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_4301059
_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_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         ' C11 H18 Cl2 F3 N3 Ti1 '
_chemical_formula_sum            'C11 H18 Cl2 F3 N3 Ti'
_chemical_formula_weight         368.08
_chemical_name_systematic        Ti(N-2-C6H4CF3)Cl2(NHMe2)2
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.1331(2)
_cell_length_b                   6.5142(2)
_cell_length_c                   32.3906(5)
_cell_measurement_reflns_used    23695
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     3404.07(12)
_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_publication_material
; 

CRYSTALS (Watkin et al, 2001) 

;
_computing_structure_refinement
; 

CRYSTALS (Watkin et al, 2001) 

;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
; 

Nonius KappaCCD 

;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            23695
_diffrn_reflns_theta_full        27.470
_diffrn_reflns_theta_max         27.470
_diffrn_reflns_theta_min         5.108
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 

 Denzo/Scalepack (Otwinowski & Minor, 1996) 

;
_exptl_crystal_colour            ' pale orange '
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.32
_refine_diff_density_min         -0.25
_refine_ls_abs_structure_details 'Flack, 3175 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.47(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0674
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4903
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.036792
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;

 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 

 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 

 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 

 Method = Robust Weighting (Prince, 1982) 

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

 A~i~ are: 

 0.455 -0.00117 0.171 

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0641
_refine_ls_wR_factor_gt          0.0343
_refine_ls_wR_factor_ref         0.0343
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              42
_reflns_limit_l_min              -41
_reflns_number_gt                4903
_reflns_number_total             7115
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic050011zsi20050104_034133_6.cif
_cod_data_source_block           COMPOUND_12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 
;
_cod_original_cell_volume        3404.07
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        ' C11 H18 Cl2 F3 N3 Ti1 '
_cod_database_code               4301059