Thiophenol-spaced 2D coordination polymers with extraordinary alkali resistance and efficient photothermal conversion.
Hou, Qin; Chen, Li-Jun; He, Jing; Chen, Er-Xia; Wang, Bo; Zhou, Xuechou; Dai, Yumei; He, Liang; Lin, Qipu; Chemical communications (Cambridge, England) 59 (2023) 7072–7075; doi:10.1039/d3cc00778b

data_7131648
_publ_section_title
;
 Thiophenol-spaced 2D coordination polymers with extraordinary alkali
 resistance and efficient photothermal conversion.
;
_journal_issue                   46
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7072
_journal_page_last               7075
_journal_paper_doi               10.1039/d3cc00778b
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C48 H32 S12 Zn2, 4(C9 H19 N2)'
_chemical_formula_sum            'C84 H108 N8 S12 Zn2'
_chemical_formula_weight         1745.24
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-19
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.35023(6)
_cell_length_b                   11.35023(6)
_cell_length_c                   34.2177(3)
_cell_measurement_reflns_used    21229
_cell_measurement_temperature    199.99(10)
_cell_measurement_theta_max      60.0340
_cell_measurement_theta_min      3.5670
_cell_volume                     4408.19(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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     59.00 150.00   0.50    0.22    --   76.57  57.00 -90.00  182
  2  \w     81.00 147.00   0.50    0.22    --   76.57 125.00  60.00  132
  3  \w     79.00 144.00   0.50    0.22    --   76.57 125.00 -30.00  130
  4  \w     86.00 150.00   0.50    0.22    --   76.57  96.00 -74.00  128
  5  \w    -37.00  11.00   0.50    0.06    --   -0.78  96.00 -74.00   96
  6  \w    -14.00  70.00   0.50    0.06    --   -0.78  57.00   0.00  168
  7  \w    -37.00 -11.00   0.50    0.22    --  -78.14  38.00-150.00   52
  8  \w    -79.00 -54.00   0.50    0.22    --  -78.14  96.00 -74.00   50
  9  \w    -38.00 -13.00   0.50    0.22    --  -78.14  38.00-120.00   50
 10  \w    -89.00 -20.00   0.50    0.22    --  -78.14 125.00 -60.00  138
 11  \w    -66.00 -35.00   0.50    0.22    --  -78.14  38.00  90.00   62
 12  \w    -30.00  -4.00   0.50    0.22    --  -78.14  38.00  90.00   52
 13  \w     17.00  91.00   0.50    0.22    --   76.57 -57.00 120.00  148
 14  \w     20.00  46.00   0.50    0.22    --   76.57-125.00 120.00   52
 15  \w     52.00 104.00   0.50    0.22    --   76.57-125.00 120.00  104
 16  \w     55.00 109.00   0.50    0.22    --   76.57-125.00  90.00  108
 17  \w     57.00 106.00   0.50    0.22    --   76.57 -96.00 176.00   98
 18  \w     32.00 103.00   0.50    0.22    --   76.57 -77.00  90.00  142
 19  \w     50.00  97.00   0.50    0.22    --   76.57-125.00   0.00   94
 20  \w     40.00  94.00   0.50    0.22    --   76.57-125.00 -60.00  108
 21  \w     -4.00  23.00   0.50    0.06    --   -0.78 -99.00  60.00   54
 22  \w     -8.00  17.00   0.50    0.06    --   -0.78 -99.00-150.00   50
 23  \w     -2.00  37.00   0.50    0.06    --   -0.78 -99.00  30.00   78
 24  \w    -17.00  33.00   0.50    0.06    --   -0.78 -96.00 176.00  100
 25  \w   -152.00 -55.00   0.50    0.22    --  -78.14 -57.00  90.00  194
 26  \w   -135.00 -85.00   0.50    0.22    --  -78.14 -96.00 176.00  100
 27  \w   -147.00 -95.00   0.50    0.22    --  -78.14 -99.00 -90.00  104
 28  \w   -145.00 -79.00   0.50    0.22    --  -78.14-125.00-120.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0853168000
_diffrn_orient_matrix_UB_12      0.0426919000
_diffrn_orient_matrix_UB_13      -0.0230333000
_diffrn_orient_matrix_UB_21      0.0788471000
_diffrn_orient_matrix_UB_22      0.0179745000
_diffrn_orient_matrix_UB_23      -0.0284868000
_diffrn_orient_matrix_UB_31      -0.0205225000
_diffrn_orient_matrix_UB_32      -0.1085368000
_diffrn_orient_matrix_UB_33      -0.0137730000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            29764
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.274
_diffrn_reflns_theta_min         3.567
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    2.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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    1.315
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2505
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0511
_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^)+(0.1010P)^2^+3.0553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1590
_refine_ls_wR_factor_ref         0.1643
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2247
_reflns_number_total             2505
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00778b2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7131647--7131649.cif.'
_cod_original_cell_volume        4408.19(6)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7131648
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.529
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1 = N00B-C3
 1.45 with sigma of 0.02
 C7-C6 = C6-C5 = C5-C4
 1.5 with sigma of 0.02
 C00A-C
 1.5 with sigma of 0.02
 C7-C6 \\sim C6-C5 \\sim C5-C4
 with sigma of 0.02
 N1-C4 \\sim N00B-C2
 with sigma of 0.02
 N1-C1 \\sim N00B-C3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C00A \\sim N00B \\sim C \\sim N1 \\sim C3 \\sim C1 \\sim C4 \\sim C5
\\sim C6 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
4. Rigid body (RIGU) restrains
 C2, C00A, N00B, C, N1, C3, C1, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: C00A(0.5) N00B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C(0.5) HA(0.5)
 HB(0.5) HC(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) N1(0.5) C1(0.5) H1A(0.5)
 H1B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5)
 H6B(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 C006(H006), C007(H007), C008(H008), C009(H009)
6.c Idealised Me refined as rotating group:
 C(HA,HB,HC), C2(H2A,H2B,H2C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              95218
_shelx_hkl_checksum              52521
_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 2.091
_oxdiff_exptl_absorpt_empirical_full_min 0.563