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_7131721
_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         'C108 H94 N18 O40 Zr12, 4(Cl), 20[C3H7NO]'
_chemical_formula_sum            'C168 H234 Cl4 N38 O60 Zr12'
_chemical_formula_weight         4982.36
_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             2021-01-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.235(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.144(3)
_cell_length_b                   26.347(3)
_cell_length_c                   29.344(3)
_cell_measurement_reflns_used    6938
_cell_measurement_temperature    150
_cell_measurement_theta_max      44.54
_cell_measurement_theta_min      2.70
_cell_volume                     22527(4)
_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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0670
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        39.970
_diffrn_reflns_theta_max         39.970
_diffrn_reflns_theta_min         2.261
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.480
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_correction_T_min  0.4957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1049 before and 0.0644 after correction.
The Ratio of minimum to maximum transmission is 0.6620.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             10144
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.793
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         6830
_refine_ls_number_restraints     2195
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0791
_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^)+(0.1448P)^2^+379.7620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4546
_reflns_number_total             6830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02015k2.cif
_cod_data_source_block           eric503
_cod_original_cell_volume        22526(4)
_cod_database_code               7131721
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.226
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H6 of O6, H2 of O2, H4 of O4, H3 of O3, H8 of O8, H7 of O7
 At 1.5 times of:
  H5 of O5, H1 of O1
2. Shared sites
{O2, O3}
{C8, C7}
{O4, O1}
{O4, O1}
{C8, C7}
{O2, O3}
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 2A
Uanis(O1_3) = Uanis(O1_4)
Uanis(O2_3) = Uanis(O2_4)
Uanis(O3_3) = Uanis(O3_4)
Uanis(O4_3) = Uanis(O4_4)
Uanis(N1_3) = Uanis(N1_4)
Uanis(N2_3) = Uanis(N2_4)
Uanis(N3_3) = Uanis(N3_4)
Uanis(C1_3) = Uanis(C1_4)
Uanis(C2_3) = Uanis(C2_4)
Uanis(C3_3) = Uanis(C3_4)
Uanis(C4_3) = Uanis(C4_4)
Uanis(C5_3) = Uanis(C5_4)
Uanis(C6_3) = Uanis(C6_4)
Uanis(C7_3) = Uanis(C7_4)
Uanis(C8_3) = Uanis(C8_4)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(N1)=Sof(N2)=Sof(N3)=Sof(C1)=Sof(C2)=
 Sof(H2)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(C8)=1-
 FVAR(1)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(N1)=Sof(N2)=Sof(N3)=Sof(C1)=Sof(C2)=
 Sof(H2)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(C8)=FVAR(1)
6.a Free rotating group:
 N1(N2,N3,C1,C2,C3,C4,C5,C6), N1(N2,N3,C1,C2,C3,C4,C5,C6), N1(N2,N3,C1,C2,C3,
 C4,C5,C6), N1(N2,N3,C1,C2,C3,C4,C5,C6)
6.b Ternary CH refined with riding coordinates:
 O1(H1), O5(H5)
6.c Aromatic/amide H refined with riding coordinates:
 O2(H2), O3(H3), O4(H4), O6(H6), O7(H7), O8(H8), C1(H1A), C2(H2A), C3(H3A),
 C4(H4A), C5(H5A), C6(H6A), C7(H7A), C8(H8A), C9(H9), C10(H10), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
  C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29), C30(H30), C2(H2), C4(H4), C6(H6), C2(H2), C4(H4),
  C6(H6), C2(H2), C4(H4), C6(H6), C2(H2), C4(H4), C6(H6)
6.d Fitted pentagon refined as free rotating group:
 C1(C2,C3,C4,C5), C6(C7,C8,C9,C10), C11(C12,C13,C14,C15), C16(C17,C18,C19,C20),
  C21(C22,C23,C24,C25), C26(C27,C28,C29,C30)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 3028 electrons were 
found in a volume of 11404\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
20[C3H7NO] per Asymmetric Unit 
which account for 3200 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96633
_shelx_hkl_checksum              24792
_shelx_fab_checksum              9200
_olex2_submission_special_instructions 'No special instructions were received'