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_7708843
_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 Lu6 O42 S15, 4(C2 H6 O S), 4(H2O)'
_chemical_formula_sum            'C80 H78 Lu6 O50 S19'
_chemical_formula_weight         3498.41
_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   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
;
2021-10-26 deposited with the CCDC.	2021-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.237(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9505(4)
_cell_length_b                   28.1937(6)
_cell_length_c                   17.1041(6)
_cell_measurement_reflns_used    13111
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.5730
_cell_measurement_theta_min      3.8140
_cell_volume                     6521.4(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.831
_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    -39.00  16.00   0.50    5.00    --   -1.10 -77.00-180.00  110
  2  \w      8.00  74.00   0.50    5.00    --    1.10  38.00  30.00  132
  3  \w    -67.00 -16.00   0.50    5.00    --    1.10 -57.00 -90.00  102
;
_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      -0.0073954762
_diffrn_orient_matrix_UB_12      -0.0119657467
_diffrn_orient_matrix_UB_13      0.0372613405
_diffrn_orient_matrix_UB_21      0.0195552555
_diffrn_orient_matrix_UB_22      0.0190504314
_diffrn_orient_matrix_UB_23      0.0335036483
_diffrn_orient_matrix_UB_31      -0.0408150782
_diffrn_orient_matrix_UB_32      0.0112432030
_diffrn_orient_matrix_UB_33      -0.0171073245
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21707
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.446
_diffrn_reflns_theta_min         3.483
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89701
_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    1.781
_exptl_crystal_description       prism
_exptl_crystal_F_000             2940
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
TITL lu_a.res in I2/m
CELL   14.9505   28.1937   17.1041     90.00    115.24     90.00
SPGR I2/m
C101 0.500 0.125-0.002 !       5.45 eA-3
C102 0.481 0.841 0.062 !       2.91 eA-3
C103 0.189 0.999 0.234 !       2.60 eA-3
C104 0.468 0.044 0.138 !       2.59 eA-3
Q105 0.237 0.978 0.468 !       2.42 eA-3
C106 1.000 0.141 0.000 !       2.39 eA-3
C107 0.513 0.177 0.044 !       2.14 eA-3
Q108 0.814 0.892 0.215 !       2.01 eA-3
Q109 0.684 0.501 0.156 !       1.79 eA-3
C110 0.436 0.905 0.001 !       1.78 eA-3
Q111 0.338 0.500 0.063 !       1.76 eA-3
Q112 0.950 0.500 0.094 !       1.70 eA-3
Q113 0.427 0.497 0.094 !       1.70 eA-3
C114 0.391 0.997 0.156 !       1.67 eA-3
C115 0.451 0.993 0.125 !       1.57 eA-3
Q116 0.829 0.898 0.156 !       1.54 eA-3
Q117 0.739 0.498 0.219 !       1.53 eA-3
C118 0.046 0.103 0.057 !       1.53 eA-3
C119 0.563 0.998 0.156 !       1.52 eA-3
Q120 0.613 0.856 0.095 !       1.38 eA-3
Q121 0.743 0.338 0.144 !       1.37 eA-3
C122 0.143 0.031 0.177 !       1.29 eA-3
C123 0.982 0.088 0.021 !       1.28 eA-3
Q124 0.550 0.156 0.105 !       1.19 eA-3
Q125 0.354 0.514 0.025 !       1.15 eA-3
C126 0.111 0.920 0.083 !       1.15 eA-3
C127 0.611 0.576 0.574 !       1.15 eA-3
C128 0.863 0.930 0.930 !       1.15 eA-3
Q129 0.170 0.948 0.485 !       1.09 eA-3
C130 0.091 0.037 0.214 !       1.06 eA-3
C131 0.079 1.000 0.234 !       1.05 eA-3
Q132 0.972 0.518 0.284 !       1.04 eA-3
Q133 0.749 0.141 0.146 !       1.01 eA-3
C134 0.216 0.496 0.328 !       1.01 eA-3
C135 0.119 0.055 0.112 !       0.91 eA-3
Q136 0.853 0.140 0.108 !       0.88 eA-3
Q137 0.737 0.301 0.124 !       0.87 eA-3
C138 0.337 0.501 0.328 !       0.86 eA-3
Q139 0.749 0.933 0.176 !       0.85 eA-3
C140 0.552 0.498 0.672 !       0.83 eA-3
C141 0.052 0.998 0.172 !       0.83 eA-3
C142 0.939 0.979 0.845 !       0.83 eA-3
Q143 0.408 0.040 0.435 !       0.78 eA-3
Q144 0.752 0.314 0.188 !       0.78 eA-3
C145 0.310 1.005 0.125 !       0.76 eA-3
C146 0.130 0.549 0.472 !       0.76 eA-3
Q147 0.140 0.555 0.046 !       0.74 eA-3
Q148 0.672 0.688 0.090 !       0.72 eA-3
C149 0.346 1.002 0.031 !       0.72 eA-3
C150 0.324 0.031 0.006 !       0.71 eA-3
Q151 0.043 0.945 0.390 !       0.70 eA-3
Q152 0.683 0.321 0.156 !       0.67 eA-3
C153 0.019 0.970 0.164 !       0.67 eA-3
C154 0.479 0.437 0.331 !       0.65 eA-3
Q155 0.879 0.447 0.139 !       0.63 eA-3
Q156 0.924 0.490 0.025 !       0.62 eA-3
Q157 0.999 0.049 0.376 !       0.61 eA-3
Q158 0.389 0.430 0.063 !       0.61 eA-3
C159 0.943 0.936 0.028 !       0.60 eA-3
Q160 0.673 0.068 0.415 !       0.59 eA-3
C161 0.530 0.498 0.359 !       0.58 eA-3
C162 0.567 1.001 0.094 !       0.56 eA-3
Q163 0.395 0.549 0.047 !       0.55 eA-3
Q164 0.705 0.555 0.387 !       0.55 eA-3
C165 0.433 0.018 0.031 !       0.51 eA-3
Q166 0.638 0.657 0.109 !       0.50 eA-3
;
_refine_diff_density_max         2.021
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         8393
_refine_ls_number_restraints     611
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0383P)^2^+28.9253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7728
_reflns_number_total             8393
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02515e2.cif
_cod_data_source_block           lu_sq
_cod_database_code               7708843
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.574
_shelx_estimated_absorpt_t_min   0.514
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 S5-C19 = S5-C18
 1.8 with sigma of 0.02
 S4-C20
 1.8 with sigma of 0.02
 O11-Lu2
 2.15 with sigma of 0.02
 O11A-Lu2
 2.15 with sigma of 0.02
 Lu1-O4 \\sim Lu1-O4A
 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-C2
 with sigma of 0.04
 Lu1-O7 \\sim Lu1-O7A
 with sigma of 0.02
 S1A-C2 \\sim S1A-C2A
 with sigma of 0.02
 O4-C15 \\sim O4A-C15A
 with sigma of 0.02
 C2-C1 \\sim C2A-C1
 with sigma of 0.02
 O1-C1 \\sim O1A-C1A
 with sigma of 0.02
 O7-H17 \\sim O7A-H17
 with sigma of 0.04
 Lu2-O1 \\sim Lu2-O1A
 with sigma of 0.02
 O4-C14 \\sim O4A-C14
 with sigma of 0.04
 O3-C15 \\sim O3A-C15A
 with sigma of 0.02
 O1-C2 \\sim O1A-C2
 with sigma of 0.04
 O8-C17 \\sim O8A-C17A
 with sigma of 0.02
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 C14-C15 \\sim C14-C15A
 with sigma of 0.02
 O8-H17 \\sim O8A-H17
 with sigma of 0.04
 C2-C1 \\sim C2-C1A
 with sigma of 0.02
 S1-C2 \\sim S1-C2A
 with sigma of 0.02
 C17-H17 \\sim C17A-H17
 with sigma of 0.02
 C3-C2 \\sim C3-C2A
 with sigma of 0.02
 Lu1-C15 \\sim Lu1-C15A
 with sigma of 0.04
 C2-C1A \\sim C2A-C1A
 with sigma of 0.02
 Lu1-C17 \\sim Lu1-C17A
 with sigma of 0.04
 O2-C1 \\sim O2A-C1A
 with sigma of 0.02
 Lu2-C1 \\sim Lu2-C1A
 with sigma of 0.04
 O7-C17 \\sim O7A-C17A
 with sigma of 0.02
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 O3-C14 \\sim O3A-C14
 with sigma of 0.04
 O11A-Lu2 \\sim Lu2-O11
 with sigma of 0.001
 Lu1-O9 \\sim Lu1-O9A
 with sigma of 0.02
 S5-O9 \\sim S5-O9A
 with sigma of 0.02
 O5-C12 \\sim O5A-C12
 with sigma of 0.02
 O6-C12 \\sim O6A-C12
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
S5 \\sim O9 \\sim C19 \\sim C18: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 3.8A
S4 \\sim O11 \\sim C20: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3.8A
Uanis(S4) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C13A) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(O7)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O9A) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O4) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(C15A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(S2A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(O11) = Uanis(O11A)
Uanis(O9) = Uanis(O9A)
Uanis(O4) = Uanis(O4A)
Uanis(O6) = Uanis(O6A)
Uanis(O5A) = Uanis(O5)
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(S2A)=Sof(S1A)=Sof(S3A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(C15A)=
 Sof(C2A)=Sof(C1A)=Sof(C3A)=Sof(H3A)=Sof(C13A)=Sof(H13A)=Sof(C10A)=Sof(H10A)=
 Sof(O6A)=Sof(O5A)=1-FVAR(1)
 Sof(S1)=Sof(S2)=Sof(S3)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(H3)=Sof(C10)=Sof(H10)=Sof(C13)=Sof(H13)=Sof(C15)=
 FVAR(1)
 Fixed Sof: S5(0.5) O7(0.5) O7A(0.5) O8(0.5) O8A(0.5) O9(0.5) O9A(0.5)
 C17(0.5) H17(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5) C17A(0.5) H17A(0.5) S4(0.25) O11(0.25) C20(0.5) H20A(0.5)
 H20B(0.5) H20C(0.5) O11A(0.25)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C13(H13), C17(H17), C3A(H3A), C17A(H17A), C13A(H13A),
 C10A(H10A), C16(H16)
5.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), 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 1.208
_oxdiff_exptl_absorpt_empirical_full_min 0.884