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_4319246
_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        '[Ti(NSiMe3)Cl2]8 + KL1'
_chemical_formula_moiety         'C30 H57 Cl N4 O Si Ti, C4 H10 O'
_chemical_formula_sum            'C34 H67 Cl N4 O2 Si Ti'
_chemical_formula_weight         675.37
_chemical_melting_point          ?
_chemical_name_systematic        '[Ti(NSiMe3)(L1)Cl]'
_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     direct
_cell_angle_alpha                90
_cell_angle_beta                 103.128(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.000(4)
_cell_length_b                   14.735(3)
_cell_length_c                   24.752(9)
_cell_measurement_reflns_used    16275
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      0
_cell_volume                     3907(2)
_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    'sir92 (giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_max 0.933
_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  0.086
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16275
_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    0.35
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.15
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1473.98
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.91
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.0510
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5657
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.0147
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
chebychev polynomial with 3 parameters, carruthers & watkin , 1979,
 2.27    0.710     1.85
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0580
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                5657
_reflns_number_total             7612
_reflns_threshold_expression     >3.00\s(i)
_cod_data_source_file            ic0009728_2.cif
_cod_data_source_block           COMPOUND_2
_cod_depositor_comments
;
 Changing the capitalization of _atom_type_symbol data item
 values and adding the _atom_site_type_symbol data item.
 Updating the _chemical_formula_sum data item value.

 Antanas Vaitkus,
 2017-01-05

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.

'_refine_ls_structure_factor_coef' value 'f' changed to
'F' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_atom_site_adp_type'
value 'uani' changed to 'Uani' according to the built-in table from
CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29 (43 times).

'_atom_site_adp_type' value 'uiso' changed to
'Uiso' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (67 times).

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        3907.1(5)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'c34 h67 cl n4 o2 si ti'
_cod_database_code               4319246