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_4135187
_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         'Zn C7 H7 N3 O3, 0.15(C5 H12 O2)'
_chemical_formula_sum            'C7.74 H8.77 N3 O3.29 Zn'
_chemical_formula_weight         261.86
_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             2019-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   28.8315(4)
_cell_length_b                   28.8315(4)
_cell_length_c                   10.1304(2)
_cell_measurement_reflns_used    20866
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4930
_cell_measurement_theta_min      2.1200
_cell_volume                     7292.8(2)
_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    'ShelXT (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
;
_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      -0.0039552000
_diffrn_orient_matrix_UB_12      -0.0262754000
_diffrn_orient_matrix_UB_13      0.0053203000
_diffrn_orient_matrix_UB_21      0.0280721000
_diffrn_orient_matrix_UB_22      0.0105132000
_diffrn_orient_matrix_UB_23      -0.0033558000
_diffrn_orient_matrix_UB_31      0.0016644000
_diffrn_orient_matrix_UB_32      0.0025237000
_diffrn_orient_matrix_UB_33      0.0697281000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30688
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         2.170
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89304
_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    1.073
_exptl_crystal_description       needle
_exptl_crystal_F_000             2386
_exptl_crystal_preparation       'Solvent Exchnage in 1,5-Pentanediol'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.145
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
;
 Flack x determined using 2401 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         6475
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0495
_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^)+(0.1065P)^2^+27.4709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.742
_reflns_Friedel_fraction_full    0.795
_reflns_Friedel_fraction_max     0.741
_reflns_number_gt                6074
_reflns_number_total             6475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_15PD_100K.cif
_cod_data_source_block           ZnAlaPyr_15PD_100K
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135187
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         ZnC7H7N3O5
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.583
_reflns_odcompleteness_completeness 99.95
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1AA-C1AA
 1.4 with sigma of 0.02
 C4AA-O0AA
 1.4 with sigma of 0.02
 C3AA-C4AA
 1.54 with sigma of 0.02
 C3AA-C5AA
 1.54 with sigma of 0.02
 C6AA-C5AA
 1.54 with sigma of 0.02
 C1AA-C6AA
 1.54 with sigma of 0.02
 N3-C6 = C1AA-C5AA
 2.5 with sigma of 0.02
 C6AA-C3AA
 2.5 with sigma of 0.02
 C5AA-C4AA
 2.5 with sigma of 0.02
 C6AA-O1AA
 2.4 with sigma of 0.02
 O0AA-C3AA
 2.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O0AA \\sim C4AA \\sim C3AA \\sim C5AA \\sim C6AA \\sim C1AA \\sim O1AA: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C3AA)=Sof(H3AA)=Sof(H3AB)=Sof(O0AA)=Sof(H0AA)=Sof(C1AA)=Sof(H1AA)=
 Sof(H1AB)=Sof(O1AA)=Sof(H1AC)=Sof(C4AA)=Sof(H4AA)=Sof(H4AB)=Sof(C5AA)=
 Sof(H5AA)=Sof(H5AB)=Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C3AA(H3AA,H3AB), C1AA(H1AA,H1AB), C4AA(H4AA,H4AB), C5AA(H5AA,H5AB), C6AA(H6AA,
 H6AB)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C8(H8), C2(H2), C1(H1), C9(H9)
5.d Tetrahedral OH refined with riding coordinates:
 O0AA(H0AA), O1AA(H1AC)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              49934
_shelx_hkl_checksum              42126
_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 1.238
_oxdiff_exptl_absorpt_empirical_full_min 0.872