#------------------------------------------------------------------------------
#$Date: 2021-12-14 10:59:43 +0200 (Tue, 14 Dec 2021) $
#$Revision: 271383 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/57/1565727.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_1565727
loop_
_publ_author_name
'Jebastin Andrews, S.G.'
'Benita Jeba Silviya, S.'
'Bhuvanesh, Nattamai S.P.'
'Janet Sylvia Jaba Rose, J.'
'Winfred Jebaraj, J.'
'Balakrishnan, Chithiraivel'
_publ_section_title
;
 Crystal structure and evaluating C H⋯π (aryl/chelate)
 interactions in
 bis(2-{[(2-hydroxyethyl)imino]-methyl}-4,6-diiodophenolato)-palladium(II)
 Schiff base complex derived from
 (E)-2-(((2-hydroxyethyl)imino)methyl)-4,6-diiodophenol
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119118
_journal_paper_doi               10.1016/j.ica.2019.119118
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C18 H16 I4 N2 O4 Pd, 2(C3 H7 N O)'
_chemical_formula_sum            'C24 H30 I4 N4 O6 Pd'
_chemical_formula_weight         1084.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 92.6510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.08440(10)
_cell_length_b                   12.9078(3)
_cell_length_c                   23.7918(6)
_cell_measurement_reflns_used    9713
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      27.463
_cell_measurement_theta_min      3.017
_cell_volume                     1559.75(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25859
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.597
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.1290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1064 before and 0.0652 after correction. The Ratio of minimum to maximum transmission is 0.3869. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.309
_exptl_crystal_description       needle
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.482
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.195
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0251
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0103P)²+3.6818P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0456
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3368
_reflns_number_total             3561
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2019-498-119118.cif
_cod_data_source_block           cbk1
_cod_database_code               1565727
_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   0.468
_shelx_estimated_absorpt_t_min   0.215
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C3S(H3S)
2.c Idealised Me refined as rotating group:
 C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
loop_
_space_group_symop_operation_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_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
I1 I 0.38870(4) 0.31980(2) 0.68526(2) 0.01348(6) Uani 1 1 d . . . . .
I2 I -0.40305(4) 0.64973(2) 0.73597(2) 0.01667(6) Uani 1 1 d . . . . .
Pd1 Pd 0.500000 0.500000 0.500000 0.00942(7) Uani 1 2 d S T P . .
O1 O 0.3797(4) 0.44900(16) 0.57336(9) 0.0123(4) Uani 1 1 d . . . . .
O2 O 0.2795(5) 0.84327(17) 0.49805(10) 0.0180(5) Uani 1 1 d . . . . .
H2 H 0.394879 0.844885 0.524473 0.027 Uiso 1 1 calc GR . . . .
N1 N 0.2235(5) 0.61364(19) 0.49703(11) 0.0108(5) Uani 1 1 d . . . . .
C1 C 0.2107(6) 0.4927(2) 0.60530(12) 0.0111(6) Uani 1 1 d . . . . .
C2 C 0.1680(6) 0.4492(2) 0.65921(12) 0.0105(5) Uani 1 1 d . . . . .
C3 C -0.0081(6) 0.4910(2) 0.69559(13) 0.0131(6) Uani 1 1 d . . . . .
H3 H -0.030384 0.459879 0.731255 0.016 Uiso 1 1 calc R . . . .
C4 C -0.1524(6) 0.5786(2) 0.67975(13) 0.0131(6) Uani 1 1 d . . . . .
C5 C -0.1246(6) 0.6224(2) 0.62768(13) 0.0139(6) Uani 1 1 d . . . . .
H5 H -0.227508 0.681156 0.616799 0.017 Uiso 1 1 calc R . . . .
C6 C 0.0558(6) 0.5809(2) 0.59017(13) 0.0119(6) Uani 1 1 d . . . . .
C7 C 0.0679(6) 0.6326(2) 0.53686(13) 0.0119(6) Uani 1 1 d . . . . .
H7 H -0.053973 0.687524 0.530229 0.014 Uiso 1 1 calc R . . . .
C8 C 0.1933(6) 0.6821(2) 0.44745(13) 0.0120(6) Uani 1 1 d . . . . .
H8A H 0.006738 0.703359 0.442100 0.014 Uiso 1 1 calc R . . . .
H8B H 0.242285 0.643737 0.413466 0.014 Uiso 1 1 calc R . . . .
C9 C 0.3656(6) 0.7781(2) 0.45445(14) 0.0143(6) Uani 1 1 d . . . . .
H9A H 0.549901 0.756793 0.463263 0.017 Uiso 1 1 calc R . . . .
H9B H 0.361006 0.817283 0.418640 0.017 Uiso 1 1 calc R . . . .
O1S O 0.6805(5) 0.84996(19) 0.57614(11) 0.0235(5) Uani 1 1 d . . . . .
N2S N 1.0141(6) 0.9547(2) 0.60789(12) 0.0186(6) Uani 1 1 d . . . . .
C3S C 0.8225(7) 0.9271(3) 0.57168(14) 0.0193(7) Uani 1 1 d . . . . .
H3S H 0.791043 0.969818 0.539571 0.023 Uiso 1 1 calc R . . . .
C4S C 1.1735(7) 1.0460(3) 0.59830(17) 0.0257(8) Uani 1 1 d . . . . .
H4SA H 1.357483 1.025231 0.594843 0.039 Uiso 1 1 calc GR . . . .
H4SB H 1.160947 1.093851 0.630024 0.039 Uiso 1 1 calc GR . . . .
H4SC H 1.109604 1.080310 0.563559 0.039 Uiso 1 1 calc GR . . . .
C5S C 1.0844(9) 0.8923(3) 0.65721(18) 0.0327(9) Uani 1 1 d . . . . .
H5SA H 0.943349 0.842496 0.663554 0.049 Uiso 1 1 calc GR . . . .
H5SB H 1.108822 0.937431 0.690167 0.049 Uiso 1 1 calc GR . . . .
H5SC H 1.248430 0.854901 0.651155 0.049 Uiso 1 1 calc GR . . . .
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'
I I -0.4742 1.8119 '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
O1 Pd1 O1 180.0 3_666 .
O1 Pd1 N1 91.66(9) 3_666 3_666
O1 Pd1 N1 88.33(9) 3_666 .
O1 Pd1 N1 88.34(9) . 3_666
O1 Pd1 N1 91.67(9) . .
N1 Pd1 N1 180.0 3_666 .
C1 O1 Pd1 127.38(19) . .
C9 O2 H2 109.5 . .
C7 N1 Pd1 124.1(2) . .
C7 N1 C8 115.5(2) . .
C8 N1 Pd1 120.43(18) . .
O1 C1 C2 119.1(3) . .
O1 C1 C6 124.9(3) . .
C6 C1 C2 116.0(2) . .
C1 C2 I1 118.6(2) . .
C3 C2 I1 118.7(2) . .
C3 C2 C1 122.6(3) . .
C2 C3 H3 120.1 . .
C2 C3 C4 119.7(3) . .
C4 C3 H3 120.1 . .
C3 C4 I2 120.7(2) . .
C5 C4 I2 119.0(2) . .
C5 C4 C3 120.3(3) . .
C4 C5 H5 119.7 . .
C4 C5 C6 120.6(3) . .
C6 C5 H5 119.7 . .
C1 C6 C7 123.3(3) . .
C5 C6 C1 120.8(3) . .
C5 C6 C7 115.9(3) . .
N1 C7 C6 128.0(3) . .
N1 C7 H7 116.0 . .
C6 C7 H7 116.0 . .
N1 C8 H8A 109.4 . .
N1 C8 H8B 109.4 . .
N1 C8 C9 111.2(3) . .
H8A C8 H8B 108.0 . .
C9 C8 H8A 109.4 . .
C9 C8 H8B 109.4 . .
O2 C9 C8 111.5(2) . .
O2 C9 H9A 109.3 . .
O2 C9 H9B 109.3 . .
C8 C9 H9A 109.3 . .
C8 C9 H9B 109.3 . .
H9A C9 H9B 108.0 . .
C3S N2S C4S 121.1(3) . .
C3S N2S C5S 121.5(3) . .
C4S N2S C5S 117.2(3) . .
O1S C3S N2S 125.3(3) . .
O1S C3S H3S 117.3 . .
N2S C3S H3S 117.3 . .
N2S C4S H4SA 109.5 . .
N2S C4S H4SB 109.5 . .
N2S C4S H4SC 109.5 . .
H4SA C4S H4SB 109.5 . .
H4SA C4S H4SC 109.5 . .
H4SB C4S H4SC 109.5 . .
N2S C5S H5SA 109.5 . .
N2S C5S H5SB 109.5 . .
N2S C5S H5SC 109.5 . .
H5SA C5S H5SB 109.5 . .
H5SA C5S H5SC 109.5 . .
H5SB C5S H5SC 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 C2 2.090(3) .
I2 C4 2.101(3) .
Pd1 O1 1.988(2) 3_666
Pd1 O1 1.988(2) .
Pd1 N1 2.031(2) 3_666
Pd1 N1 2.031(2) .
O1 C1 1.302(3) .
O2 H2 0.8400 .
O2 C9 1.420(4) .
N1 C7 1.286(4) .
N1 C8 1.476(4) .
C1 C2 1.426(4) .
C1 C6 1.422(4) .
C2 C3 1.383(4) .
C3 H3 0.9500 .
C3 C4 1.391(4) .
C4 C5 1.375(4) .
C5 H5 0.9500 .
C5 C6 1.414(4) .
C6 C7 1.437(4) .
C7 H7 0.9500 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C8 C9 1.522(4) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
O1S C3S 1.237(4) .
N2S C3S 1.320(5) .
N2S C4S 1.453(4) .
N2S C5S 1.455(5) .
C3S H3S 0.9500 .
C4S H4SA 0.9800 .
C4S H4SB 0.9800 .
C4S H4SC 0.9800 .
C5S H5SA 0.9800 .
C5S H5SB 0.9800 .
C5S H5SC 0.9800 .
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
I1 C2 C3 C4 178.4(2) . . . .
I2 C4 C5 C6 175.7(2) . . . .
Pd1 O1 C1 C2 -174.1(2) . . . .
Pd1 O1 C1 C6 7.7(4) . . . .
Pd1 N1 C7 C6 0.5(5) . . . .
Pd1 N1 C8 C9 -90.5(3) . . . .
O1 C1 C2 I1 1.9(4) . . . .
O1 C1 C2 C3 -179.9(3) . . . .
O1 C1 C6 C5 179.5(3) . . . .
O1 C1 C6 C7 0.2(5) . . . .
N1 C8 C9 O2 -67.1(3) . . . .
C1 C2 C3 C4 0.3(5) . . . .
C1 C6 C7 N1 -4.6(5) . . . .
C2 C1 C6 C5 1.2(4) . . . .
C2 C1 C6 C7 -178.1(3) . . . .
C2 C3 C4 I2 -176.0(2) . . . .
C2 C3 C4 C5 1.4(5) . . . .
C3 C4 C5 C6 -1.7(5) . . . .
C4 C5 C6 C1 0.4(5) . . . .
C4 C5 C6 C7 179.8(3) . . . .
C5 C6 C7 N1 176.1(3) . . . .
C6 C1 C2 I1 -179.6(2) . . . .
C6 C1 C2 C3 -1.5(4) . . . .
C7 N1 C8 C9 88.6(3) . . . .
C8 N1 C7 C6 -178.5(3) . . . .
C4S N2S C3S O1S 178.8(3) . . . .
C5S N2S C3S O1S 2.4(5) . . . .
