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_4301058
_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_formula_moiety         ' C10 H15 Cl6 N3 Ti1 . 0.5 (C6 H6) '
_chemical_formula_sum            'C13 H18 Cl6 N3 Ti'
_chemical_formula_weight         476.92
_chemical_name_systematic        'Ti(NC6Cl4H)Cl2(NHMe2)2 . 0.5(C6H6)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                115.6105(9)
_cell_angle_beta                 90.7721(8)
_cell_angle_gamma                106.112(1)
_cell_formula_units_Z            2
_cell_length_a                   7.3945(1)
_cell_length_b                   12.7544(2)
_cell_length_c                   12.9622(2)
_cell_measurement_reflns_used    4470
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1046.45(3)
_computing_cell_refinement
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_computing_data_collection
; 

 COLLECT (Nonius BV, 1997) 

;
_computing_data_reduction
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_computing_molecular_graphics
; 

 CAMERON (Watkin et al 1996) 

;
_computing_publication_material
; 

 CRYSTALS (Watkin et al 2001) 

;
_computing_structure_refinement
; 

 CRYSTALS (Watkin et al 2001) 

;
_computing_structure_solution
; 

 SIR97 (Altomare et al, 1999) 

;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
; 

Enraf Nonius Kappa CCD 

;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8769
_diffrn_reflns_theta_full        27.386
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         2.915
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.175
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_exptl_crystal_colour            ' orange '
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             482.000
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.62
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0539
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3727
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.009
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;

Method = Prince modified Chebychev polynomial, (Watkin, 1994) 

 W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 

 0.766 0.432 0.436 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0521
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0408
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              14
_reflns_limit_k_min              -16
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3728
_reflns_number_total             4805
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic050011zsi20050104_034133_5.cif
_cod_data_source_block           COMPOUND_11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic'
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:

'_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 
;
_cod_original_cell_volume        1046.45
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C13 H18 Cl6 N3 Ti1 '
_cod_database_code               4301058