A Modular and Efficient Synthesis of Functional Titanocenes
Andreas Gansäuer; Dieter Franke; Thorsten Lauterbach; Martin Nieger; Journal of the American Chemical Society 127 (2005) 11622–11623; doi:10.1021/ja054185r

data_4111884
_publ_contact_author
;
        Martin Nieger
        Institut f\"ur Anorganische Chemie
        Universit\"at Bonn
        Gerhard-Domagk-Str. 1
        D-53121 Bonn
        Bundesrepublik Deutschland
;
_publ_contact_author_email       NIEGER@JOYX.JOENSUU.FI
_publ_contact_author_fax         '049 228 73-5327'
_publ_contact_author_phone       '049 228 73-5823'
_publ_section_title
;
 A Modular and Efficient Synthesis of Functional Titanocenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11622
_journal_page_last               11623
_journal_paper_doi               10.1021/ja054185r
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C21 H29 Cl2 N O Ti - 1.5 CH2Cl2'
_chemical_formula_sum            'C22.5 H32 Cl5 N O Ti'
_chemical_formula_weight         557.64
_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                 105.406(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.9954(7)
_cell_length_b                   13.9007(6)
_cell_length_c                   19.1105(9)
_cell_measurement_reflns_used    4603
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     5120.9(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    XP
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'rotation in phi and omega, 1 deg.'
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12444
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  0.85719
_exptl_absorpt_correction_T_min  0.78390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Platon, cf. Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      ?
_exptl_crystal_description       pltaes
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.083
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4488
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+53.7700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1823
_refine_ls_wR_factor_ref         0.1890
_reflns_number_gt                3572
_reflns_number_total             4488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja054185rsi20050725_094151_2.cif
_cod_data_source_block           ga17_m_compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C22.50 H32 Cl5 N O Ti'
_cod_database_code               4111884