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_4118651
_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         'C46 H55 I2 N4 Pt, C32 H12 B F24'
_chemical_formula_sum            'C78 H67 B F24 I2 N4 Pt'
_chemical_formula_weight         1976.06
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
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                90.00
_cell_angle_beta                 101.828(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.6090(6)
_cell_length_b                   15.0856(3)
_cell_length_c                   33.5520(6)
_cell_measurement_reflns_used    9573
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.9349
_cell_measurement_theta_min      2.8899
_cell_volume                     7732.8(4)
_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 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0936
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26609
_diffrn_reflns_theta_full        74.10
_diffrn_reflns_theta_max         74.10
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    10.581
_exptl_absorpt_correction_T_max  0.628
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       prism
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.004
_refine_diff_density_min         -2.757
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         15003
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+2.0645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                11020
_reflns_number_total             15003
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja307139p_si_001_2.cif
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4118651