Improving the gas sorption capacity in lantern-type metal-organic polyhedra by a scrambled cage method.
Doñagueda Suso, Beatriz; Wang, Zaoming; Kennedy, Alan R.; Fletcher, Ashleigh J.; Furukawa, Shuhei; Craig, Gavin A.; Chemical science 15 (2024) 2857–2866; doi:10.1039/d3sc06140j

data_1570760
_publ_section_title
;
 Improving the gas sorption capacity in lantern-type metal-organic
 polyhedra by a scrambled cage method.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              2857
_journal_page_last               2866
_journal_paper_doi               10.1039/d3sc06140j
_journal_volume                  15
_journal_year                    2024
_chemical_formula_sum            'C148.66 H167.11 Cu4 N18.66 O46.56'
_chemical_formula_weight         3214.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.081(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.9031(2)
_cell_length_b                   16.7668(1)
_cell_length_c                   24.9964(2)
_cell_measurement_reflns_used    40619
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.9410
_cell_measurement_theta_min      2.6230
_cell_volume                     8320.43(12)
_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Synergy-i'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            89644
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.298
_diffrn_reflns_theta_min         2.745
_exptl_absorpt_coefficient_mu    1.268
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       block
_exptl_crystal_F_000             3356
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.275
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.593
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     982
_refine_ls_number_reflns         16543
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.610
_refine_ls_R_factor_all          0.1073
_refine_ls_R_factor_gt           0.0995
_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          0.3353
_refine_ls_wR_factor_ref         0.3470
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14251
_reflns_number_total             16543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06140j2.cif
_cod_data_source_block           bd280alan
_cod_depositor_comments
'Adding full bibliography for 1570759--1570762.cif.'
_cod_database_code               1570760
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.884
_shelx_estimated_absorpt_t_min   0.786
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C7S, C7T}
3. Restrained distances
 O3S-C6S = O5S-C14S = O4S-C10S = O5T-C14T = O4T-C10T = O3T-C6T
 1.26 with sigma of 0.01
 O6T-C18T = O8S-C22S
 1.26 with sigma of 0.01
 N2S-C8S = N2S-C7S = N4S-C15S = N4S-C16S = N3S-C11S = N3S-C9S
 1.47 with sigma of 0.01
 N4T-C16T = N4T-C13T = N3T-C12T = N3T-C11T = N2T-C5T = N2T-C7T
 1.47 with sigma of 0.01
 N5T-C19T = N5T-C17T = N8S-C24S = N8S-C23S
 1.47 with sigma of 0.01
 C5S-C6S = C13S-C14S = C10S-C12S = C14T-C15T = C10T-C9T
 1.52 with sigma of 0.01
 C6T-C8T = C18T-C20T = C21S-C22S
 1.52 with sigma of 0.01
 N2S-C6S = N4S-C14S = N3S-C10S = N4T-C14T = N3T-C10T = C6T-N2T
 1.33 with sigma of 0.01
 N5T-C18T = N8S-C22S
 1.33 with sigma of 0.01
 O6T-C20T
 2.45 with sigma of 0.02
 N5T-O6T
 2.3 with sigma of 0.02
 O3S-C5S
 2.44 with sigma of 0.02
 C8S-C7S
 2.4 with sigma of 0.02
 O2S-H2SA = O2S-H2SB
 0.88 with sigma of 0.01
 H2SB-H2SA
 1.33 with sigma of 0.02
 C23S-C24S
 2.4 with sigma of 0.02
 C5T-C7S
 2.4 with sigma of 0.02
 C5T-O3T
 2.4 with sigma of 0.02
4. Rigid bond restraints
 O1S, N1S, C1S, C2S, C3S, C4S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C22S, N8S, C21S, O8S, C24S, C23S
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
O1S \\sim N1S \\sim C1S \\sim C2S \\sim C3S \\sim C4S: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
C22S \\sim N8S \\sim C21S \\sim O8S \\sim C24S \\sim C23S: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
Uiso(O6S) = Uiso(O6T)
Uiso(C20S) = Uiso(C20T)
Uiso(C2) = Uiso(C2A)
Uiso(C3) = Uiso(C3A)
Uiso(C4) = Uiso(C4A)
Uiso(C5) = Uiso(C5A)
Uiso(C6) = Uiso(C6A)
Uiso(C7) = Uiso(C7A)
Uiso(C7S) = Uiso(C7T)
Uiso(C15S) = Uiso(C15T)
Uiso(C5S) = Uiso(C5T)
6. Others
 Sof(C6T)=Sof(O3T)=Sof(N2T)=Sof(C8T)=Sof(H8TA)=Sof(H8TB)=Sof(H8TC)=Sof(C5T)=
 Sof(H5TA)=Sof(H5TB)=Sof(H5TC)=Sof(C7T)=Sof(H7TA)=Sof(H7TB)=Sof(H7TC)=1-FVAR(1)
 Sof(O3S)=Sof(N2S)=Sof(C6S)=Sof(C5S)=Sof(H5SA)=Sof(H5SB)=Sof(H5SC)=Sof(C8S)=
 Sof(H8SA)=Sof(H8SB)=Sof(H8SC)=Sof(C7S)=Sof(H7SA)=Sof(H7SB)=Sof(H7SC)=FVAR(1)
 Sof(H29)=Sof(H49)=1-FVAR(2)
 Sof(C3M)=Sof(H3MA)=Sof(H3MB)=Sof(H3MC)=Sof(C4M)=Sof(H4MA)=Sof(H4MB)=Sof(H4MC)=
 FVAR(2)
 Sof(N4T)=Sof(C14T)=Sof(O5T)=Sof(C13T)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C15T)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16T)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(3)
 Sof(O5S)=Sof(N4S)=Sof(C13S)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14S)=Sof(C16S)=
 Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C15S)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(3)
 Sof(C10T)=Sof(C12T)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(N3T)=Sof(O4T)=Sof(C11T)=
 Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C9T)=Sof(H9TA)=Sof(H9TB)=Sof(H9TC)=1-FVAR(4)
 Sof(O4S)=Sof(C10S)=Sof(C12S)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(N3S)=Sof(C11S)=
 Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C9S)=Sof(H9SA)=Sof(H9SB)=Sof(H9SC)=FVAR(4)
 Sof(N5T)=Sof(C19T)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(O6T)=Sof(C17T)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C18T)=Sof(C20T)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(5)
 Sof(N5S)=Sof(O6S)=Sof(C17S)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18S)=Sof(C19S)=
 Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20S)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(5)
 Sof(C5A)=Sof(H5A)=Sof(C3A)=Sof(H3A)=Sof(C2A)=Sof(C4A)=Sof(C7A)=Sof(H7A)=
 Sof(C6A)=Sof(H6A)=1-FVAR(6)
 Sof(C2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=FVAR(6)
 Sof(H23)=1-FVAR(7)
 Sof(C2M)=Sof(H2MA)=Sof(H2MB)=Sof(H2MC)=Sof(C1M)=Sof(H1MA)=Sof(H1MB)=Sof(H1MC)=
 FVAR(7)
 Fixed Sof: O7S(0.5) C22S(0.33) N8S(0.33) C21S(0.33) H21A(0.33) H21B(0.33)
 H21C(0.33) O8S(0.33) C24S(0.33) H24A(0.33) H24B(0.33) H24C(0.33) O9S(0.2)
 C23S(0.33) H23A(0.33) H23B(0.33) H23C(0.33) O10S(0.25)
 Fixed Uiso: C2M(0.08) C1M(0.08)
7.a Fixed occupancy and ADP/Uiso:
 H2SA, H2SB
7.b Riding coordinates:
 C23(H23), C29(H29), C49(H49)
7.c Ternary CH refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
7.d Me refined with riding coordinates:
 C12S(H12A,H12B,H12C), C13S(H13A,H13B,H13C), C16S(H16A,H16B,H16C), C5S(H5SA,
 H5SB,H5SC), C8S(H8SA,H8SB,H8SC), C7S(H7SA,H7SB,H7SC), C15S(H15A,H15B,H15C),
 C17S(H17A,H17B,H17C), C19S(H19A,H19B,H19C), C20S(H20A,H20B,H20C), C11S(H11A,
 H11B,H11C), C9S(H9SA,H9SB,H9SC), C13T(H13D,H13E,H13F), C15T(H15D,H15E,H15F),
 C16T(H16D,H16E,H16F), C12T(H12D,H12E,H12F), C11T(H11D,H11E,H11F), C9T(H9TA,
 H9TB,H9TC), C8T(H8TA,H8TB,H8TC), C5T(H5TA,H5TB,H5TC), C7T(H7TA,H7TB,H7TC),
 C19T(H19D,H19E,H19F), C17T(H17D,H17E,H17F), C20T(H20D,H20E,H20F), C21S(H21A,
 H21B,H21C), C24S(H24A,H24B,H24C), C23S(H23A,H23B,H23C)
7.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C16(H16), C17(H17), C21(H21), C22(H22), C25(H25),
 C30(H30), C31(H31), C33(H33), C42(H42), C43(H43), C47(H47), C48(H48), C51(H51),
  C5A(H5A), C3A(H3A), C7A(H7A), C6A(H6A)
7.f Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C3M(H3MA,H3MB,H3MC), C3S(H3SA,H3SB,H3SC), C4M(H4MA,H4MB,
 H4MC), C4S(H4SA,H4SB,H4SC), C2M(H2MA,H2MB,H2MC), C1M(H1MA,H1MB,H1MC)
;
_shelx_res_checksum              25124
_olex2_submission_special_instructions 'No special instructions were received'