Dimeric Resorcinarene Salt Capsules with Very Tight Encapsulation of Anions and Guest Molecules
Pan, Fangfang; Beyeh, N. Kodiah; Rissanen, Kari; RSC Adv.  (2015) –; doi:10.1039/C5RA11905G

data_7220895
_publ_section_title
;
 Dimeric Resorcinarene Salt Capsules with Very Tight Encapsulation of
 Anions and Guest Molecules
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA11905G
_journal_year                    2015
_chemical_formula_moiety
'C60 H88 N4 O8, 4(C F3 O3 S), 2(C4 H8 O2), 2(H2 O)'
_chemical_formula_sum            'C72 H108 F12 N4 O26 S4'
_chemical_formula_weight         1801.86
_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   mixed
_audit_creation_date             2014-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-05-19 deposited with the CCDC.
2015-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                69.135(7)
_cell_angle_beta                 67.660(7)
_cell_angle_gamma                67.136(8)
_cell_formula_units_Z            2
_cell_length_a                   16.3576(14)
_cell_length_b                   17.0042(13)
_cell_length_c                   18.5089(13)
_cell_measurement_reflns_used    7422
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.4660
_cell_measurement_theta_min      2.4200
_cell_volume                     4254.4(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -50.00   51.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.5946   77.0000 -180.0000 101

  2 omega  -24.00   40.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.5946   77.0000  -60.0000 64

  3 omega  -49.00   48.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.5946   77.0000  -90.0000 97

  4 omega  -49.00   -7.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -      -19.5946   77.0000 -120.0000 42

  5 omega   -8.00   91.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -       20.6883   77.0000  150.0000 99

  6 omega   31.00   89.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -       20.6883   77.0000   60.0000 58

  7 omega   -9.00   79.00   1.0000   47.5000
omega____ theta____ kappa____ phi______ frames
    -       20.6883   77.0000   30.0000 88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0025621000
_diffrn_orient_matrix_UB_12      -0.0293332000
_diffrn_orient_matrix_UB_13      0.0387289000
_diffrn_orient_matrix_UB_21      -0.0415732000
_diffrn_orient_matrix_UB_22      -0.0044911000
_diffrn_orient_matrix_UB_23      0.0005328000
_diffrn_orient_matrix_UB_31      0.0258686000
_diffrn_orient_matrix_UB_32      -0.0360445000
_diffrn_orient_matrix_UB_33      -0.0180454000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39947
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.026
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.3728
_exptl_crystal_size_mid          0.2503
_exptl_crystal_size_min          0.0924
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         15415
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+2.2874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1988
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9308
_reflns_number_total             15415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra11905g2.cif
_cod_data_source_block           2dioxane.2H2O_2@4.4OTf_2
_cod_original_cell_volume        4254.4(7)
_cod_database_code               7220895
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C40 H18 N4 O4 S4'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H4 of O4, All C(H,H) groups, All C(H,H,H,H) groups, All
  N(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H6 of O6, H7 of O7, H8 of O8, H1 of O1, H2 of O2, H3
  of O3, H5 of O5, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C71) \\sim Ueq, Uanis(C70) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(F11) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O20B) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O16) \\sim Ueq, Uanis(O19B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3. Others
 Sof(H3BC)=Sof(H3BD)=Sof(C38B)=Sof(H38B)=Sof(C39B)=Sof(H39C)=Sof(H39D)=
 Sof(C40B)=Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=Sof(C42B)=
 Sof(H42C)=Sof(H42D)=Sof(H43C)=Sof(H43D)=1-FVAR(1)
 Sof(H3AA)=Sof(H3AB)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H43A)=Sof(H43B)=FVAR(1)
 Sof(S4B)=Sof(F10B)=Sof(F11B)=Sof(F12B)=Sof(O18B)=Sof(O19B)=Sof(O20B)=
 Sof(C64B)=1-FVAR(2)
 Sof(S4)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(O18)=Sof(O19)=Sof(O20)=Sof(C64)=FVAR(2)
4.a Riding coordinates:
 O22(H22C,H22D)
4.b Free rotating group:
 O21(H21A,H21B)
4.c Rotating group:
 O4(H4)
4.d Ternary CH refined with riding coordinates:
 C8(H8A), C14(H14), C28(H28), C29(H29), C38(H38), C38B(H38B), C44(H44),
 C53(H53), C59(H59)
4.e Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3AA,H3AB), N3(H3BC,H3BD), N4(H4A,H4B), C7(H7A,
 H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,
 H13B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C37(H37A,H37B), C39(H39A,H39B), C39B(H39C,
 H39D), C40(H40A,H40B), C40B(H40C,H40D), C41(H41A,H41B), C41B(H41C,H41D),
 C42(H42A,H42B), C42B(H42C,H42D), C43(H43A,H43B), C43(H43C,H43D), C52(H52A,
 H52B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
 C58(H58A,H58B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B),
  C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B)
4.f Aromatic/amide H refined with riding coordinates:
 C6(H6A), C21(H21), C36(H36), C51(H51)
4.g Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C60(H60A,H60B,
 H60C)
4.h Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O5(H5), O6(H6), O7(H7), O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'