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_4109533
_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            'C42 H49 O4 P Pd Ru Sn'
_chemical_formula_weight         974.94
_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                101.2120(10)
_cell_angle_beta                 106.4740(10)
_cell_angle_gamma                103.0630(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5256(5)
_cell_length_b                   12.7825(6)
_cell_length_c                   17.0037(8)
_cell_measurement_reflns_used    6362
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.16
_cell_volume                     2248.67(18)
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23526
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.30
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    1.349
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.707
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         11021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0469
_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^)+(0.1095P)^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         0.1729
_reflns_number_gt                8009
_reflns_number_total             11021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070617hsi20070127_041638.cif
_cod_data_source_block           p-1
_cod_database_code               4109533