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_4129483
_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
'C46 H38 Co2 N6 O6, 2(N O3), 1.53(C6 H5 N O2)'
_chemical_formula_sum            'C55.18 H45.65 Co2 N9.53 O15.06'
_chemical_formula_weight         1201.14
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0870(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2292(3)
_cell_length_b                   24.7002(7)
_cell_length_c                   11.4243(3)
_cell_measurement_reflns_used    8064
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.94
_cell_measurement_theta_min      3.57
_cell_volume                     2886.50(14)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0660
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24845
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        66.220
_diffrn_reflns_theta_max         66.768
_diffrn_reflns_theta_min         3.869
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.129
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1018 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.8029.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 3359 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.069(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         9647
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0751
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+5.1842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1967
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.916
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                8427
_reflns_number_total             9647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06760_si_002.cif
_cod_data_source_block           CMOM_1S_NB
_cod_database_code               4129483
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.715
_shelx_estimated_absorpt_t_min   0.578
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O13-H13 = O17-H17
 0.88 with sigma of 0.02
 O17-H17 = O13-H13
 0.88 with sigma of 0.02
 O7-N2 = O8-N2 = O29A-N50 = O60-N50 = O59-N49 = O57-N49 = O58-N8 = O6-N8
 1.23 with sigma of 0.02
 N2-C7 = N50-C92 = N49-C1H = N8-C1G
 1.47 with sigma of 0.02
 C40-H13
 1.889034 with sigma of 0.02
 C38-H17
 1.897478 with sigma of 0.02
 O7-O8 = O60-O29A = O59-O57 = O58-O6
 2.17 with sigma of 0.04
 O7-C7 = O60-C92 = O57-C1H = O6-C1G
 2.31 with sigma of 0.04
 O58-C1G = C1H-O59 = C92-O29A = C7-O8
 2.31 with sigma of 0.04
 N2-C29
 2.45 with sigma of 0.04
 N8-C1C = C96-N50 = N49-C1J = C7-O8
 2.45 with sigma of 0.04
 N2-C13 = N50-C93 = N49-C1I = C1F-N8
 2.45 with sigma of 0.04
3. Restrained planarity
 O7, N2, O8, C7
 with sigma of 0.02
 C13, C7, C29, N2
 with sigma of 0.02
 C1G, O58, N8, O6
 with sigma of 0.02
 C1C, C1G, N8, C1F
 with sigma of 0.02
 O59, N49, C1H, O57
 with sigma of 0.02
 N49, C1H, C1I, C1J
 with sigma of 0.02
 O29A, N50, O60, C92
 with sigma of 0.02
 N50, C92, C96, C93
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C92 \\sim C93 \\sim C96 \\sim N50 \\sim C94 \\sim O60 \\sim O29A \\sim C17A
\\sim C95 \\sim C29 \\sim N2 \\sim O7 \\sim O8 \\sim C7 \\sim C13 \\sim C9
\\sim C5 \\sim C4 \\sim C1E \\sim C1H \\sim C1I \\sim C1J \\sim N49 \\sim C1D
\\sim O57 \\sim O59 \\sim C17 \\sim O58 \\sim C1G \\sim C1C \\sim C1F \\sim N8
\\sim C1A \\sim C15 \\sim O6 \\sim C1B: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uiso(C17A) = Uiso(C17)
Uiso(C29) = Uiso(O29A)
5. Others
 Sof(C92)=Sof(C93)=Sof(H93)=Sof(C94)=Sof(H94)=Sof(C17A)=Sof(H17B)=Sof(C95)=
 Sof(H95)=Sof(C96)=Sof(H96)=Sof(N50)=Sof(O60)=Sof(O29A)=FVAR(1)
 Sof(C1H)=Sof(C1I)=Sof(H1I)=Sof(C1D)=Sof(H1D)=Sof(C17)=Sof(H17A)=Sof(C1E)=
 Sof(H1E)=Sof(C1J)=Sof(H1J)=Sof(N49)=Sof(O57)=Sof(O59)=FVAR(2)
 Sof(C1G)=Sof(C1C)=Sof(H1C)=Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(H1B)=Sof(C15)=
 Sof(H15)=Sof(C1F)=Sof(H1F)=Sof(O6)=Sof(N8)=Sof(O58)=FVAR(3)
 Sof(N2)=Sof(O7)=Sof(O8)=Sof(C29)=Sof(H29)=Sof(C9)=Sof(H9)=Sof(C4)=Sof(H4)=
 Sof(C5)=Sof(H5)=Sof(C13)=Sof(H13A)=Sof(C7)=FVAR(4)
6.a Ternary CH refined with riding coordinates:
 C38(H38), C40(H40)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C16(H16), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C30(H30), C31(H31), C32(H32), C33(H33), C41(H41), C46(H46),
  C49(H49), C50(H50), C57(H57), C59(H59), C61(H61), C62(H62), C65(H65),
 C67(H67), C68(H68), C70(H70), C75(H75), C91(H91), C72(H72), C1(H1), C6(H6),
 C3(H3), C11(H11), C2(H2), C1C(H1C), C1A(H1A), C1B(H1B), C15(H15), C1F(H1F),
 C29(H29), C9(H9), C4(H4), C5(H5), C13(H13A), C1I(H1I), C1D(H1D), C17(H17A),
 C1E(H1E), C1J(H1J), C93(H93), C94(H94), C17A(H17B), C95(H95), C96(H96)
6.c Fitted hexagon refined as free rotating group:
 C1G(C1C,C1A,C1B,C15,C1F), C29(C9,C4,C5,C13,C7), C1H(C1I,C1D,C17,C1E,C1J),
 C92(C93,C94,C17A,C95,C96)
;
_shelx_res_checksum              51523
_shelx_hkl_checksum              49836