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_4340296
_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         'C11 H11 N O17 Yb2, 7(H2 O)'
_chemical_formula_sum            'C11 H25 N O24 Yb2'
_chemical_formula_weight         901.40
_chemical_name_systematic
;
 ? 
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_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                85.39(3)
_cell_angle_beta                 89.00(3)
_cell_angle_gamma                77.26(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6697(17)
_cell_length_b                   10.155(2)
_cell_length_c                   13.455(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1151.7(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8446
_diffrn_reflns_theta_full        27.84
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         1.52
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    8.185
_exptl_absorpt_correction_T_max  0.8534
_exptl_absorpt_correction_T_min  0.7354
_exptl_crystal_density_diffrn    2.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.513
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       0.00150(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         5303
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+6.9395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0699
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                4485
_reflns_number_total             5303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402803s_si_003.cif
_cod_data_source_block           r90917h
_cod_depositor_comments
'Adding full bibliography for 4340295--4340296.cif.'
_cod_database_code               4340296
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H16A,H16B} of O16, {H17A,H17B} of O17, {H2A,H14} of O14,
  {H11A,H11B} of O11, {H2B,H2C} of O15, {H18A,H18B} of O24
 At 1.5 times of:
  {H19A,H19B} of O19, {H22A,H22B} of O22, {H23A,H23B} of O23, {H24A,H24B} of O24
2. Restrained distances
 H18B-O18
 0.85 with sigma of 0.02
 H18A-O18
 0.85 with sigma of 0.02
 H18B-H18A
 1.25 with sigma of 0.02
 H22B-O22
 0.85 with sigma of 0.02
 H22A-O22
 0.85 with sigma of 0.02
 H22B-H22A
 1.25 with sigma of 0.02
 H22B-O8
 2.95 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O21') \\sim Ueq, Uanis(O20') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O21') = Uanis(O20)
Uanis(O20') = Uanis(O21)
4. Others
 Fixed Sof: O20(0.5) O20'(0.5) O21(0.5) O21'(0.5)
5.a Riding coordinates:
 O11(H11A,H11B), O14(H2A,H14), O15(H2B,H2C), O16(H16A,H16B), O17(H17A,H17B)
5.b Free rotating group:
 O19(H19A,H19B), H22A(H22B), O23(H23A,H23B,O24,H18A,H18B,H24A,H24B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4)
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