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_4106220
_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         'C53 H59 B N P2 Ru, C32 H12 B F24 '
_chemical_formula_sum            'C85 H71 B2 F24 N P2 Ru'
_chemical_formula_weight         1747.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             10-10-06
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                90
_cell_angle_beta                 90.5650(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.77790(10)
_cell_length_b                   12.47820(10)
_cell_length_c                   35.9708(3)
_cell_measurement_reflns_used    17439
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     7979.24(10)
_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 0.987
_diffrn_measured_fraction_theta_max 0.984
_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  0.049
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            74381
_diffrn_reflns_theta_full        26.404
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         5.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.41
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9302
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1120
_refine_ls_number_reflns         18022
_refine_ls_number_restraints     486
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.0056251
_refine_ls_shift/su_mean         0.4607135
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +17.10P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1374
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1374
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                11388
_reflns_number_total             18022
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.91
_oxford_diffrn_Wilson_scale      76.40
_oxford_refine_ls_r_factor_ref   0.1072
_oxford_refine_ls_scale          0.12738(4)
_oxford_reflns_number_all        18022
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 005dvdv10
_cod_data_source_file            ja203051d_si_001.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C85 H71 B2 F24 N1 P2 Ru1'
_cod_database_code               4106220