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_4325983
_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         'C25 H46 B11 F2 N1 P2 Pd1'
_chemical_formula_sum            'C25 H46 B11 F2 N P2 Pd'
_chemical_formula_weight         685.91
_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             11-01-17
_audit_creation_method           CRYSTALS_ver_14.15
_cell_angle_alpha                90
_cell_angle_beta                 96.191(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3681(5)
_cell_length_b                   15.0979(5)
_cell_length_c                   16.8618(6)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    120
_cell_measurement_theta_max      30
_cell_measurement_theta_min      2
_cell_volume                     3383.4(2)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_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  0.095
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            69655
_diffrn_reflns_theta_full        30.210
_diffrn_reflns_theta_max         30.210
_diffrn_reflns_theta_min         1.815
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 (Bruker AXS, 2006)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.296
_exptl_crystal_size_min          0.260
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9822
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         10007
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.0038131
_refine_ls_shift/su_mean         0.0002720
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.82P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1086
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1086
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                8465
_reflns_number_total             10007
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.18
_oxford_diffrn_Wilson_scale      9.09
_oxford_refine_ls_r_factor_ref   0.0491
_oxford_refine_ls_scale          0.3476(3)
_oxford_reflns_number_all        10007
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'OZ112_0m in P2(1)/n'
_cod_data_source_file            ic2001283_si_001.cif
_cod_data_source_block           oz112
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C25 H46 B11 F2 N1 P2 Pd1'
_cod_database_code               4325983
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, PD(1,U'S) UNTIL C(23) 
CONT C(24,U[ISO]) C(25,U'S) C(241,U[ISO]) 
CONT H(501,X'S,U[ISO]) 
CONT B(1,U'S) UNTIL B(11) 
EQUIV PART(1001, OCC) PART(1002,OCC) 
WEIGHT -1 PART(1002,OCC) 
RIDE B   (   2,X'S) H   ( 502,X'S) 
RIDE B   (   3,X'S) H   ( 503,X'S) 
RIDE B   (   4,X'S) H   ( 504,X'S) 
RIDE B   (   5,X'S) H   ( 505,X'S) 
RIDE B   (   6,X'S) H   ( 506,X'S) 
RIDE B   (   7,X'S) H   ( 507,X'S) 
RIDE B   (   8,X'S) H   ( 508,X'S) 
RIDE B   (   9,X'S) H   ( 509,X'S) 
RIDE B   (  10,X'S) H   ( 510,X'S) 
RIDE B   (  11,X'S) H   ( 511,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) H   ( 143,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) H   ( 152,X'S) H   ( 153,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) H   ( 172,X'S) H   ( 173,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) H   ( 183,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) H   ( 203,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) H   ( 212,X'S) H   ( 213,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) H   ( 233,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   ( 241,X'S) H   (2411,X'S) H   (2412,X'S) H   (2413,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;