Hexakis(2-amino-4-methylpyridine-κ<i>N</i>^1^)dioxidohexa-μ~4~-sulfido-hexacopper(I)divanadium(V)
Yu, Zhang; Tang, Guodong; Zhao, Jianying; Jiang, Zhengjing; Acta Crystallographica Section E 64 (2008) m1217–; doi:10.1107/S1600536808027165

data_2219274
_publ_section_title
Hexakis(2-amino-4-methylpyridine-\k<i>N</i>^1^)dioxidohexa-\m~4~-sulfido-hexacopper(I)divanadium(V)
_journal_coeditor_code           BV2103
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1217
_journal_paper_doi               10.1107/S1600536808027165
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu6 V2 O2 S6 (C6 H8 N2)6]'
_chemical_formula_moiety         'C36 H48 Cu6 N12 O2 S6 V2'
_chemical_formula_sum            'C36 H48 Cu6 N12 O2 S6 V2'
_chemical_formula_weight         1356.34
_chemical_name_systematic
;
Hexakis(2-amino-4-methylpyridine-\kN^1^)dioxidohexa-\m~4~-sulfido-\
hexacopper(I)divanadium(V)
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.139(2)
_cell_length_b                   14.139(2)
_cell_length_c                   20.830(4)
_cell_measurement_reflns_used    6634
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.93
_cell_volume                     3606.3(10)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6168
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  5
_diffrn_standards_number         28
_exptl_absorpt_coefficient_mu    3.279
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.694
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                1092
_reflns_number_total             1837
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bv2103.cif
_cod_data_source_block           I
_cod_original_cell_volume        3606.2(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2219274
_cod_database_fobs_code          2219274