The Conformations of 13-Vertex ML~2~C~2~B~10~ Metallacarboranes: Experimental and Computational Studies
Kelly J. Dalby; David Ellis; Stefan Erhardt; Ruaraidh D. McIntosh; Stuart A. Macgregor; Karen Rae; Georgina M. Rosair; Volker Settels; Alan J. Welch; Bruce E. Hodson; Thomas D. McGrath; F. Gordon A. Stone; Journal of the American Chemical Society 129 (2007) 3302–3314; doi:10.1021/ja067698m

data_4109175
_publ_contact_author
;
        Prof Alan Welch
        Department of Chemistry
        Heriot-Watt University
        Edinburgh EH14 4AS
;
_publ_contact_author_email       A.J.Welch@hw.ac.uk
_publ_contact_author_fax         '0131 451 3180'
_publ_contact_author_phone       '0131 451-3217'
_publ_section_title
;
 The Conformations of 13-Vertex ML~2~C~2~B~10~ Metallacarboranes:
 Experimental and Computational Studies
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3302
_journal_page_last               3314
_journal_paper_doi               10.1021/ja067698m
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety
'C36 H30 N P2, C10 H24 B10 Rh, 0.5(C H2 Cl2) '
_chemical_formula_sum            'C46.5 H55 B10 Cl N P2 Rh'
_chemical_formula_weight         936.32
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                113.67(4)
_cell_angle_beta                 100.35(4)
_cell_angle_gamma                98.26(3)
_cell_formula_units_Z            2
_cell_length_a                   10.056(5)
_cell_length_b                   14.692(7)
_cell_length_c                   17.296(13)
_cell_measurement_reflns_used    4665
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.81
_cell_measurement_theta_min      2.31
_cell_volume                     2235(2)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker-Nonius X8 Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45526
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.64
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       block
_exptl_crystal_F_000             966
_exptl_crystal_size_max          0.133
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.801
_refine_diff_density_min         -1.745
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         10159
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                7644
_reflns_number_total             10159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067698msi20070131_125137_3.cif
_cod_data_source_block           beh190bcmpd8
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C46.50 H55 B10 Cl N P2 Rh'
_cod_database_code               4109175