New SO~2~ Iron-Containing Cluster Compounds [PPN]~2~[Fe~3~(CO)~9~(μ~3~,η^2^-SO~2~)], [PPN]~2~[Fe~3~(CO)~8~(μ-SO2)μ~3~-S], [PPN]~2~[Fe~3~(CO)~8~(μ-SO~2~)(μ~3~-CCO)], and [PPN]~2~[Fe~2~(CO)~6~(μ-SO~2~)~2~] From Heterometal Precursors.
Randal W. Eveland; Casey C. Raymond; T. E. Albrecht-Schmitt; Duward F. Shriver; Inorganic Chemistry 38 (1999) 1282–1287; doi:10.1021/ic980762j

data_4321826
_publ_contact_author_address
; Department of Chemistry
  Northwestern University
  Evanston, IL 60208-3113
;
_publ_contact_author_email       shriver@chem.nwu.edu
_publ_contact_author_fax         '(847) 4917713'
_publ_contact_author_name        'Duward F. Shriver'
_publ_contact_author_phone       '(847) 4915655'
_publ_section_title
;
 New SO~2~ Iron-Containing Cluster Compounds
 [PPN]~2~[Fe~3~(CO)~9~(\m~3~,\h^2^-SO~2~)],
 [PPN]~2~[Fe~3~(CO)~8~(\m-SO2)\m~3~-S],
 [PPN]~2~[Fe~3~(CO)~8~(\m-SO~2~)(\m~3~-CCO)], and
 [PPN]~2~[Fe~2~(CO)~6~(\m-SO~2~)~2~] From Heterometal Precursors.
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1282
_journal_page_last               1287
_journal_paper_doi               10.1021/ic980762j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         'C72 H60 P4 N2 Fe3 C9 O11 S 0.5(C H2 Cl2)'
_chemical_formula_sum            'C81.5 H61 Cl Fe3 N2 O11 P4 S'
_chemical_formula_weight         1603.26
_chemical_name_common            '[PPN]~2~[Fe~3~(CO)~9~(\m~3~,\h^2^-SO~2~)]'
_chemical_name_systematic
; 
Di-(Bis-triphenylphosphonium iminium)(nona-carbonyl-\m~3~,\h^2^-sulfur 
dioxide tri-ferrate)
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 123.3970(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.7648(3)
_cell_length_b                   14.64960(10)
_cell_length_c                   21.7620(3)
_cell_measurement_reflns_used    17937
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      23.21
_cell_measurement_theta_min      1.61
_cell_volume                     7922.27(17)
_computing_cell_refinement       'SAINT-PC (Bruker-AXS, 1997)'
_computing_data_collection       'ASTRO-PC (Siemens, 1996)'
_computing_data_reduction        'SAINT-PC (Bruker-AXS, 1997)'
_computing_molecular_graphics    'SHELXTL-PC (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Siemens SMART-CCD'
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17937
_diffrn_reflns_theta_max         23.21
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  'not reported'
_exptl_absorpt_correction_T_min  'not reported'
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'clear, dark red'
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_meas      ?
_exptl_crystal_description       pyramidal
_exptl_crystal_F_000             3292
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.432
_refine_ls_goodness_of_fit_gt    1.510
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         8713
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/esd_max         0.050
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+4.5634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1250
_refine_ls_wR_factor_gt          0.1180
_reflns_number_observed          7156
_reflns_number_total             8713
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980762j_1.cif
_cod_data_source_block           nu2m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+4.5634P] 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^)+(0.0400P)^2^+4.5634P] 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        7922.27(15)
_cod_original_formula_sum        'C81.50 H61 Cl Fe3 N2 O11 P4 S'
_cod_database_code               4321826