Oxidative Coupling of Silylated Nonagermanide Clusters
Wallach, Chistoph; Klein, Wilhelm; Fässler, Thomas F; Chemical Communications  (2022) –; doi:10.1039/D2CC01250B

data_7129918
_publ_section_title
;
 Oxidative Coupling of Silylated Nonagermanide Clusters
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC01250B
_journal_year                    2022
_chemical_formula_moiety         'C54 H140 Cu2 Ge18 N4 Si16'
_chemical_formula_sum            'C54 H140 Cu2 Ge18 N4 Si16'
_chemical_formula_weight         2728.83
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.416(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6540(4)
_cell_length_b                   27.2393(8)
_cell_length_c                   27.6288(6)
_cell_measurement_reflns_used    186016
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.15
_cell_measurement_theta_min      2.31
_cell_volume                     12191.6(5)
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_collection       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
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_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            122568
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.768
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.887
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       block
_exptl_crystal_F_000             5400
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         11984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0254P)^2^+42.8875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                9236
_reflns_number_total             11984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc01250b2.cif
_cod_data_source_block           CW-633
_cod_original_sg_symbol_H-M      'I 2/c'
_cod_database_code               7129918
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              62753
_shelx_hkl_checksum              5097
_shelx_fab_checksum              44130