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_1569136
_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         'C48 H48 N32 O16, C18 H15 N2 O2, C18 H14 N2 O2'
_chemical_formula_sum            'C84 H77 N36 O20'
_chemical_formula_weight         1910.81
_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   geom
_audit_creation_date             2022-03-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-05-05 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.644(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2111(8)
_cell_length_b                   20.6527(10)
_cell_length_c                   36.062(2)
_cell_measurement_reflns_used    9720
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.70
_cell_volume                     10463.9(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0855
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            279420
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.581
_diffrn_reflns_theta_min         2.448
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6726
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0802 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.9021.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             3972
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         24139
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0668P)^2^+7.4252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17050
_reflns_number_total             24139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01343j2.cif
_cod_data_source_block           HbcbpyCl_2_CB8
_cod_depositor_comments
'Adding full bibliography for 1569127--1569159.cif.'
_cod_original_cell_volume        10463.7(10)
_cod_database_code               1569136
_shelx_shelxl_version_number     2018/3
_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) groups
2. Restrained distances
 C79-C70 \\sim C84-C79 \\sim C84-C83 \\sim C83-C73 \\sim C74-C73 \\sim C74-C70
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C79) \\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C7(H7), C11(H11), C12(H12), C13(H13), C17(H17), C19(H19), C20(H20), C24(H24),
 C33(H33), C36(H36), C42(H42), C54(H54), C56(H56), C58(H58), C60(H60), C67(H67)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B), C29(H29A,H29B), C30(H30A,
 H30B), C31(H31A,H31B), C37(H37A,H37B), C39(H39A,H39B), C44(H44A,H44B),
 C45(H45A,H45B), C47(H47A,H47B), C57(H57A,H57B), C61(H61A,H61B), C62(H62A,H62B),
  C64(H64A,H64B), C65(H65A,H65B), C68(H68A,H68B), C76(H76A,H76B)
4.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C34(H34), C38(H38), C40(H40), C41(H41), C43(H43), C46(H46),
 C48(H48), C51(H51), C55(H55), C63(H63), C66(H66), C69(H69), C70(H70), C71(H71),
  C72(H72), C74(H74), C75(H75), C77(H77), C78(H78), C81(H81), C82(H82),
 C83(H83), C84(H84)
4.d Idealised tetrahedral OH refined as rotating group:
 O16(H16)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7937
_shelx_fab_checksum              63028
_olex2_submission_special_instructions 'No special instructions were received'