Aromatic Imines in the Titanocene Coordination Sphere—Titanaaziridine vs 1-Aza-2-titanacyclopent-4-ene Structures
Loose, Florian; Plettenberg, Inka; Haase, Detlev; Saak, Wolfgang; Schmidtmann, Marc; Schäfer, André; Müller, Thomas; Beckhaus, Rüdiger; Organometallics 33 (2014) 6785–; doi:10.1021/om500750y

data_4084765
_publ_section_title
;
 Aromatic Imines in the Titanocene Coordination Sphere---Titanaaziridine
 vs 1-Aza-2-titanacyclopent-4-ene Structures
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6785
_journal_paper_doi               10.1021/om500750y
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C27 H29 N O Ti'
_chemical_formula_weight         431.41
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.869(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.0161(14)
_cell_length_b                   8.1587(4)
_cell_length_c                   14.4380(5)
_cell_measurement_reflns_used    3279
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.03
_cell_measurement_theta_min      2.89
_cell_volume                     4446.0(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Diamond Crystal Impact, 2010)'
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1479
_diffrn_reflns_av_sigmaI/netI    0.1652
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24844
_diffrn_reflns_theta_full        29.10
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.8927
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5860
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0694
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                3180
_reflns_number_total             5860
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500750y_si_001.cif
_cod_data_source_block           20a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/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 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4084761--4084765.cif.
;
_cod_original_sg_symbol_H-M      'C2/c  '
_cod_database_code               4084765