Polyoxometalate/<i>s</i>-triazine hybrid heterostructures with ultrafast photochromic properties.
Chen, Yue-Chen; Di, Yi-Ming; Zhang, Shu-Quan; Lin, Mei-Jin; Dalton transactions (Cambridge, England : 2003) 53 (2024) 3215–3223; doi:10.1039/d3dt04157c

data_7714979
_publ_section_title
;
 Polyoxometalate/<i>s</i>-triazine hybrid heterostructures with ultrafast
 photochromic properties.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3215
_journal_page_last               3223
_journal_paper_doi               10.1039/d3dt04157c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'O40 P W12, 2(C18 H13.5 N6)'
_chemical_formula_sum            'C36 H27 N12 O40 P W12'
_chemical_formula_weight         3504.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-05 deposited with the CCDC.	2024-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.724(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.2182(4)
_cell_length_b                   10.4154(3)
_cell_length_c                   22.7385(7)
_cell_measurement_reflns_used    8116
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5970
_cell_measurement_theta_min      2.1750
_cell_volume                     3126.94(16)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -56.00  80.00   0.50    6.00    --   -9.80  29.00 120.00  272
  2  \w    -88.00 -62.00   0.50    6.00    --   -9.80  43.00-120.00   52
  3  \w    -92.00  63.00   0.50    6.00    --   -9.80  43.00  90.00  310
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21448
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.151
_exptl_absorpt_coefficient_mu    22.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09390
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.722
_exptl_crystal_description       plate
_exptl_crystal_F_000             3100
_exptl_crystal_size_min          0.3
_refine_diff_density_max         3.427
_refine_diff_density_min         -2.615
_refine_diff_density_rms         0.384
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         5513
_refine_ls_number_restraints     700
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0789P)^2^+124.3715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4355
_reflns_number_total             5513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04157c2.cif
_cod_data_source_block           hybrid2
_cod_depositor_comments
'Adding full bibliography for 7714976--7714979.cif.'
_cod_database_code               7714979
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 W006-O00Q \\sim W006-O00R
 with sigma of 0.02
 W005-O00Q \\sim W005-O00R
 with sigma of 0.02
 W003-O00P \\sim W003-O3
 with sigma of 0.02
 W006-O00H \\sim W006-O1
 with sigma of 0.02
 W001-O00H \\sim W001-O1
 with sigma of 0.02
 W003-O00O \\sim W003-O2
 with sigma of 0.02
3. Rigid bond restraints
 C00N, C15, C18, C3, C13, C1, N3, N4, N17, C19, C12, N5, C11, C9, C7, C6, C10,
 C8, C21, C23, C20, N22, N16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O00K, W001, O009, O00A, O00G, O00H, O00M, O14, W003, W002, W006, P07, O15,
 O00C, O00I, O00O, O00P, O13, O00D, O00L, O00Q, O18, W004, W005, O008, O00E,
 O00F
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(W006) \\sim Ueq, Uanis(W001) \\sim Ueq, Uanis(O009) \\sim Ueq,
Uanis(O00A) \\sim Ueq, Uanis(O00G) \\sim Ueq, Uanis(O00H) \\sim Ueq,
Uanis(O00M) \\sim Ueq, Uanis(W003) \\sim Ueq, Uanis(W002) \\sim Ueq,
Uanis(O00C) \\sim Ueq, Uanis(O00I) \\sim Ueq, Uanis(O00O) \\sim Ueq,
Uanis(O00P) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O00D)
\\sim Ueq, Uanis(O00L) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O00K) \\sim Ueq,
Uanis(O00Q) \\sim Ueq, Uanis(P07) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(W004)
\\sim Ueq, Uanis(W005) \\sim Ueq, Uanis(O008) \\sim Ueq, Uanis(O00E) \\sim Ueq,
Uanis(O00F) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00N) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq,
Uanis(N17) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N5)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C6) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C21)
\\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N22) \\sim Ueq,
Uanis(N16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N16) \\sim Ueq, Uanis(C00N) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N17) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(N22) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(W001) \\sim Ueq, Uanis(W002) \\sim Ueq, Uanis(W003) \\sim Ueq,
Uanis(W004) \\sim Ueq, Uanis(W005) \\sim Ueq, Uanis(W006) \\sim Ueq, Uanis(P07)
\\sim Ueq, Uanis(O008) \\sim Ueq, Uanis(O009) \\sim Ueq, Uanis(O00A) \\sim Ueq,
Uanis(O00C) \\sim Ueq, Uanis(O00D) \\sim Ueq, Uanis(O00E) \\sim Ueq,
Uanis(O00F) \\sim Ueq, Uanis(O00G) \\sim Ueq, Uanis(O00H) \\sim Ueq,
Uanis(O00I) \\sim Ueq, Uanis(O00K) \\sim Ueq, Uanis(O00L) \\sim Ueq,
Uanis(O00O) \\sim Ueq, Uanis(O00P) \\sim Ueq, Uanis(O00Q) \\sim Ueq, Uanis(O13)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O18) \\sim Ueq,
Uanis(O00M) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O00R) \\sim Ueq, Uanis(O00Q) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O008) \\sim Ueq, Uanis(W001) \\sim Ueq, Uanis(O00M) \\sim Ueq,
Uanis(O00A) \\sim Ueq, Uanis(O009) \\sim Ueq, Uanis(O00G) \\sim Ueq,
Uanis(O00H) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(W003) \\sim Ueq, Uanis(W002)
\\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(W006) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(O00C) \\sim Ueq, Uanis(O00P) \\sim Ueq, Uanis(O00I) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(O00O) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O00L) \\sim Ueq,
Uanis(O00D) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(P07) \\sim Ueq, Uanis(O00K)
\\sim Ueq, Uanis(O00R) \\sim Ueq, Uanis(O00Q) \\sim Ueq, Uanis(W005) \\sim Ueq,
Uanis(W004) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O00F) \\sim Ueq, Uanis(O00E)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N16, N3, C19, C3, N5, C11, C00N, N4, C12, C6, C7, C18, C15, C9, C23, C21, N22,
  C1, C13, N17, C8, C10, C20, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(O00R)=1-FVAR(1)
 Sof(O00Q)=FVAR(1)
 Sof(O1)=1-FVAR(2)
 Sof(O00H)=FVAR(2)
 Sof(O2)=1-FVAR(3)
 Sof(O00O)=FVAR(3)
 Sof(O3)=1-FVAR(4)
 Sof(O00P)=FVAR(4)
 Fixed Sof: O13(0.5) O14(0.5) O15(0.5) O18(0.5) H17(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C18(H18), C15(H15), C13(H13), N17(H17), C8(H8), C20(H20), N16(H16),
 C4(H4), C10(H10), C23(H23), C6(H6), C7(H7), C21(H21)
7.b Fitted hexagon refined as free rotating group:
 N3(C19,N5,C12,N4,C3), C1(C18,C00N,C15,C13,N17), C9(C8,C20,N16,C4,C10),
 N22(C23,C6,C11,C7,C21)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56193
_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
;