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_4067180
_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         'C32 H52 N3 Ti'
_chemical_formula_sum            'C32 H52 N3 Ti'
_chemical_formula_weight         526.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.0770(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7694(4)
_cell_length_b                   31.3190(11)
_cell_length_c                   10.0936(4)
_cell_measurement_reflns_used    19707
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.2
_cell_volume                     3049.6(2)
_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      610,610,610,610,610,610,610
_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      0.0033133
_diffrn_orient_matrix_UB_12      -0.0099840
_diffrn_orient_matrix_UB_13      0.0945587
_diffrn_orient_matrix_UB_21      0.0248179
_diffrn_orient_matrix_UB_22      -0.0293663
_diffrn_orient_matrix_UB_23      -0.0270160
_diffrn_orient_matrix_UB_31      0.1005889
_diffrn_orient_matrix_UB_32      0.0075772
_diffrn_orient_matrix_UB_33      0.0198621
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0151
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            50254
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1148
_exptl_crystal_id                'S '
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0316
_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^)+(0.01P)^2^+2.555P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0676
_reflns_number_gt                4750
_reflns_number_total             5363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100877d_si_008.cif
_cod_data_source_block           cmpd_10
_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 2.4.1 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 21/n'
_cod_database_code               4067180