Synthesis, Structures, and DFT Bonding Analysis of New Titanium Hydrazido(2-) Complexes
Thomas B. Parsons; Nilay Hazari; Andrew R. Cowley; Jennifer C. Green; Philip Mountford; Inorganic Chemistry 44 (2005) 8442–8458; doi:10.1021/ic051271j

data_4310029
_publ_section_title
;
Synthesis, Structures, and DFT Bonding Analysis of New Titanium
Hydrazido(2-) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8442
_journal_page_last               8458
_journal_paper_doi               10.1021/ic051271j
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C28 H32 Cl2 N8 Ti, 2(C6 H6) '
_chemical_formula_sum            'C40 H44 Cl2 N8 Ti'
_chemical_formula_weight         755.65
_chemical_name_systematic
; 
Ti(NNPh2)Cl2{(HC(Me2pz)3}
;
_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                80.3636(9)
_cell_angle_beta                 88.1593(9)
_cell_angle_gamma                86.2151(11)
_cell_formula_units_Z            2
_cell_length_a                   9.6913(2)
_cell_length_b                   13.9790(3)
_cell_length_c                   14.1852(3)
_cell_measurement_reflns_used    26144
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     1890.05(7)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.046
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26144
_diffrn_reflns_theta_full        27.477
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_min         5.179
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       ' prism '
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_thermal_history
; 
The material was crystallised at ambient temperature. A suitable crystal 
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis. 
;
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.44
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0999
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         5173
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.004317
_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: 
 0.786 0.320 0.487 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0722
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0452
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              18
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                5173
_reflns_number_total             8555
_reflns_threshold_expression     I>3.00u(I)
_cod_duplicate_entry             4310003
_cod_data_source_file            ic051271jsi20050728_105607_4.cif
_cod_data_source_block           COMPOUND_9
_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 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C40 H44 Cl2 N8 Ti '
_cod_database_code               4310029