#------------------------------------------------------------------------------
#$Date: 2025-08-20 15:06:16 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301830 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/83/4078353.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4078353
loop_
_publ_author_name
'Lütjens, Henning'
'Wahl, Günter'
'Möller, Frank'
'Knochel, Paul'
'Sundermeyer, Jörg'
_publ_contact_author
;
        Prof. Dr. Joerg Sundermeyer
        Fachbereich Chemie
        Universitaet Marburg
        Hans-Meerwein Strasse
        D-35032 Marburg  
        Deutschland
;
_publ_section_title
;
 New ChiralC3-Symmetric Triols as Ligands for Vanadium and Titanium
 Complexes†
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5869
_journal_paper_doi               10.1021/om970523o
_journal_volume                  16
_journal_year                    1997
_chemical_formula_moiety         '[V(O){(OCH-Et)3CH}]2'
_chemical_formula_sum            'C20 H38 O8 V2'
_chemical_formula_weight         508.38
_chemical_melting_point          121=F8C
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.970(4)
_cell_length_b                   13.503(2)
_cell_length_c                   14.567(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      10
_cell_volume                     2551.2(12)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'BEGIN (SDP)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'CAD4 (Enraf-Nonius)'
_diffrn_measurement_method       'Omaga-Theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3279
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.155
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3275
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_restrained_S_obs      1.052
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_obs          0.0448
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=3D1/[σ²(Fo²)+(0.0377P)²+1.0583P] where P=3D(Fo²+2Fc²)= /3''
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1129
_refine_ls_wR_factor_obs         0.0862
_reflns_number_observed          2382
_reflns_number_total             3276
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om5869.cif
_cod_data_source_block           gw4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=3D1/[\s^2^(Fo^2^)+(0.0377P)^2^+1.0583P] 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^)+(0.0377P)^2^+1.0583P] 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_sg_symbol_H-M      P212121
_cod_database_code               4078353
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
V1 V 0.24586(8) 0.02201(7) 0.72043(6) 0.0421(2) Uani 1 d .
V2 V 0.10158(7) 0.17312(7) 0.63541(6) 0.0376(2) Uani 1 d .
O1 O 0.0428(3) 0.0883(3) 0.5573(2) 0.0473(10) Uani 1 d .
O2 O 0.1006(3) 0.0634(2) 0.7271(2) 0.0401(8) Uani 1 d .
O3 O 0.1956(3) -0.0987(3) 0.7011(3) 0.0472(10) Uani 1 d .
O4 O 0.1708(3) 0.2449(3) 0.5538(3) 0.0449(9) Uani 1 d .
O5 O 0.2331(3) 0.1690(3) 0.7029(2) 0.0413(8) Uani 1 d .
O6 O 0.3334(3) 0.0241(3) 0.6268(3) 0.0583(11) Uani 1 d .
O7 O 0.0214(3) 0.2492(3) 0.6775(3) 0.0514(10) Uani 1 d .
O8 O 0.3005(3) 0.0140(3) 0.8174(3) 0.0642(12) Uani 1 d .
C1 C -0.0142(4) -0.0014(4) 0.5589(4) 0.0416(13) Uani 1 d .
H1 H -0.0865(4) 0.0153(4) 0.5708(4) 0.050 Uiso 1 calc R
C2 C 0.0196(4) -0.0113(4) 0.7280(4) 0.0428(13) Uani 1 d .
H2 H 0.0354(4) -0.0585(4) 0.7772(4) 0.051 Uiso 1 calc R
C3 C 0.1320(4) -0.1122(4) 0.6214(4) 0.0442(14) Uani 1 d .
H3 H 0.1644(4) -0.0780(4) 0.5695(4) 0.053 Uiso 1 calc R
C4 C 0.0232(4) -0.0669(4) 0.6375(4) 0.0435(13) Uani 1 d .
H4 H -0.0253(4) -0.1223(4) 0.6424(4) 0.052 Uiso 1 calc R
C5 C 0.1287(5) -0.2231(5) 0.6005(5) 0.065(2) Uani 1 d .
H5A H 0.0996(5) -0.2576(5) 0.6528(5) 0.078 Uiso 1 calc R
H5B H 0.0836(5) -0.2342(5) 0.5484(5) 0.078 Uiso 1 calc R
C6 C 0.2338(6) -0.2664(6) 0.5793(6) 0.091(3) Uani 1 d .
H6A H 0.2270(6) -0.3360(6) 0.5670(6) 0.137 Uiso 1 calc R
H6B H 0.2787(6) -0.2569(6) 0.6310(6) 0.137 Uiso 1 calc R
H6C H 0.2624(6) -0.2339(6) 0.5265(6) 0.137 Uiso 1 calc R
C7 C -0.0082(5) -0.0488(5) 0.4643(4) 0.054(2) Uani 1 d .
H7A H -0.0447(5) -0.1115(5) 0.4654(4) 0.065 Uiso 1 calc R
H7B H 0.0634(5) -0.0623(5) 0.4496(4) 0.065 Uiso 1 calc R
C8 C -0.0540(5) 0.0164(6) 0.3900(4) 0.075(2) Uani 1 d .
H8A H -0.0486(5) -0.0165(6) 0.3318(4) 0.113 Uiso 1 calc R
H8B H -0.0172(5) 0.0780(6) 0.3877(4) 0.113 Uiso 1 calc R
H8C H -0.1253(5) 0.0289(6) 0.4036(4) 0.113 Uiso 1 calc R
C9 C -0.0820(4) 0.0391(5) 0.7516(4) 0.054(2) Uani 1 d .
H9A H -0.0728(4) 0.0786(5) 0.8066(4) 0.065 Uiso 1 calc R
H9B H -0.1008(4) 0.0835(5) 0.7020(4) 0.065 Uiso 1 calc R
C10 C -0.1687(5) -0.0340(5) 0.7670(6) 0.082(2) Uani 1 d .
H10A H -0.2309(5) 0.0013(5) 0.7815(6) 0.123 Uiso 1 calc R
H10B H -0.1512(5) -0.0772(5) 0.8170(6) 0.123 Uiso 1 calc R
H10C H -0.1791(5) -0.0724(5) 0.7124(6) 0.123 Uiso 1 calc R
C11 C 0.2583(4) 0.2010(4) 0.5093(4) 0.0448(13) Uani 1 d .
H11 H 0.2400(4) 0.1340(4) 0.4894(4) 0.054 Uiso 1 calc R
C12 C 0.3191(4) 0.2284(4) 0.6715(4) 0.0463(14) Uani 1 d .
H12 H 0.2947(4) 0.2969(4) 0.6663(4) 0.056 Uiso 1 calc R
C13 C 0.4003(5) 0.0910(5) 0.5821(4) 0.0537(15) Uani 1 d .
H13 H 0.4634(5) 0.0963(5) 0.6188(4) 0.064 Uiso 1 calc R
C14 C 0.3511(4) 0.1948(4) 0.5764(4) 0.0469(15) Uani 1 d .
H14 H 0.4040(4) 0.2407(4) 0.5543(4) 0.056 Uiso 1 calc R
C15 C 0.4293(6) 0.0467(6) 0.4888(5) 0.081(2) Uani 1 d .
H15A H 0.3674(6) 0.0374(6) 0.4525(5) 0.097 Uiso 1 calc R
H15B H 0.4738(6) 0.0925(6) 0.4562(5) 0.097 Uiso 1 calc R
C16 C 0.4841(9) -0.0518(7) 0.4999(7) 0.151(6) Uani 1 d .
H16A H 0.5011(9) -0.0779(7) 0.4405(7) 0.227 Uiso 1 calc R
H16B H 0.4398(9) -0.0975(7) 0.5314(7) 0.227 Uiso 1 calc R
H16C H 0.5461(9) -0.0425(7) 0.5348(7) 0.227 Uiso 1 calc R
C17 C 0.2812(5) 0.2635(5) 0.4256(4) 0.064(2) Uani 1 d .
H17A H 0.3408(5) 0.2363(5) 0.3943(4) 0.076 Uiso 1 calc R
H17B H 0.2984(5) 0.3301(5) 0.4452(4) 0.076 Uiso 1 calc R
C18 C 0.1911(6) 0.2683(6) 0.3586(5) 0.081(2) Uani 1 d .
H18A H 0.2096(6) 0.3088(6) 0.3070(5) 0.121 Uiso 1 calc R
H18B H 0.1322(6) 0.2963(6) 0.3888(5) 0.121 Uiso 1 calc R
H18C H 0.1747(6) 0.2027(6) 0.3377(5) 0.121 Uiso 1 calc R
C19 C 0.4045(5) 0.2271(5) 0.7433(4) 0.062(2) Uani 1 d .
H19A H 0.4248(5) 0.1591(5) 0.7547(4) 0.074 Uiso 1 calc R
H19B H 0.4640(5) 0.2621(5) 0.7194(4) 0.074 Uiso 1 calc R
C20 C 0.3725(7) 0.2735(6) 0.8312(5) 0.100(3) Uani 1 d .
H20A H 0.4287(7) 0.2709(6) 0.8741(5) 0.150 Uiso 1 calc R
H20B H 0.3145(7) 0.2383(6) 0.8560(5) 0.150 Uiso 1 calc R
H20C H 0.3537(7) 0.3413(6) 0.8206(5) 0.150 Uiso 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O8 V1 O6 113.6(2)
O8 V1 O3 104.0(2)
O6 V1 O3 97.3(2)
O8 V1 O2 113.8(2)
O6 V1 O2 130.2(2)
O3 V1 O2 85.2(2)
O8 V1 O5 102.6(2)
O6 V1 O5 86.5(2)
O3 V1 O5 148.9(2)
O2 V1 O5 69.31(14)
O8 V1 V2 133.3(2)
O6 V1 V2 94.01(14)
O3 V1 V2 109.04(12)
O2 V1 V2 40.39(10)
O5 V1 V2 39.84(10)
O7 V2 O4 103.7(2)
O7 V2 O1 112.5(2)
O4 V2 O1 98.0(2)
O7 V2 O5 113.2(2)
O4 V2 O5 85.0(2)
O1 V2 O5 132.1(2)
O7 V2 O2 102.6(2)
O4 V2 O2 148.9(2)
O1 V2 O2 86.9(2)
O5 V2 O2 69.56(15)
O7 V2 V1 133.1(2)
O4 V2 V1 109.18(13)
O1 V2 V1 95.26(13)
O5 V2 V1 40.80(11)
O2 V2 V1 39.73(11)
C1 O1 V2 139.5(3)
C2 O2 V1 119.7(3)
C2 O2 V2 121.7(3)
V1 O2 V2 99.9(2)
C3 O3 V1 117.0(3)
C11 O4 V2 118.4(3)
C12 O5 V2 119.6(3)
C12 O5 V1 121.6(3)
V2 O5 V1 99.4(2)
C13 O6 V1 139.4(4)
O1 C1 C7 108.5(5)
O1 C1 C4 109.9(4)
C7 C1 C4 114.8(5)
O2 C2 C9 108.5(4)
O2 C2 C4 108.1(4)
C9 C2 C4 116.4(5)
O3 C3 C5 107.5(5)
O3 C3 C4 110.5(4)
C5 C3 C4 112.9(5)
C1 C4 C2 110.8(4)
C1 C4 C3 113.8(5)
C2 C4 C3 110.7(5)
C6 C5 C3 113.2(6)
C1 C7 C8 112.5(5)
C10 C9 C2 112.7(5)
O4 C11 C17 106.8(4)
O4 C11 C14 110.6(4)
C17 C11 C14 112.7(5)
O5 C12 C14 109.5(4)
O5 C12 C19 109.7(5)
C14 C12 C19 115.1(5)
O6 C13 C15 108.1(6)
O6 C13 C14 110.5(5)
C15 C13 C14 114.1(5)
C12 C14 C13 109.7(5)
C12 C14 C11 110.3(4)
C13 C14 C11 113.8(5)
C16 C15 C13 111.3(6)
C11 C17 C18 112.9(5)
C20 C19 C12 112.6(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
V1 O8 1.584(4)
V1 O6 1.774(4)
V1 O3 1.778(4)
V1 O2 1.968(4)
V1 O5 2.009(4)
V1 V2 3.0330(14)
V2 O7 1.585(4)
V2 O4 1.778(4)
V2 O1 1.785(4)
V2 O5 1.969(3)
V2 O2 1.995(3)
O1 C1 1.419(6)
O2 C2 1.456(6)
O3 C3 1.436(6)
O4 C11 1.434(6)
O5 C12 1.448(6)
O6 C13 1.412(7)
C1 C7 1.522(7)
C1 C4 1.526(7)
C2 C9 1.521(8)
C2 C4 1.519(7)
C3 C5 1.528(8)
C3 C4 1.556(7)
C5 C6 1.515(9)
C7 C8 1.515(8)
C9 C10 1.513(8)
C11 C17 1.511(8)
C11 C14 1.553(8)
C12 C14 1.517(8)
C12 C19 1.523(8)
C13 C15 1.531(9)
C13 C14 1.542(8)
C15 C16 1.517(11)
C17 C18 1.524(9)
C19 C20 1.485(9)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139107113
