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_7021682
_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 H31 Br N O9 V, 2(C H4 O)'
_chemical_formula_sum            'C31 H39 Br N O11 V'
_chemical_formula_weight         732.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5230(3)
_cell_length_b                   11.3226(2)
_cell_length_c                   28.4192(7)
_cell_measurement_temperature    273(2)
_cell_volume                     3386.08(14)
_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
;
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20740
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.461
_diffrn_reflns_theta_min         2.738
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.531
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_description       prism
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1971 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.033(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0010P)^2^+2.7000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                5892
_reflns_number_total             7706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt50890k.txt
_cod_data_source_block           fo4351
_cod_database_code               7021682
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.055) H2(0.048) H3(0.05) H4(0.049) H5(0.051) H6A(0.065)
 H6B(0.065) H7(0.053) H9(0.06) H11(0.062) H12(0.061) H14A(0.084) H14B(0.084)
 H16(0.087) H17(0.114) H18(0.107) H19(0.104) H20(0.087) H21(0.055) H23(0.074)
 H24(0.091) H25(0.086) H26(0.087) H27(0.07) H28A(0.12) H28B(0.12) H28C(0.12)
 H1M(0.082) H1MA(0.147) H1MB(0.147) H1MC(0.147) H2M(0.204) H2MA(0.172)
 H2MB(0.172) H2MC(0.172) H3MA(0.155) H3MB(0.229) H3MC(0.229) H3MD(0.229)
 H3ME(0.168) H3MF(0.122) H3MG(0.122) H3MH(0.122)
 Fixed X: H1(-0.4505) H2(-0.3766) H3(-0.318) H4(-0.504) H5(-0.543) H6A(-0.729)
 H6B(-0.7615) H7(-0.2426) H9(-0.0843) H11(0.28) H12(0.2361) H14A(-0.4914) H14B(-
 0.5633) H16(-0.2422) H17(-0.1442) H18(-0.2627) H19(-0.4753) H20(-0.5724) H21(-
 0.6335) H23(-0.8035) H24(-0.8149) H25(-0.6331) H26(-0.4405) H27(-0.4268)
 H28A(0.0999) H28B(0.0656) H28C(-0.0314) H1M(-0.1537) H1MA(-0.1801) H1MB(-
 0.1374) H1MC(-0.0397) H2M(-0.2951) H2MA(-0.4305) H2MB(-0.3272) H2MC(-0.3039)
 H3MA(-0.2361) H3MB(-0.1497) H3MC(-0.1203) H3MD(-0.0499) H3ME(-0.1894) H3MF(-
 0.2288) H3MG(-0.1641) H3MH(-0.2925)
 Fixed Y: H1(0.2523) H2(0.23) H3(0.475) H4(0.3495) H5(0.5101) H6A(0.3846)
 H6B(0.4698) H7(0.2543) H9(0.2523) H11(0.1945) H12(0.1963) H14A(0.3678)
 H14B(0.4702) H16(0.5202) H17(0.6487) H18(0.7369) H19(0.698) H20(0.5716)
 H21(0.4668) H23(0.6398) H24(0.8105) H25(0.9154) H26(0.8498) H27(0.6807)
 H28A(0.3903) H28B(0.4771) H28C(0.4557) H1M(0.1399) H1MA(-0.0319) H1MB(0.0263)
 H1MC(0.0117) H2M(0.3553) H2MA(0.4294) H2MB(0.4156) H2MC(0.502) H3MA(0.1903)
 H3MB(0.0957) H3MC(-0.0065) H3MD(0.115) H3ME(0.1907) H3MF(-0.0191) H3MG(0.0328)
 H3MH(0.0862)
 Fixed Z: H1(0.2795) H2(0.2029) H3(0.2005) H4(0.1483) H5(0.2241) H6A(0.1708)
 H6B(0.2129) H7(0.2984) H9(0.3583) H11(0.3288) H12(0.2494) H14A(0.3435)
 H14B(0.3174) H16(0.33) H17(0.3819) H18(0.44) H19(0.4464) H20(0.3936)
 H21(0.1007) H23(0.0768) H24(0.0316) H25(0.0154) H26(0.0419) H27(0.0873)
 H28A(0.0736) H28B(0.1146) H28C(0.0737) H1M(0.1225) H1MA(0.1547) H1MB(0.2022)
 H1MC(0.161) H2M(0.0854) H2MA(0.0396) H2MB(0.0003) H2MC(0.0425) H3MA(0.0556)
 H3MB(-0.0025) H3MC(0.0331) H3MD(0.0377) H3ME(0.0554) H3MF(0.0399) H3MG(-
 0.0052) H3MH(0.013)
;