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_4325986
_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         'C46 H65 B13 F3 N1 O4 P2 Pd1'
_chemical_formula_sum            'C46 H65 B13 F3 N O4 P2 Pd'
_chemical_formula_weight         1061.91
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 95.6420(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5684(8)
_cell_length_b                   16.5154(7)
_cell_length_c                   33.9184(13)
_cell_measurement_reflns_used    9347
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     10908.6(8)
_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 0.999
_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  0.033
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            145552
_diffrn_reflns_theta_full        29.996
_diffrn_reflns_theta_max         29.996
_diffrn_reflns_theta_min         1.617
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       prism
_exptl_crystal_F_000             4384
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0609
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         15886
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001841
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +13.68P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0741
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0741
_reflns_limit_h_max              27
_reflns_limit_h_min              -27
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              47
_reflns_limit_l_min              0
_reflns_number_gt                14450
_reflns_number_total             15886
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.28
_oxford_diffrn_Wilson_scale      900.39
_oxford_refine_ls_r_factor_ref   0.0328
_oxford_refine_ls_scale          0.0347950(15)
_oxford_reflns_number_all        15886
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            ic2001283_si_004.cif
_cod_data_source_block           oz170
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C46 H65 B13 F3 N1 O4 P2 Pd1'
_cod_database_code               4325986