Lanthanide-based near-infrared emitting metal-organic frameworks with tunable excitation wavelengths and high quantum yields.
Nguyen, Tu N.; Capano, Gloria; Gładysiak, Andrzej; Ebrahim, Fatmah Mish; Eliseeva, Svetlana V.; Chidambaram, Arunraj; Valizadeh, Bardiya; Petoud, Stéphane; Smit, Berend; Stylianou, Kyriakos C.; Chemical communications (Cambridge, England) 54 (2018) 6816–6819; doi:10.1039/c8cc01294f

data_7121445
_publ_section_title
;
 Lanthanide-based near-infrared emitting metal-organic frameworks with
 tunable excitation wavelengths and high quantum yields.
;
_journal_issue                   50
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6816
_journal_page_last               6819
_journal_paper_doi               10.1039/c8cc01294f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C39 H24 N3 O6 Yb, 2(C3 H7 N O), H2 O'
_chemical_formula_sum            'C45 H40 N5 O9 Yb'
_chemical_formula_weight         967.86
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-12 deposited with the CCDC.
2018-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.16010(10)
_cell_length_b                   17.58130(10)
_cell_length_c                   22.5318(3)
_cell_measurement_reflns_used    7893
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.6560
_cell_measurement_theta_min      1.4930
_cell_volume                     4001.17(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.759
_diffrn_measured_fraction_theta_max 0.759
_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      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0107678000
_diffrn_orient_matrix_UB_12      0.0233246000
_diffrn_orient_matrix_UB_13      -0.0264515000
_diffrn_orient_matrix_UB_21      0.0563660000
_diffrn_orient_matrix_UB_22      0.0231174000
_diffrn_orient_matrix_UB_23      0.0107040000
_diffrn_orient_matrix_UB_31      0.0426022000
_diffrn_orient_matrix_UB_32      -0.0246447000
_diffrn_orient_matrix_UB_33      -0.0149596000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72179
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.759
_diffrn_reflns_Laue_measured_fraction_max 0.759
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14648
_diffrn_reflns_point_group_measured_fraction_full 0.759
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        25.643
_diffrn_reflns_theta_max         25.643
_diffrn_reflns_theta_min         1.495
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    2.487
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_description       block
_exptl_crystal_F_000             1948
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.885
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         5477
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+13.3300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5303
_reflns_number_total             5477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01294f2.cif
_cod_data_source_block           SION-100-NH2
_cod_depositor_comments
'Adding full bibliography for 7121444--7121445.cif.'
_cod_database_code               7121445
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.807
_reflns_odcompleteness_completeness 75.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.64
_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
 H3A-N3
 0.86 with sigma of 0.02
 N3-H3B
 0.86 with sigma of 0.02
 H3A-N3 \\sim N3-H3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(O1D) = Uiso(O1B) = Uiso(O1C)
Uiso(C1D) = Uiso(C1B) = Uiso(C1C)
Uiso(N1C) = Uiso(N1D) = Uiso(N1B)
Uiso(C2B) = Uiso(C3B) = Uiso(C2D) = Uiso(C3D) = Uiso(C2C) = Uiso(C3C)
4. Others
 1*[Sof(O1B)+Sof(C1B)+Sof(H1B)+Sof(C2B)+Sof(H2BA)+Sof(H2BB)+Sof(H2BC)+Sof(C3B)+
 Sof(H3BA)+Sof(H3BB)+Sof(H3BC)+Sof(N1B)]+1*[Sof(O1C)+Sof(C1C)+Sof(H1C)+Sof(C2C)+
 Sof(H2CA)+Sof(H2CB)+Sof(H2CC)+Sof(C3C)+Sof(H3CA)+Sof(H3CB)+Sof(H3CC)+Sof(N1C)]+
 1*[Sof(O1D)+Sof(C1D)+Sof(H1D)+Sof(C2D)+Sof(H2DA)+Sof(H2DB)+Sof(H2DC)+Sof(C3D)+
 Sof(H3DA)+Sof(H3DB)+Sof(H3DC)+Sof(N1D)]=1 with esd of 0.001
 Sof(O1B)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=
 Sof(H3BA)=Sof(H3BB)=Sof(H3BC)=Sof(N1B)=FVAR(1)
 Sof(O1C)=Sof(C1C)=Sof(H1C)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=Sof(H2CC)=Sof(C3C)=
 Sof(H3CA)=Sof(H3CB)=Sof(H3CC)=Sof(N1C)=FVAR(2)
 Sof(O1D)=Sof(C1D)=Sof(H1D)=Sof(C2D)=Sof(H2DA)=Sof(H2DB)=Sof(H2DC)=Sof(C3D)=
 Sof(H3DA)=Sof(H3DB)=Sof(H3DC)=Sof(N1D)=FVAR(3)
5.a Free rotating group:
 O1B(C1B,C2B,C3B,N1B), O1C(C1C,C2C,C3C,N1C), O1D(C1D,C2D,C3D,N1D), O1W(H1WA,
 H1WB)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15),
 C16(H16), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28),
  C29(H29), C30(H30), C32(H32), C35(H35), C36(H36), C37(H37), C1A(H1A),
 C1B(H1B), C1C(H1C), C1D(H1D)
5.c Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C2B(H2BA,H2BB,H2BC), C3B(H3BA,H3BB,
 H3BC), C2C(H2CA,H2CB,H2CC), C3C(H3CA,H3CB,H3CC), C2D(H2DA,H2DB,H2DC), C3D(H3DA,
 H3DB,H3DC)
;
_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 1.244
_oxdiff_exptl_absorpt_empirical_full_min 0.862