Amino Acid Residues Determine the Response of Flexible Metal-Organic Frameworks to Guests.
Yan, Yong; Carrington, Elliot J.; Pétuya, Rémi; Whitehead, George F. S.; Verma, Ajay; Hylton, Rebecca K.; Tang, Chiu C.; Berry, Neil G.; Darling, George R.; Dyer, Matthew S.; Antypov, Dmytro; Katsoulidis, Alexandros P.; Rosseinsky, Matthew J.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c03853

data_4135179
_publ_section_title
;
 Amino Acid Residues Determine the Response of Flexible Metal-Organic
 Frameworks to Guests.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c03853
_journal_year                    2020
_chemical_formula_moiety         'C6 H5 N3 O3 Zn, 1.21(C6 H6)'
_chemical_formula_sum            'C13.24 H12.24 N3 O3 Zn'
_chemical_formula_weight         326.71
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   29.5677(11)
_cell_length_b                   29.5677(11)
_cell_length_c                   10.1237(3)
_cell_measurement_reflns_used    8486
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.9840
_cell_measurement_theta_min      2.3840
_cell_volume                     7664.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -110.00  15.00   1.00   30.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   30.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   30.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   30.00    --  -20.00 -30.00  90.00  125
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Rigaku Mo Rotating Anode Source With Saturn Detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0010138000
_diffrn_orient_matrix_UB_12      -0.0242185000
_diffrn_orient_matrix_UB_13      -0.0106015000
_diffrn_orient_matrix_UB_21      -0.0258499000
_diffrn_orient_matrix_UB_22      -0.0134046000
_diffrn_orient_matrix_UB_23      0.0250770000
_diffrn_orient_matrix_UB_31      -0.0098743000
_diffrn_orient_matrix_UB_32      -0.0012619000
_diffrn_orient_matrix_UB_33      -0.0645534000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1016
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26341
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.023
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.386
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.450
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       needle
_exptl_crystal_F_000             3000
_exptl_crystal_preparation       'Solvent Exchnage in Benzene'
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Flack x determined using 950 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2920
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0767
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0926P)^2^+19.1218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1549
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    0.945
_reflns_Friedel_fraction_max     0.945
_reflns_number_gt                2433
_reflns_number_total             2920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnGlyPyr_Benzene_100K.cif
_cod_data_source_block           ZnGlyPyr_Benzene_100K
_cod_original_cell_volume        7664.8(6)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4135179
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C8 H8 N3 O3'
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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. Uiso/Uaniso restraints and constraints
C8C \\sim C7C \\sim C12C \\sim C11C \\sim C10C \\sim C9C: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04
C8A \\sim C7A \\sim C12A \\sim C11A \\sim C10A \\sim C9A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.04
Uanis(N1) = Uanis(N2)
3. Others
 Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=FVAR(1)
 Sof(C12B)=Sof(H12B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9B)=
 Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=FVAR(2)
 Sof(C10C)=Sof(H10C)=Sof(C11C)=Sof(H11C)=Sof(C12C)=Sof(H12C)=Sof(C7C)=Sof(H7C)=
 Sof(C8C)=Sof(H8C)=Sof(C9C)=Sof(H9C)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), N3(H3), C12B(H12B), C7B(H7B), C8B(H8B), C9B(H9B), C10B(H10B),
 C11B(H11B), C10C(H10C), C11C(H11C), C12C(H12C), C7C(H7C), C8C(H8C), C9C(H9C),
 C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A)
4.c Fitted hexagon refined as free rotating group:
 C12B(C7B,C8B,C9B,C10B,C11B), C10C(C11C,C12C,C7C,C8C,C9C), C7A(C8A,C9A,C10A,
 C11A,C12A)
;
_shelx_res_checksum              31967
_shelx_hkl_checksum              88339
_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 1.257
_oxdiff_exptl_absorpt_empirical_full_min 0.800