Synthesis and characterisation of a very low-coordinate diferrous [2Fe-2S]<sup>0</sup> unit.
Schneider, Christian; Groß, Sophie J; Demeshko, Serhiy; Bontemps, Sébastien; Meyer, Franc; Werncke, C. Gunnar; Chemical communications (Cambridge, England) 57 (2021) 10751–10754; doi:10.1039/d1cc04196g

data_7129041
_publ_section_title
;
 Synthesis and characterisation of a very low-coordinate diferrous
 [2Fe-2S]<sup>0</sup> unit.
;
_journal_issue                   82
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10751
_journal_page_last               10754
_journal_paper_doi               10.1039/d1cc04196g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C24 H72 Fe2 N4 S2 Si8, 2(C12 H24 K O6), 0.5(C4 H10 O)'
_chemical_formula_sum            'C50 H125 Fe2 K2 N4 O12.5 S2 Si8'
_chemical_formula_weight         1461.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-07-20
_audit_creation_method
;
FinalCif V85 by Daniel Kratzert, Freiburg 2021,
https://github.com/dkratzert/FinalCif
;
_audit_update_record
;
2021-07-20 deposited with the CCDC.	2021-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                96.877(2)
_cell_angle_beta                 100.9140(10)
_cell_angle_gamma                102.872(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2287(5)
_cell_length_b                   13.8939(6)
_cell_length_c                   24.4874(10)
_cell_measurement_reflns_used    9724
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.98
_cell_measurement_theta_min      2.48
_cell_volume                     3925.2(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            123101
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.008
_diffrn_reflns_theta_min         2.096
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1621 before and 0.0630 after correction. The Ratio of minimum to maximum transmission is 0.8933. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1574
_exptl_crystal_size_max          0.561
_exptl_crystal_size_mid          0.372
_exptl_crystal_size_min          0.359
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         20844
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+2.4835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16385
_reflns_number_total             20844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04196g2.cif
_cod_data_source_block           FeIII_2S2_2
_cod_depositor_comments
'Adding full bibliography for 7129039--7129041.cif.'
_cod_original_formula_sum        'C50 H125 Fe2 K2 N4 O12.50 S2 Si8'
_cod_database_code               7129041
_shelx_shelxl_version_number     2018/1
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.694
_shelx_estimated_absorpt_t_max   0.787
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O00V-C02A \\sim O00V-C02B
 with sigma of 0.02
 C028-C02A \\sim C0-C02B
 with sigma of 0.02
 O00V-C028 \\sim O00V-C0
 with sigma of 0.04
3. Others
 Sof(C02B)=Sof(H02V)=Sof(H02W)=Sof(C0)=Sof(H0A)=Sof(H0B)=Sof(H0C)=1-FVAR(1)
 Sof(C028)=Sof(H02Q)=Sof(H02R)=Sof(H02S)=Sof(C02A)=Sof(H02T)=Sof(H02U)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C017(H9AA,H), C018(H0BA,HA), C01A(H1BA,HB), C01C(H2BA,HE), C01K(H3BA,HT),
 C01M(H4BA,HW), C01O(H5BA,HZ), C01P(H6BA,H5CA), C01Q(H7BA,H6CA), C01S(H8BA,
 H9CA), C01T(H9BA,H0DA), C01U(H0CA,H1DA), C01V(H1CA,H2DA), C01X(H2CA,H5DA),
 C01Y(H3CA,H6DA), C01Z(H4CA,H7DA), C020(H02A,H02B), C021(H02C,H02D), C022(H02E,
 H02F), C023(H02G,H02H), C024(H02I,H02J), C025(H02K,H02L), C026(H02M,H02N),
 C027(H02O,H02P), C02A(H02T,H02U), C02B(H02V,H02W)
4.b Idealised Me refined as rotating group:
 C00W(H00A,H00B,H00C), C00X(H00D,H00E,H00F), C00Y(H00G,H00H,H00I), C00Z(H00J,
 H00K,H00L), C010(H01A,H01B,H01C), C011(H01D,H01E,H01F), C012(H01G,H01H,H01I),
 C013(H01J,H01K,H01L), C014(H01M,H01N,H01O), C015(H01P,H01Q,H01R), C016(H01S,
 H01T,H01U), C019(H01V,H01W,H01X), C01B(H01Y,HC,HD), C01D(H01Z,HF,HG), C01E(H01,
 HH,HI), C01F(H0AA,HJ,HK), C01G(H1AA,HL,HM), C01H(H2AA,HN,HO), C01I(H3AA,HP,HQ),
  C01J(H4AA,HR,HS), C01L(H5AA,HU,HV), C01N(H6AA,HX,HY), C01R(H7AA,H7CA,H8CA),
 C01W(H8AA,H3DA,H4DA), C028(H02Q,H02R,H02S), C0(H0A,H0B,H0C)
;