Characterization of a Paramagnetic, Mononuclear Pt(III)-Alkyl Complex Intermediate in Carbon-Halogen Bond Coupling Reactions
Orestes Rivada-Wheelaghan; Manuel A. Ortuño; Josefina Díez; Sergio E. García-Garrido; Celia Maya; Agustí Lledós; Salvador Conejero; Journal of the American Chemical Society 134 (2012) 15261–15264; doi:10.1021/ja307139p

data_4118652
_publ_section_title
;
 Characterization of a Paramagnetic, Mononuclear Pt(III)-Alkyl Complex
 Intermediate in Carbon-Halogen Bond Coupling Reactions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15261
_journal_page_last               15264
_journal_paper_doi               10.1021/ja307139p
_journal_volume                  134
_journal_year                    2012
_chemical_formula_sum            'C90 H91 B Br F24 N4 O Pt'
_chemical_formula_weight         1986.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.4560(10)
_cell_angle_beta                 79.2270(10)
_cell_angle_gamma                75.1580(10)
_cell_formula_units_Z            2
_cell_length_a                   16.7829(5)
_cell_length_b                   17.3523(5)
_cell_length_c                   18.2034(5)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.36
_cell_volume                     4851.3(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            49904
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.948
_exptl_absorpt_correction_T_max  0.792
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS, Bruker (2006). APEX 2. Version 2.1. Bruker Analytical
 X-ray Solutions, Madison, Wisconsin, USA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       prism
_exptl_crystal_F_000             2002
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_platon_squeeze_details          ' '
_refine_diff_density_max         0.905
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         16623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0830
_reflns_number_gt                14678
_reflns_number_total             16623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja307139p_si_001_3.cif
_cod_data_source_block           4a
_cod_original_formula_sum        'C45 H45.50 B0.50 Br0.50 F12 N2 O0.50 Pt0.50'
_cod_database_code               4118652