Ammonolysis of Mono(pentamethylcyclopentadienyl) Titanium(IV) Derivatives
Angel Abarca; Pilar Gómez-Sal; Avelino Martín; Miguel Mena; Josep María Poblet; Carlos Yélamos; Inorganic Chemistry 39 (2000) 642–651; doi:10.1021/ic9907718

data_4300083
_publ_section_title
;
Ammonolysis of Mono(pentamethylcyclopentadienyl) Titanium(IV) Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              642
_journal_page_last               651
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C40 H58 N2 Ti2'
_chemical_formula_weight         662.68
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                66.11(1)
_cell_angle_beta                 71.44(1)
_cell_angle_gamma                87.92(1)
_cell_formula_units_Z            1
_cell_length_a                   8.684(1)
_cell_length_b                   11.074(1)
_cell_length_c                   11.174(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      6
_cell_volume                     926.07(19)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       omega-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3474
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  7200
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_type   N/A
_exptl_crystal_colour            Dark_orange
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.577
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.577
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1711P)^2^+4.8380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                2561
_reflns_number_total             3243
_reflns_threshold_expression     >2sigma(I)
_cod_original_cell_volume        926.1(2)
_cod_database_code               4300083
_journal_paper_doi 10.1021/ic9907718