Net Heterolytic Cleavage of B-H and B-B Bonds Across the N-Pd Bond in a Cationic (PNP)Pd Fragment
Yanjun Zhu; Chun-Hsing Chen; Claudia M. Fafard; Bruce M. Foxman; Oleg V. Ozerov; Inorganic Chemistry 50 (2011) 7980–7987; doi:10.1021/ic2001283

data_4325985
_publ_section_title
;
 Net Heterolytic Cleavage of B-H and B-B Bonds Across the N-Pd Bond in a
 Cationic (PNP)Pd Fragment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7980
_journal_page_last               7987
_journal_paper_doi               10.1021/ic2001283
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C64.70 H59 B2 Cl1.40 F24 N1 O2.30 P2 Pd1'
_chemical_formula_sum            'C64.7 H59 B2 Cl1.4 F24 N O2.3 P2 Pd'
_chemical_formula_weight         1582.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-03-18
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 107.121(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1660(8)
_cell_length_b                   18.3171(9)
_cell_length_c                   22.9978(11)
_cell_measurement_reflns_used    9849
_cell_measurement_temperature    120
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     6910.8(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.051
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            101948
_diffrn_reflns_theta_full        27.458
_diffrn_reflns_theta_max         28.019
_diffrn_reflns_theta_min         1.312
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       plate
_exptl_crystal_F_000             3193.544
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.69
_refine_diff_density_min         -1.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9765
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     953
_refine_ls_number_reflns         16624
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.015254
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ +15.87P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1298
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1298
_reflns_limit_h_max              21
_reflns_limit_h_min              -22
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                10930
_reflns_number_total             16624
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0775
_oxford_refine_ls_scale          0.051764(6)
_oxford_reflns_number_all        16624
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ148_0m in P2(1)/n'
_cod_data_source_file            ic2001283_si_003.cif
_cod_data_source_block           oz148
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C64.70 H59 B2 Cl1.40 F24 N1 O2.30 P2 Pd1'
_cod_database_code               4325985