Inclusion of viologen cations leads to switchable metal-organic frameworks.
Cadman, Laura K.; Mahon, Mary F.; Burrows, Andrew D.; Faraday discussions 225 (2021) 414–430; doi:10.1039/c9fd00137a

data_1558875
_publ_section_title
;
 Inclusion of viologen cations leads to switchable metal-organic
 frameworks.
;
_journal_name_full               'Faraday discussions'
_journal_page_first              414
_journal_page_last               430
_journal_paper_doi               10.1039/c9fd00137a
_journal_volume                  225
_journal_year                    2021
_chemical_formula_moiety         '0.25(C128 H64 O64 Zn12), C9.6 H11.92 N0.8'
_chemical_formula_sum            'C44.2 H35.32 N2.6 O16.6 Zn3'
_chemical_formula_weight         1064.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-03-22
_audit_creation_method           'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_audit_update_record
;
2019-12-04 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.453(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.7998(10)
_cell_length_b                   9.7204(4)
_cell_length_c                   18.3042(6)
_cell_measurement_reflns_used    4359
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.3700
_cell_measurement_theta_min      4.7460
_cell_volume                     5798.9(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13781
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.85
_diffrn_reflns_theta_min         2.71
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84472
_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            orange-yellow
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       block
_exptl_crystal_F_000             2166
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.311
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         5632
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0655
_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^)+(0.1170P)^2^+8.6579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2023
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4409
_reflns_number_total             5632
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00137a2.cif
_cod_data_source_block           s16lkc21-2-ht
_cod_depositor_comments
'Adding full bibliography for 1558875--1558878.cif.'
_cod_original_cell_volume        5798.9(3)
_cod_original_formula_sum        'C44.20 H35.32 N2.60 O16.60 Zn3'
_cod_database_code               1558875
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C1 \\sim O2-C1 \\sim O7-C13 \\sim O8-C13
 with sigma of 0.005
 O8-C15 \\sim O7-C16 \\sim O1-C3 \\sim O2-C7
 with sigma of 0.005
 O8-C14 \\sim O1-C2
 with sigma of 0.005
 C16-C13 \\sim C15-C13 \\sim C7-C1
 with sigma of 0.005
 N1-C22A \\sim N1-C22
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim N1 \\sim C22 \\sim C22A:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.003
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: N1(0.4) H1(0.36) C21(0.8) H21(0.8) C20(0.8) H20(0.8) C19(0.8)
 C18(0.8) H18(0.8) C17(0.8) H17(0.8) C22(0.44) H22A(0.44) H22B(0.44) H22C(0.44)
 C22A(0.36) H22D(0.36) H22E(0.36) H22F(0.36)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Me refined with riding coordinates:
 C22(H22A,H22B,H22C), C22A(H22D,H22E,H22F)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C15(H15), C16(H16),
 C21(H21), C20(H20), C18(H18), C17(H17)
5.d Fitted hexagon refined as free rotating group:
 N1(C21,C20,C19,C18,C17)
;
_shelx_fab_checksum              5584