The crystal structure of poly[2-(4-carboxypyridin-3-yl)terephthalpoly[diaqua-(μ4-2-(6-carboxylatopyridin-3-yl)terephthalato-κ5O,N:O′:O″,O‴)]) cadmium(II)] dihydrate, C28H20Cd3N2O16
Li, Wenqiang; Zhang, Jingxiao; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 977–979; doi:10.1515/ncrs-2023-0306

data_8107616
_publ_section_title
;
 The crystal structure of
 poly[2-(4-carboxypyridin-3-yl)terephthalpoly[diaqua-(\m4-2-(6-carboxylatopyridin-3-yl)terephthalato-\k5O,N:O&#x2032;:O&#x2033;,O&#x2034;)])
 cadmium(II)] dihydrate, C28H20Cd3N2O16
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              977
_journal_page_last               979
_journal_paper_doi               10.1515/ncrs-2023-0306
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C28 H20 Cd3 N2 O16'
_chemical_formula_sum            'C28 H20 Cd3 N2 O16'
_chemical_formula_weight         977.66
_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   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                104.473(4)
_cell_angle_beta                 91.566(4)
_cell_angle_gamma                90.191(4)
_cell_formula_units_Z            1
_cell_length_a                   7.3205(3)
_cell_length_b                   9.9488(5)
_cell_length_c                   10.0326(5)
_cell_measurement_reflns_used    3981
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.4020
_cell_measurement_theta_min      4.1900
_cell_volume                     707.19(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293
_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 0.857
_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    -78.00   6.00   1.00   10.00    --  -15.61 -19.00  90.00   84
  2  \w    -26.00  35.00   1.00   10.00    --  -15.61  77.00  30.00   61
  3  \w    -13.00  42.00   1.00   10.00    --  -15.61  77.00 -90.00   55
  4  \w    -73.00  -1.00   1.00   10.00    --  -15.61 -57.00-150.00   72
  5  \w    -10.00  40.00   1.00   10.00    --   16.78  77.00 150.00   50
  6  \w     -3.00  56.00   1.00   10.00    --   16.78 -99.00  30.00   59
;
_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      -0.0921433000
_diffrn_orient_matrix_UB_12      -0.0114529000
_diffrn_orient_matrix_UB_13      0.0147153000
_diffrn_orient_matrix_UB_21      0.0300859000
_diffrn_orient_matrix_UB_22      -0.0306883000
_diffrn_orient_matrix_UB_23      0.0532854000
_diffrn_orient_matrix_UB_31      -0.0008645000
_diffrn_orient_matrix_UB_32      0.0659490000
_diffrn_orient_matrix_UB_33      0.0477505000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0152
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.857
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6111
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.857
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.969
_diffrn_reflns_theta_min         3.437
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
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    2.296
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3206
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0242P)^2^+0.6574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0576
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2917
_reflns_number_total             3206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0306_suppl_001.cif
_cod_data_source_block           h3cd_auto
_cod_database_code               8107616
_reflns_odcompleteness_completeness 99.76
_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. Restrained distances
 Cd1-H8A \\sim Cd1-H8B
 with sigma of 0.02
3.a Free rotating group:
 O8(H8A,H8B)
3.b Rotating group:
 O7(H7A,H7B)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C2(H2), C5(H5), C11(H11), C10(H10)
;
_shelx_res_checksum              98565
_shelx_hkl_checksum              19137
_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 1.546
_oxdiff_exptl_absorpt_empirical_full_min 0.597