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_1551329
_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         '11(C H4 O), 4(H2 O), C72 H85 N12'
_chemical_formula_sum            'C83 H137 N12 O15'
_chemical_formula_weight         1543.05
_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     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.7040(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.6440(9)
_cell_length_b                   19.7822(8)
_cell_length_c                   23.2696(15)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.13
_cell_measurement_theta_min      2.18
_cell_volume                     9591.4(8)
_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    '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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80290
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         1.14
_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    0.074
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.2926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1599 before and 0.1001 after correction.
The Ratio of minimum to maximum transmission is 0.3928.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3356
_exptl_crystal_size_max          0.421
_exptl_crystal_size_mid          0.417
_exptl_crystal_size_min          0.389
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.600
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         13676
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.600
_refine_ls_R_factor_all          0.1234
_refine_ls_R_factor_gt           0.1152
_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          0.3264
_refine_ls_wR_factor_ref         0.3387
_reflns_number_gt                12573
_reflns_number_total             13676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.2156-s12.cif
_cod_data_source_block           Phase_1_CHCl3
_cod_original_cell_volume        9591.3(8)
_cod_database_code               1551329
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Shared sites
{C83A, C83B}
{O4A, O4B}
{C80A, C80B}
3. Restrained distances
 O3-C73
 1.43 with sigma of 0.005
 O9-C90
 1.43 with sigma of 0.005
 O22-C80A
 1.43 with sigma of 0.005
 O6-C83A = O5-C83A = O20-C85 = O21-C79 = O23-C80A = O2-C76 = O1-C74
 1.43 with sigma of 0.005
 H81B-H10
 2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(C83A) = Uiso(C83B)
Uiso(O4A) = Uiso(O4B)
Uiso(C80A) = Uiso(C80B)
5. Others
 Fixed Sof: O1(0.5) H1A(0.5) O2(0.5) H2(0.5) O3(0.5) H3A(0.5) O4A(0.5)
 H4A(0.5) O4B(0.5) H4B(0.5) O5(0.5) H5A(0.5) O6(0.5) H6(0.5) O7(0.5) H7A(0.5)
 O8(0.5) O9(0.5) H9A(0.5) O10(0.5) O13(0.5) O14(0.5) H14(0.5) O15(0.5)
 H15A(0.5) O16(0.5) H16A(0.5) O17(0.75) H17(0.75) H84A(0.5) H84B(0.5) H84C(0.5)
 O19(0.5) O21(0.75) H21A(0.75) O22(0.5) H22A(0.5) O23(0.5) H23(0.5) O24(0.5)
 H24(0.5) O25(0.5) H25(0.5) C73(0.5) H73A(0.5) H73B(0.5) H73C(0.5) C74(0.5)
 H74A(0.5) H74B(0.5) H74C(0.5) C75(0.5) H75A(0.5) H75B(0.5) H75C(0.5) C76(0.5)
 H76A(0.5) H76B(0.5) H76C(0.5) C77(0.5) H77A(0.5) H77B(0.5) H77C(0.5) C79(0.75)
 H79A(0.75) H79B(0.75) H79C(0.75) C80A(0.5) H80D(0.5) H80E(0.5) H80F(0.5)
 C80B(0.5) H80A(0.5) H80B(0.5) H80C(0.5) H82A(0.5) H82B(0.5) H82C(0.5)
 H82D(0.5) H82E(0.5) H82F(0.5) C83A(0.5) H83A(0.5) H83B(0.5) H83C(0.5)
 C83B(0.5) H83D(0.5) H83E(0.5) H83F(0.5) O18(0.5) H18(0.5) C86(0.75) H86A(0.75)
 H86B(0.75) H86C(0.75) C87(0.5) H87A(0.5) H87B(0.5) H87C(0.5) C88(0.5)
 H88A(0.5) H88B(0.5) H88C(0.5) C89(0.5) H89A(0.5) H89B(0.5) H89C(0.5) C90(0.5)
 H90A(0.5) H90B(0.5) H90C(0.5) C81(0.5) H81A(0.5) H81B(0.5) H81C(0.5)
6.a Ternary CH refined with riding coordinates:
 C10(H10A), C15(H15), C16(H16), C21(H21), C22(H22), C27(H27), C37(H37),
 C42(H42), C43(H43), C48(H48), C58(H58), C63(H63)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C23(H23A,H23B),
 C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C41(H41A,H41B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B),
 C62(H62A,H62B)
6.c Me refined with riding coordinates:
 C84(H84A,H84B,H84C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C),
 C80A(H80D,H80E,H80F), C80B(H80A,H80B,H80C), C82(H82A,H82B,H82C), C82(H82D,H82E,
 H82F), C83A(H83A,H83B,H83C), C83B(H83D,H83E,H83F), C85(H85A,H85B,H85C),
 C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C), C89(H89A,H89B,
 H89C), C90(H90A,H90B,H90C), C81(H81A,H81B,H81C)
6.d Aromatic/amide H refined with riding coordinates:
 N10(H10), C1(H1), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C29(H29), C31(H31),
 C33(H33), C34(H34), C35(H35), C36(H36), C49(H49), C51(H51), C53(H53), C55(H55),
  C56(H56), C57(H57), C64(H64), C66(H66), C68(H68), C70(H70), C71(H71), C72(H72)
6.e Tetrahedral OH refined with riding coordinates:
 O1(H1A), O2(H2), O3(H3A), O4A(H4A), O4B(H4B), O5(H5A), O6(H6), O7(H7A),
 O9(H9A), O14(H14), O15(H15A), O16(H16A), O17(H17), O20(H20), O21(H21A),
 O22(H22A), O23(H23), O24(H24), O25(H25), O18(H18)
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