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_1551328
_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 ad
_chemical_formula_moiety         'C H2 Cl2, 7(C H4 O), 2.5(H2 O), C72 H84 N12'
_chemical_formula_sum            'C80 H119 Cl2 N12 O9.5'
_chemical_formula_weight         1471.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 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                 105.506(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7305(17)
_cell_length_b                   19.7370(15)
_cell_length_c                   22.9973(17)
_cell_measurement_reflns_used    9992
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.18
_cell_volume                     9504.4(13)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0720
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            96510
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1471 before and 0.0813 after correction.
The Ratio of minimum to maximum transmission is 0.6400.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.029
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3172
_exptl_crystal_size_max          0.482
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.143
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         18701
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1861P)^2^+10.5703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2458
_refine_ls_wR_factor_ref         0.2563
_reflns_number_gt                16974
_reflns_number_total             18701
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s11.cif
_cod_data_source_block           Phase_1_CH2Cl2
_cod_original_formula_sum        'C80 H119 Cl2 N12 O9.50'
_cod_database_code               1551328
_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
 Cl2-C73 = Cl1-C73
 1.74 with sigma of 0.02
 Cl3-C74 = Cl4-C74
 1.74 with sigma of 0.02
3. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) Cl4(0.5) O1(0.5) H1(0.5) O2(0.5) H2A(0.5)
 O3(0.5) H3(0.5) O5(0.5) H5(0.5) O7(0.5) H7A(0.5) O8(0.5) O9(0.5) H9A(0.5)
 O11(0.5) O13(0.5) O14(0.5) O15(0.5) C73(0.5) H73A(0.5) H73B(0.5) H74A(0.5)
 H74B(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5) C78(0.5) H78A(0.5) H78B(0.5)
 H78C(0.5) C79(0.5) H79A(0.5) H79B(0.5) H79C(0.5) C82(0.5) H82A(0.5) H82B(0.5)
 H82C(0.5) C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5) C84(0.5) H84A(0.5) H84B(0.5)
 H84C(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)
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), C73(H73A,H73B), C74(H74A,H74B)
4.c Me refined with riding coordinates:
 C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C78(H78A,H78B,
 H78C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C82(H82A,
 H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C)
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), C25(H25), C26(H26),
  C27(H27), C29(H29), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36)
4.e Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2A), O3(H3), O4(H4A), O5(H5), O6(H6A), O7(H7A), O9(H9A), O10(H10),
  O12(H12)
;