Site-Selective Binding of Peripheral Chiral Guests Induces Stereospecificity in A<sub>4</sub>L<sub>6</sub> Tetrahedral Anion Cages.
Li, Boyang; Zheng, Bo; Zhang, Wenyao; Zhang, Dan; Yang, Xiao-Juan; Wu, Biao; Journal of the American Chemical Society 142 (2020) 6304–6311; doi:10.1021/jacs.0c00882

data_4134526
_publ_section_title
;
 Site-Selective Binding of Peripheral Chiral Guests Induces
 Stereospecificity in A<sub>4</sub>L<sub>6</sub> Tetrahedral Anion Cages.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6304
_journal_page_last               6311
_journal_paper_doi               10.1021/jacs.0c00882
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety
'4(O1.33 P0.33), 2(C34 H28 N10 O8), 8(C1.33 H4 N0.33), 2(C2 H3 N), C6 H16 N O, C1.33 N0.33'
_chemical_formula_sum            'C90 H110 N26 O22.33 P1.33'
_chemical_formula_weight         1954.66
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   42.271(6)
_cell_length_b                   42.271
_cell_length_c                   42.271
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      64.79
_cell_measurement_theta_min      2.34
_cell_volume                     75531(11)
_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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.02
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Venture photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            176505
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.282
_diffrn_reflns_theta_min         1.810
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.782
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0933 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.8708.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             24736
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
;
_refine_diff_density_max         1.605
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         23069
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1427
_refine_ls_R_factor_gt           0.1080
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2926
_refine_ls_wR_factor_ref         0.3237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12599
_reflns_number_total             23069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00882_si_002.cif
_cod_data_source_block           complex_1-sr
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'none' was changed to
'?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4134525--4134528.cif.
;
_cod_original_cell_volume        75529(34)
_cod_database_code               4134526
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N24-C83 = N24-C84
 1.48 with sigma of 0.02
 C83-C84
 2.4 with sigma of 0.02
 N26-C87 = N26-C88
 1.48 with sigma of 0.02
 C87-C88
 2.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N26) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(N24)
\\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
Uanis(N26) = Uanis(C87) = Uanis(C88) = Uanis(N24) = Uanis(C83) = Uanis(C84)
4. Others
 Fixed Sof: H85A(0.33333) H85B(0.33333) H85C(0.33333) H84A(0.33333)
 H84B(0.33333) H84C(0.33333)
5.a Ternary CH refined with riding coordinates:
 C72(H72)
5.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B)
5.c Aromatic/amide H refined with riding coordinates:
 N8(H8), N7(H7), N9(H9), N6(H6), N16(H16A), N5(H5), N17(H17A), N18(H18),
 N19(H19A), N15(H15), N12(H12A), N4(H4), N3(H3), N14(H14), N13(H13), N2(H2),
 C26(H26), C17(H17), C16(H16), C30(H30), C34(H34), C20(H20), C53(H53), C19(H19),
  C54(H54), C31(H31), C50(H50), C24(H24), C51(H51), C33(H33), C25(H25),
 C57(H57), C23(H23), C60(H60), C3(H3A), C58(H58), C59(H59), C39(H39), C37(H37),
 C65(H65), C9(H9A), C64(H64), C36(H36), C40(H40), C12(H12), C68(H68), C6(H6A),
 C5(H5A), C10(H10), C11(H11), C67(H67), C43(H43), C2(H2A), C44(H44), C46(H46),
 C45(H45)
5.d Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C85(H85A,H85B,H85C), C69(H69A,H69B,H69C), C76(H76A,H76B,
 H76C), C73(H73A,H73B,H73C), C70(H70A,H70B,H70C), C86(H86A,H86B,H86C), C71(H71A,
 H71B,H71C), C77(H77A,H77B,H77C), C81(H81A,H81B,H81C), C75(H75A,H75B,H75C),
 C80(H80A,H80B,H80C), C78(H78A,H78B,H78C), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C79(H79A,H79B,H79C), C84(H84A,H84B,H84C), C91(H91A,H91B,H91C)
5.e Idealised tetrahedral OH refined as rotating group:
 O23(H23A)
;
_olex2_submission_special_instructions 'No special instructions were received'