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_7131649
_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         'C24 H16 Fe S6, 2(C9 H17 N2)'
_chemical_formula_sum            'C42 H50 Fe N4 S6'
_chemical_formula_weight         859.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.751(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.9805(8)
_cell_length_b                   16.3895(5)
_cell_length_c                   17.0828(8)
_cell_measurement_reflns_used    36511
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      60.6630
_cell_measurement_theta_min      2.5110
_cell_volume                     4245.3(4)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_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     85.00 146.00   0.50    0.09    --   72.80  95.00 -10.00  122
  2  \w     35.00  97.00   0.50    0.09    --   72.80 -77.00 120.00  124
  3  \w     59.00 141.00   0.50    0.09    --   72.80  19.00 120.00  164
  4  \w      2.00  91.00   0.50    0.09    --   72.80 -77.00   0.00  178
  5  \w      2.00  70.00   0.50    0.09    --   72.80 -38.00 -90.00  136
  6  \w     45.00  83.00   0.50    0.09    --   72.80 -77.00-120.00   76
  7  \w     37.00  66.00   0.50    0.09    --   72.80 -95.00-120.00   58
  8  \w      0.00 105.00   0.50    0.09    --   72.80 -99.00   0.00  210
  9  \w      8.00  34.00   0.50    0.09    --   72.80 -99.00 120.00   52
 10  \w     39.00 106.00   0.50    0.09    --   72.80 -99.00 120.00  134
 11  \w   -107.00 -30.00   0.50    0.09    --  -74.99 125.00-120.00  154
 12  \w    -96.00 -53.00   0.50    0.09    --  -74.99  95.00 -10.00   86
 13  \w    -83.00 -22.00   0.50    0.09    --  -74.99 125.00 150.00  122
 14  \w     -9.00  17.00   0.50    0.05    --   -1.09  95.00 -10.00   52
 15  \w      1.00  70.00   0.50    0.05    --   -1.09  77.00  30.00  138
 16  \w    -13.00  72.00   0.50    0.05    --   -1.09  38.00 -30.00  170
 17  \w    -50.00  -2.00   0.50    0.09    --  -74.99  57.00-180.00   96
 18  \w    -85.00 -53.00   0.50    0.09    --  -74.99  57.00-180.00   64
 19  \w    -70.00  -6.00   0.50    0.09    --  -74.99  38.00-180.00  128
 20  \w    -46.00  -5.00   0.50    0.09    --  -74.99  38.00 -90.00   82
 21  \w    -71.00  -1.00   0.50    0.09    --  -74.99  38.00 -60.00  140
 22  \w    -71.00 -15.00   0.50    0.09    --  -74.99  38.00 120.00  112
 23  \w   -119.00 -93.00   0.50    0.09    --  -74.99 -99.00   0.00   52
 24  \w   -132.00 -85.00   0.50    0.09    --  -74.99 -95.00-120.00   94
 25  \w    -26.00  26.00   0.50    0.05    --   -1.09 -95.00-120.00  104
;
_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      -0.0459610000
_diffrn_orient_matrix_UB_12      0.0310474000
_diffrn_orient_matrix_UB_13      -0.0804934000
_diffrn_orient_matrix_UB_21      0.0109738000
_diffrn_orient_matrix_UB_22      -0.0696886000
_diffrn_orient_matrix_UB_23      -0.0348656000
_diffrn_orient_matrix_UB_31      -0.0745931000
_diffrn_orient_matrix_UB_32      -0.0293987000
_diffrn_orient_matrix_UB_33      -0.0022757000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61423
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.575
_diffrn_reflns_theta_min         1.404
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71053
_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            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         9629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0330P)^2^+4.1177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8869
_reflns_number_total             9629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00778b2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7131647--7131649.cif.'
_cod_database_code               7131649
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.821
_diffrn_oxdiff_digest_frames
;
010cbc57d52dafd50d0adb11c0445865eb02848b88b
;
_diffrn_oxdiff_digest_hkl
;
01923caf5f9f89f977d777c04074ee6a305467
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_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.a Secondary CH2 refined with riding coordinates:
 C013(H01E,H01F), C014(H01G,H01H), C015(H01I,H01J), C01B(H01U,H01V), C01E(H01W,
 H01X), C01F(H01Y,H)
2.b Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00G(H00G), C00H(H00H), C00K(H00K), C00L(H00L), C00O(H00O),
 C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00W(H00W),
 C00X(H00X), C011(H011), C012(H012), C016(H016), C017(H017), C019(H019),
 C01C(H01K), C01D(H01D)
2.c Idealised Me refined as rotating group:
 C00Y(H00A,H00B,H00C), C010(H01A,H01B,H01C), C018(H01O,H01P,H01Q), C01A(H01R,
 H01S,H01T), C01G(H01L,H01M,H01N), C01H(H01Z,HA,HB)
;
_shelx_res_checksum              86679
_shelx_hkl_checksum              43495
_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 5.883
_oxdiff_exptl_absorpt_empirical_full_min 0.795