Tantallacarborane Mediated Consecutive C‒C and C‒N Coupling Reactions of Alkyl Isonitriles: A Facile Route to N-Heterocycles
Xiang, Li; Xie, Zuowei; Organometallics 35 (2016) 233–; doi:10.1021/acs.organomet.5b00953

data_4088241
_publ_section_title
;
 Tantallacarborane Mediated Consecutive C--C and C--N Coupling Reactions
 of Alkyl Isonitriles: A Facile Route to N-Heterocycles
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              233
_journal_paper_doi               10.1021/acs.organomet.5b00953
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C36 H70 B9 N4 O Ta'
_chemical_formula_weight         853.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 95.392(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.8636(10)
_cell_length_b                   15.6146(16)
_cell_length_c                   24.205(3)
_cell_measurement_reflns_used    262
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     4087.7(8)
_computing_cell_refinement       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_collection       'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_data_reduction        'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_diffrn_measurement_method       'Phi & Omgea scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_av_unetI/netI     0.1036
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32021
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         1.554
_exptl_absorpt_coefficient_mu    2.723
_exptl_absorpt_correction_T_max  0.6396
_exptl_absorpt_correction_T_min  0.5365
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.851
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1419
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5887
_reflns_number_total             7391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00953_si_002.cif
_cod_data_source_block           9
_cod_original_cell_volume        4087.7(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088241
_shelx_estimated_absorpt_t_min   0.409
_shelx_estimated_absorpt_t_max   0.612
_shelxl_version_number           2014/6
_shelx_res_checksum              70607
_shelx_hkl_checksum              18215