Chirality transcription in the anion-coordination-driven assembly of tetrahedral cages.
Fu, Jin; Zheng, Bo; Zhang, Huizheng; Zhao, Yanxia; Zhang, Dan; Zhang, Wenyao; Yang, Xiao-Juan; Wu, Biao; Chemical communications (Cambridge, England) 56 (2020) 2475–2478; doi:10.1039/c9cc09752j

data_7125880
_publ_section_title
;
 Chirality transcription in the anion-coordination-driven assembly of
 tetrahedral cages.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2475
_journal_page_last               2478
_journal_paper_doi               10.1039/c9cc09752j
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety
'2(C66 H63 N13 O6), C9 H20 N, 4(C12 H28 N), C2 H3 N, 2(O4 P), 0.94(O1)'
_chemical_formula_sum            'C206 H299 N33 O21 P2'
_chemical_formula_weight         3635.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-09
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2020-01-10 deposited with the CCDC.	2020-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 129.6000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.8647(13)
_cell_length_b                   28.7021(9)
_cell_length_c                   26.5738(9)
_cell_measurement_reflns_used    9532
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      68.256
_cell_measurement_theta_min      2.266
_cell_volume                     24015.7(14)
_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      119.96
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            140147
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.690
_diffrn_reflns_theta_min         2.083
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4439
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             7856
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.4439
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 12725 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.235(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2182
_refine_ls_number_reflns         43237
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0958
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+50.5161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2211
_refine_ls_wR_factor_ref         0.2269
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                35667
_reflns_number_total             43237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09752j2.cif
_cod_data_source_block           1
_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 7125880--7125882.cif.
;
_cod_database_code               7125880
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.841
_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
2. Restrained distances
 C158-C159
 1.54 with sigma of 0.02
 C160-C161
 1.54 with sigma of 0.02
 C161-C162
 1.54 with sigma of 0.02
 C163-C164
 1.54 with sigma of 0.02
 C164-C165
 1.54 with sigma of 0.02
 C166-C167
 1.54 with sigma of 0.02
 C167-C168
 1.54 with sigma of 0.02
 C139-C140
 1.54 with sigma of 0.02
 C140-C141
 1.54 with sigma of 0.02
 C142-C143
 1.54 with sigma of 0.02
 C136-C137
 1.54 with sigma of 0.02
 C175-C176
 1.54 with sigma of 0.02
 C176-C177
 1.54 with sigma of 0.02
 C178-C179
 1.54 with sigma of 0.02
 C179-C180
 1.54 with sigma of 0.02
 C169-C170
 1.54 with sigma of 0.02
 C170-C171
 1.54 with sigma of 0.02
 C172-C173
 1.54 with sigma of 0.02
 C173-C174
 1.54 with sigma of 0.02
 C151-C152
 1.54 with sigma of 0.02
 C152-C153
 1.54 with sigma of 0.02
 C148-C149
 1.54 with sigma of 0.02
 C149-C150
 1.54 with sigma of 0.02
 C154-C155
 1.54 with sigma of 0.02
 C155-C156
 1.54 with sigma of 0.02
 C145-C146
 1.54 with sigma of 0.02
 C146-C147
 1.54 with sigma of 0.02
 C190-C191
 1.54 with sigma of 0.02
 C191-C192
 1.54 with sigma of 0.02
 C187-C188
 1.54 with sigma of 0.02
 C188-C189
 1.54 with sigma of 0.02
 C184-C185
 1.54 with sigma of 0.02
 C185-C186
 1.54 with sigma of 0.02
 C181-C182
 1.54 with sigma of 0.02
 C182-C183
 1.54 with sigma of 0.02
 C157-C158
 1.54 with sigma of 0.02
 C133-C134
 1.54 with sigma of 0.02
 N29-C157
 1.45 with sigma of 0.02
 N29-C160
 1.45 with sigma of 0.02
 N29-C163
 1.45 with sigma of 0.02
 N29-C166
 1.45 with sigma of 0.02
 N27-C139
 1.45 with sigma of 0.02
 N27-C142
 1.45 with sigma of 0.02
 N27-C136
 1.45 with sigma of 0.02
 N27-C133
 1.45 with sigma of 0.02
 N30-C175
 1.45 with sigma of 0.02
 N30-C178
 1.45 with sigma of 0.02
 N30-C169
 1.45 with sigma of 0.02
 N30-C172
 1.45 with sigma of 0.02
 N28-C151
 1.45 with sigma of 0.02
 N28-C148
 1.45 with sigma of 0.02
 N28-C154
 1.45 with sigma of 0.02
 N28-C145
 1.45 with sigma of 0.02
 N31-C190
 1.45 with sigma of 0.02
 N31-C187
 1.45 with sigma of 0.02
 N31-C184
 1.45 with sigma of 0.02
 N31-C181
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N27) \\sim Ueq, Uanis(C139) \\sim Ueq, Uanis(C140) \\sim Ueq, Uanis(C141)
\\sim Ueq, Uanis(C142) \\sim Ueq, Uanis(C143) \\sim Ueq, Uanis(C136) \\sim Ueq,
Uanis(C137) \\sim Ueq, Uanis(C133) \\sim Ueq, Uanis(C134) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C119) = Uanis(C120)
Uanis(C181) = Uanis(C182)
Uanis(C191) = Uanis(C192)
Uanis(C142) = Uanis(C143)
Uanis(C121) = Uanis(C122)
Uanis(C189) = Uanis(C188)
Uanis(C178) = Uanis(C179)
Uanis(C133) = Uanis(C134)
4. Others
 Fixed Sof: O22(0.9438)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C37(H37), C59(H59), C81(H81), C103(H103), C125(H125)
5.b Secondary CH2 refined with riding coordinates:
 C136(H13A,H13B), C139(H13F,H13G), C140(H14L,H14M), C142(H14Q,H14R), C145(H14A,
 H14B), C146(H14C,H14D), C148(H14H,H14I), C149(H14J,H14K), C151(H15E,H15F),
 C152(H15G,H15H), C154(H15L,H15M), C155(H15N,H15O), C157(H15S,H15T), C158(H15U,
 H15V), C160(H16D,H16E), C161(H16F,H16G), C163(H16K,H16L), C164(H16M,H16N),
 C166(H16R,H16S), C167(H16T,H16U), C169(H16Y,H), C170(H17A,H17B), C172(H17F,
 H17G), C173(H17H,H17I), C175(H17M,H17N), C176(H17O,H17P), C178(H17T,H17U),
 C179(H17V,H17W), C181(H18E,H18F), C182(H18G,H18H), C184(H18L,H18M), C185(H18N,
 H18O), C187(H18S,H18T), C188(H18U,H18V), C190(H19B,H19C), C191(H19D,H19E)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27),
  C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C40(H40), C41(H41),
 C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50), C53(H53),
  C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C71(H71), C72(H72), C75(H75), C76(H76), C77(H77),
  C78(H78), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C90(H90),
 C91(H91), C93(H93), C94(H94), C97(H97), C98(H98), C99(H99), C100(H100),
 C106(H106), C107(H107), C108(H108), C109(H109), C110(H110), C112(H112),
 C113(H113), C115(H115), C116(H116), C119(H119), C120(H120), C121(H121),
 C122(H122), C128(H128), C129(H129), C130(H130), C131(H131), C132(H132),
 N2(H2A), N3(H3A), N4(H4), N5(H5A), N6(H6A), N7(H7), N8(H8), N9(H9A), N10(H10A),
  N11(H11A), N12(H12A), N13(H13), N15(H15A), N16(H16), N17(H17), N18(H18A),
 N19(H19A), N20(H20A), N21(H21A), N22(H22A), N23(H23), N24(H24A), N25(H25A),
 N26(H26)
5.d Fitted hexagon refined as free rotating group:
 C127(C128,C129,C130,C131,C132)
5.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C38(H38A,H38B,H38C), C60(H60A,H60B,H60C), C82(H82A,H82B,
 H82C), C104(H10B,H10C,H10D), C126(H12B,H12C,H12D), C137(H13C,H13D,H13E),
 C141(H14N,H14O,H14P), C143(H14S,H14T,H14U), C147(H14E,H14F,H14G), C150(H15B,
 H15C,H15D), C153(H15I,H15J,H15K), C156(H15P,H15Q,H15R), C159(H15W,H15X,H15Y),
 C162(H16H,H16I,H16J), C165(H16O,H16P,H16Q), C168(H16V,H16W,H16X), C171(H17C,
 H17D,H17E), C174(H17J,H17K,H17L), C177(H17Q,H17R,H17S), C180(H18B,H18C,H18D),
 C183(H18I,H18J,H18K), C186(H18P,H18Q,H18R), C189(H18W,H18X,H18Y), C192(H19F,
 H19G,H19H), C193(H19I,H19J,H19K), C134(H13H,H13I,H13J)
;
_shelx_fab_checksum              46733
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'