Colossal negative thermal expansion in a cucurbit[8]uril-enabled uranyl-organic polythreading framework <i>via</i> thermally induced relaxation.
Jin, Qiu-Yan; Liang, Yuan-Yuan; Zhang, Zhi-Hui; Meng, Liao; Geng, Jun-Shan; Hu, Kong-Qiu; Yu, Ji-Pan; Chai, Zhi-Fang; Mei, Lei; Shi, Wei-Qun; Chemical science 14 (2023) 6330–6340; doi:10.1039/d3sc01343j

data_1569142
_publ_section_title
;
 Colossal negative thermal expansion in a cucurbit[8]uril-enabled
 uranyl-organic polythreading framework <i>via</i> thermally induced
 relaxation.
;
_journal_issue                   23
_journal_name_full               'Chemical science'
_journal_page_first              6330
_journal_page_last               6340
_journal_paper_doi               10.1039/d3sc01343j
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C156 H140 N44 O50 U6, C48 H48 N32 O16'
_chemical_formula_sum            'C204 H188 N76 O66 U6'
_chemical_formula_weight         6188.47
_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   mixed
_audit_creation_date             2022-11-07
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-10 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.806(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   50.170(3)
_cell_length_b                   17.1438(12)
_cell_length_c                   36.311(2)
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.76
_cell_volume                     25006(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0831
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            127324
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         2.423
_exptl_absorpt_coefficient_mu    3.965
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5511
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0863 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.7391.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_description       block
_exptl_crystal_F_000             12096
_refine_diff_density_max         2.931
_refine_diff_density_min         -3.379
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1586
_refine_ls_number_reflns         28315
_refine_ls_number_restraints     3798
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0623P)^2^+880.2120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19967
_reflns_number_total             28315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01343j3.cif
_cod_data_source_block           U3bcbpy3CB8_170K_B
_cod_depositor_comments
'Adding full bibliography for 1569127--1569159.cif.'
_cod_database_code               1569142
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
C97 \\sim C37 \\sim C20 \\sim C1 \\sim C83 \\sim C21 \\sim C38 \\sim C90 \\sim
C29 \\sim C51 \\sim C12 \\sim C53 \\sim C47 \\sim C93 \\sim C32 \\sim C81 \\sim
C7 \\sim C31 \\sim C8 \\sim C94 \\sim C45 \\sim C95 \\sim C42 \\sim C27 \\sim
C11 \\sim C14 \\sim C52 \\sim C28 \\sim C92 \\sim C41 \\sim C98 \\sim C30 \\sim
C24 \\sim C49 \\sim C25 \\sim C82 \\sim C46 \\sim C80 \\sim C6 \\sim C54 \\sim
C2 \\sim C88 \\sim C84 \\sim C44 \\sim C101 \\sim C79 \\sim C59 \\sim C13 \\sim
C91 \\sim C99 \\sim C36 \\sim C9 \\sim C18 \\sim C96 \\sim C39 \\sim C26 \\sim
C10 \\sim C65 \\sim C15 \\sim C87 \\sim C86 \\sim C85 \\sim C102 \\sim C48
\\sim C100 \\sim C60 \\sim C61 \\sim C33 \\sim C34 \\sim C17 \\sim C40 \\sim
C57 \\sim C63 \\sim C78 \\sim C16 \\sim C69 \\sim C35 \\sim C71 \\sim C77 \\sim
C58 \\sim C72 \\sim C56 \\sim C73 \\sim C70 \\sim C67 \\sim C76 \\sim C74 \\sim
C75 \\sim C89 \\sim C62 \\sim C64 \\sim C66 \\sim C68 \\sim C23 \\sim C22 \\sim
C19 \\sim C43 \\sim C50 \\sim C3 \\sim C4 \\sim C5 \\sim C55: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
Uanis(C19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O17) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Riding coordinates:
 O17(H17A,H17B)
4.b Rotating group:
 O16(H16A,H16B)
4.c Ternary CH refined with riding coordinates:
 C97(H97), C95(H95), C98(H98), C101(H101), C99(H99), C96(H96), C102(H102),
 C100(H100), C78(H78), C71(H71), C77(H77), C72(H72), C73(H73), C76(H76),
 C74(H74), C75(H75)
4.d Secondary CH2 refined with riding coordinates:
 C93(H93A,H93B), C8(H8A,H8B), C82(H82A,H82B), C80(H80A,H80B), C88(H88A,H88B),
 C84(H84A,H84B), C44(H44A,H44B), C91(H91A,H91B), C26(H26A,H26B), C86(H86A,H86B),
  C60(H60A,H60B), C58(H58A,H58B), C56(H56A,H56B), C70(H70A,H70B), C89(H89A,
 H89B), C62(H62A,H62B), C64(H64A,H64B), C66(H66A,H66B), C68(H68A,H68B)
4.e Aromatic/amide H refined with riding coordinates:
 C21(H21), C51(H51), C12(H12), C53(H53), C7(H7), C31(H31), C45(H45), C42(H42),
 C27(H27), C52(H52), C28(H28), C30(H30), C24(H24), C49(H49), C25(H25), C46(H46),
  C6(H6), C54(H54), C13(H13), C36(H36), C9(H9), C18(H18), C39(H39), C10(H10),
 C15(H15), C48(H48), C33(H33), C34(H34), C17(H17), C40(H40), C16(H16), C35(H35),
  C22(H22), C43(H43), C3(H3), C4(H4)
;
_shelx_res_checksum              764
_shelx_fab_checksum              57046
_olex2_submission_special_instructions 'No special instructions were received'