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_7715128
_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 ad
_chemical_formula_moiety         'C24 H48 Na O6, C40 H60 N4 Ti4'
_chemical_formula_sum            'C64 H108 N4 Na O6 Ti4'
_chemical_formula_weight         1244.13
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_IT_number           199
_space_group_name_Hall           'I 2b 2c 3'
_space_group_name_H-M_alt        'I 21 3'
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      199
_symmetry_space_group_name_Hall  'I 2b 2c 3'
_symmetry_space_group_name_H-M   'I 21 3'
_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             2023-11-13T09:28:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2024-01-22 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                   23.803(5)
_cell_length_b                   23.803(5)
_cell_length_c                   23.803(5)
_cell_measurement_reflns_used    657
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     13486(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.999
_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      -0.024729
_diffrn_orient_matrix_UB_12      0.016888
_diffrn_orient_matrix_UB_13      -0.029465
_diffrn_orient_matrix_UB_21      -0.022195
_diffrn_orient_matrix_UB_22      0.019551
_diffrn_orient_matrix_UB_23      0.029834
_diffrn_orient_matrix_UB_31      0.025705
_diffrn_orient_matrix_UB_32      0.033128
_diffrn_orient_matrix_UB_33      -0.002586
_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  0.1007
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            208791
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.584
_diffrn_reflns_theta_min         2.706
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.512
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.866
_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    1.225
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5336
_exptl_crystal_recrystallization_method
'Slow diffusion of toluene into a solution of the compound in tetrahydrofuran'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     252
_refine_ls_number_reflns         5225
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+25.0265P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1075
_reflns_Friedel_coverage         0.867
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1
_reflns_number_gt                4592
_reflns_number_total             5225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04241c2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7715128--7715131.cif.'
_cod_original_cell_volume        13487(9)
_cod_database_code               7715128
_shelx_shelxl_version_number     2018/3