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_7131720
_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         'C224 H200 Co16 N24 O84 S16, 50[C3H7NO]'
_chemical_formula_sum            'C374 H550 Co16 N74 O134 S16'
_chemical_formula_weight         9682.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-07-18 deposited with the CCDC.	2023-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                96.343(5)
_cell_angle_beta                 92.698(5)
_cell_angle_gamma                112.580(5)
_cell_formula_units_Z            1
_cell_length_a                   20.646(3)
_cell_length_b                   20.661(3)
_cell_length_c                   27.970(4)
_cell_measurement_reflns_used    9057
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      53.64
_cell_measurement_theta_min      2.33
_cell_volume                     10897(3)
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker Venture Photon'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.2168
_diffrn_reflns_av_unetI/netI     0.2617
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            98463
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        54.335
_diffrn_reflns_theta_max         54.335
_diffrn_reflns_theta_min         2.329
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.143
_exptl_absorpt_correction_T_max  0.7505
_exptl_absorpt_correction_T_min  0.3366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1691 before and 0.0965 after correction.
The Ratio of minimum to maximum transmission is 0.4485.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       plate
_exptl_crystal_F_000             5072
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.116
_refine_diff_density_max         1.448
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.00093(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1511
_refine_ls_number_reflns         25929
_refine_ls_number_restraints     3077
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.2120
_refine_ls_R_factor_gt           0.1419
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3661
_refine_ls_wR_factor_ref         0.3988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10051
_reflns_number_total             25929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02015k2.cif
_cod_data_source_block           eric627
_cod_original_cell_volume        10897(2)
_cod_database_code               7131720
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.536
_shelx_estimated_absorpt_t_min   0.280
_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. Restrained distances
 C4_3-C8_3 \\sim C4_3-C9_3 \\sim C4_3-C10_3
 with sigma of 0.02
 C7_3-C8_3 \\sim C7_3-C9_3 \\sim C7_3-C10_3
 with sigma of 0.02
 C8_3-C9_3 \\sim C9_3-C10_3 \\sim C10_3-C8_3
 with sigma of 0.02
 C4_4-C8_4 \\sim C4_4-C9_4 \\sim C4_4-C10_4
 with sigma of 0.02
 C7_4-C8_4 \\sim C7_4-C9_4 \\sim C7_4-C10_4
 with sigma of 0.02
 C8_4-C9_4 \\sim C9_4-C10_4 \\sim C10_4-C8_4
 with sigma of 0.02
 C4_5-C8_5 \\sim C4_5-C9_5 \\sim C4_5-C10_5
 with sigma of 0.02
 C7_5-C8_5 \\sim C7_5-C9_5 \\sim C7_5-C10_5
 with sigma of 0.02
 C8_5-C9_5 \\sim C9_5-C10_5 \\sim C10_5-C8_5
 with sigma of 0.02
 O1-Co4 \\sim O1-Co2
 with sigma of 0.02
 C7_6-C8_6 \\sim C1_6-C3_6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.004 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Free rotating group:
 C4(C7,C8,C9,C10)
5.b Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C),
 C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C3(H3), C5(H5), C3(H3), C5(H5), C5(H5), C3(H3),
 C5(H5), C3(H3), C2(H2), C6(H6), C4(H4), C2(H2), C4(H4), C6(H6), C3(H3), C5(H5),
  C3(H3), C5(H5), C5(H5), C3(H3), C3(H3), C5(H5), C2(H2), C6(H6), C4(H4)
5.d Fitted hexagon refined as free rotating group:
 C2(C3,C4,C5,C6,C7), C1(C2,C3,C4,C5,C6), C1(C2,C3,C4,C5,C6), C1(C6,C5,C9,C3,
 C2), C1(C6,C5,C4,C3,C2), C2(C7,C6,C5,C4,C3), C2(C3,C4,C5,C6,C7), C1(C2,C3,C8,
 C5,C6), C1(C6,C5,C4,C3,C2), C2(C7,C6,C5,C4,C3)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 2115 electrons were 
found in a volume of 6018\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
50[C3H7NO] per Asymmetric Unit 
which account for 2000 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              5106
_shelx_hkl_checksum              77847
_shelx_fab_checksum              46712
_olex2_submission_special_instructions 'No special instructions were received'