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_1546256
_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, C H Cl3'
_chemical_formula_sum            'C39 H30 Cl4 F2 N P Pt'
_chemical_formula_weight         918.50
_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             2016-07-18
_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                107.6381(9)
_cell_angle_beta                 97.2289(9)
_cell_angle_gamma                105.2604(8)
_cell_formula_units_Z            2
_cell_length_a                   10.06885(9)
_cell_length_b                   10.97968(11)
_cell_length_c                   17.46056(18)
_cell_measurement_reflns_used    47973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4450
_cell_measurement_theta_min      4.4360
_cell_volume                     1729.77(3)
_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 0.965
_diffrn_measured_fraction_theta_max 0.951
_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 -14.00   1.00    1.00    --  -41.82 -57.00   0.00  100
  2  \w   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00  30.00   99
  3  \w   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00 120.00   99
  4  \w     12.00 115.00   1.00    1.00    --   41.82  65.00 -96.98  103
  5  \w     12.00 114.00   1.00    1.00    --   41.82  64.00-145.15  102
  6  \w    -31.00  71.00   1.00    1.00    --   41.82 -63.00 147.52  102
  7  \w     12.00 115.00   1.00    1.00    --   41.82  65.00  16.68  103
  8  \w     12.00 114.00   1.00    1.00    --   41.82  64.00 144.82  102
  9  \w    -31.00  71.00   1.00    1.00    --   41.82 -64.00 -88.67  102
 10  \w    -31.00  71.00   1.00    1.00    --   41.82 -63.00  -6.57  102
 11  \w     12.00 115.00   1.00    1.00    --   41.82  65.00 -30.64  103
 12  \w    -31.00  71.00   1.00    1.00    --   41.82 -64.00  92.21  102
 13  \w     34.00 137.00   1.00    4.00    --  107.00 -65.00 -30.44  103
 14  \w     78.00 178.00   1.00    4.00    --  107.00  61.00   0.00  100
 15  \w     34.00 137.00   1.00    4.00    --  107.00 -65.00  12.97  103
 16  \w     78.00 178.00   1.00    4.00    --  107.00  61.00 -90.00  100
 17  \w     81.00 178.00   1.00    4.00    --  107.00  45.00-120.00   97
 18  \w     81.00 178.00   1.00    4.00    --  107.00  45.00-180.00   97
 19  \w     78.00 178.00   1.00    4.00    --  107.00  61.00  90.00  100
 20  \w     81.00 178.00   1.00    4.00    --  107.00  45.00  90.00   97
 21  \w     81.00 178.00   1.00    4.00    --  107.00  45.00 -30.00   97
 22  \w     78.00 178.00   1.00    4.00    --  107.00  61.00-180.00  100
 23  \w     81.00 178.00   1.00    4.00    --  107.00  45.00 -90.00   97
 24  \w     81.00 178.00   1.00    4.00    --  107.00  45.00   0.00   97
 25  \w     34.00 137.00   1.00    4.00    --  107.00 -65.00 128.93  103
 26  \w     78.00 178.00   1.00    4.00    --  107.00  61.00 -30.00  100
 27  \w     34.00 137.00   1.00    4.00    --  107.00 -65.00-104.77  103
 28  \w     78.00 178.00   1.00    4.00    --  107.00  61.00-150.00  100
 29  \w     78.00 178.00   1.00    4.00    --  107.00  61.00 120.00  100
 30  \w     34.00 137.00   1.00    4.00    --  107.00 -65.00  66.92  103
 31  \w     78.00 178.00   1.00    4.00    --  107.00  61.00  30.00  100
 32  \w     78.00 178.00   1.00    4.00    --  107.00  61.00 150.00  100
 33  \w     78.00 178.00   1.00    4.00    --  107.00  61.00 -60.00  100
 34  \w     81.00 178.00   1.00    4.00    --  107.00  45.00  30.00   97
 35  \w     81.00 178.00   1.00    4.00    --  107.00  45.00 120.00   97
 36  \w     78.00 178.00   1.00    4.00    --  107.00  61.00  60.00  100
 37  \w     81.00 178.00   1.00    4.00    --  107.00  45.00 -60.00   97
 38  \w     34.00 137.00   1.00    4.00    --  107.00 -65.00-155.12  103
 39  \w     81.00 178.00   1.00    4.00    --  107.00  45.00-150.00   97
 40  \w     78.00 178.00   1.00    4.00    --  107.00  61.00-120.00  100
 41  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00-180.00  100
 42  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00  90.00  100
 43  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00 -30.00  100
 44  \w   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00  60.00   99
 45  \w   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00 -60.00   99
 46  \w   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00 -90.00  100
 47  \w    -46.00 130.00   1.00    1.00    --   41.82   0.00 -30.00  176
 48  \w    -46.00 130.00   1.00    1.00    --   41.82   0.00 -60.00  176
 49  \w    -46.00 130.00   1.00    1.00    --   41.82   0.00 -90.00  176
 50  \w    -46.00 130.00   1.00    1.00    --   41.82   0.00-120.00  176
 51  \w    -46.00 130.00   1.00    1.00    --   41.82   0.00-150.00  176
 52  \w    -46.00 130.00   1.00    1.00    --   41.82   0.00-180.00  176
 53  \w      1.00 122.00   1.00    1.00    --   41.82  19.00-180.00  121
 54  \w    -46.00  72.00   1.00    1.00    --   41.82   0.00   0.00  118
 55  \w     12.00 115.00   1.00    1.00    --   41.82  65.00 108.71  103
;
_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      -0.0671408000
_diffrn_orient_matrix_UB_12      0.0982283000
_diffrn_orient_matrix_UB_13      -0.0236127000
_diffrn_orient_matrix_UB_21      0.1415999000
_diffrn_orient_matrix_UB_22      0.1147100000
_diffrn_orient_matrix_UB_23      0.0389863000
_diffrn_orient_matrix_UB_31      0.0437928000
_diffrn_orient_matrix_UB_32      -0.0363486000
_diffrn_orient_matrix_UB_33      -0.0833388000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59546
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.604
_diffrn_reflns_theta_min         4.332
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.208
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34516
_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    1.763
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0198
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+2.6180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0488
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6578
_reflns_number_total             6645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01361b2.cif
_cod_data_source_block           ps38
_cod_original_cell_volume        1729.76(3)
_cod_database_code               1546256
_chemical_oxdiff_formula         'C20 H20 N2 O2 F P Pt'
_reflns_odcompleteness_completeness 96.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C39(H39)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C32(H32A,H32B)
2.c 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), C19(H19), C20(H20), C21(H21), C22(H22), C27(H27), C28(H28), C29(H29),
  C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              25726
_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 2.450
_oxdiff_exptl_absorpt_empirical_full_min 0.775