An Anionic Heterosiliconoid with two Germanium Vertices
Klemmer, Lukas; Huch, Volker; Jana, Anukul; Scheschkewitz, David; Chemical Communications  (2019) –; doi:10.1039/C9CC04576G

data_7123905
_publ_section_title
;
 An Anionic Heterosiliconoid with two Germanium Vertices
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04576G
_journal_year                    2019
_chemical_formula_moiety         'C75 H115 Ge2 Si4, C12 H30 O6 Li, C6 H14'
_chemical_formula_sum            'C93 H159 Ge2 Li O6 Si4'
_chemical_formula_weight         1637.67
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-06-05 deposited with the CCDC.    2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.728(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0399(10)
_cell_length_b                   33.650(3)
_cell_length_c                   19.5422(14)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    142(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      2.36
_cell_volume                     9656.1(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      142(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            88152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.235
_diffrn_reflns_theta_min         1.210
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.354
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.753
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1060
_refine_ls_number_reflns         21451
_refine_ls_number_restraints     286
_refine_ls_restrained_S_all      1.284
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0732P)^2^+11.7680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15949
_reflns_number_total             21451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04576g2.cif
_cod_data_source_block           sh3772
_cod_original_cell_volume        9656.1(12)
_cod_database_code               7123905
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.762
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              23951