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
Jebastin Andrews, S.G.; Benita Jeba Silviya, S.; Bhuvanesh, Nattamai S.P.; Janet Sylvia Jaba Rose, J.; Winfred Jebaraj, J.; Balakrishnan, Chithiraivel; Inorganica Chimica Acta 498 (2019) 119118–; doi:10.1016/j.ica.2019.119118

data_1565727
_publ_section_title
;
 Crystal structure and evaluating C H&#x22EF;\p (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       '\f and \w 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 \l/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/[\s^2^(Fo^2^)+(0.0103P)^2^+3.6818P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119118.cif
_cod_data_source_block           cbk1
_cod_database_code               1565727
_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)
;