Convergent heteroditopic cyclo[6]aramides as macrocyclic ion-pair receptors for constructing [2]pseudorotaxanes
Jinchuan Hu; Long Chen; Jie Shen; Jian Luo; Pengchi Deng; Yi Ren; Huaqiang Zeng; Wen Feng; Lihua Yuan; Chem.Commun. 50 (2014) 8024–; doi:10.1039/C4CC02557A

data_7115301
_publ_section_title
;
 Convergent heteroditopic cyclo[6]aramides as macrocyclic ion-pair
 receptors for constructing [2]pseudorotaxanes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8024
_journal_paper_doi               10.1039/C4CC02557A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety
'Cl, 2(C H2 Cl2), C71 H88 N6 O15, H2 O, C8 H20 N'
_chemical_formula_sum            'C81 H114 Cl5 N7 O16'
_chemical_formula_weight         1619.04
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.044(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3283(4)
_cell_length_b                   24.6571(4)
_cell_length_c                   23.0091(5)
_cell_measurement_reflns_used    11647
_cell_measurement_temperature    143.00(10)
_cell_measurement_theta_max      28.9030
_cell_measurement_theta_min      3.1970
_cell_volume                     8314.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      143.00(10)
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.9980
_diffrn_measured_fraction_theta_max 0.8642
_diffrn_measurement_details
;
  1 omega  -86.00    5.20   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5174  -38.0000  150.0000 114

  2 omega  -90.00    3.60   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5174  -38.0000 -120.0000 117

  3 omega  -19.00   17.00   0.8000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.5174  -99.0000   30.0000 45
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0435049000
_diffrn_orient_matrix_UB_12      -0.0011488000
_diffrn_orient_matrix_UB_13      -0.0049619000
_diffrn_orient_matrix_UB_21      0.0211975000
_diffrn_orient_matrix_UB_22      0.0038115000
_diffrn_orient_matrix_UB_23      0.0315501000
_diffrn_orient_matrix_UB_31      0.0010704000
_diffrn_orient_matrix_UB_32      -0.0284904000
_diffrn_orient_matrix_UB_33      0.0043989000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35769
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.898
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_F_000             3448
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.305
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         16968
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+8.7136P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1869
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12536
_reflns_number_total             16968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02557a2.cif
_cod_data_source_block           131031_s1_hjc
_cod_database_code               7115301
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         c12h20n2o3cl2
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.931
_reflns_odcompleteness_completeness 99.80
_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 N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B)
2.b Ternary CH refined with riding coordinates:
 C45(H45), C50(H50), C57(H57), C62(H62), C69(H69)
2.c Secondary CH2 refined with riding coordinates:
 N7(H7A,H7B), C43(H43A,H43B), C44(H44A,H44B), C48(H48A,H48B), C49(H49A,H49B),
 C55(H55A,H55B), C56(H56A,H56B), C60(H60A,H60B), C61(H61A,H61B), C67(H67A,H67B),
  C68(H68A,H68B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C76(H76A,
 H76B), C77(H77A,H77B), C78(H78A,H78B), C80(H80A,H80B), C81(H81A,H81B)
2.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), C1(H1A), C3(H3A), C5(H5A),
 C9(H9), C10(H10), C13(H13), C17(H17), C20(H20), C24(H24), C27(H27), C31(H31),
 C34(H34), C38(H38), C39(H39), C41(H41)
2.e Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C59(H59A,
 H59B,H59C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C75(H75A,H75B,
 H75C), C79(H79A,H79B,H79C)
;
_shelx_res_checksum              88902