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_1551325
_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 H72 N11, 2(C0.25 H0.25 Cl0.75), 1.5 (C1 O1 H4)'
_chemical_formula_sum            'C218.02 H246.5 Cl1.5 N35 O1.5'
_chemical_formula_weight         3432.40
_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     dual
_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                   20.718(2)
_cell_length_b                   20.718(2)
_cell_length_c                   44.992(5)
_cell_measurement_reflns_used    9140
_cell_measurement_temperature    300
_cell_measurement_theta_max      21.638
_cell_measurement_theta_min      2.315
_cell_volume                     16725(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      300.00
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            92330
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.45
_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    0.079
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1336 before and 0.0817 after correction.
The Ratio of minimum to maximum transmission is 0.6949.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5511
_exptl_crystal_size_max          0.224
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     477
_refine_ls_number_reflns         6816
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0737
_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^)+(0.1479P)^2^+3.8550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2022
_refine_ls_wR_factor_ref         0.2282
_reflns_number_gt                4858
_reflns_number_total             6816
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s10.cif
_cod_data_source_block           2(CC3-R)(3+2#5)_350K
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_original_formula_sum        'C218.02 H246.50 Cl1.50 N35 O1.50'
_cod_database_code               1551325
_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
 O2-C50
 1.43 with sigma of 0.005
 O1-C49
 1.43 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uiso(O2) = Uiso(C50)
Uiso(C49) = Uiso(O1)
4. Others
 Fixed Sof: N6(0.5) C42(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5)
 H45(0.5) C46(0.5) H46(0.5) C47(0.5) H47(0.5) N7(0.5) C36(0.5) C35(0.5)
 H35(0.5) C34(0.5) H34(0.5) C33(0.5) C38(0.5) H38(0.5) C37(0.5) H37(0.5)
 C39(0.5) H39(0.5) C40(0.5) H40A(0.5) H40B(0.5) C41(0.5) H41A(0.5) H41B(0.5)
 N5(0.5) C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5)
 C26(0.5) H26(0.5) C27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5) C30(0.5)
 C31(0.5) H31(0.5) C32(0.5) H32(0.5) Cl1(0.25) C48(0.08333) H48(0.08333)
 O1(0.16667) C49(0.17) O2(0.08333) C50(0.08333)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C9(H9), C18(H18), C22(H22), C48(H48)
5.b Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C19(H19A,
 H19B), C20(H20A,H20B), C23(H23A,H23B), C40(H40A,H40B), C41(H41A,H41B),
 C25(H25A,H25B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C10(H10), C12(H12), C14(H14), C16(H16), C17(H17), C21(H21),
 C031(H031), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47), C35(H35),
 C34(H34), C38(H38), C37(H37), C39(H39), C26(H26), C28(H28), C29(H29), C31(H31),
  C32(H32)
5.d Fitted hexagon refined as free rotating group:
 C42(C43,C44,C45,C46,C47), C36(C35,C34,C33,C38,C37), C27(C28,C29,C30,C31,C32)
5.e Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
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