Hydrothermal Synthesis and Crystal Structure of a Novel Two-Dimensional Vanadium Oxide Complex with a 6,14-Net Sinusoidal Ruffling Anionic Layer: [Ni(phen)2V4O11] (phen = 1,10-Phenanthroline)
Cai-Ming Liu; Yang-Long Hou; Jing Zhang; Song Gao; Inorganic Chemistry 41 (2002) 140–143; doi:10.1021/ic010735k

data_4317397
_publ_section_title
;
 Hydrothermal Synthesis and Crystal Structure of a Novel Two-Dimensional
 Vanadium Oxide Complex with a 6,14-Net Sinusoidal Ruffling Anionic Layer:
 [Ni(phen)2V4O11] (phen = 1,10-Phenanthroline)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              140
_journal_page_last               143
_journal_paper_doi               10.1021/ic010735k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C24 H15 N4 Ni O11 V4'
_chemical_formula_weight         797.87
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 95.2600(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6518(2)
_cell_length_b                   18.4585(4)
_cell_length_c                   17.7056(4)
_cell_measurement_reflns_used    50360
_cell_measurement_temperature    293(2)
_cell_volume                     3141.11(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49487
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    1.794
_exptl_absorpt_correction_T_max  0.739
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7899
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0470P)^2^+2.4828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                6435
_reflns_number_total             7899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010735k_1.cif
_cod_data_source_block           last
_cod_database_code               4317397