Group 4 Metallocene Complexes of Tris(trimethylsilyl)silylacetylene and Related Alkynes
Zirngast, Michaela; Marschner, Christoph; Baumgartner, Judith; Organometallics 27 (2008) 2570–; doi:10.1021/om800038h

data_4071221
_publ_section_title
;
 Group 4 Metallocene Complexes of Tris(trimethylsilyl)silylacetylene and
 Related Alkynes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2570
_journal_paper_doi               10.1021/om800038h
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C32 H64 Si8 Zr'
_chemical_formula_weight         764.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           40
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2a'
_symmetry_space_group_name_H-M   'A m a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.738(6)
_cell_length_b                   16.791(6)
_cell_length_c                   9.5167(19)
_cell_measurement_reflns_used    2134
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     4592(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SMART APEX'
_diffrn_measurement_method       '\w scans'
_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  0.1565
_diffrn_reflns_av_sigmaI/netI    0.1137
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13467
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_T_max  0.9207
_exptl_absorpt_correction_T_min  0.8500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.129
_refine_diff_density_min         -1.960
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3271
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.1347
_refine_ls_shift/su_max          0.639
_refine_ls_shift/su_mean         0.034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+165.7207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2873
_refine_ls_wR_factor_ref         0.2927
_reflns_number_gt                2905
_reflns_number_total             3271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800038h-file001.cif
_cod_data_source_block           26_546j
_cod_original_sg_symbol_H-M      Ama2
_cod_database_code               4071221