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_4121155
_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            'C37.5 H31 B F10 Si Zr'
_chemical_formula_weight         801.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.9410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.58050(10)
_cell_length_b                   31.8728(4)
_cell_length_c                   21.7498(3)
_cell_measurement_reflns_used    17020
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     7148.40(15)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.072
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            82752
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.11
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  0.9875
_exptl_absorpt_correction_T_min  0.8951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       plate
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         12520
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0227P)^2^+10.0612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                9697
_reflns_number_total             12520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja408385h_si_002_06.cif
_cod_data_source_block           erk6871
_cod_original_formula_sum        'C37.50 H31 B F10 Si Zr'
_cod_database_code               4121155