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_1551267
_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 syn
_chemical_formula_moiety         'C20 H26 N10 O8 Zn2'
_chemical_formula_sum            'C20 H26 N10 O8 Zn2'
_chemical_formula_weight         665.25
_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
_cell_angle_beta                 99.356(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6138(10)
_cell_length_b                   9.1020(8)
_cell_length_c                   20.131(3)
_cell_measurement_reflns_used    10509
_cell_measurement_temperature    100
_cell_measurement_theta_max      20.798
_cell_measurement_theta_min      2.051
_cell_volume                     1738.1(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.0957
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10509
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        20.798
_diffrn_reflns_theta_max         20.798
_diffrn_reflns_theta_min         2.051
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84594
_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    1.271
_exptl_crystal_description       irregular
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Flack x determined using 805 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         3404
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1092P)^2^+6.2671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.2034
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    0.890
_reflns_Friedel_fraction_max     0.890
_reflns_number_gt                2461
_reflns_number_total             3404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1000004.cif
_cod_data_source_block           PCOD1000004
_cod_original_cell_volume        1738.2(3)
_cod_database_code               1551267
_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
2. Uiso/Uaniso restraints and constraints
Uanis(O00A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N00B, Zn01, O005, C00F, C00K, C00S, C00U, C00O, O008, C00J, N009, C00V, N00L,
 C007, N00N, C014, O00G, C016, N00W, Zn02, N00Q, C00R, C012, C00H, C00M, N00D,
 C00P, N00I, C00T, C011, O003, O004, O006, C013, N00Z, C00X, O00E, C00Y, N00C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C00K(H00K), C00P(H00P)
4.b Secondary CH2 refined with riding coordinates:
 N00C(H00A,H00C), C00J(H00D,H00E), C00M(H00F,H00G), C00S(H00J,H00M), N00W(H00N,
 H00O), C00Y(H00Q,H00R), C013(H01A,H01B), C016(H01C,H01D)
4.c Aromatic/amide H refined with riding coordinates:
 C007(H007), N00B(H00B), C00H(H00H), N00I(H00I), N00L(H00L), C00V(H00V),
 N00Z(H00Z), C012(H012)
;
_shelx_res_checksum              5537
_shelx_hkl_checksum              28030
_shelx_fab_checksum              62270
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'