[V@Ge8As4]^3-^ and [Nb@Ge8As6]^3-^: encapsulation of electron-poor transition metal atoms
Stefan Mitzinger; Lies Broeckaert; Werner Massa; Florian Weigend; Stefanie Dehnen; Chem.Commun. 51 (2015) 3866–; doi:10.1039/C4cc10086G

data_7116586
_publ_section_title
;
 [V@Ge8As4]^3-^ and [Nb@Ge8As6]^3-^: encapsulation of electron-poor
 transition metal atoms
;
_journal_name_full               Chem.Commun.
_journal_page_first              3866
_journal_paper_doi               10.1039/C4cc10086G
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
;
3(C18 H36 N2 O6 K), As6 Ge8 Nb, C7 H8, C2 H8 N2
;
_chemical_formula_sum            'C63 H124 As6 Ge8 K3 N8 Nb O18'
_chemical_formula_weight         2522.14
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-12-03 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                89.184(3)
_cell_angle_beta                 80.452(3)
_cell_angle_gamma                79.420(3)
_cell_formula_units_Z            2
_cell_length_a                   16.1475(7)
_cell_length_b                   16.7769(6)
_cell_length_c                   18.0373(8)
_cell_measurement_reflns_used    26279
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.74
_cell_measurement_theta_min      1.235
_cell_volume                     4736.1(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.7
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'IPDS2 (Stoe)'
_diffrn_measurement_method       omega-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.1575
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       -22
_diffrn_reflns_number            66699
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.013
_exptl_absorpt_coefficient_mu    4.889
_exptl_absorpt_correction_T_max  0.127
_exptl_absorpt_correction_T_min  0.066
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Coppens et al. (1965)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.633
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         18581
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.633
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8558
_reflns_number_total             18581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc10086g2.cif
_cod_data_source_block           shelx_1
_cod_database_code               7116586
_shelxl_version_number           2013-4