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_7121444
_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 H23 N2 O6 Yb, 2(C3 H7 N O)'
_chemical_formula_sum            'C45 H37 N4 O8 Yb'
_chemical_formula_weight         934.82
_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     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                 95.1330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4314(2)
_cell_length_b                   17.63950(10)
_cell_length_c                   21.5389(2)
_cell_measurement_reflns_used    8531
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.6970
_cell_measurement_theta_min      1.5080
_cell_volume                     3947.36(9)
_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_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.592
_diffrn_measured_fraction_theta_max 0.592
_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    0.25    --    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      -0.0154577000
_diffrn_orient_matrix_UB_12      -0.0348161000
_diffrn_orient_matrix_UB_13      -0.0166094000
_diffrn_orient_matrix_UB_21      0.0298648000
_diffrn_orient_matrix_UB_22      -0.0214291000
_diffrn_orient_matrix_UB_23      0.0259359000
_diffrn_orient_matrix_UB_31      -0.0608000000
_diffrn_orient_matrix_UB_32      -0.0016766000
_diffrn_orient_matrix_UB_33      0.0135386000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.72179
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 0.592
_diffrn_reflns_Laue_measured_fraction_max 0.592
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14461
_diffrn_reflns_point_group_measured_fraction_full 0.592
_diffrn_reflns_point_group_measured_fraction_max 0.592
_diffrn_reflns_theta_full        25.723
_diffrn_reflns_theta_max         25.723
_diffrn_reflns_theta_min         1.518
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    2.516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76927
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       prism
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.403
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+7.3006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4124
_reflns_number_total             4266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc01294f2.cif
_cod_data_source_block           SION-100
_cod_depositor_comments
'Adding full bibliography for 7121444--7121445.cif.'
_cod_database_code               7121444
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.660
_reflns_odcompleteness_completeness 58.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.72
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2B-C1B \\sim C1B-O1B
 with sigma of 0.02
 C2B-O1B \\sim O2B-C3B
 with sigma of 0.02
 C3B-O1B \\sim C2B-O2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1B \\sim N1B: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C13) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.02
Uanis(O2B) \\sim Ueq, Uanis(O1B) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.016
Uanis(O2B) = Uanis(O1B)
4. Rigid body (RIGU) restrains
 N2, C39, C38, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C22, C23, C24, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2B, C1B, O1B, N1B, C3B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H1BA)=Sof(O2B)=1-FVAR(1)
 Sof(O1B)=Sof(H1B)=FVAR(1)
6.a Free rotating group:
 O1B(C1B,C2B,C3B,N1B)
6.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), C33(H33), C35(H35), C36(H36), C37(H37),
 C1A(H1A), C1B(H1B), C1B(H1BA)
6.c Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C2B(H2BA,H2BB,H2BC), C3B(H3BA,H3BB,
 H3BC)
;
_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 1.440
_oxdiff_exptl_absorpt_empirical_full_min 0.717