Bis(tetra-<i>n</i>-butylammonium) bis[(mandelato)oxo(peroxo)vanadate(V)] mandelic acid solvate
Kutá Smatanová, Ivana; Marek, Jaromír; Švančárek, Peter; Schwendt, Peter; Acta Crystallographica Section C 56 (2000) 154–155; doi:10.1107/S0108270199013475

data_2010611
_publ_section_title
;
 Bis(tetra-<i>n</i>-butylammonium)
 bis[(mandelato)oxo(peroxo)vanadate(V)] mandelic acid solvate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              154
_journal_page_last               155
_journal_paper_doi               10.1107/S0108270199013475
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac
'(C16 H36 N)2 [V2 O2 (O2)2 (C8 H6 O3)2] , C8 H8 O3'
_chemical_formula_moiety         'C48 H84 N2 O12 V2 , C8 H8 O3'
_chemical_formula_sum            'C56 H92 N2 O15 V2'
_chemical_formula_weight         1135.20
_chemical_name_systematic
;
Bis(tetra-n-butylammonium) Bis[\m-2-hydroxy-2-phenyl-
ethanoato(2-)]-bis[oxomonoperoxovanadate(V)]
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.657(12)
_cell_length_b                   17.066(3)
_cell_length_c                   17.670(5)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      1.58
_cell_volume                     5928(4)
_computing_cell_refinement       'KM-4 Software'
_computing_data_collection       'KM-4 Software (Galdecki et al., 1996)'
_computing_data_reduction        'KM-4 Software'
_computing_molecular_graphics    'ORTEPIII (Johnson & Burnett, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_measured_fraction_theta_full .990
_diffrn_measured_fraction_theta_max .990
_diffrn_measurement_device_type
;
4-circle \k-axis Kuma KM-4 diffractometer with Oxford Cryosytems Cryostream
cooler
;
_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     .71073
_diffrn_reflns_av_R_equivalents  .023
_diffrn_reflns_av_sigmaI/netI    .050
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5680
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .380
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         .663
_refine_diff_density_min         -.399
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          .098
_refine_ls_R_factor_gt           .052
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0838P)^2^+5.65P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .168
_reflns_number_gt                3329
_reflns_number_total             5210
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf1306.cif
_cod_data_source_block           I
_cod_database_code               2010611
_cod_database_fobs_code          2010611