#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/29/7012978.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_7012978
loop_
_publ_author_name
'Neculai, Dante'
'Mirela Neculai, Ana'
'Roesky, Herbert W.'
'Herbst-Irmer, Regine'
'Walfort, Bernhard'
'Stalke, Dietmar'
_publ_section_title
;
 Vanadium complexes incorporating the ?-diketiminato ligand L.
 Syntheses and structures of LV(OSO2CF3)2 and LVPPh2
;
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              2831
_journal_paper_doi               10.1039/b303196a
_journal_year                    2003
_chemical_formula_sum            'C33 H51 F6 N4 O6 S2 V'
_chemical_formula_weight         828.84
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 97.774(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.329(2)
_cell_length_b                   13.388(2)
_cell_length_c                   19.652(3)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      2.16
_cell_volume                     3996.0(10)
_computing_cell_refinement       'SAINT-NT V5/6.0'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SAINT-NT V5/6.0'
_computing_molecular_graphics    'XP in SHELXTL-97'
_computing_publication_material  'XP in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.918
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_device_type  'Bruker Smart Apex CCD'
_diffrn_measurement_method       'omega 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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30036
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.34
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.8480
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs2
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         9058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0740P)²+1.6935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                6850
_reflns_number_total             9058
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303196a.txt
_cod_data_source_block           2
_cod_original_cell_volume        3995.8(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7012978
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.17187(2) 0.93504(3) 0.327204(19) 0.02805(11) Uani 1 1 d . . .
C1 C 0.0058(2) 1.1565(2) 0.41511(16) 0.0570(7) Uani 1 1 d . . .
H1A H 0.0544 1.1901 0.4438 0.085 Uiso 1 1 calc R . .
H1B H -0.0422 1.1440 0.4423 0.085 Uiso 1 1 calc R . .
H1C H -0.0156 1.1991 0.3758 0.085 Uiso 1 1 calc R . .
C2 C 0.03785(16) 1.05840(18) 0.38965(12) 0.0391(5) Uani 1 1 d . . .
C3 C -0.01186(16) 0.9734(2) 0.40034(13) 0.0447(6) Uani 1 1 d . . .
H3 H -0.0631 0.9840 0.4218 0.054 Uiso 1 1 calc R . .
C4 C 0.00553(15) 0.87408(19) 0.38290(12) 0.0391(5) Uani 1 1 d . . .
C5 C -0.06295(18) 0.7970(2) 0.39490(16) 0.0573(7) Uani 1 1 d . . .
H5A H -0.0836 0.7628 0.3516 0.086 Uiso 1 1 calc R . .
H5B H -0.1127 0.8302 0.4120 0.086 Uiso 1 1 calc R . .
H5C H -0.0369 0.7482 0.4289 0.086 Uiso 1 1 calc R . .
N1 N 0.10877(13) 1.05506(13) 0.35779(10) 0.0351(4) Uani 1 1 d . . .
C6 C 0.14885(18) 1.15185(18) 0.34342(16) 0.0507(7) Uani 1 1 d . . .
H6A H 0.1883 1.1746 0.3846 0.061 Uiso 1 1 calc R . .
H6B H 0.1021 1.2026 0.3324 0.061 Uiso 1 1 calc R . .
C7 C 0.20074(17) 1.14117(18) 0.28376(14) 0.0452(6) Uani 1 1 d . . .
H7A H 0.1601 1.1273 0.2413 0.054 Uiso 1 1 calc R . .
H7B H 0.2319 1.2045 0.2772 0.054 Uiso 1 1 calc R . .
N2 N 0.26594(12) 1.05822(13) 0.29667(10) 0.0334(4) Uani 1 1 d . . .
C8 C 0.33673(17) 1.09072(19) 0.35211(13) 0.0433(6) Uani 1 1 d . . .
H8A H 0.3118 1.0929 0.3960 0.052 Uiso 1 1 calc R . .
H8B H 0.3547 1.1595 0.3418 0.052 Uiso 1 1 calc R . .
C9 C 0.41794(17) 1.0254(2) 0.36171(16) 0.0568(7) Uani 1 1 d . . .
H9A H 0.4007 0.9559 0.3679 0.085 Uiso 1 1 calc R . .
H9B H 0.4573 1.0475 0.4024 0.085 Uiso 1 1 calc R . .
H9C H 0.4484 1.0305 0.3211 0.085 Uiso 1 1 calc R . .
C10 C 0.30383(19) 1.0402(2) 0.23085(13) 0.0473(6) Uani 1 1 d . . .
H10A H 0.2550 1.0221 0.1947 0.057 Uiso 1 1 calc R . .
H10B H 0.3438 0.9819 0.2377 0.057 Uiso 1 1 calc R . .
C11 C 0.3542(2) 1.1267(2) 0.20474(16) 0.0662(9) Uani 1 1 d . . .
H11A H 0.3147 1.1841 0.1952 0.099 Uiso 1 1 calc R . .
H11B H 0.3769 1.1068 0.1625 0.099 Uiso 1 1 calc R . .
H11C H 0.4034 1.1452 0.2397 0.099 Uiso 1 1 calc R . .
N3 N 0.07820(12) 0.84744(14) 0.35780(10) 0.0341(4) Uani 1 1 d . . .
C12 C 0.09128(17) 0.73961(18) 0.34644(15) 0.0473(6) Uani 1 1 d . . .
H12A H 0.0589 0.7197 0.3014 0.057 Uiso 1 1 calc R . .
H12B H 0.0676 0.7006 0.3826 0.057 Uiso 1 1 calc R . .
C13 C 0.18764(17) 0.71752(17) 0.34794(14) 0.0440(6) Uani 1 1 d . . .
H13A H 0.2184 0.7293 0.3949 0.053 Uiso 1 1 calc R . .
H13B H 0.1952 0.6462 0.3366 0.053 Uiso 1 1 calc R . .
N4 N 0.22859(12) 0.78102(13) 0.29823(10) 0.0351(4) Uani 1 1 d . . .
C14 C 0.19767(17) 0.74205(18) 0.22734(13) 0.0439(6) Uani 1 1 d . . .
H14A H 0.1335 0.7538 0.2170 0.053 Uiso 1 1 calc R . .
H14B H 0.2072 0.6689 0.2273 0.053 Uiso 1 1 calc R . .
C15 C 0.24186(19) 0.7875(2) 0.17046(14) 0.0517(7) Uani 1 1 d . . .
H15A H 0.2349 0.8602 0.1709 0.078 Uiso 1 1 calc R . .
H15B H 0.2147 0.7610 0.1261 0.078 Uiso 1 1 calc R . .
H15C H 0.3046 0.7706 0.1775 0.078 Uiso 1 1 calc R . .
C16 C 0.32653(15) 0.77397(18) 0.31418(13) 0.0413(6) Uani 1 1 d . . .
H16A H 0.3438 0.7976 0.3618 0.050 Uiso 1 1 calc R . .
H16B H 0.3527 0.8205 0.2834 0.050 Uiso 1 1 calc R . .
C17 C 0.36726(19) 0.6707(2) 0.30742(17) 0.0579(8) Uani 1 1 d . . .
H17A H 0.3447 0.6243 0.3395 0.087 Uiso 1 1 calc R . .
H17B H 0.4315 0.6753 0.3181 0.087 Uiso 1 1 calc R . .
H17C H 0.3517 0.6462 0.2603 0.087 Uiso 1 1 calc R . .
O1 O 0.25431(10) 0.91996(11) 0.41855(8) 0.0329(3) Uani 1 1 d . . .
S1 S 0.23847(4) 0.92063(5) 0.49084(3) 0.03996(16) Uani 1 1 d . . .
O2 O 0.18897(14) 0.83755(19) 0.50903(10) 0.0732(7) Uani 1 1 d . . .
O3 O 0.21591(17) 1.01556(18) 0.51499(11) 0.0765(7) Uani 1 1 d . . .
C18 C 0.34913(18) 0.8959(3) 0.53247(14) 0.0560(7) Uani 1 1 d . . .
F1 F 0.35275(12) 0.89213(15) 0.60020(8) 0.0702(5) Uani 1 1 d . . .
F2 F 0.40186(14) 0.9700(2) 0.51905(11) 0.1152(10) Uani 1 1 d . . .
F3 F 0.37983(17) 0.8135(2) 0.51231(12) 0.1205(11) Uani 1 1 d . . .
O4 O 0.11319(10) 0.94475(11) 0.22653(8) 0.0348(4) Uani 1 1 d . . .
S2 S 0.01903(4) 0.94875(4) 0.19766(3) 0.03652(15) Uani 1 1 d . . .
O5 O -0.02466(11) 0.85464(13) 0.19993(10) 0.0486(4) Uani 1 1 d . . .
O6 O -0.02572(12) 1.03572(13) 0.21693(10) 0.0508(5) Uani 1 1 d . . .
C19 C 0.0284(2) 0.9677(2) 0.10673(14) 0.0520(7) Uani 1 1 d . . .
F4 F 0.07552(15) 1.04816(13) 0.09767(9) 0.0744(6) Uani 1 1 d . . .
F5 F 0.06607(13) 0.89057(13) 0.08023(8) 0.0659(5) Uani 1 1 d . . .
F6 F -0.05110(14) 0.98050(19) 0.07159(10) 0.0898(7) Uani 1 1 d . . .
C20 C 0.4916(2) 0.3539(3) 0.3215(2) 0.0894(12) Uani 1 1 d . . .
H20A H 0.5275 0.4145 0.3290 0.134 Uiso 1 1 calc R . .
H20B H 0.5158 0.3109 0.2883 0.134 Uiso 1 1 calc R . .
H20C H 0.4922 0.3182 0.3650 0.134 Uiso 1 1 calc R . .
C21 C 0.39843(19) 0.3820(2) 0.29388(16) 0.0535(7) Uani 1 1 d . . .
C22 C 0.33499(19) 0.3903(2) 0.33716(15) 0.0506(6) Uani 1 1 d . . .
H22 H 0.3507 0.3784 0.3849 0.061 Uiso 1 1 calc R . .
C23 C 0.24892(19) 0.4155(2) 0.31242(17) 0.0544(7) Uani 1 1 d . . .
H23 H 0.2065 0.4213 0.3433 0.065 Uiso 1 1 calc R . .
C24 C 0.2247(2) 0.4323(2) 0.24399(18) 0.0627(8) Uani 1 1 d . . .
H24 H 0.1655 0.4490 0.2272 0.075 Uiso 1 1 calc R . .
C25 C 0.2854(3) 0.4249(2) 0.19978(17) 0.0685(9) Uani 1 1 d . . .
H25 H 0.2684 0.4369 0.1522 0.082 Uiso 1 1 calc R . .
C26 C 0.3725(2) 0.3998(3) 0.22396(17) 0.0676(9) Uani 1 1 d . . .
H26 H 0.4144 0.3948 0.1927 0.081 Uiso 1 1 calc R . .
C27 C 0.2749(4) -0.0419(4) 0.0107(3) 0.127(2) Uani 1 1 d . . .
H27A H 0.2204 -0.0423 0.0317 0.190 Uiso 1 1 calc R . .
H27B H 0.3159 -0.0914 0.0337 0.190 Uiso 1 1 calc R . .
H27C H 0.2616 -0.0585 -0.0381 0.190 Uiso 1 1 calc R . .
C28 C 0.3148(3) 0.0568(3) 0.01812(17) 0.0777(11) Uani 1 1 d . . .
C29 C 0.2608(3) 0.1424(3) 0.01397(17) 0.0751(10) Uani 1 1 d . . .
H29 H 0.1986 0.1352 0.0068 0.090 Uiso 1 1 calc R . .
C30 C 0.2964(3) 0.2335(3) 0.02000(18) 0.0860(12) Uani 1 1 d . . .
H30 H 0.2590 0.2903 0.0172 0.103 Uiso 1 1 calc R . .
C31 C 0.3886(4) 0.2473(4) 0.0305(2) 0.1035(15) Uani 1 1 d . . .
H31 H 0.4136 0.3123 0.0350 0.124 Uiso 1 1 calc R . .
C32 C 0.4394(3) 0.1661(5) 0.0338(2) 0.1042(16) Uani 1 1 d . . .
H32 H 0.5016 0.1739 0.0399 0.125 Uiso 1 1 calc R . .
C33 C 0.4050(3) 0.0727(3) 0.02868(17) 0.0749(10) Uani 1 1 d . . .
H33 H 0.4435 0.0169 0.0324 0.090 Uiso 1 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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 V1 N1 89.13(8) . . ?
N3 V1 O1 93.50(7) . . ?
N1 V1 O1 94.65(7) . . ?
N3 V1 O4 95.01(7) . . ?
N1 V1 O4 94.10(7) . . ?
O1 V1 O4 167.89(6) . . ?
N3 V1 N2 170.49(7) . . ?
N1 V1 N2 81.39(7) . . ?
O1 V1 N2 88.03(6) . . ?
O4 V1 N2 85.00(6) . . ?
N3 V1 N4 82.09(7) . . ?
N1 V1 N4 171.20(7) . . ?
O1 V1 N4 85.49(6) . . ?
O4 V1 N4 87.15(6) . . ?
N2 V1 N4 107.40(7) . . ?
N1 C2 C3 122.7(2) . . ?
N1 C2 C1 120.6(2) . . ?
C3 C2 C1 116.7(2) . . ?
C2 C3 C4 127.3(2) . . ?
N3 C4 C3 122.7(2) . . ?
N3 C4 C5 120.7(2) . . ?
C3 C4 C5 116.6(2) . . ?
C2 N1 C6 116.69(19) . . ?
C2 N1 V1 128.80(16) . . ?
C6 N1 V1 114.50(15) . . ?
N1 C6 C7 110.0(2) . . ?
N2 C7 C6 110.4(2) . . ?
C7 N2 C8 108.10(18) . . ?
C7 N2 C10 107.5(2) . . ?
C8 N2 C10 110.25(19) . . ?
C7 N2 V1 98.48(13) . . ?
C8 N2 V1 115.67(14) . . ?
C10 N2 V1 115.64(14) . . ?
N2 C8 C9 115.3(2) . . ?
N2 C10 C11 116.1(2) . . ?
C4 N3 C12 117.16(19) . . ?
C4 N3 V1 128.66(16) . . ?
C12 N3 V1 114.07(15) . . ?
N3 C12 C13 110.01(19) . . ?
N4 C13 C12 111.9(2) . . ?
C16 N4 C13 109.00(19) . . ?
C16 N4 C14 110.76(18) . . ?
C13 N4 C14 107.49(19) . . ?
C16 N4 V1 113.62(13) . . ?
C13 N4 V1 98.02(13) . . ?
C14 N4 V1 116.80(14) . . ?
N4 C14 C15 115.4(2) . . ?
N4 C16 C17 116.7(2) . . ?
S1 O1 V1 132.67(10) . . ?
O3 S1 O2 117.12(16) . . ?
O3 S1 O1 114.10(12) . . ?
O2 S1 O1 113.68(11) . . ?
O3 S1 C18 105.58(16) . . ?
O2 S1 C18 104.08(14) . . ?
O1 S1 C18 99.68(11) . . ?
F3 C18 F1 108.0(3) . . ?
F3 C18 F2 108.8(3) . . ?
F1 C18 F2 106.5(3) . . ?
F3 C18 S1 112.2(2) . . ?
F1 C18 S1 111.7(2) . . ?
F2 C18 S1 109.4(2) . . ?
S2 O4 V1 130.27(10) . . ?
O6 S2 O5 117.79(12) . . ?
O6 S2 O4 113.99(10) . . ?
O5 S2 O4 113.14(10) . . ?
O6 S2 C19 104.49(13) . . ?
O5 S2 C19 104.57(12) . . ?
O4 S2 C19 100.26(12) . . ?
F4 C19 F5 107.9(3) . . ?
F4 C19 F6 107.7(2) . . ?
F5 C19 F6 108.3(2) . . ?
F4 C19 S2 111.16(19) . . ?
F5 C19 S2 111.87(19) . . ?
F6 C19 S2 109.7(2) . . ?
C22 C21 C26 117.5(3) . . ?
C22 C21 C20 120.8(3) . . ?
C26 C21 C20 121.8(3) . . ?
C21 C22 C23 121.3(3) . . ?
C24 C23 C22 120.3(3) . . ?
C25 C24 C23 120.0(3) . . ?
C24 C25 C26 120.3(3) . . ?
C25 C26 C21 120.5(3) . . ?
C33 C28 C29 116.7(4) . . ?
C33 C28 C27 123.5(5) . . ?
C29 C28 C27 119.8(5) . . ?
C30 C29 C28 120.5(4) . . ?
C29 C30 C31 121.5(4) . . ?
C32 C31 C30 117.8(5) . . ?
C31 C32 C33 122.0(5) . . ?
C32 C33 C28 121.6(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 N3 2.0080(18) . ?
V1 N1 2.0090(18) . ?
V1 O1 2.0606(16) . ?
V1 O4 2.0637(16) . ?
V1 N2 2.3223(18) . ?
V1 N4 2.3379(19) . ?
C1 C2 1.512(3) . ?
C2 N1 1.327(3) . ?
C2 C3 1.401(4) . ?
C3 C4 1.408(4) . ?
C4 N3 1.327(3) . ?
C4 C5 1.513(3) . ?
N1 C6 1.478(3) . ?
C6 C7 1.510(4) . ?
C7 N2 1.493(3) . ?
N2 C8 1.495(3) . ?
N2 C10 1.507(3) . ?
C8 C9 1.512(4) . ?
C10 C11 1.520(4) . ?
N3 C12 1.479(3) . ?
C12 C13 1.503(4) . ?
C13 N4 1.496(3) . ?
N4 C16 1.495(3) . ?
N4 C14 1.503(3) . ?
C14 C15 1.511(4) . ?
C16 C17 1.531(3) . ?
O1 S1 1.4733(16) . ?
S1 O3 1.416(2) . ?
S1 O2 1.419(2) . ?
S1 C18 1.811(3) . ?
C18 F3 1.283(4) . ?
C18 F1 1.326(3) . ?
C18 F2 1.328(4) . ?
O4 S2 1.4788(16) . ?
S2 O6 1.4283(18) . ?
S2 O5 1.4304(18) . ?
S2 C19 1.830(3) . ?
C19 F4 1.322(3) . ?
C19 F5 1.323(3) . ?
C19 F6 1.328(3) . ?
C20 C21 1.505(5) . ?
C21 C22 1.380(4) . ?
C21 C26 1.398(5) . ?
C22 C23 1.385(4) . ?
C23 C24 1.364(4) . ?
C24 C25 1.359(5) . ?
C25 C26 1.396(5) . ?
C27 C28 1.455(6) . ?
C28 C33 1.386(5) . ?
C28 C29 1.410(5) . ?
C29 C30 1.335(6) . ?
C30 C31 1.412(6) . ?
C31 C32 1.333(7) . ?
C32 C33 1.355(6) . ?
