# Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 1999
# CCDC Number: 186/1731
data_jd3_6
_audit_creation_method SHELXL
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_formula_moiety ?
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C36 H29 Br N Ni P S'
_chemical_formula_weight 677.25
_chemical_melting_point ?
_chemical_compound_source ?
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'
'P' 'P' 0.1023 0.0942
'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'
'Br' 'Br' -0.2901 2.4595
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting ?
_symmetry_space_group_name_H-M ?
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 10.8322(5)
_cell_length_b 14.8477(7)
_cell_length_c 19.7415(9)
_cell_angle_alpha 90.00
_cell_angle_beta 102.8990(10)
_cell_angle_gamma 90.00
_cell_volume 3095.0(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 296(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max ?
_exptl_crystal_size_mid ?
_exptl_crystal_size_min ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.453
_exptl_crystal_density_method ?
_exptl_crystal_F_000 1384
_exptl_absorpt_coefficient_mu 2.063
_exptl_absorpt_correction_type ?
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_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 ?
_diffrn_measurement_method ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 17906
_diffrn_reflns_av_R_equivalents 0.0454
_diffrn_reflns_av_sigmaI/netI 0.0570
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 1.73
_diffrn_reflns_theta_max 28.28
_reflns_number_total 6929
_reflns_number_observed 4866
_reflns_observed_criterion >2sigma(I)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^
or flagged by the user for potential systematic errors. Weighted R-factors
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R
are based on F, with F set to zero for negative F^2^. The observed criterion
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment ?
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6929
_refine_ls_number_parameters 486
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0847
_refine_ls_R_factor_obs 0.0525
_refine_ls_wR_factor_all 0.1568
_refine_ls_wR_factor_obs 0.1363
_refine_ls_goodness_of_fit_all 0.971
_refine_ls_goodness_of_fit_obs 1.018
_refine_ls_restrained_S_all 0.971
_refine_ls_restrained_S_obs 1.018
_refine_ls_shift/esd_max 0.001
_refine_ls_shift/esd_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ni Ni 0.43203(4) 0.28509(3) 0.12413(2) 0.03748(15) Uani 1 d . .
Br1 Br 1.05952(5) 0.67542(4) 0.75715(2) 0.0750(2) Uani 1 d . .
P1 P 0.26839(8) 0.35731(6) 0.06957(4) 0.0382(2) Uani 1 d . .
S1 S 0.36761(10) 0.29383(8) 0.22112(5) 0.0539(3) Uani 1 d . .
N1 N 0.7306(3) 0.4756(2) 0.4555(2) 0.0538(8) Uani 1 d . .
C1 C 0.9527(4) 0.6128(3) 0.6826(2) 0.0489(9) Uani 1 d . .
C2 C 0.9856(5) 0.6073(4) 0.6193(2) 0.0688(14) Uani 1 d . .
H2 H 1.0527(41) 0.6372(30) 0.6136(21) 0.055(12) Uiso 1 d . .
C3 C 0.9046(5) 0.5653(3) 0.5646(2) 0.0613(12) Uani 1 d . .
H3 H 0.9297(38) 0.5554(28) 0.5229(23) 0.058(12) Uiso 1 d . .
C4 C 0.7937(4) 0.5277(3) 0.5729(2) 0.0453(8) Uani 1 d . .
C5 C 0.7641(5) 0.5316(4) 0.6374(2) 0.0625(12) Uani 1 d . .
H5 H 0.6904(45) 0.5129(34) 0.6449(24) 0.074(15) Uiso 1 d . .
C6 C 0.8444(5) 0.5750(3) 0.6920(2) 0.0633(12) Uani 1 d . .
H6 H 0.8193(41) 0.5829(31) 0.7313(25) 0.067(13) Uiso 1 d . .
C7 C 0.7056(4) 0.4842(3) 0.5145(2) 0.0496(9) Uani 1 d . .
H7 H 0.6268(43) 0.4645(30) 0.5223(23) 0.067(14) Uiso 1 d . .
C8 C 0.6420(4) 0.4319(3) 0.4010(2) 0.0462(9) Uani 1 d . .
C9 C 0.6514(4) 0.4493(3) 0.3334(2) 0.0578(11) Uani 1 d . .
H9 H 0.7053(52) 0.4959(40) 0.3254(28) 0.096(18) Uiso 1 d . .
C10 C 0.5701(4) 0.4093(3) 0.2776(2) 0.0552(11) Uani 1 d . .
H10 H 0.5723(37) 0.4235(27) 0.2379(22) 0.050(11) Uiso 1 d . .
C11 C 0.4791(4) 0.3487(3) 0.2872(2) 0.0450(8) Uani 1 d . .
C12 C 0.4729(4) 0.3290(3) 0.3556(2) 0.0532(10) Uani 1 d . .
H12 H 0.4115(44) 0.2904(31) 0.3610(24) 0.063(13) Uiso 1 d . .
C13 C 0.5519(4) 0.3708(3) 0.4110(2) 0.0526(10) Uani 1 d . .
H13 H 0.5415(38) 0.3575(28) 0.4578(22) 0.057(11) Uiso 1 d . .
C14 C 0.6202(4) 0.2959(4) 0.1116(3) 0.0659(12) Uani 1 d . .
H14 H 0.6635(45) 0.3507(35) 0.1210(24) 0.071(15) Uiso 1 d . .
C15 C 0.6123(4) 0.2327(4) 0.1620(3) 0.0663(13) Uani 1 d . .
H15 H 0.6545(41) 0.2344(30) 0.2080(24) 0.060(12) Uiso 1 d . .
C16 C 0.5349(5) 0.1600(4) 0.1307(3) 0.0688(13) Uani 1 d . .
H16 H 0.5130(54) 0.1145(39) 0.1552(28) 0.093(19) Uiso 1 d . .
C17 C 0.4878(5) 0.1801(4) 0.0631(3) 0.0645(13) Uani 1 d . .
H17 H 0.4361(41) 0.1462(31) 0.0301(24) 0.062(12) Uiso 1 d . .
C18 C 0.5369(4) 0.2656(4) 0.0498(3) 0.0650(13) Uani 1 d . .
H18 H 0.5219(49) 0.2908(34) 0.0121(28) 0.075(17) Uiso 1 d . .
C191 C 0.2650(4) 0.4695(3) 0.1069(2) 0.0475(9) Uani 1 d . .
C192 C 0.3734(5) 0.5209(3) 0.1148(3) 0.0691(13) Uani 1 d . .
H192 H 0.4377(48) 0.5004(37) 0.1046(28) 0.081(18) Uiso 1 d . .
C193 C 0.3829(5) 0.6050(3) 0.1454(3) 0.0777(15) Uani 1 d . .
H193 H 0.4622(52) 0.6399(40) 0.1531(28) 0.094(17) Uiso 1 d . .
C194 C 0.2839(5) 0.6358(4) 0.1716(3) 0.0775(15) Uani 1 d . .
H194 H 0.2863(49) 0.6953(37) 0.1982(28) 0.088(16) Uiso 1 d . .
C195 C 0.1749(6) 0.5875(3) 0.1633(3) 0.0719(14) Uani 1 d . .
H195 H 0.1050(49) 0.6091(36) 0.1776(26) 0.082(16) Uiso 1 d . .
C196 C 0.1642(5) 0.5028(3) 0.1303(2) 0.0599(11) Uani 1 d . .
H196 H 0.0840(44) 0.4714(32) 0.1236(23) 0.068(14) Uiso 1 d . .
C201 C 0.1163(3) 0.3019(3) 0.0678(2) 0.0425(8) Uani 1 d . .
C202 C 0.1123(4) 0.2237(3) 0.1052(2) 0.0504(9) Uani 1 d . .
H202 H 0.1851(37) 0.2011(25) 0.1364(20) 0.042(10) Uiso 1 d . .
C203 C -0.0021(5) 0.1791(3) 0.1012(3) 0.0600(11) Uani 1 d . .
H203 H -0.0015(41) 0.1257(31) 0.1322(21) 0.059(12) Uiso 1 d . .
C204 C -0.1118(4) 0.2126(4) 0.0597(3) 0.0647(13) Uani 1 d . .
H204 H -0.1830(40) 0.1808(25) 0.0573(19) 0.043(10) Uiso 1 d . .
C205 C -0.1082(4) 0.2900(4) 0.0223(3) 0.0669(13) Uani 1 d . .
H205 H -0.1784(45) 0.3128(30) -0.0080(24) 0.065(13) Uiso 1 d . .
C206 C 0.0041(4) 0.3348(3) 0.0255(2) 0.0560(10) Uani 1 d . .
H206 H 0.0116(49) 0.3994(36) 0.0026(26) 0.089(16) Uiso 1 d . .
C211 C 0.2548(3) 0.3789(3) -0.0232(2) 0.0448(8) Uani 1 d . .
C212 C 0.2323(6) 0.4616(4) -0.0538(3) 0.0752(14) Uani 1 d . .
H212 H 0.2129(35) 0.5051(27) -0.0278(20) 0.041(10) Uiso 1 d . .
C213 C 0.2140(7) 0.4719(5) -0.1256(3) 0.102(2) Uani 1 d . .
H213 H 0.1900(64) 0.5329(50) -0.1360(36) 0.128(24) Uiso 1 d . .
C214 C 0.2239(6) 0.3997(5) -0.1657(3) 0.095(2) Uani 1 d . .
H214 H 0.2360(56) 0.4026(40) -0.2097(34) 0.108(20) Uiso 1 d . .
C215 C 0.2463(6) 0.3161(4) -0.1374(2) 0.0777(15) Uani 1 d . .
H215 H 0.2569(52) 0.2565(45) -0.1667(30) 0.111(21) Uiso 1 d . .
C216 C 0.2608(5) 0.3058(3) -0.0658(2) 0.0604(11) Uani 1 d . .
H216 H 0.2652(49) 0.2442(40) -0.0472(27) 0.089(17) Uiso 1 d . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni 0.0348(3) 0.0437(3) 0.0315(2) -0.0038(2) 0.0025(2) 0.0006(2)
Br1 0.0821(4) 0.0819(4) 0.0486(3) -0.0140(2) -0.0116(2) -0.0113(3)
P1 0.0359(5) 0.0390(5) 0.0375(4) -0.0056(4) 0.0035(3) 0.0000(4)
S1 0.0506(6) 0.0761(7) 0.0340(5) -0.0076(4) 0.0072(4) -0.0174(5)
N1 0.061(2) 0.060(2) 0.037(2) -0.0021(15) 0.0014(14) -0.012(2)
C1 0.054(2) 0.052(2) 0.034(2) -0.006(2) -0.004(2) -0.001(2)
C2 0.071(3) 0.084(3) 0.052(2) -0.012(2) 0.014(2) -0.038(3)
C3 0.077(3) 0.074(3) 0.034(2) -0.007(2) 0.016(2) -0.026(2)
C4 0.049(2) 0.045(2) 0.039(2) -0.002(2) 0.006(2) -0.002(2)
C5 0.053(3) 0.084(3) 0.053(2) -0.013(2) 0.017(2) -0.012(2)
C6 0.072(3) 0.084(3) 0.035(2) -0.012(2) 0.014(2) -0.002(2)
C7 0.049(2) 0.052(2) 0.044(2) -0.003(2) 0.001(2) -0.003(2)
C8 0.053(2) 0.049(2) 0.032(2) -0.003(2) 0.0008(15) -0.003(2)
C9 0.068(3) 0.060(3) 0.044(2) -0.002(2) 0.010(2) -0.023(2)
C10 0.070(3) 0.064(3) 0.030(2) -0.001(2) 0.007(2) -0.017(2)
C11 0.047(2) 0.054(2) 0.032(2) -0.004(2) 0.0053(15) 0.001(2)
C12 0.055(2) 0.068(3) 0.038(2) 0.000(2) 0.012(2) -0.020(2)
C13 0.060(2) 0.066(3) 0.030(2) 0.003(2) 0.007(2) -0.015(2)
C14 0.039(2) 0.078(3) 0.082(3) -0.009(3) 0.015(2) -0.001(2)
C15 0.047(3) 0.085(4) 0.057(3) -0.004(2) -0.007(2) 0.017(2)
C16 0.064(3) 0.060(3) 0.078(3) 0.000(3) 0.007(3) 0.019(2)
C17 0.059(3) 0.070(3) 0.061(3) -0.026(2) 0.007(2) 0.012(2)
C18 0.051(3) 0.099(4) 0.050(3) -0.003(3) 0.023(2) 0.017(3)
C191 0.047(2) 0.041(2) 0.051(2) -0.009(2) 0.004(2) 0.006(2)
C192 0.050(3) 0.057(3) 0.095(4) -0.024(2) 0.004(2) 0.002(2)
C193 0.061(3) 0.052(3) 0.113(4) -0.029(3) 0.003(3) -0.007(2)
C194 0.083(4) 0.058(3) 0.083(4) -0.023(3) 0.001(3) 0.000(3)
C195 0.082(4) 0.059(3) 0.081(3) -0.010(2) 0.031(3) 0.016(3)
C196 0.063(3) 0.057(3) 0.061(3) -0.011(2) 0.016(2) 0.001(2)
C201 0.033(2) 0.049(2) 0.044(2) -0.011(2) 0.0068(15) -0.0013(15)
C202 0.045(2) 0.053(2) 0.050(2) -0.011(2) 0.005(2) -0.004(2)
C203 0.063(3) 0.056(3) 0.066(3) -0.014(2) 0.025(2) -0.015(2)
C204 0.035(2) 0.073(3) 0.088(3) -0.031(3) 0.018(2) -0.011(2)
C205 0.038(2) 0.079(3) 0.080(3) -0.016(3) 0.004(2) 0.005(2)
C206 0.040(2) 0.060(3) 0.065(3) -0.007(2) 0.005(2) 0.003(2)
C211 0.044(2) 0.046(2) 0.041(2) 0.000(2) 0.0009(15) -0.005(2)
C212 0.105(4) 0.051(3) 0.061(3) 0.000(2) -0.002(3) -0.008(3)
C213 0.147(6) 0.072(4) 0.069(4) 0.027(3) -0.013(3) -0.030(4)
C214 0.123(5) 0.107(5) 0.044(3) 0.007(3) -0.002(3) -0.048(4)
C215 0.096(4) 0.088(4) 0.042(2) -0.010(3) 0.000(2) -0.011(3)
C216 0.076(3) 0.062(3) 0.037(2) -0.005(2) 0.001(2) -0.001(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni C18 2.067(4) . ?
Ni C15 2.080(4) . ?
Ni C14 2.114(5) . ?
Ni C17 2.138(4) . ?
Ni P1 2.1447(10) . ?
Ni C16 2.156(5) . ?
Ni S1 2.1834(10) . ?
Br1 C1 1.900(4) . ?
P1 C191 1.826(4) . ?
P1 C211 1.833(4) . ?
P1 C201 1.835(4) . ?
S1 C11 1.766(4) . ?
N1 C7 1.261(5) . ?
N1 C8 1.427(4) . ?
C1 C6 1.350(6) . ?
C1 C2 1.376(6) . ?
C2 C3 1.380(6) . ?
C3 C4 1.368(6) . ?
C4 C5 1.382(6) . ?
C4 C7 1.471(5) . ?
C5 C6 1.383(6) . ?
C8 C13 1.379(5) . ?
C8 C9 1.385(5) . ?
C9 C10 1.383(6) . ?
C10 C11 1.379(6) . ?
C11 C12 1.398(5) . ?
C12 C13 1.377(5) . ?
C14 C15 1.384(7) . ?
C14 C18 1.419(7) . ?
C15 C16 1.420(7) . ?
C16 C17 1.353(7) . ?
C17 C18 1.422(8) . ?
C191 C196 1.370(6) . ?
C191 C192 1.380(6) . ?
C192 C193 1.381(6) . ?
C193 C194 1.369(7) . ?
C194 C195 1.359(7) . ?
C195 C196 1.408(7) . ?
C201 C202 1.382(6) . ?
C201 C206 1.400(5) . ?
C202 C203 1.393(6) . ?
C203 C204 1.377(7) . ?
C204 C205 1.372(8) . ?
C205 C206 1.375(6) . ?
C211 C212 1.367(6) . ?
C211 C216 1.384(6) . ?
C212 C213 1.394(8) . ?
C213 C214 1.351(9) . ?
C214 C215 1.362(8) . ?
C215 C216 1.394(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C18 Ni C15 65.3(2) . . ?
C18 Ni C14 39.7(2) . . ?
C15 Ni C14 38.5(2) . . ?
C18 Ni C17 39.5(2) . . ?
C15 Ni C17 64.5(2) . . ?
C14 Ni C17 65.7(2) . . ?
C18 Ni P1 103.7(2) . . ?
C15 Ni P1 166.4(2) . . ?
C14 Ni P1 127.9(2) . . ?
C17 Ni P1 112.77(14) . . ?
C18 Ni C16 64.1(2) . . ?
C15 Ni C16 39.1(2) . . ?
C14 Ni C16 64.7(2) . . ?
C17 Ni C16 36.7(2) . . ?
P1 Ni C16 145.04(14) . . ?
C18 Ni S1 164.79(15) . . ?
C15 Ni S1 99.53(15) . . ?
C14 Ni S1 127.14(15) . . ?
C17 Ni S1 136.4(2) . . ?
P1 Ni S1 91.18(4) . . ?
C16 Ni S1 105.1(2) . . ?
C191 P1 C211 103.8(2) . . ?
C191 P1 C201 108.5(2) . . ?
C211 P1 C201 100.8(2) . . ?
C191 P1 Ni 110.04(12) . . ?
C211 P1 Ni 117.55(13) . . ?
C201 P1 Ni 115.06(13) . . ?
C11 S1 Ni 112.04(13) . . ?
C7 N1 C8 119.8(4) . . ?
C6 C1 C2 120.6(4) . . ?
C6 C1 Br1 119.7(3) . . ?
C2 C1 Br1 119.7(3) . . ?
C1 C2 C3 119.3(4) . . ?
C4 C3 C2 120.8(4) . . ?
C3 C4 C5 119.0(4) . . ?
C3 C4 C7 121.2(3) . . ?
C5 C4 C7 119.8(4) . . ?
C4 C5 C6 120.1(4) . . ?
C1 C6 C5 120.1(4) . . ?
N1 C7 C4 122.3(4) . . ?
C13 C8 C9 117.9(3) . . ?
C13 C8 N1 124.7(3) . . ?
C9 C8 N1 117.4(4) . . ?
C10 C9 C8 121.1(4) . . ?
C11 C10 C9 121.2(4) . . ?
C10 C11 C12 117.3(3) . . ?
C10 C11 S1 126.3(3) . . ?
C12 C11 S1 116.4(3) . . ?
C13 C12 C11 121.2(4) . . ?
C12 C13 C8 121.1(3) . . ?
C15 C14 C18 105.9(5) . . ?
C15 C14 Ni 69.4(3) . . ?
C18 C14 Ni 68.4(3) . . ?
C14 C15 C16 109.2(5) . . ?
C14 C15 Ni 72.1(3) . . ?
C16 C15 Ni 73.3(3) . . ?
C17 C16 C15 108.4(5) . . ?
C17 C16 Ni 70.9(3) . . ?
C15 C16 Ni 67.5(3) . . ?
C16 C17 C18 107.8(5) . . ?
C16 C17 Ni 72.3(3) . . ?
C18 C17 Ni 67.6(2) . . ?
C14 C18 C17 108.4(5) . . ?
C14 C18 Ni 71.9(3) . . ?
C17 C18 Ni 72.9(3) . . ?
C196 C191 C192 119.0(4) . . ?
C196 C191 P1 123.7(3) . . ?
C192 C191 P1 117.2(3) . . ?
C191 C192 C193 121.9(5) . . ?
C194 C193 C192 118.6(5) . . ?
C195 C194 C193 120.7(5) . . ?
C194 C195 C196 120.4(5) . . ?
C191 C196 C195 119.2(5) . . ?
C202 C201 C206 119.0(4) . . ?
C202 C201 P1 120.1(3) . . ?
C206 C201 P1 120.8(3) . . ?
C201 C202 C203 120.2(4) . . ?
C204 C203 C202 120.0(5) . . ?
C205 C204 C203 119.9(4) . . ?
C204 C205 C206 120.8(5) . . ?
C205 C206 C201 120.0(5) . . ?
C212 C211 C216 117.7(4) . . ?
C212 C211 P1 124.5(3) . . ?
C216 C211 P1 117.8(3) . . ?
C211 C212 C213 121.2(5) . . ?
C214 C213 C212 119.8(6) . . ?
C213 C214 C215 120.8(5) . . ?
C214 C215 C216 119.1(5) . . ?
C211 C216 C215 121.3(5) . . ?
_refine_diff_density_max 0.584
_refine_diff_density_min -0.462
_refine_diff_density_rms 0.067
#==============================================================================
data_4c
#==============================================================================
_audit_creation_date 'Oct 6 17:51:34 1999'
_audit_creation_method 'PLATON
option'
#===============================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name 'Prof. James Darkwa'
_publ_contact_author_address
;
Department of Chemistry
University of the Western Cape
South Africa
;
_publ_contact_author_email 'Jdarkwa@uwc.ac.za'
_publ_contact_author_fax ?
_publ_contact_author_phone ?
_publ_requested_journal ?
_publ_requested_category ?
_publ_requested_coeditor_name ?
_publ_contact_letter ?
#===============================================================================
# TITLE AND AUTHOR LIST
_publ_section_title
;
?
;
_publ_section_title_footnote
;
?
;
loop_
_publ_author_name
_publ_author_address
?
;
?
;
#===============================================================================
_publ_section_synopsis
;
?
;
_publ_section_abstract
;
?
;
_publ_section_comment
;
?
;
_publ_section_exptl_prep
;
?
;
_publ_section_exptl_refinement
;
?
;
_publ_section_references
;
?
;
_publ_section_figure_captions
;
?
;
_publ_section_acknowledgements
;
?
;
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'C31 H44 N Ni P S'
_chemical_formula_structural ?
_chemical_formula_sum
'C31 H44 N Ni P S'
_chemical_formula_weight 552.40
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942
'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'
N N 0.0061 0.0033
'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'
C C 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
_cell_length_a 10.8090(3)
_cell_length_b 10.9160(4)
_cell_length_c 14.4300(6)
_cell_angle_alpha 80.813(2)
_cell_angle_beta 73.796(2)
_cell_angle_gamma 68.446(2)
_cell_volume 1517.53(10)
_cell_formula_units_Z 2
_cell_measurement_temperature 293
_cell_measurement_reflns_used 333
_cell_measurement_theta_min 2
_cell_measurement_theta_max 18
_cell_special_details
; ?
;
_exptl_crystal_description 'block'
_exptl_crystal_colour 'black'
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.27
_exptl_crystal_size_min 0.21
_exptl_crystal_size_rad 0.13
_exptl_crystal_density_meas 'Not Measured'
_exptl_crystal_density_diffrn 1.209
_exptl_crystal_density_method 'Not Measured'
_exptl_crystal_F_000 592
_exptl_absorpt_coefficient_mu 0.78
_exptl_crystal_density_meas_temp 'Not Measured'
_exptl_absorpt_correction_type 'Semi-empirical'
_exptl_absorpt_process_details
;
A data set with a high redundancy was collected. Variation
in intensity due to absorption were corrected by allow the scale factor to
vary.
;
_exptl_absorpt_correction_T_min 'Not Measured'
_exptl_absorpt_correction_T_max 'Not Measured'
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
; ?
;
_diffrn_ambient_temperature 207
_diffrn_radiation_wavelength 0.71070
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator 'graphite'
_diffrn_measurement_device_type 'Nonius KappaCCD diffractometer'
_diffrn_measurement_method ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
_diffrn_reflns_number_diffrn_reflns_number 6774
_diffrn_reflns_av_R_equivalents 0.0000
_diffrn_reflns_av_sigmaI/netI 0.0375
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 3.81
_diffrn_reflns_theta_max 27.53
_reflns_number_total 6774
_reflns_number_gt 5710
_reflns_threshold_expression >2sigma(I)
_diffrn_measured_fraction_theta_full ?
_diffrn_reflns_reduction_process
;
The 4 sets of data were scaled using Denzo-SMN.
Unit cell dimensions were refined on all data.
;
_computing_data_collection 'Collect (Nonius B.V., 1998)'
_computing_cell_refinement
'Denzo-SMN (Z.Otwinowski and W.Minor,1997)'
_computing_data_reduction
'Denzo-SMN (Z.Otwinowski and W.Minor,1997)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'PLATON (Spek, 1990)'
_computing_publication_material 'PLATON (Spek, 1990)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.1131P)^2^+4.1902P] where P=(Fo^2^+2Fc^2^)/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 SHELXL
_refine_ls_extinction_coef 0.002(3)
_refine_ls_extinction_expression
'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns 6774
_refine_ls_number_parameters 332
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0765
_refine_ls_R_factor_gt 0.0643
_refine_ls_wR_factor_ref 0.1852
_refine_ls_wR_factor_gt 0.1727
_refine_ls_goodness_of_fit_ref 0.903
_refine_ls_restrained_S_all 0.903
_refine_ls_shift/su_max 1.450
_refine_ls_shift/su_mean 0.113
_diffrn_measured_fraction_theta_max 0.969
_diffrn_reflns_theta_full 27.53
_refine_diff_density_max 3.270
_refine_diff_density_min -3.048
_refine_diff_density_rms 0.089
#===============================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
Ni1 Ni Uani 0.18810 0.55000 0.23360 1.000 0.0292
S1B S Uani 0.26673 0.68028 0.12344 1.000 0.0370
P1 P Uani 0.37820 0.39115 0.20291 1.000 0.0301
N1B N Uani 0.00278 0.81296 -0.21178 1.000 0.0390
C1 C Uani 0.00178 0.69044 0.30181 1.000 0.0555
C2 C Uani -0.02989 0.60758 0.25101 1.000 0.0490
C3 C Uani 0.01903 0.47851 0.28885 1.000 0.0422
C4 C Uani 0.08084 0.48142 0.36358 1.000 0.0424
C5 C Uani 0.06169 0.61309 0.37558 1.000 0.0507
C6 C Uani 0.18182 0.71666 0.02908 1.000 0.0324
C7 C Uani 0.13448 0.63023 -0.00025 1.000 0.0371
C8 C Uani 0.07684 0.66201 -0.07916 1.000 0.0380
C9 C Uani 0.06150 0.78447 -0.13071 1.000 0.0355
C10 C Uani 0.10998 0.87112 -0.10287 1.000 0.0392
C11 C Uani 0.16930 0.83756 -0.02451 1.000 0.0385
C12 C Uani -0.07342 0.93082 -0.22768 1.000 0.0393
C13 C Uani -0.12579 0.97579 -0.31490 1.000 0.0367
C14 C Uani -0.09456 0.89377 -0.38931 1.000 0.0392
C15 C Uani -0.13950 0.94403 -0.47295 1.000 0.0432
C16 C Uani -0.21518 1.07780 -0.48542 1.000 0.0429
C17 C Uani -0.24775 1.15763 -0.41137 1.000 0.0455
C18 C Uani -0.20440 1.10873 -0.32689 1.000 0.0444
C19 C Uani -0.26039 1.13264 -0.57785 1.000 0.0641
C20 C Uani 0.38747 0.24448 0.28593 1.000 0.0383
C21 C Uani 0.51885 0.12413 0.26487 1.000 0.0488
C22 C Uani 0.51274 0.01079 0.33841 1.000 0.0802
C23 C Uani 0.35004 0.23213 -0.03359 1.000 0.0749
C24 C Uani 0.42054 0.33213 0.08262 1.000 0.0413
C25 C Uani 0.32861 0.26084 0.07150 1.000 0.0454
C26 C Uani 0.64214 -0.11048 0.31977 1.000 0.1166
C27 C Uani 0.28240 0.14342 -0.04426 1.000 0.1473
C28 C Uani 0.52763 0.43164 0.20367 1.000 0.0352
C29 C Uani 0.52270 0.47338 0.30142 1.000 0.0392
C30 C Uani 0.64790 0.50523 0.30207 1.000 0.0446
C31 C Uani 0.64805 0.53600 0.40046 1.000 0.0530
H1 H Uiso -0.01466 0.78043 0.28811 1.000 0.0666
H2 H Uiso -0.07532 0.63535 0.20132 1.000 0.0589
H3 H Uiso 0.01272 0.40434 0.26923 1.000 0.0506
H4 H Uiso 0.12654 0.40788 0.39878 1.000 0.0509
H5 H Uiso 0.08441 0.64296 0.42326 1.000 0.0609
H6 H Uiso 0.23104 0.31202 0.09932 1.000 0.0439
H7 H Uiso 0.14172 0.54912 0.03398 1.000 0.0446
H8 H Uiso 0.04808 0.60140 -0.09807 1.000 0.0456
H10 H Uiso 0.10256 0.95226 -0.13707 1.000 0.0470
H11 H Uiso 0.20146 0.89668 -0.00718 1.000 0.0462
H12 H Uiso -0.09698 0.99134 -0.18163 1.000 0.0472
H14 H Uiso -0.04321 0.80478 -0.38258 1.000 0.0470
H15 H Uiso -0.11908 0.88808 -0.52155 1.000 0.0518
H17 H Uiso -0.29999 1.24635 -0.41811 1.000 0.0546
H18 H Uiso -0.22777 1.16475 -0.27778 1.000 0.0533
H19A H Uiso -0.22363 1.20126 -0.60720 1.000 0.0961
H19B H Uiso -0.22770 1.06350 -0.62142 1.000 0.0961
H19C H Uiso -0.35863 1.16813 -0.56381 1.000 0.0961
H20A H Uiso 0.31101 0.21746 0.28699 1.000 0.0460
H20B H Uiso 0.37462 0.26963 0.35038 1.000 0.0460
H22A H Uiso 0.49814 0.03925 0.40213 1.000 0.0963
H22B H Uiso 0.43492 -0.01330 0.33821 1.000 0.0963
H23A H Uiso 0.44754 0.19365 -0.06146 1.000 0.0899
H23B H Uiso 0.31602 0.31491 -0.07007 1.000 0.0899
H24A H Uiso 0.51478 0.27269 0.06844 1.000 0.0495
H24B H Uiso 0.41395 0.40680 0.03540 1.000 0.0495
H26A H Uiso 0.63302 -0.17868 0.36943 1.000 0.1750
H26B H Uiso 0.65523 -0.14154 0.25795 1.000 0.1750
H26C H Uiso 0.71966 -0.08760 0.32019 1.000 0.1750
H27A H Uiso 0.29802 0.13187 -0.11164 1.000 0.2209
H27B H Uiso 0.31891 0.05946 -0.01131 1.000 0.2209
H27C H Uiso 0.18575 0.18053 -0.01685 1.000 0.2209
H28 H Uiso 0.33708 0.18037 0.11108 1.000 0.0582
H28A H Uiso 0.53498 0.50265 0.15498 1.000 0.0423
H28B H Uiso 0.60931 0.35530 0.18592 1.000 0.0423
H29 H Uiso 0.60117 0.14766 0.26012 1.000 0.0481
H29A H Uiso 0.51419 0.40286 0.35030 1.000 0.0471
H29B H Uiso 0.44170 0.55046 0.31879 1.000 0.0471
H30 H Uiso 0.53893 0.09861 0.20301 1.000 0.0754
H30A H Uiso 0.65229 0.58040 0.25690 1.000 0.0535
H30B H Uiso 0.72944 0.43070 0.27973 1.000 0.0535
H31A H Uiso 0.72928 0.55546 0.39605 1.000 0.0794
H31B H Uiso 0.56867 0.61090 0.42257 1.000 0.0794
H31C H Uiso 0.64630 0.46118 0.44528 1.000 0.0794
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0254 0.0294 0.0283 -0.0020 -0.0020 -0.0074
S1B 0.0406 0.0403 0.0338 0.0046 -0.0105 -0.0196
P1 0.0242 0.0313 0.0313 -0.0044 -0.0015 -0.0083
N1B 0.0434 0.0401 0.0338 0.0026 -0.0098 -0.0162
C1 0.0280 0.0357 0.0824 -0.0136 0.0106 -0.0011
C2 0.0237 0.0566 0.0570 0.0021 -0.0066 -0.0071
C3 0.0308 0.0468 0.0468 -0.0054 0.0045 -0.0200
C4 0.0362 0.0477 0.0328 0.0050 0.0057 -0.0156
C5 0.0458 0.0625 0.0375 -0.0198 0.0108 -0.0197
C6 0.0329 0.0313 0.0279 -0.0005 -0.0030 -0.0088
C7 0.0415 0.0315 0.0375 0.0042 -0.0101 -0.0136
C8 0.0439 0.0339 0.0375 -0.0014 -0.0091 -0.0157
C9 0.0367 0.0352 0.0308 -0.0005 -0.0055 -0.0104
C10 0.0443 0.0313 0.0397 0.0068 -0.0097 -0.0142
C11 0.0437 0.0317 0.0408 0.0010 -0.0100 -0.0152
C12 0.0421 0.0398 0.0353 -0.0045 -0.0083 -0.0130
C13 0.0388 0.0350 0.0367 -0.0010 -0.0105 -0.0124
C14 0.0449 0.0316 0.0421 0.0002 -0.0124 -0.0138
C15 0.0493 0.0426 0.0426 -0.0044 -0.0146 -0.0180
C16 0.0448 0.0452 0.0439 0.0052 -0.0192 -0.0182
C17 0.0461 0.0325 0.0589 -0.0004 -0.0216 -0.0091
C18 0.0482 0.0361 0.0501 -0.0096 -0.0173 -0.0090
C19 0.0709 0.0658 0.0606 0.0065 -0.0371 -0.0178
C20 0.0321 0.0328 0.0488 0.0025 -0.0099 -0.0116
C21 0.0430 0.0365 0.0644 -0.0084 -0.0190 -0.0042
C22 0.0547 0.0387 0.1464 0.0272 -0.0389 -0.0177
C23 0.0909 0.0876 0.0594 -0.0300 -0.0059 -0.0441
C24 0.0331 0.0488 0.0366 -0.0144 0.0028 -0.0114
C25 0.0495 0.0428 0.0461 -0.0124 -0.0080 -0.0169
C26 0.1110 0.0366 0.2066 -0.0016 -0.0869 0.0033
C27 0.1411 0.1990 0.1319 -0.0812 -0.0013 -0.0866
C28 0.0286 0.0366 0.0376 -0.0032 -0.0032 -0.0109
C29 0.0320 0.0429 0.0414 -0.0070 -0.0035 -0.0134
C30 0.0405 0.0524 0.0434 -0.0025 -0.0056 -0.0222
C31 0.0478 0.0671 0.0529 -0.0099 -0.0097 -0.0292
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;
Bond distances, angles etc. have been calculated using the
rounded fractional coordinates. All esds are estimated
from the variances of the (full) variance-covariance matrix.
The cell esds are taken into account in the estimation of
distances, angles and torsion angles
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 S1B 2.1642 . . yes
Ni1 P1 2.1318 . . yes
Ni1 C1 2.1170 . . yes
Ni1 C2 2.1545 . . yes
Ni1 C3 2.1495 . . yes
Ni1 C4 2.0972 . . yes
Ni1 C5 2.1761 . . yes
S1B C6 1.7639 . . yes
P1 C20 1.8289 . . yes
P1 C24 1.8261 . . yes
P1 C28 1.8277 . . yes
N1B C9 1.4217 . . yes
N1B C12 1.2724 . . yes
C1 C2 1.4325 . . no
C1 C5 1.4006 . . no
C2 C3 1.3896 . . no
C3 C4 1.4280 . . no
C4 C5 1.4069 . . no
C6 C7 1.3907 . . no
C6 C11 1.3997 . . no
C7 C8 1.3842 . . no
C8 C9 1.3987 . . no
C9 C10 1.3906 . . no
C10 C11 1.3870 . . no
C12 C13 1.4634 . . no
C13 C14 1.3968 . . no
C13 C18 1.3978 . . no
C14 C15 1.3834 . . no
C15 C16 1.3979 . . no
C16 C17 1.3738 . . no
C16 C19 1.5065 . . no
C17 C18 1.3848 . . no
C20 C21 1.5332 . . no
C21 C22 1.5043 . . no
C22 C26 1.5246 . . no
C23 C25 1.5342 . . no
C23 C27 1.4583 . . no
C24 C25 1.5217 . . no
C28 C29 1.5316 . . no
C29 C30 1.5187 . . no
C30 C31 1.5107 . . no
C1 H1 0.9300 . . no
C2 H2 0.9300 . . no
C3 H3 0.9300 . . no
C4 H4 0.9300 . . no
C5 H5 0.9300 . . no
C7 H7 0.9300 . . no
C8 H8 0.9300 . . no
C10 H10 0.9300 . . no
C11 H11 0.9300 . . no
C12 H12 0.9300 . . no
C14 H14 0.9300 . . no
C15 H15 0.9300 . . no
C17 H17 0.9300 . . no
C18 H18 0.9300 . . no
C19 H19A 0.9600 . . no
C19 H19B 0.9600 . . no
C19 H19C 0.9600 . . no
C20 H20A 0.9700 . . no
C20 H20B 0.9700 . . no
C21 H29 0.9953 . . no
C21 H30 0.9210 . . no
C22 H22A 0.9700 . . no
C22 H22B 0.9700 . . no
C23 H23A 0.9700 . . no
C23 H23B 0.9700 . . no
C24 H24A 0.9700 . . no
C24 H24B 0.9700 . . no
C25 H6 0.9940 . . no
C25 H28 0.9572 . . no
C26 H26A 0.9600 . . no
C26 H26B 0.9600 . . no
C26 H26C 0.9600 . . no
C27 H27A 0.9600 . . no
C27 H27B 0.9600 . . no
C27 H27C 0.9600 . . no
C28 H28A 0.9700 . . no
C28 H28B 0.9700 . . no
C29 H29A 0.9700 . . no
C29 H29B 0.9700 . . no
C30 H30A 0.9700 . . no
C30 H30B 0.9700 . . no
C31 H31A 0.9600 . . no
C31 H31B 0.9600 . . no
C31 H31C 0.9600 . . no
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1B Ni1 P1 92.00 . . . yes
S1B Ni1 C1 98.89 . . . yes
S1B Ni1 C2 109.29 . . . yes
S1B Ni1 C3 143.72 . . . yes
S1B Ni1 C4 161.17 . . . yes
S1B Ni1 C5 122.85 . . . yes
P1 Ni1 C1 165.02 . . . yes
P1 Ni1 C2 144.65 . . . yes
P1 Ni1 C3 111.27 . . . yes
P1 Ni1 C4 102.78 . . . yes
P1 Ni1 C5 126.99 . . . yes
C1 Ni1 C2 39.18 . . . yes
C1 Ni1 C3 64.78 . . . yes
C1 Ni1 C4 64.62 . . . yes
C1 Ni1 C5 38.05 . . . yes
C2 Ni1 C3 37.67 . . . yes
C2 Ni1 C4 64.34 . . . yes
C2 Ni1 C5 64.13 . . . yes
C3 Ni1 C4 39.27 . . . yes
C3 Ni1 C5 64.61 . . . yes
C4 Ni1 C5 38.39 . . . yes
Ni1 S1B C6 109.40 . . . yes
Ni1 P1 C20 114.80 . . . yes
Ni1 P1 C24 113.02 . . . yes
Ni1 P1 C28 114.64 . . . yes
C20 P1 C24 105.10 . . . yes
C20 P1 C28 104.64 . . . yes
C24 P1 C28 103.46 . . . yes
C9 N1B C12 118.20 . . . yes
Ni1 C1 C2 71.83 . . . yes
Ni1 C1 C5 73.26 . . . yes
C2 C1 C5 108.49 . . . no
Ni1 C2 C1 69.00 . . . yes
Ni1 C2 C3 70.97 . . . yes
C1 C2 C3 108.16 . . . no
Ni1 C3 C2 71.36 . . . yes
Ni1 C3 C4 68.39 . . . yes
C2 C3 C4 106.96 . . . no
Ni1 C4 C3 72.34 . . . yes
Ni1 C4 C5 73.84 . . . yes
C3 C4 C5 109.26 . . . no
Ni1 C5 C1 68.69 . . . yes
Ni1 C5 C4 67.77 . . . yes
C1 C5 C4 106.71 . . . no
S1B C6 C7 124.68 . . . yes
S1B C6 C11 117.76 . . . yes
C7 C6 C11 117.41 . . . no
C6 C7 C8 121.59 . . . no
C7 C8 C9 120.57 . . . no
N1B C9 C8 118.86 . . . yes
N1B C9 C10 122.70 . . . yes
C8 C9 C10 118.38 . . . no
C9 C10 C11 120.56 . . . no
C6 C11 C10 121.46 . . . no
N1B C12 C13 123.19 . . . yes
C12 C13 C14 123.05 . . . no
C12 C13 C18 118.53 . . . no
C14 C13 C18 118.33 . . . no
C13 C14 C15 120.44 . . . no
C14 C15 C16 120.90 . . . no
C15 C16 C17 118.46 . . . no
C15 C16 C19 120.62 . . . no
C17 C16 C19 120.91 . . . no
C16 C17 C18 121.36 . . . no
C13 C18 C17 120.49 . . . no
P1 C20 C21 117.40 . . . yes
C20 C21 C22 111.87 . . . no
C21 C22 C26 113.22 . . . no
C25 C23 C27 114.02 . . . no
P1 C24 C25 113.83 . . . yes
C23 C25 C24 112.99 . . . no
P1 C28 C29 113.77 . . . yes
C28 C29 C30 113.59 . . . no
C29 C30 C31 113.50 . . . no
Ni1 C1 H1 120.89 . . . no
C2 C1 H1 125.76 . . . no
C5 C1 H1 125.76 . . . no
Ni1 C2 H2 125.69 . . . no
C1 C2 H2 125.92 . . . no
C3 C2 H2 125.92 . . . no
Ni1 C3 H3 125.31 . . . no
C2 C3 H3 126.52 . . . no
C4 C3 H3 126.52 . . . no
Ni1 C4 H4 120.16 . . . no
C3 C4 H4 125.37 . . . no
C5 C4 H4 125.37 . . . no
Ni1 C5 H5 128.42 . . . no
C1 C5 H5 126.65 . . . no
C4 C5 H5 126.65 . . . no
C6 C7 H7 119.21 . . . no
C8 C7 H7 119.21 . . . no
C7 C8 H8 119.71 . . . no
C9 C8 H8 119.71 . . . no
C9 C10 H10 119.72 . . . no
C11 C10 H10 119.72 . . . no
C6 C11 H11 119.27 . . . no
C10 C11 H11 119.27 . . . no
N1B C12 H12 118.40 . . . no
C13 C12 H12 118.40 . . . no
C13 C14 H14 119.78 . . . no
C15 C14 H14 119.78 . . . no
C14 C15 H15 119.55 . . . no
C16 C15 H15 119.55 . . . no
C16 C17 H17 119.32 . . . no
C18 C17 H17 119.32 . . . no
C13 C18 H18 119.76 . . . no
C17 C18 H18 119.76 . . . no
C16 C19 H19A 109.47 . . . no
C16 C19 H19B 109.47 . . . no
C16 C19 H19C 109.47 . . . no
H19A C19 H19B 109.47 . . . no
H19A C19 H19C 109.47 . . . no
H19B C19 H19C 109.47 . . . no
P1 C20 H20A 107.95 . . . no
P1 C20 H20B 107.95 . . . no
C21 C20 H20A 107.95 . . . no
C21 C20 H20B 107.95 . . . no
H20A C20 H20B 107.22 . . . no
C20 C21 H29 111.16 . . . no
C20 C21 H30 111.79 . . . no
C22 C21 H29 111.06 . . . no
C22 C21 H30 111.11 . . . no
H29 C21 H30 99.24 . . . no
C21 C22 H22A 108.93 . . . no
C21 C22 H22B 108.93 . . . no
C26 C22 H22A 108.93 . . . no
C26 C22 H22B 108.93 . . . no
H22A C22 H22B 107.75 . . . no
C25 C23 H23A 108.75 . . . no
C25 C23 H23B 108.75 . . . no
C27 C23 H23A 108.75 . . . no
C27 C23 H23B 108.75 . . . no
H23A C23 H23B 107.65 . . . no
P1 C24 H24A 108.79 . . . no
P1 C24 H24B 108.79 . . . no
C25 C24 H24A 108.79 . . . no
C25 C24 H24B 108.79 . . . no
H24A C24 H24B 107.67 . . . no
C23 C25 H6 110.84 . . . no
C23 C25 H28 108.78 . . . no
C24 C25 H6 110.02 . . . no
C24 C25 H28 113.66 . . . no
H6 C25 H28 99.81 . . . no
C22 C26 H26A 109.47 . . . no
C22 C26 H26B 109.47 . . . no
C22 C26 H26C 109.47 . . . no
H26A C26 H26B 109.47 . . . no
H26A C26 H26C 109.47 . . . no
H26B C26 H26C 109.47 . . . no
C23 C27 H27A 109.47 . . . no
C23 C27 H27B 109.47 . . . no
C23 C27 H27C 109.47 . . . no
H27A C27 H27B 109.47 . . . no
H27A C27 H27C 109.47 . . . no
H27B C27 H27C 109.47 . . . no
P1 C28 H28A 108.81 . . . no
P1 C28 H28B 108.81 . . . no
C29 C28 H28A 108.80 . . . no
C29 C28 H28B 108.81 . . . no
H28A C28 H28B 107.68 . . . no
C28 C29 H29A 108.85 . . . no
C28 C29 H29B 108.85 . . . no
C30 C29 H29A 108.85 . . . no
C30 C29 H29B 108.85 . . . no
H29A C29 H29B 107.70 . . . no
C29 C30 H30A 108.87 . . . no
C29 C30 H30B 108.87 . . . no
C31 C30 H30A 108.87 . . . no
C31 C30 H30B 108.87 . . . no
H30A C30 H30B 107.71 . . . no
C30 C31 H31A 109.47 . . . no
C30 C31 H31B 109.47 . . . no
C30 C31 H31C 109.47 . . . no
H31A C31 H31B 109.47 . . . no
H31A C31 H31C 109.47 . . . no
H31B C31 H31C 109.47 . . . no
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
P1 Ni1 S1B C6 112.60 . . . . no
C1 Ni1 S1B C6 -77.72 . . . . no
C2 Ni1 S1B C6 -38.67 . . . . no
C3 Ni1 S1B C6 -18.77 . . . . no
C5 Ni1 S1B C6 -109.75 . . . . no
S1B Ni1 P1 C20 173.46 . . . . no
C2 Ni1 P1 C20 -58.19 . . . . no
C3 Ni1 P1 C20 -35.01 . . . . no
C4 Ni1 P1 C20 5.21 . . . . no
C5 Ni1 P1 C20 38.56 . . . . no
S1B Ni1 P1 C24 -66.00 . . . . no
C2 Ni1 P1 C24 62.35 . . . . no
C3 Ni1 P1 C24 85.53 . . . . no
C4 Ni1 P1 C24 125.76 . . . . no
C5 Ni1 P1 C24 159.10 . . . . no
S1B Ni1 P1 C28 52.24 . . . . no
C2 Ni1 P1 C28 -179.40 . . . . no
C3 Ni1 P1 C28 -156.22 . . . . no
C4 Ni1 P1 C28 -116.00 . . . . no
C5 Ni1 P1 C28 -82.65 . . . . no
S1B Ni1 C1 C2 109.72 . . . . no
C3 Ni1 C1 C2 -36.19 . . . . no
C4 Ni1 C1 C2 -79.84 . . . . no
C5 Ni1 C1 C2 -116.57 . . . . no
S1B Ni1 C1 C5 -133.71 . . . . no
C2 Ni1 C1 C5 116.57 . . . . no
C3 Ni1 C1 C5 80.37 . . . . no
C4 Ni1 C1 C5 36.73 . . . . no
C5 Ni1 C2 C3 -81.27 . . . . no
P1 Ni1 C4 C3 -108.08 . . . . no
C1 Ni1 C4 C3 80.51 . . . . no
C2 Ni1 C4 C3 36.89 . . . . no
C5 Ni1 C4 C3 116.92 . . . . no
P1 Ni1 C4 C5 135.00 . . . . no
S1B Ni1 C2 C1 -80.19 . . . . no
P1 Ni1 C2 C1 155.95 . . . . no
C3 Ni1 C2 C1 119.05 . . . . no
C4 Ni1 C2 C1 80.60 . . . . no
C5 Ni1 C2 C1 37.78 . . . . no
S1B Ni1 C2 C3 160.76 . . . . no
P1 Ni1 C2 C3 36.89 . . . . no
C1 Ni1 C2 C3 -119.05 . . . . no
C4 Ni1 C2 C3 -38.45 . . . . no
C2 Ni1 C5 C1 -38.90 . . . . no
C4 Ni1 C5 C1 -119.53 . . . . no
S1B Ni1 C5 C4 177.75 . . . . no
P1 Ni1 C5 C4 -59.68 . . . . no
S1B Ni1 C3 C2 -31.71 . . . . no
P1 Ni1 C3 C2 -158.11 . . . . no
C1 Ni1 C3 C2 37.62 . . . . no
C4 Ni1 C3 C2 117.69 . . . . no
C5 Ni1 C3 C2 79.89 . . . . no
S1B Ni1 C3 C4 -149.40 . . . . no
P1 Ni1 C3 C4 84.20 . . . . no
C1 Ni1 C3 C4 -80.07 . . . . no
C2 Ni1 C3 C4 -117.69 . . . . no
C5 Ni1 C3 C4 -37.80 . . . . no
P1 Ni1 C5 C1 -179.21 . . . . no
C1 Ni1 C4 C5 -36.41 . . . . no
C3 Ni1 C5 C1 -80.86 . . . . no
C3 Ni1 C4 C5 -116.92 . . . . no
C2 Ni1 C5 C4 80.63 . . . . no
S1B Ni1 C5 C1 58.22 . . . . no
C1 Ni1 C5 C4 119.53 . . . . no
C3 Ni1 C5 C4 38.67 . . . . no
C2 Ni1 C4 C5 -80.03 . . . . no
Ni1 S1B C6 C7 -32.69 . . . . no
Ni1 S1B C6 C11 151.87 . . . . no
C28 P1 C24 C25 165.95 . . . . no
C20 P1 C28 C29 -65.29 . . . . no
C24 P1 C28 C29 -175.13 . . . . no
Ni1 P1 C24 C25 -69.47 . . . . no
Ni1 P1 C28 C29 61.34 . . . . no
C20 P1 C24 C25 56.46 . . . . no
Ni1 P1 C20 C21 177.00 . . . . no
C24 P1 C20 C21 52.19 . . . . no
C28 P1 C20 C21 -56.46 . . . . no
C9 N1B C12 C13 172.25 . . . . no
C12 N1B C9 C8 144.50 . . . . no
C12 N1B C9 C10 -38.39 . . . . no
C2 C1 C5 C4 6.40 . . . . no
C5 C1 C2 C3 -4.15 . . . . no
C2 C1 C5 Ni1 63.64 . . . . no
Ni1 C1 C2 C3 60.43 . . . . no
C5 C1 C2 Ni1 -64.57 . . . . no
Ni1 C1 C5 C4 -57.24 . . . . no
C1 C2 C3 Ni1 -59.19 . . . . no
C1 C2 C3 C4 0.20 . . . . no
Ni1 C2 C3 C4 59.39 . . . . no
C2 C3 C4 Ni1 -61.30 . . . . no
Ni1 C3 C4 C5 65.12 . . . . no
C2 C3 C4 C5 3.82 . . . . no
C3 C4 C5 C1 -6.34 . . . . no
C3 C4 C5 Ni1 -64.16 . . . . no
Ni1 C4 C5 C1 57.82 . . . . no
S1B C6 C11 C10 176.82 . . . . no
C7 C6 C11 C10 1.05 . . . . no
C11 C6 C7 C8 -0.14 . . . . no
S1B C6 C7 C8 -175.59 . . . . no
C6 C7 C8 C9 -1.54 . . . . no
C7 C8 C9 N1B 179.53 . . . . no
C7 C8 C9 C10 2.28 . . . . no
C8 C9 C10 C11 -1.39 . . . . no
N1B C9 C10 C11 -178.52 . . . . no
C9 C10 C11 C6 -0.28 . . . . no
N1B C12 C13 C14 -1.25 . . . . no
N1B C12 C13 C18 -177.55 . . . . no
C12 C13 C18 C17 175.34 . . . . no
C14 C13 C18 C17 -1.14 . . . . no
C18 C13 C14 C15 0.68 . . . . no
C12 C13 C14 C15 -175.62 . . . . no
C13 C14 C15 C16 0.91 . . . . no
C14 C15 C16 C17 -2.03 . . . . no
C14 C15 C16 C19 178.26 . . . . no
C19 C16 C17 C18 -178.71 . . . . no
C15 C16 C17 C18 1.58 . . . . no
C16 C17 C18 C13 -0.02 . . . . no
P1 C20 C21 C22 -179.92 . . . . no
C20 C21 C22 C26 -179.80 . . . . no
C27 C23 C25 C24 169.35 . . . . no
P1 C24 C25 C23 170.59 . . . . no
P1 C28 C29 C30 179.26 . . . . no
C28 C29 C30 C31 -175.48 . . . . no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Ni1 H6 3.3072 . . no
Ni1 H7 3.0606 . . no
Ni1 H29B 3.3043 . . no
Ni1 H18 3.4719 . 2_575 no
S1B H24B 3.1066 . . no
S1B H28A 2.9493 . . no
S1B H18 2.8557 . 2_575 no
N1B H14 2.6675 . . no
N1B H3 2.7090 . 2_565 no
C2 C7 3.5784 . . no
C7 C2 3.5784 . . no
C14 C15 3.5842 . 2_574 no
C14 C16 3.4321 . 2_574 no
C15 C15 3.5050 . 2_574 no
C15 C14 3.5842 . 2_574 no
C16 C14 3.4321 . 2_574 no
C1 H26C 3.0928 . 1_465 no
C2 H31A 3.0245 . 1_455 no
C3 H31A 2.9471 . 1_455 no
C8 H27C 2.8127 . 2_565 no
C9 H27C 2.8559 . 2_565 no
C10 H12 2.6084 . . no
C11 H24A 3.0866 . 2_665 no
C12 H10 2.6824 . . no
C14 H20A 2.9521 . 2_565 no
C16 H22B 2.9299 . 2_565 no
C17 H22B 2.8824 . 2_565 no
C18 H22B 3.0836 . 2_565 no
C19 H29 3.0633 . 1_464 no
C20 H4 2.9078 . . no
C20 H28 2.9603 . . no
C20 H29A 2.9480 . . no
C21 H24A 3.0356 . . no
C21 H28B 2.9825 . . no
C24 H30 2.9297 . . no
C25 H20A 3.0324 . . no
C26 H19B 3.0742 . 1_646 no
C26 H27A 2.9192 . 2_655 no
C27 H11 3.0522 . 1_545 no
C27 H26B 2.9687 . 2_655 no
C28 H29 2.9411 . . no
C29 H20B 3.0806 . . no
C31 H26A 3.0250 . 1_565 no
H3 N1B 2.7090 . 2_565 no
H3 H14 2.5594 . 2_565 no
H4 C20 2.9078 . . no
H4 H20B 2.5047 . . no
H6 Ni1 3.3072 . . no
H6 H7 2.5324 . . no
H7 Ni1 3.0606 . . no
H7 H6 2.5324 . . no
H10 C12 2.6824 . . no
H10 H12 2.2929 . . no
H11 C27 3.0522 . 1_565 no
H11 H27B 2.5207 . 1_565 no
H12 C10 2.6084 . . no
H12 H10 2.2929 . . no
H12 H18 2.4076 . . no
H14 N1B 2.6675 . . no
H14 H3 2.5594 . 2_565 no
H15 H19B 2.3523 . . no
H17 H29B 2.5716 . 2_575 no
H18 H12 2.4076 . . no
H18 Ni1 3.4719 . 2_575 no
H18 S1B 2.8557 . 2_575 no
H19B C26 3.0742 . 1_464 no
H19B H15 2.3523 . . no
H19B H26C 2.2704 . 1_464 no
H20A C25 3.0324 . . no
H20A H22B 2.4828 . . no
H20A H28 2.5557 . . no
H20A C14 2.9521 . 2_565 no
H20B C29 3.0806 . . no
H20B H4 2.5047 . . no
H20B H22A 2.4809 . . no
H20B H29A 2.4498 . . no
H22A H20B 2.4809 . . no
H22B H20A 2.4828 . . no
H22B C16 2.9299 . 2_565 no
H22B C17 2.8824 . 2_565 no
H22B C18 3.0836 . 2_565 no
H23A H24A 2.5541 . . no
H23B H24B 2.5710 . . no
H24A C21 3.0356 . . no
H24A H23A 2.5541 . . no
H24A H30 2.4879 . . no
H24A C11 3.0866 . 2_665 no
H24B S1B 3.1066 . . no
H24B H23B 2.5710 . . no
H26A C31 3.0250 . 1_545 no
H26A H31B 2.5809 . 1_545 no
H26B H30 2.5597 . . no
H26B C27 2.9687 . 2_655 no
H26B H27A 2.0240 . 2_655 no
H26C C1 3.0928 . 1_645 no
H26C H19B 2.2704 . 1_646 no
H26C H29 2.5453 . . no
H27A C26 2.9192 . 2_655 no
H27A H26B 2.0240 . 2_655 no
H27B H11 2.5207 . 1_545 no
H27B H28 2.4552 . . no
H27C C8 2.8127 . 2_565 no
H27C C9 2.8559 . 2_565 no
H28 C20 2.9603 . . no
H28 H20A 2.5557 . . no
H28 H27B 2.4552 . . no
H28A S1B 2.9493 . . no
H28A H30A 2.5926 . . no
H28B C21 2.9825 . . no
H28B H29 2.3688 . . no
H28B H30B 2.5136 . . no
H29 C19 3.0633 . 1_646 no
H29 C28 2.9411 . . no
H29 H26C 2.5453 . . no
H29 H28B 2.3688 . . no
H29A C20 2.9480 . . no
H29A H20B 2.4498 . . no
H29A H31C 2.5222 . . no
H29B Ni1 3.3043 . . no
H29B H31B 2.5863 . . no
H29B H17 2.5716 . 2_575 no
H30 C24 2.9297 . . no
H30 H24A 2.4879 . . no
H30 H26B 2.5597 . . no
H30A H28A 2.5926 . . no
H30B H28B 2.5136 . . no
H31A C2 3.0245 . 1_655 no
H31A C3 2.9471 . 1_655 no
H31B H26A 2.5809 . 1_565 no
H31B H29B 2.5863 . . no
H31C H29A 2.5222 . . no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
#
#D H A D - H H...A D...A D - H...A symm(A)
#
C18 H18 S1B 0.9300 2.8557 3.7805 173.00 2_575 yes
# End of Crystallographic Information File