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_7027524
_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            'C68 H56 Ag B F4 Fe2 P4'
_chemical_formula_weight         1303.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 100.917(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.627(5)
_cell_length_b                   23.575(6)
_cell_length_c                   22.970(6)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.18
_cell_measurement_theta_min      3.98
_cell_volume                     12031(5)
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_sigmaI/netI    0.1381
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8166
_diffrn_reflns_theta_max         59.98
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        17.11
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.840
_exptl_absorpt_correction_T_max  0.9916
_exptl_absorpt_correction_T_min  0.4455
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Orange/yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       Prisms
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.077
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.000068(13)
_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   1.030
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         7886
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      3.801
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.1494
_refine_ls_R_factor_obs          0.0852
_refine_ls_shift/esd_max         -0.012
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1227P)^2^+22.1416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.6861
_refine_ls_wR_factor_obs         0.1970
_reflns_number_observed          4658
_reflns_number_total             7891
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            903539gsup1.cif
_cod_data_source_block           NL9607
_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^)+(0.1227P)^2^+22.1416P] 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^)+(0.1227P)^2^+22.1416P] 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        12030.8(52)
_cod_original_sg_symbol_H-M      I2/a
_cod_original_formula_sum        'C68 H56 B F4 P4 Fe2 Ag'
_cod_database_code               7027524