Synthesis and Characterization of a Borophosphate Anion Containing a Single Vanadium Atom: [N~2~C~6~H~14~]~2~[VO(PO~3~OH)~4~(B~3~O~3~OH)]4H~2~O
Ranko P. Bontchev; Junghwan Do; Allan J. Jacobson; Inorganic Chemistry 38 (1999) 2231–2233; doi:10.1021/ic981278j

data_4321965
_publ_contact_author_email       ajjacob@uh.edu
_publ_contact_author_fax         '713 743 2787'
_publ_contact_author_phone       '713 743 2785'
_publ_section_title
;
 Synthesis and Characterization of a Borophosphate Anion Containing a
 Single Vanadium Atom:
 [N~2~C~6~H~14~]~2~[VO(PO~3~OH)~4~(B~3~O~3~OH)]4H~2~O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2231
_journal_page_last               2233
_journal_paper_doi               10.1021/ic981278j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         '(C6 H14 N2 2+)2, H5 B3 O21 P4 V 4-, 4(H2 O)'
_chemical_formula_structural
;
 (C6 H14 N2)2 ((V O)(P O3 O H)4 (B3 O3 O H)) 4(H2 O)
;
_chemical_formula_sum            'C12 H41 B3 N4 O25 P4 V'
_chemical_formula_weight         848.73
_chemical_name_systematic
;
Bis(diprotonated1,4-diazabicyclo(2.2.2)octane)vanadyl(IV)tetra(hydrogen 
phosphate)hydrogenboratetetrahydrate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 100.8300(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6625(10)
_cell_length_b                   10.6130(6)
_cell_length_c                   17.8888(10)
_cell_measurement_reflns_used    4607
_cell_measurement_temperature    293(2)
_cell_volume                     3107.1(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    DIAMOND
_computing_publication_material  'MS-DOS 6.22 EDITOR'
_computing_structure_refinement  'SHELXTL 5.03'
_computing_structure_solution    'SHELXTL 5.03'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18029
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.056
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         7101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_obs          0.0382
_refine_ls_shift/esd_max         0.944
_refine_ls_shift/esd_mean        0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+2.5994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0976
_refine_ls_wR_factor_obs         0.0907
_reflns_number_observed          5793
_reflns_number_total             7101
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981278j.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+2.5994P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+2.5994P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321965