Designed Synthesis of New ortho-Carborane Derivatives: from Mono- to Polysubstituted Frameworks
Gemma Barberà; Albert Vaca; Francesc Teixidor; Reijo Sillanpää; Raikko Kivekäs; Clara Viñas; Inorganic Chemistry 47 (2008) 7309–7316; doi:10.1021/ic800362z

data_4305382
_publ_contact_author
;
     Prof. Clara Vi\~nas
     Institute of Material Sciences 
     Campus UAB
     E-08193 Bellaterra
     Spain
;
_publ_contact_author_email       clara@icmab.es
_publ_contact_author_fax         '+34 93 5805729'
_publ_contact_author_phone       '+34 93 5801853'
_publ_section_title
;
Designed Synthesis of New ortho-Carborane Derivatives: from Mono- to
Polysubstituted Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7309
_journal_page_last               7316
_journal_paper_doi               10.1021/ic800362z
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C4 H16 B10'
_chemical_formula_sum            'C4 H16 B10'
_chemical_formula_weight         172.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 114.220(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8528(7)
_cell_length_b                   6.8281(3)
_cell_length_c                   11.5332(6)
_cell_measurement_reflns_used    1721
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.91
_cell_volume                     1066.70(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3110
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.046
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0942
_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^)+(0.1857P)^2^+1.3403P] where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2524
_refine_ls_wR_factor_ref         0.2678
_reflns_number_gt                728
_reflns_number_total             934
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800362z-file001_3.cif
_cod_data_source_block           3,6-Me2-1,2-C2B10H10
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4305382