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_4135190
_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, 1.08(C2 H3 F3 O)'
_chemical_formula_sum            'C8.17 H8.25 F3.25 N3 O4.08 Zn'
_chemical_formula_weight         340.88
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-31
_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                   27.4717(8)
_cell_length_b                   27.4717(8)
_cell_length_c                   10.1111(2)
_cell_measurement_reflns_used    14535
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.5250
_cell_measurement_theta_min      2.9540
_cell_volume                     6608.5(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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_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   10.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   10.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   10.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   10.00    --  -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      0.0196732000
_diffrn_orient_matrix_UB_12      -0.0092981000
_diffrn_orient_matrix_UB_13      -0.0090347000
_diffrn_orient_matrix_UB_21      0.0207477000
_diffrn_orient_matrix_UB_22      0.0276038000
_diffrn_orient_matrix_UB_23      -0.0185643000
_diffrn_orient_matrix_UB_31      0.0083953000
_diffrn_orient_matrix_UB_32      0.0063607000
_diffrn_orient_matrix_UB_33      0.0670177000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32444
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.501
_diffrn_reflns_theta_min         2.966
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64884
_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    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             3063
_exptl_crystal_preparation       'Solvent Exchange in TrifluoroEthanol'
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.039
_refine_diff_density_max         1.482
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Flack x determined using 1246 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3833
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1363P)^2^+19.7668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.1903
_reflns_Friedel_coverage         0.701
_reflns_Friedel_fraction_full    0.821
_reflns_Friedel_fraction_max     0.706
_reflns_number_gt                3468
_reflns_number_total             3833
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnGlyPyr_CF3CH2OH_100K.cif
_cod_data_source_block           ZnGlyPyr_CF3CH2OH_100K
_cod_original_cell_volume        6608.4(4)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4135190
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C8 H8 N3 O3'
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.656
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.43
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 F2-C8
 1.34 with sigma of 0.02
 C8-C7
 1.5 with sigma of 0.02
 F1-C8
 1.34 with sigma of 0.02
 C8-F3
 1.34 with sigma of 0.02
 C7-O4
 1.25 with sigma of 0.02
 C8-O4
 2.4 with sigma of 0.02
 C10-C9
 1.5 with sigma of 0.02
 C9-F6
 1.34 with sigma of 0.02
 C9-F5
 1.34 with sigma of 0.02
 C9-F4
 1.34 with sigma of 0.02
 F4-C10
 2.4 with sigma of 0.02
 C10-F6
 2.4 with sigma of 0.02
 C10-F5
 2.4 with sigma of 0.02
 O5-C9
 2.4 with sigma of 0.02
 O5-C10
 1.4 with sigma of 0.02
 F6-F5
 2.15 with sigma of 0.02
 F6-F4
 2.15 with sigma of 0.02
 F4-F5
 2.15 with sigma of 0.02
 F3-C8 \\sim F1-C8 \\sim F2-C8
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F2 \\sim C8 \\sim F1 \\sim F3 \\sim C7 \\sim O4: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04
4. Others
 Sof(F2)=Sof(F1)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(O4)=Sof(H4)=Sof(F3)=
 FVAR(1)
 Sof(C9)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(O5)=Sof(H5)=Sof(F4)=Sof(F5)=Sof(F6)=
 FVAR(2)
5.a Riding coordinates:
 O4(H4)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), N3(H3A)
5.d Tetrahedral OH refined with riding coordinates:
 O5(H5)
;
_shelx_res_checksum              21036
_shelx_hkl_checksum              76452
_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 1.586
_oxdiff_exptl_absorpt_empirical_full_min 0.713