Synthesis and characterisation of 1-(diphenylphosphino)-1′-(methylsulfanyl)ferrocene and a series of metal (CuI, AgI)‒ferrocenylene complexes
Long, Nicholas J.; Martin, Jeff; Opromolla, Giuliana; White, Andrew J. P.; Williams, David J.; Zanello, Piero; Journal of the Chemical Society, Dalton Transactions  (1999) 1981–; doi:10.1039/a903539g

data_7027523
_publ_section_title
;
 Synthesis and characterisation of
 1-(diphenylphosphino)-1&#x2032;-(methylsulfanyl)ferrocene and a series of
 metal (CuI, AgI)--ferrocenylene complexes
;
_journal_issue                   12
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1981
_journal_paper_doi               10.1039/a903539g
_journal_year                    1999
_chemical_formula_sum            'C24 H28 Cu F6 Fe2 P S4'
_chemical_formula_weight         764.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4930(8)
_cell_length_b                   10.4930(8)
_cell_length_c                   13.3402(11)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      4.98
_cell_volume                     1468.8(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1216
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        5.78
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.083
_exptl_absorpt_correction_T_max  0.5007
_exptl_absorpt_correction_T_min  0.3815
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       Tetrahdra
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(4)
_refine_ls_extinction_coef       0.0051(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.084
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      12.699
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_obs          0.0307
_refine_ls_shift/esd_max         -0.049
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+0.2489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.7055
_refine_ls_wR_factor_obs         0.0781
_reflns_number_observed          1060
_reflns_number_total             1209
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903539gsup1.cif
_cod_data_source_block           NL9605
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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^)+(0.0395P)^2^+0.2489P] 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^)+(0.0395P)^2^+0.2489P] 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      I-4
_cod_original_formula_sum        'C24 H28 S4 Fe2 Cu F6 P'
_cod_database_code               7027523