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_1551274
_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, 0.5(H2 O)'
_chemical_formula_sum            'C10 H14 N5 O4.5 Zn'
_chemical_formula_weight         341.63
_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
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90.887(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2589(8)
_cell_length_b                   9.1136(6)
_cell_length_c                   19.0252(11)
_cell_measurement_reflns_used    2127
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.0280
_cell_measurement_theta_min      2.1350
_cell_volume                     1258.46(18)
_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)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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
;
List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -110.00  15.00   1.00  230.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00  230.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00  230.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00  230.00    --  -20.00 -30.00  90.00  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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0378027000
_diffrn_orient_matrix_UB_12      -0.0168177000
_diffrn_orient_matrix_UB_13      0.0332010000
_diffrn_orient_matrix_UB_21      0.0900773000
_diffrn_orient_matrix_UB_22      -0.0095174000
_diffrn_orient_matrix_UB_23      0.0142385000
_diffrn_orient_matrix_UB_31      0.0030956000
_diffrn_orient_matrix_UB_32      0.0753924000
_diffrn_orient_matrix_UB_33      0.0092139000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1349
_diffrn_reflns_av_unetI/netI     0.1441
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12491
_diffrn_reflns_point_group_measured_fraction_full 0.852
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88232
_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    1.803
_exptl_crystal_description       plate
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.075
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 557 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         3794
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1537
_refine_ls_R_factor_gt           0.0809
_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^)+(0.0934P)^2^+1.1757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.2106
_reflns_Friedel_coverage         0.593
_reflns_Friedel_fraction_full    0.681
_reflns_Friedel_fraction_max     0.681
_reflns_number_gt                2188
_reflns_number_total             3794
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000011.cif
_cod_data_source_block           PCOD1000011
_cod_original_cell_volume        1258.45(18)
_cod_original_formula_sum        'C10 H14 N5 O4.50 Zn'
_cod_database_code               1551274
_chemical_oxdiff_formula         'Zn C10 H10 N5 O4'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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 O(H,H) groups
2. Rigid bond restraints
 O29, C27, O28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O28 \\sim C27 \\sim O29: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.02
C7 \\sim C8 \\sim N11 \\sim C6: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
C26 \\sim C25 \\sim N30 \\sim C27: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(N20) = Uanis(C21) = Uanis(C22) = Uanis(C24) = Uanis(N23)
Uanis(C5) = Uanis(C4) = Uanis(N3) = Uanis(C2) = Uanis(N1)
4.a Free rotating group:
 O5(H5A,H5B)
4.b Ternary CH refined with riding coordinates:
 C26(H26), C7(H7)
4.c Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C6(H6A,H6B), N38(H38A,H38B), N19(H19A,H19B), C37(H37A,H37B),
 C18(H18A,H18B), C33(H33A,H33B), C14(H14A,H14B)
4.d Aromatic/amide H refined with riding coordinates:
 C22(H22), C5(H5), C2(H2), C24(H24), N15(H15), N34(H34), N30(H30), N11(H11)
4.e Fitted pentagon refined as free rotating group:
 N1(C5,C4,N3,C2)
;
_shelx_res_checksum              53290