Isolation of singlet carbene derived 2-arsa-1,3-butadiene radical cations and dications.
Sharma, Mahendra K.; Blomeyer, Sebastian; Neumann, Beate; Stammler, Hans-Georg; Hinz, Alexander; van Gastel, Maurice; Ghadwal, Rajendra S.; Chemical communications (Cambridge, England) 56 (2020) 3575–3578; doi:10.1039/d0cc00624f

data_7126046
_publ_section_title
;
 Isolation of singlet carbene derived 2-arsa-1,3-butadiene radical cations
 and dications.
;
_journal_issue                   24
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3575
_journal_page_last               3578
_journal_paper_doi               10.1039/d0cc00624f
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C54 H72 As N3, Cl4 Ga'
_chemical_formula_sum            'C54 H72 As Cl4 Ga N3'
_chemical_formula_weight         1049.58
_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             2019-08-07
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2019-11-19 deposited with the CCDC.	2020-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                76.229(2)
_cell_angle_beta                 89.254(2)
_cell_angle_gamma                88.856(2)
_cell_formula_units_Z            4
_cell_length_a                   11.4502(3)
_cell_length_b                   19.3524(5)
_cell_length_c                   25.1018(7)
_cell_measurement_reflns_used    19253
_cell_measurement_temperature    99.99(16)
_cell_measurement_theta_max      30.3970
_cell_measurement_theta_min      1.9580
_cell_volume                     5401.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  42.00   1.00   49.50    --   26.03  77.00-180.00   46
  2  \w     -4.00  42.00   1.00   49.50    --   26.03  77.00  30.00   46
  3  \w      1.00  98.00   1.00   49.50    --   26.03  38.00-180.00   97
  4  \w    -15.00  68.00   1.00   49.50    --   26.03 -99.00 -30.00   83
  5  \w    -47.00  99.00   1.00   49.50    --   26.03   0.00  30.00  146
  6  \w    -42.00  56.00   1.00   49.50    --   26.03 -77.00  30.00   98
  7  \w    -15.00  68.00   1.00   49.50    --   26.03 -99.00-120.00   83
  8  \w     -4.00  42.00   1.00   49.50    --   26.03  77.00  90.00   46
  9  \w     -4.00  42.00   1.00   49.50    --   26.03  77.00 -30.00   46
 10  \w    -15.00  23.00   1.00   49.50    --   26.03 -99.00 120.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0345595000
_diffrn_orient_matrix_UB_12      -0.0069268000
_diffrn_orient_matrix_UB_13      -0.0213324000
_diffrn_orient_matrix_UB_21      -0.0203447000
_diffrn_orient_matrix_UB_22      -0.0315519000
_diffrn_orient_matrix_UB_23      0.0180167000
_diffrn_orient_matrix_UB_31      -0.0472324000
_diffrn_orient_matrix_UB_32      0.0195185000
_diffrn_orient_matrix_UB_33      0.0081730000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            96628
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.154
_diffrn_reflns_theta_min         1.517
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.352
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.56a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.153
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.029
_refine_diff_density_max         1.391
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1167
_refine_ls_number_reflns         34476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0506P)^2^+2.6202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1294
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23488
_reflns_number_total             34476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00624f2.cif
_cod_data_source_block           compound3a
_cod_depositor_comments
'Adding full bibliography for 7126045--7126050.cif.'
_cod_database_code               7126046
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C57 H79 As Cl4 Ga N3'
_diffrn_oxdiff_digest_frames
;
014a6d4cd053fd2c42fe317489a5b552580075943dd
;
_diffrn_oxdiff_digest_hkl
;
015e0db2508abfa97aa227657d422d2dcf30df
;
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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 Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C49(H49), C52(H52), C64(H64),
 C67(H67), C76(H76), C79(H79), C103(H103), C106(H106)
2.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C91(H91A,H91B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C45(H45), C46(H46), C47(H47),
  C56(H56), C57(H57), C60(H60), C61(H61), C62(H62), C72(H72), C73(H73),
 C74(H74), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C99(H99),
 C100(H100), C101(H101)
2.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C54(H54A,H54B,H54C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,
 H68B,H68C), C69(H69A,H69B,H69C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C),
 C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C93(H93A,H93B,H93C), C94(H94A,H94B,
 H94C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C104(H10A,H10B,H10C),
 C105(H10D,H10E,H10F), C107(H10G,H10H,H10I), C108(H10J,H10K,H10L)
;
_shelx_res_checksum              64339
_olex2_date_sample_data_collection 2019-08-06
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.819