Microwave-Assisted Synthesis of Tricarbonyl Rhenacarboranes: Steric and Electronic Effects on the 1,2 →1,7 Carborane Cage Isomerization
Andrea F. Armstrong; John F. Valliant; Inorganic Chemistry 46 (2007) 2148–2158; doi:10.1021/ic0617543

data_4307217
_publ_contact_author_address
;Departments of Chemistry and Medical Physics &
  Applied Radiation Sciences
  McMaster University
  1280 Main Street West
  Hamilton, ON, Canada, L8S 4M1
;
_publ_contact_author_email       valliant@mcmaster.ca
_publ_contact_author_fax         1-905-522-2509
_publ_contact_author_name        'John F. Valliant'
_publ_contact_author_phone       1-905-525-9140-22840
_publ_section_title
;
Microwave-Assisted Synthesis of Tricarbonyl Rhenacarboranes: Steric and
Electronic Effects on the 1,2 \\rightarrow 1,7 Carborane Cage Isomerization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2148
_journal_page_last               2158
_journal_paper_doi               10.1021/ic0617543
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C9 H20 B10 N, C F3 O3 S'
_chemical_formula_sum            'C10 H20 B10 F3 N O3 S'
_chemical_formula_weight         399.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 95.531(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.8158(6)
_cell_length_b                   10.9599(9)
_cell_length_c                   12.8039(10)
_cell_measurement_reflns_used    3902
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.11
_cell_measurement_theta_min      3.47
_cell_volume                     952.00(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'cross-coupled parallel focusing mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5050
_diffrn_reflns_theta_full        68.11
_diffrn_reflns_theta_max         68.11
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         2754
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0758P)^2^+0.4019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                2667
_reflns_number_total             2754
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0617543si20060915_122600_1.cif
_cod_data_source_block           Compound11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4307217