data_1008235
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C8 H15 Cl2 N O3 Pt S'
_chemical_formula_weight          471.26
 
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'
 '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    'P 21/n'
 
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                    11.55050(10)
_cell_length_b                    8.94670(10)
_cell_length_c                    14.6047(2)
_cell_angle_alpha                 90.00
_cell_angle_beta                  112.3919(6)
_cell_angle_gamma                 90.00
_cell_volume                      1395.44(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     3321
_cell_measurement_theta_min       2.55
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             yellow
_exptl_crystal_size_max           0.08
_exptl_crystal_size_mid           0.07
_exptl_crystal_size_min           0.06
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.243
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              888
_exptl_absorpt_coefficient_mu     10.579
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4849
_exptl_absorpt_correction_T_max   0.5694
_exptl_absorpt_process_details    
;
HKL SCALEPACK (Otwinowski & Minor, 1997)
; 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       293(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   'Nonius Kappa CCD diffractometer' 
_diffrn_measurement_method        \w 
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             6055
_diffrn_reflns_av_R_equivalents   0.0243
_diffrn_reflns_av_sigmaI/netI     0.0293
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -18
_diffrn_reflns_limit_l_max        18
_diffrn_reflns_theta_min          2.98
_diffrn_reflns_theta_max          27.49
_reflns_number_total              3149
_reflns_number_gt                 3027
_reflns_threshold_expression      >2\s(I)
 
_computing_data_collection        'COLLECT (Nonius, 1998)' 
_computing_cell_refinement        
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)' 
_computing_data_reduction         
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)' 
_computing_structure_solution     'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics     'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material   
'SHELXL97 (Sheldrick, 1997) and PLATON (Spek, 2003)' 
 
_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^ > 2\s(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^)+(0.0554P)^2^+0.5633P] 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     constr
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0193(8)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          3149
_refine_ls_number_parameters      150
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0320
_refine_ls_R_factor_gt            0.0310
_refine_ls_wR_factor_ref          0.0809
_refine_ls_wR_factor_gt           0.0798
_refine_ls_goodness_of_fit_ref    1.135
_refine_ls_restrained_S_all       1.135
_refine_ls_shift/su_max           0.002
_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 -0.086651(11) 0.030233(14) 0.678842(9) 0.02892(11) Uani 1 1 d . . .
Cl1 Cl -0.07892(11) 0.27624(12) 0.72615(10) 0.0590(3) Uani 1 1 d . . .
Cl2 Cl -0.07881(9) -0.21567(10) 0.63846(7) 0.0434(2) Uani 1 1 d . . .
S S -0.29019(11) 0.04586(10) 0.59096(9) 0.0337(2) Uani 1 1 d . . .
O O -0.3560(3) -0.0899(4) 0.5405(2) 0.0508(7) Uani 1 1 d . . .
C1 C -0.3699(4) 0.1177(6) 0.6635(4) 0.0498(10) Uani 1 1 d . . .
H1A H -0.4574 0.1277 0.6233 0.075 Uiso 1 1 calc R . .
H1B H -0.3361 0.2138 0.6893 0.075 Uiso 1 1 calc R . .
H1C H -0.3596 0.0506 0.7174 0.075 Uiso 1 1 calc R . .
C2 C -0.3193(5) 0.1882(6) 0.5012(4) 0.0623(13) Uani 1 1 d . . .
H2A H -0.2806 0.1624 0.4557 0.093 Uiso 1 1 calc R . .
H2B H -0.2850 0.2808 0.5334 0.093 Uiso 1 1 calc R . .
H2C H -0.4079 0.1989 0.4659 0.093 Uiso 1 1 calc R . .
O1 O 0.1497(3) -0.0961(4) 1.0792(2) 0.0517(8) Uani 1 1 d . . .
N1 N 0.1041(4) 0.0191(4) 0.7595(3) 0.0307(7) Uani 1 1 d . . .
C11 C 0.1879(4) 0.0474(5) 0.7157(3) 0.0400(9) Uani 1 1 d . . .
C12 C 0.3142(5) 0.0406(6) 0.7704(5) 0.0602(15) Uani 1 1 d . . .
H12 H 0.3707 0.0616 0.7407 0.072 Uiso 1 1 calc R . .
C13 C 0.3569(4) 0.0030(8) 0.8681(5) 0.0644(14) Uani 1 1 d . . .
H13 H 0.4426 -0.0016 0.9050 0.077 Uiso 1 1 calc R . .
C14 C 0.2734(5) -0.0281(6) 0.9125(4) 0.0511(12) Uani 1 1 d . . .
H14 H 0.3012 -0.0554 0.9788 0.061 Uiso 1 1 calc R . .
C15 C 0.1463(4) -0.0173(5) 0.8546(3) 0.0353(8) Uani 1 1 d . . .
C16 C 0.1353(5) 0.0844(7) 0.6069(3) 0.0587(12) Uani 1 1 d . . .
H16A H 0.0942 -0.0020 0.5698 0.088 Uiso 1 1 calc R . .
H16B H 0.2020 0.1143 0.5870 0.088 Uiso 1 1 calc R . .
H16C H 0.0760 0.1646 0.5947 0.088 Uiso 1 1 calc R . .
O17 O 0.0579(3) -0.0442(4) 0.8905(2) 0.0452(8) Uani 1 1 d . . .
H17 H 0.0909 -0.0670 0.9491 0.068 Uiso 1 1 calc R . .
 
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 0.02546(14) 0.03413(14) 0.02297(14) 0.00081(4) 0.00451(9) 0.00142(4)
Cl1 0.0513(6) 0.0411(5) 0.0749(8) -0.0171(5) 0.0131(5) -0.0016(4)
Cl2 0.0412(5) 0.0372(4) 0.0448(5) -0.0024(4) 0.0086(4) 0.0049(4)
S 0.0267(5) 0.0380(4) 0.0282(5) 0.0023(3) 0.0012(4) 0.0040(3)
O 0.0355(15) 0.0493(17) 0.0501(17) -0.0073(14) -0.0035(13) 0.0000(13)
C1 0.036(2) 0.059(2) 0.053(3) -0.001(2) 0.0159(19) 0.0079(19)
C2 0.062(3) 0.070(3) 0.044(2) 0.024(2) 0.008(2) 0.019(3)
O1 0.0552(18) 0.065(2) 0.0370(15) 0.0138(14) 0.0196(14) 0.0187(16)
N1 0.0238(17) 0.0399(18) 0.0242(17) -0.0012(12) 0.0045(14) -0.0010(12)
C11 0.031(2) 0.055(2) 0.034(2) -0.0025(16) 0.0125(17) -0.0053(16)
C12 0.032(2) 0.092(4) 0.056(3) -0.004(2) 0.016(2) -0.010(2)
C13 0.023(2) 0.113(4) 0.045(3) 0.006(3) 0.000(2) -0.004(3)
C14 0.037(2) 0.077(4) 0.028(2) 0.0053(18) 0.0000(19) -0.0007(19)
C15 0.029(2) 0.048(2) 0.0247(18) 0.0011(14) 0.0062(16) 0.0043(14)
C16 0.049(3) 0.090(4) 0.040(2) 0.009(3) 0.020(2) -0.006(3)
O17 0.0330(16) 0.070(2) 0.0304(15) 0.0101(13) 0.0097(13) 0.0044(13)
 
_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
Pt N1 2.067(4) . ?
Pt S 2.2125(12) . ?
Pt Cl2 2.2884(9) . ?
Pt Cl1 2.2984(10) . ?
S O 1.473(3) . ?
S C2 1.765(5) . ?
S C1 1.769(4) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
N1 C15 1.326(6) . ?
N1 C11 1.372(5) . ?
C11 C12 1.372(7) . ?
C11 C16 1.505(6) . ?
C12 C13 1.363(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.380(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.390(6) . ?
C14 H14 0.9300 . ?
C15 O17 1.334(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O17 H17 0.8200 . ?
 
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 Pt S 178.90(10) . . ?
N1 Pt Cl2 87.83(10) . . ?
S Pt Cl2 92.80(3) . . ?
N1 Pt Cl1 87.94(10) . . ?
S Pt Cl1 91.43(4) . . ?
Cl2 Pt Cl1 175.77(4) . . ?
O S C2 107.9(3) . . ?
O S C1 108.2(2) . . ?
C2 S C1 100.8(3) . . ?
O S Pt 118.03(13) . . ?
C2 S Pt 109.62(19) . . ?
C1 S Pt 110.86(16) . . ?
S C1 H1A 109.5 . . ?
S C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
S C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
S C2 H2A 109.5 . . ?
S C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
S C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C15 N1 C11 119.4(4) . . ?
C15 N1 Pt 119.7(3) . . ?
C11 N1 Pt 120.9(3) . . ?
C12 C11 N1 120.2(4) . . ?
C12 C11 C16 122.5(4) . . ?
N1 C11 C16 117.4(4) . . ?
C13 C12 C11 120.1(5) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 120.1(4) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 117.8(5) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
N1 C15 O17 115.1(4) . . ?
N1 C15 C14 122.3(4) . . ?
O17 C15 C14 122.5(4) . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 O17 H17 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.985
_diffrn_reflns_theta_full              27.49
_diffrn_measured_fraction_theta_full   0.985
_refine_diff_density_max    1.520
_refine_diff_density_min   -1.988
_refine_diff_density_rms    0.225