[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_7220171
_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         'F6 P, C37 H45 N O14, C7 H9 N, C2 H3 N, H2 O'
_chemical_formula_sum            'C46 H59 F6 N3 O15 P'
_chemical_formula_weight         1038.93
_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             2014-05-08
_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                101.306(4)
_cell_angle_beta                 99.715(4)
_cell_angle_gamma                94.513(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9381(5)
_cell_length_b                   11.7474(7)
_cell_length_c                   19.8477(9)
_cell_measurement_reflns_used    3398
_cell_measurement_temperature    170.1
_cell_measurement_theta_max      29.5932
_cell_measurement_theta_min      2.9889
_cell_volume                     2448.4(2)
_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  'ShelXL (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      -0.0249641000
_diffrn_orient_matrix_UB_12      0.0502574000
_diffrn_orient_matrix_UB_13      0.0157963000
_diffrn_orient_matrix_UB_21      -0.0343277000
_diffrn_orient_matrix_UB_22      -0.0347147000
_diffrn_orient_matrix_UB_23      0.0174854000
_diffrn_orient_matrix_UB_31      0.0508470000
_diffrn_orient_matrix_UB_32      0.0105758000
_diffrn_orient_matrix_UB_33      0.0286671000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15160
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.99
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65760
_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    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         8937
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.1174
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1816
_refine_ls_wR_factor_ref         0.2234
_reflns_number_gt                5447
_reflns_number_total             8937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra06927k2.cif
_cod_data_source_block           140507_ljy_046_b_g4
_cod_database_code               7220171
_chemical_oxdiff_formula         'c10 h10 n2 o8 p1 f6'
_reflns_odcompleteness_completeness 99.64
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C44-C40
 1.51 with sigma of 0.02
 C40-C44A
 1.51 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C44) = Uanis(C44A)
4. Others
 Sof(H33C)=Sof(H33D)=Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C34A)=Sof(H34C)=
 Sof(H34D)=Sof(O12A)=1-FVAR(1)
 Sof(O12)=Sof(H33A)=Sof(H33B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C34)=Sof(H34A)=
 Sof(H34B)=FVAR(1)
 Sof(C44A)=Sof(H44C)=Sof(H44D)=1-FVAR(2)
 Sof(C44)=Sof(H44A)=Sof(H44B)=FVAR(2)
5.a Free rotating group:
 O15(H15C,H15D)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C14(H14A,H14B), C28(H28A,H28B), C21(H21A,H21B), C19(H19A,
 H19B), C20(H20A,H20B), C18(H18A,H18B), C16(H16A,H16B), C15(H15A,H15B),
 C31(H31A,H31B), C7(H7A,H7B), C17(H17A,H17B), C37(H37A,H37B), C36(H36A,H36B),
 C33(H33A,H33B), C33(H33C,H33D), C32(H32A,H32B), C35(H35A,H35B), C34(H34A,H34B),
  C44(H44A,H44B), C35A(H35C,H35D), C34A(H34C,H34D), C44A(H44C,H44D)
5.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C11(H11), C9(H9), C23(H23), C26(H26), C12(H12), C2(H2), C3(H3),
 C4(H4), C42(H42), C38(H38), C41(H41), C39(H39)
5.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C46(H46A,H46B,H46C)
;