Structural elucidation of a methylenation reagent of esters: synthesis and reactivity of a dinuclear titanium(iii) methylene complex
Kurogi, Takashi; Kuroki, Kaito; Moritani, Shunsuke; Takai, Kazuhiko; Chemical Science 12 (2021) 3509–3515; doi:10.1039/D0SC06366E

data_1560117
_publ_section_title
;
 Structural elucidation of a methylenation reagent of esters: synthesis
 and reactivity of a dinuclear titanium(iii) methylene complex
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3509
_journal_page_last               3515
_journal_paper_doi               10.1039/D0SC06366E
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         '2(C6 H16 Cl3 N2 Ti), 2(C H2 Cl2)'
_chemical_formula_sum            'C14 H36 Cl10 N4 Ti2'
_chemical_formula_weight         710.77
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-19 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.468(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.348(3)
_cell_length_b                   13.855(3)
_cell_length_c                   17.166(4)
_cell_measurement_reflns_used    7872
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
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_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
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'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
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'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
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_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
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_diffrn_measurement_device_type
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
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_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0433
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_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_l_min       -22
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_exptl_absorpt_process_details
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.609
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_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/hexane'
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0562
_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^)+(0.0316P)^2^+6.2137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6256
_reflns_number_total             6710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06366e2.cif
_cod_data_source_block           TiCl3tmeda_dimer
_cod_depositor_comments
'Adding full bibliography for 1560116--1560121.cif.'
_cod_database_code               1560117
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.867
_olex2_submission_special_instructions 'No special instructions were received'