Studies on the chemical reduction of polynuclear titanium(IV) nitrido complexes.
Caballo, Jorge; Calvo-Molina, Adrián; Claramonte, Sergio; Greño, Maider; Pérez-Redondo, Adrián; Yélamos, Carlos; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4844–4855; doi:10.1039/d3dt04241c

data_7715130
_publ_section_title
;
 Studies on the chemical reduction of polynuclear titanium(IV) nitrido
 complexes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4844
_journal_page_last               4855
_journal_paper_doi               10.1039/d3dt04241c
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C38 H58 N4 Si Ti4, C18 H36 K N2 O6, C6 H6'
_chemical_formula_sum            'C62 H100 K N6 O6 Si Ti4'
_chemical_formula_weight         1284.26
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   dual
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.5
_audit_creation_date             2023-11-13T16:35:00-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2023-11-20 deposited with the CCDC.	2024-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.739(3)
_cell_length_b                   33.351(3)
_cell_length_c                   16.799(3)
_cell_measurement_reflns_used    177
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     13300(3)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_UB_11      -0.011627
_diffrn_orient_matrix_UB_12      0.041307
_diffrn_orient_matrix_UB_13      -0.000517
_diffrn_orient_matrix_UB_21      0.046724
_diffrn_orient_matrix_UB_22      0.007028
_diffrn_orient_matrix_UB_23      0.017893
_diffrn_orient_matrix_UB_31      0.035006
_diffrn_orient_matrix_UB_32      0.00434
_diffrn_orient_matrix_UB_33      -0.024054
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            111322
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        23.299
_diffrn_reflns_theta_max         23.299
_diffrn_reflns_theta_min         3.033
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5464
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
The asymmetric unit of this structure was constituted by two molecules of
compound (two ionic pairs) and two molecules of benzene. One of the benzene
molecules and a half of the cation [K(krypt-222)]+ were held on a crystallographic 
special position, so it was not possible to get a chemical sensible model 
for them. So Squeeze procedure was used to remove their contribution to 
the structure factors.
;
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.3
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.42(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     1275
_refine_ls_number_reflns         19134
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.057
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+9.2104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1178
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                13416
_reflns_number_total             19134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04241c2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7715128--7715131.cif.'
_cod_database_code               7715130
_shelx_shelxl_version_number     2018/3
_platon_squeeze_void_probe_radius 1.20