Tetrapiperidinium di-μ-methoxy-di-μ~5~-oxo-tetra-μ~3~-oxo-dodeca-μ~2~-oxo-octaoxodecavanadate
Fen Sun; Yan-Tuan Li; Zhi-Yong Wu; Da-Qi Wang; Jian-Min Dou; Acta Crystallographica Section C 62 (2006) m60–m62; doi:10.1107/S0108270105042241

data_2014310
_publ_section_title
;Tetrapiperidinium
 di-\m-methoxy-di-\m~5~-oxo-tetra-\m~3~-oxo-dodeca-\m~2~-oxo-octaoxodecavanadate
;
_journal_coeditor_code           BG1023
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m60
_journal_page_last               m62
_journal_paper_doi               10.1107/S0108270105042241
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C5 H12 N)4 [V10 (C1 H3 O1)2 O26]'
_chemical_formula_moiety         '4C5 H12 N + , V10 O28 C2 H6 -'
_chemical_formula_sum            'C22 H54 N4 O28 V10'
_chemical_formula_weight         1332.09
_chemical_name_systematic
;Tetrapiperidinium
di-\m-methoxy-di-\m~5~-oxo-tetra-\m~3~-oxo-dodeca-\m~2~-oxo-octaoxodecavanadate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.58(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.546(2)
_cell_length_b                   12.950(3)
_cell_length_c                   16.033(3)
_cell_measurement_reflns_used    5269
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.257
_cell_measurement_theta_min      2.301
_cell_volume                     2189.5(8)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XP (Siemens, 1994))'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11580
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.126
_exptl_absorpt_correction_T_max  0.7340
_exptl_absorpt_correction_T_min  0.6390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.450
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0502P)^2^+2.2417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                3226
_reflns_number_total             3957
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg1023.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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 21/n'
_cod_database_code               2014310
_cod_database_fobs_code          2014310