A solution-processable dissymmetric porous organic cage
Slater, A. G.; Little, M. A.; Briggs, M. E.; Jelfs, K. E.; Cooper, A. I.; Molecular Systems Design & Engineering 3 (2018) 223–; doi:10.1039/C7ME00090A

data_1553656
_publ_section_title
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 A solution-processable dissymmetric porous organic cage
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_journal_issue                   1
_journal_name_full               'Molecular Systems Design &amp; Engineering'
_journal_page_first              223
_journal_paper_doi               10.1039/C7ME00090A
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety
'C72 H84 N12, 0.77(C H2 Cl2), 0.32(C H4 O), 1.57(H2 O)'
_chemical_formula_sum            'C73.1 H89.96 Cl1.55 N12 O1.89'
_chemical_formula_weight         1221.97
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-08-28
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.08.17 svn.r3210 for OlexSys, GUI svn.r5083)
;
_audit_update_record
;
2017-08-31 deposited with the CCDC.
2017-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.4830(11)
_cell_length_b                   24.4830(11)
_cell_length_c                   19.6123(9)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.200
_cell_measurement_theta_min      2.745
_cell_volume                     10181.0(8)
_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, 2015)'
_computing_structure_solution    'ShelXD (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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31027
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         1.414
_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    0.132
_exptl_absorpt_correction_T_max  0.9925
_exptl_absorpt_correction_T_min  0.7092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1165 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.7146.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       needle
_exptl_crystal_F_000             3924
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4632
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0960P)^2^+10.7810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3961
_reflns_number_total             4632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7me00090a2.cif
_cod_data_source_block           ags_169_v_100k_solvate
_cod_original_cell_volume        10180.9(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C73.10 H89.96 Cl1.55 N12 O1.89'
_cod_database_code               1553656
_shelxl_version_number           2014/6
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.5121(19) 0.4879(19)
2. 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, All O(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl1, C25
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C26
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C25)=Sof(H25A)=Sof(H25B)=0.33333*FVAR(2)
 Sof(Cl1)=0.66667*FVAR(2)
 Sof(O1)=Sof(H1)=FVAR(2)
 Sof(H26B)=Sof(H26C)=Sof(H26A)=0.33333*FVAR(4)
 Sof(C26)=FVAR(3)
 Fixed X: H26B(0.63531) H26C(0.686629) H26A(0.69773)
 Fixed Y: H26B(0.29229) H26C(0.360241) H26A(0.32979)
 Fixed Z: H26B(0.434009) H26C(0.456889) H26A(0.391881)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C24(H24), C18(H18), C19(H19)
6.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C17(H17A,H17B), C15(H15A,H15B), C21(H21A,H21B), C20(H20A,
 H20B), C23(H23A,H23B), C22(H22A,H22B), C16(H16A,H16B), C25(H25A,H25B)
6.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C2(H2), C6(H6), C7(H7), C9(H9), C4(H4), C8(H8)
6.d Tetrahedral OH refined with riding coordinates:
 O1(H1)
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_shelx_res_checksum              52675
_olex2_submission_special_instructions 'No special instructions were received'