Temperature-induced large amplitude conformational change in the complex of oxatub[4]arene revealed via rotaxane synthesis
Li, Dong-Hao; Yang, Liu-Pan; Chai, Hongxin; Jia, Fei; Ke, Hua; Jiang, Wei; Organic Chemistry Frontiers 6 (2019) 1027–; doi:10.1039/C9QO00159J

data_1554754
_publ_section_title
;
 Temperature-induced large amplitude conformational change in the complex
 of oxatub[4]arene revealed via rotaxane synthesis
;
_journal_issue                   7
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1027
_journal_paper_doi               10.1039/C9QO00159J
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C80 H104 O12, C28 H42 N2 O4, 2(F6 P), 2(H2 O)'
_chemical_formula_sum            'C108 H150 F12 N2 O18 P2'
_chemical_formula_weight         2054.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2019-02-22 deposited with the CCDC.	2019-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.616(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6358(9)
_cell_length_b                   25.0174(12)
_cell_length_c                   26.0640(13)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    100
_cell_measurement_theta_max      65.93
_cell_measurement_theta_min      2.52
_cell_volume                     10832.1(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            244296
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.127
_diffrn_reflns_theta_max         67.127
_diffrn_reflns_theta_min         2.521
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.6233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0994 before and 0.0732 after correction. The Ratio of minimum to maximum transmission is 0.8279. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_description       block
_exptl_crystal_F_000             4376
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.236
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         18969
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+10.1705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1741
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16293
_reflns_number_total             18969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00159j2.cif
_cod_data_source_block           cxy614_0m
_cod_database_code               1554754
_shelx_shelxl_version_number     2016/6
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C75A-C74A = C75-C74 = C75A-C76A = C76-C75
 1.53 with sigma of 0.02
 C74A-C76A = C76-C74
 2.52 with sigma of 0.04
 C75A-C73
 2.52 with sigma of 0.04
 C75-C73
 2.52 with sigma of 0.04
 H18D-H95A
 2.56 with sigma of 0.04
 H18D-H93B
 2.78 with sigma of 0.04
 P2A-F19 \\sim P2A-F18 \\sim P2A-F21 \\sim P2A-F20 \\sim P2A-F17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F10) = Uanis(F19)
Uanis(F11) = Uanis(F20)
Uanis(F12) = Uanis(F21)
Uanis(F9) = Uanis(F18)
Uanis(F3) = Uanis(F16)
Uanis(F6) = Uanis(F15)
Uanis(F4) = Uanis(F13)
Uanis(F5) = Uanis(F14)
Uanis(P2) = Uanis(P2A)
Uanis(F8) = Uanis(F17)
Uanis(C74) = Uanis(C74A)
Uanis(C75) = Uanis(C75A)
Uanis(C76) = Uanis(C76A)
4. Others
 Sof(P2A)=Sof(F17)=Sof(F18)=Sof(F19)=Sof(F20)=Sof(F21)=1-FVAR(1)
 Sof(P2)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=1-FVAR(2)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74C)=Sof(H74D)=Sof(C75A)=Sof(H75C)=
 Sof(H75D)=Sof(C76A)=Sof(H76D)=Sof(H76E)=Sof(H76F)=1-FVAR(3)
 Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(C75)=Sof(H75A)=Sof(H75B)=
 Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=FVAR(3)
5.a Free rotating group:
 O17(H17C,H17D), O18(H18C,H18D)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,
 H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C31(H31A,H31B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C57(H57A,H57B), C58(H58A,H58B),
 C59(H59A,H59B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C73(H73C,H73D),
  C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C74(H74A,H74B), C75(H75A,
 H75B), C74A(H74C,H74D), C75A(H75C,H75D), C82(H82A,H82B), C84(H84A,H84B),
 C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
  C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C105(H10A,H10B), C107(H10F,
 H10G)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C23(H23), C24(H24), C28(H28), C29(H29),
 C43(H43), C44(H44), C48(H48), C49(H49), C63(H63), C64(H64), C68(H68), C69(H69),
  C85(H85), C87(H87), C89(H89), C100(H100), C102(H102), C104(H104)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C36(H36A,H36B,H36C), C40(H40A,H40B,
 H40C), C56(H56A,H56B,H56C), C60(H60A,H60B,H60C), C80(H80A,H80B,H80C), C76(H76A,
 H76B,H76C), C76A(H76D,H76E,H76F), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C),
 C106(H10C,H10D,H10E), C108(H10H,H10I,H10J)
;
_olex2_submission_special_instructions 'No special instructions were received'