# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_compound1
_database_code_depnum_ccdc_archive 'CCDC 1043870'
_audit_update_record             
;
2015-01-23 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H26 Br2 N4 Ni O12'
_chemical_formula_weight         732.98

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   12.3321(6)
_cell_length_b                   9.5827(4)
_cell_length_c                   21.5074(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.157(4)
_cell_angle_gamma                90.00
_cell_volume                     2534.95(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5664
_cell_measurement_theta_min      1.9674
_cell_measurement_theta_max      29.0359

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.3006
_exptl_crystal_size_mid          0.1611
_exptl_crystal_size_min          0.0542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_exptl_absorpt_coefficient_mu    3.990
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.395
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16816
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         29.03
_reflns_number_total             5889
_reflns_number_gt                4775
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1997)'


_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0378P)²+1.3766P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5889
_refine_ls_number_parameters     378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0843
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.75696(4) 0.14012(4) 0.180031(18) 0.01080(11) Uani 1 1 d . . .
Br1A Br 0.96925(3) 0.21439(3) -0.133097(15) 0.01511(10) Uani 1 1 d . . .
Br2A Br 0.55008(3) 0.31893(3) 0.485253(15) 0.01630(10) Uani 1 1 d . . .
C1A C 0.7995(3) 0.0008(3) 0.06306(15) 0.0142(7) Uani 1 1 d . . .
H1A H 0.8051 -0.0803 0.0397 0.017 Uiso 1 1 calc R . .
C2A C 0.8369(3) 0.1263(3) 0.03546(14) 0.0116(7) Uani 1 1 d . . .
C3A C 0.8286(3) 0.2591(3) 0.06378(14) 0.0106(7) Uani 1 1 d . . .
C4A C 0.8598(3) 0.3787(3) 0.02993(15) 0.0111(7) Uani 1 1 d . . .
C5A C 0.8987(3) 0.3643(3) -0.02823(14) 0.0128(7) Uani 1 1 d . . .
H5A H 0.9163 0.4431 -0.0507 0.015 Uiso 1 1 calc R . .
C6A C 0.9116(3) 0.2315(3) -0.05354(15) 0.0119(7) Uani 1 1 d . . .
C7A C 0.8810(3) 0.1154(3) -0.02303(14) 0.0121(7) Uani 1 1 d . . .
H7A H 0.8893 0.0280 -0.0409 0.015 Uiso 1 1 calc R . .
C8A C 0.8508(3) 0.5177(3) 0.06158(15) 0.0115(7) Uani 1 1 d . . .
H8A1 H 0.8668 0.5917 0.0329 0.014 Uiso 1 1 calc R . .
H8A2 H 0.9035 0.5227 0.0972 0.014 Uiso 1 1 calc R . .
C9A C 0.6569(3) 0.5455(4) 0.02876(15) 0.0168(7) Uani 1 1 d . . .
H9A1 H 0.5849 0.5449 0.0430 0.025 Uiso 1 1 calc R . .
H9A2 H 0.6657 0.4666 0.0021 0.025 Uiso 1 1 calc R . .
H9A3 H 0.6677 0.6299 0.0060 0.025 Uiso 1 1 calc R . .
C10A C 0.7309(3) 0.6650(3) 0.12332(15) 0.0152(7) Uani 1 1 d . . .
H10A H 0.6555 0.6944 0.1224 0.018 Uiso 1 1 calc R . .
H10B H 0.7716 0.7396 0.1054 0.018 Uiso 1 1 calc R . .
C11A C 0.7732(3) 0.6459(3) 0.19061(15) 0.0153(7) Uani 1 1 d . . .
H11A H 0.8414 0.5954 0.1916 0.018 Uiso 1 1 calc R . .
H11B H 0.7881 0.7371 0.2088 0.018 Uiso 1 1 calc R . .
C12A C 0.5898(3) 0.6383(4) 0.23291(17) 0.0195(8) Uani 1 1 d . . .
H12A H 0.6000 0.7341 0.2449 0.029 Uiso 1 1 calc R . .
H12B H 0.5488 0.5912 0.2629 0.029 Uiso 1 1 calc R . .
H12C H 0.5510 0.6337 0.1926 0.029 Uiso 1 1 calc R . .
C13A C 0.7490(3) 0.5475(3) 0.29573(15) 0.0147(7) Uani 1 1 d . . .
H13A H 0.8268 0.5348 0.2942 0.018 Uiso 1 1 calc R . .
H13B H 0.7371 0.6295 0.3208 0.018 Uiso 1 1 calc R . .
C14A C 0.7012(3) 0.4218(3) 0.32534(15) 0.0131(7) Uani 1 1 d . . .
C15A C 0.7144(3) 0.2915(3) 0.29427(15) 0.0117(7) Uani 1 1 d . . .
C16A C 0.6796(3) 0.1680(3) 0.32386(14) 0.0108(7) Uani 1 1 d . . .
C17A C 0.6318(3) 0.1780(3) 0.38148(15) 0.0116(7) Uani 1 1 d . . .
H17A H 0.6101 0.0973 0.4012 0.014 Uiso 1 1 calc R . .
C18A C 0.6170(3) 0.3055(3) 0.40857(15) 0.0131(7) Uani 1 1 d . . .
C19A C 0.6524(3) 0.4281(3) 0.38075(15) 0.0142(7) Uani 1 1 d . . .
H19A H 0.6428 0.5139 0.3998 0.017 Uiso 1 1 calc R . .
C20A C 0.6908(3) 0.0302(3) 0.29834(15) 0.0124(7) Uani 1 1 d . . .
H20A H 0.6734 -0.0438 0.3238 0.015 Uiso 1 1 calc R . .
N1A N 0.7375(2) 0.5380(3) 0.08298(12) 0.0110(6) Uani 1 1 d . . .
N2A N 0.6977(2) 0.5695(3) 0.23028(12) 0.0102(6) Uani 1 1 d . . .
O1A O 0.7605(2) -0.0129(2) 0.11439(10) 0.0152(5) Uani 1 1 d . . .
O2A O 0.79139(19) 0.2807(2) 0.11796(10) 0.0123(5) Uani 1 1 d . . .
O3A O 0.75885(19) 0.2940(2) 0.24163(10) 0.0128(5) Uani 1 1 d . . .
O4A O 0.72101(19) -0.0012(2) 0.24649(10) 0.0140(5) Uani 1 1 d . . .
N1C N 0.5341(2) 0.2688(3) 0.14122(12) 0.0144(6) Uani 1 1 d . . .
O1C O 0.5869(2) 0.1592(2) 0.15821(11) 0.0166(5) Uani 1 1 d . . .
O2C O 0.5771(2) 0.3876(2) 0.14848(11) 0.0181(5) Uani 1 1 d . . .
O3C O 0.4402(2) 0.2580(3) 0.11810(12) 0.0217(6) Uani 1 1 d . . .
N1D N 1.1199(2) 0.2581(3) 0.09567(13) 0.0156(6) Uani 1 1 d . . .
O1D O 1.1151(2) 0.3688(3) 0.12692(12) 0.0305(7) Uani 1 1 d . . .
O2D O 1.0662(2) 0.1538(2) 0.11032(11) 0.0192(5) Uani 1 1 d . . .
O3D O 1.1789(2) 0.2514(3) 0.05156(12) 0.0255(6) Uani 1 1 d . . .
O1W O 0.9224(2) 0.1130(3) 0.20143(12) 0.0160(5) Uani 1 1 d . . .
O2W O 0.9817(3) 0.4185(3) 0.22139(14) 0.0244(6) Uani 1 1 d . . .
H1N1 H 0.717(3) 0.452(5) 0.1016(19) 0.037(12) Uiso 1 1 d . . .
H1W1 H 0.946(3) 0.056(4) 0.2257(17) 0.017(11) Uiso 1 1 d . . .
H1N2 H 0.688(3) 0.499(4) 0.2141(18) 0.026(12) Uiso 1 1 d . . .
H2W1 H 0.963(4) 0.126(5) 0.172(2) 0.035(13) Uiso 1 1 d . . .
H1W2 H 1.017(4) 0.393(5) 0.195(2) 0.037(15) Uiso 1 1 d . . .
H2W2 H 0.934(5) 0.356(5) 0.232(2) 0.058(17) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2A 1.965(2) . ?
Ni1 O3A 1.981(2) . ?
Ni1 O1A 2.039(2) . ?
Ni1 O4A 2.041(2) . ?
Ni1 O1W 2.074(3) . ?
Ni1 O1C 2.123(2) . ?
Br1A C6A 1.907(3) . ?
Br2A C18A 1.901(3) . ?
C1A O1A 1.243(4) . ?
C1A C2A 1.432(4) . ?
C2A C7A 1.410(5) . ?
C2A C3A 1.418(4) . ?
C3A O2A 1.300(4) . ?
C3A C4A 1.425(4) . ?
C4A C5A 1.379(5) . ?
C4A C8A 1.503(4) . ?
C5A C6A 1.397(5) . ?
C6A C7A 1.359(5) . ?
C8A N1A 1.515(4) . ?
C9A N1A 1.478(4) . ?
C10A N1A 1.500(4) . ?
C10A C11A 1.514(4) . ?
C11A N2A 1.498(4) . ?
C12A N2A 1.490(4) . ?
C13A C14A 1.503(5) . ?
C13A N2A 1.516(4) . ?
C14A C19A 1.375(4) . ?
C14A C15A 1.431(4) . ?
C15A O3A 1.293(4) . ?
C15A C16A 1.425(4) . ?
C16A C17A 1.413(5) . ?
C16A C20A 1.441(4) . ?
C17A C18A 1.371(4) . ?
C18A C19A 1.403(5) . ?
C20A O4A 1.238(4) . ?
N1C O3C 1.232(3) . ?
N1C O2C 1.261(3) . ?
N1C O1C 1.276(3) . ?
N1D O3D 1.238(4) . ?
N1D O2D 1.252(4) . ?
N1D O1D 1.260(4) . ?

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
O2A Ni1 O3A 87.22(9) . . ?
O2A Ni1 O1A 90.36(9) . . ?
O3A Ni1 O1A 177.20(10) . . ?
O2A Ni1 O4A 178.27(9) . . ?
O3A Ni1 O4A 91.05(9) . . ?
O1A Ni1 O4A 91.38(9) . . ?
O2A Ni1 O1W 88.82(10) . . ?
O3A Ni1 O1W 88.93(10) . . ?
O1A Ni1 O1W 89.62(10) . . ?
O4A Ni1 O1W 91.22(10) . . ?
O2A Ni1 O1C 92.84(9) . . ?
O3A Ni1 O1C 92.72(9) . . ?
O1A Ni1 O1C 88.80(9) . . ?
O4A Ni1 O1C 87.17(9) . . ?
O1W Ni1 O1C 177.72(9) . . ?
O1A C1A C2A 127.9(3) . . ?
C7A C2A C3A 119.6(3) . . ?
C7A C2A C1A 117.7(3) . . ?
C3A C2A C1A 122.7(3) . . ?
O2A C3A C2A 124.7(3) . . ?
O2A C3A C4A 117.1(3) . . ?
C2A C3A C4A 118.2(3) . . ?
C5A C4A C3A 120.5(3) . . ?
C5A C4A C8A 122.8(3) . . ?
C3A C4A C8A 116.7(3) . . ?
C4A C5A C6A 120.1(3) . . ?
C7A C6A C5A 121.0(3) . . ?
C7A C6A Br1A 119.8(2) . . ?
C5A C6A Br1A 119.2(2) . . ?
C6A C7A C2A 120.5(3) . . ?
C4A C8A N1A 110.6(3) . . ?
N1A C10A C11A 115.2(3) . . ?
N2A C11A C10A 114.7(3) . . ?
C14A C13A N2A 110.8(3) . . ?
C19A C14A C15A 121.0(3) . . ?
C19A C14A C13A 122.8(3) . . ?
C15A C14A C13A 116.1(3) . . ?
O3A C15A C16A 124.5(3) . . ?
O3A C15A C14A 117.6(3) . . ?
C16A C15A C14A 117.9(3) . . ?
C17A C16A C15A 119.6(3) . . ?
C17A C16A C20A 117.0(3) . . ?
C15A C16A C20A 123.4(3) . . ?
C18A C17A C16A 120.6(3) . . ?
C17A C18A C19A 120.7(3) . . ?
C17A C18A Br2A 120.5(2) . . ?
C19A C18A Br2A 118.8(2) . . ?
C14A C19A C18A 120.1(3) . . ?
O4A C20A C16A 127.6(3) . . ?
C9A N1A C10A 110.8(3) . . ?
C9A N1A C8A 110.4(3) . . ?
C10A N1A C8A 111.7(3) . . ?
C12A N2A C11A 113.5(3) . . ?
C12A N2A C13A 109.9(3) . . ?
C11A N2A C13A 111.2(3) . . ?
C1A O1A Ni1 124.6(2) . . ?
C3A O2A Ni1 127.4(2) . . ?
C15A O3A Ni1 125.9(2) . . ?
C20A O4A Ni1 124.3(2) . . ?
O3C N1C O2C 120.0(3) . . ?
O3C N1C O1C 119.5(3) . . ?
O2C N1C O1C 120.4(3) . . ?
N1C O1C Ni1 127.6(2) . . ?
O3D N1D O2D 120.1(3) . . ?
O3D N1D O1D 120.3(3) . . ?
O2D N1D O1D 119.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.872
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.220
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.133
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1043871'
_audit_update_record             
;
2015-02-26 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H39 Br2 N3 Ni2 O9'
_chemical_formula_weight         886.90

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           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                   20.9791(14)
_cell_length_b                   14.469(2)
_cell_length_c                   26.9753(19)
_cell_angle_alpha                90
_cell_angle_beta                 118.361(9)
_cell_angle_gamma                90
_cell_volume                     7205.3(14)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13825
_cell_measurement_theta_min      1.7123
_cell_measurement_theta_max      28.2028

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_F_000             3600
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_exptl_absorpt_coefficient_mu    3.318
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27066
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.716
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6345
_reflns_number_gt                5721
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_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)+(0.0218P)²+17.8997P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6345
_refine_ls_number_parameters     477
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0297
_refine_ls_wR_factor_ref         0.0669
_refine_ls_wR_factor_gt          0.0649
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_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 0.23849(2) 0.34594(2) 0.16646(2) 0.02019(9) Uani 1 1 d . . . . .
Ni2 Ni 0.08321(2) 0.37920(2) 0.15900(2) 0.02354(9) Uani 1 1 d . . . . .
Br1A Br 0.32287(2) 0.36320(2) 0.47052(2) 0.04029(9) Uani 1 1 d . . . . .
Br2A Br 0.02473(2) 0.03435(2) -0.06245(2) 0.05347(12) Uani 1 1 d . . . . .
C1A C 0.09483(15) 0.4010(2) 0.27083(12) 0.0279(6) Uani 1 1 d . . . . .
H1A H 0.0723 0.4023 0.2933 0.033 Uiso 1 1 calc R U . . .
C2A C 0.17238(14) 0.38334(18) 0.29974(11) 0.0214(6) Uani 1 1 d . . . . .
C3A C 0.21614(14) 0.37809(17) 0.27264(11) 0.0197(5) Uani 1 1 d . . . . .
C4A C 0.29274(14) 0.38294(17) 0.30751(11) 0.0214(6) Uani 1 1 d . . . . .
C5A C 0.32185(14) 0.37829(18) 0.36517(11) 0.0241(6) Uani 1 1 d . . . . .
H5A H 0.3719 0.3780 0.3875 0.029 Uiso 1 1 calc R U . . .
C6A C 0.27775(15) 0.37397(18) 0.39084(11) 0.0246(6) Uani 1 1 d . . . . .
C7A C 0.20450(15) 0.37928(18) 0.35908(11) 0.0252(6) Uani 1 1 d . . . . .
H7A H 0.1754 0.3803 0.3765 0.030 Uiso 1 1 calc R U . . .
C8A C 0.34206(14) 0.4046(2) 0.28275(11) 0.0259(6) Uani 1 1 d . . . . .
H8AA H 0.3295 0.4656 0.2659 0.031 Uiso 1 1 calc R U . . .
H8AB H 0.3912 0.4080 0.3135 0.031 Uiso 1 1 calc R U . . .
C9A C 0.39902(15) 0.3709(2) 0.22672(13) 0.0387(8) Uani 1 1 d . . . . .
H9AA H 0.3892 0.4331 0.2127 0.058 Uiso 1 1 calc R U . . .
H9AB H 0.4002 0.3311 0.1987 0.058 Uiso 1 1 calc R U . . .
H9AC H 0.4450 0.3687 0.2603 0.058 Uiso 1 1 calc R U . . .
C10A C 0.35522(15) 0.2421(2) 0.26105(12) 0.0317(7) Uani 1 1 d . . . . .
H10A H 0.3762 0.2424 0.3018 0.038 Uiso 1 1 calc R U . . .
H10B H 0.3897 0.2133 0.2514 0.038 Uiso 1 1 calc R U . . .
C11A C 0.28532(16) 0.1863(2) 0.23570(12) 0.0307(7) Uani 1 1 d . . . . .
H11A H 0.2964 0.1213 0.2445 0.037 Uiso 1 1 calc R U . . .
H11B H 0.2551 0.2062 0.2519 0.037 Uiso 1 1 calc R U . . .
C12A C 0.28589(16) 0.1542(2) 0.14768(13) 0.0327(7) Uani 1 1 d . . . . .
H12A H 0.3316 0.1847 0.1599 0.049 Uiso 1 1 calc R U . . .
H12B H 0.2579 0.1587 0.1074 0.049 Uiso 1 1 calc R U . . .
H12C H 0.2940 0.0903 0.1585 0.049 Uiso 1 1 calc R U . . .
C13A C 0.17305(15) 0.15661(19) 0.15043(12) 0.0290(6) Uani 1 1 d . . . . .
H13A H 0.1492 0.1785 0.1715 0.035 Uiso 1 1 calc R U . . .
H13B H 0.1781 0.0901 0.1550 0.035 Uiso 1 1 calc R U . . .
C14A C 0.12606(15) 0.17897(19) 0.08871(12) 0.0271(6) Uani 1 1 d . . . . .
C15A C 0.10391(14) 0.27187(18) 0.07272(11) 0.0230(6) Uani 1 1 d . . . . .
C16A C 0.05225(15) 0.28872(19) 0.01628(11) 0.0258(6) Uani 1 1 d . . . . .
C17A C 0.02760(15) 0.2175(2) -0.02366(12) 0.0300(7) Uani 1 1 d . . . . .
H17A H -0.0067 0.2296 -0.0608 0.036 Uiso 1 1 calc R U . . .
C18A C 0.05415(16) 0.1307(2) -0.00779(13) 0.0334(7) Uani 1 1 d . . . . .
C19A C 0.10232(15) 0.1106(2) 0.04836(13) 0.0338(7) Uani 1 1 d . . . . .
H19A H 0.1186 0.0503 0.0587 0.041 Uiso 1 1 calc R U . . .
C20A C 0.02300(16) 0.3815(2) -0.00202(12) 0.0309(7) Uani 1 1 d . . . . .
H20A H 0.0436 0.4305 0.0229 0.037 Uiso 1 1 calc R U . . .
N1A N 0.34163(12) 0.33974(17) 0.23974(10) 0.0267(5) Uani 1 1 d . . . . .
N2A N 0.24611(11) 0.19899(15) 0.17416(9) 0.0232(5) Uani 1 1 d . . . . .
O1A O 0.05543(10) 0.41438(14) 0.22017(8) 0.0302(5) Uani 1 1 d . . . . .
O2A O 0.18903(9) 0.36947(13) 0.21819(7) 0.0223(4) Uani 1 1 d . . . . .
O3A O 0.12955(9) 0.33995(12) 0.11002(7) 0.0213(4) Uani 1 1 d . . . . .
O4A O -0.02741(12) 0.39747(15) -0.04869(9) 0.0427(6) Uani 1 1 d . . . . .
C1B C 0.2557(2) 0.6375(2) 0.13576(15) 0.0458(9) Uani 1 1 d . . . . .
H1BA H 0.2082 0.6559 0.1288 0.069 Uiso 1 1 calc R U . . .
H1BB H 0.2671 0.6671 0.1091 0.069 Uiso 1 1 calc R U . . .
H1BC H 0.2906 0.6553 0.1732 0.069 Uiso 1 1 calc R U . . .
C2B C 0.25771(15) 0.53407(19) 0.12980(12) 0.0271(6) Uani 1 1 d . . . . .
C3B C 0.27475(16) 0.4979(2) 0.09014(12) 0.0293(6) Uani 1 1 d . . . . .
H3B H 0.2865 0.5396 0.0695 0.035 Uiso 1 1 calc R U . . .
C4B C 0.27584(14) 0.4033(2) 0.07842(12) 0.0269(6) Uani 1 1 d . . . . .
C5B C 0.2874(2) 0.3761(2) 0.02925(14) 0.0454(9) Uani 1 1 d . . . . .
H5BA H 0.3278 0.3345 0.0419 0.068 Uiso 1 1 calc R U . . .
H5BB H 0.2972 0.4304 0.0135 0.068 Uiso 1 1 calc R U . . .
H5BC H 0.2447 0.3463 0.0010 0.068 Uiso 1 1 calc R U . . .
O1B O 0.24168(10) 0.48656(13) 0.16259(8) 0.0254(4) Uani 1 1 d . . . . .
O2B O 0.26740(10) 0.33762(13) 0.10541(8) 0.0272(4) Uani 1 1 d . . . . .
C1C C -0.13599(17) 0.3806(3) 0.02708(13) 0.0461(9) Uani 1 1 d . . . . .
H1CA H -0.1470 0.4420 0.0342 0.069 Uiso 1 1 calc R U . . .
H1CB H -0.1757 0.3402 0.0200 0.069 Uiso 1 1 calc R U . . .
H1CC H -0.1281 0.3812 -0.0052 0.069 Uiso 1 1 calc R U . . .
C2C C -0.06801(16) 0.3463(2) 0.07814(12) 0.0330(7) Uani 1 1 d . . . . .
C3C C -0.06885(17) 0.2619(2) 0.10230(13) 0.0366(7) Uani 1 1 d . . . . .
H3C H -0.1130 0.2312 0.0879 0.044 Uiso 1 1 calc R U . . .
C4C C -0.00894(17) 0.2187(2) 0.14656(12) 0.0326(7) Uani 1 1 d . . . . .
C5C C -0.0194(2) 0.1271(2) 0.16782(15) 0.0521(10) Uani 1 1 d . . . . .
H5CA H 0.0220 0.0886 0.1771 0.078 Uiso 1 1 calc R U . . .
H5CB H -0.0620 0.0977 0.1391 0.078 Uiso 1 1 calc R U . . .
H5CC H -0.0250 0.1365 0.2008 0.078 Uiso 1 1 calc R U . . .
O1C O -0.01441(10) 0.40093(14) 0.09489(8) 0.0317(5) Uani 1 1 d . . . . .
O2C O 0.05491(10) 0.25138(14) 0.17106(8) 0.0321(5) Uani 1 1 d . . . . .
O1W O 0.10760(12) 0.51730(14) 0.15246(9) 0.0273(4) Uani 1 1 d . . . . .
C1E C -0.0608(3) 0.5939(4) 0.1280(3) 0.0747(13) Uani 1 1 d . . . . .
H1EA H -0.0706 0.5677 0.0846 0.112 Uiso 0.48(8) 1 d R U . A 1
H1EB H -0.0096 0.6047 0.1390 0.112 Uiso 0.19(9) 1 d R U . A 1
H1EC H -0.0624 0.5429 0.1516 0.112 Uiso 0.26(9) 1 d R U . A 1
H1ED H -0.0548 0.6460 0.1072 0.112 Uiso 0.43(11) 1 d R U . B 2
H1EE H -0.0361 0.5393 0.1236 0.112 Uiso 0.69(9) 1 d R U . B 2
H1EF H -0.1127 0.5802 0.1125 0.112 Uiso 0.82(9) 1 d R U . B 2
N1E N -0.0366(4) 0.7683(7) 0.1430(3) 0.053(3) Uani 0.433(12) 1 d . . . C 1
C2E C -0.0470(4) 0.6896(8) 0.1378(3) 0.043(4) Uani 0.440(17) 1 d . . . C 1
N1E' N -0.0093(5) 0.6306(5) 0.2297(5) 0.065(4) Uani 0.487(14) 1 d . . . C 2
C2E' C -0.0327(4) 0.6154(5) 0.1822(5) 0.054(5) Uani 0.52(2) 1 d . . . C 2
H1WA H 0.149(2) 0.519(2) 0.1564(13) 0.038(10) Uiso 1 1 d . . . . .
H1WB H 0.084(3) 0.541(3) 0.121(2) 0.089(17) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O2B 2.0108(19) . ?
Ni1 O1B 2.0400(19) . ?
Ni1 O3A 2.0599(18) . ?
Ni1 O2A 2.1251(17) . ?
Ni1 N1A 2.129(2) . ?
Ni1 N2A 2.135(2) . ?
Ni2 O1C 1.9796(19) . ?
Ni2 O2C 2.016(2) . ?
Ni2 O2A 2.0323(17) . ?
Ni2 O3A 2.0576(18) . ?
Ni2 O1A 2.0578(19) . ?
Ni2 O1W 2.091(2) . ?
Br1A C6A 1.899(3) . ?
Br2A C18A 1.906(3) . ?
C1A O1A 1.231(3) . ?
C1A C2A 1.454(4) . ?
C2A C7A 1.413(4) . ?
C2A C3A 1.421(4) . ?
C3A O2A 1.305(3) . ?
C3A C4A 1.427(4) . ?
C4A C5A 1.376(4) . ?
C4A C8A 1.507(4) . ?
C5A C6A 1.396(4) . ?
C6A C7A 1.360(4) . ?
C8A N1A 1.489(4) . ?
C9A N1A 1.476(4) . ?
C10A N1A 1.500(4) . ?
C10A C11A 1.523(4) . ?
C11A N2A 1.473(3) . ?
C12A N2A 1.481(4) . ?
C13A N2A 1.484(3) . ?
C13A C14A 1.513(4) . ?
C14A C19A 1.377(4) . ?
C14A C15A 1.421(4) . ?
C15A O3A 1.326(3) . ?
C15A C16A 1.409(4) . ?
C16A C17A 1.400(4) . ?
C16A C20A 1.461(4) . ?
C17A C18A 1.359(4) . ?
C18A C19A 1.395(4) . ?
C20A O4A 1.221(3) . ?
C1B C2B 1.507(4) . ?
C2B O1B 1.285(3) . ?
C2B C3B 1.382(4) . ?
C3B C4B 1.408(4) . ?
C4B O2B 1.259(3) . ?
C4B C5B 1.510(4) . ?
C1C C2C 1.521(4) . ?
C2C O1C 1.269(4) . ?
C2C C3C 1.388(5) . ?
C3C C4C 1.403(4) . ?
C4C O2C 1.270(4) . ?
C4C C5C 1.502(4) . ?
C1E C2E' 1.326(14) . ?
C1E C2E 1.413(12) . ?
N1E C2E 1.155(11) . ?
N1E' N1E' 0.97(2) 2 ?
N1E' C2E' 1.157(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2B Ni1 O1B 89.31(7) . . ?
O2B Ni1 O3A 93.01(7) . . ?
O1B Ni1 O3A 93.21(7) . . ?
O2B Ni1 O2A 168.17(7) . . ?
O1B Ni1 O2A 84.94(7) . . ?
O3A Ni1 O2A 77.03(7) . . ?
O2B Ni1 N1A 100.90(8) . . ?
O1B Ni1 N1A 92.63(8) . . ?
O3A Ni1 N1A 164.97(8) . . ?
O2A Ni1 N1A 89.71(8) . . ?
O2B Ni1 N2A 88.99(8) . . ?
O1B Ni1 N2A 174.56(8) . . ?
O3A Ni1 N2A 92.04(8) . . ?
O2A Ni1 N2A 97.64(8) . . ?
N1A Ni1 N2A 82.62(9) . . ?
O1C Ni2 O2C 91.43(8) . . ?
O1C Ni2 O2A 171.12(8) . . ?
O2C Ni2 O2A 96.04(8) . . ?
O1C Ni2 O3A 95.23(8) . . ?
O2C Ni2 O3A 96.65(8) . . ?
O2A Ni2 O3A 79.18(7) . . ?
O1C Ni2 O1A 95.27(8) . . ?
O2C Ni2 O1A 83.12(8) . . ?
O2A Ni2 O1A 90.40(7) . . ?
O3A Ni2 O1A 169.51(7) . . ?
O1C Ni2 O1W 88.14(9) . . ?
O2C Ni2 O1W 173.33(8) . . ?
O2A Ni2 O1W 84.99(8) . . ?
O3A Ni2 O1W 90.02(8) . . ?
O1A Ni2 O1W 90.29(8) . . ?
O1A C1A C2A 127.8(3) . . ?
C7A C2A C3A 120.2(2) . . ?
C7A C2A C1A 115.1(2) . . ?
C3A C2A C1A 124.4(2) . . ?
O2A C3A C2A 122.8(2) . . ?
O2A C3A C4A 119.9(2) . . ?
C2A C3A C4A 117.3(2) . . ?
C5A C4A C3A 119.9(2) . . ?
C5A C4A C8A 118.8(2) . . ?
C3A C4A C8A 120.9(2) . . ?
C4A C5A C6A 121.3(2) . . ?
C7A C6A C5A 120.1(2) . . ?
C7A C6A Br1A 121.6(2) . . ?
C5A C6A Br1A 118.3(2) . . ?
C6A C7A C2A 120.3(3) . . ?
N1A C8A C4A 117.6(2) . . ?
N1A C10A C11A 111.1(2) . . ?
N2A C11A C10A 110.1(2) . . ?
N2A C13A C14A 112.7(2) . . ?
C19A C14A C15A 119.8(3) . . ?
C19A C14A C13A 121.2(3) . . ?
C15A C14A C13A 119.0(2) . . ?
O3A C15A C16A 121.2(2) . . ?
O3A C15A C14A 121.1(2) . . ?
C16A C15A C14A 117.7(2) . . ?
C17A C16A C15A 121.2(3) . . ?
C17A C16A C20A 118.3(3) . . ?
C15A C16A C20A 120.5(3) . . ?
C18A C17A C16A 119.5(3) . . ?
C17A C18A C19A 120.8(3) . . ?
C17A C18A Br2A 119.9(2) . . ?
C19A C18A Br2A 119.3(2) . . ?
C14A C19A C18A 120.8(3) . . ?
O4A C20A C16A 122.7(3) . . ?
C9A N1A C8A 106.8(2) . . ?
C9A N1A C10A 110.5(2) . . ?
C8A N1A C10A 111.4(2) . . ?
C9A N1A Ni1 110.51(18) . . ?
C8A N1A Ni1 108.91(16) . . ?
C10A N1A Ni1 108.65(17) . . ?
C11A N2A C12A 110.4(2) . . ?
C11A N2A C13A 110.1(2) . . ?
C12A N2A C13A 108.3(2) . . ?
C11A N2A Ni1 102.11(17) . . ?
C12A N2A Ni1 114.96(17) . . ?
C13A N2A Ni1 110.80(16) . . ?
C1A O1A Ni2 123.69(18) . . ?
C3A O2A Ni2 127.38(16) . . ?
C3A O2A Ni1 131.82(16) . . ?
Ni2 O2A Ni1 100.79(7) . . ?
C15A O3A Ni2 123.18(16) . . ?
C15A O3A Ni1 119.99(15) . . ?
Ni2 O3A Ni1 102.16(8) . . ?
O1B C2B C3B 125.4(3) . . ?
O1B C2B C1B 115.3(3) . . ?
C3B C2B C1B 119.3(3) . . ?
C2B C3B C4B 125.4(3) . . ?
O2B C4B C3B 125.6(3) . . ?
O2B C4B C5B 115.9(3) . . ?
C3B C4B C5B 118.5(3) . . ?
C2B O1B Ni1 126.47(18) . . ?
C4B O2B Ni1 127.46(18) . . ?
O1C C2C C3C 126.0(3) . . ?
O1C C2C C1C 114.2(3) . . ?
C3C C2C C1C 119.8(3) . . ?
C2C C3C C4C 125.8(3) . . ?
O2C C4C C3C 125.1(3) . . ?
O2C C4C C5C 116.1(3) . . ?
C3C C4C C5C 118.9(3) . . ?
C2C O1C Ni2 125.86(19) . . ?
C4C O2C Ni2 125.16(19) . . ?
N1E C2E C1E 176.6(8) . . ?
N1E' N1E' C2E' 168.9(6) 2 . ?
N1E' C2E' C1E 177.1(9) . . ?

_refine_diff_density_max         0.914
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.060

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1043872'
_audit_update_record             
;
2015-01-23 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C23 H23 Br2 N3 Ni2 O6 S'
_chemical_formula_weight         746.74

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   I2/a

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

_cell_length_a                   21.9768(3)
_cell_length_b                   9.7423(10)
_cell_length_c                   24.826(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.237(2)
_cell_angle_gamma                90.00
_cell_volume                     5293.2(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9469
_cell_measurement_theta_min      4.0010
_cell_measurement_theta_max      73.9580

_exptl_crystal_description       Primatic
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2976
_exptl_absorpt_coefficient_mu    6.426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86096
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22451
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.58
_diffrn_reflns_theta_max         74.30
_reflns_number_total             5329
_reflns_number_gt                4677
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0328P)²+60.3153P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5329
_refine_ls_number_parameters     337
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1071
_refine_ls_wR_factor_gt          0.1030
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.13918(3) 0.16941(7) 0.12864(3) 0.01572(15) Uani 1 1 d . . .
Ni2 Ni 0.13564(3) 0.47213(7) 0.12191(3) 0.01535(15) Uani 1 1 d . . .
Br1A Br -0.174466(19) 0.24170(5) 0.014562(18) 0.02757(13) Uani 1 1 d . . .
Br2A Br 0.46504(2) 0.31555(6) 0.19924(3) 0.04399(17) Uani 1 1 d . . .
C1A C 0.01619(19) 0.5500(4) 0.07061(17) 0.0214(8) Uani 1 1 d . . .
H1A H -0.0100 0.6145 0.0533 0.026 Uiso 1 1 calc R . .
C2A C -0.00941(18) 0.4141(4) 0.07587(16) 0.0189(8) Uani 1 1 d . . .
C3A C 0.02076(18) 0.3050(4) 0.10483(15) 0.0168(8) Uani 1 1 d . . .
C4A C -0.01089(19) 0.1796(5) 0.10896(18) 0.0231(9) Uani 1 1 d . . .
C5A C -0.0679(2) 0.1615(5) 0.08164(18) 0.0245(9) Uani 1 1 d . . .
H5A H -0.0877 0.0773 0.0833 0.029 Uiso 1 1 calc R . .
C6A C -0.09627(17) 0.2690(5) 0.05151(16) 0.0199(8) Uani 1 1 d . . .
C7A C -0.06871(18) 0.3940(4) 0.04960(16) 0.0202(8) Uani 1 1 d . . .
H7A H -0.0888 0.4662 0.0310 0.024 Uiso 1 1 calc R . .
C8A C 0.0170(2) 0.0699(5) 0.1464(2) 0.0386(13) Uani 1 1 d . . .
H8A1 H 0.0232 0.1072 0.1827 0.046 Uiso 1 1 calc R . .
H8A2 H -0.0116 -0.0057 0.1471 0.046 Uiso 1 1 calc R . .
C9A C 0.0623(3) -0.0610(7) 0.0806(4) 0.070(2) Uani 1 1 d . . .
H9A1 H 0.0277 -0.1198 0.0837 0.105 Uiso 1 1 calc R . .
H9A2 H 0.0972 -0.1156 0.0741 0.105 Uiso 1 1 calc R . .
H9A3 H 0.0534 0.0015 0.0510 0.105 Uiso 1 1 calc R . .
C10A C 0.1040(3) -0.0662(7) 0.1771(3) 0.0566(18) Uani 1 1 d . . .
H10A H 0.1007 -0.0170 0.2107 0.068 Uiso 1 1 calc R . .
H10B H 0.0820 -0.1522 0.1790 0.068 Uiso 1 1 calc R . .
C11A C 0.1683(2) -0.0948(5) 0.1710(2) 0.0360(12) Uani 1 1 d . . .
H11A H 0.1705 -0.1679 0.1448 0.043 Uiso 1 1 calc R . .
H11B H 0.1873 -0.1282 0.2054 0.043 Uiso 1 1 calc R . .
C12A C 0.2434(2) -0.0219(5) 0.11177(18) 0.0257(9) Uani 1 1 d . . .
H12A H 0.2708 -0.0920 0.1265 0.039 Uiso 1 1 calc R . .
H12B H 0.2666 0.0543 0.1002 0.039 Uiso 1 1 calc R . .
H12C H 0.2183 -0.0582 0.0814 0.039 Uiso 1 1 calc R . .
C13A C 0.2435(2) 0.0832(4) 0.20037(16) 0.0211(8) Uani 1 1 d . . .
H13A H 0.2709 0.0123 0.2156 0.025 Uiso 1 1 calc R . .
H13B H 0.2177 0.1110 0.2281 0.025 Uiso 1 1 calc R . .
C14A C 0.28100(19) 0.2052(4) 0.18532(16) 0.0193(8) Uani 1 1 d . . .
C15A C 0.25168(18) 0.3249(4) 0.16329(15) 0.0164(7) Uani 1 1 d . . .
C16A C 0.28727(18) 0.4412(4) 0.15337(15) 0.0171(8) Uani 1 1 d . . .
C17A C 0.35132(19) 0.4373(4) 0.16504(17) 0.0215(8) Uani 1 1 d . . .
H17A H 0.3748 0.5143 0.1591 0.026 Uiso 1 1 calc R . .
C18A C 0.37849(19) 0.3197(5) 0.18504(19) 0.0249(9) Uani 1 1 d . . .
C19A C 0.3439(2) 0.2034(5) 0.19535(18) 0.0252(9) Uani 1 1 d . . .
H19A H 0.3634 0.1244 0.2090 0.030 Uiso 1 1 calc R . .
C20A C 0.26277(19) 0.5695(4) 0.13044(16) 0.0208(8) Uani 1 1 d . . .
H20A H 0.2911 0.6391 0.1270 0.025 Uiso 1 1 calc R . .
N1A N 0.07531(19) 0.0171(4) 0.1311(2) 0.0374(10) Uani 1 1 d . . .
N2A N 0.20425(15) 0.0244(3) 0.15369(14) 0.0179(7) Uani 1 1 d . . .
O1A O 0.06762(13) 0.5922(3) 0.08572(11) 0.0194(6) Uani 1 1 d . . .
O2A O 0.07560(12) 0.3185(3) 0.13027(11) 0.0174(5) Uani 1 1 d . . .
O3A O 0.19167(12) 0.3253(3) 0.15500(11) 0.0173(5) Uani 1 1 d . . .
O4A O 0.20942(13) 0.5979(3) 0.11496(12) 0.0219(6) Uani 1 1 d . . .
C1B C 0.1538(3) 0.2849(5) 0.02651(19) 0.0348(12) Uani 1 1 d . . .
C2B C 0.1656(4) 0.2697(8) -0.0325(2) 0.077(3) Uani 1 1 d . . .
H2B1 H 0.1277 0.2785 -0.0548 0.115 Uiso 1 1 calc R . .
H2B2 H 0.1830 0.1811 -0.0381 0.115 Uiso 1 1 calc R . .
H2B3 H 0.1934 0.3398 -0.0419 0.115 Uiso 1 1 calc R . .
O1B O 0.1508(2) 0.1715(4) 0.05197(13) 0.0393(9) Uani 1 1 d . . .
O2B O 0.14682(14) 0.4026(3) 0.04427(12) 0.0229(6) Uani 1 1 d . . .
C1C C 0.12184(17) 0.6157(4) 0.23476(16) 0.0173(8) Uani 1 1 d . . .
N1C N 0.12527(17) 0.5611(4) 0.19377(14) 0.0225(7) Uani 1 1 d . . .
S1C S 0.11681(5) 0.69288(12) 0.29263(4) 0.0286(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1B 1.943(3) . ?
Ni1 O3A 1.982(3) . ?
Ni1 O2A 2.018(3) . ?
Ni1 N1A 2.047(4) . ?
Ni1 N2A 2.066(3) . ?
Ni1 Ni2 2.9545(10) . ?
Ni2 O3A 2.014(3) . ?
Ni2 N1C 2.015(4) . ?
Ni2 O2A 2.019(3) . ?
Ni2 O1A 2.041(3) . ?
Ni2 O4A 2.052(3) . ?
Ni2 O2B 2.079(3) . ?
Br1A C6A 1.891(4) . ?
Br2A C18A 1.903(4) . ?
C1A O1A 1.229(5) . ?
C1A C2A 1.449(6) . ?
C2A C3A 1.414(6) . ?
C2A C7A 1.417(6) . ?
C3A O2A 1.315(5) . ?
C3A C4A 1.414(6) . ?
C4A C5A 1.381(6) . ?
C4A C8A 1.509(6) . ?
C5A C6A 1.400(6) . ?
C6A C7A 1.363(6) . ?
C8A N1A 1.464(7) . ?
C9A N1A 1.472(8) . ?
C10A C11A 1.461(8) . ?
C10A N1A 1.493(7) . ?
C11A N2A 1.490(5) . ?
C12A N2A 1.480(5) . ?
C13A N2A 1.495(5) . ?
C13A C14A 1.512(6) . ?
C14A C19A 1.382(6) . ?
C14A C15A 1.418(6) . ?
C15A O3A 1.316(5) . ?
C15A C16A 1.411(6) . ?
C16A C17A 1.412(6) . ?
C16A C20A 1.456(6) . ?
C17A C18A 1.364(6) . ?
C18A C19A 1.401(7) . ?
C20A O4A 1.232(5) . ?
C1B O2B 1.243(6) . ?
C1B O1B 1.278(6) . ?
C1B C2B 1.518(7) . ?
C1C N1C 1.157(6) . ?
C1C S1C 1.634(4) . ?

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
O1B Ni1 O3A 101.02(15) . . ?
O1B Ni1 O2A 99.50(13) . . ?
O3A Ni1 O2A 79.94(11) . . ?
O1B Ni1 N1A 100.82(19) . . ?
O3A Ni1 N1A 157.78(17) . . ?
O2A Ni1 N1A 92.48(14) . . ?
O1B Ni1 N2A 98.80(14) . . ?
O3A Ni1 N2A 93.36(12) . . ?
O2A Ni1 N2A 161.41(13) . . ?
N1A Ni1 N2A 87.30(15) . . ?
O1B Ni1 Ni2 86.52(11) . . ?
O3A Ni1 Ni2 42.73(8) . . ?
O2A Ni1 Ni2 42.96(8) . . ?
N1A Ni1 Ni2 135.29(12) . . ?
N2A Ni1 Ni2 135.55(10) . . ?
O3A Ni2 N1C 93.37(13) . . ?
O3A Ni2 O2A 79.17(11) . . ?
N1C Ni2 O2A 95.76(13) . . ?
O3A Ni2 O1A 169.44(12) . . ?
N1C Ni2 O1A 90.33(13) . . ?
O2A Ni2 O1A 90.63(11) . . ?
O3A Ni2 O4A 90.01(11) . . ?
N1C Ni2 O4A 88.37(14) . . ?
O2A Ni2 O4A 168.62(12) . . ?
O1A Ni2 O4A 99.98(12) . . ?
O3A Ni2 O2B 91.55(12) . . ?
N1C Ni2 O2B 173.54(14) . . ?
O2A Ni2 O2B 89.28(12) . . ?
O1A Ni2 O2B 85.55(12) . . ?
O4A Ni2 O2B 87.45(13) . . ?
O3A Ni2 Ni1 41.89(8) . . ?
N1C Ni2 Ni1 112.58(10) . . ?
O2A Ni2 Ni1 42.95(8) . . ?
O1A Ni2 Ni1 127.70(9) . . ?
O4A Ni2 Ni1 125.73(9) . . ?
O2B Ni2 Ni1 73.88(8) . . ?
O1A C1A C2A 129.2(4) . . ?
C3A C2A C7A 119.9(4) . . ?
C3A C2A C1A 124.4(4) . . ?
C7A C2A C1A 115.7(4) . . ?
O2A C3A C4A 119.1(4) . . ?
O2A C3A C2A 122.4(4) . . ?
C4A C3A C2A 118.4(4) . . ?
C5A C4A C3A 120.4(4) . . ?
C5A C4A C8A 120.7(4) . . ?
C3A C4A C8A 118.8(4) . . ?
C4A C5A C6A 120.4(4) . . ?
C7A C6A C5A 120.7(4) . . ?
C7A C6A Br1A 119.7(3) . . ?
C5A C6A Br1A 119.6(3) . . ?
C6A C7A C2A 120.0(4) . . ?
N1A C8A C4A 113.9(4) . . ?
C11A C10A N1A 111.7(5) . . ?
C10A C11A N2A 115.1(4) . . ?
N2A C13A C14A 113.5(3) . . ?
C19A C14A C15A 119.5(4) . . ?
C19A C14A C13A 120.2(4) . . ?
C15A C14A C13A 120.2(4) . . ?
O3A C15A C16A 122.3(4) . . ?
O3A C15A C14A 118.4(4) . . ?
C16A C15A C14A 119.2(4) . . ?
C15A C16A C17A 120.1(4) . . ?
C15A C16A C20A 124.5(4) . . ?
C17A C16A C20A 115.4(4) . . ?
C18A C17A C16A 119.5(4) . . ?
C17A C18A C19A 121.3(4) . . ?
C17A C18A Br2A 118.8(3) . . ?
C19A C18A Br2A 119.9(3) . . ?
C14A C19A C18A 120.5(4) . . ?
O4A C20A C16A 128.5(4) . . ?
C8A N1A C9A 107.3(4) . . ?
C8A N1A C10A 108.1(5) . . ?
C9A N1A C10A 114.0(5) . . ?
C8A N1A Ni1 111.8(3) . . ?
C9A N1A Ni1 115.5(4) . . ?
C10A N1A Ni1 100.0(3) . . ?
C12A N2A C11A 108.9(4) . . ?
C12A N2A C13A 109.3(3) . . ?
C11A N2A C13A 111.0(3) . . ?
C12A N2A Ni1 115.3(3) . . ?
C11A N2A Ni1 104.4(3) . . ?
C13A N2A Ni1 107.8(2) . . ?
C1A O1A Ni2 124.0(3) . . ?
C3A O2A Ni1 121.6(2) . . ?
C3A O2A Ni2 127.1(2) . . ?
Ni1 O2A Ni2 94.09(12) . . ?
C15A O3A Ni1 126.5(3) . . ?
C15A O3A Ni2 129.2(3) . . ?
Ni1 O3A Ni2 95.38(11) . . ?
C20A O4A Ni2 125.2(3) . . ?
O2B C1B O1B 127.5(4) . . ?
O2B C1B C2B 118.0(5) . . ?
O1B C1B C2B 114.5(5) . . ?
C1B O1B Ni1 120.7(3) . . ?
C1B O2B Ni2 131.2(3) . . ?
N1C C1C S1C 179.8(4) . . ?
C1C N1C Ni2 176.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        74.30
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         2.544
_refine_diff_density_min         -1.891
_refine_diff_density_rms         0.113
####################################################################### 
# 
# 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_Compound4
_database_code_depnum_ccdc_archive 'CCDC 1043873'
_audit_update_record             
;
2015-01-23 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H61 Br4 N11 Ni3 O17'
_chemical_formula_weight         1583.87

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   21.6387(9)
_cell_length_b                   10.6943(12)
_cell_length_c                   27.2254(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.474(2)
_cell_angle_gamma                90.00
_cell_volume                     5862.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7131
_cell_measurement_theta_min      2.0620
_cell_measurement_theta_max      27.6140

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.794
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3192
_exptl_absorpt_coefficient_mu    3.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68571
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27651
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0556
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.55
_diffrn_reflns_theta_max         25.00
_reflns_number_total             10308
_reflns_number_gt                7841
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0448P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10308
_refine_ls_number_parameters     748
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0862
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.32224(2) 0.30416(5) 0.72428(2) 0.01198(13) Uani 1 1 d . . .
Ni2 Ni 0.20470(2) 0.13688(5) 0.65484(2) 0.01268(13) Uani 1 1 d . . .
Ni3 Ni 0.15480(2) -0.01727(5) 0.73113(2) 0.01196(12) Uani 1 1 d . . .
Br1A Br 0.46712(2) -0.02545(5) 0.54859(2) 0.03139(13) Uani 1 1 d . . .
Br1B Br -0.15944(2) 0.26329(4) 0.541335(17) 0.02341(12) Uani 1 1 d . . .
Br2A Br 0.43704(3) 0.15738(5) 1.013513(18) 0.03296(13) Uani 1 1 d . . .
Br2B Br 0.24200(3) 0.21719(5) 1.00661(2) 0.04162(15) Uani 1 1 d . . .
C1A C 0.2458(2) -0.0217(4) 0.58572(16) 0.0186(10) Uani 1 1 d . . .
H1A H 0.2376 -0.0880 0.5621 0.022 Uiso 1 1 calc R . .
C2A C 0.3100(2) 0.0377(4) 0.59940(16) 0.0156(9) Uani 1 1 d . . .
C3A C 0.33223(19) 0.1390(4) 0.63498(16) 0.0134(9) Uani 1 1 d . . .
C4A C 0.39429(19) 0.1943(4) 0.64139(17) 0.0166(9) Uani 1 1 d . . .
C5A C 0.4329(2) 0.1414(4) 0.61576(17) 0.0184(10) Uani 1 1 d . . .
H5A H 0.4744 0.1753 0.6212 0.022 Uiso 1 1 calc R . .
C6A C 0.4115(2) 0.0408(4) 0.58272(17) 0.0207(10) Uani 1 1 d . . .
C7A C 0.3502(2) -0.0112(4) 0.57354(17) 0.0197(10) Uani 1 1 d . . .
H7A H 0.3355 -0.0783 0.5504 0.024 Uiso 1 1 calc R . .
C8A C 0.4185(2) 0.3132(4) 0.67235(16) 0.0185(10) Uani 1 1 d . . .
H8A1 H 0.4632 0.3306 0.6739 0.022 Uiso 1 1 calc R . .
H8A2 H 0.3903 0.3819 0.6538 0.022 Uiso 1 1 calc R . .
C9A C 0.4609(2) 0.2000(4) 0.75485(18) 0.0219(10) Uani 1 1 d . . .
H9A1 H 0.5044 0.2081 0.7534 0.033 Uiso 1 1 calc R . .
H9A2 H 0.4409 0.1236 0.7379 0.033 Uiso 1 1 calc R . .
H9A3 H 0.4644 0.1988 0.7910 0.033 Uiso 1 1 calc R . .
C10A C 0.4458(2) 0.4255(4) 0.75532(18) 0.0220(10) Uani 1 1 d . . .
H10A H 0.4287 0.4959 0.7318 0.026 Uiso 1 1 calc R . .
H10B H 0.4938 0.4256 0.7664 0.026 Uiso 1 1 calc R . .
C11A C 0.42625(19) 0.4387(4) 0.80298(16) 0.0173(10) Uani 1 1 d . . .
H11A H 0.4462 0.3719 0.8278 0.021 Uiso 1 1 calc R . .
H11B H 0.4425 0.5177 0.8204 0.021 Uiso 1 1 calc R . .
C12A C 0.3245(2) 0.5601(4) 0.77052(17) 0.0197(10) Uani 1 1 d . . .
H12A H 0.3397 0.6149 0.8005 0.030 Uiso 1 1 calc R . .
H12B H 0.2769 0.5558 0.7574 0.030 Uiso 1 1 calc R . .
H12C H 0.3388 0.5916 0.7434 0.030 Uiso 1 1 calc R . .
C13A C 0.3304(2) 0.3924(4) 0.82972(16) 0.0171(9) Uani 1 1 d . . .
H13A H 0.2824 0.3835 0.8153 0.020 Uiso 1 1 calc R . .
H13B H 0.3410 0.4581 0.8561 0.020 Uiso 1 1 calc R . .
C14A C 0.35984(19) 0.2722(4) 0.85684(16) 0.0157(9) Uani 1 1 d . . .
C15A C 0.36200(18) 0.1625(4) 0.82788(16) 0.0139(9) Uani 1 1 d . . .
C16A C 0.39230(18) 0.0542(4) 0.85707(16) 0.0138(9) Uani 1 1 d . . .
C17A C 0.41363(18) 0.0529(4) 0.91215(17) 0.0171(10) Uani 1 1 d . . .
H17A H 0.4319 -0.0194 0.9307 0.021 Uiso 1 1 calc R . .
C18A C 0.4076(2) 0.1573(4) 0.93862(16) 0.0202(10) Uani 1 1 d . . .
C19A C 0.38235(19) 0.2678(4) 0.91169(17) 0.0169(9) Uani 1 1 d . . .
H19A H 0.3805 0.3393 0.9305 0.020 Uiso 1 1 calc R . .
C20A C 0.40393(19) -0.0556(4) 0.82954(18) 0.0196(10) Uani 1 1 d . . .
H20A H 0.3903 -0.0517 0.7930 0.023 Uiso 1 1 calc R . .
N1A N 0.41900(15) 0.3080(3) 0.72720(13) 0.0141(8) Uani 1 1 d . . .
N2A N 0.35245(15) 0.4336(3) 0.78639(13) 0.0141(8) Uani 1 1 d . . .
O1A O 0.20040(13) 0.0043(3) 0.60148(11) 0.0187(7) Uani 1 1 d . . .
O2A O 0.29606(12) 0.1829(2) 0.66118(11) 0.0140(6) Uani 1 1 d . . .
O3A O 0.33674(12) 0.1605(2) 0.77547(10) 0.0134(6) Uani 1 1 d . . .
O4A O 0.43031(15) -0.1518(3) 0.85137(12) 0.0275(8) Uani 1 1 d . . .
C1B C 0.0971(2) 0.2815(4) 0.58176(16) 0.0182(10) Uani 1 1 d . . .
H1B H 0.0819 0.3448 0.5568 0.022 Uiso 1 1 calc R . .
C2B C 0.04660(19) 0.2187(4) 0.59573(16) 0.0158(9) Uani 1 1 d . . .
C3B C 0.05937(19) 0.1247(4) 0.63420(16) 0.0158(9) Uani 1 1 d . . .
C4B C 0.00380(19) 0.0678(4) 0.64196(16) 0.0170(9) Uani 1 1 d . . .
C5B C -0.0592(2) 0.1129(4) 0.61446(17) 0.0212(10) Uani 1 1 d . . .
H5B H -0.0950 0.0779 0.6206 0.025 Uiso 1 1 calc R . .
C6B C -0.07068(19) 0.2088(4) 0.57798(17) 0.0181(10) Uani 1 1 d . . .
C7B C -0.0190(2) 0.2593(4) 0.56785(17) 0.0197(10) Uani 1 1 d . . .
H7B H -0.0269 0.3212 0.5423 0.024 Uiso 1 1 calc R . .
C8B C 0.0116(2) -0.0457(4) 0.67628(17) 0.0194(10) Uani 1 1 d . . .
H8B1 H -0.0314 -0.0676 0.6773 0.023 Uiso 1 1 calc R . .
H8B2 H 0.0264 -0.1151 0.6604 0.023 Uiso 1 1 calc R . .
C9B C 0.0384(2) 0.0826(4) 0.75426(18) 0.0220(10) Uani 1 1 d . . .
H9B1 H -0.0070 0.0721 0.7512 0.033 Uiso 1 1 calc R . .
H9B2 H 0.0421 0.1564 0.7354 0.033 Uiso 1 1 calc R . .
H9B3 H 0.0661 0.0911 0.7908 0.033 Uiso 1 1 calc R . .
C10B C 0.0605(2) -0.1416(4) 0.76316(17) 0.0209(10) Uani 1 1 d . . .
H10C H 0.0597 -0.2157 0.7424 0.025 Uiso 1 1 calc R . .
H10D H 0.0214 -0.1427 0.7725 0.025 Uiso 1 1 calc R . .
C11B C 0.12251(19) -0.1423(4) 0.81293(16) 0.0171(9) Uani 1 1 d . . .
H11C H 0.1200 -0.0749 0.8360 0.021 Uiso 1 1 calc R . .
H11D H 0.1250 -0.2206 0.8315 0.021 Uiso 1 1 calc R . .
C12B C 0.2084(2) -0.2508(4) 0.79181(18) 0.0217(10) Uani 1 1 d . . .
H12D H 0.2262 -0.2944 0.8249 0.033 Uiso 1 1 calc R . .
H12E H 0.2426 -0.2398 0.7776 0.033 Uiso 1 1 calc R . .
H12F H 0.1727 -0.2986 0.7675 0.033 Uiso 1 1 calc R . .
C13B C 0.23782(19) -0.0658(4) 0.84435(16) 0.0178(10) Uani 1 1 d . . .
H13C H 0.2756 -0.0550 0.8336 0.021 Uiso 1 1 calc R . .
H13D H 0.2514 -0.1218 0.8745 0.021 Uiso 1 1 calc R . .
C14B C 0.22091(19) 0.0595(4) 0.86175(16) 0.0147(9) Uani 1 1 d . . .
C15B C 0.19554(18) 0.1579(4) 0.82519(16) 0.0128(9) Uani 1 1 d . . .
C16B C 0.18407(19) 0.2750(4) 0.84482(16) 0.0149(9) Uani 1 1 d . . .
C17B C 0.1996(2) 0.2935(4) 0.89884(17) 0.0190(10) Uani 1 1 d . . .
H17B H 0.1929 0.3714 0.9114 0.023 Uiso 1 1 calc R . .
C18B C 0.2246(2) 0.1965(4) 0.93326(17) 0.0221(10) Uani 1 1 d . . .
C19B C 0.23472(19) 0.0793(4) 0.91488(17) 0.0203(10) Uani 1 1 d . . .
H19B H 0.2510 0.0139 0.9386 0.024 Uiso 1 1 calc R . .
C20B C 0.15371(19) 0.3768(4) 0.80781(18) 0.0198(10) Uani 1 1 d . . .
H20B H 0.1392 0.3587 0.7719 0.024 Uiso 1 1 calc R . .
N1B N 0.05975(15) -0.0281(3) 0.73161(13) 0.0132(7) Uani 1 1 d . . .
N2B N 0.18315(15) -0.1269(3) 0.80018(13) 0.0143(8) Uani 1 1 d . . .
O1B O 0.15779(13) 0.2623(3) 0.59862(11) 0.0173(7) Uani 1 1 d . . .
O2B O 0.12015(12) 0.0854(2) 0.66185(11) 0.0147(6) Uani 1 1 d . . .
O3B O 0.18302(13) 0.1422(2) 0.77428(11) 0.0139(6) Uani 1 1 d . . .
O4B O 0.14602(15) 0.4836(3) 0.82044(13) 0.0260(7) Uani 1 1 d . . .
C1P C 0.2538(2) 0.5065(4) 0.63461(18) 0.0188(10) Uani 1 1 d . . .
C2P C 0.2120(2) 0.5906(5) 0.59355(19) 0.0306(12) Uani 1 1 d . . .
H2P1 H 0.2217 0.6756 0.6050 0.046 Uiso 1 1 calc R . .
H2P2 H 0.1661 0.5731 0.5869 0.046 Uiso 1 1 calc R . .
H2P3 H 0.2207 0.5782 0.5618 0.046 Uiso 1 1 calc R . .
N1P N 0.28649(16) 0.4409(3) 0.66660(14) 0.0154(8) Uani 1 1 d . . .
O1P O 0.21984(12) 0.2785(2) 0.71252(10) 0.0121(6) Uani 1 1 d D . .
O2P O 0.24514(12) 0.0080(2) 0.71815(11) 0.0151(6) Uani 1 1 d D . .
N1C N 0.09696(17) 0.5136(3) 0.68465(13) 0.0175(8) Uani 1 1 d . . .
O1C O 0.06179(14) 0.4206(3) 0.68248(12) 0.0242(7) Uani 1 1 d . . .
O2C O 0.07302(14) 0.6225(3) 0.68181(12) 0.0217(7) Uani 1 1 d . . .
O3C O 0.15692(14) 0.5022(3) 0.69008(12) 0.0232(7) Uani 1 1 d . . .
N1D N 0.34855(17) -0.1951(3) 0.68879(14) 0.0195(8) Uani 1 1 d . . .
O1D O 0.28914(14) -0.1947(3) 0.68755(13) 0.0267(8) Uani 1 1 d . . .
O2D O 0.36876(16) -0.2871(3) 0.67111(13) 0.0332(8) Uani 1 1 d . . .
O3D O 0.38495(14) -0.1036(3) 0.70697(12) 0.0257(7) Uani 1 1 d . . .
C1E C 0.3303(4) -0.1296(8) 0.4358(3) 0.079(2) Uani 1 1 d . . .
C2E C 0.3779(4) -0.2184(8) 0.4319(4) 0.103(3) Uani 1 1 d . . .
H2E1 H 0.3702 -0.2336 0.3953 0.154 Uiso 1 1 calc R . .
H2E2 H 0.3734 -0.2953 0.4484 0.154 Uiso 1 1 calc R . .
H2E3 H 0.4219 -0.1858 0.4492 0.154 Uiso 1 1 calc R . .
N1E N 0.2910(4) -0.0552(7) 0.4381(3) 0.103(2) Uani 1 1 d . . .
C1F C 0.3634(2) -0.3533(5) 0.5493(2) 0.0335(12) Uani 1 1 d . . .
C2F C 0.4304(2) -0.3602(5) 0.5885(2) 0.0366(13) Uani 1 1 d . . .
H2F1 H 0.4348 -0.3027 0.6167 0.055 Uiso 1 1 calc R . .
H2F2 H 0.4617 -0.3388 0.5724 0.055 Uiso 1 1 calc R . .
H2F3 H 0.4390 -0.4436 0.6024 0.055 Uiso 1 1 calc R . .
N1F N 0.3113(2) -0.3483(4) 0.51847(19) 0.0442(12) Uani 1 1 d . . .
C1G C -0.0086(4) 0.5907(8) 0.5637(3) 0.080(2) Uani 1 1 d . . .
C2G C -0.0625(3) 0.5960(6) 0.5814(2) 0.0576(18) Uani 1 1 d . . .
H2G1 H -0.0983 0.5452 0.5590 0.086 Uiso 1 1 calc R . .
H2G2 H -0.0773 0.6809 0.5804 0.086 Uiso 1 1 calc R . .
H2G3 H -0.0484 0.5653 0.6170 0.086 Uiso 1 1 calc R . .
N1G N 0.0340(4) 0.5819(9) 0.5479(3) 0.137(4) Uani 1 1 d . . .
O1W O 0.14512(13) -0.1702(2) 0.67971(11) 0.0179(7) Uani 1 1 d D . .
H2PB H 0.2768 0.0437 0.7401 0.027 Uiso 1 1 d RD . .
H2PA H 0.2647 -0.0615 0.7146 0.027 Uiso 1 1 d RD . .
H1PA H 0.2158 0.2456 0.7390 0.027 Uiso 1 1 d RD . .
H2W1 H 0.1264 -0.2412 0.6787 0.027 Uiso 1 1 d RD . .
H1PB H 0.1938 0.3431 0.7037 0.027 Uiso 1 1 d RD . .
H1W1 H 0.1769 -0.1898 0.6670 0.027 Uiso 1 1 d RD . .


_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 O3A 2.020(3) . ?
Ni1 O2A 2.059(3) . ?
Ni1 N1A 2.066(3) . ?
Ni1 N1P 2.077(4) . ?
Ni1 N2A 2.096(3) . ?
Ni1 O1P 2.137(3) . ?
Ni2 O2A 1.983(3) . ?
Ni2 O2B 1.985(3) . ?
Ni2 O1A 2.007(3) . ?
Ni2 O1B 2.008(3) . ?
Ni2 O1P 2.119(3) . ?
Ni2 O2P 2.129(3) . ?
Ni3 O3B 2.034(3) . ?
Ni3 N1B 2.065(3) . ?
Ni3 O2B 2.071(3) . ?
Ni3 N2B 2.107(3) . ?
Ni3 O1W 2.113(3) . ?
Ni3 O2P 2.127(3) . ?
Br1A C6A 1.906(4) . ?
Br1B C6B 1.903(4) . ?
Br2A C18A 1.901(4) . ?
Br2B C18B 1.905(4) . ?
C1A O1A 1.240(5) . ?
C1A C2A 1.446(6) . ?
C2A C7A 1.407(5) . ?
C2A C3A 1.415(6) . ?
C3A O2A 1.323(4) . ?
C3A C4A 1.418(5) . ?
C4A C5A 1.389(5) . ?
C4A C8A 1.510(6) . ?
C5A C6A 1.370(6) . ?
C6A C7A 1.373(6) . ?
C8A N1A 1.491(5) . ?
C9A N1A 1.492(5) . ?
C10A N1A 1.474(5) . ?
C10A C11A 1.511(6) . ?
C11A N2A 1.493(5) . ?
C12A N2A 1.480(5) . ?
C13A N2A 1.492(5) . ?
C13A C14A 1.503(6) . ?
C14A C19A 1.392(6) . ?
C14A C15A 1.424(6) . ?
C15A O3A 1.328(5) . ?
C15A C16A 1.422(5) . ?
C16A C17A 1.398(6) . ?
C16A C20A 1.463(6) . ?
C17A C18A 1.361(6) . ?
C18A C19A 1.392(6) . ?
C20A O4A 1.221(5) . ?
C1B O1B 1.240(5) . ?
C1B C2B 1.446(5) . ?
C2B C3B 1.405(6) . ?
C2B C7B 1.410(6) . ?
C3B O2B 1.322(5) . ?
C3B C4B 1.431(5) . ?
C4B C5B 1.380(6) . ?
C4B C8B 1.502(6) . ?
C5B C6B 1.385(6) . ?
C6B C7B 1.359(6) . ?
C8B N1B 1.497(5) . ?
C9B N1B 1.485(5) . ?
C10B N1B 1.483(5) . ?
C10B C11B 1.518(6) . ?
C11B N2B 1.484(5) . ?
C12B N2B 1.482(5) . ?
C13B N2B 1.494(5) . ?
C13B C14B 1.510(5) . ?
C14B C19B 1.382(6) . ?
C14B C15B 1.414(6) . ?
C15B O3B 1.322(5) . ?
C15B C16B 1.418(5) . ?
C16B C17B 1.398(6) . ?
C16B C20B 1.465(6) . ?
C17B C18B 1.370(6) . ?
C18B C19B 1.396(6) . ?
C20B O4B 1.222(5) . ?
C1P N1P 1.140(5) . ?
C1P C2P 1.462(6) . ?
N1C O1C 1.240(4) . ?
N1C O3C 1.257(4) . ?
N1C O2C 1.266(4) . ?
N1D O3D 1.239(4) . ?
N1D O2D 1.243(4) . ?
N1D O1D 1.274(4) . ?
C1E N1E 1.183(8) . ?
C1E C2E 1.432(10) . ?
C1F N1F 1.134(6) . ?
C1F C2F 1.455(7) . ?
C1G N1G 1.155(8) . ?
C1G C2G 1.417(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
O3A Ni1 O2A 91.29(11) . . ?
O3A Ni1 N1A 95.13(12) . . ?
O2A Ni1 N1A 90.59(12) . . ?
O3A Ni1 N1P 167.94(11) . . ?
O2A Ni1 N1P 84.28(12) . . ?
N1A Ni1 N1P 96.12(13) . . ?
O3A Ni1 N2A 91.25(12) . . ?
O2A Ni1 N2A 176.47(11) . . ?
N1A Ni1 N2A 86.75(13) . . ?
N1P Ni1 N2A 93.71(13) . . ?
O3A Ni1 O1P 84.06(10) . . ?
O2A Ni1 O1P 80.84(10) . . ?
N1A Ni1 O1P 171.36(12) . . ?
N1P Ni1 O1P 84.16(11) . . ?
N2A Ni1 O1P 101.86(11) . . ?
O2A Ni2 O2B 170.07(11) . . ?
O2A Ni2 O1A 91.08(11) . . ?
O2B Ni2 O1A 94.21(11) . . ?
O2A Ni2 O1B 96.33(11) . . ?
O2B Ni2 O1B 91.83(11) . . ?
O1A Ni2 O1B 92.48(12) . . ?
O2A Ni2 O1P 83.07(10) . . ?
O2B Ni2 O1P 91.44(11) . . ?
O1A Ni2 O1P 174.06(10) . . ?
O1B Ni2 O1P 89.16(11) . . ?
O2A Ni2 O2P 89.37(10) . . ?
O2B Ni2 O2P 82.11(10) . . ?
O1A Ni2 O2P 91.44(11) . . ?
O1B Ni2 O2P 173.02(10) . . ?
O1P Ni2 O2P 87.52(10) . . ?
O3B Ni3 N1B 97.62(12) . . ?
O3B Ni3 O2B 90.78(11) . . ?
N1B Ni3 O2B 90.36(11) . . ?
O3B Ni3 N2B 91.35(12) . . ?
N1B Ni3 N2B 85.90(12) . . ?
O2B Ni3 N2B 175.91(11) . . ?
O3B Ni3 O1W 165.43(10) . . ?
N1B Ni3 O1W 95.93(12) . . ?
O2B Ni3 O1W 83.79(11) . . ?
N2B Ni3 O1W 94.94(12) . . ?
O3B Ni3 O2P 83.67(10) . . ?
N1B Ni3 O2P 170.49(12) . . ?
O2B Ni3 O2P 80.19(10) . . ?
N2B Ni3 O2P 103.51(11) . . ?
O1W Ni3 O2P 82.09(10) . . ?
O1A C1A C2A 128.3(4) . . ?
C7A C2A C3A 120.6(4) . . ?
C7A C2A C1A 114.8(4) . . ?
C3A C2A C1A 124.6(4) . . ?
O2A C3A C2A 121.4(3) . . ?
O2A C3A C4A 120.4(4) . . ?
C2A C3A C4A 118.2(3) . . ?
C5A C4A C3A 119.0(4) . . ?
C5A C4A C8A 118.3(4) . . ?
C3A C4A C8A 122.7(3) . . ?
C6A C5A C4A 121.9(4) . . ?
C5A C6A C7A 120.6(4) . . ?
C5A C6A Br1A 119.3(3) . . ?
C7A C6A Br1A 120.0(3) . . ?
C6A C7A C2A 119.4(4) . . ?
N1A C8A C4A 113.7(3) . . ?
N1A C10A C11A 110.2(3) . . ?
N2A C11A C10A 109.9(3) . . ?
N2A C13A C14A 116.1(3) . . ?
C19A C14A C15A 119.8(4) . . ?
C19A C14A C13A 118.4(4) . . ?
C15A C14A C13A 121.8(4) . . ?
O3A C15A C16A 120.7(4) . . ?
O3A C15A C14A 121.6(4) . . ?
C16A C15A C14A 117.6(4) . . ?
C17A C16A C15A 120.7(4) . . ?
C17A C16A C20A 119.4(4) . . ?
C15A C16A C20A 119.9(4) . . ?
C18A C17A C16A 120.1(4) . . ?
C17A C18A C19A 120.8(4) . . ?
C17A C18A Br2A 120.6(3) . . ?
C19A C18A Br2A 118.5(3) . . ?
C14A C19A C18A 120.7(4) . . ?
O4A C20A C16A 124.4(4) . . ?
C10A N1A C8A 110.2(3) . . ?
C10A N1A C9A 110.3(3) . . ?
C8A N1A C9A 108.3(3) . . ?
C10A N1A Ni1 103.7(2) . . ?
C8A N1A Ni1 109.1(2) . . ?
C9A N1A Ni1 115.1(2) . . ?
C12A N2A C13A 106.6(3) . . ?
C12A N2A C11A 109.4(3) . . ?
C13A N2A C11A 112.8(3) . . ?
C12A N2A Ni1 113.2(3) . . ?
C13A N2A Ni1 110.3(2) . . ?
C11A N2A Ni1 104.6(2) . . ?
C1A O1A Ni2 125.2(3) . . ?
C3A O2A Ni2 129.3(2) . . ?
C3A O2A Ni1 129.6(2) . . ?
Ni2 O2A Ni1 100.95(11) . . ?
C15A O3A Ni1 128.9(2) . . ?
O1B C1B C2B 128.7(4) . . ?
C3B C2B C7B 120.4(4) . . ?
C3B C2B C1B 124.5(4) . . ?
C7B C2B C1B 115.0(4) . . ?
O2B C3B C2B 122.4(4) . . ?
O2B C3B C4B 119.7(4) . . ?
C2B C3B C4B 117.9(4) . . ?
C5B C4B C3B 119.2(4) . . ?
C5B C4B C8B 118.9(4) . . ?
C3B C4B C8B 121.7(4) . . ?
C4B C5B C6B 122.0(4) . . ?
C7B C6B C5B 119.7(4) . . ?
C7B C6B Br1B 121.3(3) . . ?
C5B C6B Br1B 119.0(3) . . ?
C6B C7B C2B 120.6(4) . . ?
N1B C8B C4B 113.8(3) . . ?
N1B C10B C11B 109.9(3) . . ?
N2B C11B C10B 111.0(3) . . ?
N2B C13B C14B 115.4(3) . . ?
C19B C14B C15B 120.1(4) . . ?
C19B C14B C13B 118.7(4) . . ?
C15B C14B C13B 121.1(4) . . ?
O3B C15B C14B 121.4(3) . . ?
O3B C15B C16B 120.7(3) . . ?
C14B C15B C16B 117.9(4) . . ?
C17B C16B C15B 120.9(4) . . ?
C17B C16B C20B 119.5(4) . . ?
C15B C16B C20B 119.5(4) . . ?
C18B C17B C16B 119.6(4) . . ?
C17B C18B C19B 120.6(4) . . ?
C17B C18B Br2B 120.4(3) . . ?
C19B C18B Br2B 118.9(3) . . ?
C14B C19B C18B 120.7(4) . . ?
O4B C20B C16B 125.0(4) . . ?
C10B N1B C9B 110.5(3) . . ?
C10B N1B C8B 109.7(3) . . ?
C9B N1B C8B 108.1(3) . . ?
C10B N1B Ni3 104.5(2) . . ?
C9B N1B Ni3 114.8(2) . . ?
C8B N1B Ni3 109.2(2) . . ?
C12B N2B C11B 110.1(3) . . ?
C12B N2B C13B 106.7(3) . . ?
C11B N2B C13B 111.6(3) . . ?
C12B N2B Ni3 111.3(2) . . ?
C11B N2B Ni3 106.1(2) . . ?
C13B N2B Ni3 111.2(2) . . ?
C1B O1B Ni2 124.3(3) . . ?
C3B O2B Ni2 128.1(3) . . ?
C3B O2B Ni3 129.8(2) . . ?
Ni2 O2B Ni3 101.27(11) . . ?
C15B O3B Ni3 128.0(2) . . ?
N1P C1P C2P 179.9(6) . . ?
C1P N1P Ni1 165.0(3) . . ?
Ni2 O1P Ni1 94.20(10) . . ?
Ni3 O2P Ni2 94.95(10) . . ?
O1C N1C O3C 121.1(3) . . ?
O1C N1C O2C 120.3(3) . . ?
O3C N1C O2C 118.6(3) . . ?
O3D N1D O2D 121.1(3) . . ?
O3D N1D O1D 119.8(3) . . ?
O2D N1D O1D 119.1(4) . . ?
N1E C1E C2E 178.8(9) . . ?
N1F C1F C2F 179.5(6) . . ?
N1G C1G C2G 177.0(10) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.175
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.102

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 1.000 0.000 0.500 135 31 ' '
2 1.000 0.500 1.000 135 31 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_Compound5
_database_code_depnum_ccdc_archive 'CCDC 1043874'
_audit_update_record             
;
2015-01-23 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H72 Br4 N4 Ni4 O22'
_chemical_formula_weight         1611.58

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.7285(10)
_cell_length_b                   12.3966(13)
_cell_length_c                   12.6195(15)
_cell_angle_alpha                89.018(9)
_cell_angle_beta                 70.217(9)
_cell_angle_gamma                64.859(9)
_cell_volume                     1545.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4880
_cell_measurement_theta_min      3.7641
_cell_measurement_theta_max      74.0036

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.731
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816
_exptl_absorpt_coefficient_mu    5.046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10660
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.76
_diffrn_reflns_theta_max         74.24
_reflns_number_total             6058
_reflns_number_gt                4762
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger. The components of the anisotropic displacement parameters along the O1M - C1M chemical bond are restrained to be equal by the DELU order.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0732P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6058
_refine_ls_number_parameters     329
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1298
_refine_ls_wR_factor_gt          0.1239
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.096
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1A Br 0.09141(5) 0.88807(4) 0.09515(4) 0.04439(14) Uani 1 1 d . . .
Br2A Br 0.88534(5) 0.95177(5) 0.47421(5) 0.05002(15) Uani 1 1 d . . .
Ni1 Ni 0.46989(6) 0.63235(5) 0.68478(5) 0.02491(15) Uani 1 1 d . . .
Ni2 Ni 0.54934(7) 0.57514(6) 0.41520(6) 0.02746(16) Uani 1 1 d . . .
C1A C 0.4221(5) 0.7930(4) 0.3170(4) 0.0389(9) Uani 1 1 d . . .
H1A H 0.4133 0.8688 0.3000 0.047 Uiso 1 1 calc R . .
C2A C 0.3534(4) 0.7446(3) 0.2709(3) 0.0319(8) Uani 1 1 d . . .
C3A C 0.6357(4) 0.3735(3) 0.7182(3) 0.0279(7) Uani 1 1 d . . .
C4A C 0.7108(4) 0.4096(3) 0.7663(3) 0.0287(7) Uani 1 1 d . . .
C5A C 0.7907(4) 0.3307(4) 0.8194(3) 0.0342(8) Uani 1 1 d . . .
H5A H 0.8393 0.3550 0.8501 0.041 Uiso 1 1 calc R . .
C6A C 0.2003(4) 0.7838(4) 0.1722(3) 0.0320(8) Uani 1 1 d . . .
C7A C 0.2716(4) 0.8222(4) 0.2154(3) 0.0361(9) Uani 1 1 d . . .
H7A H 0.2660 0.8989 0.2081 0.043 Uiso 1 1 calc R . .
C8A C 0.7043(4) 0.5331(4) 0.7578(4) 0.0336(8) Uani 1 1 d . . .
H8A1 H 0.7542 0.5447 0.8005 0.040 Uiso 1 1 calc R . .
H8A2 H 0.7484 0.5378 0.6787 0.040 Uiso 1 1 calc R . .
C9A C 0.4904(4) 0.6210(4) 0.9179(3) 0.0339(8) Uani 1 1 d . . .
H9A1 H 0.5399 0.6193 0.9654 0.051 Uiso 1 1 calc R . .
H9A2 H 0.4808 0.5478 0.9173 0.051 Uiso 1 1 calc R . .
H9A3 H 0.4024 0.6886 0.9471 0.051 Uiso 1 1 calc R . .
C10A C 0.5719(5) 0.7481(4) 0.8015(4) 0.0350(9) Uani 1 1 d . . .
H10A H 0.6441 0.7448 0.7332 0.042 Uiso 1 1 calc R . .
H10B H 0.5919 0.7628 0.8669 0.042 Uiso 1 1 calc R . .
C11A C 0.4394(5) 0.8487(4) 0.8065(4) 0.0365(9) Uani 1 1 d . . .
H11A H 0.3704 0.8602 0.8804 0.044 Uiso 1 1 calc R . .
H11B H 0.4485 0.9229 0.7977 0.044 Uiso 1 1 calc R . .
C12A C 0.2461(4) 0.8867(4) 0.7552(5) 0.0444(11) Uani 1 1 d . . .
H12A H 0.2161 0.9704 0.7797 0.067 Uiso 1 1 calc R . .
H12B H 0.2076 0.8521 0.8176 0.067 Uiso 1 1 calc R . .
H12C H 0.2179 0.8792 0.6938 0.067 Uiso 1 1 calc R . .
C13A C 0.4495(4) 0.8693(3) 0.6110(3) 0.0310(8) Uani 1 1 d . . .
H13A H 0.4132 0.9559 0.6293 0.037 Uiso 1 1 calc R . .
H13B H 0.4152 0.8546 0.5556 0.037 Uiso 1 1 calc R . .
C14A C 0.6005(4) 0.8174(3) 0.5566(3) 0.0277(7) Uani 1 1 d . . .
C15A C 0.6801(4) 0.6923(3) 0.5131(3) 0.0258(7) Uani 1 1 d . . .
C16A C 0.8198(4) 0.6485(4) 0.4552(4) 0.0375(9) Uani 1 1 d . . .
C17A C 0.8806(4) 0.7264(4) 0.4426(4) 0.0431(10) Uani 1 1 d . . .
H17A H 0.9735 0.6969 0.4040 0.052 Uiso 1 1 calc R . .
C18A C 0.8027(4) 0.8464(4) 0.4875(4) 0.0362(9) Uani 1 1 d . . .
C19A C 0.6633(4) 0.8924(4) 0.5437(3) 0.0313(8) Uani 1 1 d . . .
H19A H 0.6119 0.9739 0.5728 0.038 Uiso 1 1 calc R . .
C20A C 0.9021(5) 0.5213(4) 0.4050(5) 0.0527(13) Uani 1 1 d . . .
H20A H 0.8611 0.4701 0.4230 0.063 Uiso 1 1 calc R . .
N1A N 0.5641(3) 0.6318(3) 0.8011(3) 0.0283(6) Uani 1 1 d . . .
N2A N 0.3967(3) 0.8223(3) 0.7156(3) 0.0301(7) Uani 1 1 d . . .
O1A O 0.4901(3) 0.7480(3) 0.3751(3) 0.0380(7) Uani 1 1 d . . .
O2A O 0.5622(3) 0.4464(2) 0.6670(2) 0.0297(5) Uani 1 1 d . . .
O3A O 0.6226(3) 0.6189(2) 0.5297(2) 0.0264(5) Uani 1 1 d . . .
O4A O 1.0167(5) 0.4790(5) 0.3434(7) 0.114(3) Uani 1 1 d . . .
C1B C 0.1255(6) 0.5827(6) 0.9149(5) 0.0679(18) Uani 1 1 d . . .
H1B1 H 0.1483 0.5187 0.9593 0.102 Uiso 1 1 calc R . .
H1B2 H 0.0545 0.5852 0.8918 0.102 Uiso 1 1 calc R . .
H1B3 H 0.0954 0.6581 0.9599 0.102 Uiso 1 1 calc R . .
C2B C 0.2480(5) 0.5611(4) 0.8111(4) 0.0393(9) Uani 1 1 d . . .
O1B O 0.3029(3) 0.6295(3) 0.8086(2) 0.0354(6) Uani 1 1 d . . .
O2B O 0.7127(3) 0.5252(3) 0.2666(2) 0.0372(6) Uani 1 1 d . . .
C1M C 0.2590(6) 0.6827(6) 0.5722(6) 0.0661(16) Uani 1 1 d U . .
H1M1 H 0.2558 0.7557 0.5434 0.099 Uiso 1 1 calc R . .
H1M2 H 0.1978 0.7017 0.6500 0.099 Uiso 1 1 calc R . .
H1M3 H 0.2329 0.6423 0.5273 0.099 Uiso 1 1 calc R . .
O1M O 0.3978(3) 0.6035(2) 0.5657(2) 0.0288(5) Uani 1 1 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
Br1A C6A 1.909(4) . ?
Br2A C18A 1.906(4) . ?
Ni1 O1M 2.058(3) . ?
Ni1 O1B 2.065(3) . ?
Ni1 O2A 2.066(3) . ?
Ni1 O3A 2.109(3) . ?
Ni1 N1A 2.114(3) . ?
Ni1 N2A 2.126(3) . ?
Ni2 O2A 2.021(3) 2_666 ?
Ni2 O1M 2.024(3) . ?
Ni2 O2B 2.043(3) . ?
Ni2 O1A 2.065(3) . ?
Ni2 O1M 2.065(3) 2_666 ?
Ni2 O3A 2.094(3) . ?
C1A O1A 1.220(6) . ?
C1A C2A 1.444(6) . ?
C2A C7A 1.409(6) . ?
C2A C3A 1.423(5) 2_666 ?
C3A O2A 1.293(5) . ?
C3A C2A 1.423(5) 2_666 ?
C3A C4A 1.432(5) . ?
C4A C5A 1.382(6) . ?
C4A C8A 1.504(5) . ?
C5A C6A 1.382(6) 2_666 ?
C6A C7A 1.371(6) . ?
C6A C5A 1.382(6) 2_666 ?
C8A N1A 1.485(5) . ?
C9A N1A 1.473(5) . ?
C10A N1A 1.483(5) . ?
C10A C11A 1.504(6) . ?
C11A N2A 1.488(5) . ?
C12A N2A 1.491(5) . ?
C13A N2A 1.481(5) . ?
C13A C14A 1.498(5) . ?
C14A C19A 1.389(5) . ?
C14A C15A 1.424(5) . ?
C15A O3A 1.322(4) . ?
C15A C16A 1.400(5) . ?
C16A C17A 1.404(6) . ?
C16A C20A 1.465(6) . ?
C17A C18A 1.376(6) . ?
C18A C19A 1.392(6) . ?
C20A O4A 1.180(6) . ?
O2A Ni2 2.021(3) 2_666 ?
C1B C2B 1.505(6) . ?
C2B O1B 1.259(5) . ?
C2B O2B 1.277(5) 2_666 ?
O2B C2B 1.277(5) 2_666 ?
C1M O1M 1.475(6) . ?
O1M Ni2 2.065(3) 2_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1M Ni1 O1B 87.69(11) . . ?
O1M Ni1 O2A 83.47(11) . . ?
O1B Ni1 O2A 87.72(12) . . ?
O1M Ni1 O3A 77.53(10) . . ?
O1B Ni1 O3A 164.97(11) . . ?
O2A Ni1 O3A 87.91(11) . . ?
O1M Ni1 N1A 170.80(12) . . ?
O1B Ni1 N1A 93.57(12) . . ?
O2A Ni1 N1A 87.46(12) . . ?
O3A Ni1 N1A 100.60(11) . . ?
O1M Ni1 N2A 105.29(12) . . ?
O1B Ni1 N2A 95.07(12) . . ?
O2A Ni1 N2A 170.87(12) . . ?
O3A Ni1 N2A 91.48(11) . . ?
N1A Ni1 N2A 83.69(13) . . ?
O2A Ni2 O1M 89.48(11) 2_666 . ?
O2A Ni2 O2B 91.30(12) 2_666 . ?
O1M Ni2 O2B 173.02(12) . . ?
O2A Ni2 O1A 87.50(11) 2_666 . ?
O1M Ni2 O1A 100.60(12) . . ?
O2B Ni2 O1A 86.36(13) . . ?
O2A Ni2 O1M 84.44(11) 2_666 2_666 ?
O1M Ni2 O1M 82.80(12) . 2_666 ?
O2B Ni2 O1M 90.38(12) . 2_666 ?
O1A Ni2 O1M 171.24(11) . 2_666 ?
O2A Ni2 O3A 167.10(11) 2_666 . ?
O1M Ni2 O3A 78.63(10) . . ?
O2B Ni2 O3A 101.12(11) . . ?
O1A Ni2 O3A 89.79(11) . . ?
O1M Ni2 O3A 98.83(10) 2_666 . ?
O1A C1A C2A 128.8(4) . . ?
C7A C2A C3A 121.0(4) . 2_666 ?
C7A C2A C1A 116.1(4) . . ?
C3A C2A C1A 122.9(4) 2_666 . ?
O2A C3A C2A 122.4(3) . 2_666 ?
O2A C3A C4A 120.4(3) . . ?
C2A C3A C4A 117.2(3) 2_666 . ?
C5A C4A C3A 120.2(4) . . ?
C5A C4A C8A 119.8(4) . . ?
C3A C4A C8A 120.0(3) . . ?
C4A C5A C6A 121.1(4) . 2_666 ?
C7A C6A C5A 121.0(4) . 2_666 ?
C7A C6A Br1A 119.5(3) . . ?
C5A C6A Br1A 119.5(3) 2_666 . ?
C6A C7A C2A 119.5(4) . . ?
N1A C8A C4A 113.5(3) . . ?
N1A C10A C11A 109.8(3) . . ?
N2A C11A C10A 111.4(3) . . ?
N2A C13A C14A 115.9(3) . . ?
C19A C14A C15A 119.4(3) . . ?
C19A C14A C13A 119.9(3) . . ?
C15A C14A C13A 120.6(3) . . ?
O3A C15A C16A 120.8(3) . . ?
O3A C15A C14A 120.1(3) . . ?
C16A C15A C14A 119.1(3) . . ?
C15A C16A C17A 120.3(4) . . ?
C15A C16A C20A 119.7(4) . . ?
C17A C16A C20A 119.9(4) . . ?
C18A C17A C16A 119.8(4) . . ?
C17A C18A C19A 120.8(4) . . ?
C17A C18A Br2A 120.1(3) . . ?
C19A C18A Br2A 119.1(3) . . ?
C14A C19A C18A 120.5(4) . . ?
O4A C20A C16A 124.7(5) . . ?
C9A N1A C10A 109.2(3) . . ?
C9A N1A C8A 110.2(3) . . ?
C10A N1A C8A 108.2(3) . . ?
C9A N1A Ni1 114.0(2) . . ?
C10A N1A Ni1 105.9(2) . . ?
C8A N1A Ni1 109.0(2) . . ?
C13A N2A C11A 110.8(3) . . ?
C13A N2A C12A 106.6(3) . . ?
C11A N2A C12A 108.6(3) . . ?
C13A N2A Ni1 111.4(2) . . ?
C11A N2A Ni1 107.5(2) . . ?
C12A N2A Ni1 111.9(2) . . ?
C1A O1A Ni2 126.7(3) . . ?
C3A O2A Ni2 131.4(2) . 2_666 ?
C3A O2A Ni1 131.2(2) . . ?
Ni2 O2A Ni1 94.82(11) 2_666 . ?
C15A O3A Ni2 124.0(2) . . ?
C15A O3A Ni1 122.7(2) . . ?
Ni2 O3A Ni1 99.68(10) . . ?
O1B C2B O2B 125.8(4) . 2_666 ?
O1B C2B C1B 117.1(4) . . ?
O2B C2B C1B 117.1(4) 2_666 . ?
C2B O1B Ni1 130.0(3) . . ?
C2B O2B Ni2 125.3(3) 2_666 . ?
C1M O1M Ni2 116.8(3) . . ?
C1M O1M Ni1 121.3(3) . . ?
Ni2 O1M Ni1 103.78(12) . . ?
C1M O1M Ni2 119.3(3) . 2_666 ?
Ni2 O1M Ni2 97.20(12) . 2_666 ?
Ni1 O1M Ni2 93.74(11) . 2_666 ?

_diffrn_measured_fraction_theta_max 0.962
_diffrn_reflns_theta_full        74.24
_diffrn_measured_fraction_theta_full 0.962
_refine_diff_density_max         1.744
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.100

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.000 389 91 ' '
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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_Compound6
_database_code_depnum_ccdc_archive 'CCDC 1043875'
_audit_update_record             
;
2015-01-23 deposited with the CCDC.
2015-03-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H54 Br4 N10 Ni4 O15'
_chemical_formula_weight         1529.46

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.3880(4)
_cell_length_b                   14.4846(5)
_cell_length_c                   14.9568(5)
_cell_angle_alpha                106.726(3)
_cell_angle_beta                 95.185(3)
_cell_angle_gamma                93.111(3)
_cell_volume                     2756.53(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5166
_cell_measurement_theta_min      1.4703
_cell_measurement_theta_max      28.2561

_exptl_crystal_description       Prismatic
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532
_exptl_absorpt_coefficient_mu    4.318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.62950
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'CrysAlisPro, Agilent Technologies'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17673
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         25.00
_reflns_number_total             9673
_reflns_number_gt                7112
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger. The components of the anisotropic displacement parameters along the O1M - C1M chemical bond are restrained to be equal by the DELU order.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0635P)²+1.7423P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9673
_refine_ls_number_parameters     694
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0496
_refine_ls_wR_factor_ref         0.1302
_refine_ls_wR_factor_gt          0.1192
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.52048(5) 0.34507(5) 0.34965(5) 0.01984(18) Uani 1 1 d . . .
Ni2 Ni 0.38335(5) 0.47610(5) 0.46852(5) 0.01905(17) Uani 1 1 d . . .
Ni3 Ni 1.01393(5) 0.15102(5) -0.07309(5) 0.02429(19) Uani 1 1 d . . .
Ni4 Ni 1.09610(5) 0.05455(5) 0.06966(5) 0.02288(18) Uani 1 1 d . . .
Br1A Br 0.23997(5) 0.00217(5) 0.55415(5) 0.03810(18) Uani 1 1 d . . .
Br2A Br 1.00021(4) 0.15863(5) 0.43573(5) 0.03806(18) Uani 1 1 d . . .
Br1D Br 1.00797(5) 0.54716(5) 0.37592(5) 0.0451(2) Uani 1 1 d . . .
Br2D Br 0.52358(5) 0.14326(6) -0.33885(6) 0.0490(2) Uani 1 1 d . . .
C1A C 0.2380(4) 0.3596(4) 0.5376(4) 0.0259(13) Uani 1 1 d . . .
H1A H 0.1820 0.3566 0.5694 0.031 Uiso 1 1 calc R . .
C2A C 0.2883(4) 0.2732(4) 0.5124(4) 0.0229(13) Uani 1 1 d . . .
C3A C 0.3748(4) 0.2636(4) 0.4620(4) 0.0201(12) Uani 1 1 d . . .
C4A C 0.4169(4) 0.1727(4) 0.4389(4) 0.0223(13) Uani 1 1 d . . .
C5A C 0.3741(4) 0.0974(4) 0.4655(4) 0.0277(14) Uani 1 1 d . . .
H5A H 0.4008 0.0377 0.4487 0.033 Uiso 1 1 calc R . .
C6A C 0.2914(4) 0.1092(4) 0.5173(4) 0.0250(13) Uani 1 1 d . . .
C7A C 0.2501(4) 0.1941(5) 0.5413(4) 0.0275(14) Uani 1 1 d . . .
H7A H 0.1961 0.2012 0.5770 0.033 Uiso 1 1 calc R . .
C8A C 0.5114(4) 0.1573(4) 0.3905(4) 0.0277(14) Uani 1 1 d . . .
H8A1 H 0.5686 0.1902 0.4348 0.033 Uiso 1 1 calc R . .
H8A2 H 0.5209 0.0887 0.3714 0.033 Uiso 1 1 calc R . .
C9A C 0.4185(4) 0.1506(5) 0.2397(4) 0.0354(16) Uani 1 1 d . . .
H9A1 H 0.4227 0.1671 0.1824 0.053 Uiso 1 1 calc R . .
H9A2 H 0.3598 0.1754 0.2674 0.053 Uiso 1 1 calc R . .
H9A3 H 0.4140 0.0815 0.2266 0.053 Uiso 1 1 calc R . .
C10A C 0.6002(5) 0.1637(4) 0.2580(5) 0.0333(15) Uani 1 1 d . . .
H10A H 0.5877 0.0979 0.2170 0.040 Uiso 1 1 calc R . .
H10B H 0.6564 0.1659 0.3045 0.040 Uiso 1 1 calc R . .
C11A C 0.6251(4) 0.2314(4) 0.2014(4) 0.0312(15) Uani 1 1 d . . .
H11A H 0.6891 0.2171 0.1771 0.037 Uiso 1 1 calc R . .
H11B H 0.5741 0.2200 0.1483 0.037 Uiso 1 1 calc R . .
C12A C 0.6144(5) 0.3912(5) 0.1889(4) 0.0383(17) Uani 1 1 d . . .
H12A H 0.6659 0.3811 0.1473 0.057 Uiso 1 1 calc R . .
H12B H 0.6168 0.4587 0.2229 0.057 Uiso 1 1 calc R . .
H12C H 0.5497 0.3709 0.1531 0.057 Uiso 1 1 calc R . .
C13A C 0.7339(4) 0.3665(4) 0.3079(4) 0.0240(13) Uani 1 1 d . . .
H13A H 0.7371 0.4360 0.3366 0.029 Uiso 1 1 calc R . .
H13B H 0.7823 0.3544 0.2622 0.029 Uiso 1 1 calc R . .
C14A C 0.7664(4) 0.3208(4) 0.3828(4) 0.0250(13) Uani 1 1 d . . .
C15A C 0.7147(4) 0.3351(4) 0.4640(4) 0.0208(12) Uani 1 1 d . . .
C16A C 0.7538(4) 0.3008(4) 0.5386(4) 0.0253(13) Uani 1 1 d . . .
C17A C 0.8403(4) 0.2490(4) 0.5289(4) 0.0287(14) Uani 1 1 d . . .
H17A H 0.8667 0.2271 0.5781 0.034 Uiso 1 1 calc R . .
C18A C 0.8853(4) 0.2308(4) 0.4487(4) 0.0274(14) Uani 1 1 d . . .
C19A C 0.8506(4) 0.2689(4) 0.3755(4) 0.0255(13) Uani 1 1 d . . .
H19A H 0.8845 0.2590 0.3224 0.031 Uiso 1 1 calc R . .
C20A C 0.7108(5) 0.3241(5) 0.6267(5) 0.0332(15) Uani 1 1 d . . .
H20A H 0.6485 0.3497 0.6283 0.040 Uiso 1 1 calc R . .
N1A N 0.5092(3) 0.1933(3) 0.3056(3) 0.0223(11) Uani 1 1 d . . .
N2A N 0.6311(4) 0.3338(4) 0.2566(3) 0.0255(11) Uani 1 1 d . . .
O1A O 0.2583(3) 0.4377(3) 0.5232(3) 0.0265(9) Uani 1 1 d . . .
O2A O 0.4141(3) 0.3363(3) 0.4370(3) 0.0209(8) Uani 1 1 d . . .
O3A O 0.6294(3) 0.3781(3) 0.4680(3) 0.0222(9) Uani 1 1 d . . .
O4A O 0.7504(3) 0.3127(4) 0.6996(3) 0.0440(12) Uani 1 1 d . . .
C1B C 0.2698(5) 0.4097(5) 0.1762(4) 0.0367(16) Uani 1 1 d . . .
H1B1 H 0.3084 0.4434 0.1424 0.055 Uiso 1 1 calc R . .
H1B2 H 0.2109 0.4427 0.1930 0.055 Uiso 1 1 calc R . .
H1B3 H 0.2500 0.3449 0.1372 0.055 Uiso 1 1 calc R . .
C2B C 0.3324(4) 0.4067(4) 0.2635(4) 0.0243(13) Uani 1 1 d . . .
O1B O 0.4063(3) 0.3556(3) 0.2522(3) 0.0269(9) Uani 1 1 d . . .
O2B O 0.3066(3) 0.4562(3) 0.3418(3) 0.0235(9) Uani 1 1 d . . .
N1C N 0.5185(3) 0.4960(3) 0.4090(3) 0.0181(9) Uani 1 1 d U . .
N2C N 0.5218(4) 0.5534(4) 0.3606(4) 0.0305(12) Uani 1 1 d U . .
N3C N 0.5259(5) 0.6051(5) 0.3158(4) 0.0523(16) Uani 1 1 d . . .
C1D C 1.1340(4) 0.2003(4) 0.2550(4) 0.0244(13) Uani 1 1 d . . .
H1D H 1.1696 0.2209 0.3146 0.029 Uiso 1 1 calc R . .
C2D C 1.0741(4) 0.2692(4) 0.2301(4) 0.0233(13) Uani 1 1 d . . .
C3D C 1.0223(4) 0.2534(4) 0.1376(4) 0.0244(13) Uani 1 1 d . . .
C4D C 0.9646(4) 0.3291(4) 0.1213(4) 0.0257(13) Uani 1 1 d . . .
C5D C 0.9612(4) 0.4134(4) 0.1925(5) 0.0322(15) Uani 1 1 d . . .
H5D H 0.9237 0.4618 0.1810 0.039 Uiso 1 1 calc R . .
C6D C 1.0127(4) 0.4281(4) 0.2818(4) 0.0297(14) Uani 1 1 d . . .
C7D C 1.0699(4) 0.3584(4) 0.3009(4) 0.0303(14) Uani 1 1 d . . .
H7D H 1.1057 0.3697 0.3598 0.036 Uiso 1 1 calc R . .
C8D C 0.9084(4) 0.3157(5) 0.0271(4) 0.0332(15) Uani 1 1 d . . .
H8D1 H 0.8757 0.3739 0.0276 0.040 Uiso 1 1 calc R . .
H8D2 H 0.8564 0.2629 0.0147 0.040 Uiso 1 1 calc R . .
C9D C 1.0637(4) 0.3676(4) -0.0258(5) 0.0334(15) Uani 1 1 d . . .
H9D1 H 1.1032 0.3573 -0.0777 0.050 Uiso 1 1 calc R . .
H9D2 H 1.1043 0.3616 0.0283 0.050 Uiso 1 1 calc R . .
H9D3 H 1.0406 0.4313 -0.0120 0.050 Uiso 1 1 calc R . .
C10D C 0.9173(5) 0.2975(5) -0.1386(4) 0.0354(16) Uani 1 1 d . . .
H10C H 0.9137 0.3640 -0.1392 0.043 Uiso 1 1 calc R . .
H10D H 0.8492 0.2685 -0.1432 0.043 Uiso 1 1 calc R . .
C11D C 0.9701(5) 0.2418(5) -0.2208(4) 0.0365(16) Uani 1 1 d . . .
H11C H 0.9284 0.2364 -0.2789 0.044 Uiso 1 1 calc R . .
H11D H 1.0330 0.2780 -0.2215 0.044 Uiso 1 1 calc R . .
C12D C 1.0788(5) 0.1125(5) -0.2679(4) 0.0365(16) Uani 1 1 d . . .
H12D H 1.0668 0.1173 -0.3307 0.055 Uiso 1 1 calc R . .
H12E H 1.0889 0.0468 -0.2704 0.055 Uiso 1 1 calc R . .
H12F H 1.1377 0.1536 -0.2359 0.055 Uiso 1 1 calc R . .
C13D C 0.9041(5) 0.0715(5) -0.2666(4) 0.0332(15) Uani 1 1 d . . .
H13C H 0.8972 0.0692 -0.3323 0.040 Uiso 1 1 calc R . .
H13D H 0.9205 0.0081 -0.2634 0.040 Uiso 1 1 calc R . .
C14D C 0.8042(4) 0.0904(4) -0.2302(4) 0.0284(14) Uani 1 1 d . . .
C15D C 0.7905(4) 0.0884(4) -0.1384(4) 0.0248(13) Uani 1 1 d . . .
C16D C 0.6931(4) 0.0978(4) -0.1101(4) 0.0289(14) Uani 1 1 d . . .
C17D C 0.6137(4) 0.1127(5) -0.1705(5) 0.0339(16) Uani 1 1 d . . .
H17D H 0.5495 0.1179 -0.1515 0.041 Uiso 1 1 calc R . .
C18D C 0.6297(5) 0.1199(5) -0.2576(5) 0.0360(16) Uani 1 1 d . . .
C19D C 0.7250(5) 0.1068(5) -0.2883(5) 0.0344(15) Uani 1 1 d . . .
H19D H 0.7353 0.1091 -0.3483 0.041 Uiso 1 1 calc R . .
C20D C 0.6716(5) 0.0885(5) -0.0187(5) 0.0387(17) Uani 1 1 d . . .
H20D H 0.7254 0.0846 0.0236 0.046 Uiso 1 1 calc R . .
N1D N 0.9756(4) 0.2942(4) -0.0503(3) 0.0288(12) Uani 1 1 d . . .
N2D N 0.9913(4) 0.1431(4) -0.2170(3) 0.0283(12) Uani 1 1 d . . .
O1D O 1.1452(3) 0.1173(3) 0.2086(3) 0.0280(10) Uani 1 1 d . . .
O2D O 1.0270(3) 0.1750(3) 0.0706(3) 0.0244(9) Uani 1 1 d . . .
O3D O 0.8686(3) 0.0800(3) -0.0794(3) 0.0257(9) Uani 1 1 d . . .
O4D O 0.5860(3) 0.0856(4) 0.0052(3) 0.0532(14) Uani 1 1 d . . .
C1E C 1.3450(5) 0.1787(6) -0.0309(6) 0.053(2) Uani 1 1 d . . .
H1E1 H 1.3728 0.2354 0.0182 0.080 Uiso 1 1 calc R . .
H1E2 H 1.3456 0.1909 -0.0906 0.080 Uiso 1 1 calc R . .
H1E3 H 1.3846 0.1257 -0.0297 0.080 Uiso 1 1 calc R . .
C2E C 1.2384(4) 0.1538(4) -0.0159(4) 0.0283(14) Uani 1 1 d . . .
O1E O 1.1673(3) 0.1842(3) -0.0614(3) 0.0322(10) Uani 1 1 d . . .
O2E O 1.2267(3) 0.1048(3) 0.0395(3) 0.0295(10) Uani 1 1 d . . .
N1F N 1.0449(3) 0.0082(3) -0.0785(3) 0.0215(10) Uani 1 1 d . . .
N2F N 1.1028(4) -0.0397(4) -0.1304(4) 0.0317(12) Uani 1 1 d . . .
N3F N 1.1557(4) -0.0843(5) -0.1780(4) 0.0495(16) Uani 1 1 d . . .
C1M C 1.4200(8) 0.6281(8) 0.1064(8) 0.095(4) Uani 1 1 d . . .
H1M1 H 1.4430 0.6913 0.1044 0.143 Uiso 1 1 calc R . .
H1M2 H 1.4323 0.5807 0.0497 0.143 Uiso 1 1 calc R . .
H1M3 H 1.4556 0.6147 0.1594 0.143 Uiso 1 1 calc R . .
O1M O 1.3205(6) 0.6247(7) 0.1148(6) 0.118(3) Uani 1 1 d . . .
H1M H 1.3118 0.6349 0.1702 0.177 Uiso 1 1 calc R . .


_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 O2A 2.040(4) . ?
Ni1 O1B 2.057(4) . ?
Ni1 N1A 2.098(5) . ?
Ni1 N2A 2.104(5) . ?
Ni1 N1C 2.113(5) . ?
Ni1 O3A 2.112(4) . ?
Ni2 O2B 2.008(4) . ?
Ni2 O2A 2.017(4) . ?
Ni2 O1A 2.047(4) . ?
Ni2 O3A 2.075(4) 2_666 ?
Ni2 N1C 2.081(4) 2_666 ?
Ni2 N1C 2.129(4) . ?
Ni3 O2D 2.065(4) . ?
Ni3 O1E 2.063(4) . ?
Ni3 N1D 2.103(5) . ?
Ni3 N1F 2.111(5) . ?
Ni3 N2D 2.115(5) . ?
Ni3 O3D 2.133(4) . ?
Ni4 O2E 1.995(4) . ?
Ni4 O2D 2.016(4) . ?
Ni4 O1D 2.044(4) . ?
Ni4 O3D 2.072(4) 2_755 ?
Ni4 N1F 2.082(5) 2_755 ?
Ni4 N1F 2.156(5) . ?
Br1A C6A 1.904(6) . ?
Br2A C18A 1.900(5) . ?
Br1D C6D 1.894(6) . ?
Br2D C18D 1.894(6) . ?
C1A O1A 1.232(7) . ?
C1A C2A 1.423(8) . ?
C2A C7A 1.423(8) . ?
C2A C3A 1.429(7) . ?
C3A O2A 1.314(6) . ?
C3A C4A 1.422(8) . ?
C4A C5A 1.377(8) . ?
C4A C8A 1.511(7) . ?
C5A C6A 1.398(8) . ?
C6A C7A 1.342(8) . ?
C8A N1A 1.504(7) . ?
C9A N1A 1.477(7) . ?
C10A N1A 1.487(7) . ?
C10A C11A 1.512(9) . ?
C11A N2A 1.469(7) . ?
C12A N2A 1.494(7) . ?
C13A N2A 1.496(7) . ?
C13A C14A 1.501(8) . ?
C14A C19A 1.385(8) . ?
C14A C15A 1.421(8) . ?
C15A O3A 1.328(6) . ?
C15A C16A 1.416(8) . ?
C16A C17A 1.410(8) . ?
C16A C20A 1.444(8) . ?
C17A C18A 1.356(8) . ?
C18A C19A 1.414(8) . ?
C20A O4A 1.228(7) . ?
O3A Ni2 2.075(4) 2_666 ?
C1B C2B 1.500(8) . ?
C2B O1B 1.262(7) . ?
C2B O2B 1.274(7) . ?
N1C N2C 1.251(7) . ?
N1C Ni2 2.081(4) 2_666 ?
N2C N3C 1.142(7) . ?
C1D O1D 1.228(7) . ?
C1D C2D 1.423(8) . ?
C2D C7D 1.423(8) . ?
C2D C3D 1.440(8) . ?
C3D O2D 1.290(7) . ?
C3D C4D 1.438(8) . ?
C4D C5D 1.377(8) . ?
C4D C8D 1.491(8) . ?
C5D C6D 1.399(9) . ?
C6D C7D 1.378(8) . ?
C8D N1D 1.504(8) . ?
C9D N1D 1.489(7) . ?
C10D N1D 1.487(8) . ?
C10D C11D 1.520(9) . ?
C11D N2D 1.489(8) . ?
C12D N2D 1.474(7) . ?
C13D C14D 1.498(8) . ?
C13D N2D 1.502(8) . ?
C14D C19D 1.384(8) . ?
C14D C15D 1.409(8) . ?
C15D O3D 1.340(7) . ?
C15D C16D 1.409(8) . ?
C16D C17D 1.399(8) . ?
C16D C20D 1.463(9) . ?
C17D C18D 1.371(9) . ?
C18D C19D 1.398(9) . ?
C20D O4D 1.233(7) . ?
O3D Ni4 2.072(4) 2_755 ?
C1E C2E 1.505(8) . ?
C2E O2E 1.251(7) . ?
C2E O1E 1.290(7) . ?
N1F N2F 1.243(6) . ?
N1F Ni4 2.082(5) 2_755 ?
N2F N3F 1.140(7) . ?
C1M O1M 1.349(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2A Ni1 O1B 88.12(15) . . ?
O2A Ni1 N1A 87.34(16) . . ?
O1B Ni1 N1A 94.38(17) . . ?
O2A Ni1 N2A 172.19(17) . . ?
O1B Ni1 N2A 93.85(17) . . ?
N1A Ni1 N2A 84.97(18) . . ?
O2A Ni1 N1C 84.47(15) . . ?
O1B Ni1 N1C 86.56(16) . . ?
N1A Ni1 N1C 171.73(17) . . ?
N2A Ni1 N1C 103.18(18) . . ?
O2A Ni1 O3A 87.83(14) . . ?
O1B Ni1 O3A 162.70(16) . . ?
N1A Ni1 O3A 102.22(16) . . ?
N2A Ni1 O3A 92.43(16) . . ?
N1C Ni1 O3A 76.32(16) . . ?
O2B Ni2 O2A 92.39(15) . . ?
O2B Ni2 O1A 92.39(15) . . ?
O2A Ni2 O1A 87.53(15) . . ?
O2B Ni2 O3A 101.46(15) . 2_666 ?
O2A Ni2 O3A 166.14(15) . 2_666 ?
O1A Ni2 O3A 91.55(15) . 2_666 ?
O2B Ni2 N1C 171.23(16) . 2_666 ?
O2A Ni2 N1C 88.56(16) . 2_666 ?
O1A Ni2 N1C 96.36(16) . 2_666 ?
O3A Ni2 N1C 77.80(16) 2_666 2_666 ?
O2B Ni2 N1C 88.65(16) . . ?
O2A Ni2 N1C 84.62(16) . . ?
O1A Ni2 N1C 172.11(17) . . ?
O3A Ni2 N1C 95.91(16) 2_666 . ?
N1C Ni2 N1C 82.75(17) 2_666 . ?
O2D Ni3 O1E 88.06(15) . . ?
O2D Ni3 N1D 88.30(17) . . ?
O1E Ni3 N1D 95.58(18) . . ?
O2D Ni3 N1F 84.73(16) . . ?
O1E Ni3 N1F 87.54(17) . . ?
N1D Ni3 N1F 172.27(18) . . ?
O2D Ni3 N2D 172.66(17) . . ?
O1E Ni3 N2D 94.29(17) . . ?
N1D Ni3 N2D 84.56(19) . . ?
N1F Ni3 N2D 102.30(18) . . ?
O2D Ni3 O3D 87.81(15) . . ?
O1E Ni3 O3D 163.92(16) . . ?
N1D Ni3 O3D 99.83(17) . . ?
N1F Ni3 O3D 76.61(16) . . ?
N2D Ni3 O3D 91.75(17) . . ?
O2E Ni4 O2D 94.26(16) . . ?
O2E Ni4 O1D 87.99(16) . . ?
O2D Ni4 O1D 88.38(16) . . ?
O2E Ni4 O3D 100.85(16) . 2_755 ?
O2D Ni4 O3D 164.85(15) . 2_755 ?
O1D Ni4 O3D 91.09(16) . 2_755 ?
O2E Ni4 N1F 170.98(17) . 2_755 ?
O2D Ni4 N1F 86.67(16) . 2_755 ?
O1D Ni4 N1F 101.01(17) . 2_755 ?
O3D Ni4 N1F 78.57(16) 2_755 2_755 ?
O2E Ni4 N1F 88.62(17) . . ?
O2D Ni4 N1F 84.79(16) . . ?
O1D Ni4 N1F 172.13(18) . . ?
O3D Ni4 N1F 96.52(16) 2_755 . ?
N1F Ni4 N1F 82.52(19) 2_755 . ?
O1A C1A C2A 129.2(5) . . ?
C7A C2A C1A 117.1(5) . . ?
C7A C2A C3A 119.5(5) . . ?
C1A C2A C3A 123.4(5) . . ?
O2A C3A C4A 120.8(5) . . ?
O2A C3A C2A 121.1(5) . . ?
C4A C3A C2A 118.1(5) . . ?
C5A C4A C3A 119.7(5) . . ?
C5A C4A C8A 118.3(5) . . ?
C3A C4A C8A 121.9(5) . . ?
C4A C5A C6A 121.3(6) . . ?
C7A C6A C5A 120.8(5) . . ?
C7A C6A Br1A 120.9(4) . . ?
C5A C6A Br1A 118.3(4) . . ?
C6A C7A C2A 120.5(5) . . ?
N1A C8A C4A 113.3(4) . . ?
N1A C10A C11A 109.3(5) . . ?
N2A C11A C10A 112.8(5) . . ?
N2A C13A C14A 116.6(5) . . ?
C19A C14A C15A 119.6(5) . . ?
C19A C14A C13A 119.9(5) . . ?
C15A C14A C13A 120.4(5) . . ?
O3A C15A C16A 121.0(5) . . ?
O3A C15A C14A 119.8(5) . . ?
C16A C15A C14A 119.2(5) . . ?
C17A C16A C15A 119.5(5) . . ?
C17A C16A C20A 119.4(5) . . ?
C15A C16A C20A 121.0(5) . . ?
C18A C17A C16A 120.6(6) . . ?
C17A C18A C19A 120.8(5) . . ?
C17A C18A Br2A 120.1(5) . . ?
C19A C18A Br2A 119.0(4) . . ?
C14A C19A C18A 120.1(5) . . ?
O4A C20A C16A 124.8(6) . . ?
C9A N1A C10A 109.1(5) . . ?
C9A N1A C8A 110.5(4) . . ?
C10A N1A C8A 108.1(4) . . ?
C9A N1A Ni1 113.1(4) . . ?
C10A N1A Ni1 106.8(3) . . ?
C8A N1A Ni1 109.1(3) . . ?
C11A N2A C12A 107.4(5) . . ?
C11A N2A C13A 111.0(4) . . ?
C12A N2A C13A 106.9(5) . . ?
C11A N2A Ni1 106.1(3) . . ?
C12A N2A Ni1 113.7(3) . . ?
C13A N2A Ni1 111.7(3) . . ?
C1A O1A Ni2 126.5(4) . . ?
C3A O2A Ni2 131.1(3) . . ?
C3A O2A Ni1 132.4(3) . . ?
Ni2 O2A Ni1 96.46(16) . . ?
C15A O3A Ni2 125.4(3) . 2_666 ?
C15A O3A Ni1 120.7(3) . . ?
Ni2 O3A Ni1 102.85(16) 2_666 . ?
O1B C2B O2B 126.1(5) . . ?
O1B C2B C1B 116.7(5) . . ?
O2B C2B C1B 117.2(5) . . ?
C2B O1B Ni1 129.3(4) . . ?
C2B O2B Ni2 125.9(3) . . ?
N2C N1C Ni2 119.2(4) . 2_666 ?
N2C N1C Ni1 122.2(4) . . ?
Ni2 N1C Ni1 102.61(19) 2_666 . ?
N2C N1C Ni2 118.7(3) . . ?
Ni2 N1C Ni2 97.25(17) 2_666 . ?
Ni1 N1C Ni2 91.05(17) . . ?
N3C N2C N1C 179.0(6) . . ?
O1D C1D C2D 128.8(5) . . ?
C1D C2D C7D 116.7(5) . . ?
C1D C2D C3D 123.2(5) . . ?
C7D C2D C3D 120.1(5) . . ?
O2D C3D C4D 120.2(5) . . ?
O2D C3D C2D 122.1(5) . . ?
C4D C3D C2D 117.7(5) . . ?
C5D C4D C3D 120.0(5) . . ?
C5D C4D C8D 120.2(5) . . ?
C3D C4D C8D 119.8(5) . . ?
C4D C5D C6D 121.7(6) . . ?
C7D C6D C5D 120.7(6) . . ?
C7D C6D Br1D 119.7(5) . . ?
C5D C6D Br1D 119.6(5) . . ?
C6D C7D C2D 119.8(6) . . ?
C4D C8D N1D 112.5(5) . . ?
N1D C10D C11D 108.2(5) . . ?
N2D C11D C10D 113.1(5) . . ?
C14D C13D N2D 116.5(5) . . ?
C19D C14D C15D 120.4(6) . . ?
C19D C14D C13D 119.5(6) . . ?
C15D C14D C13D 120.0(5) . . ?
O3D C15D C14D 120.7(5) . . ?
O3D C15D C16D 121.2(5) . . ?
C14D C15D C16D 118.1(5) . . ?
C17D C16D C15D 120.4(6) . . ?
C17D C16D C20D 118.5(6) . . ?
C15D C16D C20D 121.1(5) . . ?
C18D C17D C16D 120.6(6) . . ?
C17D C18D C19D 119.7(6) . . ?
C17D C18D Br2D 120.9(5) . . ?
C19D C18D Br2D 119.4(5) . . ?
C14D C19D C18D 120.6(6) . . ?
O4D C20D C16D 123.5(6) . . ?
C10D N1D C9D 109.8(5) . . ?
C10D N1D C8D 108.8(4) . . ?
C9D N1D C8D 109.7(5) . . ?
C10D N1D Ni3 106.4(4) . . ?
C9D N1D Ni3 114.1(4) . . ?
C8D N1D Ni3 107.9(4) . . ?
C12D N2D C11D 109.4(5) . . ?
C12D N2D C13D 106.5(5) . . ?
C11D N2D C13D 110.2(5) . . ?
C12D N2D Ni3 113.5(4) . . ?
C11D N2D Ni3 106.5(4) . . ?
C13D N2D Ni3 110.8(4) . . ?
C1D O1D Ni4 126.4(4) . . ?
C3D O2D Ni4 130.6(4) . . ?
C3D O2D Ni3 130.3(4) . . ?
Ni4 O2D Ni3 95.88(16) . . ?
C15D O3D Ni4 120.9(3) . 2_755 ?
C15D O3D Ni3 122.2(4) . . ?
Ni4 O3D Ni3 101.91(15) 2_755 . ?
O2E C2E O1E 125.7(5) . . ?
O2E C2E C1E 116.8(5) . . ?
O1E C2E C1E 117.5(6) . . ?
C2E O1E Ni3 129.0(4) . . ?
C2E O2E Ni4 126.8(4) . . ?
N2F N1F Ni4 119.8(4) . 2_755 ?
N2F N1F Ni3 124.4(4) . . ?
Ni4 N1F Ni3 102.29(18) 2_755 . ?
N2F N1F Ni4 115.9(4) . . ?
Ni4 N1F Ni4 97.48(19) 2_755 . ?
Ni3 N1F Ni4 90.46(18) . . ?
N3F N2F N1F 179.6(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.127

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.289 0.371 0.839 90 19 ' '
2 0.322 0.046 0.768 13 0 ' '
3 0.711 0.629 0.161 90 19 ' '
4 0.678 0.954 0.232 14 0 ' '
_platon_squeeze_details          
;
;

