Photochromic and Electrochromic Properties of Viologen-Based Multifunctional Cd-MOF
Zang, Shuang-Quan; Li, Hai-Yang; Hua, Xue; Fu, Ting; Liu, Xiao-Fei; Chemical Communications  (2022) –; doi:10.1039/D2CC02703H

data_7130210
_publ_section_title
;
 Photochromic and Electrochromic Properties of Viologen-Based
 Multifunctional Cd-MOF
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC02703H
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H34 Cd2 N4 O16, 5(H2 O)'
_chemical_formula_sum            'C42 H44 Cd2 N4 O21'
_chemical_formula_weight         1165.61
_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     iterative
_audit_creation_date             2021-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-21 deposited with the CCDC.	2022-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.01
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.81340(15)
_cell_length_b                   24.0719(4)
_cell_length_c                   10.19512(14)
_cell_measurement_reflns_used    4897
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.9830
_cell_measurement_theta_min      3.6860
_cell_volume                     2162.95(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_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    -29.00  46.00   0.50    0.50    --    0.00  57.00  60.00  150
  2  \w     13.00  39.00   0.50    0.50    --    0.00  57.00 -60.00   52
  3  \w     11.00 131.00   0.50    0.91    --   97.60 -30.00 -60.00  240
  4  \w     33.00  69.00   0.50    0.91    --   97.60 -82.00 150.00   72
  5  \w     83.00 109.00   0.50    0.91    --   97.60 -82.00 150.00   52
  6  \w     56.00 122.00   0.50    0.91    --   97.60 -82.00  90.00  132
  7  \w     36.00 112.00   0.50    0.91    --   97.60 -45.00-150.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0206199000
_diffrn_orient_matrix_UB_12      0.0214854000
_diffrn_orient_matrix_UB_13      0.1411268000
_diffrn_orient_matrix_UB_21      -0.0035709000
_diffrn_orient_matrix_UB_22      0.0602866000
_diffrn_orient_matrix_UB_23      -0.0506682000
_diffrn_orient_matrix_UB_31      -0.1736230000
_diffrn_orient_matrix_UB_32      0.0013157000
_diffrn_orient_matrix_UB_33      0.0177990000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0595
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6188
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.244
_diffrn_reflns_theta_min         3.672
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 1466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         5140
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0645P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1166
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.864
_reflns_Friedel_fraction_max     0.812
_reflns_number_gt                4934
_reflns_number_total             5140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02703h2.cif
_cod_data_source_block           D-Cd-MOF
_cod_database_code               7130210
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N Cd'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.240
_shelx_estimated_absorpt_t_min   0.180
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.523(2)
 0.477(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
3. Restrained distances
 C42-C41 = C40-C39
 1.5 with sigma of 0.01
 C40-C41
 1.55 with sigma of 0.01
 O11-C40 = C41-O12
 1.4 with sigma of 0.01
 O13-C42 = O14-C42 = O9-C39 = O10-C39
 1.25 with sigma of 0.01
 C28-C25 = C9-C6
 1.5 with sigma of 0.01
 N1-C9 = N4-C28
 1.45 with sigma of 0.01
 Cd2-N3_$1
 2.27 with sigma of 0.01
 O2W-H2Wb = O2W-H2Wa = O1W-H1Wb = O1W-H1Wa
 0.85 with sigma of 0.01
 H28a-H4Wa
 2.1 with sigma of 0.01
 H7Wa-H1Wa_$2
 2.1 with sigma of 0.01
 O5W-H5Wa
 0.85 with sigma of 0.01
 H5Wa_$3-H2Wa_$4
 2.1 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C35
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Everything fixed:
 O3W, H3Wa, H3Wb, O4W, H4Wa, H4Wb, O5W, H5Wa, H5Wb, O6W, H6Wa, H6Wb
6.b Free rotating group:
 O7W(H7Wa,H7Wb)
6.c Rotating group:
 O1W(H1Wa,H1Wb), O2W(H2Wa,H2Wb)
6.d Ternary CH refined with riding coordinates:
 C40(H40), C41(H41)
6.e Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C28(H28a,H28b)
6.f Aromatic/amide H refined with riding coordinates:
 C19(H19), C18(H18), C16(H16), C15(H15), C33(H33), C32(H32), C30(H30),
 C29(H29), C3(H3), C5(H5), C7(H7), C11(H11a), C10(H10), C14(H14), C13(H13),
 C22(H22), C24(H24), C26(H26), C34(H34), C35(H35), C37(H37), C38(H38)
6.g Fitted hexagon refined as free rotating group:
 N2(C19,C18,C17,C16,C15), N4(C33,C32,C31,C30,C29), C12(C11,C10,N1,C14,C13)
6.h Idealised tetrahedral OH refined as rotating group:
 O11(H11), O12(H12)
;
_shelx_res_checksum              1828
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.635
_oxdiff_exptl_absorpt_empirical_full_min 0.564