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_1551326
_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 H69 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                   20.6071(11)
_cell_length_b                   20.6071(11)
_cell_length_c                   44.949(3)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    293
_cell_measurement_theta_max      23.456
_cell_measurement_theta_min      2.325
_cell_volume                     16530.4(17)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1180
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            47559
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.41
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6785
_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 0.0784 before and 0.0484 after correction.
The Ratio of minimum to maximum transmission is 0.9105.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5334
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.174
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0583
_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^)+(0.1055P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1801
_reflns_number_gt                5185
_reflns_number_total             7538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s8.cif
_cod_data_source_block           2(CC3-R)(3+2#5)_EGC_Dynamic_Vacuum
_cod_original_cell_volume        16530.4(16)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               1551326
_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. Others
 Fixed Sof: 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) N7(0.5) C40(0.5) H40(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) C41(0.5) H41A(0.5) H41B(0.5) C43(0.5) C48(0.5) H48(0.5) C47(0.5)
 H47(0.5) C46(0.5) H46(0.5) C45(0.5) H45(0.5) C44(0.5) H44(0.5) N5(0.5)
 C26(0.5) H26A(0.5) H26B(0.5) C25(0.5) H25A(0.5) H25B(0.5) C28(0.5) C33(0.5)
 H33(0.5) C32(0.5) H32(0.5) C31(0.5) C30(0.5) H30(0.5) C29(0.5) H29(0.5)
 C27(0.5) H27(0.5) N6(0.5)
3.a Ternary CH refined with riding coordinates:
 C16(H16), C7(H7), C21(H21), C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C19(H19A,H19B), C18(H18A,H18B), C17(H17A,H17B), C6(H6A,H6B),
 C4(H4A,H4B), C5(H5A,H5B), C3(H3A,H3B), C42(H42A,H42B), C41(H41A,H41B),
 C26(H26A,H26B), C25(H25A,H25B)
3.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C24(H24), C15(H15), C14(H14), C12(H12), C38(H38), C39(H39),
 C35(H35), C36(H36), C22(H22), C1(H1), C40(H40), C48(H48), C47(H47), C46(H46),
 C45(H45), C44(H44), C33(H33), C32(H32), C30(H30), C29(H29), C27(H27)
3.d Fitted hexagon refined as free rotating group:
 C37(C38,C39,C34,C35,C36), C43(C48,C47,C46,C45,C44), C28(C33,C32,C31,C30,C29)
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