Facile synthesis of diverse rotaxanes via successive supramolecular transformations
Hu, Yang; Wang, Wei; Yao, Rui; Wang, Xu-Qing; Wang, Yu-Xuan; Sun, Bin; Chen, Li-Jun; Zhang, Ying; Zhao, Xiao-Li; Xu, Lin; Tan, Hong-Wei; Yu, Yihua; Li, Xiaopeng; Yang, Hai-Bo; Materials Chemistry Frontiers 3 (2019) 2397–; doi:10.1039/C9QM00430K

data_1554686
_publ_section_title
;
 Facile synthesis of diverse rotaxanes via successive supramolecular
 transformations
;
_journal_issue                   11
_journal_name_full               'Materials Chemistry Frontiers'
_journal_page_first              2397
_journal_paper_doi               10.1039/C9QM00430K
_journal_volume                  3
_journal_year                    2019
_chemical_formula_moiety         '2(C65 H90 O10), C88 H96 O8 P2 Pt'
_chemical_formula_sum            'C218 H276 O28 P2 Pt'
_chemical_formula_weight         3601.40
_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             2016-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2019-07-03 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                80.979(3)
_cell_angle_beta                 89.471(3)
_cell_angle_gamma                65.725(3)
_cell_formula_units_Z            1
_cell_length_a                   12.2995(12)
_cell_length_b                   12.7098(12)
_cell_length_c                   38.043(3)
_cell_measurement_reflns_used    7547
_cell_measurement_temperature    170
_cell_measurement_theta_max      19.17
_cell_measurement_theta_min      2.42
_cell_volume                     5344.1(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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
_diffrn_measured_fraction_theta_full 0.968
_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  0.1073
_diffrn_reflns_av_unetI/netI     0.1565
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            73645
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.086
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0901 before and 0.0657 after correction.
The Ratio of minimum to maximum transmission is 0.7164.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_F_000             1916
_refine_diff_density_max         2.579
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1089
_refine_ls_number_reflns         18724
_refine_ls_number_restraints     1328
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.1622
_refine_ls_R_factor_gt           0.1225
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3177
_refine_ls_wR_factor_ref         0.3454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12542
_reflns_number_total             18724
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qm00430k2.cif
_cod_data_source_block           z
_cod_original_cell_volume        5344.1(8)
_cod_database_code               1554686
_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 C(H,H,H) groups
2. Restrained distances
 C1B-C1A = C1E-C1B = C91-C1C = C103-C102 = C104-C103 = C89-C88 = C88-C87 = C79-
 C78 = C80-C79 = C77-C76 = C76-C75 = C66-C65 = C67-C66 = C50-C49 = C51-C50 =
 C53-C52 = C54-C53
 1.53 with sigma of 0.01
 O3-C1F
 1.48 with sigma of 0.02
 O4-C1D
 1.48 with sigma of 0.02
 C98-C1A = C1E-C1A = C90-C1C
 2.48 with sigma of 0.02
 O13-C98 = O13-C1A = O12-C90 = O12-C86 = O10-C75 = O10-C70 = O7-C65 = O7-C61
 1.48 with sigma of 0.02
 O13-C1B
 2.38 with sigma of 0.02
 O12-C91
 2.38 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim
C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73 \\sim C74 \\sim
C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81 \\sim C82 \\sim
C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim
C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98 \\sim
C102 \\sim C103 \\sim C104 \\sim C105 \\sim C107 \\sim C1 \\sim C2 \\sim C3
\\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim
C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim
C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42: within 2A with
sigma of 0.005 and sigma for terminal atoms of 0.01
C96 \\sim C95 \\sim C94 \\sim C93 \\sim C98 \\sim C97 \\sim O13 \\sim C1A \\sim
C1B \\sim C1E: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
C36 \\sim O2 \\sim C37 \\sim C42 \\sim C41 \\sim C40 \\sim C39 \\sim C38 \\sim
O3 \\sim C1F \\sim O4 \\sim C1D \\sim C35 \\sim C34: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
C86 \\sim O12 \\sim C90 \\sim C91 \\sim C1C: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq,
Uanis(C50) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C53)
\\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq,
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq,
Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq,
Uanis(C71) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C74)
\\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(C77) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81)
\\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq,
Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88)
\\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq,
Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C95)
\\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C98) \\sim Ueq,
Uanis(C102) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C45) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C98) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C1D) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Pt1(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C52(H52A,H52B), C53(H53A,H53B), C55(H55A,
 H55B), C62(H62A,H62B), C63(H63A,H63B), C65(H65A,H65B), C66(H66A,H66B),
 C68(H68A,H68B), C75(H75A,H75B), C76(H76A,H76B), C78(H78A,H78B), C79(H79A,H79B),
  C87(H87A,H87B), C88(H88A,H88B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,
 H92B), C102(H10A,H10B), C103(H10C,H10D), C105(H10H,H10I), C107(H10J,H10K),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
  C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C1A(H1AA,H1AB), C1B(H1BA,H1BB)
5.b Me refined with riding coordinates:
 C1D(H1DA,H1DB,H1DC)
5.c Aromatic/amide H refined with riding coordinates:
 C45(H45), C48(H48), C57(H57), C60(H60), C71(H71), C74(H74), C82(H82),
 C85(H85), C94(H94), C97(H97), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C22(H22), C23(H23), C25(H25), C26(H26), C39(H39), C40(H40), C41(H41)
5.d Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,C48), C81(C82,C83,C84,C85,C86), C93(C94,C95,C96,C97,C98),
 C37(C38,C39,C40,C41,C42)
5.e Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C54(H54A,H54B,H54C), C64(H64A,H64B,H64C), C67(H67A,H67B,
 H67C), C77(H77A,H77B,H77C), C80(H80A,H80B,H80C), C89(H89A,H89B,H89C),
 C104(H10E,H10F,H10G), C1C(H1CA,H1CB,H1CC), C1E(H1EA,H1EB,H1EC), C1F(H1FA,H1FB,
 H1FC)
;
_shelx_res_checksum              13175
_shelx_hkl_checksum              79353
_olex2_submission_special_instructions 'No special instructions were received'