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_1551268
_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         '0.25(C40 H52 N20 O16 Zn4), C H3 O'
_chemical_formula_sum            'C11 H16 N5 O5 Zn'
_chemical_formula_weight         363.66
_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
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.0
_cell_angle_beta                 94.870(3)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   9.5741(3)
_cell_length_b                   9.0550(2)
_cell_length_c                   20.4299(7)
_cell_measurement_reflns_used    11630
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.2420
_cell_measurement_theta_min      2.1040
_cell_volume                     1764.75(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.963
_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   60.00    --  -20.00 -68.00   0.00  125
  2  \w   -110.00  15.00   1.00   60.00    --  -20.00 -68.00 120.00  125
  3  \w   -110.00  15.00   1.00   60.00    --  -20.00 -68.00 240.00  125
  4  \w   -110.00  15.00   1.00   60.00    --  -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      -0.0438075000
_diffrn_orient_matrix_UB_12      0.0297044000
_diffrn_orient_matrix_UB_13      0.0230540000
_diffrn_orient_matrix_UB_21      -0.0551329000
_diffrn_orient_matrix_UB_22      0.0077927000
_diffrn_orient_matrix_UB_23      -0.0252307000
_diffrn_orient_matrix_UB_31      -0.0239924000
_diffrn_orient_matrix_UB_32      -0.0720280000
_diffrn_orient_matrix_UB_33      0.0067562000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19799
_diffrn_reflns_point_group_measured_fraction_full 0.808
_diffrn_reflns_point_group_measured_fraction_max 0.773
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.001
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.418
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       irregular
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 1705 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6776
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+1.8126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.513
_reflns_Friedel_fraction_full    0.622
_reflns_Friedel_fraction_max     0.559
_reflns_number_gt                5836
_reflns_number_total             6776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000005.cif
_cod_data_source_block           PCOD1000005
_cod_database_code               1551268
_chemical_oxdiff_formula         'Zn1 C6 H6 O6 N6'
_cell_oxdiff_angle_alpha         90.035(3)
_cell_oxdiff_angle_beta          94.847(3)
_cell_oxdiff_angle_gamma         89.970(3)
_cell_oxdiff_length_a            9.5687(3)
_cell_oxdiff_length_b            9.0586(3)
_cell_oxdiff_length_c            20.4327(6)
_cell_oxdiff_measurement_reflns_used 11630
_cell_oxdiff_volume              1764.75(10)
_reflns_odcompleteness_completeness 96.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Shared sites
{N0, N009}
3. Restrained distances
 C18-O3
 1.43 with sigma of 0.02
4. Rigid bond restraints
 O00L, N00O, O00S, C00W, N011, C012, C013, C015, O2, C4, C15, N17, N13, C19,
 O6, C7, Zn01
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O00L \\sim N00O \\sim O00S \\sim C00W \\sim N011 \\sim C012 \\sim C013 \\sim
C015 \\sim O2 \\sim C4 \\sim C15 \\sim N17 \\sim N13 \\sim C19 \\sim O6 \\sim
C7 \\sim Zn01: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N0) = Uanis(N009)
Uanis(N0) = Uanis(N009)
6. Others
 Sof(H00E)=Sof(O2)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C15)=Sof(N17)=Sof(H17)=
 Sof(N13)=Sof(H13A)=Sof(H13B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(O6)=Sof(C7)=
 Sof(N0)=Sof(H0)=Sof(O3)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=1-FVAR(1)
 Sof(N009)=Sof(H009)=Sof(H00H)=Sof(O00L)=Sof(N00O)=Sof(H00L)=Sof(H00M)=
 Sof(O00S)=Sof(C00W)=Sof(H00P)=Sof(H00Q)=Sof(N011)=Sof(H011)=Sof(C012)=
 Sof(C013)=Sof(C015)=Sof(H01C)=Sof(H01D)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=
 Sof(H0AC)=Sof(O5)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C00H(H00H), C00H(H00E), C00V(H00V)
7.b Secondary CH2 refined with riding coordinates:
 N00D(H00C,H00D), C00M(H00F,H00G), C00N(H00J,H00K), N00O(H00L,H00M), C00Q(H00N,
 H00O), C00W(H00P,H00Q), C010(H01A,H01B), C015(H01C,H01D), C4(H4A,H4B),
 N13(H13A,H13B), C19(H19A,H19B)
7.c Aromatic/amide H refined with riding coordinates:
 N009(H009), N00A(H00A), C00B(H00B), C00I(H00I), N00T(H00T), C00X(H00X),
 C00Y(H00Y), N011(H011), N17(H17), N0(H0)
7.d Idealised Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C0AA(H0AA,H0AB,H0AC), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              90127
_shelx_hkl_checksum              14447
_shelx_fab_checksum              37937
_shelx_shelxl_version_number     2014/7