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_1569137
_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             2022-04-29
_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.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.581(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   49.939(10)
_cell_length_b                   17.159(3)
_cell_length_c                   35.770(10)
_cell_measurement_reflns_used    8384
_cell_measurement_temperature    310.00
_cell_measurement_theta_max      27.477
_cell_measurement_theta_min      2.733
_cell_volume                     24614(10)
_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      310.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-III PHOTON'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            151637
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.576
_diffrn_reflns_theta_min         2.438
_exptl_absorpt_coefficient_mu    4.029
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0762 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.8015.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             12096
_refine_diff_density_max         2.019
_refine_diff_density_min         -2.834
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1595
_refine_ls_number_reflns         28361
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+152.2775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21778
_reflns_number_total             28361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01343j2.cif
_cod_data_source_block           U3bcbpy3CB8_310K_A
_cod_depositor_comments
'Adding full bibliography for 1569127--1569159.cif.'
_cod_database_code               1569137
_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
Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O17') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(O17')=Sof(H17C)=Sof(H17D)=1-FVAR(1)
 Sof(O17)=Sof(H17A)=Sof(H17B)=FVAR(1)
4.a Riding coordinates:
 O16(H16A,H16B), O17(H17A,H17B), O17'(H17C,H17D)
4.b Ternary CH refined with riding coordinates:
 C96(H96), C101(H101), C102(H102), C100(H100), C95(H95), C99(H99), C97(H97),
 C98(H98), C76(H76), C75(H75), C74(H74), C77(H77), C78(H78), C72(H72), C73(H73),
  C71(H71)
4.c Secondary CH2 refined with riding coordinates:
 C85(H85A,H85B), C88(H88A,H88B), C79(H79A,H79B), C90(H90A,H90B), C81(H81A,
 H81B), C92(H92A,H92B), C8(H8A,H8B), C26(H26A,H26B), C44(H44A,H44B), C94(H94A,
 H94B), C62(H62A,H62B), C83(H83A,H83B), C58(H58A,H58B), C64(H64A,H64B),
 C70(H70A,H70B), C66(H66A,H66B), C56(H56A,H56B), C68(H68A,H68B), C60(H60A,H60B)
4.d Aromatic/amide H refined with riding coordinates:
 C24(H24), C21(H21), C13(H13), C46(H46), C12(H12), C25(H25), C30(H30),
 C27(H27), C43(H43), C45(H45), C22(H22), C28(H28), C3(H3), C51(H51), C4(H4),
 C31(H31), C9(H9), C6(H6), C52(H52), C10(H10), C49(H49), C54(H54), C36(H36),
 C7(H7), C42(H42), C53(H53), C48(H48), C39(H39), C33(H33), C15(H15), C40(H40),
 C35(H35), C18(H18), C17(H17), C34(H34), C16(H16)
;
_shelx_res_checksum              90375
_shelx_fab_checksum              21466
_olex2_submission_special_instructions 'No special instructions were received'