Trapping virtual pores by crystal retro-engineering
Marc A. Little; Michael E. Briggs; James T. A. Jones; Marc Schmidtmann; Tom Hasell; Samantha Y. Chong; Kim E. Jelfs; Linjiang Chen; Andrew I. Cooper; Nature Chemistry 7 (2015) 153–159; doi:10.1038/nchem.2156

data_1551322
_publ_section_title
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 Trapping virtual pores by crystal retro-engineering
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_journal_name_full               'Nature Chemistry'
_journal_page_first              153
_journal_page_last               159
_journal_paper_doi               10.1038/nchem.2156
_journal_volume                  7
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         '2(C72 H84 N12), C72 H66 N11'
_chemical_formula_sum            'C216 H237 N35'
_chemical_formula_weight         3323.41
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.804(3)
_cell_length_b                   20.804(3)
_cell_length_c                   45.126(7)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    400(2)
_cell_measurement_theta_max      19.98
_cell_measurement_theta_min      2.31
_cell_volume                     16914(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker,2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker,2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      450.0
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            78509
_diffrn_reflns_theta_full        20.80
_diffrn_reflns_theta_max         20.80
_diffrn_reflns_theta_min         1.96
_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    0.059
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0948 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.6877.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.979
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5334
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         3947
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1112P)^2^+19.8732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1934
_refine_ls_wR_factor_ref         0.2233
_reflns_number_gt                3011
_reflns_number_total             3947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s5.cif
_cod_data_source_block           2(CC3-R)(3+2#5)_450K
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               1551322
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N6-C34 = N6-C31
 1.43 with sigma of 0.005
3. Restrained planarity
 C27, C28, C33, C32, C31, C30, C29, N6
 with sigma of 0.01
4. Rigid bond restraints
 C37, C38, C39, C34, C35, C36, N6, C43, C45, N7, C40, C41, H40, C42, H41A,
 H41B, H42A, H42B, N8, H38, H36, H39, H35, C31, C48, C44, C30, C32, H48, C47,
 C29, H30, H32, C33, H47, C46, C28, H29, H33, H46, C27, N5, H27, C26, C25, H26A,
  H26B, H25A, H25B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: N7(0.5) C37(0.5) C38(0.5) H38(0.5) C39(0.5) H39(0.5) C34(0.5)
 C35(0.5) H35(0.5) C36(0.5) H36(0.5) C42(0.5) H42A(0.5) H42B(0.5) C40(0.5)
 H40(0.5) C41(0.5) H41A(0.5) H41B(0.5) C48(0.5) H48(0.5) C47(0.5) H47(0.5)
 C46(0.5) H46(0.5) C45(0.5) C44(0.5) H44(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 C26(0.5) H26A(0.5) H26B(0.5) N5(0.5) C27(0.5) H27(0.5) C28(0.5) C29(0.5)
 H29(0.5) C30(0.5) H30(0.5) C31(0.5) C32(0.5) H32(0.5) C33(0.5) H33(0.5)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C20(H20), C4(H4), C19(H19)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C21(H21A,H21B), C5(H5A,H5B), C42(H42A,H42B), C22(H22A,H22B),
 C41(H41A,H41B), C23(H23A,H23B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C25(H25A,H25B), C26(H26A,H26B)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C18(H18), C16(H16), C38(H38), C39(H39), C35(H35), C36(H36),
 C12(H12), C17(H17), C40(H40), C3(H3), C14(H14), C1(H1), C48(H48), C47(H47),
 C46(H46), C44(H44), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33)
6.d Fitted hexagon refined as free rotating group:
 C37(C38,C39,C34,C35,C36), C43(C48,C47,C46,C45,C44), C28(C29,C30,C31,C32,C33)
;