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_4134525
_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
'2(C34 H28 N10 O8), 2(C2 H3 N), C6 H16 N O, 3(C4 H12 N), 1.33(O4 P)'
_chemical_formula_sum            'C90 H114 N26 O22.33 P1.33'
_chemical_formula_weight         1958.69
_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             2019-08-27
_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                   42.4955(11)
_cell_length_b                   42.4955(11)
_cell_length_c                   42.4955(11)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      64.83
_cell_measurement_theta_min      2.55
_cell_volume                     76741(3)
_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      150.01
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0792
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            126535
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.561
_diffrn_reflns_theta_max         66.561
_diffrn_reflns_theta_min         2.325
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1038 before and 0.0721 after correction.
The Ratio of minimum to maximum transmission is 0.7398.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             24832
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_transmission_factor_max   0.7528
_exptl_transmission_factor_min   0.5569
_platon_squeeze_details
;
;
_refine_diff_density_max         1.418
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1265
_refine_ls_number_reflns         22569
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1561
_refine_ls_R_factor_gt           0.1173
_refine_ls_shift/su_max          0.004
_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          0.3064
_refine_ls_wR_factor_ref         0.3463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10188
_reflns_number_total             22569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00882_si_003.cif
_cod_data_source_block           complex_2-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        76741(6)
_cod_database_code               4134525
_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 = N26-C87 = N26-C88 = N21-C69 = N21-C70 = N21-C71
 1.48 with sigma of 0.02
 C83-C84 = C87-C88
 2.4 with sigma of 0.02
 C70-C71 = C71-C69
 2.5 with sigma of 0.02
3. Rigid bond restraints
 N26, C87, C88, N24, C83, C84
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N26 \\sim C87 \\sim C88 \\sim N24 \\sim C83 \\sim C84: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
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)
5. Others
 Fixed Sof: H84A(0.33333) H84C(0.33333) H84B(0.33333) H86A(0.33333)
 H86B(0.33333) H86C(0.33333) H87A(0.33333) H87B(0.33333) H87C(0.33333)
6.a Ternary CH refined with riding coordinates:
 C72(H72)
6.b Secondary CH2 refined with riding coordinates:
 C74(H74A,H74B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
  C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37), C39(H39),
 C40(H40), C43(H43), C44(H44), C45(H45), C46(H46), C50(H50), C51(H51), C53(H53),
  C54(H54), C57(H57), C58(H58), C59(H59), C60(H60), C64(H64), C65(H65),
 C67(H67), C68(H68), N2(H2A), N3(H3A), N4(H4), N5(H5A), N6(H6A), N7(H7), N8(H8),
  N9(H9A), N12(H12A), N13(H13), N14(H14), N15(H15), N16(H16A), N17(H17A),
 N18(H18), N19(H19A)
6.d Idealised Me refined as rotating group:
 C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C73(H73A,H73B,
 H73C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,
 H78B,H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C),
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84C,H84B), C85(H85A,H85B,
 H85C), C86(H86A,H86B,H86C), C89(H89A,H89B,H89C), C88(H88A,H88B,H88C), C87(H87A,
 H87B,H87C), C91(H91A,H91B,H91C)
6.e Idealised tetrahedral OH refined as rotating group:
 O23(H23A)
;
_olex2_submission_special_instructions 'No special instructions were received'