Synthesis of vinyl germylenes
Malgorzata Walewska; Judith Baumgartner; Christoph Marschner; Chem.Commun. 51 (2015) 276–; doi:10.1039/C4CC07675C

data_7116358
_publ_section_title
;
 Synthesis of vinyl germylenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              276
_journal_paper_doi               10.1039/C4CC07675C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C29 H74 Ge N2 Si8'
_chemical_formula_weight         748.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.081(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.106(3)
_cell_length_b                   23.293(5)
_cell_length_c                   16.666(4)
_cell_measurement_reflns_used    10667
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.246
_cell_measurement_theta_min      4.904
_cell_volume                     4577.6(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0533
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36156
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.8771
_exptl_absorpt_correction_T_min  0.7559
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         9341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                7432
_reflns_number_total             9341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc07675c2.cif
_cod_data_source_block           973j
_cod_original_cell_volume        4577.9(18)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7116358