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_7714978
_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         'Mo12 O40 P1, 1(Cl), C18 H15 N6, 3(C5 H9 N O)'
_chemical_formula_sum            'C33 H42 Cl Mo12 N9 O43 P'
_chemical_formula_weight         2470.45
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-11
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   14.4362(3)
_cell_length_b                   14.4362(3)
_cell_length_c                   18.6730(4)
_cell_measurement_reflns_used    11707
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.2150
_cell_measurement_theta_min      2.1570
_cell_volume                     3370.16(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.904
_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    -10.00  15.00   0.50    8.00    --   -9.80  51.00 102.00   50
  2  \w    -27.00  -1.00   0.50    8.00    --   -9.80  50.00  21.00   52
  3  \w    -98.00  74.00   0.50    8.00    --   -9.80  55.00 150.00  344
;
_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  0.0201
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18893
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.741
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.290
_diffrn_reflns_theta_min         2.723
_exptl_absorpt_coefficient_mu    2.318
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57702
_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 green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.434
_exptl_crystal_description       block
_exptl_crystal_F_000             2366
_refine_diff_density_max         2.725
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Flack x determined using 1629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.039(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         4570
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+5.2181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0905
_reflns_Friedel_coverage         0.593
_reflns_Friedel_fraction_full    0.771
_reflns_Friedel_fraction_max     0.568
_reflns_number_gt                4446
_reflns_number_total             4570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04157c2.cif
_cod_data_source_block           hybrid4
_cod_depositor_comments
'Adding full bibliography for 7714976--7714979.cif.'
_cod_original_cell_volume        3370.16(16)
_cod_database_code               7714978
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Rigid bond restraints
 O00T, O00D, N00R, C00P, O008, C2, P05, O007, C00S, N00Q, Mo01, Mo03, C00U,
 N00C, Mo04, O00K, C00J, O00L, O2, C00N, O00H, O00I, C00X, C00W, C4, Mo02, C6,
 O00E, Cl06, C00O, O00A, O00F, O009, O00B, O00G
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(O00T) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C6) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N00R)
\\sim Ueq, Uanis(O00T) \\sim Ueq, Uanis(C00X) \\sim Ueq, Uanis(C00W) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C00W(H00A,H00B), C4(H4A,H4B), C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00S(H00S), N00Q(H00Q), C00U(H00U), C00O(H00O)
3.c Fitted hexagon refined as free rotating group:
 C00P(C00S,N00Q,C00U,C00O,C00J)
3.d Idealised Me refined as rotating group:
 C00X(H00C,H00D,H00E)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25083
_shelx_fab_checksum              50468
_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
;