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_7714898
_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         'C100 H78 Ag8 Cl2 N12 O56 Ti12'
_chemical_formula_sum            'C100 H78 Ag8 Cl2 N12 O56 Ti12'
_chemical_formula_weight         3852.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 111.7980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.3284(2)
_cell_length_b                   30.6769(3)
_cell_length_c                   15.5639(2)
_cell_measurement_reflns_used    27928
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      60.1260
_cell_measurement_theta_min      2.8100
_cell_volume                     7238.60(16)
_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      100.0(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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     84.00 133.00   0.50    0.42    --   76.57-160.00-151.00   98
  2  \w     30.00  70.00   0.50    0.42    --   76.57 -38.00 -60.00   80
  3  \w     94.00 119.00   0.50    0.42    --   76.57 118.00  86.00   50
  4  \w     79.00 104.00   0.50    0.42    --   76.57 160.00-121.00   50
  5  \w     -6.00  25.00   0.50    0.10    --   -0.78 -99.00-120.00   62
  6  \w      2.00  28.00   0.50    0.10    --   -0.78 -99.00 -90.00   52
  7  \w     -3.00  23.00   0.50    0.10    --   -0.78 -99.00 -60.00   52
  8  \w     -8.00  17.00   0.50    0.10    --   -0.78 -99.00  90.00   50
  9  \w    -73.00  15.00   0.50    0.10    --   -0.78 -57.00  60.00  176
 10  \w   -120.00 -94.00   0.50    0.42    --  -78.14 -99.00  60.00   52
 11  \w   -150.00 -90.00   0.50    0.42    --  -78.14 -99.00  30.00  120
 12  \w   -119.00 -94.00   0.50    0.42    --  -78.14-118.00   0.00   50
 13  \w   -152.00 -55.00   0.50    0.42    --  -78.14-160.00-151.00  194
 14  \w   -131.00 -80.00   0.50    0.42    --  -78.14-125.00-120.00  102
 15  \w    -59.00  -1.00   0.50    0.42    --  -78.14  38.00  90.00  116
 16  \w    -70.00  -2.00   0.50    0.42    --  -78.14  38.00 150.00  136
 17  \w    -96.00 -29.00   0.50    0.42    --  -78.14  57.00  90.00  134
 18  \w    -69.00 -13.00   0.50    0.42    --  -78.14  38.00-150.00  112
 19  \w   -123.00 -98.00   0.50    0.42    --  -78.14 160.00-121.00   50
 20  \w   -108.00 -75.00   0.50    0.42    --  -78.14 125.00-180.00   66
 21  \w    -51.00 -25.00   0.50    0.42    --  -78.14 125.00-180.00   52
 22  \w    -80.00 -55.00   0.50    0.42    --  -78.14 118.00  86.00   50
;
_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      0.0315046000
_diffrn_orient_matrix_UB_12      -0.0314481000
_diffrn_orient_matrix_UB_13      -0.0388592000
_diffrn_orient_matrix_UB_21      -0.0471752000
_diffrn_orient_matrix_UB_22      -0.0296791000
_diffrn_orient_matrix_UB_23      0.0249801000
_diffrn_orient_matrix_UB_31      -0.0677446000
_diffrn_orient_matrix_UB_32      0.0059920000
_diffrn_orient_matrix_UB_33      -0.0802885000
_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  0.0381
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54153
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        52.931
_diffrn_reflns_theta_max         52.931
_diffrn_reflns_theta_min         2.827
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    10.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic orangish orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       block
_exptl_crystal_F_000             3768
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.155
_refine_diff_density_min         -2.861
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         12768
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0870
_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^)+(0.1485P)^2^+67.4846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2460
_refine_ls_wR_factor_ref         0.2533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10993
_reflns_number_total             12768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03941b2.cif
_cod_data_source_block           PTC-350
_cod_depositor_comments
'Adding full bibliography for 7714898--7714899.cif.'
_cod_original_cell_volume        7238.60(15)
_cod_database_code               7714898
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ag Ti C N O'
_shelx_estimated_absorpt_t_max   0.432
_shelx_estimated_absorpt_t_min   0.432
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq, Uanis(C02K) \\sim Ueq, Uanis(C02P) \\sim Ueq, Uanis(C02O)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C02I) \\sim Ueq, Uanis(C02H) \\sim Ueq, Uanis(C02E) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O027) \\sim Ueq, Uanis(C02T) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C02P)
\\sim Ueq, Uanis(C02M) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(O027) \\sim Ueq, Uanis(O01S) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O017) \\sim Ueq, Uanis(O027) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
2. Others
 Fixed Sof: Ag2A(0.9) Ag1A(0.7) Ag4A(0.6) Ag4B(0.4) Ag1B(0.3) Ag2B(0.1)
 H1BC(0.7) H1BD(0.7) H1AA(0.3) H1AB(0.3)
3.a Aromatic/amide H refined with riding coordinates:
 C01G(H01G), C01I(H01I), C01K(H01K), C01L(H01L), C01N(H01N), C01O(H01O),
 C01Q(H01Q), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y),
 C01Z(H01Z), C020(H020), C022(H022), C025(H025), C028(H028), C02A(H02G),
 C02D(H02H), C02H(H02I), C02K(H02K), C02L(H02L), C02N(H02O), C02O(H02P),
 C02P(H02Q), C02I(H02R), C02T(H02T), C23(H23)
3.b Fitted hexagon refined as free rotating group:
 C02P(C02I,N01A,C02F,C02T,C23)
3.c X=CH2 refined with riding coordinates:
 O1(H1BC,H1BD), O1(H1AA,H1AB)
3.d Idealised Me refined as rotating group:
 C021(H02A,H02B,H02C), C023(H02D,H02E,H02F), C02M(H02J,H02M,H02N)
;
_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 1.910
_oxdiff_exptl_absorpt_empirical_full_min 0.632