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_7702092
_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_absolute_configuration ad
_chemical_formula_moiety         'C26 H30 Cl2 F2 N P Pt'
_chemical_formula_sum            'C26 H30 Cl2 F2 N P Pt'
_chemical_formula_weight         691.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_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            4
_cell_length_a                   18.3851(2)
_cell_length_b                   12.6327(2)
_cell_length_c                   11.03420(10)
_cell_measurement_reflns_used    17208
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.6220
_cell_measurement_theta_min      3.2060
_cell_volume                     2562.73(5)
_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_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
  1 omega  -25.00   54.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       13.2579  -99.0000 -180.0000 79

  2 omega  -88.00   10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.1954  -38.0000  -30.0000 98

  3 omega  -25.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.1954  -99.0000  120.0000 52

  4 omega  -88.00   10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.1954  -38.0000 -150.0000 98

  5 omega  -47.00   62.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.1954   77.0000  -60.0000 109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0314940000
_diffrn_orient_matrix_UB_12      -0.0157192000
_diffrn_orient_matrix_UB_13      -0.0305221000
_diffrn_orient_matrix_UB_21      0.0435723000
_diffrn_orient_matrix_UB_22      0.0114378000
_diffrn_orient_matrix_UB_23      -0.0233428000
_diffrn_orient_matrix_UB_31      0.0162006000
_diffrn_orient_matrix_UB_32      -0.0612665000
_diffrn_orient_matrix_UB_33      0.0034724000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31888
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.722
_diffrn_reflns_theta_min         3.225
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.776
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70434
_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.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       block
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details
;
 Flack x determined using 2698 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         7234
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0139P)^2^+0.4687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0412
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.859
_reflns_number_gt                6460
_reflns_number_total             7234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02088g3.cif
_cod_data_source_block           ps10
_cod_database_code               7702092
_chemical_oxdiff_formula         'C20 H20 N2 O2 F2 P Pt'
_olex2_refinement_description
;
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.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C24(H24A,H24B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,
 H22B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C5(H5), C2(H2), C13(H13), C9(H9), C4(H4), C8(H8), C10(H10)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'