Titanium Hydrazides Supported by Diamide-Amine and Related Ligands: A Combined Experimental and DFT Study
Selby, Jonathan D.; Manley, Catherine D.; Schwarz, Andrew D.; Clot, Eric; Mountford, Philip; Organometallics 27 (2008) 6479–; doi:10.1021/om8007597

data_4072315
_publ_section_title
;
 Titanium Hydrazides Supported by Diamide-Amine and Related Ligands: A
 Combined Experimental and DFT Study
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6479
_journal_paper_doi               10.1021/om8007597
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C39 H49 Cl2 N5 Ti '
_chemical_formula_sum            'C39 H49 Cl2 N5 Ti'
_chemical_formula_weight         706.66
_chemical_name_systematic
; 
Ti(NNPh2)Cl2(py')3
;
_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                 91.9807(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.2899(2)
_cell_length_b                   17.6264(2)
_cell_length_c                   19.8028(2)
_cell_measurement_reflns_used    68416
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     7775.69(14)
_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 0.996
_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  0.046
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68416
_diffrn_reflns_theta_full        27.449
_diffrn_reflns_theta_max         27.449
_diffrn_reflns_theta_min         5.123
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Denzo/Scalepack (Otwinowski & Minor, 1996) 
;
_exptl_crystal_colour            ' green-yellow '
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_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         0.41
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1118
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     958
_refine_ls_number_reflns         10967
_refine_ls_number_restraints     316
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.015100
_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: 
 0.891 0.596 0.570 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0700
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0474
_reflns_limit_h_max              28
_reflns_limit_h_min              -28
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10967
_reflns_number_total             18156
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            om8007597_si_002.cif
_cod_data_source_block           compound_8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_refinement_disorder_assembly' tag replaced with
'_atom_site_disorder_assembly'.

'_atom_site_refinement_disorder_group'
tag replaced with '_atom_site_disorder_group'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C39 H49 Cl2 N5 Ti '
_cod_database_code               4072315