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_1570759
_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            'C120 H104 Cu4 N12 O38'
_chemical_formula_weight         2576.31
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-10-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-10-26 deposited with the CCDC.	2024-01-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.538(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.7309(2)
_cell_length_b                   16.8006(2)
_cell_length_c                   24.9013(2)
_cell_measurement_reflns_used    36415
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.5980
_cell_measurement_theta_min      2.7750
_cell_volume                     8238.82(15)
_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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.0294
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            88490
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         73.239
_diffrn_reflns_theta_min         2.775
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.92a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
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    1.039
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.717
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         16376
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0782
_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^)+(0.1418P)^2^+11.0328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2422
_refine_ls_wR_factor_ref         0.2468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14452
_reflns_number_total             16376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc06140j2.cif
_cod_data_source_block           bd652_100k
_cod_depositor_comments
'Adding full bibliography for 1570759--1570762.cif.'
_cod_database_code               1570759
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.806
_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, All O(H,H) groups
2. Restrained distances
 O300-C302 = O1D-C1D = C202-O200 = O100-C100
 1.28 with sigma of 0.01
 N300-C303 = N300-C304 = N1D-C3D = N1D-C4D = N201-C201 = N201-C204
 1.48 with sigma of 0.01
 N100-C102 = N100-C103
 1.48 with sigma of 0.01
 C302-C301 = C1D-C2D = C202-C203 = C100-C101
 1.51 with sigma of 0.01
 C302-N300 = C1D-N1D = N201-C202 = C100-N100
 1.33 with sigma of 0.01
3. Rigid bond restraints
 O1D, N1D, C3D, C1D, C2D, C4D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C22, C20, C25A, C24A, C23A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N100, C100, C101, O100, C102, C103
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1D, N1D, C1D, C2D, C3D, C4D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N300, C301, O300, C302, C303, C304
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O200, N201, C201, C202, C203, C204
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1D \\sim N1D \\sim C3D \\sim C1D \\sim C2D \\sim C4D: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
C21 \\sim C22 \\sim C20 \\sim C25A \\sim C24A \\sim C23A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
N100 \\sim C100 \\sim C101 \\sim O100 \\sim C102 \\sim C103: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
O1D \\sim N1D \\sim C1D \\sim C2D \\sim C3D \\sim C4D: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
N300 \\sim C301 \\sim O300 \\sim C302 \\sim C303 \\sim C304: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
O200 \\sim N201 \\sim C201 \\sim C202 \\sim C203 \\sim C204: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
Uanis(C23B) = Uanis(C23A)
Uanis(C24B) = Uanis(C24A)
Uanis(C25B) = Uanis(C25A)
Uanis(O300) = Uanis(O200)
Uanis(N300) = Uanis(C202)
Uanis(C302) = Uanis(N201)
Uanis(C301) = Uanis(C204)
Uanis(C304) = Uanis(C203)
Uanis(O1D) = Uanis(O100)
Uanis(C4D) = Uanis(C101)
Uanis(C3D) = Uanis(C103)
Uanis(C2D) = Uanis(C102)
Uanis(O11) = Uanis(O11A)
5. Others
 Sof(C23B)=Sof(H23B)=Sof(C25B)=Sof(H25B)=Sof(C24B)=Sof(H24B)=Sof(O11A)=1-FVAR(1)
 Sof(C25A)=Sof(H25A)=Sof(C24A)=Sof(H24A)=Sof(C23A)=Sof(H23A)=Sof(O11)=FVAR(1)
 Sof(O200)=Sof(N201)=Sof(C201)=Sof(H20a)=Sof(H20b)=Sof(H20c)=Sof(C202)=
 Sof(C203)=Sof(H20d)=Sof(H20e)=Sof(H20f)=Sof(C204)=Sof(H20g)=Sof(H20h)=
 Sof(H20i)=1-FVAR(2)
 Sof(N300)=Sof(C301)=Sof(H30a)=Sof(H30b)=Sof(H30c)=Sof(O300)=Sof(C302)=
 Sof(C303)=Sof(H30d)=Sof(H30e)=Sof(H30f)=Sof(C304)=Sof(H30g)=Sof(H30h)=
 Sof(H30i)=FVAR(2)
 Sof(N100)=Sof(C100)=Sof(C101)=Sof(H10a)=Sof(H10b)=Sof(H10c)=Sof(O100)=
 Sof(C102)=Sof(H10d)=Sof(H10e)=Sof(H10f)=Sof(C103)=Sof(H10g)=Sof(H10h)=
 Sof(H10i)=1-FVAR(3)
 Sof(O1D)=Sof(N1D)=Sof(C1D)=Sof(C2D)=Sof(H2Da)=Sof(H2Db)=Sof(H2Dc)=Sof(C3D)=
 Sof(H3Da)=Sof(H3Db)=Sof(H3Dc)=Sof(C4D)=Sof(H4Da)=Sof(H4Db)=Sof(H4Dc)=FVAR(3)
6.a Rotating group:
 O1W(H1Wa,H1Wb)
6.b Ternary CH refined with riding coordinates:
 C36(H36), C38(H38), C17(H17), C37(H37), C11(H11), C15(H15), C10(H10),
 C43(H43), C42(H42), C41(H41), C16(H16), C12(H12)
6.c Me refined with riding coordinates:
 C2D(H2Da,H2Db,H2Dc), C3D(H3Da,H3Db,H3Dc), C301(H30a,H30b,H30c), C4D(H4Da,H4Db,
 H4Dc), C303(H30d,H30e,H30f), C304(H30g,H30h,H30i), C201(H20a,H20b,H20c),
 C203(H20d,H20e,H20f), C204(H20g,H20h,H20i), C101(H10a,H10b,H10c), C102(H10d,
 H10e,H10f), C103(H10g,H10h,H10i)
6.d Aromatic/amide H refined with riding coordinates:
 C47(H47), C29(H29), C49(H49), C40(H40), C51(H51), C39(H39), C3(H3), C21(H21),
 C50(H50), C14(H14), C33(H33), C13(H13), C31(H31), C7(H7), C5(H5), C32(H32),
 C6(H6), C23B(H23B), C25B(H25B), C24B(H24B), C25A(H25A), C24A(H24A), C23A(H23A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74773
_shelx_fab_checksum              10898
_olex2_submission_special_instructions 'No special instructions were received'