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_1534393
_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
'2(C H2 Cl2), 2(F6 P), C28 H38 N2 O, C56 H32 N4 O4'
_chemical_formula_sum            'C86 H74 Cl4 F12 N6 O5 P2'
_chemical_formula_weight         1703.25
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_audit_update_record
;
2014-06-24 deposited with the CCDC.
2015-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.044(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1928(19)
_cell_length_b                   21.893(4)
_cell_length_c                   32.961(6)
_cell_measurement_reflns_used    22542
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4753
_cell_measurement_theta_min      0.9301
_cell_volume                     8072(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., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
'XS (Sheldrick, 2008)' 
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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      0.0409
_diffrn_orient_matrix_UB_12      0.0739
_diffrn_orient_matrix_UB_13      -0.0291
_diffrn_orient_matrix_UB_21      0.0301
_diffrn_orient_matrix_UB_22      -0.0032
_diffrn_orient_matrix_UB_23      0.0342
_diffrn_orient_matrix_UB_31      0.0186
_diffrn_orient_matrix_UB_32      -0.0160
_diffrn_orient_matrix_UB_33      -0.0179
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            54637
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             3512
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         18426
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.1526
_refine_ls_R_factor_gt           0.1285
_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^)+(0.1126P)^2^+13.6909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3020
_refine_ls_wR_factor_ref         0.3181
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14464
_reflns_number_total             18426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03511b2.cif
_cod_data_source_block           mx2839
_cod_depositor_comments
'Adding full bibliography for 1534393--1534395.cif.'
_cod_database_code               1534393
_shelxl_version_number           2013-4
_diffrn_number_total             18911
_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) groups
2. Restrained distances
 O5A-C57 = O5-C57
 1.43 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O5 \\sim O5A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(O5A) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C78) \\sim Ueq, Uanis(C79A) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C80A)
\\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C78A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(H57C)=Sof(H57D)=Sof(O5A)=Sof(H5AA)=1-FVAR(1)
 Sof(O5)=Sof(H5A)=Sof(H57A)=Sof(H57B)=FVAR(1)
 Sof(C78A)=Sof(H78D)=Sof(H78E)=Sof(H78F)=Sof(C80A)=Sof(H80D)=Sof(H80E)=
 Sof(H80F)=Sof(C79A)=Sof(H79D)=Sof(H79E)=Sof(H79F)=1-FVAR(2)
 Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=
 Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C49(H49), C50(H50)
5.b Secondary CH2 refined with riding coordinates:
 C86(H86A,H86B), C85(H85A,H85B), C57(H57A,H57B), C57(H57C,H57D), C58(H58A,
 H58B), C59(H59A,H59B), C70(H70A,H70B)
5.c Aromatic/amide H refined with riding coordinates:
 C60(H60), C61(H61), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68),
 C69(H69), C72(H72), C74(H74), C76(H76), C2(H2), C3(H3), C5(H5), C6(H6),
 C10(H10), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C25(H25),
  C26(H26), C28(H28), C30(H30), C31(H31), C34(H34), C35(H35), C38(H38),
 C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C53(H53), C54(H54),
  C56(H56)
5.d Idealised Me refined as rotating group:
 C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C82(H82A,H82B,
 H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C78A(H78D,H78E,H78F),
 C80A(H80D,H80E,H80F), C79A(H79D,H79E,H79F)
5.e Idealised tetrahedral OH refined as rotating group:
 O5(H5A), O5A(H5AA)
;
_shelx_res_checksum              1564
_shelx_hkl_checksum              8646