Probing the Intrinisic Structure and Dynamics of Aminoborane Coordination at Late Transition Metal Centers: Mono(σ-BH) Binding in [CpRu(PR3)2(H2BNCy2)]+
Dragoslav Vidovic; David A. Addy; Tobias Krämer; John McGrady; Simon Aldridge; Journal of the American Chemical Society 133 (2011) 8494–8497; doi:10.1021/ja203051d

data_4106221
_publ_section_title
;
 Probing the Intrinisic Structure and Dynamics of Aminoborane Coordination
 at Late Transition Metal Centers: Mono(\s-BH) Binding in
 [CpRu(PR3)2(H2BNCy2)]+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8494
_journal_page_last               8497
_journal_paper_doi               10.1021/ja203051d
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C43 H77 B N P2 Ru, C32 H12 B F24'
_chemical_formula_sum            'C75 H89 B2 F24 N P2 Ru'
_chemical_formula_weight         1645.13
_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             10-10-07
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                92.5084(7)
_cell_angle_beta                 103.5033(6)
_cell_angle_gamma                93.3378(7)
_cell_formula_units_Z            2
_cell_length_a                   13.2296(2)
_cell_length_b                   17.2074(3)
_cell_length_c                   17.6001(3)
_cell_measurement_reflns_used    15360
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3882.45(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      150
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58703
_diffrn_reflns_theta_full        25.258
_diffrn_reflns_theta_max         27.454
_diffrn_reflns_theta_min         5.105
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             1692.000
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.20
_refine_diff_density_min         -1.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9283
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1141
_refine_ls_number_reflns         15764
_refine_ls_number_restraints     1026
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0735
_refine_ls_shift/su_max          0.0369768
_refine_ls_shift/su_mean         0.0325613
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +21.53P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1930
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1929
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                12119
_reflns_number_total             17192
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.24
_oxford_diffrn_Wilson_scale      10.62
_oxford_refine_ls_r_factor_ref   0.0969
_oxford_refine_ls_scale          0.3422(4)
_oxford_reflns_number_all        15767
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 030dvdv10
_cod_data_source_file            ja203051d_si_002.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C75 H89 B2 F24 N1 P2 Ru1'
_cod_database_code               4106221