Synthesis of the Cationic Silyleneiron Complex [(.eta.-C5H5)Fe(CO)2:SiMe{2-(Me2NCH2)C6H4}]PF6 by Hydride Abstraction from a (Hydrosilyl)iron Complex with Ph3CPF6
Kobayashi, Hideki; Ueno, Keiji; Ogino, Hiroshi; Organometallics 14 (1995) 5490–; doi:10.1021/om00012a014

data_4078347
_publ_section_title
;
 Synthesis of the Cationic Silyleneiron Complex
 [(.eta.-C5H5)Fe(CO)2:SiMe{2-(Me2NCH2)C6H4}]PF6 by Hydride Abstraction
 from a (Hydrosilyl)iron Complex with Ph3CPF6
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              5490
_journal_paper_doi               10.1021/om00012a014
_journal_volume                  14
_journal_year                    1995
_chemical_formula_moiety         'C17 H20 Fe N O2 Si 1+, F6 P 1-'
_chemical_formula_structural
'(Fe (C5 H5) (C O)2 Si (C H3) (C9 H12 N)) (P F6)''
_chemical_formula_sum            'C17 H20 F6 Fe N O2 P Si'
_chemical_formula_weight         499.25
_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                104.94(2)
_cell_angle_beta                 102.778(14)
_cell_angle_gamma                79.516(13)
_cell_formula_units_Z            2
_cell_length_a                   9.4771(14)
_cell_length_b                   13.267(2)
_cell_length_c                   8.8592(14)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      12.5
_cell_volume                     1040.3(3)
_computing_cell_refinement       URLAP2
_computing_data_reduction        'LP-F2 & DCLT4'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_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       'Rigaku AFC-6A'
_diffrn_measurement_method       '2theta/omega scans'
_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    0.1103
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7524
_diffrn_reflns_theta_max         32.49
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       'Transparent blocks'
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.120
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         7521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.1662
_refine_ls_R_factor_obs          0.0637
_refine_ls_shift/esd_max         0.027
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+0.0195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1846
_refine_ls_wR_factor_obs         0.1399
_reflns_number_observed          3647
_reflns_number_total             7524
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om5490.cif
_cod_data_source_block           silyleneiron(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0774P)^2^+0.0195P] 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^)+(0.0774P)^2^+0.0195P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4078347