#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:41:20 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179257 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/77/4317771.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4317771
loop_
_publ_author_name
'Paul V. Bernhardt'
'Carlos Gallego'
'Manuel Martinez'
'Teodor Parella'
_publ_section_title
;
 Substitution Reactions on Cyclometalated Pt(IV) Complexes. Associative
 Tuning by Fluoro Ligands and Fluorinated Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1747
_journal_page_last               1754
_journal_paper_doi               10.1021/ic0108179
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H28 Cl5 N Pt S'
_chemical_formula_weight         806.93
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.436(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8180(10)
_cell_length_b                   12.2240(7)
_cell_length_c                   12.162(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      10
_cell_volume                     1507.1(3)
_computing_cell_refinement       'SET4 in CAD4'
_computing_data_collection       CAD4
_computing_data_reduction        XCAD4
_computing_molecular_graphics    PLATON
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'ENRAF NONIUS CAD4'
_diffrn_measurement_method       'omega-2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2950
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        'less than 5%'
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.189
_exptl_absorpt_correction_T_max  0.3051
_exptl_absorpt_correction_T_min  0.1812
_exptl_absorpt_process_details   psi-scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         2796
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0300P)²+0.5090P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0471
_reflns_number_gt                2657
_reflns_number_total             2796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0108179.cif
_cod_data_source_block           1683mm4
_cod_database_code               4317771
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
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
C1 C 1.0484(7) 0.7452(6) 0.5296(6) 0.058(2) Uani 1 1 d . . .
H1A H 1.1390 0.7677 0.5543 0.087 Uiso 1 1 calc R . .
H1B H 0.9982 0.7849 0.4603 0.087 Uiso 1 1 calc R . .
H1C H 1.0423 0.6683 0.5129 0.087 Uiso 1 1 calc R . .
C2 C 0.9076(7) 0.9236(5) 0.5782(6) 0.0537(16) Uani 1 1 d . . .
H2A H 0.9796 0.9744 0.5964 0.081 Uiso 1 1 calc R . .
H2B H 0.8400 0.9529 0.6040 0.081 Uiso 1 1 calc R . .
H2C H 0.8723 0.9117 0.4950 0.081 Uiso 1 1 calc R . .
C3 C 0.7848(5) 0.7233(4) 0.5872(4) 0.0318(11) Uani 1 1 d . . .
C4 C 0.7208(6) 0.6620(5) 0.4860(5) 0.0410(13) Uani 1 1 d . . .
C5 C 0.5864(6) 0.6366(5) 0.4509(5) 0.0465(15) Uani 1 1 d . . .
C6 C 0.5112(6) 0.6705(5) 0.5161(6) 0.0456(14) Uani 1 1 d . . .
C7 C 0.5715(6) 0.7299(5) 0.6173(5) 0.0407(13) Uani 1 1 d . . .
C8 C 0.7042(5) 0.7571(4) 0.6521(5) 0.0359(16) Uani 1 1 d . . .
C9 C 0.7697(5) 0.8142(4) 0.7600(5) 0.0379(13) Uani 1 1 d . . .
H9 H 0.7219 0.8415 0.8044 0.045 Uiso 1 1 calc R . .
C10 C 0.9623(6) 0.8821(5) 0.9070(5) 0.0440(14) Uani 1 1 d . . .
H10A H 0.9027 0.9339 0.9230 0.053 Uiso 1 1 calc R . .
H10B H 1.0371 0.9226 0.9017 0.053 Uiso 1 1 calc R . .
C11 C 1.0093(6) 0.8019(4) 1.0059(5) 0.0412(16) Uani 1 1 d . . .
C12 C 0.9244(8) 0.7610(8) 1.0587(6) 0.065(3) Uani 1 1 d . . .
H12 H 0.8366 0.7829 1.0325 0.078 Uiso 1 1 calc R . .
C13 C 0.9706(11) 0.6879(10) 1.1501(7) 0.091(4) Uani 1 1 d . . .
H13 H 0.9134 0.6605 1.1854 0.109 Uiso 1 1 calc R . .
C14 C 1.0964(14) 0.6560(8) 1.1885(8) 0.096(4) Uani 1 1 d . . .
H14 H 1.1252 0.6068 1.2506 0.116 Uiso 1 1 calc R . .
C15 C 1.1851(11) 0.6939(9) 1.1389(8) 0.091(3) Uani 1 1 d . . .
H15 H 1.2725 0.6706 1.1671 0.109 Uiso 1 1 calc R . .
C16 C 1.1416(8) 0.7674(12) 1.0461(6) 0.068(2) Uani 1 1 d . . .
H16 H 1.1996 0.7936 1.0110 0.081 Uiso 1 1 calc R . .
C17 C 1.2118(7) 0.5717(7) 0.7469(7) 0.0604(19) Uani 1 1 d . . .
H17A H 1.1890 0.5441 0.6675 0.073 Uiso 1 1 calc R . .
H17B H 1.2656 0.6366 0.7539 0.073 Uiso 1 1 calc R . .
C18 C 1.2910(6) 0.4856(6) 0.8326(6) 0.0528(17) Uani 1 1 d . . .
C19 C 1.3641(8) 0.5092(8) 0.9468(7) 0.067(2) Uani 1 1 d . . .
H19 H 1.3600 0.5789 0.9759 0.080 Uiso 1 1 calc R . .
C20 C 1.4436(9) 0.4313(9) 1.0195(7) 0.080(3) Uani 1 1 d . . .
H20 H 1.4933 0.4488 1.0968 0.096 Uiso 1 1 calc R . .
C21 C 1.4492(9) 0.3294(8) 0.9782(8) 0.078(3) Uani 1 1 d . . .
H21 H 1.5048 0.2773 1.0266 0.094 Uiso 1 1 calc R . .
C22 C 1.3752(8) 0.3031(6) 0.8682(8) 0.072(2) Uani 1 1 d . . .
H22 H 1.3775 0.2320 0.8419 0.087 Uiso 1 1 calc R . .
C23 C 1.2957(7) 0.3790(7) 0.7932(7) 0.064(2) Uani 1 1 d . . .
H23 H 1.2454 0.3595 0.7167 0.077 Uiso 1 1 calc R . .
C24 C 0.9631(7) 0.4893(6) 0.7160(7) 0.0549(16) Uani 1 1 d . . .
H24A H 0.9401 0.4870 0.6315 0.066 Uiso 1 1 calc R . .
H24B H 1.0130 0.4238 0.7486 0.066 Uiso 1 1 calc R . .
C25 C 0.8386(6) 0.4908(5) 0.7450(6) 0.0506(16) Uani 1 1 d . . .
C26 C 0.7269(9) 0.4390(8) 0.6616(8) 0.077(2) Uani 1 1 d . . .
H26 H 0.7317 0.4101 0.5925 0.093 Uiso 1 1 calc R . .
C27 C 0.6095(9) 0.4327(9) 0.6861(12) 0.095(3) Uani 1 1 d . . .
H27 H 0.5353 0.3971 0.6358 0.114 Uiso 1 1 calc R . .
C28 C 0.6093(10) 0.4821(10) 0.7887(13) 0.103(4) Uani 1 1 d . . .
H28 H 0.5312 0.4807 0.8045 0.124 Uiso 1 1 calc R . .
C29 C 0.7131(11) 0.5314(9) 0.8662(12) 0.099(4) Uani 1 1 d . . .
H29 H 0.7076 0.5633 0.9337 0.119 Uiso 1 1 calc R . .
C30 C 0.8283(9) 0.5333(7) 0.8432(8) 0.068(2) Uani 1 1 d . . .
H30 H 0.9024 0.5654 0.8978 0.082 Uiso 1 1 calc R . .
N1 N 0.8933(5) 0.8267(4) 0.7936(4) 0.0363(10) Uani 1 1 d . . .
S1 S 1.06384(15) 0.60766(13) 0.77327(15) 0.0467(4) Uani 1 1 d . . .
Cl1 Cl 1.18469(16) 0.85744(16) 0.76900(16) 0.0576(4) Uani 1 1 d . . .
Cl2 Cl 0.80489(18) 0.60368(18) 0.40345(16) 0.0671(5) Uani 1 1 d . . .
Cl3 Cl 0.5125(2) 0.5592(2) 0.32776(19) 0.0830(7) Uani 1 1 d . . .
Cl4 Cl 0.34825(18) 0.6345(2) 0.4764(2) 0.0844(7) Uani 1 1 d . . .
Cl5 Cl 0.47687(16) 0.7693(3) 0.69933(17) 0.0634(6) Uani 1 1 d . . .
Pt1 Pt 0.973857(16) 0.77743(2) 0.662403(14) 0.03426(7) Uani 1 1 d . . .
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'
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'
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
C4 C3 C8 115.6(5) . . ?
C4 C3 Pt1 132.7(4) . . ?
C8 C3 Pt1 111.7(4) . . ?
C5 C4 C3 121.9(5) . . ?
C5 C4 Cl2 115.7(5) . . ?
C3 C4 Cl2 122.2(5) . . ?
C6 C5 C4 121.0(6) . . ?
C6 C5 Cl3 118.5(5) . . ?
C4 C5 Cl3 120.4(5) . . ?
C7 C6 C5 118.6(6) . . ?
C7 C6 Cl4 120.3(5) . . ?
C5 C6 Cl4 121.0(5) . . ?
C6 C7 C8 120.9(6) . . ?
C6 C7 Cl5 118.0(5) . . ?
C8 C7 Cl5 121.0(5) . . ?
C7 C8 C3 122.0(5) . . ?
C7 C8 C9 121.5(5) . . ?
C3 C8 C9 116.4(5) . . ?
N1 C9 C8 118.9(5) . . ?
N1 C10 C11 111.6(5) . . ?
C12 C11 C16 119.3(7) . . ?
C12 C11 C10 121.0(6) . . ?
C16 C11 C10 119.7(7) . . ?
C13 C12 C11 119.8(9) . . ?
C14 C13 C12 120.7(9) . . ?
C13 C14 C15 121.9(9) . . ?
C14 C15 C16 118.8(9) . . ?
C15 C16 C11 119.4(9) . . ?
C18 C17 S1 111.9(5) . . ?
C19 C18 C23 117.9(7) . . ?
C19 C18 C17 122.6(8) . . ?
C23 C18 C17 119.5(7) . . ?
C18 C19 C20 121.1(8) . . ?
C21 C20 C19 119.8(8) . . ?
C22 C21 C20 120.2(8) . . ?
C21 C22 C23 121.4(8) . . ?
C22 C23 C18 119.5(7) . . ?
C25 C24 S1 111.7(5) . . ?
C30 C25 C26 119.5(7) . . ?
C30 C25 C24 124.9(7) . . ?
C26 C25 C24 115.6(7) . . ?
C27 C26 C25 118.5(9) . . ?
C28 C27 C26 116.9(9) . . ?
C29 C28 C27 124.7(9) . . ?
C28 C29 C30 117.8(11) . . ?
C25 C30 C29 122.6(10) . . ?
C9 N1 C10 119.2(5) . . ?
C9 N1 Pt1 112.5(4) . . ?
C10 N1 Pt1 127.9(4) . . ?
C17 S1 C24 101.1(4) . . ?
C17 S1 Pt1 108.3(2) . . ?
C24 S1 Pt1 113.1(2) . . ?
C3 Pt1 C2 86.5(2) . . ?
C3 Pt1 C1 101.0(3) . . ?
C2 Pt1 C1 86.6(3) . . ?
C3 Pt1 N1 79.69(19) . . ?
C2 Pt1 N1 88.0(2) . . ?
C1 Pt1 N1 174.5(2) . . ?
C3 Pt1 Cl1 171.60(15) . . ?
C2 Pt1 Cl1 90.9(2) . . ?
C1 Pt1 Cl1 86.8(2) . . ?
N1 Pt1 Cl1 92.27(13) . . ?
C3 Pt1 S1 96.54(15) . . ?
C2 Pt1 S1 176.5(2) . . ?
C1 Pt1 S1 94.5(2) . . ?
N1 Pt1 S1 90.85(13) . . ?
Cl1 Pt1 S1 85.92(6) . . ?
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
C1 Pt1 2.079(6) . ?
C2 Pt1 2.060(6) . ?
C3 C4 1.401(8) . ?
C3 C8 1.425(7) . ?
C3 Pt1 2.037(5) . ?
C4 C5 1.400(9) . ?
C4 Cl2 1.726(6) . ?
C5 C6 1.383(9) . ?
C5 Cl3 1.715(6) . ?
C6 C7 1.382(9) . ?
C6 Cl4 1.714(6) . ?
C7 C8 1.388(8) . ?
C7 Cl5 1.728(6) . ?
C8 C9 1.436(8) . ?
C9 N1 1.264(7) . ?
C10 N1 1.483(7) . ?
C10 C11 1.496(8) . ?
C11 C12 1.384(10) . ?
C11 C16 1.406(10) . ?
C12 C13 1.377(13) . ?
C13 C14 1.333(15) . ?
C14 C15 1.380(14) . ?
C15 C16 1.390(14) . ?
C17 C18 1.517(10) . ?
C17 S1 1.794(7) . ?
C18 C19 1.368(10) . ?
C18 C23 1.395(12) . ?
C19 C20 1.377(12) . ?
C20 C21 1.353(14) . ?
C21 C22 1.337(12) . ?
C22 C23 1.372(11) . ?
C24 C25 1.506(9) . ?
C24 S1 1.799(7) . ?
C25 C30 1.342(11) . ?
C25 C26 1.427(11) . ?
C26 C27 1.405(13) . ?
C27 C28 1.387(16) . ?
C28 C29 1.332(16) . ?
C29 C30 1.369(11) . ?
N1 Pt1 2.154(5) . ?
S1 Pt1 2.4811(16) . ?
Cl1 Pt1 2.4030(16) . ?
