A microporous anionic metal–organic framework for aqueous encapsulation and highly reversible sensitization of light-emitting Tb3+ ions
Jin, J. C.; Liu, X. Y.; Yang, G. P.; Hou, L.; Wang, Y. Y.; New Journal of Chemistry 46 (2022) 5201–5205; doi:10.1039/D1NJ02418C

data_7061289
_publ_section_title
;
 A microporous anionic metal--organic framework for aqueous encapsulation
 and highly reversible sensitization of light-emitting Tb3+ ions
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5201
_journal_page_last               5205
_journal_paper_doi               10.1039/D1NJ02418C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C57 H33 K N3 O12 Zn2, C2 H8 N'
_chemical_formula_sum            'C59 H41 K N4 O12 Zn2'
_chemical_formula_weight         1167.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-08-31 deposited with the CCDC.	2022-01-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.205(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.347(2)
_cell_length_b                   22.155(4)
_cell_length_c                   25.424(4)
_cell_measurement_reflns_used    4837
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.62
_cell_measurement_theta_min      2.58
_cell_volume                     7421(2)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22681
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.256
_diffrn_reflns_theta_min         1.623
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.752
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6216
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0866 before and 0.0547 after correction.
The Ratio of minimum to maximum transmission is 0.8336.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.900
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         8991
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1592P)^2^+1.9362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.2465
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6130
_reflns_number_total             8991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02418c2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7061289.cif.'
_cod_database_code               7061289
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.829
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C29, N3}
3. Restrained distances
 C30-N2
 1.45 with sigma of 0.02
 N2-C31
 1.45 with sigma of 0.02
 C30-N2 \\sim N2-C31
 with sigma of 0.02
 K1A-O6 \\sim K1A-O2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
N2 \\sim C30: within 3.8A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 3.8A
C31 \\sim N2 \\sim C30: within 3.8A with sigma of 0.001 and sigma for terminal
atoms of 0.001 within 3.8A
Uanis(C29) = Uanis(N3)
5. Others
 Fixed Sof: C29(0.5) H29(0.5) N2(0.5) H2A(0.5) H2B(0.5) C30(0.5) H30A(0.5)
 H30B(0.5) H30C(0.5) N3(0.5) C31(0.5) H31A(0.5) H31B(0.5) H31C(0.5) K1A(0.5)
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C7(H7), C4(H4), C21(H21), C20(H20), C18(H18), C12(H12),
 C10(H10), C14(H14), C25(H25), C24(H24), C23(H23), C22(H22), C28(H28), C29(H29),
  C17(H17)
6.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'