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_1569129
_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                 126.5400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   50.174(2)
_cell_length_b                   17.1013(7)
_cell_length_c                   36.5414(18)
_cell_measurement_reflns_used    9908
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      27.520
_cell_measurement_theta_min      2.776
_cell_volume                     25191.1(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-III PHOTON'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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            156008
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         2.518
_exptl_absorpt_coefficient_mu    3.936
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0678 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.8124.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             12096
_refine_diff_density_max         3.136
_refine_diff_density_min         -7.901
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1586
_refine_ls_number_reflns         29020
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0272P)^2^+444.4807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23486
_reflns_number_total             29020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01343j2.cif
_cod_data_source_block           U3bcbpy3CB8_170K_A
_cod_depositor_comments
'Adding full bibliography for 1569127--1569159.cif.'
_cod_original_cell_volume        25191(2)
_cod_database_code               1569129
_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(N7) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78)
\\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3.a Riding coordinates:
 O16(H16A,H16B)
3.b Rotating group:
 O17(H17A,H17B)
3.c Ternary CH refined with riding coordinates:
 C81(H81), C86(H86), C80(H80), C87(H87), C98(H98), C99(H99), C92(H92),
 C93(H93), C57(H57), C62(H62), C63(H63), C74(H74), C75(H75), C56(H56), C69(H69),
  C68(H68)
3.d Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C8(H8A,H8B), C90(H90A,H90B), C89(H89A,H89B),
  C95(H95A,H95B), C83(H83A,H83B), C84(H84A,H84B), C44(H44A,H44B), C26(H26A,
 H26B), C96(H96A,H96B), C71(H71A,H71B), C59(H59A,H59B), C77(H77A,H77B),
 C60(H60A,H60B), C66(H66A,H66B), C78(H78A,H78B), C65(H65A,H65B), C72(H72A,H72B)
3.e Aromatic/amide H refined with riding coordinates:
 C28(H28), C25(H25), C3(H3), C7(H7), C53(H53), C52(H52), C54(H54), C39(H39),
 C22(H22), C6(H6), C4(H4), C21(H21), C27(H27), C13(H13), C51(H51), C31(H31),
 C43(H43), C42(H42), C33(H33), C40(H40), C35(H35), C48(H48), C49(H49), C18(H18),
  C12(H12), C10(H10), C36(H36), C15(H15), C9(H9), C34(H34), C45(H45), C17(H17),
 C16(H16), C46(H46), C30(H30), C24(H24)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              80781
_shelx_fab_checksum              86291
_olex2_submission_special_instructions 'No special instructions were received'