Guest-dependent directional complexation based on triptycene derived oxacalixarene: formation of oriented rotaxanes
Wang, Han-Xiao; Meng, Zheng; Xiang, Jun-Feng; Xia, Yu-Xiang; Sun, Yihua; Hu, Shu-Zhen; Chen, Hui; Yao, Jiannian; Chen, Chuan-Feng; Chem. Sci. 7 (2016) 469–; doi:10.1039/C5SC03511B

data_1534394
_publ_section_title
;
 Guest-dependent directional complexation based on triptycene derived
 oxacalixarene: formation of oriented rotaxanes
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              469
_journal_paper_doi               10.1039/C5SC03511B
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety
'C56 H32 N4 O4, C43 H58 N2 O2, 2(F6 P), 7(C H Cl3)'
_chemical_formula_sum            'C106 H97 Cl21 F12 N6 O6 P2'
_chemical_formula_weight         2585.28
_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
_audit_creation_date             2014-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2014-06-24 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                103.44(3)
_cell_angle_beta                 93.42(3)
_cell_angle_gamma                103.76(3)
_cell_formula_units_Z            2
_cell_length_a                   11.354(2)
_cell_length_b                   17.925(4)
_cell_length_c                   30.835(6)
_cell_measurement_reflns_used    18514
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4815
_cell_measurement_theta_min      1.2093
_cell_volume                     5884(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2013)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2013)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2013)'
_computing_structure_solution
;
 'XS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0107
_diffrn_orient_matrix_UB_12      -0.0791
_diffrn_orient_matrix_UB_13      0.0445
_diffrn_orient_matrix_UB_21      0.0360
_diffrn_orient_matrix_UB_22      -0.0173
_diffrn_orient_matrix_UB_23      -0.0452
_diffrn_orient_matrix_UB_31      0.0191
_diffrn_orient_matrix_UB_32      0.0152
_diffrn_orient_matrix_UB_33      0.0231
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0874
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            52898
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         0.684
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.62411
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       plate
_exptl_crystal_F_000             2636
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.817
_refine_diff_density_rms         0.081
_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     1560
_refine_ls_number_reflns         26219
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1317
_refine_ls_R_factor_gt           0.1055
_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^)+(0.1179P)^2^+6.6460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2671
_refine_ls_wR_factor_ref         0.2908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19728
_reflns_number_total             26219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03511b2.cif
_cod_data_source_block           mx2966a
_cod_depositor_comments
'Adding full bibliography for 1534393--1534395.cif.'
_cod_original_cell_volume        5885(2)
_cod_database_code               1534394
_shelxl_version_number           2013-4
_diffrn_number_total             26221
_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
 C93A-C92 = C94-C92 = C94A-C92
 1.54 with sigma of 0.01
 Cl0A-C102 = Cl1-C102 = Cl3A-C102 = Cl3-C102 = Cl2-C102 = Cl2A-C102
 1.76 with sigma of 0.01
 Cl1D-C1B = Cl1C-C1B = Cl1E-C1B = Cl19-C105 = Cl21-C105 = Cl20-C105
 1.76 with sigma of 0.01
 Cl7-C101 = Cl7A-C1C = Cl8A-C1C = Cl8-C101 = Cl9-C101 = Cl9A-C1C
 1.76 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl13 \\sim Cl15 \\sim C104 \\sim C1A \\sim Cl \\sim Cl1A \\sim Cl1B \\sim Cl14
\\sim C93 \\sim C94 \\sim C95 \\sim C94A \\sim C93A \\sim C95A \\sim Cl2 \\sim
Cl3 \\sim C102 \\sim Cl3A \\sim Cl2A \\sim Cl1 \\sim Cl0A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.04
Cl19 \\sim Cl20 \\sim Cl21 \\sim C105 \\sim Cl1C \\sim Cl1D \\sim Cl1E \\sim
C1B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Cl7 \\sim Cl8 \\sim Cl9 \\sim C101 \\sim C1C \\sim Cl7A \\sim Cl9A \\sim Cl8A:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(Cl3) \\sim Ueq, Uanis(Cl3A) \\sim Ueq, Uanis(C102) \\sim Ueq, Uanis(Cl2A)
\\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl0A) \\sim Ueq, Uanis(Cl2) \\sim Ueq,
Uanis(C95) \\sim Ueq, Uanis(C93A) \\sim Ueq, Uanis(C94A) \\sim Ueq, Uanis(C94)
\\sim Ueq, Uanis(C95A) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(Cl13) \\sim Ueq,
Uanis(Cl15) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(Cl)
\\sim Ueq, Uanis(Cl14) \\sim Ueq, Uanis(Cl1B) \\sim Ueq, Uanis(Cl1A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl19) \\sim Ueq, Uanis(Cl20) \\sim Ueq, Uanis(Cl21) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(Cl1C) \\sim Ueq, Uanis(Cl1D) \\sim Ueq,
Uanis(Cl1E) \\sim Ueq, Uanis(C1B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl7) \\sim Ueq, Uanis(Cl8) \\sim Ueq, Uanis(Cl9) \\sim Ueq, Uanis(C101)
\\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(Cl7A) \\sim Ueq, Uanis(Cl9A) \\sim Ueq,
Uanis(Cl8A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C1A)=Sof(H1A)=Sof(Cl)=Sof(Cl1A)=Sof(Cl1B)=1-FVAR(1)
 Sof(Cl13)=Sof(Cl14)=Sof(Cl15)=Sof(C104)=Sof(H104)=FVAR(1)
 Sof(H10A)=Sof(Cl3A)=Sof(Cl0A)=Sof(Cl2A)=1-FVAR(2)
 Sof(Cl1)=Sof(Cl2)=Sof(Cl3)=Sof(H102)=FVAR(2)
 Sof(C94A)=Sof(H94D)=Sof(H94E)=Sof(H94F)=Sof(C93A)=Sof(H93D)=Sof(H93E)=
 Sof(H93F)=Sof(C95A)=Sof(H95D)=Sof(H95E)=Sof(H95F)=1-FVAR(3)
 Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=Sof(C94)=Sof(H94A)=Sof(H94B)=Sof(H94C)=
 Sof(C95)=Sof(H95A)=Sof(H95B)=Sof(H95C)=FVAR(3)
 Sof(Cl1C)=Sof(Cl1D)=Sof(Cl1E)=Sof(C1B)=Sof(H1B)=1-FVAR(4)
 Sof(Cl19)=Sof(Cl20)=Sof(Cl21)=Sof(C105)=Sof(H105)=FVAR(4)
 Sof(C1C)=Sof(H1C)=Sof(Cl7A)=Sof(Cl9A)=Sof(Cl8A)=1-FVAR(5)
 Sof(Cl7)=Sof(Cl8)=Sof(Cl9)=Sof(C101)=Sof(H101)=FVAR(5)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C29(H29), C32(H32), C104(H104), C103(H103), C102(H102),
 C102(H10A), C106(H106), C101(H101), C105(H105), C100(H100), C1A(H1A), C1B(H1B),
  C1C(H1C)
5.b Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C11(H11), C13(H13), C14(H14), C16(H16),
 C17(H17), C21(H21), C22(H22), C24(H24), C25(H25), C28(H28), C33(H33), C34(H34),
  C35(H35), C36(H36), C39(H39), C40(H40), C42(H42), C44(H44), C45(H45),
 C49(H49), C50(H50), C52(H52), C53(H53), C56(H56), C58(H58), C60(H60), C62(H62),
  C72(H72), C73(H73), C75(H75), C76(H76), C78(H78), C79(H79), C80(H80),
 C81(H81), C87(H87), C89(H89), C91(H91)
5.d Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C93(H93A,H93B,H93C), C94(H94A,
 H94B,H94C), C95(H95A,H95B,H95C), C97(H97A,H97B,H97C), C98(H98A,H98B,H98C),
 C99(H99A,H99B,H99C), C94A(H94D,H94E,H94F), C93A(H93D,H93E,H93F), C95A(H95D,
 H95E,H95F)
;
_shelx_res_checksum              49493
_shelx_hkl_checksum              16325