The crystal structure of pentakis(carbonyl)-{μ-[2,3-bis(sulfanyl)propan-1-olato]}-(triphenylphosphane)diiron (Fe–Fe)C26H21Fe2O6PS2
Gao, Wei; Bai, Yan-Jie; Mao, Jia-Le; Guo, Xue-Quan; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 587–589; doi:10.1515/ncrs-2021-0003

data_8104774
_publ_section_title
;
 The crystal structure of
 pentakis(carbonyl)-{\m-[2,3-bis(sulfanyl)propan-1-olato]}-(triphenylphosphane)diiron
 (Fe--Fe)C26H21Fe2O6PS2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              587
_journal_page_last               589
_journal_paper_doi               10.1515/ncrs-2021-0003
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C26 H21 Fe2 O6 P S2'
_chemical_formula_sum            'C26 H21 Fe2 O6 P S2'
_chemical_formula_weight         636.22
_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                 106.409(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0892(6)
_cell_length_b                   27.6631(18)
_cell_length_c                   11.3409(8)
_cell_measurement_reflns_used    9877
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      2.38
_cell_volume                     2735.4(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009) [1]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009) [1]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015) [2]'
_computing_structure_solution    'ShelXS (Sheldrick, 2008) [3]'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 QUEST CCD'
_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  0.0897
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            63350
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.067
_diffrn_reflns_theta_max         25.067
_diffrn_reflns_theta_min         2.449
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1397 before and 0.0629 after correction. The Ratio of minimum to maximum transmission is 0.8716. 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    1.545
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.461
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4837
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0491P)^2^+11.5614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1620
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3418
_reflns_number_total             4837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0003_suppl.cif
_cod_data_source_block           20190703c_0m
_cod_database_code               8104774
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.679
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Rigid bond restraints
 O6, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Others
 Sof(O6A)=Sof(H6A)=Sof(H8BC)=Sof(H8BD)=1-FVAR(1)
 Sof(O6)=Sof(H6)=Sof(H8AA)=Sof(H8AB)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C7(H7)
4.b Secondary CH2 refined with riding coordinates:
 C6(H6B,H6C), C8(H8AA,H8AB), C8(H8BC,H8BD)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), 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)
4.d Tetrahedral OH refined with riding coordinates:
 O6(H6), O6A(H6A)
;