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_4135166
_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_absolute_configuration syn
_chemical_formula_moiety         'C7 H7 N3 O3 Zn, 0.21(C4 H8 O)'
_chemical_formula_sum            'C7.83 H8.66 N3 O3.21 Zn'
_chemical_formula_weight         261.50
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   28.6590(13)
_cell_length_b                   28.6590(13)
_cell_length_c                   10.1251(4)
_cell_measurement_reflns_used    17059
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.5840
_cell_measurement_theta_min      2.1550
_cell_volume                     7202.0(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    'XT (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    5.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00    5.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00    5.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00    5.00    --  -20.00 -30.00  90.00  125
  5  \w    -50.00  70.00   1.00    5.00    --  -20.00  68.00   0.00  120
  6  \w    -50.00  70.00   1.00    5.00    --  -20.00  68.00 120.00  120
;
_diffrn_measurement_device
'Rigaku Mo Source Rotating Anode 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      -0.0136510000
_diffrn_orient_matrix_UB_12      0.0149496000
_diffrn_orient_matrix_UB_13      -0.0031789000
_diffrn_orient_matrix_UB_21      -0.0215727000
_diffrn_orient_matrix_UB_22      -0.0217501000
_diffrn_orient_matrix_UB_23      -0.0335420000
_diffrn_orient_matrix_UB_31      -0.0125556000
_diffrn_orient_matrix_UB_32      -0.0110573000
_diffrn_orient_matrix_UB_33      0.0614095000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_av_unetI/netI     0.0496
_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       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            36260
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62519
_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    1.085
_exptl_crystal_description       needle
_exptl_crystal_F_000             2382
_exptl_crystal_preparation       'Solvent Exchange in THF'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.195
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Flack x determined using 2309 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.050(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5553
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0780
_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^)+(0.1250P)^2^+93.4628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2261
_reflns_Friedel_coverage         0.971
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                5374
_reflns_number_total             5553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_THF_100K.cif
_cod_data_source_block           ZnAlaPyr_THF_100K
_cod_original_cell_volume        7202.0(7)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135166
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.941
_shelx_estimated_absorpt_t_min   0.792
_reflns_odcompleteness_completeness 98.09
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.74
_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 C(H,H,H) groups
2. Restrained distances
 C17-C16
 1.52 with sigma of 0.02
 C16-O7
 1.42 with sigma of 0.02
 C17-C18
 1.52 with sigma of 0.02
 C16-C18
 2.3 with sigma of 0.02
 O7-C15
 1.42 with sigma of 0.02
 C18-C15
 1.52 with sigma of 0.02
 C17-C15
 2.3 with sigma of 0.02
3. Rigid bond restraints
 N3, C6, C5, C7, N2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zn2, N2, N3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
N2 \\sim N3 \\sim C7 \\sim C6 \\sim C5: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
N3 \\sim C6 \\sim C5 \\sim C7 \\sim N2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Zn2 \\sim N2 \\sim N3: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C15 \\sim C18 \\sim C17 \\sim C16 \\sim O7: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Others
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(O7)=Sof(C15)=
 Sof(H15A)=Sof(H15B)=Sof(C18)=Sof(H18A)=Sof(H18B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C16(H16A,H16B), C15(H15A,H15B), C18(H18A,H18B)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), C6(H6), C14(H14), C13(H13), C7(H7)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              35171
_shelx_hkl_checksum              70046
_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 1.781
_oxdiff_exptl_absorpt_empirical_full_min 0.601