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_7121930
_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
'2(Cl O4), C36 H36 N24 O12, 6(H2 O), C18 H22 N2 O4'
_chemical_formula_sum            'C54 H70 Cl2 N26 O30'
_chemical_formula_weight         1634.26
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-24 deposited with the CCDC.
2018-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                106.917(4)
_cell_angle_beta                 112.567(4)
_cell_angle_gamma                92.559(4)
_cell_formula_units_Z            1
_cell_length_a                   12.1092(6)
_cell_length_b                   12.2000(7)
_cell_length_c                   12.8040(7)
_cell_measurement_reflns_used    2578
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      59.705
_cell_measurement_theta_min      3.966
_cell_volume                     1644.78(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18355
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.588
_diffrn_reflns_theta_min         3.848
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.885
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0722 before and 0.0618 after correction. The Ratio of minimum to maximum transmission is 0.9198. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       block
_exptl_crystal_F_000             850
_refine_diff_density_max         0.528
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         5995
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+0.9348P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3369
_reflns_number_total             5995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05122d2.cif
_cod_data_source_block           H2L_ClO4_1
_cod_depositor_comments
'Adding full bibliography for 7121928--7121931.cif.'
_cod_original_cell_volume        1644.78(16)
_cod_database_code               7121930
_shelxl_version_number           2014-3
_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,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Free rotating group:
 O14(H14C,H14D), O15(H15A,H15B), O13(H13A,H13B)
3.b Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C17(H17), C20(H20), C16(H16), C25(H25)
3.c Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C12(H12A,H12B), C9(H9A,H9B), C27(H27A,H27B), C19(H19A,H19B),
 C7(H7A,H7B), C14(H14A,H14B), C8(H8A,H8B), C10(H10A,H10B)
3.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C3(H3)
;
_shelx_res_checksum              89224
_olex2_submission_special_instructions 'No special instructions were received'