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_4106222
_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         'C31 H53 N2 P2 Ru, C32 H12 B F24, C6 H5 F'
_chemical_formula_sum            'C69 H70 B F25 N2 P2 Ru'
_chemical_formula_weight         1576.11
_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             10-10-09
_audit_creation_method           CRYSTALS_ver_14.03
_cell_angle_alpha                90
_cell_angle_beta                 93.5095(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8044(2)
_cell_length_b                   24.7611(4)
_cell_length_c                   22.1693(3)
_cell_measurement_reflns_used    12324
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     7015.62(18)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.039
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61695
_diffrn_reflns_theta_full        25.109
_diffrn_reflns_theta_max         25.109
_diffrn_reflns_theta_min         5.157
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.39
_refine_diff_density_min         -1.41
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9759
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         12282
_refine_ls_number_restraints     2410
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.1080
_refine_ls_shift/su_max          0.0450861
_refine_ls_shift/su_mean         1.0133337
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 39.0 58.5 26.7 6.15 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3318
_refine_ls_wR_factor_gt          0.2855
_refine_ls_wR_factor_ref         0.3318
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                8369
_reflns_number_total             12282
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   4.92
_oxford_diffrn_Wilson_scale      32.50
_oxford_refine_ls_r_factor_ref   0.1407
_oxford_refine_ls_scale          0.2055(3)
_oxford_reflns_number_all        12282
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 038dvdv10
_cod_data_source_file            ja203051d_si_003.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C69 H70 B1 F25 N2 P2 Ru1'
_cod_database_code               4106222