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_4321827
_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         'C36 H30 P2 N Fe2 C6 S2 O10 (C2 H3 N)'
_chemical_formula_sum            'C80 H63 Fe2 N3 O10 P4 S2'
_chemical_formula_weight         1526.03
_chemical_name_common            '[PPN]~2~[Fe~2~(CO)~6~(\m-SO~2~)~2~]'
_chemical_name_systematic
; 
Di-(Bis-triphenylphosphonium iminium)(hexacarbonyl \m-sulfur dioxide diferrate) 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.6914(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0295(5)
_cell_length_b                   26.3564(13)
_cell_length_c                   14.1032(7)
_cell_measurement_reflns_used    24070
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.45
_cell_volume                     3715.6(3)
_computing_cell_refinement       'SAINTPLUS-NT (Bruker-AXS, 1997)'
_computing_data_collection       'ASTRO-NT (Bruker-AXS, 1997)'
_computing_data_reduction        'SAINTPLUS-NT (Bruker-AXS, 1997)'
_computing_molecular_graphics    'SHELXTL-NT (Bruker-AXS, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'BRUKER-AXS SMART-1000 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     0.71069
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0734
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            24070
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  'not reported'
_exptl_absorpt_correction_T_min  'not reported'
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.001
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.477(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         15572
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1137P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1717
_refine_ls_wR_factor_ref         0.1825
_reflns_number_gt                11223
_reflns_number_total             15572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980762j_2.cif
_cod_data_source_block           s28g
_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 
;
_cod_database_code               4321827