A series of new vanadium(iii) chalcogenido-antimonates: an unusual seven-coordinate nitro-selenidovanadium(iii) complex.
Luo, Hai-Ying; Zhou, Jian; Zou, Hua-Hong; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3090–3097; doi:10.1039/c9dt00268e

data_7048928
_publ_section_title
;
 A series of new vanadium(iii) chalcogenido-antimonates: an unusual
 seven-coordinate nitro-selenidovanadium(iii) complex.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3090
_journal_page_last               3097
_journal_paper_doi               10.1039/c9dt00268e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C6 H20 N4 S3 Sb V'
_chemical_formula_sum            'C6 H20 N4 S3 Sb V'
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_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-02-05 deposited with the CCDC.
2019-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.500(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
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_cell_length_b                   17.708(9)
_cell_length_c                   13.526(7)
_cell_measurement_reflns_used    9708
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.13
_cell_measurement_theta_min      2.79
_cell_volume                     1469.1(14)
_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  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            46736
_diffrn_reflns_theta_full        29.26
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    2.879
_exptl_absorpt_correction_T_max  0.8694
_exptl_absorpt_correction_T_min  0.7424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.11
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_refine_ls_extinction_coef       0.0042(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         3977
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                3449
_reflns_number_total             3977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9dt00268e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7048928--7048931.cif.'
_cod_original_cell_volume        1469.1(13)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7048928