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_4076608
_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            'C36 H52 I0.04 N1.96 Ti2'
_chemical_formula_weight         613.46
_chemical_name_systematic
;
 ?
;
_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                 92.4910(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7481(4)
_cell_length_b                   9.7643(2)
_cell_length_c                   16.3729(3)
_cell_measurement_reflns_used    8939
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.90
_cell_measurement_theta_min      4.27
_cell_volume                     3313.86(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 (Farraguia, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 'ACTA 50'
_diffrn_measured_fraction_theta_max 0.978
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10807
_diffrn_reflns_theta_full        'ACTA 50'
_diffrn_reflns_theta_max         66.21
_diffrn_reflns_theta_min         4.27
_exptl_absorpt_coefficient_mu    4.589
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1313.2
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2854
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+7.1682P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1201
_reflns_number_gt                2800
_reflns_number_total             2854
_reflns_threshold_expression     >2\s(I)
_cod_duplicate_entry             4079026
_cod_data_source_file            om300156z_si_003.cif
_cod_data_source_block           sps37
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4076608