Synthesis and Structural Characterization of Metallocrown Ethers Containing Butterfly Fe2S2Cluster Cores. Biomimetic Hydrogen Evolution Catalyzed by Fe2(μ-SCH2CH2OCH2CH2S-μ)(CO)6
Song, Li-Cheng; Gao, Jie; Wang, Hu-Ting; Hua, Yu-Juan; Fan, Hong-Tao; Zhang, Xiao-Guang; Hu, Qing-Mei; Organometallics 25 (2006) 5724–; doi:10.1021/om060711r

data_4074503
_publ_section_title
;
 Synthesis and Structural Characterization of Metallocrown Ethers
 Containing Butterfly Fe2S2Cluster Cores. Biomimetic Hydrogen Evolution
 Catalyzed by Fe2(\m-SCH2CH2OCH2CH2S-\m)(CO)6
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5724
_journal_paper_doi               10.1021/om060711r
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C14 H16 Fe2 O9 S2'
_chemical_formula_weight         504.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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-97
_cell_angle_alpha                68.1460(10)
_cell_angle_beta                 68.9940(10)
_cell_angle_gamma                88.697(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3991(10)
_cell_length_b                   14.2960(16)
_cell_length_c                   14.8001(11)
_cell_measurement_temperature    298(2)
_cell_volume                     2072.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11317
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    3.284
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    3.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         9841
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.586
_refine_ls_shift/su_mean         0.099
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.3516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                8048
_reflns_number_total             9841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060711rsi20060925_014106.cif
_cod_data_source_block           000927c
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074503