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_4064370
_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         'C27 H25 N3 Ti1'
_chemical_formula_sum            'C27 H25 N3 Ti'
_chemical_formula_weight         439.42
_chemical_name_systematic
;
Cp2Ti(NNPh2)(py)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 101.1737(4)
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   29.3869(2)
_cell_length_b                   16.55440(10)
_cell_length_c                   36.7180(3)
_cell_measurement_reflns_used    17580
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     17524.1(2)
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.965
_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  0.033
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            35849
_diffrn_reflns_theta_full        25.260
_diffrn_reflns_theta_max         27.456
_diffrn_reflns_theta_min         5.090
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             7360
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.39
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0791
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         10812
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.0008
_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: 
 1.51 0.663 1.02 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0711
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0547
_reflns_limit_h_max              36
_reflns_limit_h_min              -38
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              47
_reflns_limit_l_min              0
_reflns_number_gt                10812
_reflns_number_total             19339
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.61
_oxford_diffrn_Wilson_scale      45.88
_oxford_refine_ls_scale          0.1543(2)
_cod_data_source_file            om200068k_si_001.cif
_cod_data_source_block           Compound_14
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C27 H25 N3 Ti1'
_cod_database_code               4064370