Structural Insight into Guest Binding Sites in a Porous Homochiral Metal-Organic Material.
Zhang, Shi-Yuan; Wojtas, Lukasz; Zaworotko, Michael J.; Journal of the American Chemical Society 137 (2015) 12045–12049; doi:10.1021/jacs.5b06760

data_4129484
_publ_section_title
;
 Structural Insight into Guest Binding Sites in a Porous Homochiral
 Metal-Organic Material.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12045
_journal_page_last               12049
_journal_paper_doi               10.1021/jacs.5b06760
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'C92 H76 Co4 N12 O12, 3(N O3), N O3.33, 1.75(C9 H12 O), 0.59(C H2 Cl2), C7.2 H8.8 O0.8'
_chemical_formula_sum            'C115.49 H106.92 Cl1.18 Co4 N16 O26.88'
_chemical_formula_weight         2426.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.12 svn.r2899 for OlexSys, GUI svn.r4794)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.3471(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4393(2)
_cell_length_b                   24.6749(5)
_cell_length_c                   20.3245(4)
_cell_measurement_temperature    100(2)
_cell_volume                     5732.05(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0592
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65965
_diffrn_reflns_point_group_measured_fraction_full 0.847
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.656
_diffrn_reflns_theta_min         2.818
_exptl_absorpt_coefficient_mu    5.385
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_F_000             2510
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.017(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1668
_refine_ls_number_reflns         17590
_refine_ls_number_restraints     278
_refine_ls_restrained_S_all      13.874
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+1.0070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1077
_reflns_Friedel_coverage         0.704
_reflns_Friedel_fraction_full    0.718
_reflns_Friedel_fraction_max     0.735
_reflns_number_gt                15080
_reflns_number_total             17590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06760_si_005.cif
_cod_data_source_block           CMOM_1S_PPex
_cod_database_code               4129484
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
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
 O29-C126 = O30-C122
 1.43 with sigma of 0.02
 C126-C115 = C123-C122
 1.52 with sigma of 0.02
 C124-C116 = C129-C128
 1.51 with sigma of 0.02
 C126-C124 = C128-C122
 1.53 with sigma of 0.02
 O10-H10
 0.9 with sigma of 0.02
 O12-H12
 0.9 with sigma of 0.02
 O11-H11
 0.9 with sigma of 0.02
 C125-C123 = C127-C123 = C127-C120 = C120-C119 = C121-C119 = C125-C121
 1.39 with sigma of 0.02
 C125-C111 = C125-C112 = C113-C112 = C114-C113 = C115-C114 = C115-C111
 1.39 with sigma of 0.02
 O8-H8
 0.9 with sigma of 0.02
 H21-H8
 -2.2 with sigma of 0.02
 O11-O11_$1 = O11_$1-O11_$2
 0.9 with sigma of 0.02
 H11G_$2-H81
 -2.2 with sigma of 0.02
 C36-H10
 1.9 with sigma of 0.04
 H12-C35
 1.9 with sigma of 0.04
 C49-H11
 1.9 with sigma of 0.04
 H10-O18
 2 with sigma of 0.04
 C125-C120 = C123-C119 = C121-C127
 2.76 with sigma of 0.04
 C125-C127 = C121-C120
 2.38 with sigma of 0.04
 C115-C112 = C111-C113 = C114-C125
 2.76 with sigma of 0.04
 C111-C114 = C125-C113
 2.38 with sigma of 0.04
 H8-C21
 1.9 with sigma of 0.04
3. Restrained planarity
 C123, C125, C121, C119, C120, C127, C122
 with sigma of 0.02
 C111, C125, C112, C113, C114, C115, C126
 with sigma of 0.02
4. Rigid bond restraints
 C114, C126, C115, C124, C111, C116, C113, C112, C121, C123, C119, C122, C127,
 C120, C128, C129
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C122 \\sim C128 \\sim C124 \\sim C116 \\sim C129 \\sim C126 \\sim C115 \\sim
C123 \\sim C111 \\sim C112 \\sim C121 \\sim C119 \\sim C120 \\sim C113 \\sim
C127 \\sim C114: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
6. Others
 1*[Sof(O29)+Sof(C111)+Sof(H111)+Sof(C112)+Sof(H112)+Sof(C113)+Sof(H113)+
 Sof(C114)+Sof(H114)+Sof(C115)+Sof(C116)+Sof(H11B)+Sof(H11C)+Sof(H11D)+
 Sof(C124)+Sof(H12A)+Sof(H12B)+Sof(H125)+Sof(C126)+Sof(H126)]+1*[Sof(O30)+
 Sof(C119)+Sof(H119)+Sof(C120)+Sof(H120)+Sof(C121)+Sof(H121)+Sof(C122)+
 Sof(H122)+Sof(C123)+Sof(H12C)+Sof(C127)+Sof(H127)+Sof(C128)+Sof(H12D)+
 Sof(H12E)+Sof(C129)+Sof(H12F)+Sof(H12G)+Sof(H12H)]-1*[Sof(C125)]=0 with esd of
 0
 Sof(Cl3)=Sof(Cl4)=Sof(C117)=Sof(H11J)=Sof(H11K)=FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C118)=Sof(H11H)=Sof(H11I)=FVAR(2)
 Sof(O27)=Sof(N17)=Sof(O28)=1-FVAR(3)
 Sof(N14)=Sof(O21)=FVAR(3)
 Sof(C96)=Sof(H96)=Sof(O23)=Sof(H23A)=Sof(C99)=Sof(H99)=Sof(C100)=Sof(H100)=
 Sof(C103)=Sof(C104)=Sof(H104)=Sof(C106)=Sof(H10C)=Sof(H10D)=Sof(C108)=
 Sof(H108)=Sof(C109)=Sof(H109)=Sof(C110)=Sof(H11E)=Sof(H11F)=Sof(H11G)=FVAR(4)
 Sof(C76)=Sof(H76)=Sof(C77)=Sof(H77)=Sof(C79)=Sof(C88)=Sof(H88)=Sof(C94)=
 Sof(H94)=Sof(C95)=Sof(H95)=Sof(O22)=Sof(H22A)=Sof(C98)=Sof(H98A)=Sof(H98B)=
 Sof(H98C)=Sof(C101)=Sof(H101)=Sof(C102)=Sof(H10A)=Sof(H10B)=FVAR(5)
 Sof(O29)=Sof(C111)=Sof(H111)=Sof(C112)=Sof(H112)=Sof(C113)=Sof(H113)=
 Sof(C114)=Sof(H114)=Sof(C115)=Sof(C116)=Sof(H11B)=Sof(H11C)=Sof(H11D)=
 Sof(C124)=Sof(H12A)=Sof(H12B)=Sof(H125)=Sof(C126)=Sof(H126)=FVAR(6)
 Sof(O30)=Sof(C119)=Sof(H119)=Sof(C120)=Sof(H120)=Sof(C121)=Sof(H121)=
 Sof(C122)=Sof(H122)=Sof(C123)=Sof(H12C)=Sof(C127)=Sof(H127)=Sof(C128)=
 Sof(H12D)=Sof(H12E)=Sof(C129)=Sof(H12F)=Sof(H12G)=Sof(H12H)=FVAR(7)
7.a Ternary CH refined with riding coordinates:
 C21(H21), C35(H35), C36(H36), C49(H49), C100(H100), C101(H101), C122(H122),
 C126(H126)
7.b Secondary CH2 refined with riding coordinates:
 C102(H10A,H10B), C106(H10C,H10D), C117(H11J,H11K), C118(H11H,H11I), C124(H12A,
 H12B), C128(H12D,H12E)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8A), C9(H9), C11(H11),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C38(H38), C39(H39), C41(H41), C42(H42), C45(H45), C47(H47), C50(H50), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C70(H70),
  C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77),
 C78(H78), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86),
  C87(H87), C88(H88), C89(H89), C90(H90), C92(H92), C93(H93), C94(H94),
 C95(H95), C96(H96), C97(H97), C99(H99), C104(H104), C105(H105), C107(H107),
 C108(H108), C109(H109), C111(H111), C112(H112), C113(H113), C114(H114),
 C119(H119), C120(H120), C121(H121), C125(H125), C125(H12C), C127(H127)
7.d Idealised Me refined as rotating group:
 C98(H98A,H98B,H98C), C110(H11E,H11F,H11G), C116(H11B,H11C,H11D), C129(H12F,
 H12G,H12H)
7.e Idealised tetrahedral OH refined as rotating group:
 O22(H22A), O23(H23A)
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_shelx_res_checksum              12030
_shelx_hkl_checksum              43965