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_7241187
_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         'C29 H24 N2 O15 Zn3, H2 O'
_chemical_formula_sum            'C29 H26 N2 O16 Zn3'
_chemical_formula_weight         854.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-08-27 deposited with the CCDC.	2020-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.033(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8756(6)
_cell_length_b                   17.0258(7)
_cell_length_c                   14.8329(8)
_cell_measurement_reflns_used    6658
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.0370
_cell_measurement_theta_min      3.8500
_cell_volume                     3191.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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  (Sheldrick, 2015)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     34.00  86.00   1.00   14.73    --   13.55-178.00   0.00   52
  2  \w     34.00  86.00   1.00   14.73    --   13.55-178.00 -90.00   52
  3  \w    -13.00  81.00   1.00   14.73    --   13.55  77.00  30.00   94
  4  \w      4.00  79.00   1.00   14.73    --   13.55  38.00 150.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0005334000
_diffrn_orient_matrix_UB_12      0.0346042000
_diffrn_orient_matrix_UB_13      0.0265066000
_diffrn_orient_matrix_UB_21      -0.0370569000
_diffrn_orient_matrix_UB_22      0.0172029000
_diffrn_orient_matrix_UB_23      -0.0361893000
_diffrn_orient_matrix_UB_31      -0.0421696000
_diffrn_orient_matrix_UB_32      -0.0155257000
_diffrn_orient_matrix_UB_33      0.0190270000
_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  0.0294
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16990
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.339
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
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    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         5593
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0359P)^2^+3.3365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4654
_reflns_number_total             5593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01004a2.cif
_cod_data_source_block           1588500
_cod_database_code               7241187
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.543
_shelx_estimated_absorpt_t_min   0.506
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C28' \\sim C28 \\sim N2 \\sim C27 \\sim C29: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 3.8A
C26 \\sim N1 \\sim C24 \\sim C25: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
3. Others
 Sof(C28')=Sof(H28d)=Sof(H28e)=Sof(H28f)=1-FVAR(1)
 Sof(C28)=Sof(H28a)=Sof(H28b)=Sof(H28c)=FVAR(1)
4.a Riding coordinates:
 O13(H13), C25(H25a,H25b,H25c), C28(H28a,H28b,H28c), C28'(H28d,H28e,H28f),
 C26(H26a,H26b,H26c), C29(H29a,H29b,H29c), O1W(H1Wa,H1Wb)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C10(H10), C12(H12), C14(H14), C16(H16),
 C18(H18), C27(H27), C24(H24)
;
_shelx_res_checksum              89877
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.740