Combining Ti<sub>4</sub>(embonate)<sub>6</sub> anionic cages and π-conjugated coordination cations for highly effective optical limiting.
Yuan, Yuan; Zhang, Dong-Hui; Li, Qiao-Hong; Chen, Shu-Mei; He, Yan-Ping; Zhang, Jian; Chemical communications (Cambridge, England) 60 (2024) 8748–8751; doi:10.1039/d4cc02938k

data_7133387
_publ_section_title
;
 Combining Ti<sub>4</sub>(embonate)<sub>6</sub> anionic cages and
 &#x3c0;-conjugated coordination cations for highly effective optical
 limiting.
;
_journal_issue                   66
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8748
_journal_page_last               8751
_journal_paper_doi               10.1039/d4cc02938k
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C294 H224 Ag8 N8 O36 P8 Ti4'
_chemical_formula_sum            'C294 H224 Ag8 N8 O36 P8 Ti4'
_chemical_formula_weight         5747.12
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-19
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.160(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.6145(4)
_cell_length_b                   22.6414(2)
_cell_length_c                   47.7519(7)
_cell_measurement_reflns_used    91548
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      55.6710
_cell_measurement_theta_min      1.8120
_cell_volume                     36146.3(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_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      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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     45.00 140.76   0.38    0.23    --   67.52  49.00  -2.00  252
  2  \w     79.00 137.90   0.38    0.23    --   67.52 125.00-150.00  155
  3  \w     39.00  98.28   0.38    0.23    --   67.52  77.00 -90.00  156
  4  \w   -144.00 -42.16   0.38    0.23    --  -69.71 -77.00 150.00  268
  5  \w   -144.00 -42.16   0.38    0.23    --  -69.71 -77.00  90.00  268
  6  \w   -144.00 -42.16   0.38    0.23    --  -69.71 -77.00  90.00  268
  7  \w    -76.00  19.76   0.38    0.06    --   -1.09 -49.00-150.00  252
  8  \w   -144.00 -48.24   0.38    0.23    --  -69.71 -49.00-150.00  252
  9  \w   -143.00 -89.04   0.38    0.23    --  -69.71 -99.00-180.00  142
 10  \w   -141.00 -80.20   0.38    0.23    --  -69.71-125.00 -30.00  160
 11  \w   -141.00 -80.20   0.38    0.23    --  -69.71-125.00   0.00  160
 12  \w    -71.00   6.90   0.38    0.23    --  -69.71  38.00 -90.00  205
 13  \w    -82.00   3.88   0.38    0.23    --  -69.71  49.00  -2.00  226
 14  \w   -111.00 -21.32   0.38    0.23    --  -69.71 125.00 -30.00  236
 15  \w   -111.00 -21.32   0.38    0.23    --  -69.71 125.00  90.00  236
 16  \w    -23.00  72.76   0.38    0.06    --   -1.09  49.00  -2.00  252
 17  \w     -8.00  35.70   0.38    0.06    --   -1.09 -99.00-180.00  115
 18  \w     -8.00  35.70   0.38    0.06    --   -1.09 -99.00-150.00  115
 19  \w     -8.00  35.70   0.38    0.06    --   -1.09 -99.00-120.00  115
 20  \w     -8.00  35.70   0.38    0.06    --   -1.09 -99.00 -90.00  115
 21  \w     -8.00  35.70   0.38    0.06    --   -1.09 -99.00   0.00  115
 22  \w     20.00 109.68   0.38    0.23    --   67.52-125.00 -30.00  236
 23  \w     20.00 109.68   0.38    0.23    --   67.52-125.00 -30.00  236
 24  \w     20.00 109.68   0.38    0.23    --   67.52-125.00  90.00  236
 25  \w     -7.00  95.98   0.38    0.23    --   67.52 -77.00-150.00  271
 26  \w     -6.00 104.96   0.38    0.23    --   67.52 -99.00-180.00  292
 27  \w     -7.00  80.78   0.38    0.23    --   67.52 -49.00-150.00  231
;
_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      0.0082273000
_diffrn_orient_matrix_UB_12      0.0154122000
_diffrn_orient_matrix_UB_13      -0.0243425000
_diffrn_orient_matrix_UB_21      -0.0268057000
_diffrn_orient_matrix_UB_22      0.0438925000
_diffrn_orient_matrix_UB_23      -0.0052238000
_diffrn_orient_matrix_UB_31      0.0286101000
_diffrn_orient_matrix_UB_32      0.0365137000
_diffrn_orient_matrix_UB_33      0.0165164000
_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  0.1501
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            281738
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.362
_diffrn_reflns_theta_min         1.714
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    3.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_description       block
_exptl_crystal_F_000             11664
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.438
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1601
_refine_ls_number_reflns         35521
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.1090
_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^)+(0.1672P)^2^+372.0801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2924
_refine_ls_wR_factor_ref         0.3120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26485
_reflns_number_total             35521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02938k2.cif
_cod_data_source_block           PTC-381
_cod_depositor_comments
'Adding full bibliography for 7133385--7133387.cif.'
_cod_original_cell_volume        36146.2(9)
_cod_database_code               7133387
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ti Ag C H O N P'
_shelx_estimated_absorpt_t_max   0.734
_shelx_estimated_absorpt_t_min   0.438
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     53.78
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
2. Restrained distances
 Ag1-O1
 2.45 with sigma of 0.02
3. Others
 Fixed Sof: H89a(0.5) H89b(0.5) H43a(0.5) H43b(0.5)
4.a Ternary CH refined with riding coordinates:
 C87(H87), C99(H99), C80(H80), C23(H23)
4.b Secondary CH2 refined with riding coordinates:
 N2(H2a,H2b), N4(H4a,H4b), N3(H3a,H3b), C19(H19a,H19b), C37(H37a,H37b),
 C89(H89a,H89b), C122(H12a,H12b), C43(H43a,H43b), C101(H10a,H10b)
4.c Aromatic/amide H refined with riding coordinates:
 C67(H67), C29(H29), C68(H68), C116(H116), C20(H20), C118(H118), C60(H60),
 C75(H75), C15(H15), C11(H11), C13(H13), C81(H81), C84(H84), C5(H5), C93(H93),
 C96(H96), C55(H55), C102(H102), C105(H105), C108(H108), C2(H2), C111(H111),
 C131(H131), C8(H8), C98(H98), C16(H16), C132(H132), C57(H57), C30(H30),
 C133(H133), C21(H21), C47(H47), C42(H42), C134(H134), C31(H31), C54(H54),
 C135(H135), C61(H61), C18(H18), C136(H136), C44(H44), C59(H59), C25(H25),
 C137(H137), C76(H76), C24(H24), C82(H82), C138(H138), C17(H17), C94(H94),
 C139(H139), C100(H100), C104(H104), C106(H106), C140(H140), C4(H4), C40(H40),
 C14(H14), C141(H141), C34(H34), C26(H26), C46(H46), C142(H142), C58(H58),
 C33(H33), C32(H32), C143(H143), C51(H51), C107(H107), C144(H144), C97(H97),
 C62(H62), C109(H109), C145(H145), C27(H27), C83(H83), C119(H119), C146(H146),
 C56(H56), C9(H9), C91(H91), C147(H147), C12(H12), C110(H110), C65(H65),
 C148(H148), C103(H103), C64(H64), C79(H79), C149(H149)
4.d Fitted hexagon refined as free rotating group:
 C33(C32,C143,C51,C107,C85)
4.e X=CH2 refined with riding coordinates:
 N5(H5a,H5b)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4077
_shelx_hkl_checksum              81379
_shelx_fab_checksum              41356
_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 8.898
_oxdiff_exptl_absorpt_empirical_full_min 0.333
_publcif_funding_html
;
;