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_1546251
_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 Cl3 F2 N P Pt, C H Cl3'
_chemical_formula_sum            'C39 H30 Cl6 F2 N P Pt'
_chemical_formula_weight         989.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-09
_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                90
_cell_angle_beta                 91.1028(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.49295(19)
_cell_length_b                   22.2749(4)
_cell_length_c                   14.2990(2)
_cell_measurement_reflns_used    34933
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3840
_cell_measurement_theta_min      2.8370
_cell_volume                     3659.93(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.952
_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    -20.00  25.00   1.00   15.00    --  -16.15 -99.00 -90.00   45
  2  \w    -20.00  25.00   1.00   15.00    --  -16.15 -99.00  90.00   45
  3  \w    -91.00   8.00   1.00   15.00    --  -16.15 -37.00-180.00   99
  4  \w    -11.00  90.00   1.00   15.00    --   17.24  57.00 150.00  101
  5  \w    -20.00  58.00   1.00   15.00    --   17.24 -99.00   0.00   78
  6  \w     34.00 104.00   1.00   15.00    --   17.24-178.00  90.00   70
  7  \w     -7.00  92.00   1.00   15.00    --   17.24  37.00   0.00   99
  8  \w    -11.00  90.00   1.00   15.00    --   17.24  57.00  60.00  101
  9  \w   -103.00 -55.00   1.00   15.00    --  -16.15 178.00 -30.00   48
 10  \w   -103.00 -55.00   1.00   15.00    --  -16.15 178.00  60.00   48
 11  \w   -105.00 -57.00   1.00   15.00    --  -16.15-178.00 120.00   48
 12  \w    -20.00  24.00   1.00   15.00    --   17.24 -99.00-150.00   44
 13  \w      0.00  72.00   1.00   15.00    --   17.24-123.00 151.00   72
 14  \w    -20.00  58.00   1.00   15.00    --   17.24 -99.00 -90.00   78
;
_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      0.0122534000
_diffrn_orient_matrix_UB_12      0.0311197000
_diffrn_orient_matrix_UB_13      -0.0035991000
_diffrn_orient_matrix_UB_21      -0.0604321000
_diffrn_orient_matrix_UB_22      0.0061634000
_diffrn_orient_matrix_UB_23      -0.0040825000
_diffrn_orient_matrix_UB_31      -0.0029423000
_diffrn_orient_matrix_UB_32      0.0028022000
_diffrn_orient_matrix_UB_33      0.0493033000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            104681
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.865
_diffrn_reflns_theta_min         2.252
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.357
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.796
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.458
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         11956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0179P)^2^+2.7387P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10295
_reflns_number_total             11956
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01361b2.cif
_cod_data_source_block           ps39
_cod_database_code               1546251
_chemical_oxdiff_formula         'C20 H20 N2 O2 F2 P Cl6 Pt'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.98
_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:
 C25(H25A,H25B), C32(H32A,H32B), C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C28(H28), C13(H13), C22(H22), C31(H31), C5(H5), C30(H30),
 C29(H29), C27(H27), C4(H4), C10(H10), C21(H21), C34(H34), C14(H14), C16(H16),
 C35(H35), C9(H9), C20(H20), C19(H19), C38(H38), C36(H36), C37(H37)
;
_shelx_res_checksum              52244
_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 2.255
_oxdiff_exptl_absorpt_empirical_full_min 0.462