Phosphine-substituted diiron complexes Fe2(μ-Rodt)(CO)6−n(PPh3)n (R = Ph, Me, H and n = 1, 2) featuring desymmetrized oxadithiolate bridges: structures, protonation, and electrocatalysis
Gu, Xiao-Li; Li, Jian-Rong; Jin, Bo; Guo, Yang; Jing, Xing-Bin; Zhao, Pei-Hua; New Journal of Chemistry 45 (2021) 17996–18007; doi:10.1039/D1NJ03398K

data_7060934
_publ_section_title
;
 Phosphine-substituted diiron complexes Fe2(\m-Rodt)(CO)6&#x2212;n(PPh3)n
 (R = Ph, Me, H and n = 1, 2) featuring desymmetrized oxadithiolate
 bridges: structures, protonation, and electrocatalysis
;
_journal_issue                   38
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17996
_journal_page_last               18007
_journal_paper_doi               10.1039/D1NJ03398K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C43 H36 Fe2 O5 P2 S2'
_chemical_formula_sum            'C43 H36 Fe2 O5 P2 S2'
_chemical_formula_weight         870.532
_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_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-03-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                77.746(3)
_cell_angle_beta                 89.450(3)
_cell_angle_gamma                70.192(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2488(6)
_cell_length_b                   13.4812(8)
_cell_length_c                   17.0713(11)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.35
_cell_volume                     1952.5(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.9890
_diffrn_measured_fraction_theta_max 0.9865
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.9890
_diffrn_reflns_Laue_measured_fraction_max 0.9865
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32807
_diffrn_reflns_point_group_measured_fraction_full 0.9890
_diffrn_reflns_point_group_measured_fraction_max 0.9865
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         2.26
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  0.0277
_exptl_absorpt_correction_T_min  0.0096
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0806 before and 0.0576 after correction. The Ratio of minimum to maximum transmission is 0.3466. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             898.697
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.1564
_refine_diff_density_min         -0.7433
_refine_diff_density_rms         0.1155
_refine_ls_d_res_high            0.7974
_refine_ls_d_res_low             9.0141
_refine_ls_goodness_of_fit_ref   1.0347
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    75
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0347
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.1047
_refine_ls_shift/su_mean         0.0016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+1.7831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1271
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                5696
_reflns_number_total             7955
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj03398k2.cif
_cod_data_source_block           mo_0116_2_0m
_cod_depositor_comments
'Adding full bibliography for 7060931--7060934.cif.'
_cod_database_code               7060934
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'