Synthesis, Cycloaddition, and Cycloreversion Reactions of Mononuclear Titanocene‒oxo Complexes
Nguyen, Trang T.; Kortman, Gregory D.; Hull, Kami L.; Organometallics 35 (2016) 1713–; doi:10.1021/acs.organomet.6b00111

data_4086505
_publ_contact_author
; 
Kami L. Hull
University of Illinois 
361 RAL, Box 23-5
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Synthesis, Cycloaddition, and Cycloreversion Reactions of Mononuclear
 Titanocene--oxo Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1713
_journal_paper_doi               10.1021/acs.organomet.6b00111
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C35 H42 O2 Ti, C6 H14'
_chemical_formula_sum            'C41 H56 O2 Ti'
_chemical_formula_weight         628.75
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1458(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8456(7)
_cell_length_b                   11.0731(5)
_cell_length_c                   19.6639(9)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      68.28
_cell_measurement_theta_min      4.88
_cell_volume                     3423.4(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics
; 
SHELXTL v2013-4 (Bruker, 2013), CrystalMaker v2.7.3 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2013-1 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  cd15msa_sq
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40461
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.452
_diffrn_reflns_theta_min         4.532
_exptl_absorpt_coefficient_mu    2.364
_exptl_absorpt_correction_T_max  0.5843
_exptl_absorpt_correction_T_min  0.3259
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS 2014/3 (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_id                cd15msa_sq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (2 3 0) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.675
_exptl_crystal_size_mid          0.604
_exptl_crystal_size_min          0.372
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3156
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+2.7481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.0982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3131
_reflns_number_total             3156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00111_si_002.cif
_cod_data_source_block           cd15msa_sq
_cod_depositor_comments
'Adding full bibliography for 4086503--4086505.cif.'
_cod_database_code               4086505
_shelx_estimated_absorpt_t_min   0.298
_shelx_estimated_absorpt_t_max   0.473
_shelxl_version_number           2014-3
_shelx_res_checksum              75818
_shelx_hkl_checksum              53770
_shelx_fab_checksum              57920