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_7225639
_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 H60 Eu3 N5 O22'
_chemical_formula_sum            'C82 H60 Eu3 N5 O22'
_chemical_formula_weight         1923.23
_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
_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                 99.5310(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0457(10)
_cell_length_b                   24.685(2)
_cell_length_c                   13.3843(11)
_cell_measurement_reflns_used    6873
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.86
_cell_measurement_theta_min      2.26
_cell_volume                     3924.9(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22484
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.450
_diffrn_reflns_theta_min         1.543
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_type   none
_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    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.600
_refine_diff_density_min         -1.990
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.527(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1034
_refine_ls_number_reflns         14659
_refine_ls_number_restraints     98
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+17.6044P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                12212
_reflns_number_total             14659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00885b2.cif
_cod_data_source_block           p1
_cod_depositor_comments
'Adding full bibliography for 7225639--7225643.cif.'
_cod_database_code               7225639
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.473(12) 0.527(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H72 of C72, H75 of C75, H78A of C78, H77 of C77, H73 of
  C73, H82 of C82, H71 of C71, H34 of C34, H11 of C11, H35 of C35, H9 of C9,
  H14 of C14, H17 of C17, H22 of C22, H4 of C4, H12 of C12, H24 of C24, H7 of
  C7, H18 of C18, H23 of C23, H31 of C31, H5 of C5, H33 of C33, H28 of C28, H37
  of C37, H41 of C41, H3 of C3, H16 of C16, H29 of C29, H26 of C26, H54 of C54,
  H60 of C60, H61 of C61, H48 of C48, H52 of C52, H66 of C66, H43 of C43, H68
  of C68, H42 of C42, H62 of C62, H56 of C56, H64 of C64, H47 of C47, H69 of
  C69, H50 of C50, H53 of C53, H45 of C45
 At 1.5 times of:
  All C(H,H,H) groups, H78B of C78, All O(H,H) groups
3. Restrained distances
 N5-C80A = N5-C80B
 1.5 with sigma of 0.02
 C80A-C81A = C80B-C81B
 1.54 with sigma of 0.02
 N5-C81A = N5-C81B
 2.4 with sigma of 0.02
 H78B-H80D
 2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C80A \\sim C80B \\sim C81A \\sim C81B: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
C78 \\sim C79 \\sim C80A \\sim C81B \\sim C80B \\sim N5 \\sim C81A: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C80A) \\sim Ueq, Uanis(C80B) \\sim Ueq, Uanis(C81A) \\sim Ueq,
Uanis(C81B) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
5. Others
 Sof(C80B)=Sof(H80C)=Sof(H80D)=Sof(C81B)=Sof(H81D)=Sof(H81E)=Sof(H81F)=1-FVAR(1)
 Sof(C80A)=Sof(H80A)=Sof(H80B)=Sof(C81A)=Sof(H81A)=Sof(H81B)=Sof(H81C)=FVAR(1)
6.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
6.b Secondary CH2 refined with riding coordinates:
 C78(H78A,H78B), C80A(H80A,H80B), C80B(H80C,H80D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C11(H11), C12(H12), C14(H14),
 C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C26(H26), C28(H28),
  C29(H29), C31(H31), C33(H33), C34(H34), C35(H35), C37(H37), C41(H41),
 C42(H42), C43(H43), C45(H45), C47(H47), C48(H48), C50(H50), C52(H52), C53(H53),
  C54(H54), C56(H56), C60(H60), C61(H61), C62(H62), C64(H64), C66(H66),
 C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C75(H75), C77(H77), C82(H82)
6.d Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C81A(H81A,H81B,H81C), C81B(H81D,H81E,H81F)
;
_olex2_submission_special_instructions 'No special instructions were received'