Magneto-structural correlation for binuclear octahedral vanadium(IV)–oxo complexes. Synthesis, structure and magnetic properties of a VIVO2+ complex with a new ligand derived from glycine
Ceccato, Augusto S.; Neves, Ademir; de Brito, Marcos A.; Drechsel, Sueli M.; Mangrich, Antonio S.; Werner, Rüdiger; Haase, Wolfgang; Bortoluzzi, Adailton J.; Journal of the Chemical Society, Dalton Transactions  (2000) 1573–; doi:10.1039/a909846a

data_7009302
_publ_section_title
;
 Magneto-structural correlation for binuclear octahedral
 vanadium(IV)--oxo complexes. Synthesis, structure and magnetic
 properties of a VIVO2+ complex with a new ligand derived from glycine
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1573
_journal_paper_doi               10.1039/a909846a
_journal_year                    2000
_chemical_formula_moiety
;
C32 H28 N2 O12 V2, 2(C6 H16 N), 4(C H2 Cl2)
;
_chemical_formula_sum            'C48 H68 Cl8 N4 O10 V2'
_chemical_formula_weight         1246.54
_chemical_name_systematic
;
Triethylammonium-bis{[N,N-bis(2-oxyphenyl)glycinate]
oxovanadium(IV)} dichloromethane solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL97 and manual editing'
_cell_angle_alpha                98.11(3)
_cell_angle_beta                 102.00(3)
_cell_angle_gamma                110.17(3)
_cell_formula_units_Z            1
_cell_length_a                   10.638(2)
_cell_length_b                   11.380(2)
_cell_length_c                   13.512(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      13.85
_cell_measurement_theta_min      7.57
_cell_volume                     1461.0(6)
_computing_cell_refinement
;
SET4 in CAD4 EXPRESS (Enraf-Nonius, 1994)  
;
_computing_data_collection       'CAD4-EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'HELENA (Spek, 1996)'
_computing_molecular_graphics
;
ZORTEP (Zsolnai et al., 1996)
;
_computing_publication_material
;
SHELXL97. All calculations were performed on a PC/Pentim II  computer
running LINUX.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5432
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.17
_diffrn_standards_decay_%        4.1
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.9143
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'PLATON (Spek, 1990)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             646
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0031(14)
_refine_ls_extinction_expression Fc^*^=3DkFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5133
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.8873P] where P=3D(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                4570
_reflns_number_total             5133
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            a909846a.txt
_cod_data_source_block           9/02385B
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.8873P] where P=3D(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=3D1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.8873P] where
P=3D(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1461.0(4)
_cod_database_code               7009302