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_1551327
_publ_section_title
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 Trapping virtual pores by crystal retro-engineering
;
_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 ad
_chemical_formula_moiety
'2(C1 H1 Cl3), 8(C H4 O), 2(C72 H84 N12), C72 H66 N11'
_chemical_formula_sum            'C226 H268 Cl6 N35 O8'
_chemical_formula_weight         3815.45
_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                   20.5397(11)
_cell_length_b                   20.5397(11)
_cell_length_c                   44.747(3)
_cell_measurement_reflns_used    9716
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.15
_cell_volume                     16348.7(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    '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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            93107
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.98
_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    0.143
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1108 before and 0.0793 after correction.
The Ratio of minimum to maximum transmission is 0.6511.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6105
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7399
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0662
_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^)+(0.1283P)^2^+15.0332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2001
_reflns_number_gt                6528
_reflns_number_total             7399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s9.cif
_cod_data_source_block           2(CC3-R)(3+2#5)_Solvate_100K
_cod_original_cell_volume        16348.5(15)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               1551327
_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, All O(H) groups
2. Shared sites
{C50A, C50B}
3. Restrained distances
 C52-O3 = O4-C53
 1.43 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(C50A) = Uiso(C50B)
5. Others
 Fixed Sof: O1(0.16667) O2(0.5) H2(0.5) C52(0.25) H52A(0.25) H52B(0.25)
 H52C(0.25) O4(0.25) H4A(0.25) O5(0.16667) N5(0.5) N6(0.5) N7(0.5) C25(0.5)
 H25A(0.5) H25B(0.5) C26(0.5) H26A(0.5) H26B(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) C34(0.5) C35(0.5) C36(0.5) H36(0.5) C37(0.5) C38(0.5) H38(0.5)
 C39(0.5) H39(0.5) C40(0.5) H40(0.5) C41(0.5) H41A(0.5) H41B(0.5) C42(0.5)
 H42A(0.5) H42B(0.5) C43(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) C48(0.5) H48(0.5) C50A(0.16667) C50B(0.16667)
 C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) O3(0.25) H3(0.25) C53(0.25) H53A(0.25)
 H53B(0.25) H53C(0.25)
6.a Ternary CH refined with riding coordinates:
 C10(H10), C15(H15), C17(H17), C18(H18), C49(H49)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C19(H19A,
 H19B), C1A(H1AA,H1AB), C20(H20A,H20B), C21(H21A,H21B), C25(H25A,H25B),
 C26(H26A,H26B), C41(H41A,H41B), C42(H42A,H42B)
6.c Me refined with riding coordinates:
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C6(H6), C8(H8), C9(H9), C16(H16), C22(H22), C24(H24),
 C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C36(H36), C38(H38), C39(H39),
  C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48)
6.e Tetrahedral OH refined with riding coordinates:
 O2(H2), O4(H4A), O3(H3)
;