Synthesis, Structure, and Electrocatalysis of Butterfly [Fe2SP] Cluster Complexes Relevant to [FeFe]-Hydrogenases
Song, Li-Cheng; Gu, Zhen-Chao; Zhang, Wei-Wei; Li, Qian-Li; Wang, Yong-Xiang; Wang, Hong-Fa; Organometallics 34 (2015) 4147–; doi:10.1021/acs.organomet.5b00560

data_4086204
_publ_section_title
;
 Synthesis, Structure, and Electrocatalysis of Butterfly [Fe2SP] Cluster
 Complexes Relevant to [FeFe]-Hydrogenases
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4147
_journal_paper_doi               10.1021/acs.organomet.5b00560
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C13 H7 Fe2 O8 P S'
_chemical_formula_sum            'C13 H7 Fe2 O8 P S'
_chemical_formula_weight         465.92
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2013
_cell_angle_alpha                72.272(10)
_cell_angle_beta                 84.076(16)
_cell_angle_gamma                83.405(17)
_cell_formula_units_Z            2
_cell_length_a                   7.9950(13)
_cell_length_b                   8.0320(13)
_cell_length_c                   13.723(2)
_cell_measurement_reflns_used    2965
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      1.60
_cell_volume                     831.7(2)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r4'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r4'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7643
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.894
_diffrn_reflns_theta_min         1.562
_exptl_absorpt_coefficient_mu    2.005
_exptl_absorpt_correction_T_max  0.697
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3916
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0158P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2696
_reflns_number_total             3916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00560_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4086199--4086206.cif.'
_cod_database_code               4086204
_shelx_estimated_absorpt_t_min   0.645
_shelx_estimated_absorpt_t_max   0.714
_shelxl_version_number           2013-2
_shelx_res_checksum              77768
_shelx_hkl_checksum              34262