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_4328456
_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         'C19 H26 B11 P'
_chemical_formula_sum            'C19 H26 B11 P'
_chemical_formula_weight         404.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                85.88(3)
_cell_angle_beta                 86.36(3)
_cell_angle_gamma                75.45(3)
_cell_formula_units_Z            2
_cell_length_a                   7.979(3)
_cell_length_b                   10.106(4)
_cell_length_c                   14.852(6)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      21.50
_cell_measurement_theta_min      3.40
_cell_volume                     1154.9(8)
_computing_cell_refinement       'CrysAlis RED (Kuma Diffraction, 2000)'
_computing_data_collection       'CrysAlis CCD (Kuma Diffraction, 2000)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'Diamond3.1 (Crystal Impact GbR, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe STADI CCD'
_diffrn_measurement_method       \f-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  0.0698
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15883
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0546
_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^)+(0.0283P)^2^+1.3728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                3558
_reflns_number_total             4048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202638k_si_001_4.cif
_cod_data_source_block           ph3pcb11h11
_cod_database_code               4328456