Synthesis and X-ray Crystal Structure Determination of New Zwitterionic Complexes of Titanocene
Burlakov, V. V.; Arndt, P.; Baumann, W.; Spannenberg, A.; Rosenthal, U.; Letov, A. V.; Lyssenko, K. A.; Korlyukov, A. A.; Strunkina, L. I.; Minacheva, M. Kh.; Shur, V. B.; Organometallics 20 (2001) 4072–; doi:10.1021/om0103052

data_4077350
_publ_section_title
;
 Synthesis and X-ray Crystal Structure Determination of New Zwitterionic
 Complexes of Titanocene
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4072
_journal_paper_doi               10.1021/om0103052
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         'C31 H15 B F15 O Ti, 0.5 (C7 H8)'
_chemical_formula_sum            'C34.5 H19 B F15 O Ti'
_chemical_formula_weight         793.21
_chemical_melting_point          '469-470 K (decom)'
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.83(3)
_cell_angle_beta                 77.16(3)
_cell_angle_gamma                71.89(3)
_cell_formula_units_Z            2
_cell_length_a                   9.096(2)
_cell_length_b                   13.153(3)
_cell_length_c                   15.561(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     1627.0(7)
_computing_cell_refinement       STOE-CELL
_computing_data_collection       STOE-EXPOSE
_computing_data_reduction        STOE-INTEGRATE
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device       STOE-IPDS
_diffrn_measurement_method       'laser scanned imaging plate'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0607
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4858
_diffrn_reflns_theta_full        24.19
_diffrn_reflns_theta_max         24.19
_diffrn_reflns_theta_min         1.84
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       prism
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.895
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         4858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0706P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1117
_reflns_number_observed          3612
_reflns_number_total             4858
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om0103052.cif
_cod_data_source_block           sample6
_cod_original_cell_volume        1627.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C34.50 H19 B F15 O Ti'
_cod_database_code               4077350