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_4135183
_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, 0.69(C H2 Cl2)'
_chemical_formula_sum            'C7.69 H8.37 Cl1.37 N3 O3 Zn'
_chemical_formula_weight         304.73
_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                   27.7361(9)
_cell_length_b                   27.7361(9)
_cell_length_c                   10.1353(3)
_cell_measurement_reflns_used    7339
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.54
_cell_volume                     6752.4(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19483
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.056
_diffrn_reflns_theta_max         25.056
_diffrn_reflns_theta_min         2.181
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.876
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0613 before and 0.0520 after correction. The Ratio of minimum to maximum transmission is 0.9173. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       needle
_exptl_crystal_F_000             2750
_exptl_crystal_preparation       'Solvent Exchange DCM'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.026
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
;
 Flack x determined using 2094 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.026(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5298
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0662
_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^)+(0.1291P)^2^+71.4845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.1953
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                4771
_reflns_number_total             5298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_DCM_150K.cif
_cod_data_source_block           ZnAlaPyr_DCM_150K
_cod_original_cell_volume        6752.4(5)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135183
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.835
_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
 Cl3-C16
 1.7 with sigma of 0.02
 C16-Cl4
 1.7 with sigma of 0.02
3. Rigid bond restraints
 O4, C13, O5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C1, C3, C2
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C13 \\sim O5 \\sim O4: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C1 \\sim C3 \\sim C2: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.04
Uanis(C16) = Uanis(Cl4) = Uanis(Cl3)
5. Others
 Sof(Cl2)=Sof(Cl1)=Sof(C15)=Sof(H15A)=Sof(H15B)=FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C5(H5), C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B)
6.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N3(H3), C2(H2), C8(H8), C1(H1), C9(H9)
6.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              30683
_shelx_hkl_checksum              62282
_olex2_submission_special_instructions 'No special instructions were received'