Hydrothermal synthesis, structure and characterization of a novel layered vanadium oxide with metal coordination complexes: [Ni(en)2][V6O14]
Bi-Zhou Lin; Shi-Xiong Liu; J. Chem. Soc., Dalton Trans.  (2002) 865–869; doi:10.1039/b105934n

data_7010961
_publ_section_title
;
 Hydrothermal synthesis, structure and characterization of a novel
 layered vanadium oxide with metal coordination complexes:
 [Ni(en)2][V6O14]
;
_journal_issue                   6
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              865
_journal_page_last               869
_journal_paper_doi               10.1039/b105934n
_journal_year                    2002
_chemical_compound_source        synthesis
_chemical_formula_moiety         'Ni C4 H16 N4 V6 O14 '
_chemical_formula_sum            'C4 H16 N4 Ni O14 V6'
_chemical_formula_weight         708.56
_chemical_name_systematic
; 
[bis-ethylenediamine nickel(II)] hexavanadate(V) 
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.597(3)
_cell_length_b                   6.6200(10)
_cell_length_c                   17.117(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1880.7(6)
_computing_cell_refinement
;
RIGAKU/AFC (Molecuar Structure Corporation, 1987a)
;
_computing_data_collection
;
RIGAKU/AFC (Molecuar Structure Corporation, 1987a)
;
_computing_data_reduction
;
TEXRAY (Molecuar Structure Corporation, 1987b)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  RIGAKU--AFC5R
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_sigmaI/netI    0.1017
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1060
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.38
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.905
_exptl_absorpt_correction_T_max  0.8287
_exptl_absorpt_correction_T_min  0.1957
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, phillips & Mathews, 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.00002(14)
_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_ref   1.024
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0212P)^2^+51.3841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                650
_reflns_number_total             956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b105934n.txt
_cod_data_source_block           (I)
_cod_depositor_comments
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The following automatic conversions were performed:
data name '_geom_hbond_atom_label_d' replaced with
'_geom_hbond_atom_site_label_D' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_hbond_atom_label_h' replaced with
'_geom_hbond_atom_site_label_H' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_hbond_atom_label_a' replaced with
'_geom_hbond_atom_site_label_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
;
_cod_original_sg_symbol_H-M      'C mca'
_cod_database_code               7010961