#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:21:07 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179891 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/87/7018787.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_7018787
loop_
_publ_author_name
'Reytman, Lilia'
'Braitbard, Ori'
'Tshuva, Edit Y.'
_publ_section_title
;
 Highly cytotoxic vanadium(v) complexes of salan ligands; insights on the
 role of hydrolysis.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5241
_journal_page_last               5247
_journal_paper_doi               10.1039/c2dt11514j
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C44 H60 N4 O7 V2, 2(C7 H8)'
_chemical_formula_sum            'C58 H68 N4 O7 V2'
_chemical_formula_weight         1035.04
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 101.532(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7043(12)
_cell_length_b                   24.115(3)
_cell_length_c                   19.876(2)
_cell_measurement_temperature    173(1)
_cell_volume                     5496.7(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            29432
_diffrn_reflns_theta_full        28.18
_diffrn_reflns_theta_max         28.18
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.059
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.1199
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0842P)²+27.1252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2447
_refine_ls_wR_factor_ref         0.2613
_reflns_number_gt                4781
_reflns_number_total             6544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt11514j.txt
_cod_data_source_block           (L1VO)2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5496.8(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7018787
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
C1 C 0.3958(4) 0.4459(2) 0.8547(2) 0.0380(12) Uani 1 1 d .
C2 C 0.4713(5) 0.4007(2) 0.8697(3) 0.0374(11) Uani 1 1 d .
C3 C 0.4333(5) 0.3529(2) 0.8980(3) 0.0432(13) Uani 1 1 d .
H3 H 0.4847 0.3222 0.9081 0.052 Uiso 1 1 calc R
C4 C 0.3219(5) 0.3492(2) 0.9117(3) 0.0436(14) Uani 1 1 d .
C5 C 0.2486(5) 0.3940(3) 0.8960(3) 0.0462(14) Uani 1 1 d .
H5 H 0.1723 0.3918 0.9055 0.055 Uiso 1 1 calc R
C6 C 0.2818(5) 0.4425(3) 0.8668(3) 0.0421(13) Uani 1 1 d .
C7 C 0.1938(5) 0.4885(3) 0.8477(3) 0.0545(17) Uani 1 1 d .
H7A H 0.1509 0.4819 0.8002 0.065 Uiso 1 1 calc R
H7B H 0.1366 0.4860 0.8781 0.065 Uiso 1 1 calc R
C8 C 0.2990(5) 0.5603(3) 0.9231(3) 0.0499(16) Uani 1 1 d .
H8A H 0.3477 0.5286 0.9434 0.060 Uiso 1 1 calc R
H8B H 0.2392 0.5669 0.9511 0.060 Uiso 1 1 calc R
C9 C 0.3747(5) 0.6113(3) 0.9250(3) 0.0477(15) Uani 1 1 d .
H9A H 0.3258 0.6437 0.9071 0.057 Uiso 1 1 calc R
H9B H 0.4137 0.6194 0.9729 0.057 Uiso 1 1 calc R
C10 C 0.5139(4) 0.6550(3) 0.8636(3) 0.0449(14) Uani 1 1 d .
H10A H 0.5738 0.6463 0.8364 0.054 Uiso 1 1 calc R
H10B H 0.5541 0.6734 0.9064 0.054 Uiso 1 1 calc R
C11 C 0.4288(4) 0.6956(2) 0.8236(3) 0.0381(12) Uani 1 1 d .
C12 C 0.4480(5) 0.7529(3) 0.8326(3) 0.0482(15) Uani 1 1 d .
H12 H 0.5149 0.7650 0.8646 0.058 Uiso 1 1 calc R
C13 C 0.3746(5) 0.7924(3) 0.7971(3) 0.0486(14) Uani 1 1 d .
C14 C 0.2754(6) 0.7742(3) 0.7520(3) 0.0494(14) Uani 1 1 d .
H14 H 0.2222 0.8007 0.7282 0.059 Uiso 1 1 calc R
C15 C 0.2524(5) 0.7178(2) 0.7408(3) 0.0414(12) Uani 1 1 d .
C16 C 0.3304(4) 0.6781(2) 0.7753(2) 0.0333(11) Uani 1 1 d .
C17 C 0.5940(5) 0.4051(3) 0.8554(4) 0.0515(15) Uani 1 1 d .
H17A H 0.6386 0.4324 0.8865 0.077 Uiso 1 1 calc R
H17B H 0.5898 0.4167 0.8078 0.077 Uiso 1 1 calc R
H17C H 0.6325 0.3689 0.8629 0.077 Uiso 1 1 calc R
C18 C 0.2827(7) 0.2972(3) 0.9438(4) 0.0648(19) Uani 1 1 d .
H18A H 0.2350 0.3076 0.9771 0.097 Uiso 1 1 calc R
H18B H 0.3512 0.2764 0.9672 0.097 Uiso 1 1 calc R
H18C H 0.2366 0.2740 0.9078 0.097 Uiso 1 1 calc R
C19 C 0.1385(5) 0.5831(3) 0.8290(3) 0.0588(18) Uani 1 1 d .
H19A H 0.0782 0.5746 0.8554 0.088 Uiso 1 1 calc R
H19B H 0.1071 0.5772 0.7800 0.088 Uiso 1 1 calc R
H19C H 0.1629 0.6218 0.8368 0.088 Uiso 1 1 calc R
C20 C 0.5626(5) 0.5689(3) 0.9214(3) 0.0560(18) Uani 1 1 d .
H20A H 0.6024 0.5903 0.9611 0.084 Uiso 1 1 calc R
H20B H 0.6177 0.5605 0.8916 0.084 Uiso 1 1 calc R
H20C H 0.5330 0.5342 0.9372 0.084 Uiso 1 1 calc R
C21 C 0.3974(7) 0.8543(3) 0.8085(4) 0.070(2) Uani 1 1 d .
H21A H 0.3588 0.8674 0.8450 0.106 Uiso 1 1 calc R
H21B H 0.3665 0.8744 0.7660 0.106 Uiso 1 1 calc R
H21C H 0.4815 0.8608 0.8220 0.106 Uiso 1 1 calc R
C22 C 0.1454(6) 0.6991(3) 0.6905(3) 0.0572(17) Uani 1 1 d .
H22A H 0.1018 0.6725 0.7129 0.086 Uiso 1 1 calc R
H22B H 0.1689 0.6814 0.6510 0.086 Uiso 1 1 calc R
H22C H 0.0960 0.7312 0.6748 0.086 Uiso 1 1 calc R
C23 C 0.2949(12) 0.7662(6) 1.0070(8) 0.061(3) Uani 0.50 1 d P
C24 C 0.2457(8) 0.7333(3) 1.0559(5) 0.077(2) Uani 1 1 d .
C25 C 0.1439(15) 0.7003(7) 1.0183(9) 0.071(4) Uani 0.50 1 d P
C26 C 0.1027(8) 0.6987(4) 0.9549(6) 0.089(3) Uani 1 1 d .
C27 C 0.1521(15) 0.7329(7) 0.9093(7) 0.071(4) Uani 0.50 1 d P
C28 C -0.1019(14) 0.5065(11) 0.4307(9) 0.189(9) Uani 1 1 d .
C29 C -0.0319(8) 0.5445(5) 0.4689(5) 0.093(4) Uani 1 1 d .
C30 C 0.0568(13) 0.5477(9) 0.5278(8) 0.170(7) Uani 1 1 d .
C31 C 0.1232(11) 0.5670(11) 0.5650(8) 0.086(7) Uani 0.50 1 d P
N1 N 0.2404(4) 0.5461(2) 0.8516(2) 0.0432(12) Uani 1 1 d .
N2 N 0.4637(4) 0.6018(2) 0.8824(2) 0.0393(11) Uani 1 1 d .
O1 O 0.4372(3) 0.49246(15) 0.83111(18) 0.0399(9) Uani 1 1 d .
O2 O 0.3069(3) 0.62469(14) 0.75977(16) 0.0331(8) Uani 1 1 d .
O3 O 0.5000 0.56696(19) 0.7500 0.0308(10) Uani 1 2 d S
O4 O 0.2800(3) 0.52177(15) 0.72286(18) 0.0404(9) Uani 1 1 d .
V1 V 0.36986(7) 0.55388(4) 0.78133(4) 0.0280(2) Uani 1 1 d .
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'
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
O1 C1 C2 118.0(4) . .
O1 C1 C6 122.0(5) . .
C2 C1 C6 120.0(5) . .
C3 C2 C1 119.5(5) . .
C3 C2 C17 121.4(5) . .
C1 C2 C17 119.1(5) . .
C4 C3 C2 121.3(6) . .
C4 C3 H3 119.3 . .
C2 C3 H3 119.3 . .
C5 C4 C3 118.3(5) . .
C5 C4 C18 121.1(6) . .
C3 C4 C18 120.6(6) . .
C4 C5 C6 122.6(5) . .
C4 C5 H5 118.7 . .
C6 C5 H5 118.7 . .
C5 C6 C1 118.3(5) . .
C5 C6 C7 119.2(5) . .
C1 C6 C7 122.6(5) . .
N1 C7 C6 116.6(5) . .
N1 C7 H7A 108.2 . .
C6 C7 H7A 108.2 . .
N1 C7 H7B 108.2 . .
C6 C7 H7B 108.2 . .
H7A C7 H7B 107.3 . .
N1 C8 C9 111.5(4) . .
N1 C8 H8A 109.3 . .
C9 C8 H8A 109.3 . .
N1 C8 H8B 109.3 . .
C9 C8 H8B 109.3 . .
H8A C8 H8B 108.0 . .
N2 C9 C8 109.5(5) . .
N2 C9 H9A 109.8 . .
C8 C9 H9A 109.8 . .
N2 C9 H9B 109.8 . .
C8 C9 H9B 109.8 . .
H9A C9 H9B 108.2 . .
N2 C10 C11 116.1(4) . .
N2 C10 H10A 108.3 . .
C11 C10 H10A 108.3 . .
N2 C10 H10B 108.3 . .
C11 C10 H10B 108.3 . .
H10A C10 H10B 107.4 . .
C12 C11 C16 118.0(5) . .
C12 C11 C10 120.0(5) . .
C16 C11 C10 121.9(5) . .
C13 C12 C11 123.1(5) . .
C13 C12 H12 118.4 . .
C11 C12 H12 118.4 . .
C12 C13 C14 117.9(6) . .
C12 C13 C21 121.8(6) . .
C14 C13 C21 120.2(6) . .
C13 C14 C15 121.3(6) . .
C13 C14 H14 119.4 . .
C15 C14 H14 119.4 . .
C14 C15 C16 120.1(5) . .
C14 C15 C22 120.4(5) . .
C16 C15 C22 119.5(5) . .
O2 C16 C15 117.4(4) . .
O2 C16 C11 123.2(5) . .
C15 C16 C11 119.4(5) . .
C2 C17 H17A 109.5 . .
C2 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C2 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C4 C18 H18A 109.5 . .
C4 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C4 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
N1 C19 H19A 109.5 . .
N1 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
N1 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
N2 C20 H20A 109.5 . .
N2 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
N2 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C13 C21 H21A 109.5 . .
C13 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C13 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C15 C22 H22A 109.5 . .
C15 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C15 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C24 C23 C25 73.9(13) 7_567 7_567
C24 C23 C23 70.1(14) 7_567 7_567
C25 C23 C23 144(2) 7_567 7_567
C24 C23 C24 123.5(12) 7_567 .
C25 C23 C24 162.5(17) 7_567 .
C23 C23 C24 53.5(12) 7_567 .
C24 C23 C26 126.2(13) 7_567 7_567
C25 C23 C26 52.3(10) 7_567 7_567
C23 C23 C26 163(2) 7_567 7_567
C24 C23 C26 110.2(13) . 7_567
C24 C23 C27 178.6(13) 7_567 7_567
C25 C23 C27 105.4(15) 7_567 7_567
C23 C23 C27 110.6(19) 7_567 7_567
C24 C23 C27 57.1(10) . 7_567
C26 C23 C27 53.1(9) 7_567 7_567
C23 C24 C23 56.5(12) 7_567 .
C23 C24 C27 124.5(11) 7_567 7_567
C23 C24 C27 68.0(9) . 7_567
C23 C24 C25 53.2(10) 7_567 .
C23 C24 C25 109.6(12) . .
C27 C24 C25 177.6(11) 7_567 .
C23 C25 C26 75.7(13) 7_567 .
C23 C25 C24 52.9(10) 7_567 .
C26 C25 C24 128.6(13) . .
C25 C26 C27 119.6(12) . .
C25 C26 C23 52.0(10) . 7_567
C27 C26 C23 67.6(10) . 7_567
C26 C27 C24 114.1(11) . 7_567
C26 C27 C23 59.3(8) . 7_567
C24 C27 C23 54.9(8) 7_567 7_567
C29 C28 C30 99.5(16) . 5_566
C29 C28 C31 135.7(15) . 5_566
C30 C28 C31 36.2(9) 5_566 5_566
C28 C29 C30 140.1(14) . .
C31 C30 C29 156(3) . .
C31 C30 C28 83.0(19) . 5_566
C29 C30 C28 120.4(19) . 5_566
C30 C31 C28 60.8(17) . 5_566
C19 N1 C8 109.8(5) . .
C19 N1 C7 106.3(5) . .
C8 N1 C7 111.0(5) . .
C19 N1 V1 111.1(3) . .
C8 N1 V1 109.4(3) . .
C7 N1 V1 109.2(3) . .
C9 N2 C20 110.3(4) . .
C9 N2 C10 111.5(4) . .
C20 N2 C10 106.6(5) . .
C9 N2 V1 107.3(3) . .
C20 N2 V1 111.1(3) . .
C10 N2 V1 110.2(3) . .
C1 O1 V1 134.8(3) . .
C16 O2 V1 140.3(3) . .
V1 O3 V1 159.6(3) 2_656 .
O4 V1 O3 108.34(15) . .
O4 V1 O1 98.48(19) . .
O3 V1 O1 91.48(15) . .
O4 V1 O2 95.93(17) . .
O3 V1 O2 94.77(17) . .
O1 V1 O2 161.62(16) . .
O4 V1 N1 89.09(18) . .
O3 V1 N1 162.28(13) . .
O1 V1 N1 82.58(15) . .
O2 V1 N1 86.32(16) . .
O4 V1 N2 165.78(17) . .
O3 V1 N2 85.81(13) . .
O1 V1 N2 82.15(17) . .
O2 V1 N2 81.09(15) . .
N1 V1 N2 76.87(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.344(6) .
C1 C2 1.397(7) .
C1 C6 1.404(7) .
C2 C3 1.394(7) .
C2 C17 1.522(7) .
C3 C4 1.387(8) .
C3 H3 0.9500 .
C4 C5 1.375(9) .
C4 C18 1.520(8) .
C5 C6 1.396(8) .
C5 H5 0.9500 .
C6 C7 1.510(8) .
C7 N1 1.488(8) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 N1 1.488(7) .
C8 C9 1.513(9) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 N2 1.485(6) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 N2 1.490(8) .
C10 C11 1.507(8) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.406(8) .
C11 C16 1.408(7) .
C12 C13 1.377(9) .
C12 H12 0.9500 .
C13 C14 1.388(8) .
C13 C21 1.525(9) .
C14 C15 1.396(8) .
C14 H14 0.9500 .
C15 C16 1.404(7) .
C15 C22 1.508(8) .
C16 O2 1.340(6) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
C19 N1 1.485(7) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 N2 1.487(6) .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 C24 1.247(17) 7_567
C23 C25 1.25(2) 7_567
C23 C23 1.29(3) 7_567
C23 C24 1.459(18) .
C23 C26 1.538(17) 7_567
C23 C27 1.65(2) 7_567
C24 C23 1.247(17) 7_567
C24 C27 1.498(19) 7_567
C24 C25 1.501(19) .
C25 C23 1.25(2) 7_567
C25 C26 1.256(18) .
C26 C27 1.430(19) .
C26 C23 1.538(17) 7_567
C27 C24 1.498(19) 7_567
C27 C23 1.65(2) 7_567
C28 C29 1.36(2) .
C28 C30 1.58(2) 5_566
C28 C31 1.79(3) 5_566
C29 C30 1.403(18) .
C30 C31 1.07(2) .
C30 C28 1.58(2) 5_566
C31 C28 1.79(3) 5_566
N1 V1 2.264(4) .
N2 V1 2.387(4) .
O1 V1 1.866(3) .
O2 V1 1.875(3) .
O3 V1 1.7851(11) 2_656
O3 V1 1.7851(11) .
O4 V1 1.603(4) .
