Reaction of B(C6F5)3 with zirconium and hafnium benzyl diene complexes. The crystal and molecular structures of Cp″Zr(C6F5){η4-CH2CMeCHCHB(C6F5)2} and [Cp″Hf(2,3-Me2C4H4)(OEt2)][PhCH2B(C6F5)3] [Cp″ = 1,3-(SiMe3)2C5H3]
Pindado, Gerardo Jiménez; Thornton-Pett, Mark; Hursthouse, Michael B.; Coles, Simon J.; Bochmann, M.; Journal of the Chemical Society, Dalton Transactions  (1999) 1663–; doi:10.1039/a901347d

data_7027322
_publ_section_title
;
 Reaction of B(C6F5)3 with zirconium and hafnium benzyl diene complexes.
 The crystal and molecular structures of
 Cp&#x2033;Zr(C6F5){\h4-CH2CMeCHCHB(C6F5)2} and
 [Cp&#x2033;Hf(2,3-Me2C4H4)(OEt2)][PhCH2B(C6F5)3]
 [Cp&#x2033;&#x2005;=&#x2005;1,3-(SiMe3)2C5H3]
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1663
_journal_paper_doi               10.1039/a901347d
_journal_year                    1999
_chemical_formula_sum            'C46 H48 B F15 Hf O Si2'
_chemical_formula_weight         1147.32
_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_date             97-05-23
_audit_creation_method           'STADI4, X-RED'
_cell_angle_alpha                104.763(10)
_cell_angle_beta                 94.315(11)
_cell_angle_gamma                103.276(10)
_cell_formula_units_Z            2
_cell_length_a                   11.1910(15)
_cell_length_b                   13.1465(15)
_cell_length_c                   17.506(2)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      14.9
_cell_volume                     2399.3(5)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 2.05 - 2.20, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_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    0.0133
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8418
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.66
_diffrn_standards_decay_%        5.0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.317
_exptl_absorpt_correction_T_max  0.4930
_exptl_absorpt_correction_T_min  0.2493
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.49  

    H   K   L   2Theta   Chi   Imin/Imax
   -2  -3   1    13.5   -84.5    0.504
    2   3  -1    13.5    84.5    0.491
    3   5  -3    21.7    86.4    0.534
   -3  -5   3    21.7   -86.4    0.555
   -3  -6   4    24.6   -81.8    0.564
    3   6  -4    24.6    81.8    0.539
   -4  -7   4    29.9   -86.6    0.533
    4   7  -4    29.9    86.6    0.526
    5   8  -4    35.5    89.8    0.519
   -5  -8   4    35.5   -89.8    0.523
   -6  -8   3    38.5   -84.0    0.525
    6   8  -3    38.5    84.0    0.527
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.417
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         8418
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0202
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+2.4073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0465
_refine_ls_wR_factor_ref         0.0483
_reflns_number_gt                7965
_reflns_number_total             8418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            901347dsup1.cif
_cod_data_source_block           MB19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+2.4073P] 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^)+(0.0210P)^2^+2.4073P] 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               7027322
_audit_contact_author            'J. Richter'