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_1560118
_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         'C10 H24 Cl3 N2 O Ti'
_chemical_formula_sum            'C10 H24 Cl3 N2 O Ti'
_chemical_formula_weight         342.56
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
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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                 101.587(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.972(4)
_cell_length_b                   12.308(4)
_cell_length_c                   12.075(4)
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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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'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 0.997
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
;
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;
Rigaku Saturn724+ (4x4 bin mode)
;
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_exptl_absorpt_process_details
;
Jacobson, R. (1998). REQAB. Private communication to the 
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            blue
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'Re-crystallisation from solvent: THF/hexane'
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_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0633P)^2^+1.8356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1447
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_reflns_number_gt                2930
_reflns_number_total             3644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06366e2.cif
_cod_data_source_block           TiCl3tmedathf
_cod_depositor_comments
'Adding full bibliography for 1560116--1560121.cif.'
_cod_database_code               1560118
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.887
_olex2_submission_special_instructions 'No special instructions were received'