Chiral vanadium(v) complexes with 2-aminoglucose Schiff-base ligands and their solution configurations: synthesis, structures, and DFT calculations.
Mohammadnezhad, Gholamhossein; Böhme, Michael; Geibig, Daniel; Burkhardt, Anja; Görls, Helmar; Plass, Winfried; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11812–11823; doi:10.1039/c3dt50890k

data_7021681
_publ_section_title
;
 Chiral vanadium(v) complexes with 2-aminoglucose Schiff-base ligands and
 their solution configurations: synthesis, structures, and DFT
 calculations.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11812
_journal_page_last               11823
_journal_paper_doi               10.1039/c3dt50890k
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C29 H30 N O9 V, C H Cl3'
_chemical_formula_sum            'C30 H31 Cl3 N O9 V'
_chemical_formula_weight         706.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-05-12
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1380(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.10390(10)
_cell_length_b                   18.2392(4)
_cell_length_c                   14.3543(3)
_cell_measurement_temperature    133(2)
_cell_volume                     1585.68(5)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10948
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         2.652
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       prism
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 2935 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6790
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0257
_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=1/[\s^2^(Fo^2^)+(0.0130P)^2^+0.7800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.887
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                6681
_reflns_number_total             6790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt50890k.txt
_cod_data_source_block           fo4341
_cod_database_code               7021681
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.023) H2(0.02) H3(0.018) H4(0.02) H5(0.022) H6A(0.031)
 H6B(0.031) H7(0.023) H9(0.03) H10(0.035) H11(0.033) H14A(0.035) H14B(0.035)
 H16(0.036) H17(0.045) H18(0.043) H19(0.044) H20(0.037) H21(0.022) H23(0.026)
 H24(0.031) H25(0.036) H26(0.037) H27(0.029) H28A(0.054) H28B(0.054)
 H28C(0.054) H29A(0.046) H29B(0.046) H29C(0.046) H1CL(0.034)
 Fixed X: H1(0.3171) H2(0.1488) H3(-0.1578) H4(0.1655) H5(0.172) H6A(0.4906)
 H6B(0.5169) H7(0.0207) H9(-0.0996) H10(-0.3464) H11(-0.6598) H14A(0.405)
 H14B(0.1986) H16(0.5233) H17(0.4805) H18(0.1639) H19(-0.1108) H20(-0.0712)
 H21(0.1908) H23(-0.3057) H24(-0.5144) H25(-0.3564) H26(0.0105) H27(0.2217)
 H28A(-0.7966) H28B(-0.5952) H28C(-0.7893) H29A(-1.031) H29B(-0.8279) H29C(-
 0.9827) H1CL(-0.2627)
 Fixed Y: H1(-0.3981) H2(-0.3286) H3(-0.4467) H4(-0.3884) H5(-0.5246) H6A(-
 0.4695) H6B(-0.5452) H7(-0.3653) H9(-0.3249) H10(-0.2623) H11(-0.2058) H14A(-
 0.526) H14B(-0.5796) H16(-0.4471) H17(-0.4023) H18(-0.4291) H19(-0.5022) H20(-
 0.5473) H21(-0.4598) H23(-0.4864) H24(-0.5563) H25(-0.6584) H26(-0.689) H27(-
 0.6187) H28A(-0.2081) H28B(-0.163) H28C(-0.1921) H29A(-0.1377) H29B(-0.1153)
 H29C(-0.1829) H1CL(-0.3235)
 Fixed Z: H1(-0.4016) H2(-0.5293) H3(-0.5706) H4(-0.6815) H5(-0.5781) H6A(-
 0.6924) H6B(-0.6347) H7(-0.3308) H9(-0.1816) H10(-0.1002) H11(-0.1804) H14A(-
 0.3676) H14B(-0.3624) H16(-0.2361) H17(-0.0872) H18(-0.0189) H19(-0.0986) H20(-
 0.2478) H21(-0.8219) H23(-0.8693) H24(-0.9837) H25(-1.049) H26(-0.9994) H27(-
 0.8855) H28A(-0.7184) H28B(-0.664) H28C(-0.6084) H29A(-0.3703) H29B(-0.2943)
 H29C(-0.2744) H1CL(-0.7733)
;