Fluoroalkylation of a Methylplatinum(II) Complex under Photoirradiation
Suzaki, Yuji; Kiho, Minetada; Osakada, Kohtaro; Organometallics 36 (2017) 1391–; doi:10.1021/acs.organomet.7b00098

data_4089250
_publ_section_title
;
 Fluoroalkylation of a Methylplatinum(II) Complex under Photoirradiation
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1391
_journal_paper_doi               10.1021/acs.organomet.7b00098
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C35 H26 F18 P2 Pt'
_chemical_formula_weight         1045.59
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.4620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5231(8)
_cell_length_b                   11.2614(6)
_cell_length_c                   21.4757(11)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    90
_cell_measurement_theta_max      25.3635
_cell_measurement_theta_min      2.282
_cell_volume                     3539.7(3)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHELL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0132
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15383
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.106
_diffrn_reflns_theta_max         24.106
_diffrn_reflns_theta_min         1.419
_exptl_absorpt_coefficient_mu    4.177
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.048
_refine_diff_density_max         2.434
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5607
_refine_ls_number_restraints     672
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0352P)^2^+13.2555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5400
_reflns_number_total             5607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om7b00098_si_002.cif
_cod_data_source_block           Pt_n-C4F9_2_dppp
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089250
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.471
_shelx_estimated_absorpt_t_max   0.825
_shelx_res_checksum              93893
_shelx_hkl_checksum              22090