Coordination Chemistry of Disilylated Germylenes with Group 4 Metallocenes.
Hlina, Johann; Baumgartner, Judith; Marschner, Christoph; Zark, Patrick; Müller, Thomas; Organometallics 32 (2013) 3300–3308; doi:10.1021/om400215v

data_4089458
_publ_section_title
;
 Coordination Chemistry of Disilylated Germylenes with Group 4
 Metallocenes.
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3300
_journal_page_last               3308
_journal_paper_doi               10.1021/om400215v
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C32 H73 Ge P Si8 Zr'
_chemical_formula_weight         877.40
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                83.87(3)
_cell_angle_beta                 84.48(3)
_cell_angle_gamma                65.90(3)
_cell_formula_units_Z            2
_cell_length_a                   11.914(2)
_cell_length_b                   12.350(3)
_cell_length_c                   19.437(4)
_cell_measurement_reflns_used    5084
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.459
_cell_measurement_theta_min      4.377
_cell_volume                     2591.3(11)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.1039
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18625
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.8075
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.259
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         9038
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+6.9433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1738
_refine_ls_wR_factor_ref         0.1842
_reflns_number_gt                7009
_reflns_number_total             9038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400215v_si_002.cif
_cod_data_source_block           3_822j
_cod_original_cell_volume        2591.4(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089458