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_7708841
_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         'C72 H36 Yb6 O42 S15, 4(C2 H6 O S), 4(H2O)'
_chemical_formula_sum            'C80 H78 O50 S19 Yb6'
_chemical_formula_weight         3486.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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                 115.487(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9644(3)
_cell_length_b                   28.2692(5)
_cell_length_c                   17.0535(4)
_cell_measurement_reflns_used    22665
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.2840
_cell_measurement_theta_min      3.8050
_cell_volume                     6512.1(3)
_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    'olex2.solve 1.3 (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_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.836
_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    -40.00  35.00   0.50    4.00    --   -1.30 -82.00 120.00  150
  2  \w    -87.00  18.00   0.50    4.00    --   -1.30 -38.00 150.00  210
;
_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      -0.0280348000
_diffrn_orient_matrix_UB_12      0.0167995000
_diffrn_orient_matrix_UB_13      0.0108863000
_diffrn_orient_matrix_UB_21      0.0232041000
_diffrn_orient_matrix_UB_22      0.0186097000
_diffrn_orient_matrix_UB_23      -0.0122372000
_diffrn_orient_matrix_UB_31      -0.0378314000
_diffrn_orient_matrix_UB_32      -0.0010699000
_diffrn_orient_matrix_UB_33      -0.0430696000
_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  0.0197
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21802
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.134
_diffrn_reflns_theta_min         3.590
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.647
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68559
_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            'light yellow'
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
TITL yb-2_a.res in I2/m
CELL   14.9644   28.2692   17.0535     90.00    115.49     90.00
SPGR I2/m
C101 0.500 0.125 0.000 !       4.92 eA-3
Q102 0.262 0.524 0.035 !       3.37 eA-3
C103 0.469 0.043 0.134 !       2.67 eA-3
Q104 0.356 0.523 0.011 !       2.63 eA-3
C105 0.200 0.998 0.234 !       2.51 eA-3
C106 0.479 0.160 0.050 !       2.45 eA-3
C107 1.000 0.859 0.003 !       2.38 eA-3
C108 0.516 0.180 0.046 !       1.91 eA-3
Q109 0.344 0.504 0.063 !       1.86 eA-3
Q110 0.331 0.444 0.016 !       1.75 eA-3
C111 0.050 0.497 0.391 !       1.71 eA-3
C112 0.739 0.498 0.219 !       1.71 eA-3
Q113 0.677 0.502 0.156 !       1.69 eA-3
Q114 0.747 0.338 0.146 !       1.67 eA-3
Q115 0.142 0.553 0.047 !       1.64 eA-3
Q116 0.889 0.350 0.407 !       1.63 eA-3
C117 0.549 1.000 0.156 !       1.59 eA-3
Q118 0.736 0.146 0.138 !       1.55 eA-3
Q119 0.618 0.948 0.345 !       1.52 eA-3
Q120 0.828 0.118 0.215 !       1.47 eA-3
C121 0.124 0.921 0.082 !       1.42 eA-3
C122 0.438 0.093-0.002 !       1.39 eA-3
C123 0.405 1.002 0.141 !       1.38 eA-3
C124 0.398 0.980 0.158 !       1.36 eA-3
C125 0.411 0.965 0.147 !       1.35 eA-3
Q126 0.422 0.504 0.078 !       1.29 eA-3
C127 0.548 0.590 0.575 !       1.22 eA-3
C128 0.048 0.090 0.075 !       1.22 eA-3
Q129 0.809 0.541 0.093 !       1.20 eA-3
C130 0.114 0.036 0.178 !       1.20 eA-3
C131 0.522 0.607 0.559 !       1.20 eA-3
Q132 0.085 0.542 0.061 !       1.16 eA-3
Q133 0.552 0.149 0.113 !       1.15 eA-3
C134 0.530 0.414 0.481 !       1.15 eA-3
Q135 0.812 0.900 0.140 !       1.12 eA-3
C136 0.524 0.992 0.202 !       1.11 eA-3
C137 0.158 0.025 0.168 !       1.10 eA-3
Q138 0.731 0.703 0.125 !       1.10 eA-3
C139 0.412 0.115 0.027 !       1.06 eA-3
Q140 0.779 0.064 0.187 !       1.06 eA-3
C141 0.137 0.048 0.125 !       1.04 eA-3
Q142 0.827 0.622 0.183 !       1.03 eA-3
Q143 0.483 0.047 0.346 !       1.01 eA-3
C144 0.088 0.986 0.239 !       0.99 eA-3
C145 0.082 0.034 0.217 !       0.98 eA-3
Q146 0.750 0.313 0.184 !       0.98 eA-3
Q147 0.684 0.679 0.155 !       0.97 eA-3
Q148 0.065 0.554 0.124 !       0.97 eA-3
C149 0.138 0.499 0.469 !       0.94 eA-3
C150 1.000 0.922-0.013 !       0.93 eA-3
Q151 0.686 0.680 0.090 !       0.93 eA-3
Q152 0.564 0.016 0.455 !       0.89 eA-3
C153 0.278 1.003 0.172 !       0.89 eA-3
C154 0.388 0.946 0.036 !       0.88 eA-3
Q155 0.947 0.865 0.046 !       0.87 eA-3
Q156 0.630 0.344 0.092 !       0.83 eA-3
Q157 0.794 0.281 0.194 !       0.83 eA-3
Q158 0.906 0.510 0.097 !       0.81 eA-3
C159 0.014 1.000 0.141 !       0.80 eA-3
C160 0.381 0.496 0.328 !       0.79 eA-3
Q161 0.451 0.439 0.100 !       0.79 eA-3
Q162 0.485 0.446 0.329 !       0.78 eA-3
Q163 0.642 0.633 0.395 !       0.78 eA-3
Q164 0.373 0.931 0.393 !       0.77 eA-3
C165 0.477 0.467 0.325 !       0.72 eA-3
C166 0.055 0.062 0.146 !       0.69 eA-3
Q167 0.668 0.360 0.110 !       0.69 eA-3
Q168 0.987 0.079 0.140 !       0.69 eA-3
Q169 0.762 0.601 0.146 !       0.68 eA-3
C170 0.348 0.451 0.429 !       0.65 eA-3
C171 0.928 0.945 0.030 !       0.63 eA-3
Q172 0.706 0.501 0.047 !       0.62 eA-3
C173 0.153 0.078 0.137 !       0.62 eA-3
Q174 0.091 0.969 0.377 !       0.62 eA-3
Q175 0.887 0.250 0.309 !       0.62 eA-3
C176 0.529 0.499 0.344 !       0.61 eA-3
Q177 0.637 0.537 0.079 !       0.59 eA-3
Q178 0.988 0.548 0.249 !       0.59 eA-3
Q179 0.517 0.552 0.145 !       0.58 eA-3
Q180 0.935 0.054 0.107 !       0.58 eA-3
C181 0.700 0.969 0.026 !       0.57 eA-3
C182 0.910 0.499 0.406 !       0.57 eA-3
Q183 0.874 0.462 0.079 !       0.56 eA-3
Q184 0.577 0.884 0.214 !       0.56 eA-3
C185 0.390 0.905 0.069 !       0.53 eA-3
Q186 0.406 0.503 0.187 !       0.52 eA-3
Q187 0.738 0.857 0.080 !       0.52 eA-3
C188 0.347 0.025 0.082 !       0.52 eA-3
Q189 0.845 0.045 0.145 !       0.52 eA-3
Q190 1.000 0.500 0.000 !       0.52 eA-3
Q191 0.880 0.410 0.150 !       0.51 eA-3
Q192 0.815 0.260 0.197 !       0.51 eA-3
Q193 0.699 0.126 0.176 !       0.51 eA-3
C194 0.879 0.998 0.109 !       0.50 eA-3
C195 0.386 0.500 0.375 !       0.50 eA-3
Q196 0.189 0.406 0.154 !       0.50 eA-3
;
_refine_diff_density_max         3.150
_refine_diff_density_min         -3.641
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8198
_refine_ls_number_restraints     612
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0352P)^2^+125.1646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7819
_reflns_number_total             8198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02515e2.cif
_cod_data_source_block           yb-2_sq
_cod_original_formula_sum        'C80 H78 Yb6 O50 S19'
_cod_database_code               7708841
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 S4-C19 = S4-C18
 1.8 with sigma of 0.02
 S5-C20
 1.8 with sigma of 0.02
 C18-C19
 2.7 with sigma of 0.04
 S1-C2 \\sim S1-C2A
 with sigma of 0.02
 O9-C17 \\sim O9A-C17A
 with sigma of 0.02
 O1-C2 \\sim O1A-C2A
 with sigma of 0.04
 S1A-C2 \\sim S1A-C2A
 with sigma of 0.02
 S3A-C14 \\sim S3A-C14A
 with sigma of 0.02
 O3-C15 \\sim O3A-C15A
 with sigma of 0.02
 C3-C1 \\sim C3-C1A
 with sigma of 0.04
 O4-C15 \\sim O4A-C15A
 with sigma of 0.02
 O5-C12 \\sim O5A-C12
 with sigma of 0.02
 O4-C14 \\sim O4A-C14A
 with sigma of 0.04
 O6-C12 \\sim O6A-C12
 with sigma of 0.02
 C13-C15 \\sim C13-C15A
 with sigma of 0.04
 Yb1-O4 \\sim Yb1-O4A
 with sigma of 0.02
 Yb1-O8 \\sim Yb1-O8A
 with sigma of 0.02
 O2-C1 \\sim O2A-C1A
 with sigma of 0.02
 Yb1-C17 \\sim Yb1-C17A
 with sigma of 0.04
 C13-C14 \\sim C13-C14A
 with sigma of 0.02
 S5-O11 \\sim S5-O11A
 with sigma of 0.02
 C13A-C14 \\sim C13A-C14A
 with sigma of 0.02
 O3-C14 \\sim O3A-C14A
 with sigma of 0.04
 C3-C2 \\sim C3-C2A
 with sigma of 0.02
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
 C3A-C2 \\sim C3A-C2A
 with sigma of 0.02
 O2-C2 \\sim O2A-C2A
 with sigma of 0.04
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C13A-C15 \\sim C13A-C15A
 with sigma of 0.04
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
 C3A-C1 \\sim C3A-C1A
 with sigma of 0.04
 Yb1-C15 \\sim Yb1-C15A
 with sigma of 0.04
 O8-C17 \\sim O8A-C17A
 with sigma of 0.02
 Yb2-C1 \\sim Yb2-C1A
 with sigma of 0.04
 S3-C15 \\sim S3-C15A
 with sigma of 0.04
 O8-O9 \\sim O8A-O9A
 with sigma of 0.04
 S4-O10 \\sim S4-O10A
 with sigma of 0.02
 Yb2-O1 \\sim Yb2-O1A
 with sigma of 0.02
 Yb1-O10 \\sim Yb1-O10A
 with sigma of 0.02
 S3-C14 \\sim S3-C14A
 with sigma of 0.02
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 S3A-C15 \\sim S3A-C15A
 with sigma of 0.04
 O1-C1 \\sim O1A-C1A
 with sigma of 0.02
 S1-C1 \\sim S1-C1A
 with sigma of 0.04
 S1A-C1 \\sim S1A-C1A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
S4 \\sim O10 \\sim C18 \\sim C19: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 3.8A
Uanis(S5) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C13A) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9)
\\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O4) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15A)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.001
Uanis(S3) \\sim Ueq, Uanis(C13A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(S5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(S1) \\sim Ueq, Uanis(S4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(S4) \\sim Ueq, Uanis(S1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(O11) = Uanis(O11A)
Uanis(O1) = Uanis(O1A)
Uanis(C1) = Uanis(C1A)
Uanis(S3) = Uanis(C13A)
Uanis(S1) = Uanis(C3A)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(S3A)=Sof(S2A)=Sof(S1A)=Sof(C13A)=Sof(H13A)=Sof(C10A)=Sof(H10A)=Sof(C3A)=
 Sof(H3A)=Sof(O1A)=Sof(O2A)=Sof(C2A)=Sof(C1A)=Sof(O3A)=Sof(O4A)=Sof(C14A)=
 Sof(C15A)=Sof(O5A)=Sof(O6A)=1-FVAR(1)
 Sof(S3)=Sof(S2)=Sof(S1)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O1)=Sof(O2)=
 Sof(C13)=Sof(H13)=Sof(C10)=Sof(H10)=Sof(C3)=Sof(H3)=Sof(C14)=Sof(C15)=Sof(C2)=
 Sof(C1)=FVAR(1)
 Fixed Sof: S4(0.5) S5(0.25) O8(0.5) O9(0.5) O10(0.5) O11(0.25) C17(0.5)
 H17(0.5) C18(0.5) H18A(0.5) H18B(0.5) H18C(0.5) C19(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) O8A(0.5) O9A(0.5) C17A(0.5)
 H17A(0.5) O11A(0.25) O10A(0.5)
5.a Riding coordinates:
 C16(H16)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C13A(H13A), C10(H10), C10A(H10A), C3(H3), C3A(H3A), C17(H17),
 C17A(H17A)
5.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_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 1.933
_oxdiff_exptl_absorpt_empirical_full_min 0.658