 
data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C28 H26 Cl4 Ni2 O2 P2'
_chemical_formula_sum
 'C28 H26 Cl4 Ni2 O2 P2'
_chemical_formula_weight          715.65
 
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'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Ni'  'Ni'   0.3393   1.1124
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 '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   -P1
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    7.9894(12)
_cell_length_b                    14.1019(19)
_cell_length_c                    14.478(2)
_cell_angle_alpha                 96.289(8)
_cell_angle_beta                  89.803(6)
_cell_angle_gamma                 97.961(9)
_cell_volume                      1605.7(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        unk
_exptl_crystal_colour             unk
_exptl_crystal_size_max           0.11
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.07
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.480
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              728
_exptl_absorpt_coefficient_mu     1.629
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.8412
_exptl_absorpt_correction_T_max   0.8945
_exptl_absorpt_process_details    'SORTAV (R.H. Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             6496
_diffrn_reflns_av_R_equivalents   0.0722
_diffrn_reflns_av_sigmaI/netI     0.0928
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          1.92
_diffrn_reflns_theta_max          25.09
_reflns_number_total              4270
_reflns_number_gt                 3244
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97

 
_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)+(0.1966P)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          4270
_refine_ls_number_parameters      343
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0963
_refine_ls_R_factor_gt            0.0821
_refine_ls_wR_factor_ref          0.2566
_refine_ls_wR_factor_gt           0.2449
_refine_ls_goodness_of_fit_ref    1.006
_refine_ls_restrained_S_all       1.006
_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 -0.08822(13) 0.43087(7) 0.58375(7) 0.0323(4) Uani 1 1 d . . .
Ni2 Ni 0.40693(11) 0.08175(6) 0.94393(6) 0.0245(4) Uani 1 1 d . . .
Cl1 Cl -0.0497(6) 0.4372(4) 0.7411(3) 0.1175(16) Uani 1 1 d . . .
Cl2 Cl -0.1124(5) 0.4257(3) 0.4248(2) 0.0973(12) Uani 1 1 d . . .
Cl3 Cl 0.4633(5) 0.0626(3) 1.0976(2) 0.0922(12) Uani 1 1 d . . .
Cl4 Cl 0.3704(4) 0.0983(3) 0.7907(2) 0.0771(9) Uani 1 1 d . . .
P1 P -0.2614(4) 0.2952(2) 0.5898(2) 0.0660(9) Uani 1 1 d . A .
P2 P 0.3000(4) 0.2172(2) 0.9874(2) 0.0596(8) Uani 1 1 d . . .
C1 C -0.4128(17) 0.2970(10) 0.6864(9) 0.080(4) Uani 1 1 d . . .
H1A H -0.4946 0.2390 0.6784 0.096 Uiso 1 1 calc R A .
H1B H -0.3529 0.2978 0.7447 0.096 Uiso 1 1 calc R . .
C2 C -0.502(3) 0.3829(18) 0.6897(12) 0.138(8) Uani 1 1 d . A -1
H2 H -0.4264 0.4368 0.7115 0.166 Uiso 1 1 calc R A -1
C4 C -0.3925(15) 0.2578(9) 0.4901(9) 0.070(3) Uani 1 1 d . . .
C5 C -0.5092(18) 0.3207(12) 0.4581(10) 0.092(4) Uani 1 1 d . A .
H5 H -0.5082 0.3824 0.4884 0.110 Uiso 1 1 calc R . .
C6 C -0.613(2) 0.2913(13) 0.3882(11) 0.097(5) Uani 1 1 d . . .
H6 H -0.6916 0.3302 0.3727 0.117 Uiso 1 1 calc R A .
C7 C -0.609(2) 0.1993(14) 0.3351(13) 0.113(6) Uani 1 1 d . A .
H7 H -0.6805 0.1804 0.2838 0.136 Uiso 1 1 calc R . .
C8 C -0.500(2) 0.1400(13) 0.3600(12) 0.100(5) Uani 1 1 d . . .
H8 H -0.4928 0.0816 0.3246 0.120 Uiso 1 1 calc R A .
C9 C -0.3992(17) 0.1678(10) 0.4388(10) 0.084(4) Uani 1 1 d . A .
H9 H -0.3329 0.1243 0.4583 0.101 Uiso 1 1 calc R . .
C10 C -0.1395(15) 0.1965(10) 0.6006(9) 0.075(4) Uani 1 1 d . . .
C11 C 0.0180(19) 0.2036(12) 0.5615(11) 0.100(5) Uani 1 1 d . A .
H11 H 0.0597 0.2596 0.5357 0.120 Uiso 1 1 calc R . .
C12 C 0.123(2) 0.1256(14) 0.5590(19) 0.144(9) Uani 1 1 d . . .
H12 H 0.2200 0.1250 0.5237 0.173 Uiso 1 1 calc R A .
C13 C 0.060(3) 0.0473(16) 0.6178(16) 0.132(8) Uani 1 1 d . A .
H13 H 0.1272 0.0008 0.6296 0.158 Uiso 1 1 calc R . .
C14 C -0.098(3) 0.0469(14) 0.6534(14) 0.136(8) Uani 1 1 d . . .
H14 H -0.1442 -0.0065 0.6821 0.163 Uiso 1 1 calc R A .
C15 C -0.1963(19) 0.1203(11) 0.6499(12) 0.100(5) Uani 1 1 d . A .
H15 H -0.2992 0.1181 0.6804 0.119 Uiso 1 1 calc R . .
C16 C 0.1735(16) 0.2609(10) 0.9041(10) 0.085(4) Uani 1 1 d . . .
H16A H 0.1394 0.3213 0.9309 0.102 Uiso 1 1 calc R . .
H16B H 0.2418 0.2740 0.8502 0.102 Uiso 1 1 calc R . .
C17 C 0.0144(17) 0.1905(13) 0.8721(12) 0.098(5) Uani 1 1 d . . .
H17 H 0.0235 0.1410 0.8252 0.117 Uiso 1 1 calc R . .
O2 O -0.140(3) 0.199(2) 0.9109(16) 0.303(15) Uani 1 1 d . . .
C19 C 0.1660(14) 0.2121(8) 1.0882(8) 0.061(3) Uani 1 1 d . . .
C20 C 0.1470(15) 0.2961(9) 1.1443(9) 0.075(3) Uani 1 1 d . . .
H20 H 0.2116 0.3540 1.1338 0.090 Uiso 1 1 calc R . .
C21 C 0.031(2) 0.2937(14) 1.2163(11) 0.103(5) Uani 1 1 d . . .
H21 H 0.0147 0.3506 1.2517 0.124 Uiso 1 1 calc R . .
C22 C -0.0583(18) 0.2087(17) 1.2354(13) 0.119(7) Uani 1 1 d . . .
H22 H -0.1319 0.2075 1.2853 0.143 Uiso 1 1 calc R . .
C23 C -0.039(2) 0.1203(14) 1.1779(12) 0.111(6) Uani 1 1 d . . .
H23 H -0.0982 0.0615 1.1897 0.134 Uiso 1 1 calc R . .
C24 C 0.0731(15) 0.1268(10) 1.1043(9) 0.076(3) Uani 1 1 d . . .
H24 H 0.0849 0.0715 1.0648 0.091 Uiso 1 1 calc R . .
C25 C 0.4777(15) 0.3112(9) 1.0160(9) 0.075(4) Uani 1 1 d . . .
C26 C 0.5544(17) 0.3214(10) 1.1056(10) 0.082(4) Uani 1 1 d . . .
H26 H 0.5115 0.2831 1.1509 0.099 Uiso 1 1 calc R . .
C27 C 0.7020(17) 0.3935(11) 1.1241(13) 0.094(5) Uani 1 1 d . . .
H27 H 0.7544 0.4012 1.1822 0.113 Uiso 1 1 calc R . .
C28 C 0.7626(18) 0.4475(12) 1.0611(14) 0.101(5) Uani 1 1 d . . .
H28 H 0.8552 0.4947 1.0747 0.121 Uiso 1 1 calc R . .
C29 C 0.684(2) 0.4332(12) 0.9694(14) 0.111(5) Uani 1 1 d . . .
H29 H 0.7326 0.4697 0.9240 0.133 Uiso 1 1 calc R . .
C30 C 0.5414(18) 0.3688(10) 0.9461(10) 0.085(4) Uani 1 1 d . . .
H30 H 0.4898 0.3632 0.8879 0.102 Uiso 1 1 calc R . .
O1 O -0.640(4) 0.410(3) 0.674(2) 0.41(3) Uani 1 1 d . . .
 
 
_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 P1 2.210(3) . ?
Ni1 Cl1 2.290(4) . ?
Ni1 Cl2 2.303(4) . ?
Ni1 Cl2 2.415(4) 2_566 ?
Ni2 P2 2.227(3) . ?
Ni2 Cl4 2.279(3) . ?
Ni2 Cl3 2.324(3) . ?
Ni2 Cl3 2.427(3) 2_657 ?
Cl2 Ni1 2.415(4) 2_566 ?
Cl3 Ni2 2.427(3) 2_657 ?
P1 C4 1.776(13) . ?
P1 C10 1.825(13) . ?
P1 C1 1.846(13) . ?
P2 C16 1.788(14) . ?
P2 C19 1.809(12) . ?
P2 C25 1.818(14) . ?
C1 C2 1.49(2) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 O1 1.24(3) . ?
C2 H2 0.9300 . ?
C4 C9 1.392(18) . ?
C4 C5 1.480(18) . ?
C5 C6 1.307(19) . ?
C5 H5 0.9300 . ?
C6 C7 1.44(2) . ?
C6 H6 0.9300 . ?
C7 C8 1.37(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.39(2) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.374(18) . ?
C10 C15 1.379(18) . ?
C11 C12 1.47(2) . ?
C11 H11 0.9300 . ?
C12 C13 1.50(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.37(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.39(2) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.54(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 O2 1.37(3) . ?
C17 H17 0.9300 . ?
C19 C24 1.366(17) . ?
C19 C20 1.387(16) . ?
C20 C21 1.391(18) . ?
C20 H20 0.9300 . ?
C21 C22 1.36(2) . ?
C21 H21 0.9300 . ?
C22 C23 1.45(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.390(19) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C30 1.415(18) . ?
C25 C26 1.421(18) . ?
C26 C27 1.451(19) . ?
C26 H26 0.9300 . ?
C27 C28 1.30(2) . ?
C27 H27 0.9300 . ?
C28 C29 1.45(2) . ?
C28 H28 0.9300 . ?
C29 C30 1.37(2) . ?
C29 H29 0.9300 . ?
C30 H30 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
P1 Ni1 Cl1 88.09(14) . . ?
P1 Ni1 Cl2 93.74(12) . . ?
Cl1 Ni1 Cl2 177.13(16) . . ?
P1 Ni1 Cl2 177.08(15) . 2_566 ?
Cl1 Ni1 Cl2 92.11(14) . 2_566 ?
Cl2 Ni1 Cl2 85.95(12) . 2_566 ?
P2 Ni2 Cl4 91.60(12) . . ?
P2 Ni2 Cl3 91.17(12) . . ?
Cl4 Ni2 Cl3 175.97(13) . . ?
P2 Ni2 Cl3 176.82(13) . 2_657 ?
Cl4 Ni2 Cl3 90.46(12) . 2_657 ?
Cl3 Ni2 Cl3 86.65(12) . 2_657 ?
Ni1 Cl2 Ni1 94.05(12) . 2_566 ?
Ni2 Cl3 Ni2 93.35(12) . 2_657 ?
C4 P1 C10 105.4(6) . . ?
C4 P1 C1 103.5(6) . . ?
C10 P1 C1 107.5(6) . . ?
C4 P1 Ni1 115.0(4) . . ?
C10 P1 Ni1 109.8(4) . . ?
C1 P1 Ni1 114.9(5) . . ?
C16 P2 C19 103.4(6) . . ?
C16 P2 C25 106.3(6) . . ?
C19 P2 C25 107.8(6) . . ?
C16 P2 Ni2 117.4(5) . . ?
C19 P2 Ni2 114.4(4) . . ?
C25 P2 Ni2 107.0(4) . . ?
C2 C1 P1 110.8(10) . . ?
C2 C1 H1A 109.5 . . ?
P1 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
O1 C2 C1 144(3) . . ?
O1 C2 H2 108.2 . . ?
C1 C2 H2 108.2 . . ?
C9 C4 C5 115.2(13) . . ?
C9 C4 P1 123.6(10) . . ?
C5 C4 P1 121.1(10) . . ?
C6 C5 C4 121.4(15) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 120.8(16) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 119.8(16) . . ?
C8 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C7 C8 C9 119.2(16) . . ?
C7 C8 H8 120.4 . . ?
C9 C8 H8 120.4 . . ?
C8 C9 C4 123.2(15) . . ?
C8 C9 H9 118.4 . . ?
C4 C9 H9 118.4 . . ?
C11 C10 C15 120.4(13) . . ?
C11 C10 P1 117.0(11) . . ?
C15 C10 P1 122.5(11) . . ?
C10 C11 C12 122.1(16) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 H11 118.9 . . ?
C11 C12 C13 114.8(19) . . ?
C11 C12 H12 122.6 . . ?
C13 C12 H12 122.6 . . ?
C14 C13 C12 117(2) . . ?
C14 C13 H13 121.4 . . ?
C12 C13 H13 121.4 . . ?
C13 C14 C15 125(2) . . ?
C13 C14 H14 117.6 . . ?
C15 C14 H14 117.6 . . ?
C10 C15 C14 119.3(17) . . ?
C10 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C17 C16 P2 113.7(11) . . ?
C17 C16 H16A 108.8 . . ?
P2 C16 H16A 108.8 . . ?
C17 C16 H16B 108.8 . . ?
P2 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
O2 C17 C16 121.8(17) . . ?
O2 C17 H17 119.1 . . ?
C16 C17 H17 119.1 . . ?
C24 C19 C20 120.2(11) . . ?
C24 C19 P2 119.7(9) . . ?
C20 C19 P2 119.9(9) . . ?
C19 C20 C21 119.9(13) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 120.7(16) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C21 C22 C23 119.9(15) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 117.4(14) . . ?
C24 C23 H23 121.3 . . ?
C22 C23 H23 121.3 . . ?
C19 C24 C23 121.8(14) . . ?
C19 C24 H24 119.1 . . ?
C23 C24 H24 119.1 . . ?
C30 C25 C26 121.9(13) . . ?
C30 C25 P2 118.6(10) . . ?
C26 C25 P2 119.4(11) . . ?
C25 C26 C27 117.9(15) . . ?
C25 C26 H26 121.1 . . ?
C27 C26 H26 121.1 . . ?
C28 C27 C26 121.4(16) . . ?
C28 C27 H27 119.3 . . ?
C26 C27 H27 119.3 . . ?
C27 C28 C29 119.2(15) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 123.5(15) . . ?
C30 C29 H29 118.2 . . ?
C28 C29 H29 118.2 . . ?
C29 C30 C25 116.0(15) . . ?
C29 C30 H30 122.0 . . ?
C25 C30 H30 122.0 . . ?
 
_diffrn_measured_fraction_theta_max    0.745
_diffrn_reflns_theta_full              25.09
_diffrn_measured_fraction_theta_full   0.745
_refine_diff_density_max    1.909
_refine_diff_density_min   -0.995
_refine_diff_density_rms    0.174
