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_4089084
_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 H33 F2 I N P Pt'
_chemical_formula_sum            'C27 H33 F2 I N P Pt'
_chemical_formula_weight         762.50
_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
_audit_creation_date             2016-02-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.9357(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1855(2)
_cell_length_b                   12.17889(16)
_cell_length_c                   13.62801(18)
_cell_measurement_reflns_used    15752
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.9150
_cell_measurement_theta_min      4.4640
_cell_volume                     2728.65(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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   -114.00 -13.00   1.00    1.25    --  -41.46 -57.00   0.00  101
  2  \w   -114.00 -13.00   1.00    1.25    --  -41.46 -57.00 120.00  101
  3  \w   -116.00 -17.00   1.00    1.25    --  -41.46 -38.00-150.00   99
  4  \w     32.00 109.00   1.00    5.00    --  114.00 -95.00  30.00   77
  5  \w     88.00 178.00   1.00    5.00    --  114.00  45.00 -30.00   90
  6  \w     38.00 142.00   1.00    5.00    --  114.00 -30.00 150.00  104
  7  \w     41.00 140.00   1.00    5.00    --  114.00 -45.00   0.00   99
  8  \w     61.00 178.00   1.00    5.00    --  114.00  15.00  60.00  117
  9  \w    -70.00  32.00   1.00    1.25    --  -41.46  57.00 150.00  102
 10  \w     18.00  97.00   1.00    1.25    --   41.46-125.00   0.00   79
 11  \w     86.00 178.00   1.00    5.00    --  114.00  30.00-180.00   92
 12  \w     81.00 178.00   1.00    5.00    --  114.00  77.00  90.00   97
 13  \w     86.00 178.00   1.00    5.00    --  114.00  30.00 -90.00   92
 14  \w     32.00 109.00   1.00    5.00    --  114.00 -95.00-180.00   77
 15  \w    -70.00  32.00   1.00    1.25    --  -41.46  57.00 -90.00  102
 16  \w      9.00 118.00   1.00    1.25    --   41.46  77.00 -60.00  109
 17  \w     32.00 109.00   1.00    5.00    --  114.00 -95.00 -60.00   77
 18  \w     81.00 131.00   1.00    5.00    --  114.00  77.00 120.00   50
;
_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      -0.0418608000
_diffrn_orient_matrix_UB_12      -0.0419185000
_diffrn_orient_matrix_UB_13      -0.1094078000
_diffrn_orient_matrix_UB_21      0.0794988000
_diffrn_orient_matrix_UB_22      -0.0572573000
_diffrn_orient_matrix_UB_23      -0.0018057000
_diffrn_orient_matrix_UB_31      -0.0267172000
_diffrn_orient_matrix_UB_32      -0.1046604000
_diffrn_orient_matrix_UB_33      0.0447509000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26064
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.198
_diffrn_reflns_theta_min         4.518
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.291
_exptl_absorpt_correction_T_max  0.185
_exptl_absorpt_correction_T_min  0.024
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.856
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.303
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.858
_refine_diff_density_min         -2.054
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0646P)^2^+2.6691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5517
_reflns_number_total             5784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00697_si_003.cif
_cod_data_source_block           ps25
_cod_original_cell_volume        2728.64(6)
_cod_database_code               4089084
_chemical_oxdiff_formula         'C27 H20 N2 O2 F I Pt'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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), C13(H13), 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'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.508
_oxdiff_exptl_absorpt_empirical_full_min 0.656