Soluble imidazolium-functionalized coordination cages for efficient homogeneous catalysis of CO<sub>2</sub> cycloaddition reactions.
Tong, Hui-Ying; Liang, Jun; Wu, Qiu-Jin; Zou, Yu-Huang; Huang, Yuan-Biao; Cao, Rong; Chemical communications (Cambridge, England) 57 (2021) 2140–2143; doi:10.1039/d0cc08098e

data_7127863
_publ_section_title
;
 Soluble imidazolium-functionalized coordination cages for efficient
 homogeneous catalysis of CO<sub>2</sub> cycloaddition reactions.
;
_journal_issue                   17
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2140
_journal_page_last               2143
_journal_paper_doi               10.1039/d0cc08098e
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C390 H343.329 N24 Ni24 O126 S24, 2.274(I)'
_chemical_formula_sum            'C390 H343.33 I2.28 N24 Ni24 O126 S24'
_chemical_formula_weight         9849.37
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-18
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-01-13 deposited with the CCDC.	2021-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.1997(5)
_cell_length_b                   29.1997(5)
_cell_length_c                   40.4454(12)
_cell_measurement_reflns_used    12865
_cell_measurement_temperature    293
_cell_measurement_theta_max      48.916
_cell_measurement_theta_min      1.86
_cell_volume                     34484.7(13)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            69306
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        48.916
_diffrn_reflns_theta_max         48.916
_diffrn_reflns_theta_min         1.860
_exptl_absorpt_coefficient_mu    4.833
_exptl_absorpt_correction_T_max  0.437
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.949
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             10072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.206
_refine_diff_density_min         -2.178
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.000079(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.325
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1015
_refine_ls_number_reflns         12857
_refine_ls_number_restraints     3589
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.1524
_refine_ls_R_factor_gt           0.1121
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3317
_refine_ls_wR_factor_ref         0.3583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7693
_reflns_number_total             12857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc08098e2.cif
_cod_data_source_block           x_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7127862--7127863.cif.'
_cod_original_cell_volume        34484.7(16)
_cod_database_code               7127863
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.445
_shelx_estimated_absorpt_t_min   0.445
_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
 N1-C50 = N2-C49 = C49-C51 = C50-C51 = N1B-C50B = N2B-C49B = C49B-C51B = C50B-
 C51B = N1C-C50C = N2C-C49C = C49C-C51C = C50C-C51C = N1D-C50D = N2D-C49D =
 C49D-C51D = C50D-C51D = N4-C53 = N3-C54 = N4B-C53B = N3B-C54B = C53-C55 = C54-
 C55 = C53B-C55B = C54B-C55B
 2.3 with sigma of 0.02
 C37-N1 = C38-N1B = C40-N1C = C41-N1D = N2-C52 = N2B-C52B = N2C-C52C = N2D-C52D
 1.45 with sigma of 0.02
 N1-C49 = N2-C50 = N1-C51 = N2-C51 = N1B-C49B = N2B-C50B = N1B-C51B = N2B-C51B
 = N1C-C49C = N2C-C50C = N1C-C51C = N2C-C51C = N1D-C49D = N2D-C50D = N1D-C51D =
 N2D-C51D
 1.42 with sigma of 0.01
 C49-C50 = C49B-C50B = C49C-C50C = C49D-C50D
 1.39 with sigma of 0.01
 C7-C8 = C7-C9 = C7-C10
 1.55 with sigma of 0.02
 C7-C8 = C7-C9 = C7-C10 = C7B-C8B = C7B-C9B = C7B-C10B = C7-C4 = C4-C7B = C15-
 C16 = C15-C17 = C15-C16B = C15-C17B = C28-C31 = C31-C32 = C31-C33 = C31-C34 =
 C31-C32B = C31-C33B = C31-C34B
 1.55 with sigma of 0.02
 N3-C53 = N4-C54 = N3-C55 = N4-C55 = N3B-C53B = N3B-C55B = N4B-C54B = N4B-C55B
 1.42 with sigma of 0.01
 C53-C54 = C53B-C54B
 1.39 with sigma of 0.01
 N4-C56 = N4B-C56B = C45-N3 = C46-N3B
 1.45 with sigma of 0.02
 C45-C53 \\sim C45-C55
 with sigma of 0.02
 C52-C50 \\sim C52-C51 \\sim C52B-C50B \\sim C52B-C51B \\sim C52C-C51C \\sim
C52C-C50C \\sim C52D-C50D
 \\sim C52D-C51D
 with sigma of 0.02
 C56-C54 \\sim C56-C55 \\sim C56B-C55B \\sim C56B-C54B
 with sigma of 0.01
 C8-C9 \\sim C8-C10 \\sim C9-C10
 with sigma of 0.01
 C8-C9 \\sim C8-C10 \\sim C9-C10 \\sim C8B-C9B \\sim C8B-C10B \\sim C8B-C10B
\\sim C16-C17 \\sim C16B-C17B
 \\sim C32-C33 \\sim C32-C34 \\sim C33-C34 \\sim C32B-C33B \\sim C32B-C34B
\\sim C33B-C34B
 with sigma of 0.01
3. Restrained planarity
 C37, N1, N2, C49, C50, C51, C52
 with sigma of 0.1
 C38, N1B, N2B, C49B, C50B, C51B, C52B
 with sigma of 0.1
 C40, N1C, N2C, C49C, C50C, C51C, C52C
 with sigma of 0.1
 C41, N1D, N2D, C49D, C50D, C51D, C52D
 with sigma of 0.1
 N3, N4, C53, C54, C55, C56
 with sigma of 0.1
 N3B, N4B, C53B, C54B, C55B, C56B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim N1B \\sim N2B \\sim N1C \\sim N2C \\sim N1D \\sim N2D \\sim
N3 \\sim N4 \\sim N3B \\sim N4B \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5
\\sim C6 \\sim C7 \\sim C7B \\sim C8 \\sim C8B \\sim C9 \\sim C9B \\sim C10
\\sim C10B \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C16B \\sim C17 \\sim C17B \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22
\\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C35 \\sim C36 \\sim C37
\\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45
\\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim
C49B \\sim C50B \\sim C51B \\sim C52B \\sim C49C \\sim C50C \\sim C51C \\sim
C52C \\sim C49D \\sim C50D \\sim C51D \\sim C52D \\sim C28 \\sim C29 \\sim C30
\\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C32B \\sim C33B \\sim C34B \\sim
C53 \\sim C54 \\sim C55 \\sim C56 \\sim C55B \\sim C53B \\sim C54B \\sim C56B
\\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim
O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim
O17 \\sim O18: within 3.8A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 3.8A
5. Others
 Sof(C7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=
 Sof(H9BC)=Sof(C10B)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C16B)=Sof(C32B)=
 Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=Sof(H33D)=Sof(H33E)=Sof(H33F)=
 Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=0.5*(1-FVAR(2))
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=0.5*FVAR(2)
 Sof(C7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Fixed Sof: H24A(0.5) H24B(0.5) H24C(0.5) N1(0.25) N2(0.25) C49(0.25)
 H49(0.25) C50(0.25) H50(0.25) C51(0.25) H51(0.25) N1B(0.25) N2B(0.25)
 C49B(0.25) H49B(0.25) C50B(0.25) H50B(0.25) C51B(0.25) H51B(0.25) C52B(0.25)
 H52D(0.25) H52E(0.25) H52F(0.25) N1C(0.25) N2C(0.25) C49C(0.25) H49C(0.25)
 C50C(0.25) H50C(0.25) C51C(0.25) H51C(0.25) C52C(0.25) H52G(0.25) H52H(0.25)
 H52I(0.25) N1D(0.25) N2D(0.25) C49D(0.25) H49D(0.25) C50D(0.25) H50D(0.25)
 C51D(0.25) H51D(0.25) C52D(0.25) H52J(0.25) H52K(0.25) H52L(0.25) N3(0.25)
 N4(0.25) C53(0.25) H53(0.25) C54(0.25) H54(0.25) C55(0.25) H55(0.25) C56(0.25)
 H56A(0.25) H56B(0.25) H56C(0.25) N3B(0.25) N4B(0.25) C55B(0.25) H55B(0.25)
 C53B(0.25) H53B(0.25) C54B(0.25) H54B(0.25) C56B(0.25) H56D(0.25) H56E(0.25)
 H56F(0.25)
6.a Me refined with riding coordinates:
 C8(H8A,H8B,H8C), C8B(H8BA,H8BB,H8BC), C9(H9A,H9B,H9C), C9B(H9BA,H9BB,H9BC),
 C10(H10A,H10B,H10C), C10B(H10D,H10E,H10F), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C17B(H17D,H17E,H17F), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C52(H52A,H52B,H52C), C52B(H52D,H52E,H52F), C52C(H52G,H52H,H52I), C52D(H52J,
 H52K,H52L), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C),
 C32B(H32D,H32E,H32F), C33B(H33D,H33E,H33F), C34B(H34D,H34E,H34F), C56(H56A,
 H56B,H56C), C56B(H56D,H56E,H56F)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C20(H20), C27(H27), C49(H49), C50(H50), C51(H51),
 C49B(H49B), C50B(H50B), C51B(H51B), C49C(H49C), C50C(H50C), C51C(H51C),
 C49D(H49D), C50D(H50D), C51D(H51D), C29(H29), C53(H53), C54(H54), C55(H55),
 C55B(H55B), C53B(H53B), C54B(H54B)
;
_shelx_res_checksum              59857
_shelx_fab_checksum              62119
_olex2_submission_special_instructions 'No special instructions were received'