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_4105239
_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 Hf Si6 Sn3'
_chemical_formula_weight         1103.89
_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                86.81(3)
_cell_angle_beta                 87.77(3)
_cell_angle_gamma                75.29(3)
_cell_formula_units_Z            2
_cell_length_a                   10.982(2)
_cell_length_b                   11.835(2)
_cell_length_c                   17.500(4)
_cell_measurement_reflns_used    10649
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.515
_cell_measurement_theta_min      4.431
_cell_volume                     2195.8(8)
_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 0.853
_diffrn_measured_fraction_theta_max 0.853
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12276
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    4.222
_exptl_absorpt_correction_T_max  0.5170
_exptl_absorpt_correction_T_min  0.3640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       plates
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.267
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6576
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0701
_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^)+(0.1416P)^2^+39.5008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2332
_reflns_number_gt                5969
_reflns_number_total             6576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905654r_si_002_6.cif
_cod_data_source_block           444j_13
_cod_original_cell_volume        2195.7(8)
_cod_database_code               4105239