Crystal engineering of coordination-polymer-based iodine absorbents using π-electron-rich polycarboxylate aryl ether ligand
Chen, Junling; Li, Bo; Shi, Zhen-Zhen; He, Cheng; Duan, Chunying; Zhang, Tiexin; Wang, Liya; CrystEngComm  (2020) –; doi:10.1039/D0CE01004A

data_7241190
_publ_section_title
;
 Crystal engineering of coordination-polymer-based iodine absorbents using
 \p-electron-rich polycarboxylate aryl ether ligand
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01004A
_journal_year                    2020
_chemical_formula_moiety         'C23 H16 O16 Zn3, H2 O'
_chemical_formula_sum            'C23 H18 O17 Zn3'
_chemical_formula_weight         762.48
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-08-27 deposited with the CCDC.	2020-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.6198(4)
_cell_length_b                   11.9264(3)
_cell_length_c                   14.1457(4)
_cell_measurement_reflns_used    11049
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7370
_cell_measurement_theta_min      3.5970
_cell_volume                     2972.59(13)
_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 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      293.0
_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 0.932
_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    -20.00  25.00   1.00    5.00    --  -13.80 -99.00 -30.00   45
  2  \w    -41.00  54.00   1.00    5.00    --  -13.80  77.00 -90.00   95
  3  \w     -2.00  82.00   1.00    5.00    --   14.82  57.00 150.00   84
  4  \w    -52.00  32.00   1.00    5.00    --   14.82 -57.00 -60.00   84
  5  \w    -53.00  37.00   1.00    5.00    --   14.82 -77.00  60.00   90
  6  \w    -12.00  82.00   1.00    5.00    --   14.82  77.00-180.00   94
  7  \w    -11.00  54.00   1.00    5.00    --   14.82 -99.00  60.00   65
;
_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      0.0279149000
_diffrn_orient_matrix_UB_12      -0.0191098000
_diffrn_orient_matrix_UB_13      -0.0323443000
_diffrn_orient_matrix_UB_21      -0.0036604000
_diffrn_orient_matrix_UB_22      0.0504966000
_diffrn_orient_matrix_UB_23      -0.0261285000
_diffrn_orient_matrix_UB_31      0.0287617000
_diffrn_orient_matrix_UB_32      0.0249072000
_diffrn_orient_matrix_UB_33      0.0280633000
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34558
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.473
_diffrn_reflns_theta_min         3.349
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71264
_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_density_diffrn    0.852
_exptl_crystal_description       block
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2125 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         6885
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0517P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.842
_reflns_number_gt                5524
_reflns_number_total             6885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01004a2.cif
_cod_data_source_block           1911376
_cod_database_code               7241190
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.693
_shelx_estimated_absorpt_t_min   0.678
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2') \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O4') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2') = Uanis(O2)
Uanis(O4) = Uanis(O4')
3. Others
 Sof(O2')=1-FVAR(1)
 Sof(O2)=FVAR(1)
 Sof(O4')=1-FVAR(2)
 Sof(O4)=FVAR(2)
4.a Riding coordinates:
 O7(H7), O8(H8), O9(H9A,H9B), O10(H10A)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8A), C10(H10)
;
_shelx_res_checksum              76376
_shelx_fab_checksum              74153
_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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.723