Five- and Six-Coordinate Group 4 Compounds Stabilized by β-Ketiminate and Diketiminate Ligands: Syntheses and Comparisons between Solid-State and Solution Structures
Lena Kakaliou; Scanlon; Baixin Qian; Sung W. Baek; Milton R. Smith; Douglas H. Motry; Inorganic Chemistry 38 (1999) 5964–5977; doi:10.1021/ic981364j

data_4322533
_publ_section_title
;
 Five- and Six-Coordinate Group 4 Compounds Stabilized by \b-Ketiminate
 and Diketiminate Ligands: Syntheses and Comparisons between Solid-State
 and Solution Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5964
_journal_page_last               5977
_journal_paper_doi               10.1021/ic981364j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C24 H28 Cl2 N2 O2 Ti'
_chemical_formula_weight         495.28
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.5548(2)
_cell_length_b                   20.0716(3)
_cell_length_c                   21.58750(10)
_cell_measurement_temperature    132(2)
_cell_volume                     5006.64(12)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      132(2)
_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  0.0992
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51611
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.577
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.094
_refine_ls_goodness_of_fit_obs   1.181
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_restrained_S_obs      1.181
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_obs          0.0634
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+4.2462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1086
_refine_ls_wR_factor_obs         0.0958
_reflns_number_observed          4118
_reflns_number_total             6048
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981364j_06.cif
_cod_data_source_block           (TP)2TiCl2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+4.2462P] 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^)+(0.0316P)^2^+4.2462P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322533