Triple-Interpenetrated Lanthanide-Organic Framework as Dual Wave Bands Self-Calibrated pH Luminescent Probe.
Hou, Sheng-Li; Dong, Jie; Tang, Meng-Hua; Jiang, Xiao-Lei; Jiao, Zhuo-Hao; Zhao, Bin; Analytical chemistry 91 (2019) 5455–5460; doi:10.1021/acs.analchem.9b00848

data_1552493
_publ_section_title
;
 Triple-Interpenetrated Lanthanide-Organic Framework as Dual Wave Bands
 Self-Calibrated pH Luminescent Probe.
;
_journal_issue                   8
_journal_name_full               'Analytical chemistry'
_journal_page_first              5455
_journal_page_last               5460
_journal_paper_doi               10.1021/acs.analchem.9b00848
_journal_volume                  91
_journal_year                    2019
_chemical_formula_moiety         'C28 H26 Eu N4 O9, H2 O'
_chemical_formula_sum            'C28 H28 Eu N4 O10'
_chemical_formula_weight         732.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.581(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2038(2)
_cell_length_b                   22.0069(5)
_cell_length_c                   10.8009(2)
_cell_measurement_reflns_used    7560
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      28.9550
_cell_measurement_theta_min      3.4660
_cell_volume                     2891.51(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w      1.00  89.00   1.00    6.78    --   18.63  37.00  90.00   88
  2  \w    -28.00  73.00   1.00    6.78    --   18.63   0.00-120.00  101
  3  \w    -94.00 -62.00   1.00    6.78    --  -19.56-178.00-150.00   32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0560938000
_diffrn_orient_matrix_UB_12      0.0081474000
_diffrn_orient_matrix_UB_13      0.0119334000
_diffrn_orient_matrix_UB_21      0.0108693000
_diffrn_orient_matrix_UB_22      -0.0106534000
_diffrn_orient_matrix_UB_23      -0.0597645000
_diffrn_orient_matrix_UB_31      -0.0116062000
_diffrn_orient_matrix_UB_32      0.0292836000
_diffrn_orient_matrix_UB_33      -0.0251688000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            10802
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.233
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_refine_diff_density_max         1.301
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         5092
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+10.6330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4614
_reflns_number_total             5092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac9b00848_si_002.cif
_cod_data_source_block           p171006f1
_cod_original_cell_volume        2891.51(11)
_cod_database_code               1552493
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C N O Eu'
_chemical_oxdiff_usercomment     HSL-Eu
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 HA-O0AA
 0.85 with sigma of 0.02
3. Rigid bond restraints
 N2BA, O1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O3, N2BA
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 Eu1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
 Eu1, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(N0AA) \\sim Ueq, Uanis(C5BA) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(Eu1) \\sim Ueq: with sigma of 0.000005 and sigma for terminal atoms of
0.000005
5. Rigid body (RIGU) restrains
 O6, C4BA, N0AA, C5, C5BA
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
6.a Riding coordinates:
 O0AA(H,HA)
6.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C7(H7), C15(H15), C0AA(H0AA), C4(H4), C12(H12), C3AA(H3AA),
 C2AA(H2AA), C5AA(H5AA), C6AA(H6AA), C4AA(H4AA), C10(H10), C7AA(H7AA),
 C4BA(H4BA)
6.c Idealised Me refined as rotating group:
 C8AA(H8AC,H8AB,H8AA), C9AA(H9AC,H9AB,H9AA), C5BA(H5BB,H5BC,H5BA), C5(H5A,H5B,
 H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.651