Synthesis and Reactivity of Titanium Hydrazido Complexes Supported by Diamido-Ether Ligands
Unruangsri, Junjuda; Morgan, Hannah; Schwarz, Andrew D.; Schofield, A. Daniel; Mountford, Philip; Organometallics 32 (2013) 3091–; doi:10.1021/om400311w

data_4080886
_publ_section_title
;
 Synthesis and Reactivity of Titanium Hydrazido Complexes Supported by
 Diamido-Ether Ligands
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              3091
_journal_paper_doi               10.1021/om400311w
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C20 H52 N4 O2 Se2 Si4 Ti2'
_chemical_formula_sum            'C20 H52 N4 O2 Se2 Si4 Ti2'
_chemical_formula_weight         746.72
_chemical_name_systematic
;
Ti2(N2O)2(u-Se)2
;
_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
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                64.159(7)
_cell_angle_beta                 71.134(7)
_cell_angle_gamma                69.448(7)
_cell_formula_units_Z            2
_cell_length_a                   11.6769(9)
_cell_length_b                   13.0496(9)
_cell_length_c                   14.0198(11)
_cell_measurement_reflns_used    11201
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      4
_cell_volume                     1763.2(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.076
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7306
_diffrn_reflns_theta_full        74.092
_diffrn_reflns_theta_max         76.383
_diffrn_reflns_theta_min         3.577
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.692
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         4.09
_refine_diff_density_min         -1.93
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1927
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         5970
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0962
_refine_ls_shift/su_max          0.0002220
_refine_ls_shift/su_mean         0.0000122
_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: 
 8.59 -2.51 3.57 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0981
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0880
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6241
_reflns_number_total             7306
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.47
_oxford_diffrn_Wilson_scale      0.08
_oxford_refine_ls_r_factor_ref   0.0944
_oxford_refine_ls_scale          2.599(7)
_oxford_reflns_number_all        7277
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            om400311w_si_002.cif
_cod_data_source_block           COMPOUND_21
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.3.1 from 2005-06-27.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4080886