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_1551332
_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
'3(C H Cl3), 7(C H4 O), 4.75(H2 O), 2(C72 H84 N12)'
_chemical_formula_sum            'C154 H208.5 Cl9 N24 O11.75'
_chemical_formula_weight         2902.996
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 93.452(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.796(3)
_cell_length_b                   19.8984(14)
_cell_length_c                   26.7636(18)
_cell_measurement_reflns_used    9789
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.526
_cell_measurement_theta_min      2.458
_cell_volume                     18497(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
;45
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_publication_material
;
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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0530
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            162101
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         0.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1211 before and 0.0759 after correction.
The Ratio of minimum to maximum transmission is 0.6908.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             6162
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.121
_refine_diff_density_max         1.214
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.203
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1679
_refine_ls_number_reflns         26569
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.942
_refine_ls_R_factor_all          0.1833
_refine_ls_R_factor_gt           0.1641
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4202
_refine_ls_wR_factor_ref         0.4368
_reflns_number_gt                21994
_reflns_number_total             26569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s15.cif
_cod_data_source_block           Phase_3_CHCl3
_cod_database_code               1551332
_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. Shared sites
{C156, C56B}
{C155, C55B}
{C149, C49B}
3. Restrained distances
 O20-C156 = O19-C156
 1.43 with sigma of 0.02
 O16-C154
 1.43 with sigma of 0.02
 O11-C152
 1.43 with sigma of 0.02
 O8-C149
 1.43 with sigma of 0.005
 Cl8-C145 = Cl9-C145 = Cl7-C145
 1.73 with sigma of 0.005
4. Rigid bond restraints
 N12, C49, C50, C51, C52, C53, C54, N11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C55, C56, C57, C58, C59, C60, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uiso(C156) = Uiso(C56B)
Uiso(C155) = Uiso(C55B)
Uiso(C149) = Uiso(C49B)
6. Others
 Fixed Sof: O2(0.5) H2(0.5) O3(0.5) O4(0.5) O5(0.25) O6(0.5) O8(0.5) H8A(0.5)
 O9(0.5) O10(0.5) H10(0.5) O11(0.5) H11Q(0.5) O12(0.5) O13(0.5) H13M(0.5)
 O14(0.5) H14(0.5) O15(0.5) H15P(0.5) O16(0.5) H16A(0.5) O17(0.5) O18(0.5)
 O19(0.5) H19(0.5) O20(0.5) H20A(0.5) C49B(0.5) H49A(0.5) H49B(0.5) H49C(0.5)
 C55B(0.5) H55A(0.5) H55B(0.5) H55C(0.5) C56B(0.5) H56C(0.5) H56D(0.5)
 H56E(0.5) C149(0.5) H14L(0.5) H14M(0.5) H14N(0.5) C152(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) H15M(0.5) H15N(0.5) H15O(0.5)
 C156(0.5) H15T(0.5) H15U(0.5) H15V(0.5) C157(0.5) H15J(0.5) H15K(0.5) H15L(0.5)
7.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), C145(H145), C146(H146),
 C147(H147)
7.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)
7.c Me refined with riding coordinates:
 C49B(H49A,H49B,H49C), C55B(H55A,H55B,H55C), C56B(H56C,H56D,H56E), C148(H14I,
 H14J,H14K), C149(H14L,H14M,H14N), C150(H15A,H15B,H15C), C152(H15G,H15H,H15I),
 C153(H15D,H15E,H15F), C154(H15Q,H15R,H15S), C155(H15M,H15N,H15O), C156(H15T,
 H15U,H15V), C157(H15J,H15K,H15L)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C13(H13), C15(H15),
 C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36),
 C73(H73), C75(H75), C77(H77), 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)
7.e Tetrahedral OH refined with riding coordinates:
 O1(H1A), O2(H2), O7(H7A), O8(H8A), O10(H10), O11(H11Q), O13(H13M), O14(H14),
 O15(H15P), O16(H16A), O19(H19), O20(H20A)
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