# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1857025'
_audit_update_record             
;
2018-08-29 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 N2 Ni O2'
_chemical_formula_weight         353.05

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   7.644(5)
_cell_length_b                   17.654(5)
_cell_length_c                   22.775(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     3073(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    34281
_cell_measurement_theta_min      1.788
_cell_measurement_theta_max      25.967

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_F_000             1472
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.273
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.955
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34278
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_av_R_equivalents  0.0936
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.307
_diffrn_reflns_theta_max         25.967
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3004
_reflns_number_gt                2184
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'
_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)+(0.0497P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3004
_refine_ls_number_parameters     209
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0377
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.89102(4) 0.22211(2) 0.02247(2) 0.02907(13) Uani 1 1 d . . . . .
O11 O 0.9216(3) 0.16345(12) 0.09024(8) 0.0465(6) Uani 1 1 d . . . . .
C12 C 0.8042(4) 0.16797(16) 0.13173(12) 0.0358(7) Uani 1 1 d . . . . .
C13 C 0.7474(4) 0.10107(18) 0.15971(13) 0.0470(8) Uani 1 1 d . . . . .
H13 H 0.793326 0.054798 0.147756 0.056 Uiso 1 1 calc R U . . .
C14 C 0.6265(4) 0.1025(2) 0.20394(15) 0.0576(9) Uani 1 1 d . . . . .
H14 H 0.590459 0.057330 0.221170 0.069 Uiso 1 1 calc R U . . .
C15 C 0.5577(4) 0.1702(2) 0.22324(15) 0.0603(10) Uani 1 1 d . . . . .
H15 H 0.475264 0.171054 0.253259 0.072 Uiso 1 1 calc R U . . .
C16 C 0.6120(4) 0.23596(19) 0.19776(14) 0.0505(8) Uani 1 1 d . . . . .
H16 H 0.567097 0.281547 0.211613 0.061 Uiso 1 1 calc R U . . .
C17 C 0.7336(3) 0.23763(16) 0.15122(12) 0.0348(7) Uani 1 1 d . . . . .
C18 C 0.7886(4) 0.30930(16) 0.12470(12) 0.0363(7) Uani 1 1 d . . . . .
N19 N 0.8531(3) 0.31226(12) 0.07186(10) 0.0346(6) Uani 1 1 d . . . . .
C20 C 0.9032(4) 0.38856(16) 0.04997(14) 0.0428(7) Uani 1 1 d . . . . .
H20A H 0.991543 0.409716 0.075785 0.051 Uiso 1 1 calc R U . . .
H20B H 0.801695 0.421465 0.051457 0.051 Uiso 1 1 calc R U . . .
C21 C 0.9727(4) 0.38736(17) -0.01146(13) 0.0444(8) Uani 1 1 d . . . . .
H21A H 1.078564 0.357093 -0.012585 0.053 Uiso 1 1 calc R U . . .
H21B H 1.002945 0.438539 -0.023175 0.053 Uiso 1 1 calc R U . . .
C22 C 0.8422(4) 0.35534(15) -0.05443(13) 0.0400(7) Uani 1 1 d . . . . .
H22A H 0.726364 0.374712 -0.045614 0.048 Uiso 1 1 calc R U . . .
H22B H 0.872732 0.370846 -0.093978 0.048 Uiso 1 1 calc R U . . .
N23 N 0.8418(3) 0.27206(12) -0.05057(10) 0.0339(5) Uani 1 1 d . . . . .
C24 C 0.8021(4) 0.23710(16) -0.09895(13) 0.0363(7) Uani 1 1 d . . . . .
H24 H 0.765009 0.267042 -0.130148 0.044 Uiso 1 1 calc R U . . .
C25 C 0.8098(4) 0.15746(16) -0.10910(12) 0.0363(7) Uani 1 1 d . . . . .
C26 C 0.7521(4) 0.12935(18) -0.16309(13) 0.0465(8) Uani 1 1 d . . . . .
H26 H 0.703881 0.162639 -0.190294 0.056 Uiso 1 1 calc R U . . .
C27 C 0.7646(4) 0.05391(18) -0.17702(14) 0.0520(9) Uani 1 1 d . . . . .
H27 H 0.723972 0.035892 -0.212890 0.062 Uiso 1 1 calc R U . . .
C28 C 0.8394(4) 0.00502(17) -0.13624(13) 0.0490(8) Uani 1 1 d . . . . .
H28 H 0.848983 -0.046178 -0.145324 0.059 Uiso 1 1 calc R U . . .
C29 C 0.8992(4) 0.03016(17) -0.08329(13) 0.0428(8) Uani 1 1 d . . . . .
H29 H 0.950577 -0.003911 -0.057346 0.051 Uiso 1 1 calc R U . . .
C30 C 0.8843(3) 0.10752(16) -0.06721(13) 0.0362(7) Uani 1 1 d . . . . .
O31 O 0.9414(3) 0.13006(11) -0.01621(8) 0.0411(5) Uani 1 1 d . . . . .
C181 C 0.7707(4) 0.37897(18) 0.16236(14) 0.0540(9) Uani 1 1 d . . . . .
H18A H 0.873505 0.409771 0.158295 0.081 Uiso 1 1 calc R U . . .
H18B H 0.757274 0.364241 0.202686 0.081 Uiso 1 1 calc R U . . .
H18C H 0.669949 0.407332 0.150120 0.081 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 O11 1.8733(19) . ?
Ni1 O31 1.888(2) . ?
Ni1 N23 1.920(2) . ?
Ni1 N19 1.970(2) . ?
O11 C12 1.306(3) . ?
C12 C13 1.411(4) . ?
C12 C17 1.414(4) . ?
C13 C14 1.367(4) . ?
C14 C15 1.379(5) . ?
C15 C16 1.362(4) . ?
C16 C17 1.410(4) . ?
C17 C18 1.464(4) . ?
C18 N19 1.302(3) . ?
C18 C181 1.506(4) . ?
N19 C20 1.486(3) . ?
C20 C21 1.497(4) . ?
C21 C22 1.508(4) . ?
C22 N23 1.473(3) . ?
N23 C24 1.299(3) . ?
C24 C25 1.426(4) . ?
C25 C26 1.398(4) . ?
C25 C30 1.418(4) . ?
C26 C27 1.372(4) . ?
C27 C28 1.391(4) . ?
C28 C29 1.364(4) . ?
C29 C30 1.419(4) . ?
C30 O31 1.303(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O11 Ni1 O31 83.30(8) . . ?
O11 Ni1 N23 172.83(10) . . ?
O31 Ni1 N23 91.78(9) . . ?
O11 Ni1 N19 89.68(9) . . ?
O31 Ni1 N19 172.54(9) . . ?
N23 Ni1 N19 95.44(9) . . ?
C12 O11 Ni1 118.49(17) . . ?
O11 C12 C13 119.2(3) . . ?
O11 C12 C17 122.8(3) . . ?
C13 C12 C17 118.0(3) . . ?
C14 C13 C12 121.7(3) . . ?
C13 C14 C15 120.6(3) . . ?
C16 C15 C14 119.2(3) . . ?
C15 C16 C17 122.6(3) . . ?
C16 C17 C12 118.0(3) . . ?
C16 C17 C18 121.2(3) . . ?
C12 C17 C18 120.9(3) . . ?
N19 C18 C17 121.7(3) . . ?
N19 C18 C181 121.9(3) . . ?
C17 C18 C181 116.4(3) . . ?
C18 N19 C20 116.4(2) . . ?
C18 N19 Ni1 123.4(2) . . ?
C20 N19 Ni1 120.18(19) . . ?
N19 C20 C21 113.1(2) . . ?
C20 C21 C22 112.2(2) . . ?
N23 C22 C21 109.7(2) . . ?
C24 N23 C22 115.1(2) . . ?
C24 N23 Ni1 124.23(19) . . ?
C22 N23 Ni1 120.64(19) . . ?
N23 C24 C25 126.6(3) . . ?
C26 C25 C30 119.9(3) . . ?
C26 C25 C24 118.7(3) . . ?
C30 C25 C24 121.4(3) . . ?
C27 C26 C25 121.7(3) . . ?
C26 C27 C28 118.5(3) . . ?
C29 C28 C27 121.8(3) . . ?
C28 C29 C30 121.0(3) . . ?
O31 C30 C25 123.0(3) . . ?
O31 C30 C29 119.8(3) . . ?
C25 C30 C29 117.2(3) . . ?
C30 O31 Ni1 127.61(18) . . ?

_refine_diff_density_max         0.260
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1857027'
_audit_update_record             
;
2018-08-29 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H40 Cl Mn N7 Ni2 O10'
_chemical_formula_weight         938.56

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

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

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

_cell_length_a                   25.090(2)
_cell_length_b                   10.1029(6)
_cell_length_c                   15.1546(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.576(6)
_cell_angle_gamma                90
_cell_volume                     3829.1(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    11720
_cell_measurement_theta_min      3.414
_cell_measurement_theta_max      29.998

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_F_000             1932
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_exptl_absorpt_coefficient_mu    1.435
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.901
_exptl_absorpt_correction_T_max  1.000

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Oxford Diffaction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            11720
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.414
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             5830
_reflns_number_gt                5182
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_max     0.952
_reflns_Friedel_fraction_full    0.969

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

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0441P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5830
_refine_ls_number_parameters     529
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0461
_refine_ls_wR_factor_ref         0.0913
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.66633(3) 0.96082(5) 0.77328(4) 0.01874(14) Uani 1 1 d . . . . .
Ni2 Ni 0.53431(3) 0.98069(5) 0.61120(4) 0.01949(14) Uani 1 1 d . . . . .
Mn3 Mn 0.60568(3) 0.72865(6) 0.67308(4) 0.01996(16) Uani 1 1 d . . . . .
O11 O 0.68342(14) 0.7930(3) 0.7223(2) 0.0217(7) Uani 1 1 d . . . . .
C12 C 0.7282(2) 0.7375(5) 0.7601(3) 0.0216(10) Uani 1 1 d . . . . .
C13 C 0.7272(2) 0.6062(5) 0.7886(3) 0.0268(11) Uani 1 1 d . . . . .
H13 H 0.696134 0.556443 0.778730 0.032 Uiso 1 1 calc R U . . .
C14 C 0.7724(3) 0.5501(5) 0.8316(4) 0.0337(13) Uani 1 1 d . . . . .
H14 H 0.771270 0.462889 0.851009 0.040 Uiso 1 1 calc R U . . .
C15 C 0.8187(3) 0.6210(6) 0.8459(4) 0.0347(13) Uani 1 1 d . . . . .
H15 H 0.848356 0.583485 0.877008 0.042 Uiso 1 1 calc R U . . .
C16 C 0.8210(2) 0.7479(6) 0.8142(3) 0.0308(12) Uani 1 1 d . . . . .
H16 H 0.853290 0.793481 0.820748 0.037 Uiso 1 1 calc R U . . .
C17 C 0.7761(2) 0.8104(5) 0.7722(3) 0.0226(10) Uani 1 1 d . . . . .
C18 C 0.7793(2) 0.9507(5) 0.7462(3) 0.0259(11) Uani 1 1 d . . . . .
C181 C 0.8326(3) 1.0026(6) 0.7206(4) 0.0429(16) Uani 1 1 d . . . . .
H18A H 0.847152 1.062747 0.765239 0.064 Uiso 1 1 calc R U . . .
H18B H 0.827529 1.047967 0.664897 0.064 Uiso 1 1 calc R U . . .
H18C H 0.856786 0.929937 0.715432 0.064 Uiso 1 1 calc R U . . .
N19 N 0.7375(2) 1.0272(4) 0.7465(3) 0.0258(10) Uani 1 1 d . . . . .
C20 C 0.7445(3) 1.1674(5) 0.7204(3) 0.0347(14) Uani 1 1 d . . . . .
H20A H 0.751678 1.170534 0.658459 0.042 Uiso 1 1 calc R U . . .
H20B H 0.775283 1.203878 0.754748 0.042 Uiso 1 1 calc R U . . .
C21 C 0.6964(3) 1.2520(4) 0.7337(3) 0.0319(13) Uani 1 1 d . . . . .
H21A H 0.667333 1.227072 0.690881 0.038 Uiso 1 1 calc R U . . .
H21B H 0.705075 1.344017 0.723388 0.038 Uiso 1 1 calc R U . . .
C22 C 0.6782(3) 1.2376(5) 0.8266(3) 0.0320(13) Uani 1 1 d . . . . .
H22A H 0.708901 1.225956 0.868936 0.038 Uiso 1 1 calc R U . . .
H22B H 0.659105 1.316411 0.842563 0.038 Uiso 1 1 calc R U . . .
N23 N 0.64289(19) 1.1213(4) 0.8276(3) 0.0242(9) Uani 1 1 d . . . . .
C24 C 0.5983(2) 1.1345(5) 0.8632(3) 0.0295(13) Uani 1 1 d . . . . .
H24 H 0.592194 1.216262 0.888745 0.035 Uiso 1 1 calc R U . . .
C25 C 0.5572(2) 1.0377(5) 0.8680(3) 0.0273(12) Uani 1 1 d . . . . .
C26 C 0.5116(3) 1.0738(6) 0.9130(3) 0.0337(13) Uani 1 1 d . . . . .
H26 H 0.510526 1.156870 0.939258 0.040 Uiso 1 1 calc R U . . .
C27 C 0.4691(3) 0.9886(6) 0.9184(4) 0.0354(14) Uani 1 1 d . . . . .
H27 H 0.439548 1.013703 0.947646 0.042 Uiso 1 1 calc R U . . .
C28 C 0.4713(2) 0.8644(6) 0.8792(3) 0.0344(13) Uani 1 1 d . . . . .
H28 H 0.442898 0.806046 0.882978 0.041 Uiso 1 1 calc R U . . .
C29 C 0.5145(2) 0.8259(5) 0.8350(3) 0.0302(12) Uani 1 1 d . . . . .
H29 H 0.514789 0.742226 0.809492 0.036 Uiso 1 1 calc R U . . .
C30 C 0.5586(2) 0.9118(5) 0.8278(3) 0.0247(11) Uani 1 1 d . . . . .
O31 O 0.59917(15) 0.8737(3) 0.7838(2) 0.0259(8) Uani 1 1 d . . . . .
O41 O 0.52770(15) 0.7932(3) 0.6251(2) 0.0243(8) Uani 1 1 d . . . . .
C42 C 0.4841(2) 0.7329(5) 0.5895(3) 0.0241(11) Uani 1 1 d . . . . .
C43 C 0.4889(3) 0.6136(5) 0.5446(4) 0.0334(13) Uani 1 1 d . . . . .
H43 H 0.522291 0.573747 0.543486 0.040 Uiso 1 1 calc R U . . .
C44 C 0.4443(3) 0.5539(6) 0.5014(4) 0.0413(15) Uani 1 1 d . . . . .
H44 H 0.448144 0.475021 0.470959 0.050 Uiso 1 1 calc R U . . .
C45 C 0.3942(3) 0.6104(6) 0.5033(4) 0.0476(18) Uani 1 1 d . . . . .
H45 H 0.364411 0.570077 0.474220 0.057 Uiso 1 1 calc R U . . .
C46 C 0.3889(3) 0.7267(6) 0.5485(4) 0.0385(15) Uani 1 1 d . . . . .
H46 H 0.355190 0.764515 0.549860 0.046 Uiso 1 1 calc R U . . .
C47 C 0.4333(2) 0.7904(5) 0.5931(3) 0.0309(13) Uani 1 1 d . . . . .
C48 C 0.4251(2) 0.9132(6) 0.6414(3) 0.0309(12) Uani 1 1 d . . . . .
C481 C 0.3730(3) 0.9275(7) 0.6834(5) 0.0477(17) Uani 1 1 d . . . . .
H48A H 0.352131 0.996628 0.654088 0.072 Uiso 1 1 calc R U . . .
H48B H 0.380038 0.949428 0.744893 0.072 Uiso 1 1 calc R U . . .
H48C H 0.353565 0.845667 0.678092 0.072 Uiso 1 1 calc R U . . .
N49 N 0.4613(2) 1.0046(5) 0.6501(3) 0.0269(10) Uani 1 1 d . . . . .
C50 C 0.4471(3) 1.1272(6) 0.6970(4) 0.0353(14) Uani 1 1 d . . . . .
H50A H 0.444092 1.106271 0.758871 0.042 Uiso 1 1 calc R U . . .
H50B H 0.412290 1.157308 0.672421 0.042 Uiso 1 1 calc R U . . .
C51 C 0.4866(3) 1.2380(6) 0.6911(4) 0.0383(14) Uani 1 1 d . . . . .
H51A H 0.518185 1.218710 0.730205 0.046 Uiso 1 1 calc R U . . .
H51B H 0.471013 1.319108 0.711555 0.046 Uiso 1 1 calc R U . . .
C52 C 0.5032(3) 1.2593(6) 0.5979(4) 0.0383(14) Uani 1 1 d . . . . .
H52A H 0.472678 1.247196 0.555331 0.046 Uiso 1 1 calc R U . . .
H52B H 0.516498 1.348747 0.591989 0.046 Uiso 1 1 calc R U . . .
N53 N 0.54554(19) 1.1631(4) 0.5806(3) 0.0285(10) Uani 1 1 d . . . . .
C54 C 0.5858(2) 1.2057(5) 0.5409(3) 0.0281(11) Uani 1 1 d . . . . .
H54 H 0.584062 1.292703 0.520819 0.034 Uiso 1 1 calc R U . . .
C55 C 0.6331(2) 1.1316(5) 0.5245(3) 0.0270(12) Uani 1 1 d . . . . .
C56 C 0.6725(2) 1.1998(5) 0.4800(3) 0.0326(13) Uani 1 1 d . . . . .
H56 H 0.665592 1.285138 0.459196 0.039 Uiso 1 1 calc R U . . .
C57 C 0.7197(2) 1.1427(6) 0.4674(3) 0.0325(12) Uani 1 1 d . . . . .
H57 H 0.745325 1.189140 0.438741 0.039 Uiso 1 1 calc R U . . .
C58 C 0.7305(3) 1.0133(6) 0.4974(3) 0.0324(13) Uani 1 1 d . . . . .
H58 H 0.763301 0.974292 0.488962 0.039 Uiso 1 1 calc R U . . .
C59 C 0.6923(2) 0.9435(5) 0.5396(3) 0.0262(11) Uani 1 1 d . . . . .
H59 H 0.699504 0.857047 0.558098 0.031 Uiso 1 1 calc R U . . .
C60 C 0.6429(2) 1.0015(5) 0.5549(3) 0.0239(11) Uani 1 1 d . . . . .
O61 O 0.60768(15) 0.9340(3) 0.5977(2) 0.0268(8) Uani 1 1 d . . . . .
N1 N 0.5874(2) 0.5560(4) 0.7486(3) 0.0311(11) Uani 1 1 d . . . . .
N2 N 0.5881(2) 0.5298(4) 0.8236(3) 0.0287(10) Uani 1 1 d . . . . .
N3 N 0.5888(2) 0.5013(5) 0.8987(3) 0.0446(14) Uani 1 1 d . . . . .
O1W O 0.63399(19) 0.6151(4) 0.5631(3) 0.0382(10) Uani 1 1 d D . . . .
O2W O 0.7321(3) 0.4948(7) 0.5734(4) 0.0763(17) Uani 1 1 d D . . . .
Cl8 Cl 0.83553(6) 0.27243(14) 0.99206(9) 0.0356(3) Uani 1 1 d . . . . .
O81 O 0.8607(2) 0.3982(5) 0.9986(3) 0.0599(14) Uani 1 1 d . . . . .
O82 O 0.8401(3) 0.2148(7) 0.9086(4) 0.110(3) Uani 1 1 d . . . . .
O83 O 0.7798(2) 0.2927(6) 0.9976(6) 0.100(2) Uani 1 1 d . . . . .
O84 O 0.8568(3) 0.1890(5) 1.0580(4) 0.095(2) Uani 1 1 d . . . . .
H11W H 0.665(2) 0.583(10) 0.574(6) 0.143 Uiso 1 1 d D U . . .
H21W H 0.743(5) 0.576(4) 0.576(7) 0.143 Uiso 1 1 d D U . . .
H12W H 0.621(4) 0.582(10) 0.515(4) 0.143 Uiso 1 1 d D U . . .
H22W H 0.739(5) 0.466(9) 0.522(4) 0.143 Uiso 1 1 d D U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O31 1.919(4) . ?
Ni1 O11 1.926(3) . ?
Ni1 N23 1.931(4) . ?
Ni1 N19 1.979(5) . ?
Ni2 O41 1.915(3) . ?
Ni2 N53 1.926(4) . ?
Ni2 O61 1.927(4) . ?
Ni2 N49 1.984(5) . ?
Mn3 O11 2.133(4) . ?
Mn3 O41 2.134(4) . ?
Mn3 N1 2.156(4) . ?
Mn3 O1W 2.187(4) . ?
Mn3 O31 2.243(3) . ?
Mn3 O61 2.371(3) . ?
O11 C12 1.342(6) . ?
C12 C13 1.395(7) . ?
C12 C17 1.410(7) . ?
C13 C14 1.383(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.367(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.372(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.400(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.476(7) . ?
C18 N19 1.303(8) . ?
C18 C181 1.514(8) . ?
C181 H18A 0.9600 . ?
C181 H18B 0.9600 . ?
C181 H18C 0.9600 . ?
N19 C20 1.485(6) . ?
C20 C21 1.506(8) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.520(8) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N23 1.472(7) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N23 C24 1.288(7) . ?
C24 C25 1.427(8) . ?
C24 H24 0.9300 . ?
C25 C30 1.412(7) . ?
C25 C26 1.424(8) . ?
C26 C27 1.378(9) . ?
C26 H26 0.9300 . ?
C27 C28 1.392(8) . ?
C27 H27 0.9300 . ?
C28 C29 1.374(8) . ?
C28 H28 0.9300 . ?
C29 C30 1.417(8) . ?
C29 H29 0.9300 . ?
C30 O31 1.319(6) . ?
O41 C42 1.328(6) . ?
C42 C43 1.394(7) . ?
C42 C47 1.406(8) . ?
C43 C44 1.389(8) . ?
C43 H43 0.9300 . ?
C44 C45 1.384(10) . ?
C44 H44 0.9300 . ?
C45 C46 1.372(9) . ?
C45 H45 0.9300 . ?
C46 C47 1.411(8) . ?
C46 H46 0.9300 . ?
C47 C48 1.463(8) . ?
C48 N49 1.294(8) . ?
C48 C481 1.507(8) . ?
C481 H48A 0.9600 . ?
C481 H48B 0.9600 . ?
C481 H48C 0.9600 . ?
N49 C50 1.485(7) . ?
C50 C51 1.504(9) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
C51 C52 1.519(8) . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C52 N53 1.478(7) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
N53 C54 1.290(7) . ?
C54 C55 1.441(8) . ?
C54 H54 0.9300 . ?
C55 C60 1.408(7) . ?
C55 C56 1.419(7) . ?
C56 C57 1.345(8) . ?
C56 H56 0.9300 . ?
C57 C58 1.404(8) . ?
C57 H57 0.9300 . ?
C58 C59 1.386(8) . ?
C58 H58 0.9300 . ?
C59 C60 1.409(8) . ?
C59 H59 0.9300 . ?
C60 O61 1.326(6) . ?
N1 N2 1.165(6) . ?
N2 N3 1.174(6) . ?
O1W H11W 0.86(2) . ?
O1W H12W 0.85(2) . ?
O2W H21W 0.86(2) . ?
O2W H22W 0.85(2) . ?
Cl8 O84 1.383(5) . ?
Cl8 O82 1.405(6) . ?
Cl8 O81 1.419(4) . ?
Cl8 O83 1.421(6) . ?

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
O31 Ni1 O11 81.63(15) . . ?
O31 Ni1 N23 92.90(17) . . ?
O11 Ni1 N23 174.47(18) . . ?
O31 Ni1 N19 170.01(15) . . ?
O11 Ni1 N19 89.00(16) . . ?
N23 Ni1 N19 96.51(18) . . ?
O41 Ni2 N53 171.33(18) . . ?
O41 Ni2 O61 82.03(15) . . ?
N53 Ni2 O61 92.83(17) . . ?
O41 Ni2 N49 89.87(18) . . ?
N53 Ni2 N49 96.4(2) . . ?
O61 Ni2 N49 166.95(16) . . ?
O11 Mn3 O41 144.45(12) . . ?
O11 Mn3 N1 106.77(16) . . ?
O41 Mn3 N1 101.54(16) . . ?
O11 Mn3 O1W 94.74(15) . . ?
O41 Mn3 O1W 104.20(16) . . ?
N1 Mn3 O1W 94.35(18) . . ?
O11 Mn3 O31 70.04(13) . . ?
O41 Mn3 O31 86.31(13) . . ?
N1 Mn3 O31 95.76(16) . . ?
O1W Mn3 O31 163.66(16) . . ?
O11 Mn3 O61 81.23(13) . . ?
O41 Mn3 O61 67.83(13) . . ?
N1 Mn3 O61 167.83(16) . . ?
O1W Mn3 O61 94.09(15) . . ?
O31 Mn3 O61 78.12(12) . . ?
C12 O11 Ni1 113.7(3) . . ?
C12 O11 Mn3 137.1(3) . . ?
Ni1 O11 Mn3 100.49(15) . . ?
O11 C12 C13 119.7(5) . . ?
O11 C12 C17 120.9(4) . . ?
C13 C12 C17 119.5(5) . . ?
C14 C13 C12 120.1(5) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C13 120.9(5) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 119.6(5) . . ?
C14 C15 H15 120.2 . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C17 121.7(6) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C16 C17 C12 118.1(5) . . ?
C16 C17 C18 119.7(5) . . ?
C12 C17 C18 122.1(5) . . ?
N19 C18 C17 120.5(5) . . ?
N19 C18 C181 121.5(5) . . ?
C17 C18 C181 118.0(5) . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 N19 C20 116.9(5) . . ?
C18 N19 Ni1 122.7(3) . . ?
C20 N19 Ni1 120.3(4) . . ?
N19 C20 C21 113.2(5) . . ?
N19 C20 H20A 108.9 . . ?
C21 C20 H20A 108.9 . . ?
N19 C20 H20B 108.9 . . ?
C21 C20 H20B 108.9 . . ?
H20A C20 H20B 107.8 . . ?
C20 C21 C22 111.9(4) . . ?
C20 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N23 C22 C21 108.2(4) . . ?
N23 C22 H22A 110.1 . . ?
C21 C22 H22A 110.1 . . ?
N23 C22 H22B 110.1 . . ?
C21 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?
C24 N23 C22 117.7(4) . . ?
C24 N23 Ni1 124.8(4) . . ?
C22 N23 Ni1 117.5(4) . . ?
N23 C24 C25 127.3(5) . . ?
N23 C24 H24 116.4 . . ?
C25 C24 H24 116.4 . . ?
C30 C25 C26 119.0(5) . . ?
C30 C25 C24 123.6(5) . . ?
C26 C25 C24 117.3(5) . . ?
C27 C26 C25 121.5(5) . . ?
C27 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C26 C27 C28 118.8(5) . . ?
C26 C27 H27 120.6 . . ?
C28 C27 H27 120.6 . . ?
C29 C28 C27 121.5(6) . . ?
C29 C28 H28 119.3 . . ?
C27 C28 H28 119.3 . . ?
C28 C29 C30 121.0(5) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
O31 C30 C25 121.8(5) . . ?
O31 C30 C29 120.0(5) . . ?
C25 C30 C29 118.2(5) . . ?
C30 O31 Ni1 128.8(3) . . ?
C30 O31 Mn3 132.4(3) . . ?
Ni1 O31 Mn3 96.95(15) . . ?
C42 O41 Ni2 119.0(3) . . ?
C42 O41 Mn3 134.5(3) . . ?
Ni2 O41 Mn3 104.76(17) . . ?
O41 C42 C43 119.6(5) . . ?
O41 C42 C47 121.0(5) . . ?
C43 C42 C47 119.4(5) . . ?
C44 C43 C42 120.5(6) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C45 C44 C43 120.8(6) . . ?
C45 C44 H44 119.6 . . ?
C43 C44 H44 119.6 . . ?
C46 C45 C44 119.2(6) . . ?
C46 C45 H45 120.4 . . ?
C44 C45 H45 120.4 . . ?
C45 C46 C47 121.8(6) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 H46 119.1 . . ?
C42 C47 C46 118.4(5) . . ?
C42 C47 C48 122.3(5) . . ?
C46 C47 C48 119.3(5) . . ?
N49 C48 C47 122.0(5) . . ?
N49 C48 C481 120.9(6) . . ?
C47 C48 C481 117.0(6) . . ?
C48 C481 H48A 109.5 . . ?
C48 C481 H48B 109.5 . . ?
H48A C481 H48B 109.5 . . ?
C48 C481 H48C 109.5 . . ?
H48A C481 H48C 109.5 . . ?
H48B C481 H48C 109.5 . . ?
C48 N49 C50 116.8(5) . . ?
C48 N49 Ni2 122.6(4) . . ?
C50 N49 Ni2 120.4(4) . . ?
N49 C50 C51 114.1(5) . . ?
N49 C50 H50A 108.7 . . ?
C51 C50 H50A 108.7 . . ?
N49 C50 H50B 108.7 . . ?
C51 C50 H50B 108.7 . . ?
H50A C50 H50B 107.6 . . ?
C50 C51 C52 113.1(5) . . ?
C50 C51 H51A 109.0 . . ?
C52 C51 H51A 109.0 . . ?
C50 C51 H51B 109.0 . . ?
C52 C51 H51B 109.0 . . ?
H51A C51 H51B 107.8 . . ?
N53 C52 C51 109.0(4) . . ?
N53 C52 H52A 109.9 . . ?
C51 C52 H52A 109.9 . . ?
N53 C52 H52B 109.9 . . ?
C51 C52 H52B 109.9 . . ?
H52A C52 H52B 108.3 . . ?
C54 N53 C52 117.6(5) . . ?
C54 N53 Ni2 124.5(4) . . ?
C52 N53 Ni2 117.7(4) . . ?
N53 C54 C55 126.4(5) . . ?
N53 C54 H54 116.8 . . ?
C55 C54 H54 116.8 . . ?
C60 C55 C56 119.9(5) . . ?
C60 C55 C54 123.6(5) . . ?
C56 C55 C54 116.4(5) . . ?
C57 C56 C55 121.0(5) . . ?
C57 C56 H56 119.5 . . ?
C55 C56 H56 119.5 . . ?
C56 C57 C58 120.1(5) . . ?
C56 C57 H57 119.9 . . ?
C58 C57 H57 119.9 . . ?
C59 C58 C57 120.1(6) . . ?
C59 C58 H58 120.0 . . ?
C57 C58 H58 120.0 . . ?
C58 C59 C60 120.9(5) . . ?
C58 C59 H59 119.5 . . ?
C60 C59 H59 119.5 . . ?
O61 C60 C55 122.3(5) . . ?
O61 C60 C59 119.7(4) . . ?
C55 C60 C59 117.9(5) . . ?
C60 O61 Ni2 127.2(3) . . ?
C60 O61 Mn3 136.6(3) . . ?
Ni2 O61 Mn3 96.08(14) . . ?
N2 N1 Mn3 135.5(4) . . ?
N1 N2 N3 178.8(6) . . ?
Mn3 O1W H11W 114(7) . . ?
Mn3 O1W H12W 137(7) . . ?
H11W O1W H12W 108(4) . . ?
H21W O2W H22W 106(4) . . ?
O84 Cl8 O82 110.1(4) . . ?
O84 Cl8 O81 110.5(4) . . ?
O82 Cl8 O81 111.5(4) . . ?
O84 Cl8 O83 111.7(5) . . ?
O82 Cl8 O83 105.3(5) . . ?
O81 Cl8 O83 107.5(4) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O2W 0.86(2) 1.90(3) 2.738(8) 168(9) .
O2W H21W O83 0.86(2) 2.05(7) 2.754(9) 138(9) 2_564
O1W H12W N3 0.85(2) 2.06(2) 2.902(6) 179(11) 2_564

_refine_diff_density_max         0.787
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.083

####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1857028'
_audit_update_record             
;
2018-08-29 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H76 Cl3 Mn2 N11 Ni4 O22'
_chemical_formula_weight         1898.50

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   21.8470(7)
_cell_length_b                   13.0063(7)
_cell_length_c                   30.2495(11)
_cell_angle_alpha                90
_cell_angle_beta                 101.600(3)
_cell_angle_gamma                90
_cell_volume                     8419.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    67197
_cell_measurement_theta_min      2.612
_cell_measurement_theta_max      26.457

_exptl_crystal_description       Prisamatic
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_F_000             3896
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.338
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67197
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.612
_diffrn_reflns_theta_max         26.457
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8649
_reflns_number_gt                6584
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'

_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)+(0.1262P)²+22.0480P] 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         8649
_refine_ls_number_parameters     551
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0686
_refine_ls_wR_factor_ref         0.2215
_refine_ls_wR_factor_gt          0.2006
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.002
_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 0.90098(3) 0.16900(4) 0.63535(2) 0.04775(19) Uani 1 1 d . . . . .
Ni2 Ni 1.06100(3) 0.08866(5) 0.59423(2) 0.0636(2) Uani 1 1 d . . . . .
Mn3 Mn 0.97715(3) -0.03296(6) 0.64742(2) 0.0567(2) Uani 1 1 d . . . . .
O11 O 0.88607(15) 0.0289(3) 0.64088(11) 0.0559(7) Uani 1 1 d . . . . .
C12 C 0.8360(2) 0.0075(4) 0.65786(15) 0.0558(11) Uani 1 1 d . . . . .
C13 C 0.8400(3) -0.0612(5) 0.69324(19) 0.0744(15) Uani 1 1 d . . . . .
H13 H 0.877398 -0.095101 0.704322 0.089 Uiso 1 1 calc R U . . .
C14 C 0.7879(4) -0.0800(6) 0.7124(3) 0.101(2) Uani 1 1 d . . . . .
H14 H 0.791046 -0.123834 0.737041 0.121 Uiso 1 1 calc R U . . .
C15 C 0.7322(4) -0.0332(7) 0.6945(3) 0.111(3) Uani 1 1 d . . . . .
H15 H 0.697370 -0.045426 0.707094 0.134 Uiso 1 1 calc R U . . .
C16 C 0.7273(3) 0.0307(5) 0.6586(3) 0.092(2) Uani 1 1 d . . . . .
H16 H 0.688637 0.059015 0.646118 0.110 Uiso 1 1 calc R U . . .
C17 C 0.7792(2) 0.0555(4) 0.63987(19) 0.0647(13) Uani 1 1 d . . . . .
C18 C 0.7748(2) 0.1254(5) 0.60195(19) 0.0670(13) Uani 1 1 d . . . . .
N19 N 0.82137(19) 0.1819(3) 0.59666(13) 0.0574(9) Uani 1 1 d . . . . .
C20 C 0.8137(3) 0.2476(5) 0.55662(18) 0.0780(16) Uani 1 1 d . . . . .
H20A H 0.774739 0.285206 0.553622 0.094 Uiso 1 1 calc R U . . .
H20B H 0.810862 0.204549 0.530116 0.094 Uiso 1 1 calc R U . . .
C21 C 0.8652(3) 0.3217(5) 0.5581(2) 0.0846(18) Uani 1 1 d . . . . .
H21C H 0.853296 0.372065 0.534237 0.102 Uiso 1 1 calc R U . . .
H21D H 0.901878 0.285678 0.552703 0.102 Uiso 1 1 calc R U . . .
C22 C 0.8809(3) 0.3764(5) 0.6033(2) 0.0750(15) Uani 1 1 d . . . . .
H22A H 0.902772 0.440126 0.600258 0.090 Uiso 1 1 calc R U . . .
H22B H 0.842910 0.392590 0.613764 0.090 Uiso 1 1 calc R U . . .
N23 N 0.9203(2) 0.3092(3) 0.63551(13) 0.0563(9) Uani 1 1 d . . . . .
C24 C 0.9677(2) 0.3504(4) 0.66129(17) 0.0593(11) Uani 1 1 d . . . . .
H24 H 0.970970 0.421575 0.659758 0.071 Uiso 1 1 calc R U . . .
C25 C 1.0163(2) 0.2985(4) 0.69224(16) 0.0573(11) Uani 1 1 d . . . . .
C26 C 1.0630(3) 0.3578(5) 0.7194(2) 0.0739(15) Uani 1 1 d . . . . .
H26 H 1.060626 0.429103 0.717687 0.089 Uiso 1 1 calc R U . . .
C27 C 1.1107(3) 0.3142(5) 0.7477(2) 0.0771(16) Uani 1 1 d . . . . .
H27 H 1.140653 0.354809 0.765873 0.093 Uiso 1 1 calc R U . . .
C28 C 1.1154(3) 0.2084(5) 0.74970(18) 0.0723(15) Uani 1 1 d . . . . .
H28 H 1.149018 0.178066 0.769001 0.087 Uiso 1 1 calc R U . . .
C29 C 1.0712(2) 0.1475(4) 0.72373(16) 0.0627(12) Uani 1 1 d . . . . .
H29 H 1.074759 0.076324 0.725627 0.075 Uiso 1 1 calc R U . . .
C30 C 1.0204(2) 0.1925(4) 0.69424(14) 0.0507(10) Uani 1 1 d . . . . .
O31 O 0.97752(14) 0.1325(3) 0.66922(10) 0.0545(7) Uani 1 1 d . . . . .
O41 O 1.06953(15) -0.0076(3) 0.63963(12) 0.0644(9) Uani 1 1 d . . . . .
C42 C 1.1245(3) -0.0579(5) 0.65214(17) 0.0691(15) Uani 1 1 d . . . . .
C43 C 1.1238(3) -0.1597(5) 0.6629(2) 0.088(2) Uani 1 1 d . . . . .
H43 H 1.085677 -0.191667 0.662763 0.105 Uiso 1 1 calc R U . . .
C44 C 1.1777(5) -0.2164(7) 0.6737(3) 0.119(3) Uani 1 1 d . . . . .
H44 H 1.176717 -0.285454 0.681582 0.142 Uiso 1 1 calc R U . . .
C45 C 1.2340(5) -0.1668(10) 0.6726(3) 0.130(4) Uani 1 1 d . . . . .
H45 H 1.270931 -0.204590 0.677429 0.156 Uiso 1 1 calc R U . . .
C46 C 1.2358(3) -0.0630(8) 0.6646(2) 0.106(3) Uani 1 1 d . . . . .
H46 H 1.274053 -0.030549 0.665801 0.127 Uiso 1 1 calc R U . . .
C47 C 1.1809(3) -0.0062(6) 0.6546(2) 0.0813(18) Uani 1 1 d . . . . .
C48 C 1.1825(3) 0.1032(7) 0.6494(2) 0.090(2) Uani 1 1 d . . . . .
N49 N 1.1371(3) 0.1506(4) 0.6240(2) 0.0811(14) Uani 1 1 d . . . . .
C181 C 0.7136(3) 0.1278(7) 0.5672(3) 0.109(3) Uani 1 1 d . . . . .
H18A H 0.720866 0.104116 0.538607 0.164 Uiso 1 1 calc R U . . .
H18B H 0.697864 0.196945 0.564040 0.164 Uiso 1 1 calc R U . . .
H18C H 0.683557 0.083983 0.576940 0.164 Uiso 1 1 calc R U . . .
C50 C 1.1366(4) 0.2646(7) 0.6227(3) 0.111(2) Uani 1 1 d . U . . .
H50D H 1.107882 0.289562 0.640900 0.133 Uiso 1 1 calc R U . . .
H50E H 1.177954 0.289580 0.636145 0.133 Uiso 1 1 calc R U . . .
C51 C 1.1183(8) 0.3076(12) 0.5771(6) 0.206(6) Uani 1 1 d . U . . .
H51A H 1.081762 0.350274 0.576659 0.247 Uiso 1 1 calc R U . . .
H51B H 1.151668 0.352894 0.572397 0.247 Uiso 1 1 calc R U . . .
C52 C 1.1041(5) 0.2392(8) 0.5384(4) 0.134(3) Uani 1 1 d . U . . .
H52A H 1.140731 0.198554 0.536505 0.161 Uiso 1 1 calc R U . . .
H52B H 1.093013 0.279446 0.510918 0.161 Uiso 1 1 calc R U . . .
N53 N 1.0520(3) 0.1708(4) 0.5426(2) 0.0876(16) Uani 1 1 d . . . . .
C481 C 1.2374(4) 0.1616(9) 0.6765(4) 0.141(4) Uani 1 1 d . . . . .
H48A H 1.222360 0.215828 0.693019 0.212 Uiso 1 1 calc R U . . .
H48B H 1.261773 0.190480 0.656440 0.212 Uiso 1 1 calc R U . . .
H48C H 1.262943 0.115563 0.697199 0.212 Uiso 1 1 calc R U . . .
C54 C 1.0057(5) 0.1673(6) 0.5104(2) 0.093(2) Uani 1 1 d . . . . .
H54 H 1.008459 0.208759 0.485861 0.112 Uiso 1 1 calc R U . . .
C55 C 0.9492(4) 0.1087(6) 0.50598(18) 0.089(2) Uani 1 1 d . . . . .
C56 C 0.9026(5) 0.1168(8) 0.4674(2) 0.107(3) Uani 1 1 d . . . . .
H56 H 0.909506 0.159117 0.444096 0.129 Uiso 1 1 calc R U . . .
C57 C 0.8500(5) 0.0680(9) 0.4624(2) 0.127(4) Uani 1 1 d . . . . .
H57 H 0.819975 0.076202 0.436116 0.152 Uiso 1 1 calc R U . . .
C58 C 0.8382(4) 0.0031(8) 0.4965(3) 0.120(3) Uani 1 1 d . . . . .
H58 H 0.800186 -0.031283 0.492761 0.144 Uiso 1 1 calc R U . . .
C59 C 0.8825(3) -0.0108(6) 0.5356(2) 0.089(2) Uani 1 1 d . . . . .
H59 H 0.874745 -0.054836 0.558082 0.107 Uiso 1 1 calc R U . . .
C60 C 0.9387(3) 0.0423(5) 0.54089(17) 0.0763(17) Uani 1 1 d . . . . .
O61 O 0.98166(17) 0.0294(3) 0.57831(11) 0.0671(9) Uani 1 1 d . . . . .
N1 N 1.0043(3) -0.1008(4) 0.71265(19) 0.0880(15) Uani 1 1 d . . . . .
N2 N 1.000000 -0.0967(4) 0.750000 0.0600(15) Uani 1 2 d S T P . .
O1W O 0.9487(3) -0.1844(4) 0.6215(2) 0.121(2) Uani 1 1 d . . . . .
Cl8 Cl 0.9763(3) 0.4185(4) 0.4268(3) 0.178(3) Uani 0.5 1 d D . P . .
Cl7 Cl 1.4168(2) 0.1235(3) 0.7161(3) 0.154(2) Uani 0.5 1 d D . P . .
Cl9 Cl 0.6869(3) -0.1610(5) 0.4407(3) 0.174(3) Uani 0.5 1 d D . P . .
O72 O 1.3796(12) 0.0439(18) 0.7086(10) 0.169(4) Uiso 0.25 1 d D U P A 1
O73 O 1.3968(13) 0.2130(15) 0.7275(10) 0.169(4) Uiso 0.25 1 d D U P A 1
O74 O 1.4640(12) 0.094(2) 0.7569(8) 0.169(4) Uiso 0.25 1 d D U P A 1
O71 O 1.4578(13) 0.130(2) 0.6855(9) 0.169(4) Uiso 0.25 1 d D U P A 1
O81 O 1.0032(16) 0.5120(17) 0.4391(11) 0.201(6) Uiso 0.25 1 d D U P B 1
O82 O 0.9413(15) 0.423(3) 0.3833(7) 0.201(6) Uiso 0.25 1 d D U P B 1
O83 O 0.9443(15) 0.386(3) 0.4577(10) 0.201(6) Uiso 0.25 1 d D U P B 1
O84 O 1.0255(13) 0.351(2) 0.4254(12) 0.201(6) Uiso 0.25 1 d D U P B 1
O91 O 0.7149(16) -0.094(2) 0.4190(12) 0.192(5) Uiso 0.25 1 d D U P C 1
O92 O 0.6842(17) -0.2605(17) 0.4225(11) 0.192(5) Uiso 0.25 1 d D U P C 1
O93 O 0.7262(14) -0.180(3) 0.4846(7) 0.192(5) Uiso 0.25 1 d D U P C 1
O94 O 0.6306(10) -0.134(3) 0.4479(12) 0.192(5) Uiso 0.25 1 d D U P C 1
O95 O 0.6848(17) -0.109(2) 0.4809(8) 0.192(5) Uiso 0.25 1 d D U P C 2
O96 O 0.7161(15) -0.2546(18) 0.4524(12) 0.192(5) Uiso 0.25 1 d D U P C 2
O97 O 0.7251(15) -0.106(3) 0.4188(12) 0.192(5) Uiso 0.25 1 d D U P C 2
O98 O 0.6293(10) -0.173(3) 0.4170(10) 0.192(5) Uiso 0.25 1 d D U P C 2
O75 O 1.3989(13) 0.2102(17) 0.6909(9) 0.169(4) Uiso 0.25 1 d D U P A 2
O76 O 1.3917(13) 0.0407(18) 0.6905(9) 0.169(4) Uiso 0.25 1 d D U P A 2
O77 O 1.4807(7) 0.114(2) 0.7230(11) 0.169(4) Uiso 0.25 1 d D U P A 2
O78 O 1.3953(13) 0.128(2) 0.7555(7) 0.169(4) Uiso 0.25 1 d D U P A 2
O85 O 0.9770(17) 0.3204(14) 0.4141(11) 0.201(6) Uiso 0.25 1 d D U P B 2
O87 O 1.0309(11) 0.456(3) 0.4527(11) 0.201(6) Uiso 0.25 1 d D U P B 2
O86 O 0.9350(15) 0.427(3) 0.4580(10) 0.201(6) Uiso 0.25 1 d D U P B 2
O88 O 0.9554(16) 0.482(2) 0.3918(9) 0.201(6) Uiso 0.25 1 d D U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O31 1.839(3) . ?
Ni1 O11 1.864(3) . ?
Ni1 N23 1.871(4) . ?
Ni1 N19 1.899(4) . ?
Ni1 Mn3 3.0915(9) . ?
Ni2 O41 1.840(4) . ?
Ni2 N53 1.869(5) . ?
Ni2 O61 1.870(4) . ?
Ni2 N49 1.903(6) . ?
Ni2 Mn3 3.1036(10) . ?
Mn3 O41 2.105(4) . ?
Mn3 O11 2.118(3) . ?
Mn3 N1 2.134(5) . ?
Mn3 O1W 2.165(5) . ?
Mn3 O31 2.250(3) . ?
Mn3 O61 2.263(4) . ?
O11 C12 1.327(6) . ?
C12 C13 1.384(7) . ?
C12 C17 1.398(7) . ?
C13 C14 1.397(9) . ?
C14 C15 1.373(12) . ?
C15 C16 1.353(12) . ?
C16 C17 1.404(8) . ?
C17 C18 1.452(8) . ?
C18 N19 1.291(7) . ?
C18 C181 1.526(7) . ?
N19 C20 1.465(7) . ?
C20 C21 1.474(9) . ?
C21 C22 1.519(9) . ?
C22 N23 1.455(7) . ?
N23 C24 1.282(6) . ?
C24 C25 1.434(7) . ?
C25 C30 1.383(7) . ?
C25 C26 1.406(7) . ?
C26 C27 1.334(9) . ?
C27 C28 1.380(9) . ?
C28 C29 1.368(7) . ?
C29 C30 1.403(7) . ?
C30 O31 1.332(5) . ?
O41 C42 1.352(6) . ?
C42 C43 1.365(9) . ?
C42 C47 1.392(9) . ?
C43 C44 1.372(10) . ?
C44 C45 1.397(15) . ?
C45 C46 1.373(14) . ?
C46 C47 1.391(9) . ?
C47 C48 1.432(11) . ?
C48 N49 1.283(9) . ?
C48 C481 1.515(10) . ?
N49 C50 1.483(10) . ?
C50 C51 1.467(17) . ?
C51 C52 1.453(17) . ?
C52 N53 1.471(11) . ?
N53 C54 1.257(10) . ?
C54 C55 1.432(11) . ?
C55 C56 1.390(10) . ?
C55 C60 1.419(10) . ?
C56 C57 1.296(13) . ?
C57 C58 1.394(15) . ?
C58 C59 1.382(9) . ?
C59 C60 1.389(10) . ?
C60 O61 1.328(6) . ?
N1 N2 1.154(6) . ?
Cl8 O85 1.334(15) . ?
Cl8 O83 1.343(15) . ?
Cl8 O88 1.351(16) . ?
Cl8 O81 1.368(16) . ?
Cl8 O87 1.378(16) . ?
Cl8 O82 1.384(15) . ?
Cl8 O84 1.397(16) . ?
Cl8 O86 1.434(16) . ?
Cl7 O72 1.307(15) . ?
Cl7 O73 1.313(14) . ?
Cl7 O78 1.368(14) . ?
Cl7 O75 1.373(15) . ?
Cl7 O77 1.375(14) . ?
Cl7 O76 1.375(15) . ?
Cl7 O71 1.416(15) . ?
Cl7 O74 1.491(15) . ?
Cl9 O91 1.313(15) . ?
Cl9 O98 1.326(15) . ?
Cl9 O94 1.340(15) . ?
Cl9 O97 1.368(15) . ?
Cl9 O96 1.386(15) . ?
Cl9 O95 1.400(16) . ?
Cl9 O92 1.402(16) . ?
Cl9 O93 1.450(16) . ?
O74 O74 1.71(6) 2_856 ?
O77 O77 1.68(6) 2_856 ?

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
O31 Ni1 O11 81.58(14) . . ?
O31 Ni1 N23 94.05(17) . . ?
O11 Ni1 N23 174.49(16) . . ?
O31 Ni1 N19 169.69(16) . . ?
O11 Ni1 N19 89.23(16) . . ?
N23 Ni1 N19 95.39(18) . . ?
O31 Ni1 Mn3 46.17(10) . . ?
O11 Ni1 Mn3 42.15(10) . . ?
N23 Ni1 Mn3 135.39(13) . . ?
N19 Ni1 Mn3 123.53(13) . . ?
O41 Ni2 N53 171.9(2) . . ?
O41 Ni2 O61 82.02(16) . . ?
N53 Ni2 O61 94.8(2) . . ?
O41 Ni2 N49 89.3(2) . . ?
N53 Ni2 N49 95.1(3) . . ?
O61 Ni2 N49 166.67(19) . . ?
O41 Ni2 Mn3 41.24(11) . . ?
N53 Ni2 Mn3 138.6(2) . . ?
O61 Ni2 Mn3 46.37(11) . . ?
N49 Ni2 Mn3 121.43(17) . . ?
O41 Mn3 O11 146.51(14) . . ?
O41 Mn3 N1 94.2(2) . . ?
O11 Mn3 N1 108.95(19) . . ?
O41 Mn3 O1W 108.3(2) . . ?
O11 Mn3 O1W 96.65(19) . . ?
N1 Mn3 O1W 88.0(2) . . ?
O41 Mn3 O31 86.33(13) . . ?
O11 Mn3 O31 67.18(12) . . ?
N1 Mn3 O31 98.09(18) . . ?
O1W Mn3 O31 163.79(19) . . ?
O41 Mn3 O61 67.63(14) . . ?
O11 Mn3 O61 89.55(13) . . ?
N1 Mn3 O61 161.2(2) . . ?
O1W Mn3 O61 93.1(2) . . ?
O31 Mn3 O61 85.97(13) . . ?
O41 Mn3 Ni1 111.05(10) . . ?
O11 Mn3 Ni1 36.21(9) . . ?
N1 Mn3 Ni1 120.24(17) . . ?
O1W Mn3 Ni1 128.45(16) . . ?
O31 Mn3 Ni1 36.12(8) . . ?
O61 Mn3 Ni1 73.07(9) . . ?
O41 Mn3 Ni2 35.19(10) . . ?
O11 Mn3 Ni2 113.53(9) . . ?
N1 Mn3 Ni2 127.36(17) . . ?
O1W Mn3 Ni2 115.6(2) . . ?
O31 Mn3 Ni2 72.35(9) . . ?
O61 Mn3 Ni2 36.73(10) . . ?
Ni1 Mn3 Ni2 82.27(2) . . ?
C12 O11 Ni1 114.4(3) . . ?
C12 O11 Mn3 135.6(3) . . ?
Ni1 O11 Mn3 101.64(14) . . ?
O11 C12 C13 120.5(5) . . ?
O11 C12 C17 119.4(5) . . ?
C13 C12 C17 120.1(5) . . ?
C12 C13 C14 120.3(7) . . ?
C15 C14 C13 119.4(7) . . ?
C16 C15 C14 120.6(7) . . ?
C15 C16 C17 121.7(7) . . ?
C12 C17 C16 117.8(6) . . ?
C12 C17 C18 120.1(5) . . ?
C16 C17 C18 122.1(6) . . ?
N19 C18 C17 121.7(4) . . ?
N19 C18 C181 120.4(6) . . ?
C17 C18 C181 117.9(6) . . ?
C18 N19 C20 118.2(5) . . ?
C18 N19 Ni1 121.4(4) . . ?
C20 N19 Ni1 120.0(4) . . ?
N19 C20 C21 113.4(5) . . ?
C20 C21 C22 111.5(5) . . ?
N23 C22 C21 108.6(5) . . ?
C24 N23 C22 116.9(5) . . ?
C24 N23 Ni1 124.3(3) . . ?
C22 N23 Ni1 118.8(4) . . ?
N23 C24 C25 126.9(5) . . ?
C30 C25 C26 119.2(5) . . ?
C30 C25 C24 122.1(4) . . ?
C26 C25 C24 118.6(5) . . ?
C27 C26 C25 121.6(6) . . ?
C26 C27 C28 119.5(5) . . ?
C29 C28 C27 121.0(6) . . ?
C28 C29 C30 120.0(5) . . ?
O31 C30 C25 121.8(4) . . ?
O31 C30 C29 119.5(4) . . ?
C25 C30 C29 118.7(4) . . ?
C30 O31 Ni1 128.5(3) . . ?
C30 O31 Mn3 133.4(3) . . ?
Ni1 O31 Mn3 97.71(13) . . ?
C42 O41 Ni2 119.3(4) . . ?
C42 O41 Mn3 135.3(4) . . ?
Ni2 O41 Mn3 103.57(15) . . ?
O41 C42 C43 118.9(6) . . ?
O41 C42 C47 120.5(6) . . ?
C43 C42 C47 120.5(6) . . ?
C42 C43 C44 121.9(9) . . ?
C43 C44 C45 117.7(9) . . ?
C46 C45 C44 121.0(8) . . ?
C45 C46 C47 120.5(9) . . ?
C46 C47 C42 118.1(8) . . ?
C46 C47 C48 120.8(7) . . ?
C42 C47 C48 121.0(5) . . ?
N49 C48 C47 120.7(6) . . ?
N49 C48 C481 121.0(8) . . ?
C47 C48 C481 118.2(8) . . ?
C48 N49 C50 119.8(7) . . ?
C48 N49 Ni2 125.1(5) . . ?
C50 N49 Ni2 114.2(5) . . ?
C51 C50 N49 113.9(9) . . ?
C52 C51 C50 119.9(13) . . ?
C51 C52 N53 110.0(11) . . ?
C54 N53 C52 118.1(7) . . ?
C54 N53 Ni2 124.1(6) . . ?
C52 N53 Ni2 117.8(6) . . ?
N53 C54 C55 129.5(7) . . ?
C56 C55 C60 118.0(9) . . ?
C56 C55 C54 120.7(8) . . ?
C60 C55 C54 121.3(6) . . ?
C57 C56 C55 122.9(9) . . ?
C56 C57 C58 120.2(7) . . ?
C59 C58 C57 120.7(9) . . ?
C58 C59 C60 118.9(8) . . ?
O61 C60 C59 119.5(6) . . ?
O61 C60 C55 121.2(7) . . ?
C59 C60 C55 119.3(6) . . ?
C60 O61 Ni2 128.9(4) . . ?
C60 O61 Mn3 132.7(4) . . ?
Ni2 O61 Mn3 96.90(14) . . ?
N2 N1 Mn3 145.5(5) . . ?
N1 N2 N1 174.6(8) . 2_756 ?
O85 Cl8 O88 112.6(15) . . ?
O83 Cl8 O81 110.2(15) . . ?
O85 Cl8 O87 116.4(15) . . ?
O88 Cl8 O87 110.3(15) . . ?
O83 Cl8 O82 114.2(15) . . ?
O81 Cl8 O82 110.3(15) . . ?
O83 Cl8 O84 109.5(15) . . ?
O81 Cl8 O84 106.2(14) . . ?
O82 Cl8 O84 106.0(14) . . ?
O85 Cl8 O86 108.2(15) . . ?
O88 Cl8 O86 107.8(14) . . ?
O87 Cl8 O86 100.6(14) . . ?
O72 Cl7 O73 121.3(15) . . ?
O78 Cl7 O75 109.8(13) . . ?
O78 Cl7 O77 112.8(14) . . ?
O75 Cl7 O77 108.9(14) . . ?
O78 Cl7 O76 110.9(14) . . ?
O75 Cl7 O76 107.1(14) . . ?
O77 Cl7 O76 107.1(13) . . ?
O72 Cl7 O71 112.9(14) . . ?
O73 Cl7 O71 113.9(14) . . ?
O72 Cl7 O74 104.1(13) . . ?
O73 Cl7 O74 102.7(13) . . ?
O71 Cl7 O74 97.7(12) . . ?
O91 Cl9 O94 116.3(16) . . ?
O98 Cl9 O97 113.9(16) . . ?
O98 Cl9 O96 111.8(15) . . ?
O97 Cl9 O96 107.0(14) . . ?
O98 Cl9 O95 109.4(14) . . ?
O97 Cl9 O95 107.3(15) . . ?
O96 Cl9 O95 107.1(14) . . ?
O91 Cl9 O92 113.9(16) . . ?
O94 Cl9 O92 109.8(15) . . ?
O91 Cl9 O93 108.9(15) . . ?
O94 Cl9 O93 106.7(14) . . ?
O92 Cl9 O93 99.8(13) . . ?

_refine_diff_density_max         1.396
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.102

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1857026'
_audit_update_record             
;
2018-08-29 deposited with the CCDC.
2018-09-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H37.50 Mn N6.50 Ni2 O4 S2'
_chemical_formula_weight         897.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   17.790(4)
_cell_length_b                   13.0863(17)
_cell_length_c                   19.171(5)
_cell_angle_alpha                90
_cell_angle_beta                 116.90(3)
_cell_angle_gamma                90
_cell_volume                     3980.1(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    20559
_cell_measurement_theta_min      3.334
_cell_measurement_theta_max      27.499

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_F_000             1848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_T_max  0.766

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_measurement_device_type  'Oxford Diffraction X-Calibor System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_decay_%        n/a
_diffrn_reflns_number            20559
_diffrn_reflns_av_unetI/netI     0.1349
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.334
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             9030
_reflns_number_gt                5714
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_publication_material  'SHELXL-2016/6, PLATON, WINGX (Ferrugia, 2012)'
_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)+(0.0549P)²+14.2790P] 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         9030
_refine_ls_number_parameters     520
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.1635
_refine_ls_R_factor_gt           0.1093
_refine_ls_wR_factor_ref         0.2323
_refine_ls_wR_factor_gt          0.2100
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.145
_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
Ni2 Ni 0.26802(7) 0.44098(9) 1.10652(7) 0.0454(3) Uani 1 1 d . . . . .
Ni1 Ni 0.44536(6) 0.63370(7) 1.11629(6) 0.0266(2) Uani 1 1 d . . . . .
Mn3 Mn 0.24579(7) 0.62328(8) 0.99815(7) 0.0309(3) Uani 1 1 d . . . . .
N1 N 0.2359(4) 0.6137(5) 0.8832(5) 0.0433(18) Uani 1 1 d . . . . .
C1 C 0.2227(5) 0.6153(5) 0.8175(5) 0.0350(19) Uani 1 1 d . . . . .
S1 S 0.20227(18) 0.6165(2) 0.72723(15) 0.0574(7) Uani 1 1 d . . . . .
N2 N 0.1539(4) 0.7376(5) 0.9787(4) 0.0410(17) Uani 1 1 d . . . . .
S2 S 0.08498(17) 0.91426(17) 1.00713(17) 0.0598(7) Uani 1 1 d . . . . .
C2 C 0.1263(5) 0.8119(7) 0.9908(5) 0.045(2) Uani 1 1 d . . . . .
O11 O 0.3525(3) 0.7185(3) 1.0533(3) 0.0333(13) Uani 1 1 d . . . . .
C12 C 0.3659(5) 0.8165(5) 1.0409(5) 0.0336(18) Uani 1 1 d . . . . .
C13 C 0.3182(6) 0.8573(6) 0.9670(6) 0.051(2) Uani 1 1 d . . . . .
H13 H 0.276329 0.817899 0.928667 0.062 Uiso 1 1 calc R U . . .
C14 C 0.3320(7) 0.9552(7) 0.9498(7) 0.065(3) Uani 1 1 d . . . . .
H14 H 0.300302 0.981896 0.900010 0.078 Uiso 1 1 calc R U . . .
C15 C 0.3938(7) 1.0140(8) 1.0078(8) 0.073(4) Uani 1 1 d . . . . .
H15 H 0.405063 1.079468 0.996145 0.088 Uiso 1 1 calc R U . . .
C16 C 0.4380(7) 0.9765(6) 1.0816(7) 0.063(3) Uani 1 1 d . . . . .
H16 H 0.476857 1.018321 1.120324 0.075 Uiso 1 1 calc R U . . .
C17 C 0.4261(5) 0.8748(6) 1.1008(6) 0.042(2) Uani 1 1 d . . . . .
C18 C 0.4740(5) 0.8369(6) 1.1808(6) 0.042(2) Uani 1 1 d . . . . .
N19 N 0.4927(4) 0.7411(5) 1.1961(4) 0.0325(15) Uani 1 1 d . . . . .
C20 C 0.5460(6) 0.7155(7) 1.2795(5) 0.048(2) Uani 1 1 d . . . . .
H20A H 0.513718 0.726177 1.308294 0.058 Uiso 1 1 calc R U . . .
H20B H 0.594050 0.761227 1.300838 0.058 Uiso 1 1 calc R U . . .
C21 C 0.5772(6) 0.6061(7) 1.2909(5) 0.052(2) Uani 1 1 d . . . . .
H21A H 0.530881 0.560523 1.282626 0.063 Uiso 1 1 calc R U . . .
H21B H 0.620362 0.597236 1.344324 0.063 Uiso 1 1 calc R U . . .
C22 C 0.6133(5) 0.5771(7) 1.2349(5) 0.050(2) Uani 1 1 d . . . . .
H22A H 0.642214 0.635207 1.226637 0.059 Uiso 1 1 calc R U . . .
H22B H 0.653366 0.521663 1.256712 0.059 Uiso 1 1 calc R U . . .
N23 N 0.5429(4) 0.5453(5) 1.1601(4) 0.0404(17) Uani 1 1 d . . . . .
C24 C 0.5499(5) 0.4620(6) 1.1270(5) 0.0375(19) Uani 1 1 d . . . . .
H24 H 0.602063 0.429658 1.149516 0.045 Uiso 1 1 calc R U . . .
C25 C 0.4844(5) 0.4146(5) 1.0586(5) 0.0313(17) Uani 1 1 d . . . . .
C26 C 0.5077(6) 0.3283(6) 1.0286(5) 0.041(2) Uani 1 1 d . . . . .
H26 H 0.563663 0.307373 1.051884 0.049 Uiso 1 1 calc R U . . .
C27 C 0.4503(7) 0.2754(6) 0.9669(6) 0.049(2) Uani 1 1 d . . . . .
H27 H 0.466642 0.218758 0.947740 0.059 Uiso 1 1 calc R U . . .
C28 C 0.3666(6) 0.3065(6) 0.9324(6) 0.047(2) Uani 1 1 d . . . . .
H28 H 0.326857 0.269936 0.890273 0.057 Uiso 1 1 calc R U . . .
C29 C 0.3415(5) 0.3913(5) 0.9599(5) 0.0353(19) Uani 1 1 d . . . . .
H29 H 0.285140 0.410618 0.936073 0.042 Uiso 1 1 calc R U . . .
C30 C 0.3993(5) 0.4477(5) 1.0224(5) 0.0330(18) Uani 1 1 d . . . . .
O31 O 0.3737(3) 0.5279(4) 1.0488(3) 0.0347(13) Uani 1 1 d . . . . .
O41 O 0.1935(4) 0.4794(4) 1.0011(4) 0.0436(15) Uani 1 1 d . . . . .
C42 C 0.1153(5) 0.4396(6) 0.9698(5) 0.038(2) Uani 1 1 d . . . . .
C43 C 0.0451(5) 0.5014(8) 0.9293(5) 0.049(2) Uani 1 1 d . . . . .
H43 H 0.051795 0.570686 0.923043 0.058 Uiso 1 1 calc R U . . .
C44 C -0.0333(6) 0.4597(8) 0.8990(6) 0.059(3) Uani 1 1 d . . . . .
H44 H -0.080118 0.501348 0.872808 0.071 Uiso 1 1 calc R U . . .
C45 C -0.0449(7) 0.3556(10) 0.9065(6) 0.070(3) Uani 1 1 d . . . . .
H45 H -0.098997 0.328290 0.886145 0.084 Uiso 1 1 calc R U . . .
C46 C 0.0242(9) 0.2937(9) 0.9442(6) 0.071(4) Uani 1 1 d . . . . .
H46 H 0.016818 0.224134 0.948873 0.085 Uiso 1 1 calc R U . . .
C47 C 0.1067(7) 0.3348(6) 0.9761(6) 0.051(2) Uani 1 1 d . . . . .
C48 C 0.1822(10) 0.2659(7) 1.0173(8) 0.073(4) Uani 1 1 d . . . . .
C481 C 0.1721(11) 0.1576(8) 0.9880(9) 0.118(6) Uani 1 1 d . . . . .
H48A H 0.116123 0.148322 0.946465 0.176 Uiso 0.5 1 calc R U P . .
H48B H 0.212424 0.143968 0.968821 0.176 Uiso 0.5 1 calc R U P . .
H48C H 0.181104 0.111475 1.029987 0.176 Uiso 0.5 1 calc R U P . .
H48D H 0.223645 0.120855 1.017050 0.176 Uiso 0.5 1 calc R U P . .
H48E H 0.127344 0.125209 0.994694 0.176 Uiso 0.5 1 calc R U P . .
H48F H 0.158663 0.157702 0.933528 0.176 Uiso 0.5 1 calc R U P . .
N49 N 0.2490(7) 0.2984(7) 1.0712(6) 0.069(3) Uani 1 1 d . . . . .
C50A C 0.3030(18) 0.211(2) 1.0872(19) 0.039(7) Uani 0.36(3) 1 d . U P A 1
H50A H 0.312475 0.193486 1.042645 0.046 Uiso 0.36(3) 1 calc R U P A 1
H50B H 0.279574 0.151948 1.101348 0.046 Uiso 0.36(3) 1 calc R U P A 1
C51A C 0.381(2) 0.246(2) 1.154(2) 0.041(8) Uani 0.36(3) 1 d . U P A 1
H51A H 0.406410 0.298279 1.135312 0.050 Uiso 0.36(3) 1 calc R U P A 1
H51B H 0.420080 0.189137 1.172578 0.050 Uiso 0.36(3) 1 calc R U P A 1
C52A C 0.3679(18) 0.290(2) 1.2226(17) 0.038(7) Uani 0.36(3) 1 d . U P A 1
H52A H 0.419544 0.280001 1.270504 0.046 Uiso 0.36(3) 1 calc R U P A 1
H52B H 0.324154 0.250232 1.227154 0.046 Uiso 0.36(3) 1 calc R U P A 1
C50B C 0.3306(16) 0.2338(15) 1.1196(15) 0.069(6) Uani 0.64(3) 1 d . U P A 2
H50C H 0.313115 0.172383 1.136650 0.083 Uiso 0.64(3) 1 calc R U P A 2
H50D H 0.352195 0.212255 1.083697 0.083 Uiso 0.64(3) 1 calc R U P A 2
C51B C 0.4022(12) 0.2771(15) 1.1889(13) 0.056(5) Uani 0.64(3) 1 d . U P A 2
H51C H 0.428645 0.329280 1.171539 0.067 Uiso 0.64(3) 1 calc R U P A 2
H51D H 0.443432 0.223464 1.213704 0.067 Uiso 0.64(3) 1 calc R U P A 2
C52B C 0.3804(13) 0.3224(14) 1.2481(13) 0.064(6) Uani 0.64(3) 1 d . U P A 2
H52C H 0.342496 0.278088 1.257904 0.076 Uiso 0.64(3) 1 calc DR U P A 2
H52D H 0.430630 0.333917 1.296914 0.076 Uiso 0.64(3) 1 calc DR U P A 2
N53 N 0.3411(5) 0.4148(8) 1.2154(6) 0.070(3) Uani 1 1 d . . . . .
C54 C 0.3656(6) 0.4877(12) 1.2716(7) 0.086(5) Uani 1 1 d . . . . .
H54 H 0.400356 0.466318 1.322402 0.103 Uiso 1 1 calc DR U . . .
C55 C 0.3444(6) 0.5915(11) 1.2618(6) 0.068(3) Uani 1 1 d . . . . .
C56 C 0.3788(8) 0.6560(10) 1.3319(7) 0.076(3) Uani 1 1 d . U . . .
H56 H 0.410143 0.626989 1.380937 0.092 Uiso 1 1 calc R U . . .
C57 C 0.3657(8) 0.7507(10) 1.3253(8) 0.082(4) Uani 1 1 d . U . . .
H57 H 0.387728 0.788850 1.371265 0.098 Uiso 1 1 calc R U . . .
C58 C 0.3201(7) 0.8053(11) 1.2536(7) 0.080(4) Uani 1 1 d . . . . .
H58 H 0.312949 0.875807 1.251253 0.095 Uiso 1 1 calc R U . . .
C59 C 0.2871(6) 0.7422(9) 1.1872(6) 0.061(3) Uani 1 1 d . . . . .
H59 H 0.254226 0.772680 1.139039 0.073 Uiso 1 1 calc R U . . .
C60 C 0.3001(6) 0.6381(10) 1.1883(5) 0.060(3) Uani 1 1 d . . . . .
C181 C 0.4985(6) 0.9168(7) 1.2449(6) 0.064(3) Uani 1 1 d . . . . .
H18A H 0.556957 0.934071 1.263860 0.095 Uiso 1 1 calc R U . . .
H18B H 0.489456 0.889979 1.287097 0.095 Uiso 1 1 calc R U . . .
H18C H 0.464684 0.976914 1.224301 0.095 Uiso 1 1 calc R U . . .
O61 O 0.2688(4) 0.5846(5) 1.1216(3) 0.0473(15) Uani 1 1 d . . . . .
C3 C 0.6177(11) 0.2411(13) 1.2718(11) 0.046(4) Uiso 0.5 1 d . . P . .
N3 N 0.5941(11) 0.3046(14) 1.2898(11) 0.068(5) Uiso 0.5 1 d . . P . .
C4 C 0.6478(13) 0.1660(14) 1.2374(12) 0.057(5) Uiso 0.5 1 d . . P . .
H4A H 0.701366 0.187087 1.241447 0.086 Uiso 0.5 1 calc R U P . .
H4B H 0.608342 0.157980 1.183256 0.086 Uiso 0.5 1 calc R U P . .
H4C H 0.654213 0.102158 1.264113 0.086 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
Ni2 O61 1.901(6) . ?
Ni2 O41 1.915(6) . ?
Ni2 N53 1.925(10) . ?
Ni2 N49 1.961(10) . ?
Ni2 Mn3 3.0694(16) . ?
Ni1 O11 1.901(5) . ?
Ni1 O31 1.930(5) . ?
Ni1 N23 1.933(7) . ?
Ni1 N19 1.965(6) . ?
Mn3 O11 2.111(5) . ?
Mn3 O41 2.112(5) . ?
Mn3 N2 2.121(7) . ?
Mn3 N1 2.133(8) . ?
Mn3 O61 2.269(6) . ?
Mn3 O31 2.383(5) . ?
N1 C1 1.173(10) . ?
C1 S1 1.599(9) . ?
N2 C2 1.160(10) . ?
S2 C2 1.624(10) . ?
O11 C12 1.345(8) . ?
C12 C13 1.387(12) . ?
C12 C17 1.391(11) . ?
C13 C14 1.372(12) . ?
C13 H13 0.9300 . ?
C14 C15 1.390(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.361(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.422(12) . ?
C16 H16 0.9300 . ?
C17 C18 1.462(13) . ?
C18 N19 1.296(9) . ?
C18 C181 1.520(11) . ?
N19 C20 1.481(10) . ?
C20 C21 1.515(12) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.528(13) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N23 1.473(11) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
N23 C24 1.295(10) . ?
C24 C25 1.442(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.411(10) . ?
C25 C30 1.419(11) . ?
C26 C27 1.353(12) . ?
C26 H26 0.9300 . ?
C27 C28 1.388(13) . ?
C27 H27 0.9300 . ?
C28 C29 1.386(11) . ?
C28 H28 0.9300 . ?
C29 C30 1.386(11) . ?
C29 H29 0.9300 . ?
C30 O31 1.332(8) . ?
O41 C42 1.346(9) . ?
C42 C43 1.392(12) . ?
C42 C47 1.391(11) . ?
C43 C44 1.359(12) . ?
C43 H43 0.9300 . ?
C44 C45 1.395(14) . ?
C44 H44 0.9300 . ?
C45 C46 1.374(16) . ?
C45 H45 0.9300 . ?
C46 C47 1.415(14) . ?
C46 H46 0.9300 . ?
C47 C48 1.511(16) . ?
C48 N49 1.245(15) . ?
C48 C481 1.504(14) . ?
C481 H48A 0.9600 . ?
C481 H48B 0.9600 . ?
C481 H48C 0.9600 . ?
C481 H48D 0.9600 . ?
C481 H48E 0.9600 . ?
C481 H48F 0.9600 . ?
N49 C50A 1.44(3) . ?
N49 C50B 1.57(2) . ?
C50A C51A 1.47(4) . ?
C50A H50A 0.9700 . ?
C50A H50B 0.9700 . ?
C51A C52A 1.55(4) . ?
C51A H51A 0.9700 . ?
C51A H51B 0.9700 . ?
C52A N53 1.69(3) . ?
C52A H52A 0.9700 . ?
C52A H52B 0.9700 . ?
C50B C51B 1.47(2) . ?
C50B H50C 0.9700 . ?
C50B H50D 0.9700 . ?
C51B C52B 1.48(3) . ?
C51B H51C 0.9700 . ?
C51B H51D 0.9700 . ?
C52B N53 1.395(18) . ?
C52B H52C 0.9700 . ?
C52B H52D 0.9700 . ?
N53 C54 1.355(15) . ?
C54 C55 1.400(17) . ?
C54 H54 0.9300 . ?
C55 C60 1.405(14) . ?
C55 C56 1.465(16) . ?
C56 C57 1.257(15) . ?
C56 H56 0.9300 . ?
C57 C58 1.431(16) . ?
C57 H57 0.9300 . ?
C58 C59 1.404(14) . ?
C58 H58 0.9300 . ?
C59 C60 1.380(14) . ?
C59 H59 0.9300 . ?
C60 O61 1.338(11) . ?
C181 H18A 0.9600 . ?
C181 H18B 0.9600 . ?
C181 H18C 0.9600 . ?
C3 N3 1.06(2) . ?
C3 C4 1.42(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 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
O61 Ni2 O41 81.7(2) . . ?
O61 Ni2 N53 93.2(4) . . ?
O41 Ni2 N53 174.7(4) . . ?
O61 Ni2 N49 168.9(3) . . ?
O41 Ni2 N49 87.5(3) . . ?
N53 Ni2 N49 97.5(4) . . ?
O61 Ni2 Mn3 47.48(18) . . ?
O41 Ni2 Mn3 42.79(15) . . ?
N53 Ni2 Mn3 133.6(3) . . ?
N49 Ni2 Mn3 123.8(3) . . ?
O11 Ni1 O31 82.6(2) . . ?
O11 Ni1 N23 167.6(3) . . ?
O31 Ni1 N23 93.0(3) . . ?
O11 Ni1 N19 91.2(2) . . ?
O31 Ni1 N19 162.9(3) . . ?
N23 Ni1 N19 96.0(3) . . ?
O11 Mn3 O41 145.0(2) . . ?
O11 Mn3 N2 96.8(2) . . ?
O41 Mn3 N2 108.7(3) . . ?
O11 Mn3 N1 100.8(2) . . ?
O41 Mn3 N1 98.3(2) . . ?
N2 Mn3 N1 99.4(3) . . ?
O11 Mn3 O61 85.0(2) . . ?
O41 Mn3 O61 69.3(2) . . ?
N2 Mn3 O61 95.8(3) . . ?
N1 Mn3 O61 162.9(2) . . ?
O11 Mn3 O31 68.21(18) . . ?
O41 Mn3 O31 82.7(2) . . ?
N2 Mn3 O31 163.5(2) . . ?
N1 Mn3 O31 90.5(2) . . ?
O61 Mn3 O31 76.7(2) . . ?
O11 Mn3 Ni2 107.98(14) . . ?
O41 Mn3 Ni2 38.02(16) . . ?
N2 Mn3 Ni2 121.3(2) . . ?
N1 Mn3 Ni2 125.37(18) . . ?
O61 Mn3 Ni2 38.13(16) . . ?
O31 Mn3 Ni2 60.67(14) . . ?
C1 N1 Mn3 172.5(6) . . ?
N1 C1 S1 178.5(8) . . ?
C2 N2 Mn3 156.8(7) . . ?
N2 C2 S2 178.3(8) . . ?
C12 O11 Ni1 119.7(5) . . ?
C12 O11 Mn3 131.7(5) . . ?
Ni1 O11 Mn3 107.4(2) . . ?
O11 C12 C13 118.1(7) . . ?
O11 C12 C17 120.6(7) . . ?
C13 C12 C17 121.3(8) . . ?
C14 C13 C12 120.7(9) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C15 119.2(10) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 120.5(10) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 121.6(10) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C12 C17 C16 116.6(9) . . ?
C12 C17 C18 123.1(7) . . ?
C16 C17 C18 120.3(8) . . ?
N19 C18 C17 122.3(7) . . ?
N19 C18 C181 122.1(9) . . ?
C17 C18 C181 115.6(8) . . ?
C18 N19 C20 116.0(7) . . ?
C18 N19 Ni1 122.6(6) . . ?
C20 N19 Ni1 121.2(5) . . ?
N19 C20 C21 112.6(7) . . ?
N19 C20 H20A 109.1 . . ?
C21 C20 H20A 109.1 . . ?
N19 C20 H20B 109.1 . . ?
C21 C20 H20B 109.1 . . ?
H20A C20 H20B 107.8 . . ?
C20 C21 C22 112.1(8) . . ?
C20 C21 H21A 109.2 . . ?
C22 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C22 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
N23 C22 C21 108.2(7) . . ?
N23 C22 H22A 110.1 . . ?
C21 C22 H22A 110.1 . . ?
N23 C22 H22B 110.1 . . ?
C21 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?
C24 N23 C22 119.2(7) . . ?
C24 N23 Ni1 123.8(6) . . ?
C22 N23 Ni1 117.0(5) . . ?
N23 C24 C25 126.2(7) . . ?
N23 C24 H24 116.9 . . ?
C25 C24 H24 116.9 . . ?
C26 C25 C30 119.3(8) . . ?
C26 C25 C24 116.7(7) . . ?
C30 C25 C24 123.9(7) . . ?
C27 C26 C25 121.5(8) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C26 C27 C28 119.2(8) . . ?
C26 C27 H27 120.4 . . ?
C28 C27 H27 120.4 . . ?
C29 C28 C27 120.9(8) . . ?
C29 C28 H28 119.5 . . ?
C27 C28 H28 119.5 . . ?
C28 C29 C30 121.0(8) . . ?
C28 C29 H29 119.5 . . ?
C30 C29 H29 119.5 . . ?
O31 C30 C29 120.1(7) . . ?
O31 C30 C25 121.8(7) . . ?
C29 C30 C25 118.0(7) . . ?
C30 O31 Ni1 125.8(5) . . ?
C30 O31 Mn3 133.3(5) . . ?
Ni1 O31 Mn3 96.72(19) . . ?
C42 O41 Ni2 116.8(5) . . ?
C42 O41 Mn3 135.3(5) . . ?
Ni2 O41 Mn3 99.2(2) . . ?
O41 C42 C43 120.7(7) . . ?
O41 C42 C47 118.3(8) . . ?
C43 C42 C47 120.9(8) . . ?
C44 C43 C42 119.6(9) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C45 121.3(10) . . ?
C43 C44 H44 119.4 . . ?
C45 C44 H44 119.4 . . ?
C46 C45 C44 119.4(10) . . ?
C46 C45 H45 120.3 . . ?
C44 C45 H45 120.3 . . ?
C45 C46 C47 120.7(10) . . ?
C45 C46 H46 119.7 . . ?
C47 C46 H46 119.7 . . ?
C42 C47 C46 118.1(10) . . ?
C42 C47 C48 121.8(9) . . ?
C46 C47 C48 120.1(9) . . ?
N49 C48 C47 121.2(10) . . ?
N49 C48 C481 122.7(13) . . ?
C47 C48 C481 116.0(13) . . ?
C48 C481 H48A 109.5 . . ?
C48 C481 H48B 109.5 . . ?
H48A C481 H48B 109.5 . . ?
C48 C481 H48C 109.5 . . ?
H48A C481 H48C 109.5 . . ?
H48B C481 H48C 109.5 . . ?
C48 C481 H48D 109.5 . . ?
H48A C481 H48D 141.1 . . ?
H48B C481 H48D 56.3 . . ?
H48C C481 H48D 56.3 . . ?
C48 C481 H48E 109.5 . . ?
H48A C481 H48E 56.3 . . ?
H48B C481 H48E 141.1 . . ?
H48C C481 H48E 56.3 . . ?
H48D C481 H48E 109.5 . . ?
C48 C481 H48F 109.5 . . ?
H48A C481 H48F 56.3 . . ?
H48B C481 H48F 56.3 . . ?
H48C C481 H48F 141.1 . . ?
H48D C481 H48F 109.5 . . ?
H48E C481 H48F 109.5 . . ?
C48 N49 C50A 101.5(16) . . ?
C48 N49 C50B 125.9(13) . . ?
C48 N49 Ni2 124.2(8) . . ?
C50A N49 Ni2 133.8(15) . . ?
C50B N49 Ni2 109.9(11) . . ?
N49 C50A C51A 102(2) . . ?
N49 C50A H50A 111.3 . . ?
C51A C50A H50A 111.3 . . ?
N49 C50A H50B 111.3 . . ?
C51A C50A H50B 111.3 . . ?
H50A C50A H50B 109.2 . . ?
C50A C51A C52A 114(2) . . ?
C50A C51A H51A 108.7 . . ?
C52A C51A H51A 108.7 . . ?
C50A C51A H51B 108.7 . . ?
C52A C51A H51B 108.7 . . ?
H51A C51A H51B 107.6 . . ?
C51A C52A N53 115.6(19) . . ?
C51A C52A H52A 108.4 . . ?
N53 C52A H52A 108.4 . . ?
C51A C52A H52B 108.4 . . ?
N53 C52A H52B 108.4 . . ?
H52A C52A H52B 107.4 . . ?
C51B C50B N49 121.1(15) . . ?
C51B C50B H50C 107.1 . . ?
N49 C50B H50C 107.1 . . ?
C51B C50B H50D 107.1 . . ?
N49 C50B H50D 107.1 . . ?
H50C C50B H50D 106.8 . . ?
C50B C51B C52B 115.2(17) . . ?
C50B C51B H51C 108.5 . . ?
C52B C51B H51C 108.5 . . ?
C50B C51B H51D 108.5 . . ?
C52B C51B H51D 108.5 . . ?
H51C C51B H51D 107.5 . . ?
N53 C52B C51B 104.7(15) . . ?
N53 C52B H52C 110.8 . . ?
C51B C52B H52C 110.8 . . ?
N53 C52B H52D 110.8 . . ?
C51B C52B H52D 110.8 . . ?
H52C C52B H52D 108.9 . . ?
C54 N53 C52B 109.7(12) . . ?
C54 N53 C52A 129.7(12) . . ?
C54 N53 Ni2 123.5(8) . . ?
C52B N53 Ni2 126.6(12) . . ?
C52A N53 Ni2 106.7(11) . . ?
N53 C54 C55 127.4(11) . . ?
N53 C54 H54 116.3 . . ?
C55 C54 H54 116.3 . . ?
C60 C55 C54 123.4(11) . . ?
C60 C55 C56 118.8(12) . . ?
C54 C55 C56 117.5(11) . . ?
C57 C56 C55 119.7(13) . . ?
C57 C56 H56 120.2 . . ?
C55 C56 H56 120.2 . . ?
C56 C57 C58 125.9(13) . . ?
C56 C57 H57 117.1 . . ?
C58 C57 H57 117.1 . . ?
C59 C58 C57 113.6(13) . . ?
C59 C58 H58 123.2 . . ?
C57 C58 H58 123.2 . . ?
C60 C59 C58 124.6(11) . . ?
C60 C59 H59 117.7 . . ?
C58 C59 H59 117.7 . . ?
O61 C60 C59 120.5(9) . . ?
O61 C60 C55 122.3(12) . . ?
C59 C60 C55 117.2(10) . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C60 O61 Ni2 129.3(7) . . ?
C60 O61 Mn3 132.9(7) . . ?
Ni2 O61 Mn3 94.4(2) . . ?
N3 C3 C4 171(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

_refine_diff_density_max         0.998
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.120

