Unexpected Synthesis of Tetrahedral Fe/S Clusters via Highly Reactive Butterfly Intermediates (μ-HS)2Fe2(CO)5[RP(CH2OH)2]
Song, Li-Cheng; Zhao, Pei-Hua; Du, Zong-Qiang; Tang, Ming-Yi; Hu, Qing-Mei; Organometallics 29 (2010) 5751–; doi:10.1021/om100793d

data_4067045
_publ_section_title
;
 Unexpected Synthesis of Tetrahedral Fe/S Clusters via Highly Reactive
 Butterfly Intermediates (\m-HS)2Fe2(CO)5[RP(CH2OH)2]
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5751
_journal_paper_doi               10.1021/om100793d
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C18.50 H18 Cl Fe3 O7 P S2'
_chemical_formula_sum            'C18.5 H18 Cl Fe3 O7 P S2'
_chemical_formula_weight         650.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.729(4)
_cell_length_b                   8.5970(10)
_cell_length_c                   18.939(3)
_cell_measurement_reflns_used    13263
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      1.40
_cell_volume                     4840.4(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD camera'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36601
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         1.37
_exptl_absorpt_coefficient_mu    2.161
_exptl_absorpt_correction_T_max  0.9185
_exptl_absorpt_correction_T_min  0.8129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.273
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5775
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.283
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+10.6368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1052
_reflns_number_gt                5536
_reflns_number_total             5775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100793d_si_001.cif
_cod_data_source_block           shelxl
_cod_original_formula_sum        'C18.50 H18 Cl Fe3 O7 P S2'
_cod_database_code               4067045