Titanium tert-Butyl- and Trimethylsilyl-imido Complexes with Monopendant Arm Triazacyclononane Ligands
Jonathan D. Gardner; David A. Robson; Leigh H. Rees; Philip Mountford; Inorganic Chemistry 40 (2001) 820–824; doi:10.1021/ic0009728

data_4319245
_publ_contact_author
;
 Dr P. Mountford           
 Inorganic Chemistry Laboratory
 South Parks Road
 Oxford
 OX1 3QR
 UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 272679'
_publ_section_title
;
 Titanium tert-Butyl- and Trimethylsilyl-imido Complexes with Monopendant
 Arm Triazacyclononane Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              820
_journal_page_last               824
_journal_paper_doi               10.1021/ic0009728
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source
;
 L2 + [Ti(N-t-Bu)Cl2(py)3]
;
_chemical_formula_moiety         'C22 H41 Cl N5 Ti, 3(C H2 Cl2), Cl'
_chemical_formula_sum            'C25 H47 Cl8 N5 Ti'
_chemical_formula_weight         749.21
_chemical_melting_point          ?
_chemical_name_systematic
;                                                                               
 [Ti(N-t-Bu)(L2)Cl]Cl      
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 108.49(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.034(7)
_cell_length_b                   11.534(5)
_cell_length_c                   19.534(4)
_cell_measurement_reflns_used    12239
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     3640(3)
_computing_cell_refinement
;                                                                               
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)                             
;
_computing_data_collection
;                                                                               
DIP2000 software 'Xpress' (MAC Science, 1989)                                   
;
_computing_data_reduction
;                                                                               
DIP2000 software 'DENZO' (Otwinowski & Minor, 1996)                             
;
_computing_molecular_graphics
;                                                                               
 CAMERON (Watkin, Prout & Pearce,  1996)                                        
;
_computing_publication_material
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_refinement
;                                                                               
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)                
;
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type
;                                                                               
Enraf-nonius DIP2000                                                            
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12239
_diffrn_reflns_theta_max         26.57
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.85
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.37
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1565.32
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0808
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         3998
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.0004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 
 2.63    0.527     2.29    
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0539
_reflns_limit_h_max              19
_reflns_limit_h_min              -21
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                3998
_reflns_number_total             6969
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic0009728_1.cif
_cod_data_source_block           COMPOUND_3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3639.7(5)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4319245