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_1546252
_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 H30 F2 N P Pt'
_chemical_formula_sum            'C38 H30 F2 N P Pt'
_chemical_formula_weight         764.69
_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             2016-06-02
_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                68.816(6)
_cell_angle_beta                 69.917(6)
_cell_angle_gamma                64.636(6)
_cell_formula_units_Z            2
_cell_length_a                   12.1213(8)
_cell_length_b                   12.1909(7)
_cell_length_c                   12.2729(8)
_cell_measurement_reflns_used    18316
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4320
_cell_measurement_theta_min      3.9460
_cell_volume                     1489.24(19)
_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 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.975
_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   -122.00  -1.00   1.00    1.00    --  -41.57 -19.00 -90.00  121
  2  \w    -66.00  33.00   1.00    1.00    --  -41.57  37.00  90.00   99
  3  \w      1.00  82.00   1.00    1.00    --   41.57 -99.00 -30.00   81
  4  \w      1.00  82.00   1.00    1.00    --   41.57 -99.00-180.00   81
  5  \w     25.00 160.00   1.00    4.00    --  107.00 -15.00 -60.00  135
  6  \w     34.00 121.00   1.00    4.00    --  107.00-125.00  60.00   87
  7  \w     79.00 178.00   1.00    4.00    --  107.00  30.00 120.00   99
  8  \w     79.00 178.00   1.00    4.00    --  107.00  30.00 -30.00   99
  9  \w     34.00 121.00   1.00    4.00    --  107.00-125.00-120.00   87
 10  \w     35.00 136.00   1.00    4.00    --  107.00 -61.00-150.00  101
 11  \w     35.00 136.00   1.00    4.00    --  107.00 -61.00  30.00  101
 12  \w   -118.00  -9.00   1.00    1.00    --  -41.57 -77.00  90.00  109
 13  \w   -115.00 -13.00   1.00    1.00    --  -41.57 -57.00-180.00  102
 14  \w      9.00 118.00   1.00    1.00    --   41.57  77.00   0.00  109
 15  \w     74.00 178.00   1.00    4.00    --  107.00  77.00-120.00  104
 16  \w     79.00 178.00   1.00    4.00    --  107.00  30.00-150.00   99
 17  \w     78.00 178.00   1.00    4.00    --  107.00  61.00   0.00  100
 18  \w     78.00 178.00   1.00    4.00    --  107.00  61.00  60.00  100
 19  \w     81.00 178.00   1.00    4.00    --  107.00  45.00 150.00   97
 20  \w     78.00 178.00   1.00    4.00    --  107.00  61.00  30.00  100
 21  \w   -118.00  -9.00   1.00    1.00    --  -41.57 -77.00   0.00  109
 22  \w   -115.00 -13.00   1.00    1.00    --  -41.57 -57.00 120.00  102
 23  \w      9.00 118.00   1.00    1.00    --   41.57  77.00 -90.00  109
 24  \w     74.00 178.00   1.00    4.00    --  107.00  77.00  90.00  104
 25  \w     74.00 178.00   1.00    4.00    --  107.00  77.00 -60.00  104
 26  \w     74.00 178.00   1.00    4.00    --  107.00  77.00 -90.00  104
 27  \w     74.00 178.00   1.00    4.00    --  107.00  77.00 -30.00  104
 28  \w     74.00 178.00   1.00    4.00    --  107.00  77.00 150.00  104
 29  \w     74.00 178.00   1.00    4.00    --  107.00  77.00-150.00  104
 30  \w   -116.00 -17.00   1.00    1.00    --  -41.57 -37.00-120.00   99
 31  \w     57.00 130.00   1.00    1.00    --   41.57 178.00   0.00   73
;
_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      -0.0804362000
_diffrn_orient_matrix_UB_12      0.1402359000
_diffrn_orient_matrix_UB_13      -0.0157062000
_diffrn_orient_matrix_UB_21      -0.0986092000
_diffrn_orient_matrix_UB_22      -0.0331272000
_diffrn_orient_matrix_UB_23      0.1124038000
_diffrn_orient_matrix_UB_31      0.0680692000
_diffrn_orient_matrix_UB_32      0.0112499000
_diffrn_orient_matrix_UB_33      0.0787269000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27666
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.900
_diffrn_reflns_theta_min         3.964
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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    1.705
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.480
_refine_diff_density_min         -1.235
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5891
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0506P)^2^+0.6526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5672
_reflns_number_total             5891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01361b2.cif
_cod_data_source_block           ps33
_cod_original_cell_volume        1489.22(19)
_cod_database_code               1546252
_chemical_oxdiff_formula         'C20 H20 N2 O2 F Pt'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;

SIMU restraints were used to make the thermal ellipsoids of some of the atoms at the 
back edge of the pyridine ligand less elongated

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim F3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim F15: within
1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
3.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C25(H25A,H25B), C18(H18A,H18B)
3.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C37(H37), C27(H27), C28(H28), C38(H38), C29(H29), C31(H31), C2(H2),
 C21(H21), C16(H16), C34(H34), C30(H30), C24(H24), C36(H36), C22(H22), C35(H35),
  C23(H23), C13(H13), C10(H10), C5(H5), C9(H9), C8(H8), C14(H14), C4(H4)
;
_shelx_res_checksum              23295
_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 4.531
_oxdiff_exptl_absorpt_empirical_full_min 0.514