Redox-Active Behavior of the [{Ti(η5-C5Me5)(μ-NH)}3(μ3-N)] Metalloligand
Jorge Caballo; Jorge J. Carbó; Miguel Mena; Adrián Pérez-Redondo; Josep-M. Poblet; Carlos Yélamos; Inorganic Chemistry 52 (2013) 6103–6109; doi:10.1021/ic400463a

data_4334923
_publ_contact_author_address
;
Departamento de Qu\'imica Inorg\'anica
Universidad de Alcal\'a
28871, Alcal\'a de Henares
Madrid, Spain
;
_publ_contact_author_email       adrian.perez@uah.es
_publ_contact_author_fax         '+34 91 8854683'
_publ_contact_author_name        'P\'erez-Redondo, Adri\'an'
_publ_contact_author_phone       '+34 91 8854677'
_publ_section_title
;
 Redox-Active Behavior of the [{Ti(\h5-C5Me5)(\m-NH)}3(\m3-N)]
 Metalloligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6103
_journal_page_last               6109
_journal_paper_doi               10.1021/ic400463a
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety
'C30 H48 Cl3 N4 Ti3 Y, C12 H24 K O6, 7(C6 H6)'
_chemical_formula_sum            'C84 H114 Cl3 K N4 O6 Ti3 Y'
_chemical_formula_weight         1653.85
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2012-07-09T16:22:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.527(4)
_cell_length_b                   16.527(3)
_cell_length_c                   18.067(4)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     4273.7(16)
_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, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(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_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            58887
_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        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1738
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
Compound 5 crystallized with seven molecules of benzene, which were found in 
the difference Fourier map (two and 1/3 of benzene molecules per asymmetric 
unit), but it was not possible to get a chemically sensible model for them, so 
the Squeeze procedure was employed to remove their contribution to 
the structure factors.
;
_refine_diff_density_max         0.79
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         6547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1353P)^2^+0.4158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2225
_refine_ls_wR_factor_ref         0.2386
_reflns_number_gt                4243
_reflns_number_total             6547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400463a_si_002_3.cif
_cod_data_source_block           5
_cod_database_code               4334923