Cluster expansion and vertex substitution pathways in nickel germanide Zintl clusters
Townrow, Oliver P. E.; Weller, Andrew S.; Goicoechea, Jose M.; Chemical Communications  (2021) –; doi:10.1039/D1CC02912F

data_7128545
_publ_section_title
;
 Cluster expansion and vertex substitution pathways in nickel germanide
 Zintl clusters
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC02912F
_journal_year                    2021
_chemical_formula_moiety
'C54 H162 Ge18 Ni Si24, 2(C18 H36 K N2 O6), 2(C4 H8 O)'
_chemical_formula_sum            'C98 H250 Ge18 K2 N4 Ni O14 Si24'
_chemical_formula_weight         3826.69
_chemical_name_systematic
;
 [K(2,2,2-crypt)]2Ni[Ge9{Si(SiMe3)}3]2*2THF
;
_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   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-06-22 deposited with the CCDC.	2021-06-22 downloaded from the CCDC.
;
_cell_angle_alpha                85.101(2)
_cell_angle_beta                 69.035(2)
_cell_angle_gamma                82.861(2)
_cell_formula_units_Z            1
_cell_length_a                   15.6461(3)
_cell_length_b                   16.2709(4)
_cell_length_c                   18.7924(3)
_cell_measurement_reflns_used    24710
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.9880
_cell_measurement_theta_min      3.6040
_cell_volume                     4428.42(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.81a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55057
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.197
_diffrn_reflns_theta_min         3.196
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.81a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         18293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0345P)^2^+1.6066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15053
_reflns_number_total             18293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02912f2.cif
_cod_data_source_block           OT422_2
_cod_original_cell_volume        4428.43(17)
_cod_database_code               7128545
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.422
_shelx_estimated_absorpt_t_max   0.655
_shelx_res_checksum              40259