New Titanium Imido Synthons: Syntheses and Supramolecular Structures
Adams, Nico; Bigmore, Helen R.; Blundell, Timothy L.; Boyd, Catherine L.; Dubberley, Stuart R.; Sealey, Andrew J.; Cowley, Andrew R.; Skinner, Michael E. G.; Mountford, Philip; Inorganic Chemistry 44 (2005) 2882–2894; doi:10.1021/ic050011z

data_4301061
_publ_section_title
;
 New Titanium Imido Synthons: Syntheses and Supramolecular Structures
;
_journal_coden_ASTM              INOCAJ
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2882
_journal_page_last               2894
_journal_paper_doi               10.1021/ic050011z
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        '[Ti(N-t-Bu)Cl2(py)3] + C6F5NH2'
_chemical_formula_moiety         ' C32 H20 Cl2 F10 N6 Ti2 '
_chemical_formula_sum            'C32 H20 Cl2 F10 N6 Ti2'
_chemical_formula_weight         916.14
_chemical_name_systematic        '[Ti2(NC6F5)2Cl2(mu-Cl)2(NC5H5)4]'
_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                90.00
_cell_angle_beta                 103.425(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.2324(2)
_cell_length_b                   18.1474(5)
_cell_length_c                   13.7813(3)
_cell_measurement_reflns_used    3116
_cell_measurement_temperature    150
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      2.910
_cell_volume                     1759.36(8)
_computing_cell_refinement
;

KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)

;
_computing_data_collection
;

KappaCCD software 'Collect' (Nonius, 2000)

;
_computing_data_reduction
;

KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)

;
_computing_molecular_graphics    'CAMERON (Watkin, Prout and Pearce, 1996)'
_computing_publication_material
;

CRYSTALS Issue 10 (Watkin et al, 1996)

;
_computing_structure_refinement
;

CRYSTALS Issue 10 (Watkin et al, 1996)

;
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.01
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5740
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    0.84
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.73
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.33
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       47.4(72)
_refine_ls_extinction_method
;

 Larson 1970 Crystallographic Computing eq 22

;
_refine_ls_goodness_of_fit_obs   0.4836
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         2411
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0294
_refine_ls_shift/esd_max         0.0043
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0407
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_observed          2411
_reflns_number_total             3196
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic050011zsi20050104_034133_1.cif
_cod_data_source_block           COMPOUND_17
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'unit weights' was changed to
'unit'.

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

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 

The following automatic conversions were performed:

data name '_diffrn_measurement_device-type' was replaced with
'_diffrn_measurement_device_type' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        1759.4
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C32 H20 Cl2 F10 N6 Ti2 '
_cod_database_code               4301061