 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C21 H22 N4 NI O2 S2, 4.5(H2 O)'
_chemical_formula_sum
 'C21 H31 N4 Ni O6.50 S2'
_chemical_formula_weight          566.33
 
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'
 '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            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                    8.2431(5)
_cell_length_b                    17.0179(11)
_cell_length_c                    19.4384(12)
_cell_angle_alpha                 74.385(2)
_cell_angle_beta                  83.143(3)
_cell_angle_gamma                 82.030(4)
_cell_volume                      2591.2(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     159895
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        Rod
_exptl_crystal_colour             Orange
_exptl_crystal_size_max           0.15
_exptl_crystal_size_mid           0.04
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.452
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1188
_exptl_absorpt_coefficient_mu     0.955
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8700
_exptl_absorpt_correction_T_max   0.9628
_exptl_absorpt_process_details    
'SORTAV (R. H. Blessing, Acta Cryst. A51 '
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Enraf Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf Nonius KappaCCD area detector'
_diffrn_measurement_method        'ω and φ scans to fill Ewald sphere'
_diffrn_detector_area_resol_mean  '9.091 pixels/mm'
_diffrn_standards_number          'n/a'
_diffrn_standards_interval_count  'n/a'
_diffrn_standards_interval_time   'n/a'
_diffrn_standards_decay_%         'n/a'
_diffrn_reflns_number             39020
_diffrn_reflns_av_R_equivalents   0.0961
_diffrn_reflns_av_sigmaI/netI     0.0745
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -20
_diffrn_reflns_limit_k_max        20
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        23
_diffrn_reflns_theta_min          2.92
_diffrn_reflns_theta_max          25.02
_reflns_number_total              9082
_reflns_number_gt                 6418
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
;
'DENZO (Otwinowski and Minor, 1997) & COLLECT (Hooft, 1998) '
;
_computing_cell_refinement        'DENZO and COLLECT'
_computing_data_reduction         'DENZO and COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'PLATON (Watkin, Pearce 1995)'
_computing_publication_material   SHELXL-97
 
_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 > 2σ(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)+(0.1119P)²+8.9352P] 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          9082
_refine_ls_number_parameters      628
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1022
_refine_ls_R_factor_gt            0.0662
_refine_ls_wR_factor_ref          0.1971
_refine_ls_wR_factor_gt           0.1761
_refine_ls_goodness_of_fit_ref    0.950
_refine_ls_restrained_S_all       0.950
_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
O1W O 0.0468(8) 0.5254(4) 0.3468(3) 0.0749(17) Uani 1 1 d . . .
O2W O 0.8894(8) 0.3288(5) 0.7591(4) 0.087(2) Uani 1 1 d . . .
O3W O 0.3305(8) 0.4109(4) 0.3553(4) 0.0841(19) Uani 1 1 d . . .
O4W O 0.8463(9) 0.3999(4) 0.3737(4) 0.096(2) Uani 1 1 d . . .
O5W O 0.8744(9) 0.7118(4) 0.6049(4) 0.099(2) Uani 1 1 d . . .
O6W O 0.6753(10) 0.3071(5) 0.6614(5) 0.105(2) Uani 1 1 d . . .
O7W O 0.6670(10) 0.5650(5) 0.5132(4) 0.107(2) Uani 1 1 d . . .
O8W O 0.3309(11) 0.5998(5) 0.4849(5) 0.113(3) Uani 1 1 d . . .
O9W O 0.3825(9) 0.5736(6) 0.7323(4) 0.104(2) Uani 1 1 d . . .
Ni1 Ni 0.76233(8) 0.01216(4) 0.50596(4) 0.0250(2) Uani 1 1 d . . .
S1 S 0.87038(17) -0.09179(9) 0.46502(8) 0.0284(3) Uani 1 1 d . . .
S2 S 0.77560(18) -0.07697(9) 0.60841(7) 0.0287(3) Uani 1 1 d . . .
N1 N 0.7597(5) 0.0856(3) 0.4126(2) 0.0270(10) Uani 1 1 d . . .
N2 N 0.6639(5) 0.0984(3) 0.5488(3) 0.0298(11) Uani 1 1 d . . .
N3 N 0.8674(9) -0.3000(4) 0.3811(4) 0.0600(17) Uani 1 1 d . . .
N4 N 1.0239(6) -0.2088(3) 0.7917(3) 0.0346(12) Uani 1 1 d . . .
O1 O 0.9500(8) -0.3693(3) 0.4292(3) 0.0652(15) Uani 1 1 d . . .
H1 H 0.9345 -0.4127 0.4193 0.098 Uiso 1 1 calc R . .
O2 O 1.0395(5) -0.2920(3) 0.7908(2) 0.0393(10) Uani 1 1 d . . .
H2 H 1.0963 -0.3202 0.8238 0.059 Uiso 1 1 calc R . .
C1 C 0.5482(7) 0.1597(4) 0.5036(3) 0.0325(13) Uani 1 1 d . . .
H1A H 0.4797 0.1929 0.5333 0.039 Uiso 1 1 calc R . .
H1B H 0.4741 0.1309 0.4848 0.039 Uiso 1 1 calc R . .
C2 C 0.6392(8) 0.2163(4) 0.4412(3) 0.0346(14) Uani 1 1 d . . .
H2A H 0.6764 0.2602 0.4581 0.042 Uiso 1 1 calc R . .
H2B H 0.5629 0.2426 0.4038 0.042 Uiso 1 1 calc R . .
C3 C 0.7875(7) 0.1701(3) 0.4087(3) 0.0298(13) Uani 1 1 d . . .
H3A H 0.8113 0.1997 0.3579 0.036 Uiso 1 1 calc R . .
H3B H 0.8847 0.1690 0.4345 0.036 Uiso 1 1 calc R . .
C4 C 0.7366(7) 0.0696(4) 0.3540(3) 0.0283(12) Uani 1 1 d . . .
H4 H 0.7295 0.1154 0.3134 0.034 Uiso 1 1 calc R . .
C5 C 0.7201(6) -0.0086(3) 0.3413(3) 0.0260(12) Uani 1 1 d . . .
C6 C 0.6495(7) -0.0066(4) 0.2787(3) 0.0289(13) Uani 1 1 d . . .
H6 H 0.6051 0.0447 0.2502 0.035 Uiso 1 1 calc R . .
C7 C 0.6422(7) -0.0774(4) 0.2570(3) 0.0310(13) Uani 1 1 d . . .
C8 C 0.7136(7) -0.1502(4) 0.2976(3) 0.0335(14) Uani 1 1 d . . .
H8 H 0.7136 -0.1988 0.2823 0.040 Uiso 1 1 calc R . .
C9 C 0.7864(7) -0.1559(4) 0.3605(3) 0.0319(13) Uani 1 1 d . . .
C10 C 0.7869(7) -0.0842(4) 0.3847(3) 0.0279(12) Uani 1 1 d . . .
C11 C 0.5624(8) -0.0732(4) 0.1901(3) 0.0364(14) Uani 1 1 d . . .
H11A H 0.6437 -0.0625 0.1486 0.055 Uiso 1 1 calc R . .
H11B H 0.4715 -0.0289 0.1837 0.055 Uiso 1 1 calc R . .
H11C H 0.5201 -0.1256 0.1946 0.055 Uiso 1 1 calc R . .
C12 C 0.8650(9) -0.2355(4) 0.4013(4) 0.0433(16) Uani 1 1 d . . .
H12 H 0.9145 -0.2381 0.4437 0.052 Uiso 1 1 calc R . .
C13 C 0.6855(7) 0.1102(4) 0.6093(3) 0.0295(13) Uani 1 1 d . . .
H13 H 0.6336 0.1602 0.6186 0.035 Uiso 1 1 calc R . .
C14 C 0.7794(7) 0.0564(4) 0.6647(3) 0.0313(13) Uani 1 1 d . . .
C15 C 0.8223(7) 0.0915(4) 0.7166(3) 0.0349(14) Uani 1 1 d . . .
H15 H 0.7957 0.1488 0.7111 0.042 Uiso 1 1 calc R . .
C16 C 0.9021(7) 0.0453(4) 0.7756(3) 0.0360(14) Uani 1 1 d . . .
C17 C 0.9355(7) -0.0386(4) 0.7834(3) 0.0344(14) Uani 1 1 d . . .
H17 H 0.9881 -0.0713 0.8242 0.041 Uiso 1 1 calc R . .
C18 C 0.8949(7) -0.0769(4) 0.7338(3) 0.0311(13) Uani 1 1 d . . .
C19 C 0.8185(7) -0.0288(4) 0.6721(3) 0.0303(13) Uani 1 1 d . . .
C20 C 0.9460(9) 0.0861(5) 0.8301(4) 0.0465(17) Uani 1 1 d . . .
H20A H 0.9964 0.1361 0.8052 0.070 Uiso 1 1 calc R . .
H20B H 1.0238 0.0483 0.8613 0.070 Uiso 1 1 calc R . .
H20C H 0.8462 0.1002 0.8591 0.070 Uiso 1 1 calc R . .
C21 C 0.9319(7) -0.1658(4) 0.7446(3) 0.0324(13) Uani 1 1 d . . .
H21 H 0.8855 -0.1919 0.7154 0.039 Uiso 1 1 calc R . .
Ni1' Ni 0.26488(8) 0.50663(4) 0.00530(4) 0.0232(2) Uani 1 1 d . . .
S1' S 0.27511(17) 0.61178(8) -0.08613(7) 0.0271(3) Uani 1 1 d . . .
S2' S 0.36531(18) 0.43945(9) -0.07349(8) 0.0289(3) Uani 1 1 d . . .
N1' N 0.1661(5) 0.5720(3) 0.0681(2) 0.0264(10) Uani 1 1 d . . .
N2' N 0.2661(5) 0.4103(3) 0.0825(2) 0.0246(10) Uani 1 1 d . . .
N3' N 0.5259(6) 0.8052(3) -0.2258(3) 0.0314(11) Uani 1 1 d . . .
N4' N 0.2614(11) 0.3223(4) -0.2289(3) 0.072(2) Uani 1 1 d . . .
O1' O 0.5453(5) 0.7896(3) -0.2942(2) 0.0372(10) Uani 1 1 d . . .
H1' H 0.6107 0.8204 -0.3214 0.056 Uiso 1 1 calc R . .
O2' O 0.3342(10) 0.3584(4) -0.2975(3) 0.0832(19) Uani 1 1 d . . .
H2' H 0.3121 0.3343 -0.3271 0.125 Uiso 1 1 calc R . .
C1' C 0.2981(7) 0.4216(4) 0.1527(3) 0.0285(12) Uani 1 1 d . . .
H1'1 H 0.3945 0.4525 0.1463 0.034 Uiso 1 1 calc R . .
H1'2 H 0.3237 0.3673 0.1864 0.034 Uiso 1 1 calc R . .
C2' C 0.1488(8) 0.4682(4) 0.1842(3) 0.0338(14) Uani 1 1 d . . .
H2'1 H 0.0748 0.4284 0.2136 0.041 Uiso 1 1 calc R . .
H2'2 H 0.1857 0.4975 0.2161 0.041 Uiso 1 1 calc R . .
C3' C 0.0549(7) 0.5290(4) 0.1273(3) 0.0303(13) Uani 1 1 d . . .
H3'1 H -0.0180 0.5000 0.1080 0.036 Uiso 1 1 calc R . .
H3'2 H -0.0151 0.5698 0.1490 0.036 Uiso 1 1 calc R . .
C4' C 0.1848(7) 0.6460(3) 0.0667(3) 0.0282(13) Uani 1 1 d . . .
H4' H 0.1321 0.6654 0.1061 0.034 Uiso 1 1 calc R . .
C5' C 0.2761(7) 0.7035(3) 0.0125(3) 0.0280(12) Uani 1 1 d . . .
C6' C 0.3148(7) 0.7719(4) 0.0316(3) 0.0317(13) Uani 1 1 d . . .
H6' H 0.2877 0.7758 0.0795 0.038 Uiso 1 1 calc R . .
C7' C 0.3915(7) 0.8342(3) -0.0173(3) 0.0295(13) Uani 1 1 d . . .
C8' C 0.4253(7) 0.8276(3) -0.0871(3) 0.0292(13) Uani 1 1 d . . .
H8' H 0.4763 0.8701 -0.1214 0.035 Uiso 1 1 calc R . .
C9' C 0.3883(7) 0.7618(3) -0.1096(3) 0.0267(12) Uani 1 1 d . . .
C10' C 0.3144(6) 0.6968(3) -0.0587(3) 0.0251(12) Uani 1 1 d . . .
C11' C 0.4339(8) 0.9073(4) 0.0044(4) 0.0382(15) Uani 1 1 d . . .
H11D H 0.3358 0.9470 0.0047 0.057 Uiso 1 1 calc R . .
H11E H 0.5203 0.9331 -0.0299 0.057 Uiso 1 1 calc R . .
H11F H 0.4730 0.8890 0.0524 0.057 Uiso 1 1 calc R . .
C12' C 0.4267(7) 0.7584(3) -0.1839(3) 0.0284(12) Uani 1 1 d . . .
H12' H 0.3777 0.7211 -0.2014 0.034 Uiso 1 1 calc R . .
C13' C 0.2464(7) 0.3367(3) 0.0820(3) 0.0262(12) Uani 1 1 d . . .
H13' H 0.2435 0.2975 0.1272 0.031 Uiso 1 1 calc R . .
C14' C 0.2280(7) 0.3064(3) 0.0205(3) 0.0266(12) Uani 1 1 d . . .
C15' C 0.1636(7) 0.2311(3) 0.0362(3) 0.0277(12) Uani 1 1 d . . .
H15' H 0.1289 0.2058 0.0846 0.033 Uiso 1 1 calc R . .
C16' C 0.1486(7) 0.1922(4) -0.0169(3) 0.0324(13) Uani 1 1 d . . .
C17' C 0.2071(8) 0.2295(4) -0.0857(3) 0.0356(14) Uani 1 1 d . . .
H17' H 0.2007 0.2034 -0.1227 0.043 Uiso 1 1 calc R . .
C18' C 0.2754(8) 0.3041(4) -0.1036(3) 0.0353(14) Uani 1 1 d . . .
C19' C 0.2849(7) 0.3448(3) -0.0502(3) 0.0284(13) Uani 1 1 d . . .
C20' C 0.0797(8) 0.1117(4) 0.0008(4) 0.0412(15) Uani 1 1 d . . .
H20D H -0.0387 0.1213 -0.0044 0.062 Uiso 1 1 calc R . .
H20E H 0.0990 0.0817 0.0503 0.062 Uiso 1 1 calc R . .
H20F H 0.1338 0.0793 -0.0319 0.062 Uiso 1 1 calc R . .
C21' C 0.3304(10) 0.3401(4) -0.1785(4) 0.0478(17) Uani 1 1 d . . .
H21' H 0.4144 0.3757 -0.1904 0.057 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Ni1 N1 1.906(5) . ?
Ni1 N2 1.916(5) . ?
Ni1 S2 2.1584(16) . ?
Ni1 S1 2.1698(16) . ?
S1 C10 1.747(6) . ?
S2 C19 1.750(6) . ?
N1 C4 1.281(7) . ?
N1 C3 1.469(7) . ?
N2 C13 1.281(7) . ?
N2 C1 1.484(7) . ?
N3 C12 1.258(9) . ?
N3 O1 1.437(8) . ?
N4 C21 1.265(8) . ?
N4 O2 1.409(7) . ?
O1 H1 0.8400 . ?
O2 H2 0.8400 . ?
C1 C2 1.521(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.526(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.444(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(8) . ?
C5 C10 1.415(8) . ?
C6 C7 1.390(8) . ?
C6 H6 0.9500 . ?
C7 C8 1.374(9) . ?
C7 C11 1.507(8) . ?
C8 C9 1.399(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.422(8) . ?
C9 C12 1.478(9) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12 0.9500 . ?
C13 C14 1.439(8) . ?
C13 H13 0.9500 . ?
C14 C15 1.404(8) . ?
C14 C19 1.412(9) . ?
C15 C16 1.384(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(9) . ?
C16 C20 1.514(8) . ?
C17 C18 1.394(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.419(8) . ?
C18 C21 1.463(9) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 0.9500 . ?
Ni1' N2' 1.901(5) . ?
Ni1' N1' 1.906(4) . ?
Ni1' S1' 2.1592(16) . ?
Ni1' S2' 2.1715(16) . ?
S1' C10' 1.752(6) . ?
S2' C19' 1.753(6) . ?
N1' C4' 1.282(7) . ?
N1' C3' 1.477(7) . ?
N2' C13' 1.287(7) . ?
N2' C1' 1.488(7) . ?
N3' C12' 1.281(7) . ?
N3' O1' 1.411(6) . ?
N4' C21' 1.310(10) . ?
N4' O2' 1.408(9) . ?
O1' H1' 0.8400 . ?
O2' H2' 0.8400 . ?
C1' C2' 1.525(8) . ?
C1' H1'1 0.9900 . ?
C1' H1'2 0.9900 . ?
C2' C3' 1.503(8) . ?
C2' H2'1 0.9900 . ?
C2' H2'2 0.9900 . ?
C3' H3'1 0.9900 . ?
C3' H3'2 0.9900 . ?
C4' C5' 1.447(8) . ?
C4' H4' 0.9500 . ?
C5' C6' 1.400(8) . ?
C5' C10' 1.414(8) . ?
C6' C7' 1.388(8) . ?
C6' H6' 0.9500 . ?
C7' C8' 1.384(8) . ?
C7' C11' 1.511(8) . ?
C8' C9' 1.387(8) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.423(8) . ?
C9' C12' 1.456(8) . ?
C11' H11D 0.9800 . ?
C11' H11E 0.9800 . ?
C11' H11F 0.9800 . ?
C12' H12' 0.9500 . ?
C13' C14' 1.454(8) . ?
C13' H13' 0.9500 . ?
C14' C15' 1.398(8) . ?
C14' C19' 1.408(8) . ?
C15' C16' 1.393(8) . ?
C15' H15' 0.9500 . ?
C16' C17' 1.378(9) . ?
C16' C20' 1.495(8) . ?
C17' C18' 1.401(9) . ?
C17' H17' 0.9500 . ?
C18' C19' 1.409(8) . ?
C18' C21' 1.463(9) . ?
C20' H20D 0.9800 . ?
C20' H20E 0.9800 . ?
C20' H20F 0.9800 . ?
C21' H21' 0.9500 . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
N1 Ni1 N2 91.1(2) . . ?
N1 Ni1 S2 176.13(15) . . ?
N2 Ni1 S2 92.76(15) . . ?
N1 Ni1 S1 93.06(15) . . ?
N2 Ni1 S1 175.81(15) . . ?
S2 Ni1 S1 83.14(6) . . ?
C10 S1 Ni1 108.5(2) . . ?
C19 S2 Ni1 109.1(2) . . ?
C4 N1 C3 117.2(5) . . ?
C4 N1 Ni1 127.7(4) . . ?
C3 N1 Ni1 115.1(4) . . ?
C13 N2 C1 117.0(5) . . ?
C13 N2 Ni1 129.3(4) . . ?
C1 N2 Ni1 113.7(4) . . ?
C12 N3 O1 111.1(6) . . ?
C21 N4 O2 110.5(5) . . ?
N3 O1 H1 109.5 . . ?
N4 O2 H2 109.5 . . ?
N2 C1 C2 111.5(5) . . ?
N2 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N2 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 C3 112.0(5) . . ?
C1 C2 H2A 109.2 . . ?
C3 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
C3 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
N1 C3 C2 112.0(5) . . ?
N1 C3 H3A 109.2 . . ?
C2 C3 H3A 109.2 . . ?
N1 C3 H3B 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
N1 C4 C5 128.9(5) . . ?
N1 C4 H4 115.6 . . ?
C5 C4 H4 115.6 . . ?
C6 C5 C10 120.1(5) . . ?
C6 C5 C4 116.9(5) . . ?
C10 C5 C4 122.7(5) . . ?
C7 C6 C5 122.1(5) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C8 C7 C6 117.6(5) . . ?
C8 C7 C11 121.7(5) . . ?
C6 C7 C11 120.7(5) . . ?
C7 C8 C9 122.8(6) . . ?
C7 C8 H8 118.6 . . ?
C9 C8 H8 118.6 . . ?
C8 C9 C10 119.7(5) . . ?
C8 C9 C12 120.6(5) . . ?
C10 C9 C12 119.7(5) . . ?
C5 C10 C9 117.6(5) . . ?
C5 C10 S1 122.6(4) . . ?
C9 C10 S1 119.8(4) . . ?
C7 C11 H11A 109.5 . . ?
C7 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C7 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C9 121.2(6) . . ?
N3 C12 H12 119.4 . . ?
C9 C12 H12 119.4 . . ?
N2 C13 C14 127.4(5) . . ?
N2 C13 H13 116.3 . . ?
C14 C13 H13 116.3 . . ?
C15 C14 C19 119.5(6) . . ?
C15 C14 C13 116.4(6) . . ?
C19 C14 C13 124.0(5) . . ?
C16 C15 C14 122.2(6) . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C17 C16 C15 117.8(6) . . ?
C17 C16 C20 122.0(6) . . ?
C15 C16 C20 120.2(6) . . ?
C16 C17 C18 122.5(6) . . ?
C16 C17 H17 118.7 . . ?
C18 C17 H17 118.7 . . ?
C17 C18 C19 119.4(6) . . ?
C17 C18 C21 120.6(5) . . ?
C19 C18 C21 120.1(5) . . ?
C14 C19 C18 118.6(5) . . ?
C14 C19 S2 122.4(4) . . ?
C18 C19 S2 119.0(5) . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N4 C21 C18 121.9(5) . . ?
N4 C21 H21 119.0 . . ?
C18 C21 H21 119.0 . . ?
N2' Ni1' N1' 90.8(2) . . ?
N2' Ni1' S1' 176.32(14) . . ?
N1' Ni1' S1' 92.74(15) . . ?
N2' Ni1' S2' 93.38(14) . . ?
N1' Ni1' S2' 175.02(15) . . ?
S1' Ni1' S2' 83.18(6) . . ?
C10' S1' Ni1' 109.60(19) . . ?
C19' S2' Ni1' 108.6(2) . . ?
C4' N1' C3' 116.7(5) . . ?
C4' N1' Ni1' 129.4(4) . . ?
C3' N1' Ni1' 113.9(3) . . ?
C13' N2' C1' 115.8(5) . . ?
C13' N2' Ni1' 129.1(4) . . ?
C1' N2' Ni1' 115.1(3) . . ?
C12' N3' O1' 110.0(5) . . ?
C21' N4' O2' 111.3(7) . . ?
N3' O1' H1' 109.5 . . ?
N4' O2' H2' 109.5 . . ?
N2' C1' C2' 110.7(4) . . ?
N2' C1' H1'1 109.5 . . ?
C2' C1' H1'1 109.5 . . ?
N2' C1' H1'2 109.5 . . ?
C2' C1' H1'2 109.5 . . ?
H1'1 C1' H1'2 108.1 . . ?
C3' C2' C1' 112.5(5) . . ?
C3' C2' H2'1 109.1 . . ?
C1' C2' H2'1 109.1 . . ?
C3' C2' H2'2 109.1 . . ?
C1' C2' H2'2 109.1 . . ?
H2'1 C2' H2'2 107.8 . . ?
N1' C3' C2' 111.7(5) . . ?
N1' C3' H3'1 109.3 . . ?
C2' C3' H3'1 109.3 . . ?
N1' C3' H3'2 109.3 . . ?
C2' C3' H3'2 109.3 . . ?
H3'1 C3' H3'2 107.9 . . ?
N1' C4' C5' 128.1(5) . . ?
N1' C4' H4' 116.0 . . ?
C5' C4' H4' 116.0 . . ?
C6' C5' C10' 119.7(5) . . ?
C6' C5' C4' 116.9(5) . . ?
C10' C5' C4' 123.2(5) . . ?
C7' C6' C5' 122.1(5) . . ?
C7' C6' H6' 118.9 . . ?
C5' C6' H6' 118.9 . . ?
C8' C7' C6' 117.4(5) . . ?
C8' C7' C11' 121.2(5) . . ?
C6' C7' C11' 121.4(5) . . ?
C7' C8' C9' 123.2(5) . . ?
C7' C8' H8' 118.4 . . ?
C9' C8' H8' 118.4 . . ?
C8' C9' C10' 119.1(5) . . ?
C8' C9' C12' 120.6(5) . . ?
C10' C9' C12' 120.2(5) . . ?
C5' C10' C9' 118.3(5) . . ?
C5' C10' S1' 122.4(4) . . ?
C9' C10' S1' 119.2(4) . . ?
C7' C11' H11D 109.5 . . ?
C7' C11' H11E 109.5 . . ?
H11D C11' H11E 109.5 . . ?
C7' C11' H11F 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
N3' C12' C9' 120.7(5) . . ?
N3' C12' H12' 119.7 . . ?
C9' C12' H12' 119.7 . . ?
N2' C13' C14' 127.8(5) . . ?
N2' C13' H13' 116.1 . . ?
C14' C13' H13' 116.1 . . ?
C15' C14' C19' 120.7(5) . . ?
C15' C14' C13' 115.7(5) . . ?
C19' C14' C13' 123.3(5) . . ?
C16' C15' C14' 121.9(5) . . ?
C16' C15' H15' 119.0 . . ?
C14' C15' H15' 119.0 . . ?
C17' C16' C15' 117.0(5) . . ?
C17' C16' C20' 121.6(5) . . ?
C15' C16' C20' 121.3(6) . . ?
C16' C17' C18' 122.9(5) . . ?
C16' C17' H17' 118.6 . . ?
C18' C17' H17' 118.6 . . ?
C17' C18' C19' 120.0(6) . . ?
C17' C18' C21' 119.1(5) . . ?
C19' C18' C21' 120.9(6) . . ?
C14' C19' C18' 117.4(5) . . ?
C14' C19' S2' 122.9(4) . . ?
C18' C19' S2' 119.7(5) . . ?
C16' C20' H20D 109.5 . . ?
C16' C20' H20E 109.5 . . ?
H20D C20' H20E 109.5 . . ?
C16' C20' H20F 109.5 . . ?
H20D C20' H20F 109.5 . . ?
H20E C20' H20F 109.5 . . ?
N4' C21' C18' 118.7(7) . . ?
N4' C21' H21' 120.7 . . ?
C18' C21' H21' 120.7 . . ?
 
_diffrn_measured_fraction_theta_max    0.991
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.991
_refine_diff_density_max    1.224
_refine_diff_density_min   -0.692
_refine_diff_density_rms    0.107
