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

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

data_t
_audit_block_doi                 10.5517/ccdc.csd.cc1zflqq
_database_code_depnum_ccdc_archive 'CCDC 1830324'
_audit_update_record             
;
2018-03-16 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H28 Br4 N2 Ni O2'
_chemical_formula_sum            'C40 H28 Br4 N2 Ni O2'
_chemical_formula_weight         946.93

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   ' C 2/c    '
_symmetry_space_group_name_Hall  '-C 2yc'

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

_cell_length_a                   24.331(8)
_cell_length_b                   8.402(3)
_cell_length_c                   20.590(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.627(3)
_cell_angle_gamma                90.00
_cell_volume                     3584(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3202
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      24.35

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1864
_exptl_absorpt_coefficient_mu    5.039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.295
_exptl_absorpt_correction_T_max  0.365
_exptl_absorpt_process_details   'SADABS, v2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14549
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.66
_reflns_number_total             4178
_reflns_number_gt                2249
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0100P)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_number_reflns         4128
_refine_ls_number_parameters     222
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1206
_refine_ls_R_factor_gt           0.0434
_refine_ls_wR_factor_ref         0.0651
_refine_ls_wR_factor_gt          0.0562
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_restrained_S_all      1.264
_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 -0.16108(2) 1.04396(6) -0.01301(2) 0.06003(16) Uani 1 1 d . . .
Br2 Br 0.03290(2) 1.34351(5) -0.04121(2) 0.05621(16) Uani 1 1 d . . .
Ni1 Ni 0.0000 0.95449(8) 0.2500 0.03035(18) Uani 1 2 d S . .
O1 O -0.04724(11) 0.9730(3) 0.14543(12) 0.0371(6) Uani 1 1 d . . .
N1 N 0.07969(13) 0.9479(3) 0.25386(15) 0.0309(7) Uani 1 1 d . . .
C18 C -0.0553(2) 1.1871(4) -0.0115(2) 0.0432(11) Uani 1 1 d . . .
H18 H -0.0864 1.2222 -0.0600 0.052 Uiso 1 1 calc R . .
C19 C -0.07376(18) 1.1001(4) 0.03059(19) 0.0352(10) Uani 1 1 d . . .
C17 C 0.0090(2) 1.2227(4) 0.0178(2) 0.0375(10) Uani 1 1 d . . .
C7 C 0.13608(17) 0.8694(4) 0.32048(18) 0.0304(9) Uani 1 1 d . . .
H7 H 0.1402 0.9166 0.3664 0.036 Uiso 1 1 calc R . .
C20 C 0.08680(18) 1.0140(4) 0.20230(19) 0.0352(10) Uani 1 1 d . . .
H20 H 0.1285 1.0175 0.2115 0.042 Uiso 1 1 calc R . .
C16 C 0.0547(2) 1.1687(4) 0.0878(2) 0.0392(10) Uani 1 1 d . . .
H16 H 0.0980 1.1889 0.1065 0.047 Uiso 1 1 calc R . .
C15 C 0.03699(18) 1.0826(4) 0.13229(18) 0.0310(9) Uani 1 1 d . . .
C14 C -0.02845(19) 1.0500(4) 0.10557(19) 0.0327(9) Uani 1 1 d . . .
C12 C 0.2993(3) 1.0381(6) 0.3805(3) 0.0785(15) Uani 1 1 d . . .
H12 H 0.3266 1.1158 0.4142 0.094 Uiso 1 1 calc R . .
C5 C 0.1436(3) 0.4552(6) 0.3952(3) 0.0759(16) Uani 1 1 d . . .
H5 H 0.1642 0.4050 0.4425 0.091 Uiso 1 1 calc R . .
C4 C 0.1059(3) 0.3681(6) 0.3309(3) 0.0706(15) Uani 1 1 d . . .
H4 H 0.1002 0.2594 0.3340 0.085 Uiso 1 1 calc R . .
C10 C 0.2766(2) 0.8413(6) 0.2891(3) 0.0670(14) Uani 1 1 d . . .
H10 H 0.2880 0.7846 0.2591 0.080 Uiso 1 1 calc R . .
C6 C 0.1517(2) 0.6158(6) 0.3913(2) 0.0587(13) Uani 1 1 d . . .
H6 H 0.1774 0.6733 0.4359 0.070 Uiso 1 1 calc R . .
C3 C 0.0766(2) 0.4433(6) 0.2622(3) 0.0639(13) Uani 1 1 d . . .
H3 H 0.0516 0.3844 0.2179 0.077 Uiso 1 1 calc R . .
C13 C 0.2413(2) 1.0089(5) 0.3741(2) 0.0570(13) Uani 1 1 d . . .
H13 H 0.2298 1.0683 0.4032 0.068 Uiso 1 1 calc R . .
C11 C 0.3172(2) 0.9551(7) 0.3384(3) 0.0712(15) Uani 1 1 d . . .
H11 H 0.3566 0.9752 0.3428 0.085 Uiso 1 1 calc R . .
C2 C 0.0833(2) 0.6055(5) 0.2568(2) 0.0515(12) Uani 1 1 d . . .
H2 H 0.0617 0.6554 0.2094 0.062 Uiso 1 1 calc R . .
C9 C 0.2187(2) 0.8108(5) 0.2839(2) 0.0571(12) Uani 1 1 d . . .
H9 H 0.1919 0.7314 0.2511 0.069 Uiso 1 1 calc R . .
C8 C 0.19986(19) 0.8951(5) 0.3261(2) 0.0356(10) Uani 1 1 d . . .
C1 C 0.12206(18) 0.6928(4) 0.3218(2) 0.0354(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C19 1.882(4) . ?
Br2 C17 1.893(3) . ?
Ni1 O1 1.840(2) . ?
Ni1 O1 1.840(2) 2 ?
Ni1 N1 1.899(3) 2 ?
Ni1 N1 1.899(3) . ?
O1 C14 1.302(4) . ?
N1 C20 1.288(4) . ?
N1 C7 1.492(4) . ?
C18 C19 1.376(5) . ?
C18 C17 1.384(5) . ?
C18 H18 0.9300 . ?
C19 C14 1.411(5) . ?
C17 C16 1.356(5) . ?
C7 C8 1.509(5) . ?
C7 C1 1.526(5) . ?
C7 H7 0.9800 . ?
C20 C15 1.431(5) . ?
C20 H20 0.9300 . ?
C16 C15 1.400(4) . ?
C16 H16 0.9300 . ?
C15 C14 1.412(5) . ?
C12 C11 1.352(6) . ?
C12 C13 1.368(6) . ?
C12 H12 0.9300 . ?
C5 C4 1.362(6) . ?
C5 C6 1.372(6) . ?
C5 H5 0.9300 . ?
C4 C3 1.361(6) . ?
C4 H4 0.9300 . ?
C10 C11 1.367(6) . ?
C10 C9 1.379(6) . ?
C10 H10 0.9300 . ?
C6 C1 1.380(5) . ?
C6 H6 0.9300 . ?
C3 C2 1.384(6) . ?
C3 H3 0.9300 . ?
C13 C8 1.364(5) . ?
C13 H13 0.9300 . ?
C11 H11 0.9300 . ?
C2 C1 1.377(5) . ?
C2 H2 0.9300 . ?
C9 C8 1.374(5) . ?
C9 H9 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 170.30(15) . 2 ?
O1 Ni1 N1 87.47(10) . 2 ?
O1 Ni1 N1 92.81(11) 2 2 ?
O1 Ni1 N1 92.81(10) . . ?
O1 Ni1 N1 87.47(10) 2 . ?
N1 Ni1 N1 176.68(18) 2 . ?
C14 O1 Ni1 124.7(2) . . ?
C20 N1 C7 119.5(3) . . ?
C20 N1 Ni1 121.9(2) . . ?
C7 N1 Ni1 118.5(2) . . ?
C19 C18 C17 120.6(3) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C14 121.5(4) . . ?
C18 C19 Br1 119.5(3) . . ?
C14 C19 Br1 119.1(3) . . ?
C16 C17 C18 120.0(3) . . ?
C16 C17 Br2 120.4(3) . . ?
C18 C17 Br2 119.6(3) . . ?
N1 C7 C8 114.9(3) . . ?
N1 C7 C1 109.9(3) . . ?
C8 C7 C1 111.6(3) . . ?
N1 C7 H7 106.7 . . ?
C8 C7 H7 106.7 . . ?
C1 C7 H7 106.7 . . ?
N1 C20 C15 126.5(3) . . ?
N1 C20 H20 116.7 . . ?
C15 C20 H20 116.7 . . ?
C17 C16 C15 120.5(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C15 C14 121.1(3) . . ?
C16 C15 C20 118.6(4) . . ?
C14 C15 C20 120.0(3) . . ?
O1 C14 C19 120.4(3) . . ?
O1 C14 C15 123.2(3) . . ?
C19 C14 C15 116.3(3) . . ?
C11 C12 C13 120.6(5) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C3 C4 C5 118.6(5) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C5 C6 C1 120.6(4) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C8 C13 C12 122.0(4) . . ?
C8 C13 H13 119.0 . . ?
C12 C13 H13 119.0 . . ?
C12 C11 C10 119.2(5) . . ?
C12 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C1 C2 C3 119.7(4) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C8 C9 C10 121.4(4) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?
C13 C8 C9 117.0(4) . . ?
C13 C8 C7 119.7(4) . . ?
C9 C8 C7 123.3(4) . . ?
C2 C1 C6 118.5(4) . . ?
C2 C1 C7 123.1(3) . . ?
C6 C1 C7 118.3(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ni1 O1 C14 56.8(3) 2 . . . ?
N1 Ni1 O1 C14 148.7(3) 2 . . . ?
N1 Ni1 O1 C14 -34.6(3) . . . . ?
O1 Ni1 N1 C20 27.0(3) . . . . ?
O1 Ni1 N1 C20 -143.3(3) 2 . . . ?
N1 Ni1 N1 C20 121.8(3) 2 . . . ?
O1 Ni1 N1 C7 -155.6(2) . . . . ?
O1 Ni1 N1 C7 34.1(2) 2 . . . ?
N1 Ni1 N1 C7 -60.8(2) 2 . . . ?
C17 C18 C19 C14 2.6(5) . . . . ?
C17 C18 C19 Br1 -176.6(3) . . . . ?
C19 C18 C17 C16 1.5(5) . . . . ?
C19 C18 C17 Br2 -179.7(3) . . . . ?
C20 N1 C7 C8 7.9(4) . . . . ?
Ni1 N1 C7 C8 -169.6(2) . . . . ?
C20 N1 C7 C1 -118.8(3) . . . . ?
Ni1 N1 C7 C1 63.7(3) . . . . ?
C7 N1 C20 C15 174.6(3) . . . . ?
Ni1 N1 C20 C15 -8.0(5) . . . . ?
C18 C17 C16 C15 -2.8(5) . . . . ?
Br2 C17 C16 C15 178.5(2) . . . . ?
C17 C16 C15 C14 0.0(5) . . . . ?
C17 C16 C15 C20 173.7(3) . . . . ?
N1 C20 C15 C16 171.3(3) . . . . ?
N1 C20 C15 C14 -14.9(5) . . . . ?
Ni1 O1 C14 C19 -160.3(2) . . . . ?
Ni1 O1 C14 C15 22.3(5) . . . . ?
C18 C19 C14 O1 177.4(3) . . . . ?
Br1 C19 C14 O1 -3.5(5) . . . . ?
C18 C19 C14 C15 -5.1(5) . . . . ?
Br1 C19 C14 C15 174.1(3) . . . . ?
C16 C15 C14 O1 -178.7(3) . . . . ?
C20 C15 C14 O1 7.6(5) . . . . ?
C16 C15 C14 C19 3.8(5) . . . . ?
C20 C15 C14 C19 -169.8(3) . . . . ?
C6 C5 C4 C3 0.6(7) . . . . ?
C4 C5 C6 C1 -0.5(7) . . . . ?
C5 C4 C3 C2 -1.6(7) . . . . ?
C11 C12 C13 C8 0.7(7) . . . . ?
C13 C12 C11 C10 0.0(8) . . . . ?
C9 C10 C11 C12 -1.1(7) . . . . ?
C4 C3 C2 C1 2.3(7) . . . . ?
C11 C10 C9 C8 1.5(7) . . . . ?
C12 C13 C8 C9 -0.3(6) . . . . ?
C12 C13 C8 C7 -179.1(4) . . . . ?
C10 C9 C8 C13 -0.8(6) . . . . ?
C10 C9 C8 C7 178.0(4) . . . . ?
N1 C7 C8 C13 98.9(4) . . . . ?
C1 C7 C8 C13 -135.3(4) . . . . ?
N1 C7 C8 C9 -79.9(4) . . . . ?
C1 C7 C8 C9 46.0(5) . . . . ?
C3 C2 C1 C6 -2.1(6) . . . . ?
C3 C2 C1 C7 175.3(4) . . . . ?
C5 C6 C1 C2 1.2(6) . . . . ?
C5 C6 C1 C7 -176.3(4) . . . . ?
N1 C7 C1 C2 31.0(5) . . . . ?
C8 C7 C1 C2 -97.6(4) . . . . ?
N1 C7 C1 C6 -151.6(3) . . . . ?
C8 C7 C1 C6 79.8(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.66
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.53
_refine_diff_density_rms         0.115
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1587113'
_audit_update_record             
;
2017-11-22 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H32 N2 Ni O2'
_chemical_formula_weight         631.39

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   17.482(8)
_cell_length_b                   10.366(5)
_cell_length_c                   18.537(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.601(5)
_cell_angle_gamma                90.00
_cell_volume                     3144(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6425
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      26.63

_exptl_crystal_description       Block
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18086
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         26.63
_reflns_number_total             6425
_reflns_number_gt                4498
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0521P)²+7.1764P] 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         6425
_refine_ls_number_parameters     412
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1784
_refine_ls_wR_factor_gt          0.1583
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6972(3) 0.1737(5) 0.8658(2) 0.0463(11) Uani 1 1 d . . .
C2 C 0.3811(3) 0.0618(5) 0.8741(3) 0.0486(11) Uani 1 1 d . . .
C3 C 0.6603(3) -0.0475(4) 0.8347(2) 0.0421(10) Uani 1 1 d . . .
H3A H 0.6371 -0.1073 0.8626 0.050 Uiso 1 1 calc R . .
C4 C 0.3841(3) 0.2718(4) 0.8208(3) 0.0475(11) Uani 1 1 d . . .
H4A H 0.4192 0.3398 0.8521 0.057 Uiso 1 1 calc R . .
C5 C 0.6100(3) 0.3612(4) 0.8659(2) 0.0437(10) Uani 1 1 d . . .
C6 C 0.6879(3) 0.3084(4) 0.8779(2) 0.0433(10) Uani 1 1 d . . .
C7 C 0.7560(3) 0.3895(5) 0.8966(3) 0.0554(12) Uani 1 1 d . . .
H7A H 0.8070 0.3539 0.9039 0.066 Uiso 1 1 calc R . .
C8 C 0.7495(3) 0.5206(5) 0.9045(3) 0.0632(14) Uani 1 1 d . . .
H8A H 0.7952 0.5739 0.9169 0.076 Uiso 1 1 calc R . .
C9 C 0.6730(4) 0.5704(5) 0.8932(3) 0.0631(13) Uani 1 1 d . . .
H9A H 0.6678 0.6587 0.8994 0.076 Uiso 1 1 calc R . .
C10 C 0.6048(3) 0.4956(5) 0.8734(3) 0.0588(13) Uani 1 1 d . . .
H10A H 0.5542 0.5337 0.8648 0.071 Uiso 1 1 calc R . .
C11 C 0.5824(3) 0.0249(6) 0.6960(3) 0.0625(13) Uani 1 1 d . . .
H11A H 0.5889 0.1106 0.7117 0.075 Uiso 1 1 calc R . .
C12 C 0.6139(3) -0.0713(4) 0.7493(2) 0.0440(10) Uani 1 1 d . . .
C13 C 0.6022(3) -0.1976(5) 0.7231(3) 0.0607(13) Uani 1 1 d . . .
H13A H 0.6226 -0.2644 0.7581 0.073 Uiso 1 1 calc R . .
C14 C 0.5613(3) -0.2270(6) 0.6468(3) 0.0703(15) Uani 1 1 d . . .
H14A H 0.5546 -0.3125 0.6306 0.084 Uiso 1 1 calc R . .
C15 C 0.5306(3) -0.1294(7) 0.5947(3) 0.0710(16) Uani 1 1 d . . .
H15A H 0.5027 -0.1482 0.5430 0.085 Uiso 1 1 calc R . .
C16 C 0.5411(4) -0.0044(6) 0.6193(3) 0.0714(16) Uani 1 1 d . . .
H16A H 0.5202 0.0619 0.5841 0.086 Uiso 1 1 calc R . .
C17 C 0.7508(3) -0.0785(4) 0.8605(2) 0.0461(10) Uani 1 1 d . . .
C18 C 0.7908(3) -0.1124(5) 0.9367(3) 0.0556(12) Uani 1 1 d . . .
H18A H 0.7617 -0.1168 0.9700 0.067 Uiso 1 1 calc R . .
C19 C 0.8728(3) -0.1395(6) 0.9639(3) 0.0707(16) Uani 1 1 d . . .
H19A H 0.8986 -0.1623 1.0153 0.085 Uiso 1 1 calc R . .
C20 C 0.9167(3) -0.1332(6) 0.9158(4) 0.0758(17) Uani 1 1 d . . .
H20A H 0.9723 -0.1516 0.9344 0.091 Uiso 1 1 calc R . .
C21 C 0.8782(3) -0.0996(5) 0.8400(3) 0.0681(15) Uani 1 1 d . . .
H21A H 0.9078 -0.0951 0.8071 0.082 Uiso 1 1 calc R . .
C22 C 0.7954(3) -0.0724(5) 0.8123(3) 0.0585(13) Uani 1 1 d . . .
H22A H 0.7697 -0.0498 0.7608 0.070 Uiso 1 1 calc R . .
C23 C 0.4059(3) -0.0637(4) 0.9053(2) 0.0438(10) Uani 1 1 d . . .
C24 C 0.3508(3) -0.1407(5) 0.9259(3) 0.0562(12) Uani 1 1 d . . .
H24A H 0.2997 -0.1075 0.9207 0.067 Uiso 1 1 calc R . .
C25 C 0.3702(3) -0.2627(5) 0.9533(3) 0.0627(14) Uani 1 1 d . . .
H25A H 0.3327 -0.3129 0.9661 0.075 Uiso 1 1 calc R . .
C26 C 0.4463(3) -0.3103(5) 0.9618(3) 0.0639(14) Uani 1 1 d . . .
H26A H 0.4604 -0.3932 0.9811 0.077 Uiso 1 1 calc R . .
C27 C 0.5015(3) -0.2387(5) 0.9426(3) 0.0576(12) Uani 1 1 d . . .
H27A H 0.5526 -0.2735 0.9492 0.069 Uiso 1 1 calc R . .
C28 C 0.4829(3) -0.1134(4) 0.9129(2) 0.0442(10) Uani 1 1 d . . .
C29 C 0.2996(3) 0.2920(5) 0.8253(3) 0.0505(11) Uani 1 1 d . . .
C30 C 0.2923(4) 0.3550(6) 0.8883(3) 0.0696(15) Uani 1 1 d . . .
H30A H 0.3389 0.3847 0.9272 0.084 Uiso 1 1 calc R . .
C31 C 0.2165(5) 0.3742(7) 0.8941(4) 0.092(2) Uani 1 1 d . . .
H31A H 0.2125 0.4151 0.9372 0.111 Uiso 1 1 calc R . .
C32 C 0.1479(4) 0.3338(7) 0.8370(4) 0.086(2) Uani 1 1 d . . .
H32A H 0.0970 0.3481 0.8409 0.103 Uiso 1 1 calc R . .
C33 C 0.1535(3) 0.2723(6) 0.7742(3) 0.0711(16) Uani 1 1 d . . .
H33A H 0.1063 0.2447 0.7352 0.085 Uiso 1 1 calc R . .
C34 C 0.2289(3) 0.2509(5) 0.7683(3) 0.0604(13) Uani 1 1 d . . .
H34A H 0.2322 0.2082 0.7254 0.072 Uiso 1 1 calc R . .
C35 C 0.3823(3) 0.2912(5) 0.7388(3) 0.0499(11) Uani 1 1 d . . .
C36 C 0.3749(3) 0.1930(6) 0.6882(3) 0.0639(14) Uani 1 1 d . . .
H36A H 0.3739 0.1082 0.7041 0.077 Uiso 1 1 calc R . .
C37 C 0.3686(4) 0.2186(7) 0.6123(3) 0.0779(17) Uani 1 1 d . . .
H37A H 0.3634 0.1505 0.5782 0.094 Uiso 1 1 calc R . .
C38 C 0.3785(4) 0.4415(7) 0.6394(4) 0.0837(19) Uani 1 1 d . . .
H38A H 0.3804 0.5260 0.6233 0.100 Uiso 1 1 calc R . .
C39 C 0.3839(3) 0.4177(5) 0.7134(3) 0.0674(14) Uani 1 1 d . . .
H39A H 0.3887 0.4862 0.7472 0.081 Uiso 1 1 calc R . .
C40 C 0.3700(4) 0.3408(8) 0.5879(4) 0.083(2) Uani 1 1 d . . .
H40A H 0.3653 0.3573 0.5372 0.100 Uiso 1 1 calc R . .
N1 N 0.6421(2) 0.0862(3) 0.85620(19) 0.0424(8) Uani 1 1 d . . .
N2 N 0.4237(2) 0.1454(4) 0.85317(19) 0.0438(8) Uani 1 1 d . . .
Ni1 Ni 0.53583(3) 0.11808(6) 0.86208(3) 0.04339(18) Uani 1 1 d . . .
O1 O 0.54398(19) 0.2905(3) 0.8475(2) 0.0601(9) Uani 1 1 d . . .
O2 O 0.53664(19) -0.0484(3) 0.8928(2) 0.0557(8) Uani 1 1 d . . .
H2 H 0.329(3) 0.077(5) 0.870(3) 0.067 Uiso 1 1 d . . .
H1 H 0.750(3) 0.157(5) 0.866(3) 0.067 Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.289(6) . ?
C1 C6 1.432(6) . ?
C1 H1 0.94(5) . ?
C2 N2 1.288(6) . ?
C2 C23 1.429(6) . ?
C2 H2 0.91(5) . ?
C3 N1 1.507(5) . ?
C3 C17 1.517(6) . ?
C3 C12 1.525(6) . ?
C3 H3A 0.9800 . ?
C4 N2 1.505(5) . ?
C4 C35 1.522(6) . ?
C4 C29 1.523(6) . ?
C4 H4A 0.9800 . ?
C5 O1 1.307(5) . ?
C5 C10 1.406(6) . ?
C5 C6 1.410(6) . ?
C6 C7 1.398(6) . ?
C7 C8 1.376(7) . ?
C7 H7A 0.9300 . ?
C8 C9 1.380(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.360(7) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C11 C12 1.374(7) . ?
C11 C16 1.383(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.387(7) . ?
C13 C14 1.376(7) . ?
C13 H13A 0.9300 . ?
C14 C15 1.371(8) . ?
C14 H14A 0.9300 . ?
C15 C16 1.364(8) . ?
C15 H15A 0.9300 . ?
C16 H16A 0.9300 . ?
C17 C22 1.380(6) . ?
C17 C18 1.383(6) . ?
C18 C19 1.370(7) . ?
C18 H18A 0.9300 . ?
C19 C20 1.367(8) . ?
C19 H19A 0.9300 . ?
C20 C21 1.373(8) . ?
C20 H20A 0.9300 . ?
C21 C22 1.384(7) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C23 C28 1.401(6) . ?
C23 C24 1.404(6) . ?
C24 C25 1.360(7) . ?
C24 H24A 0.9300 . ?
C25 C26 1.376(7) . ?
C25 H25A 0.9300 . ?
C26 C27 1.360(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.403(6) . ?
C27 H27A 0.9300 . ?
C28 O2 1.313(5) . ?
C29 C34 1.381(7) . ?
C29 C30 1.383(7) . ?
C30 C31 1.380(8) . ?
C30 H30A 0.9300 . ?
C31 C32 1.357(9) . ?
C31 H31A 0.9300 . ?
C32 C33 1.360(9) . ?
C32 H32A 0.9300 . ?
C33 C34 1.379(7) . ?
C33 H33A 0.9300 . ?
C34 H34A 0.9300 . ?
C35 C36 1.360(7) . ?
C35 C39 1.397(7) . ?
C36 C37 1.397(7) . ?
C36 H36A 0.9300 . ?
C37 C40 1.348(9) . ?
C37 H37A 0.9300 . ?
C38 C39 1.364(8) . ?
C38 C40 1.387(9) . ?
C38 H38A 0.9300 . ?
C39 H39A 0.9300 . ?
C40 H40A 0.9300 . ?
N1 Ni1 1.927(4) . ?
N2 Ni1 1.930(4) . ?
Ni1 O2 1.816(3) . ?
Ni1 O1 1.821(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C6 125.9(4) . . ?
N1 C1 H1 124(3) . . ?
C6 C1 H1 110(3) . . ?
N2 C2 C23 127.5(4) . . ?
N2 C2 H2 122(3) . . ?
C23 C2 H2 111(3) . . ?
N1 C3 C17 113.9(3) . . ?
N1 C3 C12 109.8(3) . . ?
C17 C3 C12 114.1(3) . . ?
N1 C3 H3A 106.1 . . ?
C17 C3 H3A 106.1 . . ?
C12 C3 H3A 106.1 . . ?
N2 C4 C35 111.0(4) . . ?
N2 C4 C29 114.6(4) . . ?
C35 C4 C29 111.0(3) . . ?
N2 C4 H4A 106.6 . . ?
C35 C4 H4A 106.6 . . ?
C29 C4 H4A 106.6 . . ?
O1 C5 C10 119.9(4) . . ?
O1 C5 C6 122.6(4) . . ?
C10 C5 C6 117.5(4) . . ?
C7 C6 C5 119.8(4) . . ?
C7 C6 C1 119.4(4) . . ?
C5 C6 C1 120.7(4) . . ?
C8 C7 C6 121.7(5) . . ?
C8 C7 H7A 119.2 . . ?
C6 C7 H7A 119.2 . . ?
C7 C8 C9 117.7(5) . . ?
C7 C8 H8A 121.1 . . ?
C9 C8 H8A 121.1 . . ?
C10 C9 C8 122.6(5) . . ?
C10 C9 H9A 118.7 . . ?
C8 C9 H9A 118.7 . . ?
C9 C10 C5 120.7(5) . . ?
C9 C10 H10A 119.6 . . ?
C5 C10 H10A 119.6 . . ?
C12 C11 C16 120.8(5) . . ?
C12 C11 H11A 119.6 . . ?
C16 C11 H11A 119.6 . . ?
C11 C12 C13 117.5(4) . . ?
C11 C12 C3 124.2(4) . . ?
C13 C12 C3 118.3(4) . . ?
C14 C13 C12 121.8(5) . . ?
C14 C13 H13A 119.1 . . ?
C12 C13 H13A 119.1 . . ?
C15 C14 C13 119.6(5) . . ?
C15 C14 H14A 120.2 . . ?
C13 C14 H14A 120.2 . . ?
C16 C15 C14 119.5(5) . . ?
C16 C15 H15A 120.3 . . ?
C14 C15 H15A 120.3 . . ?
C15 C16 C11 120.8(5) . . ?
C15 C16 H16A 119.6 . . ?
C11 C16 H16A 119.6 . . ?
C22 C17 C18 118.4(4) . . ?
C22 C17 C3 123.4(4) . . ?
C18 C17 C3 118.2(4) . . ?
C19 C18 C17 121.1(5) . . ?
C19 C18 H18A 119.4 . . ?
C17 C18 H18A 119.4 . . ?
C20 C19 C18 120.3(5) . . ?
C20 C19 H19A 119.9 . . ?
C18 C19 H19A 119.9 . . ?
C19 C20 C21 119.6(5) . . ?
C19 C20 H20A 120.2 . . ?
C21 C20 H20A 120.2 . . ?
C20 C21 C22 120.3(5) . . ?
C20 C21 H21A 119.9 . . ?
C22 C21 H21A 119.9 . . ?
C17 C22 C21 120.4(5) . . ?
C17 C22 H22A 119.8 . . ?
C21 C22 H22A 119.8 . . ?
C28 C23 C24 119.4(4) . . ?
C28 C23 C2 121.3(4) . . ?
C24 C23 C2 119.2(4) . . ?
C25 C24 C23 121.7(5) . . ?
C25 C24 H24A 119.2 . . ?
C23 C24 H24A 119.2 . . ?
C24 C25 C26 118.7(5) . . ?
C24 C25 H25A 120.6 . . ?
C26 C25 H25A 120.6 . . ?
C27 C26 C25 121.4(5) . . ?
C27 C26 H26A 119.3 . . ?
C25 C26 H26A 119.3 . . ?
C26 C27 C28 121.3(5) . . ?
C26 C27 H27A 119.3 . . ?
C28 C27 H27A 119.3 . . ?
O2 C28 C23 122.8(4) . . ?
O2 C28 C27 119.7(4) . . ?
C23 C28 C27 117.5(4) . . ?
C34 C29 C30 117.9(5) . . ?
C34 C29 C4 122.6(4) . . ?
C30 C29 C4 119.5(4) . . ?
C31 C30 C29 120.7(6) . . ?
C31 C30 H30A 119.7 . . ?
C29 C30 H30A 119.7 . . ?
C32 C31 C30 120.3(6) . . ?
C32 C31 H31A 119.8 . . ?
C30 C31 H31A 119.8 . . ?
C31 C32 C33 120.2(6) . . ?
C31 C32 H32A 119.9 . . ?
C33 C32 H32A 119.9 . . ?
C32 C33 C34 120.1(6) . . ?
C32 C33 H33A 120.0 . . ?
C34 C33 H33A 120.0 . . ?
C33 C34 C29 120.9(5) . . ?
C33 C34 H34A 119.5 . . ?
C29 C34 H34A 119.5 . . ?
C36 C35 C39 118.6(5) . . ?
C36 C35 C4 123.6(4) . . ?
C39 C35 C4 117.7(5) . . ?
C35 C36 C37 120.5(6) . . ?
C35 C36 H36A 119.8 . . ?
C37 C36 H36A 119.8 . . ?
C40 C37 C36 120.8(6) . . ?
C40 C37 H37A 119.6 . . ?
C36 C37 H37A 119.6 . . ?
C39 C38 C40 120.6(6) . . ?
C39 C38 H38A 119.7 . . ?
C40 C38 H38A 119.7 . . ?
C38 C39 C35 120.4(6) . . ?
C38 C39 H39A 119.8 . . ?
C35 C39 H39A 119.8 . . ?
C37 C40 C38 119.1(6) . . ?
C37 C40 H40A 120.5 . . ?
C38 C40 H40A 120.5 . . ?
C1 N1 C3 117.8(4) . . ?
C1 N1 Ni1 124.1(3) . . ?
C3 N1 Ni1 118.0(3) . . ?
C2 N2 C4 118.2(4) . . ?
C2 N2 Ni1 123.6(3) . . ?
C4 N2 Ni1 118.2(3) . . ?
O2 Ni1 O1 170.83(16) . . ?
O2 Ni1 N1 87.33(15) . . ?
O1 Ni1 N1 91.86(15) . . ?
O2 Ni1 N2 93.55(15) . . ?
O1 Ni1 N2 88.48(15) . . ?
N1 Ni1 N2 172.24(14) . . ?
C5 O1 Ni1 128.3(3) . . ?
C28 O2 Ni1 130.5(3) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        26.63
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.509
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.075
####################################################################### 
# 
# 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_t_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1843971'
_audit_update_record             
;
2018-05-18 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H38 N2 Ni O2'
_chemical_formula_sum            'C42 H38 N2 Ni O2'
_chemical_formula_weight         661.43

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
_symmetry_space_group_name_Hall  '-P 2yn  '

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                   7.6601(6)
_cell_length_b                   13.1771(10)
_cell_length_c                   16.4976(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.9180(10)
_cell_angle_gamma                90.00
_cell_volume                     1645.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5687
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.44

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696.0
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14543
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         27.59
_reflns_number_total             3798
_reflns_number_gt                3058
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1000P)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_number_reflns         3798
_refine_ls_number_parameters     214
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1499
_refine_ls_wR_factor_gt          0.1371
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 1.0000 1.0000 0.0000 0.03043(15) Uani 1 2 d S . .
O1 O 0.86651(19) 1.10708(11) 0.02891(10) 0.0407(4) Uani 1 1 d . . .
N1 N 0.9131(2) 0.91140(13) 0.07761(10) 0.0342(4) Uani 1 1 d . . .
C1 C 1.3824(4) 0.8982(2) 0.33136(18) 0.0632(7) Uani 1 1 d . . .
H1A H 1.4634 0.9146 0.3775 0.076 Uiso 1 1 calc R . .
C2 C 1.3972(4) 0.8082(2) 0.2909(2) 0.0684(8) Uani 1 1 d . . .
H2A H 1.4870 0.7628 0.3104 0.082 Uiso 1 1 calc R . .
C3 C 1.2781(4) 0.7849(2) 0.22105(17) 0.0572(7) Uani 1 1 d . . .
H3A H 1.2896 0.7241 0.1937 0.069 Uiso 1 1 calc R . .
C4 C 1.1422(3) 0.85125(16) 0.19138(13) 0.0395(5) Uani 1 1 d . . .
C5 C 1.1284(3) 0.94050(19) 0.23352(16) 0.0512(6) Uani 1 1 d . . .
H5A H 1.0380 0.9860 0.2151 0.061 Uiso 1 1 calc R . .
C6 C 1.2488(4) 0.9631(3) 0.30354(18) 0.0640(7) Uani 1 1 d . . .
H6A H 1.2376 1.0234 0.3315 0.077 Uiso 1 1 calc R . .
C7 C 1.0193(3) 0.82196(15) 0.11316(13) 0.0371(4) Uani 1 1 d . . .
H7A H 1.0962 0.8037 0.0731 0.045 Uiso 1 1 calc R . .
C8 C 0.7551(4) 0.5813(2) 0.0605(2) 0.0645(7) Uani 1 1 d . . .
H8A H 0.7248 0.5398 0.0149 0.077 Uiso 1 1 calc R . .
C9 C 0.6977(4) 0.5580(2) 0.1332(2) 0.0657(8) Uani 1 1 d . . .
H9A H 0.6259 0.5018 0.1367 0.079 Uiso 1 1 calc R . .
C10 C 0.7472(4) 0.6182(2) 0.20053(18) 0.0635(7) Uani 1 1 d . . .
H10A H 0.7106 0.6016 0.2500 0.076 Uiso 1 1 calc R . .
C11 C 0.8507(4) 0.70327(19) 0.19595(15) 0.0512(6) Uani 1 1 d . . .
H11A H 0.8822 0.7436 0.2422 0.061 Uiso 1 1 calc R . .
C12 C 0.9082(3) 0.72904(15) 0.12252(13) 0.0389(5) Uani 1 1 d . . .
C13 C 0.8586(3) 0.66708(18) 0.05532(16) 0.0508(6) Uani 1 1 d . . .
H13A H 0.8951 0.6831 0.0057 0.061 Uiso 1 1 calc R . .
C14 C 0.6754(4) 1.28979(19) 0.0241(2) 0.0631(7) Uani 1 1 d . . .
H14A H 0.5904 1.3423 0.0283 0.095 Uiso 1 1 calc R . .
H14B H 0.6888 1.2810 -0.0324 0.095 Uiso 1 1 calc R . .
H14C H 0.7870 1.3084 0.0554 0.095 Uiso 1 1 calc R . .
C15 C 0.6124(3) 1.19176(16) 0.05693(13) 0.0402(5) Uani 1 1 d . . .
C16 C 0.4524(3) 1.18737(18) 0.08641(15) 0.0461(5) Uani 1 1 d . . .
H16A H 0.3851 1.2462 0.0861 0.055 Uiso 1 1 calc R . .
C17 C 0.3890(3) 1.0985(2) 0.11640(15) 0.0488(6) Uani 1 1 d . . .
H17A H 0.2801 1.0976 0.1347 0.059 Uiso 1 1 calc R . .
C18 C 0.4889(3) 1.01283(17) 0.11864(16) 0.0436(5) Uani 1 1 d . . .
H18A H 0.4484 0.9532 0.1394 0.052 Uiso 1 1 calc R . .
C19 C 0.6534(3) 1.01337(15) 0.08979(14) 0.0357(5) Uani 1 1 d . . .
C20 C 0.7143(3) 1.10295(15) 0.05732(12) 0.0337(4) Uani 1 1 d . . .
C21 C 0.7617(3) 0.92535(16) 0.10190(13) 0.0366(4) Uani 1 1 d . . .
H21A H 0.7829 0.9142 0.1607 0.044 Uiso 1 1 calc R . .
H21B H 0.6875 0.8697 0.0787 0.044 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 O1 1.8480(14) 3_775 ?
Ni1 O1 1.8480(14) . ?
Ni1 N1 1.9261(16) . ?
Ni1 N1 1.9261(16) 3_775 ?
O1 C20 1.323(2) . ?
N1 C21 1.298(3) . ?
N1 C7 1.499(2) . ?
C1 C6 1.358(4) . ?
C1 C2 1.374(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.389(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.389(3) . ?
C3 H3A 0.9300 . ?
C4 C5 1.379(3) . ?
C4 C7 1.524(3) . ?
C5 C6 1.394(4) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C12 1.513(3) . ?
C7 H7A 0.9800 . ?
C8 C9 1.375(4) . ?
C8 C13 1.391(4) . ?
C8 H8A 0.9300 . ?
C9 C10 1.369(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.382(3) . ?
C10 H10A 0.9300 . ?
C11 C12 1.394(3) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(3) . ?
C13 H13A 0.9300 . ?
C14 C15 1.509(3) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 C16 1.388(3) . ?
C15 C20 1.406(3) . ?
C16 C17 1.387(4) . ?
C16 H16A 0.9300 . ?
C17 C18 1.361(3) . ?
C17 H17A 0.9300 . ?
C18 C19 1.414(3) . ?
C18 H18A 0.9300 . ?
C19 C20 1.406(3) . ?
C19 C21 1.422(3) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.00(9) 3_775 . ?
O1 Ni1 N1 88.33(7) 3_775 . ?
O1 Ni1 N1 91.67(7) . . ?
O1 Ni1 N1 91.67(7) 3_775 3_775 ?
O1 Ni1 N1 88.33(7) . 3_775 ?
N1 Ni1 N1 180.00(8) . 3_775 ?
C20 O1 Ni1 127.81(13) . . ?
C21 N1 C7 116.59(16) . . ?
C21 N1 Ni1 122.49(14) . . ?
C7 N1 Ni1 120.92(13) . . ?
C6 C1 C2 119.6(3) . . ?
C6 C1 H1A 120.2 . . ?
C2 C1 H1A 120.2 . . ?
C1 C2 C3 120.0(2) . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C4 C3 C2 120.9(3) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C5 C4 C3 118.1(2) . . ?
C5 C4 C7 123.86(19) . . ?
C3 C4 C7 118.0(2) . . ?
C4 C5 C6 120.5(2) . . ?
C4 C5 H5A 119.8 . . ?
C6 C5 H5A 119.8 . . ?
C1 C6 C5 120.8(3) . . ?
C1 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
N1 C7 C12 113.33(16) . . ?
N1 C7 C4 111.02(17) . . ?
C12 C7 C4 113.70(17) . . ?
N1 C7 H7A 106.0 . . ?
C12 C7 H7A 106.0 . . ?
C4 C7 H7A 106.0 . . ?
C9 C8 C13 119.8(3) . . ?
C9 C8 H8A 120.1 . . ?
C13 C8 H8A 120.1 . . ?
C10 C9 C8 119.5(2) . . ?
C10 C9 H9A 120.2 . . ?
C8 C9 H9A 120.2 . . ?
C9 C10 C11 121.0(3) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 H10A 119.5 . . ?
C10 C11 C12 120.4(2) . . ?
C10 C11 H11A 119.8 . . ?
C12 C11 H11A 119.8 . . ?
C13 C12 C11 118.0(2) . . ?
C13 C12 C7 119.0(2) . . ?
C11 C12 C7 123.0(2) . . ?
C12 C13 C8 121.3(2) . . ?
C12 C13 H13A 119.4 . . ?
C8 C13 H13A 119.4 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C20 118.9(2) . . ?
C16 C15 C14 120.7(2) . . ?
C20 C15 C14 120.4(2) . . ?
C17 C16 C15 122.5(2) . . ?
C17 C16 H16A 118.8 . . ?
C15 C16 H16A 118.8 . . ?
C18 C17 C16 118.9(2) . . ?
C18 C17 H17A 120.5 . . ?
C16 C17 H17A 120.5 . . ?
C17 C18 C19 120.9(2) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C20 C19 C18 119.89(19) . . ?
C20 C19 C21 121.2(2) . . ?
C18 C19 C21 118.65(19) . . ?
O1 C20 C19 122.17(19) . . ?
O1 C20 C15 118.89(18) . . ?
C19 C20 C15 118.91(18) . . ?
N1 C21 C19 127.02(19) . . ?
N1 C21 H21A 105.6 . . ?
C19 C21 H21A 105.6 . . ?
N1 C21 H21B 105.6 . . ?
C19 C21 H21B 105.6 . . ?
H21A C21 H21B 106.1 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.063
####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1575909'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H36 N2 Ni O2'
_chemical_formula_weight         659.44

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/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                   11.0313(11)
_cell_length_b                   11.2443(11)
_cell_length_c                   13.3797(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.0940(10)
_cell_angle_gamma                90.00
_cell_volume                     1638.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8861
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      29.51

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             692
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8580
_exptl_absorpt_correction_T_max  0.9111
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12279
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3050
_reflns_number_gt                2774
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0497P)²+0.5220P] 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         3050
_refine_ls_number_parameters     215
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0864
_refine_ls_wR_factor_gt          0.0836
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.001

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 0.5000 0.0000 0.0000 0.02816(11) Uani 1 2 d S . .
C1 C 0.31159(15) 0.27094(15) 0.03174(12) 0.0331(3) Uani 1 1 d . . .
C6 C 0.18584(17) 0.28872(18) 0.00513(15) 0.0465(4) Uani 1 1 d . . .
H6 H 0.1315 0.2399 0.0325 0.056 Uiso 1 1 calc R . .
C4 C 0.2194(2) 0.4522(2) -0.10132(15) 0.0577(6) Uani 1 1 d . . .
H4 H 0.1888 0.5129 -0.1454 0.069 Uiso 1 1 calc R . .
C2 C 0.38979(17) 0.34570(17) -0.00974(14) 0.0435(4) Uani 1 1 d . . .
H2 H 0.4742 0.3354 0.0066 0.052 Uiso 1 1 calc R . .
C5 C 0.1406(2) 0.3781(2) -0.06162(17) 0.0581(5) Uani 1 1 d . . .
H5 H 0.0562 0.3880 -0.0796 0.070 Uiso 1 1 calc R . .
C3 C 0.3434(2) 0.43620(19) -0.07564(15) 0.0547(5) Uani 1 1 d . . .
H3 H 0.3971 0.4863 -0.1025 0.066 Uiso 1 1 calc R . .
C8 C 0.34002(13) 0.19480(14) 0.21370(12) 0.0301(3) Uani 1 1 d . . .
C7 C 0.35384(13) 0.16963(14) 0.10409(12) 0.0305(3) Uani 1 1 d . . .
H7 H 0.2985 0.1031 0.0826 0.037 Uiso 1 1 calc R . .
C10 C 0.34458(17) 0.32198(18) 0.35949(14) 0.0454(4) Uani 1 1 d . . .
H10 H 0.3580 0.3965 0.3893 0.054 Uiso 1 1 calc R . .
C9 C 0.35661(16) 0.30634(15) 0.25829(13) 0.0373(4) Uani 1 1 d . . .
H9 H 0.3759 0.3710 0.2203 0.045 Uiso 1 1 calc R . .
C12 C 0.29475(19) 0.1165(2) 0.37128(15) 0.0516(5) Uani 1 1 d . . .
H12 H 0.2726 0.0526 0.4087 0.062 Uiso 1 1 calc R . .
C13 C 0.30947(15) 0.10043(16) 0.27170(14) 0.0396(4) Uani 1 1 d . . .
H13 H 0.2987 0.0251 0.2430 0.048 Uiso 1 1 calc R . .
C11 C 0.31302(19) 0.2277(2) 0.41553(14) 0.0516(5) Uani 1 1 d . . .
H11 H 0.3040 0.2386 0.4829 0.062 Uiso 1 1 calc R . .
N1 N 0.48005(11) 0.12684(11) 0.09322(10) 0.0291(3) Uani 1 1 d . . .
C15 C 0.69826(14) 0.15795(14) 0.15145(11) 0.0307(3) Uani 1 1 d . . .
C16 C 0.78471(15) 0.23586(15) 0.20605(12) 0.0353(4) Uani 1 1 d . . .
H16 H 0.7568 0.3020 0.2374 0.042 Uiso 1 1 calc R . .
C20 C 0.73800(14) 0.05564(15) 0.10580(12) 0.0334(3) Uani 1 1 d . . .
C14 C 0.57044(14) 0.18200(14) 0.14744(12) 0.0321(3) Uani 1 1 d . . .
H14 H 0.5500 0.2437 0.1880 0.039 Uiso 1 1 calc R . .
C17 C 0.90893(15) 0.21693(17) 0.21435(13) 0.0395(4) Uani 1 1 d . . .
C19 C 0.86502(16) 0.03347(18) 0.11956(15) 0.0432(4) Uani 1 1 d . . .
H19 H 0.8941 -0.0357 0.0935 0.052 Uiso 1 1 calc R . .
C18 C 0.94669(15) 0.11302(18) 0.17117(14) 0.0438(4) Uani 1 1 d . . .
H18 H 1.0303 0.0970 0.1775 0.053 Uiso 1 1 calc R . .
C21 C 1.00094(18) 0.3032(2) 0.27005(19) 0.0591(6) Uani 1 1 d . . .
H21A H 1.0528 0.3331 0.2245 0.089 Uiso 1 1 calc R . .
H21B H 1.0502 0.2631 0.3255 0.089 Uiso 1 1 calc R . .
H21C H 0.9582 0.3681 0.2955 0.089 Uiso 1 1 calc R . .
O1 O 0.66224(11) -0.01880(11) 0.05279(10) 0.0428(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.8295(12) . ?
Ni1 O1 1.8295(12) 3_655 ?
Ni1 N1 1.9300(13) 3_655 ?
Ni1 N1 1.9300(13) . ?
C1 C2 1.382(3) . ?
C1 C6 1.391(2) . ?
C1 C7 1.520(2) . ?
C6 C5 1.385(3) . ?
C6 H6 0.9300 . ?
C4 C5 1.370(3) . ?
C4 C3 1.369(3) . ?
C4 H4 0.9300 . ?
C2 C3 1.390(3) . ?
C2 H2 0.9300 . ?
C5 H5 0.9300 . ?
C3 H3 0.9300 . ?
C8 C9 1.388(2) . ?
C8 C13 1.387(2) . ?
C8 C7 1.525(2) . ?
C7 N1 1.5017(19) . ?
C7 H7 0.9800 . ?
C10 C11 1.374(3) . ?
C10 C9 1.392(3) . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?
C12 C13 1.379(3) . ?
C12 C11 1.385(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C11 H11 0.9300 . ?
N1 C14 1.295(2) . ?
C15 C20 1.405(2) . ?
C15 C16 1.411(2) . ?
C15 C14 1.428(2) . ?
C16 C17 1.374(2) . ?
C16 H16 0.9300 . ?
C20 O1 1.309(2) . ?
C20 C19 1.406(2) . ?
C14 H14 0.9300 . ?
C17 C18 1.396(3) . ?
C17 C21 1.512(2) . ?
C19 C18 1.375(3) . ?
C19 H19 0.9300 . ?
C18 H18 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.0 . 3_655 ?
O1 Ni1 N1 87.69(5) . 3_655 ?
O1 Ni1 N1 92.31(5) 3_655 3_655 ?
O1 Ni1 N1 92.32(5) . . ?
O1 Ni1 N1 87.69(5) 3_655 . ?
N1 Ni1 N1 180.0 3_655 . ?
C2 C1 C6 118.05(16) . . ?
C2 C1 C7 124.31(15) . . ?
C6 C1 C7 117.63(15) . . ?
C5 C6 C1 120.86(19) . . ?
C5 C6 H6 119.6 . . ?
C1 C6 H6 119.6 . . ?
C5 C4 C3 119.57(19) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C1 C2 C3 120.62(18) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C9 C8 C13 118.54(15) . . ?
C9 C8 C7 123.68(15) . . ?
C13 C8 C7 117.78(15) . . ?
N1 C7 C1 111.97(12) . . ?
N1 C7 C8 112.82(12) . . ?
C1 C7 C8 113.97(13) . . ?
N1 C7 H7 105.7 . . ?
C1 C7 H7 105.7 . . ?
C8 C7 H7 105.7 . . ?
C11 C10 C9 120.29(18) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C8 C9 C10 120.36(17) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C13 C12 C11 119.98(18) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C8 121.09(17) . . ?
C12 C13 H13 119.5 . . ?
C8 C13 H13 119.5 . . ?
C10 C11 C12 119.71(17) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C14 N1 C7 115.84(13) . . ?
C14 N1 Ni1 124.03(11) . . ?
C7 N1 Ni1 120.10(9) . . ?
C20 C15 C16 120.11(14) . . ?
C20 C15 C14 120.85(14) . . ?
C16 C15 C14 118.98(15) . . ?
C17 C16 C15 121.99(16) . . ?
C17 C16 H16 119.0 . . ?
C15 C16 H16 119.0 . . ?
O1 C20 C15 122.86(14) . . ?
O1 C20 C19 119.67(15) . . ?
C15 C20 C19 117.47(15) . . ?
N1 C14 C15 126.77(15) . . ?
N1 C14 H14 116.6 . . ?
C15 C14 H14 116.6 . . ?
C16 C17 C18 117.08(16) . . ?
C16 C17 C21 121.58(17) . . ?
C18 C17 C21 121.32(16) . . ?
C18 C19 C20 120.69(17) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C19 C18 C17 122.52(16) . . ?
C19 C18 H18 118.7 . . ?
C17 C18 H18 118.7 . . ?
C17 C21 H21A 109.5 . . ?
C17 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C17 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 O1 Ni1 129.56(11) . . ?

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
C2 C1 C6 C5 0.5(3) . . . . ?
C7 C1 C6 C5 -179.01(17) . . . . ?
C6 C1 C2 C3 0.3(3) . . . . ?
C7 C1 C2 C3 179.84(17) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C1 C6 C5 C4 -1.1(3) . . . . ?
C5 C4 C3 C2 0.0(3) . . . . ?
C1 C2 C3 C4 -0.6(3) . . . . ?
C2 C1 C7 N1 -23.6(2) . . . . ?
C6 C1 C7 N1 155.92(15) . . . . ?
C2 C1 C7 C8 106.00(18) . . . . ?
C6 C1 C7 C8 -74.51(19) . . . . ?
C9 C8 C7 N1 94.09(18) . . . . ?
C13 C8 C7 N1 -85.73(17) . . . . ?
C9 C8 C7 C1 -35.1(2) . . . . ?
C13 C8 C7 C1 145.12(15) . . . . ?
C13 C8 C9 C10 1.0(2) . . . . ?
C7 C8 C9 C10 -178.81(15) . . . . ?
C11 C10 C9 C8 -1.7(3) . . . . ?
C11 C12 C13 C8 -1.4(3) . . . . ?
C9 C8 C13 C12 0.5(2) . . . . ?
C7 C8 C13 C12 -179.66(16) . . . . ?
C9 C10 C11 C12 0.9(3) . . . . ?
C13 C12 C11 C10 0.7(3) . . . . ?
C1 C7 N1 C14 87.68(16) . . . . ?
C8 C7 N1 C14 -42.49(19) . . . . ?
C1 C7 N1 Ni1 -90.68(14) . . . . ?
C8 C7 N1 Ni1 139.15(11) . . . . ?
O1 Ni1 N1 C14 14.04(14) . . . . ?
O1 Ni1 N1 C14 -165.96(14) 3_655 . . . ?
N1 Ni1 N1 C14 144(8) 3_655 . . . ?
O1 Ni1 N1 C7 -167.75(11) . . . . ?
O1 Ni1 N1 C7 12.25(11) 3_655 . . . ?
N1 Ni1 N1 C7 -38(8) 3_655 . . . ?
C20 C15 C16 C17 1.8(3) . . . . ?
C14 C15 C16 C17 178.92(16) . . . . ?
C16 C15 C20 O1 -178.81(16) . . . . ?
C14 C15 C20 O1 4.1(3) . . . . ?
C16 C15 C20 C19 1.8(2) . . . . ?
C14 C15 C20 C19 -175.27(16) . . . . ?
C7 N1 C14 C15 179.45(15) . . . . ?
Ni1 N1 C14 C15 -2.3(2) . . . . ?
C20 C15 C14 N1 -10.1(3) . . . . ?
C16 C15 C14 N1 172.80(16) . . . . ?
C15 C16 C17 C18 -3.6(3) . . . . ?
C15 C16 C17 C21 177.88(18) . . . . ?
O1 C20 C19 C18 177.13(18) . . . . ?
C15 C20 C19 C18 -3.5(3) . . . . ?
C20 C19 C18 C17 1.7(3) . . . . ?
C16 C17 C18 C19 1.9(3) . . . . ?
C21 C17 C18 C19 -179.6(2) . . . . ?
C15 C20 O1 Ni1 14.9(3) . . . . ?
C19 C20 O1 Ni1 -165.80(13) . . . . ?
O1 Ni1 O1 C20 95(2) 3_655 . . . ?
N1 Ni1 O1 C20 159.16(16) 3_655 . . . ?
N1 Ni1 O1 C20 -20.84(16) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.042
####################################################################### 
# 
# 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_t_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1851039'
_audit_update_record             
;
2018-06-22 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H30 Br2 N2 Ni O2'
_chemical_formula_sum            'C40 H30 Br2 N2 Ni O2'
_chemical_formula_weight         789.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '
_symmetry_space_group_name_Hall  '-P 2ybc  '

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

_cell_length_a                   17.8459(14)
_cell_length_b                   9.8816(7)
_cell_length_c                   20.2608(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.6450(10)
_cell_angle_gamma                90.00
_cell_volume                     3343.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3803
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      22.13

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1592.0
_exptl_absorpt_coefficient_mu    3.009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.491
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28519
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         27.76
_reflns_number_total             7821
_reflns_number_gt                4229
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1000P)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_number_reflns         7821
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.2086
_refine_ls_R_factor_gt           0.1327
_refine_ls_wR_factor_ref         0.3587
_refine_ls_wR_factor_gt          0.3291
_refine_ls_goodness_of_fit_ref   2.001
_refine_ls_restrained_S_all      2.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 1.0000 0.5000 0.0246(4) Uiso 1 2 d S . .
Ni2 Ni 0.0000 1.0000 0.5000 0.0334(5) Uiso 1 2 d S . .
Br1 Br 0.34412(7) 0.30345(13) 0.44309(6) 0.0549(4) Uiso 1 1 d . . .
Br2 Br 0.19525(10) 1.66342(18) 0.52457(9) 0.0865(6) Uiso 1 1 d . . .
O1 O 0.4662(4) 0.8673(7) 0.4340(3) 0.0376(16) Uiso 1 1 d . . .
O2 O -0.0107(5) 0.8338(8) 0.4583(4) 0.058(2) Uiso 1 1 d . . .
N1 N 0.4531(4) 0.9120(8) 0.5606(4) 0.0265(17) Uiso 1 1 d . . .
N2 N 0.0472(5) 1.0637(9) 0.4325(4) 0.0360(19) Uiso 1 1 d . . .
C1 C 0.2333(8) 1.0350(14) 0.6047(7) 0.062(3) Uiso 1 1 d . . .
H1A H 0.1900 1.0860 0.5765 0.075 Uiso 1 1 calc R . .
C2 C 0.3074(7) 1.0448(12) 0.5956(6) 0.050(3) Uiso 1 1 d . . .
H2A H 0.3134 1.1027 0.5617 0.060 Uiso 1 1 calc R . .
C3 C 0.3726(5) 0.9669(9) 0.6379(5) 0.029(2) Uiso 1 1 d . . .
C4 C 0.3609(7) 0.8857(11) 0.6867(5) 0.045(3) Uiso 1 1 d . . .
H4A H 0.4036 0.8349 0.7159 0.054 Uiso 1 1 calc R . .
C5 C 0.2866(7) 0.8755(13) 0.6945(6) 0.053(3) Uiso 1 1 d . . .
H5A H 0.2796 0.8161 0.7276 0.064 Uiso 1 1 calc R . .
C6 C 0.2248(8) 0.9519(13) 0.6542(6) 0.059(3) Uiso 1 1 d . . .
H6A H 0.1758 0.9471 0.6606 0.071 Uiso 1 1 calc R . .
C7 C 0.5229(5) 0.9428(10) 0.6904(4) 0.027(2) Uiso 1 1 d . . .
C8 C 0.5503(6) 1.0369(12) 0.7452(5) 0.047(3) Uiso 1 1 d . . .
H8A H 0.5255 1.1207 0.7413 0.056 Uiso 1 1 calc R . .
C9 C 0.6149(8) 1.0044(14) 0.8054(7) 0.066(4) Uiso 1 1 d . . .
H9A H 0.6315 1.0677 0.8416 0.079 Uiso 1 1 calc R . .
C10 C 0.6548(7) 0.8854(13) 0.8142(6) 0.055(3) Uiso 1 1 d . . .
H10A H 0.6980 0.8664 0.8551 0.066 Uiso 1 1 calc R . .
C11 C 0.6278(7) 0.7919(13) 0.7584(6) 0.056(3) Uiso 1 1 d . . .
H11A H 0.6529 0.7083 0.7619 0.067 Uiso 1 1 calc R . .
C12 C 0.5630(6) 0.8249(11) 0.6975(5) 0.040(2) Uiso 1 1 d . . .
H12A H 0.5469 0.7631 0.6606 0.048 Uiso 1 1 calc R . .
C13 C 0.4518(5) 0.9822(9) 0.6266(4) 0.026(2) Uiso 1 1 d . . .
H13A H 0.4579 1.0790 0.6192 0.032 Uiso 1 1 calc R . .
C14 C 0.4233(5) 0.7939(10) 0.5519(5) 0.031(2) Uiso 1 1 d . . .
H14A H 0.4023 0.7641 0.5854 0.037 Uiso 1 1 calc R . .
C15 C 0.4186(5) 0.7019(9) 0.4961(4) 0.027(2) Uiso 1 1 d . . .
C16 C 0.4407(5) 0.7476(10) 0.4386(5) 0.031(2) Uiso 1 1 d . . .
C17 C 0.4310(7) 0.6535(12) 0.3829(6) 0.050(3) Uiso 1 1 d . . .
H17A H 0.4438 0.6799 0.3440 0.060 Uiso 1 1 calc R . .
C18 C 0.4034(6) 0.5252(11) 0.3855(5) 0.043(3) Uiso 1 1 d . . .
H18A H 0.3984 0.4658 0.3486 0.051 Uiso 1 1 calc R . .
C19 C 0.3825(6) 0.4815(10) 0.4423(5) 0.034(2) Uiso 1 1 d . . .
C20 C 0.3901(6) 0.5690(10) 0.4959(5) 0.035(2) Uiso 1 1 d . . .
H20A H 0.3759 0.5403 0.5337 0.042 Uiso 1 1 calc R . .
C21 C -0.1241(8) 1.1437(14) 0.2201(7) 0.062(3) Uiso 1 1 d . . .
H21 H -0.1397 1.2300 0.2022 0.074 Uiso 1 1 calc R . .
C22 C -0.1674(7) 1.0315(13) 0.1871(6) 0.056(3) Uiso 1 1 d . . .
H22 H -0.2123 1.0409 0.1464 0.067 Uiso 1 1 calc R . .
C23 C -0.1440(8) 0.9107(14) 0.2144(7) 0.064(4) Uiso 1 1 d . . .
H23 H -0.1746 0.8359 0.1933 0.076 Uiso 1 1 calc R . .
C24 C -0.0753(7) 0.8905(12) 0.2735(6) 0.050(3) Uiso 1 1 d . . .
H24 H -0.0594 0.8038 0.2905 0.060 Uiso 1 1 calc R . .
C25 C -0.0316(6) 1.0018(10) 0.3063(5) 0.033(2) Uiso 1 1 d . . .
C26 C -0.0566(7) 1.1260(13) 0.2806(6) 0.053(3) Uiso 1 1 d . . .
H26 H -0.0283 1.2016 0.3037 0.064 Uiso 1 1 calc R . .
C27 C 0.1196(6) 0.9866(10) 0.3531(5) 0.032(2) Uiso 1 1 d . . .
C28 C 0.1941(7) 0.9581(12) 0.4063(6) 0.051(3) Uiso 1 1 d . . .
H28 H 0.1950 0.9405 0.4517 0.062 Uiso 1 1 calc R . .
C29 C 0.2645(7) 0.9553(12) 0.3945(6) 0.048(3) Uiso 1 1 d . . .
H29 H 0.3118 0.9317 0.4305 0.058 Uiso 1 1 calc R . .
C30 C 0.2651(7) 0.9881(12) 0.3276(6) 0.052(3) Uiso 1 1 d . . .
H30 H 0.3130 0.9878 0.3192 0.063 Uiso 1 1 calc R . .
C31 C 0.1947(7) 1.0211(11) 0.2743(6) 0.051(3) Uiso 1 1 d . . .
H31 H 0.1951 1.0440 0.2300 0.061 Uiso 1 1 calc R . .
C32 C 0.1223(7) 1.0199(11) 0.2869(6) 0.043(3) Uiso 1 1 d . . .
H32 H 0.0751 1.0419 0.2504 0.052 Uiso 1 1 calc R . .
C33 C 0.0455(5) 0.9762(10) 0.3716(5) 0.032(2) Uiso 1 1 d . . .
H33 H 0.0426 0.8824 0.3862 0.038 Uiso 1 1 calc R . .
C34 C 0.0817(6) 1.1787(10) 0.4358(6) 0.042(3) Uiso 1 1 d . . .
H34 H 0.1047 1.1951 0.4019 0.050 Uiso 1 1 calc R . .
C35 C 0.0887(6) 1.2840(11) 0.4855(5) 0.038(2) Uiso 1 1 d . . .
C36 C 0.1320(6) 1.4055(11) 0.4826(6) 0.046(3) Uiso 1 1 d . . .
H36 H 0.1572 1.4142 0.4496 0.056 Uiso 1 1 calc R . .
C37 C 0.1353(7) 1.5041(12) 0.5273(6) 0.048(3) Uiso 1 1 d . . .
C38 C 0.0969(7) 1.5000(13) 0.5753(6) 0.055(3) Uiso 1 1 d . . .
H38 H 0.0997 1.5741 0.6043 0.066 Uiso 1 1 calc R . .
C39 C -0.0500(6) 0.7245(11) 0.4648(5) 0.042(3) Uiso 1 1 d . . .
C40 C -0.0552(7) 0.6107(12) 0.4195(6) 0.048(3) Uiso 1 1 d . . .
H40 H -0.0298 0.6132 0.3866 0.058 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 O1 1.817(7) . ?
Ni1 O1 1.817(7) 3_676 ?
Ni1 N1 1.921(7) . ?
Ni1 N1 1.921(7) 3_676 ?
Ni2 O2 1.826(8) . ?
Ni2 O2 1.826(8) 3_576 ?
Ni2 N2 1.947(8) 3_576 ?
Ni2 N2 1.947(8) . ?
Br1 C19 1.890(10) . ?
Br2 C37 1.915(12) . ?
O1 C16 1.283(12) . ?
O2 C39 1.319(13) . ?
N1 C14 1.268(11) . ?
N1 C13 1.513(11) . ?
N2 C34 1.283(13) . ?
N2 C33 1.498(12) . ?
C1 C6 1.345(17) . ?
C1 C2 1.401(17) . ?
C1 H1A 0.9300 . ?
C2 C3 1.406(14) . ?
C2 H2A 0.9300 . ?
C3 C4 1.345(14) . ?
C3 C13 1.519(12) . ?
C4 C5 1.394(16) . ?
C4 H4A 0.9300 . ?
C5 C6 1.349(16) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 C12 1.347(13) . ?
C7 C8 1.397(14) . ?
C7 C13 1.509(11) . ?
C8 C9 1.389(15) . ?
C8 H8A 0.9300 . ?
C9 C10 1.354(16) . ?
C9 H9A 0.9300 . ?
C10 C11 1.407(16) . ?
C10 H10A 0.9300 . ?
C11 C12 1.399(14) . ?
C11 H11A 0.9300 . ?
C12 H12A 0.9300 . ?
C13 H13A 0.9800 . ?
C14 C15 1.430(12) . ?
C14 H14A 0.9300 . ?
C15 C20 1.408(13) . ?
C15 C16 1.430(12) . ?
C16 C17 1.424(14) . ?
C17 C18 1.368(15) . ?
C17 H17A 0.9300 . ?
C18 C19 1.397(14) . ?
C18 H18A 0.9300 . ?
C19 C20 1.358(13) . ?
C20 H20A 0.9300 . ?
C21 C22 1.382(17) . ?
C21 C26 1.393(16) . ?
C21 H21 0.9300 . ?
C22 C23 1.320(17) . ?
C22 H22 0.9300 . ?
C23 C24 1.393(15) . ?
C23 H23 0.9300 . ?
C24 C25 1.376(14) . ?
C24 H24 0.9300 . ?
C25 C26 1.347(14) . ?
C25 C33 1.557(12) . ?
C26 H26 0.9300 . ?
C27 C32 1.399(14) . ?
C27 C28 1.414(14) . ?
C27 C33 1.500(13) . ?
C28 C29 1.360(16) . ?
C28 H28 0.9300 . ?
C29 C30 1.396(15) . ?
C29 H29 0.9300 . ?
C30 C31 1.376(15) . ?
C30 H30 0.9300 . ?
C31 C32 1.401(16) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 H33 0.9800 . ?
C34 C35 1.422(14) . ?
C34 H34 0.9300 . ?
C35 C39 1.410(14) 3_576 ?
C35 C36 1.440(15) . ?
C36 C37 1.318(15) . ?
C36 H36 0.9300 . ?
C37 C38 1.373(16) . ?
C38 C40 1.348(16) 3_576 ?
C38 H38 0.9300 . ?
C39 C35 1.410(14) 3_576 ?
C39 C40 1.434(15) . ?
C40 C38 1.348(16) 3_576 ?
C40 H40 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.000(1) . 3_676 ?
O1 Ni1 N1 92.1(3) . . ?
O1 Ni1 N1 87.9(3) 3_676 . ?
O1 Ni1 N1 87.9(3) . 3_676 ?
O1 Ni1 N1 92.1(3) 3_676 3_676 ?
N1 Ni1 N1 180.000(1) . 3_676 ?
O2 Ni2 O2 180.000(2) . 3_576 ?
O2 Ni2 N2 91.9(4) . 3_576 ?
O2 Ni2 N2 88.1(4) 3_576 3_576 ?
O2 Ni2 N2 88.1(4) . . ?
O2 Ni2 N2 91.9(4) 3_576 . ?
N2 Ni2 N2 180.000(1) 3_576 . ?
C16 O1 Ni1 130.3(6) . . ?
C39 O2 Ni2 131.4(7) . . ?
C14 N1 C13 114.1(7) . . ?
C14 N1 Ni1 125.8(6) . . ?
C13 N1 Ni1 120.1(6) . . ?
C34 N2 C33 115.2(9) . . ?
C34 N2 Ni2 124.6(7) . . ?
C33 N2 Ni2 120.2(6) . . ?
C6 C1 C2 120.0(13) . . ?
C6 C1 H1A 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C1 C2 C3 119.9(11) . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 H2A 120.0 . . ?
C4 C3 C2 117.7(10) . . ?
C4 C3 C13 124.4(9) . . ?
C2 C3 C13 117.9(9) . . ?
C3 C4 C5 121.8(11) . . ?
C3 C4 H4A 119.1 . . ?
C5 C4 H4A 119.1 . . ?
C6 C5 C4 119.8(12) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C1 C6 C5 120.7(13) . . ?
C1 C6 H6A 119.6 . . ?
C5 C6 H6A 119.6 . . ?
C12 C7 C8 117.8(9) . . ?
C12 C7 C13 124.6(8) . . ?
C8 C7 C13 117.5(9) . . ?
C9 C8 C7 119.6(11) . . ?
C9 C8 H8A 120.2 . . ?
C7 C8 H8A 120.2 . . ?
C10 C9 C8 123.5(13) . . ?
C10 C9 H9A 118.3 . . ?
C8 C9 H9A 118.3 . . ?
C9 C10 C11 116.7(12) . . ?
C9 C10 H10A 121.7 . . ?
C11 C10 H10A 121.7 . . ?
C12 C11 C10 119.8(12) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C7 C12 C11 122.6(10) . . ?
C7 C12 H12A 118.7 . . ?
C11 C12 H12A 118.7 . . ?
C7 C13 N1 111.7(7) . . ?
C7 C13 C3 113.0(7) . . ?
N1 C13 C3 113.1(7) . . ?
C7 C13 H13A 106.1 . . ?
N1 C13 H13A 106.1 . . ?
C3 C13 H13A 106.1 . . ?
N1 C14 C15 126.8(9) . . ?
N1 C14 H14A 116.6 . . ?
C15 C14 H14A 116.6 . . ?
C20 C15 C16 119.7(8) . . ?
C20 C15 C14 121.1(8) . . ?
C16 C15 C14 119.2(9) . . ?
O1 C16 C17 119.5(9) . . ?
O1 C16 C15 123.8(8) . . ?
C17 C16 C15 116.7(9) . . ?
C18 C17 C16 121.2(11) . . ?
C18 C17 H17A 119.4 . . ?
C16 C17 H17A 119.4 . . ?
C17 C18 C19 121.5(10) . . ?
C17 C18 H18A 119.2 . . ?
C19 C18 H18A 119.2 . . ?
C20 C19 C18 118.8(10) . . ?
C20 C19 Br1 121.3(8) . . ?
C18 C19 Br1 119.9(7) . . ?
C19 C20 C15 122.0(9) . . ?
C19 C20 H20A 119.0 . . ?
C15 C20 H20A 119.0 . . ?
C22 C21 C26 119.2(13) . . ?
C22 C21 H21 120.4 . . ?
C26 C21 H21 120.4 . . ?
C23 C22 C21 118.8(13) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C22 C23 C24 122.9(13) . . ?
C22 C23 H23 118.6 . . ?
C24 C23 H23 118.6 . . ?
C25 C24 C23 118.5(11) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C26 C25 C24 119.1(10) . . ?
C26 C25 C33 123.4(9) . . ?
C24 C25 C33 117.5(9) . . ?
C25 C26 C21 121.4(12) . . ?
C25 C26 H26 119.3 . . ?
C21 C26 H26 119.3 . . ?
C32 C27 C28 115.9(10) . . ?
C32 C27 C33 126.0(9) . . ?
C28 C27 C33 118.1(9) . . ?
C29 C28 C27 123.3(11) . . ?
C29 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
C28 C29 C30 119.3(11) . . ?
C28 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C31 C30 C29 120.0(12) . . ?
C31 C30 H30 120.0 . . ?
C29 C30 H30 120.0 . . ?
C30 C31 C32 120.0(11) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C27 C32 C31 121.5(10) . . ?
C27 C32 H32 119.3 . . ?
C31 C32 H32 119.3 . . ?
N2 C33 C27 113.8(8) . . ?
N2 C33 C25 111.2(7) . . ?
C27 C33 C25 111.6(7) . . ?
N2 C33 H33 106.6 . . ?
C27 C33 H33 106.6 . . ?
C25 C33 H33 106.6 . . ?
N2 C34 C35 127.3(10) . . ?
N2 C34 H34 116.3 . . ?
C35 C34 H34 116.3 . . ?
C39 C35 C34 121.2(10) 3_576 . ?
C39 C35 C36 119.0(10) 3_576 . ?
C34 C35 C36 119.7(10) . . ?
C37 C36 C35 118.8(11) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
C36 C37 C38 123.6(12) . . ?
C36 C37 Br2 118.6(9) . . ?
C38 C37 Br2 117.9(9) . . ?
C40 C38 C37 120.4(12) 3_576 . ?
C40 C38 H38 119.8 3_576 . ?
C37 C38 H38 119.8 . . ?
O2 C39 C35 122.2(10) . 3_576 ?
O2 C39 C40 119.6(10) . . ?
C35 C39 C40 118.2(10) 3_576 . ?
C38 C40 C39 120.0(11) 3_576 . ?
C38 C40 H40 120.0 3_576 . ?
C39 C40 H40 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.76
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         4.723
_refine_diff_density_min         -5.169
_refine_diff_density_rms         0.221
####################################################################### 
# 
# 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_a-sr
_database_code_depnum_ccdc_archive 'CCDC 1575905'
_audit_update_record             
;
2017-10-12 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H36 N2 Ni O4'
_chemical_formula_weight         691.44

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c

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

_cell_length_a                   10.243(4)
_cell_length_b                   16.148(6)
_cell_length_c                   12.283(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.351(4)
_cell_angle_gamma                90.00
_cell_volume                     2028.2(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8530
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      29.10

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             724
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8816
_exptl_absorpt_correction_T_max  0.9036
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15329
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         25.50
_reflns_number_total             3776
_reflns_number_gt                3255
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0709P)²+0.8893P] 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         3776
_refine_ls_number_parameters     224
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1353
_refine_ls_wR_factor_gt          0.1257
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.5000 0.5000 0.03783(16) Uani 1 2 d S . .
O1 O 0.46073(16) 0.58428(11) 0.40404(14) 0.0555(5) Uani 1 1 d . . .
N1 N 0.32884(19) 0.50311(10) 0.55557(16) 0.0390(4) Uani 1 1 d . . .
C9 C 0.2784(2) 0.42826(14) 0.61132(18) 0.0408(5) Uani 1 1 d . . .
H9 H 0.3533 0.4037 0.6528 0.049 Uiso 1 1 calc R . .
O2 O 0.4788(2) 0.70798(14) 0.26891(18) 0.0764(7) Uani 1 1 d . . .
C16 C 0.1777(2) 0.44831(14) 0.69315(17) 0.0411(5) Uani 1 1 d . . .
C1 C 0.3708(2) 0.64104(15) 0.40734(19) 0.0453(5) Uani 1 1 d . . .
C6 C 0.2674(2) 0.63750(14) 0.4767(2) 0.0440(5) Uani 1 1 d . . .
C8 C 0.2505(2) 0.56509(14) 0.54258(18) 0.0418(5) Uani 1 1 d . . .
H8 H 0.1743 0.5628 0.5800 0.050 Uiso 1 1 calc R . .
C21 C 0.0465(2) 0.43046(16) 0.67583(19) 0.0493(6) Uani 1 1 d . . .
H21 H 0.0165 0.4050 0.6113 0.059 Uiso 1 1 calc R . .
C2 C 0.3748(3) 0.70918(17) 0.3341(2) 0.0571(7) Uani 1 1 d . . .
C5 C 0.1727(3) 0.70063(15) 0.4754(3) 0.0582(7) Uani 1 1 d . . .
H5 H 0.1058 0.6985 0.5234 0.070 Uiso 1 1 calc R . .
C10 C 0.2320(2) 0.36403(15) 0.52638(19) 0.0454(5) Uani 1 1 d . . .
C11 C 0.1826(3) 0.38510(18) 0.4229(2) 0.0627(7) Uani 1 1 d . . .
H11 H 0.1805 0.4405 0.4020 0.075 Uiso 1 1 calc R . .
C3 C 0.2800(3) 0.76881(19) 0.3322(3) 0.0736(9) Uani 1 1 d . . .
H3 H 0.2828 0.8124 0.2828 0.088 Uiso 1 1 calc R . .
C20 C -0.0409(3) 0.4502(2) 0.7538(2) 0.0645(8) Uani 1 1 d . . .
H20 H -0.1290 0.4370 0.7419 0.077 Uiso 1 1 calc R . .
C17 C 0.2200(3) 0.48541(17) 0.7908(2) 0.0558(6) Uani 1 1 d . . .
H17 H 0.3084 0.4964 0.8050 0.067 Uiso 1 1 calc R . .
C19 C 0.0020(4) 0.4890(2) 0.8483(2) 0.0712(9) Uani 1 1 d . . .
H19 H -0.0570 0.5036 0.8997 0.085 Uiso 1 1 calc R . .
C15 C 0.2357(3) 0.28181(17) 0.5555(3) 0.0663(7) Uani 1 1 d . . .
H15 H 0.2706 0.2663 0.6242 0.080 Uiso 1 1 calc R . .
C18 C 0.1322(4) 0.50610(18) 0.8668(2) 0.0694(9) Uani 1 1 d . . .
H18 H 0.1616 0.5319 0.9313 0.083 Uiso 1 1 calc R . .
C4 C 0.1789(3) 0.76498(18) 0.4038(3) 0.0747(9) Uani 1 1 d . . .
H4 H 0.1157 0.8064 0.4025 0.090 Uiso 1 1 calc R . .
C14 C 0.1874(4) 0.2217(2) 0.4824(4) 0.0888(11) Uani 1 1 d . . .
H14 H 0.1885 0.1663 0.5032 0.107 Uiso 1 1 calc R . .
C13 C 0.1382(4) 0.2434(2) 0.3797(3) 0.0841(11) Uani 1 1 d . . .
H13 H 0.1066 0.2031 0.3310 0.101 Uiso 1 1 calc R . .
C12 C 0.1363(4) 0.3254(2) 0.3502(3) 0.0796(9) Uani 1 1 d . . .
H12 H 0.1038 0.3407 0.2808 0.096 Uiso 1 1 calc R . .
C7 C 0.4799(4) 0.7678(3) 0.1831(3) 0.0982(13) Uani 1 1 d . . .
H7A H 0.4026 0.7616 0.1358 0.147 Uiso 1 1 calc R . .
H7B H 0.5558 0.7595 0.1421 0.147 Uiso 1 1 calc R . .
H7C H 0.4821 0.8225 0.2137 0.147 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 O1 1.8298(16) . ?
Ni1 O1 1.8298(16) 3_666 ?
Ni1 N1 1.919(2) 3_666 ?
Ni1 N1 1.919(2) . ?
O1 C1 1.302(3) . ?
N1 C8 1.287(3) . ?
N1 C9 1.496(3) . ?
C9 C16 1.517(3) . ?
C9 C10 1.527(3) . ?
C9 H9 0.9800 . ?
O2 C2 1.370(3) . ?
O2 C7 1.430(3) . ?
C16 C21 1.378(3) . ?
C16 C17 1.387(3) . ?
C1 C6 1.399(3) . ?
C1 C2 1.423(3) . ?
C6 C5 1.407(3) . ?
C6 C8 1.438(3) . ?
C8 H8 0.9300 . ?
C21 C20 1.386(3) . ?
C21 H21 0.9300 . ?
C2 C3 1.366(4) . ?
C5 C4 1.366(4) . ?
C5 H5 0.9300 . ?
C10 C15 1.375(4) . ?
C10 C11 1.382(4) . ?
C11 C12 1.380(4) . ?
C11 H11 0.9300 . ?
C3 C4 1.399(5) . ?
C3 H3 0.9300 . ?
C20 C19 1.369(4) . ?
C20 H20 0.9300 . ?
C17 C18 1.374(4) . ?
C17 H17 0.9300 . ?
C19 C18 1.368(5) . ?
C19 H19 0.9300 . ?
C15 C14 1.394(5) . ?
C15 H15 0.9300 . ?
C18 H18 0.9300 . ?
C4 H4 0.9300 . ?
C14 C13 1.376(6) . ?
C14 H14 0.9300 . ?
C13 C12 1.372(5) . ?
C13 H13 0.9300 . ?
C12 H12 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.00(10) . 3_666 ?
O1 Ni1 N1 87.78(7) . 3_666 ?
O1 Ni1 N1 92.22(7) 3_666 3_666 ?
O1 Ni1 N1 92.22(7) . . ?
O1 Ni1 N1 87.78(7) 3_666 . ?
N1 Ni1 N1 180.0 3_666 . ?
C1 O1 Ni1 129.27(15) . . ?
C8 N1 C9 117.10(19) . . ?
C8 N1 Ni1 123.52(15) . . ?
C9 N1 Ni1 119.27(13) . . ?
N1 C9 C16 113.41(18) . . ?
N1 C9 C10 109.76(18) . . ?
C16 C9 C10 113.64(18) . . ?
N1 C9 H9 106.5 . . ?
C16 C9 H9 106.5 . . ?
C10 C9 H9 106.5 . . ?
C2 O2 C7 117.5(3) . . ?
C21 C16 C17 118.4(2) . . ?
C21 C16 C9 123.2(2) . . ?
C17 C16 C9 118.4(2) . . ?
O1 C1 C6 123.5(2) . . ?
O1 C1 C2 118.6(2) . . ?
C6 C1 C2 117.9(2) . . ?
C1 C6 C5 120.6(2) . . ?
C1 C6 C8 119.8(2) . . ?
C5 C6 C8 119.3(2) . . ?
N1 C8 C6 127.4(2) . . ?
N1 C8 H8 116.3 . . ?
C6 C8 H8 116.3 . . ?
C16 C21 C20 120.6(2) . . ?
C16 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
C3 C2 O2 125.1(2) . . ?
C3 C2 C1 120.6(3) . . ?
O2 C2 C1 114.2(2) . . ?
C4 C5 C6 120.0(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C15 C10 C11 118.7(3) . . ?
C15 C10 C9 118.3(2) . . ?
C11 C10 C9 122.9(2) . . ?
C12 C11 C10 121.1(3) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C2 C3 C4 120.6(3) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C19 C20 C21 120.2(3) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C18 C17 C16 120.6(3) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C18 C19 C20 119.7(3) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C10 C15 C14 120.1(3) . . ?
C10 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C19 C18 C17 120.5(3) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C5 C4 C3 120.2(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C13 C14 C15 120.7(3) . . ?
C13 C14 H14 119.7 . . ?
C15 C14 H14 119.7 . . ?
C14 C13 C12 119.2(3) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 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
O1 Ni1 O1 C1 -9(14) 3_666 . . . ?
N1 Ni1 O1 C1 -157.9(2) 3_666 . . . ?
N1 Ni1 O1 C1 22.1(2) . . . . ?
O1 Ni1 N1 C8 -18.1(2) . . . . ?
O1 Ni1 N1 C8 161.9(2) 3_666 . . . ?
N1 Ni1 N1 C8 -180(100) 3_666 . . . ?
O1 Ni1 N1 C9 157.97(17) . . . . ?
O1 Ni1 N1 C9 -22.03(17) 3_666 . . . ?
N1 Ni1 N1 C9 -4(100) 3_666 . . . ?
C8 N1 C9 C16 -29.9(3) . . . . ?
Ni1 N1 C9 C16 153.75(15) . . . . ?
C8 N1 C9 C10 98.4(2) . . . . ?
Ni1 N1 C9 C10 -77.9(2) . . . . ?
N1 C9 C16 C21 108.2(3) . . . . ?
C10 C9 C16 C21 -18.0(3) . . . . ?
N1 C9 C16 C17 -72.6(3) . . . . ?
C10 C9 C16 C17 161.1(2) . . . . ?
Ni1 O1 C1 C6 -13.7(4) . . . . ?
Ni1 O1 C1 C2 168.44(19) . . . . ?
O1 C1 C6 C5 -179.4(2) . . . . ?
C2 C1 C6 C5 -1.5(4) . . . . ?
O1 C1 C6 C8 -5.3(4) . . . . ?
C2 C1 C6 C8 172.5(2) . . . . ?
C9 N1 C8 C6 -168.9(2) . . . . ?
Ni1 N1 C8 C6 7.3(3) . . . . ?
C1 C6 C8 N1 8.0(4) . . . . ?
C5 C6 C8 N1 -177.9(2) . . . . ?
C17 C16 C21 C20 0.8(4) . . . . ?
C9 C16 C21 C20 179.9(2) . . . . ?
C7 O2 C2 C3 -8.2(5) . . . . ?
C7 O2 C2 C1 171.6(3) . . . . ?
O1 C1 C2 C3 177.8(3) . . . . ?
C6 C1 C2 C3 -0.1(4) . . . . ?
O1 C1 C2 O2 -1.9(4) . . . . ?
C6 C1 C2 O2 -179.9(2) . . . . ?
C1 C6 C5 C4 1.9(4) . . . . ?
C8 C6 C5 C4 -172.2(3) . . . . ?
N1 C9 C10 C15 152.3(2) . . . . ?
C16 C9 C10 C15 -79.5(3) . . . . ?
N1 C9 C10 C11 -29.8(3) . . . . ?
C16 C9 C10 C11 98.4(3) . . . . ?
C15 C10 C11 C12 0.7(4) . . . . ?
C9 C10 C11 C12 -177.1(3) . . . . ?
O2 C2 C3 C4 -178.9(3) . . . . ?
C1 C2 C3 C4 1.4(5) . . . . ?
C16 C21 C20 C19 1.1(4) . . . . ?
C21 C16 C17 C18 -2.0(4) . . . . ?
C9 C16 C17 C18 178.9(2) . . . . ?
C21 C20 C19 C18 -1.8(5) . . . . ?
C11 C10 C15 C14 -1.6(4) . . . . ?
C9 C10 C15 C14 176.4(3) . . . . ?
C20 C19 C18 C17 0.7(5) . . . . ?
C16 C17 C18 C19 1.3(5) . . . . ?
C6 C5 C4 C3 -0.6(5) . . . . ?
C2 C3 C4 C5 -1.0(5) . . . . ?
C10 C15 C14 C13 1.4(5) . . . . ?
C15 C14 C13 C12 -0.4(6) . . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
C14 C13 C12 C11 -0.4(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_t_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1817084'
_audit_update_record             
;
2018-01-15 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H36 N2 Ni O4, 2(C Cl2)'
_chemical_formula_sum            ' C44 H36 Cl4 N2 Ni O4'
_chemical_formula_weight         857.24

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'
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   ' P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   9.960(7)
_cell_length_b                   24.935(16)
_cell_length_c                   8.698(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.781(8)
_cell_angle_gamma                90.00
_cell_volume                     2089(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3649
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      27.45

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_process_details   'SADABS, v2.10 (Sheldrick, G.M., 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18164
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         27.61
_reflns_number_total             4844
_reflns_number_gt                3052
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0753P)²+0.1183P] 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         4796
_refine_ls_number_parameters     270
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0541
_refine_ls_wR_factor_ref         0.1469
_refine_ls_wR_factor_gt          0.1312
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0000 0.5000 1.0000 0.03580(17) Uani 1 2 d S . .
O1 O 0.17413(19) 0.49837(7) 0.9665(2) 0.0452(5) Uani 1 1 d . . .
N1 N 0.0524(2) 0.44061(8) 1.1424(2) 0.0373(5) Uani 1 1 d . . .
C20 C 0.1202(3) 0.54115(10) 0.7123(3) 0.0379(6) Uani 1 1 d . . .
O2 O 0.3273(2) 0.53723(8) 0.4137(2) 0.0579(6) Uani 1 1 d . . .
C15 C 0.2062(3) 0.51025(10) 0.8331(3) 0.0392(6) Uani 1 1 d . . .
C8 C 0.2313(3) 0.36874(10) 1.2556(3) 0.0419(6) Uani 1 1 d . . .
C18 C 0.2811(3) 0.53133(10) 0.5491(3) 0.0444(6) Uani 1 1 d . . .
C4 C 0.0838(3) 0.36772(10) 0.9692(3) 0.0464(7) Uani 1 1 d . . .
C7 C 0.1563(3) 0.40097(10) 1.1111(3) 0.0405(6) Uani 1 1 d . . .
H7 H 0.2274 0.4219 1.0782 0.049 Uiso 1 1 calc R . .
C19 C 0.1593(3) 0.55100(11) 0.5699(3) 0.0440(6) Uani 1 1 d . . .
H19 H 0.1015 0.5711 0.4896 0.053 Uiso 1 1 calc R . .
C14 C -0.0026(3) 0.43173(10) 1.2593(3) 0.0412(6) Uani 1 1 d . . .
H14 H 0.0380 0.4053 1.3315 0.049 Uiso 1 1 calc R . .
C16 C 0.3334(3) 0.49252(10) 0.8101(3) 0.0450(7) Uani 1 1 d . . .
H16 H 0.3940 0.4735 0.8907 0.054 Uiso 1 1 calc R . .
C17 C 0.3701(3) 0.50268(10) 0.6707(3) 0.0472(7) Uani 1 1 d . . .
H17 H 0.4547 0.4904 0.6578 0.057 Uiso 1 1 calc R . .
C9 C 0.3222(3) 0.39479(12) 1.3801(3) 0.0550(8) Uani 1 1 d . . .
H9 H 0.3331 0.4317 1.3749 0.066 Uiso 1 1 calc R . .
C13 C 0.2195(3) 0.31377(11) 1.2679(3) 0.0600(8) Uani 1 1 d . . .
H13 H 0.1592 0.2951 1.1863 0.072 Uiso 1 1 calc R . .
C5 C -0.0373(3) 0.34027(13) 0.9660(4) 0.0600(8) Uani 1 1 d . . .
H5 H -0.0773 0.3436 1.0512 0.072 Uiso 1 1 calc R . .
C21 C 0.2502(3) 0.57170(14) 0.2956(3) 0.0638(9) Uani 1 1 d . . .
H21A H 0.1564 0.5589 0.2608 0.096 Uiso 1 1 calc R . .
H21B H 0.2913 0.5725 0.2071 0.096 Uiso 1 1 calc R . .
H21C H 0.2504 0.6072 0.3384 0.096 Uiso 1 1 calc R . .
C3 C 0.1388(4) 0.36353(12) 0.8394(4) 0.0645(9) Uani 1 1 d . . .
H3 H 0.2193 0.3822 0.8377 0.077 Uiso 1 1 calc R . .
C12 C 0.2953(4) 0.28602(13) 1.3989(4) 0.0784(11) Uani 1 1 d . . .
H12 H 0.2857 0.2490 1.4046 0.094 Uiso 1 1 calc R . .
C11 C 0.3841(4) 0.31282(14) 1.5199(4) 0.0761(10) Uani 1 1 d . . .
H11 H 0.4355 0.2941 1.6077 0.091 Uiso 1 1 calc R . .
C6 C -0.0995(4) 0.30836(13) 0.8404(4) 0.0791(11) Uani 1 1 d . . .
H6 H -0.1801 0.2897 0.8415 0.095 Uiso 1 1 calc R . .
C2 C 0.0742(6) 0.33152(18) 0.7111(4) 0.0915(13) Uani 1 1 d . . .
H2 H 0.1114 0.3290 0.6236 0.110 Uiso 1 1 calc R . .
C10 C 0.3973(4) 0.36723(14) 1.5119(4) 0.0707(10) Uani 1 1 d . . .
H10 H 0.4567 0.3857 1.5950 0.085 Uiso 1 1 calc R . .
C1 C -0.0430(5) 0.30377(16) 0.7126(5) 0.0920(14) Uani 1 1 d . . .
H1 H -0.0847 0.2818 0.6274 0.110 Uiso 1 1 calc R . .
Cl2 Cl 0.7198(7) 0.31299(18) 1.2624(9) 0.135(2) Uani 0.64(2) 1 d PU A 1
Cl1 Cl 0.5458(7) 0.3545(3) 0.9706(7) 0.147(2) Uani 0.64(2) 1 d PU A 1
Cl2A Cl 0.659(3) 0.3101(5) 1.2955(16) 0.194(5) Uani 0.36(2) 1 d PU A 2
Cl1A Cl 0.5365(14) 0.3367(7) 0.9931(16) 0.194(5) Uani 0.36(2) 1 d PU A 2
C22 C 0.5832(5) 0.35699(18) 1.1763(5) 0.1064(15) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.831(2) . ?
Ni1 O1 1.831(2) 3_567 ?
Ni1 N1 1.916(2) . ?
Ni1 N1 1.916(2) 3_567 ?
O1 C15 1.313(3) . ?
N1 C14 1.291(3) . ?
N1 C7 1.505(3) . ?
C20 C15 1.404(3) . ?
C20 C19 1.412(3) . ?
C20 C14 1.427(3) 3_567 ?
O2 C18 1.377(3) . ?
O2 C21 1.408(3) . ?
C15 C16 1.403(4) . ?
C8 C13 1.382(4) . ?
C8 C9 1.384(4) . ?
C8 C7 1.518(3) . ?
C18 C19 1.363(4) . ?
C18 C17 1.391(4) . ?
C4 C3 1.378(4) . ?
C4 C5 1.381(4) . ?
C4 C7 1.509(4) . ?
C7 H7 0.9800 . ?
C19 H19 0.9300 . ?
C14 C20 1.427(3) 3_567 ?
C14 H14 0.9300 . ?
C16 C17 1.376(4) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9300 . ?
C13 C12 1.381(4) . ?
C13 H13 0.9300 . ?
C5 C6 1.366(4) . ?
C5 H5 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C3 C2 1.389(5) . ?
C3 H3 0.9300 . ?
C12 C11 1.364(5) . ?
C12 H12 0.9300 . ?
C11 C10 1.367(5) . ?
C11 H11 0.9300 . ?
C6 C1 1.373(6) . ?
C6 H6 0.9300 . ?
C2 C1 1.360(6) . ?
C2 H2 0.9300 . ?
C10 H10 0.9300 . ?
C1 H1 0.9300 . ?
Cl2 C22 1.759(6) . ?
Cl1 C22 1.733(7) . ?
Cl2A C22 1.617(11) . ?
Cl1A C22 1.624(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.000(1) . 3_567 ?
O1 Ni1 N1 88.47(8) . . ?
O1 Ni1 N1 91.53(8) 3_567 . ?
O1 Ni1 N1 91.53(8) . 3_567 ?
O1 Ni1 N1 88.47(8) 3_567 3_567 ?
N1 Ni1 N1 180.000(1) . 3_567 ?
C15 O1 Ni1 126.13(16) . . ?
C14 N1 C7 118.6(2) . . ?
C14 N1 Ni1 122.78(17) . . ?
C7 N1 Ni1 118.49(15) . . ?
C15 C20 C19 120.0(2) . . ?
C15 C20 C14 120.1(2) . 3_567 ?
C19 C20 C14 119.4(2) . 3_567 ?
C18 O2 C21 116.8(2) . . ?
O1 C15 C16 119.1(2) . . ?
O1 C15 C20 123.0(2) . . ?
C16 C15 C20 117.8(2) . . ?
C13 C8 C9 117.2(2) . . ?
C13 C8 C7 123.8(2) . . ?
C9 C8 C7 119.0(2) . . ?
C19 C18 O2 125.3(2) . . ?
C19 C18 C17 120.0(2) . . ?
O2 C18 C17 114.7(2) . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 C7 120.3(3) . . ?
C5 C4 C7 121.4(2) . . ?
N1 C7 C4 107.6(2) . . ?
N1 C7 C8 114.4(2) . . ?
C4 C7 C8 114.7(2) . . ?
N1 C7 H7 106.5 . . ?
C4 C7 H7 106.5 . . ?
C8 C7 H7 106.5 . . ?
C18 C19 C20 120.5(2) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
N1 C14 C20 125.9(2) . 3_567 ?
N1 C14 H14 117.0 . . ?
C20 C14 H14 117.0 3_567 . ?
C17 C16 C15 121.4(2) . . ?
C17 C16 H16 119.3 . . ?
C15 C16 H16 119.3 . . ?
C16 C17 C18 120.2(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C10 C9 C8 121.6(3) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C8 C13 C12 121.4(3) . . ?
C8 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C6 C5 C4 121.3(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
O2 C21 H21A 109.5 . . ?
O2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
O2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C4 C3 C2 120.1(4) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C11 C12 C13 120.1(3) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C11 C10 120.0(3) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C5 C6 C1 120.1(4) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
C1 C2 C3 120.5(4) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C11 C10 C9 119.8(3) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C2 C1 C6 119.7(4) . . ?
C2 C1 H1 120.2 . . ?
C6 C1 H1 120.2 . . ?
Cl1A C22 Cl2A 112.0(8) . . ?
Cl1A C22 Cl1 16.8(6) . . ?
Cl2A C22 Cl1 125.3(6) . . ?
Cl1A C22 Cl2 102.7(6) . . ?
Cl2A C22 Cl2 24.7(8) . . ?
Cl1 C22 Cl2 110.9(4) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        27.61
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.40
_refine_diff_density_rms         0.052
####################################################################### 
# 
# 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_t_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1843964'
_audit_update_record             
;
2018-05-18 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H46 Cl4 N2 Ni O4, C40 H30 Cl4 N2 Ni O2'
_chemical_formula_sum            'C88 H76 Cl8 N4 Ni2 O6'
_chemical_formula_weight         1686.51

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1   '

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

_cell_length_a                   9.1018(10)
_cell_length_b                   13.8097(15)
_cell_length_c                   16.5217(17)
_cell_angle_alpha                73.923(2)
_cell_angle_beta                 74.3970(10)
_cell_angle_gamma                81.837(2)
_cell_volume                     1916.8(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1685
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      21.51

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872.0
_exptl_absorpt_coefficient_mu    0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17280
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.1509
_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       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         27.42
_reflns_number_total             8567
_reflns_number_gt                3708
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0100P)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_number_reflns         8567
_refine_ls_number_parameters     490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1887
_refine_ls_R_factor_gt           0.0702
_refine_ls_wR_factor_ref         0.0905
_refine_ls_wR_factor_gt          0.0762
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_restrained_S_all      1.167
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.5000 0.0387(2) Uani 1 2 d S . .
Ni2 Ni 1.0000 0.5000 0.0000 0.0368(2) Uani 1 2 d S . .
Cl1 Cl 0.90616(15) -0.23708(11) 0.43159(9) 0.0808(5) Uani 1 1 d . . .
Cl2 Cl 1.21277(12) -0.13886(9) 0.62861(7) 0.0546(4) Uani 1 1 d . . .
Cl3 Cl 1.43029(15) 0.27403(11) -0.08819(10) 0.0931(5) Uani 1 1 d . . .
Cl4 Cl 1.20267(16) -0.03958(10) 0.16805(9) 0.0820(5) Uani 1 1 d . . .
C1 C 0.3262(7) -0.0787(4) 0.8632(4) 0.0825(19) Uani 1 1 d . . .
H1A H 0.3524 -0.1452 0.8900 0.099 Uiso 1 1 calc R . .
C2 C 0.2178(7) -0.0234(5) 0.9093(4) 0.0786(18) Uani 1 1 d . . .
H2A H 0.1707 -0.0507 0.9672 0.094 Uiso 1 1 calc R . .
C3 C 0.1801(6) 0.0731(5) 0.8685(4) 0.0805(19) Uani 1 1 d . . .
H3A H 0.1053 0.1123 0.8985 0.097 Uiso 1 1 calc R . .
C4 C 0.2512(6) 0.1132(4) 0.7835(4) 0.0717(17) Uani 1 1 d . . .
H4A H 0.2233 0.1794 0.7567 0.086 Uiso 1 1 calc R . .
C5 C 0.3638(5) 0.0576(4) 0.7364(3) 0.0430(13) Uani 1 1 d . . .
C6 C 0.3981(6) -0.0393(4) 0.7782(4) 0.0697(17) Uani 1 1 d . . .
H6A H 0.4716 -0.0795 0.7486 0.084 Uiso 1 1 calc R . .
C7 C 0.4332(5) 0.1089(3) 0.6430(3) 0.0393(12) Uani 1 1 d . . .
H7A H 0.3479 0.1290 0.6147 0.047 Uiso 1 1 calc R . .
C8 C 0.6015(6) 0.3614(4) 0.5310(4) 0.0647(16) Uani 1 1 d . . .
H8A H 0.6130 0.4066 0.4766 0.078 Uiso 1 1 calc R . .
C9 C 0.6558(6) 0.3815(4) 0.5937(4) 0.0708(17) Uani 1 1 d . . .
H9A H 0.7037 0.4406 0.5826 0.085 Uiso 1 1 calc R . .
C10 C 0.6384(6) 0.3128(4) 0.6739(4) 0.0668(17) Uani 1 1 d . . .
H10A H 0.6751 0.3259 0.7169 0.080 Uiso 1 1 calc R . .
C11 C 0.5679(5) 0.2259(4) 0.6906(3) 0.0548(14) Uani 1 1 d . . .
H11A H 0.5589 0.1799 0.7445 0.066 Uiso 1 1 calc R . .
C12 C 0.5101(5) 0.2055(3) 0.6286(3) 0.0369(12) Uani 1 1 d . . .
C13 C 0.5302(5) 0.2742(4) 0.5487(3) 0.0488(13) Uani 1 1 d . . .
H13A H 0.4942 0.2610 0.5054 0.059 Uiso 1 1 calc R . .
N1 N 0.5416(4) 0.0395(3) 0.5945(2) 0.0394(10) Uani 1 1 d . . .
C15 C 0.6691(5) 0.0148(3) 0.6184(3) 0.0396(12) Uani 1 1 d . . .
H15A H 0.6397 -0.0120 0.6808 0.048 Uiso 1 1 calc R . .
H15B H 0.7130 0.0782 0.6089 0.048 Uiso 1 1 calc R . .
C16 C 0.7950(5) -0.0522(3) 0.5878(3) 0.0324(11) Uani 1 1 d . . .
C17 C 0.9256(5) -0.0623(3) 0.6196(3) 0.0373(11) Uani 1 1 d . . .
H17A H 0.9300 -0.0261 0.6585 0.045 Uiso 1 1 calc R . .
C18 C 1.0470(5) -0.1263(3) 0.5924(3) 0.0376(12) Uani 1 1 d . . .
C19 C 1.0404(5) -0.1799(3) 0.5346(3) 0.0419(12) Uani 1 1 d . . .
H19A H 1.1230 -0.2235 0.5167 0.050 Uiso 1 1 calc R . .
C20 C 0.9122(5) -0.1692(3) 0.5035(3) 0.0396(12) Uani 1 1 d . . .
C21 C 0.7828(5) -0.1048(3) 0.5294(3) 0.0348(11) Uani 1 1 d . . .
O1 O 0.6626(3) -0.0966(2) 0.49916(17) 0.0436(8) Uani 1 1 d . . .
C23 C 0.7431(7) 0.4294(4) -0.1606(4) 0.100(2) Uani 1 1 d . . .
H23A H 0.7808 0.4649 -0.2208 0.120 Uiso 1 1 calc R . .
H23B H 0.6350 0.4215 -0.1509 0.120 Uiso 1 1 calc R . .
C24 C 0.7652(5) 0.4879(4) -0.1033(3) 0.0666(17) Uani 1 1 d . . .
H24A H 0.8002 0.5537 -0.1367 0.080 Uiso 1 1 calc R . .
H24B H 0.6703 0.4975 -0.0613 0.080 Uiso 1 1 calc R . .
O3 O 0.8775(3) 0.4300(2) -0.06081(19) 0.0546(9) Uani 1 1 d . . .
C26 C 0.9088(6) 0.3340(4) -0.0801(3) 0.0737(17) Uani 1 1 d . . .
H26A H 0.8783 0.2815 -0.0273 0.088 Uiso 1 1 calc R . .
H26B H 1.0177 0.3226 -0.1035 0.088 Uiso 1 1 calc R . .
C27 C 0.8268(7) 0.3292(5) -0.1422(4) 0.109(2) Uani 1 1 d . . .
H27A H 0.7565 0.2761 -0.1180 0.130 Uiso 1 1 calc R . .
H27B H 0.8970 0.3167 -0.1946 0.130 Uiso 1 1 calc R . .
C31 C 0.4135(6) 0.3146(4) 0.3213(4) 0.0782(19) Uani 1 1 d . . .
H31A H 0.3613 0.2984 0.3794 0.094 Uiso 1 1 calc R . .
C32 C 0.3634(6) 0.2863(4) 0.2614(4) 0.0697(18) Uani 1 1 d . . .
H32A H 0.2745 0.2525 0.2785 0.084 Uiso 1 1 calc R . .
C33 C 0.4423(6) 0.3070(4) 0.1768(4) 0.0640(16) Uani 1 1 d . . .
H33A H 0.4093 0.2857 0.1363 0.077 Uiso 1 1 calc R . .
C34 C 0.5714(5) 0.3600(4) 0.1514(3) 0.0546(14) Uani 1 1 d . . .
H34A H 0.6234 0.3759 0.0931 0.065 Uiso 1 1 calc R . .
C35 C 0.6250(5) 0.3896(3) 0.2104(3) 0.0397(12) Uani 1 1 d . . .
C36 C 0.5418(6) 0.3672(4) 0.2948(3) 0.0589(14) Uani 1 1 d . . .
H36A H 0.5736 0.3885 0.3356 0.071 Uiso 1 1 calc R . .
C37 C 0.7649(5) 0.4521(3) 0.1785(3) 0.0378(12) Uani 1 1 d . . .
H37A H 0.7326 0.5176 0.1439 0.045 Uiso 1 1 calc R . .
C38 C 0.9650(5) 0.4375(4) 0.3576(3) 0.0542(14) Uani 1 1 d . . .
H38A H 1.0354 0.3945 0.3849 0.065 Uiso 1 1 calc R . .
C39 C 0.9057(6) 0.5251(4) 0.3824(3) 0.0617(15) Uani 1 1 d . . .
H39A H 0.9348 0.5418 0.4264 0.074 Uiso 1 1 calc R . .
C40 C 0.8026(6) 0.5872(4) 0.3407(3) 0.0641(15) Uani 1 1 d . . .
H40A H 0.7622 0.6470 0.3562 0.077 Uiso 1 1 calc R . .
C41 C 0.7579(5) 0.5617(4) 0.2756(3) 0.0571(15) Uani 1 1 d . . .
H41A H 0.6865 0.6039 0.2487 0.069 Uiso 1 1 calc R . .
C42 C 0.8182(5) 0.4748(3) 0.2510(3) 0.0384(12) Uani 1 1 d . . .
C43 C 0.9205(5) 0.4130(3) 0.2925(3) 0.0460(13) Uani 1 1 d . . .
H43A H 0.9610 0.3533 0.2766 0.055 Uiso 1 1 calc R . .
N2 N 0.8956(4) 0.4093(3) 0.1190(2) 0.0372(9) Uani 1 1 d . . .
C45 C 0.9287(5) 0.3136(3) 0.1435(3) 0.0419(12) Uani 1 1 d . . .
H45A H 0.8388 0.2822 0.1451 0.050 Uiso 1 1 calc R . .
H45B H 0.9335 0.3013 0.2035 0.050 Uiso 1 1 calc R . .
C46 C 1.0570(5) 0.2530(3) 0.1051(3) 0.0399(12) Uani 1 1 d . . .
C47 C 1.0679(5) 0.1506(3) 0.1460(3) 0.0492(13) Uani 1 1 d . . .
H47A H 0.9914 0.1239 0.1941 0.059 Uiso 1 1 calc R . .
C48 C 1.1893(6) 0.0888(3) 0.1165(3) 0.0496(14) Uani 1 1 d . . .
C49 C 1.3026(5) 0.1275(4) 0.0438(3) 0.0548(14) Uani 1 1 d . . .
H49A H 1.3851 0.0855 0.0231 0.066 Uiso 1 1 calc R . .
C50 C 1.2917(5) 0.2275(4) 0.0033(3) 0.0449(13) Uani 1 1 d . . .
C51 C 1.1699(5) 0.2972(3) 0.0315(3) 0.0352(11) Uani 1 1 d . . .
O2 O 1.1668(3) 0.3910(2) -0.00966(18) 0.0424(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.846(3) 2_656 ?
Ni1 O1 1.846(3) . ?
Ni1 N1 1.931(3) . ?
Ni1 N1 1.931(3) 2_656 ?
Ni2 O2 1.987(3) 2_765 ?
Ni2 O2 1.987(3) . ?
Ni2 N2 2.075(3) 2_765 ?
Ni2 N2 2.075(3) . ?
Ni2 O3 2.153(3) 2_765 ?
Ni2 O3 2.153(3) . ?
Cl1 C20 1.721(4) . ?
Cl2 C18 1.737(4) . ?
Cl3 C50 1.719(4) . ?
Cl4 C48 1.744(4) . ?
C1 C2 1.357(6) . ?
C1 C6 1.372(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.359(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.371(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.360(6) . ?
C5 C7 1.509(5) . ?
C6 H6A 0.9300 . ?
C7 N1 1.505(5) . ?
C7 C12 1.525(5) . ?
C7 H7A 0.9800 . ?
C8 C9 1.366(6) . ?
C8 C13 1.372(6) . ?
C8 H8A 0.9300 . ?
C9 C10 1.384(6) . ?
C9 H9A 0.9300 . ?
C10 C11 1.367(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.377(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.380(5) . ?
C13 H13A 0.9300 . ?
N1 C15 1.295(4) . ?
C15 C16 1.440(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C21 1.392(5) . ?
C16 C17 1.398(5) . ?
C17 C18 1.371(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.378(5) . ?
C19 C20 1.371(5) . ?
C19 H19A 0.9300 . ?
C20 C21 1.415(5) . ?
C21 O1 1.299(4) . ?
C23 C24 1.471(6) . ?
C23 C27 1.477(6) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 O3 1.421(4) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
O3 C26 1.420(5) . ?
C26 C27 1.442(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C31 C32 1.358(6) . ?
C31 C36 1.369(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.360(6) . ?
C32 H32A 0.9300 . ?
C33 C34 1.379(6) . ?
C33 H33A 0.9300 . ?
C34 C35 1.375(5) . ?
C34 H34A 0.9300 . ?
C35 C36 1.368(6) . ?
C35 C37 1.530(5) . ?
C36 H36A 0.9300 . ?
C37 N2 1.491(4) . ?
C37 C42 1.528(5) . ?
C37 H37A 0.9800 . ?
C38 C39 1.375(6) . ?
C38 C43 1.383(5) . ?
C38 H38A 0.9300 . ?
C39 C40 1.372(6) . ?
C39 H39A 0.9300 . ?
C40 C41 1.390(5) . ?
C40 H40A 0.9300 . ?
C41 C42 1.367(5) . ?
C41 H41A 0.9300 . ?
C42 C43 1.363(5) . ?
C43 H43A 0.9300 . ?
N2 C45 1.288(4) . ?
C45 C46 1.444(5) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.390(5) . ?
C46 C51 1.415(5) . ?
C47 C48 1.364(5) . ?
C47 H47A 0.9300 . ?
C48 C49 1.388(6) . ?
C49 C50 1.361(5) . ?
C49 H49A 0.9300 . ?
C50 C51 1.428(5) . ?
C51 O2 1.286(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 180.00(18) 2_656 . ?
O1 Ni1 N1 88.31(13) 2_656 . ?
O1 Ni1 N1 91.69(13) . . ?
O1 Ni1 N1 91.69(13) 2_656 2_656 ?
O1 Ni1 N1 88.31(13) . 2_656 ?
N1 Ni1 N1 180.000(1) . 2_656 ?
O2 Ni2 O2 180.00(13) 2_765 . ?
O2 Ni2 N2 88.04(12) 2_765 2_765 ?
O2 Ni2 N2 91.96(12) . 2_765 ?
O2 Ni2 N2 91.96(12) 2_765 . ?
O2 Ni2 N2 88.04(12) . . ?
N2 Ni2 N2 180.00(14) 2_765 . ?
O2 Ni2 O3 89.30(12) 2_765 2_765 ?
O2 Ni2 O3 90.70(12) . 2_765 ?
N2 Ni2 O3 88.54(12) 2_765 2_765 ?
N2 Ni2 O3 91.46(12) . 2_765 ?
O2 Ni2 O3 90.70(12) 2_765 . ?
O2 Ni2 O3 89.30(12) . . ?
N2 Ni2 O3 91.46(12) 2_765 . ?
N2 Ni2 O3 88.54(12) . . ?
O3 Ni2 O3 180.00(11) 2_765 . ?
C2 C1 C6 121.8(6) . . ?
C2 C1 H1A 119.1 . . ?
C6 C1 H1A 119.1 . . ?
C1 C2 C3 118.0(6) . . ?
C1 C2 H2A 121.0 . . ?
C3 C2 H2A 121.0 . . ?
C2 C3 C4 120.7(6) . . ?
C2 C3 H3A 119.7 . . ?
C4 C3 H3A 119.7 . . ?
C3 C4 C5 121.6(5) . . ?
C3 C4 H4A 119.2 . . ?
C5 C4 H4A 119.2 . . ?
C6 C5 C4 116.7(5) . . ?
C6 C5 C7 126.1(5) . . ?
C4 C5 C7 117.1(5) . . ?
C5 C6 C1 121.2(5) . . ?
C5 C6 H6A 119.4 . . ?
C1 C6 H6A 119.4 . . ?
N1 C7 C5 113.3(4) . . ?
N1 C7 C12 109.1(3) . . ?
C5 C7 C12 115.7(4) . . ?
N1 C7 H7A 106.0 . . ?
C5 C7 H7A 106.0 . . ?
C12 C7 H7A 106.0 . . ?
C9 C8 C13 119.6(5) . . ?
C9 C8 H8A 120.2 . . ?
C13 C8 H8A 120.2 . . ?
C8 C9 C10 119.2(5) . . ?
C8 C9 H9A 120.4 . . ?
C10 C9 H9A 120.4 . . ?
C11 C10 C9 120.7(5) . . ?
C11 C10 H10A 119.7 . . ?
C9 C10 H10A 119.7 . . ?
C10 C11 C12 120.9(5) . . ?
C10 C11 H11A 119.6 . . ?
C12 C11 H11A 119.6 . . ?
C11 C12 C13 117.6(5) . . ?
C11 C12 C7 123.1(5) . . ?
C13 C12 C7 119.2(4) . . ?
C8 C13 C12 122.0(5) . . ?
C8 C13 H13A 119.0 . . ?
C12 C13 H13A 119.0 . . ?
C15 N1 C7 113.4(3) . . ?
C15 N1 Ni1 123.5(3) . . ?
C7 N1 Ni1 122.9(3) . . ?
N1 C15 C16 128.0(4) . . ?
N1 C15 H15A 105.3 . . ?
C16 C15 H15A 105.3 . . ?
N1 C15 H15B 105.3 . . ?
C16 C15 H15B 105.3 . . ?
H15A C15 H15B 106.0 . . ?
C21 C16 C17 122.6(4) . . ?
C21 C16 C15 119.8(4) . . ?
C17 C16 C15 117.6(4) . . ?
C18 C17 C16 119.1(4) . . ?
C18 C17 H17A 120.5 . . ?
C16 C17 H17A 120.5 . . ?
C17 C18 C19 120.5(4) . . ?
C17 C18 Cl2 120.4(4) . . ?
C19 C18 Cl2 119.1(4) . . ?
C20 C19 C18 120.1(4) . . ?
C20 C19 H19A 120.0 . . ?
C18 C19 H19A 120.0 . . ?
C19 C20 C21 122.2(4) . . ?
C19 C20 Cl1 119.3(3) . . ?
C21 C20 Cl1 118.5(3) . . ?
O1 C21 C16 123.6(4) . . ?
O1 C21 C20 120.8(4) . . ?
C16 C21 C20 115.6(4) . . ?
C21 O1 Ni1 130.0(3) . . ?
C24 C23 C27 109.1(4) . . ?
C24 C23 H23A 109.9 . . ?
C27 C23 H23A 109.9 . . ?
C24 C23 H23B 109.9 . . ?
C27 C23 H23B 109.9 . . ?
H23A C23 H23B 108.3 . . ?
O3 C24 C23 105.7(4) . . ?
O3 C24 H24A 110.6 . . ?
C23 C24 H24A 110.6 . . ?
O3 C24 H24B 110.6 . . ?
C23 C24 H24B 110.6 . . ?
H24A C24 H24B 108.7 . . ?
C26 O3 C24 109.8(3) . . ?
C26 O3 Ni2 129.1(3) . . ?
C24 O3 Ni2 120.1(3) . . ?
O3 C26 C27 110.2(4) . . ?
O3 C26 H26A 109.6 . . ?
C27 C26 H26A 109.6 . . ?
O3 C26 H26B 109.6 . . ?
C27 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
C26 C27 C23 104.5(5) . . ?
C26 C27 H27A 110.9 . . ?
C23 C27 H27A 110.9 . . ?
C26 C27 H27B 110.9 . . ?
C23 C27 H27B 110.9 . . ?
H27A C27 H27B 108.9 . . ?
C32 C31 C36 119.1(6) . . ?
C32 C31 H31A 120.5 . . ?
C36 C31 H31A 120.5 . . ?
C31 C32 C33 120.6(6) . . ?
C31 C32 H32A 119.7 . . ?
C33 C32 H32A 119.7 . . ?
C32 C33 C34 119.5(5) . . ?
C32 C33 H33A 120.3 . . ?
C34 C33 H33A 120.3 . . ?
C35 C34 C33 121.3(5) . . ?
C35 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
C36 C35 C34 117.1(5) . . ?
C36 C35 C37 123.4(4) . . ?
C34 C35 C37 119.3(5) . . ?
C35 C36 C31 122.4(5) . . ?
C35 C36 H36A 118.8 . . ?
C31 C36 H36A 118.8 . . ?
N2 C37 C42 110.6(3) . . ?
N2 C37 C35 113.4(3) . . ?
C42 C37 C35 114.1(4) . . ?
N2 C37 H37A 106.0 . . ?
C42 C37 H37A 106.0 . . ?
C35 C37 H37A 106.0 . . ?
C39 C38 C43 120.4(5) . . ?
C39 C38 H38A 119.8 . . ?
C43 C38 H38A 119.8 . . ?
C40 C39 C38 118.4(5) . . ?
C40 C39 H39A 120.8 . . ?
C38 C39 H39A 120.8 . . ?
C39 C40 C41 120.8(5) . . ?
C39 C40 H40A 119.6 . . ?
C41 C40 H40A 119.6 . . ?
C42 C41 C40 120.4(5) . . ?
C42 C41 H41A 119.8 . . ?
C40 C41 H41A 119.8 . . ?
C43 C42 C41 118.9(5) . . ?
C43 C42 C37 123.6(4) . . ?
C41 C42 C37 117.5(4) . . ?
C42 C43 C38 121.1(4) . . ?
C42 C43 H43A 119.4 . . ?
C38 C43 H43A 119.4 . . ?
C45 N2 C37 115.8(4) . . ?
C45 N2 Ni2 123.8(3) . . ?
C37 N2 Ni2 120.2(3) . . ?
N2 C45 C46 128.6(4) . . ?
N2 C45 H45A 105.1 . . ?
C46 C45 H45A 105.1 . . ?
N2 C45 H45B 105.1 . . ?
C46 C45 H45B 105.1 . . ?
H45A C45 H45B 105.9 . . ?
C47 C46 C51 121.8(4) . . ?
C47 C46 C45 117.0(4) . . ?
C51 C46 C45 121.2(4) . . ?
C48 C47 C46 120.8(5) . . ?
C48 C47 H47A 119.6 . . ?
C46 C47 H47A 119.6 . . ?
C47 C48 C49 120.1(4) . . ?
C47 C48 Cl4 120.7(4) . . ?
C49 C48 Cl4 119.2(4) . . ?
C50 C49 C48 119.3(4) . . ?
C50 C49 H49A 120.4 . . ?
C48 C49 H49A 120.4 . . ?
C49 C50 C51 123.8(5) . . ?
C49 C50 Cl3 118.9(4) . . ?
C51 C50 Cl3 117.3(4) . . ?
O2 C51 C46 125.1(4) . . ?
O2 C51 C50 120.7(4) . . ?
C46 C51 C50 114.2(4) . . ?
C51 O2 Ni2 130.2(3) . . ?

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
C6 C1 C2 C3 0.8(9) . . . . ?
C1 C2 C3 C4 -0.8(9) . . . . ?
C2 C3 C4 C5 -0.2(9) . . . . ?
C3 C4 C5 C6 1.2(8) . . . . ?
C3 C4 C5 C7 179.4(5) . . . . ?
C4 C5 C6 C1 -1.2(8) . . . . ?
C7 C5 C6 C1 -179.1(5) . . . . ?
C2 C1 C6 C5 0.2(9) . . . . ?
C6 C5 C7 N1 4.2(6) . . . . ?
C4 C5 C7 N1 -173.8(4) . . . . ?
C6 C5 C7 C12 -122.9(5) . . . . ?
C4 C5 C7 C12 59.1(5) . . . . ?
C13 C8 C9 C10 0.5(8) . . . . ?
C8 C9 C10 C11 -0.1(8) . . . . ?
C9 C10 C11 C12 -1.2(8) . . . . ?
C10 C11 C12 C13 2.0(7) . . . . ?
C10 C11 C12 C7 178.8(4) . . . . ?
N1 C7 C12 C11 -104.4(4) . . . . ?
C5 C7 C12 C11 24.8(6) . . . . ?
N1 C7 C12 C13 72.3(5) . . . . ?
C5 C7 C12 C13 -158.4(4) . . . . ?
C9 C8 C13 C12 0.4(7) . . . . ?
C11 C12 C13 C8 -1.6(7) . . . . ?
C7 C12 C13 C8 -178.5(4) . . . . ?
C5 C7 N1 C15 -71.2(5) . . . . ?
C12 C7 N1 C15 59.3(5) . . . . ?
C5 C7 N1 Ni1 113.2(3) . . . . ?
C12 C7 N1 Ni1 -116.3(3) . . . . ?
O1 Ni1 N1 C15 -164.7(4) 2_656 . . . ?
O1 Ni1 N1 C15 15.3(4) . . . . ?
N1 Ni1 N1 C15 52(100) 2_656 . . . ?
O1 Ni1 N1 C7 10.4(3) 2_656 . . . ?
O1 Ni1 N1 C7 -169.6(3) . . . . ?
N1 Ni1 N1 C7 -133(100) 2_656 . . . ?
C7 N1 C15 C16 177.9(4) . . . . ?
Ni1 N1 C15 C16 -6.6(6) . . . . ?
N1 C15 C16 C21 -4.6(7) . . . . ?
N1 C15 C16 C17 176.0(4) . . . . ?
C21 C16 C17 C18 0.0(6) . . . . ?
C15 C16 C17 C18 179.3(4) . . . . ?
C16 C17 C18 C19 0.1(6) . . . . ?
C16 C17 C18 Cl2 178.6(3) . . . . ?
C17 C18 C19 C20 0.3(7) . . . . ?
Cl2 C18 C19 C20 -178.3(3) . . . . ?
C18 C19 C20 C21 -0.7(7) . . . . ?
C18 C19 C20 Cl1 -179.8(3) . . . . ?
C17 C16 C21 O1 179.9(4) . . . . ?
C15 C16 C21 O1 0.6(6) . . . . ?
C17 C16 C21 C20 -0.3(6) . . . . ?
C15 C16 C21 C20 -179.7(4) . . . . ?
C19 C20 C21 O1 -179.6(4) . . . . ?
Cl1 C20 C21 O1 -0.4(6) . . . . ?
C19 C20 C21 C16 0.7(6) . . . . ?
Cl1 C20 C21 C16 179.8(3) . . . . ?
C16 C21 O1 Ni1 15.8(6) . . . . ?
C20 C21 O1 Ni1 -163.9(3) . . . . ?
O1 Ni1 O1 C21 -151(5) 2_656 . . . ?
N1 Ni1 O1 C21 -20.7(4) . . . . ?
N1 Ni1 O1 C21 159.3(4) 2_656 . . . ?
C27 C23 C24 O3 8.3(7) . . . . ?
C23 C24 O3 C26 -8.0(5) . . . . ?
C23 C24 O3 Ni2 161.5(3) . . . . ?
O2 Ni2 O3 C26 -170.2(4) 2_765 . . . ?
O2 Ni2 O3 C26 9.8(4) . . . . ?
N2 Ni2 O3 C26 101.7(4) 2_765 . . . ?
N2 Ni2 O3 C26 -78.3(4) . . . . ?
O3 Ni2 O3 C26 -14(100) 2_765 . . . ?
O2 Ni2 O3 C24 22.5(3) 2_765 . . . ?
O2 Ni2 O3 C24 -157.5(3) . . . . ?
N2 Ni2 O3 C24 -65.5(3) 2_765 . . . ?
N2 Ni2 O3 C24 114.5(3) . . . . ?
O3 Ni2 O3 C24 179(100) 2_765 . . . ?
C24 O3 C26 C27 4.9(6) . . . . ?
Ni2 O3 C26 C27 -163.4(4) . . . . ?
O3 C26 C27 C23 0.4(7) . . . . ?
C24 C23 C27 C26 -5.3(7) . . . . ?
C36 C31 C32 C33 2.1(8) . . . . ?
C31 C32 C33 C34 -2.0(8) . . . . ?
C32 C33 C34 C35 2.0(7) . . . . ?
C33 C34 C35 C36 -2.1(7) . . . . ?
C33 C34 C35 C37 -177.4(4) . . . . ?
C34 C35 C36 C31 2.2(7) . . . . ?
C37 C35 C36 C31 177.4(4) . . . . ?
C32 C31 C36 C35 -2.3(8) . . . . ?
C36 C35 C37 N2 136.2(4) . . . . ?
C34 C35 C37 N2 -48.8(5) . . . . ?
C36 C35 C37 C42 8.4(6) . . . . ?
C34 C35 C37 C42 -176.6(4) . . . . ?
C43 C38 C39 C40 -0.3(8) . . . . ?
C38 C39 C40 C41 0.7(8) . . . . ?
C39 C40 C41 C42 -1.2(8) . . . . ?
C40 C41 C42 C43 1.2(7) . . . . ?
C40 C41 C42 C37 -179.4(4) . . . . ?
N2 C37 C42 C43 -40.5(6) . . . . ?
C35 C37 C42 C43 88.8(5) . . . . ?
N2 C37 C42 C41 140.2(4) . . . . ?
C35 C37 C42 C41 -90.5(5) . . . . ?
C41 C42 C43 C38 -0.9(7) . . . . ?
C37 C42 C43 C38 179.8(4) . . . . ?
C39 C38 C43 C42 0.4(7) . . . . ?
C42 C37 N2 C45 83.5(4) . . . . ?
C35 C37 N2 C45 -46.1(5) . . . . ?
C42 C37 N2 Ni2 -101.7(3) . . . . ?
C35 C37 N2 Ni2 128.7(3) . . . . ?
O2 Ni2 N2 C45 162.4(3) 2_765 . . . ?
O2 Ni2 N2 C45 -17.6(3) . . . . ?
N2 Ni2 N2 C45 46(100) 2_765 . . . ?
O3 Ni2 N2 C45 -108.2(3) 2_765 . . . ?
O3 Ni2 N2 C45 71.8(3) . . . . ?
O2 Ni2 N2 C37 -11.9(3) 2_765 . . . ?
O2 Ni2 N2 C37 168.1(3) . . . . ?
N2 Ni2 N2 C37 -128(100) 2_765 . . . ?
O3 Ni2 N2 C37 77.4(3) 2_765 . . . ?
O3 Ni2 N2 C37 -102.6(3) . . . . ?
C37 N2 C45 C46 -172.9(4) . . . . ?
Ni2 N2 C45 C46 12.5(6) . . . . ?
N2 C45 C46 C47 178.5(4) . . . . ?
N2 C45 C46 C51 1.4(7) . . . . ?
C51 C46 C47 C48 0.3(7) . . . . ?
C45 C46 C47 C48 -176.8(4) . . . . ?
C46 C47 C48 C49 -1.2(7) . . . . ?
C46 C47 C48 Cl4 180.0(3) . . . . ?
C47 C48 C49 C50 0.7(7) . . . . ?
Cl4 C48 C49 C50 179.5(3) . . . . ?
C48 C49 C50 C51 0.7(7) . . . . ?
C48 C49 C50 Cl3 -178.5(3) . . . . ?
C47 C46 C51 O2 179.7(4) . . . . ?
C45 C46 C51 O2 -3.3(7) . . . . ?
C47 C46 C51 C50 1.1(6) . . . . ?
C45 C46 C51 C50 178.0(4) . . . . ?
C49 C50 C51 O2 179.7(4) . . . . ?
Cl3 C50 C51 O2 -1.1(6) . . . . ?
C49 C50 C51 C46 -1.6(7) . . . . ?
Cl3 C50 C51 C46 177.7(3) . . . . ?
C46 C51 O2 Ni2 -10.4(6) . . . . ?
C50 C51 O2 Ni2 168.2(3) . . . . ?
O2 Ni2 O2 C51 -40(100) 2_765 . . . ?
N2 Ni2 O2 C51 -162.5(4) 2_765 . . . ?
N2 Ni2 O2 C51 17.5(4) . . . . ?
O3 Ni2 O2 C51 108.9(4) 2_765 . . . ?
O3 Ni2 O2 C51 -71.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.981
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.075
