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_4135181
_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, 0.44(C8 H10)'
_chemical_formula_sum            'C10.53 H11.41 N3 O3 Zn'
_chemical_formula_weight         293.33
_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             2019-08-12
_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                   28.1677(4)
_cell_length_b                   28.1677(4)
_cell_length_c                   10.15790(10)
_cell_measurement_reflns_used    28071
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4720
_cell_measurement_theta_min      2.1590
_cell_volume                     6979.71(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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
  5  \w    -50.00  70.00   1.00   15.00    --  -20.00  68.00   0.00  120
  6  \w    -50.00  70.00   1.00   15.00    --  -20.00  68.00 120.00  120
  7  \w    -50.00  70.00   1.00   15.00    --  -20.00  68.00 240.00  120
  8  \w    -50.00  70.00   1.00   15.00    --  -20.00  30.00 -90.00  120
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0287173000
_diffrn_orient_matrix_UB_12      -0.0106744000
_diffrn_orient_matrix_UB_13      0.0041384000
_diffrn_orient_matrix_UB_21      0.0043769000
_diffrn_orient_matrix_UB_22      0.0270014000
_diffrn_orient_matrix_UB_23      0.0058902000
_diffrn_orient_matrix_UB_31      -0.0013360000
_diffrn_orient_matrix_UB_32      0.0016534000
_diffrn_orient_matrix_UB_33      -0.0694266000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            57566
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.585
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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    1.256
_exptl_crystal_description       needle
_exptl_crystal_F_000             2692
_exptl_crystal_preparation       'Solvent Exchnage in Ethylbenzene'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 3165 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         7121
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0717P)^2^+13.2648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6743
_reflns_number_total             7121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_Ethylbenzene_100K.cif
_cod_data_source_block           ZnAlaPyr_Ethylbenzene_100K
_cod_original_cell_volume        6979.7(2)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135181
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         ZnC7H7N3O5
_reflns_odcompleteness_completeness 99.86
_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
2. Restrained distances
 C22A-C18A
 2.6 with sigma of 0.02
 C21A-C22A
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C15B \\sim C16B \\sim C17B \\sim C18B \\sim C19B \\sim C20B \\sim C21B \\sim
C22B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C22A \\sim C21A \\sim C18A \\sim C17A \\sim C16A \\sim C15A \\sim C20A \\sim
C19A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C20A)=Sof(H20A)=Sof(C19A)=Sof(H19A)=Sof(C18A)=Sof(C17A)=Sof(H17A)=
 Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C21A)=Sof(H21A)=Sof(H21B)=
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(C19B)=Sof(H19B)=
 Sof(C20B)=Sof(H20B)=Sof(C15B)=Sof(H15B)=Sof(C22B)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C21B)=Sof(H21C)=Sof(H21D)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C21B(H21C,H21D), C21A(H21A,H21B)
5.c Me refined with riding coordinates:
 C22B(H22D,H22E,H22F), C22A(H22A,H22B,H22C)
5.d Aromatic/amide H refined with riding coordinates:
 N6(H6), N3(H3), C9(H9), C8(H8), C1(H1), C2(H2), C20A(H20A), C19A(H19A),
 C17A(H17A), C16A(H16A), C15A(H15A), C16B(H16B), C17B(H17B), C19B(H19B),
 C20B(H20B), C15B(H15B)
5.e Fitted hexagon refined as free rotating group:
 C20A(C19A,C18A,C17A,C16A,C15A), C16B(C17B,C18B,C19B,C20B,C15B)
5.f Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              15178
_shelx_hkl_checksum              79703
_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 1.861
_oxdiff_exptl_absorpt_empirical_full_min 0.675