Synthesis of the Ferrocene Derivative FcCHN(CH~2~)~2~SH [Fc = (η5-C~5~H~5~)Fe(η5-C~5~H~4~)]: Reactivity toward (Phosphine)gold(I) Cations
Eva M. Barranco; M. Concepción Gimeno; Peter G. Jones; Antonio Laguna; M. Dolores Villacampa; Inorganic Chemistry 38 (1999) 702–706; doi:10.1021/ic980379e

data_4321783
_publ_section_title
;
 Synthesis of the Ferrocene Derivative FcCHN(CH~2~)~2~SH [Fc =
 (\h5-C~5~H~5~)Fe(\h5-C~5~H~4~)]: Reactivity toward (Phosphine)gold(I)
 Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              702
_journal_page_last               706
_journal_paper_doi               10.1021/ic980379e
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C74 H69 Au3 Cl10 F6 Fe N O6 P3 S3'
_chemical_formula_weight         2372.64
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.367(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   60.200(6)
_cell_length_b                   14.977(2)
_cell_length_c                   19.066(3)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      4.9
_cell_volume                     17007(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w-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  0.0618
_diffrn_reflns_av_sigmaI/netI    0.1777
_diffrn_reflns_limit_h_max       64
_diffrn_reflns_limit_h_min       -64
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11580
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.834
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.393
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             9184
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.278
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.776
_refine_ls_goodness_of_fit_obs   0.977
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     581
_refine_ls_number_reflns         10792
_refine_ls_number_restraints     395
_refine_ls_restrained_S_all      0.813
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.1192
_refine_ls_R_factor_obs          0.0520
_refine_ls_shift/esd_max         -0.023
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1050
_refine_ls_wR_factor_obs         0.0918
_reflns_number_observed          5462
_reflns_number_total             10792
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980379e.cif
_cod_data_source_block           rust
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0357P)^2^] 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^)+(0.0357P)^2^]
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        17007.1(39)
_cod_database_code               4321783