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_7705090
_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         'Mo12 O40 Si, C48 H24 Cd2 N8 O12'
_chemical_formula_sum            'C48 H24 Cd2 Mo12 N8 O52 Si'
_chemical_formula_weight         2948.92
_space_group_crystal_system      tetragonal
_space_group_IT_number           141
_space_group_name_Hall           '-I 4bd 2'
_space_group_name_H-M_alt        'I 41/a m d :2'
_atom_sites_solution_hydrogens   geom
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8634(12)
_cell_length_b                   19.8634(12)
_cell_length_c                   39.282(9)
_cell_measurement_reflns_used    2572
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.8640
_cell_measurement_theta_min      3.6800
_cell_volume                     15499(4)
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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    -69.00  31.00   0.50   30.00    --   -9.60  51.00-162.00  200
;
_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      0.0318318000
_diffrn_orient_matrix_UB_12      0.0090321000
_diffrn_orient_matrix_UB_13      -0.0066853000
_diffrn_orient_matrix_UB_21      -0.0022390000
_diffrn_orient_matrix_UB_22      -0.0266431000
_diffrn_orient_matrix_UB_23      -0.0120805000
_diffrn_orient_matrix_UB_31      -0.0158335000
_diffrn_orient_matrix_UB_32      0.0219261000
_diffrn_orient_matrix_UB_33      -0.0117374000
_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  0.1395
_diffrn_reflns_av_unetI/netI     0.1386
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3568
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.462
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45114
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             5592
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.843
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         3568
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0985
_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^)+(0.1814P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2675
_refine_ls_wR_factor_ref         0.2965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2157
_reflns_number_total             3568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02532a2.cif
_cod_data_source_block           dpndi-cd-simo
_cod_depositor_comments
'Adding full bibliography for 7705089--7705090.cif.'
_cod_original_sg_symbol_H-M      'I 41/a m d'
_cod_database_code               7705090
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.863
_shelx_estimated_absorpt_t_min   0.768
_reflns_odcompleteness_completeness 96.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C4-C2
 1.3 with sigma of 0.2
 C2-C4
 1.35 with sigma of 0.01
 Cd-N1 \\sim N1-Cd03
 with sigma of 0.02
 Cd-O1 \\sim O1-Cd03
 with sigma of 0.02
3. Restrained planarity
 C5, C6, C7, N1
 with sigma of 0.1
4. Rigid bond restraints
 O2, O1, N1, C7, C6, H7, C5, H6, N2, C4, C2, C1, C3, H3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 Cd03
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
Cd03: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within
2A
Uanis(C5) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(O2)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, :
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cd03) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(Cd03) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(Cd) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 N1, Cd03
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, Cd
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(Cd)=0.25*(1-FVAR(2))
 Sof(Cd03)=0.25*FVAR(2)
8.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C7(H7)
;
_shelx_res_checksum              93050
_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 1.798
_oxdiff_exptl_absorpt_empirical_full_min 0.604