The crystal structure of tris(carbonyl)-bis(carbonyl)-[μ-propane-1,2- dithiolato]-(benzyldiphenylphosphine)diiron (Fe—Fe), C27H23Fe2O5PS2
Wu, Ming-Gang; Liu, Xu-Feng; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 133–135; doi:10.1515/ncrs-2022-0520

data_8107374
_publ_section_title
;
 The crystal structure of tris(carbonyl)-bis(carbonyl)-[\m-propane-1,2-
 dithiolato]-(benzyldiphenylphosphine)diiron (Fe---Fe), C27H23Fe2O5PS2
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              133
_journal_page_last               135
_journal_paper_doi               10.1515/ncrs-2022-0520
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C27 H23 Fe2 O5 P S2'
_chemical_formula_sum            'C27 H23 Fe2 O5 P S2'
_chemical_formula_weight         634.24
_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
_cell_angle_alpha                90
_cell_angle_beta                 92.9330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3170(5)
_cell_length_b                   16.1774(8)
_cell_length_c                   15.2170(7)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.43
_cell_measurement_theta_min      2.20
_cell_volume                     2782.3(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0426
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            55006
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.094
_diffrn_reflns_theta_max         25.094
_diffrn_reflns_theta_min         2.518
_exptl_absorpt_coefficient_mu    1.285
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;   
 SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
 wR2(int) was 0.0908 before and 0.0520 after correction. The Ratio of
 minimum to maximum transmission is 0.8048. 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    1.514
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4918
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0863P)^2^+3.2729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1636
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3952
_reflns_number_total             4918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0520_suppl.cif
_cod_data_source_block           0m
_cod_database_code               8107374
_shelx_estimated_absorpt_t_max   0.748
_shelx_estimated_absorpt_t_min   0.715
_olex2_refinement_description
;
1. 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
2. Rigid bond restraints
 C7, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Ternary CH refined with riding coordinates:
 C7(H7)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              13461
_shelx_hkl_checksum              92401
_olex2_submission_special_instructions 'No special instructions were received'