Synthesis of Tröger Base-Based[3]arenes for Efficient Iodine Adsorption
Niu, Pengbo; Shi, Conghao; Jiao, Jianmin; Xie, Wang; Qiu, Heng; Yang, Zhen; Jiang, Juli; Wang, Leyong; Chemical Communications  (2023) –; doi:10.1039/D3CC02804F

data_7132015
_publ_section_title
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 Synthesis of Tr\"oger Base-Based[3]arenes for Efficient Iodine Adsorption
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02804F
_journal_year                    2023
_chemical_formula_moiety         'C33 H34 N2 O4'
_chemical_formula_sum            'C33 H34 N2 O4'
_chemical_formula_weight         522.62
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-31
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
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2022-12-05 deposited with the CCDC.	2023-08-11 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 108.6850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8793(8)
_cell_length_b                   5.2883(2)
_cell_length_c                   25.9027(10)
_cell_measurement_reflns_used    6549
_cell_measurement_temperature    193.0
_cell_measurement_theta_max      53.98
_cell_measurement_theta_min      3.70
_cell_volume                     2709.33(18)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            14157
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.982
_diffrn_reflns_theta_min         3.134
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1343 before and 0.0667 after correction.
The Ratio of minimum to maximum transmission is 0.8842.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.247
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0551P)^2^+3.7027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2142
_reflns_number_total             2470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02804f2.cif
_cod_data_source_block           npb_16_a
_cod_database_code               7132015
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.911
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H00E)=Sof(H00F)=Sof(C2)=Sof(C1)=Sof(H1)=Sof(C4)=Sof(H4)=Sof(C10)=Sof(C3)=
 Sof(C6)=Sof(H6)=Sof(C5)=Sof(H5A)=Sof(H5B)=1-FVAR(1)
 Sof(H00C)=Sof(H00D)=Sof(C00A)=Sof(C00D)=Sof(C00E)=Sof(C00G)=Sof(H00L)=
 Sof(H00M)=Sof(C00H)=Sof(H00N)=Sof(C00I)=Sof(H00O)=Sof(C00K)=Sof(H00S)=FVAR(1)
 Fixed Sof: H00A(0.5) H00B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C004(H00A,H00B), C005(H00C,H00D), C005(H00E,H00F), C00G(H00L,H00M), C5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C007(H007), C00C(H00J), C00F(H00K), C00H(H00N), C00I(H00O), C00K(H00S),
 C1(H1), C4(H4), C6(H6)
3.c Fitted hexagon refined as free rotating group:
 C2(C1,C4,C10,C3,C6)
3.d Idealised Me refined as rotating group:
 C009(H00G,H00H,H00I), C00J(H00P,H00Q,H00R)
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_shelx_res_checksum              16136
_shelx_hkl_checksum              60161
_olex2_submission_special_instructions 'No special instructions were received'