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_4105242
_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            'C24 H72 Ge4 Si8'
_chemical_formula_weight         875.90
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 117.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.289(4)
_cell_length_b                   12.751(3)
_cell_length_c                   10.290(2)
_cell_measurement_reflns_used    1915
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.684
_cell_measurement_theta_min      4.764
_cell_volume                     2240.0(10)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0878
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8886
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.886
_exptl_absorpt_correction_T_max  0.5566
_exptl_absorpt_correction_T_min  0.3770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       blocks
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.22(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2397
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0631
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0514P)^2^+10.8536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1235
_reflns_number_gt                2056
_reflns_number_total             2397
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905654r_si_002_9.cif
_cod_data_source_block           265j_18
_cod_original_cell_volume        2239.8(8)
_cod_database_code               4105242