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_7225643
_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 Gd3 N5 O22, C5 H11 N O'
_chemical_formula_sum            'C87 H70 Gd3 N6 O23'
_chemical_formula_weight         2039.24
_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             2016-03-21
_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                 99.519(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0505(12)
_cell_length_b                   24.708(3)
_cell_length_c                   13.4026(13)
_cell_measurement_reflns_used    4043
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.88
_cell_measurement_theta_min      2.26
_cell_volume                     3935.6(7)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.999
_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  0.0457
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20105
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.100
_diffrn_reflns_theta_min         1.541
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.582
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6589
_exptl_absorpt_correction_type   multi-scan
_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    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.588
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1087
_refine_ls_number_reflns         12515
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0213P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.984
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                10360
_reflns_number_total             12515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00885b2.cif
_cod_data_source_block           p21
_cod_depositor_comments
'Adding full bibliography for 7225639--7225643.cif.'
_cod_database_code               7225643
_shelxl_version_number           2013-2
_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 C(H,H,H,H)
  groups, All O(H,H) groups
2. Restrained distances
 C78A-C79
 1.54 with sigma of 0.02
 N6-C83
 1.35 with sigma of 0.01
 C83-O1BA
 1.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C87) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C85) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N5B) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C78A) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N5B) \\sim Ueq, Uanis(N5A) \\sim Ueq, Uanis(C80) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O1BA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C83) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.1
4. Others
 Fixed Sof: H77(0.45) H83(0.55) H78A(0.35) H78B(0.35) H10A(0.65) H10B(0.65)
 N5B(0.35) H80A(0.45) H80B(0.45) H4AA(0.55) H4AB(0.55) N5A(0.65)
5.a Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C78A(H78A,H78B), C78A(H10A,H10B), C80(H80A,H80B), C80(H4AA,H4AB), C86(H86A,
 H86B), C84(H84A,H84B)
5.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C52(H52), C56(H56), C54(H54), C71(H71), C73(H73), C72(H72),
 C75(H75), C60(H60), C5(H5), C3(H3), C4(H4), C7(H7), C67(H67), C69(H69),
 C37(H37), C50(H50), C66(H66), C64(H64), C14(H14), C26(H26), C9(H9), C48(H48),
 C35(H35), C47(H47), C31(H31), C33(H33), C34(H34), C29(H29), C45(H45), C28(H28),
  C62(H62), C16(H16), C41(H41), C17(H17), C24(H24), C12(H12), C22(H22),
 C18(H18), C43(H43), C61(H61), C23(H23), C42(H42), C77(H77), C77(H83), C11(H11),
  C83(H8AA)
5.d Idealised Me refined as rotating group:
 C79(H79A,H79B,H79C), C81(H81A,H81B,H81C), C87(H87A,H87B,H87C), C85(H85A,H85B,
 H85C)
;
_olex2_submission_special_instructions 'No special instructions were received'