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_4072320
_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         'C52 H64 N8 O4 Ti2 . 0.5(C5 H12)'
_chemical_formula_sum            'C54.5 H70 N8 O4 Ti2'
_chemical_formula_weight         997.01
_chemical_name_systematic        'Ti2(O2NN')2(u-NNMe2)2 . 0.5(C5H12)'
_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                71.2220(3)
_cell_angle_beta                 89.4679(3)
_cell_angle_gamma                71.0947(4)
_cell_formula_units_Z            4
_cell_length_a                   14.13980(10)
_cell_length_b                   20.4771(2)
_cell_length_c                   23.2038(2)
_cell_measurement_reflns_used    22707
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     5983.79(9)
_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 0.977
_diffrn_measured_fraction_theta_max 0.969
_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  0.043
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47079
_diffrn_reflns_theta_full        25.273
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         5.097
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       plate
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.03
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0513
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1222
_refine_ls_number_reflns         17772
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.009
_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: 
 1.88 0.889 1.33 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0884
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0712
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              26
_reflns_limit_k_min              -24
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                17772
_reflns_number_total             26558
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.3680(5)
_cod_data_source_file            om8007597_si_002.cif
_cod_data_source_block           compound_16
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C54.50 H70 N8 O4 Ti2'
_cod_database_code               4072320