Crystal structure of coordination polymer catena-poly[diaqua-(2,6-dichloropyridine-4-carboxyliato-κ2 O,O′)-bis(μ2-2,6-dichloropyridine-4-carboxyliato-κ2 O:O′)terbium(III), C18H10Cl6N3O8Tb
Liu, Guang-Zhen; Xin, Ling-Yun; Li, Xiao-Ling; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 449–450; doi:10.1515/ncrs-2018-0461

data_8105677
_publ_section_title
;
 Crystal structure of coordination polymer
 catena-poly[diaqua-(2,6-dichloropyridine-4-carboxyliato-\k2
 O,O&#x2032;)-bis(\m2-2,6-dichloropyridine-4-carboxyliato-\k2
 O:O&#x2032;)terbium(III), C18H10Cl6N3O8Tb
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              449
_journal_page_last               450
_journal_paper_doi               10.1515/ncrs-2018-0461
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C9 H5 Cl3 N1.5 O4 Tb0.5'
_chemical_formula_sum            'C9 H5 Cl3 N1.5 O4 Tb0.5'
_chemical_formula_weight         383.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 91.1599(19)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.8281(2)
_cell_length_b                   11.8792(2)
_cell_length_c                   21.1568(4)
_cell_measurement_reflns_used    7199
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1410
_cell_measurement_theta_min      4.1060
_cell_volume                     2469.55(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -89.00 -63.00   1.00    3.76    --  -16.00 178.00-120.00   26
  2  \w    -48.00  44.00   1.00    3.76    --   16.93 -77.00   0.00   92
  3  \w     -2.00  82.00   1.00    3.76    --   16.93  38.00 -90.00   84
  4  \w     -9.00  84.00   1.00    3.76    --   16.93  77.00 -90.00   93
  5  \w    -10.00  40.00   1.00    3.76    --   16.93  77.00 120.00   50
;
_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      -0.0620308000
_diffrn_orient_matrix_UB_12      -0.0106023000
_diffrn_orient_matrix_UB_13      -0.0166306000
_diffrn_orient_matrix_UB_21      0.0238747000
_diffrn_orient_matrix_UB_22      0.0307099000
_diffrn_orient_matrix_UB_23      -0.0262535000
_diffrn_orient_matrix_UB_31      0.0278281000
_diffrn_orient_matrix_UB_32      -0.0501064000
_diffrn_orient_matrix_UB_33      -0.0126130000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9301
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         3.285
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.563
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60038
_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    2.065
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.00016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         2297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0196
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+5.7161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0473
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2240
_reflns_number_total             2297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0461_suppl.cif
_cod_data_source_block           xly-24
_cod_original_cell_volume        2469.54(9)
_cod_original_formula_sum        'C9 H5 Cl3 N1.50 O4 Tb0.50'
_cod_database_code               8105677
_shelx_estimated_absorpt_t_max   0.405
_shelx_estimated_absorpt_t_min   0.352
_reflns_odcompleteness_completeness 91.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9)
;