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_1551270
_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, C3 H7 N O, 3(H2 O)'
_chemical_formula_sum            'C13 H26 N6 O8 Zn'
_chemical_formula_weight         459.77
_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   mixed
_cell_angle_alpha                90
_cell_angle_beta                 106.106(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6861(4)
_cell_length_b                   8.9799(3)
_cell_length_c                   11.4935(6)
_cell_measurement_reflns_used    10643
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.4120
_cell_measurement_theta_min      1.8230
_cell_volume                     960.47(8)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   60.0000 125
  3 omega -110.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  120.0000 125
  4 omega -110.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  180.0000 125
  5 omega -110.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  240.0000 125
  6 omega -110.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000  -68.0000  300.0000 125
  7 omega -110.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000    0.0000    0.0000 125
  8 omega -110.00   15.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.0000    0.0000  180.0000 125
;
_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      -0.0146807000
_diffrn_orient_matrix_UB_12      0.0077271000
_diffrn_orient_matrix_UB_13      -0.0637262000
_diffrn_orient_matrix_UB_21      0.0689711000
_diffrn_orient_matrix_UB_22      -0.0289031000
_diffrn_orient_matrix_UB_23      0.0028074000
_diffrn_orient_matrix_UB_31      -0.0288311000
_diffrn_orient_matrix_UB_32      -0.0730819000
_diffrn_orient_matrix_UB_33      -0.0079074000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19470
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_min         1.844
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89062
_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    1.590
_exptl_crystal_description       irregular
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 1290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3768
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0565P)^2^+0.6810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.922
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                3346
_reflns_number_total             3768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000007.cif
_cod_data_source_block           PCOD1000007
_cod_original_cell_volume        960.47(7)
_cod_database_code               1551270
_reflns_odcompleteness_completeness 100.00
_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, All O(H,H) groups
2.a Free rotating group:
 O008(H00T,H00U), O009(H00V,H00W), O00E(H00X,H00Y)
2.b Ternary CH refined with riding coordinates:
 C00N(H00N)
2.c Secondary CH2 refined with riding coordinates:
 N00A(H00A,H00B), C00K(H00C,H00E), C00L(H00G,H00H), C00O(H00J,H00K)
2.d Aromatic/amide H refined with riding coordinates:
 N006(H006), N00D(H00D), C00F(H00F), C00I(H00I), C00P(H00P)
2.e Idealised Me refined as rotating group:
 C00R(H00L,H00M,H00O), C00S(H00Q,H00R,H00S)
;
_shelx_res_checksum              92876
_shelx_hkl_checksum              53244
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'