Reduction of 1,4-dichlorobut-2-yne by titanocene to a 1,2,3-butatriene. Formation of a 1-titanacyclopent-3-yne and a 2,5-dititanabicyclo[2.2.0]hex-1(4)-ene
Burlakov, Vladimir V.; Arndt, Perdita; Baumann, Wolfgang; Spannenberg, Anke; Rosenthal, Uwe; Parameswaran, Pattiyil; Jemmis, Eluvathingal D.; Chemical Communications  (2004) 2074–2075; doi:10.1039/b406494a

data_7111345
_publ_section_title
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 Reduction of 1,4-dichlorobut-2-yne by titanocene to a 1,2,3-butatriene.
 Formation of a 1-titanacyclopent-3-yne and a
 2,5-dititanabicyclo[2.2.0]hex-1(4)-ene
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_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2074
_journal_page_last               2075
_journal_paper_doi               10.1039/b406494a
_journal_year                    2004
_chemical_formula_sum            'C24 H24 Ti2'
_chemical_formula_weight         408.23
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.687(2)
_cell_length_b                   7.887(2)
_cell_length_c                   13.353(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     914.9(4)
_computing_cell_refinement       STOE-CELL
_computing_data_collection       STOE-EXPOSE
_computing_data_reduction        STOE-INTEGRATE
_computing_molecular_graphics    XP
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       STOE-IPDS
_diffrn_measurement_method       'laser scanned imaging plate'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2621
_diffrn_reflns_theta_max         24.22
_diffrn_reflns_theta_min         2.80
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_type   no
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       prism
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         1428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_obs          0.0364
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.6738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0963
_refine_ls_wR_factor_obs         0.0888
_reflns_number_observed          1221
_reflns_number_total             1429
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b406494asup1.cif
_cod_data_source_block           ks248
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.6738P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.6738P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7111345