[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_7116585
_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 O6 N2 K), Ge8 As4 V, 2(C7 H8), C2 H8 N2
;
_chemical_formula_sum            'C70 H132 As4 Ge8 K3 N8 O18 V'
_chemical_formula_weight         2422.47
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-11-24 deposited with the CCDC.
2015-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                80.709(6)
_cell_angle_beta                 88.755(5)
_cell_angle_gamma                69.258(5)
_cell_formula_units_Z            2
_cell_length_a                   11.9985(7)
_cell_length_b                   16.7415(11)
_cell_length_c                   25.3291(18)
_cell_measurement_reflns_used    12356
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      1.32
_cell_volume                     4692.3(6)
_computing_cell_refinement       'XAREA 1.66 (Stoe 2013)'
_computing_data_collection       'XAREA 1.66 (Stoe 2013)'
_computing_data_reduction        'XAREA 1.66 (Stoe 2013)'
_computing_molecular_graphics    'DIAMOND 3.2i (Brandenburg 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.7
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.995
_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  0.1089
_diffrn_reflns_av_unetI/netI     0.2813
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41618
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         2.545
_exptl_absorpt_coefficient_mu    4.215
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.262
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Coppens et al. (1965)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.687
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         16426
_refine_ls_number_restraints     579
_refine_ls_restrained_S_all      0.720
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4761
_reflns_number_total             16426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc10086g2.cif
_cod_data_source_block           shelx
_cod_database_code               7116585
_shelxl_version_number           2013-4