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_7130445
_publ_section_title
;
 A Diarsene Radical Anion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03237F
_journal_year                    2022
_chemical_formula_moiety
'C52 H58.5 As2 O, C18 H36 K N2 O6, 0.5(C4 H10 O)'
_chemical_formula_sum            'C72 H99.5 As2 K N2 O7.5'
_chemical_formula_weight         1301.97
_chemical_name_systematic        '[K{crypt.222}][MesTer2As2(EtO(CH)(CH2))]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     dual
_audit_creation_date             2022-05-24
_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                81.2590(10)
_cell_angle_beta                 73.0790(10)
_cell_angle_gamma                86.2510(10)
_cell_formula_units_Z            2
_cell_length_a                   13.0764(3)
_cell_length_b                   16.9176(4)
_cell_length_c                   18.5206(4)
_cell_measurement_reflns_used    55190
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      0.910
_cell_measurement_theta_min      0.724
_cell_volume                     3873.28(15)
_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      150.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII Duo'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_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       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55190
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.691
_diffrn_reflns_theta_max         66.691
_diffrn_reflns_theta_min         2.518
_exptl_absorpt_coefficient_mu    1.918
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS, APEX2 was used for absorption correction'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       plate
_exptl_crystal_F_000             1381
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         13657
_refine_ls_number_restraints     1002
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0526
_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^)+(0.1071P)^2^+1.1476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11573
_reflns_number_total             13657
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03237f2.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C72 H99.50 As2 K N2 O7.50'
_cod_database_code               7130445
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.724
_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. Restrained distances
 C51A-C52A
 1.5 with sigma of 0.1
 O1-C50 = O1A-C50A
 1.43 with sigma of 0.01
 C71-C72 = C74-C73
 1.5 with sigma of 0.01
 C49-C50
 1.5 with sigma of 0.01
 O8-C72 = O8-C73
 1.43 with sigma of 0.01
 O8-C73 = O8-C72
 1.43 with sigma of 0.001
 C51-C52 = C51A-C52A
 1.5 with sigma of 0.01
 O1-C51 = O1A-C51A
 1.43 with sigma of 0.01
 As1-C50 \\sim As1-C50A
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C49A \\sim C49 \\sim C50A \\sim C50 \\sim O1 \\sim O1A \\sim C51 \\sim C51A
\\sim C52A \\sim C52: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.005 within 2A
C72 \\sim C71 \\sim O8 \\sim C73 \\sim C74: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(O1) = Uanis(O1A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 C74, O8, C72, C73, C71, H73A, H73B, H71A, H71B, H71C, H74A, H74B, H74C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Fixed Sof: O8(0.5) C52(0.5) H52A(0.5) H52B(0.5) H52C(0.5) C50A(0.5) H50A(0.5)
 C50(0.5) H50(0.5) O1(0.5) O1A(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5)
 C49A(0.5) H49D(0.5) H49E(0.5) H49F(0.5) C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5)
 C72(0.5) H72A(0.5) H72B(0.5) C73(0.5) H73A(0.5) H73B(0.5) C74(0.5) H74A(0.5)
 H74B(0.5) H74C(0.5) C51(0.5) H51A(0.5) H51B(0.5) C51A(0.5) H51C(0.5) C52A(0.5)
 H52D(0.5) H52E(0.5) H52F(0.5)
6.a Everything fixed:
 C50A, C50
6.b Ternary CH refined with riding coordinates:
 C50A(H50A), C50(H50)
6.c Secondary CH2 refined with riding coordinates:
 C62(H62A,H62B), C61(H61A,H61B), C59(H59A,H59B), C60(H60A,H60B), C53(H53A,
 H53B), C54(H54A,H54B), C58(H58A,H58B), C57(H57A,H57B), C56(H56A,H56B),
 C55(H55A,H55B), C70(H70A,H70B), C63(H63A,H63B), C67(H67A,H67B), C64(H64A,H64B),
  C65(H65A,H65B), C69(H69A,H69B), C66(H66A,H66B), C68(H68A,H68B), C72(H72A,
 H72B), C73(H73A,H73B), C51(H51A,H51B)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C18(H18), C5(H5), C44(H44), C9(H9), C20(H20), C27(H27),
 C42(H42), C28(H28), C29(H29), C11(H11), C33(H33), C35(H35), C51A(H51C)
6.e Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C13(H13A,H13B,H13C), C37(H37A,H37B,H37C), C22(H22A,H22B,
 H22C), C46(H46A,H46B,H46C), C23(H23A,H23B,H23C), C38(H38A,H38B,H38C), C24(H24A,
 H24B,H24C), C15(H15A,H15B,H15C), C47(H47A,H47B,H47C), C14(H14A,H14B,H14C),
 C39(H39A,H39B,H39C), C52(H52A,H52B,H52C), C49(H49A,H49B,H49C), C49A(H49D,H49E,
 H49F), C71(H71A,H71B,H71C), C74(H74A,H74B,H74C), C52A(H52D,H52E,H52F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60083
_shelx_hkl_checksum              35398
_shelx_fab_checksum              38228
_olex2_submission_special_instructions 'No special instructions were received'