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_4077731
_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]
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_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 H16 Cl N O2 Ti'
_chemical_formula_weight         289.61
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 96.677(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5279(9)
_cell_length_b                   6.7169(5)
_cell_length_c                   15.4844(12)
_cell_measurement_reflns_used    6211
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      2.65
_cell_volume                     1294.15(17)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.841
_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  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8043
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.320
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         3063
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+3.2732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1546
_reflns_number_gt                2718
_reflns_number_total             3063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om980510q.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+3.2732P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+3.2732P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4077731