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_4089086
_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         'C27 H32 F2 N P Pt'
_chemical_formula_sum            'C27 H32 F2 N P Pt'
_chemical_formula_weight         634.59
_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             2015-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.217(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9623(3)
_cell_length_b                   9.2215(3)
_cell_length_c                   27.2996(8)
_cell_measurement_reflns_used    14782
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0380
_cell_measurement_theta_min      2.9680
_cell_volume                     2468.17(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.925
_diffrn_measurement_details
;
  1 omega  -64.00   31.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1389    0.0000   60.0000 95

  2 omega  -10.00   89.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1389   57.0000 -120.0000 99

  3 omega  -14.00   20.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0764  -99.0000 -120.0000 34

  4 omega   32.00  105.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1389 -178.0000  -30.0000 73

  5 omega  -95.00  -67.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.0764  -77.0000   60.0000 28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0670812000
_diffrn_orient_matrix_UB_12      0.0119021000
_diffrn_orient_matrix_UB_13      0.0044620000
_diffrn_orient_matrix_UB_21      0.0233607000
_diffrn_orient_matrix_UB_22      -0.0094279000
_diffrn_orient_matrix_UB_23      0.0259292000
_diffrn_orient_matrix_UB_31      0.0135926000
_diffrn_orient_matrix_UB_32      0.0754107000
_diffrn_orient_matrix_UB_33      0.0025888000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            24451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.663
_diffrn_reflns_theta_min         2.344
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.716
_refine_diff_density_min         -3.421
_refine_diff_density_rms         0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         8370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0668P)^2^+2.0803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6288
_reflns_number_total             8370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00697_si_003.cif
_cod_data_source_block           ps19
_cod_original_cell_volume        2468.17(14)
_cod_database_code               4089086
_chemical_oxdiff_formula         'C20 H20 N2 F2 P Pt'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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:
 C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,
 H25B), C26(H26A,H26B)
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:
 C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C27(H27A,H27B,
 H27C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'