Chiral metal‒organic frameworks constructed from four-fold helical chain SBUs for enantioselective recognition of α-hydroxy/amino acids
Yao, Ru-Xin; Fu, Huan-Huan; Yu, Bo; Zhang, Xian-Ming; Inorganic Chemistry Frontiers 5 (2018) 153–; doi:10.1039/C7QI00615B

data_4349789
_publ_section_title
;
 Chiral metal--organic frameworks constructed from four-fold helical chain
 SBUs for enantioselective recognition of \a-hydroxy/amino acids
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              153
_journal_paper_doi               10.1039/C7QI00615B
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         '0.25(C70 H24 Co4 Ni4 O40)'
_chemical_formula_sum            'C17.5 H6 Co Ni O10'
_chemical_formula_weight         493.86
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
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Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
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2017-08-01 deposited with the CCDC.
2017-11-09 downloaded from the CCDC.
;
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2512(5)
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_cell_length_c                   12.1084(5)
_cell_measurement_reflns_used    1622
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8950
_cell_measurement_theta_min      4.6520
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
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_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -76.00  -38.00   1.0000   18.2050
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -60.0000 38

  2 omega  -73.00  -48.00   1.0000   18.2050
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  120.0000 25

  3 omega   16.00   60.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   19.0000 -180.0000 44

  4 omega  -13.00   74.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  -90.0000 87

  5 omega   65.00   93.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000  -30.0000 28

  6 omega   41.00   68.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  -30.0000 27

  7 omega  112.00  138.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000  150.0000 26

  8 omega  100.00  126.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -60.0000 26

  9 omega   59.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000  150.0000 25

 10 omega  150.00  176.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -60.0000 26

 11 omega  103.00  165.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000    0.0000 62

 12 omega  108.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000  -30.0000 26

 13 omega   39.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   30.0000 25

 14 omega   49.00   86.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000   60.0000 37

 15 omega  141.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   50.0000  150.0000 33

 16 omega   49.00   74.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000 -120.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0169808000
_diffrn_orient_matrix_UB_12      0.0839219000
_diffrn_orient_matrix_UB_13      -0.0674682000
_diffrn_orient_matrix_UB_21      -0.0752812000
_diffrn_orient_matrix_UB_22      0.0246868000
_diffrn_orient_matrix_UB_23      0.0788468000
_diffrn_orient_matrix_UB_31      0.0651740000
_diffrn_orient_matrix_UB_32      0.0506798000
_diffrn_orient_matrix_UB_33      0.0734296000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3197
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.494
_diffrn_reflns_theta_min         4.099
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.791
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72020
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.2
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_platon_squeeze_details
;
;
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_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0944
_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^)+(0.1960P)^2^+20.8660P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2659
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_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                1152
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qi00615b2.cif
_cod_data_source_block           2
_cod_original_cell_volume        2816.4(2)
_cod_original_formula_sum        'C17.50 H6 Co Ni O10'
_cod_database_code               4349789
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 96.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Ni01, Co}
3. Uiso/Uaniso restraints and constraints
Uanis(Ni01) = Uanis(Co)
4. Others
 Fixed Sof: Ni01(0.25) Co(0.25) C6(0.375)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'