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_4135173
_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 O5 Zn, 0.95(C2 H3 N)'
_chemical_formula_sum            'C8.9 H9.85 N3.95 O3 Zn'
_chemical_formula_weight         285.49
_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             2018-08-06
_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                   27.8332(3)
_cell_length_b                   27.8332(3)
_cell_length_c                   10.14011(14)
_cell_measurement_reflns_used    39702
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5480
_cell_measurement_theta_min      2.1550
_cell_volume                     6802.99(14)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (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    3.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00    3.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00    3.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00    3.00    --  -20.00 -30.00  90.00  125
  5  \w    -50.00  70.00   1.00    3.00    --  -20.00  68.00   0.00  120
  6  \w    -50.00  70.00   1.00    3.00    --  -20.00  68.00 120.00  120
  7  \w    -50.00  70.00   1.00    3.00    --  -20.00  68.00 240.00  120
  8  \w    -50.00  70.00   1.00    3.00    --  -20.00  30.00 -90.00  120
;
_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      -0.0106134000
_diffrn_orient_matrix_UB_12      -0.0276457000
_diffrn_orient_matrix_UB_13      -0.0222884000
_diffrn_orient_matrix_UB_21      0.0274306000
_diffrn_orient_matrix_UB_22      0.0048037000
_diffrn_orient_matrix_UB_23      -0.0065581000
_diffrn_orient_matrix_UB_31      -0.0008563000
_diffrn_orient_matrix_UB_32      -0.0088712000
_diffrn_orient_matrix_UB_33      0.0659763000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            55832
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         2.179
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.625
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88219
_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    1.254
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2608
_exptl_crystal_preparation       'Solvent Exchange in MeCN'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.113
_refine_ls_abs_structure_details
;
 Flack x determined using 3270 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         6933
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0815P)^2^+13.1604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6734
_reflns_number_total             6933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_MeCN_100K.cif
_cod_data_source_block           ZnAlaPyr_MeCN_100K
_cod_original_cell_volume        6802.97(19)
_cod_original_sg_symbol_H-M      'R 3'
_cod_original_formula_sum        'C8.90 H9.85 N3.95 O3 Zn'
_cod_database_code               4135173
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Zn C7 H7 N3 O5'
_reflns_odcompleteness_completeness 99.83
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17A-C18A
 1.45 with sigma of 0.02
 C17B-C18B
 1.45 with sigma of 0.02
 C18A-N8A
 2.55 with sigma of 0.02
 C17A-N8A
 1.15 with sigma of 0.02
 N8B-C17B
 1.15 with sigma of 0.02
 N8B-C18B
 2.55 with sigma of 0.02
 N9-C19
 1.15 with sigma of 0.02
 C19-C20
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N9 \\sim C19 \\sim C20: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04
4. Others
 Sof(C15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(N7)=FVAR(1)
 Sof(N8A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
 Sof(C17B)=Sof(N8B)=Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=FVAR(3)
 Sof(C19)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(N9)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C9(H9)
5.b Me refined with riding coordinates:
 C20(H20A,H20B,H20C)
5.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N1(H1), C13(H13), C6(H6), C7(H7), C14(H14)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C18A(H18A,H18B,
 H18C), C18B(H18D,H18E,H18F)
;
_shelx_res_checksum              98343
_shelx_hkl_checksum              48732
_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 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.810