Taming the Stilbene Radical Anion
Sieg, Grégoire; Müller, Igor; Weißer, Kilian; Werncke, Gunnar; Chemical Science  (2022) –; doi:10.1039/D2SC04451J

data_1567938
_publ_section_title
;
 Taming the Stilbene Radical Anion
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04451J
_journal_year                    2022
_chemical_formula_moiety         'C38 H72 Fe K N2 O6 Si4, 0.5(C4 H10 O)'
_chemical_formula_sum            'C40 H77 Fe K N2 O6.5 Si4'
_chemical_formula_weight         897.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-19
_audit_creation_method
;FinalCif V113 by Daniel Kratzert, Freiburg 2022,
https://dkratzert.de/finalcif.html
;
_audit_update_record
;
2022-10-19 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 130.575(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.3486(17)
_cell_length_b                   13.2014(4)
_cell_length_c                   27.113(2)
_cell_measurement_reflns_used    9680
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.261
_cell_measurement_theta_min      2.183
_cell_volume                     10153.9(10)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker BIS V6.2.14/2020-04-30'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            145841
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.978
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  0.7432
_exptl_absorpt_correction_T_min  0.7074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1361 before and 0.0709 after correction.
The Ratio of minimum to maximum transmission is 0.9518.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       plank
_exptl_crystal_F_000             3872
_exptl_crystal_size_max          0.731
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.017
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         9995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+48.3143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8298
_reflns_number_total             9995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04451j2.cif
_cod_data_source_block           3
_cod_original_cell_volume        10154.0(10)
_cod_original_formula_sum        'C40 H77 Fe K N2 O6.50 Si4'
_cod_database_code               1567938
_shelx_shelxl_version_number     2017/1
_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. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C3)
3. Others
 Fixed Sof: H39A(0.5) H39B(0.5) H39C(0.5) C40(0.5) H40A(0.5) H40B(0.5)
 C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C41(0.5) H41A(0.5) H41B(0.5)
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
4.b Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C27(H27A,
 H27B), C37(H37A,H37B), C35(H35A,H35B), C36(H36A,H36B), C28(H28A,H28B),
 C34(H34A,H34B), C33(H33A,H33B), C38(H38A,H38B), C40(H40A,H40B), C41(H41A,H41B)
4.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C13(H13), C12(H12), C10(H10), C4(H4), C5(H5), C7(H7),
 C11(H11), C6(H6)
4.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C25(H25A,
 H25B,H25C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C22(H22A,H22B,H22C),
 C21(H21A,H21B,H21C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_shelx_estimated_absorpt_t_min   0.705
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              32108
_shelx_hkl_checksum              45423