data_s92
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C33 H30 Cl N O3 P2 Pt'
_chemical_formula_sum
 'C33 H30 Cl N O3 P2 Pt'
_chemical_formula_weight          781.06
 
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'
 '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'
 'Pt'  'Pt'  -1.7033   8.3905
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
_symmetry_space_group_name_hall   '-P 2ybc'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    10.647(2)
_cell_length_b                    17.517(4)
_cell_length_c                    16.715(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  105.06(3)
_cell_angle_gamma                 90.00
_cell_volume                      3010.3(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     34591
_cell_measurement_theta_min       3.01
_cell_measurement_theta_max       27.47
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.723
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1536
_exptl_absorpt_coefficient_mu     4.892
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.2450
_exptl_absorpt_correction_T_max   0.8875
_exptl_absorpt_process_details    'SORTAV (R.H>Blessing, 1995, 1997)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'Phi and Omega scans to fill Ewald Sphere'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             34591
_diffrn_reflns_av_R_equivalents   0.0603
_diffrn_reflns_av_sigmaI/netI     0.0409
_diffrn_reflns_limit_h_min        -13
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -22
_diffrn_reflns_limit_k_max        22
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        21
_diffrn_reflns_theta_min          3.01
_diffrn_reflns_theta_max          27.47
_reflns_number_total              6881
_reflns_number_gt                 6130
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'CAMERON (Watkin, Pearce 1995)'
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00081(19)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          6881
_refine_ls_number_parameters      373
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0423
_refine_ls_R_factor_gt            0.0363
_refine_ls_wR_factor_ref          0.1076
_refine_ls_wR_factor_gt           0.1003
_refine_ls_goodness_of_fit_ref    0.871
_refine_ls_restrained_S_all       0.871
_refine_ls_shift/su_max           0.004
_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
Pt1 Pt 0.733884(14) 0.153556(7) 0.242347(8) 0.01660(9) Uani 1 1 d . . .
Cl1 Cl 0.51102(9) 0.13518(6) 0.23296(6) 0.0253(2) Uani 1 1 d . . .
P1 P 0.93673(10) 0.17026(6) 0.23885(6) 0.0187(2) Uani 1 1 d . . .
P2 P 0.72781(9) 0.24881(5) 0.33470(5) 0.0193(2) Uani 1 1 d . . .
O1 O 0.8432(3) -0.08133(16) -0.07793(16) 0.0277(6) Uani 1 1 d . . .
O2 O 0.7235(3) -0.15966(14) -0.0220(2) 0.0284(7) Uani 1 1 d . . .
O3 O 0.8723(3) 0.27973(16) 0.37541(16) 0.0265(6) Uani 1 1 d . . .
N1 N 0.9495(3) 0.11939(18) 0.15734(19) 0.0228(7) Uani 1 1 d . . .
H1 H 1.0151 0.1244 0.1367 0.027 Uiso 1 1 calc R . .
C1 C 0.7361(4) 0.0717(2) 0.1541(2) 0.0188(7) Uani 1 1 d . . .
C2 C 0.6388(3) 0.0195(2) 0.1211(2) 0.0203(7) Uani 1 1 d . . .
H2 H 0.5626 0.0212 0.1385 0.024 Uiso 1 1 calc R . .
C3 C 0.6499(3) -0.0358(2) 0.0627(2) 0.0223(7) Uani 1 1 d . . .
H3 H 0.5843 -0.0716 0.0443 0.027 Uiso 1 1 calc R . .
C4 C 0.7594(3) -0.0365(2) 0.0327(2) 0.0201(7) Uani 1 1 d . . .
C5 C 0.7792(3) -0.0928(2) -0.0288(2) 0.0208(8) Uani 1 1 d . . .
C6 C 0.7442(4) -0.2200(2) -0.0767(3) 0.0313(9) Uani 1 1 d . . .
H6A H 0.7129 -0.2036 -0.1333 0.047 Uiso 1 1 calc R . .
H6B H 0.6980 -0.2649 -0.0680 0.047 Uiso 1 1 calc R . .
H6C H 0.8354 -0.2312 -0.0652 0.047 Uiso 1 1 calc R . .
C7 C 0.8593(3) 0.0156(2) 0.0633(2) 0.0198(7) Uani 1 1 d . . .
H7 H 0.9330 0.0155 0.0433 0.024 Uiso 1 1 calc R . .
C8 C 0.8485(3) 0.0679(2) 0.1238(2) 0.0186(7) Uani 1 1 d . . .
C9 C 0.9844(3) 0.2665(2) 0.2184(2) 0.0202(7) Uani 1 1 d . . .
C10 C 0.9233(4) 0.2992(2) 0.1418(2) 0.0268(8) Uani 1 1 d . . .
H10 H 0.8654 0.2705 0.1018 0.032 Uiso 1 1 calc R . .
C11 C 0.9492(4) 0.3745(3) 0.1259(3) 0.0343(10) Uani 1 1 d . . .
H11 H 0.9074 0.3967 0.0755 0.041 Uiso 1 1 calc R . .
C12 C 1.0380(4) 0.4167(2) 0.1854(3) 0.0337(9) Uani 1 1 d . . .
H12 H 1.0565 0.4669 0.1742 0.040 Uiso 1 1 calc R . .
C13 C 1.0982(4) 0.3845(3) 0.2605(3) 0.0298(9) Uani 1 1 d . . .
H13 H 1.1570 0.4132 0.2999 0.036 Uiso 1 1 calc R . .
C14 C 1.0722(4) 0.3099(2) 0.2781(2) 0.0251(8) Uani 1 1 d . . .
H14 H 1.1128 0.2887 0.3293 0.030 Uiso 1 1 calc R . .
C15 C 1.0653(4) 0.1395(2) 0.3272(2) 0.0218(8) Uani 1 1 d . . .
C16 C 1.0372(4) 0.1146(2) 0.3997(2) 0.0294(9) Uani 1 1 d . . .
H16 H 0.9516 0.1141 0.4036 0.035 Uiso 1 1 calc R . .
C17 C 1.1372(4) 0.0904(3) 0.4664(2) 0.0356(10) Uani 1 1 d . . .
H17 H 1.1181 0.0730 0.5145 0.043 Uiso 1 1 calc R . .
C18 C 1.2646(4) 0.0921(3) 0.4613(3) 0.0366(10) Uani 1 1 d . . .
H18 H 1.3313 0.0765 0.5062 0.044 Uiso 1 1 calc R . .
C19 C 1.2927(4) 0.1171(3) 0.3896(3) 0.0342(10) Uani 1 1 d . . .
H19 H 1.3784 0.1183 0.3861 0.041 Uiso 1 1 calc R . .
C20 C 1.1937(4) 0.1405(3) 0.3228(3) 0.0295(9) Uani 1 1 d . . .
H20 H 1.2133 0.1570 0.2746 0.035 Uiso 1 1 calc R . .
C21 C 0.8995(5) 0.3403(2) 0.4355(3) 0.0335(11) Uani 1 1 d . . .
H21A H 0.8286 0.3760 0.4238 0.050 Uiso 1 1 calc R . .
H21B H 0.9780 0.3660 0.4329 0.050 Uiso 1 1 calc R . .
H21C H 0.9100 0.3194 0.4900 0.050 Uiso 1 1 calc R . .
C22 C 0.6606(3) 0.2266(2) 0.4212(2) 0.0222(7) Uani 1 1 d . . .
C23 C 0.6147(4) 0.2833(2) 0.4645(2) 0.0249(8) Uani 1 1 d . . .
H23 H 0.6127 0.3339 0.4471 0.030 Uiso 1 1 calc R . .
C24 C 0.5717(4) 0.2647(3) 0.5337(2) 0.0292(9) Uani 1 1 d . . .
H24 H 0.5405 0.3027 0.5624 0.035 Uiso 1 1 calc R . .
C25 C 0.5751(4) 0.1903(3) 0.5598(2) 0.0283(9) Uani 1 1 d . . .
H25 H 0.5471 0.1783 0.6065 0.034 Uiso 1 1 calc R . .
C26 C 0.6204(4) 0.1322(3) 0.5169(2) 0.0268(8) Uani 1 1 d . . .
H26 H 0.6218 0.0817 0.5343 0.032 Uiso 1 1 calc R . .
C27 C 0.6634(4) 0.1515(2) 0.4477(2) 0.0217(8) Uani 1 1 d . . .
H27 H 0.6943 0.1135 0.4189 0.026 Uiso 1 1 calc R . .
C28 C 0.6368(4) 0.3311(2) 0.2858(2) 0.0254(8) Uani 1 1 d . . .
C29 C 0.5021(5) 0.3327(3) 0.2691(3) 0.0310(10) Uani 1 1 d . . .
H29 H 0.4582 0.2933 0.2875 0.037 Uiso 1 1 calc R . .
C30 C 0.4327(5) 0.3934(3) 0.2247(3) 0.0410(12) Uani 1 1 d . . .
H30 H 0.3423 0.3938 0.2121 0.049 Uiso 1 1 calc R . .
C31 C 0.4983(6) 0.4526(3) 0.1996(3) 0.0495(14) Uani 1 1 d . . .
H31 H 0.4520 0.4936 0.1710 0.059 Uiso 1 1 calc R . .
C32 C 0.6298(6) 0.4517(3) 0.2161(3) 0.0502(14) Uani 1 1 d . . .
H32 H 0.6731 0.4920 0.1987 0.060 Uiso 1 1 calc R . .
C33 C 0.7006(5) 0.3909(3) 0.2588(3) 0.0373(10) Uani 1 1 d . . .
H33 H 0.7908 0.3903 0.2693 0.045 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pt1 C1 2.062(3) . ?
Pt1 P1 2.1951(11) . ?
Pt1 P2 2.2855(10) . ?
Pt1 Cl1 2.3590(11) . ?
P1 N1 1.663(3) . ?
P1 C15 1.816(4) . ?
P1 C9 1.818(4) . ?
P2 O3 1.606(3) . ?
P2 C28 1.809(4) . ?
P2 C22 1.814(3) . ?
O1 C5 1.211(5) . ?
O2 C5 1.331(5) . ?
O2 C6 1.452(4) . ?
O3 C21 1.439(5) . ?
N1 C8 1.404(4) . ?
C1 C2 1.385(5) . ?
C1 C8 1.417(5) . ?
C2 C3 1.402(5) . ?
C3 C4 1.384(5) . ?
C4 C7 1.394(5) . ?
C4 C5 1.479(5) . ?
C7 C8 1.390(5) . ?
C9 C10 1.399(5) . ?
C9 C14 1.402(5) . ?
C10 C11 1.388(6) . ?
C11 C12 1.393(6) . ?
C12 C13 1.373(6) . ?
C13 C14 1.384(6) . ?
C15 C20 1.388(6) . ?
C15 C16 1.392(5) . ?
C16 C17 1.392(6) . ?
C17 C18 1.381(6) . ?
C18 C19 1.381(6) . ?
C19 C20 1.382(6) . ?
C22 C27 1.387(5) . ?
C22 C23 1.390(5) . ?
C23 C24 1.389(5) . ?
C24 C25 1.371(6) . ?
C25 C26 1.401(6) . ?
C26 C27 1.391(5) . ?
C28 C33 1.386(6) . ?
C28 C29 1.388(7) . ?
C29 C30 1.393(7) . ?
C30 C31 1.376(7) . ?
C31 C32 1.356(8) . ?
C32 C33 1.391(7) . ?
 
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
C1 Pt1 P1 83.08(11) . . ?
C1 Pt1 P2 176.98(10) . . ?
P1 Pt1 P2 96.97(4) . . ?
C1 Pt1 Cl1 93.20(11) . . ?
P1 Pt1 Cl1 174.84(3) . . ?
P2 Pt1 Cl1 86.57(4) . . ?
N1 P1 C15 107.62(18) . . ?
N1 P1 C9 104.84(16) . . ?
C15 P1 C9 103.87(18) . . ?
N1 P1 Pt1 103.94(12) . . ?
C15 P1 Pt1 118.55(13) . . ?
C9 P1 Pt1 116.96(12) . . ?
O3 P2 C28 105.35(18) . . ?
O3 P2 C22 105.51(15) . . ?
C28 P2 C22 104.74(17) . . ?
O3 P2 Pt1 109.90(10) . . ?
C28 P2 Pt1 112.48(13) . . ?
C22 P2 Pt1 117.91(13) . . ?
C5 O2 C6 116.2(3) . . ?
C21 O3 P2 122.8(3) . . ?
C8 N1 P1 117.0(2) . . ?
C2 C1 C8 116.2(3) . . ?
C2 C1 Pt1 126.7(3) . . ?
C8 C1 Pt1 117.2(3) . . ?
C1 C2 C3 122.9(3) . . ?
C4 C3 C2 119.4(3) . . ?
C3 C4 C7 119.7(3) . . ?
C3 C4 C5 122.9(3) . . ?
C7 C4 C5 117.3(3) . . ?
O1 C5 O2 123.1(4) . . ?
O1 C5 C4 124.5(3) . . ?
O2 C5 C4 112.3(3) . . ?
C8 C7 C4 120.0(3) . . ?
C7 C8 N1 121.0(3) . . ?
C7 C8 C1 121.8(3) . . ?
N1 C8 C1 117.2(3) . . ?
C10 C9 C14 119.7(4) . . ?
C10 C9 P1 117.7(3) . . ?
C14 C9 P1 122.4(3) . . ?
C11 C10 C9 119.8(4) . . ?
C10 C11 C12 120.0(4) . . ?
C13 C12 C11 120.2(4) . . ?
C12 C13 C14 120.7(4) . . ?
C13 C14 C9 119.6(4) . . ?
C20 C15 C16 119.2(4) . . ?
C20 C15 P1 119.8(3) . . ?
C16 C15 P1 120.9(3) . . ?
C15 C16 C17 119.9(4) . . ?
C18 C17 C16 120.2(4) . . ?
C17 C18 C19 119.8(4) . . ?
C18 C19 C20 120.2(4) . . ?
C19 C20 C15 120.5(4) . . ?
C27 C22 C23 119.5(3) . . ?
C27 C22 P2 118.5(3) . . ?
C23 C22 P2 121.8(3) . . ?
C24 C23 C22 120.1(4) . . ?
C25 C24 C23 120.1(4) . . ?
C24 C25 C26 120.8(4) . . ?
C27 C26 C25 118.7(4) . . ?
C22 C27 C26 120.8(3) . . ?
C33 C28 C29 119.2(4) . . ?
C33 C28 P2 119.9(4) . . ?
C29 C28 P2 120.8(3) . . ?
C28 C29 C30 120.0(5) . . ?
C31 C30 C29 119.8(5) . . ?
C32 C31 C30 120.6(4) . . ?
C31 C32 C33 120.5(5) . . ?
C28 C33 C32 120.0(5) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.47
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    3.063
_refine_diff_density_min   -2.924
_refine_diff_density_rms    0.176
