2D and 3D lanthanide metal‒organic frameworks constructed from three benzenedicarboxylate ligands: synthesis, structure and luminescent properties
You, Li-Xin; Zhao, Bai-Bei; Liu, Hui-Jie; Wang, Shu-Ju; Xiong, Gang; He, Yong-Ke; Ding, Fu; Joos, Jonas J.; Smet, Philippe F.; Sun, Ya-Guang; CrystEngComm 20 (2018) 615–; doi:10.1039/C7CE01773A

data_7229816
_publ_section_title
;
 2D and 3D lanthanide metal--organic frameworks constructed from three
 benzenedicarboxylate ligands: synthesis, structure and luminescent
 properties
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              615
_journal_paper_doi               10.1039/C7CE01773A
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety
'C51 H39 N O29 Tb4, C3 H7 N O, 0.5(O2), 0.5(H2 O)'
_chemical_formula_sum            'C54 H49 N2 O31.5 Tb4'
_chemical_formula_weight         1865.63
_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_block_doi                 10.5517/cc1j7mq3
_audit_creation_date             2017-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2015-06-18 deposited with the CCDC.
2017-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                86.63(3)
_cell_angle_beta                 83.76(3)
_cell_angle_gamma                78.72(3)
_cell_formula_units_Z            2
_cell_length_a                   10.860(2)
_cell_length_b                   14.210(3)
_cell_length_c                   20.130(4)
_cell_measurement_reflns_used    8991
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3026.2(11)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r1 (Rigaku, 2009)
;
_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
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 0.0000
                 XTD: 50.2259
              2theta: 29.8061
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 120.0000
                 XTD: 50.2259
              2theta: 29.8061
scan:
    Number of images: 180
               Slice: -60.0000 - 120.0000
         Image width: 1.0000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 54.0000
                 Phi: 240.0000
                 XTD: 50.2259
              2theta: 29.8061
;
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Mercury375R (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.083955
_diffrn_orient_matrix_UB_12      -0.009393
_diffrn_orient_matrix_UB_13      0.042009
_diffrn_orient_matrix_UB_21      -0.030705
_diffrn_orient_matrix_UB_22      -0.062737
_diffrn_orient_matrix_UB_23      0.016605
_diffrn_orient_matrix_UB_31      0.014872
_diffrn_orient_matrix_UB_32      -0.016890
_diffrn_orient_matrix_UB_33      -0.044640
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1304
_diffrn_reflns_av_unetI/netI     0.1219
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25032
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.150
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.713
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.047
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1798
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.544
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         10586
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0129P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9388
_reflns_number_total             10586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01773a2.cif
_cod_data_source_block           shelxl_CCDC8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7229803--7229819.cif.
;
_cod_original_formula_sum        'C54 H49 N2 O31.50 Tb4'
_cod_database_code               7229816
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H25A,H25B} of O25, {H27A,H27B} of O27, {H26A,H26B} of O26,
   {H28A,H28B} of O28
 At 1.5 times of:
  All C(H,H,H) groups, {H1AA,H1AB} of O1A
2. Restrained distances
 H27B-H27A
 1.39 with sigma of 0.01
 H27B-O27
 0.85 with sigma of 0.01
 O27-H27A
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C44 \\sim O29 \\sim N2 \\sim C45 \\sim C46: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(O1B) \\sim Ueq, Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O1B) = Uanis(O31)
4. Others
 Fixed Sof: O31(0.5) O1A(0.5) H1AA(0.5) H1AB(0.5) O1B(0.5)
5.a Fixed occupancy and ADP/Uiso:
 H27A, H27B
5.b Riding coordinates:
 O25(H25A,H25B), O26(H26A,H26B), O28(H28A,H28B)
5.c Free rotating group:
 O1A(H1AA,H1AB)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C16(H16),
 C19(H19), C20(H20), C21(H21), C23(H23), C27(H27), C28(H28), C29(H29), C32(H32),
  C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C49(H49), C50(H50),
 C51(H51), C53(H53), C44(H44)
5.e Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C)
;
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'