Stereospecific Formation of Dinuclear Vanadium(V) Tartrato Complexes
Jana Gáliková; Peter Schwendt; Jozef Tatiersky; Alan S. Tracey; Zdirad Žák; Inorganic Chemistry 48 (2009) 8423–8430; doi:10.1021/ic901024p

data_4303065
_publ_section_title
;
Stereospecific Formation of Dinuclear Vanadium(V) Tartrato Complexes
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8423
_journal_page_last               8430
_journal_paper_doi               10.1021/ic901024p
_journal_volume                  48
_journal_year                    2009
_chemical_absolute_configuration ad
_chemical_formula_sum            'C16 H44 N2 O22 V2'
_chemical_formula_weight         718.41
_chemical_name_systematic
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 ? 
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_space_group_IT_number           23
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 2'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0275(16)
_cell_length_b                   8.3123(17)
_cell_length_c                   22.674(5)
_cell_measurement_reflns_used    6683
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1809
_cell_measurement_theta_min      2.6864
_cell_volume                     1513.0(5)
_computing_cell_refinement
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.6 
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 
;
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.4353
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'KUMA KM-4 CCD'
_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  0.0115
_diffrn_reflns_av_sigmaI/netI    0.0122
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6153
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         3.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 'after every 100 frames'
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.9011
_exptl_absorpt_correction_T_min  0.7645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1552
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.7948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                1476
_reflns_number_total             1552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901024p_si_002.cif
_cod_data_source_block           galik
_cod_database_code               4303065