Synthesis and characterisation of three diiron tetracarbonyl complexes related to the diiron centre of [FeFe]-hydrogenase and their protonating, electrochemical investigations
Wang, Yanwei; Li, Zhimei; Zeng, Xianghua; Wang, Xiufeng; Zhan, Caixia; Liu, Yinqiu; Zeng, Xirui; Luo, Qiuyan; Liu, Xiaoming; New Journal of Chemistry 33 (2009) 1780–; doi:10.1039/b903758f

data_7051715
_publ_section_title
;
 Synthesis and characterisation of three diiron tetracarbonyl complexes
 related to the diiron centre of [FeFe]-hydrogenase and their
 protonating, electrochemical investigations
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1780
_journal_paper_doi               10.1039/b903758f
_journal_volume                  33
_journal_year                    2009
_chemical_formula_moiety         'C46 H42 Fe2 N2 O7 P2 S3, 2(H2 O)'
_chemical_formula_sum            'C46 H46 Fe2 N2 O9 P2 S3'
_chemical_formula_weight         1040.70
_chemical_name_systematic
;
?
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.192(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5760(18)
_cell_length_b                   20.7486(18)
_cell_length_c                   17.305(3)
_cell_measurement_reflns_used    3420
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      21.5745
_cell_measurement_theta_min      2.2774
_cell_volume                     4824.8(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_sigmaI/netI    0.1249
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15465
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.853
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         8600
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1609
_reflns_number_gt                4511
_reflns_number_total             8600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903758f.txt
_cod_data_source_block           zz
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               7051715