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_7708340
_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         '3(C18 H36 K N2 O6), Co Ge10, 9(H3 N)'
_chemical_formula_sum            'C54 H135 Co Ge10 K3 N15 O18'
_chemical_formula_weight         2184.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                72.851(9)
_cell_angle_beta                 89.887(9)
_cell_angle_gamma                70.505(9)
_cell_formula_units_Z            2
_cell_length_a                   12.4142(14)
_cell_length_b                   16.1395(17)
_cell_length_c                   25.212(3)
_cell_measurement_reflns_used    6696
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.07
_cell_measurement_theta_min      1.55
_cell_volume                     4524.0(10)
_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                 STOE
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.746
_diffrn_measured_fraction_theta_max 0.739
_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  0.0965
_diffrn_reflns_av_unetI/netI     0.1500
_diffrn_reflns_Laue_measured_fraction_full 0.746
_diffrn_reflns_Laue_measured_fraction_max 0.739
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15796
_diffrn_reflns_point_group_measured_fraction_full 0.746
_diffrn_reflns_point_group_measured_fraction_max 0.739
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.818
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.649
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.651
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     910
_refine_ls_number_reflns         13148
_refine_ls_number_restraints     104
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.0757
_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^)+(0.1083P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1682
_refine_ls_wR_factor_ref         0.2110
_reflns_number_gt                6137
_reflns_number_total             13148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03078g2.cif
_cod_data_source_block           BW-514-3
_cod_original_cell_volume        4524.1(9)
_cod_database_code               7708340
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              68073