Structure and optical limiting effects of heterometallic Ag<sub>6</sub>@Ti<sub>12</sub> and Ag<sub>8</sub>@Ti<sub>12</sub> oxo clusters regulated by alkynyl ligands.
Rong, Li-Jun; Ye, Yu-Ting; Lin, Xin; Sun, Xiaohui; Chen, Shumei; Zhang, Jian; Zhang, Lei; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1947–1950; doi:10.1039/d3dt03941b

data_7714899
_publ_section_title
;
 Structure and optical limiting effects of heterometallic
 Ag<sub>6</sub>@Ti<sub>12</sub> and Ag<sub>8</sub>@Ti<sub>12</sub> oxo
 clusters regulated by alkynyl ligands.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1947
_journal_page_last               1950
_journal_paper_doi               10.1039/d3dt03941b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C114 H78 Ag6 N12 O54 Ti12'
_chemical_formula_sum            'C126 H72 Ag6 N12 O56 Ti12'
_chemical_formula_weight         3871.97
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-12-21 deposited with the CCDC.	2024-01-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   27.7454(3)
_cell_length_b                   27.7454(3)
_cell_length_c                   42.2217(7)
_cell_measurement_reflns_used    27463
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.4220
_cell_measurement_theta_min      2.0530
_cell_volume                     28148.1(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -39.00  19.14   0.38    6.88    --   -5.26 -78.00 161.00  153
  2  \w    -18.00  28.36   0.38    6.88    --   -5.26 -99.00 120.00  122
  3  \w    -18.00  28.36   0.38    6.88    --   -5.26 -99.00   0.00  122
  4  \w    -18.00  40.14   0.38    6.88    --    6.82 -99.00   0.00  153
  5  \w    -78.00 -52.92   0.38    6.88    --   -5.26 -57.00 -90.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0193639000
_diffrn_orient_matrix_UB_12      0.0211046000
_diffrn_orient_matrix_UB_13      -0.0101994000
_diffrn_orient_matrix_UB_21      0.0002678000
_diffrn_orient_matrix_UB_22      -0.0205845000
_diffrn_orient_matrix_UB_23      -0.0098597000
_diffrn_orient_matrix_UB_31      -0.0222656000
_diffrn_orient_matrix_UB_32      -0.0014283000
_diffrn_orient_matrix_UB_33      -0.0090013000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            60675
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.021
_diffrn_reflns_theta_max         25.021
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.160
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       sphere
_exptl_crystal_F_000             11436
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         3.059
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1131P)^2^+106.8824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4377
_reflns_number_total             5509
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03941b2.cif
_cod_data_source_block           PTC-349
_cod_depositor_comments
'Adding full bibliography for 7714898--7714899.cif.'
_cod_original_cell_volume        28148.0(8)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7714899
_publcif_datablock.id            {49b39300-c6c9-419f-b8f2-78e8a45f2785}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ti Ag C N O H'
_olex2_refinement_description
;
1. Others
 Fixed Sof: Ag1A(0.7) Ag1B(0.3)
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C18(H18), C20(H20), C21(H21), C11(H11), C3(H3), C7(H7),
 C15(H15), C17(H17), C2(H2), C19(H19), C5(H5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.704
_oxdiff_exptl_absorpt_empirical_full_min 0.588
_publcif_funding_html
;
;