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_4089459
_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 Hf P Si8'
_chemical_formula_weight         964.67
_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                83.91(3)
_cell_angle_beta                 84.47(3)
_cell_angle_gamma                65.88(3)
_cell_formula_units_Z            2
_cell_length_a                   11.885(2)
_cell_length_b                   12.335(3)
_cell_length_c                   19.400(4)
_cell_measurement_reflns_used    4360
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      52.547
_cell_measurement_theta_min      4.756
_cell_volume                     2576.7(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      110(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  0.0684
_diffrn_reflns_av_sigmaI/netI    0.1148
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18449
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    2.832
_exptl_absorpt_correction_T_max  0.5747
_exptl_absorpt_correction_T_min  0.4461
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.571
_refine_diff_density_min         -4.961
_refine_diff_density_rms         0.223
_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         8976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+27.1952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1731
_reflns_number_gt                7347
_reflns_number_total             8976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400215v_si_002.cif
_cod_data_source_block           4_823j
_cod_original_cell_volume        2576.8(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089459