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_7129040
_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         'C25 H60 Fe K N2 O6 S3 Si4'
_chemical_formula_sum            'C25 H58 Fe K N2 O6 S3 Si4'
_chemical_formula_weight         786.22
_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                65.2010(10)
_cell_angle_beta                 87.0280(10)
_cell_angle_gamma                83.5690(10)
_cell_formula_units_Z            4
_cell_length_a                   13.1814(7)
_cell_length_b                   17.5638(8)
_cell_length_c                   19.7643(9)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.33
_cell_volume                     4127.6(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Image Plate'
_diffrn_detector_type            'Rigaku Image Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63125
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.113
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0696 before and 0.0609 after correction. The Ratio of minimum to maximum transmission is 0.8857. 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    1.265
_exptl_crystal_description       prism
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         14536
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0691P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9779
_reflns_number_total             14536
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04196g2.cif
_cod_data_source_block           FeIII_CS3_3
_cod_depositor_comments
'Adding full bibliography for 7129039--7129041.cif.'
_cod_database_code               7129040
_shelx_shelxl_version_number     2018/1
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.887
_olex2_diffrn_ambient_temperature_device 'Bruker Kryoflex II'
_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
 Si0I-N2 \\sim Si0J-N2
 with sigma of 0.02
 Si0I-C027 \\sim Si0J-C0
 with sigma of 0.02
 Si0I-C02A \\sim Si0J-C1AA
 with sigma of 0.02
 Si0I-C02B \\sim Si0J-C0AA
 with sigma of 0.02
 N2-C027 \\sim N2-C0
 with sigma of 0.04
 N2-C02A \\sim N2-C1AA
 with sigma of 0.04
 N2-C02B \\sim N2-C0AA
 with sigma of 0.04
 C027-C02A \\sim C0-C1AA
 with sigma of 0.04
 C027-C02B \\sim C0-C0AA
 with sigma of 0.04
 C02A-C02B \\sim C1AA-C0AA
 with sigma of 0.04
 Si0H-N2 \\sim Si0A-N2
 with sigma of 0.02
 Si0H-C028 \\sim Si0A-C2AA
 with sigma of 0.02
 Si0H-C029 \\sim Si0A-C3AA
 with sigma of 0.02
 Si0H-C02C \\sim Si0A-C02D
 with sigma of 0.02
 N2-C028 \\sim N2-C2AA
 with sigma of 0.04
 N2-C029 \\sim N2-C3AA
 with sigma of 0.04
 N2-C02C \\sim N2-C02D
 with sigma of 0.04
 C028-C029 \\sim C2AA-C3AA
 with sigma of 0.04
 C028-C02C \\sim C2AA-C02D
 with sigma of 0.04
 C029-C02C \\sim C3AA-C02D
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C1AA) \\sim Ueq, Uanis(C0AA) \\sim Ueq, Uanis(C0) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C028) \\sim Ueq, Uanis(C02C) \\sim Ueq, Uanis(C029) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C02C) \\sim Ueq, Uanis(C028) \\sim Ueq, Uanis(C029) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2AA) \\sim Ueq, Uanis(C3AA) \\sim Ueq, Uanis(C02D) \\sim Ueq,
Uanis(C028) \\sim Ueq, Uanis(C029) \\sim Ueq, Uanis(C02C) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(Si0H) \\sim Ueq, Uanis(Si0A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N4) \\sim Ueq, Uanis(N3) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C02C, C028, C029
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Si0J)=Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C0)=Sof(H0A)=Sof(H0B)=
 Sof(H0C)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(Si0I)=Sof(C027)=Sof(H02L)=Sof(H02M)=Sof(H02N)=Sof(C02A)=Sof(H02U)=
 Sof(H02V)=Sof(H02W)=Sof(C02B)=Sof(H02X)=Sof(H02Y)=Sof(H9DA)=FVAR(1)
 Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(Si0A)=Sof(C3AA)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=Sof(C02D)=Sof(H02)=Sof(H2EA)=Sof(H3EA)=1-FVAR(2)
 Sof(Si0H)=Sof(C028)=Sof(H02O)=Sof(H02P)=Sof(H02Q)=Sof(C029)=Sof(H02R)=
 Sof(H02S)=Sof(H02T)=Sof(C02C)=Sof(H02Z)=Sof(H0EA)=Sof(H1EA)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C00Z(H00A,H00B), C010(H4AA,H), C013(H01A,H01B), C015(H6AA,HC), C016(H7AA,HD),
 C017(H01C,H01D), C018(H8AA,HE), C019(H9AA,HF), C01A(H01E,H01F), C01B(H0BA,HG),
 C01C(H01G,H01H), C01D(H01I,H01J), C01F(H01K,H01L), C01G(H01M,H01N), C01H(H01O,
 H01P), C01I(H01Q,H01R), C01J(H2BA,HJ), C01N(H4BA,HM), C01O(H01Y,HN), C01Q(H01Z,
 HQ), C01R(H6BA,HR), C01T(H8BA,HU), C01V(H0CA,HX), C026(H02J,H02K)
6.b Idealised Me refined as rotating group:
 C014(H5AA,HA,HB), C01E(H1BA,HH,HI), C01K(H01S,H01T,H01U), C01L(H01V,H01W,
 H01X), C01M(H3BA,HK,HL), C01P(H5BA,HO,HP), C01S(H7BA,HS,HT), C01U(H9BA,HV,HW),
 C01W(H1CA,HY,HZ), C01X(H2CA,H7CA,H8CA), C01Y(H01,H9CA,H0DA), C01Z(H3CA,H1DA,
 H2DA), C020(H4CA,H3DA,H4DA), C021(H5CA,H5DA,H6DA), C022(H02A,H02B,H02C),
 C023(H02D,H02E,H02F), C024(H6CA,H7DA,H8DA), C025(H02G,H02H,H02I), C027(H02L,
 H02M,H02N), C028(H02O,H02P,H02Q), C029(H02R,H02S,H02T), C02A(H02U,H02V,H02W),
 C02B(H02X,H02Y,H9DA), C02C(H02Z,H0EA,H1EA), C0AA(H0AA,H0AB,H0AC), C0(H0A,H0B,
 H0C), C1AA(H1AA,H1AB,H1AC), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC),
 C02D(H02,H2EA,H3EA)
;