Long-Lived Five-Coordinate Platinum(IV) Intermediates: Regiospecific C‒C Coupling
Shaw, Paul A.; Clarkson, Guy J.; Rourke, Jonathan P.; Organometallics 35 (2016) 3751–; doi:10.1021/acs.organomet.6b00697

data_4089087
_publ_section_title
;
 Long-Lived Five-Coordinate Platinum(IV) Intermediates: Regiospecific C--C
 Coupling
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              3751
_journal_paper_doi               10.1021/acs.organomet.6b00697
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C28 H35 F2 I N P Pt'
_chemical_formula_sum            'C28 H35 F2 I N P Pt'
_chemical_formula_weight         776.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.9421(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.56227(7)
_cell_length_b                   17.96588(15)
_cell_length_c                   18.24470(15)
_cell_measurement_reflns_used    41910
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.1960
_cell_measurement_theta_min      2.9820
_cell_volume                     2785.98(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -7.00  92.00   1.00    3.25    --   17.29  38.00 120.00   99
  2  \w    -24.00  97.00   1.00    3.25    --   17.29  19.00  30.00  121
  3  \w     35.00 106.00   1.00    3.25    --   17.29 178.00 -30.00   71
  4  \w     -7.00  92.00   1.00    3.25    --   17.29  38.00-150.00   99
  5  \w    -15.00  93.00   1.00    3.25    --   17.29  77.00 150.00  108
  6  \w    -25.00  23.00   1.00    3.25    --  -18.22 -99.00 -60.00   48
  7  \w    -57.00  42.00   1.00    3.25    --   17.29 -38.00  30.00   99
  8  \w   -107.00 -57.00   1.00    3.25    --  -18.22-178.00  30.00   50
  9  \w   -105.00 -53.00   1.00    3.25    --  -18.22 178.00-180.00   52
 10  \w    -25.00  23.00   1.00    3.25    --  -18.22 -99.00-150.00   48
 11  \w   -107.00 -57.00   1.00    3.25    --  -18.22-178.00 -90.00   50
 12  \w    -25.00  27.00   1.00    3.25    --   17.29 -99.00-180.00   52
 13  \w    -25.00  58.00   1.00    3.25    --   17.29 -99.00   0.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0409473000
_diffrn_orient_matrix_UB_12      -0.0338068000
_diffrn_orient_matrix_UB_13      0.0085845000
_diffrn_orient_matrix_UB_21      -0.0564065000
_diffrn_orient_matrix_UB_22      -0.0101457000
_diffrn_orient_matrix_UB_23      0.0236501000
_diffrn_orient_matrix_UB_31      -0.0459243000
_diffrn_orient_matrix_UB_32      -0.0176696000
_diffrn_orient_matrix_UB_33      -0.0300140000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            85124
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.415
_diffrn_reflns_theta_min         2.396
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         9618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0151P)^2^+2.0508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0437
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8462
_reflns_number_total             9618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00697_si_003.cif
_cod_data_source_block           ps37
_cod_database_code               4089087
_chemical_oxdiff_formula         'C20 H20 N2 O2 P Cl Pt'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,
 H24B), C25(H25A,H25B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16)
2.c Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C17A(H17A,H17B,H17C), C20(H20A,H20B,H20C), C23(H23A,
 H23B,H23C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              14519
_shelx_hkl_checksum              54445
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.759