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_4089457
_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 Ti'
_chemical_formula_weight         834.08
_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
_audit_update_record
;
2013-05-02 # Formatted by publCIF
;
_cell_angle_alpha                84.17(3)
_cell_angle_beta                 85.39(3)
_cell_angle_gamma                66.11(3)
_cell_formula_units_Z            2
_cell_length_a                   11.874(2)
_cell_length_b                   12.293(3)
_cell_length_c                   19.195(4)
_cell_measurement_reflns_used    6461
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.00
_cell_measurement_theta_min      4.389
_cell_volume                     2546.2(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 0.961
_diffrn_measured_fraction_theta_max 0.961
_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  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18203
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.8124
_exptl_absorpt_correction_T_min  0.7059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         10011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+1.3600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1331
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                8274
_reflns_number_total             10011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400215v_si_002.cif
_cod_data_source_block           2_821j
_cod_original_cell_volume        2546.3(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4089457