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_1551269
_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 syn
_chemical_formula_moiety         '0.25(C40 H52 N20 O16 Zn4)'
_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
_cell_angle_alpha                90
_cell_angle_beta                 95.22(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6206(16)
_cell_length_b                   9.0406(12)
_cell_length_c                   20.395(5)
_cell_measurement_reflns_used    2382
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.9170
_cell_measurement_theta_min      2.4220
_cell_volume                     1766.5(6)
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_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   0.00   1.00   50.00    --  -20.00 -68.00   0.00  110
  2  \w   -110.00 -30.00   1.00   50.00    --  -20.00 -68.00 120.00   80
  3  \w   -110.00 -30.00   1.00   50.00    --  -20.00 -68.00 240.00   80
;
_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      0.0205986000
_diffrn_orient_matrix_UB_12      0.0102833000
_diffrn_orient_matrix_UB_13      0.0340017000
_diffrn_orient_matrix_UB_21      0.0069178000
_diffrn_orient_matrix_UB_22      -0.0774902000
_diffrn_orient_matrix_UB_23      0.0041019000
_diffrn_orient_matrix_UB_31      0.0709031000
_diffrn_orient_matrix_UB_32      0.0044083000
_diffrn_orient_matrix_UB_33      -0.0069128000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0887
_diffrn_reflns_av_unetI/netI     0.1664
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9657
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.013
_diffrn_reflns_theta_max         25.013
_diffrn_reflns_theta_min         2.005
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26619
_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    1.251
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_preparation       'Solvent Exchange in Formamide'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.115
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.130
_refine_ls_abs_structure_details
;
 Flack x determined using 906 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5623
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1467
_refine_ls_R_factor_gt           0.0958
_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^)+(0.1357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2610
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    0.836
_reflns_Friedel_fraction_max     0.836
_reflns_number_gt                3375
_reflns_number_total             5623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000006.cif
_cod_data_source_block           PCOD1000006
_cod_database_code               1551269
_chemical_oxdiff_formula         'Zn C10 H10 N5 O3'
_shelx_estimated_absorpt_t_max   0.972
_shelx_estimated_absorpt_t_min   0.896
_reflns_odcompleteness_completeness 95.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.96
_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. Restrained distances
 O5-C12
 1.2 with sigma of 0.02
 C12-C11
 1.5 with sigma of 0.02
 C12-N7
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16 \\sim C15 \\sim C20 \\sim O7 \\sim O8: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
N10 \\sim C19 \\sim N9 \\sim C17 \\sim C18: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C12 \\sim O5 \\sim C11 \\sim N7: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C9) = Uanis(N4) = Uanis(N5) = Uanis(C7) = Uanis(C8)
Uanis(C10) = Uanis(C6) = Uanis(C5) = Uanis(O4) = Uanis(O3)
4.a Ternary CH refined with riding coordinates:
 C15(H15), C5(H5)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C6(H6A,H6B), C16(H16A,H16B), C3(H3A,H3B), C1(H1C,H1D), C13(H13A,
 H13B), N6(H6C,H6D), C11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C9(H9), N2(H2), C8(H8), C19(H19), C17(H17), N7(H7), N8(H8A)
4.d Fitted pentagon refined as free rotating group:
 C19(N10,C18,C17,N9)
;
_shelx_res_checksum              25729
_shelx_hkl_checksum              17288
_shelx_fab_checksum              35904