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_1534395
_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 H56 N O3, F6 P'
_chemical_formula_sum            'C99 H88 F6 N5 O7 P'
_chemical_formula_weight         1604.71
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-20 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   33.379(5)
_cell_length_b                   33.379(5)
_cell_length_c                   40.257(8)
_cell_measurement_reflns_used    71179
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      31.3162
_cell_measurement_theta_min      0.7922
_cell_volume                     44853(13)
_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., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 45.2618
              2theta: -20.0938
scan:
    Number of images: 268
               Slice: -80.0000 - 54.0000
         Image width: 0.5000
            Exp time: 10.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 45.2618
              2theta: -20.0938
;
_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       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0134
_diffrn_orient_matrix_UB_12      -0.0345
_diffrn_orient_matrix_UB_13      -0.0121
_diffrn_orient_matrix_UB_21      -0.0249
_diffrn_orient_matrix_UB_22      -0.0296
_diffrn_orient_matrix_UB_23      -0.0173
_diffrn_orient_matrix_UB_31      -0.0029
_diffrn_orient_matrix_UB_32      -0.0055
_diffrn_orient_matrix_UB_33      -0.0384
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            136082
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.198
_diffrn_reflns_theta_min         0.792
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    0.951
_exptl_crystal_description       block
_exptl_crystal_F_000             13472
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1057
_refine_ls_number_reflns         20189
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      2.025
_refine_ls_R_factor_all          0.1898
_refine_ls_R_factor_gt           0.1781
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4830
_refine_ls_wR_factor_ref         0.4905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17498
_reflns_number_total             20189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03511b2.cif
_cod_data_source_block           a_sq
_cod_depositor_comments
'Adding full bibliography for 1534393--1534395.cif.'
_cod_original_cell_volume        44854(16)
_cod_database_code               1534395
_shelxl_version_number           2013-4
_diffrn_number_total             91378
_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
 C99-C96 = C97-C96 = C98-C96 = C95-C92 = C93-C92 = C94-C92
 1.54 with sigma of 0.01
 C98-C90
 2.5 with sigma of 0.02
 C99-C96
 2.5 with sigma of 0.02
 C99-C98
 2.5 with sigma of 0.02
 C90-C97
 2.5 with sigma of 0.02
 C98-C97
 2.5 with sigma of 0.02
 C99-C97
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O6 \\sim O7 \\sim C85 \\sim C86 \\sim C87 \\sim C91 \\sim C92 \\sim C99: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O7) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C90)
\\sim Ueq, Uanis(C89) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C87) \\sim Ueq,
Uanis(C85) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C95)
\\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C98) \\sim Ueq,
Uanis(C94) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C97) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 C93(H93A,H93B,H93C), C94(H94A,H94B,H94C), C95(H95A,H95B,H95C), C97(H97A,H97B,
 H97C), C98(H98A,H98B,H98C), C99(H99A,H99B,H99C)
4.b Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C43(H43), C46(H46)
4.c Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C83(H83A,H83B), C84(H84A,H84B)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C14(H14), C19(H19),
 C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31),
  C33(H33), C34(H34), C38(H38), C41(H41), C42(H42), C47(H47), C48(H48),
 C50(H50), C53(H53), C54(H54), C55(H55), C56(H56), C66(H66), C68(H68), C70(H70),
  C72(H72), C73(H73), C75(H75), C76(H76), C78(H78), C79(H79), C81(H81),
 C82(H82), C91(H91), C89(H89), C87(H87)
4.e Fitted hexagon refined as free rotating group:
 C86(C91,C90,C89,C88,C87)
4.f Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              4882
_shelx_hkl_checksum              66220
_shelx_fab_checksum              92164
_olex2_submission_special_instructions 'No special instructions were received'