Construction of a series of Ln-MOFs Luminescent sensors based a functional “V” shaped ligand
Liu, Xueguang; Liu, Wei; Yang, Xiaoshan; Kou, Yao; Chen, Wan-Min; Liu, Wei-Sheng; Dalton Transactions  (2022) –; doi:10.1039/D2DT01381A

data_7710787
_publ_section_title
;
 Construction of a series of Ln-MOFs Luminescent sensors based a
 functional &#x201C;V&#x201D; shaped ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01381A
_journal_year                    2022
_chemical_formula_moiety         'C23 H19 Eu N2 O11, 2(C3 H7 N O)'
_chemical_formula_sum            'C29 H33 Eu N4 O13'
_chemical_formula_weight         797.55
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-16
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-19 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                91.242(4)
_cell_angle_beta                 90.620(4)
_cell_angle_gamma                91.585(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6558(4)
_cell_length_b                   11.8403(3)
_cell_length_c                   14.3912(9)
_cell_measurement_reflns_used    6020
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.8300
_cell_measurement_theta_min      2.5730
_cell_volume                     1644.19(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -56.00  37.00   1.00    1.50    --   11.90 -57.00  60.00   93
  2  \w    -15.00  79.00   1.00    1.50    --   11.90  77.00 -30.00   94
  3  \w     37.00  64.00   1.00    1.50    --   11.90 178.00  30.00   27
  4  \w    -16.00  85.00   1.00    1.50    --   11.90  57.00-150.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0388265000
_diffrn_orient_matrix_UB_12      -0.0398029000
_diffrn_orient_matrix_UB_13      -0.0279427000
_diffrn_orient_matrix_UB_21      0.0374625000
_diffrn_orient_matrix_UB_22      0.0171738000
_diffrn_orient_matrix_UB_23      -0.0396444000
_diffrn_orient_matrix_UB_31      0.0499001000
_diffrn_orient_matrix_UB_32      -0.0413998000
_diffrn_orient_matrix_UB_33      0.0088503000
_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  0.0430
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11952
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.110
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.161
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         5805
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0562P)^2^+7.3745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5165
_reflns_number_total             5805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01381a2.cif
_cod_data_source_block           eu_2
_cod_database_code               7710787
_shelx_shelxl_version_number     2018/3
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
N3 \\sim C27 \\sim C28 \\sim C29 \\sim N3A \\sim C27A \\sim C29A \\sim C28A:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
3. Rigid body (RIGU) restrains
 O6, N3, C27, C28, C29, N3A, C27A, C29A, C28A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Same fragment restrains
{N3, C27, C28, C29} sigma for 1-2: 0.01, 1-3: 0.02
as in
{N3A, C27A, C29A, C28A}
5. Others
 Sof(N3A)=Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(1)
 Sof(N3)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(1)
6.a Free rotating group:
 O5(H5A,H5B)
6.b Rotating group:
 O3(H3A,H3B), O4(H4A,H4B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C5(H5), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C18(H18), C19(H19), C22(H22), C23(H23), C27(H27), C27A(H27A),
 C24(H24)
6.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C29A(H29D,H29E,H29F), C28A(H28D,
 H28E,H28F), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              15701
_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 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.841