Sulfur heteroatom-based MOFs with long-lasting room-temperature phosphorescence and high photoelectric response.
Yang, Xiao-Gang; Zhai, Zhi-Min; Liu, Xin-Yi; Li, Jin-Yao; Li, Fei-Fei; Ma, Lu-Fang; Dalton transactions (Cambridge, England : 2003) 49 (2020) 598–602; doi:10.1039/c9dt04046c

data_7703084
_publ_section_title
;
 Sulfur heteroatom-based MOFs with long-lasting room-temperature
 phosphorescence and high photoelectric response.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              598
_journal_page_last               602
_journal_paper_doi               10.1039/c9dt04046c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C33 H29 N3 O19 S4 Zn3.5'
_chemical_formula_sum            'C33 H29 N3 O19 S4 Zn3.5'
_chemical_formula_weight         1128.63
_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
_audit_creation_date             2019-11-26
_audit_creation_method
;
Olex2 1.3-dev
(compiled Nov 20 2019 14:42:27 for OlexSys, GUI svn.r5830)
;
_audit_update_record
;
2019-11-28 deposited with the CCDC.	2019-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                66.763(6)
_cell_angle_beta                 66.652(6)
_cell_angle_gamma                69.687(5)
_cell_formula_units_Z            2
_cell_length_a                   15.4577(9)
_cell_length_b                   16.9810(11)
_cell_length_c                   19.2095(12)
_cell_measurement_reflns_used    9029
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.5910
_cell_measurement_theta_min      3.6320
_cell_volume                     4143.6(5)
_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-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -18.00  54.00   1.00    3.50    --  -13.80  77.00  60.00   72
  2  \w    -15.00  25.00   1.00    3.50    --  -13.80  77.00-150.00   40
  3  \w    -33.00  49.00   1.00    3.50    --  -13.80  77.00 -30.00   82
  4  \w    -10.00  82.00   1.00    3.50    --   14.82  77.00-180.00   92
  5  \w     -6.00  79.00   1.00    3.50    --   14.82  77.00 -60.00   85
  6  \w    -12.00  50.00   1.00    3.50    --   14.82  77.00  90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0865
_diffrn_reflns_av_unetI/netI     0.1185
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34945
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.338
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71272
_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_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.905
_exptl_crystal_description       block
_exptl_crystal_F_000             1138
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.290
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         14542
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0922
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1417P)^2^+3.9362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9956
_reflns_number_total             14542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04046c2.cif
_cod_data_source_block           y964
_cod_depositor_comments
'Adding full bibliography for 7703084--7703085.cif.'
_cod_original_formula_sum        'C33 H29 N3 O19 S4 Zn3.50'
_cod_database_code               7703084
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.747
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C26
 1.53 with sigma of 0.02
 C14-C16 \\sim C14A-C16A
 with sigma of 0.04
 S3-C14 \\sim S3-C14A
 with sigma of 0.02
 O9-C13 \\sim O9A-C13A
 with sigma of 0.02
 O10-C13 \\sim O10-C13A
 with sigma of 0.02
 O10-C14 \\sim O10-C14A
 with sigma of 0.04
 O11-C18 \\sim O11A-C18
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 C15-C17 \\sim C15A-C17
 with sigma of 0.04
 O9-C14 \\sim O9A-C14A
 with sigma of 0.04
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C13-C15 \\sim C13A-C15A
 with sigma of 0.04
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C16-C17 \\sim C16A-C17
 with sigma of 0.02
 S3-C13 \\sim S3-C13A
 with sigma of 0.04
 S3-C15 \\sim S3-C15A
 with sigma of 0.04
 O9-O10 \\sim O9A-O10
 with sigma of 0.04
 N3-C31 \\sim N3A-C31A
 with sigma of 0.02
 N3-C33 \\sim N3A-C33A
 with sigma of 0.02
 N3-C32 \\sim N3A-C32A
 with sigma of 0.02
 C32-C33 \\sim C32A-C33A
 with sigma of 0.04
 C31-C32 \\sim C31A-C32A
 with sigma of 0.04
 C31-C33 \\sim C31A-C33A
 with sigma of 0.04
 Zn3-C31 \\sim Zn3-C31A
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 S3, O10, O12, C17, C18, O11A, C14A, C15A, C16A, O9A, C13A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 S3, O9, O10, O11, O12, C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N3, C31, C32, C33
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O19A, N3A, C31A, C32A, C33A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(O11A)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(O9A)=
 Sof(C13A)=1-FVAR(1)
 Sof(O9)=Sof(O11)=Sof(C13)=Sof(C14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=FVAR(1)
 Sof(N3A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(2)
 Sof(N3)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(2)
5.a Riding coordinates:
 C30(H30A,H30B,H30C)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C15(H15), C16(H16), C21(H21), C22(H22),
 C25(H25), C28(H28), C31(H31), C15A(H15A), C16A(H16A), C31A(H31A)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C32A(H32D,H32E,H32F), C33A(H33D,H33E,H33F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              46411
_shelx_fab_checksum              95035
_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
;