Synthesis, characterisation and catalytic activity of metal complexes of neutral, unsymmetrical P/S ferrocenediyl ligands
Gibson, Vernon C.; Long, Nicholas J.; White, Andrew J. P.; Williams, Charlotte K.; Williams, David J.; Fontani, Marco; Zanello, Piero; Journal of the Chemical Society, Dalton Transactions  (2002) 3280–; doi:10.1039/b205653d

data_7011909
_publ_section_title
;
 Synthesis, characterisation and catalytic activity of metal complexes
 of neutral, unsymmetrical P/S ferrocenediyl ligands
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3280
_journal_paper_doi               10.1039/b205653d
_journal_year                    2002
_chemical_formula_sum            'C23 H21 Br2 Fe Ni P S'
_chemical_formula_weight         634.81
_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                64.824(10)
_cell_angle_beta                 78.563(7)
_cell_angle_gamma                87.622(11)
_cell_formula_units_Z            4
_cell_length_a                   9.9282(8)
_cell_length_b                   15.880(3)
_cell_length_c                   17.155(2)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      5.36
_cell_volume                     2396.3(6)
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8622
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.887
_exptl_absorpt_correction_T_max  0.4295
_exptl_absorpt_correction_T_min  0.0801
_exptl_absorpt_correction_type   'Face-indexed numerical'
_exptl_crystal_colour            'Dark olive green'
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.57
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.00004(15)
_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   1.010
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7158
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.092
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_obs          0.0487
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1153
_refine_ls_wR_factor_obs         0.0948
_reflns_number_observed          5159
_reflns_number_total             8109
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b205653d.txt
_cod_data_source_block           NL0001
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.0000P] 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^)+(0.0419P)^2^+0.0000P] 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        2396.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C23 H21 P S Br2 Fe Ni'
_cod_database_code               7011909