#------------------------------------------------------------------------------
#$Date: 2021-07-05 20:45:25 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267201 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/74/7707467.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_7707467
loop_
_publ_author_name
'Omondi, Reinner O.'
'Sibuyi, Nicole R. S.'
'Fadaka, Adewale O.'
'Meyer, Mervin'
'Jaganyi, Deogratius'
'Ojwach, Stephen O.'
_publ_section_title
;
 Role of π-conjugation on the coordination behaviour, substitution
 kinetics, DNA/BSA interactions, and in vitro cytotoxicity of
 carboxamide palladium(II) complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8127
_journal_page_last               8143
_journal_paper_doi               10.1039/d1dt00412c
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C19 H12 Cl N3 O Pd'
_chemical_formula_sum            'C19 H12 Cl N3 O Pd'
_chemical_formula_weight         440.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-04-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-21 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.978(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.5553(3)
_cell_length_b                   18.3946(9)
_cell_length_c                   9.1957(4)
_cell_measurement_reflns_used    4659
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.48
_cell_volume                     767.63(7)
_computing_cell_refinement       'COSMOS (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5873
_diffrn_reflns_point_group_measured_fraction_full 0.717
_diffrn_reflns_point_group_measured_fraction_max 0.707
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.978
_diffrn_reflns_theta_min         2.214
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1686 before and 0.0282 after correction.
The Ratio of minimum to maximum transmission is 0.7771.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       Needle
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.863
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2134
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0474
_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)+(0.0875P)²+2.5432P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.481
_reflns_Friedel_fraction_full    0.474
_reflns_Friedel_fraction_max     0.462
_reflns_number_gt                2103
_reflns_number_total             2134
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt00412c2.cif
_cod_data_source_block           PdL4
_cod_depositor_comments
'Adding full bibliography for 7707465--7707467.cif.'
_cod_database_code               7707467
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.634
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54311
 0.45689
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.002 within 2A
3. Others
 Fixed U11: N2(0.018199)
 Fixed U22: N2(0.015)
 Fixed U33: N2(0.022)
4.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C14(H14), C3(H3), C2(H2), C16(H16), C7(H7), C13(H13),
 C18(H18), C17(H17), C5(H5), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y, 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_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 0.46355(13) 0.23708(3) 0.85095(10) 0.0155(2) Uani 1 1 d . U . . .
Cl1 Cl 0.3625(6) 0.16794(12) 1.0524(2) 0.0223(5) Uani 1 1 d . . . . .
O1 O 0.5747(17) 0.3152(4) 0.4481(7) 0.0193(11) Uani 1 1 d . U . . .
C1 C 0.008(2) 0.1369(5) 0.6585(10) 0.0190(7) Uani 1 1 d . U . . .
C19 C 0.889(3) 0.3513(5) 0.8943(10) 0.0197(7) Uani 1 1 d . U . . .
N2 N 0.605(2) 0.2978(4) 0.6960(9) 0.01805(6) Uani 1 1 d . U . . .
N3 N 0.745(2) 0.3025(4) 0.9773(9) 0.0199(8) Uani 1 1 d . U . . .
C12 C 0.958(3) 0.3970(5) 0.6535(11) 0.0201(8) Uani 1 1 d . U . . .
H12 H 0.910267 0.397177 0.550809 0.024 Uiso 1 1 calc R U . . .
C8 C 0.177(2) 0.1989(5) 0.4067(10) 0.0190(8) Uani 1 1 d . U . . .
H8 H 0.241254 0.222053 0.322698 0.023 Uiso 1 1 calc R U . . .
C15 C 1.092(3) 0.4009(5) 0.9598(11) 0.0203(7) Uani 1 1 d . U . . .
C14 C 1.238(3) 0.4487(5) 0.8691(11) 0.0205(8) Uani 1 1 d . U . . .
H14 H 1.379372 0.482388 0.910859 0.025 Uiso 1 1 calc R U . . .
C11 C 0.820(3) 0.3497(5) 0.7422(11) 0.0193(6) Uani 1 1 d . U . . .
C3 C -0.307(2) 0.0530(5) 0.7750(10) 0.0195(9) Uani 1 1 d . U . . .
H3 H -0.379280 0.033111 0.860348 0.023 Uiso 1 1 calc R U . . .
C6 C -0.117(3) 0.1120(5) 0.5207(10) 0.0194(8) Uani 1 1 d . U . . .
C2 C -0.098(3) 0.1059(5) 0.7891(11) 0.0193(8) Uani 1 1 d . U . . .
H2 H -0.022044 0.122215 0.882955 0.023 Uiso 1 1 calc R U . . .
C16 C 1.147(3) 0.3994(5) 1.1143(11) 0.0205(8) Uani 1 1 d . U . . .
H16 H 1.286486 0.431577 1.162379 0.025 Uiso 1 1 calc R U . . .
N1 N 0.213(2) 0.1917(4) 0.6717(9) 0.0187(7) Uani 1 1 d . U . . .
C7 C -0.019(3) 0.1443(5) 0.3916(10) 0.0192(8) Uani 1 1 d . U . . .
H7 H -0.091689 0.127554 0.297576 0.023 Uiso 1 1 calc R U . . .
C13 C 1.175(2) 0.4460(5) 0.7201(11) 0.0205(8) Uani 1 1 d . U . . .
H13 H 1.277579 0.477313 0.659876 0.025 Uiso 1 1 calc R U . . .
C18 C 0.795(3) 0.3035(5) 1.1201(11) 0.0203(9) Uani 1 1 d . U . . .
H18 H 0.692120 0.270545 1.176756 0.024 Uiso 1 1 calc R U . . .
C17 C 0.998(3) 0.3522(5) 1.1917(11) 0.0204(9) Uani 1 1 d . U . . .
H17 H 1.030661 0.351554 1.295122 0.024 Uiso 1 1 calc R U . . .
C5 C -0.327(3) 0.0567(5) 0.5118(10) 0.0199(9) Uani 1 1 d . U . . .
H5 H -0.404840 0.039566 0.418891 0.024 Uiso 1 1 calc R U . . .
C9 C 0.289(3) 0.2219(5) 0.5485(11) 0.0187(7) Uani 1 1 d . U . . .
C10 C 0.507(2) 0.2832(5) 0.5569(10) 0.0185(6) Uani 1 1 d . U . . .
C4 C -0.422(3) 0.0268(5) 0.6356(10) 0.0200(9) Uani 1 1 d . U . . .
H4 H -0.562975 -0.011347 0.628688 0.024 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'
Cl Cl 0.1484 0.1585 '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'
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
N2 Pd1 Cl1 171.7(3) . . ?
N2 Pd1 N3 81.3(3) . . ?
N2 Pd1 N1 81.1(3) . . ?
N3 Pd1 Cl1 91.5(3) . . ?
N3 Pd1 N1 162.4(3) . . ?
N1 Pd1 Cl1 106.1(2) . . ?
C6 C1 C2 118.4(9) . . ?
N1 C1 C6 122.2(9) . . ?
N1 C1 C2 119.3(8) . . ?
N3 C19 C15 121.0(9) . . ?
N3 C19 C11 117.5(9) . . ?
C15 C19 C11 121.5(10) . . ?
C11 N2 Pd1 115.5(6) . . ?
C10 N2 Pd1 118.4(7) . . ?
C10 N2 C11 125.9(9) . . ?
C19 N3 Pd1 111.9(6) . . ?
C18 N3 Pd1 128.6(8) . . ?
C18 N3 C19 119.5(9) . . ?
C11 C12 H12 120.8 . . ?
C11 C12 C13 118.4(9) . . ?
C13 C12 H12 120.8 . . ?
C7 C8 H8 120.0 . . ?
C7 C8 C9 120.0(9) . . ?
C9 C8 H8 120.0 . . ?
C19 C15 C14 118.6(9) . . ?
C19 C15 C16 118.0(9) . . ?
C14 C15 C16 123.4(9) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 C15 119.7(10) . . ?
C13 C14 H14 120.2 . . ?
C19 C11 N2 113.7(9) . . ?
C12 C11 C19 120.1(10) . . ?
C12 C11 N2 126.2(9) . . ?
C2 C3 H3 119.1 . . ?
C2 C3 C4 121.7(9) . . ?
C4 C3 H3 119.1 . . ?
C1 C6 C7 118.4(9) . . ?
C5 C6 C1 120.5(9) . . ?
C5 C6 C7 121.0(8) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 C1 119.0(9) . . ?
C3 C2 H2 120.5 . . ?
C15 C16 H16 120.3 . . ?
C17 C16 C15 119.4(9) . . ?
C17 C16 H16 120.3 . . ?
C1 N1 Pd1 133.0(7) . . ?
C9 N1 Pd1 109.8(7) . . ?
C9 N1 C1 117.1(8) . . ?
C8 C7 C6 118.4(8) . . ?
C8 C7 H7 120.8 . . ?
C6 C7 H7 120.8 . . ?
C12 C13 H13 119.2 . . ?
C14 C13 C12 121.7(10) . . ?
C14 C13 H13 119.2 . . ?
N3 C18 H18 119.1 . . ?
N3 C18 C17 121.8(10) . . ?
C17 C18 H18 119.1 . . ?
C16 C17 C18 120.3(10) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C6 C5 H5 119.7 . . ?
C4 C5 C6 120.6(9) . . ?
C4 C5 H5 119.7 . . ?
C8 C9 C10 117.0(9) . . ?
N1 C9 C8 123.7(10) . . ?
N1 C9 C10 119.2(9) . . ?
O1 C10 N2 126.7(10) . . ?
O1 C10 C9 122.1(9) . . ?
N2 C10 C9 111.2(9) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.7(9) . . ?
C5 C4 H4 120.2 . . ?
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
Pd1 Cl1 2.326(2) . ?
Pd1 N2 1.962(8) . ?
Pd1 N3 2.044(9) . ?
Pd1 N1 2.095(8) . ?
O1 C10 1.223(13) . ?
C1 C6 1.420(13) . ?
C1 C2 1.450(15) . ?
C1 N1 1.371(13) . ?
C19 N3 1.380(14) . ?
C19 C15 1.400(14) . ?
C19 C11 1.407(14) . ?
N2 C11 1.408(13) . ?
N2 C10 1.344(13) . ?
N3 C18 1.314(13) . ?
C12 H12 0.9500 . ?
C12 C11 1.381(15) . ?
C12 C13 1.435(14) . ?
C8 H8 0.9500 . ?
C8 C7 1.344(15) . ?
C8 C9 1.423(13) . ?
C15 C14 1.417(15) . ?
C15 C16 1.421(13) . ?
C14 H14 0.9500 . ?
C14 C13 1.376(14) . ?
C3 H3 0.9500 . ?
C3 C2 1.361(15) . ?
C3 C4 1.426(13) . ?
C6 C7 1.432(14) . ?
C6 C5 1.395(15) . ?
C2 H2 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.341(15) . ?
N1 C9 1.334(14) . ?
C7 H7 0.9500 . ?
C13 H13 0.9500 . ?
C18 H18 0.9500 . ?
C18 C17 1.409(14) . ?
C17 H17 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.367(15) . ?
C9 C10 1.501(15) . ?
C4 H4 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N2 C11 C19 -2.7(11) . . . . ?
Pd1 N2 C11 C12 178.1(9) . . . . ?
Pd1 N2 C10 O1 -179.5(9) . . . . ?
Pd1 N2 C10 C9 2.4(11) . . . . ?
Pd1 N3 C18 C17 179.8(8) . . . . ?
Pd1 N1 C9 C8 174.7(8) . . . . ?
Pd1 N1 C9 C10 -4.6(11) . . . . ?
C1 C6 C7 C8 -2.8(14) . . . . ?
C1 C6 C5 C4 1.8(15) . . . . ?
C1 N1 C9 C8 -2.0(15) . . . . ?
C1 N1 C9 C10 178.6(9) . . . . ?
C19 N3 C18 C17 -1.5(16) . . . . ?
C19 C15 C14 C13 0.9(15) . . . . ?
C19 C15 C16 C17 -1.5(15) . . . . ?
N3 C19 C15 C14 178.6(9) . . . . ?
N3 C19 C15 C16 0.2(16) . . . . ?
N3 C19 C11 N2 1.1(13) . . . . ?
N3 C19 C11 C12 -179.7(10) . . . . ?
N3 C18 C17 C16 0.2(17) . . . . ?
C8 C9 C10 O1 4.2(15) . . . . ?
C8 C9 C10 N2 -177.6(9) . . . . ?
C15 C19 N3 Pd1 -179.8(8) . . . . ?
C15 C19 N3 C18 1.3(15) . . . . ?
C15 C19 C11 N2 -178.2(10) . . . . ?
C15 C19 C11 C12 1.1(16) . . . . ?
C15 C14 C13 C12 1.6(16) . . . . ?
C15 C16 C17 C18 1.3(16) . . . . ?
C14 C15 C16 C17 -179.7(10) . . . . ?
C11 C19 N3 Pd1 1.0(11) . . . . ?
C11 C19 N3 C18 -178.0(9) . . . . ?
C11 C19 C15 C14 -2.2(15) . . . . ?
C11 C19 C15 C16 179.4(9) . . . . ?
C11 N2 C10 O1 -5.0(17) . . . . ?
C11 N2 C10 C9 176.9(9) . . . . ?
C11 C12 C13 C14 -2.7(16) . . . . ?
C6 C1 C2 C3 1.6(14) . . . . ?
C6 C1 N1 Pd1 -175.0(7) . . . . ?
C6 C1 N1 C9 0.7(14) . . . . ?
C6 C5 C4 C3 0.8(15) . . . . ?
C2 C1 C6 C7 178.0(9) . . . . ?
C2 C1 C6 C5 -3.0(14) . . . . ?
C2 C1 N1 Pd1 8.7(14) . . . . ?
C2 C1 N1 C9 -175.6(9) . . . . ?
C2 C3 C4 C5 -2.2(15) . . . . ?
C16 C15 C14 C13 179.2(10) . . . . ?
N1 C1 C6 C7 1.6(15) . . . . ?
N1 C1 C6 C5 -179.3(9) . . . . ?
N1 C1 C2 C3 178.1(9) . . . . ?
N1 C9 C10 O1 -176.4(10) . . . . ?
N1 C9 C10 N2 1.8(13) . . . . ?
C7 C8 C9 N1 0.8(16) . . . . ?
C7 C8 C9 C10 -179.9(9) . . . . ?
C7 C6 C5 C4 -179.2(10) . . . . ?
C13 C12 C11 C19 1.4(15) . . . . ?
C13 C12 C11 N2 -179.5(10) . . . . ?
C5 C6 C7 C8 178.1(10) . . . . ?
C9 C8 C7 C6 1.7(15) . . . . ?
C10 N2 C11 C19 -177.3(9) . . . . ?
C10 N2 C11 C12 3.5(17) . . . . ?
C4 C3 C2 C1 0.9(15) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.54311
2 0.45689
