# Electronic Supplementary Material (ESI) for ChemComm.
# 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_sg454_done
_database_code_depnum_ccdc_archive 'CCDC 1040543'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Ni(L1)Cl2
_chemical_name_common            'compound 1'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H39 Cl2 N3 Ni'
_chemical_formula_weight         583.26

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121

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

_cell_length_a                   13.6222(7)
_cell_length_b                   14.2676(8)
_cell_length_c                   15.7854(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3068.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prisms
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7889
_exptl_absorpt_correction_T_max  0.9216
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            85516
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         31.36
_reflns_number_total             10063
_reflns_number_gt                9073
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0480P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(7)
_refine_ls_number_reflns         10063
_refine_ls_number_parameters     342
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0782
_refine_ls_wR_factor_gt          0.0765
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.437743(13) 0.787174(12) 0.890664(12) 0.01092(5) Uani 1 1 d . . .
Cl1 Cl 0.31269(3) 0.69227(3) 0.93111(2) 0.01703(8) Uani 1 1 d . . .
Cl2 Cl 0.38134(3) 0.92964(3) 0.85344(3) 0.02243(9) Uani 1 1 d . . .
N1 N 0.54598(8) 0.69447(8) 0.90368(8) 0.0102(2) Uani 1 1 d . . .
N2 N 0.48957(9) 0.80928(9) 1.02228(8) 0.0114(2) Uani 1 1 d . . .
C1 C 0.56871(11) 0.63751(10) 0.83936(9) 0.0128(3) Uani 1 1 d . . .
C2 C 0.63919(11) 0.56794(11) 0.84722(10) 0.0154(3) Uani 1 1 d . . .
H21 H 0.6528 0.5265 0.8016 0.019 Uiso 1 1 calc R . .
C3 C 0.68937(11) 0.56036(11) 0.92342(11) 0.0169(3) Uani 1 1 d . . .
H20 H 0.7389 0.5140 0.9300 0.020 Uiso 1 1 calc R . .
C4 C 0.66750(11) 0.62024(11) 0.99000(10) 0.0148(3) Uani 1 1 d . . .
H19 H 0.7019 0.6165 1.0422 0.018 Uiso 1 1 calc R . .
C5 C 0.59286(10) 0.68649(10) 0.97755(9) 0.0119(3) Uani 1 1 d . . .
C6 C 0.55884(11) 0.75278(10) 1.04174(9) 0.0127(3) Uani 1 1 d . . .
H18 H 0.5875 0.7539 1.0966 0.015 Uiso 1 1 calc R . .
C7 C 0.44882(10) 0.86273(10) 1.09119(9) 0.0119(3) Uani 1 1 d . . .
C8 C 0.39537(11) 0.81545(11) 1.15464(9) 0.0150(3) Uani 1 1 d . . .
C9 C 0.35970(12) 0.86837(12) 1.22169(10) 0.0196(3) Uani 1 1 d . . .
H1 H 0.3247 0.8380 1.2659 0.024 Uiso 1 1 calc R . .
C10 C 0.37395(13) 0.96462(13) 1.22571(11) 0.0230(4) Uani 1 1 d . . .
H2 H 0.3496 0.9994 1.2726 0.028 Uiso 1 1 calc R . .
C11 C 0.42393(12) 1.00974(11) 1.16092(10) 0.0189(3) Uani 1 1 d . . .
H3 H 0.4313 1.0759 1.1626 0.023 Uiso 1 1 calc R . .
C12 C 0.46345(11) 0.95953(11) 1.09338(10) 0.0136(3) Uani 1 1 d . . .
C13 C 0.52803(12) 1.00810(11) 1.02800(10) 0.0155(3) Uani 1 1 d . . .
H7 H 0.5289 0.9684 0.9758 0.019 Uiso 1 1 calc R . .
C14 C 0.49016(15) 1.10473(12) 1.00343(13) 0.0281(4) Uani 1 1 d . . .
H4 H 0.4232 1.0992 0.9812 0.042 Uiso 1 1 calc R . .
H5 H 0.5329 1.1317 0.9599 0.042 Uiso 1 1 calc R . .
H6 H 0.4900 1.1455 1.0534 0.042 Uiso 1 1 calc R . .
C15 C 0.63326(12) 1.01360(13) 1.06222(12) 0.0239(4) Uani 1 1 d . . .
H9 H 0.6335 1.0484 1.1158 0.036 Uiso 1 1 calc R . .
H10 H 0.6751 1.0458 1.0210 0.036 Uiso 1 1 calc R . .
H8 H 0.6584 0.9501 1.0718 0.036 Uiso 1 1 calc R . .
C16 C 0.37443(11) 0.71061(11) 1.15160(10) 0.0164(3) Uani 1 1 d . . .
H11 H 0.3977 0.6865 1.0956 0.020 Uiso 1 1 calc R . .
C17 C 0.43009(14) 0.65844(13) 1.22072(13) 0.0301(4) Uani 1 1 d . . .
H13 H 0.5007 0.6687 1.2136 0.045 Uiso 1 1 calc R . .
H12 H 0.4159 0.5913 1.2167 0.045 Uiso 1 1 calc R . .
H14 H 0.4095 0.6818 1.2763 0.045 Uiso 1 1 calc R . .
C18 C 0.26422(11) 0.69076(12) 1.15815(11) 0.0214(3) Uani 1 1 d . . .
H17 H 0.2395 0.7139 1.2126 0.032 Uiso 1 1 calc R . .
H16 H 0.2528 0.6231 1.1542 0.032 Uiso 1 1 calc R . .
H15 H 0.2298 0.7226 1.1119 0.032 Uiso 1 1 calc R . .
C19 C 0.51767(11) 0.66226(10) 0.76004(10) 0.0131(3) Uani 1 1 d . . .
H22 H 0.5282 0.6276 0.7095 0.016 Uiso 1 1 calc R . .
N3 N 0.45888(9) 0.73178(9) 0.76165(8) 0.0128(3) Uani 1 1 d . . .
C21 C 0.42220(11) 0.76659(10) 0.68186(9) 0.0142(3) Uani 1 1 d . . .
C22 C 0.32702(11) 0.74323(11) 0.65614(10) 0.0163(3) Uani 1 1 d . . .
C23 C 0.26155(12) 0.67971(12) 0.70802(10) 0.0191(3) Uani 1 1 d . . .
H23 H 0.2954 0.6675 0.7632 0.023 Uiso 1 1 calc R . .
C24 C 0.24690(16) 0.58500(13) 0.66374(13) 0.0322(4) Uani 1 1 d . . .
H25 H 0.2159 0.5950 0.6084 0.048 Uiso 1 1 calc R . .
H24 H 0.2047 0.5450 0.6986 0.048 Uiso 1 1 calc R . .
H26 H 0.3107 0.5545 0.6558 0.048 Uiso 1 1 calc R . .
C25 C 0.16349(14) 0.72557(14) 0.72756(13) 0.0322(4) Uani 1 1 d . . .
H27 H 0.1746 0.7846 0.7578 0.048 Uiso 1 1 calc R . .
H28 H 0.1241 0.6835 0.7630 0.048 Uiso 1 1 calc R . .
H29 H 0.1285 0.7381 0.6745 0.048 Uiso 1 1 calc R . .
C26 C 0.29526(12) 0.77898(12) 0.57868(10) 0.0206(3) Uani 1 1 d . . .
H30 H 0.2307 0.7649 0.5597 0.025 Uiso 1 1 calc R . .
C27 C 0.35505(13) 0.83434(12) 0.52870(11) 0.0218(4) Uani 1 1 d . . .
H39 H 0.3321 0.8566 0.4755 0.026 Uiso 1 1 calc R . .
C28 C 0.44847(13) 0.85729(11) 0.55631(10) 0.0195(3) Uani 1 1 d . . .
H38 H 0.4891 0.8958 0.5219 0.023 Uiso 1 1 calc R . .
C29 C 0.48401(12) 0.82470(10) 0.63391(9) 0.0140(3) Uani 1 1 d . . .
C30 C 0.58692(11) 0.84997(11) 0.66269(10) 0.0163(3) Uani 1 1 d . . .
H31 H 0.5941 0.8286 0.7227 0.020 Uiso 1 1 calc R . .
C31 C 0.60629(15) 0.95515(12) 0.66086(14) 0.0327(5) Uani 1 1 d . . .
H32 H 0.6045 0.9775 0.6022 0.049 Uiso 1 1 calc R . .
H34 H 0.6710 0.9681 0.6853 0.049 Uiso 1 1 calc R . .
H33 H 0.5558 0.9876 0.6940 0.049 Uiso 1 1 calc R . .
C32 C 0.66366(13) 0.79819(13) 0.60990(13) 0.0312(4) Uani 1 1 d . . .
H36 H 0.6555 0.7305 0.6175 0.047 Uiso 1 1 calc R . .
H37 H 0.7295 0.8167 0.6284 0.047 Uiso 1 1 calc R . .
H35 H 0.6552 0.8141 0.5500 0.047 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 N1 1.9914(11) . ?
Ni1 N3 2.2034(12) . ?
Ni1 N2 2.2168(12) . ?
Ni1 Cl2 2.2511(4) . ?
Ni1 Cl1 2.2678(4) . ?
N1 C5 1.3344(19) . ?
N1 C1 1.3368(18) . ?
N2 C6 1.279(2) . ?
N2 C7 1.4397(19) . ?
C1 C2 1.387(2) . ?
C1 C19 1.475(2) . ?
C2 C3 1.388(2) . ?
C2 H21 0.9500 . ?
C3 C4 1.387(2) . ?
C3 H20 0.9500 . ?
C4 C5 1.402(2) . ?
C4 H19 0.9500 . ?
C5 C6 1.461(2) . ?
C6 H18 0.9500 . ?
C7 C12 1.396(2) . ?
C7 C8 1.410(2) . ?
C8 C9 1.388(2) . ?
C8 C16 1.523(2) . ?
C9 C10 1.388(2) . ?
C9 H1 0.9500 . ?
C10 C11 1.387(2) . ?
C10 H2 0.9500 . ?
C11 C12 1.393(2) . ?
C11 H3 0.9500 . ?
C12 C13 1.523(2) . ?
C13 C14 1.522(2) . ?
C13 C15 1.534(2) . ?
C13 H7 1.0000 . ?
C14 H4 0.9800 . ?
C14 H5 0.9800 . ?
C14 H6 0.9800 . ?
C15 H9 0.9800 . ?
C15 H10 0.9800 . ?
C15 H8 0.9800 . ?
C16 C17 1.523(2) . ?
C16 C18 1.531(2) . ?
C16 H11 1.0000 . ?
C17 H13 0.9800 . ?
C17 H12 0.9800 . ?
C17 H14 0.9800 . ?
C18 H17 0.9800 . ?
C18 H16 0.9800 . ?
C18 H15 0.9800 . ?
C19 N3 1.2751(19) . ?
C19 H22 0.9500 . ?
N3 C21 1.443(2) . ?
C21 C22 1.399(2) . ?
C21 C29 1.403(2) . ?
C22 C26 1.394(2) . ?
C22 C23 1.512(2) . ?
C23 C25 1.519(2) . ?
C23 C24 1.535(2) . ?
C23 H23 1.0000 . ?
C24 H25 0.9800 . ?
C24 H24 0.9800 . ?
C24 H26 0.9800 . ?
C25 H27 0.9800 . ?
C25 H28 0.9800 . ?
C25 H29 0.9800 . ?
C26 C27 1.382(2) . ?
C26 H30 0.9500 . ?
C27 C28 1.384(2) . ?
C27 H39 0.9500 . ?
C28 C29 1.397(2) . ?
C28 H38 0.9500 . ?
C29 C30 1.517(2) . ?
C30 C31 1.524(2) . ?
C30 C32 1.527(2) . ?
C30 H31 1.0000 . ?
C31 H32 0.9800 . ?
C31 H34 0.9800 . ?
C31 H33 0.9800 . ?
C32 H36 0.9800 . ?
C32 H37 0.9800 . ?
C32 H35 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 76.13(5) . . ?
N1 Ni1 N2 76.23(5) . . ?
N3 Ni1 N2 151.12(5) . . ?
N1 Ni1 Cl2 151.57(4) . . ?
N3 Ni1 Cl2 97.31(3) . . ?
N2 Ni1 Cl2 102.99(3) . . ?
N1 Ni1 Cl1 97.50(4) . . ?
N3 Ni1 Cl1 98.29(3) . . ?
N2 Ni1 Cl1 93.46(3) . . ?
Cl2 Ni1 Cl1 110.869(17) . . ?
C5 N1 C1 120.07(12) . . ?
C5 N1 Ni1 120.08(10) . . ?
C1 N1 Ni1 119.79(10) . . ?
C6 N2 C7 115.91(12) . . ?
C6 N2 Ni1 111.75(10) . . ?
C7 N2 Ni1 131.35(9) . . ?
N1 C1 C2 121.84(14) . . ?
N1 C1 C19 112.96(13) . . ?
C2 C1 C19 125.01(14) . . ?
C1 C2 C3 118.33(14) . . ?
C1 C2 H21 120.8 . . ?
C3 C2 H21 120.8 . . ?
C4 C3 C2 120.20(14) . . ?
C4 C3 H20 119.9 . . ?
C2 C3 H20 119.9 . . ?
C3 C4 C5 117.71(14) . . ?
C3 C4 H19 121.1 . . ?
C5 C4 H19 121.1 . . ?
N1 C5 C4 121.81(13) . . ?
N1 C5 C6 113.51(12) . . ?
C4 C5 C6 124.68(13) . . ?
N2 C6 C5 118.39(13) . . ?
N2 C6 H18 120.8 . . ?
C5 C6 H18 120.8 . . ?
C12 C7 C8 121.97(14) . . ?
C12 C7 N2 119.19(13) . . ?
C8 C7 N2 118.84(13) . . ?
C9 C8 C7 117.52(14) . . ?
C9 C8 C16 119.51(14) . . ?
C7 C8 C16 122.96(13) . . ?
C10 C9 C8 121.60(15) . . ?
C10 C9 H1 119.2 . . ?
C8 C9 H1 119.2 . . ?
C11 C10 C9 119.60(15) . . ?
C11 C10 H2 120.2 . . ?
C9 C10 H2 120.2 . . ?
C10 C11 C12 121.02(15) . . ?
C10 C11 H3 119.5 . . ?
C12 C11 H3 119.5 . . ?
C11 C12 C7 118.21(14) . . ?
C11 C12 C13 120.53(14) . . ?
C7 C12 C13 121.06(14) . . ?
C12 C13 C14 112.90(14) . . ?
C12 C13 C15 108.93(13) . . ?
C14 C13 C15 111.11(14) . . ?
C12 C13 H7 107.9 . . ?
C14 C13 H7 107.9 . . ?
C15 C13 H7 107.9 . . ?
C13 C14 H4 109.5 . . ?
C13 C14 H5 109.5 . . ?
H4 C14 H5 109.5 . . ?
C13 C14 H6 109.5 . . ?
H4 C14 H6 109.5 . . ?
H5 C14 H6 109.5 . . ?
C13 C15 H9 109.5 . . ?
C13 C15 H10 109.5 . . ?
H9 C15 H10 109.5 . . ?
C13 C15 H8 109.5 . . ?
H9 C15 H8 109.5 . . ?
H10 C15 H8 109.5 . . ?
C17 C16 C8 111.35(14) . . ?
C17 C16 C18 110.45(13) . . ?
C8 C16 C18 111.29(14) . . ?
C17 C16 H11 107.9 . . ?
C8 C16 H11 107.9 . . ?
C18 C16 H11 107.9 . . ?
C16 C17 H13 109.5 . . ?
C16 C17 H12 109.5 . . ?
H13 C17 H12 109.5 . . ?
C16 C17 H14 109.5 . . ?
H13 C17 H14 109.5 . . ?
H12 C17 H14 109.5 . . ?
C16 C18 H17 109.5 . . ?
C16 C18 H16 109.5 . . ?
H17 C18 H16 109.5 . . ?
C16 C18 H15 109.5 . . ?
H17 C18 H15 109.5 . . ?
H16 C18 H15 109.5 . . ?
N3 C19 C1 117.72(14) . . ?
N3 C19 H22 121.1 . . ?
C1 C19 H22 121.1 . . ?
C19 N3 C21 117.88(13) . . ?
C19 N3 Ni1 112.31(10) . . ?
C21 N3 Ni1 129.64(9) . . ?
C22 C21 C29 122.71(14) . . ?
C22 C21 N3 119.48(14) . . ?
C29 C21 N3 117.79(13) . . ?
C26 C22 C21 117.07(15) . . ?
C26 C22 C23 120.75(14) . . ?
C21 C22 C23 122.15(14) . . ?
C22 C23 C25 111.74(15) . . ?
C22 C23 C24 110.96(14) . . ?
C25 C23 C24 110.94(15) . . ?
C22 C23 H23 107.7 . . ?
C25 C23 H23 107.7 . . ?
C24 C23 H23 107.7 . . ?
C23 C24 H25 109.5 . . ?
C23 C24 H24 109.5 . . ?
H25 C24 H24 109.5 . . ?
C23 C24 H26 109.5 . . ?
H25 C24 H26 109.5 . . ?
H24 C24 H26 109.5 . . ?
C23 C25 H27 109.5 . . ?
C23 C25 H28 109.5 . . ?
H27 C25 H28 109.5 . . ?
C23 C25 H29 109.5 . . ?
H27 C25 H29 109.5 . . ?
H28 C25 H29 109.5 . . ?
C27 C26 C22 121.81(15) . . ?
C27 C26 H30 119.1 . . ?
C22 C26 H30 119.1 . . ?
C26 C27 C28 119.82(15) . . ?
C26 C27 H39 120.1 . . ?
C28 C27 H39 120.1 . . ?
C27 C28 C29 121.06(16) . . ?
C27 C28 H38 119.5 . . ?
C29 C28 H38 119.5 . . ?
C28 C29 C21 117.49(14) . . ?
C28 C29 C30 120.25(14) . . ?
C21 C29 C30 122.23(14) . . ?
C29 C30 C31 112.85(14) . . ?
C29 C30 C32 110.74(13) . . ?
C31 C30 C32 110.33(15) . . ?
C29 C30 H31 107.6 . . ?
C31 C30 H31 107.6 . . ?
C32 C30 H31 107.6 . . ?
C30 C31 H32 109.5 . . ?
C30 C31 H34 109.5 . . ?
H32 C31 H34 109.5 . . ?
C30 C31 H33 109.5 . . ?
H32 C31 H33 109.5 . . ?
H34 C31 H33 109.5 . . ?
C30 C32 H36 109.5 . . ?
C30 C32 H37 109.5 . . ?
H36 C32 H37 109.5 . . ?
C30 C32 H35 109.5 . . ?
H36 C32 H35 109.5 . . ?
H37 C32 H35 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N3 Ni1 N1 C5 173.45(11) . . . . ?
N2 Ni1 N1 C5 1.93(10) . . . . ?
Cl2 Ni1 N1 C5 93.86(12) . . . . ?
Cl1 Ni1 N1 C5 -89.81(10) . . . . ?
N3 Ni1 N1 C1 -9.41(11) . . . . ?
N2 Ni1 N1 C1 179.07(12) . . . . ?
Cl2 Ni1 N1 C1 -88.99(13) . . . . ?
Cl1 Ni1 N1 C1 87.33(11) . . . . ?
N1 Ni1 N2 C6 -1.44(10) . . . . ?
N3 Ni1 N2 C6 -18.68(16) . . . . ?
Cl2 Ni1 N2 C6 -152.21(9) . . . . ?
Cl1 Ni1 N2 C6 95.44(10) . . . . ?
N1 Ni1 N2 C7 -169.34(13) . . . . ?
N3 Ni1 N2 C7 173.42(11) . . . . ?
Cl2 Ni1 N2 C7 39.89(12) . . . . ?
Cl1 Ni1 N2 C7 -72.45(12) . . . . ?
C5 N1 C1 C2 1.3(2) . . . . ?
Ni1 N1 C1 C2 -175.84(11) . . . . ?
C5 N1 C1 C19 -173.89(12) . . . . ?
Ni1 N1 C1 C19 8.96(17) . . . . ?
N1 C1 C2 C3 -2.4(2) . . . . ?
C19 C1 C2 C3 172.23(14) . . . . ?
C1 C2 C3 C4 1.2(2) . . . . ?
C2 C3 C4 C5 1.0(2) . . . . ?
C1 N1 C5 C4 1.0(2) . . . . ?
Ni1 N1 C5 C4 178.12(11) . . . . ?
C1 N1 C5 C6 -179.22(13) . . . . ?
Ni1 N1 C5 C6 -2.08(16) . . . . ?
C3 C4 C5 N1 -2.1(2) . . . . ?
C3 C4 C5 C6 178.14(14) . . . . ?
C7 N2 C6 C5 170.77(12) . . . . ?
Ni1 N2 C6 C5 0.85(16) . . . . ?
N1 C5 C6 N2 0.65(19) . . . . ?
C4 C5 C6 N2 -179.56(14) . . . . ?
C6 N2 C7 C12 112.41(16) . . . . ?
Ni1 N2 C7 C12 -80.09(16) . . . . ?
C6 N2 C7 C8 -67.46(17) . . . . ?
Ni1 N2 C7 C8 100.03(15) . . . . ?
C12 C7 C8 C9 -1.9(2) . . . . ?
N2 C7 C8 C9 177.96(13) . . . . ?
C12 C7 C8 C16 177.13(14) . . . . ?
N2 C7 C8 C16 -3.0(2) . . . . ?
C7 C8 C9 C10 1.4(2) . . . . ?
C16 C8 C9 C10 -177.72(15) . . . . ?
C8 C9 C10 C11 0.8(3) . . . . ?
C9 C10 C11 C12 -2.5(3) . . . . ?
C10 C11 C12 C7 2.0(2) . . . . ?
C10 C11 C12 C13 -172.97(15) . . . . ?
C8 C7 C12 C11 0.3(2) . . . . ?
N2 C7 C12 C11 -179.58(13) . . . . ?
C8 C7 C12 C13 175.19(14) . . . . ?
N2 C7 C12 C13 -4.7(2) . . . . ?
C11 C12 C13 C14 -40.9(2) . . . . ?
C7 C12 C13 C14 144.28(15) . . . . ?
C11 C12 C13 C15 82.99(18) . . . . ?
C7 C12 C13 C15 -91.79(17) . . . . ?
C9 C8 C16 C17 -69.38(19) . . . . ?
C7 C8 C16 C17 111.59(17) . . . . ?
C9 C8 C16 C18 54.32(19) . . . . ?
C7 C8 C16 C18 -124.71(16) . . . . ?
N1 C1 C19 N3 -0.8(2) . . . . ?
C2 C1 C19 N3 -175.82(14) . . . . ?
C1 C19 N3 C21 169.31(13) . . . . ?
C1 C19 N3 Ni1 -6.47(17) . . . . ?
N1 Ni1 N3 C19 8.35(10) . . . . ?
N2 Ni1 N3 C19 25.60(16) . . . . ?
Cl2 Ni1 N3 C19 160.18(10) . . . . ?
Cl1 Ni1 N3 C19 -87.38(10) . . . . ?
N1 Ni1 N3 C21 -166.79(13) . . . . ?
N2 Ni1 N3 C21 -149.54(11) . . . . ?
Cl2 Ni1 N3 C21 -14.96(12) . . . . ?
Cl1 Ni1 N3 C21 97.47(12) . . . . ?
C19 N3 C21 C22 102.06(17) . . . . ?
Ni1 N3 C21 C22 -83.02(16) . . . . ?
C19 N3 C21 C29 -79.23(18) . . . . ?
Ni1 N3 C21 C29 95.69(15) . . . . ?
C29 C21 C22 C26 1.2(2) . . . . ?
N3 C21 C22 C26 179.81(13) . . . . ?
C29 C21 C22 C23 179.37(14) . . . . ?
N3 C21 C22 C23 -2.0(2) . . . . ?
C26 C22 C23 C25 -56.4(2) . . . . ?
C21 C22 C23 C25 125.47(16) . . . . ?
C26 C22 C23 C24 68.0(2) . . . . ?
C21 C22 C23 C24 -110.14(18) . . . . ?
C21 C22 C26 C27 0.6(2) . . . . ?
C23 C22 C26 C27 -177.60(16) . . . . ?
C22 C26 C27 C28 -1.5(3) . . . . ?
C26 C27 C28 C29 0.5(3) . . . . ?
C27 C28 C29 C21 1.1(2) . . . . ?
C27 C28 C29 C30 179.48(15) . . . . ?
C22 C21 C29 C28 -2.0(2) . . . . ?
N3 C21 C29 C28 179.30(13) . . . . ?
C22 C21 C29 C30 179.66(14) . . . . ?
N3 C21 C29 C30 1.0(2) . . . . ?
C28 C29 C30 C31 52.9(2) . . . . ?
C21 C29 C30 C31 -128.83(17) . . . . ?
C28 C29 C30 C32 -71.34(19) . . . . ?
C21 C29 C30 C32 106.92(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        31.36
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.069
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
####################################################################### 
# 
# 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_sg33
_database_code_depnum_ccdc_archive 'CCDC 1040544'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H39 Br2 Cl2 N3 Ni'
_chemical_formula_weight         755.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   9.7870(6)
_cell_length_b                   26.3927(17)
_cell_length_c                   13.7739(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.906(3)
_cell_angle_gamma                90.00
_cell_volume                     3365.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    3.135
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5079
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            118495
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.54
_diffrn_reflns_theta_max         28.52
_reflns_number_total             8496
_reflns_number_gt                7018
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0273P)²+4.3230P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8496
_refine_ls_number_parameters     388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0301
_refine_ls_wR_factor_ref         0.0700
_refine_ls_wR_factor_gt          0.0653
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.69510(2) 0.237725(8) 0.905114(16) 0.01922(6) Uani 1 1 d . . .
Br2 Br 0.89772(2) 0.122083(8) 0.81979(2) 0.02459(6) Uani 1 1 d . . .
Ni1 Ni 0.67477(3) 0.158845(9) 0.81043(2) 0.01193(6) Uani 1 1 d . . .
Cl1 Cl 0.2767(3) 0.05604(10) 0.62804(18) 0.0503(5) Uani 0.596(3) 1 d P A 1
Cl2 Cl 0.06936(17) 0.05637(6) 0.42974(10) 0.0554(6) Uani 0.596(3) 1 d P A 1
N1 N 0.46235(18) 0.16352(6) 0.76688(13) 0.0135(3) Uani 1 1 d . . .
N2 N 0.62047(18) 0.19260(6) 0.66090(13) 0.0146(3) Uani 1 1 d . . .
C1 C 0.3941(2) 0.19201(8) 0.68554(16) 0.0177(4) Uani 1 1 d . . .
C6 C 0.4883(2) 0.20542(8) 0.62488(17) 0.0188(4) Uani 1 1 d . . .
H6 H 0.4518 0.2229 0.5614 0.023 Uiso 1 1 calc R . .
C7 C 0.7095(2) 0.19688(8) 0.59609(16) 0.0167(4) Uani 1 1 d . . .
C12 C 0.7885(2) 0.24088(8) 0.59549(17) 0.0191(4) Uani 1 1 d . . .
C11 C 0.8718(2) 0.24164(9) 0.53032(18) 0.0228(5) Uani 1 1 d . . .
H11 H 0.9261 0.2712 0.5276 0.027 Uiso 1 1 calc R . .
C10 C 0.8774(3) 0.20082(10) 0.46998(18) 0.0258(5) Uani 1 1 d . . .
H10 H 0.9334 0.2025 0.4252 0.031 Uiso 1 1 calc R . .
C9 C 0.8016(3) 0.15731(9) 0.47447(18) 0.0284(5) Uani 1 1 d . . .
H9 H 0.8071 0.1290 0.4332 0.034 Uiso 1 1 calc R . .
C8 C 0.7171(3) 0.15405(9) 0.53828(17) 0.0230(5) Uani 1 1 d . . .
C16 C 0.6328(4) 0.10624(10) 0.5420(2) 0.0375(7) Uani 1 1 d . . .
H16 H 0.6115 0.1067 0.6083 0.045 Uiso 1 1 calc R . .
C17 C 0.7191(5) 0.05846(11) 0.5413(3) 0.0695(13) Uani 1 1 d . . .
H17A H 0.7389 0.0562 0.4761 0.104 Uiso 1 1 calc R . .
H17B H 0.6635 0.0288 0.5491 0.104 Uiso 1 1 calc R . .
H17C H 0.8105 0.0597 0.5981 0.104 Uiso 1 1 calc R . .
C18 C 0.4881(4) 0.10566(14) 0.4556(2) 0.0641(12) Uani 1 1 d . . .
H18A H 0.4354 0.1370 0.4575 0.096 Uiso 1 1 calc R . .
H18B H 0.4310 0.0765 0.4643 0.096 Uiso 1 1 calc R . .
H18C H 0.5049 0.1030 0.3894 0.096 Uiso 1 1 calc R . .
C13 C 0.7939(3) 0.28455(9) 0.6677(2) 0.0294(6) Uani 1 1 d . . .
H13 H 0.7088 0.2815 0.6924 0.035 Uiso 1 1 calc R . .
C15 C 0.7842(4) 0.33594(10) 0.6139(3) 0.0536(10) Uani 1 1 d . . .
H15A H 0.8683 0.3403 0.5908 0.080 Uiso 1 1 calc R . .
H15B H 0.7825 0.3631 0.6619 0.080 Uiso 1 1 calc R . .
H15C H 0.6957 0.3372 0.5546 0.080 Uiso 1 1 calc R . .
C14 C 0.9312(3) 0.28042(11) 0.7612(2) 0.0406(7) Uani 1 1 d . . .
H14A H 0.9328 0.2475 0.7946 0.061 Uiso 1 1 calc R . .
H14B H 0.9321 0.3076 0.8099 0.061 Uiso 1 1 calc R . .
H14C H 1.0163 0.2835 0.7390 0.061 Uiso 1 1 calc R . .
C2 C 0.2481(2) 0.20275(9) 0.66131(18) 0.0245(5) Uani 1 1 d . . .
H2 H 0.1997 0.2231 0.6035 0.029 Uiso 1 1 calc R . .
C3 C 0.1743(2) 0.18302(9) 0.72363(19) 0.0256(5) Uani 1 1 d . . .
H3 H 0.0742 0.1897 0.7085 0.031 Uiso 1 1 calc R . .
C4 C 0.2471(2) 0.15341(9) 0.80818(18) 0.0204(4) Uani 1 1 d . . .
H4 H 0.1981 0.1398 0.8516 0.024 Uiso 1 1 calc R . .
C5 C 0.3927(2) 0.14440(8) 0.82727(16) 0.0153(4) Uani 1 1 d . . .
C19 C 0.4855(2) 0.11111(8) 0.90730(15) 0.0149(4) Uani 1 1 d . . .
H19 H 0.4471 0.0919 0.9507 0.018 Uiso 1 1 calc R . .
N3 N 0.61897(18) 0.10889(6) 0.91649(13) 0.0137(3) Uani 1 1 d . . .
C20 C 0.7075(2) 0.07108(8) 0.98293(16) 0.0142(4) Uani 1 1 d . . .
C25 C 0.7084(2) 0.02246(8) 0.94282(17) 0.0176(4) Uani 1 1 d . . .
C24 C 0.7951(3) -0.01384(8) 1.00786(19) 0.0238(5) Uani 1 1 d . . .
H24 H 0.7975 -0.0473 0.9833 0.029 Uiso 1 1 calc R . .
C23 C 0.8774(3) -0.00200(9) 1.10707(19) 0.0264(5) Uani 1 1 d . . .
H23 H 0.9341 -0.0274 1.1507 0.032 Uiso 1 1 calc R . .
C22 C 0.8774(2) 0.04667(9) 1.14297(18) 0.0237(5) Uani 1 1 d . . .
H22 H 0.9360 0.0546 1.2110 0.028 Uiso 1 1 calc R . .
C21 C 0.7933(2) 0.08462(8) 1.08150(17) 0.0180(4) Uani 1 1 d . . .
C27 C 0.7976(3) 0.13828(8) 1.12155(17) 0.0226(5) Uani 1 1 d . . .
H27 H 0.7318 0.1595 1.0656 0.027 Uiso 1 1 calc R . .
C28 C 0.9448(4) 0.16001(13) 1.1487(4) 0.0701(13) Uani 1 1 d . . .
H28A H 1.0102 0.1411 1.2064 0.105 Uiso 1 1 calc R . .
H28B H 0.9425 0.1956 1.1681 0.105 Uiso 1 1 calc R . .
H28C H 0.9792 0.1577 1.0894 0.105 Uiso 1 1 calc R . .
C29 C 0.7446(4) 0.14081(12) 1.2129(3) 0.0532(9) Uani 1 1 d . . .
H29A H 0.8047 0.1190 1.2677 0.080 Uiso 1 1 calc R . .
H29B H 0.6441 0.1293 1.1927 0.080 Uiso 1 1 calc R . .
H29C H 0.7507 0.1758 1.2377 0.080 Uiso 1 1 calc R . .
C26 C 0.6208(3) 0.00860(8) 0.83356(17) 0.0214(5) Uani 1 1 d . . .
H26 H 0.5787 0.0406 0.7970 0.026 Uiso 1 1 calc R . .
C30 C 0.4961(3) -0.02622(10) 0.8321(2) 0.0285(5) Uani 1 1 d . . .
H30A H 0.5344 -0.0583 0.8659 0.043 Uiso 1 1 calc R . .
H30B H 0.4367 -0.0328 0.7609 0.043 Uiso 1 1 calc R . .
H30C H 0.4370 -0.0100 0.8686 0.043 Uiso 1 1 calc R . .
C31 C 0.7148(3) -0.01521(9) 0.7762(2) 0.0296(5) Uani 1 1 d . . .
H31A H 0.7932 0.0081 0.7772 0.044 Uiso 1 1 calc R . .
H31B H 0.6558 -0.0219 0.7050 0.044 Uiso 1 1 calc R . .
H31C H 0.7558 -0.0471 0.8096 0.044 Uiso 1 1 calc R . .
C32 C 0.1180(6) 0.0795(2) 0.5462(4) 0.113(2) Uani 1 1 d . . .
Cl3 Cl 0.1305(3) 0.10058(13) 0.4389(2) 0.0746(11) Uani 0.404(3) 1 d P A 2
Cl4 Cl 0.2243(7) 0.04236(17) 0.6497(3) 0.0977(19) Uani 0.404(3) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Ni1 2.4303(3) . ?
Br2 Ni1 2.3530(3) . ?
Ni1 N1 1.9720(17) . ?
Ni1 N2 2.1468(17) . ?
Ni1 N3 2.1651(17) . ?
Cl1 C32 1.712(5) . ?
Cl2 C32 1.636(5) . ?
N1 C5 1.333(3) . ?
N1 C1 1.335(3) . ?
N2 C6 1.272(3) . ?
N2 C7 1.440(3) . ?
C1 C2 1.387(3) . ?
C1 C6 1.474(3) . ?
C6 H6 0.9500 . ?
C7 C12 1.397(3) . ?
C7 C8 1.399(3) . ?
C12 C11 1.395(3) . ?
C12 C13 1.512(3) . ?
C11 C10 1.373(3) . ?
C11 H11 0.9500 . ?
C10 C9 1.380(4) . ?
C10 H10 0.9500 . ?
C9 C8 1.391(3) . ?
C9 H9 0.9500 . ?
C8 C16 1.518(3) . ?
C16 C17 1.520(4) . ?
C16 C18 1.527(5) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C13 C15 1.534(4) . ?
C13 C14 1.535(4) . ?
C13 H13 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C2 C3 1.390(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.392(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(3) . ?
C4 H4 0.9500 . ?
C5 C19 1.471(3) . ?
C19 N3 1.272(3) . ?
C19 H19 0.9500 . ?
N3 C20 1.439(3) . ?
C20 C21 1.392(3) . ?
C20 C25 1.398(3) . ?
C25 C24 1.395(3) . ?
C25 C26 1.516(3) . ?
C24 C23 1.379(3) . ?
C24 H24 0.9500 . ?
C23 C22 1.377(3) . ?
C23 H23 0.9500 . ?
C22 C21 1.395(3) . ?
C22 H22 0.9500 . ?
C21 C27 1.516(3) . ?
C27 C28 1.482(4) . ?
C27 C29 1.510(4) . ?
C27 H27 1.0000 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C26 C30 1.523(3) . ?
C26 C31 1.529(3) . ?
C26 H26 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 Cl3 1.620(6) . ?
C32 Cl4 1.765(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 76.90(7) . . ?
N1 Ni1 N3 76.81(7) . . ?
N2 Ni1 N3 149.53(7) . . ?
N1 Ni1 Br2 155.50(5) . . ?
N2 Ni1 Br2 99.24(5) . . ?
N3 Ni1 Br2 98.29(5) . . ?
N1 Ni1 Br1 90.26(5) . . ?
N2 Ni1 Br1 96.38(5) . . ?
N3 Ni1 Br1 98.87(5) . . ?
Br2 Ni1 Br1 114.240(13) . . ?
C5 N1 C1 121.24(18) . . ?
C5 N1 Ni1 119.21(14) . . ?
C1 N1 Ni1 118.84(14) . . ?
C6 N2 C7 118.72(18) . . ?
C6 N2 Ni1 112.88(14) . . ?
C7 N2 Ni1 128.03(13) . . ?
N1 C1 C2 120.91(19) . . ?
N1 C1 C6 112.07(18) . . ?
C2 C1 C6 126.8(2) . . ?
N2 C6 C1 117.33(19) . . ?
N2 C6 H6 121.3 . . ?
C1 C6 H6 121.3 . . ?
C12 C7 C8 122.46(19) . . ?
C12 C7 N2 121.10(19) . . ?
C8 C7 N2 116.38(19) . . ?
C11 C12 C7 117.1(2) . . ?
C11 C12 C13 120.6(2) . . ?
C7 C12 C13 122.08(19) . . ?
C10 C11 C12 121.6(2) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C10 C9 119.9(2) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C9 C8 121.2(2) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C8 C7 117.5(2) . . ?
C9 C8 C16 120.9(2) . . ?
C7 C8 C16 121.5(2) . . ?
C8 C16 C17 112.3(3) . . ?
C8 C16 C18 111.0(2) . . ?
C17 C16 C18 111.3(3) . . ?
C8 C16 H16 107.3 . . ?
C17 C16 H16 107.3 . . ?
C18 C16 H16 107.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C13 C15 111.9(2) . . ?
C12 C13 C14 109.4(2) . . ?
C15 C13 C14 111.6(2) . . ?
C12 C13 H13 107.9 . . ?
C15 C13 H13 107.9 . . ?
C14 C13 H13 107.9 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C1 C2 C3 118.4(2) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 118.2(2) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N1 C5 C4 121.29(19) . . ?
N1 C5 C19 112.16(17) . . ?
C4 C5 C19 126.39(19) . . ?
N3 C19 C5 117.84(18) . . ?
N3 C19 H19 121.1 . . ?
C5 C19 H19 121.1 . . ?
C19 N3 C20 118.84(17) . . ?
C19 N3 Ni1 112.34(14) . . ?
C20 N3 Ni1 128.32(13) . . ?
C21 C20 C25 122.81(19) . . ?
C21 C20 N3 119.39(18) . . ?
C25 C20 N3 117.71(18) . . ?
C24 C25 C20 117.2(2) . . ?
C24 C25 C26 120.2(2) . . ?
C20 C25 C26 122.65(19) . . ?
C23 C24 C25 121.3(2) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C22 C23 C24 120.0(2) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C22 C21 121.4(2) . . ?
C23 C22 H22 119.3 . . ?
C21 C22 H22 119.3 . . ?
C20 C21 C22 117.3(2) . . ?
C20 C21 C27 122.14(19) . . ?
C22 C21 C27 120.6(2) . . ?
C28 C27 C29 110.0(3) . . ?
C28 C27 C21 111.3(2) . . ?
C29 C27 C21 111.6(2) . . ?
C28 C27 H27 107.9 . . ?
C29 C27 H27 107.9 . . ?
C21 C27 H27 107.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C25 C26 C30 110.59(19) . . ?
C25 C26 C31 111.8(2) . . ?
C30 C26 C31 111.05(19) . . ?
C25 C26 H26 107.8 . . ?
C30 C26 H26 107.8 . . ?
C31 C26 H26 107.8 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Cl3 C32 Cl2 47.00(18) . . ?
Cl3 C32 Cl1 113.8(4) . . ?
Cl2 C32 Cl1 115.1(3) . . ?
Cl3 C32 Cl4 136.8(4) . . ?
Cl2 C32 Cl4 119.5(3) . . ?
Cl1 C32 Cl4 25.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 Ni1 N1 C5 176.35(17) . . . . ?
N3 Ni1 N1 C5 11.89(15) . . . . ?
Br2 Ni1 N1 C5 92.84(19) . . . . ?
Br1 Ni1 N1 C5 -87.16(15) . . . . ?
N2 Ni1 N1 C1 -13.22(15) . . . . ?
N3 Ni1 N1 C1 -177.68(17) . . . . ?
Br2 Ni1 N1 C1 -96.73(18) . . . . ?
Br1 Ni1 N1 C1 83.27(16) . . . . ?
N1 Ni1 N2 C6 9.21(15) . . . . ?
N3 Ni1 N2 C6 40.2(2) . . . . ?
Br2 Ni1 N2 C6 164.53(14) . . . . ?
Br1 Ni1 N2 C6 -79.57(15) . . . . ?
N1 Ni1 N2 C7 -163.66(18) . . . . ?
N3 Ni1 N2 C7 -132.69(17) . . . . ?
Br2 Ni1 N2 C7 -8.33(17) . . . . ?
Br1 Ni1 N2 C7 107.56(16) . . . . ?
C5 N1 C1 C2 0.1(3) . . . . ?
Ni1 N1 C1 C2 -170.09(18) . . . . ?
C5 N1 C1 C6 -175.10(19) . . . . ?
Ni1 N1 C1 C6 14.7(2) . . . . ?
C7 N2 C6 C1 169.11(19) . . . . ?
Ni1 N2 C6 C1 -4.5(2) . . . . ?
N1 C1 C6 N2 -5.9(3) . . . . ?
C2 C1 C6 N2 179.2(2) . . . . ?
C6 N2 C7 C12 91.8(3) . . . . ?
Ni1 N2 C7 C12 -95.7(2) . . . . ?
C6 N2 C7 C8 -91.1(3) . . . . ?
Ni1 N2 C7 C8 81.4(2) . . . . ?
C8 C7 C12 C11 3.0(3) . . . . ?
N2 C7 C12 C11 179.97(19) . . . . ?
C8 C7 C12 C13 -172.4(2) . . . . ?
N2 C7 C12 C13 4.6(3) . . . . ?
C7 C12 C11 C10 -0.6(3) . . . . ?
C13 C12 C11 C10 174.8(2) . . . . ?
C12 C11 C10 C9 -1.3(4) . . . . ?
C11 C10 C9 C8 0.9(4) . . . . ?
C10 C9 C8 C7 1.3(4) . . . . ?
C10 C9 C8 C16 179.4(2) . . . . ?
C12 C7 C8 C9 -3.4(3) . . . . ?
N2 C7 C8 C9 179.6(2) . . . . ?
C12 C7 C8 C16 178.6(2) . . . . ?
N2 C7 C8 C16 1.5(3) . . . . ?
C9 C8 C16 C17 41.5(4) . . . . ?
C7 C8 C16 C17 -140.5(3) . . . . ?
C9 C8 C16 C18 -83.9(3) . . . . ?
C7 C8 C16 C18 94.1(3) . . . . ?
C11 C12 C13 C15 45.9(3) . . . . ?
C7 C12 C13 C15 -138.9(2) . . . . ?
C11 C12 C13 C14 -78.4(3) . . . . ?
C7 C12 C13 C14 96.9(3) . . . . ?
N1 C1 C2 C3 -0.2(4) . . . . ?
C6 C1 C2 C3 174.3(2) . . . . ?
C1 C2 C3 C4 0.2(4) . . . . ?
C2 C3 C4 C5 -0.2(4) . . . . ?
C1 N1 C5 C4 -0.1(3) . . . . ?
Ni1 N1 C5 C4 170.05(17) . . . . ?
C1 N1 C5 C19 175.60(19) . . . . ?
Ni1 N1 C5 C19 -14.2(2) . . . . ?
C3 C4 C5 N1 0.2(3) . . . . ?
C3 C4 C5 C19 -174.9(2) . . . . ?
N1 C5 C19 N3 7.3(3) . . . . ?
C4 C5 C19 N3 -177.2(2) . . . . ?
C5 C19 N3 C20 -170.57(18) . . . . ?
C5 C19 N3 Ni1 2.0(2) . . . . ?
N1 Ni1 N3 C19 -7.10(14) . . . . ?
N2 Ni1 N3 C19 -38.1(2) . . . . ?
Br2 Ni1 N3 C19 -162.65(14) . . . . ?
Br1 Ni1 N3 C19 81.08(14) . . . . ?
N1 Ni1 N3 C20 164.60(18) . . . . ?
N2 Ni1 N3 C20 133.62(17) . . . . ?
Br2 Ni1 N3 C20 9.05(17) . . . . ?
Br1 Ni1 N3 C20 -107.22(16) . . . . ?
C19 N3 C20 C21 -99.3(2) . . . . ?
Ni1 N3 C20 C21 89.4(2) . . . . ?
C19 N3 C20 C25 83.9(2) . . . . ?
Ni1 N3 C20 C25 -87.4(2) . . . . ?
C21 C20 C25 C24 3.1(3) . . . . ?
N3 C20 C25 C24 179.75(19) . . . . ?
C21 C20 C25 C26 -176.7(2) . . . . ?
N3 C20 C25 C26 0.0(3) . . . . ?
C20 C25 C24 C23 -0.7(3) . . . . ?
C26 C25 C24 C23 179.1(2) . . . . ?
C25 C24 C23 C22 -1.4(4) . . . . ?
C24 C23 C22 C21 1.2(4) . . . . ?
C25 C20 C21 C22 -3.2(3) . . . . ?
N3 C20 C21 C22 -179.85(19) . . . . ?
C25 C20 C21 C27 176.3(2) . . . . ?
N3 C20 C21 C27 -0.4(3) . . . . ?
C23 C22 C21 C20 1.0(3) . . . . ?
C23 C22 C21 C27 -178.5(2) . . . . ?
C20 C21 C27 C28 -118.9(3) . . . . ?
C22 C21 C27 C28 60.5(3) . . . . ?
C20 C21 C27 C29 117.8(3) . . . . ?
C22 C21 C27 C29 -62.8(3) . . . . ?
C24 C25 C26 C30 70.9(3) . . . . ?
C20 C25 C26 C30 -109.4(2) . . . . ?
C24 C25 C26 C31 -53.4(3) . . . . ?
C20 C25 C26 C31 126.4(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.52
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.343
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_sg456_0m
_database_code_depnum_ccdc_archive 'CCDC 1040545'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H47 Cl N3 Ni O2'
_chemical_formula_weight         683.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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                   9.7349(5)
_cell_length_b                   12.3308(7)
_cell_length_c                   15.6197(8)
_cell_angle_alpha                87.490(3)
_cell_angle_beta                 75.776(2)
_cell_angle_gamma                85.562(3)
_cell_volume                     1811.45(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plates
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             726
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9093
_exptl_absorpt_correction_T_max  0.9809
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49443
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         28.52
_reflns_number_total             8948
_reflns_number_gt                7875
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0631P)²+3.0932P] 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         8948
_refine_ls_number_parameters     415
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1307
_refine_ls_wR_factor_gt          0.1257
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.86808(3) 0.82359(2) 0.728542(17) 0.01058(8) Uani 1 1 d . . .
Cl1 Cl 1.07001(6) 0.87518(5) 0.74443(4) 0.02301(13) Uani 1 1 d . . .
O2 O 0.6395(2) 0.72402(15) 0.35413(13) 0.0308(4) Uani 1 1 d . . .
N2 N 0.69631(18) 0.82118(14) 0.69695(11) 0.0117(3) Uani 1 1 d . . .
O1 O 0.4184(5) 0.5575(4) 0.8163(3) 0.1113(14) Uiso 1 1 d D . .
C1 C 0.5740(2) 0.85088(17) 0.75687(14) 0.0129(4) Uani 1 1 d . . .
C2 C 0.6040(2) 0.88739(17) 0.83654(14) 0.0130(4) Uani 1 1 d . . .
H2 H 0.5322 0.9203 0.8825 0.016 Uiso 1 1 calc R . .
N3 N 0.73628(18) 0.87229(14) 0.84146(11) 0.0125(3) Uani 1 1 d . . .
C4 C 0.7727(2) 0.91117(17) 0.91774(13) 0.0126(4) Uani 1 1 d . . .
C5 C 0.8315(2) 0.83489(18) 0.97110(14) 0.0150(4) Uani 1 1 d . . .
C6 C 0.8593(2) 0.87193(19) 1.04792(14) 0.0174(4) Uani 1 1 d . . .
H6 H 0.8959 0.8215 1.0859 0.021 Uiso 1 1 calc R . .
C7 C 0.8349(2) 0.98032(19) 1.07019(14) 0.0178(4) Uani 1 1 d . . .
H7 H 0.8533 1.0036 1.1232 0.021 Uiso 1 1 calc R . .
C8 C 0.7833(2) 1.05481(18) 1.01443(14) 0.0166(4) Uani 1 1 d . . .
H8 H 0.7689 1.1294 1.0292 0.020 Uiso 1 1 calc R . .
C9 C 0.7521(2) 1.02254(18) 0.93710(14) 0.0138(4) Uani 1 1 d . . .
C10 C 0.7081(2) 1.10976(18) 0.87483(14) 0.0159(4) Uani 1 1 d . . .
H10 H 0.6929 1.0727 0.8225 0.019 Uiso 1 1 calc R . .
C11 C 0.8268(3) 1.1876(2) 0.84171(16) 0.0246(5) Uani 1 1 d . . .
H11A H 0.8418 1.2264 0.8918 0.037 Uiso 1 1 calc R . .
H11B H 0.7996 1.2403 0.7989 0.037 Uiso 1 1 calc R . .
H11C H 0.9148 1.1459 0.8133 0.037 Uiso 1 1 calc R . .
C12 C 0.5687(3) 1.1731(2) 0.91890(16) 0.0237(5) Uani 1 1 d . . .
H12A H 0.4927 1.1229 0.9360 0.036 Uiso 1 1 calc R . .
H12B H 0.5441 1.2286 0.8773 0.036 Uiso 1 1 calc R . .
H12C H 0.5802 1.2083 0.9715 0.036 Uiso 1 1 calc R . .
C13 C 0.8648(2) 0.71579(18) 0.94778(15) 0.0185(4) Uani 1 1 d . . .
H13 H 0.8450 0.7062 0.8888 0.022 Uiso 1 1 calc R . .
C14 C 0.7713(3) 0.6422(2) 1.01486(19) 0.0311(6) Uani 1 1 d . . .
H14A H 0.7902 0.6494 1.0731 0.047 Uiso 1 1 calc R . .
H14B H 0.7925 0.5665 0.9967 0.047 Uiso 1 1 calc R . .
H14C H 0.6712 0.6635 1.0180 0.047 Uiso 1 1 calc R . .
C16 C 0.4428(2) 0.83927(18) 0.73881(14) 0.0160(4) Uani 1 1 d . . .
H16 H 0.3573 0.8618 0.7801 0.019 Uiso 1 1 calc R . .
C17 C 0.4386(2) 0.79411(19) 0.65931(15) 0.0182(4) Uani 1 1 d . . .
H17 H 0.3499 0.7875 0.6455 0.022 Uiso 1 1 calc R . .
C18 C 0.5647(2) 0.75864(19) 0.60008(15) 0.0174(4) Uani 1 1 d . . .
H18 H 0.5632 0.7267 0.5461 0.021 Uiso 1 1 calc R . .
C19 C 0.6928(2) 0.77122(17) 0.62191(14) 0.0133(4) Uani 1 1 d . . .
C20 C 0.8340(2) 0.73042(17) 0.57692(14) 0.0134(4) Uani 1 1 d . . .
H20 H 0.8542 0.7004 0.5198 0.016 Uiso 1 1 calc R . .
C22 C 1.0732(2) 0.69359(17) 0.58010(13) 0.0125(4) Uani 1 1 d . . .
C23 C 1.1139(2) 0.58930(17) 0.60925(14) 0.0156(4) Uani 1 1 d . . .
C24 C 1.2492(2) 0.54394(19) 0.56872(16) 0.0197(4) Uani 1 1 d . . .
H24 H 1.2792 0.4731 0.5863 0.024 Uiso 1 1 calc R . .
C25 C 1.3400(2) 0.6015(2) 0.50296(16) 0.0206(5) Uani 1 1 d . . .
H25 H 1.4309 0.5693 0.4751 0.025 Uiso 1 1 calc R . .
C26 C 1.2987(2) 0.70544(19) 0.47779(15) 0.0181(4) Uani 1 1 d . . .
H26 H 1.3629 0.7444 0.4336 0.022 Uiso 1 1 calc R . .
C27 C 1.1648(2) 0.75427(17) 0.51594(14) 0.0141(4) Uani 1 1 d . . .
C28 C 1.1232(2) 0.86889(18) 0.48667(14) 0.0156(4) Uani 1 1 d . . .
H28 H 1.0286 0.8924 0.5256 0.019 Uiso 1 1 calc R . .
C29 C 1.2302(3) 0.9492(2) 0.49698(17) 0.0230(5) Uani 1 1 d . . .
H29A H 1.2360 0.9485 0.5588 0.035 Uiso 1 1 calc R . .
H29B H 1.1992 1.0226 0.4796 0.035 Uiso 1 1 calc R . .
H29C H 1.3238 0.9279 0.4592 0.035 Uiso 1 1 calc R . .
C30 C 1.1080(3) 0.8711(2) 0.39125(16) 0.0238(5) Uani 1 1 d . . .
H30A H 1.1997 0.8487 0.3517 0.036 Uiso 1 1 calc R . .
H30B H 1.0775 0.9450 0.3747 0.036 Uiso 1 1 calc R . .
H30C H 1.0372 0.8209 0.3863 0.036 Uiso 1 1 calc R . .
C31 C 1.0119(2) 0.52638(18) 0.67974(15) 0.0192(4) Uani 1 1 d . . .
H31 H 0.9332 0.5790 0.7096 0.023 Uiso 1 1 calc R . .
C32 C 1.0821(3) 0.4746(3) 0.75013(19) 0.0378(7) Uani 1 1 d . . .
H32A H 1.1566 0.4197 0.7232 0.057 Uiso 1 1 calc R . .
H32B H 1.0107 0.4400 0.7965 0.057 Uiso 1 1 calc R . .
H32C H 1.1241 0.5308 0.7760 0.057 Uiso 1 1 calc R . .
C33 C 0.9465(4) 0.4405(3) 0.6381(2) 0.0404(7) Uani 1 1 d . . .
H33A H 0.9011 0.4752 0.5934 0.061 Uiso 1 1 calc R . .
H33B H 0.8752 0.4050 0.6839 0.061 Uiso 1 1 calc R . .
H33C H 1.0209 0.3861 0.6102 0.061 Uiso 1 1 calc R . .
C34 C 0.5166(6) 0.5763(5) 0.8919(4) 0.0567(14) Uiso 0.779(7) 1 d P A 1
C35 C 0.6079(4) 0.4375(3) 0.7842(3) 0.0325(9) Uiso 0.779(7) 1 d P A 1
C36 C 0.6336(6) 0.4900(5) 0.8572(4) 0.0529(13) Uiso 0.779(7) 1 d P A 1
C50 C 0.5250(7) 0.5131(5) 0.7427(4) 0.0647(15) Uiso 0.779(7) 1 d P A 1
C55 C 0.4058(11) 0.6069(9) 0.8840(7) 0.020(3) Uiso 0.221(7) 1 d P A 2
C54 C 0.5435(15) 0.6324(12) 0.8921(9) 0.032(3) Uiso 0.221(7) 1 d P A 2
C53 C 0.6436(16) 0.5546(13) 0.8362(10) 0.039(4) Uiso 0.221(7) 1 d P A 2
C52 C 0.5793(14) 0.5192(12) 0.7678(10) 0.039(4) Uiso 0.221(7) 1 d PD A 2
C37 C 0.7316(3) 0.8088(2) 0.3557(2) 0.0342(6) Uani 1 1 d . . .
H37A H 0.8241 0.7950 0.3126 0.041 Uiso 1 1 calc R . .
H37B H 0.7487 0.8136 0.4153 0.041 Uiso 1 1 calc R . .
C38 C 0.5866(3) 0.7497(2) 0.27719(18) 0.0282(5) Uani 1 1 d . . .
H38A H 0.4945 0.7176 0.2830 0.034 Uiso 1 1 calc R . .
H38B H 0.6547 0.7209 0.2237 0.034 Uiso 1 1 calc R . .
C39 C 0.5684(3) 0.8728(2) 0.27088(18) 0.0267(5) Uani 1 1 d . . .
H39A H 0.4672 0.8986 0.2915 0.032 Uiso 1 1 calc R . .
H39B H 0.6047 0.8994 0.2093 0.032 Uiso 1 1 calc R . .
C40 C 0.6561(3) 0.9117(2) 0.3314(2) 0.0354(6) Uani 1 1 d . . .
H40A H 0.7245 0.9641 0.2998 0.042 Uiso 1 1 calc R . .
H40B H 0.5940 0.9464 0.3844 0.042 Uiso 1 1 calc R . .
N1 N 0.93192(18) 0.73761(14) 0.62003(11) 0.0118(3) Uani 1 1 d . . .
C51 C 1.0221(3) 0.6819(2) 0.9408(2) 0.0316(6) Uani 1 1 d . . .
H51A H 1.0812 0.7276 0.8957 0.047 Uiso 1 1 calc R . .
H51B H 1.0416 0.6055 0.9243 0.047 Uiso 1 1 calc R . .
H51C H 1.0440 0.6911 0.9979 0.047 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 N2 1.8588(17) . ?
Ni1 N1 1.9801(17) . ?
Ni1 N3 1.9947(17) . ?
Ni1 Cl1 2.1857(6) . ?
O2 C38 1.434(3) . ?
O2 C37 1.434(3) . ?
N2 C19 1.357(3) . ?
N2 C1 1.358(3) . ?
O1 C55 1.219(11) . ?
O1 C50 1.442(7) . ?
O1 C52 1.608(13) . ?
O1 C34 1.725(7) . ?
C1 C16 1.393(3) . ?
C1 C2 1.444(3) . ?
C2 N3 1.307(3) . ?
C2 H2 0.9500 . ?
N3 C4 1.435(3) . ?
C4 C9 1.408(3) . ?
C4 C5 1.410(3) . ?
C5 C6 1.396(3) . ?
C5 C13 1.520(3) . ?
C6 C7 1.384(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.397(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.526(3) . ?
C10 C12 1.533(3) . ?
C10 C11 1.536(3) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.525(3) . ?
C13 C51 1.535(3) . ?
C13 H13 1.0000 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C16 C17 1.394(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.396(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.393(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.444(3) . ?
C20 N1 1.305(3) . ?
C20 H20 0.9500 . ?
C22 C27 1.399(3) . ?
C22 C23 1.406(3) . ?
C22 N1 1.438(3) . ?
C23 C24 1.398(3) . ?
C23 C31 1.519(3) . ?
C24 C25 1.388(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.383(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.395(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.522(3) . ?
C28 C30 1.532(3) . ?
C28 C29 1.533(3) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C33 1.523(4) . ?
C31 C32 1.525(4) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.511(8) . ?
C35 C36 1.418(6) . ?
C35 C50 1.425(8) . ?
C55 C54 1.436(18) . ?
C54 C53 1.46(2) . ?
C53 C52 1.46(2) . ?
C37 C40 1.499(4) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.516(4) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.533(4) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Ni1 N1 80.45(7) . . ?
N2 Ni1 N3 80.71(7) . . ?
N1 Ni1 N3 156.13(7) . . ?
N2 Ni1 Cl1 162.26(6) . . ?
N1 Ni1 Cl1 101.24(5) . . ?
N3 Ni1 Cl1 101.18(5) . . ?
C38 O2 C37 104.13(19) . . ?
C19 N2 C1 120.52(18) . . ?
C19 N2 Ni1 119.29(14) . . ?
C1 N2 Ni1 119.04(14) . . ?
C55 O1 C50 141.4(7) . . ?
C55 O1 C52 114.6(9) . . ?
C50 O1 C52 27.5(6) . . ?
C55 O1 C34 41.7(6) . . ?
C50 O1 C34 102.2(4) . . ?
C52 O1 C34 74.7(7) . . ?
N2 C1 C16 120.51(19) . . ?
N2 C1 C2 110.60(18) . . ?
C16 C1 C2 128.82(19) . . ?
N3 C2 C1 115.73(18) . . ?
N3 C2 H2 122.1 . . ?
C1 C2 H2 122.1 . . ?
C2 N3 C4 117.87(17) . . ?
C2 N3 Ni1 113.24(14) . . ?
C4 N3 Ni1 127.68(13) . . ?
C9 C4 C5 121.58(19) . . ?
C9 C4 N3 120.44(18) . . ?
C5 C4 N3 117.97(19) . . ?
C6 C5 C4 117.8(2) . . ?
C6 C5 C13 119.76(19) . . ?
C4 C5 C13 122.47(19) . . ?
C7 C6 C5 121.6(2) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C6 C7 C8 119.5(2) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C7 C8 C9 121.5(2) . . ?
C7 C8 H8 119.2 . . ?
C9 C8 H8 119.2 . . ?
C8 C9 C4 117.84(19) . . ?
C8 C9 C10 118.74(19) . . ?
C4 C9 C10 123.27(19) . . ?
C9 C10 C12 111.69(18) . . ?
C9 C10 C11 110.41(18) . . ?
C12 C10 C11 110.5(2) . . ?
C9 C10 H10 108.0 . . ?
C12 C10 H10 108.0 . . ?
C11 C10 H10 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C5 C13 C14 111.49(19) . . ?
C5 C13 C51 110.9(2) . . ?
C14 C13 C51 110.1(2) . . ?
C5 C13 H13 108.1 . . ?
C14 C13 H13 108.1 . . ?
C51 C13 H13 108.1 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C1 C16 C17 119.1(2) . . ?
C1 C16 H16 120.4 . . ?
C17 C16 H16 120.4 . . ?
C16 C17 C18 119.9(2) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C17 118.5(2) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
N2 C19 C18 121.12(19) . . ?
N2 C19 C20 110.24(18) . . ?
C18 C19 C20 128.50(19) . . ?
N1 C20 C19 115.45(18) . . ?
N1 C20 H20 122.3 . . ?
C19 C20 H20 122.3 . . ?
C27 C22 C23 122.52(19) . . ?
C27 C22 N1 120.31(18) . . ?
C23 C22 N1 117.16(18) . . ?
C24 C23 C22 117.7(2) . . ?
C24 C23 C31 121.2(2) . . ?
C22 C23 C31 120.98(19) . . ?
C25 C24 C23 120.6(2) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C24 120.4(2) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 121.3(2) . . ?
C25 C26 H26 119.3 . . ?
C27 C26 H26 119.3 . . ?
C26 C27 C22 117.4(2) . . ?
C26 C27 C28 119.88(19) . . ?
C22 C27 C28 122.71(18) . . ?
C27 C28 C30 110.97(18) . . ?
C27 C28 C29 111.21(18) . . ?
C30 C28 C29 110.64(19) . . ?
C27 C28 H28 108.0 . . ?
C30 C28 H28 108.0 . . ?
C29 C28 H28 108.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C23 C31 C33 110.6(2) . . ?
C23 C31 C32 112.4(2) . . ?
C33 C31 C32 110.5(2) . . ?
C23 C31 H31 107.7 . . ?
C33 C31 H31 107.7 . . ?
C32 C31 H31 107.7 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 O1 96.3(4) . . ?
C36 C35 C50 107.2(4) . . ?
C35 C36 C34 111.0(4) . . ?
C35 C50 O1 103.0(5) . . ?
O1 C55 C54 109.5(10) . . ?
C55 C54 C53 105.0(12) . . ?
C52 C53 C54 108.9(12) . . ?
C53 C52 O1 96.2(10) . . ?
O2 C37 C40 105.7(2) . . ?
O2 C37 H37A 110.6 . . ?
C40 C37 H37A 110.6 . . ?
O2 C37 H37B 110.6 . . ?
C40 C37 H37B 110.6 . . ?
H37A C37 H37B 108.7 . . ?
O2 C38 C39 106.3(2) . . ?
O2 C38 H38A 110.5 . . ?
C39 C38 H38A 110.5 . . ?
O2 C38 H38B 110.5 . . ?
C39 C38 H38B 110.5 . . ?
H38A C38 H38B 108.7 . . ?
C38 C39 C40 104.4(2) . . ?
C38 C39 H39A 110.9 . . ?
C40 C39 H39A 110.9 . . ?
C38 C39 H39B 110.9 . . ?
C40 C39 H39B 110.9 . . ?
H39A C39 H39B 108.9 . . ?
C37 C40 C39 103.2(2) . . ?
C37 C40 H40A 111.1 . . ?
C39 C40 H40A 111.1 . . ?
C37 C40 H40B 111.1 . . ?
C39 C40 H40B 111.1 . . ?
H40A C40 H40B 109.1 . . ?
C20 N1 C22 117.81(17) . . ?
C20 N1 Ni1 113.93(14) . . ?
C22 N1 Ni1 127.91(13) . . ?
C13 C51 H51A 109.5 . . ?
C13 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C13 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 N2 C19 -1.92(15) . . . . ?
N3 Ni1 N2 C19 -167.19(17) . . . . ?
Cl1 Ni1 N2 C19 95.1(2) . . . . ?
N1 Ni1 N2 C1 165.86(17) . . . . ?
N3 Ni1 N2 C1 0.59(15) . . . . ?
Cl1 Ni1 N2 C1 -97.1(2) . . . . ?
C19 N2 C1 C16 -5.7(3) . . . . ?
Ni1 N2 C1 C16 -173.28(16) . . . . ?
C19 N2 C1 C2 171.48(18) . . . . ?
Ni1 N2 C1 C2 3.9(2) . . . . ?
N2 C1 C2 N3 -8.5(3) . . . . ?
C16 C1 C2 N3 168.3(2) . . . . ?
C1 C2 N3 C4 177.53(18) . . . . ?
C1 C2 N3 Ni1 9.1(2) . . . . ?
N2 Ni1 N3 C2 -5.46(15) . . . . ?
N1 Ni1 N3 C2 -43.7(3) . . . . ?
Cl1 Ni1 N3 C2 156.61(14) . . . . ?
N2 Ni1 N3 C4 -172.49(18) . . . . ?
N1 Ni1 N3 C4 149.23(18) . . . . ?
Cl1 Ni1 N3 C4 -10.42(17) . . . . ?
C2 N3 C4 C9 -60.4(3) . . . . ?
Ni1 N3 C4 C9 106.1(2) . . . . ?
C2 N3 C4 C5 120.7(2) . . . . ?
Ni1 N3 C4 C5 -72.8(2) . . . . ?
C9 C4 C5 C6 4.6(3) . . . . ?
N3 C4 C5 C6 -176.45(18) . . . . ?
C9 C4 C5 C13 -175.4(2) . . . . ?
N3 C4 C5 C13 3.5(3) . . . . ?
C4 C5 C6 C7 -2.1(3) . . . . ?
C13 C5 C6 C7 177.9(2) . . . . ?
C5 C6 C7 C8 -0.9(3) . . . . ?
C6 C7 C8 C9 1.5(3) . . . . ?
C7 C8 C9 C4 0.9(3) . . . . ?
C7 C8 C9 C10 -174.8(2) . . . . ?
C5 C4 C9 C8 -4.1(3) . . . . ?
N3 C4 C9 C8 177.07(18) . . . . ?
C5 C4 C9 C10 171.39(19) . . . . ?
N3 C4 C9 C10 -7.5(3) . . . . ?
C8 C9 C10 C12 -63.1(3) . . . . ?
C4 C9 C10 C12 121.5(2) . . . . ?
C8 C9 C10 C11 60.3(3) . . . . ?
C4 C9 C10 C11 -115.1(2) . . . . ?
C6 C5 C13 C14 65.7(3) . . . . ?
C4 C5 C13 C14 -114.3(2) . . . . ?
C6 C5 C13 C51 -57.3(3) . . . . ?
C4 C5 C13 C51 122.7(2) . . . . ?
N2 C1 C16 C17 1.6(3) . . . . ?
C2 C1 C16 C17 -174.9(2) . . . . ?
C1 C16 C17 C18 1.7(3) . . . . ?
C16 C17 C18 C19 -1.0(3) . . . . ?
C1 N2 C19 C18 6.4(3) . . . . ?
Ni1 N2 C19 C18 173.95(16) . . . . ?
C1 N2 C19 C20 -169.74(18) . . . . ?
Ni1 N2 C19 C20 -2.1(2) . . . . ?
C17 C18 C19 N2 -3.0(3) . . . . ?
C17 C18 C19 C20 172.3(2) . . . . ?
N2 C19 C20 N1 7.4(3) . . . . ?
C18 C19 C20 N1 -168.4(2) . . . . ?
C27 C22 C23 C24 -3.1(3) . . . . ?
N1 C22 C23 C24 177.75(19) . . . . ?
C27 C22 C23 C31 179.4(2) . . . . ?
N1 C22 C23 C31 0.2(3) . . . . ?
C22 C23 C24 C25 1.0(3) . . . . ?
C31 C23 C24 C25 178.5(2) . . . . ?
C23 C24 C25 C26 1.2(4) . . . . ?
C24 C25 C26 C27 -1.4(4) . . . . ?
C25 C26 C27 C22 -0.6(3) . . . . ?
C25 C26 C27 C28 179.9(2) . . . . ?
C23 C22 C27 C26 2.9(3) . . . . ?
N1 C22 C27 C26 -177.97(19) . . . . ?
C23 C22 C27 C28 -177.6(2) . . . . ?
N1 C22 C27 C28 1.5(3) . . . . ?
C26 C27 C28 C30 67.8(3) . . . . ?
C22 C27 C28 C30 -111.6(2) . . . . ?
C26 C27 C28 C29 -55.8(3) . . . . ?
C22 C27 C28 C29 124.7(2) . . . . ?
C24 C23 C31 C33 -76.1(3) . . . . ?
C22 C23 C31 C33 101.3(3) . . . . ?
C24 C23 C31 C32 47.9(3) . . . . ?
C22 C23 C31 C32 -134.6(2) . . . . ?
C55 O1 C34 C36 170.6(9) . . . . ?
C50 O1 C34 C36 -25.5(5) . . . . ?
C52 O1 C34 C36 -26.6(7) . . . . ?
C50 C35 C36 C34 27.3(6) . . . . ?
O1 C34 C36 C35 -0.4(5) . . . . ?
C36 C35 C50 O1 -45.2(6) . . . . ?
C55 O1 C50 C35 59.6(12) . . . . ?
C52 O1 C50 C35 44.7(13) . . . . ?
C34 O1 C50 C35 42.4(5) . . . . ?
C50 O1 C55 C54 2.4(16) . . . . ?
C52 O1 C55 C54 9.9(13) . . . . ?
C34 O1 C55 C54 28.1(7) . . . . ?
O1 C55 C54 C53 -21.3(14) . . . . ?
C55 C54 C53 C52 25.1(16) . . . . ?
C54 C53 C52 O1 -18.0(14) . . . . ?
C55 O1 C52 C53 5.4(13) . . . . ?
C50 O1 C52 C53 175(2) . . . . ?
C34 O1 C52 C53 -7.0(8) . . . . ?
C38 O2 C37 C40 41.4(3) . . . . ?
C37 O2 C38 C39 -35.9(3) . . . . ?
O2 C38 C39 C40 16.7(3) . . . . ?
O2 C37 C40 C39 -29.9(3) . . . . ?
C38 C39 C40 C37 7.8(3) . . . . ?
C19 C20 N1 C22 177.17(18) . . . . ?
C19 C20 N1 Ni1 -9.0(2) . . . . ?
C27 C22 N1 C20 81.9(2) . . . . ?
C23 C22 N1 C20 -98.9(2) . . . . ?
C27 C22 N1 Ni1 -90.9(2) . . . . ?
C23 C22 N1 Ni1 88.3(2) . . . . ?
N2 Ni1 N1 C20 6.11(15) . . . . ?
N3 Ni1 N1 C20 44.4(3) . . . . ?
Cl1 Ni1 N1 C20 -155.94(14) . . . . ?
N2 Ni1 N1 C22 179.16(18) . . . . ?
N3 Ni1 N1 C22 -142.53(18) . . . . ?
Cl1 Ni1 N1 C22 17.11(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        28.52
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         1.297
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_sg224_0m_new
_database_code_depnum_ccdc_archive 'CCDC 1040546'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H47 Br N3 Ni O2'
_chemical_formula_weight         728.42

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'
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'
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'
H H 0.0000 0.0000 '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                   9.8908(13)
_cell_length_b                   12.3807(14)
_cell_length_c                   15.5767(18)
_cell_angle_alpha                86.987(3)
_cell_angle_beta                 75.727(5)
_cell_angle_gamma                85.167(4)
_cell_volume                     1841.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plates
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             762
_exptl_absorpt_coefficient_mu    1.648
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7340
_exptl_absorpt_correction_T_max  0.9221
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25276
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         24.50
_reflns_number_total             5897
_reflns_number_gt                4854
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0449P)²+3.5481P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5897
_refine_ls_number_parameters     393
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.046
_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
Br1 Br 1.07720(4) 0.87505(3) 0.74596(2) 0.02770(13) Uani 1 1 d . . .
Ni1 Ni 0.86844(4) 0.82027(3) 0.72857(2) 0.01049(12) Uani 1 1 d . . .
N2 N 0.9332(3) 0.7356(2) 0.61961(17) 0.0117(6) Uani 1 1 d . . .
C1 C 0.6977(3) 0.7697(3) 0.6202(2) 0.0128(7) Uani 1 1 d . . .
C5 C 0.5784(3) 0.8492(2) 0.7553(2) 0.0117(7) Uani 1 1 d . . .
N1 N 0.7007(3) 0.8196(2) 0.69570(16) 0.0112(6) Uani 1 1 d . . .
C4 C 0.4508(3) 0.8386(3) 0.7363(2) 0.0156(7) Uani 1 1 d . . .
H4 H 0.3662 0.8617 0.7770 0.019 Uiso 1 1 calc R . .
C3 C 0.4478(4) 0.7937(3) 0.6566(2) 0.0185(8) Uani 1 1 d . . .
H3 H 0.3611 0.7872 0.6421 0.022 Uiso 1 1 calc R . .
C2 C 0.5734(4) 0.7582(3) 0.5981(2) 0.0176(8) Uani 1 1 d . . .
H2 H 0.5729 0.7266 0.5439 0.021 Uiso 1 1 calc R . .
C28 C 0.7517(3) 1.0189(3) 0.9373(2) 0.0145(7) Uani 1 1 d . . .
C27 C 0.7823(4) 1.0495(3) 1.0146(2) 0.0173(8) Uani 1 1 d . . .
H27 H 0.7683 1.1238 1.0295 0.021 Uiso 1 1 calc R . .
C26 C 0.8323(4) 0.9751(3) 1.0702(2) 0.0201(8) Uani 1 1 d . . .
H26 H 0.8501 0.9978 1.1234 0.024 Uiso 1 1 calc R . .
C25 C 0.8568(4) 0.8672(3) 1.0484(2) 0.0180(8) Uani 1 1 d . . .
H25 H 0.8930 0.8167 1.0866 0.022 Uiso 1 1 calc R . .
C21 C 0.8294(3) 0.8312(3) 0.9718(2) 0.0144(7) Uani 1 1 d . . .
C22 C 0.8625(4) 0.7122(3) 0.9490(2) 0.0193(8) Uani 1 1 d . . .
H22 H 0.8501 0.7041 0.8879 0.023 Uiso 1 1 calc R . .
C23 C 1.0137(5) 0.6737(3) 0.9491(3) 0.0369(10) Uani 1 1 d . . .
H23A H 1.0776 0.7208 0.9090 0.055 Uiso 1 1 calc R . .
H23B H 1.0333 0.5990 0.9291 0.055 Uiso 1 1 calc R . .
H23C H 1.0269 0.6765 1.0092 0.055 Uiso 1 1 calc R . .
C24 C 0.7609(5) 0.6409(3) 1.0126(3) 0.0383(11) Uani 1 1 d . . .
H24A H 0.7690 0.6490 1.0734 0.058 Uiso 1 1 calc R . .
H24B H 0.7836 0.5649 0.9965 0.058 Uiso 1 1 calc R . .
H24C H 0.6650 0.6630 1.0088 0.058 Uiso 1 1 calc R . .
C29 C 0.7092(4) 1.1064(3) 0.8747(2) 0.0170(8) Uani 1 1 d . . .
H29 H 0.6964 1.0700 0.8217 0.020 Uiso 1 1 calc R . .
C31 C 0.5698(4) 1.1685(3) 0.9177(2) 0.0247(8) Uani 1 1 d . . .
H31A H 0.4965 1.1176 0.9356 0.037 Uiso 1 1 calc R . .
H31B H 0.5446 1.2227 0.8750 0.037 Uiso 1 1 calc R . .
H31C H 0.5796 1.2049 0.9700 0.037 Uiso 1 1 calc R . .
C30 C 0.8249(4) 1.1842(3) 0.8427(2) 0.0252(9) Uani 1 1 d . . .
H30A H 0.8396 1.2209 0.8936 0.038 Uiso 1 1 calc R . .
H30B H 0.7974 1.2383 0.8007 0.038 Uiso 1 1 calc R . .
H30C H 0.9118 1.1434 0.8134 0.038 Uiso 1 1 calc R . .
C7 C 0.8371(3) 0.7295(2) 0.5763(2) 0.0123(7) Uani 1 1 d . . .
H7 H 0.8579 0.7002 0.5190 0.015 Uiso 1 1 calc R . .
C13 C 1.1644(3) 0.7535(3) 0.5167(2) 0.0136(7) Uani 1 1 d . . .
C12 C 1.2967(4) 0.7048(3) 0.4799(2) 0.0189(8) Uani 1 1 d . . .
H12 H 1.3606 0.7438 0.4360 0.023 Uiso 1 1 calc R . .
C11 C 1.3373(4) 0.6015(3) 0.5056(2) 0.0221(8) Uani 1 1 d . . .
H11 H 1.4275 0.5697 0.4785 0.027 Uiso 1 1 calc R . .
C10 C 1.2476(4) 0.5438(3) 0.5706(2) 0.0197(8) Uani 1 1 d . . .
H10 H 1.2776 0.4731 0.5886 0.024 Uiso 1 1 calc R . .
C9 C 1.1133(4) 0.5882(3) 0.6101(2) 0.0154(7) Uani 1 1 d . . .
C8 C 1.0730(3) 0.6918(3) 0.5802(2) 0.0120(7) Uani 1 1 d . . .
C17 C 1.0124(4) 0.5249(3) 0.6808(2) 0.0207(8) Uani 1 1 d . . .
H17 H 0.9337 0.5772 0.7096 0.025 Uiso 1 1 calc R . .
C19 C 1.0797(5) 0.4752(4) 0.7528(3) 0.0434(12) Uani 1 1 d . . .
H19A H 1.0098 0.4386 0.7982 0.065 Uiso 1 1 calc R . .
H19B H 1.1162 0.5324 0.7800 0.065 Uiso 1 1 calc R . .
H19C H 1.1566 0.4224 0.7268 0.065 Uiso 1 1 calc R . .
C18 C 0.9505(5) 0.4390(4) 0.6397(3) 0.0445(12) Uani 1 1 d . . .
H18A H 0.9112 0.4722 0.5918 0.067 Uiso 1 1 calc R . .
H18B H 0.8765 0.4065 0.6849 0.067 Uiso 1 1 calc R . .
H18C H 1.0238 0.3827 0.6157 0.067 Uiso 1 1 calc R . .
C14 C 1.1224(4) 0.8674(3) 0.4867(2) 0.0163(7) Uani 1 1 d . . .
H14 H 1.0302 0.8914 0.5266 0.020 Uiso 1 1 calc R . .
C16 C 1.1041(4) 0.8690(3) 0.3922(2) 0.0254(9) Uani 1 1 d . . .
H16A H 1.1937 0.8469 0.3516 0.038 Uiso 1 1 calc R . .
H16B H 1.0726 0.9425 0.3754 0.038 Uiso 1 1 calc R . .
H16C H 1.0344 0.8187 0.3889 0.038 Uiso 1 1 calc R . .
C15 C 1.2287(4) 0.9480(3) 0.4938(2) 0.0223(8) Uani 1 1 d . . .
H15A H 1.2393 0.9464 0.5548 0.033 Uiso 1 1 calc R . .
H15B H 1.1954 1.0213 0.4777 0.033 Uiso 1 1 calc R . .
H15C H 1.3192 0.9278 0.4535 0.033 Uiso 1 1 calc R . .
C37 C 0.4358(4) 0.1276(3) 0.7259(3) 0.0274(9) Uiso 1 1 d . . .
H37A H 0.4005 0.0990 0.7873 0.033 Uiso 1 1 calc R . .
H37B H 0.5364 0.1044 0.7054 0.033 Uiso 1 1 calc R . .
C34 C 0.3525(4) 0.0891(3) 0.6640(3) 0.0325(10) Uiso 1 1 d . . .
H34A H 0.4156 0.0601 0.6091 0.039 Uiso 1 1 calc R . .
H34B H 0.2905 0.0324 0.6935 0.039 Uiso 1 1 calc R . .
O1 O 0.3555(3) 0.2761(2) 0.64577(18) 0.0343(7) Uiso 1 1 d . . .
N3 N 0.7360(3) 0.8694(2) 0.84145(16) 0.0112(6) Uani 1 1 d . . .
C6 C 0.6077(3) 0.8850(2) 0.8352(2) 0.0123(7) Uani 1 1 d . . .
H6 H 0.5366 0.9182 0.8808 0.015 Uiso 1 1 calc R . .
C20 C 0.7720(3) 0.9077(3) 0.9183(2) 0.0126(7) Uani 1 1 d . . .
C32 C 0.4118(4) 0.2502(3) 0.7208(3) 0.0312(9) Uiso 1 1 d . . .
H32A H 0.3454 0.2766 0.7754 0.037 Uiso 1 1 calc R . .
H32B H 0.5010 0.2844 0.7138 0.037 Uiso 1 1 calc R . .
C35 C 0.2696(5) 0.1892(3) 0.6443(3) 0.0352(10) Uiso 1 1 d . . .
H35A H 0.2493 0.1860 0.5854 0.042 Uiso 1 1 calc R . .
H35B H 0.1801 0.1986 0.6897 0.042 Uiso 1 1 calc R . .
C41 C 0.5143(14) 0.5141(9) 0.7423(7) 0.083(3) Uiso 0.70 1 d P A 1
O2 O 0.6055(6) 0.4379(5) 0.7823(4) 0.0723(16) Uiso 0.70 1 d P A 1
C39 C 0.6277(9) 0.4880(7) 0.8574(6) 0.063(2) Uiso 0.70 1 d P A 1
C40 C 0.4138(9) 0.5627(8) 0.8202(7) 0.055(3) Uiso 0.70 1 d P A 1
C38 C 0.5127(10) 0.5720(7) 0.8919(5) 0.060(2) Uiso 0.70 1 d P A 1
C83 C 0.6440(18) 0.5537(14) 0.8334(11) 0.048(4) Uiso 0.30 1 d P B 2
C80 C 0.4295(19) 0.5378(14) 0.7906(13) 0.035(4) Uiso 0.30 1 d P B 2
C84 C 0.583(2) 0.5194(16) 0.7541(13) 0.055(5) Uiso 0.30 1 d P B 2
O10 O 0.4113(15) 0.6032(11) 0.8785(10) 0.071(4) Uiso 0.30 1 d P B 2
C82 C 0.5375(16) 0.6317(13) 0.8890(9) 0.036(3) Uiso 0.30 1 d P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Ni1 2.3081(6) . ?
Ni1 N1 1.854(3) . ?
Ni1 N2 1.982(2) . ?
Ni1 N3 2.005(3) . ?
N2 C7 1.303(4) . ?
N2 C8 1.440(4) . ?
C1 N1 1.364(4) . ?
C1 C2 1.376(5) . ?
C1 C7 1.440(4) . ?
C5 N1 1.366(4) . ?
C5 C4 1.384(5) . ?
C5 C6 1.445(4) . ?
C4 C3 1.395(5) . ?
C4 H4 0.9500 . ?
C3 C2 1.399(5) . ?
C3 H3 0.9500 . ?
C2 H2 0.9500 . ?
C28 C27 1.391(5) . ?
C28 C20 1.411(5) . ?
C28 C29 1.522(5) . ?
C27 C26 1.376(5) . ?
C27 H27 0.9500 . ?
C26 C25 1.381(5) . ?
C26 H26 0.9500 . ?
C25 C21 1.390(5) . ?
C25 H25 0.9500 . ?
C21 C20 1.404(5) . ?
C21 C22 1.523(5) . ?
C22 C24 1.529(5) . ?
C22 C23 1.531(5) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C29 C30 1.530(5) . ?
C29 C31 1.537(5) . ?
C29 H29 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C7 H7 0.9500 . ?
C13 C12 1.392(5) . ?
C13 C8 1.406(5) . ?
C13 C14 1.519(5) . ?
C12 C11 1.377(5) . ?
C12 H12 0.9500 . ?
C11 C10 1.381(5) . ?
C11 H11 0.9500 . ?
C10 C9 1.399(5) . ?
C10 H10 0.9500 . ?
C9 C8 1.401(5) . ?
C9 C17 1.524(5) . ?
C17 C18 1.514(5) . ?
C17 C19 1.519(5) . ?
C17 H17 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C14 C16 1.525(5) . ?
C14 C15 1.536(5) . ?
C14 H14 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C37 C32 1.518(5) . ?
C37 C34 1.531(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C34 C35 1.488(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
O1 C32 1.424(5) . ?
O1 C35 1.430(5) . ?
N3 C6 1.294(4) . ?
N3 C20 1.443(4) . ?
C6 H6 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C41 O2 1.471(13) . ?
C41 C40 1.484(14) . ?
O2 C39 1.424(10) . ?
C39 C38 1.490(12) . ?
C40 C38 1.670(13) . ?
C83 C82 1.50(2) . ?
C83 C84 1.59(3) . ?
C80 C84 1.48(3) . ?
C80 O10 1.59(2) . ?
O10 C82 1.37(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N2 80.54(11) . . ?
N1 Ni1 N3 80.52(11) . . ?
N2 Ni1 N3 156.29(11) . . ?
N1 Ni1 Br1 161.44(8) . . ?
N2 Ni1 Br1 101.22(8) . . ?
N3 Ni1 Br1 101.28(8) . . ?
C7 N2 C8 118.3(3) . . ?
C7 N2 Ni1 113.5(2) . . ?
C8 N2 Ni1 127.9(2) . . ?
N1 C1 C2 121.3(3) . . ?
N1 C1 C7 109.5(3) . . ?
C2 C1 C7 129.1(3) . . ?
N1 C5 C4 120.7(3) . . ?
N1 C5 C6 109.9(3) . . ?
C4 C5 C6 129.3(3) . . ?
C1 N1 C5 119.9(3) . . ?
C1 N1 Ni1 119.5(2) . . ?
C5 N1 Ni1 119.3(2) . . ?
C5 C4 C3 119.3(3) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C3 C2 119.6(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C1 C2 C3 119.0(3) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C27 C28 C20 117.4(3) . . ?
C27 C28 C29 119.0(3) . . ?
C20 C28 C29 123.5(3) . . ?
C26 C27 C28 121.7(3) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C26 C25 119.9(3) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C25 C21 121.3(3) . . ?
C26 C25 H25 119.3 . . ?
C21 C25 H25 119.3 . . ?
C25 C21 C20 117.7(3) . . ?
C25 C21 C22 119.5(3) . . ?
C20 C21 C22 122.8(3) . . ?
C21 C22 C24 110.9(3) . . ?
C21 C22 C23 112.0(3) . . ?
C24 C22 C23 110.2(3) . . ?
C21 C22 H22 107.9 . . ?
C24 C22 H22 107.9 . . ?
C23 C22 H22 107.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C28 C29 C30 110.5(3) . . ?
C28 C29 C31 111.8(3) . . ?
C30 C29 C31 110.8(3) . . ?
C28 C29 H29 107.9 . . ?
C30 C29 H29 107.9 . . ?
C31 C29 H29 107.9 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N2 C7 C1 116.2(3) . . ?
N2 C7 H7 121.9 . . ?
C1 C7 H7 121.9 . . ?
C12 C13 C8 117.0(3) . . ?
C12 C13 C14 120.4(3) . . ?
C8 C13 C14 122.6(3) . . ?
C11 C12 C13 121.6(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C11 C10 120.5(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C10 C9 C8 117.6(3) . . ?
C10 C9 C17 121.3(3) . . ?
C8 C9 C17 121.1(3) . . ?
C9 C8 C13 122.6(3) . . ?
C9 C8 N2 117.1(3) . . ?
C13 C8 N2 120.3(3) . . ?
C18 C17 C19 110.8(3) . . ?
C18 C17 C9 110.9(3) . . ?
C19 C17 C9 112.5(3) . . ?
C18 C17 H17 107.5 . . ?
C19 C17 H17 107.5 . . ?
C9 C17 H17 107.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C14 C16 111.0(3) . . ?
C13 C14 C15 111.6(3) . . ?
C16 C14 C15 110.2(3) . . ?
C13 C14 H14 107.9 . . ?
C16 C14 H14 107.9 . . ?
C15 C14 H14 107.9 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C32 C37 C34 103.6(3) . . ?
C32 C37 H37A 111.0 . . ?
C34 C37 H37A 111.0 . . ?
C32 C37 H37B 111.0 . . ?
C34 C37 H37B 111.0 . . ?
H37A C37 H37B 109.0 . . ?
C35 C34 C37 103.5(3) . . ?
C35 C34 H34A 111.1 . . ?
C37 C34 H34A 111.1 . . ?
C35 C34 H34B 111.1 . . ?
C37 C34 H34B 111.1 . . ?
H34A C34 H34B 109.0 . . ?
C32 O1 C35 104.1(3) . . ?
C6 N3 C20 118.6(3) . . ?
C6 N3 Ni1 113.1(2) . . ?
C20 N3 Ni1 127.0(2) . . ?
N3 C6 C5 116.4(3) . . ?
N3 C6 H6 121.8 . . ?
C5 C6 H6 121.8 . . ?
C21 C20 C28 121.8(3) . . ?
C21 C20 N3 117.9(3) . . ?
C28 C20 N3 120.4(3) . . ?
O1 C32 C37 106.7(3) . . ?
O1 C32 H32A 110.4 . . ?
C37 C32 H32A 110.4 . . ?
O1 C32 H32B 110.4 . . ?
C37 C32 H32B 110.4 . . ?
H32A C32 H32B 108.6 . . ?
O1 C35 C34 105.2(3) . . ?
O1 C35 H35A 110.7 . . ?
C34 C35 H35A 110.7 . . ?
O1 C35 H35B 110.7 . . ?
C34 C35 H35B 110.7 . . ?
H35A C35 H35B 108.8 . . ?
O2 C41 C40 103.5(8) . . ?
C39 O2 C41 107.4(7) . . ?
O2 C39 C38 111.1(7) . . ?
C41 C40 C38 102.9(8) . . ?
C39 C38 C40 100.1(7) . . ?
C82 C83 C84 108.1(14) . . ?
C84 C80 O10 105.5(14) . . ?
C80 C84 C83 102.5(15) . . ?
C82 O10 C80 111.8(12) . . ?
O10 C82 C83 104.4(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 N2 C7 5.7(2) . . . . ?
N3 Ni1 N2 C7 43.1(4) . . . . ?
Br1 Ni1 N2 C7 -155.5(2) . . . . ?
N1 Ni1 N2 C8 178.8(3) . . . . ?
N3 Ni1 N2 C8 -143.8(3) . . . . ?
Br1 Ni1 N2 C8 17.6(3) . . . . ?
C2 C1 N1 C5 6.6(5) . . . . ?
C7 C1 N1 C5 -169.9(3) . . . . ?
C2 C1 N1 Ni1 173.6(2) . . . . ?
C7 C1 N1 Ni1 -2.9(3) . . . . ?
C4 C5 N1 C1 -6.2(4) . . . . ?
C6 C5 N1 C1 171.4(3) . . . . ?
C4 C5 N1 Ni1 -173.1(2) . . . . ?
C6 C5 N1 Ni1 4.4(3) . . . . ?
N2 Ni1 N1 C1 -1.2(2) . . . . ?
N3 Ni1 N1 C1 -166.9(2) . . . . ?
Br1 Ni1 N1 C1 95.9(3) . . . . ?
N2 Ni1 N1 C5 165.8(2) . . . . ?
N3 Ni1 N1 C5 0.1(2) . . . . ?
Br1 Ni1 N1 C5 -97.1(3) . . . . ?
N1 C5 C4 C3 2.2(5) . . . . ?
C6 C5 C4 C3 -174.7(3) . . . . ?
C5 C4 C3 C2 1.2(5) . . . . ?
N1 C1 C2 C3 -3.2(5) . . . . ?
C7 C1 C2 C3 172.6(3) . . . . ?
C4 C3 C2 C1 -0.8(5) . . . . ?
C20 C28 C27 C26 0.9(5) . . . . ?
C29 C28 C27 C26 -174.6(3) . . . . ?
C28 C27 C26 C25 1.7(5) . . . . ?
C27 C26 C25 C21 -1.2(5) . . . . ?
C26 C25 C21 C20 -1.9(5) . . . . ?
C26 C25 C21 C22 178.0(3) . . . . ?
C25 C21 C22 C24 70.8(4) . . . . ?
C20 C21 C22 C24 -109.4(4) . . . . ?
C25 C21 C22 C23 -52.8(4) . . . . ?
C20 C21 C22 C23 127.1(4) . . . . ?
C27 C28 C29 C30 59.3(4) . . . . ?
C20 C28 C29 C30 -115.9(3) . . . . ?
C27 C28 C29 C31 -64.6(4) . . . . ?
C20 C28 C29 C31 120.2(3) . . . . ?
C8 N2 C7 C1 177.1(3) . . . . ?
Ni1 N2 C7 C1 -9.0(4) . . . . ?
N1 C1 C7 N2 7.8(4) . . . . ?
C2 C1 C7 N2 -168.3(3) . . . . ?
C8 C13 C12 C11 -1.1(5) . . . . ?
C14 C13 C12 C11 -179.7(3) . . . . ?
C13 C12 C11 C10 -1.3(5) . . . . ?
C12 C11 C10 C9 1.3(5) . . . . ?
C11 C10 C9 C8 1.1(5) . . . . ?
C11 C10 C9 C17 179.1(3) . . . . ?
C10 C9 C8 C13 -3.6(5) . . . . ?
C17 C9 C8 C13 178.4(3) . . . . ?
C10 C9 C8 N2 178.4(3) . . . . ?
C17 C9 C8 N2 0.4(4) . . . . ?
C12 C13 C8 C9 3.6(5) . . . . ?
C14 C13 C8 C9 -177.8(3) . . . . ?
C12 C13 C8 N2 -178.4(3) . . . . ?
C14 C13 C8 N2 0.1(5) . . . . ?
C7 N2 C8 C9 -99.4(3) . . . . ?
Ni1 N2 C8 C9 87.8(3) . . . . ?
C7 N2 C8 C13 82.6(4) . . . . ?
Ni1 N2 C8 C13 -90.3(3) . . . . ?
C10 C9 C17 C18 -76.2(4) . . . . ?
C8 C9 C17 C18 101.8(4) . . . . ?
C10 C9 C17 C19 48.5(4) . . . . ?
C8 C9 C17 C19 -133.5(3) . . . . ?
C12 C13 C14 C16 69.9(4) . . . . ?
C8 C13 C14 C16 -108.7(4) . . . . ?
C12 C13 C14 C15 -53.5(4) . . . . ?
C8 C13 C14 C15 127.9(3) . . . . ?
C32 C37 C34 C35 -10.4(4) . . . . ?
N1 Ni1 N3 C6 -5.3(2) . . . . ?
N2 Ni1 N3 C6 -42.7(4) . . . . ?
Br1 Ni1 N3 C6 155.9(2) . . . . ?
N1 Ni1 N3 C20 -172.3(3) . . . . ?
N2 Ni1 N3 C20 150.3(3) . . . . ?
Br1 Ni1 N3 C20 -11.1(3) . . . . ?
C20 N3 C6 C5 177.5(3) . . . . ?
Ni1 N3 C6 C5 9.2(3) . . . . ?
N1 C5 C6 N3 -9.0(4) . . . . ?
C4 C5 C6 N3 168.3(3) . . . . ?
C25 C21 C20 C28 4.6(5) . . . . ?
C22 C21 C20 C28 -175.3(3) . . . . ?
C25 C21 C20 N3 -176.5(3) . . . . ?
C22 C21 C20 N3 3.6(5) . . . . ?
C27 C28 C20 C21 -4.1(5) . . . . ?
C29 C28 C20 C21 171.2(3) . . . . ?
C27 C28 C20 N3 177.0(3) . . . . ?
C29 C28 C20 N3 -7.7(5) . . . . ?
C6 N3 C20 C21 121.0(3) . . . . ?
Ni1 N3 C20 C21 -72.5(4) . . . . ?
C6 N3 C20 C28 -60.0(4) . . . . ?
Ni1 N3 C20 C28 106.4(3) . . . . ?
C35 O1 C32 C37 35.3(4) . . . . ?
C34 C37 C32 O1 -14.7(4) . . . . ?
C32 O1 C35 C34 -42.5(4) . . . . ?
C37 C34 C35 O1 32.2(4) . . . . ?
C40 C41 O2 C39 -38.5(10) . . . . ?
C41 O2 C39 C38 23.6(10) . . . . ?
O2 C41 C40 C38 36.4(9) . . . . ?
O2 C39 C38 C40 -0.2(9) . . . . ?
C41 C40 C38 C39 -22.5(9) . . . . ?
O10 C80 C84 C83 11.3(16) . . . . ?
C82 C83 C84 C80 -24.6(18) . . . . ?
C84 C80 O10 C82 6.1(17) . . . . ?
C80 O10 C82 C83 -21.4(17) . . . . ?
C84 C83 C82 O10 28.7(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        24.50
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_sg496_0m
_database_code_depnum_ccdc_archive 'CCDC 1040547'
_audit_update_record             
;
2014-12-19 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C37 H49 Br N3 Ni O1.50'
_chemical_formula_weight         698.41

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                   9.7274(10)
_cell_length_b                   14.2320(15)
_cell_length_c                   14.9719(13)
_cell_angle_alpha                111.974(4)
_cell_angle_beta                 99.695(3)
_cell_angle_gamma                101.376(2)
_cell_volume                     1816.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       needles
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             734
_exptl_absorpt_coefficient_mu    1.666
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7316
_exptl_absorpt_correction_T_max  0.9674
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30741
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         26.00
_reflns_number_total             7121
_reflns_number_gt                5114
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0602P)²+5.2596P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7121
_refine_ls_number_parameters     366
_refine_ls_number_restraints     441
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1421
_refine_ls_wR_factor_gt          0.1263
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      0.995
_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
Br1 Br 0.81450(4) 0.78404(4) 0.69170(3) 0.03081(15) Uani 1 1 d U . .
Ni1 Ni 0.59317(5) 0.81374(4) 0.64420(4) 0.01609(15) Uani 1 1 d U . .
N3 N 0.5481(3) 0.7524(2) 0.4946(2) 0.0158(7) Uani 1 1 d U . .
O2 O 0.9017(5) 0.4503(4) 0.7445(4) 0.0791(14) Uiso 1 1 d U . .
O1PD O 0.5000 0.5000 0.0000 0.0704(18) Uiso 1 2 d SU . .
N1 N 0.3913(3) 0.7865(2) 0.6116(2) 0.0158(7) Uani 1 1 d U . .
N2 N 0.5692(3) 0.9015(3) 0.7789(2) 0.0177(7) Uani 1 1 d U . .
C1 C 0.3262(4) 0.8283(3) 0.6845(3) 0.0185(9) Uani 1 1 d U . .
C2 C 0.4326(4) 0.8876(3) 0.7803(3) 0.0211(9) Uani 1 1 d U . .
H2 H 0.4050 0.9148 0.8407 0.025 Uiso 1 1 calc R . .
C3 C 0.6778(4) 0.9553(3) 0.8730(3) 0.0189(9) Uani 1 1 d U . .
C4 C 0.6797(4) 0.9144(3) 0.9451(3) 0.0201(9) Uani 1 1 d U . .
C5 C 0.7828(4) 0.9734(3) 1.0371(3) 0.0236(9) Uani 1 1 d U . .
H5 H 0.7844 0.9487 1.0880 0.028 Uiso 1 1 calc R . .
C6 C 0.8828(4) 1.0670(3) 1.0561(3) 0.0256(10) Uani 1 1 d U . .
H6 H 0.9502 1.1071 1.1199 0.031 Uiso 1 1 calc R . .
C7 C 0.8841(4) 1.1017(3) 0.9816(3) 0.0241(10) Uani 1 1 d U . .
H7 H 0.9551 1.1649 0.9944 0.029 Uiso 1 1 calc R . .
C8 C 0.7844(4) 1.0469(3) 0.8884(3) 0.0197(9) Uani 1 1 d U . .
C9 C 0.7918(4) 1.0857(4) 0.8074(3) 0.0269(10) Uani 1 1 d U . .
H9 H 0.7216 1.0300 0.7440 0.032 Uiso 1 1 calc R . .
C10 C 0.9432(5) 1.1010(5) 0.7898(4) 0.0499(15) Uani 1 1 d U . .
H10A H 1.0136 1.1579 0.8497 0.075 Uiso 1 1 calc R . .
H10B H 0.9423 1.1197 0.7330 0.075 Uiso 1 1 calc R . .
H10C H 0.9708 1.0353 0.7754 0.075 Uiso 1 1 calc R . .
C11 C 0.7476(7) 1.1866(5) 0.8301(5) 0.0554(16) Uani 1 1 d U . .
H11A H 0.6485 1.1748 0.8379 0.083 Uiso 1 1 calc R . .
H11B H 0.7510 1.2076 0.7750 0.083 Uiso 1 1 calc R . .
H11C H 0.8147 1.2427 0.8920 0.083 Uiso 1 1 calc R . .
C12 C 0.5828(4) 0.8069(3) 0.9252(3) 0.0241(9) Uani 1 1 d U . .
H12 H 0.5207 0.7746 0.8548 0.029 Uiso 1 1 calc R . .
C13 C 0.6754(5) 0.7340(4) 0.9348(4) 0.0372(12) Uani 1 1 d U . .
H13A H 0.7369 0.7275 0.8885 0.056 Uiso 1 1 calc R . .
H13B H 0.6116 0.6640 0.9187 0.056 Uiso 1 1 calc R . .
H13C H 0.7370 0.7638 1.0034 0.056 Uiso 1 1 calc R . .
C14 C 0.4810(5) 0.8159(4) 0.9948(4) 0.0363(12) Uani 1 1 d U . .
H14A H 0.5394 0.8474 1.0644 0.054 Uiso 1 1 calc R . .
H14B H 0.4188 0.7453 0.9785 0.054 Uiso 1 1 calc R . .
H14C H 0.4201 0.8606 0.9857 0.054 Uiso 1 1 calc R . .
C15 C 0.1770(4) 0.8146(3) 0.6618(3) 0.0222(9) Uani 1 1 d U . .
H15 H 0.1309 0.8412 0.7132 0.027 Uiso 1 1 calc R . .
C16 C 0.0966(4) 0.7614(3) 0.5627(3) 0.0234(9) Uani 1 1 d U . .
H16 H -0.0056 0.7508 0.5459 0.028 Uiso 1 1 calc R . .
C17 C 0.1650(4) 0.7236(3) 0.4876(3) 0.0206(9) Uani 1 1 d U . .
H17 H 0.1112 0.6882 0.4194 0.025 Uiso 1 1 calc R . .
C18 C 0.3141(4) 0.7392(3) 0.5152(3) 0.0172(8) Uani 1 1 d U . .
C19 C 0.4089(4) 0.7147(3) 0.4500(3) 0.0169(8) Uani 1 1 d U . .
H19 H 0.3725 0.6741 0.3798 0.020 Uiso 1 1 calc R . .
C20 C 0.6495(4) 0.7364(3) 0.4337(3) 0.0182(9) Uani 1 1 d U . .
C21 C 0.6851(4) 0.6411(3) 0.3998(3) 0.0200(9) Uani 1 1 d U . .
C22 C 0.6200(5) 0.5499(3) 0.4221(4) 0.0296(11) Uani 1 1 d U . .
H22 H 0.5680 0.5767 0.4744 0.036 Uiso 1 1 calc R . .
C23 C 0.5075(6) 0.4619(4) 0.3304(4) 0.0451(14) Uani 1 1 d U . .
H23A H 0.4313 0.4899 0.3074 0.068 Uiso 1 1 calc R . .
H23B H 0.4642 0.4049 0.3477 0.068 Uiso 1 1 calc R . .
H23C H 0.5546 0.4343 0.2772 0.068 Uiso 1 1 calc R . .
C24 C 0.7346(6) 0.5071(4) 0.4644(4) 0.0389(12) Uani 1 1 d U . .
H24A H 0.7803 0.4728 0.4124 0.058 Uiso 1 1 calc R . .
H24B H 0.6882 0.4556 0.4869 0.058 Uiso 1 1 calc R . .
H24C H 0.8088 0.5655 0.5210 0.058 Uiso 1 1 calc R . .
C25 C 0.7860(4) 0.6326(3) 0.3429(3) 0.0230(9) Uani 1 1 d U . .
H25 H 0.8131 0.5689 0.3192 0.028 Uiso 1 1 calc R . .
C26 C 0.8469(5) 0.7133(4) 0.3201(4) 0.0278(10) Uani 1 1 d U . .
H26 H 0.9136 0.7049 0.2801 0.033 Uiso 1 1 calc R . .
C27 C 0.8102(5) 0.8073(4) 0.3560(4) 0.0383(13) Uani 1 1 d U . .
H27 H 0.8529 0.8634 0.3406 0.046 Uiso 1 1 calc R . .
C28 C 0.7120(5) 0.8211(4) 0.4143(4) 0.0347(12) Uani 1 1 d U . .
C29 C 0.6758(8) 0.9265(5) 0.4560(6) 0.071(2) Uani 1 1 d U . .
H29 H 0.6095 0.9206 0.4992 0.085 Uiso 1 1 calc R . .
C30 C 0.8069(13) 1.0166(6) 0.5199(6) 0.134(5) Uani 1 1 d U . .
H30A H 0.8626 1.0359 0.4775 0.201 Uiso 1 1 calc R . .
H30B H 0.8676 0.9960 0.5644 0.201 Uiso 1 1 calc R . .
H30C H 0.7768 1.0772 0.5599 0.201 Uiso 1 1 calc R . .
C31 C 0.5975(9) 0.9488(6) 0.3765(7) 0.112(4) Uani 1 1 d U . .
H31A H 0.5836 1.0192 0.4058 0.168 Uiso 1 1 calc R . .
H31B H 0.5026 0.8957 0.3429 0.168 Uiso 1 1 calc R . .
H31C H 0.6544 0.9463 0.3279 0.168 Uiso 1 1 calc R . .
C32 C 1.0399(16) 0.5909(12) 0.8831(11) 0.182(6) Uiso 1 1 d U . .
H32A H 1.1348 0.6100 0.9315 0.218 Uiso 1 1 calc R . .
H32B H 0.9788 0.6317 0.9184 0.218 Uiso 1 1 calc R . .
C33 C 1.0622(9) 0.6184(7) 0.8028(6) 0.094(3) Uiso 1 1 d U . .
H33A H 1.1542 0.6079 0.7867 0.112 Uiso 1 1 calc R . .
H33B H 1.0620 0.6923 0.8181 0.112 Uiso 1 1 calc R . .
C34 C 0.9363(8) 0.5436(5) 0.7226(6) 0.0702(19) Uiso 1 1 d U . .
H34A H 0.9590 0.5243 0.6572 0.084 Uiso 1 1 calc R . .
H34B H 0.8533 0.5741 0.7212 0.084 Uiso 1 1 calc R . .
C35 C 0.9716(10) 0.4820(7) 0.8475(7) 0.102(3) Uiso 1 1 d U . .
H35A H 0.8996 0.4692 0.8842 0.123 Uiso 1 1 calc R . .
H35B H 1.0439 0.4433 0.8545 0.123 Uiso 1 1 calc R . .
C36 C 0.4623(9) 0.6121(7) 0.1491(7) 0.089(2) Uiso 1 1 d U . .
C50 C 0.3794(14) 0.5452(10) 0.0517(10) 0.058(3) Uiso 0.50 1 d PU A 1
C51 C 0.5814(14) 0.5647(10) 0.0973(10) 0.058(3) Uiso 0.50 1 d PU A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Ni1 2.3212(7) . ?
Ni1 N1 1.865(3) . ?
Ni1 N3 2.006(3) . ?
Ni1 N2 2.018(3) . ?
N3 C19 1.307(5) . ?
N3 C20 1.447(5) . ?
O2 C35 1.432(10) . ?
O2 C34 1.473(8) . ?
O1PD C51 1.384(13) . ?
O1PD C51 1.384(13) 2_665 ?
O1PD C50 1.619(13) . ?
O1PD C50 1.619(13) 2_665 ?
N1 C18 1.345(5) . ?
N1 C1 1.357(5) . ?
N2 C2 1.309(5) . ?
N2 C3 1.435(5) . ?
C1 C15 1.390(5) . ?
C1 C2 1.446(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.404(6) . ?
C3 C8 1.411(6) . ?
C4 C5 1.395(6) . ?
C4 C12 1.521(6) . ?
C5 C6 1.384(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.379(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.515(6) . ?
C9 C11 1.513(7) . ?
C9 C10 1.527(6) . ?
C9 H9 1.0000 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.532(6) . ?
C12 C14 1.543(6) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.386(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.391(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.450(5) . ?
C19 H19 0.9500 . ?
C20 C28 1.394(6) . ?
C20 C21 1.395(6) . ?
C21 C25 1.399(6) . ?
C21 C22 1.506(6) . ?
C22 C23 1.522(7) . ?
C22 C24 1.527(7) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.371(6) . ?
C25 H25 0.9500 . ?
C26 C27 1.386(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.531(7) . ?
C29 C31 1.473(11) . ?
C29 C30 1.487(11) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C35 1.408(15) . ?
C32 C33 1.433(15) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.451(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C50 1.395(15) . ?
C36 C51 1.618(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N3 79.86(13) . . ?
N1 Ni1 N2 80.45(13) . . ?
N3 Ni1 N2 155.07(13) . . ?
N1 Ni1 Br1 156.51(10) . . ?
N3 Ni1 Br1 103.55(9) . . ?
N2 Ni1 Br1 100.61(9) . . ?
C19 N3 C20 118.3(3) . . ?
C19 N3 Ni1 113.7(3) . . ?
C20 N3 Ni1 127.7(3) . . ?
C35 O2 C34 107.8(6) . . ?
C51 O1PD C51 180.0(12) . 2_665 ?
C51 O1PD C50 77.9(7) . . ?
C51 O1PD C50 102.1(7) 2_665 . ?
C51 O1PD C50 102.1(7) . 2_665 ?
C51 O1PD C50 77.9(7) 2_665 2_665 ?
C50 O1PD C50 180.0(9) . 2_665 ?
C18 N1 C1 120.1(3) . . ?
C18 N1 Ni1 119.9(3) . . ?
C1 N1 Ni1 119.3(3) . . ?
C2 N2 C3 117.8(3) . . ?
C2 N2 Ni1 112.6(3) . . ?
C3 N2 Ni1 128.1(2) . . ?
N1 C1 C15 120.7(4) . . ?
N1 C1 C2 110.7(3) . . ?
C15 C1 C2 128.5(4) . . ?
N2 C2 C1 116.2(4) . . ?
N2 C2 H2 121.9 . . ?
C1 C2 H2 121.9 . . ?
C4 C3 C8 121.7(4) . . ?
C4 C3 N2 120.3(3) . . ?
C8 C3 N2 118.0(4) . . ?
C5 C4 C3 117.5(4) . . ?
C5 C4 C12 119.1(4) . . ?
C3 C4 C12 123.3(4) . . ?
C6 C5 C4 121.6(4) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C7 C6 C5 119.6(4) . . ?
C7 C6 H6 120.2 . . ?
C5 C6 H6 120.2 . . ?
C6 C7 C8 121.8(4) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C7 C8 C3 117.6(4) . . ?
C7 C8 C9 120.3(4) . . ?
C3 C8 C9 122.1(4) . . ?
C11 C9 C8 112.2(4) . . ?
C11 C9 C10 110.2(4) . . ?
C8 C9 C10 111.3(4) . . ?
C11 C9 H9 107.7 . . ?
C8 C9 H9 107.7 . . ?
C10 C9 H9 107.7 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C4 C12 C13 110.3(4) . . ?
C4 C12 C14 112.0(4) . . ?
C13 C12 C14 110.7(4) . . ?
C4 C12 H12 107.9 . . ?
C13 C12 H12 107.9 . . ?
C14 C12 H12 107.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C1 118.8(4) . . ?
C16 C15 H15 120.6 . . ?
C1 C15 H15 120.6 . . ?
C15 C16 C17 120.3(4) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 118.1(4) . . ?
C18 C17 H17 120.9 . . ?
C16 C17 H17 120.9 . . ?
N1 C18 C17 121.7(4) . . ?
N1 C18 C19 110.7(3) . . ?
C17 C18 C19 127.5(4) . . ?
N3 C19 C18 115.2(4) . . ?
N3 C19 H19 122.4 . . ?
C18 C19 H19 122.4 . . ?
C28 C20 C21 122.6(4) . . ?
C28 C20 N3 116.9(3) . . ?
C21 C20 N3 120.5(3) . . ?
C20 C21 C25 117.0(4) . . ?
C20 C21 C22 122.9(4) . . ?
C25 C21 C22 120.1(4) . . ?
C21 C22 C23 111.1(4) . . ?
C21 C22 C24 112.9(4) . . ?
C23 C22 C24 110.8(4) . . ?
C21 C22 H22 107.2 . . ?
C23 C22 H22 107.2 . . ?
C24 C22 H22 107.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C21 122.0(4) . . ?
C26 C25 H25 119.0 . . ?
C21 C25 H25 119.0 . . ?
C25 C26 C27 119.4(4) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C26 C27 C28 121.3(4) . . ?
C26 C27 H27 119.4 . . ?
C28 C27 H27 119.4 . . ?
C27 C28 C20 117.7(4) . . ?
C27 C28 C29 120.7(4) . . ?
C20 C28 C29 121.5(4) . . ?
C31 C29 C30 110.1(5) . . ?
C31 C29 C28 112.2(6) . . ?
C30 C29 C28 112.4(6) . . ?
C31 C29 H29 107.3 . . ?
C30 C29 H29 107.3 . . ?
C28 C29 H29 107.3 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C35 C32 C33 111.1(12) . . ?
C35 C32 H32A 109.4 . . ?
C33 C32 H32A 109.4 . . ?
C35 C32 H32B 109.4 . . ?
C33 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
C32 C33 C34 100.9(9) . . ?
C32 C33 H33A 111.6 . . ?
C34 C33 H33A 111.6 . . ?
C32 C33 H33B 111.6 . . ?
C34 C33 H33B 111.6 . . ?
H33A C33 H33B 109.4 . . ?
C33 C34 O2 105.6(6) . . ?
C33 C34 H34A 110.6 . . ?
O2 C34 H34A 110.6 . . ?
C33 C34 H34B 110.6 . . ?
O2 C34 H34B 110.6 . . ?
H34A C34 H34B 108.8 . . ?
C32 C35 O2 104.0(9) . . ?
C32 C35 H35A 111.0 . . ?
O2 C35 H35A 111.0 . . ?
C32 C35 H35B 111.0 . . ?
O2 C35 H35B 111.0 . . ?
H35A C35 H35B 109.0 . . ?
C50 C36 C51 77.6(8) . . ?
C36 C50 O1PD 102.0(8) . . ?
O1PD C51 C36 102.5(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 Ni1 N3 C19 -7.0(3) . . . . ?
N2 Ni1 N3 C19 -45.3(4) . . . . ?
Br1 Ni1 N3 C19 149.2(2) . . . . ?
N1 Ni1 N3 C20 179.8(3) . . . . ?
N2 Ni1 N3 C20 141.5(3) . . . . ?
Br1 Ni1 N3 C20 -23.9(3) . . . . ?
N3 Ni1 N1 C18 3.0(3) . . . . ?
N2 Ni1 N1 C18 167.6(3) . . . . ?
Br1 Ni1 N1 C18 -97.7(4) . . . . ?
N3 Ni1 N1 C1 -167.3(3) . . . . ?
N2 Ni1 N1 C1 -2.7(3) . . . . ?
Br1 Ni1 N1 C1 92.0(4) . . . . ?
N1 Ni1 N2 C2 7.0(3) . . . . ?
N3 Ni1 N2 C2 45.3(5) . . . . ?
Br1 Ni1 N2 C2 -149.1(3) . . . . ?
N1 Ni1 N2 C3 172.2(3) . . . . ?
N3 Ni1 N2 C3 -149.6(3) . . . . ?
Br1 Ni1 N2 C3 16.0(3) . . . . ?
C18 N1 C1 C15 6.0(6) . . . . ?
Ni1 N1 C1 C15 176.2(3) . . . . ?
C18 N1 C1 C2 -172.0(3) . . . . ?
Ni1 N1 C1 C2 -1.7(4) . . . . ?
C3 N2 C2 C1 -176.9(3) . . . . ?
Ni1 N2 C2 C1 -10.1(5) . . . . ?
N1 C1 C2 N2 8.0(5) . . . . ?
C15 C1 C2 N2 -169.8(4) . . . . ?
C2 N2 C3 C4 59.3(5) . . . . ?
Ni1 N2 C3 C4 -105.2(4) . . . . ?
C2 N2 C3 C8 -123.3(4) . . . . ?
Ni1 N2 C3 C8 72.3(4) . . . . ?
C8 C3 C4 C5 6.2(6) . . . . ?
N2 C3 C4 C5 -176.5(3) . . . . ?
C8 C3 C4 C12 -169.7(4) . . . . ?
N2 C3 C4 C12 7.7(6) . . . . ?
C3 C4 C5 C6 -2.1(6) . . . . ?
C12 C4 C5 C6 174.0(4) . . . . ?
C4 C5 C6 C7 -1.9(6) . . . . ?
C5 C6 C7 C8 2.0(6) . . . . ?
C6 C7 C8 C3 1.9(6) . . . . ?
C6 C7 C8 C9 -178.2(4) . . . . ?
C4 C3 C8 C7 -6.1(6) . . . . ?
N2 C3 C8 C7 176.5(3) . . . . ?
C4 C3 C8 C9 174.0(4) . . . . ?
N2 C3 C8 C9 -3.4(5) . . . . ?
C7 C8 C9 C11 -70.3(5) . . . . ?
C3 C8 C9 C11 109.6(5) . . . . ?
C7 C8 C9 C10 53.6(6) . . . . ?
C3 C8 C9 C10 -126.5(4) . . . . ?
C5 C4 C12 C13 -59.0(5) . . . . ?
C3 C4 C12 C13 116.8(4) . . . . ?
C5 C4 C12 C14 64.8(5) . . . . ?
C3 C4 C12 C14 -119.4(4) . . . . ?
N1 C1 C15 C16 -2.9(6) . . . . ?
C2 C1 C15 C16 174.7(4) . . . . ?
C1 C15 C16 C17 -0.7(6) . . . . ?
C15 C16 C17 C18 1.1(6) . . . . ?
C1 N1 C18 C17 -5.6(6) . . . . ?
Ni1 N1 C18 C17 -175.8(3) . . . . ?
C1 N1 C18 C19 171.4(3) . . . . ?
Ni1 N1 C18 C19 1.2(4) . . . . ?
C16 C17 C18 N1 2.0(6) . . . . ?
C16 C17 C18 C19 -174.4(4) . . . . ?
C20 N3 C19 C18 -176.5(3) . . . . ?
Ni1 N3 C19 C18 9.7(4) . . . . ?
N1 C18 C19 N3 -7.3(5) . . . . ?
C17 C18 C19 N3 169.5(4) . . . . ?
C19 N3 C20 C28 100.2(5) . . . . ?
Ni1 N3 C20 C28 -86.9(4) . . . . ?
C19 N3 C20 C21 -81.9(5) . . . . ?
Ni1 N3 C20 C21 91.0(4) . . . . ?
C28 C20 C21 C25 -1.2(6) . . . . ?
N3 C20 C21 C25 -178.9(4) . . . . ?
C28 C20 C21 C22 178.8(4) . . . . ?
N3 C20 C21 C22 1.1(6) . . . . ?
C20 C21 C22 C23 105.5(5) . . . . ?
C25 C21 C22 C23 -74.5(5) . . . . ?
C20 C21 C22 C24 -129.3(4) . . . . ?
C25 C21 C22 C24 50.7(6) . . . . ?
C20 C21 C25 C26 -0.6(6) . . . . ?
C22 C21 C25 C26 179.4(4) . . . . ?
C21 C25 C26 C27 1.3(7) . . . . ?
C25 C26 C27 C28 -0.4(8) . . . . ?
C26 C27 C28 C20 -1.2(8) . . . . ?
C26 C27 C28 C29 178.2(6) . . . . ?
C21 C20 C28 C27 2.0(7) . . . . ?
N3 C20 C28 C27 179.8(4) . . . . ?
C21 C20 C28 C29 -177.4(5) . . . . ?
N3 C20 C28 C29 0.4(7) . . . . ?
C27 C28 C29 C31 66.5(8) . . . . ?
C20 C28 C29 C31 -114.0(6) . . . . ?
C27 C28 C29 C30 -58.3(9) . . . . ?
C20 C28 C29 C30 121.2(7) . . . . ?
C35 C32 C33 C34 32.7(13) . . . . ?
C32 C33 C34 O2 -29.5(10) . . . . ?
C35 O2 C34 C33 18.1(8) . . . . ?
C33 C32 C35 O2 -21.9(14) . . . . ?
C34 O2 C35 C32 1.7(11) . . . . ?
C51 C36 C50 O1PD -1.0(7) . . . . ?
C51 O1PD C50 C36 1.2(8) . . . . ?
C51 O1PD C50 C36 -178.8(8) 2_665 . . . ?
C50 O1PD C50 C36 95(100) 2_665 . . . ?
C51 O1PD C51 C36 -53(100) 2_665 . . . ?
C50 O1PD C51 C36 -1.0(7) . . . . ?
C50 O1PD C51 C36 179.0(7) 2_665 . . . ?
C50 C36 C51 O1PD 1.2(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.392
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.102
