Synthesis and characterization of 2-pyridylalkoxide complexes of titanium, zirconium and tantalum. Crystal structures of TiCp*Me2(OCMePy2) and TaCp*Cl3(OCPy3) (Cp* = η5-C5Me5, Py = C5H4N)
Fandos, Rosa; Hernández, Carolina; Otero, Antonio; Rodríguez, Ana; Ruiz, Maria José; Terreros, Pilar; Journal of the Chemical Society, Dalton Transactions  (2000) 2990–; doi:10.1039/b002693j

data_7009681
_publ_section_title
;
 Synthesis and characterization of 2-pyridylalkoxide complexes of
 titanium, zirconium and tantalum. Crystal structures of
 TiCp*Me2(OCMePy2) and TaCp*Cl3(OCPy3)
 (Cp*&#x200A;&#x200A;=&#x200A;&#x200A;\h5-C5Me5,
 Py&#x200A;&#x200A;=&#x200A;&#x200A;C5H4N)
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2990
_journal_paper_doi               10.1039/b002693j
_journal_year                    2000
_chemical_formula_sum            'C26 H27 Cl3 N3 O Ta'
_chemical_formula_weight         684.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.369(6)
_cell_length_b                   16.6090(6)
_cell_length_c                   12.455(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     3179(2)
_computing_cell_refinement       'Nonius (control program)'
_computing_data_collection       'Nonius (control program)'
_computing_data_reduction        'XRAY80 (Stewart, 1976)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.835
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_device_type  'four circle diffractometer Nonius-Mach3'
_diffrn_measurement_method       '\w/2\2q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3351
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_interval_time  90
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.729
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         4.264
_refine_diff_density_min         -2.713
_refine_diff_density_rms         0.353
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3351
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1877P)^2^+0.5361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2214
_refine_ls_wR_factor_ref         0.2443
_reflns_number_gt                2781
_reflns_number_total             3351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b002693j.txt
_cod_data_source_block           9
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7009681