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_1551264
_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, 0.91(C3 H7 N O)'
_chemical_formula_sum            'C12.73 H19.38 N5.91 O4.91 Zn'
_chemical_formula_weight         399.21
_chemical_name_systematic        Zn-GGH
_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                 112.735(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6261(6)
_cell_length_b                   9.0444(5)
_cell_length_c                   11.6284(10)
_cell_measurement_reflns_used    8514
_cell_measurement_temperature    300
_cell_measurement_theta_max      32.5120
_cell_measurement_theta_min      2.3250
_cell_volume                     933.73(12)
_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      300
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13803
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.503
_diffrn_reflns_theta_min         2.346
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.348
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.75492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_description       irregular
_exptl_crystal_F_000             413
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.593
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.105
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         5203
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1093P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1647
_reflns_Friedel_coverage         0.891
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                4107
_reflns_number_total             5203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000001.cif
_cod_data_source_block           PCOD1000001
_cod_database_code               1551264
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.688
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.98(3)
 0.02(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. Restrained distances
 O2-C6
 2.8 with sigma of 0.02
 N5-C6
 1.45 with sigma of 0.02
 C10-C6
 2.5 with sigma of 0.02
 N5-C10
 1.45 with sigma of 0.02
 C6-C3
 2.5 with sigma of 0.02
 C10-C3
 2.45 with sigma of 0.02
 N5-C3
 1.35 with sigma of 0.02
 C3-O2
 1.2 with sigma of 0.02
4. Restrained planarity
 O2, C3, N5, C10, C6
 with sigma of 0.05
5. Uiso/Uaniso restraints and constraints
O2 \\sim C3 \\sim N5 \\sim C6 \\sim C10: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
6. Others
 Sof(O2)=Sof(C3)=Sof(H3)=Sof(N5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C10)=
 Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C00B(H00B)
7.b Secondary CH2 refined with riding coordinates:
 N00D(H00A,H00D), C00F(H00E,H00F), C00H(H00G,H00H), C00J(H00I,H00J)
7.c Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C)
7.d Aromatic/amide H refined with riding coordinates:
 N005(H005), C009(H009), C00C(H00C), N00K(H00K), C3(H3)
;
_shelx_res_checksum              71077
_shelx_hkl_checksum              77350