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_1570644
_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         'C140 H120 O56 Ti16, 2(C7 H8)'
_chemical_formula_sum            'C154 H136 O56 Ti16'
_chemical_formula_weight         3649.02
_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   geom
_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                113.206(7)
_cell_angle_beta                 113.379(6)
_cell_angle_gamma                98.474(7)
_cell_formula_units_Z            1
_cell_length_a                   16.790(3)
_cell_length_b                   16.977(3)
_cell_length_c                   17.003(3)
_cell_measurement_reflns_used    7442
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      66.698
_cell_measurement_theta_min      3.075
_cell_volume                     3814.6(13)
_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      173.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0873
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            50385
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.594
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_min         3.073
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    7.481
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0735 after correction.
The Ratio of minimum to maximum transmission is 0.6471.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dull dark red'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       block
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         13381
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0894
_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^)+(0.1503P)^2^+13.9018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2563
_refine_ls_wR_factor_ref         0.2961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8316
_reflns_number_total             13381
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05617a2.cif
_cod_data_source_block           cu_230411a_0m
_cod_depositor_comments
'Adding full bibliography for 1570642--1570645.cif.'
_cod_original_cell_volume        3814.6(12)
_cod_database_code               1570644
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.522
_shelx_estimated_absorpt_t_min   0.400
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C77-C75
 1.55 with sigma of 0.01
 C69-C70 = C63-C62 = C24-C28 = C20-C21 = C3-C7 = C14-C13
 1.55 with sigma of 0.01
 C47-C49
 1.55 with sigma of 0.01
 C39-C42 = C34-C35
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O11 \\sim C69 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C70 \\sim
O12: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 within
2A
C72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C71 \\sim C77: within 2A with
sigma of 0.002 and sigma for terminal atoms of 0.004 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C46(H46), C45(H45), C44(H44), C4(H4), C5(H5), C6(H6), C59(H59), C60(H60),
 C61(H61), C27(H27), C26(H26), C25(H25), C33(H33), C32(H32), C31(H31), C54(H54),
  C53(H53), C52(H52), C38(H38), C37(H37), C36(H36), C10(H10), C11(H11),
 C12(H12), C17(H17), C18(H18), C19(H19), C66(H66), C67(H67), C68(H68), C76(H76),
  C71(H71), C72(H72), C73(H73), C74(H74)
4.b Fitted hexagon refined as free rotating group:
 C43(C48,C47,C46,C45,C44), C1(C2,C3,C4,C5,C6), C58(C57,C59,C60,C61,C62),
 C23(C22,C27,C26,C25,C24), C30(C29,C34,C33,C32,C31), C51(C50,C55,C54,C53,C52),
 C41(C40,C39,C38,C37,C36), C9(C10,C11,C12,C13,C8), C15(C17,C18,C19,C20,C16),
 C69(C64,C65,C66,C67,C68), C76(C71,C72,C73,C74,C75)
4.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C7(H7A,H7B,H7C), C42(H42A,H42B,H42C), C56(H56A,H56B,
 H56C), C28(H28A,H28B,H28C), C63(H63A,H63B,H63C), C49(H49A,H49B,H49C), C21(H21A,
 H21B,H21C), C14(H14A,H14B,H14C), C77(H77A,H77B,H77C), C70(H70A,H70B,H70C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              41492
_shelx_hkl_checksum              14896
_shelx_fab_checksum              28707
_olex2_submission_special_instructions 'No special instructions were received'