Synthesis, Structure, and Catecholase Reaction of a Vanadate Ester System Incorporating Monoionized Catechol Chelation
Sankar Prasad Rath; Kajal Krishna Rajak; Animesh Chakravorty; Inorganic Chemistry 38 (1999) 4376–4377; doi:10.1021/ic990551u

data_4322292
_publ_section_title
;
 Synthesis, Structure, and Catecholase Reaction of a Vanadate Ester System
 Incorporating Monoionized Catechol Chelation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4376
_journal_page_last               4377
_journal_paper_doi               10.1021/ic990551u
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H31 N2 O5 V'
_chemical_formula_weight         526.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 92.71(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.336(7)
_cell_length_b                   9.713(4)
_cell_length_c                   19.524(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2716(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3799
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.147
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         3562
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_restrained_S_obs      1.147
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_obs          0.0636
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.9298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1844
_refine_ls_wR_factor_obs         0.1350
_reflns_number_observed          2039
_reflns_number_total             3564
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990551u.cif
_cod_data_source_block           VO(Hdbcat)(A1),1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+0.9298P] 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^)+(0.0716P)^2^+0.9298P] 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        2715.6(21)
_cod_database_code               4322292