Investigations on the Active Site Models of [FeFe]-Hydrogenases: Synthesis, Structure, and Properties of N-Functionalized Azadithiolatodiiron Complexes Containing Mono- and Diphosphine Ligands
Song, Li-Cheng; Wang, Hu-Ting; Ge, Jian-Hua; Mei, Shu-Zhen; Gao, Jie; Wang, Liang-Xing; Gai, Bin; Zhao, Li-Qun; Yan, Jing; Wang, Yong-Zhen; Organometallics 27 (2008) 1409–; doi:10.1021/om700956e

data_4070704
_publ_section_title
;
 Investigations on the Active Site Models of [FeFe]-Hydrogenases:
 Synthesis, Structure, and Properties of N-Functionalized
 Azadithiolatodiiron Complexes Containing Mono- and Diphosphine Ligands
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1409
_journal_paper_doi               10.1021/om700956e
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C21 H18 Fe2 N O6 P S2'
_chemical_formula_weight         587.15
_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                 119.186(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.519(2)
_cell_length_b                   17.022(3)
_cell_length_c                   12.706(2)
_cell_measurement_reflns_used    3170
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.21
_cell_volume                     2363.9(7)
_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      294(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13169
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.510
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.670851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.636
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                3192
_reflns_number_total             4799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700956e-file004.cif
_cod_data_source_block           060330d
_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.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed
to 'constr' 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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'NONE' 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_original_cell_volume        2363.8(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4070704