Experimental Studies and Mechanism Analysis of High-Sensitivity Luminescent Sensing of Pollutional Small Molecules and Ions in Ln4O4Cluster Based Microporous Metal‒Organic Frameworks
Zhou, Jing-Min; Shi, Wei; Li, Hui-Min; Li, Han; Cheng, Peng; The Journal of Physical Chemistry C 118 (2014) 416–; doi:10.1021/jp4097502

data_1513380
_publ_section_title
;
 Experimental Studies and Mechanism Analysis of High-Sensitivity
 Luminescent Sensing of Pollutional Small Molecules and Ions in
 Ln4O4Cluster Based Microporous Metal--Organic Frameworks
;
_journal_issue                   1
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              416
_journal_paper_doi               10.1021/jp4097502
_journal_volume                  118
_journal_year                    2014
_chemical_formula_moiety         'C43 H34 Gd4 N6 O24, Cl O4, O'
_chemical_formula_sum            'C43 H34 Cl Gd4 N6 O29'
_chemical_formula_weight         1763.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4713)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 128.1880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.5583(8)
_cell_length_b                   19.0573(3)
_cell_length_c                   23.6880(4)
_cell_measurement_reflns_used    16718
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0290
_cell_measurement_theta_min      2.9133
_cell_volume                     12261.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   39.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935 -130.0000   10.0000 40

  2 omega   37.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  178.0000 -120.0000 26

  3 omega   28.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   57.0000  -30.0000 59

  4 omega    8.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935   37.0000   60.0000 73

  5 omega  -35.00   33.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.1935  -77.0000 -150.0000 68
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0040768000
_diffrn_orient_matrix_UB_12      0.0271260000
_diffrn_orient_matrix_UB_13      -0.0177598000
_diffrn_orient_matrix_UB_21      0.0014011000
_diffrn_orient_matrix_UB_22      -0.0250161000
_diffrn_orient_matrix_UB_23      -0.0191343000
_diffrn_orient_matrix_UB_31      -0.0297355000
_diffrn_orient_matrix_UB_32      -0.0049043000
_diffrn_orient_matrix_UB_33      -0.0007276000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27717
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.401
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             6711
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.436
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         10805
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+180.7128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                9607
_reflns_number_total             10805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp4097502_si_002.cif
_cod_data_source_block           2
_cod_database_code               1513380
_reflns_odcompleteness_completeness 99.76
_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 O(H,H) groups
2. Restrained distances
 O26-Cl1
 1.44 with sigma of 0.02
 Cl1-O29
 1.44 with sigma of 0.02
 Cl1-O25
 1.44 with sigma of 0.02
 Cl1-O24
 1.44 with sigma of 0.02
 Cl1-O30
 1.44 with sigma of 0.02
 Cl1-O27
 1.44 with sigma of 0.02
 O29-O30
 2.35 with sigma of 0.02
 O29-O26
 2.35 with sigma of 0.02
 O26-O30
 2.35 with sigma of 0.02
 O25-O27
 2.35 with sigma of 0.02
 O25-O24
 2.35 with sigma of 0.02
 O24-O27
 2.35 with sigma of 0.02
 O27-O26
 2.35 with sigma of 0.02
 O26-O25
 2.35 with sigma of 0.02
 O26-O24
 2.35 with sigma of 0.02
 Cl1-O31
 1.44 with sigma of 0.02
 O31-O29
 2.35 with sigma of 0.02
 O30-O31
 2.35 with sigma of 0.02
 O26-O31
 2.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C18)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O29) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O27) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O24(0.5) O25(0.5) O27(0.5) O29(0.5) O30(0.5) O31(0.5)
5.a Rotating group:
 O19(H19A,H19B), O20(H20A,H20B), O21(H21A,H21B), O22(H22A,H22B), O23(H23A,
 H23B), O49(H49A,H49B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C27(H27), C28(H28), C29(H29), C32(H32),
  C33(H33), C34(H34), C39(H39), C40(H40), C42(H42), C43(H43)
;