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_4135200
_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, 0.6(C8 H10)'
_chemical_formula_sum            'C10.82 H11.03 N3 O3 Zn'
_chemical_formula_weight         296.47
_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   geom
_atom_sites_solution_primary     direct
_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                   26.4227(7)
_cell_length_b                   26.4227(7)
_cell_length_c                   10.1231(2)
_cell_measurement_reflns_used    8936
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.9660
_cell_measurement_theta_min      2.6410
_cell_volume                     6120.7(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 0.999
_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   20.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   20.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   20.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   20.00    --  -20.00 -30.00  90.00  125
;
_diffrn_measurement_device
'Rigaku Mo Rotating Anode Source With Saturn Detector'
_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      -0.0046220000
_diffrn_orient_matrix_UB_12      0.0242366000
_diffrn_orient_matrix_UB_13      -0.0010832000
_diffrn_orient_matrix_UB_21      0.0288609000
_diffrn_orient_matrix_UB_22      0.0183277000
_diffrn_orient_matrix_UB_23      0.0234044000
_diffrn_orient_matrix_UB_31      0.0103059000
_diffrn_orient_matrix_UB_32      0.0061177000
_diffrn_orient_matrix_UB_33      -0.0660266000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0579
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            20223
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         2.670
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75329
_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    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             2717
_exptl_crystal_preparation       'Solvent Exchanged in ortho-xylene'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.288
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.147
_refine_ls_abs_structure_details
;
 Flack x determined using 949 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2284
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0585
_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^)+(0.1216P)^2^+16.3712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1596
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_full    0.900
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                2156
_reflns_number_total             2284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnGlyPyr_O-xylene_100K.cif
_cod_data_source_block           ZnGlyPyr_O-xylene_100K
_cod_original_cell_volume        6120.7(4)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4135200
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C6 H5 N3 O3 Zn'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.96
_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
 C13-C7
 1.5 with sigma of 0.02
 C8-C14
 1.5 with sigma of 0.02
 C14-C9 \\sim C14-C7
 with sigma of 0.02
3. Restrained planarity
 C14, C8, C7, C13, C9, C12
 with sigma of 0.1
4. Rigid bond restraints
 N1, N2, C2, C1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C2 \\sim C1 \\sim C3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
O3 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C14 \\sim C8 \\sim C7 \\sim C13 \\sim C12 \\sim C11 \\sim C10 \\sim C9: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
6. Others
 Sof(C9)=Sof(H9)=Sof(C8)=Sof(C7)=Sof(C12)=Sof(H12)=Sof(C11)=Sof(H11)=Sof(C10)=
 Sof(H10)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(H13C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
7.b Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
7.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C3(H3A), C9(H9), C12(H12), C11(H11), C10(H10)
7.d Fitted hexagon refined as free rotating group:
 C9(C8,C7,C12,C11,C10)
;
_shelx_res_checksum              321
_shelx_hkl_checksum              37049
_olex2_date_sample_data_collection 2017-04-27
_olex2_date_sample_submission    2017-04-27
_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 1.319
_oxdiff_exptl_absorpt_empirical_full_min 0.784