(C~6~H~14~N~2~)~2~[VO(HPO~4~)~5~B~2~O]·H~2~O·H~3~PO~4~, a novel borophosphate cluster containing a single vanadium centre and linked by hydrogen bonds into a three-dimensional framework
Wikstad, Emma; Kritikos, Mikael; Acta Crystallographica Section C 59 (2003) m87–m89; doi:10.1107/S0108270103002683

data_2013140
_publ_section_title
;
 (C~6~H~14~N~2~)~2~[VO(HPO~4~)~5~B~2~O]&#x00B7;H~2~O&#x00B7;H~3~PO~4~,
 a novel borophosphate cluster containing a single vanadium centre and
 linked by hydrogen bonds into a three-dimensional framework
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m87
_journal_page_last               m89
_journal_paper_doi               10.1107/S0108270103002683
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac
'(N2 C6 H14)2 [V O (P O4 H)5 B2 O] , H2 O , H3 P O4'
_chemical_formula_moiety
'2C6 H14 N2 2+ , H5 B2 O22 P5 V 4- , H3 O4 P, H2 O'
_chemical_formula_sum            'C12 H38 B2 N4 O27 P6 V'
_chemical_formula_weight         928.84
_chemical_name_systematic
;\m~3~-oxo-oxopenta-\m-phosphato-diboron vanadium
 bis(1,4-diazonia[2.2.2]octane)
monohydrate phosphoric acid solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 94.113(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4882(15)
_cell_length_b                   12.2569(13)
_cell_length_c                   19.6281(18)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.25
_cell_volume                     3236.6(6)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1997)'
_computing_data_reduction        IPDS
_computing_molecular_graphics
'PLATON99 (Spek, 2003) and DIAMOND (Brandenburg, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f oscillation'
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30473
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-SHAPE and X-RED; Stoe & Cie, 1997)'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.906
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.81
_refine_diff_density_min         -0.66
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.051
_refine_ls_R_factor_gt           0.037
_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^)+(0.0701P)^2^+0.9891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.098
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                6006
_reflns_number_total             7428
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1684.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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_Hall     '-P  2ybc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2013140
_cod_database_fobs_code          2013140