Two Three-Dimensional Lanthanide Frameworks Exhibiting Luminescence Increases upon Dehydration and Novel Water Layer Involving in Situ Decarboxylation.
Yang, Ai-Hong; Zou, Ji-Yong; Wang, Wen-Min; Shi, Xue-Ying; Gao, Hong-Ling; Cui, Jian-Zhong; Zhao, Bin; Inorganic chemistry 53 (2014) 7092–7100; doi:10.1021/ic402803s

data_4340295
_publ_section_title
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 Two Three-Dimensional Lanthanide Frameworks Exhibiting Luminescence
 Increases upon Dehydration and Novel Water Layer Involving in Situ
 Decarboxylation.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7092
_journal_page_last               7100
_journal_paper_doi               10.1021/ic402803s
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C25 H18 N3 O26 Tb3, 2(H2 O)'
_chemical_formula_sum            'C25 H22 N3 O28 Tb3'
_chemical_formula_weight         1289.22
_chemical_name_systematic
;
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-17
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.90(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.780(6)
_cell_length_b                   6.6928(13)
_cell_length_c                   17.125(3)
_cell_measurement_temperature    113(2)
_cell_volume                     3179.9(11)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16951
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.20
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.726
_exptl_absorpt_correction_T_max  0.8772
_exptl_absorpt_correction_T_min  0.7747
_exptl_crystal_density_diffrn    2.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.310
_refine_diff_density_min         -2.068
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         5372
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0437P)^2^+43.7351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                4638
_reflns_number_total             5372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402803s_si_002.cif
_cod_data_source_block           r90918e1
_cod_depositor_comments
'Adding full bibliography for 4340295--4340296.cif.'
_cod_original_cell_volume        3179.8(11)
_cod_database_code               4340295
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H25A,H25B} of O25, {H22A,H22B} of O22, {H21A,H21B} of O21,
   {H24A,H24B} of O24, {H26A,H26B} of O26, All O(H) groups
 At 1.5 times of:
  {H28A,H28B} of O28, {H23A,H23B} of O23
2. Restrained distances
 H27A-O27
 0.85 with sigma of 0.02
 H27B-O27
 0.85 with sigma of 0.02
 H27A-H27B
 1.25 with sigma of 0.02
 H22A-H27B
 2.11 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O27) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O21(H21A,H21B), O22(H22A,H22B), O24(H24A,H24B), O25(H25A,H25B), O26(H26A,
 H26B), O28(H28A,H28B)
4.b Rotating group:
 O23(H23A,H23B)
4.c Aromatic/amide H refined with riding coordinates:
 O3(H3), C3(H3A), C12(H12), C14(H14), C15(H15), C20(H20)
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