Homoleptic seven-coordinate Ti(0) and Zr(0) through a new stabilization mode
Antsiburov, Ivan; Bühler, Raphael; Stephan, Johannes; Erdyakov, Maxim; Gemel, Christian; Kahlal, Samia; Cador, Olivier; Guizouarn, Thierry; Saillard, Jean-Yves; Meyer, Karsten; Fischer, Roland A.; Chemical Science  (2026) –; doi:10.1039/D6SC00226A

data_1576879
_publ_section_title
;
 Homoleptic seven-coordinate Ti(0) and Zr(0) through a new stabilization
 mode.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              8989
_journal_page_last               8997
_journal_paper_doi               10.1039/d6sc00226a
_journal_volume                  17
_journal_year                    2026
_chemical_formula_sum            'C124 H109 B2 F50 Ga5 N2 Ni'
_chemical_formula_weight         3006.06
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2mk8r7
_audit_creation_method
;FinalCif V149 by Daniel Kratzert, Freiburg 2025, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-05-20 deposited with the CCDC.	2026-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                86.988(9)
_cell_angle_beta                 77.697(8)
_cell_angle_gamma                86.723(8)
_cell_formula_units_Z            2
_cell_length_a                   14.954(4)
_cell_length_b                   15.115(4)
_cell_length_c                   31.972(8)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.2755
_cell_measurement_theta_min      2.424
_cell_volume                     7043(3)
_computing_cell_refinement       'SAINT V8.40B'
_computing_data_collection
'Bruker BIS V6.2.16/2021-10-23 and APEX4 2021.10-0'
_computing_data_reduction        'SAINT V8.40B'
_computing_molecular_graphics    'Mercury (Macrae, 2008), PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement
'SHELXL (Sheldrick, 2015), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 16
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-angle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'TXS rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            405245
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.987
_diffrn_source                   'TXS rotating anode'
_diffrn_source_current           50.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker, 2016)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       fragment
_exptl_crystal_F_000             3020
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.098
_platon_squeeze_details
;
The unit cell contains 2 disordered molecules of 1,2-difluorobenzene and 
n-hexane which were treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2461
_refine_ls_number_reflns         24832
_refine_ls_number_restraints     4728
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+6.3568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19184
_reflns_number_total             24832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6sc00226a2.cif
_cod_data_source_block           stejo25_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 1576879--1576881.cif.'
_cod_database_code               1576879
_shelx_shelxl_version_number     2019/1
_diffrn_measurement_ambient_temperature_make 'Oxford Cryostream'
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              2411
_shelx_fab_checksum              42211