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_7121929
_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(C36 H36 N24 O12), C9 H11 N O2, C18 H21 N2 O4, C9 H10 N O2, 4(Cl O4), 14(O)'
_chemical_formula_sum            'C108 H114 Cl4 N52 O62'
_chemical_formula_weight         3274.31
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-03
_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                86.375(5)
_cell_angle_beta                 88.628(5)
_cell_angle_gamma                67.119(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6870(12)
_cell_length_b                   15.9445(15)
_cell_length_c                   35.622(3)
_cell_measurement_reflns_used    9772
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      58.34
_cell_measurement_theta_min      3.19
_cell_volume                     6625.6(11)
_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 0.722
_diffrn_measured_fraction_theta_max 0.922
_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  0.0678
_diffrn_reflns_av_unetI/netI     0.1125
_diffrn_reflns_Laue_measured_fraction_full 0.722
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            38233
_diffrn_reflns_point_group_measured_fraction_full 0.722
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.447
_diffrn_reflns_theta_min         3.192
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.889
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.6254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1038 before and 0.0601 after correction. The Ratio of minimum to maximum transmission is 0.8323. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_description       block
_exptl_crystal_F_000             3380
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2047
_refine_ls_number_reflns         17292
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.2023
_refine_ls_R_factor_gt           0.1290
_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^)+(0.3200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3611
_refine_ls_wR_factor_ref         0.4344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10733
_reflns_number_total             17292
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05122d2.cif
_cod_data_source_block           H2L_ClO4_2
_cod_depositor_comments
'Adding full bibliography for 7121928--7121931.cif.'
_cod_original_cell_volume        6625.7(11)
_cod_database_code               7121929
_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) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O37) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O48) \\sim Ueq, Uanis(O49)
\\sim Ueq, Uanis(O55) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3. Others
 Sof(O50')=1-FVAR(1)
 Sof(O50)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C02Q(H02Q), C02R(H02R), C02S(H02S), C02T(H02T), C02X(H02X), C03A(H03A),
 C03F(H03F), C03G(H03G), C03N(H03N), C04K(H04K), C031(H031), C035(H035),
 C02V(H02V), C03C(H03Q), C03O(H03T), C04C(H04I), C04F(H04J), C047(H047),
 C03T(H03W), C04A(H04R), C05E(H05K), C05F(H05L), C05Y(H05Y), C049(H049)
4.b Secondary CH2 refined with riding coordinates:
 C03B(H03B,H03C), C03I(H03D,H03E), C03P(H03H,H03I), C03Q(H03J,H03K), C03S(H03L,
 H03M), C04B(H04A,H04B), C04E(H04C,H04D), C05R(H05A,H05B), C038(H03O,H03P),
 C044(H04E,H04F), C046(H04G,H04H), C055(H05C,H05D), C03M(H03R,H03S), C04J(H04L,
 H04M), C04O(H04N,H04O), C05L(H05E,H05F), C041(H04P,H04Q), C059(H05G,H05H),
 C03K(H03U,H03V), C03Y(H03X,H03Y), C04G(H04S,H04T), C05D(H05I,H05J), C05X(H05M,
 H05N), C050(H05O,H05P), C04V(H04,H), C042(H1AA,HA), C056(H2AA,HB), C03H(H03Z,
 HC), C04U(H04W,H04X), C05J(H05S,H05T), C05N(H05U,H05V), C05V(H05W,H05X),
 C052(H05Z,HD), C04N(H4AA,HE), C05A(H5AA,HF), C05M(H6AA,HG)
4.c Aromatic/amide H refined with riding coordinates:
 C04P(H04Y), C04S(H04Z), C05B(H05), C05C(H0AA), C04Q(H04U), C04T(H04V),
 C05G(H05Q), C05H(H05R), C051(H051), C053(H053), C058(H058), C060(H060),
 C04L(H3AA), C05S(H7AA), C05W(H8AA), C054(H054)
4.d Idealised tetrahedral OH refined as rotating group:
 O4(H4), O6(H6)
;
_shelx_res_checksum              36957
_olex2_submission_special_instructions 'No special instructions were received'