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_4128965
_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, C65 H90 O10'
_chemical_formula_sum            'C69 H90 Ag2 F6 O14'
_chemical_formula_weight         1473.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                104.4020(10)
_cell_angle_beta                 94.9610(10)
_cell_angle_gamma                111.9960(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1081(3)
_cell_length_b                   14.8255(3)
_cell_length_c                   21.7369(5)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.69
_cell_measurement_theta_min      2.42
_cell_volume                     3433.43(14)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42841
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.406
_diffrn_reflns_theta_max         24.406
_diffrn_reflns_theta_min         2.422
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0808 before and 0.0662 after correction.
The Ratio of minimum to maximum transmission is 0.9324.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.158
_refine_diff_density_max         2.954
_refine_diff_density_min         -1.627
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     844
_refine_ls_number_reflns         11238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0844P)^2^+10.4128P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9477
_reflns_number_total             11238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b08257_si_003.cif
_cod_data_source_block           181127_hb_pp5ag_0m
_cod_original_cell_volume        3433.42(14)
_cod_database_code               4128965
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.796
_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. Uiso/Uaniso restraints and constraints
Uanis(Ag2) = Uanis(Ag2A)
3. Others
 Sof(Ag1A)=1-FVAR(1)
 Sof(Ag1)=FVAR(1)
 Sof(Ag2A)=1-FVAR(2)
 Sof(Ag2)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B), C25(H25A,H25B),
  C27(H27A,H27B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,
 H38B), C40(H40A,H40B), C47(H47A,H47B), C48(H48A,H48B), C50(H50A,H50B),
 C51(H51A,H51B), C53(H53A,H53B), C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B),
  C64(H64A,H64B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C16(H16), C19(H19), C29(H29), C32(H32), C42(H42), C45(H45),
 C55(H55), C58(H58)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C), C26(H26A,H26B,
 H26C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C49(H49A,H49B,H49C), C52(H52A,
 H52B,H52C), C62(H62A,H62B,H62C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              53957
_shelx_hkl_checksum              21121
_olex2_submission_special_instructions 'No special instructions were received'