Synthesis and Structure of (4,4'-H2bpy)[V2(HPO4)4(4,4'-bpy)2], a Novel Two-Dimensional Network Compound
Ching-Hui Huang; Li-Hsun Huang; Kwang-Hwa Lii; Inorganic Chemistry 40 (2001) 2625–2627; doi:10.1021/ic001169g

data_4319674
_publ_contact_author
;
Kwang-Hwa Lii,
Department of Chemistry,
National Central University,
Chungli, Taiwan 320
;
_publ_contact_author_email       liikh@cc.ncu.edu.tw
_publ_section_title
;
 Synthesis and Structure of (4,4'-H2bpy)[V2(HPO4)4(4,4'-bpy)2], a Novel
 Two-Dimensional Network Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2625
_journal_page_last               2627
_journal_paper_doi               10.1021/ic001169g
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'hydrothermal synthesis'
_chemical_formula_structural     (4,4'H2bpy)[V2(HPO4)4(4,4'-bpy)2]
_chemical_formula_sum            'C30 H30 N6 O16 P4 V2'
_chemical_formula_weight         956.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           3
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2y'
_symmetry_space_group_name_H-M   'P 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 107.060(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   8.1434(9)
_cell_length_b                   11.4343(12)
_cell_length_c                   10.0905(11)
_cell_measurement_reflns_used    911
_cell_measurement_temperature    296(2)
_cell_volume                     898.22(17)
_computing_molecular_graphics    ATOMS
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Siemens Smart 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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5942
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.938
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       plate
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.35(4)
_refine_ls_extinction_coef       0.0000(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3986
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.111
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_obs          0.0449
_refine_ls_shift/esd_max         -0.575
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.2984P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1096
_refine_ls_wR_factor_obs         0.1034
_reflns_number_observed          3354
_reflns_number_total             3986
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001169g.cif
_cod_data_source_block           mr06m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.2984P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.2984P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        898.2(2)
_cod_database_code               4319674