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_7121928
_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 N14 Np O13, C18 H18 N12 O6, Cl O4, H2 O'
_chemical_formula_sum            'C54 H60 Cl N26 Np O24'
_chemical_formula_weight         1729.73
_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                73.052(2)
_cell_angle_beta                 82.550(2)
_cell_angle_gamma                67.868(2)
_cell_formula_units_Z            2
_cell_length_a                   15.2162(9)
_cell_length_b                   15.3864(9)
_cell_length_c                   15.6650(9)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.495
_cell_measurement_theta_min      3.05
_cell_volume                     3248.9(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            83878
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         2.916
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0609 before and 0.0518 after correction. The Ratio of minimum to maximum transmission is 0.9414. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'yellow green'
_exptl_crystal_colour_modifier   yellow
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.178
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         14959
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+8.6489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13448
_reflns_number_total             14959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc05122d2.cif
_cod_data_source_block           NRCP1
_cod_depositor_comments
'Adding full bibliography for 7121928--7121931.cif.'
_cod_database_code               7121928
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.630
_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(O19) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Free rotating group:
 O2W(H2WA,H2WB)
3.b Rotating group:
 O1W(H1WA,H1WB)
3.c Ternary CH refined with riding coordinates:
 C01K(H01K), C02J(H02J), C02L(H02L), C02M(H02M), C023(H023), C025(H025),
 C01H(H01H), C01W(H01W), C01Z(H01Z), C02A(H02I), C02K(H02O), C021(H021)
3.d Secondary CH2 refined with riding coordinates:
 C01F(H01A,H01B), C01X(H01C,H01D), C02R(H02A,H02B), C02T(H02C,H02D), C024(H02E,
 H02F), C028(H02G,H02H), C01Y(H01M,H01N), C02B(H02T,H02U), C02C(H02V,H02W),
 C02P(H02Z,H), C02S(H02,HA), C020(H0AA,HB), C01M(H01E,H01F), C01S(H01G,H01I),
 C01V(H01J,H01L), C02G(H02K,H02N), C02N(H02P,H02Q), C02Q(H02R,H02S)
3.e Aromatic/amide H refined with riding coordinates:
 C01O(H01O), C01P(H01P), C01T(H01T), C01U(H01U), C02F(H02X), C02O(H02Y),
 C026(H026), C029(H029)
;
_shelx_res_checksum              4762
_shelx_fab_checksum              535
_olex2_submission_special_instructions 'No special instructions were received'