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_4334922
_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         'C40 H58 Cl2 N6 Ti3 Y, C5 H5 N'
_chemical_formula_sum            'C45 H63 Cl2 N7 Ti3 Y'
_chemical_formula_weight         1005.53
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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             2012-07-09T12:24:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.58(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.574(10)
_cell_length_b                   12.113(5)
_cell_length_c                   22.576(15)
_cell_measurement_reflns_used    344
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     4790(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, 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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0654
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            100604
_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    1.831
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.433
_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    1.394
_exptl_crystal_description       prism
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         10986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+1.7043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                7610
_reflns_number_total             10986
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400463a_si_002_2.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4334922