The cyclic vanadylacetate (C~24~H~20~P)[V~4~O~8~(C~2~H~3~O~2~)~4~(NO~3~)]
Wulff-Molder, Dirk; Meisel, Manfred; Acta Crystallographica Section C 56 (2000) 33–34; doi:10.1107/S0108270199012214

data_2010537
_publ_section_title
;
 The cyclic vanadylacetate
 (C~24~H~20~P)[V~4~O~8~(C~2~H~3~O~2~)~4~(NO~3~)]
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              33
_journal_page_last               34
_journal_paper_doi               10.1107/S0108270199012214
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '(C24 H20 P) [V4 O8 (C2 H3 O2)4 (N O3)]'
_chemical_formula_moiety         '(PPh4) + , [V4 O8 (Me C O O)4 (N O3)] -'
_chemical_formula_structural     '(PPh4) [V4 O8 (Me C O O)4 (N O3)]'
_chemical_formula_sum            'C32 H32 N O19 P V4'
_chemical_formula_weight         969.32
_chemical_name_common            Oxovanadiumacetate
_chemical_name_systematic
;
tetraphenylphosphonium \m~4~-nitrato-\k^4^O-cyclo-
tetrakis(\m-acetato-\kO:\kO')tetra-\m-oxo-tetrakis[oxovanadium(V)]
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.856(2)
_cell_length_b                   15.856(2)
_cell_length_c                   29.753(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.7
_cell_measurement_theta_min      8.1
_cell_volume                     7480.3(18)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       oscillation
_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  .071
_diffrn_reflns_av_sigmaI/netI    .036
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32401
_diffrn_reflns_theta_max         26.06
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  .867
_exptl_absorpt_correction_T_min  .547
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(DIFABS; Walker & Stuart, 1983)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          .23
_exptl_crystal_size_mid          .23
_exptl_crystal_size_min          .15
_refine_diff_density_max         .503
_refine_diff_density_min         -.747
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          .064
_refine_ls_R_factor_obs          .042
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.7778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .112
_refine_ls_wR_factor_obs         .100
_reflns_number_observed          2503
_reflns_number_total             3685
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            jz1345.cif
_cod_data_source_block           I
_cod_depositor_comments
;
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.7778P] 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^)+(0.0636P)^2^+2.7778P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               2010537
_cod_database_fobs_code          2010537