[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_7220172
_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         'C37 H45 N O14, C14 H16 N2, 2(F6 P), C2 H3 N'
_chemical_formula_sum            'C53 H64 F12 N4 O14 P2'
_chemical_formula_weight         1271.02
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-05-07
_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                90.00
_cell_angle_beta                 98.733(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   54.999(2)
_cell_length_b                   11.2922(4)
_cell_length_c                   19.9536(9)
_cell_measurement_reflns_used    7569
_cell_measurement_temperature    170.1
_cell_measurement_theta_max      29.4923
_cell_measurement_theta_min      3.0745
_cell_volume                     12248.7(8)
_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 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0075924000
_diffrn_orient_matrix_UB_12      -0.0170225000
_diffrn_orient_matrix_UB_13      0.0240808000
_diffrn_orient_matrix_UB_21      0.0066571000
_diffrn_orient_matrix_UB_22      0.0384363000
_diffrn_orient_matrix_UB_23      0.0242706000
_diffrn_orient_matrix_UB_31      -0.0082628000
_diffrn_orient_matrix_UB_32      0.0466522000
_diffrn_orient_matrix_UB_33      -0.0111842000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_limit_h_max       66
_diffrn_reflns_limit_h_min       -63
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23172
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.08
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88686
_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    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             5280
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.438
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         11014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0884
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1672P)^2^+31.9460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2631
_refine_ls_wR_factor_ref         0.2919
_reflns_number_gt                8007
_reflns_number_total             11014
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra06927k2.cif
_cod_data_source_block           140506_ljy_046_b_g10
_cod_original_cell_volume        12248.8(9)
_cod_database_code               7220172
_chemical_oxdiff_formula         'c10 h10 n2 O8 p1 F1'
_reflns_odcompleteness_completeness 97.44
_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. Others
 Fixed Sof: P3(0.5) F13(0.5) F14(0.5) F15(0.5) F16(0.5) F17(0.5) F18(0.5)
 P2(0.5) F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C28(H28A,H28B),
  C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C11(H11), C12(H12), C23(H23), C24(H24),
 C26(H26), C38(H38), C39(H39), C41(H41), C42(H42), C44(H44), C45(H45), C47(H47),
  C48(H48), C49(H49), C50(H50)
3.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C)
;