Benzotrithiophene-based MOFs: interchromophoric interactions affected Ln(iii) crystallization selectivity and optoelectronic properties
Xie, Feng-Yang; Yang, Qi; Wang, Jia-Si; Yu, Hong-Yi; Li, Yue; Ruan, Wen-Juan; Dalton Transactions  (2021) –; doi:10.1039/D1DT02515E

data_7708840
_publ_section_title
;
 Benzotrithiophene-based MOFs: interchromophoric interactions affected
 Ln(iii) crystallization selectivity and optoelectronic properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02515E
_journal_year                    2021
_chemical_formula_moiety         'C32 H18 Lu2 O16 S7,8(C2 H6 O S)'
_chemical_formula_sum            'C48 H66 Lu2 O24 S15'
_chemical_formula_weight         1857.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-10-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-10-25 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.341(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.5391(10)
_cell_length_b                   15.4070(9)
_cell_length_c                   26.8983(9)
_cell_measurement_reflns_used    5644
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.8850
_cell_measurement_theta_min      4.2300
_cell_volume                     9337.3(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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    -27.00  89.00   1.00    4.00    --    0.00  19.00  90.00  116
  2  \w     87.00 132.00   1.00   12.00    --  101.30 -82.00  30.00   45
  3  \w     79.00 155.00   1.00   12.00    --  101.30  38.00-120.00   76
  4  \w     24.00 123.00   1.00   12.00    --  101.30 -77.00  90.00   99
  5  \w     17.00  71.00   1.00   12.00    --  101.30 -82.00  30.00   54
  6  \w     31.00 116.00   1.00   12.00    --  101.30 -38.00 -90.00   85
  7  \w     81.00 191.00   1.00   12.00    --  101.30  38.00-150.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0417660000
_diffrn_orient_matrix_UB_12      0.0717767000
_diffrn_orient_matrix_UB_13      0.0042932000
_diffrn_orient_matrix_UB_21      0.0287717000
_diffrn_orient_matrix_UB_22      -0.0066714000
_diffrn_orient_matrix_UB_23      0.0621999000
_diffrn_orient_matrix_UB_31      0.0458297000
_diffrn_orient_matrix_UB_32      0.0692324000
_diffrn_orient_matrix_UB_33      0.0015494000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18776
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        66.991
_diffrn_reflns_theta_max         66.991
_diffrn_reflns_theta_min         4.133
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    7.548
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (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    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
TITL 1_a.res in C2/c
CELL   24.5391   15.4070   26.8983     90.00    113.34     90.00
SPGR C2/c
Q101 0.533 0.372 0.575 !       2.67 eA-3
C102 0.500 0.312 0.755 !       2.40 eA-3
Q103 0.515 0.188 0.400 !       2.10 eA-3
C104 0.766 0.466 0.653 !       2.02 eA-3
Q105 0.531 0.412 0.049 !       1.87 eA-3
C106 0.884 0.330 0.061 !       1.80 eA-3
C107 0.198 0.217 0.783 !       1.79 eA-3
C108 0.648 0.221 0.252 !       1.78 eA-3
Q109 0.047 0.263 0.904 !       1.72 eA-3
C110 0.264 0.471 0.882 !       1.67 eA-3
C111 0.937 0.394 0.082 !       1.51 eA-3
C112 0.094 0.407 0.488 !       1.50 eA-3
Q113 0.584 0.410 0.072 !       1.47 eA-3
Q114 0.531 0.300 0.050 !       1.46 eA-3
C115 0.413 0.064 0.488 !       1.45 eA-3
C116 0.886 0.401 0.036 !       1.43 eA-3
C117 0.766 0.404 0.184 !       1.43 eA-3
C118 0.788 0.157 0.535 !       1.43 eA-3
C119 0.243 0.251 0.789 !       1.42 eA-3
C120 0.432 0.252 0.704 !       1.41 eA-3
C121 0.213 0.373 0.187 !       1.41 eA-3
C122 0.267 0.290 0.229 !       1.40 eA-3
C123 0.276 0.311 0.186 !       1.37 eA-3
C124 0.961 0.221 0.232 !       1.37 eA-3
Q125 0.087 0.191 0.571 !       1.36 eA-3
C126 0.216 0.297 0.210 !       1.35 eA-3
Q127 0.562 0.309 0.554 !       1.35 eA-3
C128 0.700 0.315 0.423 !       1.32 eA-3
C129 0.272 0.239 0.197 !       1.31 eA-3
C130 0.783 0.058 0.395 !       1.29 eA-3
C131 0.741 0.952 0.395 !       1.29 eA-3
C132 0.241 0.452 0.395 !       1.29 eA-3
Q133 0.500 0.360 0.025 !       1.21 eA-3
C134 0.180 0.293 0.194 !       1.20 eA-3
Q135 0.032 0.216 0.077 !       1.20 eA-3
C136 0.712 0.188 0.680 !       1.19 eA-3
C137 0.686 0.314 0.492 !       1.18 eA-3
Q138 0.076 0.137 0.117 !       1.18 eA-3
C139 0.306 0.317 0.031 !       1.17 eA-3
C140 0.738 0.105 0.586 !       1.14 eA-3
C141 0.203 0.169 0.009 !       1.14 eA-3
C142 0.742 0.373 0.478 !       1.11 eA-3
C143 0.737 0.276 0.481 !       1.10 eA-3
C144 0.750 0.339 0.331 !       1.10 eA-3
Q145 0.503 0.287 0.219 !       1.10 eA-3
C146 0.925 0.232 0.231 !       1.04 eA-3
C147 0.972 0.234 0.695 !       1.02 eA-3
C148 0.218 0.435 0.030 !       1.02 eA-3
C149 0.208 0.405 0.211 !       1.01 eA-3
C150 0.728 0.199 0.495 !       1.01 eA-3
Q151 0.565 0.469 0.360 !       1.00 eA-3
C152 0.135 0.404 0.179 !       0.99 eA-3
Q153 0.762 0.347 0.928 !       0.99 eA-3
C154 0.883 0.484 0.837 !       0.98 eA-3
C155 0.259 0.293 0.071 !       0.97 eA-3
Q156 0.545 0.354 0.032 !       0.96 eA-3
C157 0.168 0.478 0.049 !       0.96 eA-3
C158 0.117 0.328 0.315 !       0.96 eA-3
C159 0.833 0.491 0.455 !       0.96 eA-3
C160 0.719 0.205 0.652 !       0.95 eA-3
Q161 0.564 0.354 0.094 !       0.95 eA-3
C162 0.836 0.460 0.315 !       0.94 eA-3
C163 0.311 0.296 0.117 !       0.94 eA-3
C164 0.189 0.204 0.883 !       0.94 eA-3
Q165 0.962 0.051 0.000 !       0.93 eA-3
C166 0.292 0.101 0.844 !       0.93 eA-3
C167 0.189 0.375 0.208 !       0.93 eA-3
C168 0.643 0.123 0.244 !       0.93 eA-3
Q169 0.612 0.355 0.100 !       0.93 eA-3
C170 0.206 0.359 0.084 !       0.93 eA-3
C171 0.275 0.345 0.088 !       0.91 eA-3
Q172 0.626 0.469 0.865 !       0.91 eA-3
C173 0.539 0.262 0.807 !       0.91 eA-3
C174 0.170 0.454 0.086 !       0.90 eA-3
C175 0.814 0.435 0.382 !       0.90 eA-3
C176 0.675 0.167 0.271 !       0.90 eA-3
Q177 0.672 0.307 0.516 !       0.90 eA-3
C178 0.838 0.484 0.001 !       0.90 eA-3
Q179 0.006 0.162 0.468 !       0.89 eA-3
Q180 0.539 0.092 0.424 !       0.89 eA-3
Q181 0.428 0.112 0.067 !       0.88 eA-3
C182 0.325 0.197 0.748 !       0.88 eA-3
Q183 0.400 0.433 0.387 !       0.88 eA-3
C184 0.253 0.344 0.141 !       0.87 eA-3
C185 0.279 0.238 0.082 !       0.87 eA-3
C186 0.221 0.262 0.918 !       0.87 eA-3
C187 0.640 0.019 0.653 !       0.87 eA-3
C188 0.085 0.295 0.319 !       0.87 eA-3
C189 0.706 0.276 0.506 !       0.87 eA-3
C190 0.161 0.320 0.212 !       0.87 eA-3
C191 0.901 0.275 0.221 !       0.86 eA-3
C192 0.695 0.115 0.556 !       0.86 eA-3
C193 0.305 0.104 0.946 !       0.86 eA-3
C194 0.576 0.019 0.305 !       0.85 eA-3
C195 0.678 0.019 0.523 !       0.85 eA-3
C196 0.302 0.097 0.916 !       0.85 eA-3
Q197 0.390 0.476 0.347 !       0.83 eA-3
C198 0.462 0.059 0.492 !       0.83 eA-3
C199 0.773 0.355 0.384 !       0.83 eA-3
;
_refine_diff_density_max         2.161
_refine_diff_density_min         -1.637
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         8214
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0937
_refine_ls_R_factor_gt           0.0810
_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^)+(0.1731P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2462
_refine_ls_wR_factor_ref         0.2558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6060
_reflns_number_total             8214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02515e2.cif
_cod_data_source_block           1_sq
_cod_database_code               7708840
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.504
_shelx_estimated_absorpt_t_min   0.483
_reflns_odcompleteness_completeness 98.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 S4-C16 = S4-C17
 1.76 with sigma of 0.02
 C16-C17
 2.7 with sigma of 0.04
 Lu1-O7 \\sim Lu1-O7A
 with sigma of 0.02
 S4-O7 \\sim S4-O7A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
S4 \\sim O7 \\sim C16 \\sim C17: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C10A)
\\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C2) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) = Uanis(O7A)
Uanis(C13) = Uanis(S3A)
3. Others
 Sof(S1A)=Sof(C3A)=Sof(H3A)=Sof(S2A)=Sof(C10A)=Sof(H10A)=Sof(S3A)=Sof(C13A)=
 Sof(H13A)=1-FVAR(1)
 Sof(S1)=Sof(C3)=Sof(H3)=Sof(S2)=Sof(C10)=Sof(H10)=Sof(S3)=Sof(C13)=Sof(H13)=
 FVAR(1)
 Fixed Sof: S4(0.5) O7(0.5) C16(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C17(0.5)
 H17A(0.5) H17B(0.5) H17C(0.5) O7A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C3A(H3A), C10(H10), C10A(H10A), C13(H13), C13A(H13A)
4.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_platon_squeeze_void_probe_radius 1.20
_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 12.827
_oxdiff_exptl_absorpt_empirical_full_min 0.302