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_1551330
_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 unk
_chemical_formula_moiety         'C72 H84 N12'
_chemical_formula_sum            'C72 H84 N12'
_chemical_formula_weight         1117.51
_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                 95.249(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   33.883(8)
_cell_length_b                   20.467(5)
_cell_length_c                   25.712(6)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      2.273
_cell_measurement_theta_min      23.342
_cell_volume                     17756(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker,2009)'
_computing_data_collection       'CrystalClear-SM Expert 2.1 (Rigaku, 2011)'
_computing_data_reduction        'SAINT v7.68A (Bruker,2009)'
_computing_molecular_graphics
;
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
;
XL, 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      300(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0659
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49205
_diffrn_reflns_theta_full        19.59
_diffrn_reflns_theta_max         19.59
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.050
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SABABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.836
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.261
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1513
_refine_ls_number_reflns         15202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0907
_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^)+(0.1611P)^2^+18.8874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2331
_refine_ls_wR_factor_ref         0.2673
_reflns_number_gt                11751
_reflns_number_total             15202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s13.cif
_cod_data_source_block           Phase_2
_cod_original_cell_volume        17756(8)
_cod_database_code               1551330
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C37(H37), C42(H42), C43(H43), C48(H48), C49(H49), C50(H50), 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)
2.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), C51(H51A,H51B),
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), 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)
2.c 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), C19(H19), C21(H21), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C30(H30), C32(H32), 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)
;