Chemical control of structure and guest uptake by a conformationally mobile porous material
Alexandros P. Katsoulidis; Dmytro Antypov; George F. S. Whitehead; Elliot J. Carrington; Dave J. Adams; Neil G. Berry; George R. Darling; Matthew S. Dyer; Matthew J. Rosseinsky; Nature 565 (2019) 213–217; doi:10.1038/s41586-018-0820-9

data_1551275
_publ_section_title
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 Chemical control of structure and guest uptake by a conformationally
 mobile porous material
;
_journal_name_full               Nature
_journal_page_first              213
_journal_page_last               217
_journal_paper_doi               10.1038/s41586-018-0820-9
_journal_volume                  565
_journal_year                    2019
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C10 H13 N5 O4 Zn, C2 H6 O S'
_chemical_formula_sum            'C12 H19 N5 O5 S Zn'
_chemical_formula_weight         410.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 105.318(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5615(10)
_cell_length_b                   9.0515(13)
_cell_length_c                   10.4586(15)
_cell_measurement_reflns_used    1685
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.9650
_cell_measurement_theta_min      2.2100
_cell_volume                     873.0(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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.989
_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   50.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   50.00    --  -20.00 -68.00 120.00  125
;
_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      -0.0092526000
_diffrn_orient_matrix_UB_12      -0.0080635000
_diffrn_orient_matrix_UB_13      -0.0691946000
_diffrn_orient_matrix_UB_21      0.0398362000
_diffrn_orient_matrix_UB_22      0.0659931000
_diffrn_orient_matrix_UB_23      -0.0006136000
_diffrn_orient_matrix_UB_31      0.0651468000
_diffrn_orient_matrix_UB_32      -0.0414760000
_diffrn_orient_matrix_UB_33      0.0124341000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4260
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_min         2.019
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71813
_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    1.563
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_preparation
'Solvent Exchnaged with DMSO and immersed in Dioxane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.599
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Flack x determined using 873 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         2903
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0912P)^2^+2.5290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1784
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.862
_reflns_Friedel_fraction_max     0.881
_reflns_number_gt                2400
_reflns_number_total             2903
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000012.cif
_cod_data_source_block           PCOD1000012
_cod_database_code               1551275
_chemical_oxdiff_formula         'Zn C10 H10 N5 O3'
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.860
_reflns_odcompleteness_completeness 98.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(C6) = Uanis(O1)
3.a Ternary CH refined with riding coordinates:
 C5(H5)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), N5(H5A,H5B), C8(H8A,H8B), C10(H10A,H10B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), N4(H4), C2(H2)
3.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
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_shelx_res_checksum              47218