Bis(cyclopentadienyl) Titanium Dinitrogen Chemistry: Synthesis and Characterization of a Side-on Bound Haptomer
Hanna, Tamara E.; Bernskoetter, Wesley H.; Bouwkamp, Marco W.; Lobkovsky, Emil; Chirik, Paul J.; Organometallics 26 (2007) 2431–; doi:10.1021/om0611913

data_4072993
_publ_section_title
;
 Bis(cyclopentadienyl) Titanium Dinitrogen Chemistry:&#x00A0; Synthesis
 and Characterization of a Side-on Bound Haptomer
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2431
_journal_paper_doi               10.1021/om0611913
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety
'C40 H60 N6 Si2 Ti2, C40 H60 N2 Si2 Ti2, 2(C5 H12)'
_chemical_formula_sum            'C90 H144 N8 Si4 Ti4'
_chemical_formula_weight         1642.1
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.874(5)
_cell_angle_beta                 96.817(5)
_cell_angle_gamma                111.372(4)
_cell_formula_units_Z            2
_cell_length_a                   14.2552(16)
_cell_length_b                   14.3997(14)
_cell_length_c                   24.330(2)
_cell_measurement_reflns_used    9822
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.62
_cell_measurement_theta_min      2.39
_cell_volume                     4594.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       APEX2
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            78504
_diffrn_reflns_theta_full        26.48
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9579
_exptl_absorpt_correction_T_min  0.8809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1461
_refine_ls_number_reflns         18442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.534
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+1.6958P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                12686
_reflns_number_total             18442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0611913si20061230_110047.cif
_cod_data_source_block           th8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4072993