New ligand platforms for developing the chemistry of the Ti=N‒NR2 functional group and the insertion of alkynes into the N‒N bond of a Ti=N‒NPh2 ligand
Selby, Jonathan D.; Manley, Catherine D.; Feliz, Marta; Schwarz, Andrew D.; Clot, Eric; Mountford, Philip; Chemical Communications (Cambridge, United Kingdom)  (2007) 4937–4939; doi:10.1039/b711941k

data_7113184
_publ_section_title
;
 New ligand platforms for developing the chemistry of the Ti=N--NR2
 functional group and the insertion of alkynes into the N--N bond of a
 Ti=N--NPh2 ligand
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   46
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              4937
_journal_page_last               4939
_journal_paper_doi               10.1039/b711941k
_journal_year                    2007
_chemical_formula_moiety         'C28 H44 N6 Si2 Ti1'
_chemical_formula_sum            'C28 H44 N6 Si2 Ti'
_chemical_formula_weight         568.77
_chemical_name_common            Ti(MeN(CH2CH2SiMe3)2)(NNNPh2)(py)
_chemical_name_systematic        Ti{MeN(CH2CH2SiMe3)2}(NNNPh2)(py)
_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                89.726(3)
_cell_angle_beta                 77.178(2)
_cell_angle_gamma                85.912(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1794(5)
_cell_length_b                   11.1800(7)
_cell_length_c                   13.8952(8)
_cell_measurement_reflns_used    4943
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     1537.90(15)
_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 0.986
_diffrn_measured_fraction_theta_max 0.984
_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  0.055
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9697
_diffrn_reflns_theta_full        25.117
_diffrn_reflns_theta_max         25.630
_diffrn_reflns_theta_min         5.145
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.05
_refine_diff_density_min         -0.84
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         3146
_refine_ls_number_restraints     114
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.004
_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:
1.16 0.913E-01 0.941 -0.622E-01 0.234
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1097
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0800
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3146
_reflns_number_total             5728
_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          0.3650(12)
_cod_duplicate_entry             7102305
_cod_data_source_file            b711941k.txt
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C28 H44 N6 Si2 Ti1'
_cod_database_code               7113184