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_4135168
_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, 0.58(C9 H12)'
_chemical_formula_sum            'C11.25 H12 N3 O3 Zn'
_chemical_formula_weight         302.61
_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
_audit_creation_date             2018-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   26.5317(7)
_cell_length_b                   26.5317(7)
_cell_length_c                   10.1159(2)
_cell_measurement_reflns_used    11479
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4670
_cell_measurement_theta_min      3.0490
_cell_volume                     6166.9(3)
_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)'
_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   15.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   15.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   15.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   15.00    --  -20.00 -30.00  90.00  125
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0192529000
_diffrn_orient_matrix_UB_12      0.0109150000
_diffrn_orient_matrix_UB_13      -0.0103164000
_diffrn_orient_matrix_UB_21      0.0239133000
_diffrn_orient_matrix_UB_22      0.0288453000
_diffrn_orient_matrix_UB_23      0.0004636000
_diffrn_orient_matrix_UB_31      0.0030404000
_diffrn_orient_matrix_UB_32      -0.0013988000
_diffrn_orient_matrix_UB_33      -0.0693476000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            24557
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         2.659
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55562
_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    1.467
_exptl_crystal_description       needle
_exptl_crystal_F_000             2781
_exptl_crystal_preparation       'Solvent Exchnaged in Mesitylene'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 1093 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2824
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+19.8587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1198
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_full    0.846
_reflns_Friedel_fraction_max     0.789
_reflns_number_gt                2697
_reflns_number_total             2824
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnGlyPyr_Mesitylene_100K.cif
_cod_data_source_block           ZnGlyPyr_Mesitylene_100K
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4135168
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         ZnC6H5N3O5
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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
 C14B-C13B
 1.5 with sigma of 0.02
 C14B-C15B
 2.3 with sigma of 0.02
 C14B-C12B
 2.3 with sigma of 0.02
 C11B-C10B
 1.5 with sigma of 0.02
 C12B-C11B
 2.3 with sigma of 0.02
 C11B-C9B
 2.3 with sigma of 0.02
 C8B-C7B
 1.5 with sigma of 0.02
 C7B-C9B
 2.3 with sigma of 0.02
 C7B-C15B
 2.3 with sigma of 0.02
 C13A-C14A
 1.5 with sigma of 0.02
 C15A-C14A
 2.3 with sigma of 0.02
 C14A-C12A
 2.3 with sigma of 0.02
 C10A-C11A
 1.5 with sigma of 0.02
 C12A-C11A
 2.3 with sigma of 0.02
 C11A-C9A
 2.3 with sigma of 0.02
 C8A-C7A
 1.5 with sigma of 0.02
 C15A-C7A
 2.3 with sigma of 0.02
 C9A-C7A
 2.3 with sigma of 0.02
3. Restrained planarity
 C13B, C15B, C8B, C12B, C14B, C9B, C7B, C10B, C11B, C13B, C15B, C8B, C15B,
 C13B, C12B, C13B, C14B, C9B, C8B, C7B, C8B, C10B, C12B, C9B, C10B, C11B, C10B
 with sigma of 0.001
 C10A, C9A, C8A, C12A, C11A, C15A, C7A, C13A, C14A, C10A, C9A, C9A, C8A, C10A,
 C12A, C10A, C11A, C8A, C15A, C7A, C8A, C13A, C12A, C13A, C15A, C14A, C13A
 with sigma of 0.001
4. Rigid bond restraints
 O1, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O1 \\sim C6: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C6 \\sim O2: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C5 \\sim C6: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uiso(C11B) = Uiso(C15B) = Uiso(H15B) = Uiso(C13B) = Uiso(C8B) = Uiso(C12B) =
Uiso(C14B) = Uiso(C9B) = Uiso(C7B) = Uiso(H12B) = Uiso(C10B) = Uiso(H14D) =
Uiso(H14E) = Uiso(H14F) = Uiso(H9B) = Uiso(H7BA) = Uiso(H7BB) = Uiso(H7BC) =
Uiso(H11D) = Uiso(H11E) = Uiso(H11F) = Uiso(C15B) = Uiso(H15B) = Uiso(C13B) =
Uiso(C15B) = Uiso(C8B) = Uiso(C15B) = Uiso(C13B) = Uiso(C12B) = Uiso(C13B) =
Uiso(C14B) = Uiso(C9B) = Uiso(C8B) = Uiso(C7B) = Uiso(C8B) = Uiso(C12B) =
Uiso(H12B) = Uiso(C10B) = Uiso(C12B) = Uiso(C14B) = Uiso(H14D) = Uiso(C14B) =
Uiso(H14E) = Uiso(C14B) = Uiso(H14F) = Uiso(C9B) = Uiso(C10B) = Uiso(C9B) =
Uiso(H9B) = Uiso(C7B) = Uiso(H7BA) = Uiso(C7B) = Uiso(H7BB) = Uiso(C7B) =
Uiso(H7BC) = Uiso(C11B) = Uiso(C10B) = Uiso(C11B) = Uiso(H11D) = Uiso(C11B) =
Uiso(H11E) = Uiso(C11B) = Uiso(H11F)
Uiso(C10A) = Uiso(C9A) = Uiso(H9A) = Uiso(C8A) = Uiso(C12A) = Uiso(C11A) =
Uiso(C15A) = Uiso(C7A) = Uiso(H12A) = Uiso(C13A) = Uiso(H11A) = Uiso(H11B) =
Uiso(H11C) = Uiso(H15A) = Uiso(H7AA) = Uiso(H7AB) = Uiso(H7AC) = Uiso(C14A) =
Uiso(H14A) = Uiso(H14B) = Uiso(H14C) = Uiso(C9A) = Uiso(H9A) = Uiso(C10A) =
Uiso(C9A) = Uiso(C9A) = Uiso(C8A) = Uiso(C10A) = Uiso(C12A) = Uiso(C10A) =
Uiso(C11A) = Uiso(C8A) = Uiso(C15A) = Uiso(C7A) = Uiso(C8A) = Uiso(C12A) =
Uiso(H12A) = Uiso(C13A) = Uiso(C12A) = Uiso(C11A) = Uiso(H11A) = Uiso(C11A) =
Uiso(H11B) = Uiso(C11A) = Uiso(H11C) = Uiso(C13A) = Uiso(C15A) = Uiso(C15A) =
Uiso(H15A) = Uiso(C7A) = Uiso(H7AA) = Uiso(C7A) = Uiso(H7AB) = Uiso(C7A) =
Uiso(H7AC) = Uiso(C14A) = Uiso(C13A) = Uiso(C14A) = Uiso(H14A) = Uiso(C14A) =
Uiso(H14B) = Uiso(C14A) = Uiso(H14C)
6. Others
 Fixed Sof: C9A(0.33333) H9A(0.33333) C10A(0.33333) C12A(0.33333)
 H12A(0.33333) C13A(0.33333) C15A(0.33333) H15A(0.33333) C8A(0.33333)
 C11A(0.33333) H11A(0.33333) H11B(0.33333) H11C(0.33333) C14A(0.33333)
 H14A(0.33333) H14B(0.33333) H14C(0.33333) C7A(0.33333) H7AA(0.33333)
 H7AB(0.33333) H7AC(0.33333) C15B(0.25) H15B(0.25) C13B(0.25) C12B(0.25)
 H12B(0.25) C10B(0.25) C9B(0.25) H9B(0.25) C8B(0.25) C7B(0.25) H7BA(0.25)
 H7BB(0.25) H7BC(0.25) C11B(0.25) H11D(0.25) H11E(0.25) H11F(0.25) C14B(0.25)
 H14D(0.25) H14E(0.25) H14F(0.25)
7.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
7.b Me refined with riding coordinates:
 C11A(H11A,H11B,H11C), C14A(H14A,H14B,H14C), C7A(H7AA,H7AB,H7AC), C7B(H7BA,
 H7BB,H7BC), C11B(H11D,H11E,H11F), C14B(H14D,H14E,H14F)
7.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C3(H3A), C9A(H9A), C12A(H12A), C15A(H15A), C15B(H15B),
 C12B(H12B), C9B(H9B)
7.d Fitted hexagon refined as free rotating group:
 C9A(C10A,C12A,C13A,C15A,C8A), C15B(C13B,C12B,C10B,C9B,C8B)
;
_shelx_res_checksum              64820
_shelx_hkl_checksum              89878
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.612
_oxdiff_exptl_absorpt_empirical_full_min 0.692