Structure and Properties of a Novel 3D Straight-Channel Polyoxovanadate and an Unexpected Trimeric Barbiturate Obtained by Hydrothermal Reactions
Wenbin Yang; Canzhong Lu; Quanzheng Zhang; Shumei Chen; Xiaoping Zhan; Jiuhui Liu; Inorganic Chemistry 42 (2003) 7309–7314; doi:10.1021/ic034554p

data_4312418
_publ_contact_author_address
;
     Fujian Institute of Research  
        on the Structure of Matter,
        Chinese Academy of Sciences,
        Fuzhou, Fujian 350002, 
    P.R.China
;
_publ_contact_author_email       czlu@ms.fjirsm.ac.cn
_publ_contact_author_fax         0086-0591-3714946
_publ_contact_author_name        'Dr. Canzhong Lu'
_publ_contact_author_phone       0086-0591-3705794
_publ_section_title
;
 Structure and Properties of a Novel 3D Straight-Channel Polyoxovanadate
 and an Unexpected Trimeric Barbiturate Obtained by Hydrothermal Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7309
_journal_page_last               7314
_journal_paper_doi               10.1021/ic034554p
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C12 H20 N6 Na2 O16'
_chemical_formula_weight         550.32
_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                106.028(2)
_cell_angle_beta                 103.547(2)
_cell_angle_gamma                93.244(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0888(5)
_cell_length_b                   10.5501(7)
_cell_length_c                   13.2798(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1049.95(12)
_computing_cell_refinement       'Simens CCD SAINT'
_computing_data_collection       'Simens SMART CCD'
_computing_data_reduction        'Simens CCD SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Siemens CCD SMART'
_diffrn_measurement_method       omega-scan
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0769
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5424
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.861968
_exptl_absorpt_correction_T_min  0.484943
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         3639
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1318P)^2^+0.5435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1824
_refine_ls_wR_factor_ref         0.2205
_reflns_number_gt                2310
_reflns_number_total             3639
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034554psi20030523_062536.cif
_cod_data_source_block           C12
_cod_database_code               4312418