Isolation of the parent triplet titanocene <i>via</i> NHC stabilisation.
Meyer, Felix; Demeshko, Serhiy; Golz, Christopher; Townrow, Oliver P. E.; Fischer, Malte; Dalton transactions (Cambridge, England : 2003) 54 (2025) 8035–8040; doi:10.1039/d5dt00480b

data_7718175
_publ_section_title
;
 Isolation of the parent triplet titanocene <i>via</i> NHC stabilisation.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8035
_journal_page_last               8040
_journal_paper_doi               10.1039/d5dt00480b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C25 H40 N2 Si2 Zr'
_chemical_formula_sum            'C25 H40 N2 Si2 Zr'
_chemical_formula_weight         515.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-06-05
_audit_creation_method
;FinalCif V138 by Daniel Kratzert, Freiburg 2024, 
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2025-01-23 deposited with the CCDC.	2025-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.531(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.362(10)
_cell_length_b                   8.400(3)
_cell_length_c                   20.499(7)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.730
_cell_measurement_theta_min      2.512
_cell_volume                     5342(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
'Bruker BIS V6.2.15/2021-03-16 and APEX4 2022.1-1'
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE dual wavelength Mo/Cu'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75161
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.773
_diffrn_reflns_theta_min         2.073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6995
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1363 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.6995.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.409
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0566P)^2^+17.2629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5505
_reflns_number_total             6935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00480b3.cif
_cod_data_source_block           mo_2340_cg_0m
_cod_depositor_comments
'Adding full bibliography for 7718175--7718178.cif.'
_cod_database_code               7718175
_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.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C10(H10), C17(H17), C11(H11), C18(H18), C16(H16), C14(H14),
 C12(H12), C19(H19), C13(H13)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C22(H22A,H22B,H22C),
 C21(H21A,H21B,H21C), C25(H25A,H25B,H25C), C3(H3A,H3B,H3C), C23(H23A,H23B,H23C),
  C20(H20A,H20B,H20C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.825
_shelx_estimated_absorpt_t_max   0.980
_diffrn_measurement_ambient_temperature_device_make 'Oxford Cryostream 800'
_shelx_res_checksum              42831
_shelx_hkl_checksum              59822