The first 3, 5, 6-trichloropyridine-2-oxyacetate bridged manganese coordination polymer with features of π⋯π stacking and halogen⋯halogen interactions: Synthesis, crystal analysis and magnetic properties
Li, Jun-Xia; Du, Zhong-Xiang; Pan, Qiu-Yue; Zhang, Lu-Lu; Liu, Duo-Li; Inorganica Chimica Acta 509 (2020) 119677–; doi:10.1016/j.ica.2020.119677

data_1564447
_publ_section_title
;
 The first 3, 5, 6-trichloropyridine-2-oxyacetate bridged manganese
 coordination polymer with features of \p&#x22EF;\p stacking and
 halogen&#x22EF;halogen interactions: Synthesis, crystal analysis and
 magnetic properties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119677
_journal_paper_doi               10.1016/j.ica.2020.119677
_journal_volume                  509
_journal_year                    2020
_chemical_formula_moiety         'C24 H14 Cl6 Mn N4 O6'
_chemical_formula_sum            'C24 H14 Cl6 Mn N4 O6'
_chemical_formula_weight         722.03
_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
_atom_sites_solution_primary     iterative
_cell_angle_alpha                77.275(7)
_cell_angle_beta                 83.739(6)
_cell_angle_gamma                85.560(6)
_cell_formula_units_Z            2
_cell_length_a                   7.2516(4)
_cell_length_b                   10.5428(9)
_cell_length_c                   18.8180(16)
_cell_measurement_reflns_used    4135
_cell_measurement_temperature    289(2)
_cell_measurement_theta_max      28.1780
_cell_measurement_theta_min      3.7330
_cell_volume                     1392.85(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      289.2
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_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    -14.00  13.00   1.00   38.50    --  -13.80 -99.00-180.00   27
  2  \w    -12.00  18.00   1.00   38.50    --  -13.80 -99.00 120.00   30
  3  \w    -64.00   7.00   1.00   38.50    --  -13.80 -77.00 -90.00   71
  4  \w    -46.00  29.00   1.00   38.50    --   14.82 -57.00-150.00   75
  5  \w    -46.00  32.00   1.00   38.50    --   14.82 -57.00 -30.00   78
  6  \w     -2.00  32.00   1.00   38.50    --   14.82 -57.00   0.00   34
  7  \w     -4.00  84.00   1.00   38.50    --   14.82  38.00 150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0219605000
_diffrn_orient_matrix_UB_12      0.0465956000
_diffrn_orient_matrix_UB_13      0.0221011000
_diffrn_orient_matrix_UB_21      0.0224048000
_diffrn_orient_matrix_UB_22      0.0507268000
_diffrn_orient_matrix_UB_23      -0.0307047000
_diffrn_orient_matrix_UB_31      -0.0934218000
_diffrn_orient_matrix_UB_32      0.0052253000
_diffrn_orient_matrix_UB_33      -0.0086851000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4898
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.286
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       prism
_exptl_crystal_F_000             722
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.995
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0678
_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/[\s^2^(Fo^2^)+(0.0920P)^2^+0.7336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1855
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3568
_reflns_number_total             4898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-509-119677.cif
_cod_data_source_block           ljx091010-2_tw
_cod_database_code               1564447
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.749
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.634(5)
 0.366(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C13(H13a,H13b)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22),
 C23(H23), C24(H24)
;
_shelx_res_checksum              6463
_shelx_hkl_checksum              29162
_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 2.293
_oxdiff_exptl_absorpt_empirical_full_min 0.676