#------------------------------------------------------------------------------
#$Date: 2021-09-06 14:01:51 +0200 (lun 06 de sep de 2021) $
#$Revision: 268862 $
#$URL: svn://www.crystallography.net/cod/cif/7/06/08/7060818.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_7060818
loop_
_publ_author_name
'Nkabyo, H. A.'
'Oyenihi, O. R.'
'Olaoye, O.'
'Sikiti, P.'
'Bosman, G. W.'
'Luckay, R. C.'
_publ_section_title
;
 Photoactive PtII and PdII complexes of
 N,N-diethyl-N′-3,4,5-trimethoxybenzoylthiourea: synthesis, crystal
 structures, DFT and cytotoxicity studies
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14703
_journal_page_last               14712
_journal_paper_doi               10.1039/D1NJ02320A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C30 H42 N4 O8 Pd S2'
_chemical_formula_sum            'C30 H42 N4 O8 Pd S2'
_chemical_formula_weight         757.19
_chemical_melting_point          214.0(10)
_chemical_name_systematic
trans-bis(N,N-diethyl-N?-(3,4,5-trimethoxybenzoyl)thioureato-S,O)-palladium(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2020-01-04 deposited with the CCDC.	2021-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                89.463(2)
_cell_angle_beta                 85.447(2)
_cell_angle_gamma                79.772(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7250(5)
_cell_length_b                   8.4230(5)
_cell_length_c                   12.8460(7)
_cell_measurement_reflns_used    3884
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.32
_cell_measurement_theta_min      2.23
_cell_volume                     819.97(8)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32625
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.714
_diffrn_reflns_theta_min         1.590
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'symmetry-related measurement'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_density_meas      1.473
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       rod
_exptl_crystal_F_000             392
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetoitrile'
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.884
_exptl_transmission_factor_min   0.821
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         4245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0224P)²+0.8680P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0632
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3884
_reflns_number_total             4245
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1nj02320a2.cif
_cod_data_source_block           C
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '213-215' was changed to
'214.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7060818--7060819.cif.
;
_cod_database_code               7060818
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.000000 0.500000 0.500000 0.01169(6) Uani 1 2 d S . P . .
S1 S 0.16884(6) 0.38469(6) 0.62786(4) 0.01669(10) Uani 1 1 d . . . . .
O1 O 0.18358(16) 0.42892(16) 0.38440(10) 0.0151(3) Uani 1 1 d . . . . .
O5 O 0.73274(18) 0.24284(17) -0.00254(11) 0.0216(3) Uani 1 1 d . . . . .
O4 O 0.90251(17) 0.19122(17) 0.17326(11) 0.0199(3) Uani 1 1 d . . . . .
O3 O 0.38464(18) 0.33692(18) 0.00358(10) 0.0209(3) Uani 1 1 d . . . . .
N1 N 0.43987(19) 0.32692(18) 0.46991(12) 0.0130(3) Uani 1 1 d . . . . .
N2 N 0.5099(2) 0.28163(19) 0.63630(12) 0.0139(3) Uani 1 1 d . . . . .
C7 C 0.4473(2) 0.3345(2) 0.28535(14) 0.0129(3) Uani 1 1 d . . . . .
C6 C 0.3459(2) 0.3672(2) 0.38956(14) 0.0123(3) Uani 1 1 d . . . . .
C9 C 0.3605(2) 0.3574(2) 0.19399(14) 0.0146(4) Uani 1 1 d . . . . .
H12 H 0.239474 0.395230 0.197299 0.017 Uiso 1 1 calc R U . . .
C8 C 0.6291(2) 0.2792(2) 0.28134(15) 0.0141(4) Uani 1 1 d . . . . .
H11 H 0.686173 0.263906 0.342663 0.017 Uiso 1 1 calc R U . . .
C4 C 0.4729(3) 0.2746(2) 0.75032(14) 0.0163(4) Uani 1 1 d . . . . .
H5 H 0.381381 0.364883 0.772548 0.020 Uiso 1 1 calc R U . . .
H4 H 0.578380 0.285357 0.783866 0.020 Uiso 1 1 calc R U . . .
C12 C 0.6386(2) 0.2688(2) 0.09298(15) 0.0161(4) Uani 1 1 d . . . . .
C10 C 0.4554(2) 0.3236(2) 0.09773(15) 0.0157(4) Uani 1 1 d . . . . .
C5 C 0.3827(2) 0.3308(2) 0.57218(14) 0.0133(3) Uani 1 1 d . . . . .
C11 C 0.7240(2) 0.2472(2) 0.18527(15) 0.0155(4) Uani 1 1 d . . . . .
C2 C 0.6928(2) 0.2190(2) 0.59365(15) 0.0170(4) Uani 1 1 d . . . . .
H9 H 0.772014 0.221100 0.648350 0.020 Uiso 1 1 calc R U . . .
H10 H 0.725314 0.289659 0.538257 0.020 Uiso 1 1 calc R U . . .
C14 C 0.9886(3) 0.1508(3) 0.26675(16) 0.0226(4) Uani 1 1 d . . . . .
H13 H 0.976308 0.245256 0.309808 0.034 Uiso 1 1 calc R U . . .
H15 H 1.111520 0.110025 0.249311 0.034 Uiso 1 1 calc R U . . .
H14 H 0.935826 0.069793 0.303975 0.034 Uiso 1 1 calc R U . . .
C13 C 0.1981(3) 0.3893(3) 0.00468(16) 0.0217(4) Uani 1 1 d . . . . .
H21 H 0.138936 0.314448 0.044011 0.033 Uiso 1 1 calc R U . . .
H20 H 0.163666 0.394347 -0.065610 0.033 Uiso 1 1 calc R U . . .
H19 H 0.166543 0.494262 0.036391 0.033 Uiso 1 1 calc R U . . .
C3 C 0.4142(3) 0.1188(2) 0.78587(16) 0.0223(4) Uani 1 1 d . . . . .
H3 H 0.312366 0.105345 0.750946 0.033 Uiso 1 1 calc R U . . .
H1 H 0.385095 0.123026 0.859964 0.033 Uiso 1 1 calc R U . . .
H2 H 0.508006 0.029510 0.769188 0.033 Uiso 1 1 calc R U . . .
C1 C 0.7172(3) 0.0475(2) 0.55076(17) 0.0220(4) Uani 1 1 d . . . . .
H8 H 0.677436 -0.021863 0.603707 0.033 Uiso 1 1 calc R U . . .
H6 H 0.839764 0.009802 0.530372 0.033 Uiso 1 1 calc R U . . .
H7 H 0.649702 0.046742 0.491215 0.033 Uiso 1 1 calc R U . . .
C15 C 0.7706(3) 0.0770(3) -0.03348(17) 0.0261(5) Uani 1 1 d . . . . .
H16 H 0.832398 0.014213 0.019268 0.039 Uiso 1 1 calc R U . . .
H17 H 0.842658 0.065797 -0.098317 0.039 Uiso 1 1 calc R U . . .
H18 H 0.662262 0.039605 -0.042165 0.039 Uiso 1 1 calc R U . . .
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 '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
O1 Pd1 O1 180.0 . 2_566 ?
O1 Pd1 S1 94.50(4) . . ?
O1 Pd1 S1 85.50(4) 2_566 . ?
O1 Pd1 S1 85.50(4) . 2_566 ?
O1 Pd1 S1 94.50(4) 2_566 2_566 ?
S1 Pd1 S1 180.0 . 2_566 ?
C5 S1 Pd1 107.25(6) . . ?
C6 O1 Pd1 128.89(12) . . ?
C12 O5 C15 113.38(15) . . ?
C11 O4 C14 116.41(15) . . ?
C10 O3 C13 116.92(15) . . ?
C6 N1 C5 127.82(16) . . ?
C5 N2 C4 122.17(15) . . ?
C5 N2 C2 120.54(15) . . ?
C4 N2 C2 117.10(15) . . ?
C9 C7 C8 120.66(17) . . ?
C9 C7 C6 120.23(16) . . ?
C8 C7 C6 119.11(17) . . ?
O1 C6 N1 131.55(17) . . ?
O1 C6 C7 114.09(16) . . ?
N1 C6 C7 114.36(15) . . ?
C10 C9 C7 119.74(17) . . ?
C11 C8 C7 119.59(17) . . ?
N2 C4 C3 112.82(15) . . ?
O5 C12 C11 120.67(17) . . ?
O5 C12 C10 119.63(17) . . ?
C11 C12 C10 119.66(17) . . ?
O3 C10 C9 125.10(17) . . ?
O3 C10 C12 114.93(16) . . ?
C9 C10 C12 119.96(17) . . ?
N2 C5 N1 114.18(16) . . ?
N2 C5 S1 117.57(14) . . ?
N1 C5 S1 128.23(14) . . ?
O4 C11 C8 123.94(17) . . ?
O4 C11 C12 115.66(16) . . ?
C8 C11 C12 120.39(17) . . ?
N2 C2 C1 113.22(15) . . ?
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
Pd1 O1 1.9889(12) . ?
Pd1 O1 1.9889(12) 2_566 ?
Pd1 S1 2.2809(5) . ?
Pd1 S1 2.2809(5) 2_566 ?
S1 C5 1.7315(18) . ?
O1 C6 1.276(2) . ?
O5 C12 1.375(2) . ?
O5 C15 1.429(2) . ?
O4 C11 1.372(2) . ?
O4 C14 1.428(2) . ?
O3 C10 1.362(2) . ?
O3 C13 1.429(2) . ?
N1 C6 1.316(2) . ?
N1 C5 1.351(2) . ?
N2 C5 1.339(2) . ?
N2 C4 1.473(2) . ?
N2 C2 1.481(2) . ?
C7 C9 1.393(3) . ?
C7 C8 1.395(2) . ?
C7 C6 1.499(2) . ?
C9 C10 1.392(2) . ?
C8 C11 1.388(2) . ?
C4 C3 1.517(3) . ?
C12 C11 1.397(3) . ?
C12 C10 1.405(3) . ?
C2 C1 1.525(3) . ?
