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_7060932
_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         'C48 H38 Fe2 O5 P2 S2'
_chemical_formula_sum            'C48 H38 Fe2 O5 P2 S2'
_chemical_formula_weight         932.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-04-22
_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                90
_cell_angle_beta                 110.0960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3643(5)
_cell_length_b                   18.3822(7)
_cell_length_c                   17.9936(6)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.49
_cell_volume                     4461.9(3)
_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 0.999
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76335
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_min         2.411
_exptl_absorpt_coefficient_mu    0.861
_exptl_absorpt_correction_T_max  0.0276
_exptl_absorpt_correction_T_min  0.0113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0629 before and 0.0573 after correction. The Ratio of minimum to maximum transmission is 0.4094. 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    1.388
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.529
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0742
_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^)+(0.1334P)^2^+8.9565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2205
_refine_ls_wR_factor_ref         0.2419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7250
_reflns_number_total             9129
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03398k2.cif
_cod_data_source_block           mo_0112_1_0m
_cod_depositor_comments
'Adding full bibliography for 7060931--7060934.cif.'
_cod_database_code               7060932
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.770
_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:
 C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48)
;
_shelx_res_checksum              47759
_olex2_submission_special_instructions 'No special instructions were received'