Formation of a 'pseudosuitane'-type complex between a triptycene-derived bis(crown ether) host and 1,1'-(anthracene-9,10-diyl)bis(N-benzylmethanaminium): a new method for the synthesis of linear polyrotaxanes
Fei Zeng; Zheng Meng; Ying Han; Chuan-Feng Chen; Chem.Commun. 50 (2014) 7611–; doi:10.1039/C4CC02904F

data_7114665
_publ_section_title
;
 Formation of a 'pseudosuitane'-type complex between a triptycene-derived
 bis(crown ether) host and
 1,1'-(anthracene-9,10-diyl)bis(N-benzylmethanaminium): a new method for
 the synthesis of linear polyrotaxanes
;
_journal_name_full               Chem.Commun.
_journal_page_first              7611
_journal_paper_doi               10.1039/C4CC02904F
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '2(F6 P), C58 H70 O16, C2 H3 N, C30 H30 N2'
_chemical_formula_sum            'C90 H103 F12 N3 O16 P2'
_chemical_formula_weight         1772.69
_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             2014-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.404(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.115(4)
_cell_length_b                   34.605(11)
_cell_length_c                   20.873(7)
_cell_measurement_reflns_used    25251
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4781
_cell_measurement_theta_min      0.9919
_cell_volume                     8607(5)
_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, 2013)'
_computing_structure_solution
;
'XS (Sheldrick, 2013)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.999
_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      0.0254
_diffrn_orient_matrix_UB_12      -0.0747
_diffrn_orient_matrix_UB_13      0.0287
_diffrn_orient_matrix_UB_21      -0.0235
_diffrn_orient_matrix_UB_22      -0.0124
_diffrn_orient_matrix_UB_23      -0.0114
_diffrn_orient_matrix_UB_31      0.0265
_diffrn_orient_matrix_UB_32      -0.0154
_diffrn_orient_matrix_UB_33      -0.0378
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.1200
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49058
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         1.539
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             3720
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.236
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         15487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_R_factor_all          0.1736
_refine_ls_R_factor_gt           0.1404
_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^)+(0.0629P)^2^+18.8824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2804
_refine_ls_wR_factor_ref         0.2996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11821
_reflns_number_total             15487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02904f2.cif
_cod_data_source_block           mx2937
_cod_database_code               7114665
_shelxl_version_number           2013-4
_diffrn_number_total             19953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
  N1(H1A,H1B), N2(H2A,H2B), C65(H65A,H65B), C66(H66A,H66B), C81(H81A,H81B),
 C82(H82A,H82B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C21(H21), C24(H24), C27(H27), C28(H28),
 C29(H29), C30(H30), C37(H37), C40(H40), C54(H54), C55(H55), C56(H56), C57(H57),
  C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C69(H69), C70(H70),
 C71(H71), C72(H72), C76(H76), C77(H77), C78(H78), C79(H79), C84(H84), C85(H85),
  C86(H86), C87(H87), C88(H88)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C89(H89A,H89B,H89C)
;
_shelx_res_checksum              85872