Revelation of the chiral recognition of alanine and leucine in an l-phenylalanine-based metal-organic framework.
Ma, Xue; Zhang, Yanhao; Gao, Yu; Li, Xinglin; Wang, Cuijie; Yuan, Hang; Yu, Ajuan; Zhang, Shusheng; Cui, Yuanyuan; Chemical communications (Cambridge, England) 56 (2020) 1034–1037; doi:10.1039/c9cc05912a

data_7124022
_publ_section_title
;
 Revelation of the chiral recognition of alanine and leucine in an
 l-phenylalanine-based metal-organic framework.
;
_journal_issue                   7
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1034
_journal_page_last               1037
_journal_paper_doi               10.1039/c9cc05912a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C20.5 H17.5 N3 O2 Zn'
_chemical_formula_sum            'C21.5 H20.5 N3 O2.5 Zn'
_chemical_formula_weight         426.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-28
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-07-08 deposited with the CCDC.    2019-08-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.109(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4932(17)
_cell_length_b                   25.8736(11)
_cell_length_c                   9.6520(4)
_cell_measurement_reflns_used    6705
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.0410
_cell_measurement_theta_min      3.1390
_cell_volume                     5053.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -11.00  89.00   0.50    4.14    --   -0.40  38.00   0.00  200
  2  \w     36.00  64.00   0.50    4.14    --   -0.40  38.00-180.00   56
  3  \w     37.00  63.00   0.50    4.14    --   -0.40  38.00-150.00   52
  4  \w    -20.00  78.00   0.50    4.14    --   -0.40  38.00 -90.00  196
  5  \w     39.00  64.00   0.50    4.14    --   -0.40  38.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0283314000
_diffrn_orient_matrix_UB_12      -0.0156075000
_diffrn_orient_matrix_UB_13      -0.0202898000
_diffrn_orient_matrix_UB_21      0.0125007000
_diffrn_orient_matrix_UB_22      -0.0075969000
_diffrn_orient_matrix_UB_23      -0.0613653000
_diffrn_orient_matrix_UB_31      0.0164705000
_diffrn_orient_matrix_UB_32      -0.0212125000
_diffrn_orient_matrix_UB_33      0.0368560000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            28127
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.774
_diffrn_reflns_theta_min         2.013
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.676
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         6540
_refine_ls_number_restraints     176
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.1005
_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^)+(0.3000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3675
_refine_ls_wR_factor_ref         0.3893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4245
_reflns_number_total             6540
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05912a2.cif
_cod_data_source_block           20180205e2-1
_cod_depositor_comments          'Adding full bibliography for 7124022.cif.'
_cod_original_formula_sum        'C21.50 H20.50 N3 O2.50 Zn'
_cod_database_code               7124022
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         'Zn C H F O N S'
_chemical_oxdiff_usercomment     'C H O'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.826
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C9-C0AA
 1.4 with sigma of 0.02
 C0AA-C00J
 1.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C12 \\sim C20 \\sim C14 \\sim C13 \\sim C9 \\sim C10: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C00J) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(N008) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O004) \\sim Ueq, Uanis(C00J) \\sim Ueq, Uanis(O002) \\sim Ueq,
Uanis(N008) \\sim Ueq, Uanis(Zn01) \\sim Ueq, Uanis(N003) \\sim Ueq,
Uanis(C00C) \\sim Ueq, Uanis(C00I) \\sim Ueq, Uanis(C00A) \\sim Ueq,
Uanis(C00G) \\sim Ueq, Uanis(C009) \\sim Ueq, Uanis(C00B) \\sim Ueq,
Uanis(C0AA) \\sim Ueq, Uanis(C00F) \\sim Ueq, Uanis(C00E) \\sim Ueq,
Uanis(C007) \\sim Ueq, Uanis(C00L) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: H12(0.5) C0AA(0.5) H0AB(0.5) H0AA(0.5)
5.a Ternary CH refined with riding coordinates:
 C00J(H00J)
5.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AB,H0AA)
5.c Aromatic/amide H refined with riding coordinates:
 C007(H007), N008(H008), C00A(H00A), C00B(H00B), C00C(H00C), C00D(H00D),
 C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00I), C00L(H00L), C12(H12), C10(H10),
  C13(H13), C14(H14), C20(H20)
5.d Fitted hexagon refined as free rotating group:
 C12(C9,C10,C13,C14,C20)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              14519
_shelx_fab_checksum              93450
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.265
_oxdiff_exptl_absorpt_empirical_full_min 0.425