Trapping five-coordinate platinum(iv) intermediates.
Shaw, Paul A.; Phillips, Jessica M.; Clarkson, Guy J.; Rourke, Jonathan P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11397–11406; doi:10.1039/c6dt02088g

data_7702090
_publ_section_title
;
 Trapping five-coordinate platinum(iv) intermediates.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11397
_journal_page_last               11406
_journal_paper_doi               10.1039/c6dt02088g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C19 H15 Cl2 F2 N O Pt S, C H Cl3'
_chemical_formula_sum            'C20 H16 Cl5 F2 N O Pt S'
_chemical_formula_weight         728.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-24
_audit_creation_method
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Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
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_audit_update_record
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2016-05-24 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                78.098(4)
_cell_angle_beta                 79.630(4)
_cell_angle_gamma                75.596(4)
_cell_formula_units_Z            2
_cell_length_a                   8.1160(4)
_cell_length_b                   10.4007(5)
_cell_length_c                   14.6707(6)
_cell_measurement_reflns_used    8024
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0570
_cell_measurement_theta_min      3.8140
_cell_volume                     1162.80(10)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
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  1 omega  -10.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579   57.0000   90.0000 94

  2 omega  -15.00   10.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  -57.0000  -90.0000 25

  3 omega  -25.00    4.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579  -99.0000 -150.0000 29

  4 omega  -49.00  -22.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  -38.0000  -90.0000 27

  5 omega  -55.00   43.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2579  -57.0000  -60.0000 98

  6 omega  -10.00   19.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  -99.0000   90.0000 29

  7 omega  -82.00    2.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  -77.0000 -150.0000 84

  8 omega  -78.00  -53.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.1954  178.0000   30.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0047237000
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_diffrn_orient_matrix_UB_13      0.0429022000
_diffrn_orient_matrix_UB_21      -0.0187128000
_diffrn_orient_matrix_UB_22      0.0676726000
_diffrn_orient_matrix_UB_23      -0.0235385000
_diffrn_orient_matrix_UB_31      -0.0890147000
_diffrn_orient_matrix_UB_32      0.0006093000
_diffrn_orient_matrix_UB_33      0.0096134000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14646
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.352
_diffrn_reflns_theta_min         3.572
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.540
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         7417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0612P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                6688
_reflns_number_total             7417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02088g3.cif
_cod_data_source_block           ps6
_cod_original_cell_volume        1162.80(9)
_cod_database_code               7702090
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H20 N2 O2 F P I Pt'
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C16(H16)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'