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_4067175
_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         'C22 H41 N2 Ti'
_chemical_formula_sum            'C22 H41 N2 Ti'
_chemical_formula_weight         381.47
_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                 94.4350(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1945(5)
_cell_length_b                   16.3777(8)
_cell_length_c                   12.7894(6)
_cell_measurement_reflns_used    8983
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      29.0
_cell_measurement_theta_min      2.2
_cell_volume                     2337.79(19)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSHEL (Bruker, 1999)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker Smart1000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      306,306,306,606,606
_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      0.0322352
_diffrn_orient_matrix_UB_12      0.0425507
_diffrn_orient_matrix_UB_13      0.0506912
_diffrn_orient_matrix_UB_21      0.0267761
_diffrn_orient_matrix_UB_22      -0.0437167
_diffrn_orient_matrix_UB_23      0.0511446
_diffrn_orient_matrix_UB_31      0.0791936
_diffrn_orient_matrix_UB_32      -0.0025393
_diffrn_orient_matrix_UB_33      -0.0310655
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34995
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.21
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.13
_exptl_absorpt_coefficient_mu    0.373
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.084
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_id
;
;
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0123(6)
_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     305
_refine_ls_number_reflns         5362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0342
_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^+1.243P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                4540
_reflns_number_total             5362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100877d_si_003.cif
_cod_data_source_block           cmpd_3
_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      P21/n
_cod_database_code               4067175