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_4322529
_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            'C32 H46 Cl4 N2 O3 Ti'
_chemical_formula_weight         696.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.46(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.260(3)
_cell_length_b                   16.724(3)
_cell_length_c                   27.774(6)
_cell_measurement_temperature    133(2)
_cell_volume                     7088(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(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  0.0907
_diffrn_reflns_av_sigmaI/netI    0.1185
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            18779
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.576
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00020(5)
_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   1.052
_refine_ls_goodness_of_fit_obs   1.205
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         6162
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.203
_refine_ls_R_factor_all          0.1636
_refine_ls_R_factor_obs          0.0788
_refine_ls_shift/esd_max         2.985
_refine_ls_shift/esd_mean        0.100
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+25.7614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1313
_refine_ls_wR_factor_obs         0.1083
_reflns_number_observed          3386
_reflns_number_total             6162
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981364j_02.cif
_cod_data_source_block           (TMPH)2TiCl4
_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^)+(0.0236P)^2^+25.7614P] 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^)+(0.0236P)^2^+25.7614P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7087.9(25)
_cod_database_code               4322529