Ti(OiPr)4/nBuLi: an attractive reagent system for [2+2+2] cyclotrimerisation reactions
Rassadin, V. A.; Nicolas, E.; Six, Y.; Chemical Communications (Cambridge, United Kingdom) 50 (2014) 7666–7669; doi:10.1039/c4cc02698e

data_7114664
_publ_section_title
;
 Ti(OiPr)4/nBuLi: an attractive reagent system for [2+2+2]
 cyclotrimerisation reactions
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   57
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              7666
_journal_page_last               7669
_journal_paper_doi               10.1039/c4cc02698e
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C30 H20 Cl2'
_chemical_formula_sum            'C30 H20 Cl2'
_chemical_formula_weight         451.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_cell_formula_units_Z            2
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_cell_volume                     1127.45(8)
_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
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_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.994
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_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.032
_diffrn_reflns_theta_min         2.906
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       Plate
_exptl_crystal_F_000             468
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_refine_diff_density_max         0.399
_refine_diff_density_min         -0.807
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         6321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0641P)^2^+0.5116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5461
_reflns_number_total             6321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc02698e2.cif
_cod_data_source_block           vr-f-254-col
_cod_database_code               7114664
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.976
_shelxl_version_number           2013-4
_shelx_res_checksum              14697
_shelx_hkl_checksum              66137