[n]Pseudorotaxanes constructed by a bis(p-phenylene)-34-crown-10-based cryptand: different binding behaviors induced by minor structural changes of guests
Wang, Haoze; Wei, Peifa; Yan, Xuzhou; RSC Adv.  (2015) –; doi:10.1039/C5RA06927K

data_7220170
_publ_section_title
;
 [n]Pseudorotaxanes constructed by a bis(p-phenylene)-34-crown-10-based
 cryptand: different binding behaviors induced by minor structural changes
 of guests
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA06927K
_journal_year                    2015
_chemical_formula_moiety
'2(F6 P), C37 H44 N O14, C26 H26 N2, 2(C2 H3 N)'
_chemical_formula_sum            'C67 H76 F12 N5 O14 P2'
_chemical_formula_weight         1465.27
_chemical_name_systematic
;
 ? 
;
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2015-01-29 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                101.201(3)
_cell_angle_beta                 99.999(3)
_cell_angle_gamma                108.199(3)
_cell_formula_units_Z            4
_cell_length_a                   16.4730(6)
_cell_length_b                   21.0698(6)
_cell_length_c                   22.2668(7)
_cell_measurement_reflns_used    10614
_cell_measurement_temperature    170.1
_cell_measurement_theta_max      29.5026
_cell_measurement_theta_min      2.8824
_cell_volume                     6970.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXH-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.1
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0366385000
_diffrn_orient_matrix_UB_12      -0.0017371000
_diffrn_orient_matrix_UB_13      -0.0120061000
_diffrn_orient_matrix_UB_21      0.0082313000
_diffrn_orient_matrix_UB_22      -0.0206220000
_diffrn_orient_matrix_UB_23      0.0202908000
_diffrn_orient_matrix_UB_31      -0.0279805000
_diffrn_orient_matrix_UB_32      -0.0303777000
_diffrn_orient_matrix_UB_33      -0.0238706000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46173
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3052
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.332
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1805
_refine_ls_number_reflns         25454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1390
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1566P)^2^+6.2603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2476
_refine_ls_wR_factor_ref         0.2979
_reflns_number_gt                15140
_reflns_number_total             25454
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra06927k2.cif
_cod_data_source_block           140505_ljy_046_b_g5
_cod_database_code               7220170
_chemical_oxdiff_formula         'c10 h10 n2'
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C15(H15A,H15B), C16(H16A,H16B), C21(H21A,H21B), C22(H22A,
 H22B), C24(H24A,H24B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C34(H34A,H34B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B),
  C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B), C50(H50A,H50B), C51(H51A,
 H51B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C61(H61A,H61B),
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C69(H69A,H69B), C73(H73A,H73B),
  C75(H75A,H75B), C77(H77A,H77B), C79(H79A,H79B), C82(H82A,H82B), C83(H83A,
 H83B), C85(H85A,H85B), C89(H89A,H89B), C91(H91A,H91B), C98(H98A,H98B),
 C100(H10A,H10B), C106(H10C,H10D), C113(H11C,H11D), C121(H12A,H12B), C124(H12C,
 H12D)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C7(H7), C10(H10), C13(H13), C14(H14), C17(H17),
 C23(H23), C35(H35), C38(H38), C43(H43), C47(H47), C49(H49), C52(H52), C57(H57),
  C58(H58), C59(H59), C60(H60), C63(H63), C67(H67), C68(H68), C70(H70),
 C72(H72), C74(H74), C76(H76), C78(H78), C81(H81), C87(H87), C88(H88), C90(H90),
  C92(H92), C93(H93), C94(H94), C95(H95), C96(H96), C97(H97), C99(H99),
 C101(H101), C102(H102), C104(H104), C107(H107), C108(H108), C110(H110),
 C111(H111), C112(H112), C114(H114), C115(H115), C116(H116), C118(H118),
 C119(H119), C120(H120), C122(H122), C123(H123), C125(H125), C126(H126)
2.c Idealised Me refined as rotating group:
 C128(H12E,H12F,H12G), C129(H12H,H12I,H12J), C131(H13A,H13B,H13C), C133(H13D,
 H13E,H13F)
;