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_4072314
_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_formula_moiety         'C27 H25 Cl2 N5 Ti1'
_chemical_formula_sum            'C27 H25 Cl2 N5 Ti'
_chemical_formula_weight         538.33
_chemical_name_systematic
;
Ti(NNPh2)Cl2(py)3
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 93.9572(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0110(4)
_cell_length_b                   19.8007(6)
_cell_length_c                   9.4425(3)
_cell_measurement_reflns_used    2967
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2613.36(14)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.027
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5650
_diffrn_reflns_theta_full        26.929
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         5.119
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.28
_refine_ls_extinction_coef       23(17)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.1086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2005
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001727
_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: 
 0.395 0.135 0.161 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0538
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.0367
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2005
_reflns_number_total             2989
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.44
_oxford_diffrn_Wilson_scale      20.23
_cod_data_source_file            om8007597_si_002.cif
_cod_data_source_block           compound_7
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C27 H25 Cl2 N5 Ti1'
_cod_database_code               4072314