Microwave-Assisted Kumada-Type Cross-Coupling Reactions of Iodinated Carba-closo-dodecaborate Anions
Alexander Himmelspach; Guido J. Reiß; Maik Finze; Inorganic Chemistry 51 (2012) 2679–2688; doi:10.1021/ic202638k

data_4328453
_publ_contact_author_address
;    Institut f\"ur Anorganische Chemie
     Julius-Maximilians-Universit\"at W\"urzburg
     Am Hubland
     D-97074 W\"urzburg
     Germany
;
_publ_contact_author_email       maik.finze@uni-wuerzburg.de
_publ_contact_author_fax         '049 931 31 85857'
_publ_contact_author_name        'Maik Finze'
_publ_contact_author_phone       '049 931 31 84605'
_publ_section_title
;
 Microwave-Assisted Kumada-Type Cross-Coupling Reactions of Iodinated
 Carba-closo-dodecaborate Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2679
_journal_page_last               2688
_journal_paper_doi               10.1021/ic202638k
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C6 H16 B11, C8 H20 N'
_chemical_formula_sum            'C14 H36 B11 N'
_chemical_formula_weight         337.35
_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                   10.7180(7)
_cell_length_b                   16.8947(9)
_cell_length_c                   24.9893(14)
_cell_measurement_reflns_used    7970
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      32.2591
_cell_measurement_theta_min      3.4295
_cell_volume                     4525.0(5)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\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  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19119
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         5.11
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.049
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.990
_exptl_crystal_description       isometric
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.026
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         3942
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0100P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                2812
_reflns_number_total             3942
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202638k_si_001_1.cif
_cod_data_source_block           et4n_h2cmecccb11h11
_cod_database_code               4328453