Single and double substrate insertion into the Ti=N(alpha) bonds of terminal titanium hydrazides.
Tiong, Pei-Jen; Schofield, A Daniel; Selby, Jonathan D; Nova, Ainara; Clot, Eric; Mountford, Philip; Chemical communications (Cambridge, England) 46 (2009) 85–87; doi:10.1039/b920090h

data_7105135
_publ_section_title
;
 Single and double substrate insertion into the Ti=N(alpha) bonds of
 terminal titanium hydrazides.
;
_journal_issue                   1
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              85
_journal_page_last               87
_journal_paper_doi               10.1039/b920090h
_journal_volume                  46
_journal_year                    2009
_chemical_formula_moiety         'C35 H44 F5 N7 Si2 Ti1'
_chemical_formula_sum            'C35 H44 F5 N7 Si2 Ti'
_chemical_formula_weight         761.84
_chemical_name_systematic
;
Ti(N2NMe){NC(ArF)NNPh2}(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
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90
_cell_angle_beta                 93.8645(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7067(2)
_cell_length_b                   18.2074(2)
_cell_length_c                   15.3084(2)
_cell_measurement_reflns_used    8820
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3811.73(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 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_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       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            62187
_diffrn_reflns_theta_full        26.922
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         5.099
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7207
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000784
_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:
1.32 0.130 1.10 0.135E-01 0.277
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0397
_refine_ls_wR_factor_gt          0.0343
_refine_ls_wR_factor_ref         0.0335
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                7532
_reflns_number_total             8662
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.44
_oxford_diffrn_Wilson_scale      1.69
_oxford_refine_ls_r_factor_ref   0.0329
_oxford_refine_ls_scale          0.7899(7)
_oxford_reflns_number_all        8662
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            b920090h.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 '/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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C35 H44 F5 N7 Si2 Ti1'
_cod_database_code               7105135