Seeking a Mechanistic Analogue of the Water-Gas Shift Reaction: Carboxamido Ligand Formation and Isocyanate Elimination from Complexes Containing the Tp'PtMe Fragment
Bryan E. Frauhiger; Matthew T. Ondisco; Peter S. White; Joseph L. Templeton; Journal of the American Chemical Society 134 (2012) 8902–8910; doi:10.1021/ja301213j

data_4117983
_publ_section_title
;
 Seeking a Mechanistic Analogue of the Water-Gas Shift Reaction:
 Carboxamido Ligand Formation and Isocyanate Elimination from Complexes
 Containing the Tp'PtMe Fragment
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8902
_journal_page_last               8910
_journal_paper_doi               10.1021/ja301213j
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C25 H36 B N7 O Pt'
_chemical_formula_sum            'C25 H36 B N7 O Pt'
_chemical_formula_weight         656.51
_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                78.606(2)
_cell_angle_beta                 77.336(3)
_cell_angle_gamma                77.100(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1004(3)
_cell_length_b                   9.5201(3)
_cell_length_c                   18.1022(7)
_cell_measurement_reflns_used    6311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.74
_cell_measurement_theta_min      4.82
_cell_volume                     1311.34(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12697
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         4.82
_exptl_absorpt_coefficient_mu    10.253
_exptl_absorpt_correction_T_max  0.4331
_exptl_absorpt_correction_T_min  0.3199
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker-AXS Apex2'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.048
_refine_diff_density_min         -2.292
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         4414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+4.8657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1051
_reflns_number_gt                4161
_reflns_number_total             4414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja301213j_si_002.cif
_cod_data_source_block           x1002027
_cod_database_code               4117983