Subvalent mixed SixGey oligomers: (Cl3Si)4Ge and Cl2(Me2EtN)SiGe(SiCl3)2
Kunkel, Chantal; Bolte, Michael; Lerner, Hans-Wolfram; Albert, Philipp; Wagner, Matthias; Chemical Communications  (2021) –; doi:10.1039/D1CC05604B

data_7129162
_publ_section_title
;
 Subvalent mixed SixGey oligomers: (Cl3Si)4Ge and Cl2(Me2EtN)SiGe(SiCl3)2
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05604B
_journal_year                    2021
_chemical_formula_moiety         'C5 H13 Cl N, Cl'
_chemical_formula_sum            'C5 H13 Cl2 N'
_chemical_formula_weight         158.06
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2021-08-24 deposited with the CCDC.	2021-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   18.134(2)
_cell_length_b                   18.134(2)
_cell_length_c                   13.1827(13)
_cell_measurement_reflns_used    2906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.69
_cell_measurement_theta_min      3.38
_cell_volume                     3754.2(7)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2906
_diffrn_reflns_point_group_measured_fraction_full 0.922
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.312
_diffrn_reflns_theta_min         3.765
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.165
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
; 
 Flack x determined using 607 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.13(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1549
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0437P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.830
_reflns_number_gt                1455
_reflns_number_total             1549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05604b2.cif
_cod_data_source_block           wa2606
_cod_original_cell_volume        3754.2(9)
_cod_database_code               7129162
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.724
_shelx_estimated_absorpt_t_max   0.846
_shelx_res_checksum              90097
_shelx_hkl_checksum              80594