Synthesis and X-ray structure analysis of cytotoxic 2-picolylamino-type Hf<sup>IV</sup>-bis-chelated complexes.
Zhao, Tiankun; Zhang, Qi; Zhao, Jialiu; Mei, Dongyu; Ma, Jing; Correia, Isabel; Yang, Zhongduo; Kim, Sa-Hyun; Huhn, Thomas; Dalton transactions (Cambridge, England : 2003) 54 (2025) 6674–6683; doi:10.1039/d4dt02859g

data_1574184
_publ_section_title
;
 Synthesis and X-ray structure analysis of cytotoxic 2-picolylamino-type
 Hf<sup>IV</sup>-bis-chelated complexes.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6674
_journal_page_last               6683
_journal_paper_doi               10.1039/d4dt02859g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C43 H53 Hf N3 O6, 1[H2O], 1[C6H14]'
_chemical_formula_sum            'C49 H69 Hf N3 O7'
_chemical_formula_weight         990.56
_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
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2l7v3t
_audit_creation_date             2024-10-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-12 deposited with the CCDC.	2025-03-18 downloaded from the CCDC.
;
_cell_angle_alpha                114.844(3)
_cell_angle_beta                 102.121(3)
_cell_angle_gamma                98.221(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4131(10)
_cell_length_b                   14.6873(14)
_cell_length_c                   16.6466(16)
_cell_measurement_reflns_used    9271
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.29
_cell_measurement_theta_min      2.99
_cell_volume                     2180.8(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean ' 7.39 for PHOTON III'
_diffrn_detector_type            'Bruker Photon III 28'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker D8 Venture'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            75813
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         72.469
_diffrn_reflns_theta_min         2.668
_diffrn_source_current           3.57
_diffrn_source_power             0.24972149999999999
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.305
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3450
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS, Madison WI for PHOTON III'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.536
_refine_diff_density_min         -2.363
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0034(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         13059
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0540P)^2^+3.5393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12574
_reflns_number_total             13059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02859g2.cif
_cod_data_source_block           220629c_0m
_cod_depositor_comments
'Adding full bibliography for 1574184--1574185.cif.'
_cod_database_code               1574184
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C01C, C01I
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C01C) \\sim Ueq, Uanis(C01I) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00E(H00C,H00D), C00S(H00E,H00F)
4.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00M(H00M), C00O(H00O), C00P(H00P), C00U(H00U), C00V(H00V),
 C00W(H00W), C00X(H00X), C010(H010), C011(H011), C015(H015)
4.c Idealised Me refined as rotating group:
 C013(H01A,H01B,H01C), C014(H01D,H01E,H01F), C016(H01G,H01H,H01I), C017(H01J,
 H01K,H01L), C019(H01M,H01N,H01O), C01A(H01P,H01Q,H01R), C01D(H01S,H01T,H01U),
 C01E(H01V,H01W,H01X), C01F(H01Y,H,HA), C01G(H01Z,HB,HC), C01H(H01,HD,HE),
 C01I(H1,HG,HH)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              37702
_shelx_hkl_checksum              81275
_shelx_fab_checksum              30213
_olex2_submission_special_instructions 'No special instructions were received'