Oxidation of Half-Lantern Pt2(II,II) Compounds by Halocarbons. Evidence of Dioxygen Insertion into a Pt(III)-CH3 Bond.
Sicilia, V.; Baya, M.; Borja, P.; Martín, A; Inorganic chemistry 54 (2015) 7316–7324; doi:10.1021/acs.inorgchem.5b00846

data_4346194
_publ_section_title
;
 Oxidation of Half-Lantern Pt2(II,II) Compounds by Halocarbons. Evidence
 of Dioxygen Insertion into a Pt(III)-CH3 Bond.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7316
_journal_page_last               7324
_journal_paper_doi               10.1021/acs.inorgchem.5b00846
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C36 H26 Cl4 I2 N6 Pt2 S2'
_chemical_formula_weight         1392.53
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.140(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6909(3)
_cell_length_b                   13.1625(2)
_cell_length_c                   19.3423(4)
_cell_measurement_reflns_used    17005
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8498
_cell_measurement_theta_min      4.2064
_cell_volume                     3817.37(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details
;
  1 omega   49.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  179.0000 -120.0000 26

  2 omega  -39.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  -57.0000 -120.0000 71

  3 omega  -29.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  -19.0000  -60.0000 110

  4 omega   72.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490 -179.0000   90.0000 31

  5 omega  -25.00   25.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -99.0000 -120.0000 50

  6 omega   -2.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   57.0000  150.0000 95

  7 omega   32.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490 -179.0000 -120.0000 72

  8 omega  -10.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   37.0000  -60.0000 52

  9 omega  -11.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   77.0000    0.0000 106

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0067216000
_diffrn_orient_matrix_UB_12      -0.0477783000
_diffrn_orient_matrix_UB_13      -0.0177417000
_diffrn_orient_matrix_UB_21      -0.0467769000
_diffrn_orient_matrix_UB_22      0.0057538000
_diffrn_orient_matrix_UB_23      -0.0074214000
_diffrn_orient_matrix_UB_31      -0.0020672000
_diffrn_orient_matrix_UB_32      0.0242237000
_diffrn_orient_matrix_UB_33      -0.0332206000
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42607
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         4.22
_exptl_absorpt_coefficient_mu    9.366
_exptl_absorpt_correction_T_max  0.2121
_exptl_absorpt_correction_T_min  0.0937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9211
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0295P)^2^+9.3764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                8445
_reflns_number_total             9211
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00846_si_002.cif
_cod_data_source_block           2c
_cod_original_cell_volume        3817.37(12)
_cod_database_code               4346194