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_1551266
_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 rmad
_chemical_formula_moiety         'C10 H13 N5 O4 Zn, 1.24(C3 H7 N O)'
_chemical_formula_sum            'C13.73 H21.7 N6.24 O5.24 Zn'
_chemical_formula_weight         423.56
_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                 106.403(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5895(2)
_cell_length_b                   9.0619(2)
_cell_length_c                   11.1120(4)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.0320
_cell_measurement_theta_min      1.9030
_cell_volume                     926.32(5)
_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      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega -110.00   15.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000    0.0000 125
  2 omega -110.00   15.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  120.0000 125
  3 omega -110.00   15.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  240.0000 125
  4 omega -110.00   15.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -30.0000   90.0000 125
  5 omega  -90.00   90.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000    0.0000 180
;
_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      0.0599612000
_diffrn_orient_matrix_UB_12      0.0088228000
_diffrn_orient_matrix_UB_13      0.0540721000
_diffrn_orient_matrix_UB_21      -0.0481870000
_diffrn_orient_matrix_UB_22      0.0037257000
_diffrn_orient_matrix_UB_23      0.0379240000
_diffrn_orient_matrix_UB_31      0.0044971000
_diffrn_orient_matrix_UB_32      -0.0777616000
_diffrn_orient_matrix_UB_33      0.0080159000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14916
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.214
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77016
_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            'clear white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       irregular
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.884
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3442
_refine_ls_number_restraints     139
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0598P)^2^+0.9266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1023
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3219
_reflns_number_total             3442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000003.cif
_cod_data_source_block           PCOD1000003
_cod_original_formula_sum        'C13.73 H21.70 N6.24 O5.24 Zn'
_cod_database_code               1551266
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.00(3) 0.00(3)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C4) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(N2) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(O00L) \\sim Ueq: with sigma of 0.02 and sigma for terminal
atoms of 0.04
4. Rigid body (RIGU) restrains
 N1, C6, C7, C4, H6A, H6B, H6C, H7A, H7B, H7C, H4, O11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C11, C1, C2, H11A, H11B, H11C, O6, H1, H2A, H2B, H2C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3, C12, H12A, H12B, H12C, N2, C13, H3, O00L, H13A, H13B, H13C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N3)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(O6)=Sof(C1)=Sof(H1)=
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
 Sof(N1)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=
 Sof(C4)=Sof(H4)=Sof(O11)=FVAR(2)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(N2)=Sof(C3)=Sof(H3)=Sof(C13)=
 Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(O00L)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C00I(H00I)
6.b Secondary CH2 refined with riding coordinates:
 N007(H00A,H00B), C00D(H00E,H00F), C00J(H00H,H00J), C00K(H00K,H00L)
6.c Aromatic/amide H refined with riding coordinates:
 N008(H008), C00B(H00C), C00C(H00D), N00G(H00G), C3(H3), C4(H4), C1(H1)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C),
 C11(H11A,H11B,H11C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              13508
_shelx_hkl_checksum              19843
_shelx_shelxl_version_number     2014/7