2D lanthanide MOFs driven by a rigid 3,5-bis(3-carboxy-phenyl)pyridine building block: solvothermal syntheses, structural features, and photoluminescence and sensing properties
Yang, Li-Zi; Wang, Jun; Kirillov, Alexander M.; Dou, Wei; Xu, Cong; Fang, Ran; Xu, Cai-Ling; Liu, Wei-Sheng; CrystEngComm 18 (2016) 6425–; doi:10.1039/C6CE00885B

data_7225640
_publ_section_title
;
 2D lanthanide MOFs driven by a rigid 3,5-bis(3-carboxy-phenyl)pyridine
 building block: solvothermal syntheses, structural features, and
 photoluminescence and sensing properties
;
_journal_issue                   34
_journal_name_full               CrystEngComm
_journal_page_first              6425
_journal_paper_doi               10.1039/C6CE00885B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C82 H59 N5 O22 Tb3, C5 H11 N O'
_chemical_formula_sum            'C87 H70 N6 O23 Tb3'
_chemical_formula_weight         2044.25
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-28 deposited with the CCDC.
2016-06-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.442(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0080(3)
_cell_length_b                   24.6141(6)
_cell_length_c                   13.3586(3)
_cell_measurement_reflns_used    9306
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      28.7140
_cell_measurement_theta_min      3.5210
_cell_volume                     3894.86(16)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details
;
  1 omega    7.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291   57.0000  -60.0000 82

  2 omega    2.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -38.0000  -90.0000 44

  3 omega   26.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -99.0000 -180.0000 34

  4 omega  -52.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -38.0000 -180.0000 89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0436757000
_diffrn_orient_matrix_UB_12      -0.0020593000
_diffrn_orient_matrix_UB_13      -0.0426096000
_diffrn_orient_matrix_UB_21      -0.0409861000
_diffrn_orient_matrix_UB_22      0.0012878000
_diffrn_orient_matrix_UB_23      0.0325777000
_diffrn_orient_matrix_UB_31      -0.0013331000
_diffrn_orient_matrix_UB_32      0.0286976000
_diffrn_orient_matrix_UB_33      -0.0046542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19578
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.718
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.753
_diffrn_reflns_theta_min         3.262
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.778
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98731
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       block
_exptl_crystal_F_000             2026
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.992
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Flack x determined using 4761 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.468(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         14507
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0336P)^2^+5.9441P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.584
_reflns_Friedel_fraction_full    0.672
_reflns_Friedel_fraction_max     0.541
_reflns_number_gt                13605
_reflns_number_total             14507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00885b2.cif
_cod_data_source_block           yanglz_0301
_cod_depositor_comments
'Adding full bibliography for 7225639--7225643.cif.'
_cod_original_cell_volume        3894.86(15)
_cod_database_code               7225640
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C78) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C80(H80A,H80B), C86(H86A,H86B), C84(H84A,H84B), C78(H78A,H78B)
3.c Aromatic/amide H refined with riding coordinates:
 C69(H69), C45(H45), C47(H47), C50(H50), C66(H66), C26(H26), C68(H68),
 C14(H14), C31(H31), C7(H7), C29(H29), C16(H16), C64(H64), C22(H22), C62(H62),
 C41(H41), C11(H11), C23(H23), C18(H18), C60(H60), C61(H61), C12(H12), C48(H48),
  C9(H9), C43(H43), C3(H3), C24(H24), C28(H28), C17(H17), C5(H5), C42(H42),
 C4(H4), C77(H77), C83(H83), C75(H75), C73(H73), C71(H71), C72(H72), C37(H37),
 C33(H33), C35(H35), C34(H34), C56(H56), C53(H53), C54(H54), C52(H52)
3.d Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C87(H87A,H87B,H87C), C85(H85A,H85B,H85C), C81(H81A,H81B,
 H81C)
;
_olex2_submission_special_instructions 'No special instructions were received'