Series of 3D lanthanide MOFs derived from saddle-like alicyclic tetracarboxylate ligands: synthesis, characterization and structure‒photoluminescence correlations
Wang, Jia-Yin; Shi, Yang; Tao, Dong-Liang; Bo, Qi-Bing; CrystEngComm 21 (2019) 6591–; doi:10.1039/C9CE01337G

data_7234023
_publ_section_title
;
 Series of 3D lanthanide MOFs derived from saddle-like alicyclic
 tetracarboxylate ligands: synthesis, characterization and
 structure--photoluminescence correlations
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6591
_journal_paper_doi               10.1039/C9CE01337G
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C8 H7 O9 Tb'
_chemical_formula_sum            'C8 H7 O9 Tb'
_chemical_formula_weight         406.06
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-09-26
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2019-08-19 deposited with the CCDC.    2019-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.832(3)
_cell_angle_beta                 86.055(3)
_cell_angle_gamma                82.820(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0860(3)
_cell_length_b                   7.9756(3)
_cell_length_c                   9.2021(3)
_cell_measurement_reflns_used    6488
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9040
_cell_measurement_theta_min      3.7850
_cell_volume                     477.71(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -52.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -77.0000 -150.0000 95

  2 omega  -52.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -77.0000   90.0000 95

  3 omega  -11.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569   77.0000  -30.0000 94

  4 omega  -25.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -99.0000    0.0000 47

  5 omega  -25.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  -99.0000   90.0000 47

  6 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569   57.0000 -150.0000 84

  7 omega  -53.00   35.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -37.0000 -120.0000 88

  8 omega   35.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000   60.0000 53

  9 omega   14.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -99.0000    0.0000 41

 10 omega   35.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007   77.0000   60.0000 38

 11 omega    5.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007   57.0000 -180.0000 27

 12 omega   49.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007   57.0000 -180.0000 26

 13 omega   40.00   78.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007   57.0000 -120.0000 38

 14 omega  -70.00  -45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7944  124.0000 -175.5875 25

 15 omega  -74.00  -43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7944  131.0000   36.8766 31

 16 omega   -1.00   34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007   57.0000 -120.0000 35

 17 omega  -25.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -99.0000 -150.0000 80

 18 omega  -25.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -99.0000   30.0000 80

 19 omega  -74.00  -22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7944  131.0000   36.8766 52

 20 omega  -84.00    0.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7944  -57.0000   60.0000 84

 21 omega  -25.00   22.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.7944  -99.0000 -150.0000 47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0557225000
_diffrn_orient_matrix_UB_12      -0.0832471000
_diffrn_orient_matrix_UB_13      0.0082262000
_diffrn_orient_matrix_UB_21      -0.0840991000
_diffrn_orient_matrix_UB_22      -0.0419496000
_diffrn_orient_matrix_UB_23      0.0052379000
_diffrn_orient_matrix_UB_31      0.0026093000
_diffrn_orient_matrix_UB_32      0.0252910000
_diffrn_orient_matrix_UB_33      -0.0826823000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11396
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.714
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.448
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.823
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.275
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0203
_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^)+(0.0357P)^2^+0.6157P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1880
_reflns_number_total             1938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01337g2.cif
_cod_data_source_block           Tb-Tb
_cod_depositor_comments
'Adding full bibliography for 7234018--7234025.cif.'
_cod_database_code               7234023
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O Tb'
_shelx_estimated_absorpt_t_max   0.382
_shelx_estimated_absorpt_t_min   0.138
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O9(H9A,H9B)
2.b Ternary CH refined with riding coordinates:
 C7(H7), C3(H3), C2(H2), C5(H5)
2.c Idealised tetrahedral OH refined as rotating group:
 O6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'