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

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

data_Complex_1
_database_code_depnum_ccdc_archive 'CCDC 1889042'
loop_
_audit_author_name
_audit_author_address
'Amit Adhikary'
;IACS India
India
;
_audit_update_record             
;
2019-08-05 deposited with the CCDC.	2019-08-22 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         'C34 H44 Br2 Mn3 N4 O12'
_chemical_formula_sum            'C34 H44 Br2 Mn3 N4 O12'
_chemical_formula_weight         1025.35

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'
Br Br -0.2901 2.4595 '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                   11.784(2)
_cell_length_b                   9.5219(17)
_cell_length_c                   19.786(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.025(6)
_cell_angle_gamma                90
_cell_volume                     2122.7(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2606
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      22.68

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_F_000             1308
_exptl_transmission_factor_min   0.634
_exptl_transmission_factor_max   0.876
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.821
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_process_details   '(SADABS; Bruker, 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22788
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_av_R_equivalents  0.1485
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.813
_diffrn_reflns_theta_max         24.830
_diffrn_reflns_theta_full        24.830
_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             3635
_reflns_number_gt                2153
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0659P)²+1.3996P] 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         3635
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1661
_refine_ls_wR_factor_gt          0.1395
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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 -0.22993(9) 0.83321(12) 0.31304(5) 0.1015(4) Uani 1 1 d . . . . .
Mn1 Mn 0.21161(9) 0.80970(10) 0.09771(5) 0.0481(3) Uani 1 1 d . . . . .
Mn2 Mn 0.000000 1.000000 0.000000 0.0488(4) Uani 1 2 d S . P . .
O4 O 0.1376(4) 0.6741(5) 0.0138(3) 0.0608(12) Uani 1 1 d . . . . .
O5 O 0.0053(4) 1.1925(5) 0.0552(2) 0.0615(12) Uani 1 1 d . . . . .
O6 O 0.5013(6) 0.7077(8) 0.0144(3) 0.0981(19) Uani 1 1 d . . . . .
O3 O 0.3137(4) 1.0154(5) 0.1334(2) 0.0660(13) Uani 1 1 d . . . . .
O2 O 0.1930(4) 0.9990(4) 0.0259(2) 0.0521(11) Uani 1 1 d . . . . .
O1 O 0.0447(4) 0.8882(4) 0.1021(2) 0.0544(12) Uani 1 1 d . . . . .
C4 C -0.1432(7) 0.8453(8) 0.2458(4) 0.0593(19) Uani 1 1 d . . . . .
C3 C -0.1811(6) 0.9381(8) 0.1906(4) 0.064(2) Uani 1 1 d . . . . .
H3 H -0.249236 0.991429 0.185474 0.077 Uiso 1 1 calc R U . . .
C2 C -0.1171(6) 0.9509(7) 0.1431(3) 0.0537(17) Uani 1 1 d . . . . .
H2 H -0.143040 1.014185 0.105999 0.064 Uiso 1 1 calc R U . . .
C1 C -0.0147(6) 0.8729(7) 0.1482(3) 0.0491(16) Uani 1 1 d . . . . .
C6 C 0.0231(6) 0.7795(7) 0.2060(3) 0.0517(17) Uani 1 1 d . . . . .
C7 C 0.1273(7) 0.6945(8) 0.2209(4) 0.068(2) Uani 1 1 d . . . . .
H7 H 0.137973 0.632214 0.258413 0.082 Uiso 1 1 calc R U . . .
N1 N 0.2067(5) 0.6926(6) 0.1898(3) 0.0655(17) Uani 1 1 d . . . . .
C8 C 0.3067(8) 0.5960(10) 0.2144(5) 0.098(3) Uani 1 1 d . . . . .
H8A H 0.288610 0.508183 0.188653 0.118 Uiso 1 1 calc R U . . .
H8B H 0.320162 0.576249 0.264219 0.118 Uiso 1 1 calc R U . . .
C9 C 0.4137(8) 0.6580(10) 0.2035(4) 0.091(3) Uani 1 1 d . . . . .
H9A H 0.477967 0.590553 0.217878 0.110 Uiso 1 1 calc R U . . .
H9B H 0.436014 0.739735 0.233761 0.110 Uiso 1 1 calc R U . . .
N2 N 0.4002(5) 0.7007(6) 0.1296(3) 0.0618(16) Uani 1 1 d . . . . .
C10 C 0.5044(7) 0.7874(9) 0.1300(5) 0.083(2) Uani 1 1 d . . . . .
H10A H 0.504079 0.872573 0.156814 0.099 Uiso 1 1 calc R U . . .
H10B H 0.576492 0.735990 0.152871 0.099 Uiso 1 1 calc R U . . .
C11 C 0.5032(9) 0.8245(11) 0.0572(6) 0.102(3) Uani 1 1 d . . . . .
H11A H 0.433935 0.881919 0.035928 0.122 Uiso 1 1 calc R U . . .
H11B H 0.572989 0.880283 0.059221 0.122 Uiso 1 1 calc R U . . .
C13 C 0.4006(8) 0.6284(10) 0.0122(5) 0.089(3) Uani 1 1 d . . . . .
H13A H 0.397631 0.547274 -0.017846 0.106 Uiso 1 1 calc R U . . .
H13B H 0.330353 0.684621 -0.008567 0.106 Uiso 1 1 calc R U . . .
C12 C 0.3989(7) 0.5799(8) 0.0838(4) 0.076(2) Uani 1 1 d . . . . .
H12A H 0.328254 0.524231 0.079534 0.091 Uiso 1 1 calc R U . . .
H12B H 0.467660 0.521215 0.104399 0.091 Uiso 1 1 calc R U . . .
C17 C 0.2627(6) 1.0716(7) 0.0756(4) 0.0530(17) Uani 1 1 d . . . . .
C16 C 0.2841(7) 1.2215(8) 0.0616(5) 0.082(3) Uani 1 1 d . . . . .
H16A H 0.251097 1.280683 0.090363 0.123 Uiso 1 1 calc R U . . .
H16B H 0.246991 1.242271 0.012638 0.123 Uiso 1 1 calc R U . . .
H16C H 0.367900 1.238082 0.072873 0.123 Uiso 1 1 calc R U . . .
C5 C -0.0448(7) 0.7670(8) 0.2543(3) 0.062(2) Uani 1 1 d . . . . .
H5 H -0.021246 0.704561 0.291906 0.074 Uiso 1 1 calc R U . . .
C14 C 0.0524(7) 0.6962(8) -0.0416(4) 0.0548(18) Uani 1 1 d . . . . .
C15 C 0.0189(7) 0.5765(8) -0.0936(4) 0.076(2) Uani 1 1 d . . . . .
H15A H -0.040145 0.519185 -0.082352 0.114 Uiso 1 1 calc R U . . .
H15B H 0.087887 0.520695 -0.091035 0.114 Uiso 1 1 calc R U . . .
H15C H -0.012419 0.613362 -0.140560 0.114 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 1.903(7) . ?
Mn1 O4 2.082(5) . ?
Mn1 O1 2.130(4) . ?
Mn1 N1 2.152(6) . ?
Mn1 O2 2.266(4) . ?
Mn1 O3 2.298(5) . ?
Mn1 N2 2.365(6) . ?
Mn2 O5 2.126(5) . ?
Mn2 O5 2.126(5) 3_575 ?
Mn2 O2 2.179(4) 3_575 ?
Mn2 O2 2.179(4) . ?
Mn2 O1 2.206(4) . ?
Mn2 O1 2.206(4) 3_575 ?
O4 C14 1.268(8) . ?
O5 C14 1.245(8) 3_575 ?
O6 C11 1.394(11) . ?
O6 C13 1.397(10) . ?
O3 C17 1.246(8) . ?
O2 C17 1.283(8) . ?
O1 C1 1.310(7) . ?
C4 C5 1.347(10) . ?
C4 C3 1.374(10) . ?
C3 C2 1.372(8) . ?
C3 H3 0.9300 . ?
C2 C1 1.395(8) . ?
C2 H2 0.9300 . ?
C1 C6 1.414(9) . ?
C6 C5 1.418(9) . ?
C6 C7 1.427(9) . ?
C7 N1 1.260(9) . ?
C7 H7 0.9300 . ?
N1 C8 1.461(9) . ?
C8 C9 1.465(12) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N2 1.479(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N2 C12 1.463(9) . ?
N2 C10 1.477(9) . ?
C10 C11 1.479(12) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C13 C12 1.494(11) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C17 C16 1.489(10) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C5 H5 0.9300 . ?
C14 C15 1.510(9) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 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
O4 Mn1 O1 94.22(18) . . ?
O4 Mn1 N1 104.2(2) . . ?
O1 Mn1 N1 83.86(19) . . ?
O4 Mn1 O2 93.01(17) . . ?
O1 Mn1 O2 79.92(15) . . ?
N1 Mn1 O2 157.17(19) . . ?
O4 Mn1 O3 146.37(18) . . ?
O1 Mn1 O3 95.44(17) . . ?
N1 Mn1 O3 108.9(2) . . ?
O2 Mn1 O3 57.35(16) . . ?
O4 Mn1 N2 94.7(2) . . ?
O1 Mn1 N2 161.83(17) . . ?
N1 Mn1 N2 78.6(2) . . ?
O2 Mn1 N2 115.31(18) . . ?
O3 Mn1 N2 85.73(19) . . ?
O5 Mn2 O5 180.0 . 3_575 ?
O5 Mn2 O2 89.36(17) . 3_575 ?
O5 Mn2 O2 90.64(17) 3_575 3_575 ?
O5 Mn2 O2 90.64(17) . . ?
O5 Mn2 O2 89.36(17) 3_575 . ?
O2 Mn2 O2 180.0 3_575 . ?
O5 Mn2 O1 88.97(17) . . ?
O5 Mn2 O1 91.03(17) 3_575 . ?
O2 Mn2 O1 99.80(15) 3_575 . ?
O2 Mn2 O1 80.20(15) . . ?
O5 Mn2 O1 91.03(17) . 3_575 ?
O5 Mn2 O1 88.96(17) 3_575 3_575 ?
O2 Mn2 O1 80.20(15) 3_575 3_575 ?
O2 Mn2 O1 99.80(15) . 3_575 ?
O1 Mn2 O1 180.0 . 3_575 ?
O5 Mn2 Mn1 74.04(13) . 3_575 ?
O5 Mn2 Mn1 105.96(13) 3_575 3_575 ?
O2 Mn2 Mn1 44.51(11) 3_575 3_575 ?
O2 Mn2 Mn1 135.49(11) . 3_575 ?
O1 Mn2 Mn1 139.00(11) . 3_575 ?
O1 Mn2 Mn1 41.00(11) 3_575 3_575 ?
C14 O4 Mn1 128.8(5) . . ?
C14 O5 Mn2 133.6(5) 3_575 . ?
C11 O6 C13 108.2(6) . . ?
C17 O3 Mn1 90.9(4) . . ?
C17 O2 Mn2 124.6(4) . . ?
C17 O2 Mn1 91.4(4) . . ?
Mn2 O2 Mn1 93.09(15) . . ?
C1 O1 Mn1 132.6(4) . . ?
C1 O1 Mn2 131.2(4) . . ?
Mn1 O1 Mn2 96.19(16) . . ?
C5 C4 C3 121.5(6) . . ?
C5 C4 Br1 119.9(6) . . ?
C3 C4 Br1 118.6(6) . . ?
C2 C3 C4 119.1(7) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C2 C1 122.8(7) . . ?
C3 C2 H2 118.7 . . ?
C1 C2 H2 118.6 . . ?
O1 C1 C2 121.2(6) . . ?
O1 C1 C6 121.9(6) . . ?
C2 C1 C6 116.9(6) . . ?
C1 C6 C5 119.4(6) . . ?
C1 C6 C7 124.8(6) . . ?
C5 C6 C7 115.8(6) . . ?
N1 C7 C6 128.6(7) . . ?
N1 C7 H7 115.7 . . ?
C6 C7 H7 115.6 . . ?
C7 N1 C8 119.3(6) . . ?
C7 N1 Mn1 127.8(5) . . ?
C8 N1 Mn1 112.9(5) . . ?
N1 C8 C9 110.1(7) . . ?
N1 C8 H8A 109.6 . . ?
C9 C8 H8A 109.7 . . ?
N1 C8 H8B 109.7 . . ?
C9 C8 H8B 109.6 . . ?
H8A C8 H8B 108.2 . . ?
C8 C9 N2 114.1(7) . . ?
C8 C9 H9A 108.7 . . ?
N2 C9 H9A 108.7 . . ?
C8 C9 H9B 108.7 . . ?
N2 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C12 N2 C9 112.0(6) . . ?
C12 N2 C10 107.5(6) . . ?
C9 N2 C10 107.5(7) . . ?
C12 N2 Mn1 109.9(4) . . ?
C9 N2 Mn1 101.8(4) . . ?
C10 N2 Mn1 118.1(4) . . ?
C11 C10 N2 111.0(7) . . ?
C11 C10 H10A 109.7 . . ?
N2 C10 H10A 109.3 . . ?
C11 C10 H10B 109.2 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
O6 C11 C10 113.3(8) . . ?
O6 C11 H11A 109.0 . . ?
C10 C11 H11A 108.7 . . ?
O6 C11 H11B 108.8 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
O6 C13 C12 112.6(7) . . ?
O6 C13 H13A 108.9 . . ?
C12 C13 H13A 109.1 . . ?
O6 C13 H13B 109.2 . . ?
C12 C13 H13B 109.0 . . ?
H13A C13 H13B 107.9 . . ?
N2 C12 C13 110.1(6) . . ?
N2 C12 H12A 109.5 . . ?
C13 C12 H12A 109.9 . . ?
N2 C12 H12B 109.7 . . ?
C13 C12 H12B 109.5 . . ?
H12A C12 H12B 108.2 . . ?
O3 C17 O2 120.0(6) . . ?
O3 C17 C16 121.3(7) . . ?
O2 C17 C16 118.6(7) . . ?
C17 C16 H16A 109.4 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C17 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C4 C5 C6 120.3(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.8 . . ?
O5 C14 O4 125.0(6) 3_575 . ?
O5 C14 C15 118.5(7) 3_575 . ?
O4 C14 C15 116.5(7) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

_refine_diff_density_max         0.596
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.096

####################################################################### 
# 
# 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_Complex_2
_database_code_depnum_ccdc_archive 'CCDC 1889043'
loop_
_audit_author_name
_audit_author_address
'Amit Adhikary'
;IACS India
India
;
_audit_update_record             
;
2019-08-05 deposited with the CCDC.	2019-08-22 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         'C34 H44 Br2 Co3 N4 O12'
_chemical_formula_sum            'C34 H44 Br2 Co3 N4 O12'
_chemical_formula_weight         1037.34

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   11.4288(16)
_cell_length_b                   9.4698(13)
_cell_length_c                   19.605(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.643(3)
_cell_angle_gamma                90
_cell_volume                     2043.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    9734
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      23.04

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_F_000             1046
_exptl_transmission_factor_min   0.463
_exptl_transmission_factor_max   0.874
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.012
_exptl_absorpt_coefficient_mu    3.222
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_process_details   '(SADABS; Bruker, 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   Mo
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50126
_diffrn_reflns_av_unetI/netI     0.0669
_diffrn_reflns_av_R_equivalents  0.1343
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.406
_diffrn_reflns_theta_max         25.796
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             3884
_reflns_number_gt                2518
_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0423P)²+6.5113P] 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         3884
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1057
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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 -0.05168(6) 0.36520(10) 0.19379(4) 0.0678(3) Uani 1 1 d . . . . .
Co1 Co 0.500000 0.500000 0.500000 0.0268(3) Uani 1 2 d S . P . .
Co2 Co 0.60184(6) 0.31012(8) 0.39967(4) 0.0271(2) Uani 1 1 d . . . . .
O1 O 0.4391(3) 0.3945(4) 0.40352(18) 0.0341(9) Uani 1 1 d . . . . .
O4 O 0.6679(3) 0.4892(4) 0.46971(18) 0.0306(9) Uani 1 1 d . . . . .
O3 O 0.5434(3) 0.3136(4) 0.55310(19) 0.0361(9) Uani 1 1 d . . . . .
O5 O 0.6622(4) 0.5027(4) 0.35789(19) 0.0393(10) Uani 1 1 d . . . . .
O2 O 0.6102(3) 0.1734(4) 0.4797(2) 0.0351(9) Uani 1 1 d . . . . .
N1 N 0.5129(4) 0.1935(5) 0.3155(2) 0.0353(11) Uani 1 1 d . . . . .
N2 N 0.7667(4) 0.2044(5) 0.3742(2) 0.0341(11) Uani 1 1 d . . . . .
O6 O 0.9841(4) 0.2057(6) 0.4911(3) 0.0649(14) Uani 1 1 d . . . . .
C1 C 0.3328(5) 0.3838(6) 0.3583(2) 0.0266(12) Uani 1 1 d . . . . .
C14 C 0.6813(5) 0.5607(6) 0.4172(3) 0.0306(13) Uani 1 1 d . . . . .
C16 C 0.5839(5) 0.2006(6) 0.5373(3) 0.0330(13) Uani 1 1 d . . . . .
C6 C 0.3100(5) 0.2889(6) 0.3004(3) 0.0325(13) Uani 1 1 d . . . . .
C2 C 0.2359(5) 0.4683(6) 0.3641(3) 0.0329(14) Uani 1 1 d . . . . .
H2 H 0.248558 0.531679 0.401570 0.039 Uiso 1 1 calc R U . . .
C3 C 0.1231(5) 0.4621(7) 0.3171(3) 0.0406(16) Uani 1 1 d . . . . .
H3 H 0.060732 0.520210 0.322661 0.049 Uiso 1 1 calc R U . . .
C5 C 0.1937(5) 0.2828(6) 0.2531(3) 0.0389(15) Uani 1 1 d . . . . .
H5 H 0.178248 0.219162 0.215606 0.047 Uiso 1 1 calc R U . . .
C7 C 0.3996(5) 0.1971(7) 0.2840(3) 0.0405(15) Uani 1 1 d . . . . .
H7 H 0.371972 0.134294 0.246638 0.049 Uiso 1 1 calc R U . . .
C4 C 0.1033(5) 0.3685(7) 0.2613(3) 0.0382(15) Uani 1 1 d . . . . .
C13 C 0.8091(5) 0.0802(6) 0.4202(3) 0.0420(15) Uani 1 1 d . . . . .
H13A H 0.858249 0.020545 0.398647 0.050 Uiso 1 1 calc R U . . .
H13B H 0.739366 0.025577 0.424069 0.050 Uiso 1 1 calc R U . . .
C8 C 0.5899(6) 0.0944(7) 0.2894(3) 0.0504(18) Uani 1 1 d . . . . .
H8A H 0.554124 0.074695 0.239611 0.060 Uiso 1 1 calc R U . . .
H8B H 0.597426 0.006204 0.315413 0.060 Uiso 1 1 calc R U . . .
C15 C 0.7226(6) 0.7101(6) 0.4281(4) 0.0493(17) Uani 1 1 d . . . . .
H15A H 0.809266 0.713921 0.436288 0.074 Uiso 1 1 calc R U . . .
H15B H 0.700796 0.748251 0.468343 0.074 Uiso 1 1 calc R U . . .
H15C H 0.684539 0.764406 0.386732 0.074 Uiso 1 1 calc R U . . .
C9 C 0.7127(6) 0.1616(7) 0.3000(3) 0.0510(18) Uani 1 1 d . . . . .
H9A H 0.766666 0.095316 0.286018 0.061 Uiso 1 1 calc R U . . .
H9B H 0.704974 0.243963 0.269699 0.061 Uiso 1 1 calc R U . . .
C17 C 0.6069(6) 0.0827(7) 0.5909(3) 0.0489(17) Uani 1 1 d . . . . .
H17A H 0.613909 0.121078 0.637183 0.073 Uiso 1 1 calc R U . . .
H17B H 0.680853 0.034987 0.590676 0.073 Uiso 1 1 calc R U . . .
H17C H 0.540481 0.017023 0.579071 0.073 Uiso 1 1 calc R U . . .
C12 C 0.8830(6) 0.1236(8) 0.4934(3) 0.0560(19) Uani 1 1 d . . . . .
H12A H 0.831848 0.177159 0.516273 0.067 Uiso 1 1 calc R U . . .
H12B H 0.910393 0.039719 0.521542 0.067 Uiso 1 1 calc R U . . .
C10 C 0.8747(6) 0.2912(7) 0.3750(4) 0.0494(17) Uani 1 1 d . . . . .
H10A H 0.849214 0.377680 0.348662 0.059 Uiso 1 1 calc R U . . .
H10B H 0.926991 0.239907 0.352050 0.059 Uiso 1 1 calc R U . . .
C11 C 0.9453(6) 0.3273(8) 0.4506(4) 0.063(2) Uani 1 1 d . . . . .
H11A H 1.015418 0.384136 0.449655 0.076 Uiso 1 1 calc R U . . .
H11B H 0.894088 0.382836 0.472585 0.076 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 1.904(5) . ?
Co1 O3 2.041(4) 3_666 ?
Co1 O3 2.041(4) . ?
Co1 O1 2.086(3) 3_666 ?
Co1 O1 2.086(3) . ?
Co1 O4 2.159(3) . ?
Co1 O4 2.159(3) 3_666 ?
Co2 O2 2.017(4) . ?
Co2 N1 2.018(4) . ?
Co2 O1 2.044(4) . ?
Co2 O4 2.184(4) . ?
Co2 O5 2.186(4) . ?
Co2 N2 2.304(4) . ?
O1 C1 1.301(6) . ?
O4 C14 1.276(6) . ?
O3 C16 1.238(7) . ?
O5 C14 1.250(6) . ?
O2 C16 1.270(7) . ?
N1 C7 1.276(7) . ?
N1 C8 1.469(7) . ?
N2 C9 1.475(7) . ?
N2 C10 1.480(7) . ?
N2 C13 1.482(7) . ?
O6 C11 1.402(9) . ?
O6 C12 1.403(8) . ?
C1 C2 1.395(7) . ?
C1 C6 1.416(7) . ?
C14 C15 1.489(8) . ?
C16 C17 1.508(8) . ?
C6 C5 1.402(7) . ?
C6 C7 1.445(8) . ?
C2 C3 1.369(7) . ?
C3 C4 1.377(8) . ?
C5 C4 1.357(8) . ?
C13 C12 1.513(8) . ?
C8 C9 1.504(9) . ?
C10 C11 1.522(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Co1 O3 180.0 3_666 . ?
O3 Co1 O1 91.37(15) 3_666 3_666 ?
O3 Co1 O1 88.63(15) . 3_666 ?
O3 Co1 O1 88.63(15) 3_666 . ?
O3 Co1 O1 91.37(15) . . ?
O1 Co1 O1 180.0 3_666 . ?
O3 Co1 O4 90.72(14) 3_666 . ?
O3 Co1 O4 89.28(14) . . ?
O1 Co1 O4 99.69(13) 3_666 . ?
O1 Co1 O4 80.31(13) . . ?
O3 Co1 O4 89.28(14) 3_666 3_666 ?
O3 Co1 O4 90.72(14) . 3_666 ?
O1 Co1 O4 80.31(13) 3_666 3_666 ?
O1 Co1 O4 99.69(13) . 3_666 ?
O4 Co1 O4 180.0 . 3_666 ?
O2 Co2 N1 101.10(18) . . ?
O2 Co2 O1 94.28(15) . . ?
N1 Co2 O1 88.94(16) . . ?
O2 Co2 O4 94.21(14) . . ?
N1 Co2 O4 162.08(16) . . ?
O1 Co2 O4 80.62(13) . . ?
O2 Co2 O5 150.90(15) . . ?
N1 Co2 O5 106.89(17) . . ?
O1 Co2 O5 94.01(15) . . ?
O4 Co2 O5 59.82(14) . . ?
O2 Co2 N2 91.14(16) . . ?
N1 Co2 N2 81.15(17) . . ?
O1 Co2 N2 169.47(15) . . ?
O4 Co2 N2 108.01(15) . . ?
O5 Co2 N2 85.54(16) . . ?
C1 O1 Co2 129.5(3) . . ?
C1 O1 Co1 132.6(3) . . ?
Co2 O1 Co1 97.84(14) . . ?
C14 O4 Co1 120.4(3) . . ?
C14 O4 Co2 90.1(3) . . ?
Co1 O4 Co2 91.59(13) . . ?
C16 O3 Co1 132.5(4) . . ?
C14 O5 Co2 90.7(3) . . ?
C16 O2 Co2 126.0(4) . . ?
C7 N1 C8 118.2(5) . . ?
C7 N1 Co2 127.1(4) . . ?
C8 N1 Co2 114.7(4) . . ?
C9 N2 C10 106.8(5) . . ?
C9 N2 C13 111.3(5) . . ?
C10 N2 C13 107.4(4) . . ?
C9 N2 Co2 100.6(3) . . ?
C10 N2 Co2 119.0(4) . . ?
C13 N2 Co2 111.4(3) . . ?
C11 O6 C12 109.6(5) . . ?
O1 C1 C2 121.1(5) . . ?
O1 C1 C6 122.1(5) . . ?
C2 C1 C6 116.8(5) . . ?
O5 C14 O4 119.2(5) . . ?
O5 C14 C15 121.4(5) . . ?
O4 C14 C15 119.4(5) . . ?
O3 C16 O2 126.3(5) . . ?
O3 C16 C17 118.1(5) . . ?
O2 C16 C17 115.5(5) . . ?
C5 C6 C1 119.5(5) . . ?
C5 C6 C7 115.5(5) . . ?
C1 C6 C7 124.9(5) . . ?
C3 C2 C1 123.0(5) . . ?
C2 C3 C4 119.0(5) . . ?
C4 C5 C6 120.9(5) . . ?
N1 C7 C6 126.6(5) . . ?
C5 C4 C3 120.8(5) . . ?
C5 C4 Br1 120.2(4) . . ?
C3 C4 Br1 119.0(5) . . ?
N2 C13 C12 111.6(5) . . ?
N1 C8 C9 107.8(5) . . ?
N2 C9 C8 112.3(5) . . ?
O6 C12 C13 112.0(5) . . ?
N2 C10 C11 110.9(5) . . ?
O6 C11 C10 111.8(6) . . ?

_refine_diff_density_max         0.592
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.098

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

data_Complex_3
_database_code_depnum_ccdc_archive 'CCDC 1889359'
loop_
_audit_author_name
_audit_author_address
'Abani Sarkar'
;university of calcutta 
India
;
_audit_update_record             
;
2019-08-05 deposited with the CCDC.	2019-08-22 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_RINTA01_Complex_3           
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: Due to low angle diffraction
;
_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            'C34 H44 Br2 N4 Ni3 O12'
_chemical_formula_weight         1036.68

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      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                   11.1778(13)
_cell_length_b                   9.5533(11)
_cell_length_c                   19.611(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.854(7)
_cell_angle_gamma                90
_cell_volume                     2033.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    3857
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      22.63

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_F_000             1052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    3.403
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   '(SADABS; Bruker, 2015)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27090
_diffrn_reflns_av_unetI/netI     0.1668
_diffrn_reflns_av_R_equivalents  0.2088
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.021
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3571
_reflns_number_gt                1800
_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 APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0446P)²+18.1768P] 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         3571
_refine_ls_number_parameters     252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1904
_refine_ls_R_factor_gt           0.0832
_refine_ls_wR_factor_ref         0.1773
_refine_ls_wR_factor_gt          0.1462
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Br1 Br 1.05558(12) 0.61210(18) 0.30214(7) 0.0675(5) Uani 1 1 d . . . . .
Ni1 Ni 0.40089(12) 0.69115(15) 0.09957(7) 0.0282(4) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.500000 0.000000 0.0301(5) Uani 1 2 d S . P . .
O1 O 0.5646(6) 0.6096(8) 0.0930(3) 0.0331(19) Uani 1 1 d . . . . .
O2 O 0.4590(7) 0.6792(8) -0.0543(4) 0.039(2) Uani 1 1 d . . . . .
O3 O 0.4033(6) 0.8268(7) 0.0222(4) 0.0338(19) Uani 1 1 d . . . . .
O4 O 0.3514(7) 0.4960(8) 0.1477(4) 0.040(2) Uani 1 1 d . . . . .
O5 O 0.3331(6) 0.5179(7) 0.0332(4) 0.0344(19) Uani 1 1 d . . . . .
O11 O 0.0178(8) 0.7969(11) 0.0058(4) 0.062(3) Uani 1 1 d . . . . .
N1 N 0.4889(8) 0.8055(10) 0.1808(4) 0.036(2) Uani 1 1 d . . . . .
N2 N 0.2364(8) 0.7907(10) 0.1219(4) 0.037(2) Uani 1 1 d . . . . .
C1 C 0.6702(10) 0.6117(12) 0.1379(5) 0.033(3) Uani 1 1 d . . . . .
C2 C 0.7670(10) 0.5249(12) 0.1316(5) 0.032(3) Uani 1 1 d . . . . .
H2 H 0.754061 0.464115 0.093498 0.039 Uiso 1 1 calc R U . . .
C3 C 0.8809(10) 0.5234(13) 0.1783(6) 0.040(3) Uani 1 1 d . . . . .
H3 H 0.942660 0.463304 0.171754 0.048 Uiso 1 1 calc R U . . .
C4 C 0.9006(9) 0.6132(14) 0.2348(6) 0.040(3) Uani 1 1 d . . . . .
C5 C 0.8127(10) 0.7009(13) 0.2434(5) 0.042(3) Uani 1 1 d . . . . .
H5 H 0.830249 0.761913 0.281391 0.050 Uiso 1 1 calc R U . . .
C6 C 0.6933(9) 0.7057(12) 0.1971(5) 0.032(3) Uani 1 1 d . . . . .
C7 C 0.6019(11) 0.7978(12) 0.2129(5) 0.037(3) Uani 1 1 d . . . . .
H7 H 0.628247 0.858151 0.250763 0.044 Uiso 1 1 calc R U . . .
C8 C 0.4088(11) 0.9022(13) 0.2073(6) 0.045(3) Uani 1 1 d . . . . .
H8A H 0.401003 0.989893 0.181649 0.054 Uiso 1 1 calc R U . . .
H8B H 0.442963 0.921613 0.256685 0.054 Uiso 1 1 calc R U . . .
C9 C 0.2844(11) 0.8323(13) 0.1970(6) 0.048(3) Uani 1 1 d . . . . .
H9A H 0.291798 0.749938 0.226703 0.057 Uiso 1 1 calc R U . . .
H9B H 0.226842 0.896116 0.210731 0.057 Uiso 1 1 calc R U . . .
C10 C 0.1938(11) 0.9172(12) 0.0783(6) 0.046(3) Uani 1 1 d . . . . .
H10A H 0.264152 0.974487 0.075675 0.055 Uiso 1 1 calc R U . . .
H10B H 0.140105 0.972412 0.100020 0.055 Uiso 1 1 calc R U . . .
C11 C 0.1242(12) 0.8739(15) 0.0043(7) 0.060(4) Uani 1 1 d . . . . .
H11A H 0.101182 0.956850 -0.024382 0.071 Uiso 1 1 calc R U . . .
H11B H 0.177721 0.817591 -0.017014 0.071 Uiso 1 1 calc R U . . .
C12 C 0.0554(11) 0.6712(14) 0.0454(7) 0.052(4) Uani 1 1 d . . . . .
H12A H 0.107755 0.616464 0.022626 0.063 Uiso 1 1 calc R U . . .
H12B H -0.016754 0.615534 0.046346 0.063 Uiso 1 1 calc R U . . .
C13 C 0.1237(10) 0.7040(13) 0.1189(6) 0.042(3) Uani 1 1 d . . . . .
H13A H 0.147606 0.617064 0.144025 0.051 Uiso 1 1 calc R U . . .
H13B H 0.069321 0.753743 0.142312 0.051 Uiso 1 1 calc R U . . .
C14 C 0.3234(9) 0.4434(12) 0.0863(6) 0.032(3) Uani 1 1 d . . . . .
C15 C 0.2768(11) 0.2975(12) 0.0749(6) 0.053(4) Uani 1 1 d . . . . .
H15A H 0.315847 0.240669 0.114291 0.080 Uiso 1 1 calc R U . . .
H15B H 0.295079 0.260806 0.032959 0.080 Uiso 1 1 calc R U . . .
H15C H 0.189223 0.296877 0.069987 0.080 Uiso 1 1 calc R U . . .
C16 C 0.4224(10) 0.7962(13) -0.0371(6) 0.037(3) Uani 1 1 d . . . . .
C17 C 0.3993(12) 0.9106(13) -0.0907(6) 0.059(4) Uani 1 1 d . . . . .
H17A H 0.458955 0.983619 -0.076303 0.089 Uiso 1 1 calc R U . . .
H17B H 0.318004 0.947729 -0.095059 0.089 Uiso 1 1 calc R U . . .
H17C H 0.406040 0.873740 -0.135174 0.089 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C4 1.911(10) . ?
Ni1 N1 1.987(9) . ?
Ni1 O3 2.001(7) . ?
Ni1 O1 2.021(7) . ?
Ni1 O5 2.129(7) . ?
Ni1 N2 2.205(9) . ?
Ni1 O4 2.218(8) . ?
Ni1 C14 2.512(11) . ?
Ni2 O2 2.010(8) . ?
Ni2 O2 2.010(8) 3_665 ?
Ni2 O1 2.077(6) 3_665 ?
Ni2 O1 2.078(6) . ?
Ni2 O5 2.125(7) 3_665 ?
Ni2 O5 2.125(7) . ?
O1 C1 1.292(11) . ?
O2 C16 1.264(13) . ?
O3 C16 1.264(13) . ?
O4 C14 1.271(12) . ?
O5 C14 1.288(12) . ?
O11 C11 1.404(14) . ?
O11 C12 1.438(14) . ?
N1 C7 1.272(12) . ?
N1 C8 1.466(13) . ?
N2 C10 1.491(14) . ?
N2 C9 1.496(13) . ?
N2 C13 1.497(13) . ?
C1 C2 1.392(14) . ?
C1 C6 1.443(14) . ?
C2 C3 1.378(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.377(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.332(15) . ?
C5 C6 1.424(14) . ?
C5 H5 0.9300 . ?
C6 C7 1.437(14) . ?
C7 H7 0.9300 . ?
C8 C9 1.513(15) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.532(15) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.493(15) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.486(15) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.496(15) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 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
N1 Ni1 O3 99.1(3) . . ?
N1 Ni1 O1 88.9(3) . . ?
O3 Ni1 O1 91.4(3) . . ?
N1 Ni1 O5 162.3(3) . . ?
O3 Ni1 O5 96.1(3) . . ?
O1 Ni1 O5 81.8(3) . . ?
N1 Ni1 N2 83.1(3) . . ?
O3 Ni1 N2 92.0(3) . . ?
O1 Ni1 N2 171.7(3) . . ?
O5 Ni1 N2 105.4(3) . . ?
N1 Ni1 O4 104.3(3) . . ?
O3 Ni1 O4 156.5(3) . . ?
O1 Ni1 O4 91.4(3) . . ?
O5 Ni1 O4 61.2(3) . . ?
N2 Ni1 O4 88.5(3) . . ?
N1 Ni1 C14 133.9(4) . . ?
O3 Ni1 C14 126.8(4) . . ?
O1 Ni1 C14 85.7(3) . . ?
O5 Ni1 C14 30.8(3) . . ?
N2 Ni1 C14 98.2(3) . . ?
O4 Ni1 C14 30.4(3) . . ?
O2 Ni2 O2 180.0 . 3_665 ?
O2 Ni2 O1 88.7(3) . 3_665 ?
O2 Ni2 O1 91.3(3) 3_665 3_665 ?
O2 Ni2 O1 91.3(3) . . ?
O2 Ni2 O1 88.7(3) 3_665 . ?
O1 Ni2 O1 180.0 3_665 . ?
O2 Ni2 O5 90.7(3) . 3_665 ?
O2 Ni2 O5 89.3(3) 3_665 3_665 ?
O1 Ni2 O5 80.6(3) 3_665 3_665 ?
O1 Ni2 O5 99.4(3) . 3_665 ?
O2 Ni2 O5 89.3(3) . . ?
O2 Ni2 O5 90.7(3) 3_665 . ?
O1 Ni2 O5 99.4(3) 3_665 . ?
O1 Ni2 O5 80.6(3) . . ?
O5 Ni2 O5 180.0 3_665 . ?
C1 O1 Ni1 130.1(7) . . ?
C1 O1 Ni2 132.4(7) . . ?
Ni1 O1 Ni2 96.9(3) . . ?
C16 O2 Ni2 131.2(7) . . ?
C16 O3 Ni1 125.7(7) . . ?
C14 O4 Ni1 87.7(6) . . ?
C14 O5 Ni2 117.0(6) . . ?
C14 O5 Ni1 91.2(6) . . ?
Ni2 O5 Ni1 92.3(3) . . ?
C11 O11 C12 108.0(9) . . ?
C7 N1 C8 118.6(9) . . ?
C7 N1 Ni1 127.4(8) . . ?
C8 N1 Ni1 113.8(7) . . ?
C10 N2 C9 109.8(9) . . ?
C10 N2 C13 106.0(8) . . ?
C9 N2 C13 106.6(9) . . ?
C10 N2 Ni1 113.8(7) . . ?
C9 N2 Ni1 101.0(6) . . ?
C13 N2 Ni1 119.2(7) . . ?
O1 C1 C2 122.3(10) . . ?
O1 C1 C6 121.1(10) . . ?
C2 C1 C6 116.7(9) . . ?
C3 C2 C1 124.2(10) . . ?
C3 C2 H2 117.9 . . ?
C1 C2 H2 117.9 . . ?
C4 C3 C2 118.2(11) . . ?
C4 C3 H3 120.9 . . ?
C2 C3 H3 120.9 . . ?
C5 C4 C3 120.8(10) . . ?
C5 C4 Br1 119.3(9) . . ?
C3 C4 Br1 119.8(10) . . ?
C4 C5 C6 123.2(10) . . ?
C4 C5 H5 118.4 . . ?
C6 C5 H5 118.4 . . ?
C5 C6 C7 119.3(10) . . ?
C5 C6 C1 116.9(10) . . ?
C7 C6 C1 123.8(9) . . ?
N1 C7 C6 127.0(10) . . ?
N1 C7 H7 116.5 . . ?
C6 C7 H7 116.5 . . ?
N1 C8 C9 107.1(9) . . ?
N1 C8 H8A 110.3 . . ?
C9 C8 H8A 110.3 . . ?
N1 C8 H8B 110.3 . . ?
C9 C8 H8B 110.3 . . ?
H8A C8 H8B 108.5 . . ?
N2 C9 C8 110.5(9) . . ?
N2 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
N2 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
N2 C10 C11 110.1(10) . . ?
N2 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
N2 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
O11 C11 C10 111.2(10) . . ?
O11 C11 H11A 109.4 . . ?
C10 C11 H11A 109.4 . . ?
O11 C11 H11B 109.4 . . ?
C10 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
O11 C12 C13 111.2(10) . . ?
O11 C12 H12A 109.4 . . ?
C13 C12 H12A 109.4 . . ?
O11 C12 H12B 109.4 . . ?
C13 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?
C12 C13 N2 112.6(9) . . ?
C12 C13 H13A 109.1 . . ?
N2 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
N2 C13 H13B 109.1 . . ?
H13A C13 H13B 107.8 . . ?
O4 C14 O5 119.8(10) . . ?
O4 C14 C15 120.8(11) . . ?
O5 C14 C15 119.4(10) . . ?
O4 C14 Ni1 61.9(6) . . ?
O5 C14 Ni1 57.9(5) . . ?
C15 C14 Ni1 177.3(9) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O3 C16 O2 126.0(10) . . ?
O3 C16 C17 116.0(12) . . ?
O2 C16 C17 118.0(11) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 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 C1 C2 165.6(8) . . . . ?
Ni2 O1 C1 C2 -3.6(16) . . . . ?
Ni1 O1 C1 C6 -14.8(16) . . . . ?
Ni2 O1 C1 C6 176.1(7) . . . . ?
O1 C1 C2 C3 -179.8(10) . . . . ?
C6 C1 C2 C3 0.5(17) . . . . ?
C1 C2 C3 C4 0.0(17) . . . . ?
C2 C3 C4 C5 -1.2(18) . . . . ?
C2 C3 C4 Br1 178.6(8) . . . . ?
C3 C4 C5 C6 1.9(19) . . . . ?
Br1 C4 C5 C6 -177.9(9) . . . . ?
C4 C5 C6 C7 176.2(11) . . . . ?
C4 C5 C6 C1 -1.3(17) . . . . ?
O1 C1 C6 C5 -179.6(10) . . . . ?
C2 C1 C6 C5 0.1(15) . . . . ?
O1 C1 C6 C7 3.0(17) . . . . ?
C2 C1 C6 C7 -177.3(10) . . . . ?
C8 N1 C7 C6 177.1(11) . . . . ?
Ni1 N1 C7 C6 1.3(18) . . . . ?
C5 C6 C7 N1 -173.4(11) . . . . ?
C1 C6 C7 N1 3.9(19) . . . . ?
C7 N1 C8 C9 -143.2(11) . . . . ?
Ni1 N1 C8 C9 33.2(11) . . . . ?
C10 N2 C9 C8 -74.0(11) . . . . ?
C13 N2 C9 C8 171.6(9) . . . . ?
Ni1 N2 C9 C8 46.5(10) . . . . ?
N1 C8 C9 N2 -54.9(12) . . . . ?
C9 N2 C10 C11 -170.1(9) . . . . ?
C13 N2 C10 C11 -55.3(12) . . . . ?
Ni1 N2 C10 C11 77.5(10) . . . . ?
C12 O11 C11 C10 -62.1(13) . . . . ?
N2 C10 C11 O11 62.4(13) . . . . ?
C11 O11 C12 C13 60.1(13) . . . . ?
O11 C12 C13 N2 -58.7(13) . . . . ?
C10 N2 C13 C12 55.0(12) . . . . ?
C9 N2 C13 C12 172.0(10) . . . . ?
Ni1 N2 C13 C12 -74.8(11) . . . . ?
Ni1 O4 C14 O5 -1.2(9) . . . . ?
Ni1 O4 C14 C15 -179.9(9) . . . . ?
Ni2 O5 C14 O4 94.5(10) . . . . ?
Ni1 O5 C14 O4 1.3(9) . . . . ?
Ni2 O5 C14 C15 -86.8(10) . . . . ?
Ni1 O5 C14 C15 180.0(9) . . . . ?
Ni2 O5 C14 Ni1 93.2(5) . . . . ?
Ni1 O3 C16 O2 -9.9(15) . . . . ?
Ni1 O3 C16 C17 170.2(7) . . . . ?
Ni2 O2 C16 O3 0.4(17) . . . . ?
Ni2 O2 C16 C17 -179.8(7) . . . . ?

_refine_diff_density_max         0.686
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.139

