Synthesis and Reactions of Novel Triply Thiolate-Bridged Diiron Complexes [Cp*Fe(μ2-SR)3FeCp*] (Cp*= η5-C5Me5; R = Et, Ph)
Chen, Yanhui; Zhou, Yuhan; Qu, Jingping; Organometallics 27 (2008) 666–; doi:10.1021/om0611148

data_4070524
_publ_section_title
;
 Synthesis and Reactions of Novel Triply Thiolate-Bridged Diiron Complexes
 [Cp*Fe(\m2-SR)3FeCp*] (Cp*= \h5-C5Me5; R = Et, Ph)
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              666
_journal_paper_doi               10.1021/om0611148
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C31 H54 Fe2 N S3'
_chemical_formula_weight         648.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.452(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1039(9)
_cell_length_b                   33.854(3)
_cell_length_c                   11.6173(11)
_cell_measurement_reflns_used    5693
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.10
_cell_measurement_theta_min      2.18
_cell_volume                     3451.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21026
_diffrn_reflns_theta_full        23.39
_diffrn_reflns_theta_max         23.39
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  23.39
_exptl_absorpt_correction_T_min  1.92
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+3.4545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                4124
_reflns_number_total             4978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0611148-file005.cif
_cod_data_source_block           ds1
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3451.0(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070524