Dinitrogen Complexes of Bis(cyclopentadienyl) Titanium Derivatives: Structural Diversity Arising from Substituent Manipulation
Hanna, Tamara E.; Lobkovsky, Emil; Chirik, Paul J.; Organometallics 28 (2009) 4079–; doi:10.1021/om900282u

data_4069561
_publ_section_title
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 Dinitrogen Complexes of Bis(cyclopentadienyl) Titanium Derivatives:
 Structural Diversity Arising from Substituent Manipulation
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              4079
_journal_paper_doi               10.1021/om900282u
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C22 H34 N3 Ti'
_chemical_formula_weight         388.42
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.705(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.0056(11)
_cell_length_b                   10.0175(6)
_cell_length_c                   18.8744(9)
_cell_measurement_reflns_used    8844
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      2.47
_cell_volume                     4158.9(4)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker 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 0.865
_diffrn_measured_fraction_theta_max 0.865
_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  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30219
_diffrn_reflns_theta_full        34.20
_diffrn_reflns_theta_max         34.20
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.9590
_exptl_absorpt_correction_T_min  0.8329
_exptl_absorpt_correction_type   'semiempirical by SADABS'
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.231
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1395
_reflns_number_gt                5636
_reflns_number_total             7447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900282u_si_001.cif
_cod_data_source_block           th15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4069561