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_4105237
_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            'C32 H63 Ge2 Hf P Si4'
_chemical_formula_weight         914.82
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 110.94(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.908(3)
_cell_length_b                   10.926(2)
_cell_length_c                   23.415(5)
_cell_measurement_reflns_used    7977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.508
_cell_measurement_theta_min      4.527
_cell_volume                     4039.9(16)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31022
_diffrn_reflns_theta_full        26.35
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_T_max  0.4308
_exptl_absorpt_correction_T_min  0.2831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         3.247
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         8201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+3.8278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                6932
_reflns_number_total             8201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905654r_si_002_4.cif
_cod_data_source_block           431j_9
_cod_original_cell_volume        4039.9(14)
_cod_database_code               4105237