A Family of Vanadate Esters of Monoionized and Diionized Aromatic 1,2-Diols: Synthesis, Structure, and Redox Activity
Bharat Baruah; Samir Das; Animesh Chakravorty; Inorganic Chemistry 41 (2002) 4502–4508; doi:10.1021/ic020259d

data_4318403
_publ_section_title
;
 A Family of Vanadate Esters of Monoionized and Diionized Aromatic
 1,2-Diols: Synthesis, Structure, and Redox Activity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4502
_journal_page_last               4508
_journal_paper_doi               10.1021/ic020259d
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C26 H34 N O6 V'
_chemical_formula_weight         507.48
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_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   23.754(5)
_cell_length_b                   23.754(5)
_cell_length_c                   12.836(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     6272(2)
_computing_cell_refinement       'Siemens P3/P4-PC V4.27'
_computing_data_collection       'Siemens P3/P4-PC V4.27'
_computing_data_reduction        'Siemens P3/P4-PC V4.27'
_computing_molecular_graphics    'Siemens SHELXTL V5.03 PC'
_computing_publication_material  'Siemens SHELXTL V5.03 PC'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       '\w 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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5778
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 198
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_exptl_absorpt_coefficient_mu    0.392
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.854
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       parallelopiped
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.270
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4903
_refine_ls_number_restraints     1
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_refine_ls_restrained_S_obs      1.097
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_obs          0.0515
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_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+1.2196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1461
_refine_ls_wR_factor_obs         0.1344
_reflns_number_observed          4133
_reflns_number_total             4910
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic020259d_2.cif
_cod_data_source_block           728vo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_bond_publ_flag'
value 'Y' changed to 'y' according to the built-in table from CIF
Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8
times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+1.2196P] 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^)+(0.0944P)^2^+1.2196P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6272.4(24)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4318403