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_1546257
_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 H31 Cl F2 N P Pt'
_chemical_formula_sum            'C38 H31 Cl F2 N P Pt'
_chemical_formula_weight         801.15
_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             2016-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 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                83.1662(13)
_cell_angle_beta                 79.6553(12)
_cell_angle_gamma                76.3618(13)
_cell_formula_units_Z            2
_cell_length_a                   8.51403(11)
_cell_length_b                   10.31938(18)
_cell_length_c                   18.7511(3)
_cell_measurement_reflns_used    34593
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.4720
_cell_measurement_theta_min      2.8460
_cell_volume                     1569.92(4)
_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 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.940
_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     -4.00  95.00   1.00    5.00    --   20.29  38.00 -60.00   99
  2  \w    -60.00  61.00   1.00    5.00    --   20.29 -19.00 120.00  121
  3  \w     35.00 109.00   1.00    5.00    --   20.29 178.00 150.00   74
  4  \w    -56.00  53.00   1.00    5.00    --   20.29 -77.00-180.00  109
  5  \w    -25.00  20.00   1.00    5.00    --  -21.38 -99.00 -90.00   45
  6  \w    -25.00  20.00   1.00    5.00    --  -21.38 -99.00  60.00   45
  7  \w   -110.00 -57.00   1.00    5.00    --  -21.38-178.00-120.00   53
  8  \w     -8.00  93.00   1.00    5.00    --   20.29  57.00  60.00  101
  9  \w    -54.00  45.00   1.00    5.00    --   20.29 -38.00   0.00   99
 10  \w    -21.00 100.00   1.00    5.00    --   20.29  19.00-180.00  121
 11  \w   -110.00 -57.00   1.00    5.00    --  -21.38-178.00 150.00   53
 12  \w    -25.00  20.00   1.00    5.00    --  -21.38 -99.00   0.00   45
 13  \w    -25.00  20.00   1.00    5.00    --  -21.38 -99.00 150.00   45
 14  \w    -99.00 -57.00   1.00    5.00    --  -21.38 160.00  30.00   42
;
_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      -0.0113083000
_diffrn_orient_matrix_UB_12      -0.0253373000
_diffrn_orient_matrix_UB_13      0.0369757000
_diffrn_orient_matrix_UB_21      0.0332584000
_diffrn_orient_matrix_UB_22      0.0511961000
_diffrn_orient_matrix_UB_23      0.0095929000
_diffrn_orient_matrix_UB_31      -0.0793780000
_diffrn_orient_matrix_UB_32      0.0420944000
_diffrn_orient_matrix_UB_33      0.0053758000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54759
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.674
_diffrn_reflns_theta_min         2.396
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61193
_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    1.695
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         11737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0173P)^2^+0.5814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10822
_reflns_number_total             11737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01361b2.cif
_cod_data_source_block           ps34
_cod_database_code               1546257
_chemical_oxdiff_formula         'C20 H20 F2 N P Pt'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.54
_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), C17(H17), C20(H20), 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_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 1.441
_oxdiff_exptl_absorpt_empirical_full_min 0.800