A series of new hybrid chalcogenogermanates: the rare examples of chalcogenogermanates combined with trivalent vanadium complexes.
Luo, Hai-Ying; Zhou, Jian; Cao, Shumei; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10907–10914; doi:10.1039/c9dt02077b

data_7700377
_publ_section_title
;
 A series of new hybrid chalcogenogermanates: the rare examples of
 chalcogenogermanates combined with trivalent vanadium complexes.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10907
_journal_page_last               10914
_journal_paper_doi               10.1039/c9dt02077b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C12 H48 N12 O V2, Ge2 Se6'
_chemical_formula_sum            'C12 H48 Ge2 N12 O Se6 V2'
_chemical_formula_weight         1097.48
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-06-20 deposited with the CCDC.    2019-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                109.090(4)
_cell_angle_beta                 104.169(4)
_cell_angle_gamma                111.520(5)
_cell_formula_units_Z            1
_cell_length_a                   9.4480(12)
_cell_length_b                   10.1780(13)
_cell_length_c                   10.4361(12)
_cell_measurement_reflns_used    2858
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.52
_cell_volume                     802.73(18)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14287
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.554
_diffrn_reflns_theta_min         2.519
_exptl_absorpt_coefficient_mu    9.250
_exptl_absorpt_correction_T_max  0.207
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.271
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0204P)^2^+0.5551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3262
_reflns_number_total             4422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02077b2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7700373--7700378.cif.'
_cod_original_cell_volume        802.73(17)
_cod_database_code               7700377
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.139
_shelx_estimated_absorpt_t_max   0.303
_shelx_res_checksum              54970