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_4089085
_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         'C30 H39 F2 I N P Pt'
_chemical_formula_sum            'C30 H39 F2 I N P Pt'
_chemical_formula_weight         804.58
_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             2016-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.0913(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9485(2)
_cell_length_b                   12.31107(18)
_cell_length_c                   13.88543(18)
_cell_measurement_reflns_used    21334
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.3730
_cell_measurement_theta_min      3.5350
_cell_volume                     2881.49(7)
_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 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_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      0.00  99.00   1.00    5.00    --   24.24  37.00  60.00   99
  2  \w      0.00  99.00   1.00    5.00    --   24.24  37.00  30.00   99
  3  \w     -3.00  97.00   1.00    5.00    --   24.24  50.00 106.00  100
  4  \w     -4.00  97.00   1.00    5.00    --   24.24  57.00 -90.00  101
  5  \w    -50.00  49.00   1.00    5.00    --   24.24 -37.00  90.00   99
  6  \w    -48.00  35.00   1.00    5.00    --   24.24 -50.00 -40.00   83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0303144000
_diffrn_orient_matrix_UB_12      -0.0295300000
_diffrn_orient_matrix_UB_13      0.0373739000
_diffrn_orient_matrix_UB_21      0.0140537000
_diffrn_orient_matrix_UB_22      -0.0193659000
_diffrn_orient_matrix_UB_23      -0.0387448000
_diffrn_orient_matrix_UB_31      0.0255820000
_diffrn_orient_matrix_UB_32      0.0455288000
_diffrn_orient_matrix_UB_33      0.0077297000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56183
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         34.607
_diffrn_reflns_theta_min         3.227
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43783
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         11614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+3.1313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9200
_reflns_number_total             11614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00697_si_003.cif
_cod_data_source_block           ps35
_cod_original_cell_volume        2881.48(7)
_cod_database_code               4089085
_chemical_oxdiff_formula         'C20 H20 N2 F2 Cl P Pt'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.50
_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), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C4(H4), C8(H8), C9(H9), C10(H10), C14(H14), C16(H16), C17(H17)
2.c Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              47528
_shelx_hkl_checksum              33800
_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 1.899
_oxdiff_exptl_absorpt_empirical_full_min 0.518