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_4135174
_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         'Zn C7 H7 N3 O3, 0.77(C2 H6 O S)'
_chemical_formula_sum            'C8.54 H11.62 N3 O3.77 S0.77 Zn'
_chemical_formula_weight         306.65
_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             2019-08-09
_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                   28.3977(8)
_cell_length_b                   28.3977(8)
_cell_length_c                   10.1062(2)
_cell_measurement_reflns_used    16743
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.5950
_cell_measurement_theta_min      2.1600
_cell_volume                     7058.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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 0.964
_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   0.50    2.00    --  -20.00 -68.00   0.00  250
  2  \w   -110.00  15.00   0.50    2.00    --  -20.00 -68.00 120.00  250
  3  \w   -110.00  15.00   0.50    2.00    --  -20.00 -68.00 240.00  250
  4  \w   -110.00  15.00   0.50    2.00    --  -20.00 -30.00  90.00  250
  5  \w    -90.00  90.00   0.50    1.00    --    0.00   0.00   0.00  360
;
_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      0.0262968000
_diffrn_orient_matrix_UB_12      0.0029211000
_diffrn_orient_matrix_UB_13      -0.0021471000
_diffrn_orient_matrix_UB_21      0.0090976000
_diffrn_orient_matrix_UB_22      0.0207926000
_diffrn_orient_matrix_UB_23      0.0485604000
_diffrn_orient_matrix_UB_31      -0.0075445000
_diffrn_orient_matrix_UB_32      -0.0197854000
_diffrn_orient_matrix_UB_33      0.0505993000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            48337
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.890
_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    1.672
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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    1.299
_exptl_crystal_description       needle
_exptl_crystal_F_000             2814
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.833
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Flack x determined using 2882 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.030(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         10219
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0761
_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^)+(0.1410P)^2^+42.5599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2156
_refine_ls_wR_factor_ref         0.2273
_reflns_Friedel_coverage         0.806
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.777
_reflns_number_gt                8214
_reflns_number_total             10219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ZnAlaPyr_DMSO_100K.cif
_cod_data_source_block           ZnAlaPyr_DMSO_100K
_cod_original_cell_volume        7058.0(4)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4135174
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         ZnC15H15N3O3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.634
_reflns_odcompleteness_completeness 96.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.82
_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-S2A
 1.8 with sigma of 0.02
 S2A-O8B
 1.8 with sigma of 0.02
 S2A-O8A
 1.5 with sigma of 0.02
 C18B-S2B
 1.8 with sigma of 0.02
 S2B-C18B
 1.8 with sigma of 0.02
 S2B-C17B
 1.8 with sigma of 0.02
 S2A-C18A
 1.8 with sigma of 0.02
 S2B-O8B
 1.5 with sigma of 0.02
3. Others
 Sof(S003)=Sof(O7)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(1)
 Sof(S2B)=Sof(C18B)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C17B)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=Sof(O8B)=FVAR(2)
 Sof(S2A)=Sof(O8A)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=Sof(C18A)=Sof(H18D)=
 Sof(H18E)=Sof(H18F)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C5(H5)
4.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C18B(H18A,H18B,H18C), C15(H15A,H15B,H15C), C17B(H17A,
 H17B,H17C), C17A(H17D,H17E,H17F), C18A(H18D,H18E,H18F)
4.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C1(H1), C8(H8), C9(H9), C2(H2)
4.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              27415
_shelx_hkl_checksum              84306
_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 1.444
_oxdiff_exptl_absorpt_empirical_full_min 0.527