Threading of three rings on two stations: a convergent approach to [4]rotaxane
Zhou, Yidan; Wu, Jinyang; Liu, Zejiang; Xu, Weitao; Liu, Menglong; Jia, Along; Liu, Yuchen; Xiao, Xin; Li, Xiaowei; Yuan, Lihua; Chemical Communications  (2021) –; doi:10.1039/D1CC05501A

data_7129295
_publ_section_title
;
 Threading of three rings on two stations: a convergent approach to
 [4]rotaxane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05501A
_journal_year                    2021
_chemical_formula_moiety
'4(C2 H4 Cl2), 2(F6 P), 3(C80 H108 N8 O12), C18 H26 N2'
_chemical_formula_sum            'C266 H366 Cl8 F12 N26 O36 P2'
_chemical_formula_weight         5077.37
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-09-22 deposited with the CCDC.	2021-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                91.639(3)
_cell_angle_beta                 93.853(3)
_cell_angle_gamma                114.363(4)
_cell_formula_units_Z            1
_cell_length_a                   18.4426(7)
_cell_length_b                   19.7321(7)
_cell_length_c                   20.3347(9)
_cell_measurement_reflns_used    14024
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.6400
_cell_measurement_theta_min      4.2870
_cell_volume                     6712.9(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  angilent
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37631
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        66.008
_diffrn_reflns_theta_max         66.008
_diffrn_reflns_theta_min         3.277
_exptl_absorpt_coefficient_mu    1.538
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             2706
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.201
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1723
_refine_ls_number_reflns         23038
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0950P)^2^+6.4064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1739
_refine_ls_wR_factor_ref         0.1928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17757
_reflns_number_total             23038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05501a2.cif
_cod_data_source_block           1
_cod_database_code               7129295
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.825
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C78A-C80A
 1.5 with sigma of 0.02
 C78A-C79A
 1.5 with sigma of 0.02
 C78-C79
 1.5 with sigma of 0.02
 C78-C80
 1.5 with sigma of 0.02
 C77-C78
 1.5 with sigma of 0.02
 C80-C78
 1.5 with sigma of 0.02
 C108-C109
 1.5 with sigma of 0.02
 C108-C110
 1.5 with sigma of 0.02
 C107-C108
 1.5 with sigma of 0.02
 C10C-C10E
 1.5 with sigma of 0.02
 C10C-C10D
 1.5 with sigma of 0.02
 C10B-C10C
 1.5 with sigma of 0.02
 C10B-C10A
 1.5 with sigma of 0.02
 C10A-O17
 1.45 with sigma of 0.02
 C103-C10K
 1.5 with sigma of 0.02
 C103-C105
 1.5 with sigma of 0.02
 C77A-C79A
 2.35 with sigma of 0.02
 C77A-C78A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C77A) \\sim Ueq, Uanis(C76A) \\sim Ueq,
Uanis(C78A) \\sim Ueq, Uanis(C80A) \\sim Ueq, Uanis(C79A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq,
Uanis(C110) \\sim Ueq, Uanis(C109) \\sim Ueq, Uanis(C10A) \\sim Ueq,
Uanis(C10B) \\sim Ueq, Uanis(C10E) \\sim Ueq, Uanis(C10C) \\sim Ueq,
Uanis(C10D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C10K) \\sim Ueq, Uanis(C105) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O14) = Uanis(O14A)
Uanis(O1A) = Uanis(O1)
Uanis(C105) = Uanis(C10K)
Uanis(C10C) = Uanis(C108)
4. Others
 Sof(H3AC)=Sof(H3AD)=Sof(Cl4A)=Sof(C1W)=Sof(H1WA)=Sof(H1WB)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(Cl4)=Sof(C0AA)=Sof(H0AB)=Sof(H0AC)=FVAR(1)
 Sof(C76A)=Sof(H76C)=Sof(H76D)=Sof(C77A)=Sof(H77C)=Sof(H77D)=Sof(C78A)=
 Sof(H78A)=Sof(C79A)=Sof(H79D)=Sof(H79E)=Sof(H79F)=Sof(C80A)=Sof(H80D)=
 Sof(H80E)=Sof(H80F)=1-FVAR(2)
 Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(C78)=Sof(H78)=
 Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=
 FVAR(2)
 Sof(C10A)=Sof(H10S)=Sof(H10T)=Sof(C10B)=Sof(H10U)=Sof(H10V)=Sof(C10C)=
 Sof(H10W)=Sof(C10D)=Sof(H10X)=Sof(H10Y)=Sof(H)=Sof(C10E)=Sof(H10Z)=Sof(HA)=
 Sof(HB)=1-FVAR(3)
 Sof(C106)=Sof(H10L)=Sof(H10M)=Sof(C107)=Sof(H10N)=Sof(H10O)=Sof(C108)=
 Sof(H108)=Sof(C109)=Sof(H10P)=Sof(H10Q)=Sof(H10R)=Sof(C110)=Sof(H11R)=
 Sof(H11S)=Sof(H11T)=FVAR(3)
 Sof(H10E)=Sof(C10K)=Sof(H0AA)=Sof(HC)=Sof(HD)=1-FVAR(4)
 Sof(H103)=Sof(C105)=Sof(H10I)=Sof(H10J)=Sof(H10K)=FVAR(4)
 Sof(O14A)=1-FVAR(5)
 Sof(O14)=FVAR(5)
 Sof(O1A)=1-FVAR(6)
 Sof(O1)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C43(H43), C48(H48), C53(H53), C58(H58), C63(H63), C68(H68), C73(H73),
 C78(H78), C78A(H78A), C103(H103), C103(H10E), C113(H113), C118(H118),
 C108(H108), C10C(H10W)
5.b Secondary CH2 refined with riding coordinates:
 C2BA(H2BA,H2BB), C3BA(H3BA,H3BB), C3AA(H3AA,H3AB), C3AA(H3AC,H3AD), C0AA(H0AB,
 H0AC), C1W(H1WA,H1WB), C41(H41A,H41B), C42(H42A,H42B), C46(H46A,H46B),
 C47(H47A,H47B), C51(H51A,H51B), C52(H52A,H52B), C56(H56A,H56B), C57(H57A,H57B),
  C61(H61A,H61B), C62(H62A,H62B), C66(H66A,H66B), C67(H67A,H67B), C71(H71A,
 H71B), C72(H72A,H72B), C76(H76A,H76B), C77(H77A,H77B), C76A(H76C,H76D),
 C77A(H77C,H77D), C101(H10A,H10B), C102(H10C,H10D), C111(H11A,H11B), C112(H11C,
 H11D), C116(H11K,H11L), C117(H11M,H11N), C106(H10L,H10M), C107(H10N,H10O),
 C10A(H10S,H10T), C10B(H10U,H10V), C126(H12D,H12E), C127(H12F,H12G), C128(H12H,
 H12I)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N5(H5), N6(H6), C4(H4), C5(H5A), C7(H7), C9(H9), C10(H10),
 C13(H13), C17(H17), C20(H20), C24(H24), C25(H25), C27(H27), C29(H29), C30(H30),
  C33(H33), C37(H37), C40(H40), N11(H11), N12(H12), C84(H84), C87(H87),
 C91(H91), C92(H92), C94(H94), C96(H96), C97(H97), C100(H100), C121(H121),
 C122(H122), C124(H124), C125(H125)
5.d Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C69(H69A,H69B,H69C),
 C70(H70A,H70B,H70C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C79A(H79D,H79E,H79F), C80A(H80D,H80E,H80F),
 C104(H10F,H10G,H10H), C114(H11E,H11F,H11G), C115(H11H,H11I,H11J), C119(H11O,
 H11P,H11Q), C120(H12A,H12B,H12C), C105(H10I,H10J,H10K), C109(H10P,H10Q,H10R),
 C110(H11R,H11S,H11T), C10D(H10X,H10Y,H), C10E(H10Z,HA,HB), C10K(H0AA,HC,HD),
 C129(H12J,H12K,H12L)
;
_shelx_res_checksum              58952
_olex2_submission_special_instructions 'No special instructions were received'