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_4121326
_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            'C19 H30 B10 F5 Si'
_chemical_formula_weight         489.62
_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                94.947(5)
_cell_angle_beta                 91.027(5)
_cell_angle_gamma                110.034(5)
_cell_formula_units_Z            2
_cell_length_a                   7.698(2)
_cell_length_b                   8.822(3)
_cell_length_c                   20.149(6)
_cell_measurement_reflns_used    95
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      15
_cell_volume                     1279.1(7)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.1124
_diffrn_reflns_av_sigmaI/netI    0.1322
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13123
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.136
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4422
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4573
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.1064
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1975P)^2^+0.7142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2721
_refine_ls_wR_factor_ref         0.3204
_reflns_number_gt                2889
_reflns_number_total             4573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja410233e_si_001_5.cif
_cod_data_source_block           E-5l
_cod_original_cell_volume        1279.1(6)
_cod_database_code               4121326