Three-Component [2+2+1] Cross-cyclotrimerization of Carboryne, Unactivated Alkene, and Trimethylsilylalkyne Co-mediated by Zr and Ni
Yangjian Quan; Jiji Zhang; Zuowei Xie; Journal of the American Chemical Society 135 (2013) 18742–18745; doi:10.1021/ja410233e

data_4121327
_publ_section_title
;
 Three-Component [2+2+1] Cross-cyclotrimerization of Carboryne,
 Unactivated Alkene, and Trimethylsilylalkyne Co-mediated by Zr and Ni
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18742
_journal_page_last               18745
_journal_paper_doi               10.1021/ja410233e
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C17 H34 B10 S Si'
_chemical_formula_weight         406.69
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.428(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8786(17)
_cell_length_b                   8.7325(11)
_cell_length_c                   19.944(3)
_cell_measurement_reflns_used    148
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     2412.8(6)
_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    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'BRUKER KAPPA APEXII DUO DIFFRACTOMETER'
_diffrn_measurement_method       'PHI & OMEGA SCAN'
_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  0.1172
_diffrn_reflns_av_sigmaI/netI    0.1058
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20651
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.6995
_exptl_absorpt_correction_T_min  0.5302
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.652
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.391
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4358
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.436
_refine_ls_R_factor_all          0.1520
_refine_ls_R_factor_gt           0.1196
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3344
_refine_ls_wR_factor_ref         0.3719
_reflns_number_gt                3038
_reflns_number_total             4358
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja410233e_si_001_6.cif
_cod_data_source_block           E-5p
_cod_original_cell_volume        2412.8(5)
_cod_database_code               4121327