Rapid Post-Synthetic Modification of Porous Coordination Cages with Copper-Catalyzed Click Chemistry
Dworzak, Michael; Montone, Christine M.; Halaszynski, Nicole Irene; Yap, Glenn P. A.; Kloxin, Christopher; Bloch, Eric D.; Chemical Communications  (2023) –; doi:10.1039/D3CC02015K

data_7131722
_publ_section_title
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 Rapid Post-Synthetic Modification of Porous Coordination Cages with
 Copper-Catalyzed Click Chemistry
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02015K
_journal_year                    2023
_chemical_formula_moiety
'0.5(C144 H120 O52 Zr12), 2(Cl), 2(C3 H7 N O), 2[C3H7NO], 2[H2O]'
_chemical_formula_sum            'C78 H68 Cl2 N2 O28 Zr6'
_chemical_formula_weight         2099.56
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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2022-07-18 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.5754(18)
_cell_length_b                   33.5754(18)
_cell_length_c                   17.8640(11)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      62.35
_cell_measurement_theta_min      2.80
_cell_volume                     20138(2)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            72722
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        62.413
_diffrn_reflns_theta_max         62.413
_diffrn_reflns_theta_min         2.802
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.967
_exptl_absorpt_correction_T_max  0.7522
_exptl_absorpt_correction_T_min  0.5426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1431 before and 0.0731 after correction.
The Ratio of minimum to maximum transmission is 0.7214.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       block
_exptl_crystal_F_000             8384
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.535
_refine_diff_density_min         -1.122
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         7988
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0730
_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^)+(0.1211P)^2^+318.3777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2028
_refine_ls_wR_factor_ref         0.2214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6167
_reflns_number_total             7988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02015k2.cif
_cod_data_source_block           eric597
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7131722
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.370
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12_3-C13_3
 1.189 with sigma of 0.014
 C11_3-C12_3
 1.472 with sigma of 0.012
 C11_3-C13_3
 2.661 with sigma of 0.014
 O3_3-C8_3 \\sim O4_3-C11_3
 with sigma of 0.02
 O3_3-C9_3 \\sim O4_3-C12_3
 with sigma of 0.02
 O3_3-C10_3 \\sim O4_3-C13_3
 with sigma of 0.02
 C8_3-C10_3 \\sim C11_3-C13_3
 with sigma of 0.02
 C9_3-C10_3 \\sim C12_3-C13_3
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: O3(0.5) O4(0.5) C2(0.5) C3(0.5) C4(0.5) H4(0.5) C5(0.5) C6(0.5)
 C7(0.5) H7(0.5) C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) C10(0.5) H10(0.5) C11(0.5)
 H11A(0.5) H11B(0.5) C12(0.5) C13(0.5) H13(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C8(H8A,H8B), C11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), O1(H1), O2(H2), O3(H3), C1(H1A), C2(H2A), C3(H3A), C4(H4),
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13),
  C14(H14), C15(H15), C4(H4), C7(H7), C1(H1)
5.c Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
5.e :
 C11(H11), C14(H14), C10(H10), C13(H13)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 832 electrons were 
found in a volume of 3528\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
2[C3H7NO], 2[H2O] per Asymmetric Unit 
which account for 800 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68530
_shelx_hkl_checksum              18521
_shelx_fab_checksum              78342
_olex2_submission_special_instructions 'No special instructions were received'