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_7130449
_publ_section_title
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 A Diarsene Radical Anion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03237F
_journal_year                    2022
_chemical_formula_moiety
'C48 H50 As2, C10 H20 K0.5 O4, C6 H12 K0.5 O3, 2(C4 H8 O)'
_chemical_formula_sum            'C72 H98 As2 K O9'
_chemical_formula_weight         1296.44
_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                91.769(2)
_cell_angle_beta                 92.237(2)
_cell_angle_gamma                98.385(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6616(6)
_cell_length_b                   13.6573(7)
_cell_length_c                   20.3961(9)
_cell_measurement_reflns_used    9413
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.53
_cell_measurement_theta_min      2.27
_cell_volume                     3484.2(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_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  0.0599
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            65832
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.758
_diffrn_reflns_theta_min         2.000
_exptl_absorpt_coefficient_mu    1.072
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0506 after correction.
The Ratio of minimum to maximum transmission is 0.8636.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             1374
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.152
_refine_diff_density_max         1.194
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         17337
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0421P)^2^+3.2405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12314
_reflns_number_total             17337
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03237f2.cif
_cod_data_source_block           1asym
_cod_database_code               7130449
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.854
_shelx_estimated_absorpt_t_min   0.701
_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
C55: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C53: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C55) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C53) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C57) \\sim Ueq, Uanis(C57) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C55) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O7) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Rigid body (RIGU) restrains
 C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C18(H18A,H18B), C20(H20A,H20B), C25(H25A,H25B), C31(H31A,
 H31B), C33(H33A,H33B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B),
 C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B),
  C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,
 H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B),
 C72(H72A,H72B)
4.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C15(H15), C19(H19), C27(H27), C28(H28), C29(H29), C30(H30),
 C34(H34), C36(H36), C37(H37), C38(H38), C43(H43), C46(H46)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C56(H56A,H56B,H56C),
 C62(H62A,H62B,H62C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              69953
_shelx_hkl_checksum              62540
_shelx_fab_checksum              16023
_olex2_submission_special_instructions 'No special instructions were received'