Nonapiperidinium monohydrogen decavanadate tetranitrate
Graia, Mohsen; Ksiksi, Regaya; Driss, Ahmed; Acta Crystallographica Section E 65 (2009) m953–m954; doi:10.1107/S1600536809026555

data_2222782
_publ_section_title
;
 Nonapiperidinium monohydrogen decavanadate tetranitrate
;
_journal_coeditor_code           LH2828
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m953
_journal_page_last               m954
_journal_paper_doi               10.1107/S1600536809026555
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '(C5 H12 N)9 [H V10 O28] (N O3)4'
_chemical_formula_moiety         '9(C5 H12 N +), H O28 V10 5-, 4(N O3 -)'
_chemical_formula_sum            'C45 H109 N13 O40 V10'
_chemical_formula_weight         1981.85
_chemical_name_systematic
;
Nonapiperidinium monohydrogen decavanadate tetranitrate
;
_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                105.858(2)
_cell_angle_beta                 110.335(2)
_cell_angle_gamma                92.457(2)
_cell_formula_units_Z            1
_cell_length_a                   11.593(2)
_cell_length_b                   13.290(2)
_cell_length_c                   14.676(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.17
_cell_measurement_theta_min      11.77
_cell_volume                     2015.6(5)
_computing_cell_refinement
'CAD-4 EXPRESS (Duisenberg, 1992; Mac\'i\<cek & Yordanov, 1992)'
_computing_data_collection
'CAD-4 EXPRESS (Duisenberg, 1992; Mac\'i\<cek & Yordanov, 1992)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1998)'
_computing_publication_material  'publCIF (Westrip, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9193
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagone
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .14
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.317
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         8755
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0432
_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^)+(0.0517P)^2^+1.3683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                6099
_reflns_number_total             8755
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2828.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               2222782
_cod_database_fobs_code          2222782