Novel Addition Reactions of 2,2,7,7-Tetramethyl-3,5-octadiyne to the Methyl Groups of a η5-Pentamethylcyclopentadienyl Ligand
Michal Horáček; Petr Štěpnička; Róbert Gyepes; Ivana Císařová; Miroslav Polášek; Karel Mach; Paul-Michael Pellny; Vladimir V. Burlakov; Wolfgang Baumann; Anke Spannenberg; Uwe Rosenthal; Journal of the American Chemical Society 121 (1999) 10638–10639; doi:10.1021/ja991299s

data_4116575
_publ_contact_author_address
;
      J. Heyrovsk\'y Institute of Physical Chemistry
      Academie of Sciences of the Czech Republic
      Dolej\>skova 3
      18223 Prague 8
      Czech Republic
;
_publ_contact_author_email       mach@jh-inst.cas.cz
_publ_contact_author_fax         '++4202 8582307'
_publ_contact_author_name        'Karel Mach'
_publ_contact_author_phone       '++4202 66053735'
_publ_section_title
;
 Novel Addition Reactions of 2,2,7,7-Tetramethyl-3,5-octadiyne to the
 Methyl Groups of a \h5-Pentamethylcyclopentadienyl Ligand
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10638
_journal_page_last               10639
_journal_paper_doi               10.1021/ja991299s
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C30 H44 Ti'
_chemical_formula_weight         452.55
_chemical_name_systematic
; 
       [3,6-di-tert-butyl-9,10-dimethylbicyclo[6.3.0]undec-4-en-(5-1,8-
       11-dienyl)][ 3: 4-1,2-dimethyl-3,4-
       dimethylenecyclopentenyl]titanium(II) 
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.390(2)
_cell_length_b                   11.8747(8)
_cell_length_c                   18.655(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      12
_cell_volume                     2743.3(6)
_computing_cell_refinement       'Enraf-Nonius CAD4 Version 5.0'
_computing_data_collection       'Enraf-Nonius CAD4 Version 5.0'
_computing_data_reduction        'Jana98 (Petricek, 1998)'
_computing_molecular_graphics    PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
'SIR97(Cascarano al.,ActaCryst.,1996,A52,C-79)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  CAD4-MACHIII
_diffrn_measurement_method       'theta-2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0291
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4511
_diffrn_reflns_theta_full        23.98
_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        2.5
_diffrn_standards_interval_time  1hour
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         4300
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0632P)^2^+0.7508P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                3138
_reflns_number_total             4300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991299s.cif
_cod_data_source_block           tmodv
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0632P)^2^+0.7508P] 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^)+(0.0632P)^2^+0.7508P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4116575