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_7234022
_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 H6 Na O9 Tb'
_chemical_formula_sum            'C8 H6 Na O9 Tb'
_chemical_formula_weight         428.04
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.    2019-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9177(5)
_cell_length_b                   8.8354(6)
_cell_length_c                   14.1274(8)
_cell_measurement_reflns_used    2800
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7360
_cell_measurement_theta_min      3.6780
_cell_volume                     988.30(11)
_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    'ShelXS (Sheldrick, 2008)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -1.00   83.00   1.0000    1.6250
omega____ theta____ kappa____ phi______ frames
    -       15.8569   57.0000   90.0000 84

  2 omega   -3.00   85.00   1.0000    1.6250
omega____ theta____ kappa____ phi______ frames
    -       15.8569   37.0000   30.0000 88

  3 omega  -25.00   55.00   1.0000    1.6250
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -99.0000    0.0000 80

  4 omega  -73.00  -22.00   1.0000    1.6250
omega____ theta____ kappa____ phi______ frames
    -      -16.9507  130.0000   85.0000 51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0652410000
_diffrn_orient_matrix_UB_12      0.0527681000
_diffrn_orient_matrix_UB_13      -0.0097016000
_diffrn_orient_matrix_UB_21      0.0579172000
_diffrn_orient_matrix_UB_22      0.0604912000
_diffrn_orient_matrix_UB_23      0.0061270000
_diffrn_orient_matrix_UB_31      0.0202101000
_diffrn_orient_matrix_UB_32      -0.0029421000
_diffrn_orient_matrix_UB_33      -0.0488679000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6087
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.693
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.246
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37622
_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_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.152
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.13(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2009
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0200P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.704
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.001
_reflns_number_gt                1868
_reflns_number_total             2009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01337g2.cif
_cod_data_source_block           Tb-Na
_cod_depositor_comments
'Adding full bibliography for 7234018--7234025.cif.'
_cod_original_cell_volume        988.30(10)
_cod_database_code               7234022
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O Tb'
_shelx_estimated_absorpt_t_max   0.430
_shelx_estimated_absorpt_t_min   0.169
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.87(2) 0.13(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C8) = Uanis(C7) = Uanis(C5) = Uanis(C6) =
Uanis(C3) = Uanis(C4)
4.a Rotating group:
 O9(H9A,H9B)
4.b Ternary CH refined with riding coordinates:
 C7(H7), C5(H5), C3(H3), C2(H2)
;
_shelx_res_checksum              55690
_olex2_date_sample_data_collection 2010-06-08
_olex2_submission_special_instructions 'No special instructions were received'