A Dinuclear Vanadyl–Oxalate Compound
Zheng, Li-Min; Schmalle, Helmut W.; Ferlay, Sylvie; Decurtins, Silvio; Acta Crystallographica Section C 54 (1998) 1435–1438; doi:10.1107/S0108270198006520

data_2007763
_publ_section_title
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 A Dinuclear Vanadyl--Oxalate Compound
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1435
_journal_page_last               1438
_journal_paper_doi               10.1107/S0108270198006520
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '(C24 H20 P)2 [V2 O2 (C2 O4)3 (H2 O)2] , 8H2 O'
_chemical_formula_sum            'C54 H60 O24 P2 V2'
_chemical_formula_weight         1256.88
_chemical_name_systematic
;
 bis(tetraphenylphosphonium) \m-oxalato-O^1^,O^2^:O^1^',O^2^'
-bis[aqua(oxalato-O^1^,O^2^)oxovanadium(IV)] octahydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                66.39(3)
_cell_angle_beta                 74.97(3)
_cell_angle_gamma                80.84(3)
_cell_formula_units_Z            1
_cell_length_a                   9.571(4)
_cell_length_b                   12.773(6)
_cell_length_c                   13.486(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      11.4
_cell_measurement_theta_min      6.7
_cell_volume                     1456.1(12)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics
'PLATON (Spek, 1990) and SCHAKAL86 (Keller, 1986)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scans'
_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  0.021
_diffrn_reflns_av_sigmaI/netI    0.044
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8795
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        2.2
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   'numerical (Coppens et al., 1965)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.429
_refine_ls_extinction_coef       0.0068(7)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    'H atoms: see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.101
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.7029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.121
_reflns_number_observed          5482
_reflns_number_total             8461
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            sk1188.cif
_cod_data_source_block           limin7
_cod_depositor_comments
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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^)+(0.0343P)^2^+0.7029P] 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^)+(0.0343P)^2^+0.7029P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        1456.1(11)
_cod_database_code               2007763