A neptunium(v)-mediated interwoven transuranium-rotaxane network incorporating a mechanically interlocked [c2]daisy chain unit.
Mei, Lei; Xu, Chao; Wu, Qun-Yan; Hu, Kong-Qiu; Yuan, Li-Yong; Chen, Jing; Xiao, Cheng-Liang; Wang, Shu-Ao; Chai, Zhi-Fang; Shi, Wei-Qun; Chemical communications (Cambridge, England) 54 (2018) 8645–8648; doi:10.1039/c8cc05122d

data_7121931
_publ_section_title
;
 A neptunium(v)-mediated interwoven transuranium-rotaxane network
 incorporating a mechanically interlocked [c2]daisy chain unit.
;
_journal_issue                   62
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8645
_journal_page_last               8648
_journal_paper_doi               10.1039/c8cc05122d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety
'C36 H40 N4 O10 U, 2(Cl O4), 2(C36 H36 N24 O12)'
_chemical_formula_sum            'C108 H112 Cl2 N52 O42 U'
_chemical_formula_weight         3119.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.328(2)
_cell_angle_beta                 97.214(2)
_cell_angle_gamma                95.183(2)
_cell_formula_units_Z            1
_cell_length_a                   12.7487(6)
_cell_length_b                   15.3678(7)
_cell_length_c                   17.1021(8)
_cell_measurement_reflns_used    9640
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      2.98
_cell_volume                     3310.0(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            88859
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.939
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0520 before and 0.0451 after correction. The Ratio of minimum to maximum transmission is 0.9575. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       block
_exptl_crystal_F_000             1586
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.369
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.261
_refine_diff_density_max         1.890
_refine_diff_density_min         -2.326
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         12992
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0806P)^2^+7.8228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12498
_reflns_number_total             12992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05122d2.cif
_cod_data_source_block           UP107
_cod_depositor_comments
'Adding full bibliography for 7121928--7121931.cif.'
_cod_database_code               7121931
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.632
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O21)
\\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O5(0.5) O4(0.5) C10(0.5) O2(0.5) O3(0.5) C10'(0.5)
4.a Ternary CH refined with riding coordinates:
 C27(H27), C26(H26), C33(H33), C31(H31), C30(H30), C52(H52), C51(H51),
 C46(H46), C45(H45), C39(H39), C38(H38), C34(H34)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C18(H18A,H18B), C17(H17A,H17B),
 C16(H16A,H16B), C19(H19A,H19B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B),
  C29(H29A,H29B), C49(H49A,H49B), C48(H48A,H48B), C43(H43A,H43B), C42(H42A,
 H42B), C40(H40A,H40B), C37(H37A,H37B), C56(H56A,H56B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15)
;
_shelx_res_checksum              31220
_shelx_fab_checksum              8756
_olex2_submission_special_instructions 'No special instructions were received'