Group 4 Metallocene Complexes of Disilenes, Digermenes, and a Silagermene
Michaela Zirngast; Michaela Flock; Judith Baumgartner; Christoph Marschner; Journal of the American Chemical Society 131 (2009) 15952–15962; doi:10.1021/ja905654r

data_4105240
_publ_section_title
;
 Group 4 Metallocene Complexes of Disilenes, Digermenes, and a Silagermene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15952
_journal_page_last               15962
_journal_paper_doi               10.1021/ja905654r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C28 H64 Si6 Sn3 Zr'
_chemical_formula_weight         1016.62
_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                87.04(3)
_cell_angle_beta                 87.75(3)
_cell_angle_gamma                76.30(3)
_cell_formula_units_Z            2
_cell_length_a                   10.916(2)
_cell_length_b                   11.849(2)
_cell_length_c                   17.496(3)
_cell_measurement_reflns_used    2691
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.024
_cell_measurement_theta_min      4.426
_cell_volume                     2194.8(7)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14513
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_T_max  0.6012
_exptl_absorpt_correction_T_min  0.4588
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.253
_refine_diff_density_min         -2.040
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6849
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0885
_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^)+(0.0326P)^2^+26.9075P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                5160
_reflns_number_total             6849
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905654r_si_002_7.cif
_cod_data_source_block           467j_14
_cod_database_code               4105240