Cooperative Silver Ion-Pair Recognition by Peralkylated Pillar[5]arenes.
Hua, Bin; Shao, Li; Zhang, Zhihua; Liu, Jiyong; Huang, Feihe; Journal of the American Chemical Society 141 (2019) 15008–15012; doi:10.1021/jacs.9b08257

data_4128966
_publ_section_title
;
 Cooperative Silver Ion-Pair Recognition by Peralkylated Pillar[5]arenes.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15008
_journal_page_last               15012
_journal_paper_doi               10.1021/jacs.9b08257
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'Ag2 C4 F6 O4, C55 H70 O10'
_chemical_formula_sum            'C59 H70 Ag2 F6 O14'
_chemical_formula_weight         1332.89
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.654(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5674(6)
_cell_length_b                   20.0237(9)
_cell_length_c                   17.9980(6)
_cell_measurement_reflns_used    6167
_cell_measurement_temperature    164.7
_cell_measurement_theta_max      29.4417
_cell_measurement_theta_min      2.9329
_cell_volume                     5964.3(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      164.7
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -37.00   62.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   38.0000   30.0000 99

  2 omega  -72.00   15.00   1.0000   90.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683  -38.0000 -150.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0268398000
_diffrn_orient_matrix_UB_12      0.0177569000
_diffrn_orient_matrix_UB_13      -0.0224203000
_diffrn_orient_matrix_UB_21      0.0221107000
_diffrn_orient_matrix_UB_22      -0.0297598000
_diffrn_orient_matrix_UB_23      -0.0055544000
_diffrn_orient_matrix_UB_31      -0.0250798000
_diffrn_orient_matrix_UB_32      -0.0072858000
_diffrn_orient_matrix_UB_33      -0.0319792000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17069
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        20.815
_diffrn_reflns_theta_max         20.815
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   analytical
_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)
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)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.5106
_exptl_crystal_size_mid          0.2415
_exptl_crystal_size_min          0.1654
_refine_diff_density_max         1.392
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         6203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0652P)^2^+14.0870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5017
_reflns_number_total             6203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08257_si_002.cif
_cod_data_source_block           171219_hb_p5_ag_abs
_cod_database_code               4128966
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C59H70Ag2F6O14
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.704
_reflns_odcompleteness_completeness 99.51
_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
2. Uiso/Uaniso restraints and constraints
Uanis(Ag1) = Uanis(Ag1A)
3. Others
 Sof(Ag2A)=Sof(O14A)=Sof(O12A)=1-FVAR(1)
 Sof(O12)=Sof(O14)=Sof(Ag2)=FVAR(1)
 Sof(Ag1A)=1-FVAR(2)
 Sof(Ag1)=FVAR(2)
 Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(3)
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(3)
 Sof(F6A)=Sof(F5A)=Sof(F4A)=1-FVAR(4)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C19(H19A,H19B),
 C21(H21A,H21B), C21(H21C,H21D), C23(H23A,H23B), C30(H30A,H30B), C32(H32A,H32B),
  C34(H34A,H34B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B), C52(H52A,
 H52B), C54(H54A,H54B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C14(H14), C17(H17), C25(H25), C28(H28), C36(H36), C39(H39),
 C47(H47), C50(H50)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              81547
_shelx_hkl_checksum              10371
_olex2_submission_special_instructions 'No special instructions were received'