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_4317398
_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            'C16 H10.67 N2.67 Ni0.67 O5.67 V2'
_chemical_formula_weight         471.96
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.35(3)
_cell_angle_beta                 72.61(3)
_cell_angle_gamma                76.12(3)
_cell_formula_units_Z            3
_cell_length_a                   10.108(2)
_cell_length_b                   11.168(2)
_cell_length_c                   11.749(2)
_cell_measurement_reflns_used    24679
_cell_measurement_temperature    293(2)
_cell_volume                     1227.3(5)
_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 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24679
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  0.625
_exptl_absorpt_correction_T_min  0.577
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.610
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0502P)^2^+0.9698P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0936
_reflns_number_gt                5971
_reflns_number_total             6784
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010735k_2.cif
_cod_data_source_block           last
_cod_original_cell_volume        1227.2(4)
_cod_database_code               4317398