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_7021680
_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         'C30 H34 N O10 V, 2(C H4 O)'
_chemical_formula_sum            'C32 H42 N O12 V'
_chemical_formula_weight         683.60
_chemical_name_systematic
;
 ?
;
_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            8
_cell_length_a                   9.54420(10)
_cell_length_b                   25.1111(4)
_cell_length_c                   27.5039(4)
_cell_measurement_temperature    133(2)
_cell_volume                     6591.73(16)
_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      133.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            40163
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_min         1.783
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow-brown
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 5987 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.018(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         15122
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0260P)^2^+5.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0968
_reflns_Friedel_coverage         0.813
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                14245
_reflns_number_total             15122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt50890k.txt
_cod_data_source_block           fo4322
_cod_database_code               7021680
_olex2_refinement_description
;
1. Shared sites
{C152, C153}
{H203, H202}
2. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H14C(0.5) H14D(0.5) C152(0.5) C162(0.5)
 H162(0.5) C172(0.5) H172(0.5) C182(0.5) H182(0.5) C192(0.5) H192(0.5)
 C202(0.5) H202(0.5) C153(0.5) C163(0.5) H163(0.5) C173(0.5) H173(0.5)
 C183(0.5) H183(0.5) C193(0.5) H193(0.5) C203(0.5) H203(0.5) O3M(0.5) H3M(0.5)
 C3M(0.5) H3MA(0.5) H3MB(0.5) H3MC(0.5) O3MA(0.5) H3MD(0.5) C3MA(0.5) H3ME(0.5)
 H3MF(0.5) H3MG(0.5) O4M(0.5) H4M(0.5) C4M(0.5) H4MA(0.5) H4MB(0.5) H4MC(0.5)
 O4MA(0.5) H4MD(0.5) C4MA(0.5) H4ME(0.5) H4MF(0.5) H4MG(0.5)
 Fixed Uiso: H11(0.023) H21(0.022) H31(0.02) H41(0.021) H51(0.022) H61A(0.028)
 H61B(0.028) H71(0.025) H91(0.035) H101(0.038) H111(0.039) H14E(0.042)
 H14F(0.042) H161(0.059) H171(0.084) H181(0.07) H191(0.06) H201(0.047)
 H211(0.024) H231(0.034) H241(0.044) H251(0.043) H261(0.044) H271(0.038)
 H28D(0.1) H28E(0.1) H28F(0.1) H29D(0.063) H29E(0.063) H29F(0.063) H12(0.023)
 H22(0.022) H32(0.021) H42(0.022) H52(0.023) H62A(0.029) H62B(0.029) H72(0.026)
 H92(0.036) H102(0.043) H112(0.04) H14A(0.029) H14B(0.029) H14C(0.029)
 H14D(0.029) H162(0.048) H172(0.047) H182(0.037) H192(0.029) H202(0.02)
 H163(0.025) H173(0.034) H183(0.034) H193(0.034) H203(0.048) H212(0.026)
 H232(0.038) H242(0.045) H252(0.047) H262(0.047) H272(0.04) H28A(0.07)
 H28B(0.07) H28C(0.07) H29A(0.065) H29B(0.065) H29C(0.065) H1M1(0.029)
 H1MD(0.091) H1ME(0.091) H1MF(0.091) H1M2(0.031) H1MA(0.082) H1MB(0.082)
 H1MC(0.082) H1M(0.113) H1MG(0.062) H1MH(0.062) H1MI(0.062) H2M(0.07)
 H2MA(0.067) H2MB(0.067) H2MC(0.067) H3M(0.066) H3MA(0.088) H3MB(0.088)
 H3MC(0.088) H3MD(0.139) H3ME(0.106) H3MF(0.106) H3MG(0.106) H4M(0.075)
 H4MA(0.096) H4MB(0.096) H4MC(0.096) H4MD(0.081) H4ME(0.093) H4MF(0.093)
 H4MG(0.093)
 Fixed X: H11(-0.0475) H21(0.0273) H31(0.2756) H41(0.0378) H51(0.118) H61A(-
 0.1171) H61B(-0.0786) H71(0.1233) H91(0.2436) H101(0.3923) H111(0.5142) H14E(-
 0.0328) H14F(0.0137) H161(0.18) H171(0.3238) H181(0.3779) H191(0.2982)
 H201(0.1521) H211(0.0361) H231(0.3618) H241(0.4891) H251(0.3994) H261(0.1845)
 H271(0.064) H28D(0.5574) H28E(0.603) H28F(0.5728) H29D(0.6435) H29E(0.5616)
 H29F(0.68) H12(0.3841) H22(0.3245) H32(0.0656) H42(0.3145) H52(0.2047)
 H62A(0.4506) H62B(0.3909) H72(0.2067) H92(0.067) H102(-0.0886) H112(-0.1804)
 H14A(0.3619) H14B(0.277) H14C(0.3574) H14D(0.2871) H162(0.108) H172(-0.0409)
 H182(-0.057) H192(0.0484) H202(0.1906) H163(0.128) H173(-0.0119) H183(-0.0735)
 H193(0.0231) H203(0.1818) H212(0.3133) H232(-0.0483) H242(-0.1691) H252(-
 0.0458) H262(0.1964) H272(0.3179) H28A(-0.1651) H28B(-0.2137) H28C(-0.1342)
 H29A(-0.2808) H29B(-0.2293) H29C(-0.3279) H1M1(0.086) H1MD(-0.0411)
 H1ME(0.0791) H1MF(0.0969) H1M2(0.2805) H1MA(0.4318) H1MB(0.3164) H1MC(0.3068)
 H1M(0.3098) H1MG(0.1194) H1MH(0.2098) H1MI(0.1954) H2M(0.0898) H2MA(-0.0243)
 H2MB(-0.0507) H2MC(-0.1184) H3M(0.3809) H3MA(0.4669) H3MB(0.3132) H3MC(0.3464)
 H3MD(0.4358) H3ME(0.4629) H3MF(0.4033) H3MG(0.3205) H4M(0.2207) H4MA(0.1651)
 H4MB(0.1083) H4MC(0.2498) H4MD(0.2226) H4ME(0.1583) H4MF(0.1573) H4MG(0.2887)
 Fixed Y: H11(0.1704) H21(0.1443) H31(0.2087) H41(0.2223) H51(0.2829)
 H61A(0.3009) H61B(0.3365) H71(0.1122) H91(0.066) H101(-0.0012) H111(-0.0534)
 H14E(0.2237) H14F(0.2775) H161(0.3328) H171(0.3541) H181(0.289) H191(0.2036)
 H201(0.1824) H211(0.2995) H231(0.301) H241(0.36) H251(0.444) H261(0.4702)
 H271(0.4134) H28D(0.0246) H28E(0.0652) H28F(0.0868) H29D(-0.1025) H29E(-
 0.1106) H29F(-0.0658) H12(-0.1789) H22(-0.1491) H32(-0.2078) H42(-0.2262) H52(-
 0.2853) H62A(-0.3103) H62B(-0.3453) H72(-0.1184) H92(-0.0759) H102(-0.0095)
 H112(0.0498) H14A(-0.2431) H14B(-0.2909) H14C(-0.241) H14D(-0.2896) H162(-
 0.3347) H172(-0.3393) H182(-0.2644) H192(-0.1857) H202(-0.1814) H163(-0.3405)
 H173(-0.3537) H183(-0.2848) H193(-0.2015) H203(-0.1893) H212(-0.3012) H232(-
 0.3338) H242(-0.391) H252(-0.442) H262(-0.4349) H272(-0.3765) H28A(-0.0285)
 H28B(-0.0789) H28C(-0.0875) H29A(0.1022) H29B(0.1079) H29C(0.0592)
 H1M1(0.0336) H1MD(0.0651) H1ME(0.0287) H1MF(0.0921) H1M2(-0.0319) H1MA(-
 0.0649) H1MB(-0.0331) H1MC(-0.0965) H1M(0.1666) H1MG(0.1761) H1MH(0.1976)
 H1MI(0.2328) H2M(-0.1695) H2MA(-0.2378) H2MB(-0.199) H2MC(-0.1856) H3M(0.1208)
 H3MA(0.0249) H3MB(0.0386) H3MC(0.042) H3MD(0.1309) H3ME(0.0273) H3MF(0.0535)
 H3MG(0.0609) H4M(-0.1283) H4MA(-0.0426) H4MB(-0.072) H4MC(-0.0379) H4MD(-
 0.1342) H4ME(-0.0584) H4MF(-0.0938) H4MG(-0.0564)
 Fixed Z: H11(1.0281) H21(0.9519) H31(0.9601) H41(0.8967) H51(0.9818)
 H61A(0.9187) H61B(0.9654) H71(1.0555) H91(1.1217) H101(1.1483) H111(1.0929)
 H14E(1.0958) H14F(1.0687) H161(1.1048) H171(1.1715) H181(1.228) H191(1.2184)
 H201(1.1535) H211(0.8515) H231(0.8267) H241(0.7779) H251(0.7597) H261(0.7928)
 H271(0.8449) H28D(0.8512) H28E(0.8932) H28F(0.8394) H29D(0.9826) H29E(1.0328)
 H29F(1.0284) H12(1.0322) H22(0.9557) H32(0.9561) H42(0.8991) H52(0.9809)
 H62A(0.9245) H62B(0.9688) H72(1.058) H92(1.1212) H102(1.1453) H112(1.0888)
 H14A(1.0923) H14B(1.0669) H14C(1.0946) H14D(1.0656) H162(1.1148) H172(1.1843)
 H182(1.2333) H192(1.2124) H202(1.1449) H163(1.1101) H173(1.1776) H183(1.228)
 H193(1.2163) H203(1.1523) H212(0.8527) H232(0.8619) H242(0.8094) H252(0.7531)
 H262(0.7474) H272(0.7989) H28A(0.837) H28B(0.8683) H28C(0.8177) H29A(0.9754)
 H29B(1.0305) H29C(1.0151) H1M1(0.9234) H1MD(0.866) H1ME(0.8427) H1MF(0.8439)
 H1M2(0.9284) H1MA(0.8793) H1MB(0.8487) H1MC(0.8535) H1M(0.8386) H1MG(0.7991)
 H1MH(0.7541) H1MI(0.8023) H2M(0.8365) H2MA(0.8036) H2MB(0.7583) H2MC(0.8101)
 H3M(0.7561) H3MA(0.7365) H3MB(0.7169) H3MC(0.7738) H3MD(0.761) H3ME(0.7655)
 H3MF(0.7166) H3MG(0.7668) H4M(0.7742) H4MA(0.7751) H4MB(0.7274) H4MC(0.7251)
 H4MD(0.7765) H4ME(0.7533) H4MF(0.705) H4MG(0.7168)
;