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_1569133
_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             2022-03-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-11-10 deposited with the CCDC.	2023-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.516(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   50.309(9)
_cell_length_b                   17.123(3)
_cell_length_c                   36.562(9)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    210.00
_cell_measurement_theta_max      27.516
_cell_measurement_theta_min      2.788
_cell_volume                     25313(9)
_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      210.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -65
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            156711
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         2.691
_exptl_absorpt_coefficient_mu    3.917
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6069
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0656 before and 0.0512 after correction.
The Ratio of minimum to maximum transmission is 0.8140.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             12096
_refine_diff_density_max         1.479
_refine_diff_density_min         -2.454
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1588
_refine_ls_number_reflns         29177
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+186.7269P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23518
_reflns_number_total             29177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01343j2.cif
_cod_data_source_block           U3bcbpy3CB8_210K_A
_cod_depositor_comments
'Adding full bibliography for 1569127--1569159.cif.'
_cod_original_cell_volume        25314(9)
_cod_database_code               1569133
_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. Restrained distances
 U3-H30A \\sim U3-H30B
 with sigma of 0.02
3.a Riding coordinates:
 O1(H1A,H1B)
3.b Free rotating group:
 O30(H30A,H30B)
3.c Ternary CH refined with riding coordinates:
 C1(H1), C6(H6), C8(H8), C16(H16), C32(H32), C44(H44), C78(H78), C63(H63),
 C37(H37), C19(H19), C79(H79), C21(H21), C45(H45), C23(H23), C49(H49), C99(H99)
3.d Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C38(H38A,H38B), C82(H82A,H82B), C90(H90A,H90B), C55(H55A,
 H55B), C7(H7A,H7B), C57(H57A,H57B), C15(H15A,H15B), C2(H2A,H2B), C17(H17A,
 H17B), C35(H35A,H35B), C9(H9A,H9B), C41(H41A,H41B), C85(H85A,H85B), C87(H87A,
 H87B), C93(H93A,H93B), C47(H47A,H47B), C95(H95A,H95B), C97(H97A,H97B)
3.e Aromatic/amide H refined with riding coordinates:
 C10(H10), C24(H24), C26(H26), C28(H28), C34(H34), C46(H46), C48(H48),
 C50(H50), C52(H52), C54(H54), C58(H58), C60(H60), C62(H62), C64(H64), C80(H80),
  C84(H84), C94(H94), C96(H96), C98(H98), C102(H102), C51(H51), C53(H53),
 C29(H29), C59(H59), C61(H61), C65(H65), C33(H33), C67(H67), C69(H69), C77(H77),
  C39(H39), C5(H5), C83(H83), C43(H43), C25(H25), C101(H101)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97379
_shelx_fab_checksum              21040
_olex2_submission_special_instructions 'No special instructions were received'