All-catecholate-stabilized black titanium-oxo clusters for efficient photothermal conversion.
Hou, Jinle; Huang, Nahui; Acharya, Dinesh; Liu, Yuxin; Zhu, Jiaying; Teng, Jiaxin; Wang, Zhi; Qu, Konggang; Zhang, Xianxi; Sun, Di; Chemical science 15 (2024) 2655–2664; doi:10.1039/d3sc05617a

data_1570643
_publ_section_title
;
 All-catecholate-stabilized black titanium-oxo clusters for efficient
 photothermal conversion.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              2655
_journal_page_last               2664
_journal_paper_doi               10.1039/d3sc05617a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C120 H80 O56 Ti16, 2(H2 O), 2(C7 H8)'
_chemical_formula_sum            'C134 H100 O58 Ti16'
_chemical_formula_weight         3404.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-05-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-13 deposited with the CCDC.	2024-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                63.041(9)
_cell_angle_beta                 64.513(13)
_cell_angle_gamma                71.596(9)
_cell_formula_units_Z            1
_cell_length_a                   15.114(4)
_cell_length_b                   16.444(5)
_cell_length_c                   17.284(5)
_cell_measurement_reflns_used    1626
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      71.332
_cell_measurement_theta_min      3.422
_cell_volume                     3417.2(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.00
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8VENTURE'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0836
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11962
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.072
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         3.050
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    8.315
_exptl_absorpt_correction_T_max  0.753555
_exptl_absorpt_correction_T_min  0.542087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 50066 reflections, Rint = 0.0849
 (11652 with I > 3sig(I), Rint = 0.0554)
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.1166
_exptl_crystal_size_mid          0.0588
_exptl_crystal_size_min          0.003
_refine_diff_density_max         1.523
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         11962
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0737
_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^)+(0.1186P)^2^+5.7597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.2212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8098
_reflns_number_total             11962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05617a2.cif
_cod_data_source_block           cu_220703a_0m_5
_cod_depositor_comments
'Adding full bibliography for 1570642--1570645.cif.'
_cod_original_cell_volume        3417.3(18)
_cod_database_code               1570643
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.444
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5693(14)
 0.4307(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
O6 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 2A with
sigma of 0.004 and sigma for terminal atoms of 0.01 within 2A
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67: within 2A with
sigma of 0.004 and sigma for terminal atoms of 0.01 within 2A
O20 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.01 within 2A
4.a Free rotating group:
 O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C24(H24), C23(H23), C22(H22), C21(H21),
  C27(H27), C28(H28), C29(H29), C30(H30), C36(H36), C35(H35), C34(H34),
 C33(H33), C39(H39), C40(H40), C41(H41), C42(H42), C48(H48), C47(H47), C46(H46),
  C45(H45), C51(H51), C52(H52), C53(H53), C54(H54), C57(H57), C58(H58),
 C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65)
4.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C8(C9,C10,C11,C12,C7), C13(C14,C15,C16,C17,C18), C19(C24,
 C23,C22,C21,C20), C25(C26,C27,C28,C29,C30), C32(C31,C36,C35,C34,C33), C38(C39,
 C40,C41,C42,C37), C43(C48,C47,C46,C45,C44), C49(C50,C51,C52,C53,C54), C55(C56,
 C57,C58,C59,C60), C66(C61,C62,C63,C64,C65)
4.d Idealised Me refined as rotating group:
 C67(H67A,H67B,H67C)
;
_shelx_res_checksum              52306
_shelx_hkl_checksum              73483
_olex2_submission_special_instructions 'No special instructions were received'