Trapping five-coordinate platinum(iv) intermediates.
Shaw, Paul A.; Phillips, Jessica M.; Clarkson, Guy J.; Rourke, Jonathan P.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 11397–11406; doi:10.1039/c6dt02088g

data_7702093
_publ_section_title
;
 Trapping five-coordinate platinum(iv) intermediates.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11397
_journal_page_last               11406
_journal_paper_doi               10.1039/c6dt02088g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C26 H30 Cl2 F2 N P Pt, 0.5(C7 H8)'
_chemical_formula_sum            'C29.5 H34 Cl2 F2 N P Pt'
_chemical_formula_weight         737.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-05-24 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.2105(2)
_cell_length_b                   17.91980(10)
_cell_length_c                   17.59350(10)
_cell_measurement_reflns_used    9457
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.5040
_cell_measurement_theta_min      4.2610
_cell_volume                     5741.26(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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 0.991
_diffrn_measurement_details
;
  1 omega  -47.00   30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -180.0000 77

  2 omega -111.00   -8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -19.0000 -180.0000 103

  3 omega   38.00   88.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3790 -123.0000 -101.0000 50

  4 omega   74.00  171.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   15.0000  -90.0000 97

  5 omega   43.00   70.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -77.0000   90.0000 27

  6 omega   96.00  177.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000  150.0000 81

  7 omega   78.00  104.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000    0.0000 26

  8 omega   41.00  109.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000  -90.0000 68

  9 omega   93.00  120.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   61.0000  -90.0000 27

 10 omega  129.00  165.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   61.0000  -90.0000 36

 11 omega   87.00  117.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -123.0000 -101.0000 30

 12 omega   76.00  137.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -77.0000   90.0000 61

 13 omega   37.00   63.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000   90.0000 26

 14 omega   70.00  109.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -94.0000   90.0000 39

 15 omega   49.00   74.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -123.0000 -101.0000 25

 16 omega   44.00   75.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000    0.0000 31

 17 omega   50.00   96.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -45.0000  -60.0000 46

 18 omega   43.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000  -60.0000 44

 19 omega   50.00   95.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -45.0000   60.0000 45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0033934000
_diffrn_orient_matrix_UB_12      0.0758154000
_diffrn_orient_matrix_UB_13      0.0397553000
_diffrn_orient_matrix_UB_21      0.0073486000
_diffrn_orient_matrix_UB_22      0.0405553000
_diffrn_orient_matrix_UB_23      -0.0742464000
_diffrn_orient_matrix_UB_31      -0.0871921000
_diffrn_orient_matrix_UB_32      0.0004315000
_diffrn_orient_matrix_UB_33      -0.0078293000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16968
_diffrn_reflns_point_group_measured_fraction_full 0.826
_diffrn_reflns_point_group_measured_fraction_max 0.802
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.949
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.649
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.707
_exptl_crystal_description       block
_exptl_crystal_F_000             2904
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Flack x determined using 1557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4983
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0292P)^2^+3.9503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0656
_reflns_Friedel_coverage         0.564
_reflns_Friedel_fraction_full    0.639
_reflns_Friedel_fraction_max     0.598
_reflns_number_gt                4735
_reflns_number_total             4983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02088g3.cif
_cod_data_source_block           ps17
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_formula_sum        'C29.50 H34 Cl2 F2 N P Pt'
_cod_database_code               7702093
_chemical_oxdiff_formula         'C20 H20 N O F Pt'
_olex2_refinement_description
;
The hydrogens H20A and H20B on C20 were located in a difference map. 
Their position and Uiso were allowed to refine freely. 
They form reasonable bond lengths and angles with the carbon back bone 
and have sensible thermal parameters.
The toluene C100-C106 was modeled as a half occupancy behind a PART -1 
instruction as it is disordered across the two fold axis.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C100(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C101(0.5) H101(0.5)
 C102(0.5) H102(0.5) C103(0.5) H103(0.5) C104(0.5) H104(0.5) C105(0.5)
 H105(0.5) C106(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C25(H25A,H25B), C24(H24A,H24B), C21(H21A,H21B), C22(H22A,
 H22B), C19(H19A,H19B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C4(H4), C10(H10), C9(H9), C8(H8), C17(H17), C14(H14),
 C13(H13), C16(H16), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105)
3.c Fitted hexagon refined as free rotating group:
 C101(C102,C103,C104,C105,C106)
3.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C100(H10A,H10B,H10C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'