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_1551276
_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'
_chemical_formula_sum            'C10 H13 N5 O4 Zn'
_chemical_formula_weight         332.62
_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     dual
_cell_angle_alpha                90
_cell_angle_beta                 112.41(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.602(4)
_cell_length_b                   9.035(3)
_cell_length_c                   11.675(6)
_cell_measurement_reflns_used    673
_cell_measurement_temperature    240.00(10)
_cell_measurement_theta_max      44.7240
_cell_measurement_theta_min      4.0800
_cell_volume                     936.4(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      240.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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     30.00  57.00   1.00    3.00    --    5.00  -9.00 -65.00   27
  2  \w    -27.00   1.00   1.00    3.00    --    5.00  57.00-180.00   28
  3  \w    -59.00 -31.00   1.00    3.00    --    5.00  -9.00 -65.00   28
  4  \w    -24.00   6.00   1.00    3.00    --    5.00  -9.00 -65.00   30
  5  \w   -130.00 -11.00   1.00    3.00    --  -44.10 -59.00 134.84  119
  6  \w    -76.00  43.00   1.00    3.00    --  -44.10  57.00 172.04  119
  7  \w    -97.00  -6.00   1.00    3.00    --  -44.10 -44.00 173.34   91
  8  \w    -55.00 -26.00   1.00    3.00    --  -44.10  48.00  76.89   29
  9  \w     16.00  41.00   1.00    3.00    --  -44.10   9.00 109.00   25
 10  \w   -125.00-100.00   1.00    3.00    --  -44.10 -44.00 173.34   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1067859000
_diffrn_orient_matrix_UB_12      -0.0059349000
_diffrn_orient_matrix_UB_13      -0.0703179000
_diffrn_orient_matrix_UB_21      0.1359269000
_diffrn_orient_matrix_UB_22      -0.0056325000
_diffrn_orient_matrix_UB_23      0.1243086000
_diffrn_orient_matrix_UB_31      -0.0079782000
_diffrn_orient_matrix_UB_32      -0.1706182000
_diffrn_orient_matrix_UB_33      -0.0006383000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.1346
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2003
_diffrn_reflns_point_group_measured_fraction_full 0.825
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        44.841
_diffrn_reflns_theta_max         44.841
_diffrn_reflns_theta_min         4.096
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.982
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.04348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       plate
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.139
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.2(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1239
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_gt           0.1235
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3175
_refine_ls_wR_factor_ref         0.3551
_reflns_Friedel_coverage         0.605
_reflns_Friedel_fraction_full    0.683
_reflns_Friedel_fraction_max     0.683
_reflns_number_gt                749
_reflns_number_total             1239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000013.cif
_cod_data_source_block           PCOD1000013
_cod_database_code               1551276
_chemical_oxdiff_formula         'Zn1 C H N O'
_chemical_oxdiff_usercomment     LTH
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.697
_reflns_odcompleteness_completeness 92.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     45.18
_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
2. Uiso/Uaniso restraints and constraints
O1 \\sim Zn01 \\sim N00K \\sim C1AA \\sim C2AA \\sim N3 \\sim C00H \\sim C5
\\sim O005 \\sim N009 \\sim C00G \\sim C00A \\sim C00D \\sim O002 \\sim O006
\\sim C004 \\sim N003 \\sim C007 \\sim C00C \\sim N00E: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 O1, Zn01, N00K, C1AA, C2AA, N3, C00H, C5, O005, N009, C00G, C00A, C00D, O002,
 O006, C004, N003, C007, C00C, N00E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C00G(H00G)
4.b Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00H(H00D,H00E), N00K(H00F,H00H), C1AA(H1AA,H1AB)
4.c Aromatic/amide H refined with riding coordinates:
 C007(H007), N009(H009), C00C(H00C), N3(H3)
;
_shelx_res_checksum              70545
_shelx_hkl_checksum              28570
_shelx_fab_checksum              85256
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 6.524
_oxdiff_exptl_absorpt_empirical_full_min 0.479