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_7130211
_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         1165.63
_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     dual
_audit_creation_date             2021-06-21
_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                 90.06
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.74302(7)
_cell_length_b                   23.97044(18)
_cell_length_c                   10.19537(8)
_cell_measurement_reflns_used    19691
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      70.0010
_cell_measurement_theta_min      3.6990
_cell_volume                     2136.68(3)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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      4.00  88.00   0.50    0.50    --    0.00  57.00 120.00  168
  2  \w    -89.00  19.00   0.50    0.50    --    0.00 -38.00 150.00  216
  3  \w     30.00  76.00   0.50    0.50    --    0.00  38.00  60.00   92
  4  \w    -28.00  20.00   0.50    0.50    --    0.00  38.00  60.00   96
  5  \w    143.00 188.00   0.50    0.50    --   98.80  61.00  30.00   90
  6  \w     72.00 187.00   0.50    0.50    --   98.80  45.00  90.00  230
  7  \w     94.00 129.00   0.50    0.50    --   98.80 -61.00 150.00   70
  8  \w     14.00 129.00   0.50    0.50    --   98.80 -61.00 -60.00  230
  9  \w     90.00 116.00   0.50    0.50    --   98.80  61.00  30.00   52
 10  \w     66.00 159.00   0.50    0.50    --   98.80  30.00-120.00  186
 11  \w     12.00 133.00   0.50    0.50    --   98.80 -82.00 150.00  242
 12  \w      9.00 121.00   0.50    0.50    --   98.80 -82.00  30.00  224
 13  \w     73.00 102.00   0.50    0.50    --   98.80 -82.00 -30.00   58
 14  \w     10.00  90.00   0.50    0.50    --   98.80 -61.00 150.00  160
 15  \w     91.00 127.00   0.50    0.50    --   98.80  45.00   0.00   72
 16  \w     38.00  98.00   0.50    0.50    --   98.80 -82.00 -60.00  120
 17  \w     64.00 104.00   0.50    0.50    --   98.80 -61.00  30.00   80
 18  \w     87.00 163.00   0.50    0.50    --   98.80  30.00-150.00  152
 19  \w     94.00 120.00   0.50    0.50    --   98.80 -82.00  90.00   52
 20  \w     83.00 117.00   0.50    0.50    --   98.80 -82.00-120.00   68
 21  \w     71.00 178.00   0.50    0.50    --   98.80  45.00 120.00  214
;
_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      0.0455018000
_diffrn_orient_matrix_UB_12      -0.0601357000
_diffrn_orient_matrix_UB_13      0.0363679000
_diffrn_orient_matrix_UB_21      0.1423997000
_diffrn_orient_matrix_UB_22      0.0222856000
_diffrn_orient_matrix_UB_23      0.0717930000
_diffrn_orient_matrix_UB_31      -0.0931228000
_diffrn_orient_matrix_UB_32      0.0045790000
_diffrn_orient_matrix_UB_33      0.1278973000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20167
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.071
_diffrn_reflns_theta_min         3.688
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.788
_exptl_absorpt_correction_T_max  0.76800
_exptl_absorpt_correction_T_min  0.74100
_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    1.812
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.041
_exptl_crystal_size_mid          0.033
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.585
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 3388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         7510
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0926P)^2^+0.5913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7509
_reflns_number_total             8126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02703h2.cif
_cod_data_source_block           L-Cd-MOF
_cod_database_code               7130211
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N S Ag'
_chemical_oxdiff_usercomment     ' '
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.715
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5745(19)
 0.4255(19)
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-C41 = C40-C39
 1.48 with sigma of 0.01
 O9-C39 = O10-C39 = O14-C42 = O13-C42
 1.28 with sigma of 0.01
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C10 \\sim C11: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C31 \\sim C30: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C16 \\sim C15: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C15 \\sim C16 \\sim N2 \\sim C19 \\sim C18: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
C15 \\sim C16 \\sim N2: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6.a Everything fixed:
 C15
6.b Free rotating group:
 O6W(H6WA,H6WB), O7W(H7WA,H7WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB), O3W(H3WA,H3WB)
6.c Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
6.d Ternary CH refined with riding coordinates:
 C40(H40), C41(H41)
6.e Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C9(H9A,H9B)
6.f Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C14(H14), C34(H34), C32(H32), C24(H24), C22(H22), C5(H5),
 C18(H18), C16(H16), C26(H26), C13(H13), C35(H35), C38(H38), C37(H37), C30(H30),
  C29(H29), C33(H33), C7(H7), C15(H15), C19(H19), C11(H11A)
6.g Idealised tetrahedral OH refined as rotating group:
 O12(H12), O11(H11)
;
_shelx_res_checksum              25633
_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 1.333
_oxdiff_exptl_absorpt_empirical_full_min 0.785