Reversible C-C bond formation at a triply cyclometallated platinum(IV) centre
Shaw, Paul Anthony; Clarkson, Guy James; Rourke, Jonathan P.; Chem. Sci.  (2017) –; doi:10.1039/C7SC01361B

data_1546253
_publ_section_title
;
 Reversible C-C bond formation at a triply cyclometallated platinum(IV)
 centre
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01361B
_journal_year                    2017
_chemical_formula_moiety         'C38 H29 Cl F2 N P Pt'
_chemical_formula_sum            'C38 H29 Cl F2 N P Pt'
_chemical_formula_weight         799.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-27 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                100.845(2)
_cell_angle_beta                 97.595(2)
_cell_angle_gamma                117.163(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3911(3)
_cell_length_b                   11.7933(4)
_cell_length_c                   12.8630(3)
_cell_measurement_reflns_used    15973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.9160
_cell_measurement_theta_min      3.5800
_cell_volume                     1462.19(9)
_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 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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     19.00  44.00   1.00    3.50    --   54.00  84.00   9.69   25
  2  \w     33.00  60.00   1.00    3.50    --   66.00  77.00  37.51   27
  3  \w     38.00  76.00   1.00    3.50    --   70.00  79.00   0.87   38
  4  \w     43.00  69.00   1.00    3.50    --   70.00  77.00 -44.73   26
  5  \w     41.00  66.00   1.00    3.50    --   74.00  79.00 -71.39   25
  6  \w     31.00  59.00   1.00    3.50    --   62.00  79.00 -99.48   28
  7  \w     41.00  72.00   1.00    3.50    --   74.00  79.00-136.22   31
  8  \w    102.00 146.00   1.00    3.50    --   70.00  79.00-178.20   44
  9  \w    124.00 156.00   1.00   14.00    --  114.00  77.00 -90.00   32
 10  \w    124.00 177.00   1.00   14.00    --  114.00  77.00-150.00   53
 11  \w    122.00 178.00   1.00   14.00    --  114.00  77.00   0.00   56
 12  \w    133.00 178.00   1.00   14.00    --  114.00  77.00  30.00   45
 13  \w    123.00 149.00   1.00   14.00    --  114.00  61.00  90.00   26
 14  \w    121.00 170.00   1.00   14.00    --  114.00  77.00 120.00   49
 15  \w    117.00 148.00   1.00    3.50    --   74.00  78.00  43.11   31
 16  \w    122.00 177.00   1.00   14.00    --  114.00  77.00  60.00   55
 17  \w    111.00 178.00   1.00   14.00    --  114.00  77.00  90.00   67
 18  \w     90.00 141.00   1.00    3.50    --   70.00  79.00 114.05   51
 19  \w     86.00 148.00   1.00   14.00    --  114.00  61.00  30.00   62
 20  \w     88.00 115.00   1.00   14.00    --  114.00  61.00   0.00   27
 21  \w     87.00 114.00   1.00   14.00    --  114.00  61.00 -30.00   27
 22  \w     81.00 112.00   1.00   14.00    --  114.00  77.00 -90.00   31
 23  \w     85.00 120.00   1.00   14.00    --  114.00  61.00-120.00   35
 24  \w     85.00 111.00   1.00   14.00    --  114.00  61.00-150.00   26
 25  \w     85.00 113.00   1.00   14.00    --  114.00  61.00-180.00   28
 26  \w     81.00 177.00   1.00   14.00    --  114.00  77.00-120.00   96
 27  \w     85.00 130.00   1.00   14.00    --  114.00  61.00 -60.00   45
 28  \w     81.00 107.00   1.00   14.00    --  114.00  77.00-103.00   26
 29  \w     81.00 118.00   1.00   14.00    --  114.00  77.00-150.00   37
 30  \w     81.00 172.00   1.00   14.00    --  114.00  77.00-180.00   91
 31  \w     81.00 177.00   1.00   14.00    --  114.00  77.00 -30.00   96
 32  \w     86.00 113.00   1.00   14.00    --  114.00  61.00 150.00   27
 33  \w     85.00 111.00   1.00   14.00    --  114.00  61.00 120.00   26
 34  \w     86.00 115.00   1.00   14.00    --  114.00  61.00  90.00   29
 35  \w     85.00 130.00   1.00   14.00    --  114.00  61.00  60.00   45
 36  \w     82.00 177.00   1.00   14.00    --  114.00  77.00 150.00   95
 37  \w     81.00 107.00   1.00   14.00    --  114.00  77.00  30.00   26
 38  \w     81.00 114.00   1.00   14.00    --  114.00  77.00   0.00   33
 39  \w     82.00 172.00   1.00   14.00    --  114.00  77.00 -60.00   90
 40  \w     81.00 118.00   1.00   14.00    --  114.00  77.00 120.00   37
 41  \w     81.00 107.00   1.00   14.00    --  114.00  77.00  60.00   26
 42  \w     82.00 108.00   1.00   14.00    --  114.00  77.00  90.00   26
 43  \w     42.00 114.00   1.00    3.50    --   74.00  78.00  43.11   72
 44  \w     37.00  76.00   1.00    3.50    --   70.00  79.00 114.05   39
 45  \w     34.00  60.00   1.00    3.50    --   66.00  79.00  81.94   26
 46  \w     19.00  44.00   1.00    3.50    --   54.00  84.00 166.25   25
 47  \w      8.00  33.00   1.00    3.50    --   46.00  91.00 118.47   25
 48  \w      3.00  28.00   1.00    3.50    --   41.71  95.00 -26.93   25
 49  \w     19.00  45.00   1.00    3.50    --   54.00  84.00-133.42   26
 50  \w     37.00  65.00   1.00    3.50    --   70.00  79.00-178.20   28
 51  \w      6.00  31.00   1.00    3.50    --   42.00  88.00-170.83   25
 52  \w    -51.00  31.00   1.00    3.50    --  -41.71  57.00-150.00   82
 53  \w    -91.00  -6.00   1.00    3.50    --  -41.71 125.00  60.00   85
 54  \w   -109.00 -17.00   1.00    3.50    --  -41.71 -38.00 -90.00   92
 55  \w    114.00 144.00   1.00   14.00    --  114.00 -77.00-150.00   30
 56  \w     55.00 109.00   1.00   14.00    --  114.00 -95.00   0.00   54
 57  \w     55.00 116.00   1.00   14.00    --  114.00-111.00 120.00   61
 58  \w     49.00  91.00   1.00   14.00    --  114.00 -95.00  60.00   42
 59  \w     44.00 115.00   1.00   14.00    --  114.00-111.00 -60.00   71
 60  \w     53.00  91.00   1.00   14.00    --  114.00 -77.00-150.00   38
 61  \w     44.00 106.00   1.00   14.00    --  114.00 -95.00-180.00   62
 62  \w     35.00  86.00   1.00    3.50    --   41.71-125.00   0.00   51
 63  \w     37.00  88.00   1.00   14.00    --  114.00 -95.00 150.00   51
 64  \w    -99.00 -17.00   1.00    3.50    --  -41.71 -57.00-180.00   82
 65  \w   -115.00 -14.00   1.00    3.50    --  -41.71 -57.00  90.00  101
;
_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      0.0146788000
_diffrn_orient_matrix_UB_12      -0.0791844000
_diffrn_orient_matrix_UB_13      -0.1024146000
_diffrn_orient_matrix_UB_21      -0.1517066000
_diffrn_orient_matrix_UB_22      -0.1052457000
_diffrn_orient_matrix_UB_23      -0.0254108000
_diffrn_orient_matrix_UB_31      -0.0375596000
_diffrn_orient_matrix_UB_32      0.0779062000
_diffrn_orient_matrix_UB_33      -0.0687286000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27557
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.201
_diffrn_reflns_theta_min         3.613
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.686
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.364
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5617
_reflns_number_total             6188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01361b2.cif
_cod_data_source_block           ps29new
_cod_original_cell_volume        1462.18(7)
_cod_database_code               1546253
_chemical_oxdiff_formula         'C38 H30 N2 P F2 Pt'
_reflns_odcompleteness_completeness 100.00
_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
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C25(H25A,H25B), C32(H32A,H32B)
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), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              42460
_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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.908