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_7125882
_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_formula_moiety         'C63 H57 N13 O6, 3(C8 H20 N), O4 P'
_chemical_formula_sum            'C87 H117 N16 O10 P'
_chemical_formula_weight         1577.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           112
_space_group_name_Hall           'P -4 2c'
_space_group_name_H-M_alt        'P -4 2 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-01-10
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.958(3)
_cell_length_b                   25.958(3)
_cell_length_c                   28.548(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      68.03
_cell_measurement_theta_min      3.53
_cell_volume                     19236(6)
_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      158.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            360239
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.520
_diffrn_reflns_theta_min         1.702
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1026 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.8764.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             6768
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   0.7531
_exptl_transmission_factor_min   0.6600
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 7722 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1033
_refine_ls_number_reflns         17683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1480P)^2^+4.4950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.1955
_reflns_Friedel_coverage         0.870
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                17288
_reflns_number_total             17683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc09752j2.cif
_cod_data_source_block           5
_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_original_cell_volume        19236(7)
_cod_database_code               7125882
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.838
_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. Uiso/Uaniso restraints and constraints
Uanis(C80) = Uanis(C81)
3.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C36(H36A,H36B), C57(H57A,H57B), C64(H64A,H64B), C66(H66A,
 H66B), C68(H68A,H68B), C70(H70A,H70B), C72(H72A,H72B), C74(H74A,H74B),
 C76(H76A,H76B), C78(H78A,H78B), C80(H80A,H80B), C82(H82A,H82B), C84(H84A,H84B),
  C86(H86A,H86B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26),
  C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C47(H47), C48(H48), C51(H51),
  C52(H52), C53(H53), C54(H54), C59(H59), C60(H60), C61(H61), C62(H62),
 C63(H63), N2(H2A), N3(H3A), N4(H4), N5(H5A), N6(H6A), N7(H7), N8(H8), N9(H9A),
 N10(H10A), N11(H11A), N12(H12A), N13(H13)
3.c Idealised Me refined as rotating group:
 C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C), C71(H71A,H71B,
 H71C), C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C79(H79A,
 H79B,H79C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C),
 C87(H87A,H87B,H87C)
;
_shelx_fab_checksum              30261
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'