New Sandwich and Half-Sandwich Titanium Hydrazido Compounds
Selby, Jonathan D.; Feliz, Marta; Schwarz, Andrew D.; Clot, Eric; Mountford, Philip; Organometallics 30 (2011) 2295–; doi:10.1021/om200068k

data_4064369
_publ_section_title
;
 New Sandwich and Half-Sandwich Titanium Hydrazido Compounds
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2295
_journal_paper_doi               10.1021/om200068k
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C31 H40 N4 Ti1'
_chemical_formula_sum            'C31 H40 N4 Ti'
_chemical_formula_weight         516.59
_chemical_name_systematic
;
Cp*Ti(NNPh2)(NHtBu)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
_cell_angle_alpha                74.7095(17)
_cell_angle_beta                 70.4567(17)
_cell_angle_gamma                73.849(2)
_cell_formula_units_Z            2
_cell_length_a                   9.9483(4)
_cell_length_b                   11.9990(5)
_cell_length_c                   13.5345(6)
_cell_measurement_reflns_used    5804
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1436.21(11)
_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 0.983
_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  0.076
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11141
_diffrn_reflns_theta_full        26.019
_diffrn_reflns_theta_max         27.389
_diffrn_reflns_theta_min         5.104
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_description       plate
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.76
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0742
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         3993
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0692
_refine_ls_shift/su_max          0.000230
_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 1.48 1.47 0.209 0.187 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1099
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0799
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3993
_reflns_number_total             6400
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.62
_oxford_diffrn_Wilson_scale      2.36
_cod_data_source_file            om200068k_si_001.cif
_cod_data_source_block           Compound_11
_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        'C31 H40 N4 Ti1'
_cod_database_code               4064369