Unusual formation of a hex-3-ene-1,5-diyne-3-yl ligand from a buta-1,3-diyne in the Cp*2TiCl2‒Mg system
Pellny, Paul-Michael; Kirchbauer, Frank G.; Burlakov, Vladimir V.; Spannenberg, Anke; Rosenthal, Uwe; Chemical Communications  (1999) 2505–; doi:10.1039/a906777i

data_7110699
_publ_section_title
;
 Unusual formation of a hex-3-ene-1,5-diyne-3-yl ligand from a
 buta-1,3-diyne in the Cp*2TiCl2--Mg system
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2505
_journal_paper_doi               10.1039/a906777i
_journal_year                    1999
_chemical_formula_sum            'C35 H57 Si3 Ti'
_chemical_formula_weight         609.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                98.92(3)
_cell_angle_beta                 92.62(3)
_cell_angle_gamma                90.55(3)
_cell_formula_units_Z            2
_cell_length_a                   10.034(2)
_cell_length_b                   11.487(2)
_cell_length_c                   16.326(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     1856.8(6)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5556
_diffrn_reflns_theta_max         24.26
_diffrn_reflns_theta_min         1.79
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_type   no
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_description       prism
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.186
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_restrained_S_obs      1.186
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_obs          0.0598
_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^)+(0.0810P)^2^+1.0065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1605
_refine_ls_wR_factor_obs         0.1522
_reflns_number_observed          4084
_reflns_number_total             5556
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            906777isup1.cif
_cod_data_source_block           209
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+1.0065P] 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^)+(0.0810P)^2^+1.0065P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110699