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_1551331
_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
'0.5(C H2 Cl2), 11(C H4 O), 10.5(H2 O), 2(C72 H84 N12)'
_chemical_formula_sum            'C155.5 H234 Cl N24 O21.5'
_chemical_formula_weight         2819.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.334(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.692(2)
_cell_length_b                   19.8867(13)
_cell_length_c                   26.6702(18)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      2.36
_cell_volume                     18369(2)
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2011)'
_computing_data_reduction        'Bruker AXS SAINT V7.68A'
_computing_molecular_graphics
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
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_computing_publication_material
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O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XLMP, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXD, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.00
_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  0.0730
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            176990
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         0.76
_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    0.082
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1342 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.6559.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.019
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6096
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.4(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1711
_refine_ls_number_reflns         25720
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0977
_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^)+(0.1921P)^2^+35.7353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2645
_refine_ls_wR_factor_ref         0.2748
_reflns_number_gt                22954
_reflns_number_total             25720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s14.cif
_cod_data_source_block           2(CC3)0.5(CH2Cl2)11(MeOH)10.5(H2O)
_cod_original_formula_sum        'C155.50 H234 Cl N24 O21.50'
_cod_database_code               1551331
_olex2_refinement_description
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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. Restrained distances
 O26-C161
 1.43 with sigma of 0.005
 O17-C156
 1.43 with sigma of 0.005
 O7-C155
 1.43 with sigma of 0.005
3. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) O7(0.5) H7A(0.5) O9(0.5) H9A(0.5) O10(0.75)
 H10(0.75) O13(0.5) H13M(0.5) O14(0.5) H14(0.5) O16(0.5) H16A(0.5) O17(0.5)
 H17A(0.5) O18(0.5) O19(0.5) O22(0.5) H22A(0.5) O23(0.5) H23(0.5) O24(0.5)
 C160(0.25) H16B(0.25) H16C(0.25) H16D(0.25) O26(0.5) H26A(0.5) O27(0.5)
 O28(0.5) H28(0.5) O29(0.5) C145(0.5) H14U(0.5) H14V(0.5) C146(0.75) H14O(0.75)
 H14P(0.75) H14Q(0.75) C150(0.5) H15J(0.5) H15K(0.5) H15L(0.5) C151(0.5)
 H15G(0.5) H15H(0.5) H15I(0.5) C153(0.5) H15D(0.5) H15E(0.5) H15F(0.5)
 C154(0.5) H15Q(0.5) H15R(0.5) H15S(0.5) C155(0.5) H15A(0.5) H15B(0.5)
 H15C(0.5) C156(0.5) H15T(0.5) H15U(0.5) H15V(0.5) C158(0.5) H15Z(0.5)
 H51A(0.5) H51B(0.5) C159(0.5) H0AA(0.5) H1AA(0.5) H15C(0.5) O25(0.25)
 H25(0.25) C161(0.5) H16E(0.5) H16F(0.5) H16G(0.5) C162(0.5) H16H(0.5)
 H16I(0.5) H16J(0.5)
4.a Ternary CH refined with riding coordinates:
 C37(H37), C42(H42), C43(H43), C48(H48), C49(H49), C54(H54), C55(H55),
 C60(H60), C61(H61), C66(H66), C67(H67), C72(H72), C109(H109), C114(H114),
 C115(H115), C120(H120), C121(H121), C126(H126), C127(H127), C132(H132),
 C133(H133), C138(H138), C139(H139), C144(H144)
4.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C50(H50A,H50B),
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C56(H56A,H56B), C57(H57A,H57B),
  C58(H58A,H58B), C59(H59A,H59B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,
 H64B), C65(H65A,H65B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
 C71(H71A,H71B), C110(H11A,H11B), C111(H11C,H11D), C112(H11E,H11F), C113(H11G,
 H11H), C116(H11I,H11J), C117(H11K,H11L), C118(H11M,H11N), C119(H11O,H11P),
 C122(H12A,H12B), C123(H12C,H12D), C124(H12E,H12F), C125(H12G,H12H), C128(H12I,
 H12J), C129(H12K,H12L), C130(H13A,H13B), C131(H13C,H13D), C134(H13E,H13F),
 C135(H13G,H13H), C136(H13I,H13J), C137(H13K,H13L), C140(H14A,H14B), C141(H14C,
 H14D), C142(H14E,H14F), C143(H14G,H14H), C145(H14U,H14V)
4.c Me refined with riding coordinates:
 C160(H16B,H16C,H16D), C146(H14O,H14P,H14Q), C147(H14L,H14M,H14N), C148(H14I,
 H14J,H14K), C149(H14R,H14S,H14T), C150(H15J,H15K,H15L), C151(H15G,H15H,H15I),
 C152(H15N,H15O,H15P), C153(H15D,H15E,H15F), C154(H15Q,H15R,H15S), C155(H15A,
 H15B,H15C), C156(H15T,H15U,H15V), C157(H15W,H15X,H15Y), C158(H15Z,H79A,H79B),
 C159(H0AA,H1AA,H79C), C161(H16E,H16F,H16G), C162(H16H,H16I,H16J)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C24(H24), C1A(H1A), C26(H26),
  C27(H27), C29(H29), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36),
 C74(H74), C76(H76), C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C85(H85),
  C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C94(H94), C96(H96),
 C97(H97), C98(H98), C99(H99), C101(H101), C103(H103), C105(H105), C106(H106),
 C107(H107), C108(H108)
4.e Tetrahedral OH refined with riding coordinates:
 O1(H1), O3(H3), O7(H7A), O9(H9A), O10(H10), O12(H12), O13(H13M), O14(H14),
 O15(H15M), O16(H16A), O17(H17A), O20(H20A), O22(H22A), O23(H23), O26(H26A),
 O28(H28), O25(H25)
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