Facile C‒H, C‒F, C‒Cl, and C‒C Activation by Oxatitanacyclobutene Complexes
Nguyen, Trang T.; Bertke, Jeffery A.; Gray, Danielle L.; Hull, Kami L.; Organometallics 34 (2015) 4190–; doi:10.1021/acs.organomet.5b00470

data_4087664
_publ_contact_author
; 
Kami L. Hull 
University of Illinois 
School of Chemical Sciences 
600 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Facile C--H, C--F, C--Cl, and C--C Activation by Oxatitanacyclobutene
 Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4190
_journal_paper_doi               10.1021/acs.organomet.5b00470
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C48 H60 O6 Ti'
_chemical_formula_sum            'C48 H60 O6 Ti'
_chemical_formula_weight         780.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
; 
? 
;
_cell_angle_alpha                96.3761(15)
_cell_angle_beta                 90.3364(15)
_cell_angle_gamma                104.8609(16)
_cell_formula_units_Z            2
_cell_length_a                   8.5881(4)
_cell_length_b                   12.7845(6)
_cell_length_c                   19.5964(8)
_cell_measurement_reflns_used    9605
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.39
_cell_measurement_theta_min      2.46
_cell_volume                     2065.42(16)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4, TWINABS V2012/1 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd46qsa
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            74631
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.423
_diffrn_reflns_theta_min         2.455
_exptl_absorpt_coefficient_mu    0.256
_exptl_absorpt_correction_T_max  0.99930
_exptl_absorpt_correction_T_min  0.99864
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_id                cd46qsa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 -2 4) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0491(16)
_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   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         7605
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0452P)^2^+1.5082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7072
_reflns_number_total             7605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00470_si_002.cif
_cod_data_source_block           2a
_cod_database_code               4087664
_shelx_estimated_absorpt_t_min   0.915
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2014/6
_shelx_res_checksum              11086
_shelx_hkl_checksum              71044