Group 13 and 14 Alkyl Derivatives of the Imido-Nitrido Metalloligand [{Ti(η5-C5Me5)(μ-NH)}3(μ3-N)]
María García-Castro; Avelino Martín; Miguel Mena; Carlos Yélamos; Organometallics 26 (2007) 408–416; doi:10.1021/om060895+

data_4063282
_publ_section_title
;
 Group 13 and 14 Alkyl Derivatives of the Imido-Nitrido Metalloligand
 [{Ti(\h5-C5Me5)(\m-NH)}3(\m3-N)]
;
_journal_name_full               Organometallics
_journal_page_first              408
_journal_page_last               416
_journal_paper_doi               10.1021/om060895+
_journal_volume                  26
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C33 H56 N4 Sn1 Ti3'
_chemical_formula_sum            'C33 H56 N4 Sn Ti3'
_chemical_formula_weight         771.21
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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      2.2
_audit_creation_date             2003-04-25T10:26:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                95.601(9)
_cell_angle_beta                 100.525(8)
_cell_angle_gamma                98.434(7)
_cell_formula_units_Z            2
_cell_length_a                   11.5120(9)
_cell_length_b                   12.0957(8)
_cell_length_c                   13.3150(17)
_cell_measurement_reflns_used    108
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19
_cell_measurement_theta_min      4
_cell_measurement_wavelength     0.71073
_cell_volume                     1788.3(3)
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1881
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            67791
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         5.1
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.9043
_exptl_absorpt_correction_T_min  0.5533
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        (see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.686
_exptl_crystal_size_mid          0.431
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.544
_refine_diff_density_min         -1.988
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+6.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.139
_reflns_number_gt                6444
_reflns_number_total             8166
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4063282