#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/75/4317532.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_4317532
loop_
_publ_author_name
'B. Cashin'
'D. Cunningham'
'P. Daly'
'P. McArdle'
'M. Munroe'
'N. Ní Chonchubhair'
_publ_section_title
;
 Donor Properties of the Vanadyl Ion: Reactions of Vanadyl Salicylaldimine
 β-Ketimine and Acetylacetonato Complexes with Groups 14 and 15 Lewis
 Acids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              773
_journal_page_last               782
_journal_paper_doi               10.1021/ic010366s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C30 H28 Cl2 N2 O6 Sn V'
_chemical_formula_weight         753.07
_chemical_name_common            SnPh2Cl2.VO(vanen).H2O
_chemical_name_systematic
;
  Diphenyltin 
dichloride.[N,N'-bis(3-methoxysalicylidene)ethane-1,2-diaminato]monoaq 
ua oxovanadium(IV) (1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.8000(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.986(2)
_cell_length_b                   21.584(2)
_cell_length_c                   12.110(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     3439.6(8)
_computing_cell_refinement       'CELDIM in CAD4-PC-Software'
_computing_data_collection       'CAD4-PC-Software (Enraf-Nonius, 1992)'
_computing_data_reduction        'XCAD (McArdle & Higgins, 1995)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.888
_diffrn_measured_fraction_theta_max 0.888
_diffrn_measurement_device_type  '4-circle diffractometer'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0095
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3907
_diffrn_reflns_theta_full        21.98
_diffrn_reflns_theta_max         21.98
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    1.194
_exptl_crystal_colour            Golden
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.229
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         3736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1275P)²+29.6026P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2291
_reflns_number_gt                3296
_reflns_number_total             3736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010366s_4.cif
_cod_data_source_block           SnPh2Cl2.VO(vanen).H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        3439.5(8)
_cod_database_code               4317532
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.55320(5) 0.40891(3) 0.74885(6) 0.0387(4) Uani 1 1 d . . .
V1 V 0.82267(13) 0.48456(8) 0.85194(14) 0.0312(5) Uani 1 1 d . . .
Cl1 Cl 0.3768(2) 0.37529(17) 0.6521(3) 0.0679(10) Uani 1 1 d . . .
Cl2 Cl 0.5873(3) 0.40288(17) 0.5727(3) 0.0675(10) Uani 1 1 d . . .
O1 O 0.9214(5) 0.4203(3) 0.9150(6) 0.0363(17) Uani 1 1 d . . .
O2 O 0.8458(5) 0.5237(3) 1.0017(6) 0.0367(17) Uani 1 1 d . . .
O3 O 0.9991(6) 0.3254(3) 1.0425(7) 0.050(2) Uani 1 1 d . . .
O4 O 0.8797(7) 0.5457(4) 1.2220(6) 0.054(2) Uani 1 1 d . . .
O5 O 0.7174(5) 0.4455(3) 0.8281(6) 0.0395(17) Uani 1 1 d . . .
O6 O 0.9669(5) 0.5388(3) 0.8606(6) 0.0397(17) Uani 1 1 d . . .
N1 N 0.8357(7) 0.4695(4) 0.6903(7) 0.041(2) Uani 1 1 d . . .
N2 N 0.7582(7) 0.5654(4) 0.7707(8) 0.044(2) Uani 1 1 d . . .
C1 C 0.8180(8) 0.5786(5) 1.0277(10) 0.037(3) Uani 1 1 d . . .
C2 C 0.8340(9) 0.5919(5) 1.1468(10) 0.043(3) Uani 1 1 d . . .
C3 C 0.8057(10) 0.6486(7) 1.1787(12) 0.063(4) Uani 1 1 d . . .
H1 H 0.8163 0.6568 1.2573 0.050 Uiso 1 1 calc R . .
C4 C 0.7624(11) 0.6929(6) 1.0958(14) 0.069(4) Uani 1 1 d . . .
H2 H 0.7447 0.7310 1.1192 0.050 Uiso 1 1 calc R . .
C5 C 0.7448(10) 0.6822(6) 0.9807(13) 0.059(3) Uani 1 1 d . . .
H3 H 0.7146 0.7127 0.9257 0.050 Uiso 1 1 calc R . .
C6 C 0.7724(9) 0.6243(5) 0.9435(10) 0.046(3) Uani 1 1 d . . .
C7 C 0.7453(9) 0.6154(5) 0.8205(10) 0.046(3) Uani 1 1 d . . .
H4 H 0.7158 0.6487 0.7722 0.050 Uiso 1 1 calc R . .
C8 C 0.7243(10) 0.5596(6) 0.6417(10) 0.059(4) Uani 1 1 d . . .
H5 H 0.7166 0.6003 0.6059 0.050 Uiso 1 1 calc R . .
H6 H 0.6592 0.5386 0.6131 0.050 Uiso 1 1 calc R . .
C9 C 0.8031(10) 0.5230(6) 0.6102(10) 0.053(3) Uani 1 1 d . . .
H7 H 0.7748 0.5085 0.5298 0.050 Uiso 1 1 calc R . .
H8 H 0.8611 0.5491 0.6165 0.050 Uiso 1 1 calc R . .
C10 C 0.8633(9) 0.4184(6) 0.6579(9) 0.045(3) Uani 1 1 d . . .
H9 H 0.8570 0.4143 0.5793 0.050 Uiso 1 1 calc R . .
C11 C 0.9035(8) 0.3667(5) 0.7341(9) 0.040(3) Uani 1 1 d . . .
C12 C 0.9194(10) 0.3108(6) 0.6840(11) 0.059(3) Uani 1 1 d . . .
H10 H 0.9026 0.3085 0.6029 0.050 Uiso 1 1 calc R . .
C13 C 0.9583(11) 0.2605(7) 0.7493(13) 0.070(4) Uani 1 1 d . . .
H11 H 0.9659 0.2238 0.7130 0.050 Uiso 1 1 calc R . .
C14 C 0.9869(10) 0.2633(6) 0.8707(12) 0.055(3) Uani 1 1 d . . .
H12 H 1.0146 0.2286 0.9156 0.050 Uiso 1 1 calc R . .
C15 C 0.9745(8) 0.3165(5) 0.9240(10) 0.042(3) Uani 1 1 d . . .
C16 C 0.9324(7) 0.3695(5) 0.8575(9) 0.034(2) Uani 1 1 d . . .
C18 C 1.0400(11) 0.2738(6) 1.1179(12) 0.067(4) Uani 1 1 d . . .
H13 H 1.0542 0.2860 1.1981 0.050 Uiso 1 1 calc R . .
H14 H 1.1017 0.2603 1.1071 0.050 Uiso 1 1 calc R . .
H15 H 0.9917 0.2405 1.0990 0.050 Uiso 1 1 calc R . .
C17 C 0.8884(12) 0.5524(8) 1.3410(11) 0.072(4) Uani 1 1 d . . .
H16 H 0.9227 0.5169 1.3846 0.050 Uiso 1 1 calc R . .
H17 H 0.8219 0.5557 1.3470 0.050 Uiso 1 1 calc R . .
H18 H 0.9267 0.5891 1.3725 0.050 Uiso 1 1 calc R . .
C19 C 0.5128(9) 0.4982(5) 0.7931(11) 0.050(3) Uani 1 1 d . . .
C20 C 0.5622(10) 0.5225(6) 0.9014(12) 0.057(3) Uani 1 1 d . . .
H19 H 0.6166 0.5012 0.9537 0.050 Uiso 1 1 calc R . .
C21 C 0.5319(13) 0.5789(7) 0.9344(15) 0.068(4) Uani 1 1 d . . .
H20 H 0.5621 0.5942 1.0101 0.050 Uiso 1 1 calc R . .
C22 C 0.4582(17) 0.6105(8) 0.855(2) 0.095(6) Uani 1 1 d . . .
H21 H 0.4389 0.6486 0.8762 0.050 Uiso 1 1 calc R . .
C23 C 0.4098(16) 0.5895(8) 0.743(2) 0.104(7) Uani 1 1 d . . .
H22 H 0.3595 0.6132 0.6899 0.050 Uiso 1 1 calc R . .
C24 C 0.4374(11) 0.5315(7) 0.7103(15) 0.074(4) Uani 1 1 d . . .
H23 H 0.4058 0.5159 0.6351 0.050 Uiso 1 1 calc R . .
C25 C 0.6010(8) 0.3274(5) 0.8510(9) 0.038(3) Uani 1 1 d . . .
C26 C 0.5325(10) 0.2946(5) 0.8871(10) 0.049(3) Uani 1 1 d . . .
H24 H 0.4662 0.3087 0.8691 0.050 Uiso 1 1 calc R . .
C27 C 0.5636(12) 0.2397(7) 0.9515(12) 0.068(4) Uani 1 1 d . . .
H25 H 0.5177 0.2175 0.9763 0.050 Uiso 1 1 calc R . .
C28 C 0.6612(12) 0.2187(7) 0.9778(13) 0.072(4) Uani 1 1 d . . .
H26 H 0.6818 0.1824 1.0210 0.050 Uiso 1 1 calc R . .
C29 C 0.7279(11) 0.2512(6) 0.9404(13) 0.069(4) Uani 1 1 d . . .
H27 H 0.7937 0.2364 0.9568 0.050 Uiso 1 1 calc R . .
C30 C 0.6989(9) 0.3058(6) 0.8782(11) 0.056(3) Uani 1 1 d . . .
H28 H 0.7457 0.3280 0.8548 0.050 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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
C25 Sn1 C19 131.4(4) . . ?
C25 Sn1 O5 88.2(3) . . ?
C19 Sn1 O5 84.1(4) . . ?
C25 Sn1 Cl2 111.3(3) . . ?
C19 Sn1 Cl2 115.7(3) . . ?
O5 Sn1 Cl2 85.2(2) . . ?
C25 Sn1 Cl1 95.8(3) . . ?
C19 Sn1 Cl1 94.5(3) . . ?
O5 Sn1 Cl1 175.71(19) . . ?
Cl2 Sn1 Cl1 91.76(13) . . ?
O5 V1 O1 100.4(3) . . ?
O5 V1 O2 104.2(3) . . ?
O1 V1 O2 94.2(3) . . ?
O5 V1 N1 96.7(4) . . ?
O1 V1 N1 88.9(3) . . ?
O2 V1 N1 157.9(3) . . ?
O5 V1 N2 97.5(4) . . ?
O1 V1 N2 160.4(4) . . ?
O2 V1 N2 89.1(3) . . ?
N1 V1 N2 81.0(4) . . ?
O5 V1 O6 172.8(3) . . ?
O1 V1 O6 81.3(3) . . ?
O2 V1 O6 82.5(3) . . ?
N1 V1 O6 76.3(3) . . ?
N2 V1 O6 80.0(3) . . ?
C16 O1 V1 125.4(6) . . ?
C1 O2 V1 130.5(6) . . ?
C15 O3 C18 117.6(10) . . ?
C2 O4 C17 117.9(10) . . ?
V1 O5 Sn1 163.6(4) . . ?
C10 N1 C9 122.2(9) . . ?
C10 N1 V1 124.4(7) . . ?
C9 N1 V1 113.3(8) . . ?
C7 N2 C8 121.7(10) . . ?
C7 N2 V1 126.9(8) . . ?
C8 N2 V1 111.4(8) . . ?
O2 C1 C6 123.7(10) . . ?
O2 C1 C2 118.0(10) . . ?
C6 C1 C2 118.3(10) . . ?
O4 C2 C3 125.3(11) . . ?
O4 C2 C1 114.4(10) . . ?
C3 C2 C1 120.3(11) . . ?
C4 C3 C2 120.7(12) . . ?
C5 C4 C3 121.2(13) . . ?
C4 C5 C6 120.1(12) . . ?
C1 C6 C7 124.1(11) . . ?
C1 C6 C5 119.4(11) . . ?
C7 C6 C5 116.4(11) . . ?
N2 C7 C6 125.3(10) . . ?
N2 C8 C9 108.2(9) . . ?
N1 C9 C8 109.4(10) . . ?
N1 C10 C11 124.7(10) . . ?
C12 C11 C16 117.7(11) . . ?
C12 C11 C10 118.4(10) . . ?
C16 C11 C10 123.8(10) . . ?
C13 C12 C11 122.2(12) . . ?
C12 C13 C14 120.1(13) . . ?
C15 C14 C13 120.3(12) . . ?
C14 C15 O3 126.1(10) . . ?
C14 C15 C16 120.7(10) . . ?
O3 C15 C16 113.2(10) . . ?
O1 C16 C15 117.9(9) . . ?
O1 C16 C11 123.0(9) . . ?
C15 C16 C11 119.1(10) . . ?
C20 C19 C24 120.7(13) . . ?
C20 C19 Sn1 120.0(9) . . ?
C24 C19 Sn1 119.3(10) . . ?
C19 C20 C21 120.6(14) . . ?
C22 C21 C20 118.3(16) . . ?
C21 C22 C23 123.2(17) . . ?
C22 C23 C24 118.8(17) . . ?
C19 C24 C23 118.1(17) . . ?
C30 C25 C26 119.6(11) . . ?
C30 C25 Sn1 120.7(8) . . ?
C26 C25 Sn1 119.7(8) . . ?
C25 C26 C27 119.5(12) . . ?
C28 C27 C26 120.4(13) . . ?
C29 C28 C27 119.5(13) . . ?
C28 C29 C30 120.8(14) . . ?
C25 C30 C29 120.2(12) . . ?
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
Sn1 C25 2.125(10) . ?
Sn1 C19 2.128(12) . ?
Sn1 O5 2.308(7) . ?
Sn1 Cl2 2.342(3) . ?
Sn1 Cl1 2.456(3) . ?
V1 O5 1.635(7) . ?
V1 O1 1.923(7) . ?
V1 O2 1.926(7) . ?
V1 N1 2.052(9) . ?
V1 N2 2.056(9) . ?
V1 O6 2.304(7) . ?
O1 C16 1.337(12) . ?
O2 C1 1.318(12) . ?
O3 C15 1.371(13) . ?
O3 C18 1.431(14) . ?
O4 C2 1.356(14) . ?
O4 C17 1.412(15) . ?
N1 C10 1.273(15) . ?
N1 C9 1.477(14) . ?
N2 C7 1.277(15) . ?
N2 C8 1.477(15) . ?
C1 C6 1.406(16) . ?
C1 C2 1.412(16) . ?
C2 C3 1.381(17) . ?
C3 C4 1.370(19) . ?
C4 C5 1.35(2) . ?
C5 C6 1.426(17) . ?
C6 C7 1.421(17) . ?
C8 C9 1.507(19) . ?
C10 C11 1.436(16) . ?
C11 C12 1.401(17) . ?
C11 C16 1.411(15) . ?
C12 C13 1.35(2) . ?
C13 C14 1.388(19) . ?
C14 C15 1.357(17) . ?
C15 C16 1.407(15) . ?
C19 C20 1.364(17) . ?
C19 C24 1.384(18) . ?
C20 C21 1.390(19) . ?
C21 C22 1.34(3) . ?
C22 C23 1.37(3) . ?
C23 C24 1.41(2) . ?
C25 C30 1.376(17) . ?
C25 C26 1.376(16) . ?
C26 C27 1.403(19) . ?
C27 C28 1.37(2) . ?
C28 C29 1.36(2) . ?
C29 C30 1.384(18) . ?
