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_4135192
_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'
_chemical_formula_sum            'C6 H5 N3 O3 Zn'
_chemical_formula_weight         232.50
_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             2017-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   28.539(3)
_cell_length_b                   28.539(3)
_cell_length_c                   10.1528(6)
_cell_measurement_reflns_used    3655
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.9870
_cell_measurement_theta_min      2.4870
_cell_volume                     7161.3(11)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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
;
_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      -0.0064015000
_diffrn_orient_matrix_UB_12      -0.0272310000
_diffrn_orient_matrix_UB_13      0.0089934000
_diffrn_orient_matrix_UB_21      0.0258940000
_diffrn_orient_matrix_UB_22      0.0066037000
_diffrn_orient_matrix_UB_23      -0.0244138000
_diffrn_orient_matrix_UB_31      0.0106249000
_diffrn_orient_matrix_UB_32      0.0062599000
_diffrn_orient_matrix_UB_33      0.0647534000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1571
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20672
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        23.293
_diffrn_reflns_theta_max         23.293
_diffrn_reflns_theta_min         2.472
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57196
_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    0.970
_exptl_crystal_description       needle
_exptl_crystal_F_000             2088
_exptl_crystal_preparation       'Desolvated from Benzene'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.012
_refine_diff_density_max         1.712
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Flack x determined using 532 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         2230
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.1092
_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^)+(0.1446P)^2^+55.8135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2517
_refine_ls_wR_factor_ref         0.2676
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.941
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                1729
_reflns_number_total             2230
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnGlyPyr_BenzeneRemoved_150K.cif
_cod_data_source_block           ZnGlyPyr_BenzeneRemoved_150K
_cod_original_cell_volume        7161.3(14)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4135192
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C6 H8 N3 O5'
_reflns_odcompleteness_completeness 70.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(Zn1) \\sim
Ueq, Uanis(O1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N3) \\sim Ueq,
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) = Uanis(O2) = Uanis(C6)
Uanis(C2) = Uanis(N2) = Uanis(N1) = Uanis(C1) = Uanis(C3)
Uanis(C4) = Uanis(O3) = Uanis(N3) = Uanis(C5)
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C2(H2), C1(H1)
;
_shelx_res_checksum              21629
_shelx_hkl_checksum              32463
_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 1.641
_oxdiff_exptl_absorpt_empirical_full_min 0.778