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_7060931
_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         'C31 H23 Fe2 O6 P S2'
_chemical_formula_sum            'C31 H23 Fe2 O6 P S2'
_chemical_formula_weight         698.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2019-12-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                96.927(3)
_cell_angle_beta                 92.816(3)
_cell_angle_gamma                115.474(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0226(5)
_cell_length_b                   10.2799(6)
_cell_length_c                   17.7088(11)
_cell_measurement_reflns_used    7937
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.34
_cell_measurement_theta_min      2.22
_cell_volume                     1462.63(15)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26250
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.428
_diffrn_reflns_theta_min         2.222
_exptl_absorpt_coefficient_mu    1.233
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0762 before and 0.0583 after correction. The Ratio of minimum to maximum transmission is 0.3696. 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    1.586
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.6892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4494
_reflns_number_total             6000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03398k2.cif
_cod_data_source_block           mo_1231_5_0m
_cod_depositor_comments
'Adding full bibliography for 7060931--7060934.cif.'
_cod_database_code               7060931
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.846
_shelx_estimated_absorpt_t_min   0.740
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31)
;
_shelx_res_checksum              49595
_olex2_submission_special_instructions 'No special instructions were received'