Synthesis, Structural Characterization, and Preliminary Reactivity Profile of a Series of Monocyclopentadienyl, Monoacetamidinate Titanium(III) Alkyl Complexes Bearing β-Hydrogens
Trunkely, Emily F.; Epshteyn, Albert; Zavalij, Peter Y.; Sita, Lawrence R.; Organometallics 29 (2010) 6587–; doi:10.1021/om100877d

data_4067177
_publ_section_title
;
 Synthesis, Structural Characterization, and Preliminary Reactivity
 Profile of a Series of Monocyclopentadienyl, Monoacetamidinate
 Titanium(III) Alkyl Complexes Bearing \b-Hydrogens
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6587
_journal_paper_doi               10.1021/om100877d
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C23 H43 N2 Ti'
_chemical_formula_sum            'C23 H43 N2 Ti'
_chemical_formula_weight         395.49
_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           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0967(2)
_cell_length_b                   16.5501(2)
_cell_length_c                   18.3592(2)
_cell_measurement_reflns_used    66250
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.5
_cell_volume                     4890.93(10)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      610,610,610,1200,1200,1200
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0049317
_diffrn_orient_matrix_UB_12      0.0013500
_diffrn_orient_matrix_UB_13      0.0542833
_diffrn_orient_matrix_UB_21      -0.0029521
_diffrn_orient_matrix_UB_22      0.0603335
_diffrn_orient_matrix_UB_23      -0.0014175
_diffrn_orient_matrix_UB_31      -0.0618582
_diffrn_orient_matrix_UB_32      -0.0029874
_diffrn_orient_matrix_UB_33      -0.0042601
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0077
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            103360
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.08
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1736
_exptl_crystal_id                ' '
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.00307(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5612
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.02P)^2^+3.679P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0788
_reflns_number_gt                5132
_reflns_number_total             5612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100877d_si_005.cif
_cod_data_source_block           cmpd_5
_cod_depositor_comments
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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 2.4.1 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      Pbca
_cod_database_code               4067177