Hollow terbium metal–organic-framework spheres: preparation and their performance in Fe3+ detection
Yang, Xiaozhan; Liang, Yicun; Feng, Wenlin; Yang, Chaolong; Wang, Lian; Huang, Guojia; Wang, Daoyuan; RSC Advances 12 (2022) 4153–4161; doi:10.1039/D1RA08088A

data_7244326
_publ_section_title
;
 Hollow terbium metal--organic-framework spheres: preparation and their
 performance in Fe3+ detection
;
_journal_issue                   7
_journal_name_full               'RSC Advances'
_journal_page_first              4153
_journal_page_last               4161
_journal_paper_doi               10.1039/D1RA08088A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C15 H17 N2 O8 Tb'
_chemical_formula_sum            'C15 H17 N2 O8 Tb'
_chemical_formula_weight         512.22
_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   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc27x028
_audit_creation_date             2020-10-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-05-08 deposited with the CCDC.	2022-01-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.5040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6318(8)
_cell_length_b                   11.4451(5)
_cell_length_c                   19.7386(8)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      54.948
_cell_measurement_theta_min      3.991
_cell_volume                     4035.7(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker D8 venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15934
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.948
_diffrn_reflns_theta_min         3.991
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.804
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1526 before and 0.0796 after correction.
The Ratio of minimum to maximum transmission is 0.5270.
The \l/2 correction factor is Not present.
;
_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    1.686
_exptl_crystal_description       needle
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.504
_refine_diff_density_min         -2.022
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3746
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0606P)^2^+26.3961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3415
_reflns_number_total             3746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra08088a2.cif
_cod_data_source_block           aaad_sq
_cod_database_code               7244326
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.315
_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
2. Uiso/Uaniso restraints and constraints
C3 \\sim N2 \\sim C00Q \\sim C00N \\sim O007: within 1.7A with sigma of 0.004
and sigma for terminal atoms of 0.008 within 1.7A
3.a Riding coordinates:
 C3(H3A,H3B,H3C)
3.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00E(H00E), C00H(H00H), C00M(H00M), C00N(H00N)
3.c Idealised Me refined as rotating group:
 C00O(H00A,H00B,H00D), C00P(H00F,H00G,H00I), C00Q(H00J,H00K,H00L)
;
_shelx_res_checksum              27761
_shelx_fab_checksum              5578
_olex2_submission_special_instructions 'No special instructions were received'