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_7225642
_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 Dy3 N5 O22, C5 H11 N O'
_chemical_formula_sum            'C87 H70 Dy3 N6 O23'
_chemical_formula_weight         2054.99
_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             2016-03-21
_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                 99.538(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9691(3)
_cell_length_b                   24.5557(7)
_cell_length_c                   13.3369(4)
_cell_measurement_reflns_used    11358
_cell_measurement_temperature    294.06(10)
_cell_measurement_theta_max      28.6790
_cell_measurement_theta_min      3.5220
_cell_volume                     3865.66(19)
_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      air
_diffrn_ambient_temperature      294.06(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -33.00   38.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -38.0000   60.0000 71

  2 omega  -51.00   58.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291    0.0000  120.0000 109

  3 omega   40.00   79.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  178.0000   30.0000 39

  4 omega  -10.00   20.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000 -150.0000 30
;
_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      0.0529039000
_diffrn_orient_matrix_UB_12      0.0093352000
_diffrn_orient_matrix_UB_13      0.0263173000
_diffrn_orient_matrix_UB_21      -0.0284633000
_diffrn_orient_matrix_UB_22      0.0165405000
_diffrn_orient_matrix_UB_23      0.0313595000
_diffrn_orient_matrix_UB_31      0.0009568000
_diffrn_orient_matrix_UB_32      -0.0217588000
_diffrn_orient_matrix_UB_33      0.0351139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17555
_diffrn_reflns_point_group_measured_fraction_full 0.877
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_min         3.283
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.955
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98231
_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    1.765
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.947
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 5023 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.119(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         13208
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0259P)^2^+1.4239P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0678
_reflns_Friedel_coverage         0.694
_reflns_Friedel_fraction_full    0.751
_reflns_Friedel_fraction_max     0.728
_reflns_number_gt                12679
_reflns_number_total             13208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00885b2.cif
_cod_data_source_block           yanglz_1202_1
_cod_depositor_comments
'Adding full bibliography for 7225639--7225643.cif.'
_cod_original_cell_volume        3865.66(18)
_cod_database_code               7225642
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.74
_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(N3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C81) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O23) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C83)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C84) \\sim Ueq:
with sigma of 0.008 and sigma for terminal atoms of 0.016
3.a Rotating group:
 O20(H20A,H20B), O21(H21A,H21B)
3.b Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C79(H79A,H79B), C86(H86A,H86B), C84(H84A,H84B)
3.c Aromatic/amide H refined with riding coordinates:
 C69(H69), C66(H66), C22(H22), C26(H26), C42(H42), C45(H45), C43(H43),
 C50(H50), C68(H68), C47(H47), C23(H23), C9(H9), C5(H5), C16(H16), C78(H78),
 C14(H14), C24(H24), C7(H7), C11(H11), C41(H41), C12(H12), C30(H30), C49(H49),
 C28(H28), C18(H18), C17(H17), C31(H31), C4(H4), C3(H3), C52(H52), C54(H54),
 C55(H55), C56(H56), C71(H71), C74(H74), C73(H73), C75(H75), C64(H64), C61(H61),
  C60(H60), C62(H62), C37(H37), C33(H33), C35(H35), C34(H34), C83(H83)
3.d Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C85(H85A,H85B,H85C), C87(H87A,H87B,
 H87C)
;
_olex2_submission_special_instructions 'No special instructions were received'