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_1551265
_publ_section_title
;
 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 rm
_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
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 105.264(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5645(5)
_cell_length_b                   9.0405(5)
_cell_length_c                   10.4571(10)
_cell_measurement_reflns_used    1307
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.9660
_cell_measurement_theta_min      2.1860
_cell_volume                     872.31(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega -110.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000    0.0000 125
  2 omega -110.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  120.0000 125
  3 omega -110.00  -69.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  240.0000 41
;
_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_UB_11      0.0197800000
_diffrn_orient_matrix_UB_12      -0.0401357000
_diffrn_orient_matrix_UB_13      0.0597689000
_diffrn_orient_matrix_UB_21      0.0034971000
_diffrn_orient_matrix_UB_22      -0.0654004000
_diffrn_orient_matrix_UB_23      -0.0356513000
_diffrn_orient_matrix_UB_31      0.0737134000
_diffrn_orient_matrix_UB_32      0.0138383000
_diffrn_orient_matrix_UB_33      0.0046325000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_unetI/netI     0.1702
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5339
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.995
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.019
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.652
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Flack x determined using 517 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   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3250
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1564
_refine_ls_R_factor_gt           0.0964
_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^)+(0.0879P)^2^+3.4213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2043
_refine_ls_wR_factor_ref         0.2393
_reflns_Friedel_coverage         0.786
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.898
_reflns_number_gt                1948
_reflns_number_total             3250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000002.cif
_cod_data_source_block           PCOD1000002
_cod_original_cell_volume        872.30(11)
_cod_database_code               1551265
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.30
_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. Rigid bond restraints
 O008, Zn01, O003, C00B, O004, C00M, N006, C00A, C00K, C00I, C00F, C00H, N00E,
 C00J, O005, C00G, N00D
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C00K \\sim Zn01 \\sim O003 \\sim C00B \\sim O004 \\sim C00M \\sim C00A \\sim
C00I \\sim O008 \\sim C00F \\sim C00H \\sim N00E \\sim C00J \\sim O005 \\sim
C00G \\sim N00D: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(N007) \\sim Ueq, Uanis(C00C) \\sim Ueq, Uanis(N009) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.1
4.a Ternary CH refined with riding coordinates:
 C00M(H00M)
4.b Secondary CH2 refined with riding coordinates:
 C00A(H00A,H00B), N00D(H00D,H00E), C00F(H00G,H00H), C00G(H00I,H00J)
4.c Aromatic/amide H refined with riding coordinates:
 N006(H006), C00C(H00C), N00E(H00F), C00H(H00K)
4.d Idealised Me refined as rotating group:
 C00N(H00L,H00N,H00O), C00O(H00P,H00Q,H00R)
;
_shelx_res_checksum              49237
_shelx_hkl_checksum              49038
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'