A New Route to the Synthesis of Phosphine-Substituted Diiron Aza- and Oxadithiolate Complexes
He, Jiao; Deng, Cheng-Long; Li, Yao; Li, Yu-Long; Wu, Yu; Zou, Li-Ke; Mu, Chao; Luo, Qiang; Xie, Bin; Wei, Jian; Hu, Jing-Wen; Zhao, Pei-Hua; Zheng, Wen; Organometallics 36 (2017) 1322–; doi:10.1021/acs.organomet.7b00040

data_4087288
_publ_section_title
;
 A New Route to the Synthesis of Phosphine-Substituted Diiron Aza- and
 Oxadithiolate Complexes
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1322
_journal_paper_doi               10.1021/acs.organomet.7b00040
_journal_volume                  36
_journal_year                    2017
_chemical_formula_sum            'C25 H16 F3 Fe2 O6 P S2'
_chemical_formula_weight         676.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_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                102.405(3)
_cell_angle_beta                 94.178(3)
_cell_angle_gamma                96.563(3)
_cell_formula_units_Z            2
_cell_length_a                   8.269(2)
_cell_length_b                   9.059(3)
_cell_length_c                   18.252(5)
_cell_measurement_reflns_used    6103
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.7076
_cell_measurement_theta_min      2.2967
_cell_volume                     1319.9(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  bruker-CCD
_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  0.0276
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9086
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_T_max  0.8095
_exptl_absorpt_correction_T_min  0.7894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0322P)^2^+2.0547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                4057
_reflns_number_total             4606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00040_si_002.cif
_cod_data_source_block           10
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C25 H16 F3 Fe2  O6 P S2'
_cod_database_code               4087288