Aminoborane σ Complexes: Significance of Hydride Co-ligands in Dynamic Processes and Dehydrogenative Borylene Formation
Addy, David A.; Bates, Joshua I.; Kelly, Michael J.; Riddlestone, Ian M.; Aldridge, Simon; Organometallics 32 (2013) 1583–; doi:10.1021/om400040q

data_4080505
_publ_section_title
;
 Aminoborane \s Complexes: Significance of Hydride Co-ligands in Dynamic
 Processes and Dehydrogenative Borylene Formation
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1583
_journal_paper_doi               10.1021/om400040q
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety
'C32 H12 B F24, C23 H36 P Ru, 1.0(C3 H6), 2.0(C H2)'
_chemical_formula_sum            'C60 H58 B F24 P Ru'
_chemical_formula_weight         1377.93
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 94.5427(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.97170(10)
_cell_length_b                   17.27170(10)
_cell_length_c                   36.3666(3)
_cell_measurement_reflns_used    13542
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     11878.94(14)
_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    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_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  0.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            78601
_diffrn_reflns_theta_full        26.669
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         5.119
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5583.999
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.88
_refine_diff_density_min         -1.68
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9280
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1000
_refine_ls_number_reflns         13517
_refine_ls_number_restraints     1160
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.0528527
_refine_ls_shift/su_mean         0.0010718
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1915
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1915
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              47
_reflns_limit_l_min              0
_reflns_number_gt                8853
_reflns_number_total             13517
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.48
_oxford_diffrn_Wilson_scale      250.60
_oxford_refine_ls_r_factor_ref   0.1168
_oxford_refine_ls_scale          0.07463(2)
_oxford_reflns_number_all        13517
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            om400040q_si_002.cif
_cod_data_source_block           allyl
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               4080505