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_4089083
_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         'C29.87 H38.6 F2 I1.13 N P Pt'
_chemical_formula_sum            'C29.87 H38.6 F2 I1.13 N P Pt'
_chemical_formula_weight         819.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.312(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2244(3)
_cell_length_b                   17.8517(5)
_cell_length_c                   16.3216(4)
_cell_measurement_reflns_used    14992
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.1610
_cell_measurement_theta_min      3.9540
_cell_volume                     2970.63(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'XS (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 0.914
_diffrn_measurement_details
;
  1 omega  -17.00   58.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3516   38.0000  -60.0000 75

  2 omega  -24.00   19.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3516  -99.0000  -60.0000 43

  3 omega  -25.00    3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3516  -99.0000 -180.0000 28

  4 omega  -35.00   58.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3516   38.0000 -180.0000 93

  5 omega   35.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       15.4141  178.0000  -30.0000 63

  6 omega  -90.00    6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3516  -57.0000   30.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0448480000
_diffrn_orient_matrix_UB_12      -0.0001434000
_diffrn_orient_matrix_UB_13      0.0310986000
_diffrn_orient_matrix_UB_21      0.0011041000
_diffrn_orient_matrix_UB_22      0.0397184000
_diffrn_orient_matrix_UB_23      0.0007458000
_diffrn_orient_matrix_UB_31      -0.0532244000
_diffrn_orient_matrix_UB_32      0.0009025000
_diffrn_orient_matrix_UB_33      -0.0304966000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34214
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.606
_diffrn_reflns_theta_min         3.509
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.987
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.701
_refine_diff_density_min         -1.496
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         9116
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0342
_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^)+(0.0353P)^2^+6.5987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7731
_reflns_number_total             9116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00697_si_003.cif
_cod_data_source_block           ps4
_cod_original_cell_volume        2970.62(13)
_cod_original_formula_sum        'C29.87 H38.60 F2 I1.13 N P Pt'
_cod_database_code               4089083
_shelxl_version_number           2014-2
_chemical_oxdiff_formula         'C20 H20 N2 O2 F P I Pt'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_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. Others
 Sof(I2)=1-FVAR(1)
 Sof(C100)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
3.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)
3.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)
3.c Idealised Me refined as rotating group:
 C100(H10A,H10B,H10C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              7575
_shelx_hkl_checksum              90054
_olex2_submission_special_instructions 'No special instructions were received'