
O4 C17 C22 113.8(2) . . ?
C18 C17 C22 120.5(2) . . ?
C17 C18 C19 120.1(2) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C20 C19 C18 120.2(2) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 120.4(2) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C22 C21 C20 120.3(2) . . ?
C22 C21 C23 119.9(2) . . ?
C20 C21 C23 119.7(2) . . ?
O3 C22 C21 123.6(2) . . ?
O3 C22 C17 118.0(2) . . ?
C21 C22 C17 118.4(2) . . ?
N3 C23 C21 126.6(2) . . ?
N3 C23 H23 116.7 . . ?
C21 C23 H23 116.7 . . ?
N3 C24 C25 112.80(19) . . ?
N3 C24 H24A 109.0 . . ?
C25 C24 H24A 109.0 . . ?
N3 C24 H24B 109.0 . . ?
C25 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C26 C25 C30 119.1(2) . . ?
C26 C25 C24 122.0(2) . . ?
C30 C25 C24 118.8(2) . . ?
C25 C26 C27 119.6(2) . . ?
C25 C26 H26 120.2 . . ?
C27 C26 H26 120.2 . . ?
C28 C27 C26 121.0(2) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 119.6(2) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C28 C29 C30 119.8(3) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C29 C30 C25 120.9(2) . . ?
C29 C30 H30 119.5 . . ?
C25 C30 H30 119.5 . . ?
O6 C31 H31A 109.5 . . ?
O6 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O6 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O6 C32 C33 125.0(2) . . ?
O6 C32 C37 114.2(2) . . ?
C33 C32 C37 120.8(2) . . ?
C32 C33 C34 120.5(2) . . ?
C32 C33 H33 119.7 . . ?
C34 C33 H33 119.7 . . ?
C35 C34 C33 119.8(2) . . ?
C35 C34 H34 120.1 . . ?
C33 C34 H34 120.1 . . ?
C34 C35 C36 120.4(2) . . ?
C34 C35 H35 119.8 . . ?
C36 C35 H35 119.8 . . ?
C37 C36 C35 120.7(2) . . ?
C37 C36 C38 120.3(2) . . ?
C35 C36 C38 118.9(2) . . ?
O5 C37 C36 123.4(2) . . ?
O5 C37 C32 118.8(2) . . ?
C36 C37 C32 117.7(2) . . ?
N2 C38 C36 126.5(2) . . ?
N2 C38 H38 116.8 . . ?
C36 C38 H38 116.8 . . ?
N2 C39 C40 113.72(19) . . ?
N2 C39 H39A 108.8 . . ?
C40 C39 H39A 108.8 . . ?
N2 C39 H39B 108.8 . . ?
C40 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C45 C40 C41 118.5(2) . . ?
C45 C40 C39 120.2(2) . . ?
C41 C40 C39 121.3(2) . . ?
C42 C41 C40 120.9(3) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C43 C42 C41 120.2(3) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C44 C43 C42 119.2(3) . . ?
C44 C43 H43 120.4 . . ?
C42 C43 H43 120.4 . . ?
C43 C44 C45 120.6(3) . . ?
C43 C44 H44 119.7 . . ?
C45 C44 H44 119.7 . . ?
C40 C45 C44 120.5(3) . . ?
C40 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?

_refine_diff_density_max         0.451
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.059



# SQUEEZE RESULTS (Version = 241018)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 186 55 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_chemical_properties_physical    Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_msp11a
_database_code_depnum_ccdc_archive 'CCDC 1874845'
_audit_update_record             
;
2018-12-12 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Ni4]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H70 N4 O12 Ni4 (N2 O7 H2)'
_chemical_formula_sum            'C60 H72 N6 Ni4 O19'
_chemical_formula_weight         1416.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.0156(2)
_cell_length_b                   12.5137(2)
_cell_length_c                   14.5497(2)
_cell_angle_alpha                93.1290(10)
_cell_angle_beta                 105.662(2)
_cell_angle_gamma                105.280(2)
_cell_volume                     1510.62(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    14425
_cell_measurement_theta_min      4.5360
_cell_measurement_theta_max      70.3320

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_F_000             738
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_absorpt_coefficient_mu    2.072
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
crysalispro 1.171.39.9g (rigaku oxford diffraction, 2015)
empirical absorption correction using spherical harmonics,
 implemented in scale3 abspack scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xtalab afc11 (rcd3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28299
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.696
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5493
_reflns_number_gt                5011
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_computing_data_collection       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_cell_refinement       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_data_reduction        'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_structure_solution    
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0606P)²+1.1091P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5493
_refine_ls_number_parameters     459
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.1036
_refine_ls_wR_factor_gt          0.1010
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.112
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.55410(4) 0.57048(3) 0.69037(2) 0.02222(12) Uani 1 1 d . . . . .
O1 O 0.39588(19) 0.51080(12) 0.55082(10) 0.0246(3) Uani 1 1 d . . . . .
H1 H 0.279886 0.498165 0.538856 0.030 Uiso 1 1 calc R U . . .
H6B H 0.381(3) 0.488(2) 0.799(2) 0.040(8) Uiso 1 1 d . . . . .
H2H H 0.700(3) 0.706(2) 0.3924(19) 0.027(7) Uiso 1 1 d . . . . .
H6A H 0.287(4) 0.512(3) 0.715(3) 0.065(10) Uiso 1 1 d . . . . .
N1 N 0.7402(2) 0.60647(14) 0.82216(12) 0.0239(4) Uani 1 1 d . . . . .
H1H H 0.701618 0.640636 0.869793 0.029 Uiso 1 1 calc R U . . .
C1 C 0.7338(3) 0.2324(2) 0.48335(17) 0.0350(5) Uani 1 1 d . . . . .
H1A H 0.719894 0.160357 0.505125 0.053 Uiso 1 1 calc R U . . .
H1C H 0.843302 0.262380 0.483170 0.053 Uiso 1 1 calc R U . . .
H1B H 0.663144 0.224951 0.419302 0.053 Uiso 1 1 calc R U . . .
Ni2 Ni 0.48256(4) 0.38180(3) 0.52288(2) 0.02066(11) Uani 1 1 d . . . . .
O2 O 0.61726(17) 0.43590(12) 0.65800(10) 0.0240(3) Uani 1 1 d . . . . .
N2 N 0.6701(2) 0.74618(15) 0.42626(12) 0.0228(4) Uani 1 1 d . . . . .
C2 C 0.7996(3) 0.33770(17) 0.63979(15) 0.0250(4) Uani 1 1 d . . . . .
O3 O 0.69681(18) 0.30582(12) 0.54636(10) 0.0263(3) Uani 1 1 d . . . . .
N3 N 0.0484(5) 0.5449(3) 0.5782(3) 0.0356(9) Uani 0.5 1 d . . P A -1
C3 C 0.9352(3) 0.30373(18) 0.67705(16) 0.0283(5) Uani 1 1 d . . . . .
H3 H 0.966584 0.257551 0.638512 0.034 Uiso 1 1 calc R U . . .
O4 O 0.66158(18) 0.67691(11) 0.61349(10) 0.0250(3) Uani 1 1 d . . . . .
N4 N 0.495(4) 0.508(3) 1.0090(18) 0.031(2) Uani 0.5 1 d . . P B -1
C4 C 1.0242(3) 0.33987(18) 0.77345(17) 0.0306(5) Uani 1 1 d . . . . .
H4 H 1.116544 0.318456 0.799197 0.037 Uiso 1 1 calc R U . . .
O5 O 0.53334(19) 0.74267(12) 0.74056(10) 0.0280(3) Uani 1 1 d . . . . .
C5 C 0.9761(3) 0.40735(18) 0.83095(16) 0.0290(5) Uani 1 1 d . . . . .
H5 H 1.036181 0.430542 0.895162 0.035 Uiso 1 1 calc R U . . .
O6 O 0.3737(2) 0.48652(14) 0.74220(12) 0.0303(4) Uani 1 1 d . . . . .
C6 C 0.8384(3) 0.44111(17) 0.79388(15) 0.0255(4) Uani 1 1 d . . . . .
O7 O 0.1302(17) 0.5735(12) 0.6648(11) 0.076(4) Uani 0.5 1 d . . P A -1
C7 C 0.7511(2) 0.40786(16) 0.69695(15) 0.0233(4) Uani 1 1 d . . . . .
O8 O 0.0644(4) 0.4656(3) 0.5280(3) 0.0375(8) Uani 0.5 1 d . . P A -1
C8 C 0.7741(3) 0.50332(18) 0.85812(15) 0.0267(5) Uani 1 1 d . . . . .
H8B H 0.675691 0.453760 0.864432 0.032 Uiso 1 1 calc R U . . .
H8A H 0.851672 0.523798 0.921713 0.032 Uiso 1 1 calc R U . . .
O9 O -0.0607(4) 0.5877(3) 0.5430(3) 0.0520(10) Uani 0.5 1 d . . P A -1
C9 C 0.8891(3) 0.69028(17) 0.81719(15) 0.0259(4) Uani 1 1 d . . . . .
H9B H 0.860004 0.754201 0.791289 0.031 Uiso 1 1 calc R U . . .
H9A H 0.932646 0.657467 0.772414 0.031 Uiso 1 1 calc R U . . .
O10 O 0.4779(5) 0.5585(3) 0.9297(3) 0.0451(9) Uani 0.5 1 d . . P B -1
C10 C 1.0195(3) 0.73111(17) 0.91223(15) 0.0254(4) Uani 1 1 d . . . . .
O11 O 0.5973(5) 0.5701(3) 1.0799(2) 0.0501(10) Uani 0.5 1 d . . P B -1
C11 C 1.0009(3) 0.80368(19) 0.98159(16) 0.0296(5) Uani 1 1 d . . . . .
H11 H 0.906312 0.824296 0.970059 0.035 Uiso 1 1 calc R U . . .
O12 O 0.4233(5) 0.4131(3) 1.0037(3) 0.0451(9) Uani 0.5 1 d . . P B -1
C12 C 1.1224(3) 0.84554(19) 1.06788(16) 0.0331(5) Uani 1 1 d . . . . .
H12 H 1.108753 0.893494 1.113995 0.040 Uiso 1 1 calc R U . . .
O13 O -0.1259(10) 0.4231(8) 0.3340(7) 0.030(2) Uani 0.5 1 d G . P C -1
H13B H -0.157703 0.385072 0.278498 0.045 Uiso 0.5 1 d G U P C -1
H13A H -0.056944 0.394647 0.367468 0.045 Uiso 0.5 1 d G U P C -1
C13 C 1.2637(3) 0.81559(19) 1.08489(16) 0.0334(5) Uani 1 1 d . . . . .
H13 H 1.345408 0.843942 1.142335 0.040 Uiso 1 1 calc R U . . .
C14 C 1.2836(3) 0.74358(19) 1.01665(16) 0.0316(5) Uani 1 1 d . . . . .
H14 H 1.378599 0.723586 1.028165 0.038 Uiso 1 1 calc R U . . .
C15 C 1.1612(3) 0.70115(18) 0.93084(16) 0.0289(5) Uani 1 1 d . . . . .
H15 H 1.174603 0.652147 0.885421 0.035 Uiso 1 1 calc R U . . .
C16 C 0.4718(3) 0.7748(2) 0.81513(19) 0.0395(6) Uani 1 1 d . . . . .
H16B H 0.424985 0.709618 0.840872 0.059 Uiso 1 1 calc R U . . .
H16C H 0.391227 0.811164 0.789179 0.059 Uiso 1 1 calc R U . . .
H16A H 0.557851 0.825337 0.865450 0.059 Uiso 1 1 calc R U . . .
C17 C 0.6207(3) 0.82696(17) 0.70154(14) 0.0243(4) Uani 1 1 d . . . . .
C18 C 0.6434(3) 0.94030(18) 0.72405(16) 0.0297(5) Uani 1 1 d . . . . .
H18 H 0.601608 0.965786 0.769893 0.036 Uiso 1 1 calc R U . . .
C19 C 0.7301(3) 1.01534(18) 0.67677(16) 0.0312(5) Uani 1 1 d . . . . .
H19 H 0.748494 1.091761 0.692087 0.037 Uiso 1 1 calc R U . . .
C20 C 0.7891(3) 0.97670(18) 0.60701(16) 0.0285(5) Uani 1 1 d . . . . .
H20 H 0.845957 1.027606 0.575526 0.034 Uiso 1 1 calc R U . . .
C21 C 0.7644(2) 0.86253(17) 0.58330(14) 0.0241(4) Uani 1 1 d . . . . .
C22 C 0.6822(3) 0.78704(16) 0.63258(14) 0.0243(4) Uani 1 1 d . . . . .
C23 C 0.8159(3) 0.81371(17) 0.50409(14) 0.0246(4) Uani 1 1 d . . . . .
H23A H 0.878214 0.873376 0.478087 0.030 Uiso 1 1 calc R U . . .
H23B H 0.882968 0.766685 0.529733 0.030 Uiso 1 1 calc R U . . .
C24 C 0.5868(3) 0.81846(17) 0.36689(15) 0.0246(4) Uani 1 1 d . . . . .
H24A H 0.569445 0.873041 0.409696 0.029 Uiso 1 1 calc R U . . .
H24B H 0.481929 0.772324 0.327257 0.029 Uiso 1 1 calc R U . . .
C25 C 0.6759(3) 0.87962(18) 0.30232(15) 0.0251(4) Uani 1 1 d . . . . .
C26 C 0.7525(3) 0.99416(19) 0.32236(18) 0.0334(5) Uani 1 1 d . . . . .
H26 H 0.752261 1.034216 0.378051 0.040 Uiso 1 1 calc R U . . .
C27 C 0.8295(3) 1.0494(2) 0.2600(2) 0.0430(6) Uani 1 1 d . . . . .
H27 H 0.880930 1.125786 0.274249 0.052 Uiso 1 1 calc R U . . .
C28 C 0.8293(3) 0.9908(3) 0.1772(2) 0.0477(7) Uani 1 1 d . . . . .
H28 H 0.879646 1.027736 0.135173 0.057 Uiso 1 1 calc R U . . .
C29 C 0.7541(4) 0.8766(3) 0.15628(19) 0.0455(7) Uani 1 1 d . . . . .
H29 H 0.754472 0.836998 0.100400 0.055 Uiso 1 1 calc R U . . .
C30 C 0.6784(3) 0.8217(2) 0.21888(17) 0.0329(5) Uani 1 1 d . . . . .
H30 H 0.628758 0.745015 0.204776 0.039 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2 1.9865(15) . ?
Ni1 O4 2.0079(15) . ?
Ni1 O6 2.0414(17) . ?
Ni1 O1 2.1033(14) . ?
Ni1 N1 2.1131(17) . ?
Ni1 O5 2.3078(15) . ?
O1 Ni2 2.0364(15) . ?
O1 Ni2 2.0428(15) 2_666 ?
O1 H1 0.9800 . ?
N1 C9 1.492(3) . ?
N1 C8 1.493(3) . ?
N1 H1H 0.9800 . ?
C1 O3 1.425(3) . ?
C1 H1A 0.9600 . ?
C1 H1C 0.9600 . ?
C1 H1B 0.9600 . ?
Ni2 O2 1.9825(14) . ?
Ni2 O4 2.0274(14) 2_666 ?
Ni2 N2 2.1271(18) 2_666 ?
Ni2 O3 2.3235(15) . ?
O2 C7 1.333(3) . ?
N2 C24 1.491(3) . ?
N2 C23 1.493(3) . ?
N2 H2H 0.83(3) . ?
C2 C3 1.382(3) . ?
C2 O3 1.390(2) . ?
C2 C7 1.404(3) . ?
N3 O9 1.247(5) . ?
N3 O7 1.253(15) . ?
N3 O8 1.262(6) . ?
C3 C4 1.396(3) . ?
C3 H3 0.9300 . ?
O4 C22 1.344(2) . ?
N4 O12 1.18(4) . ?
N4 O11 1.24(3) . ?
N4 O10 1.34(3) . ?
C4 C5 1.384(3) . ?
C4 H4 0.9300 . ?
O5 C17 1.387(3) . ?
O5 C16 1.429(3) . ?
C5 C6 1.396(3) . ?
C5 H5 0.9300 . ?
O6 H6B 0.81(3) . ?
O6 H6A 0.92(4) . ?
C6 C7 1.395(3) . ?
C6 C8 1.505(3) . ?
C8 H8B 0.9700 . ?
C8 H8A 0.9700 . ?
C9 C10 1.511(3) . ?
C9 H9B 0.9700 . ?
C9 H9A 0.9700 . ?
C10 C15 1.387(3) . ?
C10 C11 1.394(3) . ?
C11 C12 1.391(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.384(4) . ?
C12 H12 0.9300 . ?
O13 H13B 0.8500 . ?
O13 H13A 0.8500 . ?
C13 C14 1.383(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.390(3) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 H16A 0.9600 . ?
C17 C18 1.386(3) . ?
C17 C22 1.399(3) . ?
C18 C19 1.393(3) . ?
C18 H18 0.9300 . ?
C19 C20 1.386(3) . ?
C19 H19 0.9300 . ?
C20 C21 1.395(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.395(3) . ?
C21 C23 1.509(3) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.508(3) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C30 1.389(3) . ?
C25 C26 1.393(3) . ?
C26 C27 1.393(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.374(4) . ?
C27 H27 0.9300 . ?
C28 C29 1.387(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.387(3) . ?
C29 H29 0.9300 . ?
C30 H30 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
O2 Ni1 O4 100.22(6) . . ?
O2 Ni1 O6 95.05(7) . . ?
O4 Ni1 O6 157.52(7) . . ?
O2 Ni1 O1 78.88(6) . . ?
O4 Ni1 O1 79.25(6) . . ?
O6 Ni1 O1 87.70(7) . . ?
O2 Ni1 N1 88.94(6) . . ?
O4 Ni1 N1 99.91(6) . . ?
O6 Ni1 N1 96.75(7) . . ?
O1 Ni1 N1 167.38(7) . . ?
O2 Ni1 O5 168.95(6) . . ?
O4 Ni1 O5 74.76(6) . . ?
O6 Ni1 O5 92.73(6) . . ?
O1 Ni1 O5 109.30(6) . . ?
N1 Ni1 O5 82.36(6) . . ?
Ni2 O1 Ni2 95.60(6) . 2_666 ?
Ni2 O1 Ni1 97.24(6) . . ?
Ni2 O1 Ni1 98.35(6) 2_666 . ?
Ni2 O1 H1 120.1 . . ?
Ni2 O1 H1 120.1 2_666 . ?
Ni1 O1 H1 120.1 . . ?
C9 N1 C8 111.81(17) . . ?
C9 N1 Ni1 112.23(12) . . ?
C8 N1 Ni1 112.29(12) . . ?
C9 N1 H1H 106.7 . . ?
C8 N1 H1H 106.7 . . ?
Ni1 N1 H1H 106.7 . . ?
O3 C1 H1A 109.5 . . ?
O3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
O3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1C C1 H1B 109.5 . . ?
O2 Ni2 O4 177.91(6) . 2_666 ?
O2 Ni2 O1 80.60(6) . . ?
O4 Ni2 O1 99.21(6) 2_666 . ?
O2 Ni2 O1 101.79(6) . 2_666 ?
O4 Ni2 O1 80.24(6) 2_666 2_666 ?
O1 Ni2 O1 84.40(6) . 2_666 ?
O2 Ni2 N2 88.78(6) . 2_666 ?
O4 Ni2 N2 89.19(6) 2_666 2_666 ?
O1 Ni2 N2 98.97(7) . 2_666 ?
O1 Ni2 N2 169.32(6) 2_666 2_666 ?
O2 Ni2 O3 73.79(6) . . ?
O4 Ni2 O3 106.98(6) 2_666 . ?
O1 Ni2 O3 149.38(6) . . ?
O1 Ni2 O3 84.67(6) 2_666 . ?
N2 Ni2 O3 97.02(6) 2_666 . ?
C7 O2 Ni2 122.75(13) . . ?
C7 O2 Ni1 130.20(12) . . ?
Ni2 O2 Ni1 103.01(6) . . ?
C24 N2 C23 111.81(16) . . ?
C24 N2 Ni2 114.70(13) . 2_666 ?
C23 N2 Ni2 112.98(13) . 2_666 ?
C24 N2 H2H 110.6(18) . . ?
C23 N2 H2H 107.5(18) . . ?
Ni2 N2 H2H 98.3(18) 2_666 . ?
C3 C2 O3 125.3(2) . . ?
C3 C2 C7 121.2(2) . . ?
O3 C2 C7 113.46(18) . . ?
C2 O3 C1 117.66(17) . . ?
C2 O3 Ni2 111.29(12) . . ?
C1 O3 Ni2 131.01(13) . . ?
O9 N3 O7 120.0(8) . . ?
O9 N3 O8 118.7(4) . . ?
O7 N3 O8 120.9(8) . . ?
C2 C3 C4 118.9(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C22 O4 Ni1 119.66(13) . . ?
C22 O4 Ni2 110.18(12) . 2_666 ?
Ni1 O4 Ni2 102.07(6) . 2_666 ?
O12 N4 O11 129(3) . . ?
O12 N4 O10 120(2) . . ?
O11 N4 O10 112(3) . . ?
C5 C4 C3 120.4(2) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C17 O5 C16 117.77(17) . . ?
C17 O5 Ni1 111.17(12) . . ?
C16 O5 Ni1 129.98(13) . . ?
C4 C5 C6 120.9(2) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
Ni1 O6 H6B 124(2) . . ?
Ni1 O6 H6A 106(2) . . ?
H6B O6 H6A 106(3) . . ?
C7 C6 C5 119.1(2) . . ?
C7 C6 C8 119.35(19) . . ?
C5 C6 C8 121.34(19) . . ?
O2 C7 C6 121.72(19) . . ?
O2 C7 C2 118.70(18) . . ?
C6 C7 C2 119.48(19) . . ?
N1 C8 C6 113.74(17) . . ?
N1 C8 H8B 108.8 . . ?
C6 C8 H8B 108.8 . . ?
N1 C8 H8A 108.8 . . ?
C6 C8 H8A 108.8 . . ?
H8B C8 H8A 107.7 . . ?
N1 C9 C10 115.01(17) . . ?
N1 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
N1 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
H9B C9 H9A 107.5 . . ?
C15 C10 C11 118.8(2) . . ?
C15 C10 C9 121.2(2) . . ?
C11 C10 C9 119.9(2) . . ?
C12 C11 C10 120.6(2) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
H13B O13 H13A 104.5 . . ?
C14 C13 C12 120.2(2) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 119.9(2) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C10 C15 C14 120.7(2) . . ?
C10 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
O5 C16 H16B 109.5 . . ?
O5 C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O5 C16 H16A 109.5 . . ?
H16B C16 H16A 109.5 . . ?
H16C C16 H16A 109.5 . . ?
C18 C17 O5 125.2(2) . . ?
C18 C17 C22 121.4(2) . . ?
O5 C17 C22 113.38(18) . . ?
C17 C18 C19 118.8(2) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
C20 C19 C18 120.3(2) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C21 121.0(2) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C20 C21 C22 119.0(2) . . ?
C20 C21 C23 124.03(19) . . ?
C22 C21 C23 116.89(18) . . ?
O4 C22 C21 120.27(19) . . ?
O4 C22 C17 120.32(18) . . ?
C21 C22 C17 119.41(19) . . ?
N2 C23 C21 109.31(17) . . ?
N2 C23 H23A 109.8 . . ?
C21 C23 H23A 109.8 . . ?
N2 C23 H23B 109.8 . . ?
C21 C23 H23B 109.8 . . ?
H23A C23 H23B 108.3 . . ?
N2 C24 C25 114.69(18) . . ?
N2 C24 H24A 108.6 . . ?
C25 C24 H24A 108.6 . . ?
N2 C24 H24B 108.6 . . ?
C25 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
C30 C25 C26 118.5(2) . . ?
C30 C25 C24 119.6(2) . . ?
C26 C25 C24 121.8(2) . . ?
C27 C26 C25 120.8(2) . . ?
C27 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C28 C27 C26 119.9(2) . . ?
C28 C27 H27 120.1 . . ?
C26 C27 H27 120.1 . . ?
C27 C28 C29 120.2(2) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C28 C29 C30 119.8(3) . . ?
C28 C29 H29 120.1 . . ?
C30 C29 H29 120.1 . . ?
C29 C30 C25 120.8(2) . . ?
C29 C30 H30 119.6 . . ?
C25 C30 H30 119.6 . . ?

_refine_diff_density_max         0.788
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.064


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

data_msp3s
_database_code_depnum_ccdc_archive 'CCDC 1874841'
_audit_update_record             
;
2018-12-18 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H44 N4 O13 Ni2, (C3 H16 O5)'
_chemical_formula_sum            'C48 H60 N4 Ni2 O18'
_chemical_formula_weight         1098.39

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

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

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

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

_cell_length_a                   12.6966(4)
_cell_length_b                   10.1709(3)
_cell_length_c                   38.0873(11)
_cell_angle_alpha                90
_cell_angle_beta                 92.904(3)
_cell_angle_gamma                90
_cell_volume                     4912.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    15137
_cell_measurement_theta_min      2.5670
_cell_measurement_theta_max      28.8260

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             2008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.829
_shelx_estimated_absorpt_T_min   0.858
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.46425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
crysalispro 1.171.39.9g (rigaku oxford diffraction, 2015)
empirical absorption correction using spherical harmonics,
 implemented in scale3 abspack scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  
'dtrek-crysalispro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50784
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.142
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8992
_reflns_number_gt                6615
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

 Structure factors included contributions from the .fab file.

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

_computing_data_collection       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_cell_refinement       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_data_reduction        'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1049P)²+9.6538P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8992
_refine_ls_number_parameters     563
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0683
_refine_ls_wR_factor_ref         0.1965
_refine_ls_wR_factor_gt          0.1796
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.69056(5) 0.07071(6) 0.88370(2) 0.03190(19) Uani 1 1 d . . . . .
O1 O 0.8264(2) 0.1203(3) 0.90819(8) 0.0308(7) Uani 1 1 d . . . . .
N1 N 0.6095(3) 0.1743(4) 0.91854(9) 0.0316(9) Uani 1 1 d . . . . .
C1 C 1.1206(4) 0.0862(5) 0.94686(13) 0.0392(12) Uani 1 1 d . . . . .
H1A H 1.146085 0.172454 0.953004 0.059 Uiso 1 1 calc R U . . .
H1B H 1.161432 0.050569 0.928593 0.059 Uiso 1 1 calc R U . . .
H1C H 1.126799 0.030168 0.967142 0.059 Uiso 1 1 calc R U . . .
Ni2 Ni 0.92459(5) -0.00665(6) 0.88843(2) 0.03258(19) Uani 1 1 d . . . . .
O2 O 1.0127(3) 0.0943(3) 0.93476(8) 0.0355(8) Uani 1 1 d . . . . .
N2 N 0.6967(3) 0.2173(4) 0.84679(9) 0.0317(9) Uani 1 1 d . . . . .
C2 C 0.9409(4) 0.1439(5) 0.95738(12) 0.0315(10) Uani 1 1 d . . . . .
O3 O 0.5303(3) 0.0320(4) 0.86656(9) 0.0413(9) Uani 1 1 d . . . . .
N3 N 1.0357(3) -0.1092(4) 0.86664(10) 0.0360(10) Uani 1 1 d . . . . .
C3 C 0.9638(4) 0.1822(5) 0.99139(12) 0.0341(11) Uani 1 1 d . . . . .
H3 H 1.032033 0.175094 1.001316 0.041 Uiso 1 1 calc R U . . .
O4 O 0.5183(3) 0.3017(4) 0.81107(8) 0.0416(9) Uani 1 1 d . . . . .
N4 N 1.2639(9) 0.0684(11) 0.6773(3) 0.184(5) Uiso 1 1 d D . . . .
C4 C 0.8823(4) 0.2322(5) 1.01087(12) 0.0377(12) Uani 1 1 d . . . . .
H4 H 0.896747 0.259351 1.033926 0.045 Uiso 1 1 calc R U . . .
O5 O 0.7912(3) -0.0331(3) 0.85448(8) 0.0371(8) Uani 1 1 d . . . . .
C5 C 0.7819(4) 0.2416(5) 0.99653(12) 0.0336(11) Uani 1 1 d . . . . .
H5 H 0.728975 0.274818 1.010008 0.040 Uiso 1 1 calc R U . . .
O6 O 0.8772(4) -0.2410(4) 0.81744(11) 0.0588(11) Uani 1 1 d . . . . .
C6 C 0.7570(4) 0.2017(5) 0.96146(11) 0.0306(10) Uani 1 1 d . . . . .
O7 O 0.9938(3) 0.1387(3) 0.85681(8) 0.0386(8) Uani 1 1 d . . . . .
C7 C 0.8380(4) 0.1543(4) 0.94184(11) 0.0292(10) Uani 1 1 d . . . . .
O8 O 0.8859(3) -0.1493(3) 0.91945(8) 0.0379(8) Uani 1 1 d . . . . .
C8 C 0.6486(4) 0.2132(5) 0.94887(12) 0.0314(10) Uani 1 1 d . . . . .
H8 H 0.602240 0.252160 0.963900 0.038 Uiso 1 1 calc R U . . .
O9 O 0.8062(3) -0.3100(3) 0.96386(9) 0.0433(9) Uani 1 1 d . . . . .
C9 C 0.5030(4) 0.1973(5) 0.90825(12) 0.0341(11) Uani 1 1 d . . . . .
O10 O 0.6804(3) -0.1005(3) 0.91281(10) 0.0494(10) Uani 1 1 d . . . . .
H10A H 0.733162 -0.121376 0.929724 0.059 Uiso 1 1 calc R U . . .
H10B H 0.623096 -0.156568 0.908956 0.059 Uiso 1 1 calc R U . . .
C10 C 0.4397(4) 0.2933(5) 0.92230(13) 0.0412(12) Uani 1 1 d . . . . .
H10 H 0.466437 0.345174 0.940791 0.049 Uiso 1 1 calc R U . . .
C11 C 0.3377(4) 0.3125(6) 0.90913(14) 0.0485(14) Uani 1 1 d . . . . .
H11 H 0.296242 0.377799 0.918488 0.058 Uiso 1 1 calc R U . . .
C12 C 0.2975(4) 0.2347(6) 0.88211(14) 0.0492(14) Uani 1 1 d . . . . .
H12 H 0.227962 0.246100 0.873813 0.059 Uiso 1 1 calc R U . . .
C13 C 0.3587(4) 0.1403(6) 0.86716(13) 0.0417(13) Uani 1 1 d . . . . .
H13 H 0.331230 0.089290 0.848604 0.050 Uiso 1 1 calc R U . . .
C14 C 0.4611(4) 0.1221(5) 0.88003(12) 0.0363(11) Uani 1 1 d . . . . .
C15 C 0.4982(5) -0.0363(6) 0.83514(14) 0.0510(15) Uani 1 1 d . . . . .
H15A H 0.438782 -0.091341 0.839490 0.076 Uiso 1 1 calc R U . . .
H15B H 0.555334 -0.089713 0.827738 0.076 Uiso 1 1 calc R U . . .
H15C H 0.478729 0.026021 0.817034 0.076 Uiso 1 1 calc R U . . .
C16 C 0.4207(5) 0.3367(6) 0.79364(15) 0.0544(16) Uani 1 1 d . . . . .
H16A H 0.367612 0.345068 0.810583 0.082 Uiso 1 1 calc R U . . .
H16B H 0.400160 0.269704 0.776903 0.082 Uiso 1 1 calc R U . . .
H16C H 0.428307 0.418930 0.781662 0.082 Uiso 1 1 calc R U . . .
C17 C 0.5593(4) 0.3854(5) 0.83683(12) 0.0367(12) Uani 1 1 d . . . . .
O18 O 1.3321(8) -0.0156(10) 0.6690(3) 0.195(4) Uiso 1 1 d D . . . .
C18 C 0.5146(5) 0.5034(6) 0.84584(14) 0.0475(14) Uani 1 1 d . . . . .
H18 H 0.453187 0.532231 0.833907 0.057 Uiso 1 1 calc R U . . .
O19 O 1.2113(9) 0.1307(11) 0.6555(3) 0.217(5) Uiso 1 1 d D . . . .
C19 C 0.5606(5) 0.5784(6) 0.87239(15) 0.0500(14) Uani 1 1 d . . . . .
H19 H 0.529842 0.657849 0.878309 0.060 Uiso 1 1 calc R U . . .
O20 O 1.2570(9) 0.0891(12) 0.7093(2) 0.218(5) Uiso 1 1 d D . . . .
C20 C 0.6518(4) 0.5374(5) 0.89040(14) 0.0432(13) Uani 1 1 d . . . . .
H20 H 0.682417 0.588395 0.908424 0.052 Uiso 1 1 calc R U . . .
C21 C 0.6968(4) 0.4195(5) 0.88127(12) 0.0377(12) Uani 1 1 d . . . . .
H21 H 0.758659 0.391534 0.893121 0.045 Uiso 1 1 calc R U . . .
C22 C 0.6510(4) 0.3422(5) 0.85464(11) 0.0320(10) Uani 1 1 d . . . . .
C23 C 0.7294(4) 0.2035(6) 0.81582(12) 0.0400(12) Uani 1 1 d . . . . .
H23 H 0.721325 0.276285 0.801158 0.048 Uiso 1 1 calc R U . . .
C24 C 0.7769(4) 0.0904(6) 0.80081(13) 0.0456(14) Uani 1 1 d . . . . .
C25 C 0.8006(6) 0.1004(8) 0.76493(15) 0.067(2) Uani 1 1 d . . . . .
H25 H 0.783007 0.176670 0.752500 0.080 Uiso 1 1 calc R U . . .
C26 C 0.8481(6) 0.0011(9) 0.74866(16) 0.078(2) Uani 1 1 d . . . . .
H26 H 0.865869 0.010280 0.725402 0.094 Uiso 1 1 calc R U . . .
C27 C 0.8703(5) -0.1136(7) 0.76628(15) 0.0625(19) Uani 1 1 d . . . . .
H27 H 0.901245 -0.182828 0.754635 0.075 Uiso 1 1 calc R U . . .
C28 C 0.8472(4) -0.1280(6) 0.80135(14) 0.0457(14) Uani 1 1 d . . . . .
C29 C 0.8032(4) -0.0234(6) 0.81972(13) 0.0409(13) Uani 1 1 d . . . . .
C30 C 0.8034(6) -0.3050(7) 0.83461(15) 0.0606(17) Uani 1 1 d . . . . .
H30A H 0.790572 -0.259326 0.856035 0.091 Uiso 1 1 calc R U . . .
H30B H 0.827314 -0.392584 0.839976 0.091 Uiso 1 1 calc R U . . .
H30C H 0.739326 -0.308933 0.820133 0.091 Uiso 1 1 calc R U . . .
C31 C 0.9708(4) 0.2766(5) 0.85433(15) 0.0451(13) Uani 1 1 d . . . . .
H31A H 1.035053 0.325922 0.857462 0.068 Uiso 1 1 calc R U . . .
H31B H 0.923854 0.300602 0.872254 0.068 Uiso 1 1 calc R U . . .
H31C H 0.938044 0.295596 0.831627 0.068 Uiso 1 1 calc R U . . .
C32 C 1.0627(4) 0.0870(5) 0.83371(12) 0.0359(11) Uani 1 1 d . . . . .
C33 C 1.1069(4) 0.1585(6) 0.80740(13) 0.0471(14) Uani 1 1 d . . . . .
H33 H 1.091488 0.247358 0.804528 0.056 Uiso 1 1 calc R U . . .
C34 C 1.1744(5) 0.0963(7) 0.78536(15) 0.0527(15) Uani 1 1 d . . . . .
H34 H 1.204918 0.143757 0.767643 0.063 Uiso 1 1 calc R U . . .
C35 C 1.1963(5) -0.0333(7) 0.78944(14) 0.0546(16) Uani 1 1 d . . . . .
H35 H 1.241826 -0.073833 0.774400 0.065 Uiso 1 1 calc R U . . .
C36 C 1.1525(4) -0.1060(6) 0.81543(14) 0.0484(14) Uani 1 1 d . . . . .
H36 H 1.166856 -0.195418 0.817326 0.058 Uiso 1 1 calc R U . . .
C37 C 1.0868(4) -0.0465(5) 0.83893(13) 0.0378(12) Uani 1 1 d . . . . .
C38 C 1.0601(4) -0.2290(5) 0.87592(13) 0.0400(13) Uani 1 1 d . . . . .
H38 H 1.115124 -0.267506 0.864421 0.048 Uiso 1 1 calc R U . . .
C39 C 1.0129(4) -0.3076(5) 0.90140(13) 0.0385(12) Uani 1 1 d . . . . .
C40 C 1.0558(5) -0.4353(5) 0.90654(15) 0.0447(13) Uani 1 1 d . . . . .
H40 H 1.112226 -0.461857 0.893604 0.054 Uiso 1 1 calc R U . . .
C41 C 1.0156(5) -0.5192(5) 0.93008(15) 0.0504(15) Uani 1 1 d . . . . .
H41 H 1.044559 -0.602574 0.933219 0.061 Uiso 1 1 calc R U . . .
C42 C 0.9304(4) -0.4805(5) 0.94970(14) 0.0426(13) Uani 1 1 d . . . . .
H42 H 0.902414 -0.538644 0.965608 0.051 Uiso 1 1 calc R U . . .
C43 C 0.8883(4) -0.3569(5) 0.94543(12) 0.0375(12) Uani 1 1 d . . . . .
C44 C 0.9277(4) -0.2659(5) 0.92160(12) 0.0364(12) Uani 1 1 d . . . . .
C45 C 0.7607(5) -0.3978(6) 0.98789(16) 0.0556(15) Uani 1 1 d . . . . .
H45A H 0.735959 -0.475076 0.975577 0.083 Uiso 1 1 calc R U . . .
H45B H 0.702591 -0.355352 0.998435 0.083 Uiso 1 1 calc R U . . .
H45C H 0.812744 -0.422144 1.005871 0.083 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.984(3) . ?
Ni1 N1 2.017(4) . ?
Ni1 O5 2.032(3) . ?
Ni1 N2 2.053(4) . ?
Ni1 O10 2.072(4) . ?
Ni1 O3 2.141(3) . ?
O1 C7 1.329(5) . ?
O1 Ni2 1.971(3) . ?
N1 C8 1.295(6) . ?
N1 C9 1.408(6) . ?
C1 O2 1.425(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
Ni2 O8 1.950(4) . ?
Ni2 N3 1.972(4) . ?
Ni2 O5 2.095(3) . ?
Ni2 O7 2.125(4) . ?
Ni2 O2 2.285(3) . ?
O2 C2 1.381(6) . ?
N2 C23 1.278(6) . ?
N2 C22 1.434(6) . ?
C2 C3 1.370(6) . ?
C2 C7 1.410(6) . ?
O3 C14 1.387(6) . ?
O3 C15 1.425(6) . ?
N3 C38 1.302(7) . ?
N3 C37 1.418(7) . ?
C3 C4 1.399(7) . ?
C3 H3 0.9300 . ?
O4 C17 1.381(6) . ?
O4 C16 1.421(6) . ?
N4 O19 1.216(8) . ?
N4 O20 1.245(8) . ?
N4 O18 1.268(8) . ?
C4 C5 1.364(7) . ?
C4 H4 0.9300 . ?
O5 C29 1.344(6) . ?
C5 C6 1.417(6) . ?
C5 H5 0.9300 . ?
O6 C30 1.338(8) . ?
O6 C28 1.349(7) . ?
C6 C7 1.388(7) . ?
C6 C8 1.439(7) . ?
O7 C32 1.376(6) . ?
O7 C31 1.435(6) . ?
O8 C44 1.300(6) . ?
C8 H8 0.9300 . ?
O9 C43 1.371(6) . ?
O9 C45 1.422(7) . ?
C9 C10 1.389(7) . ?
C9 C14 1.402(7) . ?
O10 H10A 0.9300 . ?
O10 H10B 0.9300 . ?
C10 C11 1.379(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.376(8) . ?
C11 H11 0.9300 . ?
C12 C13 1.376(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.378(7) . ?
C13 H13 0.9300 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.378(8) . ?
C17 C22 1.389(7) . ?
C18 C19 1.373(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.380(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.380(7) . ?
C20 H20 0.9300 . ?
C21 C22 1.388(7) . ?
C21 H21 0.9300 . ?
C23 C24 1.432(8) . ?
C23 H23 0.9300 . ?
C24 C29 1.395(8) . ?
C24 C25 1.417(8) . ?
C25 C26 1.344(9) . ?
C25 H25 0.9300 . ?
C26 C27 1.367(10) . ?
C26 H26 0.9300 . ?
C27 C28 1.390(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.404(7) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 C33 1.380(8) . ?
C32 C37 1.404(7) . ?
C33 C34 1.383(8) . ?
C33 H33 0.9300 . ?
C34 C35 1.355(9) . ?
C34 H34 0.9300 . ?
C35 C36 1.376(9) . ?
C35 H35 0.9300 . ?
C36 C37 1.392(7) . ?
C36 H36 0.9300 . ?
C38 C39 1.414(8) . ?
C38 H38 0.9300 . ?
C39 C40 1.418(7) . ?
C39 C44 1.423(7) . ?
C40 C41 1.356(8) . ?
C40 H40 0.9300 . ?
C41 C42 1.401(8) . ?
C41 H41 0.9300 . ?
C42 C43 1.373(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.406(7) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N1 91.04(14) . . ?
O1 Ni1 O5 80.43(13) . . ?
N1 Ni1 O5 170.94(14) . . ?
O1 Ni1 N2 94.32(14) . . ?
N1 Ni1 N2 96.28(15) . . ?
O5 Ni1 N2 87.45(15) . . ?
O1 Ni1 O10 92.20(14) . . ?
N1 Ni1 O10 92.27(16) . . ?
O5 Ni1 O10 85.08(15) . . ?
N2 Ni1 O10 169.15(15) . . ?
O1 Ni1 O3 168.51(13) . . ?
N1 Ni1 O3 77.78(14) . . ?
O5 Ni1 O3 110.58(13) . . ?
N2 Ni1 O3 89.60(15) . . ?
O10 Ni1 O3 85.67(15) . . ?
C7 O1 Ni2 119.8(3) . . ?
C7 O1 Ni1 124.8(3) . . ?
Ni2 O1 Ni1 101.87(13) . . ?
C8 N1 C9 121.1(4) . . ?
C8 N1 Ni1 124.1(3) . . ?
C9 N1 Ni1 114.7(3) . . ?
O2 C1 H1A 109.5 . . ?
O2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O8 Ni2 O1 94.14(14) . . ?
O8 Ni2 N3 93.97(16) . . ?
O1 Ni2 N3 171.00(17) . . ?
O8 Ni2 O5 93.32(14) . . ?
O1 Ni2 O5 79.19(12) . . ?
N3 Ni2 O5 104.23(14) . . ?
O8 Ni2 O7 170.17(14) . . ?
O1 Ni2 O7 92.78(14) . . ?
N3 Ni2 O7 78.70(16) . . ?
O5 Ni2 O7 94.83(14) . . ?
O8 Ni2 O2 89.70(13) . . ?
O1 Ni2 O2 72.85(12) . . ?
N3 Ni2 O2 103.29(14) . . ?
O5 Ni2 O2 152.03(13) . . ?
O7 Ni2 O2 85.68(13) . . ?
C2 O2 C1 118.3(4) . . ?
C2 O2 Ni2 109.5(3) . . ?
C1 O2 Ni2 130.5(3) . . ?
C23 N2 C22 116.3(4) . . ?
C23 N2 Ni1 125.3(4) . . ?
C22 N2 Ni1 118.1(3) . . ?
C3 C2 O2 125.3(4) . . ?
C3 C2 C7 121.6(5) . . ?
O2 C2 C7 113.1(4) . . ?
C14 O3 C15 118.2(4) . . ?
C14 O3 Ni1 112.1(3) . . ?
C15 O3 Ni1 125.0(3) . . ?
C38 N3 C37 120.8(5) . . ?
C38 N3 Ni2 123.1(4) . . ?
C37 N3 Ni2 116.1(3) . . ?
C2 C3 C4 118.5(4) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C17 O4 C16 117.8(4) . . ?
O19 N4 O20 121.1(9) . . ?
O19 N4 O18 122.7(9) . . ?
O20 N4 O18 116.1(9) . . ?
C5 C4 C3 121.0(4) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C29 O5 Ni1 127.4(3) . . ?
C29 O5 Ni2 118.0(3) . . ?
Ni1 O5 Ni2 96.11(13) . . ?
C4 C5 C6 121.2(5) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C30 O6 C28 116.6(5) . . ?
C7 C6 C5 118.1(4) . . ?
C7 C6 C8 124.9(4) . . ?
C5 C6 C8 117.1(4) . . ?
C32 O7 C31 117.7(4) . . ?
C32 O7 Ni2 113.0(3) . . ?
C31 O7 Ni2 128.9(3) . . ?
O1 C7 C6 124.1(4) . . ?
O1 C7 C2 116.1(4) . . ?
C6 C7 C2 119.7(4) . . ?
C44 O8 Ni2 127.0(3) . . ?
N1 C8 C6 126.1(4) . . ?
N1 C8 H8 117.0 . . ?
C6 C8 H8 117.0 . . ?
C43 O9 C45 117.1(4) . . ?
C10 C9 C14 118.3(5) . . ?
C10 C9 N1 125.1(4) . . ?
C14 C9 N1 116.5(4) . . ?
Ni1 O10 H10A 120.0 . . ?
Ni1 O10 H10B 120.0 . . ?
H10A O10 H10B 120.0 . . ?
C11 C10 C9 120.7(5) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 119.8(6) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 121.0(5) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C14 119.2(5) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C13 C14 O3 124.2(5) . . ?
C13 C14 C9 121.0(5) . . ?
O3 C14 C9 114.9(4) . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 H16A 109.5 . . ?
O4 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O4 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 O4 124.6(5) . . ?
C18 C17 C22 120.0(5) . . ?
O4 C17 C22 115.4(4) . . ?
C19 C18 C17 120.1(5) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 120.8(5) . . ?
C18 C19 H19 119.6 . . ?
C20 C19 H19 119.6 . . ?
C19 C20 C21 119.0(5) . . ?
C19 C20 H20 120.5 . . ?
C21 C20 H20 120.5 . . ?
C20 C21 C22 120.8(5) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C17 119.2(5) . . ?
C21 C22 N2 119.7(4) . . ?
C17 C22 N2 121.1(4) . . ?
N2 C23 C24 128.3(5) . . ?
N2 C23 H23 115.8 . . ?
C24 C23 H23 115.8 . . ?
C29 C24 C25 120.1(5) . . ?
C29 C24 C23 123.7(5) . . ?
C25 C24 C23 116.2(5) . . ?
C26 C25 C24 120.8(7) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 120.1(6) . . ?
C25 C26 H26 120.0 . . ?
C27 C26 H26 120.0 . . ?
C26 C27 C28 120.9(6) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
O6 C28 C27 117.3(5) . . ?
O6 C28 C29 122.0(5) . . ?
C27 C28 C29 120.5(6) . . ?
O5 C29 C24 122.2(5) . . ?
O5 C29 C28 120.2(5) . . ?
C24 C29 C28 117.5(5) . . ?
O6 C30 H30A 109.5 . . ?
O6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O7 C31 H31A 109.5 . . ?
O7 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O7 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
O7 C32 C33 123.9(5) . . ?
O7 C32 C37 114.8(4) . . ?
C33 C32 C37 121.2(5) . . ?
C32 C33 C34 119.2(6) . . ?
C32 C33 H33 120.4 . . ?
C34 C33 H33 120.4 . . ?
C35 C34 C33 120.4(6) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 121.1(6) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C35 C36 C37 120.5(6) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
C36 C37 C32 117.5(5) . . ?
C36 C37 N3 126.5(5) . . ?
C32 C37 N3 115.8(4) . . ?
N3 C38 C39 127.8(5) . . ?
N3 C38 H38 116.1 . . ?
C39 C38 H38 116.1 . . ?
C38 C39 C40 116.1(5) . . ?
C38 C39 C44 124.2(5) . . ?
C40 C39 C44 119.7(5) . . ?
C41 C40 C39 120.8(6) . . ?
C41 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
C40 C41 C42 120.2(5) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C43 C42 C41 120.0(5) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
O9 C43 C42 124.0(5) . . ?
O9 C43 C44 113.9(4) . . ?
C42 C43 C44 122.0(5) . . ?
O8 C44 C43 118.9(5) . . ?
O8 C44 C39 123.9(5) . . ?
C43 C44 C39 117.2(5) . . ?
O9 C45 H45A 109.5 . . ?
O9 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
O9 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?

_refine_diff_density_max         1.418
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.095



# SQUEEZE RESULTS (Version = 241018)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 -0.001 0.000 298 101 ' '
2 0.484 0.088 0.251 93 25 ' '
3 0.000 -0.035 0.500 298 101 ' '
4 0.516 -0.088 0.749 94 25 ' '
5 -0.016 0.412 0.751 94 25 ' '
6 1.016 0.588 0.249 94 25 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_chemical_properties_physical    Moisture-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ni4-br-
_database_code_depnum_ccdc_archive 'CCDC 1874846'
_audit_update_record             
;
2018-12-12 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Ni4-Br]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H62 Br4 N6 Ni4 O16), C2 H3 N'
_chemical_formula_sum            'C62 H65 Br4 N7 Ni4 O16'
_chemical_formula_weight         1718.69

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.1808(5)
_cell_length_b                   15.8405(5)
_cell_length_c                   20.5877(5)
_cell_angle_alpha                105.986(2)
_cell_angle_beta                 90.324(3)
_cell_angle_gamma                105.805(3)
_cell_volume                     3359.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    17423
_cell_measurement_theta_min      2.1820
_cell_measurement_theta_max      27.4570

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_F_000             1732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.553
_shelx_estimated_absorpt_T_min   0.600
_shelx_estimated_absorpt_T_max   0.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.63645
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35525
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.900
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12305
_reflns_number_gt                9906
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear-SM Expert 2.1 b31 (Rigaku, 2014)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1221P)²+4.8871P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12305
_refine_ls_number_parameters     851
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0580
_refine_ls_wR_factor_ref         0.1773
_refine_ls_wR_factor_gt          0.1597
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.09588(6) 0.86651(4) -0.04204(3) 0.03167(17) Uani 1 1 d . . . . .
Ni1 Ni 0.42134(7) 0.64160(4) -0.01633(3) 0.01505(17) Uani 1 1 d . . . . .
O1 O 0.7892(4) 0.6419(2) 0.07330(17) 0.0192(8) Uani 1 1 d . . . . .
N1 N 0.4874(5) 0.7479(3) -0.0608(2) 0.0177(10) Uani 1 1 d . . . . .
H1 H 0.422307 0.736113 -0.098309 0.021 Uiso 1 1 calc R U . . .
C1 C 0.8936(6) 0.6192(4) 0.0983(3) 0.0298(14) Uani 1 1 d . . . . .
H1A H 0.940270 0.670428 0.136465 0.045 Uiso 1 1 calc R U . . .
H1B H 0.948487 0.607553 0.062000 0.045 Uiso 1 1 calc R U . . .
H1C H 0.863118 0.564309 0.113525 0.045 Uiso 1 1 calc R U . . .
Br2 Br 0.61713(6) 0.48557(4) 0.40038(3) 0.02728(17) Uani 1 1 d . . . . .
Ni2 Ni 0.58403(7) 0.56346(4) 0.06325(3) 0.01525(17) Uani 1 1 d . . . . .
O2 O 0.5953(4) 0.6566(2) 0.01462(17) 0.0186(8) Uani 1 1 d . . . . .
N2 N 0.5442(4) 0.6425(3) 0.1544(2) 0.0164(9) Uani 1 1 d . . . . .
H2 H 0.486485 0.674782 0.141655 0.020 Uiso 1 1 calc R U . . .
C2 C 0.8140(6) 0.6991(3) 0.0311(2) 0.0191(12) Uani 1 1 d . . . . .
Br3 Br 0.60767(6) 0.87644(4) 0.68513(3) 0.03393(18) Uani 1 1 d . . . . .
Ni3 Ni -0.07482(7) 0.64389(4) 0.57629(3) 0.01546(17) Uani 1 1 d . . . . .
O3 O 0.7344(4) 0.3766(2) 0.14863(17) 0.0221(9) Uani 1 1 d . . . . .
N3 N 0.2740(5) 0.7099(3) 0.0590(2) 0.0200(10) Uani 1 1 d . . . . .
C3 C 0.9308(6) 0.7458(3) 0.0196(3) 0.0203(12) Uani 1 1 d . . . . .
H3 H 1.004131 0.743668 0.041832 0.024 Uiso 1 1 calc R U . . .
Br4 Br 0.12511(6) 0.49559(4) 0.09653(2) 0.02448(16) Uani 1 1 d . . . . .
Ni4 Ni 0.08219(7) 0.56214(4) 0.46337(3) 0.01535(17) Uani 1 1 d . . . . .
O4 O 0.5974(4) 0.4643(2) 0.10437(16) 0.0182(8) Uani 1 1 d . . . . .
C4 C 0.9359(6) 0.7967(3) -0.0267(3) 0.0218(12) Uani 1 1 d . . . . .
O5 O 0.5995(4) 0.4687(2) -0.02278(17) 0.0156(8) Uani 1 1 d . . . . .
C5 C 0.8313(6) 0.7976(3) -0.0616(3) 0.0214(12) Uani 1 1 d . . . . .
H5A H 0.839400 0.831552 -0.093666 0.026 Uiso 1 1 calc R U . . .
H5 H 0.672(8) 0.485(5) -0.031(4) 0.05(3) Uiso 1 1 d . . . . .
O6 O 0.2381(4) 0.6580(3) -0.00100(17) 0.0228(9) Uani 1 1 d . . . . .
C6 C 0.7143(5) 0.7493(3) -0.0501(3) 0.0171(11) Uani 1 1 d . . . . .
O7 O 0.3890(4) 0.7271(2) 0.07790(17) 0.0201(8) Uani 1 1 d . . . . .
C7 C 0.7032(5) 0.7020(3) -0.0010(2) 0.0151(11) Uani 1 1 d . . . . .
O8 O 0.2024(4) 0.7430(3) 0.09567(19) 0.0282(10) Uani 1 1 d . . . . .
C8 C 0.6001(6) 0.7377(3) -0.0953(2) 0.0189(12) Uani 1 1 d . . . . .
H8A H 0.622017 0.783230 -0.121192 0.023 Uiso 1 1 calc R U . . .
H8B H 0.579269 0.676157 -0.128480 0.023 Uiso 1 1 calc R U . . .
C9 C 0.5020(6) 0.8439(3) -0.0195(3) 0.0205(12) Uani 1 1 d . . . . .
H9A H 0.570886 0.861969 0.016508 0.025 Uiso 1 1 calc R U . . .
H9B H 0.424536 0.846860 0.002894 0.025 Uiso 1 1 calc R U . . .
C10 C 0.5291(6) 0.9110(3) -0.0603(3) 0.0215(12) Uani 1 1 d . . . . .
C11 C 0.6472(6) 0.9647(4) -0.0622(3) 0.0283(14) Uani 1 1 d . . . . .
H11 H 0.713844 0.961260 -0.035143 0.034 Uiso 1 1 calc R U . . .
C12 C 0.6727(7) 1.0242(4) -0.1023(3) 0.0318(15) Uani 1 1 d . . . . .
H12 H 0.755677 1.060549 -0.102629 0.038 Uiso 1 1 calc R U . . .
C13 C 0.5773(7) 1.0300(4) -0.1414(3) 0.0342(16) Uani 1 1 d . . . . .
H13 H 0.593135 1.070950 -0.168532 0.041 Uiso 1 1 calc R U . . .
C14 C 0.4569(8) 0.9753(4) -0.1408(3) 0.0364(18) Uani 1 1 d . . . . .
H14 H 0.390655 0.978252 -0.168333 0.044 Uiso 1 1 calc R U . . .
C15 C 0.4324(6) 0.9164(4) -0.1004(3) 0.0269(14) Uani 1 1 d . . . . .
H15 H 0.349555 0.879871 -0.100103 0.032 Uiso 1 1 calc R U . . .
C16 C 0.8128(6) 0.3302(4) 0.1712(3) 0.0248(13) Uani 1 1 d . . . . .
H16A H 0.858438 0.305269 0.133650 0.037 Uiso 1 1 calc R U . . .
H16B H 0.761253 0.280058 0.186915 0.037 Uiso 1 1 calc R U . . .
H16C H 0.872371 0.373478 0.208621 0.037 Uiso 1 1 calc R U . . .
C17 C 0.6751(5) 0.4258(3) 0.1964(3) 0.0196(12) Uani 1 1 d . . . . .
C18 C 0.6790(6) 0.4284(3) 0.2643(3) 0.0205(12) Uani 1 1 d . . . . .
H18 H 0.722821 0.393816 0.280792 0.025 Uiso 1 1 calc R U . . .
C19 C 0.6172(6) 0.4828(3) 0.3073(2) 0.0191(12) Uani 1 1 d . . . . .
C20 C 0.5515(5) 0.5326(3) 0.2845(2) 0.0190(12) Uani 1 1 d . . . . .
H20 H 0.510421 0.569736 0.315294 0.023 Uiso 1 1 calc R U . . .
C21 C 0.5457(5) 0.5281(3) 0.2158(2) 0.0183(11) Uani 1 1 d . . . . .
C22 C 0.6052(5) 0.4731(3) 0.1704(2) 0.0150(11) Uani 1 1 d . . . . .
C23 C 0.4687(6) 0.5796(3) 0.1905(2) 0.0188(12) Uani 1 1 d . . . . .
H23A H 0.397549 0.535226 0.159289 0.023 Uiso 1 1 calc R U . . .
H23B H 0.434648 0.615445 0.229369 0.023 Uiso 1 1 calc R U . . .
C24 C 0.6466(6) 0.7155(3) 0.1997(3) 0.0216(12) Uani 1 1 d . . . . .
H24A H 0.693859 0.754821 0.173011 0.026 Uiso 1 1 calc R U . . .
H24B H 0.704439 0.686797 0.216025 0.026 Uiso 1 1 calc R U . . .
C25 C 0.6039(6) 0.7754(4) 0.2605(3) 0.0250(13) Uani 1 1 d . . . . .
C26 C 0.6353(7) 0.7752(4) 0.3262(3) 0.0310(15) Uani 1 1 d . . . . .
H26 H 0.685444 0.738391 0.333512 0.037 Uiso 1 1 calc R U . . .
C27 C 0.5922(8) 0.8298(5) 0.3813(3) 0.046(2) Uani 1 1 d . . . . .
H27 H 0.611601 0.828537 0.425908 0.056 Uiso 1 1 calc R U . . .
C28 C 0.5225(8) 0.8850(5) 0.3719(3) 0.047(2) Uani 1 1 d . . . . .
H28 H 0.496190 0.923240 0.409788 0.056 Uiso 1 1 calc R U . . .
C29 C 0.4903(7) 0.8847(4) 0.3066(3) 0.0408(18) Uani 1 1 d . . . . .
H29 H 0.439871 0.921368 0.299415 0.049 Uiso 1 1 calc R U . . .
C30 C 0.5326(7) 0.8304(4) 0.2520(3) 0.0316(15) Uani 1 1 d . . . . .
H30 H 0.511616 0.831239 0.207473 0.038 Uiso 1 1 calc R U . . .
N31 N 0.1568(11) 0.9511(7) 0.5396(4) 0.112(4) Uani 1 1 d . U . . .
C31 C 0.1979(15) 1.0382(7) 0.4491(6) 0.132(6) Uani 1 1 d . U . . .
H31A H 0.208868 1.103637 0.470105 0.198 Uiso 1 1 calc R U . . .
H31B H 0.127892 1.013871 0.413903 0.198 Uiso 1 1 calc R U . . .
H31C H 0.274218 1.029605 0.428602 0.198 Uiso 1 1 calc R U . . .
C32 C 0.1722(12) 0.9901(6) 0.5001(5) 0.083(4) Uani 1 1 d . U . . .
H105 H 0.170(8) 0.491(5) 0.532(4) 0.04(2) Uiso 1 1 d . . . . .
O101 O 0.2867(4) 0.6383(2) 0.48363(17) 0.0194(8) Uani 1 1 d . . . . .
N101 N -0.0050(5) 0.7543(3) 0.6628(2) 0.0199(10) Uani 1 1 d . . . . .
H101 H -0.067327 0.744464 0.696601 0.024 Uiso 1 1 calc R U . . .
C101 C 0.3886(6) 0.6123(4) 0.4489(3) 0.0271(13) Uani 1 1 d . . . . .
H10A H 0.439940 0.596115 0.479628 0.041 Uiso 1 1 calc R U . . .
H10B H 0.439705 0.663707 0.434459 0.041 Uiso 1 1 calc R U . . .
H10C H 0.355332 0.559442 0.409102 0.041 Uiso 1 1 calc R U . . .
O102 O 0.0979(4) 0.6562(2) 0.55115(17) 0.0189(8) Uani 1 1 d . . . . .
N102 N 0.0407(5) 0.6429(3) 0.40692(19) 0.0169(10) Uani 1 1 d . . . . .
H102 H -0.018974 0.672995 0.433084 0.020 Uiso 1 1 calc R U . . .
C102 C 0.3147(6) 0.7005(3) 0.5484(2) 0.0205(12) Uani 1 1 d . . . . .
O103 O 0.2219(4) 0.3699(2) 0.29822(17) 0.0206(8) Uani 1 1 d . . . . .
N103 N -0.2309(5) 0.7041(3) 0.5263(2) 0.0205(10) Uani 1 1 d . . . . .
C103 C 0.4329(6) 0.7496(4) 0.5769(3) 0.0223(12) Uani 1 1 d . . . . .
H103 H 0.504071 0.745973 0.552511 0.027 Uiso 1 1 calc R U . . .
O104 O 0.0888(4) 0.4606(2) 0.38023(16) 0.0196(8) Uani 1 1 d . . . . .
C104 C 0.4437(6) 0.8051(4) 0.6437(3) 0.0272(14) Uani 1 1 d . . . . .
O105 O 0.1003(4) 0.4676(2) 0.50879(16) 0.0139(8) Uani 1 1 d . . . . .
C105 C 0.3430(6) 0.8087(4) 0.6816(3) 0.0238(13) Uani 1 1 d . . . . .
H10D H 0.354601 0.845332 0.727521 0.029 Uiso 1 1 calc R U . . .
O106 O -0.2612(4) 0.6548(3) 0.56618(18) 0.0252(9) Uani 1 1 d . . . . .
C106 C 0.2234(6) 0.7573(3) 0.6513(2) 0.0188(12) Uani 1 1 d . . . . .
O107 O -0.1150(4) 0.7254(2) 0.51554(17) 0.0212(9) Uani 1 1 d . . . . .
C107 C 0.2075(5) 0.7049(3) 0.5835(3) 0.0173(11) Uani 1 1 d . . . . .
O108 O -0.3054(4) 0.7301(3) 0.4986(2) 0.0310(10) Uani 1 1 d . . . . .
C108 C 0.1130(5) 0.7483(4) 0.6937(2) 0.0196(12) Uani 1 1 d . . . . .
H10E H 0.095318 0.688643 0.703706 0.024 Uiso 1 1 calc R U . . .
H10F H 0.136984 0.796911 0.737512 0.024 Uiso 1 1 calc R U . . .
C109 C 0.0052(6) 0.8485(3) 0.6583(3) 0.0196(12) Uani 1 1 d . . . . .
H10G H -0.075500 0.849246 0.638736 0.024 Uiso 1 1 calc R U . . .
H10H H 0.069402 0.864321 0.627322 0.024 Uiso 1 1 calc R U . . .
C110 C 0.0393(6) 0.9201(3) 0.7269(3) 0.0223(13) Uani 1 1 d . . . . .
C111 C 0.1573(6) 0.9814(4) 0.7439(3) 0.0272(13) Uani 1 1 d . . . . .
H111 H 0.217249 0.981475 0.711419 0.033 Uiso 1 1 calc R U . . .
C112 C 0.1888(7) 1.0438(4) 0.8092(3) 0.0358(16) Uani 1 1 d . . . . .
H112 H 0.269628 1.086084 0.820545 0.043 Uiso 1 1 calc R U . . .
C113 C 0.1027(7) 1.0436(4) 0.8566(3) 0.0335(16) Uani 1 1 d . . . . .
H113 H 0.124267 1.084575 0.901036 0.040 Uiso 1 1 calc R U . . .
C114 C -0.0151(7) 0.9835(4) 0.8390(3) 0.0317(15) Uani 1 1 d . . . . .
H114 H -0.075079 0.984205 0.871517 0.038 Uiso 1 1 calc R U . . .
C115 C -0.0479(6) 0.9222(4) 0.7752(3) 0.0239(13) Uani 1 1 d . . . . .
H115 H -0.129763 0.881319 0.764090 0.029 Uiso 1 1 calc R U . . .
C116 C 0.3022(6) 0.3248(4) 0.2575(3) 0.0241(13) Uani 1 1 d . . . . .
H11A H 0.253085 0.278000 0.217673 0.036 Uiso 1 1 calc R U . . .
H11B H 0.341949 0.295676 0.284158 0.036 Uiso 1 1 calc R U . . .
H11C H 0.366480 0.369739 0.242657 0.036 Uiso 1 1 calc R U . . .
C117 C 0.1679(6) 0.4230(3) 0.2724(2) 0.0193(12) Uani 1 1 d . . . . .
C118 C 0.1763(5) 0.4289(3) 0.2064(2) 0.0182(11) Uani 1 1 d . . . . .
H118 H 0.220153 0.394465 0.175439 0.022 Uiso 1 1 calc R U . . .
C119 C 0.1180(5) 0.4873(3) 0.1869(2) 0.0183(11) Uani 1 1 d . . . . .
C120 C 0.0563(6) 0.5381(3) 0.2309(3) 0.0209(12) Uani 1 1 d . . . . .
H120 H 0.021215 0.579316 0.217065 0.025 Uiso 1 1 calc R U . . .
C121 C 0.0446(5) 0.5296(3) 0.2969(2) 0.0176(11) Uani 1 1 d . . . . .
C122 C 0.0991(5) 0.4707(3) 0.3178(2) 0.0159(11) Uani 1 1 d . . . . .
C123 C -0.0326(6) 0.5802(4) 0.3431(3) 0.0203(12) Uani 1 1 d . . . . .
H12A H -0.066337 0.616159 0.319113 0.024 Uiso 1 1 calc R U . . .
H12B H -0.104132 0.535340 0.354310 0.024 Uiso 1 1 calc R U . . .
C124 C 0.1437(6) 0.7188(4) 0.3972(3) 0.0228(13) Uani 1 1 d . . . . .
H12C H 0.210557 0.693538 0.376027 0.027 Uiso 1 1 calc R U . . .
H12D H 0.178968 0.761925 0.442196 0.027 Uiso 1 1 calc R U . . .
C125 C 0.1046(6) 0.7713(3) 0.3537(3) 0.0230(13) Uani 1 1 d . . . . .
C126 C 0.1615(6) 0.7798(4) 0.2954(3) 0.0262(13) Uani 1 1 d . . . . .
H126 H 0.226749 0.752382 0.282475 0.031 Uiso 1 1 calc R U . . .
C127 C 0.1250(7) 0.8277(4) 0.2554(3) 0.0342(16) Uani 1 1 d . . . . .
H127 H 0.166627 0.834110 0.216197 0.041 Uiso 1 1 calc R U . . .
C128 C 0.0276(7) 0.8662(4) 0.2727(3) 0.0345(16) Uani 1 1 d . . . . .
H128 H 0.001401 0.898188 0.245039 0.041 Uiso 1 1 calc R U . . .
C129 C -0.0309(7) 0.8575(4) 0.3305(3) 0.0356(16) Uani 1 1 d . . . . .
H129 H -0.097260 0.883890 0.342786 0.043 Uiso 1 1 calc R U . . .
C130 C 0.0065(7) 0.8110(4) 0.3703(3) 0.0304(14) Uani 1 1 d . . . . .
H130 H -0.034634 0.805565 0.409860 0.036 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
Br1 C4 1.908(6) . ?
Ni1 O2 1.974(4) . ?
Ni1 O4 2.067(3) 2_665 ?
Ni1 O5 2.076(4) 2_665 ?
Ni1 N1 2.098(4) . ?
Ni1 O7 2.135(3) . ?
Ni1 O6 2.148(4) . ?
O1 C2 1.397(6) . ?
O1 C1 1.443(7) . ?
O1 Ni2 2.269(4) . ?
N1 C8 1.474(7) . ?
N1 C9 1.488(6) . ?
N1 H1 1.0000 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
Br2 C19 1.905(5) . ?
Ni2 O2 1.977(3) . ?
Ni2 O4 2.017(3) . ?
Ni2 O5 2.025(3) . ?
Ni2 N2 2.076(4) . ?
Ni2 O5 2.084(4) 2_665 ?
O2 C7 1.318(7) . ?
N2 C24 1.480(7) . ?
N2 C23 1.487(7) . ?
N2 H2 1.0000 . ?
C2 C3 1.372(8) . ?
C2 C7 1.419(8) . ?
Br3 C104 1.920(6) . ?
Ni3 O102 1.974(4) . ?
Ni3 O104 2.059(3) 2_566 ?
Ni3 O105 2.070(3) 2_566 ?
Ni3 N101 2.090(4) . ?
Ni3 O106 2.151(4) . ?
Ni3 O107 2.152(3) . ?
O3 C17 1.372(6) . ?
O3 C16 1.436(6) . ?
N3 O8 1.226(6) . ?
N3 O6 1.272(5) . ?
N3 O7 1.274(6) . ?
C3 C4 1.402(8) . ?
C3 H3 0.9500 . ?
Br4 C119 1.901(5) . ?
Ni4 O102 1.972(3) . ?
Ni4 O104 2.018(3) . ?
Ni4 O105 2.022(3) . ?
Ni4 N102 2.082(4) . ?
Ni4 O105 2.087(4) 2_566 ?
Ni4 O101 2.251(4) . ?
O4 C22 1.327(6) . ?
C4 C5 1.374(8) . ?
O5 H5 0.82(9) . ?
C5 C6 1.382(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.401(7) . ?
C6 C8 1.515(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.500(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.369(9) . ?
C10 C15 1.391(8) . ?
C11 C12 1.393(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.371(9) . ?
C12 H12 0.9500 . ?
C13 C14 1.390(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(9) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.386(7) . ?
C17 C22 1.413(7) . ?
C18 C19 1.384(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.378(7) . ?
C20 C21 1.397(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.397(7) . ?
C21 C23 1.513(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.514(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C30 1.373(8) . ?
C25 C26 1.398(8) . ?
C26 C27 1.399(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.368(10) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.386(8) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
N31 C32 1.139(12) . ?
C31 C32 1.445(13) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
O101 C102 1.397(6) . ?
O101 C101 1.442(7) . ?
N101 C109 1.493(6) . ?
N101 C108 1.498(7) . ?
N101 H101 1.0000 . ?
C101 H10A 0.9800 . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
O102 C107 1.317(7) . ?
N102 C124 1.481(7) . ?
N102 C123 1.487(6) . ?
N102 H102 1.0000 . ?
C102 C103 1.370(8) . ?
C102 C107 1.411(8) . ?
O103 C117 1.369(6) . ?
O103 C116 1.431(6) . ?
N103 O108 1.225(6) . ?
N103 O106 1.269(6) . ?
N103 O107 1.284(6) . ?
C103 C104 1.397(7) . ?
C103 H103 0.9500 . ?
O104 C122 1.340(6) . ?
C104 C105 1.379(9) . ?
O105 H105 0.84(8) . ?
C105 C106 1.399(8) . ?
C105 H10D 0.9500 . ?
C106 C107 1.395(7) . ?
C106 C108 1.515(8) . ?
C108 H10E 0.9900 . ?
C108 H10F 0.9900 . ?
C109 C110 1.517(7) . ?
C109 H10G 0.9900 . ?
C109 H10H 0.9900 . ?
C110 C111 1.385(9) . ?
C110 C115 1.397(8) . ?
C111 C112 1.407(8) . ?
C111 H111 0.9500 . ?
C112 C113 1.374(10) . ?
C112 H112 0.9500 . ?
C113 C114 1.376(10) . ?
C113 H113 0.9500 . ?
C114 C115 1.379(8) . ?
C114 H114 0.9500 . ?
C115 H115 0.9500 . ?
C116 H11A 0.9800 . ?
C116 H11B 0.9800 . ?
C116 H11C 0.9800 . ?
C117 C118 1.389(7) . ?
C117 C122 1.404(7) . ?
C118 C119 1.404(7) . ?
C118 H118 0.9500 . ?
C119 C120 1.362(7) . ?
C120 C121 1.405(7) . ?
C120 H120 0.9500 . ?
C121 C122 1.398(7) . ?
C121 C123 1.503(7) . ?
C123 H12A 0.9900 . ?
C123 H12B 0.9900 . ?
C124 C125 1.512(7) . ?
C124 H12C 0.9900 . ?
C124 H12D 0.9900 . ?
C125 C126 1.384(8) . ?
C125 C130 1.406(9) . ?
C126 C127 1.389(8) . ?
C126 H126 0.9500 . ?
C127 C128 1.390(10) . ?
C127 H127 0.9500 . ?
C128 C129 1.384(9) . ?
C128 H128 0.9500 . ?
C129 C130 1.373(8) . ?
C129 H129 0.9500 . ?
C130 H130 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O4 98.83(15) . 2_665 ?
O2 Ni1 O5 78.29(16) . 2_665 ?
O4 Ni1 O5 79.10(13) 2_665 2_665 ?
O2 Ni1 N1 88.83(17) . . ?
O4 Ni1 N1 96.10(15) 2_665 . ?
O5 Ni1 N1 165.28(17) 2_665 . ?
O2 Ni1 O7 93.06(15) . . ?
O4 Ni1 O7 163.44(16) 2_665 . ?
O5 Ni1 O7 92.18(14) 2_665 . ?
N1 Ni1 O7 95.62(15) . . ?
O2 Ni1 O6 153.31(14) . . ?
O4 Ni1 O6 106.27(15) 2_665 . ?
O5 Ni1 O6 97.43(16) 2_665 . ?
N1 Ni1 O6 97.27(16) . . ?
O7 Ni1 O6 60.56(14) . . ?
C2 O1 C1 117.1(5) . . ?
C2 O1 Ni2 111.8(3) . . ?
C1 O1 Ni2 127.8(3) . . ?
C8 N1 C9 112.2(4) . . ?
C8 N1 Ni1 110.1(3) . . ?
C9 N1 Ni1 118.8(3) . . ?
C8 N1 H1 104.8 . . ?
C9 N1 H1 104.8 . . ?
Ni1 N1 H1 104.8 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
O1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O2 Ni2 O4 170.28(16) . . ?
O2 Ni2 O5 91.85(14) . . ?
O4 Ni2 O5 81.49(13) . . ?
O2 Ni2 N2 95.24(15) . . ?
O4 Ni2 N2 92.25(15) . . ?
O5 Ni2 N2 170.19(18) . . ?
O2 Ni2 O5 78.05(15) . 2_665 ?
O4 Ni2 O5 108.04(16) . 2_665 ?
O5 Ni2 O5 83.78(16) . 2_665 ?
N2 Ni2 O5 91.06(16) . 2_665 ?
O2 Ni2 O1 74.21(14) . . ?
O4 Ni2 O1 98.95(15) . . ?
O5 Ni2 O1 93.00(15) . . ?
N2 Ni2 O1 95.44(16) . . ?
O5 Ni2 O1 151.95(14) 2_665 . ?
C7 O2 Ni1 132.2(3) . . ?
C7 O2 Ni2 121.6(3) . . ?
Ni1 O2 Ni2 105.08(18) . . ?
C24 N2 C23 112.3(4) . . ?
C24 N2 Ni2 119.4(4) . . ?
C23 N2 Ni2 108.1(3) . . ?
C24 N2 H2 105.3 . . ?
C23 N2 H2 105.3 . . ?
Ni2 N2 H2 105.3 . . ?
C3 C2 O1 125.1(5) . . ?
C3 C2 C7 122.7(5) . . ?
O1 C2 C7 112.2(5) . . ?
O102 Ni3 O104 97.14(16) . 2_566 ?
O102 Ni3 O105 78.49(15) . 2_566 ?
O104 Ni3 O105 78.72(13) 2_566 2_566 ?
O102 Ni3 N101 88.58(17) . . ?
O104 Ni3 N101 98.25(15) 2_566 . ?
O105 Ni3 N101 166.16(18) 2_566 . ?
O102 Ni3 O106 154.44(15) . . ?
O104 Ni3 O106 105.78(16) 2_566 . ?
O105 Ni3 O106 94.82(15) 2_566 . ?
N101 Ni3 O106 98.99(16) . . ?
O102 Ni3 O107 94.85(16) . . ?
O104 Ni3 O107 162.22(16) 2_566 . ?
O105 Ni3 O107 90.91(13) 2_566 . ?
N101 Ni3 O107 95.12(15) . . ?
O106 Ni3 O107 60.33(15) . . ?
C17 O3 C16 117.8(4) . . ?
O8 N3 O6 121.7(5) . . ?
O8 N3 O7 122.2(4) . . ?
O6 N3 O7 116.1(4) . . ?
C2 C3 C4 116.3(5) . . ?
C2 C3 H3 121.8 . . ?
C4 C3 H3 121.8 . . ?
O102 Ni4 O104 170.67(15) . . ?
O102 Ni4 O105 92.27(14) . . ?
O104 Ni4 O105 80.81(13) . . ?
O102 Ni4 N102 94.22(15) . . ?
O104 Ni4 N102 93.37(14) . . ?
O105 Ni4 N102 170.96(17) . . ?
O102 Ni4 O105 78.14(15) . 2_566 ?
O104 Ni4 O105 107.22(15) . 2_566 ?
O105 Ni4 O105 84.70(15) . 2_566 ?
N102 Ni4 O105 90.49(17) . 2_566 ?
O102 Ni4 O101 74.71(14) . . ?
O104 Ni4 O101 99.27(15) . . ?
O105 Ni4 O101 92.97(15) . . ?
N102 Ni4 O101 94.79(17) . . ?
O105 Ni4 O101 152.63(13) 2_566 . ?
C22 O4 Ni2 124.9(3) . . ?
C22 O4 Ni1 135.8(3) . 2_665 ?
Ni2 O4 Ni1 99.06(14) . 2_665 ?
C5 C4 C3 122.8(6) . . ?
C5 C4 Br1 119.2(4) . . ?
C3 C4 Br1 118.0(4) . . ?
Ni2 O5 Ni1 98.49(15) . 2_665 ?
Ni2 O5 Ni2 96.23(16) . 2_665 ?
Ni1 O5 Ni2 97.85(18) 2_665 2_665 ?
Ni2 O5 H5 105(6) . . ?
Ni1 O5 H5 108(6) 2_665 . ?
Ni2 O5 H5 143(6) 2_665 . ?
C4 C5 C6 120.2(5) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
N3 O6 Ni1 91.4(3) . . ?
C5 C6 C7 119.4(5) . . ?
C5 C6 C8 120.7(5) . . ?
C7 C6 C8 119.5(5) . . ?
N3 O7 Ni1 91.9(3) . . ?
O2 C7 C6 123.5(5) . . ?
O2 C7 C2 118.1(5) . . ?
C6 C7 C2 118.3(5) . . ?
N1 C8 C6 116.3(4) . . ?
N1 C8 H8A 108.2 . . ?
C6 C8 H8A 108.2 . . ?
N1 C8 H8B 108.2 . . ?
C6 C8 H8B 108.2 . . ?
H8A C8 H8B 107.4 . . ?
N1 C9 C10 113.2(4) . . ?
N1 C9 H9A 108.9 . . ?
C10 C9 H9A 108.9 . . ?
N1 C9 H9B 108.9 . . ?
C10 C9 H9B 108.9 . . ?
H9A C9 H9B 107.8 . . ?
C11 C10 C15 118.3(5) . . ?
C11 C10 C9 122.3(5) . . ?
C15 C10 C9 119.3(6) . . ?
C10 C11 C12 122.1(6) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C13 C12 C11 119.5(7) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 119.2(6) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
C15 C14 C13 120.9(6) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C10 120.0(6) . . ?
C14 C15 H15 120.0 . . ?
C10 C15 H15 120.0 . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C17 C18 124.3(5) . . ?
O3 C17 C22 114.0(4) . . ?
C18 C17 C22 121.7(5) . . ?
C19 C18 C17 118.1(5) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
C20 C19 C18 122.2(5) . . ?
C20 C19 Br2 118.6(4) . . ?
C18 C19 Br2 119.2(4) . . ?
C19 C20 C21 119.4(5) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C22 C21 C20 120.4(5) . . ?
C22 C21 C23 120.3(4) . . ?
C20 C21 C23 119.2(5) . . ?
O4 C22 C21 122.0(4) . . ?
O4 C22 C17 119.9(4) . . ?
C21 C22 C17 118.1(4) . . ?
N2 C23 C21 111.6(5) . . ?
N2 C23 H23A 109.3 . . ?
C21 C23 H23A 109.3 . . ?
N2 C23 H23B 109.3 . . ?
C21 C23 H23B 109.3 . . ?
H23A C23 H23B 108.0 . . ?
N2 C24 C25 114.3(5) . . ?
N2 C24 H24A 108.7 . . ?
C25 C24 H24A 108.7 . . ?
N2 C24 H24B 108.7 . . ?
C25 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C30 C25 C26 118.6(5) . . ?
C30 C25 C24 120.6(5) . . ?
C26 C25 C24 120.7(5) . . ?
C25 C26 C27 119.4(6) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C28 C27 C26 121.1(6) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 119.6(6) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C30 C29 C28 119.3(6) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C25 C30 C29 121.9(6) . . ?
C25 C30 H30 119.0 . . ?
C29 C30 H30 119.0 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N31 C32 C31 176.9(17) . . ?
C102 O101 C101 117.7(4) . . ?
C102 O101 Ni4 111.8(3) . . ?
C101 O101 Ni4 127.7(3) . . ?
C109 N101 C108 112.3(4) . . ?
C109 N101 Ni3 118.1(3) . . ?
C108 N101 Ni3 110.8(3) . . ?
C109 N101 H101 104.7 . . ?
C108 N101 H101 104.7 . . ?
Ni3 N101 H101 104.7 . . ?
O101 C101 H10A 109.5 . . ?
O101 C101 H10B 109.5 . . ?
H10A C101 H10B 109.5 . . ?
O101 C101 H10C 109.5 . . ?
H10A C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C107 O102 Ni4 121.7(3) . . ?
C107 O102 Ni3 133.0(3) . . ?
Ni4 O102 Ni3 104.93(17) . . ?
C124 N102 C123 114.3(4) . . ?
C124 N102 Ni4 118.1(3) . . ?
C123 N102 Ni4 107.6(3) . . ?
C124 N102 H102 105.2 . . ?
C123 N102 H102 105.2 . . ?
Ni4 N102 H102 105.2 . . ?
C103 C102 O101 124.5(5) . . ?
C103 C102 C107 122.7(5) . . ?
O101 C102 C107 112.7(5) . . ?
C117 O103 C116 118.4(4) . . ?
O108 N103 O106 123.6(5) . . ?
O108 N103 O107 120.6(5) . . ?
O106 N103 O107 115.8(4) . . ?
C102 C103 C104 116.7(5) . . ?
C102 C103 H103 121.6 . . ?
C104 C103 H103 121.6 . . ?
C122 O104 Ni4 123.8(3) . . ?
C122 O104 Ni3 136.5(3) . 2_566 ?
Ni4 O104 Ni3 99.67(15) . 2_566 ?
C105 C104 C103 123.1(6) . . ?
C105 C104 Br3 118.8(4) . . ?
C103 C104 Br3 118.1(5) . . ?
Ni4 O105 Ni3 99.16(14) . 2_566 ?
Ni4 O105 Ni4 95.30(15) . 2_566 ?
Ni3 O105 Ni4 97.64(16) 2_566 2_566 ?
Ni4 O105 H105 105(5) . . ?
Ni3 O105 H105 121(5) 2_566 . ?
Ni4 O105 H105 132(5) 2_566 . ?
C104 C105 C106 118.8(5) . . ?
C104 C105 H10D 120.6 . . ?
C106 C105 H10D 120.6 . . ?
N103 O106 Ni3 92.1(3) . . ?
C107 C106 C105 120.0(5) . . ?
C107 C106 C108 119.2(5) . . ?
C105 C106 C108 120.3(4) . . ?
N103 O107 Ni3 91.6(3) . . ?
O102 C107 C106 123.5(5) . . ?
O102 C107 C102 118.0(4) . . ?
C106 C107 C102 118.4(5) . . ?
N101 C108 C106 116.0(4) . . ?
N101 C108 H10E 108.3 . . ?
C106 C108 H10E 108.3 . . ?
N101 C108 H10F 108.3 . . ?
C106 C108 H10F 108.3 . . ?
H10E C108 H10F 107.4 . . ?
N101 C109 C110 112.3(4) . . ?
N101 C109 H10G 109.1 . . ?
C110 C109 H10G 109.1 . . ?
N101 C109 H10H 109.1 . . ?
C110 C109 H10H 109.1 . . ?
H10G C109 H10H 107.9 . . ?
C111 C110 C115 118.8(5) . . ?
C111 C110 C109 121.4(5) . . ?
C115 C110 C109 119.7(6) . . ?
C110 C111 C112 120.3(6) . . ?
C110 C111 H111 119.9 . . ?
C112 C111 H111 119.9 . . ?
C113 C112 C111 120.1(7) . . ?
C113 C112 H112 120.0 . . ?
C111 C112 H112 120.0 . . ?
C112 C113 C114 119.4(5) . . ?
C112 C113 H113 120.3 . . ?
C114 C113 H113 120.3 . . ?
C113 C114 C115 121.3(6) . . ?
C113 C114 H114 119.3 . . ?
C115 C114 H114 119.3 . . ?
C114 C115 C110 120.0(6) . . ?
C114 C115 H115 120.0 . . ?
C110 C115 H115 120.0 . . ?
O103 C116 H11A 109.5 . . ?
O103 C116 H11B 109.5 . . ?
H11A C116 H11B 109.5 . . ?
O103 C116 H11C 109.5 . . ?
H11A C116 H11C 109.5 . . ?
H11B C116 H11C 109.5 . . ?
O103 C117 C118 123.9(5) . . ?
O103 C117 C122 114.6(4) . . ?
C118 C117 C122 121.5(5) . . ?
C117 C118 C119 118.0(5) . . ?
C117 C118 H118 121.0 . . ?
C119 C118 H118 121.0 . . ?
C120 C119 C118 121.7(5) . . ?
C120 C119 Br4 119.0(4) . . ?
C118 C119 Br4 119.3(4) . . ?
C119 C120 C121 120.0(5) . . ?
C119 C120 H120 120.0 . . ?
C121 C120 H120 120.0 . . ?
C122 C121 C120 119.9(5) . . ?
C122 C121 C123 120.6(5) . . ?
C120 C121 C123 119.4(5) . . ?
O104 C122 C121 121.4(5) . . ?
O104 C122 C117 119.9(4) . . ?
C121 C122 C117 118.7(4) . . ?
N102 C123 C121 112.1(5) . . ?
N102 C123 H12A 109.2 . . ?
C121 C123 H12A 109.2 . . ?
N102 C123 H12B 109.2 . . ?
C121 C123 H12B 109.2 . . ?
H12A C123 H12B 107.9 . . ?
N102 C124 C125 113.9(5) . . ?
N102 C124 H12C 108.8 . . ?
C125 C124 H12C 108.8 . . ?
N102 C124 H12D 108.8 . . ?
C125 C124 H12D 108.8 . . ?
H12C C124 H12D 107.7 . . ?
C126 C125 C130 117.7(5) . . ?
C126 C125 C124 121.4(5) . . ?
C130 C125 C124 120.9(5) . . ?
C125 C126 C127 121.2(6) . . ?
C125 C126 H126 119.4 . . ?
C127 C126 H126 119.4 . . ?
C126 C127 C128 120.1(6) . . ?
C126 C127 H127 119.9 . . ?
C128 C127 H127 119.9 . . ?
C129 C128 C127 119.2(5) . . ?
C129 C128 H128 120.4 . . ?
C127 C128 H128 120.4 . . ?
C130 C129 C128 120.4(6) . . ?
C130 C129 H129 119.8 . . ?
C128 C129 H129 119.8 . . ?
C129 C130 C125 121.2(6) . . ?
C129 C130 H130 119.4 . . ?
C125 C130 H130 119.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 O1 C2 C3 -10.0(7) . . . . ?
Ni2 O1 C2 C3 -171.2(4) . . . . ?
C1 O1 C2 C7 168.3(4) . . . . ?
Ni2 O1 C2 C7 7.1(5) . . . . ?
O1 C2 C3 C4 177.5(4) . . . . ?
C7 C2 C3 C4 -0.7(7) . . . . ?
C2 C3 C4 C5 -2.8(7) . . . . ?
C2 C3 C4 Br1 177.8(3) . . . . ?
C3 C4 C5 C6 2.1(8) . . . . ?
Br1 C4 C5 C6 -178.5(4) . . . . ?
O8 N3 O6 Ni1 -179.9(4) . . . . ?
O7 N3 O6 Ni1 1.9(4) . . . . ?
C4 C5 C6 C7 2.2(7) . . . . ?
C4 C5 C6 C8 -170.7(4) . . . . ?
O8 N3 O7 Ni1 179.9(4) . . . . ?
O6 N3 O7 Ni1 -1.9(4) . . . . ?
Ni1 O2 C7 C6 -3.5(7) . . . . ?
Ni2 O2 C7 C6 162.1(4) . . . . ?
Ni1 O2 C7 C2 179.8(3) . . . . ?
Ni2 O2 C7 C2 -14.6(5) . . . . ?
C5 C6 C7 O2 177.9(4) . . . . ?
C8 C6 C7 O2 -9.1(7) . . . . ?
C5 C6 C7 C2 -5.4(7) . . . . ?
C8 C6 C7 C2 167.6(4) . . . . ?
C3 C2 C7 O2 -178.4(4) . . . . ?
O1 C2 C7 O2 3.3(6) . . . . ?
C3 C2 C7 C6 4.8(7) . . . . ?
O1 C2 C7 C6 -173.6(4) . . . . ?
C9 N1 C8 C6 68.7(5) . . . . ?
Ni1 N1 C8 C6 -66.0(5) . . . . ?
C5 C6 C8 N1 -138.2(5) . . . . ?
C7 C6 C8 N1 48.9(6) . . . . ?
C8 N1 C9 C10 59.3(6) . . . . ?
Ni1 N1 C9 C10 -170.3(4) . . . . ?
N1 C9 C10 C11 -100.0(6) . . . . ?
N1 C9 C10 C15 77.0(6) . . . . ?
C15 C10 C11 C12 0.3(8) . . . . ?
C9 C10 C11 C12 177.3(5) . . . . ?
C10 C11 C12 C13 0.2(9) . . . . ?
C11 C12 C13 C14 -0.9(8) . . . . ?
C12 C13 C14 C15 1.1(8) . . . . ?
C13 C14 C15 C10 -0.6(8) . . . . ?
C11 C10 C15 C14 -0.1(7) . . . . ?
C9 C10 C15 C14 -177.2(5) . . . . ?
C16 O3 C17 C18 -4.7(8) . . . . ?
C16 O3 C17 C22 176.9(5) . . . . ?
O3 C17 C18 C19 178.4(5) . . . . ?
C22 C17 C18 C19 -3.3(9) . . . . ?
C17 C18 C19 C20 1.0(9) . . . . ?
C17 C18 C19 Br2 178.4(4) . . . . ?
C18 C19 C20 C21 0.4(9) . . . . ?
Br2 C19 C20 C21 -177.0(4) . . . . ?
C19 C20 C21 C22 0.5(8) . . . . ?
C19 C20 C21 C23 177.4(5) . . . . ?
Ni2 O4 C22 C21 32.9(7) . . . . ?
Ni1 O4 C22 C21 -140.3(4) 2_665 . . . ?
Ni2 O4 C22 C17 -147.2(4) . . . . ?
Ni1 O4 C22 C17 39.6(8) 2_665 . . . ?
C20 C21 C22 O4 177.2(5) . . . . ?
C23 C21 C22 O4 0.4(8) . . . . ?
C20 C21 C22 C17 -2.6(8) . . . . ?
C23 C21 C22 C17 -179.5(5) . . . . ?
O3 C17 C22 O4 2.7(7) . . . . ?
C18 C17 C22 O4 -175.8(5) . . . . ?
O3 C17 C22 C21 -177.4(5) . . . . ?
C18 C17 C22 C21 4.1(8) . . . . ?
C24 N2 C23 C21 -63.6(5) . . . . ?
Ni2 N2 C23 C21 70.2(4) . . . . ?
C22 C21 C23 N2 -58.2(6) . . . . ?
C20 C21 C23 N2 124.9(5) . . . . ?
C23 N2 C24 C25 -58.8(6) . . . . ?
Ni2 N2 C24 C25 173.2(3) . . . . ?
N2 C24 C25 C30 -64.8(7) . . . . ?
N2 C24 C25 C26 114.5(6) . . . . ?
C30 C25 C26 C27 0.8(10) . . . . ?
C24 C25 C26 C27 -178.6(6) . . . . ?
C25 C26 C27 C28 -1.6(11) . . . . ?
C26 C27 C28 C29 2.2(13) . . . . ?
C27 C28 C29 C30 -1.9(12) . . . . ?
C26 C25 C30 C29 -0.6(10) . . . . ?
C24 C25 C30 C29 178.8(6) . . . . ?
C28 C29 C30 C25 1.1(11) . . . . ?
C101 O101 C102 C103 10.9(7) . . . . ?
Ni4 O101 C102 C103 173.3(4) . . . . ?
C101 O101 C102 C107 -166.3(4) . . . . ?
Ni4 O101 C102 C107 -3.9(5) . . . . ?
O101 C102 C103 C104 -176.7(5) . . . . ?
C107 C102 C103 C104 0.2(8) . . . . ?
C102 C103 C104 C105 3.1(8) . . . . ?
C102 C103 C104 Br3 -179.1(4) . . . . ?
C103 C104 C105 C106 -2.7(8) . . . . ?
Br3 C104 C105 C106 179.5(4) . . . . ?
O108 N103 O106 Ni3 176.0(4) . . . . ?
O107 N103 O106 Ni3 -3.4(4) . . . . ?
C104 C105 C106 C107 -1.0(8) . . . . ?
C104 C105 C106 C108 171.0(5) . . . . ?
O108 N103 O107 Ni3 -176.0(4) . . . . ?
O106 N103 O107 Ni3 3.4(4) . . . . ?
Ni4 O102 C107 C106 -165.7(4) . . . . ?
Ni3 O102 C107 C106 5.7(7) . . . . ?
Ni4 O102 C107 C102 11.6(6) . . . . ?
Ni3 O102 C107 C102 -177.0(3) . . . . ?
C105 C106 C107 O102 -178.7(5) . . . . ?
C108 C106 C107 O102 9.3(7) . . . . ?
C105 C106 C107 C102 4.0(7) . . . . ?
C108 C106 C107 C102 -168.0(5) . . . . ?
C103 C102 C107 O102 178.8(5) . . . . ?
O101 C102 C107 O102 -3.9(6) . . . . ?
C103 C102 C107 C106 -3.7(8) . . . . ?
O101 C102 C107 C106 173.5(4) . . . . ?
C109 N101 C108 C106 -69.2(5) . . . . ?
Ni3 N101 C108 C106 65.3(5) . . . . ?
C107 C106 C108 N101 -49.1(6) . . . . ?
C105 C106 C108 N101 138.9(5) . . . . ?
C108 N101 C109 C110 -57.4(6) . . . . ?
Ni3 N101 C109 C110 171.8(4) . . . . ?
N101 C109 C110 C111 106.8(6) . . . . ?
N101 C109 C110 C115 -70.5(7) . . . . ?
C115 C110 C111 C112 0.9(8) . . . . ?
C109 C110 C111 C112 -176.4(5) . . . . ?
C110 C111 C112 C113 0.5(9) . . . . ?
C111 C112 C113 C114 -1.5(9) . . . . ?
C112 C113 C114 C115 1.2(9) . . . . ?
C113 C114 C115 C110 0.1(9) . . . . ?
C111 C110 C115 C114 -1.2(8) . . . . ?
C109 C110 C115 C114 176.2(5) . . . . ?
C116 O103 C117 C118 6.5(8) . . . . ?
C116 O103 C117 C122 -174.9(5) . . . . ?
O103 C117 C118 C119 -179.0(5) . . . . ?
C122 C117 C118 C119 2.6(8) . . . . ?
C117 C118 C119 C120 1.0(8) . . . . ?
C117 C118 C119 Br4 -178.9(4) . . . . ?
C118 C119 C120 C121 -3.1(9) . . . . ?
Br4 C119 C120 C121 176.9(4) . . . . ?
C119 C120 C121 C122 1.6(8) . . . . ?
C119 C120 C121 C123 -174.9(5) . . . . ?
Ni4 O104 C122 C121 -33.4(7) . . . . ?
Ni3 O104 C122 C121 146.2(4) 2_566 . . . ?
Ni4 O104 C122 C117 145.2(4) . . . . ?
Ni3 O104 C122 C117 -35.2(8) 2_566 . . . ?
C120 C121 C122 O104 -179.5(5) . . . . ?
C123 C121 C122 O104 -3.0(8) . . . . ?
C120 C121 C122 C117 1.8(8) . . . . ?
C123 C121 C122 C117 178.4(5) . . . . ?
O103 C117 C122 O104 -1.2(7) . . . . ?
C118 C117 C122 O104 177.3(5) . . . . ?
O103 C117 C122 C121 177.4(5) . . . . ?
C118 C117 C122 C121 -4.0(8) . . . . ?
C124 N102 C123 C121 64.4(6) . . . . ?
Ni4 N102 C123 C121 -68.9(5) . . . . ?
C122 C121 C123 N102 61.4(7) . . . . ?
C120 C121 C123 N102 -122.1(5) . . . . ?
C123 N102 C124 C125 50.1(6) . . . . ?
Ni4 N102 C124 C125 178.2(3) . . . . ?
N102 C124 C125 C126 -122.7(6) . . . . ?
N102 C124 C125 C130 55.5(7) . . . . ?
C130 C125 C126 C127 1.4(9) . . . . ?
C124 C125 C126 C127 179.7(5) . . . . ?
C125 C126 C127 C128 -1.6(9) . . . . ?
C126 C127 C128 C129 1.0(10) . . . . ?
C127 C128 C129 C130 -0.3(10) . . . . ?
C128 C129 C130 C125 0.1(10) . . . . ?
C126 C125 C130 C129 -0.7(9) . . . . ?
C124 C125 C130 C129 -179.0(6) . . . . ?

_refine_diff_density_max         2.247
_refine_diff_density_min         -1.360
_refine_diff_density_rms         0.236


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

data_lfj-jd1a
_database_code_depnum_ccdc_archive 'CCDC 1874843'
_audit_update_record             
;
2018-12-12 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Co4]-(6)'
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H70 N4 O13 Co4 (N2 O6 H2 O)'
_chemical_formula_sum            'C60 H70 Co4 N6 O19'
_chemical_formula_weight         1414.94

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

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

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

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

_cell_length_a                   9.0455(6)
_cell_length_b                   12.6133(9)
_cell_length_c                   14.4430(10)
_cell_angle_alpha                92.607(6)
_cell_angle_beta                 104.914(6)
_cell_angle_gamma                103.757(6)
_cell_volume                     1536.64(19)
_cell_formula_units_Z            1
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    19357
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      25.35

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    1.139
_shelx_estimated_absorpt_T_min   0.463
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89266
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker B4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16789
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.349
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5605
_reflns_number_gt                4238
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

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

_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_structure_solution    
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0319P)²+1.4152P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5605
_refine_ls_number_parameters     460
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.0968
_refine_ls_wR_factor_gt          0.0865
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co -0.05996(5) 0.93059(4) -0.19261(3) 0.01898(13) Uani 1 1 d . . . . .
O1 O 0.1048(2) 0.99208(17) -0.05161(14) 0.0207(5) Uani 1 1 d . . . . .
H1 H 0.219142 1.006161 -0.042684 0.025 Uiso 1 1 calc R U . . .
N1 N -0.1594(3) 0.7506(2) 0.07578(19) 0.0209(6) Uani 1 1 d . . . . .
C1 C 0.0010(5) 0.7002(4) -0.3338(3) 0.0478(11) Uani 1 1 d . . . . .
H1B H 0.075862 0.657839 -0.311725 0.072 Uiso 1 1 calc R U . . .
H1C H 0.048926 0.761676 -0.362400 0.072 Uiso 1 1 calc R U . . .
H1D H -0.090395 0.655007 -0.380825 0.072 Uiso 1 1 calc R U . . .
Co2 Co -0.00628(5) 0.88051(3) 0.02436(3) 0.01783(13) Uani 1 1 d . . . . .
O2 O -0.1389(3) 0.81658(17) -0.11282(15) 0.0239(5) Uani 1 1 d . . . . .
N2 N -0.2497(3) 0.8944(2) -0.32363(19) 0.0208(6) Uani 1 1 d . . . . .
C2 C -0.1278(4) 0.6612(3) -0.2085(2) 0.0244(8) Uani 1 1 d . . . . .
H2 H -0.214(4) 0.864(3) -0.365(2) 0.019(9) Uiso 1 1 d . . . . .
H6A H 0.120(4) 0.992(3) -0.307(3) 0.046(13) Uiso 1 1 d . . . . .
O3 O -0.0457(3) 0.7390(2) -0.25392(16) 0.0308(6) Uani 1 1 d . . . . .
N3 N 0.4573(6) 0.9525(5) -0.0790(5) 0.0356(15) Uani 0.5 1 d D . P A -1
C3 C -0.1630(4) 0.5490(3) -0.2306(2) 0.0298(8) Uani 1 1 d . . . . .
H3 H -0.129734 0.519429 -0.279365 0.036 Uiso 1 1 calc R U . . .
O4 O -0.1211(2) 1.06750(17) -0.16236(15) 0.0221(5) Uani 1 1 d . . . . .
N4 N 0.004(2) 1.0182(9) -0.4938(8) 0.038(3) Uani 0.5 1 d D . P B -1
C4 C -0.2481(4) 0.4807(3) -0.1797(3) 0.0335(9) Uani 1 1 d . . . . .
H4 H -0.273856 0.404977 -0.195103 0.040 Uiso 1 1 calc R U . . .
O5 O -0.2045(2) 1.19444(18) -0.04960(15) 0.0239(5) Uani 1 1 d . . . . .
C5 C -0.2954(4) 0.5243(3) -0.1059(2) 0.0284(8) Uani 1 1 d . . . . .
H5 H -0.352510 0.477370 -0.072122 0.034 Uiso 1 1 calc R U . . .
O6 O 0.1227(3) 0.9850(3) -0.2492(2) 0.0404(7) Uani 1 1 d . . . . .
C6 C -0.2586(4) 0.6377(3) -0.0813(2) 0.0220(7) Uani 1 1 d . . . . .
O7 O 0.384(2) 0.9242(16) -0.1621(8) 0.091(6) Uani 0.5 1 d D . P A -1
C7 C -0.1754(4) 0.7066(3) -0.1335(2) 0.0216(7) Uani 1 1 d . . . . .
O8 O 0.5698(6) 0.9135(5) -0.0410(5) 0.0514(16) Uani 0.5 1 d D . P A -1
C8 C -0.3036(4) 0.6888(3) -0.0008(2) 0.0236(8) Uani 1 1 d . . . . .
H8A H -0.367548 0.738404 -0.025652 0.028 Uiso 1 1 calc R U . . .
H8B H -0.366447 0.631930 0.026518 0.028 Uiso 1 1 calc R U . . .
O9 O 0.4300(6) 1.0303(4) -0.0336(4) 0.0349(12) Uani 0.5 1 d D . P A -1
C9 C -0.0785(4) 0.6758(3) 0.1345(2) 0.0224(7) Uani 1 1 d . . . . .
H9A H 0.025390 0.718291 0.172718 0.027 Uiso 1 1 calc R U . . .
H9B H -0.063102 0.620971 0.091203 0.027 Uiso 1 1 calc R U . . .
O10 O -0.0741(8) 0.9214(5) -0.4996(6) 0.0478(17) Uani 0.5 1 d D . P B -1
C10 C -0.1663(4) 0.6178(3) 0.2014(2) 0.0227(7) Uani 1 1 d . . . . .
O11 O -0.0099(8) 1.0727(5) -0.5641(4) 0.0453(15) Uani 0.5 1 d D . P B -1
C11 C -0.2456(4) 0.5072(3) 0.1822(3) 0.0354(9) Uani 1 1 d . . . . .
H11 H -0.246850 0.467337 0.126124 0.042 Uiso 1 1 calc R U . . .
O12 O 0.1008(6) 1.0663(5) -0.4166(4) 0.0554(17) Uani 0.5 1 d D . P B -1
C12 C -0.3235(5) 0.4553(4) 0.2457(4) 0.0523(12) Uani 1 1 d . . . . .
H12 H -0.376550 0.381115 0.232013 0.063 Uiso 1 1 calc R U . . .
C13 C -0.3216(5) 0.5138(5) 0.3284(4) 0.0590(14) Uani 1 1 d . . . . .
H13 H -0.373040 0.479088 0.371202 0.071 Uiso 1 1 calc R U . . .
C14 C -0.2439(5) 0.6238(5) 0.3486(3) 0.0563(13) Uani 1 1 d . . . . .
H14 H -0.243083 0.663290 0.404809 0.068 Uiso 1 1 calc R U . . .
C15 C -0.1669(4) 0.6757(3) 0.2849(3) 0.0345(9) Uani 1 1 d . . . . .
H15 H -0.115177 0.750075 0.298576 0.041 Uiso 1 1 calc R U . . .
C16 C -0.2426(4) 1.2648(3) 0.0156(2) 0.0343(9) Uani 1 1 d . . . . .
H16A H -0.232688 1.336392 -0.006036 0.051 Uiso 1 1 calc R U . . .
H16B H -0.171419 1.270576 0.078743 0.051 Uiso 1 1 calc R U . . .
H16C H -0.349426 1.234981 0.017959 0.051 Uiso 1 1 calc R U . . .
C17 C -0.3072(4) 1.1633(3) -0.1418(2) 0.0201(7) Uani 1 1 d . . . . .
C18 C -0.4450(4) 1.1953(3) -0.1766(2) 0.0261(8) Uani 1 1 d . . . . .
H18 H -0.477209 1.240370 -0.137272 0.031 Uiso 1 1 calc R U . . .
C19 C -0.5352(4) 1.1591(3) -0.2715(2) 0.0279(8) Uani 1 1 d . . . . .
H19 H -0.628606 1.179755 -0.295764 0.034 Uiso 1 1 calc R U . . .
C20 C -0.4864(4) 1.0928(3) -0.3296(2) 0.0275(8) Uani 1 1 d . . . . .
H20 H -0.547974 1.068973 -0.392658 0.033 Uiso 1 1 calc R U . . .
C21 C -0.3462(4) 1.0604(3) -0.2957(2) 0.0240(8) Uani 1 1 d . . . . .
C22 C -0.2570(3) 1.0955(3) -0.2002(2) 0.0203(7) Uani 1 1 d . . . . .
C23 C -0.2850(4) 0.9960(3) -0.3609(2) 0.0254(8) Uani 1 1 d . . . . .
H23A H -0.362992 0.976256 -0.423335 0.030 Uiso 1 1 calc R U . . .
H23B H -0.189234 1.042593 -0.370422 0.030 Uiso 1 1 calc R U . . .
C24 C -0.3938(4) 0.8129(3) -0.3152(2) 0.0248(8) Uani 1 1 d . . . . .
H24A H -0.439088 0.846276 -0.271177 0.030 Uiso 1 1 calc R U . . .
H24B H -0.362408 0.750470 -0.287220 0.030 Uiso 1 1 calc R U . . .
C25 C -0.5202(4) 0.7720(3) -0.4099(2) 0.0227(7) Uani 1 1 d . . . . .
C26 C -0.6625(4) 0.8014(3) -0.4298(2) 0.0270(8) Uani 1 1 d . . . . .
H26 H -0.679891 0.849049 -0.385157 0.032 Uiso 1 1 calc R U . . .
C27 C -0.7789(4) 0.7606(3) -0.5155(2) 0.0266(8) Uani 1 1 d . . . . .
H27 H -0.874070 0.780696 -0.527965 0.032 Uiso 1 1 calc R U . . .
C28 C -0.7538(4) 0.6902(3) -0.5826(2) 0.0306(9) Uani 1 1 d . . . . .
H28 H -0.831686 0.662930 -0.640237 0.037 Uiso 1 1 calc R U . . .
C29 C -0.6124(4) 0.6604(3) -0.5635(2) 0.0311(9) Uani 1 1 d . . . . .
H29 H -0.595254 0.612971 -0.608457 0.037 Uiso 1 1 calc R U . . .
C30 C -0.4960(4) 0.7010(3) -0.4778(2) 0.0279(8) Uani 1 1 d . . . . .
H30 H -0.401070 0.680578 -0.465480 0.033 Uiso 1 1 calc R U . . .
H1A H -0.188(4) 0.787(3) 0.111(2) 0.018(9) Uiso 1 1 d . . . . .
O7A O 0.6150(11) 1.0803(10) 0.1634(5) 0.022(3) Uani 0.5 1 d . . P C -1
H6B H 0.204(6) 0.962(4) -0.223(4) 0.084(19) 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
Co1 O4 1.997(2) . ?
Co1 O2 1.998(2) . ?
Co1 O6 2.019(3) . ?
Co1 N2 2.148(3) . ?
Co1 O1 2.171(2) . ?
O1 Co2 2.056(2) . ?
O1 Co2 2.082(2) 2_575 ?
O1 H1 0.9800 . ?
N1 C9 1.492(4) . ?
N1 C8 1.493(4) . ?
N1 Co2 2.172(3) . ?
N1 H1A 0.80(3) . ?
C1 O3 1.431(4) . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1 H1D 0.9600 . ?
Co2 O4 2.017(2) 2_575 ?
Co2 O2 2.046(2) . ?
Co2 O5 2.279(2) 2_575 ?
O2 C7 1.348(4) . ?
N2 C23 1.484(4) . ?
N2 C24 1.492(4) . ?
N2 H2 0.87(3) . ?
C2 C3 1.377(5) . ?
C2 O3 1.381(4) . ?
C2 C7 1.411(4) . ?
N3 O7 1.202(9) . ?
N3 O8 1.247(6) . ?
N3 O9 1.262(6) . ?
C3 C4 1.382(5) . ?
C3 H3 0.9300 . ?
O4 C22 1.347(4) . ?
N4 O10 1.245(9) . ?
N4 O12 1.248(9) . ?
N4 O11 1.249(9) . ?
C4 C5 1.384(5) . ?
C4 H4 0.9300 . ?
O5 C17 1.390(4) . ?
O5 C16 1.425(4) . ?
C5 C6 1.397(5) . ?
C5 H5 0.9300 . ?
O6 H6A 0.83(4) . ?
O6 H6B 0.86(5) . ?
C6 C7 1.389(5) . ?
C6 C8 1.493(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.510(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C15 1.384(5) . ?
C10 C11 1.386(5) . ?
C11 C12 1.391(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.370(6) . ?
C12 H12 0.9300 . ?
C13 C14 1.378(7) . ?
C13 H13 0.9300 . ?
C14 C15 1.388(6) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 C18 1.380(4) . ?
C17 C22 1.402(4) . ?
C18 C19 1.395(5) . ?
C18 H18 0.9300 . ?
C19 C20 1.378(5) . ?
C19 H19 0.9300 . ?
C20 C21 1.399(4) . ?
C20 H20 0.9300 . ?
C21 C22 1.396(4) . ?
C21 C23 1.507(5) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.515(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.386(4) . ?
C25 C30 1.391(4) . ?
C26 C27 1.386(4) . ?
C26 H26 0.9300 . ?
C27 C28 1.382(5) . ?
C27 H27 0.9300 . ?
C28 C29 1.382(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.385(4) . ?
C29 H29 0.9300 . ?
C30 H30 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
O4 Co1 O2 108.99(9) . . ?
O4 Co1 O6 103.26(11) . . ?
O2 Co1 O6 141.51(12) . . ?
O4 Co1 N2 89.22(10) . . ?
O2 Co1 N2 102.12(9) . . ?
O6 Co1 N2 98.71(11) . . ?
O4 Co1 O1 78.80(8) . . ?
O2 Co1 O1 78.93(8) . . ?
O6 Co1 O1 87.45(10) . . ?
N2 Co1 O1 167.54(10) . . ?
Co2 O1 Co2 97.39(9) . 2_575 ?
Co2 O1 Co1 96.78(8) . . ?
Co2 O1 Co1 95.95(8) 2_575 . ?
Co2 O1 H1 120.4 . . ?
Co2 O1 H1 120.4 2_575 . ?
Co1 O1 H1 120.4 . . ?
C9 N1 C8 112.2(3) . . ?
C9 N1 Co2 115.50(19) . . ?
C8 N1 Co2 113.6(2) . . ?
C9 N1 H1A 108(2) . . ?
C8 N1 H1A 107(2) . . ?
Co2 N1 H1A 100(2) . . ?
O3 C1 H1B 109.5 . . ?
O3 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O3 C1 H1D 109.5 . . ?
H1B C1 H1D 109.5 . . ?
H1C C1 H1D 109.5 . . ?
O4 Co2 O2 175.88(9) 2_575 . ?
O4 Co2 O1 103.01(9) 2_575 . ?
O2 Co2 O1 80.59(8) . . ?
O4 Co2 O1 80.49(8) 2_575 2_575 ?
O2 Co2 O1 102.09(8) . 2_575 ?
O1 Co2 O1 82.61(9) . 2_575 ?
O4 Co2 N1 88.80(9) 2_575 . ?
O2 Co2 N1 87.66(9) . . ?
O1 Co2 N1 168.10(9) . . ?
O1 Co2 N1 98.14(10) 2_575 . ?
O4 Co2 O5 74.18(8) 2_575 2_575 ?
O2 Co2 O5 104.14(8) . 2_575 ?
O1 Co2 O5 88.21(8) . 2_575 ?
O1 Co2 O5 150.33(8) 2_575 2_575 ?
N1 Co2 O5 96.54(10) . 2_575 ?
C7 O2 Co1 127.38(19) . . ?
C7 O2 Co2 116.96(18) . . ?
Co1 O2 Co2 102.85(9) . . ?
C23 N2 C24 112.6(3) . . ?
C23 N2 Co1 111.64(18) . . ?
C24 N2 Co1 112.93(19) . . ?
C23 N2 H2 107(2) . . ?
C24 N2 H2 107(2) . . ?
Co1 N2 H2 105(2) . . ?
C3 C2 O3 125.8(3) . . ?
C3 C2 C7 120.6(3) . . ?
O3 C2 C7 113.6(3) . . ?
C2 O3 C1 117.3(3) . . ?
O7 N3 O8 120.4(12) . . ?
O7 N3 O9 119.2(11) . . ?
O8 N3 O9 120.0(6) . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C22 O4 Co1 129.15(18) . . ?
C22 O4 Co2 121.08(18) . 2_575 ?
Co1 O4 Co2 103.85(9) . 2_575 ?
O10 N4 O12 121.4(9) . . ?
O10 N4 O11 122.1(9) . . ?
O12 N4 O11 116.5(8) . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C17 O5 C16 118.3(2) . . ?
C17 O5 Co2 112.78(18) . 2_575 ?
C16 O5 Co2 128.87(18) . 2_575 ?
C4 C5 C6 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
Co1 O6 H6A 128(3) . . ?
Co1 O6 H6B 113(3) . . ?
H6A O6 H6B 108(4) . . ?
C7 C6 C5 118.7(3) . . ?
C7 C6 C8 118.3(3) . . ?
C5 C6 C8 123.1(3) . . ?
O2 C7 C6 120.6(3) . . ?
O2 C7 C2 119.6(3) . . ?
C6 C7 C2 119.8(3) . . ?
N1 C8 C6 110.6(3) . . ?
N1 C8 H8A 109.5 . . ?
C6 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
N1 C9 C10 114.6(3) . . ?
N1 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N1 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C15 C10 C11 118.6(3) . . ?
C15 C10 C9 119.4(3) . . ?
C11 C10 C9 122.0(3) . . ?
C10 C11 C12 120.9(4) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C13 C12 C11 119.7(4) . . ?
C13 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
C12 C13 C14 120.3(4) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C13 C14 C15 119.9(4) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C10 C15 C14 120.6(4) . . ?
C10 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
O5 C16 H16A 109.5 . . ?
O5 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O5 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 O5 125.3(3) . . ?
C18 C17 C22 121.1(3) . . ?
O5 C17 C22 113.5(3) . . ?
C17 C18 C19 119.0(3) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C20 C19 C18 120.2(3) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C19 C20 C21 121.5(3) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 118.3(3) . . ?
C22 C21 C23 119.8(3) . . ?
C20 C21 C23 121.8(3) . . ?
O4 C22 C21 121.7(3) . . ?
O4 C22 C17 118.4(3) . . ?
C21 C22 C17 119.8(3) . . ?
N2 C23 C21 113.9(3) . . ?
N2 C23 H23A 108.8 . . ?
C21 C23 H23A 108.8 . . ?
N2 C23 H23B 108.8 . . ?
C21 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
N2 C24 C25 114.3(3) . . ?
N2 C24 H24A 108.7 . . ?
C25 C24 H24A 108.7 . . ?
N2 C24 H24B 108.7 . . ?
C25 C24 H24B 108.7 . . ?
H24A C24 H24B 107.6 . . ?
C26 C25 C30 118.8(3) . . ?
C26 C25 C24 121.4(3) . . ?
C30 C25 C24 119.7(3) . . ?
C27 C26 C25 120.8(3) . . ?
C27 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
C28 C27 C26 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 119.7(3) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C28 C29 C30 120.4(3) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C25 120.3(3) . . ?
C29 C30 H30 119.8 . . ?
C25 C30 H30 119.8 . . ?

_refine_diff_density_max         0.527
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.081


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

data_co7sq
_database_code_depnum_ccdc_archive 'CCDC 1874844'
_audit_update_record             
;
2018-12-18 deposited with the CCDC.
2018-12-20 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            '[Co7]'
_chemical_melting_point          ?
_chemical_formula_moiety         'C93 H93 N6 O18 Co7 (N2 O6) (C4 H17 O4.5)'
_chemical_formula_sum            'C97 H110 Co7 N8 O28.50'
_chemical_formula_weight         2256.48

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

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

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

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

_cell_length_a                   19.8705(5)
_cell_length_b                   22.1327(4)
_cell_length_c                   23.1956(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.902(2)
_cell_angle_gamma                90
_cell_volume                     10163.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    19171
_cell_measurement_theta_min      2.7510
_cell_measurement_theta_max      27.3770

_exptl_crystal_description       Parallelepiped
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             4120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    1.177
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
crysalispro 1.171.39.9g (rigaku oxford diffraction, 2015) 
empirical absorption correction using spherical harmonics, 
 implemented in scale3 abspack scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed x-ray tube'
_diffrn_measurement_device_type  'xtalab afc12 (rcd3): kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            119343
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.691
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             23280
_reflns_number_gt                19834
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_cell_refinement       'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_data_reduction        'crysalispro 1.171.39.9g (rigaku od, 2015)'
_computing_structure_solution    
'SHELXT - G.M.Sheldrick,Acta Crystallogr.A71(2015)3-8.'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEX - P. McArdle, J.Appl.Cryst.,1995,28,65-65.'
_computing_publication_material  
'Oscail - P. McArdle, J.Appl.Cryst.,2017,50,320-326.'
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0652P)²+129.0328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         23280
_refine_ls_number_parameters     1133
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1906
_refine_ls_R_factor_gt           0.1737
_refine_ls_wR_factor_ref         0.3316
_refine_ls_wR_factor_gt          0.3229
_refine_ls_goodness_of_fit_ref   1.335
_refine_ls_restrained_S_all      1.335
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.500000 0.500000 0.500000 0.0361(5) Uani 1 2 d S . P . .
O1 O 0.4576(4) 0.4316(3) 0.6403(3) 0.0407(18) Uani 1 1 d . . . . .
N1 N 0.5239(5) 0.5217(4) 0.7108(4) 0.045(2) Uani 1 1 d . . . . .
C1 C 0.4060(7) 0.2592(5) 0.6162(5) 0.049(3) Uani 1 1 d . . . . .
H1A H 0.442818 0.230101 0.613839 0.074 Uiso 1 1 calc R U . . .
H1B H 0.375390 0.257039 0.580846 0.074 Uiso 1 1 calc R U . . .
H1C H 0.381083 0.249725 0.649729 0.074 Uiso 1 1 calc R U . . .
Co2 Co 0.41533(8) 0.40417(6) 0.56107(6) 0.0384(4) Uani 1 1 d . . . . .
O2 O 0.4334(4) 0.3188(3) 0.6223(3) 0.048(2) Uani 1 1 d . . . . .
N2 N 0.3141(5) 0.3931(4) 0.5745(4) 0.045(2) Uani 1 1 d . . . . .
C2 C 0.4729(6) 0.3308(5) 0.6735(5) 0.040(3) Uani 1 1 d . . . . .
Co3 Co 0.48389(8) 0.37029(6) 0.44745(6) 0.0359(4) Uani 1 1 d . . . . .
O3 O 0.3973(4) 0.3579(3) 0.4883(3) 0.0373(17) Uani 1 1 d . . . . .
N3 N 0.5302(5) 0.2846(4) 0.4553(4) 0.043(2) Uani 1 1 d . . . . .
C3 C 0.4982(8) 0.2904(5) 0.7131(5) 0.060(4) Uani 1 1 d . . . . .
H3 H 0.488647 0.248583 0.707627 0.072 Uiso 1 1 calc R U . . .
Co4 Co 0.52807(9) 0.47985(6) 0.37125(6) 0.0414(4) Uani 1 1 d . . . . .
O4 O 0.4055(4) 0.3222(3) 0.3837(3) 0.0428(19) Uani 1 1 d . . . . .
N4 N -0.1570(4) -0.1274(4) 0.5901(3) 0.0346(19) Uani 1 1 d . . . . .
C4 C 0.5384(8) 0.3095(5) 0.7622(6) 0.059(4) Uani 1 1 d . . . . .
H4 H 0.556334 0.280936 0.789964 0.071 Uiso 1 1 calc R U . . .
Co5 Co 0.000000 0.000000 0.500000 0.0294(4) Uani 1 2 d S . P . .
O5 O 0.5480(4) 0.3901(3) 0.3881(3) 0.0450(19) Uani 1 1 d . . . . .
N5 N 0.0941(5) -0.2016(4) 0.4885(4) 0.042(2) Uani 1 1 d . . . . .
C5 C 0.5517(7) 0.3697(6) 0.7700(5) 0.055(3) Uani 1 1 d . . . . .
H5 H 0.579511 0.382429 0.803099 0.066 Uiso 1 1 calc R U . . .
Co6 Co -0.05887(7) -0.10037(5) 0.57528(5) 0.0318(3) Uani 1 1 d . . . . .
O6 O 0.6207(5) 0.4467(3) 0.3196(3) 0.057(2) Uani 1 1 d . . . . .
N6 N -0.0268(5) -0.0515(4) 0.2971(4) 0.037(2) Uani 1 1 d . . . . .
C6 C 0.5252(6) 0.4135(5) 0.7300(5) 0.048(3) Uani 1 1 d . . . . .
Co7 Co 0.02011(7) -0.13598(5) 0.46715(5) 0.0328(3) Uani 1 1 d . . . . .
O7 O 0.5116(4) 0.4078(3) 0.5250(3) 0.0424(19) Uani 1 1 d D . . . .
C7 C 0.4857(6) 0.3946(4) 0.6810(4) 0.038(3) Uani 1 1 d . . . . .
Co8 Co 0.03085(7) -0.03170(5) 0.37420(5) 0.0280(3) Uani 1 1 d . . . . .
O8 O 0.4149(4) 0.4962(3) 0.5491(3) 0.0428(19) Uani 1 1 d D . . . .
C8 C 0.5409(7) 0.4776(5) 0.7423(5) 0.049(3) Uani 1 1 d . . . . .
H8 H 0.566624 0.486175 0.777818 0.058 Uiso 1 1 calc R U . . .
O9 O 0.4539(4) 0.4621(3) 0.4237(3) 0.0433(19) Uani 1 1 d D . . . .
C9 C 0.5422(8) 0.5842(5) 0.7318(5) 0.059(4) Uani 1 1 d . . . . .
H9A H 0.501475 0.609868 0.725596 0.071 Uiso 1 1 calc R U . . .
H9B H 0.576263 0.600554 0.707171 0.071 Uiso 1 1 calc R U . . .
O10 O -0.0622(4) -0.1608(3) 0.5118(3) 0.0337(16) Uani 1 1 d . . . . .
C10 C 0.5697(7) 0.5905(5) 0.7942(5) 0.049(3) Uani 1 1 d . . . . .
O11 O -0.0405(4) -0.2077(3) 0.4135(3) 0.0414(18) Uani 1 1 d . . . . .
C11 C 0.6357(9) 0.6028(6) 0.8096(7) 0.070(4) Uani 1 1 d . . . . .
H11 H 0.666088 0.607817 0.780502 0.084 Uiso 1 1 calc R U . . .
O12 O 0.0756(3) -0.1106(3) 0.4027(3) 0.0304(15) Uani 1 1 d . . . . .
C12 C 0.6594(9) 0.6081(7) 0.8675(9) 0.087(5) Uani 1 1 d . . . . .
H12 H 0.705598 0.617305 0.877737 0.104 Uiso 1 1 calc R U . . .
O13 O 0.1290(4) -0.0440(3) 0.3282(3) 0.0375(17) Uani 1 1 d . . . . .
C13 C 0.6164(12) 0.6002(6) 0.9098(7) 0.084(6) Uani 1 1 d . . . . .
H13 H 0.632997 0.603013 0.949317 0.100 Uiso 1 1 calc R U . . .
O14 O 0.0237(4) 0.0540(3) 0.3521(3) 0.0331(16) Uani 1 1 d . . . . .
C14 C 0.5504(10) 0.5885(6) 0.8955(6) 0.065(4) Uani 1 1 d . . . . .
H14 H 0.520494 0.583741 0.924985 0.078 Uiso 1 1 calc R U . . .
O15 O 0.0276(4) 0.1700(3) 0.3520(3) 0.0407(18) Uani 1 1 d . . . . .
C15 C 0.5263(8) 0.5835(6) 0.8380(6) 0.061(4) Uani 1 1 d . . . . .
H15 H 0.479791 0.575152 0.828206 0.073 Uiso 1 1 calc R U . . .
O16 O -0.0808(3) -0.0146(3) 0.5497(3) 0.0311(15) Uani 1 1 d D . . . .
C16 C 0.4189(7) 0.2815(5) 0.3368(5) 0.051(3) Uani 1 1 d . . . . .
H16A H 0.408590 0.239928 0.347710 0.076 Uiso 1 1 calc R U . . .
H16B H 0.466573 0.284378 0.329327 0.076 Uiso 1 1 calc R U . . .
H16C H 0.390494 0.292722 0.301846 0.076 Uiso 1 1 calc R U . . .
O17 O 0.0356(4) -0.0827(3) 0.5378(3) 0.0392(18) Uani 1 1 d D . . . .
C17 C 0.3405(6) 0.3214(4) 0.4015(4) 0.043(3) Uani 1 1 d . . . . .
O18 O -0.0341(4) -0.0581(3) 0.4313(3) 0.0352(17) Uani 1 1 d D . . . .
C18 C 0.2849(7) 0.3038(6) 0.3697(5) 0.050(3) Uani 1 1 d . . . . .
H18 H 0.287964 0.288911 0.331580 0.060 Uiso 1 1 calc R U . . .
C19 C 0.2228(7) 0.3071(7) 0.3924(6) 0.066(4) Uani 1 1 d . . . . .
H19 H 0.183223 0.293701 0.370181 0.080 Uiso 1 1 calc R U . . .
C20 C 0.2185(7) 0.3299(6) 0.4470(5) 0.059(4) Uani 1 1 d . . . . .
H20 H 0.175448 0.332874 0.461630 0.071 Uiso 1 1 calc R U . . .
C21 C 0.2743(6) 0.3484(5) 0.4808(5) 0.046(3) Uani 1 1 d . . . . .
C22 C 0.3410(6) 0.3436(4) 0.4595(5) 0.043(3) Uani 1 1 d . . . . .
C23 C 0.2675(6) 0.3726(5) 0.5395(5) 0.044(3) Uani 1 1 d . . . . .
H23 H 0.223268 0.372676 0.552164 0.053 Uiso 1 1 calc R U . . .
C24 C 0.2967(7) 0.4181(6) 0.6320(5) 0.056(3) Uani 1 1 d . . . . .
H24A H 0.316321 0.459060 0.636619 0.067 Uiso 1 1 calc R U . . .
H24B H 0.318829 0.392470 0.663068 0.067 Uiso 1 1 calc R U . . .
C25 C 0.2219(7) 0.4220(5) 0.6408(5) 0.050(3) Uani 1 1 d . . . . .
C26 C 0.1920(6) 0.3801(5) 0.6730(4) 0.048(3) Uani 1 1 d . . . . .
H26 H 0.217763 0.347097 0.689061 0.058 Uiso 1 1 calc R U . . .
C27 C 0.1244(7) 0.3850(6) 0.6828(5) 0.061(4) Uani 1 1 d . . . . .
H27 H 0.104827 0.356192 0.706686 0.073 Uiso 1 1 calc R U . . .
C28 C 0.0851(9) 0.4314(9) 0.6579(7) 0.082(5) Uani 1 1 d . . . . .
H28 H 0.038105 0.433817 0.662575 0.099 Uiso 1 1 calc R U . . .
C29 C 0.1167(11) 0.4742(8) 0.6262(7) 0.091(6) Uani 1 1 d . . . . .
H29 H 0.091319 0.507331 0.609956 0.109 Uiso 1 1 calc R U . . .
C30 C 0.1828(9) 0.4696(6) 0.6179(6) 0.070(4) Uani 1 1 d . . . . .
H30 H 0.203108 0.499720 0.595817 0.084 Uiso 1 1 calc R U . . .
C31 C 0.6452(7) 0.4762(5) 0.2704(5) 0.056(4) Uani 1 1 d . . . . .
H31A H 0.694505 0.479161 0.275685 0.084 Uiso 1 1 calc R U . . .
H31B H 0.625698 0.516854 0.266465 0.084 Uiso 1 1 calc R U . . .
H31C H 0.631967 0.452810 0.235347 0.084 Uiso 1 1 calc R U . . .
C32 C 0.6397(8) 0.3878(5) 0.3310(6) 0.064(4) Uani 1 1 d . . . . .
C33 C 0.6929(8) 0.3578(6) 0.3081(8) 0.089(6) Uani 1 1 d . . . . .
H33 H 0.719526 0.377658 0.281734 0.106 Uiso 1 1 calc R U . . .
C34 C 0.7067(10) 0.2980(7) 0.3246(9) 0.109(8) Uani 1 1 d . . . . .
H34 H 0.742729 0.276904 0.309215 0.131 Uiso 1 1 calc R U . . .
C35 C 0.6682(8) 0.2698(7) 0.3631(8) 0.089(6) Uani 1 1 d . . . . .
H35 H 0.678061 0.229221 0.374210 0.107 Uiso 1 1 calc R U . . .
C36 C 0.6150(7) 0.2999(5) 0.3862(6) 0.059(4) Uani 1 1 d . . . . .
C37 C -0.1146(6) -0.1840(4) 0.4829(4) 0.034(2) Uani 1 1 d . . . . .
C38 C 0.5793(7) 0.2670(5) 0.4281(6) 0.056(3) Uani 1 1 d . . . . .
H38 H 0.594740 0.227064 0.436327 0.067 Uiso 1 1 calc R U . . .
C39 C 0.4999(6) 0.2430(5) 0.4964(5) 0.042(3) Uani 1 1 d . . . . .
H39A H 0.450567 0.241080 0.486006 0.050 Uiso 1 1 calc R U . . .
H39B H 0.507025 0.260267 0.535764 0.050 Uiso 1 1 calc R U . . .
C40 C 0.5278(6) 0.1789(5) 0.4978(5) 0.044(3) Uani 1 1 d . . . . .
C41 C 0.5834(7) 0.1626(5) 0.5333(6) 0.062(4) Uani 1 1 d . . . . .
H41 H 0.603852 0.191204 0.559913 0.075 Uiso 1 1 calc R U . . .
C42 C 0.6104(8) 0.1042(6) 0.5308(7) 0.074(4) Uani 1 1 d . . . . .
H42 H 0.649585 0.093389 0.555060 0.089 Uiso 1 1 calc R U . . .
C43 C 0.5802(9) 0.0632(6) 0.4936(6) 0.068(4) Uani 1 1 d . . . . .
H43 H 0.598373 0.023603 0.491889 0.082 Uiso 1 1 calc R U . . .
C44 C 0.5242(9) 0.0782(6) 0.4586(6) 0.069(4) Uani 1 1 d . . . . .
H44 H 0.503246 0.048991 0.432999 0.083 Uiso 1 1 calc R U . . .
C45 C 0.4975(7) 0.1366(5) 0.4605(5) 0.053(3) Uani 1 1 d . . . . .
H45 H 0.458466 0.147158 0.435976 0.063 Uiso 1 1 calc R U . . .
C46 C 0.5789(16) 0.3799(15) 0.5618(14) 0.080(9) Uiso 0.5 1 d D . P . .
H46A H 0.572052 0.336733 0.568681 0.120 Uiso 0.5 1 calc R U P . .
H46B H 0.586332 0.400983 0.598934 0.120 Uiso 0.5 1 calc R U P . .
H46C H 0.618299 0.385364 0.539682 0.120 Uiso 0.5 1 calc R U P . .
C47 C 0.3563(9) 0.5264(9) 0.5326(8) 0.030(4) Uiso 0.5 1 d D . P . .
H47A H 0.332726 0.505867 0.499320 0.045 Uiso 0.5 1 calc R U P . .
H47B H 0.366910 0.567907 0.521933 0.045 Uiso 0.5 1 calc R U P . .
H47C H 0.327415 0.526898 0.564785 0.045 Uiso 0.5 1 calc R U P . .
C48 C 0.3848(12) 0.4759(11) 0.4020(10) 0.047(6) Uiso 0.5 1 d D . P . .
H48A H 0.382172 0.517796 0.388390 0.071 Uiso 0.5 1 calc R U P . .
H48B H 0.354932 0.470461 0.433082 0.071 Uiso 0.5 1 calc R U P . .
H48C H 0.370797 0.448650 0.369873 0.071 Uiso 0.5 1 calc R U P . .
C49 C -0.0187(7) -0.2524(5) 0.3733(4) 0.049(3) Uani 1 1 d . . . . .
H49A H -0.030307 -0.292921 0.386421 0.074 Uiso 1 1 calc R U . . .
H49B H 0.030311 -0.249553 0.371604 0.074 Uiso 1 1 calc R U . . .
H49C H -0.041360 -0.245093 0.334736 0.074 Uiso 1 1 calc R U . . .
O50 O -0.1680(8) -0.0739(7) 0.3800(7) 0.047(4) Uiso 0.5 1 d . . P . .
C50 C -0.1065(6) -0.2121(4) 0.4285(4) 0.036(2) Uani 1 1 d . . . . .
C51 C -0.1570(6) -0.2379(5) 0.3961(4) 0.046(3) Uani 1 1 d . . . . .
H51 H -0.148656 -0.256711 0.360547 0.055 Uiso 1 1 calc R U . . .
C52 C -0.2219(7) -0.2375(6) 0.4141(5) 0.057(3) Uani 1 1 d . . . . .
H52 H -0.258383 -0.255419 0.391000 0.068 Uiso 1 1 calc R U . . .
C53 C -0.2325(6) -0.2104(6) 0.4663(5) 0.048(3) Uani 1 1 d . . . . .
H53 H -0.276799 -0.210215 0.478812 0.058 Uiso 1 1 calc R U . . .
C54 C -0.1814(6) -0.1839(4) 0.5006(4) 0.034(2) Uani 1 1 d . . . . .
C55 C 0.6002(7) 0.3581(5) 0.3706(5) 0.050(3) Uani 1 1 d . . . . .
C56 C -0.1957(5) -0.1568(4) 0.5566(4) 0.035(2) Uani 1 1 d . . . . .
H56 H -0.239930 -0.162918 0.568070 0.042 Uiso 1 1 calc R U . . .
C57 C -0.1799(7) -0.1053(7) 0.6453(5) 0.059(4) Uani 1 1 d . . . . .
H57A H -0.159186 -0.065221 0.653323 0.071 Uiso 1 1 calc R U . . .
H57B H -0.161480 -0.132918 0.676345 0.071 Uiso 1 1 calc R U . . .
C58 C -0.2539(6) -0.0994(4) 0.6503(4) 0.039(2) Uani 1 1 d . . . . .
C59 C -0.2916(7) -0.0527(5) 0.6226(5) 0.049(3) Uani 1 1 d . . . . .
H59 H -0.270001 -0.025449 0.598506 0.059 Uiso 1 1 calc R U . . .
C60 C -0.3572(8) -0.0456(7) 0.6292(7) 0.071(4) Uani 1 1 d . . . . .
H60 H -0.381339 -0.013842 0.609183 0.086 Uiso 1 1 calc R U . . .
C61 C -0.3906(7) -0.0834(7) 0.6644(6) 0.067(4) Uani 1 1 d . . . . .
H61 H -0.437370 -0.078324 0.668617 0.080 Uiso 1 1 calc R U . . .
C62 C -0.3545(7) -0.1283(6) 0.6928(5) 0.058(4) Uani 1 1 d . . . . .
H62 H -0.376464 -0.154166 0.718017 0.070 Uiso 1 1 calc R U . . .
C63 C -0.2877(6) -0.1370(4) 0.6861(4) 0.037(2) Uani 1 1 d . . . . .
H63 H -0.264104 -0.169000 0.706166 0.045 Uiso 1 1 calc R U . . .
C64 C 0.1399(6) -0.0210(5) 0.2714(4) 0.036(2) Uani 1 1 d . . . . .
H64A H 0.182067 0.002176 0.273485 0.054 Uiso 1 1 calc R U . . .
H64B H 0.102147 0.005325 0.257732 0.054 Uiso 1 1 calc R U . . .
H64C H 0.142829 -0.054794 0.244471 0.054 Uiso 1 1 calc R U . . .
C65 C 0.1679(5) -0.0904(4) 0.3499(4) 0.030(2) Uani 1 1 d . . . . .
C66 C 0.2306(6) -0.1054(5) 0.3335(5) 0.049(3) Uani 1 1 d . . . . .
H66 H 0.250319 -0.082126 0.304861 0.059 Uiso 1 1 calc R U . . .
C67 C 0.2649(6) -0.1542(6) 0.3585(6) 0.053(3) Uani 1 1 d . . . . .
H67 H 0.307550 -0.165336 0.346124 0.063 Uiso 1 1 calc R U . . .
C68 C 0.2381(6) -0.1864(6) 0.4009(6) 0.053(3) Uani 1 1 d . . . . .
H68 H 0.263117 -0.218840 0.418931 0.064 Uiso 1 1 calc R U . . .
C69 C 0.1742(6) -0.1724(5) 0.4184(5) 0.043(3) Uani 1 1 d . . . . .
C70 C 0.1371(5) -0.1255(4) 0.3926(3) 0.0238(19) Uani 1 1 d . . . . .
C71 C 0.1495(6) -0.2075(5) 0.4666(5) 0.046(3) Uani 1 1 d . . . . .
H71 H 0.178853 -0.238078 0.482875 0.055 Uiso 1 1 calc R U . . .
C72 C 0.0831(8) -0.2437(5) 0.5376(5) 0.061(4) Uani 1 1 d . . . . .
H72A H 0.049590 -0.225868 0.561885 0.073 Uiso 1 1 calc R U . . .
H72B H 0.126060 -0.248839 0.562115 0.073 Uiso 1 1 calc R U . . .
C73 C 0.0584(9) -0.3045(6) 0.5157(5) 0.066(4) Uani 1 1 d . . . . .
C74 C 0.1045(11) -0.3491(6) 0.5028(8) 0.100(7) Uani 1 1 d . . . . .
H74 H 0.151711 -0.341679 0.508074 0.120 Uiso 1 1 calc R U . . .
C75 C 0.0797(14) -0.4054(8) 0.4816(9) 0.121(10) Uani 1 1 d . . . . .
H75 H 0.110602 -0.435018 0.470433 0.145 Uiso 1 1 calc R U . . .
C76 C 0.0141(14) -0.4178(7) 0.4771(7) 0.105(8) Uani 1 1 d . . . . .
H76 H -0.001139 -0.456726 0.464777 0.126 Uiso 1 1 calc R U . . .
C77 C -0.0320(10) -0.3747(8) 0.4901(6) 0.084(5) Uani 1 1 d . . . . .
H77 H -0.079026 -0.383121 0.485790 0.101 Uiso 1 1 calc R U . . .
C78 C -0.0082(10) -0.3181(6) 0.5099(5) 0.071(5) Uani 1 1 d . . . . .
H78 H -0.039914 -0.288448 0.519556 0.085 Uiso 1 1 calc R U . . .
C79 C 0.0466(7) 0.2329(5) 0.3503(5) 0.053(3) Uani 1 1 d . . . . .
H79A H 0.071737 0.240159 0.316386 0.079 Uiso 1 1 calc R U . . .
H79B H 0.075171 0.243031 0.385514 0.079 Uiso 1 1 calc R U . . .
H79C H 0.005951 0.258073 0.347834 0.079 Uiso 1 1 calc R U . . .
C80 C -0.0088(6) 0.1453(5) 0.3045(4) 0.042(3) Uani 1 1 d . . . . .
C81 C -0.0403(7) 0.1767(5) 0.2592(6) 0.057(4) Uani 1 1 d . . . . .
H81 H -0.035985 0.219376 0.257404 0.068 Uiso 1 1 calc R U . . .
C82 C -0.0786(8) 0.1459(7) 0.2159(6) 0.067(4) Uani 1 1 d . . . . .
H82 H -0.100808 0.167531 0.184394 0.080 Uiso 1 1 calc R U . . .
C83 C -0.0842(7) 0.0855(6) 0.2183(5) 0.056(3) Uani 1 1 d . . . . .
H83 H -0.111536 0.065215 0.188719 0.067 Uiso 1 1 calc R U . . .
C84 C -0.0507(6) 0.0509(4) 0.2636(5) 0.038(2) Uani 1 1 d . . . . .
C85 C -0.0110(5) 0.0812(4) 0.3073(5) 0.037(3) Uani 1 1 d . . . . .
C86 C -0.0577(5) -0.0140(5) 0.2621(5) 0.038(2) Uani 1 1 d . . . . .
H86 H -0.088154 -0.030443 0.232427 0.046 Uiso 1 1 calc R U . . .
C87 C -0.0389(6) -0.1165(5) 0.2805(5) 0.045(3) Uani 1 1 d . . . . .
H87A H -0.084522 -0.121384 0.260390 0.054 Uiso 1 1 calc R U . . .
H87B H -0.035613 -0.142284 0.315532 0.054 Uiso 1 1 calc R U . . .
C88 C 0.0694(7) -0.1669(5) 0.2608(5) 0.048(3) Uani 1 1 d . . . . .
H88 H 0.073645 -0.180188 0.299911 0.058 Uiso 1 1 calc R U . . .
C89 C 0.0142(7) -0.1344(5) 0.2411(5) 0.050(3) Uani 1 1 d . . . . .
C90 C 0.0077(9) -0.1153(6) 0.1835(5) 0.068(4) Uani 1 1 d . . . . .
H90 H -0.031716 -0.093864 0.169523 0.082 Uiso 1 1 calc R U . . .
C91 C 0.0567(10) -0.1267(6) 0.1464(6) 0.073(5) Uani 1 1 d . . . . .
H91 H 0.052138 -0.112335 0.107685 0.087 Uiso 1 1 calc R U . . .
C92 C 0.1121(9) -0.1593(6) 0.1668(5) 0.067(5) Uani 1 1 d . . . . .
H92 H 0.145986 -0.167683 0.141410 0.080 Uiso 1 1 calc R U . . .
C93 C 0.1208(7) -0.1813(6) 0.2245(6) 0.059(4) Uani 1 1 d . . . . .
H93 H 0.159160 -0.204474 0.238058 0.071 Uiso 1 1 calc R U . . .
C94 C 0.0982(12) -0.0894(12) 0.5761(11) 0.053(6) Uiso 0.5 1 d D . P . .
H94A H 0.094494 -0.124953 0.600869 0.080 Uiso 0.5 1 calc R U P . .
H94B H 0.105191 -0.053297 0.600270 0.080 Uiso 0.5 1 calc R U P . .
H94C H 0.136523 -0.094578 0.552630 0.080 Uiso 0.5 1 calc R U P . .
C95 C -0.1504(10) 0.0016(9) 0.5250(9) 0.033(4) Uiso 0.5 1 d D . P . .
H95A H -0.169183 -0.031729 0.500814 0.050 Uiso 0.5 1 calc R U P . .
H95B H -0.148472 0.038156 0.501382 0.050 Uiso 0.5 1 calc R U P . .
H95C H -0.179170 0.008886 0.556524 0.050 Uiso 0.5 1 calc R U P . .
C96 C -0.1071(15) -0.0606(14) 0.4080(13) 0.070(8) Uiso 0.5 1 d D . P . .
H96A H -0.121040 -0.020943 0.392382 0.105 Uiso 0.5 1 calc R U P . .
H96B H -0.135076 -0.071443 0.439257 0.105 Uiso 0.5 1 calc R U P . .
H96C H -0.112803 -0.090953 0.377231 0.105 Uiso 0.5 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O9 2.098(7) 3_666 ?
Co1 O9 2.098(7) . ?
Co1 O8 2.120(7) . ?
Co1 O8 2.120(7) 3_666 ?
Co1 O7 2.130(7) . ?
Co1 O7 2.130(7) 3_666 ?
O1 C7 1.335(13) . ?
O1 Co4 2.001(7) 3_666 ?
O1 Co2 2.046(7) . ?
N1 C8 1.250(14) . ?
N1 C9 1.499(14) . ?
N1 Co4 2.087(9) 3_666 ?
C1 O2 1.428(12) . ?
Co2 O3 1.981(7) . ?
Co2 O8 2.055(7) . ?
Co2 N2 2.077(10) . ?
Co2 O7 2.154(7) . ?
Co2 O2 2.374(8) . ?
O2 C2 1.392(13) . ?
N2 C23 1.264(15) . ?
N2 C24 1.509(12) . ?
C2 C3 1.349(17) . ?
C2 C7 1.442(14) . ?
Co3 O5 2.002(7) . ?
Co3 O7 2.015(7) . ?
Co3 O3 2.051(7) . ?
Co3 N3 2.108(9) . ?
Co3 O9 2.176(7) . ?
Co3 O4 2.313(8) . ?
O3 C22 1.294(14) . ?
N3 C38 1.269(14) . ?
N3 C39 1.488(12) . ?
C3 C4 1.401(19) . ?
Co4 O9 2.028(7) . ?
Co4 O5 2.057(8) . ?
Co4 O8 2.149(8) 3_666 ?
Co4 O6 2.396(8) . ?
O4 C17 1.390(13) . ?
O4 C16 1.454(11) . ?
N4 C56 1.233(13) . ?
N4 C57 1.477(12) . ?
N4 Co6 2.095(8) . ?
C4 C5 1.367(17) . ?
Co5 O16 2.080(6) 3_556 ?
Co5 O16 2.080(6) . ?
Co5 O18 2.115(7) 3_556 ?
Co5 O18 2.115(7) . ?
Co5 O17 2.125(7) . ?
Co5 O17 2.125(7) 3_556 ?
O5 C55 1.347(14) . ?
N5 C71 1.258(14) . ?
N5 C72 1.503(12) . ?
N5 Co7 2.096(9) . ?
C5 C6 1.411(17) . ?
Co6 O10 1.986(6) . ?
Co6 O16 2.025(6) . ?
Co6 O14 2.044(7) 3_556 ?
Co6 O17 2.171(7) . ?
Co6 O15 2.330(7) 3_556 ?
O6 C32 1.377(15) . ?
O6 C31 1.436(12) . ?
N6 C86 1.279(14) . ?
N6 C87 1.502(13) . ?
N6 Co8 2.087(9) . ?
C6 C7 1.391(16) . ?
C6 C8 1.475(15) . ?
Co7 O12 2.012(6) . ?
Co7 O17 2.022(6) . ?
Co7 O10 2.082(7) . ?
Co7 O18 2.161(7) . ?
Co7 O11 2.294(7) . ?
O7 C46 1.64(3) . ?
Co8 O14 1.967(6) . ?
Co8 O18 2.014(6) . ?
Co8 O12 2.043(6) . ?
Co8 O16 2.204(7) 3_556 ?
Co8 O13 2.317(7) . ?
O8 C47 1.367(19) . ?
O9 C48 1.45(2) . ?
C9 C10 1.509(16) . ?
O10 C37 1.296(12) . ?
C10 C11 1.36(2) . ?
C10 C15 1.397(17) . ?
O11 C50 1.388(13) . ?
O11 C49 1.452(11) . ?
C11 C12 1.39(2) . ?
O12 C70 1.308(11) . ?
C12 C13 1.36(2) . ?
O13 C65 1.358(12) . ?
O13 C64 1.445(10) . ?
C13 C14 1.35(2) . ?
O14 C85 1.340(13) . ?
C14 C15 1.383(19) . ?
O15 C80 1.378(13) . ?
O15 C79 1.443(12) . ?
O16 C95 1.49(2) . ?
O17 C94 1.47(3) . ?
C17 C18 1.334(17) . ?
C17 C22 1.430(14) . ?
O18 C96 1.51(3) . ?
C18 C19 1.385(18) . ?
C19 C20 1.372(17) . ?
C20 C21 1.365(17) . ?
C21 C22 1.457(16) . ?
C21 C23 1.479(14) . ?
C24 C25 1.520(17) . ?
C25 C26 1.359(15) . ?
C25 C30 1.388(19) . ?
C26 C27 1.384(18) . ?
C27 C28 1.39(2) . ?
C28 C29 1.38(2) . ?
C29 C30 1.35(2) . ?
C32 C33 1.391(17) . ?
C32 C55 1.420(14) . ?
C33 C34 1.40(2) . ?
C34 C35 1.375(19) . ?
C35 C36 1.395(16) . ?
C36 C55 1.364(17) . ?
C36 C38 1.447(15) . ?
C37 C54 1.422(15) . ?
C37 C50 1.428(12) . ?
C39 C40 1.523(15) . ?
C40 C41 1.368(18) . ?
C40 C45 1.377(17) . ?
C41 C42 1.405(18) . ?
C42 C43 1.36(2) . ?
C43 C44 1.36(2) . ?
C44 C45 1.401(18) . ?
C50 C51 1.332(16) . ?
C51 C52 1.390(17) . ?
C52 C53 1.384(15) . ?
C53 C54 1.367(15) . ?
C54 C56 1.479(12) . ?
C57 C58 1.490(16) . ?
C58 C63 1.389(14) . ?
C58 C59 1.400(16) . ?
C59 C60 1.333(19) . ?
C60 C61 1.38(2) . ?
C61 C62 1.36(2) . ?
C62 C63 1.363(17) . ?
C65 C66 1.376(15) . ?
C65 C70 1.434(13) . ?
C66 C67 1.379(17) . ?
C67 C68 1.359(17) . ?
C68 C69 1.401(16) . ?
C69 C70 1.380(14) . ?
C69 C71 1.478(15) . ?
C72 C73 1.51(2) . ?
C73 C78 1.35(2) . ?
C73 C74 1.397(19) . ?
C74 C75 1.41(3) . ?
C75 C76 1.33(3) . ?
C76 C77 1.37(2) . ?
C77 C78 1.40(2) . ?
C80 C81 1.366(16) . ?
C80 C85 1.420(13) . ?
C81 C82 1.39(2) . ?
C82 C83 1.343(18) . ?
C83 C84 1.418(15) . ?
C84 C85 1.402(15) . ?
C84 C86 1.444(14) . ?
C87 C89 1.507(17) . ?
C88 C89 1.358(18) . ?
C88 C93 1.414(16) . ?
C89 C90 1.396(16) . ?
C90 C91 1.38(2) . ?
C91 C92 1.37(2) . ?
C92 C93 1.42(2) . ?

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
O9 Co1 O9 180.0 3_666 . ?
O9 Co1 O8 82.7(3) 3_666 . ?
O9 Co1 O8 97.3(3) . . ?
O9 Co1 O8 97.3(3) 3_666 3_666 ?
O9 Co1 O8 82.7(3) . 3_666 ?
O8 Co1 O8 180.0 . 3_666 ?
O9 Co1 O7 97.1(3) 3_666 . ?
O9 Co1 O7 82.9(3) . . ?
O8 Co1 O7 83.6(3) . . ?
O8 Co1 O7 96.4(3) 3_666 . ?
O9 Co1 O7 82.9(3) 3_666 3_666 ?
O9 Co1 O7 97.1(3) . 3_666 ?
O8 Co1 O7 96.4(3) . 3_666 ?
O8 Co1 O7 83.6(3) 3_666 3_666 ?
O7 Co1 O7 180.0 . 3_666 ?
C7 O1 Co4 129.8(6) . 3_666 ?
C7 O1 Co2 124.5(6) . . ?
Co4 O1 Co2 102.9(3) 3_666 . ?
C8 N1 C9 119.0(10) . . ?
C8 N1 Co4 127.5(8) . 3_666 ?
C9 N1 Co4 113.5(7) . 3_666 ?
O3 Co2 O1 161.7(3) . . ?
O3 Co2 O8 113.5(3) . . ?
O1 Co2 O8 79.8(3) . . ?
O3 Co2 N2 87.8(3) . . ?
O1 Co2 N2 103.2(3) . . ?
O8 Co2 N2 98.3(3) . . ?
O3 Co2 O7 77.9(3) . . ?
O1 Co2 O7 91.6(3) . . ?
O8 Co2 O7 84.5(3) . . ?
N2 Co2 O7 165.2(3) . . ?
O3 Co2 O2 96.1(3) . . ?
O1 Co2 O2 70.7(3) . . ?
O8 Co2 O2 150.3(3) . . ?
N2 Co2 O2 85.1(3) . . ?
O7 Co2 O2 99.7(3) . . ?
C2 O2 C1 116.4(9) . . ?
C2 O2 Co2 113.8(6) . . ?
C1 O2 Co2 129.7(7) . . ?
C23 N2 C24 119.3(10) . . ?
C23 N2 Co2 127.7(7) . . ?
C24 N2 Co2 112.8(7) . . ?
C3 C2 O2 127.1(10) . . ?
C3 C2 C7 121.2(11) . . ?
O2 C2 C7 111.7(10) . . ?
O5 Co3 O7 112.5(3) . . ?
O5 Co3 O3 162.6(3) . . ?
O7 Co3 O3 79.6(3) . . ?
O5 Co3 N3 87.6(3) . . ?
O7 Co3 N3 102.0(3) . . ?
O3 Co3 N3 102.5(3) . . ?
O5 Co3 O9 78.4(3) . . ?
O7 Co3 O9 83.7(3) . . ?
O3 Co3 O9 91.1(3) . . ?
N3 Co3 O9 166.0(3) . . ?
O5 Co3 O4 95.4(3) . . ?
O7 Co3 O4 151.4(3) . . ?
O3 Co3 O4 71.9(3) . . ?
N3 Co3 O4 84.6(3) . . ?
O9 Co3 O4 96.5(3) . . ?
C22 O3 Co2 130.7(6) . . ?
C22 O3 Co3 121.1(6) . . ?
Co2 O3 Co3 103.1(3) . . ?
C38 N3 C39 119.9(10) . . ?
C38 N3 Co3 125.5(8) . . ?
C39 N3 Co3 114.6(7) . . ?
C2 C3 C4 120.4(11) . . ?
O1 Co4 O9 112.9(3) 3_666 . ?
O1 Co4 O5 160.7(3) 3_666 . ?
O9 Co4 O5 80.6(3) . . ?
O1 Co4 N1 87.7(3) 3_666 3_666 ?
O9 Co4 N1 102.4(4) . 3_666 ?
O5 Co4 N1 103.3(3) . 3_666 ?
O1 Co4 O8 78.6(3) 3_666 3_666 ?
O9 Co4 O8 83.7(3) . 3_666 ?
O5 Co4 O8 89.8(3) . 3_666 ?
N1 Co4 O8 166.3(3) 3_666 3_666 ?
O1 Co4 O6 96.2(3) 3_666 . ?
O9 Co4 O6 150.4(3) . . ?
O5 Co4 O6 69.9(3) . . ?
N1 Co4 O6 83.1(4) 3_666 . ?
O8 Co4 O6 97.7(3) 3_666 . ?
C17 O4 C16 116.7(8) . . ?
C17 O4 Co3 114.1(6) . . ?
C16 O4 Co3 127.4(7) . . ?
C56 N4 C57 119.9(9) . . ?
C56 N4 Co6 125.9(7) . . ?
C57 N4 Co6 114.2(7) . . ?
C5 C4 C3 119.5(12) . . ?
O16 Co5 O16 180.0 3_556 . ?
O16 Co5 O18 96.3(2) 3_556 3_556 ?
O16 Co5 O18 83.7(2) . 3_556 ?
O16 Co5 O18 83.7(2) 3_556 . ?
O16 Co5 O18 96.3(2) . . ?
O18 Co5 O18 180.0 3_556 . ?
O16 Co5 O17 96.7(3) 3_556 . ?
O16 Co5 O17 83.3(3) . . ?
O18 Co5 O17 98.0(3) 3_556 . ?
O18 Co5 O17 82.0(3) . . ?
O16 Co5 O17 83.3(3) 3_556 3_556 ?
O16 Co5 O17 96.7(3) . 3_556 ?
O18 Co5 O17 82.0(3) 3_556 3_556 ?
O18 Co5 O17 98.0(3) . 3_556 ?
O17 Co5 O17 180.0 . 3_556 ?
C55 O5 Co3 130.1(7) . . ?
C55 O5 Co4 126.2(6) . . ?
Co3 O5 Co4 102.6(3) . . ?
C71 N5 C72 115.5(9) . . ?
C71 N5 Co7 126.7(7) . . ?
C72 N5 Co7 117.7(7) . . ?
C4 C5 C6 121.7(13) . . ?
O10 Co6 O16 114.8(3) . . ?
O10 Co6 O14 159.5(3) . 3_556 ?
O16 Co6 O14 79.7(3) . 3_556 ?
O10 Co6 N4 87.6(3) . . ?
O16 Co6 N4 97.8(3) . . ?
O14 Co6 N4 105.3(3) 3_556 . ?
O10 Co6 O17 78.4(3) . . ?
O16 Co6 O17 83.4(3) . . ?
O14 Co6 O17 89.6(3) 3_556 . ?
N4 Co6 O17 165.0(3) . . ?
O10 Co6 O15 94.7(3) . 3_556 ?
O16 Co6 O15 150.5(3) . 3_556 ?
O14 Co6 O15 71.6(2) 3_556 3_556 ?
N4 Co6 O15 83.5(3) . 3_556 ?
O17 Co6 O15 102.9(3) . 3_556 ?
C32 O6 C31 118.5(9) . . ?
C32 O6 Co4 113.8(6) . . ?
C31 O6 Co4 125.8(8) . . ?
C86 N6 C87 113.7(9) . . ?
C86 N6 Co8 127.2(7) . . ?
C87 N6 Co8 118.9(7) . . ?
C7 C6 C5 118.9(11) . . ?
C7 C6 C8 122.9(11) . . ?
C5 C6 C8 118.2(11) . . ?
O12 Co7 O17 112.6(3) . . ?
O12 Co7 O10 161.2(3) . . ?
O17 Co7 O10 79.8(3) . . ?
O12 Co7 N5 87.2(3) . . ?
O17 Co7 N5 99.0(3) . . ?
O10 Co7 N5 105.4(3) . . ?
O12 Co7 O18 77.2(2) . . ?
O17 Co7 O18 83.3(3) . . ?
O10 Co7 O18 90.8(3) . . ?
N5 Co7 O18 163.8(3) . . ?
O12 Co7 O11 94.9(2) . . ?
O17 Co7 O11 151.7(3) . . ?
O10 Co7 O11 71.9(2) . . ?
N5 Co7 O11 88.5(3) . . ?
O18 Co7 O11 97.0(3) . . ?
C46 O7 Co3 117.2(12) . . ?
C46 O7 Co1 124.5(13) . . ?
Co3 O7 Co1 97.8(3) . . ?
C46 O7 Co2 119.6(12) . . ?
Co3 O7 Co2 98.5(3) . . ?
Co1 O7 Co2 93.5(3) . . ?
O1 C7 C6 124.5(9) . . ?
O1 C7 C2 117.2(10) . . ?
C6 C7 C2 118.3(10) . . ?
O14 Co8 O18 114.6(3) . . ?
O14 Co8 O12 158.1(3) . . ?
O18 Co8 O12 79.9(3) . . ?
O14 Co8 N6 87.5(3) . . ?
O18 Co8 N6 99.6(3) . . ?
O12 Co8 N6 106.8(3) . . ?
O14 Co8 O16 77.2(3) . 3_556 ?
O18 Co8 O16 83.0(3) . 3_556 ?
O12 Co8 O16 89.1(3) . 3_556 ?
N6 Co8 O16 164.0(3) . 3_556 ?
O14 Co8 O13 92.1(3) . . ?
O18 Co8 O13 151.8(3) . . ?
O12 Co8 O13 71.9(2) . . ?
N6 Co8 O13 90.1(3) . . ?
O16 Co8 O13 94.9(2) 3_556 . ?
C47 O8 Co2 121.0(9) . . ?
C47 O8 Co1 121.9(9) . . ?
Co2 O8 Co1 96.7(3) . . ?
C47 O8 Co4 119.6(9) . 3_666 ?
Co2 O8 Co4 97.6(3) . 3_666 ?
Co1 O8 Co4 93.8(3) . 3_666 ?
N1 C8 C6 126.6(12) . . ?
C48 O9 Co4 117.7(10) . . ?
C48 O9 Co1 122.7(10) . . ?
Co4 O9 Co1 98.1(3) . . ?
C48 O9 Co3 120.9(10) . . ?
Co4 O9 Co3 97.8(3) . . ?
Co1 O9 Co3 94.0(3) . . ?
N1 C9 C10 117.0(9) . . ?
C37 O10 Co6 128.6(6) . . ?
C37 O10 Co7 118.6(5) . . ?
Co6 O10 Co7 102.4(3) . . ?
C11 C10 C15 118.2(12) . . ?
C11 C10 C9 122.3(12) . . ?
C15 C10 C9 119.5(13) . . ?
C50 O11 C49 117.0(8) . . ?
C50 O11 Co7 112.0(5) . . ?
C49 O11 Co7 130.5(7) . . ?
C10 C11 C12 120.8(15) . . ?
C70 O12 Co7 130.0(6) . . ?
C70 O12 Co8 123.0(5) . . ?
Co7 O12 Co8 103.2(3) . . ?
C13 C12 C11 120.1(17) . . ?
C65 O13 C64 118.7(8) . . ?
C65 O13 Co8 113.1(5) . . ?
C64 O13 Co8 125.2(6) . . ?
C14 C13 C12 120.2(16) . . ?
C85 O14 Co8 131.1(6) . . ?
C85 O14 Co6 122.0(5) . 3_556 ?
Co8 O14 Co6 104.9(3) . 3_556 ?
C13 C14 C15 120.1(15) . . ?
C80 O15 C79 118.9(8) . . ?
C80 O15 Co6 113.9(6) . 3_556 ?
C79 O15 Co6 127.1(7) . 3_556 ?
C14 C15 C10 120.5(15) . . ?
C95 O16 Co6 120.4(9) . . ?
C95 O16 Co5 118.9(8) . . ?
Co6 O16 Co5 98.7(3) . . ?
C95 O16 Co8 122.3(8) . 3_556 ?
Co6 O16 Co8 97.5(3) . 3_556 ?
Co5 O16 Co8 93.2(3) . 3_556 ?
C94 O17 Co7 119.5(11) . . ?
C94 O17 Co5 124.8(11) . . ?
Co7 O17 Co5 98.3(3) . . ?
C94 O17 Co6 117.1(11) . . ?
Co7 O17 Co6 98.2(3) . . ?
Co5 O17 Co6 92.9(3) . . ?
C18 C17 O4 125.9(9) . . ?
C18 C17 C22 124.0(11) . . ?
O4 C17 C22 110.1(10) . . ?
C96 O18 Co8 115.3(12) . . ?
C96 O18 Co5 122.0(12) . . ?
Co8 O18 Co5 97.9(3) . . ?
C96 O18 Co7 122.9(12) . . ?
Co8 O18 Co7 99.1(3) . . ?
Co5 O18 Co7 94.5(3) . . ?
C17 C18 C19 119.8(11) . . ?
C20 C19 C18 119.9(13) . . ?
C21 C20 C19 122.0(12) . . ?
C20 C21 C22 120.0(10) . . ?
C20 C21 C23 120.3(11) . . ?
C22 C21 C23 119.8(11) . . ?
O3 C22 C17 120.3(10) . . ?
O3 C22 C21 125.4(9) . . ?
C17 C22 C21 114.3(11) . . ?
N2 C23 C21 127.1(11) . . ?
N2 C24 C25 116.1(10) . . ?
C26 C25 C30 118.2(13) . . ?
C26 C25 C24 120.9(12) . . ?
C30 C25 C24 120.9(12) . . ?
C25 C26 C27 120.8(14) . . ?
C26 C27 C28 120.7(13) . . ?
C29 C28 C27 117.6(15) . . ?
C30 C29 C28 121.2(17) . . ?
C29 C30 C25 121.4(14) . . ?
O6 C32 C33 125.7(11) . . ?
O6 C32 C55 113.8(10) . . ?
C33 C32 C55 120.4(12) . . ?
C32 C33 C34 119.0(12) . . ?
C35 C34 C33 120.1(13) . . ?
C34 C35 C36 121.0(14) . . ?
C55 C36 C35 120.2(11) . . ?
C55 C36 C38 123.1(10) . . ?
C35 C36 C38 116.7(12) . . ?
O10 C37 C54 125.5(8) . . ?
O10 C37 C50 118.8(9) . . ?
C54 C37 C50 115.8(9) . . ?
N3 C38 C36 128.5(12) . . ?
N3 C39 C40 115.1(9) . . ?
C41 C40 C45 119.2(11) . . ?
C41 C40 C39 122.1(11) . . ?
C45 C40 C39 118.7(11) . . ?
C40 C41 C42 120.6(13) . . ?
C43 C42 C41 119.4(15) . . ?
C42 C43 C44 120.8(13) . . ?
C43 C44 C45 120.0(13) . . ?
C40 C45 C44 119.9(13) . . ?
C51 C50 O11 124.8(9) . . ?
C51 C50 C37 123.3(10) . . ?
O11 C50 C37 111.9(9) . . ?
C50 C51 C52 120.1(10) . . ?
C53 C52 C51 118.7(12) . . ?
C54 C53 C52 122.3(11) . . ?
C53 C54 C37 119.8(9) . . ?
C53 C54 C56 119.7(10) . . ?
C37 C54 C56 120.5(9) . . ?
O5 C55 C36 124.8(10) . . ?
O5 C55 C32 115.8(11) . . ?
C36 C55 C32 119.3(11) . . ?
N4 C56 C54 127.7(10) . . ?
N4 C57 C58 118.4(10) . . ?
C63 C58 C59 116.6(11) . . ?
C63 C58 C57 121.7(11) . . ?
C59 C58 C57 121.5(11) . . ?
C60 C59 C58 121.6(11) . . ?
C59 C60 C61 121.4(14) . . ?
C62 C61 C60 118.0(13) . . ?
C61 C62 C63 121.6(12) . . ?
C62 C63 C58 120.7(11) . . ?
O13 C65 C66 125.5(9) . . ?
O13 C65 C70 113.8(8) . . ?
C66 C65 C70 120.7(10) . . ?
C65 C66 C67 119.9(10) . . ?
C68 C67 C66 120.4(11) . . ?
C67 C68 C69 121.0(12) . . ?
C70 C69 C68 120.2(10) . . ?
C70 C69 C71 121.7(10) . . ?
C68 C69 C71 118.1(11) . . ?
O12 C70 C69 125.7(9) . . ?
O12 C70 C65 116.6(8) . . ?
C69 C70 C65 117.7(9) . . ?
N5 C71 C69 127.5(10) . . ?
N5 C72 C73 111.3(10) . . ?
C78 C73 C74 118.3(16) . . ?
C78 C73 C72 121.5(13) . . ?
C74 C73 C72 120.2(17) . . ?
C73 C74 C75 119(2) . . ?
C76 C75 C74 121.4(17) . . ?
C75 C76 C77 120.6(19) . . ?
C76 C77 C78 119(2) . . ?
C73 C78 C77 122.1(16) . . ?
C81 C80 O15 125.9(10) . . ?
C81 C80 C85 122.0(11) . . ?
O15 C80 C85 112.1(9) . . ?
C80 C81 C82 119.6(11) . . ?
C83 C82 C81 120.1(12) . . ?
C82 C83 C84 122.1(13) . . ?
C85 C84 C83 118.6(10) . . ?
C85 C84 C86 122.7(9) . . ?
C83 C84 C86 118.7(11) . . ?
O14 C85 C84 124.5(8) . . ?
O14 C85 C80 118.0(10) . . ?
C84 C85 C80 117.5(10) . . ?
N6 C86 C84 126.2(10) . . ?
N6 C87 C89 107.5(8) . . ?
C89 C88 C93 121.5(12) . . ?
C88 C89 C90 119.2(13) . . ?
C88 C89 C87 121.5(10) . . ?
C90 C89 C87 119.3(13) . . ?
C91 C90 C89 122.0(16) . . ?
C92 C91 C90 118.1(13) . . ?
C91 C92 C93 122.4(13) . . ?
C88 C93 C92 116.6(14) . . ?

_refine_diff_density_max         1.706
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.150



# SQUEEZE RESULTS (Version = 241018)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.246 -0.051 0.782 463 140 ' '
2 0.246 0.551 0.282 464 140 ' '
3 0.418 0.671 0.801 15 1 ' '
4 0.418 0.829 0.301 14 1 ' '
5 0.584 0.175 0.697 16 1 ' '
6 0.584 0.325 0.197 16 1 ' '
7 0.754 0.051 0.218 462 140 ' '
8 0.754 0.449 0.718 461 140 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol'
_chemical_properties_physical    Moisture-sensitive
_exptl_crystal_preparation       'Magnetic properties'
