Crystal structure of pentacarbonyl-(μ 2-ethane-1,2-dithiolato-κ 4 S:S,S′:S′)-(diphenyl(o-tolyl)phosphine-κ 1 P)diiron (Fe–Fe), C26H21Fe2O5PS2
Bi, Lu-Yan; Liu, Xu-Feng; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 239–241; doi:10.1515/ncrs-2022-0570

data_8107405
_publ_section_title
;
 Crystal structure of pentacarbonyl-(\m 2-ethane-1,2-dithiolato-\k 4
 S:S,S&#x2032;:S&#x2032;)-(diphenyl(o-tolyl)phosphine-\k 1 P)diiron
 (Fe--Fe), C26H21Fe2O5PS2
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              239
_journal_page_last               241
_journal_paper_doi               10.1515/ncrs-2022-0570
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C26 H21 Fe2 O5 P S2'
_chemical_formula_sum            'C26 H21 Fe2 O5 P S2'
_chemical_formula_weight         620.22
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9559(8)
_cell_length_b                   14.1567(6)
_cell_length_c                   9.1976(4)
_cell_measurement_reflns_used    9811
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.42
_cell_volume                     2728.6(2)
_computing_cell_refinement       'SAINT (BRUKER, 2009) [1]'
_computing_data_collection       'APEX2 (BRUKER, 2009) [1]'
_computing_data_reduction        'SADABS (BRUKER, 2009) [1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [3]'
_computing_structure_solution    'ShelXS (Sheldrick, 2008) [4]'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 QUEST CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            35412
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.417
_diffrn_reflns_theta_min         2.418
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5176
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS-2016/2 (Bruker,2016/2) was used for absorption
 correction. wR2(int) was 0.1611 before and 0.0592 after
 correction. The Ratio of minimum to maximum transmission
 is 0.6946. 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    1.510
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.017(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0353P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4749
_reflns_number_total             5002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0570_suppl.cif
_cod_data_source_block           a
_cod_database_code               8107405
_shelx_estimated_absorpt_t_max   0.711
_shelx_estimated_absorpt_t_min   0.609
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.983(13)
 0.017(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              56666
_shelx_hkl_checksum              24888
_olex2_submission_special_instructions 'No special instructions were received'