Lasagna-like supramolecular polymers derived from the PdII osazone complexes via C(sp2)–H⋯Hal hydrogen bonding
Repina, Olga V.; Novikov, Alexander S.; Khoroshilova, Olesya V.; Kritchenkov, Andreii S.; Vasin, Alexander A.; Tskhovrebov, Alexander G.; Inorganica Chimica Acta 502 (2020) 119378–; doi:10.1016/j.ica.2019.119378

data_1565440
_publ_section_title
;
 Lasagna-like supramolecular polymers derived from the PdII osazone
 complexes via C(sp2)--H&#x22EF;Hal hydrogen bonding
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119378
_journal_paper_doi               10.1016/j.ica.2019.119378
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C14 H14 Cl2 N4 Pd'
_chemical_formula_sum            'C14 H14 Cl2 N4 Pd'
_chemical_formula_weight         415.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1766(3)
_cell_length_b                   27.7685(6)
_cell_length_c                   4.28810(10)
_cell_measurement_reflns_used    7388
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2990
_cell_measurement_theta_min      3.1760
_cell_volume                     1449.92(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.50a (Rigaku OD, 2019)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -59.00 -21.00   0.50    0.34    --  -38.82 141.00-175.00   76
  2  \w    -64.00 -32.00   0.50    0.34    --  -38.82 146.00  91.00   64
  3  \w    -68.00 -43.00   0.50    0.34    --  -38.82   7.00-173.00   50
  4  \w     15.00  40.00   0.50    0.34    --  -38.82   7.00-173.00   50
  5  \w     52.00  77.00   0.50    0.34    --   38.82   7.00-173.00   50
  6  \w     65.00  97.00   0.50    0.34    --   38.82-141.00 127.00   64
  7  \w      2.00  27.00   0.50    0.34    --   38.82   7.00-173.00   50
  8  \w     35.00  61.00   0.50    0.34    --   38.82-146.00  40.00   52
  9  \w     73.00 132.00   0.50    1.37    --  100.00 128.00  13.00  118
 10  \w     59.00 129.00   0.50    1.37    --  100.00-146.00  40.00  140
 11  \w     22.00  48.00   0.50    1.37    --  100.00  -7.00  10.00   52
 12  \w     85.00 110.00   0.50    1.37    --  100.00 146.00  91.00   50
 13  \w     81.00 106.00   0.50    1.37    --  100.00-141.00 127.00   50
 14  \w    -46.00  26.00   0.50    0.34    --  -38.82  43.00 150.00  144
 15  \w    -70.00 -45.00   0.50    0.34    --  -38.82 125.00 -74.00   50
 16  \w     67.00  92.00   0.50    0.34    --   38.82-138.00-150.00   50
 17  \w     35.00  66.00   0.50    0.34    --   38.82  32.00-180.00   62
 18  \w     15.00  59.00   0.50    0.34    --   38.82-138.00-150.00   88
 19  \w    -20.00   5.00   0.50    0.34    --   38.82  -7.00  10.00   50
 20  \w     31.00 109.00   0.50    1.37    --  100.00-111.00-150.00  156
 21  \w    115.00 140.00   0.50    1.37    --  100.00  30.00 -90.00   50
 22  \w     80.00 157.00   0.50    1.37    --  100.00 111.00-120.00  154
 23  \w     87.00 156.00   0.50    1.37    --  100.00  93.00 -90.00  138
 24  \w     43.00  93.00   0.50    1.37    --  100.00 -61.00-150.00  100
 25  \w     81.00 124.00   0.50    1.37    --  100.00  93.00 -60.00   86
 26  \w     40.00 103.00   0.50    1.37    --  100.00 -93.00-150.00  126
 27  \w     62.00  93.00   0.50    1.37    --  100.00 -53.00 150.00   62
 28  \w     78.00 103.00   0.50    1.37    --  100.00   7.00-173.00   50
 29  \w    -81.00 -48.00   0.50    0.34    --  -38.82 -43.00 -90.00   66
 30  \w      3.00  28.00   0.50    0.34    --  -38.82  77.00-180.00   50
 31  \w    -59.00 -33.00   0.50    0.34    --  -38.82  77.00-180.00   52
 32  \w     32.00  60.00   0.50    1.37    --  100.00-111.00 120.00   56
 33  \w     98.00 129.00   0.50    1.37    --  100.00  22.00-150.00   62
 34  \w     85.00 111.00   0.50    1.37    --  100.00  37.00-120.00   52
 35  \w     46.00  87.00   0.50    1.37    --  100.00 -69.00  90.00   82
 36  \w     33.00  60.00   0.50    1.37    --  100.00 -86.00  90.00   54
 37  \w     80.00 113.00   0.50    1.37    --  100.00 -86.00  90.00   66
 38  \w     85.00 111.00   0.50    1.37    --  100.00  22.00   0.00   52
 39  \w     79.00 105.00   0.50    1.37    --  100.00-111.00 120.00   52
 40  \w     82.00 112.00   0.50    1.37    --  100.00 -45.00  90.00   60
 41  \w     44.00  70.00   0.50    1.37    --  100.00 -93.00-120.00   52
 42  \w    129.00 154.00   0.50    1.37    --  100.00 111.00  90.00   50
 43  \w     87.00 112.00   0.50    1.37    --  100.00-133.00 -30.00   50
 44  \w     36.00  72.00   0.50    1.37    --  100.00 -45.00  90.00   72
 45  \w    119.00 145.00   0.50    1.37    --  100.00 128.00  13.00   52
 46  \w      5.00  31.00   0.50    0.34    --   38.82 -54.00  30.00   52
 47  \w    -15.00  20.00   0.50    0.34    --   38.82 -65.00-150.00   70
 48  \w     36.00  62.00   0.50    0.34    --   38.82 -65.00-150.00   52
 49  \w     64.00 111.00   0.50    1.37    --  100.00-111.00  60.00   94
 50  \w     81.00 107.00   0.50    1.37    --  100.00-111.00   0.00   52
 51  \w     42.00  74.00   0.50    1.37    --  100.00 -45.00   0.00   64
 52  \w     33.00  63.00   0.50    1.37    --  100.00-111.00-180.00   60
 53  \w     99.00 131.00   0.50    1.37    --  100.00  30.00 150.00   64
 54  \w     90.00 131.00   0.50    1.37    --  100.00 178.00 150.00   82
 55  \w     48.00  81.00   0.50    1.37    --  100.00 178.00 150.00   66
 56  \w     50.00  80.00   0.50    1.37    --  100.00-141.00 127.00   60
 57  \w    -50.00 -24.00   0.50    0.34    --  -38.82  21.00   0.00   52
 58  \w     -8.00  29.00   0.50    0.34    --  -38.82  21.00   0.00   74
 59  \w    -27.00  -2.00   0.50    0.34    --  -38.82 -11.00-180.00   50
 60  \w     -4.00  27.00   0.50    0.34    --  -38.82  43.00  60.00   62
 61  \w   -110.00 -85.00   0.50    0.34    --  -38.82 -11.00-180.00   50
 62  \w    -54.00 -28.00   0.50    0.34    --  -38.82  43.00  60.00   52
 63  \w     80.00 106.00   0.50    0.34    --   38.82  32.00 150.00   52
 64  \w     25.00  97.00   0.50    0.34    --   38.82-138.00 -90.00  144
 65  \w      5.00  31.00   0.50    0.34    --   38.82 -32.00 -60.00   52
 66  \w     35.00  63.00   0.50    0.34    --   38.82  32.00 150.00   56
 67  \w     28.00  53.00   0.50    0.34    --   38.82 -54.00-180.00   50
 68  \w    108.00 143.00   0.50    1.37    --  100.00 178.00  60.00   70
 69  \w     85.00 121.00   0.50    1.37    --  100.00 -77.00   0.00   72
 70  \w     93.00 119.00   0.50    1.37    --  100.00-133.00 150.00   52
 71  \w     52.00  78.00   0.50    1.37    --  100.00 178.00  60.00   52
 72  \w     98.00 123.00   0.50    1.37    --  100.00-133.00-150.00   50
 73  \w    132.00 157.00   0.50    1.37    --  100.00  61.00-120.00   50
 74  \w     86.00 157.00   0.50    1.37    --  100.00 133.00 120.00  142
 75  \w    101.00 127.00   0.50    1.37    --  100.00  22.00  30.00   52
 76  \w     62.00  88.00   0.50    1.37    --  100.00-133.00-150.00   52
 77  \w    119.00 156.00   0.50    1.37    --  100.00 133.00  60.00   74
 78  \w     32.00  61.00   0.50    1.37    --  100.00 -86.00 -60.00   58
 79  \w     86.00 112.00   0.50    1.37    --  100.00 -86.00 -60.00   52
 80  \w    104.00 135.00   0.50    1.37    --  100.00  77.00  60.00   62
 81  \w     37.00  90.00   0.50    1.37    --  100.00 -53.00 -30.00  106
 82  \w     95.00 154.00   0.50    1.37    --  100.00  93.00  90.00  118
 83  \w     88.00 114.00   0.50    1.37    --  100.00  61.00-120.00   52
 84  \w     93.00 121.00   0.50    1.37    --  100.00  45.00  60.00   56
 85  \w    124.00 149.00   0.50    1.37    --  100.00 178.00 -60.00   50
 86  \w     44.00  70.00   0.50    1.37    --  100.00 -77.00 -90.00   52
 87  \w     78.00 104.00   0.50    1.37    --  100.00 -77.00  90.00   52
 88  \w     84.00 114.00   0.50    1.37    --  100.00  77.00 150.00   60
 89  \w     60.00  88.00   0.50    1.37    --  100.00 -30.00 -60.00   56
 90  \w     81.00 115.00   0.50    1.37    --  100.00 111.00 -60.00   68
 91  \w     99.00 124.00   0.50    1.37    --  100.00 -77.00 -90.00   50
 92  \w     81.00 135.00   0.50    1.37    --  100.00 111.00  60.00  108
 93  \w    103.00 128.00   0.50    1.37    --  100.00-141.00 127.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1156400000
_diffrn_orient_matrix_UB_12      -0.1453219000
_diffrn_orient_matrix_UB_13      0.0008143000
_diffrn_orient_matrix_UB_21      0.0508624000
_diffrn_orient_matrix_UB_22      -0.3275789000
_diffrn_orient_matrix_UB_23      -0.0049457000
_diffrn_orient_matrix_UB_31      0.0062639000
_diffrn_orient_matrix_UB_32      -0.0267842000
_diffrn_orient_matrix_UB_33      0.0552512000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            13841
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.864
_diffrn_reflns_theta_min         3.183
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.538
_refine_diff_density_min         -1.331
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+1.4492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1331
_reflns_number_total             1429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119378.cif
_cod_data_source_block           8843-12855_at-5
_cod_database_code               1565440
_chemical_oxdiff_formula         'Pd Cl2 N4 C14'
_shelx_estimated_absorpt_t_max   0.548
_shelx_estimated_absorpt_t_min   0.170
_reflns_odcompleteness_completeness 97.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     72.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C1(H1), C7(H7), C4(H4), C3(H3), C6(H6), C5(H5)
;
_shelx_res_checksum              78592
_shelx_hkl_checksum              97146
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.441
_oxdiff_exptl_absorpt_empirical_full_min 0.593