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_4077844
_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_moiety         'C32 H46 B9 Co2 F7 O'
_chemical_formula_sum            'C32 H46 B9 Co2 F7 O'
_chemical_formula_weight         794.84
_chemical_name_common            2010src0133
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.8521(5)
_cell_length_b                   16.2817(6)
_cell_length_c                   33.9667(12)
_cell_measurement_reflns_used    87261
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     7107.7(5)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2006)'
_computing_publication_material  'SHELXTL (Bruker, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniost'
_diffrn_measurement_method       '\f & \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  0.1167
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            39726
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.9901
_exptl_absorpt_correction_T_min  0.8647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.422
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6737
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.445
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1601
_reflns_number_gt                4792
_reflns_number_total             6737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200691z_si_001.cif
_cod_data_source_block           Compound_4
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4077844