Redetermination of poly[hexa-μ~2~-oxo-tetraoxobis(1,10-phenanthroline)tetravanadium(V)]
Li, Tao-Hai; Cao, Rong; Acta Crystallographica Section E 62 (2006) m3236–m3237; doi:10.1107/S1600536806045867

data_2211537
_publ_section_title
;
 Redetermination of
 poly[hexa-\m~2~-oxo-tetraoxobis(1,10-phenanthroline)tetravanadium(V)]
;
_journal_coeditor_code           NG2140
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m3236
_journal_page_last               m3237
_journal_paper_doi               10.1107/S1600536806045867
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[V4 O10 (C12 H8 N2)2]'
_chemical_formula_moiety         'C24 H16 N4 O10 V4'
_chemical_formula_sum            'C24 H16 N4 O10 V4'
_chemical_formula_weight         724.16
_chemical_name_systematic
;
poly[hexa-\m~2~-oxo-tetraoxobis(1,10-phenanthroline)tetravanadium(V)]
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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                 100.650(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8024(7)
_cell_length_b                   6.5184(4)
_cell_length_c                   19.8144(13)
_cell_measurement_reflns_used    3073
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      2.0908
_cell_volume                     1244.25(14)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2001)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'SHELXTL (Siemens, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_method       '\f? \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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9785
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.525
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.720
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(XEMP in SHELXTL; Siemens, 1994)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2200
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1500
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.402
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         3094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0429P)^2^+0.7806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0810
_reflns_number_gt                2772
_reflns_number_total             3094
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2140.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2211537
_cod_database_fobs_code          2211537