Crystallographic Investigation of Substituted Allyl and Titanacyclobutane Complexes of Bis(2-N,N-dialkylaminoindenyl)titanium. Structure and Reactivity as a Function of the Dialkylamino Substituents
Greidanus, Grace; McDonald, Robert; Stryker, Jeffrey M.; Organometallics 20 (2001) 2492–; doi:10.1021/om000799n

data_4077227
_publ_section_title
;
 Crystallographic Investigation of Substituted Allyl and Titanacyclobutane
 Complexes of Bis(2-N,N-dialkylaminoindenyl)titanium. Structure and
 Reactivity as a Function of the Dialkylamino Substituents
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2492
_journal_paper_doi               10.1021/om000799n
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C31 H33 N2 Ti'
_chemical_formula_weight         481.49
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.8686(15)
_cell_length_b                   18.510(3)
_cell_length_c                   27.427(4)
_cell_measurement_reflns_used    3088
_cell_measurement_temperature    193(2)
_cell_volume                     5010.0(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2742
_diffrn_reflns_av_sigmaI/netI    0.2190
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25624
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.2272
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.2104
_refine_ls_R_factor_gt           0.0772
_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^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1721
_refine_ls_wR_factor_ref         0.2241
_reflns_number_gt                1687
_reflns_number_total             4778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000799n.cif
_cod_data_source_block           jms9904
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_cell_volume        5010.1(13)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4077227