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_4076609
_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            'C44 H68 N2 Ti2'
_chemical_formula_weight         720.80
_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                100.708(5)
_cell_angle_beta                 91.440(5)
_cell_angle_gamma                92.571(5)
_cell_formula_units_Z            4
_cell_length_a                   12.247(5)
_cell_length_b                   16.134(5)
_cell_length_c                   21.079(5)
_cell_measurement_reflns_used    8438
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.38
_cell_measurement_theta_min      2.79
_cell_volume                     4086(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacavazzo, 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_sigmaI/netI    0.0837
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36118
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         66.20
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    3.538
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     948
_refine_ls_number_reflns         13235
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0712
_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^)+(0.1007P)^2^+3.3923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1803
_refine_ls_wR_factor_ref         0.2029
_reflns_number_gt                9097
_reflns_number_total             13235
_reflns_threshold_expression     >2\s(I)
_cod_duplicate_entry             4079027
_cod_data_source_file            om300156z_si_003.cif
_cod_data_source_block           sps42
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4076609