Remarkable Behavior of a Bifunctional Alkynylborane Zirconocene Complex toward Donor Ligands and Acetylenes
Santhosh Kumar Podiyanachari; Gerald Kehr; Christian Mück-Lichtenfeld; Constantin G. Daniliuc; Gerhard Erker; Journal of the American Chemical Society 135 (2013) 17444–17456; doi:10.1021/ja408385h

data_4121156
_publ_section_title
;
 Remarkable Behavior of a Bifunctional Alkynylborane Zirconocene Complex
 toward Donor Ligands and Acetylenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17444
_journal_page_last               17456
_journal_paper_doi               10.1021/ja408385h
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C32 H29 B F10 Si2 Zr'
_chemical_formula_weight         761.76
_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                98.0840(10)
_cell_angle_beta                 104.5610(10)
_cell_angle_gamma                94.600(2)
_cell_formula_units_Z            4
_cell_length_a                   11.1086(3)
_cell_length_b                   16.2478(4)
_cell_length_c                   21.5154(6)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     3694.09(17)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34403
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    0.433
_exptl_absorpt_correction_T_max  0.9829
_exptl_absorpt_correction_T_min  0.9108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         12699
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0731P)^2^+8.5691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1736
_reflns_number_gt                9801
_reflns_number_total             12699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408385h_si_002_07.cif
_cod_data_source_block           erk6870
_cod_database_code               4121156