Group 10 and 11 Metal Boratranes (Ni, Pd, Pt, CuCl, AgCl, AuCl, and Au+) Derived from a Triphosphine-Borane
Marie Sircoglou; Sébastien Bontemps; Ghenwa Bouhadir; Nathalie Saffon; Karinne Miqueu; Weixing Gu; Maxime Mercy; Chun-Hsing Chen; Bruce M. Foxman; Laurent Maron; Oleg V. Ozerov; Didier Bourissou; Journal of the American Chemical Society 130 (2008) 16729–16738; doi:10.1021/ja8070072

data_4108800
_publ_section_title
;
 Group 10 and 11 Metal Boratranes (Ni, Pd, Pt, CuCl, AgCl, AuCl, and Au+)
 Derived from a Triphosphine-Borane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16729
_journal_page_last               16738
_journal_paper_doi               10.1021/ja8070072
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C36 H54 B1 P3 Pd1'
_chemical_formula_sum            'C36 H54 B P3 Pd'
_chemical_formula_weight         696.96
_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
_audit_creation_date             07-10-11
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                76.909(2)
_cell_angle_beta                 78.583(2)
_cell_angle_gamma                60.716(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0591(5)
_cell_length_b                   11.2426(6)
_cell_length_c                   16.7043(8)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     1755.09(15)
_computing_cell_refinement       'Apex2, (Bruker AXS, 2006)'
_computing_data_collection       'Apex2, (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2, (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51474
_diffrn_reflns_theta_full        29.636
_diffrn_reflns_theta_max         30.241
_diffrn_reflns_theta_min         2.101
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.689
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2, (Bruker AXS, 2006)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.71
_refine_diff_density_min         -0.49
_refine_ls_extinction_coef       55(14)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9776
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         10368
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.003649
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.87P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0914
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0914
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                9169
_reflns_number_total             10368
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.83
_oxford_diffrn_Wilson_scale      37.83
_oxford_refine_ls_r_factor_ref   0.0365
_oxford_refine_ls_scale          0.16936(7)
_oxford_reflns_number_all        10368
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ125_0m in P-1'
_cod_data_source_file            ja8070072_si_003.cif
_cod_data_source_block           oz125
_cod_original_cell_volume        1755.10(15)
_cod_original_sg_symbol_Hall     '-P  1'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H54 B1 P3 Pd1'
_cod_database_code               4108800