Filled Trivacant Icosahedra as Building Fragments in 17-atomic Endohedral Germanides [TM2@Ge17]n- (TM = Co, Ni)
Wallach, Chistoph; Selic, Yasmin; Witzel, Benedikt; Klein, Wilhelm; Fässler, Thomas F; Dalton Transactions  (2021) –; doi:10.1039/D1DT03078G

data_7708341
_publ_section_title
;
 Filled Trivacant Icosahedra as Building Fragments in 17-atomic Endohedral
 Germanides [TM2@Ge17]n- (TM = Co, Ni)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03078G
_journal_year                    2021
_chemical_formula_moiety         'C2 H8 N2, (C18 H36 N2 O6 K)4, Ni2 Ge17'
_chemical_formula_sum            'C37 H76 Ge8.5 K2 N5 Ni O12'
_chemical_formula_weight         1536.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-04-30 deposited with the CCDC.	2021-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.4600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.8620(5)
_cell_length_b                   16.5170(3)
_cell_length_c                   27.9490(5)
_cell_measurement_reflns_used    198242
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.54
_cell_measurement_theta_min      2.81
_cell_volume                     11412.9(4)
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_collection       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-97
_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 0.998
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0902
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            156231
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.812
_diffrn_source                   'Genix 3D HF Mo'
_exptl_absorpt_coefficient_mu    4.932
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.318
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_description       block
_exptl_crystal_F_000             6136
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.661
_refine_diff_density_min         -3.997
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         11193
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0734
_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^)+(0.0456P)^2^+327.8550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1600
_refine_ls_wR_factor_ref         0.1728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9267
_reflns_number_total             11193
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03078g2.cif
_cod_data_source_block           CW-112_w
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C37 H76 Ge8.50 K2 N5 Ni O12'
_cod_database_code               7708341
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   'STOE X-AREA 1.76'
_shelx_res_checksum              5026