Chiral DHIP-Based Metal-Organic Frameworks for Enantioselective Recognition and Separation.
Zhang, Jie; Li, Zijian; Gong, Wei; Han, Xing; Liu, Yan; Cui, Yong; Inorganic chemistry 55 (2016) 7229–7232; doi:10.1021/acs.inorgchem.6b00894

data_4348027
_publ_section_title
;
 Chiral DHIP-Based Metal-Organic Frameworks for Enantioselective
 Recognition and Separation.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7229
_journal_page_last               7232
_journal_paper_doi               10.1021/acs.inorgchem.6b00894
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C70 H48 N8 O12 Zn3'
_chemical_formula_sum            'C70 H48 N8 O12 Zn3'
_chemical_formula_weight         1389.27
_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
_audit_creation_date             2014-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.856(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.719(3)
_cell_length_b                   19.469(2)
_cell_length_c                   20.835(2)
_cell_measurement_temperature    298(2)
_cell_volume                     8337.2(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            107863
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         1.575
_exptl_absorpt_coefficient_mu    0.910
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 4024 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.052(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     814
_refine_ls_number_reflns         19100
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0814P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                10707
_reflns_number_total             19100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00894_si_002.cif
_cod_data_source_block           a_sq
_cod_original_cell_volume        8337.1(17)
_cod_database_code               4348027
_shelxl_version_number           2014/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C62, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C23, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O10 \\sim C70: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C63 \\sim O12: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C65 \\sim C64: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C28 \\sim N5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C27 \\sim C26: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C62 \\sim O8: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C20 \\sim C19: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C21 \\sim N4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C23 \\sim C19: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C23 \\sim C22: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C28 \\sim N5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C28 \\sim C27: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
Zn3 \\sim O7: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
Zn3 \\sim O5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
4.a Ternary CH refined with riding coordinates:
 C35(H35), C12(H12)
4.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C53(H53), C4(H4), C15(H15), C30(H30), C41(H41), C11(H11), C52(H52),
 C37(H37), C50(H50), C10(H10), C7(H7), C33(H33), C16(H16), C8(H8), C49(H49),
 C2(H2), C66(H66), C65(H65), C57(H57), C31(H31), C61(H61), C58(H58), C60(H60),
 C23(H23), C22(H22), C21(H21), C20(H20), C28(H28), C24(H24), C25(H25), C27(H27),
  C40(H40), C38(H38), C44(H44), C45(H45), C5(H5), C43(H43), C46(H46), C1(H1),
 C68(H68), C69(H69)
4.d Fitted hexagon refined as free rotating group:
 C23(C22,N4,C21,C20,C19), C28(N5,C24,C25,C26,C27)
;
_shelx_res_checksum              33480
_shelx_hkl_checksum              78251
_shelx_fab_checksum              62180
_olex2_submission_special_instructions 'No special instructions were received'