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_4348028
_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 Cd3 N8 O12'
_chemical_formula_sum            'C70 H48 Cd3 N8 O12'
_chemical_formula_weight         1530.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6274(18)
_cell_length_b                   19.663(4)
_cell_length_c                   32.678(6)
_cell_measurement_reflns_used    2989
_cell_measurement_temperature    259(2)
_cell_measurement_theta_max      21.67
_cell_measurement_theta_min      2.39
_cell_volume                     7471(2)
_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      259.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.1115
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            18498
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         1.620
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.906
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.500
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 2588 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         14829
_refine_ls_number_restraints     215
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1274P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2327
_reflns_Friedel_coverage         0.635
_reflns_Friedel_fraction_full    0.805
_reflns_Friedel_fraction_max     0.739
_reflns_number_gt                8307
_reflns_number_total             14829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00894_si_003.cif
_cod_data_source_block           p212121_sq
_cod_database_code               4348028
_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. Restrained distances
 O12-O5
 2.01 with sigma of 0.02
 O5-C55 = O12-C55
 1.21 with sigma of 0.02
 O12-C61 \\sim C57-O5
 with sigma of 0.02
3. Restrained planarity
 C57, C56, C61, C55, O5, O12
 with sigma of 0.1
4. Rigid bond restraints
 C24, N8, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C54, Cd3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8, O7, C62, C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C62, O8, C59, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C1, C3, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O12, C55, O5, C56, C61, C57, Cd1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C55, O12, C56, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C63, O10, Cd2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C60, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C60, C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C48, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C48, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C45, N5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C45, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O12, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C24 \\sim C27 \\sim N8: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O1 \\sim C54 \\sim Cd3: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O8 \\sim O7 \\sim C62 \\sim C59: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C3 \\sim C2 \\sim C1 \\sim N1: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C61 \\sim C56 \\sim C57 \\sim C55 \\sim O12 \\sim O5 \\sim Cd1: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
O10 \\sim C63 \\sim Cd2: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C60 \\sim C61: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C60 \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C48 \\sim C49: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C48 \\sim C53: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C43 \\sim C42: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C44 \\sim N5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C70 \\sim C67: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C21 \\sim C20: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
N4 \\sim C21: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C38 \\sim C39: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C37 \\sim C36: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C44 \\sim N5: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C1 \\sim N1: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C2 \\sim C3: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O12 \\sim C55: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
O5 \\sim C55: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
C55 \\sim O5: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.08
Uanis(C62) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C55) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6.a Ternary CH refined with riding coordinates:
 C35(H35), C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C34(H34A,H34B)
6.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C46(H46), C5(H5), C44(H44), C10(H10), C69(H69), C37(H37), C45(H45),
 C8(H8), C22(H22), C57(H57), C58(H58), C60(H60), C61(H61), C40(H40), C43(H43),
 C68(H68), C23(H23), C24(H24), C27(H27), C26(H26), C25(H25), C66(H66), C41(H41),
  C2(H2), C32(H32), C4(H4), C65(H65), C33(H33), C50(H50), C49(H49), C53(H53),
 C52(H52), C1(H1), C15(H15), C17(H17), C18(H18), C14(H14), C30(H30), C38(H38),
 C20(H20), C21(H21)
6.d Fitted hexagon refined as free rotating group:
 C56(C57,C58,C59,C60,C61), C24(C27,C28,C26,C25,N8), C51(C50,C49,C48,C53,C52),
 C15(C16,C17,C18,C13,C14)
;
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_shelx_hkl_checksum              4886
_shelx_fab_checksum              85323
_olex2_submission_special_instructions 'No special instructions were received'