Reactivity of Permethylzirconocene and Permethyltitanocene toward Disubstituted 1,3-Butadiynes: η4- vs η2-Complexation or C-C Coupling with the Permethyltitanocene
Paul-Michael Pellny; Frank G. Kirchbauer; Vladimir V. Burlakov; Wolfgang Baumann; Anke Spannenberg; Uwe Rosenthal; Journal of the American Chemical Society 121 (1999) 8313–8323; doi:10.1021/ja991046z

data_4116517
_publ_section_title
;
 Reactivity of Permethylzirconocene and Permethyltitanocene toward
 Disubstituted 1,3-Butadiynes: \h4- vs \h2-Complexation or C-C Coupling
 with the Permethyltitanocene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8313
_journal_page_last               8323
_journal_paper_doi               10.1021/ja991046z
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C37 H40 O2 Ti'
_chemical_formula_weight         564.59
_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                 107.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.064(3)
_cell_length_b                   8.838(2)
_cell_length_c                   21.308(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     3061.4(12)
_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      293(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  0.0485
_diffrn_reflns_av_sigmaI/netI    0.1140
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5945
_diffrn_reflns_theta_max         21.05
_diffrn_reflns_theta_min         1.83
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_type   NO
_exptl_crystal_colour            ORANGE
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.227
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.817
_refine_ls_goodness_of_fit_obs   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         3145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.817
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_obs          0.0452
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0998
_refine_ls_wR_factor_obs         0.0885
_reflns_number_observed          1669
_reflns_number_total             3145
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja991046z_5.cif
_cod_data_source_block           205
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.0000P] 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^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3061.4(10)
_cod_database_code               4116517