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_7129039
_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         'C36 H80 Fe2 K2 N2 O12 S2 Si4'
_chemical_formula_sum            'C36 H80 Fe2 K2 N2 O12 S2 Si4'
_chemical_formula_weight         1099.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 96.305(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4769(8)
_cell_length_b                   10.6369(6)
_cell_length_c                   20.1652(11)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.17
_cell_volume                     3086.4(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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0457
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            86212
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.180
_diffrn_reflns_theta_min         2.032
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1212 before and 0.0541 after correction. The Ratio of minimum to maximum transmission is 0.8954. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         6845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0418P)^2^+2.6790P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5766
_reflns_number_total             6845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04196g2.cif
_cod_data_source_block           FeII_2_S2_1
_cod_depositor_comments
'Adding full bibliography for 7129039--7129041.cif.'
_cod_database_code               7129039
_shelx_shelxl_version_number     2018/1
_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.a Ternary CH refined with riding coordinates:
 C00J(H00O), C00P(H00Z)
2.b Secondary CH2 refined with riding coordinates:
 C00E(H00D,H00E), C00G(H00I,H00J), C00H(H00K,H00L), C00I(H00M,H00N), C00L(H00S,
 H00T), C00M(H00U,H00V), C00N(H00W,H00X), C00O(H00Y,H), C00R(H0AA,HC),
 C00S(H1AA,HD)
2.c Idealised Me refined as rotating group:
 C00D(H00A,H00B,H00C), C00F(H00F,H00G,H00H), C00K(H00P,H00Q,H00R), C00Q(H00,HA,
 HB), C00T(H2AA,HE,HF), C00U(H3AA,HG,HH)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.911