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_7130448
_publ_section_title
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 A Diarsene Radical Anion
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03237F
_journal_year                    2022
_chemical_formula_moiety         'C60 H74 As2 K O6'
_chemical_formula_sum            'C60 H74 As2 K O6'
_chemical_formula_weight         1080.13
_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                69.008(2)
_cell_angle_beta                 67.573(2)
_cell_angle_gamma                82.513(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2440(5)
_cell_length_b                   11.7593(6)
_cell_length_c                   11.8985(6)
_cell_measurement_reflns_used    9664
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      2.20
_cell_volume                     1357.69(12)
_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 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0419
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 1.000
_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       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            81354
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.678
_diffrn_reflns_theta_min         1.959
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1158 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.9081.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       plate
_exptl_crystal_F_000             567
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.055
_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     319
_refine_ls_number_reflns         6960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0250P)^2^+0.7823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6263
_reflns_number_total             6960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03237f2.cif
_cod_data_source_block           1sym
_cod_database_code               7130448
_shelx_shelxl_version_number     2016/6
_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 Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C39(H39), C44(H44), C48(H48), C49(H49), C51(H51), C54(H54)
2.c Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C52(H52A,H52B,H52C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              33586
_shelx_hkl_checksum              72610
_olex2_submission_special_instructions 'No special instructions were received'