Molecular Nonvolatile Memory Based on [α-GeW12O40]4‒/Metalloviologen Hybrids Can Work at High Temperature Monitored by Chromism
Chen, Bin; Huang, You-Ren; Song, Kai-Yue; Lin, Xiang-Ling; Li, Hao-Hong; Chen, Zhi-Rong; Chemistry of Materials 33 (2021) 2178–2186; doi:10.1021/acs.chemmater.1c00090

data_4003880
_publ_section_title
;
 Molecular Nonvolatile Memory Based on [\a-GeW12O40]4--/Metalloviologen
 Hybrids Can Work at High Temperature Monitored by Chromism
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              2178
_journal_page_last               2186
_journal_paper_doi               10.1021/acs.chemmater.1c00090
_journal_volume                  33
_journal_year                    2021
_chemical_formula_moiety
'C40 H44 Co2 N8 O14, Ge O40 W12, O, [+ solvents]'
_chemical_formula_sum            'C40 H44 Co2 Ge N8 O55 W12'
_chemical_formula_weight         3913.48
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_cell_angle_alpha                92.367(4)
_cell_angle_beta                 96.922(3)
_cell_angle_gamma                98.281(4)
_cell_formula_units_Z            1
_cell_length_a                   11.8584(4)
_cell_length_b                   12.0820(6)
_cell_length_c                   13.0866(5)
_cell_measurement_reflns_used    10535
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.1110
_cell_measurement_theta_min      2.1790
_cell_volume                     1838.60(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.826
_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     24.00  67.00   0.50    5.11    --   -9.80  14.00-180.00   86
  2  \w    -11.00  79.00   0.50    5.11    --   -9.80  55.00  60.00  180
  3  \w    -89.00 -62.00   0.50    5.11    --   -9.80  55.00-150.00   54
  4  \w    -23.00  75.00   0.50    5.11    --   -9.80  55.00-150.00  196
  5  \w    -95.00 -47.00   0.50    5.11    --   -9.80  55.00 -30.00   96
  6  \w    -46.00  65.00   0.50    5.11    --   -9.80  55.00 -30.00  222
  7  \w    -84.00 -59.00   0.50    5.11    --   -9.80  43.00 120.00   50
  8  \w     -6.00  21.00   0.50    5.11    --   -9.80  43.00 120.00   54
  9  \w     45.00  80.00   0.50    5.11    --   -9.80  43.00 120.00   70
 10  \w    -40.00 -12.00   0.50    5.11    --   -9.80  14.00-180.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0045661000
_diffrn_orient_matrix_UB_12      -0.0130406000
_diffrn_orient_matrix_UB_13      -0.0538254000
_diffrn_orient_matrix_UB_21      -0.0112232000
_diffrn_orient_matrix_UB_22      -0.0579172000
_diffrn_orient_matrix_UB_23      0.0085462000
_diffrn_orient_matrix_UB_31      -0.0597282000
_diffrn_orient_matrix_UB_32      0.0027700000
_diffrn_orient_matrix_UB_33      -0.0046300000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24165
_diffrn_reflns_point_group_measured_fraction_full 0.851
_diffrn_reflns_point_group_measured_fraction_max 0.661
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.679
_diffrn_reflns_theta_min         2.249
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull light colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.534
_exptl_crystal_description       block
_exptl_crystal_F_000             1754
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.947
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.267
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.301(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         13771
_refine_ls_number_restraints     274
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0421P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.600
_reflns_Friedel_fraction_full    0.705
_reflns_Friedel_fraction_max     0.495
_reflns_number_gt                11473
_reflns_number_total             13771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm1c00090_si_003.cif
_cod_data_source_block           cojiare
_cod_depositor_comments
'Adding full bibliography for 4003879--4003880.cif.'
_cod_database_code               4003880
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.440
_shelx_estimated_absorpt_t_min   0.244
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.699(15)
 0.301(15)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 Co1-H01C \\sim Co1-H01D
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C02O) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C00V) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O00J) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O01Y) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C02F) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O02Z) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(W001) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C028) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C025) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C02P) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O026) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N01V) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01O) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N01F, C01O, C01T, C02P, C02Q, C02W, C02X, C0AA, C37, C38, C020, N017
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O00J, N015, C01E, C02C, C02I, C02N, C02S, C02T, C28, C31, N01V, C02F, C02K
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 H01I, C028, C36
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6.a Free rotating group:
 O014(H01C,H01D)
6.b Rotating group:
 O00M(H00A,H00B), O013(H01A,H01B), O01I(H01E,H01F), O01K(H01G,H01H), O01R(H01I,
 H01J)
6.c Aromatic/amide H refined with riding coordinates:
 C00V(H00V), C01O(H01O), C01T(H01T), C01W(H01W), C01Z(H01Z), C020(H020),
 C023(H023), C024(H024), C025(H025), C028(H028), C02B(H02B), C02C(H02C),
 C02F(H02F), C02I(H02I), C02K(H02K), C02L(H02L), C02N(H02N), C02P(H02P),
 C02Q(H02Q), C02T(H02T), C02W(H02W), C28(H28), C02X(H02X), C02Y(H02Y), C31(H31),
  C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C43(H43), C46(H46)
;
_shelx_res_checksum              22000
_shelx_hkl_checksum              21859
_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 2.977
_oxdiff_exptl_absorpt_empirical_full_min 0.569