Activation of Metal Hydride Complexes by Tri-tert-butylphosphine-Platinum and -Palladium Groups
Richard D. Adams; Burjor Captain; Eszter Trufan; Lei Zhu; Journal of the American Chemical Society 129 (2007) 7545–7556; doi:10.1021/ja070617h

data_4109535
_publ_section_title
;
 Activation of Metal Hydride Complexes by Tri-tert-butylphosphine-Platinum
 and -Palladium Groups
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7545
_journal_page_last               7556
_journal_paper_doi               10.1021/ja070617h
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C49 H55 O3 Os P Pt Sn'
_chemical_formula_weight         1226.88
_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                94.8840(10)
_cell_angle_beta                 91.4710(10)
_cell_angle_gamma                106.5410(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9318(3)
_cell_length_b                   12.0190(3)
_cell_length_c                   19.9237(5)
_cell_measurement_reflns_used    5838
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.33
_cell_volume                     2268.49(11)
_computing_cell_refinement       'SAINT+  V6.2 (Bruker, 2001)'
_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT+  V6.2'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24087
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.03
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    6.490
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            lightyellow
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         11179
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+0.9379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                8777
_reflns_number_total             11179
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070617hsi20070127_041725.cif
_cod_data_source_block           p-1
_cod_database_code               4109535