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_4135176
_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         'C7 H7 N3 O3 Zn'
_chemical_formula_sum            'C7 H7 N3 O3 Zn'
_chemical_formula_weight         246.53
_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     direct
_audit_creation_date             2019-08-19
_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                   24.035(3)
_cell_length_b                   24.035(3)
_cell_length_c                   10.2251(5)
_cell_measurement_reflns_used    1428
_cell_measurement_temperature    195
_cell_measurement_theta_max      24.2130
_cell_measurement_theta_min      1.6410
_cell_volume                     5115.5(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      195
_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   -112.00  26.00   0.20    0.20    --   30.00  45.00   0.00  690
  2  \w   -112.00  26.00   0.20    0.20    --   30.00  45.00  40.00  690
  3  \w   -112.00  26.00   0.20    0.20    --   30.00  45.00 160.00  690
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0092527000
_diffrn_orient_matrix_UB_12      0.0133510000
_diffrn_orient_matrix_UB_13      0.0490444000
_diffrn_orient_matrix_UB_21      -0.0316582000
_diffrn_orient_matrix_UB_22      -0.0227372000
_diffrn_orient_matrix_UB_23      -0.0106749000
_diffrn_orient_matrix_UB_31      0.0024886000
_diffrn_orient_matrix_UB_32      -0.0199847000
_diffrn_orient_matrix_UB_33      0.0450052000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5294
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        20.119
_diffrn_reflns_theta_max         20.119
_diffrn_reflns_theta_min         1.642
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.981
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_description       needle
_exptl_crystal_F_000             2232
_exptl_crystal_preparation       'In situ CO2 Loading 0.1bar CO2 195K'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.327
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.174
_refine_ls_abs_structure_details
;
 Flack x determined using 677 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         2275
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1787P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2207
_refine_ls_wR_factor_ref         0.2345
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.909
_reflns_number_gt                1837
_reflns_number_total             2275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_LowLoadingCO2_Insitu-SCXRD_195K.cif
_cod_data_source_block           ZnAlaPyr_LowLoadingCO2_Insitu_SCXRD
_cod_original_cell_volume        5115.4(11)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135176
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Zn C7 H7 N3 O3'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.627
_reflns_odcompleteness_completeness 97.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.20
_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
 C7-C5
 1.5 with sigma of 0.02
 C12-C14
 1.5 with sigma of 0.02
3. Rigid bond restraints
 C7, C5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N5 \\sim C9 \\sim C10 \\sim C8 \\sim N4: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
N2 \\sim N1 \\sim C1 \\sim C3 \\sim C2: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O4 \\sim C13 \\sim O5: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
O1 \\sim C6 \\sim O2: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
C5 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C11 \\sim O6 \\sim N6: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
N3 \\sim C4 \\sim O3: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(N4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O5) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.1
5.a Ternary CH refined with riding coordinates:
 C12(H12), C5(H5)
5.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C2(H2), C9(H9), C8(H8), C1(H1)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              34867
_shelx_hkl_checksum              33043
_shelx_fab_checksum              3298
_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 4.602
_oxdiff_exptl_absorpt_empirical_full_min 0.472