 
data_2006slh0986
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C40 H52 N Ni S4'
_chemical_formula_weight          733.78
 
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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni'  'Ni'   0.3393   1.1124
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    P2(1)2(1)2(1)
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 
_cell_length_a                    12.113(5)
_cell_length_b                    16.307(6)
_cell_length_c                    19.257(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      3804(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     944
_cell_measurement_theta_min       2.62
_cell_measurement_theta_max       24.96
 
_exptl_crystal_description        needle
_exptl_crystal_colour             red
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.02
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.281
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1564
_exptl_absorpt_coefficient_mu     0.758
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8948
_exptl_absorpt_correction_T_max   0.9850
_exptl_absorpt_process_details    'Bruker SADABS'
# absolute Tmin and Tmax unknown, but SADABS gives ratio
# as 0.626
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.69050
_diffrn_radiation_type            synchrotron
_diffrn_radiation_source          'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator   'silicon 111'
_diffrn_measurement_device_type   'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method        'fine-slice ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         5
_diffrn_reflns_number             21880
_diffrn_reflns_av_R_equivalents   0.0821
_diffrn_reflns_av_sigmaI/netI     0.0976
_diffrn_reflns_limit_h_min        -15
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -22
_diffrn_reflns_limit_l_max        24
_diffrn_reflns_theta_min          2.28
_diffrn_reflns_theta_max          25.56
_reflns_number_total              7715
_reflns_number_gt                 6360
_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, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[σ²(Fo²)+(0.0590P)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      SHELXL
_refine_ls_extinction_coef        0.0101(11)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack    0.009(16)
_refine_ls_number_reflns          7715
_refine_ls_number_parameters      420
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0679
_refine_ls_R_factor_gt            0.0529
_refine_ls_wR_factor_ref          0.1317
_refine_ls_wR_factor_gt           0.1220
_refine_ls_goodness_of_fit_ref    0.986
_refine_ls_restrained_S_all       0.986
_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
C1 C 0.2226(3) -0.2087(3) 0.6605(2) 0.0308(10) Uani 1 1 d . . .
H1 H 0.2278 -0.2650 0.6728 0.037 Uiso 1 1 calc R . .
C2 C 0.3132(3) -0.1600(3) 0.6674(2) 0.0296(9) Uani 1 1 d . . .
C3 C 0.4209(4) -0.1911(3) 0.6920(2) 0.0309(9) Uani 1 1 d . . .
C4 C 0.4273(4) -0.2617(3) 0.7367(2) 0.0332(10) Uani 1 1 d . . .
H4 H 0.3617 -0.2905 0.7482 0.040 Uiso 1 1 calc R . .
C5 C 0.5249(4) -0.2879(3) 0.7624(2) 0.0345(10) Uani 1 1 d . . .
H5 H 0.5266 -0.3346 0.7919 0.041 Uiso 1 1 calc R . .
C6 C 0.6252(4) -0.2466(2) 0.7462(2) 0.0315(9) Uani 1 1 d . . .
C7 C 0.7278(4) -0.2705(3) 0.7755(2) 0.0364(11) Uani 1 1 d . . .
H7 H 0.7313 -0.3167 0.8054 0.044 Uiso 1 1 calc R . .
C8 C 0.8221(4) -0.2271(3) 0.7607(2) 0.0363(10) Uani 1 1 d . . .
H8 H 0.8900 -0.2423 0.7817 0.044 Uiso 1 1 calc R . .
C9 C 0.8184(4) -0.1596(3) 0.7142(2) 0.0341(10) Uani 1 1 d . . .
H9 H 0.8843 -0.1311 0.7028 0.041 Uiso 1 1 calc R . .
C10 C 0.7205(3) -0.1357(3) 0.6859(2) 0.0329(10) Uani 1 1 d . . .
H10 H 0.7190 -0.0901 0.6553 0.039 Uiso 1 1 calc R . .
C11 C 0.6212(4) -0.1775(2) 0.7013(2) 0.0289(9) Uani 1 1 d . . .
C12 C 0.5181(3) -0.1523(3) 0.6753(2) 0.0287(9) Uani 1 1 d . . .
H12 H 0.5156 -0.1065 0.6449 0.034 Uiso 1 1 calc R . .
C13 C -0.0408(3) 0.0715(3) 0.5524(2) 0.0312(9) Uani 1 1 d . . .
H13 H -0.1096 0.0928 0.5370 0.037 Uiso 1 1 calc R . .
C14 C 0.0481(4) 0.1213(3) 0.5519(2) 0.0309(10) Uani 1 1 d . . .
C15 C 0.0467(3) 0.2073(3) 0.5288(2) 0.0284(9) Uani 1 1 d . . .
C16 C 0.1196(3) 0.2647(3) 0.5545(2) 0.0299(9) Uani 1 1 d . . .
H16 H 0.1734 0.2476 0.5873 0.036 Uiso 1 1 calc R . .
C17 C 0.1174(3) 0.3477(3) 0.5340(2) 0.0300(9) Uani 1 1 d . . .
C18 C 0.1920(3) 0.4068(3) 0.5613(2) 0.0324(10) Uani 1 1 d . . .
H18 H 0.2449 0.3907 0.5950 0.039 Uiso 1 1 calc R . .
C19 C 0.1884(4) 0.4864(3) 0.5394(3) 0.0390(11) Uani 1 1 d . . .
H19 H 0.2384 0.5253 0.5584 0.047 Uiso 1 1 calc R . .
C20 C 0.1111(4) 0.5116(3) 0.4888(3) 0.0423(12) Uani 1 1 d . . .
H20 H 0.1103 0.5668 0.4732 0.051 Uiso 1 1 calc R . .
C21 C 0.0376(4) 0.4563(3) 0.4622(3) 0.0387(11) Uani 1 1 d . . .
H21 H -0.0151 0.4738 0.4288 0.046 Uiso 1 1 calc R . .
C22 C 0.0388(4) 0.3735(3) 0.4839(2) 0.0312(10) Uani 1 1 d . . .
C23 C -0.0364(4) 0.3143(3) 0.4581(2) 0.0359(10) Uani 1 1 d . . .
H23 H -0.0906 0.3305 0.4252 0.043 Uiso 1 1 calc R . .
C24 C -0.0327(4) 0.2344(3) 0.4792(2) 0.0356(10) Uani 1 1 d . . .
H24 H -0.0840 0.1963 0.4605 0.043 Uiso 1 1 calc R . .
S1 S 0.09921(9) -0.17118(7) 0.63027(6) 0.0343(3) Uani 1 1 d . . .
S2 S 0.30042(8) -0.05721(6) 0.64618(6) 0.0298(2) Uani 1 1 d . . .
S3 S -0.03545(9) -0.02799(7) 0.57966(6) 0.0341(3) Uani 1 1 d . . .
S4 S 0.17187(8) 0.08028(7) 0.58289(6) 0.0300(2) Uani 1 1 d . . .
Ni1 Ni 0.13328(4) -0.04413(3) 0.61035(3) 0.02835(15) Uani 1 1 d . . .
C25 C 0.6643(4) 0.4185(3) 0.0680(2) 0.0336(10) Uani 1 1 d . . .
H25A H 0.6984 0.4462 0.0276 0.040 Uiso 1 1 calc R . .
H25B H 0.5834 0.4196 0.0610 0.040 Uiso 1 1 calc R . .
C26 C 0.7016(4) 0.3296(3) 0.0680(2) 0.0392(11) Uani 1 1 d . . .
H26A H 0.7827 0.3269 0.0619 0.047 Uiso 1 1 calc R . .
H26B H 0.6827 0.3038 0.1129 0.047 Uiso 1 1 calc R . .
C27 C 0.6452(5) 0.2838(3) 0.0093(3) 0.0454(12) Uani 1 1 d . . .
H27A H 0.6497 0.3172 -0.0335 0.054 Uiso 1 1 calc R . .
H27B H 0.5661 0.2768 0.0209 0.054 Uiso 1 1 calc R . .
C28 C 0.6956(5) 0.2000(3) -0.0048(3) 0.0527(14) Uani 1 1 d . . .
H28A H 0.7735 0.2064 -0.0174 0.079 Uiso 1 1 calc R . .
H28B H 0.6559 0.1735 -0.0430 0.079 Uiso 1 1 calc R . .
H28C H 0.6898 0.1660 0.0370 0.079 Uiso 1 1 calc R . .
C29 C 0.6241(3) 0.4372(3) 0.1942(2) 0.0307(9) Uani 1 1 d . . .
H29A H 0.6367 0.3775 0.1988 0.037 Uiso 1 1 calc R . .
H29B H 0.6531 0.4637 0.2367 0.037 Uiso 1 1 calc R . .
C30 C 0.5008(3) 0.4520(3) 0.1911(2) 0.0347(10) Uani 1 1 d . . .
H30A H 0.4721 0.4356 0.1451 0.042 Uiso 1 1 calc R . .
H30B H 0.4852 0.5111 0.1978 0.042 Uiso 1 1 calc R . .
C31 C 0.4437(3) 0.4023(3) 0.2479(3) 0.0354(10) Uani 1 1 d . . .
H31A H 0.4526 0.3431 0.2378 0.042 Uiso 1 1 calc R . .
H31B H 0.4798 0.4137 0.2930 0.042 Uiso 1 1 calc R . .
C32 C 0.3218(4) 0.4221(3) 0.2535(3) 0.0420(11) Uani 1 1 d . . .
H32A H 0.3126 0.4792 0.2683 0.063 Uiso 1 1 calc R . .
H32B H 0.2873 0.3857 0.2877 0.063 Uiso 1 1 calc R . .
H32C H 0.2865 0.4142 0.2082 0.063 Uiso 1 1 calc R . .
C33 C 0.6642(3) 0.5569(2) 0.1171(2) 0.0307(9) Uani 1 1 d . . .
H33A H 0.7089 0.5746 0.0767 0.037 Uiso 1 1 calc R . .
H33B H 0.5856 0.5607 0.1036 0.037 Uiso 1 1 calc R . .
C34 C 0.6845(4) 0.6155(3) 0.1756(2) 0.0363(10) Uani 1 1 d . . .
H34A H 0.7628 0.6121 0.1901 0.044 Uiso 1 1 calc R . .
H34B H 0.6381 0.6000 0.2159 0.044 Uiso 1 1 calc R . .
C35 C 0.6574(4) 0.7043(3) 0.1538(2) 0.0354(10) Uani 1 1 d . . .
H35A H 0.5834 0.7054 0.1318 0.043 Uiso 1 1 calc R . .
H35B H 0.6543 0.7392 0.1958 0.043 Uiso 1 1 calc R . .
C36 C 0.7410(4) 0.7403(3) 0.1034(3) 0.0422(11) Uani 1 1 d . . .
H36A H 0.8151 0.7365 0.1236 0.063 Uiso 1 1 calc R . .
H36B H 0.7230 0.7980 0.0946 0.063 Uiso 1 1 calc R . .
H36C H 0.7387 0.7097 0.0597 0.063 Uiso 1 1 calc R . .
C37 C 0.8123(3) 0.4580(3) 0.1528(2) 0.0303(9) Uani 1 1 d . . .
H37A H 0.8261 0.4898 0.1957 0.036 Uiso 1 1 calc R . .
H37B H 0.8261 0.3995 0.1634 0.036 Uiso 1 1 calc R . .
C38 C 0.8939(4) 0.4855(3) 0.0976(2) 0.0383(11) Uani 1 1 d . . .
H38A H 0.8833 0.5446 0.0879 0.046 Uiso 1 1 calc R . .
H38B H 0.8805 0.4548 0.0541 0.046 Uiso 1 1 calc R . .
C39 C 1.0130(3) 0.4705(3) 0.1223(3) 0.0394(11) Uani 1 1 d . . .
H39A H 1.0202 0.4127 0.1375 0.047 Uiso 1 1 calc R . .
H39B H 1.0640 0.4790 0.0828 0.047 Uiso 1 1 calc R . .
C40 C 1.0467(4) 0.5260(4) 0.1813(3) 0.0566(15) Uani 1 1 d . . .
H40A H 1.0345 0.5832 0.1679 0.085 Uiso 1 1 calc R . .
H40B H 1.1250 0.5176 0.1918 0.085 Uiso 1 1 calc R . .
H40C H 1.0023 0.5131 0.2225 0.085 Uiso 1 1 calc R . .
N1 N 0.6908(3) 0.4681(2) 0.13240(18) 0.0285(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
C1 C2 1.361(6) . ?
C1 S1 1.717(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.477(6) . ?
C2 S2 1.733(4) . ?
C3 C12 1.375(6) . ?
C3 C4 1.439(6) . ?
C4 C5 1.351(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.423(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.419(6) . ?
C6 C11 1.423(6) . ?
C7 C8 1.373(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.419(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.361(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.414(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.406(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.349(6) . ?
C13 S3 1.707(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.471(6) . ?
C14 S4 1.747(4) . ?
C15 C16 1.378(6) . ?
C15 C24 1.426(6) . ?
C16 C17 1.410(6) . ?
C16 H16 0.9500 . ?
C17 C22 1.420(6) . ?
C17 C18 1.422(6) . ?
C18 C19 1.365(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.412(7) . ?
C19 H19 0.9500 . ?
C20 C21 1.367(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.414(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.417(6) . ?
C23 C24 1.364(6) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
S1 Ni1 2.1470(14) . ?
S2 Ni1 2.1494(14) . ?
S3 Ni1 2.1438(14) . ?
S4 Ni1 2.1481(14) . ?
C25 N1 1.515(5) . ?
C25 C26 1.518(6) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.517(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.522(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.513(6) . ?
C29 N1 1.524(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.527(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.516(6) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.497(6) . ?
C33 N1 1.513(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.544(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.520(6) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.518(6) . ?
C37 N1 1.532(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.538(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.509(7) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
C2 C1 S1 121.8(3) . . ?
C2 C1 H1 119.1 . . ?
S1 C1 H1 119.1 . . ?
C1 C2 C3 122.9(4) . . ?
C1 C2 S2 118.0(3) . . ?
C3 C2 S2 119.1(3) . . ?
C12 C3 C4 117.5(4) . . ?
C12 C3 C2 121.6(4) . . ?
C4 C3 C2 120.9(4) . . ?
C5 C4 C3 121.3(4) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 121.1(4) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C11 119.3(4) . . ?
C7 C6 C5 122.1(4) . . ?
C11 C6 C5 118.6(4) . . ?
C8 C7 C6 120.3(4) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 120.2(4) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 121.3(4) . . ?
C9 C10 H10 119.3 . . ?
C11 C10 H10 119.3 . . ?
C12 C11 C10 122.8(4) . . ?
C12 C11 C6 118.6(4) . . ?
C10 C11 C6 118.7(4) . . ?
C3 C12 C11 122.9(4) . . ?
C3 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C14 C13 S3 123.0(3) . . ?
C14 C13 H13 118.5 . . ?
S3 C13 H13 118.5 . . ?
C13 C14 C15 124.5(4) . . ?
C13 C14 S4 116.9(3) . . ?
C15 C14 S4 118.6(3) . . ?
C16 C15 C24 117.5(4) . . ?
C16 C15 C14 122.0(4) . . ?
C24 C15 C14 120.4(4) . . ?
C15 C16 C17 122.6(4) . . ?
C15 C16 H16 118.7 . . ?
C17 C16 H16 118.7 . . ?
C16 C17 C22 119.1(4) . . ?
C16 C17 C18 122.4(4) . . ?
C22 C17 C18 118.5(4) . . ?
C19 C18 C17 120.7(4) . . ?
C19 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C18 C19 C20 120.7(4) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
C21 C20 C19 119.9(4) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.9(4) . . ?
C20 C21 H21 119.6 . . ?
C22 C21 H21 119.6 . . ?
C21 C22 C23 122.8(4) . . ?
C21 C22 C17 119.4(4) . . ?
C23 C22 C17 117.9(4) . . ?
C24 C23 C22 121.7(4) . . ?
C24 C23 H23 119.2 . . ?
C22 C23 H23 119.2 . . ?
C23 C24 C15 121.1(4) . . ?
C23 C24 H24 119.4 . . ?
C15 C24 H24 119.4 . . ?
C1 S1 Ni1 103.73(15) . . ?
C2 S2 Ni1 104.82(14) . . ?
C13 S3 Ni1 103.76(15) . . ?
C14 S4 Ni1 105.03(16) . . ?
S3 Ni1 S1 89.11(5) . . ?
S3 Ni1 S4 91.35(5) . . ?
S1 Ni1 S4 175.70(5) . . ?
S3 Ni1 S2 177.00(5) . . ?
S1 Ni1 S2 91.60(5) . . ?
S4 Ni1 S2 88.15(5) . . ?
N1 C25 C26 116.6(4) . . ?
N1 C25 H25A 108.1 . . ?
C26 C25 H25A 108.1 . . ?
N1 C25 H25B 108.1 . . ?
C26 C25 H25B 108.1 . . ?
H25A C25 H25B 107.3 . . ?
C27 C26 C25 109.7(4) . . ?
C27 C26 H26A 109.7 . . ?
C25 C26 H26A 109.7 . . ?
C27 C26 H26B 109.7 . . ?
C25 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
C26 C27 C28 113.2(4) . . ?
C26 C27 H27A 108.9 . . ?
C28 C27 H27A 108.9 . . ?
C26 C27 H27B 108.9 . . ?
C28 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 N1 116.1(3) . . ?
C30 C29 H29A 108.3 . . ?
N1 C29 H29A 108.3 . . ?
C30 C29 H29B 108.3 . . ?
N1 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
C29 C30 C31 109.5(4) . . ?
C29 C30 H30A 109.8 . . ?
C31 C30 H30A 109.8 . . ?
C29 C30 H30B 109.8 . . ?
C31 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
C32 C31 C30 112.3(4) . . ?
C32 C31 H31A 109.1 . . ?
C30 C31 H31A 109.1 . . ?
C32 C31 H31B 109.1 . . ?
C30 C31 H31B 109.1 . . ?
H31A C31 H31B 107.9 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 N1 115.5(3) . . ?
C34 C33 H33A 108.4 . . ?
N1 C33 H33A 108.4 . . ?
C34 C33 H33B 108.4 . . ?
N1 C33 H33B 108.4 . . ?
H33A C33 H33B 107.5 . . ?
C33 C34 C35 111.0(4) . . ?
C33 C34 H34A 109.4 . . ?
C35 C34 H34A 109.4 . . ?
C33 C34 H34B 109.4 . . ?
C35 C34 H34B 109.4 . . ?
H34A C34 H34B 108.0 . . ?
C36 C35 C34 113.2(4) . . ?
C36 C35 H35A 108.9 . . ?
C34 C35 H35A 108.9 . . ?
C36 C35 H35B 108.9 . . ?
C34 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 N1 114.5(3) . . ?
C38 C37 H37A 108.6 . . ?
N1 C37 H37A 108.6 . . ?
C38 C37 H37B 108.6 . . ?
N1 C37 H37B 108.6 . . ?
H37A C37 H37B 107.6 . . ?
C37 C38 C39 110.3(4) . . ?
C37 C38 H38A 109.6 . . ?
C39 C38 H38A 109.6 . . ?
C37 C38 H38B 109.6 . . ?
C39 C38 H38B 109.6 . . ?
H38A C38 H38B 108.1 . . ?
C40 C39 C38 113.0(4) . . ?
C40 C39 H39A 109.0 . . ?
C38 C39 H39A 109.0 . . ?
C40 C39 H39B 109.0 . . ?
C38 C39 H39B 109.0 . . ?
H39A C39 H39B 107.8 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C33 N1 C25 107.9(3) . . ?
C33 N1 C29 110.8(3) . . ?
C25 N1 C29 110.5(3) . . ?
C33 N1 C37 110.9(3) . . ?
C25 N1 C37 110.8(3) . . ?
C29 N1 C37 105.9(3) . . ?
 
_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              25.56
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    0.360
_refine_diff_density_min   -0.421
_refine_diff_density_rms    0.074
