Impact of diffusion methods and metal cations on photochromic three-component D-A hybrid heterostructures.
You, Ming-Hua; Li, Meng-Hua; Liu, Jing-Yan; Lin, Mei-Jin; Dalton transactions (Cambridge, England : 2003) 49 (2020) 12411–12417; doi:10.1039/d0dt02532a

data_7705089
_publ_section_title
;
 Impact of diffusion methods and metal cations on photochromic
 three-component D-A hybrid heterostructures.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12411
_journal_page_last               12417
_journal_paper_doi               10.1039/d0dt02532a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety
'2(Mo12 O40 Si), C48 H24 N8 O16 Zn4, C48 H24 N8 O12 Zn4'
_chemical_formula_sum            'C96 H48 Mo24 N16 O108 Si2 Zn8'
_chemical_formula_weight         6035.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-07-17 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.175(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.4203(5)
_cell_length_b                   27.6230(4)
_cell_length_c                   24.4269(6)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      55.8830
_cell_measurement_theta_min      3.3840
_cell_volume                     15364.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_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     -9.00  17.22   0.38    1.80    --   62.50 -67.00  11.00   69
  2  \w     37.00  81.08   0.38    1.80    --   62.50 -67.00  11.00  116
  3  \w    -11.00  25.10   0.38    0.36    --   -3.28 -99.00   0.00   95
  4  \w    -13.00  15.12   0.38    0.36    --   -3.28 -99.00-180.00   74
  5  \w    -90.00   2.34   0.38    1.80    --  -69.06  87.00-107.00  243
  6  \w   -127.00-103.06   0.38    1.80    --  -69.06 -99.00   0.00   63
  7  \w   -138.00 -88.98   0.38    1.80    --  -69.06 -99.00 -90.00  129
  8  \w   -121.00 -94.78   0.38    1.80    --  -69.06 -99.00-180.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0077032000
_diffrn_orient_matrix_UB_12      -0.0105589000
_diffrn_orient_matrix_UB_13      0.0502356000
_diffrn_orient_matrix_UB_21      -0.0027817500
_diffrn_orient_matrix_UB_22      0.0473246500
_diffrn_orient_matrix_UB_23      0.0106764500
_diffrn_orient_matrix_UB_31      -0.0582409000
_diffrn_orient_matrix_UB_32      -0.0009286000
_diffrn_orient_matrix_UB_33      -0.0285219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0168
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.871
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22631
_diffrn_reflns_point_group_measured_fraction_full 0.871
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         3.374
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    5.928
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             5752
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.783
_refine_diff_density_min         -2.035
_refine_diff_density_rms         0.273
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.602
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         11808
_refine_ls_number_restraints     322
_refine_ls_restrained_S_all      1.705
_refine_ls_R_factor_all          0.1597
_refine_ls_R_factor_gt           0.1352
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3902
_refine_ls_wR_factor_ref         0.4139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7594
_reflns_number_total             11808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02532a2.cif
_cod_data_source_block           znsif6-simo
_cod_depositor_comments
'Adding full bibliography for 7705089--7705090.cif.'
_cod_database_code               7705089
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.513
_shelx_estimated_absorpt_t_min   0.343
_reflns_odcompleteness_completeness 86.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     53.78
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C015-C00U
 1.35 with sigma of 0.01
 C014-C012
 1.4 with sigma of 0.01
 C00W-C019
 1.42 with sigma of 0.01
 C011-C14
 1.4 with sigma of 0.01
 Zn08-O6
 1.9 with sigma of 0.01
3. Rigid bond restraints
 C017, Zn08, O, O6, N2, C6, C10, H6, C7, C9, H10, H7, C8, H9, N00V, C019, C14,
 O00X, C00W, O010, C011, C00Y, C018, H018, H017, C015, Zn09, O1, N1, C2, C3, C1,
  H2, H3, C4, H1, C5, H4, N9, C00U, C012, O016, C014, O00Z, C013, C11, C12, H11,
  H12
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C013) \\sim Ueq, Uanis(Zn09) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C00U)
\\sim Ueq, Uanis(C012) \\sim Ueq, Uanis(O016) \\sim Ueq, Uanis(C015) \\sim Ueq,
Uanis(C014) \\sim Ueq, Uanis(O00Z) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(Zn08) \\sim Ueq, Uanis(O) \\sim Ueq,
Uanis(O6) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C10) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(N00V) \\sim Ueq,
Uanis(C019) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(O00X) \\sim Ueq, Uanis(C00W)
\\sim Ueq, Uanis(O010) \\sim Ueq, Uanis(C011) \\sim Ueq, Uanis(C00Y) \\sim Ueq,
Uanis(C018) \\sim Ueq, Uanis(C017) \\sim Ueq, : with sigma of 0.01 and sigma
for terminal atoms of 0.02
5.a Riding coordinates:
 C017(H017), C018(H018), C11(H11), C12(H12)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C7(H7), C9(H9), C4(H4), C3(H3), C2(H2), C1(H1)
5.c Fitted hexagon refined as free rotating group:
 C10(N2,C6,C7,C8,C9), C5(C4,C3,N1,C2,C1)
;
_shelx_res_checksum              82384
_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 2.562
_oxdiff_exptl_absorpt_empirical_full_min 0.720