# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1284

data_mar299 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             '[PtCl(PMe3)(C15H32O3P3)].2.5(CH2Cl2)' 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C20.50 H46 Cl6 O3 P4 Pt' 
_chemical_formula_weight          872.24 
  
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 'Pt'  'Pt'  -1.7033   8.3905 
 '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            orthorhombic 
_symmetry_space_group_name_H-M    Cmca 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'x, -y, -z' 
 'x, -y+1/2, z+1/2' 
 'x, y+1/2, -z+1/2' 
 'x+1/2, y+1/2, z' 
 'x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1, z+1/2' 
 'x+1/2, y+1, -z+1/2' 
 '-x, -y, -z' 
 '-x, y, z' 
 '-x, y-1/2, -z-1/2' 
 '-x, -y-1/2, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 '-x+1/2, y+1/2, z' 
 '-x+1/2, y, -z-1/2' 
 '-x+1/2, -y, z-1/2' 
  
_cell_length_a                    14.508(9) 
_cell_length_b                    15.924(9) 
_cell_length_c                    29.018(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      6704(6) 
_cell_formula_units_Z             8 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       7 
_cell_measurement_theta_max       10 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.20 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.728 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3464 
_exptl_absorpt_coefficient_mu     4.877 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.37 
_exptl_absorpt_correction_T_max   1.00 
_exptl_absorpt_process_details    ? 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       173(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_type   ? 
_diffrn_measurement_method        \w--2\q 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          2 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   120 
_diffrn_standards_decay_%         0 
_diffrn_reflns_number             2428 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0561 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        0 
_diffrn_reflns_limit_k_max        17 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        31 
_diffrn_reflns_theta_min          2.02 
_diffrn_reflns_theta_max          22.94 
_reflns_number_total              2428 
_reflns_number_gt                 1951 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'Enraf-Nonius CAD4' 
_computing_cell_refinement        'Enraf-Nonius CAD4' 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'CAMERON (Watkin and Pearce,1993)' 
_computing_publication_material   SHELXL-93 
  
_refine_special_details 
; 
 H2A was refined ; other H atoms were in riding mode. 
  
 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^)+(0.1200P)^2^+238.8816P] 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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          2428 
_refine_ls_number_parameters      188 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0921 
_refine_ls_R_factor_gt            0.0746 
_refine_ls_wR_factor_ref          0.2088 
_refine_ls_wR_factor_gt           0.1957 
_refine_ls_goodness_of_fit_ref    1.120 
_refine_ls_restrained_S_all       1.120 
_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 
Pt Pt 0.0000 0.05688(5) 0.66683(3) 0.0168(4) Uani 1 2 d S . . 
Cl1 Cl 0.0000 -0.0460(3) 0.72803(19) 0.0280(13) Uani 1 2 d S . . 
Cl2 Cl 0.2500 0.3138(4) 0.7500 0.061(2) Uani 1 2 d S . . 
Cl3 Cl 0.1996(9) 0.4350(7) 0.6773(4) 0.056(3) Uani 0.50 1 d P . . 
Cl4 Cl 0.5000 0.0355(6) 0.6188(3) 0.071(2) Uani 1 2 d S . . 
Cl5 Cl 0.6577(8) -0.0658(7) 0.6496(5) 0.056(3) Uani 0.50 1 d P . . 
Cl6 Cl 0.5000 0.0898(10) 0.4890(6) 0.156(6) Uani 1 2 d S . . 
P1 P 0.0000 0.1536(3) 0.6116(2) 0.0219(13) Uani 1 2 d S . . 
P2 P 0.1030(3) 0.0066(2) 0.58085(14) 0.0255(9) Uani 1 1 d . . . 
H2 H 0.1534 -0.0036 0.6037 0.031 Uiso 1 1 calc R . . 
P3 P 0.0000 0.1478(4) 0.7272(2) 0.0269(14) Uani 1 2 d S . . 
O1 O 0.0000 0.2454(9) 0.6192(5) 0.026(3) Uani 1 2 d S . . 
O2 O 0.1335(9) -0.0359(7) 0.5362(4) 0.044(3) Uani 1 1 d . . . 
H2A H 0.115(18) 0.0000 0.5000 0.05(7) Uiso 1 2 d S . . 
C1 C 0.0954(10) 0.1199(9) 0.5739(5) 0.024(4) Uani 1 1 d . . . 
H1 H 0.0763 0.1312 0.5414 0.029 Uiso 1 1 calc R . . 
C2 C 0.0000 -0.0311(12) 0.6067(8) 0.020(5) Uani 1 2 d S . . 
C3 C 0.1923(11) 0.1656(11) 0.5820(6) 0.033(4) Uani 1 1 d . . . 
C4 C 0.2169(11) 0.1720(12) 0.6337(6) 0.039(4) Uani 1 1 d . . . 
H4A H 0.1672 0.2009 0.6501 0.059 Uiso 1 1 calc R . . 
H4B H 0.2744 0.2037 0.6372 0.059 Uiso 1 1 calc R . . 
H4C H 0.2249 0.1155 0.6464 0.059 Uiso 1 1 calc R . . 
C5 C 0.1818(14) 0.2554(12) 0.5609(7) 0.049(5) Uani 1 1 d . . . 
H5A H 0.1319 0.2853 0.5767 0.073 Uiso 1 1 calc R . . 
H5B H 0.1673 0.2508 0.5280 0.073 Uiso 1 1 calc R . . 
H5C H 0.2396 0.2865 0.5648 0.073 Uiso 1 1 calc R . . 
C6 C 0.2704(11) 0.1196(13) 0.5562(6) 0.043(5) Uani 1 1 d . . . 
H6A H 0.2773 0.0628 0.5688 0.064 Uiso 1 1 calc R . . 
H6B H 0.3282 0.1506 0.5601 0.064 Uiso 1 1 calc R . . 
H6C H 0.2551 0.1161 0.5233 0.064 Uiso 1 1 calc R . . 
C7 C 0.0000 -0.1306(14) 0.6115(9) 0.035(6) Uani 1 2 d S . . 
C8 C -0.0861(12) -0.1589(10) 0.6398(6) 0.036(4) Uani 1 1 d . . . 
H8A H -0.1423 -0.1427 0.6234 0.055 Uiso 1 1 calc R . . 
H8B H -0.0851 -0.1317 0.6701 0.055 Uiso 1 1 calc R . . 
H8C H -0.0849 -0.2200 0.6438 0.055 Uiso 1 1 calc R . . 
C9 C 0.0000 -0.1786(15) 0.5655(9) 0.065(11) Uani 1 2 d S . . 
H9A H 0.0541 -0.1622 0.5474 0.098 Uiso 0.50 1 calc PR . . 
H9B H -0.0561 -0.1649 0.5482 0.098 Uiso 0.50 1 calc PR . . 
H9C H 0.0020 -0.2391 0.5715 0.098 Uiso 1 2 calc SR . . 
C10 C 0.0000 0.2590(14) 0.7204(8) 0.038(6) Uani 1 2 d S . . 
H10A H -0.0518 0.2756 0.7007 0.057 Uiso 0.50 1 calc PR . . 
H10B H 0.0580 0.2767 0.7060 0.057 Uiso 0.50 1 calc PR . . 
H10C H -0.0062 0.2858 0.7506 0.057 Uiso 0.50 1 calc PR . . 
C11 C 0.0997(14) 0.1333(10) 0.7644(6) 0.044(5) Uani 1 1 d . . . 
H11A H 0.1077 0.0734 0.7709 0.066 Uiso 1 1 calc R . . 
H11B H 0.0903 0.1638 0.7933 0.066 Uiso 1 1 calc R . . 
H11C H 0.1549 0.1548 0.7489 0.066 Uiso 1 1 calc R . . 
C12 C 0.241(4) 0.421(2) 0.7309(15) 0.067(17) Uani 0.50 1 d P . . 
H12A H 0.2013 0.4521 0.7527 0.081 Uiso 0.50 1 calc PR . . 
H12B H 0.3034 0.4469 0.7324 0.081 Uiso 0.50 1 calc PR . . 
C13 C 0.535(2) -0.0578(19) 0.6457(13) 0.039(9) Uiso 0.50 1 d P . . 
H13A H 0.5106 -0.1063 0.6281 0.047 Uiso 0.50 1 calc PR . . 
H13B H 0.5080 -0.0602 0.6771 0.047 Uiso 0.50 1 calc PR . . 
C14 C 0.561(5) 0.0000 0.5000 0.08(2) Uiso 0.50 2 d SP . . 
H14A H 0.6013 -0.0109 0.4732 0.095 Uiso 0.25 1 calc PR . . 
H14B H 0.6013 0.0109 0.5268 0.095 Uiso 0.25 1 calc PR . . 
  
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 
Pt 0.0060(5) 0.0225(5) 0.0220(5) -0.0006(3) 0.000 0.000 
Cl1 0.032(3) 0.028(3) 0.024(3) 0.006(2) 0.000 0.000 
Cl2 0.048(4) 0.047(4) 0.087(5) 0.000 -0.009(4) 0.000 
Cl3 0.034(6) 0.076(8) 0.057(7) 0.016(6) 0.020(6) 0.008(6) 
Cl4 0.064(6) 0.080(5) 0.069(6) 0.029(4) 0.000 0.000 
Cl5 0.032(6) 0.062(7) 0.074(8) -0.001(6) 0.010(6) -0.004(5) 
Cl6 0.195(18) 0.116(10) 0.156(14) 0.002(10) 0.000 0.000 
P1 0.017(3) 0.025(3) 0.024(3) -0.001(2) 0.000 0.000 
P2 0.015(2) 0.031(2) 0.031(2) 0.0011(18) 0.0049(17) 0.0047(18) 
P3 0.022(3) 0.028(3) 0.031(3) -0.004(3) 0.000 0.000 
O1 0.032(9) 0.024(7) 0.023(8) 0.004(6) 0.000 0.000 
O2 0.045(8) 0.039(6) 0.047(8) 0.002(6) 0.015(7) 0.012(6) 
C1 0.009(8) 0.038(9) 0.025(8) 0.004(7) -0.003(7) -0.017(7) 
C2 0.007(10) 0.015(9) 0.038(13) -0.005(9) 0.000 0.000 
C3 0.015(9) 0.048(10) 0.037(10) 0.000(8) 0.002(7) -0.016(8) 
C4 0.013(9) 0.070(12) 0.036(10) 0.007(9) 0.001(7) -0.021(8) 
C5 0.043(12) 0.056(11) 0.048(12) 0.014(9) 0.004(10) -0.017(10) 
C6 0.006(8) 0.079(13) 0.044(11) -0.002(9) 0.002(8) -0.004(8) 
C7 0.037(15) 0.028(12) 0.041(15) 0.009(11) 0.000 0.000 
C8 0.031(10) 0.041(10) 0.037(10) 0.003(8) -0.004(8) -0.017(8) 
C9 0.14(3) 0.019(12) 0.035(15) -0.003(11) 0.000 0.000 
C10 0.064(19) 0.034(13) 0.016(13) 0.001(10) 0.000 0.000 
C11 0.055(13) 0.039(9) 0.038(11) 0.007(8) -0.023(10) -0.006(9) 
C12 0.03(3) 0.05(2) 0.13(5) 0.01(2) 0.03(4) -0.01(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 
Pt P1 2.224(6) . ? 
Pt C2 2.24(2) . ? 
Pt P3 2.273(6) . ? 
Pt Cl1 2.416(5) . ? 
Cl2 C12 1.80(4) 15_557 ? 
Cl2 C12 1.80(4) . ? 
Cl3 Cl5 1.008(15) 5_455 ? 
Cl3 C12 1.68(5) . ? 
Cl4 C13 1.75(3) 10_655 ? 
Cl4 C13 1.75(3) . ? 
Cl5 Cl3 1.008(15) 5_545 ? 
Cl5 C13 1.79(4) . ? 
Cl6 C14 1.71(4) 10_655 ? 
Cl6 C14 1.71(4) . ? 
P1 O1 1.479(15) . ? 
P1 C1 1.843(16) 10 ? 
P1 C1 1.843(16) . ? 
P2 O2 1.528(12) . ? 
P2 C2 1.777(12) . ? 
P2 C1 1.818(15) . ? 
P3 C10 1.78(2) . ? 
P3 C11 1.819(18) 10 ? 
P3 C11 1.819(18) . ? 
C1 C3 1.601(19) . ? 
C2 C7 1.59(3) . ? 
C2 P2 1.777(12) 10 ? 
C3 C6 1.54(2) . ? 
C3 C4 1.54(2) . ? 
C3 C5 1.56(2) . ? 
C7 C9 1.54(3) . ? 
C7 C8 1.56(2) . ? 
C7 C8 1.56(2) 10 ? 
C14 Cl6 1.71(4) 9_656 ? 
  
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 Pt C2 82.6(6) . . ? 
P1 Pt P3 96.6(2) . . ? 
C2 Pt P3 179.2(6) . . ? 
P1 Pt Cl1 178.84(19) . . ? 
C2 Pt Cl1 98.6(6) . . ? 
P3 Pt Cl1 82.3(2) . . ? 
C12 Cl2 C12 37(3) 15_557 . ? 
Cl5 Cl3 C12 162(2) 5_455 . ? 
C13 Cl4 C13 33(2) 10_655 . ? 
Cl3 Cl5 C13 130.5(17) 5_545 . ? 
C14 Cl6 C14 62(4) 10_655 . ? 
O1 P1 C1 112.1(6) . 10 ? 
O1 P1 C1 112.1(6) . . ? 
C1 P1 C1 97.3(9) 10 . ? 
O1 P1 Pt 125.2(6) . . ? 
C1 P1 Pt 103.1(5) 10 . ? 
C1 P1 Pt 103.1(5) . . ? 
O2 P2 C2 116.8(9) . . ? 
O2 P2 C1 111.3(7) . . ? 
C2 P2 C1 109.3(8) . . ? 
C10 P3 C11 101.1(7) . 10 ? 
C10 P3 C11 101.1(7) . . ? 
C11 P3 C11 105.3(13) 10 . ? 
C10 P3 Pt 123.2(8) . . ? 
C11 P3 Pt 112.1(6) 10 . ? 
C11 P3 Pt 112.1(6) . . ? 
C3 C1 P2 112.4(11) . . ? 
C3 C1 P1 116.1(10) . . ? 
P2 C1 P1 105.6(7) . . ? 
C7 C2 P2 112.0(8) . 10 ? 
C7 C2 P2 112.0(8) . . ? 
P2 C2 P2 114.6(12) 10 . ? 
C7 C2 Pt 123.7(16) . . ? 
P2 C2 Pt 96.7(7) 10 . ? 
P2 C2 Pt 96.7(7) . . ? 
C6 C3 C4 109.4(14) . . ? 
C6 C3 C5 108.4(14) . . ? 
C4 C3 C5 110.0(14) . . ? 
C6 C3 C1 110.9(13) . . ? 
C4 C3 C1 112.1(12) . . ? 
C5 C3 C1 105.9(13) . . ? 
C9 C7 C8 108.3(13) . . ? 
C9 C7 C8 108.3(13) . 10 ? 
C8 C7 C8 106.2(19) . 10 ? 
C9 C7 C2 114.7(19) . . ? 
C8 C7 C2 109.5(13) . . ? 
C8 C7 C2 109.5(13) 10 . ? 
Cl3 C12 Cl2 116(2) . . ? 
Cl4 C13 Cl5 112.0(18) . . ? 
Cl6 C14 Cl6 118(4) 9_656 . ? 
  
_diffrn_measured_fraction_theta_max    0.999 
_diffrn_reflns_theta_full              22.94 
_diffrn_measured_fraction_theta_full   0.999 
_refine_diff_density_max    3.651 
_refine_diff_density_min   -5.303 
_refine_diff_density_rms    0.334 

#===END