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_4347463
_publ_section_title
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 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 H420 Dy20 O176), 1.5(O2)'
_chemical_formula_sum            'C164 H105 Dy5 O47'
_chemical_formula_weight         3639.98
_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             2016-03-09
_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                   24.435(2)
_cell_length_b                   27.255(3)
_cell_length_c                   30.407(3)
_cell_measurement_reflns_used    63005
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.5
_cell_volume                     20250(3)
_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, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  multi-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0500
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            158696
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.886
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7180
_platon_squeeze_details
;
;
_refine_diff_density_max         2.530
_refine_diff_density_min         -3.624
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1006
_refine_ls_number_reflns         18144
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1257P)^2^+74.6448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2183
_refine_ls_wR_factor_ref         0.2224
_reflns_number_gt                17051
_reflns_number_total             18144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00190_si_002.cif
_cod_data_source_block           Dy
_cod_database_code               4347463
_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
 C40-C41
 1.5 with sigma of 0.02
 C80-C81
 1.5 with sigma of 0.02
 O15A-C71 \\sim C71-O15B
 with sigma of 0.02
 O5-C1 \\sim C1-O15
 with sigma of 0.02
 O5-Dy1 \\sim Dy1-O15
 with sigma of 0.02
3. Rigid bond restraints
 C80, C81
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O18, Dy3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C79, C80
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(O18) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O0AA) = Uanis(Dy3)
Uanis(O3AA) = Uanis(Dy3)
Uanis(O15A) = Uanis(O15B)
Uanis(O5) = Uanis(O15)
5. Others
 Sof(O15B)=1-FVAR(1)
 Sof(O15A)=FVAR(1)
 Sof(O5)=1-FVAR(2)
 Sof(O15)=FVAR(2)
 Fixed Sof: H1AA(0.5) H1AB(0.5) H68A(0.5) H19A(0.5) H19B(0.5) H53A(0.5)
 H53B(0.5) H53C(0.5) H2AB(0.5) H0AB(0.5) H3AA(0.5) H3AB(0.5) O2(0.5) O3(0.25)
 O11(0.5) O7AA(0.25)
6.a Riding coordinates:
 O1AA(H1AA,H1AB), O68(H68A,H68B), O191(H19A,H19B), O2AA(H2AA,H2AB), O0AA(H0AA,
 H0AB), O3AA(H3AA,H3AB)
6.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C63(H63), C9(H9), C18(H18), C68(H68), C6(H6), C69(H69), C35(H35),
 C72(H72), C13(H13), C79(H79), C52(H52), C44(H44), C32(H32), C43(H43), C3(H3),
 C58(H58), C4(H4), C31(H31), C49(H49), C23(H23), C30(H30), C74(H74), C66(H66),
 C5(H5), C22(H22), C78(H78), C24(H24), C29(H29), C57(H57), C67(H67), C76(H76),
 C16(H16), C46(H46), C51(H51), C39(H39), C17(H17), C38(H38), C25(H25), C59(H59),
  C42(H42), C77(H77), C60(H60), C50(H50), C20(H20)
6.c Idealised Me refined as rotating group:
 C536(H53A,H53B,H53C)
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_olex2_submission_special_instructions 'No special instructions were received'