N-Alkoxy-β-ketoiminate Complexes of Groups 4 and 5: Synthesis and Characterization of the Complexes [(η5-C5H4R)M{CH3C(O)CHC(NCH2CHR‘O)CH3}Cln] (M = Ti,n= 1; M = Nb,n= 2; R = H, Me; R‘ = H, Me), [Ti{CH3C(O)CHC(NCH2CHR‘O)CH3}Cl2(thf)], and [Ti{CH3C(O)CHC(NCH2CHR‘O)CH3}2]
Doherty, Simon; Errington, R. John; Housley, Neil; Ridland, John; Clegg, William; Elsegood, Mark R. J.; Organometallics 18 (1999) 1018–; doi:10.1021/om980510q

data_4077733
_publ_section_title
;
 N-Alkoxy-\b-ketoiminate Complexes of Groups 4 and 5:&#x00A0; Synthesis
 and Characterization of the Complexes
 [(\h5-C5H4R)M{CH3C(O)CHC(NCH2CHR&#x2018;O)CH3}Cln] (M = Ti,n= 1; M =
 Nb,n= 2; R = H, Me; R&#x2018; = H, Me),
 [Ti{CH3C(O)CHC(NCH2CHR&#x2018;O)CH3}Cl2(thf)], and
 [Ti{CH3C(O)CHC(NCH2CHR&#x2018;O)CH3}2]
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1018
_journal_paper_doi               10.1021/om980510q
_journal_volume                  18
_journal_year                    1999
_chemical_formula_sum            'C12 H21 Cl2 N O3 Ti'
_chemical_formula_weight         346.10
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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            8
_cell_length_a                   14.4022(9)
_cell_length_b                   14.6208(9)
_cell_length_c                   14.8973(9)
_cell_measurement_reflns_used    11095
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.41
_cell_volume                     3136.9(3)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18642
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.889
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3764
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+4.6646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                3024
_reflns_number_total             3764
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om980510q.cif
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4077733