CO substitution by PPh<sub>3</sub> in Fe<sub>2</sub>S<sub>2</sub>(CO)<sub>6</sub> proceeds via a novel Fe<sub>2</sub>S intermediate.
Zhang, Fanjun; Woods, Toby J.; Rauchfuss, Thomas B.; Arrigoni, Federica; Zampella, Giuseppe; Chemical communications (Cambridge, England) 57 (2021) 5079–5081; doi:10.1039/d1cc00956g

data_7128173
_publ_section_title
;
 CO substitution by PPh<sub>3</sub> in
 Fe<sub>2</sub>S<sub>2</sub>(CO)<sub>6</sub> proceeds via a novel
 Fe<sub>2</sub>S intermediate.
;
_journal_issue                   41
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5079
_journal_page_last               5081
_journal_paper_doi               10.1039/d1cc00956g
_journal_volume                  57
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C42 H31 Fe2 O6 P2 S, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C44 H33 Cl2 F3 Fe2 O9 P2 S2'
_chemical_formula_weight         1071.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'dual space'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-17 deposited with the CCDC.	2021-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.9842(7)
_cell_length_b                   18.0922(7)
_cell_length_c                   15.4453(6)
_cell_measurement_reflns_used    99880
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.64
_cell_volume                     5025.5(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 V2018.7-2 (Bruker, 2018)'
_computing_data_reduction
; 
SAINT V8.38A, XPREP v2014/2, (Bruker, 2018), SADABS V2016/2 
(Krause et al., 2015) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2018), CrystalMaker v9.2.8 (CrystalMaker, 2016) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2018)'
_computing_structure_refinement  'SHELXL-2018-3 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT-2014-5 (Sheldrick, 2015b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Bruker D8 Venture/Photon II'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ed73gs_sq
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            177132
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.295
_diffrn_reflns_theta_min         2.251
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Krause et al., 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2176
_exptl_crystal_id                ed73gs_sq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Paratone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (6 3 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.064
_platon_squeeze_details
;
SQUEEZE removed a total of 92 electrons from each of two symmetry-
equivalent voids in the P1 cell, consistent with multiple acetonitrile
molecules in each void space.
;
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack (1983),  2998 Friedels'
_refine_ls_abs_structure_Flack   0.28(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6229
_refine_ls_number_restraints     472
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0638P)^2^+10.5710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6186
_reflns_number_total             6229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc00956g2.cif
_cod_data_source_block           ed73gs_sq
_cod_depositor_comments
'Adding full bibliography for 7128173--7128175.cif.'
_cod_database_code               7128173
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.681
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              71837
_shelx_hkl_checksum              55046
_shelx_fab_checksum              92867
_platon_squeeze_void_probe_radius 1.20