Side-on Dinitrogen Complexes of Titanocenes with Disubstituted Cyclopentadienyl Ligands: Synthesis, Structure, and Spectroscopic Characterization
Semproni, Scott P.; Milsmann, Carsten; Chirik, Paul J.; Organometallics 31 (2012) 3672–; doi:10.1021/om300156z

data_4076607
_publ_section_title
;
 Side-on Dinitrogen Complexes of Titanocenes with Disubstituted
 Cyclopentadienyl Ligands: Synthesis, Structure, and Spectroscopic
 Characterization
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              3672
_journal_paper_doi               10.1021/om300156z
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C28 H36 Ti2'
_chemical_formula_weight         468.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.1410(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3103(4)
_cell_length_b                   12.5477(4)
_cell_length_c                   16.1143(5)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0813
_cell_measurement_theta_min      11.5814
_cell_volume                     2649.26(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27493
_diffrn_reflns_theta_full        66.11
_diffrn_reflns_theta_max         66.11
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    5.185
_exptl_absorpt_correction_T_max  0.7527
_exptl_absorpt_correction_T_min  0.5088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            'clear dark blue-green'
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.055
_platon_squeeze_details
;
The unit cell contains one half of a disordered diethyl ether molecule
which was modeled as a diffuse contribution to the overall scattering without 
specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0355P)^2^+1.6627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                4407
_reflns_number_total             4560
_reflns_threshold_expression     >2\s(I)
_cod_duplicate_entry             4079025
_cod_data_source_file            om300156z_si_003.cif
_cod_data_source_block           sps23
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4076607