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_4325984
_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 H57 B2 F24 N1 O2 P2 Pd1'
_chemical_formula_sum            'C64 H57 B2 F24 N O2 P2 Pd'
_chemical_formula_weight         1518.08
_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             08-03-17
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                89.269(4)
_cell_angle_beta                 88.814(4)
_cell_angle_gamma                86.015(4)
_cell_formula_units_Z            2
_cell_length_a                   12.3756(9)
_cell_length_b                   15.6639(11)
_cell_length_c                   19.3865(14)
_cell_measurement_reflns_used    9801
_cell_measurement_temperature    120
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     3747.9(5)
_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 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.045
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22029
_diffrn_reflns_theta_full        29.586
_diffrn_reflns_theta_max         30.190
_diffrn_reflns_theta_min         1.650
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.389
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       plate
_exptl_crystal_F_000             1532
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
During the structure solution, electron density difference 
maps revealed that there was considerable disordered 
solvent molecules (from history, methylene chloride and/or 
pentane) in a volume of 654 \%A3 per unit cell; the peaks 
could not be modeled successfully.  Thus, the structure 
factors were modified using the PLATON SQUEEZE technique, 
in order to produce a ?solvate-free? structure factor set.  
PLATON reported a total electron density of 104 e- for the 
cavity, slightly larger than two methylene chloride molecules, 
with perhaps an additional pentane (110 non-H atom electrons).  
Use of the SQUEEZE technique resulted in a decrease 
of ca 4% in R
;
_refine_diff_density_max         1.63
_refine_diff_density_min         -1.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         22029
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.005654
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 4.43P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1471
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1471
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                14909
_reflns_number_total             22029
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.90
_oxford_diffrn_Wilson_scale      183.37
_oxford_refine_ls_r_factor_ref   0.0712
_oxford_refine_ls_scale          0.083271(14)
_oxford_reflns_number_all        22029
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ144_0m in P-1'
_cod_data_source_file            ic2001283_si_002.cif
_cod_data_source_block           oz144
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C64 H57 B2 F24 N1 O2 P2 Pd1'
_cod_database_code               4325984