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_4135189
_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, 0.5(C8 H10)'
_chemical_formula_sum            'C10 H10 N3 O3 Zn'
_chemical_formula_weight         285.58
_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                   26.5830(12)
_cell_length_b                   26.5830(12)
_cell_length_c                   10.1311(4)
_cell_measurement_reflns_used    7479
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.9540
_cell_measurement_theta_min      2.6150
_cell_volume                     6200.1(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    '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   10.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   10.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   10.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   10.00    --  -20.00 -30.00  90.00  125
  5  \w    -90.00  90.00   1.00    1.00    --    0.00   0.00   0.00  180
;
_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      0.0156815000
_diffrn_orient_matrix_UB_12      -0.0150697000
_diffrn_orient_matrix_UB_13      0.0040812000
_diffrn_orient_matrix_UB_21      0.0238666000
_diffrn_orient_matrix_UB_22      0.0249231000
_diffrn_orient_matrix_UB_23      0.0282082000
_diffrn_orient_matrix_UB_31      -0.0115314000
_diffrn_orient_matrix_UB_32      -0.0100198000
_diffrn_orient_matrix_UB_33      0.0639862000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1506
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29859
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.990
_diffrn_reflns_theta_max         24.990
_diffrn_reflns_theta_min         2.654
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44387
_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    1.377
_exptl_crystal_description       needle
_exptl_crystal_F_000             2610
_exptl_crystal_preparation       'Solvent Exchange M-Xylene'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.754
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details
;
 Flack x determined using 796 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2396
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0811
_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^)+(0.1422P)^2^+19.4885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2094
_reflns_Friedel_coverage         0.970
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                2126
_reflns_number_total             2396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnGlyPyr_M-xylene_100K.cif
_cod_data_source_block           ZnGlyPyr_M-xylene_100K
_cod_original_cell_volume        6200.1(6)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4135189
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C6 N3 O3 H8'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.94
_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
 C8-C14
 1.5 with sigma of 0.02
 C7-C13 \\sim C13-C11
 with sigma of 0.02
 C7-C14 \\sim C14-C9
 with sigma of 0.02
3. Restrained planarity
 C9, C8, C7, C12, C11, C10
 with sigma of 0.05
 C13, C12, C11, C10, C9, C8, C7, C14
 with sigma of 0.1
4. Rigid bond restraints
 C4, O3
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O1, O2, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Zn1, N1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C4 \\sim O3: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
O2 \\sim C6 \\sim O1: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
N2 \\sim C3 \\sim C2 \\sim C1 \\sim N1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C9 \\sim C11 \\sim C10 \\sim C12 \\sim C7 \\sim C8: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(O1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
6. Others
 Fixed Sof: C9(0.5) H9(0.5) C10(0.5) H10(0.5) C11(0.5) H11(0.5) C12(0.5)
 C7(0.5) H7(0.5) C8(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C14(0.5)
 H14A(0.5) H14B(0.5) H14C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
7.b Me refined with riding coordinates:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
7.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C3(H3A), C9(H9), C10(H10), C11(H11), C7(H7)
7.d Fitted hexagon refined as free rotating group:
 C9(C10,C11,C12,C7,C8)
;
_shelx_res_checksum              72345
_shelx_hkl_checksum              42003
_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 1.922
_oxdiff_exptl_absorpt_empirical_full_min 0.592