Unique (3,4,10)-Connected Lanthanide-Organic Framework as a Recyclable Chemical Sensor for Detecting Al(3.).
Xu, Hang; Fang, Ming; Cao, Chun-Shuai; Qiao, Wan-Zhen; Zhao, Bin; Inorganic chemistry 55 (2016) 4790–4794; doi:10.1021/acs.inorgchem.6b00190

data_4347464
_publ_section_title
;
 Unique (3,4,10)-Connected Lanthanide-Organic Framework as a Recyclable
 Chemical Sensor for Detecting Al(3.).
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4790
_journal_page_last               4794
_journal_paper_doi               10.1021/acs.inorgchem.6b00190
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'0.25(C656 H427.21 O180 Yb20), H4 O2, 0.5(O2)'
_chemical_formula_sum            'C164 H110.8 O48 Yb5'
_chemical_formula_weight         3714.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.9063(6)
_cell_length_b                   27.4059(5)
_cell_length_c                   30.3210(4)
_cell_measurement_reflns_used    13841
_cell_measurement_temperature    125(4)
_cell_measurement_theta_max      28.2000
_cell_measurement_theta_min      3.1080
_cell_volume                     19865.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      125(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2116
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     61.00  95.00   1.00   60.00    --   18.94 178.00 -60.00   34
  2  \w    -54.00  60.00   1.00   60.00    --   18.94 -19.00-120.00  114
  3  \w    -32.00  -7.00   1.00   60.00    --  -19.25 -57.00 120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0284475000
_diffrn_orient_matrix_UB_12      -0.0072061000
_diffrn_orient_matrix_UB_13      -0.0014533000
_diffrn_orient_matrix_UB_21      -0.0044241000
_diffrn_orient_matrix_UB_22      -0.0077537000
_diffrn_orient_matrix_UB_23      -0.0220337000
_diffrn_orient_matrix_UB_31      0.0072117000
_diffrn_orient_matrix_UB_32      0.0236137000
_diffrn_orient_matrix_UB_33      -0.0077108000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57151
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7315
_platon_squeeze_details
;
;
_refine_diff_density_max         2.343
_refine_diff_density_min         -2.009
_refine_diff_density_rms         0.188
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         17780
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1219P)^2^+145.2434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2001
_refine_ls_wR_factor_ref         0.2265
_reflns_number_gt                13003
_reflns_number_total             17780
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00190_si_002.cif
_cod_data_source_block           Yb
_cod_original_cell_volume        19865.6(6)
_cod_original_formula_sum        'C164 H110.80 O48 Yb5'
_cod_database_code               4347464
_chemical_oxdiff_formula         'C Yb'
_chemical_oxdiff_usercomment     XH-YB3S
_reflns_odcompleteness_completeness 99.73
_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, All O(H,H,H,H) groups
2. Restrained distances
 Yb2B-Yb2A
 0.4 with sigma of 0.02
 C105-C62
 1.45 with sigma of 0.02
 O46-Yb3B
 2.4 with sigma of 0.02
 O32-Yb3B
 2.1 with sigma of 0.02
 Yb3B-O36
 1.33 with sigma of 0.02
 O19-Yb3B
 3.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C42 \\sim C65 \\sim C12 \\sim C13 \\sim C14 \\sim C0AA: within 3.8A with sigma
of 0.005 and sigma for terminal atoms of 0.005
C73 \\sim C76 \\sim C82 \\sim C168 \\sim C1AA \\sim C2AA: within 3.8A with
sigma of 0.005 and sigma for terminal atoms of 0.005
O32 \\sim O169 \\sim C176: within 3.8A with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C105) \\sim Ueq, Uanis(C62) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(O91) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O86) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(Yb3B) = Uanis(Yb3A)
Uanis(Yb2A) = Uanis(Yb2B)
Uanis(O0AA) = Uanis(O1AA)
4. Others
 Sof(H19C)=Sof(H19D)=Sof(Yb3B)=0.5*(1-FVAR(2))
 Sof(Yb3A)=Sof(H19A)=Sof(H19B)=Sof(H36A)=Sof(H36B)=0.5*FVAR(2)
 Sof(H57C)=Sof(H57D)=Sof(H86C)=Sof(H86D)=Sof(Yb2B)=0.5*(1-FVAR(3))
 Sof(Yb2A)=Sof(H57A)=Sof(H57B)=Sof(H86A)=Sof(H86B)=0.5*FVAR(3)
 Fixed Sof: H5A(0.5) H5B(0.5) H5C(0.5) H10A(0.5) H10B(0.5) O147(0.5) H14A(0.5)
 H14B(0.5) O160(0.5) H16A(0.5) H16B(0.5) H2A(0.5) H2B(0.5) O1AA(0.25)
 O0AA(0.25) O1(0.5) H1A(0.5) H1B(0.5)
5.a Riding coordinates:
 O10(H10A,H10B), O19(H19A,H19B), O19(H19C,H19D), O36(H36A,H36B), O57(H57A,
 H57B), O57(H57C,H57D), O86(H86A,H86B), O86(H86C,H86D), O147(H14A,H14B),
 O160(H16A,H16B), O2(H2A,H2B), O1(H1A,H1B)
5.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C56(H56),
 C61(H61), C66(H66), C67(H67), C70(H70), C77(H77), C78(H78), C82(H82), C90(H90),
  C92(H92), C93(H93), C99(H99), C107(H107), C110(H110), C127(H127), C129(H129),
 C131(H131), C133(H133), C134(H134), C148(H148), C159(H159), C161(H161),
 C163(H163), C165(H165), C166(H166), C168(H168), C12(H12), C13(H13), C14(H14),
 C0AA(H0AA), C2(H2), C3(H3), C4(H4), C9(H9), C11(H11), C18(H18), C19(H19),
 C1AA(H1AA), C2AA(H2AA)
5.c Idealised Me refined as rotating group:
 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 1.421
_oxdiff_exptl_absorpt_empirical_full_min 0.797