Unsaturated amido-substituted six-vertex mixed silicon germanium clusters
Helmer, Joschua; Droste, Jörn; Hansen, Michael Ryan; Hepp, Alexander; Lips, Felicitas; Dalton Transactions  (2022) –; doi:10.1039/D2DT01746F

data_7710638
_publ_section_title
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 Unsaturated amido-substituted six-vertex mixed silicon germanium clusters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01746F
_journal_year                    2022
_chemical_formula_sum            'C60 H104 Ge2.28 N4 Si7.72'
_chemical_formula_weight         1263.60
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
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2021-06-29 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3651(5)
_cell_length_b                   16.3651(5)
_cell_length_c                   27.0314(9)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.32
_cell_volume                     7239.5(4)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0372
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            91036
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.169
_diffrn_reflns_theta_min         2.317
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       rod
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.584
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.176
_exptl_transmission_factor_min   2.32
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0175
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.9569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0493
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                7813
_reflns_number_total             8000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01746f2.cif
_cod_data_source_block           fl180217sq
_cod_original_cell_volume        7239.5(5)
_cod_database_code               7710638
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              82581
_shelx_hkl_checksum              39866
_shelx_fab_checksum              91016