Concerted reductive coupling of an alkyl chloride at Pt(IV)
Sarah H. Crosby; Helen R. Thomas; Guy J. Clarkson; Jonathan P. Rourke; Chem.Commun. 48 (2012) 5775–; doi:10.1039/c2cc31572f

data_7107775
_publ_section_title
;
 Concerted reductive coupling of an alkyl chloride at Pt(IV)
;
_journal_name_full               Chem.Commun.
_journal_page_first              5775
_journal_paper_doi               10.1039/c2cc31572f
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C21.5 H31 Cl2 F N O3.5 Pt S'
_chemical_formula_weight         676.52
_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                103.566(4)
_cell_angle_beta                 95.759(3)
_cell_angle_gamma                105.831(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8916(4)
_cell_length_b                   10.3390(5)
_cell_length_c                   13.0249(4)
_cell_measurement_reflns_used    15119
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      3.01
_cell_volume                     1226.39(10)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20461
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.38
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    6.057
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.083
_refine_diff_density_min         -2.526
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6025
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.279
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0762
_reflns_number_gt                5401
_reflns_number_total             6025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31572f.txt
_cod_data_source_block           sc16
_cod_original_cell_volume        1226.38(9)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C21.50 H31 Cl2 F N O3.50 Pt S'
_cod_database_code               7107775