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_4135185
_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
'0.06(C126 H126 N54 O54 Zn18), 0.72(C2 H3 F3 O)'
_chemical_formula_sum            'C8.44 H9.16 F2.16 N3 O3.72 Zn'
_chemical_formula_weight         318.45
_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             2019-08-13
_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                   28.2675(5)
_cell_length_b                   28.2675(5)
_cell_length_c                   10.1239(2)
_cell_measurement_reflns_used    22334
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4910
_cell_measurement_theta_min      2.1510
_cell_volume                     7005.7(2)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   25.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   25.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   25.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   25.00    --  -20.00 -30.00  90.00  125
  5  \w    -50.00  70.00   1.00   25.00    --  -20.00  68.00   0.00  120
  6  \w    -50.00  70.00   1.00   25.00    --  -20.00  68.00 120.00  120
  7  \w    -50.00  70.00   1.00   25.00    --  -20.00  68.00 240.00  120
  8  \w    -50.00 -13.00   1.00   25.00    --  -20.00  30.00 -90.00   37
;
_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      0.0164940000
_diffrn_orient_matrix_UB_12      0.0288698000
_diffrn_orient_matrix_UB_13      0.0008702000
_diffrn_orient_matrix_UB_21      0.0224607000
_diffrn_orient_matrix_UB_22      -0.0023840000
_diffrn_orient_matrix_UB_23      0.0227100000
_diffrn_orient_matrix_UB_31      0.0079173000
_diffrn_orient_matrix_UB_32      -0.0004384000
_diffrn_orient_matrix_UB_33      -0.0662576000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            53265
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.177
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86933
_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    1.359
_exptl_crystal_description       needle
_exptl_crystal_F_000             2879
_exptl_crystal_preparation       'Solvent Exchange in Trifluoroethanol'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 2681 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         7118
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0570
_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^)+(0.1078P)^2^+18.6790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1702
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6195
_reflns_number_total             7118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_CF3CH2OH_100K.cif
_cod_data_source_block           ZnAlaPyr_CF3CH2OH_100K
_cod_original_cell_volume        7005.7(3)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135185
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         ZnC7H7N3O3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.532
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, All O(H) groups
2. Restrained distances
 O8-C17
 2.3 with sigma of 0.02
 C15-O7
 2.3 with sigma of 0.02
 O7-C16
 1.45 with sigma of 0.01
 C18-O8
 1.45 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C5 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
F3 \\sim F2 \\sim C15 \\sim F1 \\sim C16 \\sim O7: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04
O8 \\sim C18 \\sim C17 \\sim F5 \\sim F4 \\sim F6: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04
4. Others
 Sof(F1)=Sof(F3)=Sof(F2)=Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(O7)=Sof(H7)=
 FVAR(1)
 Sof(O8)=Sof(H8A)=Sof(F4)=Sof(F6)=Sof(F5)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(C17)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C12(H12)
5.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B)
5.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N3(H3), C10(H10), C8(H8), C1(H1), C2(H2)
5.d Tetrahedral OH refined with riding coordinates:
 O8(H8A)
5.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C)
5.f Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              87757
_shelx_hkl_checksum              82170
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.582
_oxdiff_exptl_absorpt_empirical_full_min 0.652