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_4135170
_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, 0.91(C3 H7 N O)'
_chemical_formula_sum            'C9.73 H13.38 N3.91 O3.91 Zn'
_chemical_formula_weight         313.16
_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             2018-06-20
_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                   28.8656(10)
_cell_length_b                   28.8656(10)
_cell_length_c                   10.1277(3)
_cell_measurement_reflns_used    18805
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4390
_cell_measurement_theta_min      2.1490
_cell_volume                     7308.1(4)
_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   -120.00   5.00   0.50   15.00    --  -30.00 -68.00   0.00  250
  2  \w   -120.00   5.00   0.50   15.00    --  -30.00 -68.00  60.00  250
  3  \w   -120.00   5.00   0.50   15.00    --  -30.00 -68.00 120.00  250
  4  \w   -120.00   5.00   0.50   15.00    --  -30.00 -68.00 180.00  250
  5  \w   -120.00   5.00   0.50   15.00    --  -30.00 -68.00 240.00  250
  6  \w   -120.00   5.00   0.50   15.00    --  -30.00 -68.00 300.00  250
  7  \w   -120.00  60.00   0.50   15.00    --  -30.00   0.00   0.00  360
  8  \w   -120.00  60.00   0.50   15.00    --  -30.00   0.00 180.00  360
;
_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      0.0282653000
_diffrn_orient_matrix_UB_12      0.0142110000
_diffrn_orient_matrix_UB_13      0.0035686000
_diffrn_orient_matrix_UB_21      0.0001954000
_diffrn_orient_matrix_UB_22      -0.0245273000
_diffrn_orient_matrix_UB_23      -0.0028686000
_diffrn_orient_matrix_UB_31      0.0014983000
_diffrn_orient_matrix_UB_32      0.0017842000
_diffrn_orient_matrix_UB_33      -0.0698427000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1125
_diffrn_reflns_av_unetI/netI     0.0571
_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       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            61192
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.942
_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    1.523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81674
_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    1.281
_exptl_crystal_description       block
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 1915 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         7023
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+6.2369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1723
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.919
_reflns_Friedel_fraction_max     0.885
_reflns_number_gt                5475
_reflns_number_total             7023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_DMF_100K.cif
_cod_data_source_block           ZnAlaPyr_DMF_100K
_cod_original_cell_volume        7308.1(6)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135170
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C7 H5 N3 O5'
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.750
_reflns_odcompleteness_completeness 99.84
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-O9
 2.7 with sigma of 0.02
 N9-C22
 1.4 with sigma of 0.02
 N9-C23
 1.4 with sigma of 0.02
 N9-C21
 1.4 with sigma of 0.02
 O9-C21
 1.2 with sigma of 0.02
3. Restrained planarity
 C19, N8, O8, C20
 with sigma of 0.1
4. Rigid bond restraints
 C18, O8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C18 \\sim O8: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Zn01 \\sim N1 \\sim N2: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C2 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim
Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
6. Others
 Sof(N8)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(O8)=Sof(C18)=Sof(H18)=FVAR(1)
 Sof(N11)=Sof(O7)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(N9)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C22)=Sof(H22A)=Sof(H22B)=
 Sof(H22C)=Sof(O9)=Sof(C21)=Sof(H21)=FVAR(3)
7.a Ternary CH refined with riding coordinates:
 C12(H12), C5(H5)
7.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C19(H19A,H19B,
 H19C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C)
7.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C9(H9), C2(H2), C1(H1), C8(H8), C15(H15), C18(H18), C21(H21)
7.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              61844
_shelx_hkl_checksum              30718
_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 1.710
_oxdiff_exptl_absorpt_empirical_full_min 0.649