A Diarsene Radical Anion
Sieg, Grégoire; Fischer, Malte M.F.; Dankert, Fabian; Siewert, Jan-Erik; Hering-Junghans, Christian; Werncke, Gunnar; Chemical Communications  (2022) –; doi:10.1039/D2CC03237F

data_7130446
_publ_section_title
;
 A Diarsene Radical Anion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03237F
_journal_year                    2022
_chemical_formula_moiety         'C48 H50 As2'
_chemical_formula_sum            'C48 H50 As2'
_chemical_formula_weight         776.72
_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
_audit_creation_date             2022-05-25
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.11 svn.r3635 for OlexSys, GUI svn.r5848)
;
_audit_update_record
;
2022-05-25 deposited with the CCDC.	2022-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                97.97(5)
_cell_angle_beta                 102.80(5)
_cell_angle_gamma                94.98(5)
_cell_formula_units_Z            2
_cell_length_a                   10.701(6)
_cell_length_b                   11.234(7)
_cell_length_c                   22.349(14)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      1.79
_cell_volume                     2575(3)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
 207 frames, detector distance = 110 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0921
_diffrn_reflns_av_unetI/netI     0.1528
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18831
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.844
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  0.8324
_exptl_absorpt_correction_T_min  0.5523
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.485
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.862
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0968P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4741
_reflns_number_total             9186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03237f2.cif
_cod_data_source_block           mester2as2asym
_cod_database_code               7130446
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.879
_shelx_estimated_absorpt_t_min   0.725
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C35(H35), C33(H33), C5(H5), C27(H27), C11(H11), C20(H20), C18(H18), C9(H9),
 C29(H29), C3(H3), C28(H28), C4(H4), C44(H44), C42(H42)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C23(H23A,H23B,
 H23C), C15(H15A,H15B,H15C), C13(H13A,H13B,H13C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C14(H14A,H14B,H14C),
 C47(H47A,H47B,H47C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38086
_shelx_hkl_checksum              13909
_shelx_fab_checksum              45205
_olex2_submission_special_instructions 'No special instructions were received'