Facile Isomerization and Unprecedented Decarbonation of Metallacarboranes with Fluorinated Aryl Substituents
Ward, Jas S.; Tricas, Hugo; Scott, Greig; Ellis, David; Rosair, Georgina M.; Welch, Alan J.; Organometallics 31 (2012) 2523–; doi:10.1021/om200691z

data_4077843
_publ_section_title
;
 Facile Isomerization and Unprecedented Decarbonation of Metallacarboranes
 with Fluorinated Aryl Substituents
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2523
_journal_paper_doi               10.1021/om200691z
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C36 H40 B10 F12'
_chemical_formula_weight         808.78
_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                70.015(4)
_cell_angle_beta                 79.973(4)
_cell_angle_gamma                89.535(4)
_cell_formula_units_Z            4
_cell_length_a                   14.5973(13)
_cell_length_b                   16.0164(14)
_cell_length_c                   18.3603(16)
_cell_measurement_reflns_used    923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.73
_cell_measurement_theta_min      2.14
_cell_volume                     3966.3(6)
_computing_cell_refinement       'APEX2 (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'APEX2 (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            69711
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9561
_exptl_absorpt_correction_T_min  0.9229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Bruker, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.68
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1125
_refine_ls_number_reflns         18020
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0835
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+13.1808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2115
_refine_ls_wR_factor_ref         0.2268
_reflns_number_gt                14072
_reflns_number_total             18020
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200691z_si_001.cif
_cod_data_source_block           Compound_2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077843