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_4118650
_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_compound_source        synthesis
_chemical_formula_moiety         'C54 H71 Br2 N4 Pt, C32 H12 B F24'
_chemical_formula_sum            'C86 H83 B Br2 F24 N4 Pt'
_chemical_formula_weight         1994.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_cell_angle_alpha                91.848(3)
_cell_angle_beta                 100.505(3)
_cell_angle_gamma                91.036(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9869(5)
_cell_length_b                   15.2767(6)
_cell_length_c                   21.7730(9)
_cell_measurement_reflns_used    14068
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.4721
_cell_measurement_theta_min      2.8926
_cell_volume                     4243.8(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004(Burla, 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device
; 
165 mm Onyx CCD detector in \k-geometry diffractometer
;
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            26216
_diffrn_reflns_theta_full        74.64
_diffrn_reflns_theta_max         74.64
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    5.065
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.055
_refine_diff_density_max         3.853
_refine_diff_density_min         -3.341
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         16315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1726
_reflns_number_gt                12787
_reflns_number_total             16315
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja307139p_si_001_1.cif
_cod_data_source_block           2a
_cod_database_code               4118650