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_7113185
_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         'C37 H52 N6 Si2 Ti1'
_chemical_formula_sum            'C37 H52 N6 Si2 Ti'
_chemical_formula_weight         684.93
_chemical_name_common            Ti(MeN(CH2CH2SiMe3)2)(NC(Ph)C(Me)NPh2)(py)
_chemical_name_systematic        Ti{MeN(CH2CH2SiMe3)2}{NC(Ph)C(Me)NPh2}(py)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 92.0565(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.19100(10)
_cell_length_b                   19.6879(2)
_cell_length_c                   38.0089(4)
_cell_measurement_reflns_used    26230
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     7621.17(13)
_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 0.980
_diffrn_measured_fraction_theta_max 0.979
_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  0.087
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            54098
_diffrn_reflns_theta_full        26.933
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         5.107
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.321
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       plate
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.32
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1400
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         6837
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.006168
_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:
0.370 0.120 0.160
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1081
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0443
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              49
_reflns_limit_l_min              0
_reflns_number_gt                6837
_reflns_number_total             17133
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.12
_oxford_diffrn_Wilson_scale      78.10
_cod_duplicate_entry             7102306
_cod_data_source_file            b711941k.txt
_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
/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 21/n 1 '
_cod_original_formula_sum        'C37 H52 N6 Si2 Ti1'
_cod_database_code               7113185