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_7234021
_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 Eu Na O9'
_chemical_formula_sum            'C8 H6 Eu Na O9'
_chemical_formula_weight         421.08
_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                   7.9349(4)
_cell_length_b                   8.8716(4)
_cell_length_c                   14.1611(7)
_cell_measurement_reflns_used    3559
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6800
_cell_measurement_theta_min      3.4310
_cell_volume                     996.87(8)
_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  -11.00   83.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.7007   77.0000  -30.0000 94

  2 omega  -52.00   32.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.7007  -57.0000  150.0000 84

  3 omega   35.00   88.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.7007  178.0000  120.0000 53

  4 omega   -1.00   83.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -       15.7007   57.0000 -150.0000 84

  5 omega  -36.00   52.00   1.0000    3.3700
omega____ theta____ kappa____ phi______ frames
    -      -16.8725   37.0000  -60.0000 88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0249253000
_diffrn_orient_matrix_UB_12      0.0259436000
_diffrn_orient_matrix_UB_13      -0.0452590000
_diffrn_orient_matrix_UB_21      -0.0136964000
_diffrn_orient_matrix_UB_22      -0.0730606000
_diffrn_orient_matrix_UB_23      -0.0188178000
_diffrn_orient_matrix_UB_31      -0.0847787000
_diffrn_orient_matrix_UB_32      0.0194679000
_diffrn_orient_matrix_UB_33      -0.0102705000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8197
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         2.943
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85544
_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    2.806
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.16(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0119P)^2^+0.4017P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0432
_refine_ls_wR_factor_ref         0.0452
_reflns_Friedel_coverage         0.703
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1865
_reflns_number_total             2028
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01337g2.cif
_cod_data_source_block           Eu-Na
_cod_depositor_comments
'Adding full bibliography for 7234018--7234025.cif.'
_cod_original_cell_volume        996.86(9)
_cod_database_code               7234021
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'C H O Eu'
_shelx_estimated_absorpt_t_max   0.428
_shelx_estimated_absorpt_t_min   0.288
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.84(2) 0.16(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(C6) = Uanis(O5) = Uanis(O6)
4.a Riding coordinates:
 O9(H9A,H9B)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C7(H7), C5(H5), C3(H3)
;
_shelx_res_checksum              17556
_olex2_submission_special_instructions 'No special instructions were received'