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_1546119
_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_formula_moiety         'C54 H60 N12, 1.7(C8 H10)'
_chemical_formula_sum            'C67.59 H76.99 N12'
_chemical_formula_weight         1057.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-08
_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                   11.1553(19)
_cell_length_b                   19.490(4)
_cell_length_c                   30.332(6)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.76
_cell_measurement_theta_min      2.20
_cell_volume                     6595(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            34167
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        22.400
_diffrn_reflns_theta_max         22.501
_diffrn_reflns_theta_min         1.649
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.8285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0829 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.8928.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       needle
_exptl_crystal_F_000             2266
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 2894 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         9431
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0786
_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^)+(0.1520P)^2^+0.6927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2297
_reflns_Friedel_coverage         0.794
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7494
_reflns_number_total             9431
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nr01301a2.cif
_cod_data_source_block           CC2-R_para-xylene
_cod_database_code               1546119
_shelxl_version_number           2014/6
_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. Restrained distances
 C75-C72
 1.52 with sigma of 0.02
 C68-C74
 1.52 with sigma of 0.02
 C74-C68 = C75-C72 = C71-C77 = C69-C76
 1.49 with sigma of 0.02
 C68-C76 \\sim C76-C70
 with sigma of 0.02
 C73-C75 \\sim C71-C75
 with sigma of 0.02
 C73-C75 \\sim C75-C71
 with sigma of 0.02
 C72-C77 \\sim C77-C70
 with sigma of 0.02
 C69-C74 \\sim C73-C74
 with sigma of 0.02
 C73-C74 \\sim C74-C69
 with sigma of 0.02
3. Restrained planarity
 C60, C61, C62, C63, C64, C65, C66, C67
 with sigma of 0.001
 C68, C69, C70, C71, C72, C73, C74, C75, C76, C77
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uiso(C73) = Uiso(C68) = Uiso(C69) = Uiso(C74) = Uiso(C70) = Uiso(C76) =
Uiso(C72) = Uiso(C71) = Uiso(C75) = Uiso(C77)
5. Rigid body (RIGU) restrains
 C66, C60, C61, C62, C63, C64, C65, C67
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(H48B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=1-FVAR(1)
 Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(H50C)=FVAR(1)
 Sof(H52B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=1-FVAR(2)
 Sof(H53B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
 Sof(H37B)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=1-FVAR(3)
 Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(3)
 Sof(H57B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=1-FVAR(4)
 Sof(H56B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=FVAR(4)
 Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=1-FVAR(5)
 Sof(H41B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(5)
 Sof(H68)=Sof(H69)=Sof(H71)=Sof(H72)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=
 Sof(C77)=Sof(H77A)=Sof(H77B)=Sof(H77C)=0.5*FVAR(7)
 Sof(C60)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=
 Sof(C65)=Sof(H65)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=Sof(C67)=Sof(H67A)=
 Sof(H67B)=Sof(H67C)=Sof(C68)=Sof(C69)=Sof(C70)=Sof(H70)=Sof(C71)=Sof(C72)=
 Sof(C73)=Sof(H73)=FVAR(6)
7.a Ternary CH refined with riding coordinates:
 C46(H46)
7.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C38(H38A,H38B), C41(H41A,H41B), C42(H42A,H42B), C45(H45A,
 H45B), C48(H48A,H48B), C49(H49A,H49B), C52(H52A,H52B), C53(H53A,H53B),
 C56(H56A,H56B), C57(H57A,H57B)
7.c Me refined with riding coordinates:
 C59(H59A,H59B,H59C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,
 H76C), C77(H77A,H77B,H77C)
7.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36),
 C61(H61), C62(H62), C63(H63), C65(H65), C68(H68), C69(H69), C70(H70), C71(H71),
  C72(H72), C73(H73)
7.e Fitted hexagon refined as free rotating group:
 C68(C69,C70,C71,C72,C73)
7.f Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C51(H51A,H51B,H51C), C50(H50A,H50B,H50C), C55(H55A,H55B,
 H55C), C54(H54A,H54B,H54C), C40(H40A,H40B,H40C), C39(H39A,H39B,H39C), C58(H58A,
 H58B,H58C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C)
;
_shelx_res_checksum              39216
_olex2_submission_special_instructions 'No special instructions were received'