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_1558876
_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), 1.4(C3 H7 N1 O1), 0.9(C14 H18 N2), 0.7(O1)'
_chemical_formula_sum            'C49.2 H46.78 N3.4 O18.7 Zn3'
_chemical_formula_weight         1180.99
_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             2017-01-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289)
;
_audit_update_record
;
2019-12-04 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.534(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.6406(6)
_cell_length_b                   9.63384(16)
_cell_length_c                   18.4404(4)
_cell_measurement_reflns_used    12148
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.5940
_cell_measurement_theta_min      4.7730
_cell_volume                     5660.47(19)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26374
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.870
_diffrn_reflns_theta_min         4.796
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77967
_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            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             2422
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.034
_platon_squeeze_details
;
TITL
CELL   32.6406    9.6338   18.4404     90.00    102.53     90.00
SPGR C2/c
C101 0.541 0.472 0.033 !       6.39 eA-3
C102 0.454 0.354 0.713 !       4.20 eA-3
Q103 0.545 0.428 0.187 !       3.04 eA-3
Q104 0.081 0.228 0.858 !       1.34 eA-3
Q105 0.103 0.377 0.208 !       1.22 eA-3
Q106 0.603 0.058 0.952 !       1.06 eA-3
Q107 0.563 0.280 0.944 !       0.99 eA-3
Q108 0.125 0.191 0.884 !       0.97 eA-3
Q109 0.876 0.474 0.322 !       0.87 eA-3
Q110 0.111 0.279 0.851 !       0.84 eA-3
Q111 0.883 0.501 0.981 !       0.83 eA-3
Q112 0.946 0.125 0.639 !       0.83 eA-3
Q113 0.384 0.122 0.347 !       0.82 eA-3
Q114 0.384 0.318-0.003 !       0.82 eA-3
Q115 0.029 0.205 0.826 !       0.82 eA-3
Q116 0.624 0.191 0.952 !       0.81 eA-3
Q117 0.900 0.184 0.589 !       0.77 eA-3
C118 0.959 0.122 0.308 !       0.75 eA-3
Q119 0.328 0.039 0.113 !       0.74 eA-3
Q120 0.991 0.338 0.471 !       0.74 eA-3
Q121 0.638 0.323 0.468 !       0.73 eA-3
Q122 0.670 0.090 0.651 !       0.73 eA-3
Q123 0.661 0.028 0.644 !       0.73 eA-3
Q124 0.146 0.184 0.368 !       0.72 eA-3
Q125 0.646 0.684 0.368 !       0.72 eA-3
Q126 0.231 0.072 0.263 !       0.72 eA-3
Q127 0.866 0.115 0.551 !       0.71 eA-3
Q128 0.227 0.153 0.406 !       0.71 eA-3
Q129 0.349 0.215 0.501 !       0.69 eA-3
Q130 0.147 0.191 0.400 !       0.68 eA-3
Q131 0.407 0.349 0.068 !       0.68 eA-3
Q132 0.150 0.156 0.548 !       0.66 eA-3
Q133 0.859 0.066 0.264 !       0.65 eA-3
Q134 0.584 0.193 0.917 !       0.64 eA-3
Q135 0.045 0.101 0.801 !       0.64 eA-3
Q136 0.687 0.117 0.979 !       0.63 eA-3
Q137 0.962 0.336 0.815 !       0.61 eA-3
Q138 0.669 0.033 0.174 !       0.60 eA-3
Q139 0.723 0.245 0.002 !       0.60 eA-3
Q140 0.343 0.223 0.465 !       0.59 eA-3
Q141 0.359 0.127 0.293 !       0.57 eA-3
Q142 0.039 0.423 0.017 !       0.57 eA-3
Q143 0.679 0.203 0.965 !       0.57 eA-3
Q144 0.837 0.155 0.048 !       0.55 eA-3
Q145 0.814 0.053 0.875 !       0.54 eA-3
C146 0.500 0.342 0.744 !       0.54 eA-3
Q147 0.214 0.122 0.569 !       0.53 eA-3
Q148 0.553 0.046 0.250 !       0.51 eA-3
Q149 0.649 0.147 0.653 !       0.51 eA-3
Q150 0.373 0.079 0.294 !       0.51 eA-3
Q151 0.789 0.457 0.564 !       0.51 eA-3
Q152 0.860 0.154 0.049 !       0.50 eA-3
Q153 0.852 0.292 0.069 !       0.50 eA-3
;
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         26374
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0827P)^2^+23.4221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21569
_reflns_number_total             26374
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9fd00137a2.cif
_cod_data_source_block           s16lkc12_sq-7-prime
_cod_depositor_comments
'Adding full bibliography for 1558875--1558878.cif.'
_cod_original_cell_volume        5660.48(19)
_cod_original_formula_sum        'C49.20 H46.78 N3.40 O18.70 Zn3'
_cod_database_code               1558876
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C26 \\sim N2-C27 \\sim C28-C27 \\sim C28-C24 \\sim C25-C24 \\sim C26-C25
\\sim C22-C21 \\sim C21-C20 
 C20-C19 \\sim N1-C19 \\sim N1-C23 \\sim C23-C22
 with sigma of 0.1
 N2-C29 \\sim N1-C18
 with sigma of 0.005
 N3-C33 \\sim N3-C32 \\sim N4-C35 \\sim N4-C36
 with sigma of 0.005
 N3-C31 \\sim N4-C34
 with sigma of 0.005
 O10-C34 \\sim O9-C31
 with sigma of 0.005
 C36-C35 \\sim C33-C32
 with sigma of 0.005
 C34-C36 \\sim C33-C31
 with sigma of 0.005
3. Restrained planarity
 C34, O10, C36, N4, C35
 with sigma of 0.1
 O9, N3, C32, C31, C33
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C34 \\sim O10 \\sim C36 \\sim N4 \\sim C35: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.005
O9 \\sim N3 \\sim C32 \\sim C31 \\sim C33: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.005
C21 \\sim C20 \\sim C19 \\sim C23 \\sim C22: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(N2) = Uanis(N3)
5. Others
 Fixed Sof: O9(0.35) N3(0.35) C31(0.35) H31(0.35) C32(0.35) H32A(0.35)
 H32B(0.35) H32C(0.35) C33(0.35) H33A(0.35) H33B(0.35) H33C(0.35) O10(0.35)
 N4(0.35) C34(0.35) H34(0.35) C35(0.35) H35A(0.35) H35B(0.35) H35C(0.35)
 C36(0.35) H36A(0.35) H36B(0.35) H36C(0.35) N1(0.45) N2(0.45) C27(0.45)
 H27(0.45) C28(0.45) H28(0.45) C24(0.45) C25(0.45) H25(0.45) C26(0.45)
 H26(0.45) C17(0.45) H17A(0.45) H17B(0.45) H17C(0.45) C18(0.45) H18A(0.45)
 H18B(0.45) C19(0.45) H19(0.45) C20(0.45) H20(0.45) C21(0.45) C22(0.45)
 H22(0.45) C23(0.45) H23(0.45) C29(0.45) H29A(0.45) H29B(0.45) C30(0.45)
 H30A(0.45) H30B(0.45) H30C(0.45) O11(0.35)
6.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C29(H29A,H29B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C11(H11), C12(H12), C15(H15), C16(H16),
 C31(H31), C34(H34), C27(H27), C28(H28), C25(H25), C26(H26), C19(H19), C20(H20),
  C22(H22), C23(H23)
6.c Fitted hexagon refined as free rotating group:
 N2(C27,C28,C24,C25,C26)
6.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C17(H17A,H17B,H17C), C30(H30A,H30B,H30C)
;
_platon_squeeze_void_probe_radius 1.20