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_4134528
_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
'1.33(O4 P), 2(C34 H28 N10 O8), 8(C1.33 H4 N0.33), C6 H N O, C1.33 N0.33'
_chemical_formula_sum            'C86 H89 N24 O22.33 P1.33'
_chemical_formula_weight         1857.43
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-12-16
_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            12
_cell_length_a                   32.135(4)
_cell_length_b                   32.135
_cell_length_c                   32.135
_cell_measurement_reflns_used    9287
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      64.31
_cell_measurement_theta_min      2.38
_cell_volume                     33184(4)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker D8 Venture Photon II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            66844
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        65.251
_diffrn_reflns_theta_max         65.251
_diffrn_reflns_theta_min         1.944
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1316 before and 0.0690 after correction.
The Ratio of minimum to maximum transmission is 0.6997.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             11660
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   0.7526
_exptl_transmission_factor_min   0.5266
_platon_squeeze_details
;
;
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 6376 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.013(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1188
_refine_ls_number_reflns         18065
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0725
_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^)+(0.1732P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2144
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.913
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                15981
_reflns_number_total             18065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00882_si_005.cif
_cod_data_source_block           complex_4-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        33184(13)
_cod_database_code               4134528
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C69-N21 = C70-N21 = C71-N21 = C72-N21 = C85-N25 = C86-N25 = N26-C87 = N26-C88
 1.48 with sigma of 0.02
 C85-N25 = C86-N25
 1.48 with sigma of 0.02
 C79-N23 = C80-N23 = C81-N23 = C82-N23
 1.48 with sigma of 0.02
 C79-C80 = C79-C81 = C79-C82
 2.4 with sigma of 0.02
 C72-C73 = C73-C74
 1.53 with sigma of 0.02
 C73-O23
 1.39 with sigma of 0.02
 C85-C86 = C87-C88 = C72-C74 = C72-O23
 2.4 with sigma of 0.1
 N21-C73
 2.7 with sigma of 0.02
 C71-C73
 2.9 with sigma of 0.02
 C74-O23
 2.2 with sigma of 0.1
3. Rigid bond restraints
 C85, C88, C72, C73, C74, O23, N26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C85 \\sim C88 \\sim C72 \\sim C73 \\sim C74 \\sim O23 \\sim N26: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C85) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(N25) \\sim Ueq, Uanis(C88)
\\sim Ueq, Uanis(N26) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C72) \\sim Ueq,
Uanis(C73) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C85) = Uanis(C88) = Uanis(C72) = Uanis(C73) = Uanis(C74) = Uanis(O23) =
Uanis(N26)
5. Others
 Fixed Sof: H84A(0.33333) H84B(0.33333) H84C(0.33333) H86A(0.33333)
 H86B(0.33333) H86C(0.33333)
6.a Ternary CH refined with riding coordinates:
 C73(H73)
6.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N15(H15), N13(H13), N14(H14), N6(H6), N9(H9), N16(H16A), N8(H8),
 N17(H17A), N18(H18), N19(H19A), N4(H4), N2(H2), N12(H12A), N3(H3), N7(H7),
 C46(H46), C54(H54), C17(H17), C50(H50), C51(H51), C53(H53), C20(H20), C12(H12),
  C16(H16), C19(H19), C43(H43), C36(H36), C0AA(H0AA), C34(H34), C39(H39),
 C30(H30), C9(H9A), C45(H45), C68(H68), C10(H10), C37(H37), C33(H33), C64(H64),
 C44(H44), C5(H5A), C57(H57), C3(H3A), C58(H58), C67(H67), C65(H65), C6(H6A),
 C31(H31), C11(H11), C40(H40), C60(H60), C2(H2A), C25(H25), C59(H59), C24(H24),
 C23(H23)
6.c Idealised Me refined as rotating group:
 C75(H75A,H75B,H75C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C78(H78A,H78B,
 H78C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C76(H76A,H76B,H76C), C82(H82A,
 H82B,H82C), C84(H84A,H84B,H84C), C80(H80A,H80B,H80C), C85(H85A,H85B,H85C),
 C86(H86A,H86B,H86C)
;
_olex2_submission_special_instructions 'No special instructions were received'