#------------------------------------------------------------------------------
#$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $
#$Revision: 288183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/75/4317536.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_4317536
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            'C31 H30 Cl4 N2 O6 Pb V'
_chemical_formula_weight         926.50
_chemical_name_common            PbPh2Cl2.[VO(3-MeOsalen).H2O]
_chemical_name_systematic
;
  Diphenyllead 
dichloride.[N,N'-bis(3-methoxysalicylidene)ethane-1,2-diaminato]monoaq 
ua oxovanadium(IV) (1/1)
;
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.90(2)
_cell_angle_beta                 113.70(2)
_cell_angle_gamma                105.235(11)
_cell_formula_units_Z            2
_cell_length_a                   11.7273(14)
_cell_length_b                   13.1533(18)
_cell_length_c                   13.295(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     1720.1(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 0.629
_diffrn_measured_fraction_theta_max 0.629
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8305
_diffrn_reflns_theta_full        31.97
_diffrn_reflns_theta_max         31.97
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    5.513
_exptl_crystal_colour            Golden
_exptl_crystal_density_diffrn    1.789
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelepiped
_exptl_crystal_F_000             902
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         8.467
_refine_diff_density_min         -7.460
_refine_diff_density_rms         0.697
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.740
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         7512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.740
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.1710
_refine_ls_shift/su_max          0.289
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3825
_refine_ls_wR_factor_ref         0.4029
_reflns_number_gt                5372
_reflns_number_total             7512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010366s_8.cif
_cod_data_source_block           PbPh2Cl2.[VO(3-MeOsalen).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        1720.2(7)
_cod_original_sg_symbol_H-M      'P 1 21/c 1'
_cod_database_code               4317536
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pb1 Pb 0.06144(7) 0.45289(5) 0.36226(5) 0.0408(3) Uani 1 1 d . . .
V1 V 0.0568(3) 0.2063(2) 0.1097(2) 0.0343(6) Uani 1 1 d . . .
Cl1 Cl 0.1134(6) 0.6314(4) 0.5181(5) 0.0571(14) Uani 1 1 d . . .
Cl2 Cl 0.2115(6) 0.5718(5) 0.3009(5) 0.0606(14) Uani 1 1 d . . .
O1 O 0.0452(17) 0.2875(12) 0.2086(13) 0.052(4) Uani 1 1 d . . .
O2 O -0.1225(13) 0.0995(10) 0.0158(10) 0.045(3) Uani 1 1 d . . .
O3 O 0.1187(13) 0.1031(9) 0.1868(10) 0.040(3) Uani 1 1 d . . .
O4 O -0.3559(15) -0.0516(12) -0.0529(13) 0.054(4) Uani 1 1 d . . .
O5 O 0.1417(19) -0.0295(16) 0.3072(14) 0.067(5) Uani 1 1 d . . .
N1 N 0.0247(17) 0.2940(14) -0.0071(13) 0.044(4) Uani 1 1 d . . .
N2 N 0.2476(17) 0.2930(13) 0.1445(12) 0.042(3) Uani 1 1 d . . .
C1 C -0.229(2) 0.1052(14) -0.0702(13) 0.044(5) Uani 1 1 d . . .
C2 C -0.352(2) 0.0272(15) -0.1103(15) 0.043(4) Uani 1 1 d . . .
C3 C -0.467(3) 0.032(2) -0.1971(18) 0.058(6) Uani 1 1 d . . .
H3 H -0.5507 -0.0195 -0.2201 0.075 Uiso 1 1 calc R . .
C4 C -0.4540(19) 0.1142(18) -0.2483(17) 0.049(5) Uani 1 1 d . . .
H4 H -0.5297 0.1167 -0.3070 0.064 Uiso 1 1 calc R . .
C5 C -0.336(2) 0.1886(15) -0.2148(15) 0.048(5) Uani 1 1 d . . .
H5 H -0.3297 0.2439 -0.2498 0.063 Uiso 1 1 calc R . .
C6 C -0.217(2) 0.1873(14) -0.1261(15) 0.045(5) Uani 1 1 d . . .
C7 C -0.093(2) 0.2750(15) -0.0936(15) 0.047(5) Uani 1 1 d . . .
H7 H -0.0965 0.3229 -0.1378 0.061 Uiso 1 1 calc R . .
C8 C 0.138(2) 0.3879(19) 0.026(2) 0.053(5) Uani 1 1 d . . .
H8A H 0.1495 0.4449 0.0904 0.069 Uiso 1 1 calc R . .
H8B H 0.1261 0.4175 -0.0379 0.069 Uiso 1 1 calc R . .
C9 C 0.261(3) 0.354(2) 0.062(3) 0.094(12) Uani 1 1 d . . .
H9A H 0.2582 0.3066 -0.0041 0.122 Uiso 1 1 calc R . .
H9B H 0.3437 0.4189 0.0998 0.122 Uiso 1 1 calc R . .
C10 C 0.358(2) 0.2844(17) 0.221(2) 0.060(6) Uani 1 1 d . . .
H10 H 0.4399 0.3267 0.2284 0.077 Uiso 1 1 calc R . .
C11 C 0.357(2) 0.2118(16) 0.2923(17) 0.050(5) Uani 1 1 d . . .
C12 C 0.489(2) 0.2265(19) 0.3778(18) 0.054(5) Uani 1 1 d . . .
H12 H 0.5655 0.2800 0.3875 0.070 Uiso 1 1 calc R . .
C13 C 0.494(2) 0.1556(18) 0.444(2) 0.067(7) Uani 1 1 d . . .
H13 H 0.5761 0.1686 0.5070 0.088 Uiso 1 1 calc R . .
C14 C 0.381(3) 0.0647(19) 0.4217(19) 0.071(8) Uani 1 1 d . . .
H14 H 0.3916 0.0152 0.4639 0.092 Uiso 1 1 calc R . .
C15 C 0.255(3) 0.0490(17) 0.3363(15) 0.054(6) Uani 1 1 d . . .
C16 C 0.243(2) 0.1251(15) 0.2682(13) 0.042(4) Uani 1 1 d . . .
C17 C -0.479(3) -0.134(2) -0.087(3) 0.076(8) Uani 1 1 d . . .
H17A H -0.5203 -0.1079 -0.0430 0.106 Uiso 1 1 calc R . .
H17B H -0.4663 -0.1998 -0.0726 0.106 Uiso 1 1 calc R . .
H17C H -0.5367 -0.1494 -0.1677 0.106 Uiso 1 1 calc R . .
C18 C 0.143(4) -0.109(4) 0.368(3) 0.115(15) Uani 1 1 d . . .
H18A H 0.1898 -0.1538 0.3520 0.161 Uiso 1 1 calc R . .
H18B H 0.0521 -0.1561 0.3441 0.161 Uiso 1 1 calc R . .
H18C H 0.1862 -0.0713 0.4500 0.161 Uiso 1 1 calc R . .
C19 C -0.129(2) 0.4445(16) 0.2337(16) 0.043(4) Uani 1 1 d . . .
C20 C -0.179(3) 0.522(2) 0.255(2) 0.064(6) Uani 1 1 d . . .
H20 H -0.1303 0.5806 0.3242 0.083 Uiso 1 1 calc R . .
C21 C -0.306(4) 0.513(3) 0.173(2) 0.091(11) Uani 1 1 d . . .
H21 H -0.3416 0.5660 0.1879 0.119 Uiso 1 1 calc R . .
C22 C -0.377(3) 0.427(2) 0.0703(19) 0.066(7) Uani 1 1 d . . .
H22 H -0.4650 0.4149 0.0196 0.086 Uiso 1 1 calc R . .
C23 C -0.310(3) 0.355(2) 0.0430(19) 0.065(7) Uani 1 1 d . . .
H23 H -0.3488 0.3074 -0.0317 0.085 Uiso 1 1 calc R . .
C24 C -0.197(2) 0.3576(18) 0.1229(17) 0.049(5) Uani 1 1 d . . .
H24 H -0.1611 0.3049 0.1086 0.064 Uiso 1 1 calc R . .
C26 C 0.336(2) 0.4620(17) 0.5285(17) 0.048(5) Uani 1 1 d . . .
H26 H 0.3624 0.5325 0.5216 0.063 Uiso 1 1 calc R . .
C27 C 0.431(3) 0.425(3) 0.595(3) 0.087(11) Uani 1 1 d . . .
H27 H 0.5204 0.4711 0.6312 0.113 Uiso 1 1 calc R . .
C28 C 0.398(3) 0.324(2) 0.611(2) 0.073(8) Uani 1 1 d . . .
H28 H 0.4628 0.2997 0.6559 0.095 Uiso 1 1 calc R . .
C29 C 0.263(4) 0.260(2) 0.555(3) 0.081(9) Uani 1 1 d . . .
H29 H 0.2350 0.1914 0.5649 0.105 Uiso 1 1 calc R . .
C30 C 0.173(3) 0.2944(16) 0.489(2) 0.059(6) Uani 1 1 d . . .
H30 H 0.0829 0.2476 0.4511 0.076 Uiso 1 1 calc R . .
O6 O 0.0867(13) 0.1048(10) -0.0345(10) 0.042(3) Uani 1 1 d . . .
Cl4 Cl 0.8244(11) 0.1074(17) 0.3170(14) 0.221(11) Uani 1 1 d . . .
Cl3 Cl 0.763(2) -0.129(2) 0.225(2) 0.210(10) Uani 1 1 d . . .
C25 C 0.2062(19) 0.3965(13) 0.4733(13) 0.035(4) Uani 1 1 d . . .
C31 C 0.842(4) -0.002(4) 0.229(3) 0.124(18) Uani 1 1 d . . .
H31A H 0.8080 0.0022 0.1506 0.161 Uiso 1 1 calc R . .
H31B H 0.9365 0.0109 0.2582 0.161 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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 Pb1 C19 158.3(7) . . ?
C25 Pb1 Cl2 97.6(5) . . ?
C19 Pb1 Cl2 98.6(5) . . ?
C25 Pb1 Cl1 97.0(4) . . ?
C19 Pb1 Cl1 97.8(5) . . ?
Cl2 Pb1 Cl1 88.0(2) . . ?
C25 Pb1 O1 79.7(5) . . ?
C19 Pb1 O1 87.6(6) . . ?
Cl2 Pb1 O1 84.4(4) . . ?
Cl1 Pb1 O1 171.3(4) . . ?
O1 V1 O2 103.5(8) . . ?
O1 V1 O3 102.1(6) . . ?
O2 V1 O3 93.0(5) . . ?
O1 V1 N2 99.8(7) . . ?
O2 V1 N2 155.2(6) . . ?
O3 V1 N2 90.3(6) . . ?
O1 V1 N1 98.1(7) . . ?
O2 V1 N1 90.3(6) . . ?
O3 V1 N1 158.2(7) . . ?
N2 V1 N1 78.1(7) . . ?
O1 V1 O6 174.3(6) . . ?
O2 V1 O6 80.7(6) . . ?
O3 V1 O6 81.4(5) . . ?
N2 V1 O6 75.5(5) . . ?
N1 V1 O6 77.8(6) . . ?
V1 O1 Pb1 167.6(9) . . ?
C1 O2 V1 130.5(11) . . ?
C16 O3 V1 125.8(11) . . ?
C2 O4 C17 118.5(17) . . ?
C15 O5 C18 119(2) . . ?
C7 N1 C8 122.4(16) . . ?
C7 N1 V1 124.5(13) . . ?
C8 N1 V1 112.4(13) . . ?
C10 N2 C9 117(2) . . ?
C10 N2 V1 125.4(15) . . ?
C9 N2 V1 116.2(15) . . ?
O2 C1 C2 119.7(15) . . ?
O2 C1 C6 122.3(17) . . ?
C2 C1 C6 117.9(15) . . ?
C1 C2 O4 114.6(15) . . ?
C1 C2 C3 121.5(18) . . ?
O4 C2 C3 123.8(19) . . ?
C4 C3 C2 120(2) . . ?
C5 C4 C3 120.3(18) . . ?
C4 C5 C6 121.9(17) . . ?
C1 C6 C5 118.3(18) . . ?
C1 C6 C7 124.3(16) . . ?
C5 C6 C7 117.2(15) . . ?
N1 C7 C6 126.2(15) . . ?
N1 C8 C9 108.6(18) . . ?
N2 C9 C8 102(3) . . ?
N2 C10 C11 123(2) . . ?
C16 C11 C12 123(2) . . ?
C16 C11 C10 123.2(17) . . ?
C12 C11 C10 113(2) . . ?
C13 C12 C11 116(2) . . ?
C12 C13 C14 123.1(19) . . ?
C15 C14 C13 120(2) . . ?
O5 C15 C14 127(2) . . ?
O5 C15 C16 114.5(17) . . ?
C14 C15 C16 118(2) . . ?
O3 C16 C11 126.0(16) . . ?
O3 C16 C15 114.8(18) . . ?
C11 C16 C15 119.3(17) . . ?
C20 C19 C24 121(2) . . ?
C20 C19 Pb1 119.9(16) . . ?
C24 C19 Pb1 118.7(14) . . ?
C19 C20 C21 120(2) . . ?
C22 C21 C20 120(2) . . ?
C21 C22 C23 118(2) . . ?
C24 C23 C22 121(2) . . ?
C23 C24 C19 118(2) . . ?
C25 C26 C27 120(2) . . ?
C28 C27 C26 123(3) . . ?
C27 C28 C29 115(2) . . ?
C30 C29 C28 122(2) . . ?
C29 C30 C25 122(2) . . ?
C26 C25 C30 117.6(18) . . ?
C26 C25 Pb1 119.3(13) . . ?
C30 C25 Pb1 123.1(16) . . ?
Cl3 C31 Cl4 114(2) . . ?
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
Pb1 C25 2.153(16) . ?
Pb1 C19 2.16(2) . ?
Pb1 Cl2 2.521(5) . ?
Pb1 Cl1 2.596(5) . ?
Pb1 O1 2.624(15) . ?
V1 O1 1.620(16) . ?
V1 O2 1.921(12) . ?
V1 O3 1.955(11) . ?
V1 N2 2.041(17) . ?
V1 N1 2.062(14) . ?
V1 O6 2.343(14) . ?
O2 C1 1.342(19) . ?
O3 C16 1.33(2) . ?
O4 C2 1.39(2) . ?
O4 C17 1.40(3) . ?
O5 C15 1.30(3) . ?
O5 C18 1.43(3) . ?
N1 C7 1.32(2) . ?
N1 C8 1.40(3) . ?
N2 C10 1.33(3) . ?
N2 C9 1.50(3) . ?
C1 C2 1.36(3) . ?
C1 C6 1.42(2) . ?
C2 C3 1.40(3) . ?
C3 C4 1.38(3) . ?
C4 C5 1.31(3) . ?
C5 C6 1.43(2) . ?
C6 C7 1.44(3) . ?
C8 C9 1.54(4) . ?
C10 C11 1.46(3) . ?
C11 C16 1.38(3) . ?
C11 C12 1.44(3) . ?
C12 C13 1.39(3) . ?
C13 C14 1.41(4) . ?
C14 C15 1.39(3) . ?
C15 C16 1.46(2) . ?
C19 C20 1.35(3) . ?
C19 C24 1.45(3) . ?
C20 C21 1.41(4) . ?
C21 C22 1.38(4) . ?
C22 C23 1.46(4) . ?
C23 C24 1.32(3) . ?
C26 C25 1.34(3) . ?
C26 C27 1.38(3) . ?
C27 C28 1.36(4) . ?
C28 C29 1.38(4) . ?
C29 C30 1.32(4) . ?
C30 C25 1.37(2) . ?
Cl4 C31 1.80(4) . ?
Cl3 C31 1.67(5) . ?
