Ambient-Temperature Carbon‒Oxygen Bond Cleavage of an α-Aryloxy Ketone with Cp2Ti(BTMSA) and Selective Protonolysis of the Resulting Ti‒OR Bonds
Desnoyer, Addison N.; Fartel, Beata; MacLeod, K. Cory; Patrick, Brian O.; Smith, Kevin M.; Organometallics 31 (2012) 7625–; doi:10.1021/om300950c

data_4079693
_publ_section_title
;
 Ambient-Temperature Carbon--Oxygen Bond Cleavage of an \a-Aryloxy Ketone
 with Cp2Ti(BTMSA) and Selective Protonolysis of the Resulting Ti--OR
 Bonds
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              7625
_journal_paper_doi               10.1021/om300950c
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C24 H23 Cl O2 Ti'
_chemical_formula_weight         426.77
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.597(3)
_cell_angle_beta                 83.995(3)
_cell_angle_gamma                85.320(3)
_cell_formula_units_Z            4
_cell_length_a                   9.1320(11)
_cell_length_b                   13.5283(16)
_cell_length_c                   16.404(3)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.16
_cell_measurement_theta_min      2.50
_cell_volume                     2008.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_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  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42998
_diffrn_reflns_theta_full        30.17
_diffrn_reflns_theta_max         30.17
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         11812
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0348P)^2^+0.8938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0794
_reflns_number_gt                9946
_reflns_number_total             11812
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om300950c_si_002.cif
_cod_data_source_block           8_Cp2Ti[OCH(Ph)CH2OPh]Cl
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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 1891 2012-01-12 08:04:46Z andrius 
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_cod_database_code               4079693