Reactions of Low-Valent Titanocene(II) Fragments withtrans-4,4′-Azobispyridine (RNNR, R = C5H4N): Formation of Tetranuclear Molecular Squares bytrans−cisIsomerization
Theilmann, Oliver; Saak, Wolfgang; Haase, Detlev; Beckhaus, Rüdiger; Organometallics 28 (2009) 2799–; doi:10.1021/om801123k

data_4068835
_publ_section_title
;
 Reactions of Low-Valent Titanocene(II) Fragments
 withtrans-4,4&#x2032;-Azobispyridine (RN&#xE5FB;NR, R = C5H4N): Formation
 of Tetranuclear Molecular Squares bytrans&#x2212;cisIsomerization
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2799
_journal_paper_doi               10.1021/om801123k
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C160 H196 N8 Ti4'
_chemical_formula_weight         2422.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                84.213(4)
_cell_angle_beta                 85.555(5)
_cell_angle_gamma                84.295(5)
_cell_formula_units_Z            2
_cell_length_a                   13.8596(7)
_cell_length_b                   19.4391(6)
_cell_length_c                   26.2189(8)
_cell_measurement_temperature    153(2)
_cell_volume                     6976.8(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.0679
_diffrn_reflns_av_sigmaI/netI    0.0861
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            87010
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.9322
_exptl_absorpt_correction_T_min  0.8752
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1389
_refine_ls_number_reflns         25792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0711P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                15754
_reflns_number_total             25792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om801123k_si_003.cif
_cod_data_source_block           c:\work\oth20\oth20
_cod_database_code               4068835