Reactions of permethylmetallocene alkyne complexes of titanium and zirconium with tris(perfluorophenyl)borane
Burlakov, Vladimir V.; Shur, Vladimir B.; Pellny, Paul-Michael; Arndt, Perdita; Baumann, Wolfgang; Spannenberg, Anke; Rosenthal, Uwe; Chemical Communications  (2000) 241–; doi:10.1039/a908591b

data_7110779
_publ_section_title
;
 Reactions of permethylmetallocene alkyne complexes of titanium and
 zirconium with tris(perfluorophenyl)borane
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              241
_journal_paper_doi               10.1039/a908591b
_journal_year                    2000
_chemical_formula_sum            'C49 H44 B F15 Si Zr'
_chemical_formula_weight         1047.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.827(3)
_cell_length_b                   18.862(4)
_cell_length_c                   19.499(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      4
_cell_volume                     4704.6(18)
_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  0.0766
_diffrn_reflns_av_sigmaI/netI    0.1836
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13886
_diffrn_reflns_theta_max         24.29
_diffrn_reflns_theta_min         1.92
_diffrn_standards_interval_time  360
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_type   'MEAN IMAGING PLATE INTENSITY METHOD'
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.304
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.717
_refine_ls_goodness_of_fit_obs   0.936
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         7099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.717
_refine_ls_restrained_S_obs      0.936
_refine_ls_R_factor_all          0.1292
_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^)+(0.0029P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0744
_refine_ls_wR_factor_obs         0.0607
_reflns_number_observed          3131
_reflns_number_total             7099
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908591bsup1.cif
_cod_data_source_block           202
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0029P)^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^)+(0.0029P)^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_sg_symbol_H-M      P2(1)/C
_cod_database_code               7110779