Amidate complexes of titanium and zirconium: a new class of tunable precatalysts for the hydroamination of alkynes
Li, Chunyu; Thomson, Robert K.; Gillon, Bronwyn; Patrick, Brian O.; Schafer, Laurel L.; Chemical Communications (Cambridge, United Kingdom)  (2003) 2462–2463; doi:10.1039/b304176j

data_7113818
_publ_section_title
;
 Amidate complexes of titanium and zirconium: a new class of tunable
 precatalysts for the hydroamination of alkynes
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   19
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2462
_journal_page_last               2463
_journal_paper_doi               10.1039/b304176j
_journal_year                    2003
_chemical_formula_sum            'C30 H38 F10 N4 O2 Ti'
_chemical_formula_weight         724.54
_chemical_name_systematic
;
Bis(N-tButyl(perfluorophenyl)amidate)titanium-bis(diethylamide)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_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                 90.990(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5104(10)
_cell_length_b                   20.1035(18)
_cell_length_c                   15.8198(14)
_cell_measurement_reflns_used    8424
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      1.6
_cell_volume                     3342.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 11.76
_diffrn_measured_fraction_theta_full 0.843
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_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  0.0722
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8086
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4803
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         4988
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1398
_refine_ls_R_factor_gt           0.1039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+39.4650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2590
_refine_ls_wR_factor_ref         0.2757
_reflns_number_gt                3414
_reflns_number_total             4988
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7104811
_cod_data_source_file            b304176j.txt
_cod_data_source_block           ls005
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7113818