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_7130447
_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         'C54 H55 As2 N'
_chemical_formula_sum            'C54 H55 As2 N'
_chemical_formula_weight         867.83
_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
_audit_creation_date             2022-07-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-21 deposited with the CCDC.	2022-07-29 downloaded from the CCDC.
;
_cell_angle_alpha                98.509(3)
_cell_angle_beta                 99.330(4)
_cell_angle_gamma                102.359(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2536(14)
_cell_length_b                   11.3183(14)
_cell_length_c                   20.673(2)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.32
_cell_volume                     2492.1(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 n/a (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0542
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            77651
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.275
_diffrn_reflns_theta_min         1.891
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1285 before and 0.0674 after correction.
The Ratio of minimum to maximum transmission is 0.8748.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       plank
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.206
_exptl_crystal_size_min          0.156
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         11181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0386P)^2^+1.2775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9318
_reflns_number_total             11181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03237f2.cif
_cod_data_source_block           2_CCDC1
_cod_database_code               7130447
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.586
_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:
 C13(H13), C9(H9), C4(H4), C5(H5), C21(H21), C22(H22), C25(H25), C27(H27),
 C32(H32), C33(H33), C35(H35), C38(H38), C40(H40), C41(H41), C43(H43), C45(H45),
  C47(H47), C48(H48), C49(H49)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C44(H44A,
 H44B,H44C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C)
;
_shelx_res_checksum              50383
_shelx_hkl_checksum              47364
_shelx_fab_checksum              94687
_olex2_submission_special_instructions 'No special instructions were received'