Antimonato polyoxovanadates with structure directing transition metal complexes: pseudopolymorphic {Ni(dien)2}3[V15Sb6O42(H2O)]·nH2O compounds and {Ni(dien)2}4[V16Sb4O42(H2O)].
Antonova, Elena; Näther, Christian; Bensch, Wolfgang; Dalton transactions (Cambridge, England : 2003) 41 (2012) 1338–1344; doi:10.1039/c1dt11635e

data_7017903
_publ_section_title
;
 Antimonato polyoxovanadates with structure directing transition metal
 complexes: pseudopolymorphic {Ni(dien)2}3[V15Sb6O42(H2O)]&#x00B7;nH2O
 compounds and {Ni(dien)2}4[V16Sb4O42(H2O)].
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1338
_journal_page_last               1344
_journal_paper_doi               10.1039/c1dt11635e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'O42 Sb6 V15, 3(Ni C8 H26 N6), 9(H2 O)'
_chemical_formula_sum            'C24 H96 N18 Ni3 O51 Sb6 V15'
_chemical_formula_weight         3123.8087
_chemical_name_common            (Ni(C4N3H13)2)3(V15Sb6O42(H2O))(H2O)8
_chemical_name_systematic
;
(Ni(C4N3H13)2)3(V15Sb6O42(H2O))(H2O)8
;
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_atom_sites_solution_hydrogens   none
_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            16
_cell_length_a                   46.9378(3)
_cell_length_b                   46.9378(3)
_cell_length_c                   16.51300(10)
_cell_measurement_reflns_used    200212
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.1
_cell_measurement_theta_min      1.7
_cell_volume                     36380.7(4)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f scans'
_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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            200212
_diffrn_reflns_theta_full        19.54
_diffrn_reflns_theta_max         19.54
_diffrn_reflns_theta_min         0.87
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_T_max  0.7064
_exptl_absorpt_correction_T_min  0.3990
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             22704
_exptl_crystal_size_max          0.1476
_exptl_crystal_size_mid          0.1027
_exptl_crystal_size_min          0.0542
_platon_squeeze_details
;
;
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3037
_refine_ls_number_reflns         31512
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+48.0151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                30244
_reflns_number_total             31512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11635e.txt
_cod_data_source_block           ea1077
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-4
_cod_database_code               7017903