Zinc tungstate encapsulated into a scarce Zn(II)-viologen framework with photochromic, electrochromic and chemochromic properties.
Huang, Li; Li, Xiao-Nan; Shen, Yuan; Song, Run-Hong; Cui, Wen-Bo; Zhang, Hong; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5192–5201; doi:10.1039/d3dt03647b

data_7715180
_publ_section_title
;
 Zinc tungstate encapsulated into a scarce Zn(II)-viologen framework with
 photochromic, electrochromic and chemochromic properties.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5192
_journal_page_last               5201
_journal_paper_doi               10.1039/d3dt03647b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'O44 W12 Zn1, C78 H60 N6 O14 Zn3, 6(O)'
_chemical_formula_sum            'C78 H60 N6 O64 W12 Zn4'
_chemical_formula_weight         4573.00
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2h4syd
_audit_creation_date             2023-07-18
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-30 deposited with the CCDC.	2024-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.9542(4)
_cell_length_b                   17.9542(4)
_cell_length_c                   27.4233(8)
_cell_measurement_reflns_used    10580
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.0350
_cell_measurement_theta_min      2.0710
_cell_volume                     7655.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.91a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.852
_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    -38.00  41.00   0.50    2.00    --   -9.26  81.00  18.00  158
  2  \w    -12.00  17.00   0.50    2.00    --   -9.26 -99.00 120.00   58
  3  \w     23.00  64.00   0.50    2.00    --   -9.26  57.00  60.00   82
  4  \w    -36.00  21.00   0.50    2.00    --   -9.26 -81.00-104.00  114
  5  \w     -4.00  28.00   0.50    2.00    --   10.12 -81.00-104.00   64
  6  \w     -3.00  48.00   0.50    2.00    --   10.12 -99.00-180.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0366940000
_diffrn_orient_matrix_UB_12      0.0235484000
_diffrn_orient_matrix_UB_13      -0.0150052000
_diffrn_orient_matrix_UB_21      -0.0271334333
_diffrn_orient_matrix_UB_22      -0.0077272667
_diffrn_orient_matrix_UB_23      -0.0204346667
_diffrn_orient_matrix_UB_31      -0.0008702000
_diffrn_orient_matrix_UB_32      0.0382670000
_diffrn_orient_matrix_UB_33      0.0051189000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            21341
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.418
_diffrn_reflns_theta_min         2.228
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.490
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.91a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.976
_exptl_crystal_description       block
_exptl_crystal_F_000             6270
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.982
_refine_diff_density_min         -7.753
_refine_diff_density_rms         0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4404
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0996P)^2^+309.1270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3334
_reflns_number_total             4404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03647b2.cif
_cod_data_source_block           hl-4_auto
_cod_depositor_comments
'Adding full bibliography for 7715180--7715181.cif.'
_cod_original_cell_volume        7655.7(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7715180
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Zn W C N O H'
_shelx_estimated_absorpt_t_max   0.390
_shelx_estimated_absorpt_t_min   0.205
_reflns_odcompleteness_completeness 96.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O1W) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq,
Uanis(O2W) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(N1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C12(H12)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.086
_oxdiff_exptl_absorpt_empirical_full_min 0.491