Chirality as a tool for function in porous organic cages.
Hasell, T.; Little, M. A.; Chong, S. Y.; Schmidtmann, M.; Briggs, M. E.; Santolini, V.; Jelfs, K. E.; Cooper, A. I.; Nanoscale 9 (2017) 6783–6790; doi:10.1039/c7nr01301a

data_1546121
_publ_section_title
;
 Chirality as a tool for function in porous organic cages.
;
_journal_issue                   20
_journal_name_full               Nanoscale
_journal_page_first              6783
_journal_page_last               6790
_journal_paper_doi               10.1039/c7nr01301a
_journal_volume                  9
_journal_year                    2017
_chemical_absolute_configuration R
_chemical_formula_moiety         '2(C54 H54 N12), 5.5(C4 H8 O2), 4.25(H2 O)'
_chemical_formula_sum            'C130 H160.5 N24 O15.25'
_chemical_formula_weight         2303.31
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-12-02 deposited with the CCDC.
2017-05-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.318(2)
_cell_length_b                   24.318(2)
_cell_length_c                   24.318(2)
_cell_measurement_reflns_used    4073
_cell_measurement_temperature    100
_cell_measurement_theta_max      9.905
_cell_measurement_theta_min      2.300
_cell_volume                     14381(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'CrystalClear v2 (Rigaku)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45501
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.517
_diffrn_reflns_theta_min         1.148
_diffrn_source                   Synchrotron
_diffrn_source_target            Cu
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.9568
_exptl_absorpt_correction_T_min  0.7928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1759 before and 0.1032 after correction.
The Ratio of minimum to maximum transmission is 0.8286.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_description       block
_exptl_crystal_F_000             4922
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 2208 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         6914
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0722
_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^)+(0.1553P)^2^+0.0650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2134
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5558
_reflns_number_total             6914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nr01301a2.cif
_cod_data_source_block           CC2-R_1-4-dioxane
_cod_original_cell_volume        14381(4)
_cod_original_formula_sum        'C130 H160.50 N24 O15.25'
_cod_database_code               1546121
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.990
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O50, O47, C48, C48, C48, C49, C49, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O44, O43, C45, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11, C10, O12, O13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C42, O3, C41, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H5A)=Sof(H5B)=Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(H6BC)=1-FVAR(1)
 Sof(H4A)=Sof(H4B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(C17B)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2)
 Sof(H15A)=Sof(H15B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(H22A)=Sof(H22B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(3)
 Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(3)
 Sof(H33A)=Sof(H33B)=Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(4)
 Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(4)
 Fixed Sof: O1(0.75) O2(0.75) C37(0.75) H37A(0.75) H37B(0.75) C38(0.75)
 H38A(0.75) H38B(0.75) C39(0.75) H39A(0.75) H39B(0.75) C40(0.75) H40A(0.75)
 H40B(0.75) O3(0.33333) O4(0.33333) C41(0.66667) C42(0.66667) O43(0.33333)
 O44(0.33333) C45(0.66667) C46(0.66667) O47(0.25) C48(0.5) C49(0.5) O50(0.25)
 O5(0.16667) O6(0.25) O7(0.25) O8(0.25) O9(0.5) C10(0.33333) C11(0.33333)
 O12(0.16667) O13(0.16667)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B),
 C23(H23A,H23B), C33(H33A,H33B), C34(H34A,H34B), C37(H37A,H37B), C38(H38A,H38B),
  C39(H39A,H39B), C40(H40A,H40B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C7(H7), C9(H9), C1AA(H1AA), C13(H13), C14(H14), C18(H18),
 C19(H19), C21(H21), C25(H25), C27(H27), C29(H29), C31(H31), C32(H32), C36(H36)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C6B(H6BA,H6BB,H6BC), C17(H17A,H17B,H17C), C17B(H17D,H17E,
 H17F), C24(H24A,H24B,H24C), C24B(H24D,H24E,H24F), C35(H35A,H35B,H35C),
 C35B(H35D,H35E,H35F)
;
_shelx_res_checksum              27110
_olex2_submission_special_instructions 'No special instructions were received'