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_4307218
_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         'C12 H19 B9 N O3 Re'
_chemical_formula_sum            'C12 H19 B9 N O3 Re'
_chemical_formula_weight         508.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.328(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4000(2)
_cell_length_b                   15.4930(4)
_cell_length_c                   15.3055(4)
_cell_measurement_reflns_used    5348
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      2.63
_cell_volume                     1753.30(8)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            25094
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    6.942
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00235(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0477
_refine_ls_wR_factor_ref         0.0514
_reflns_number_gt                4210
_reflns_number_total             5302
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0617543si20060915_122600_2.cif
_cod_data_source_block           compound12
_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               4307218