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_4087665
_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
; 
C60 H62 F6 O7 Ti, 0.632(C7 H8), 0.368(C5 H12) 
;
_chemical_formula_sum            'C66.26 H71.47 F6 O7 Ti'
_chemical_formula_weight         1141.78
_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-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90.607(8)
_cell_angle_beta                 98.046(9)
_cell_angle_gamma                97.865(9)
_cell_formula_units_Z            2
_cell_length_a                   11.695(2)
_cell_length_b                   14.142(2)
_cell_length_c                   17.854(3)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.07
_cell_measurement_theta_min      2.25
_cell_volume                     2895.0(8)
_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-2014-7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm26ssa
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            79102
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         1.776
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9178
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1202
_exptl_crystal_id                cm26ssa
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (0 -4 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         14405
_refine_ls_number_restraints     527
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0588P)^2^+2.0884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11719
_reflns_number_total             14405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00470_si_002.cif
_cod_data_source_block           3
_cod_original_cell_volume        2895.1(8)
_cod_database_code               4087665
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.917
_shelx_estimated_absorpt_t_max   0.967
_exptl_absorpt_special_details
; 
 The following wavelength and cell were deduced by SADABS from the 
 direction cosines etc. They are given here for emergency use only: 
 CELL 0.71067   11.695   14.121   17.863   90.612   98.206   97.747 
;
_shelx_res_checksum              56087
_shelx_hkl_checksum              55086