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_7708339
_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
'2(C18 H36 K N2 O6), 4(K), 15(H3 N), Co2 Ge17'
_chemical_formula_sum            'C36 H117 Co2 Ge17 K6 N19 O12'
_chemical_formula_weight         2594.97
_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'
_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                 110.634(2)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            4
_cell_length_a                   19.6865(6)
_cell_length_b                   32.1696(10)
_cell_length_c                   15.3982(4)
_cell_measurement_reflns_used    28227
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      1.30
_cell_volume                     9126.2(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'
_computing_molecular_graphics    'DIAMOND 3.2k'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1763
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            277912
_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         26.000
_diffrn_reflns_theta_min         2.722
_diffrn_source                   'Genix 3D HF Mo'
_exptl_absorpt_coefficient_mu    6.181
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       block
_exptl_crystal_F_000             5096
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         17914
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0484P)^2^+34.3816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1142
_reflns_number_gt                13812
_reflns_number_total             17914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03078g2.cif
_cod_data_source_block           BW514
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7708339
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              11478