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_7126048
_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         'C57 H76 As N3, 2(Cl4 Ga)'
_chemical_formula_sum            'C57 H76 As Cl8 Ga2 N3'
_chemical_formula_weight         1301.16
_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             2019-07-04
_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                100.452(2)
_cell_angle_beta                 98.045(3)
_cell_angle_gamma                98.408(3)
_cell_formula_units_Z            4
_cell_length_a                   13.7117(5)
_cell_length_b                   24.2939(7)
_cell_length_c                   24.8610(8)
_cell_measurement_reflns_used    13698
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      24.2980
_cell_measurement_theta_min      1.7510
_cell_volume                     7937.7(5)
_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      100.01(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -47.00  99.00   1.00   55.50    --   26.03   0.00-120.00  146
  2  \w    -43.00  47.00   1.00   55.50    --   26.03 -57.00-150.00   90
  3  \w    -15.00  68.00   1.00   55.50    --   26.03 -99.00  60.00   83
  4  \w      6.00  95.00   1.00   55.50    --   26.03  57.00   0.00   89
  5  \w      1.00  98.00   1.00   55.50    --   26.03  38.00 -90.00   97
  6  \w     -4.00  42.00   1.00   55.50    --   26.03  77.00-180.00   46
  7  \w      6.00  95.00   1.00   55.50    --   26.03  57.00  90.00   89
  8  \w     -4.00  42.00   1.00   55.50    --   26.03  77.00 -60.00   46
  9  \w    -15.00  28.00   1.00   55.50    --   26.03 -99.00 -60.00   43
;
_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      0.0444936000
_diffrn_orient_matrix_UB_12      -0.0113967000
_diffrn_orient_matrix_UB_13      -0.0017235000
_diffrn_orient_matrix_UB_21      0.0251601000
_diffrn_orient_matrix_UB_22      0.0266751000
_diffrn_orient_matrix_UB_23      -0.0029340000
_diffrn_orient_matrix_UB_31      0.0142890000
_diffrn_orient_matrix_UB_32      0.0082624000
_diffrn_orient_matrix_UB_33      0.0292490000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0755
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            97309
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.524
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.728
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       plate
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.873
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1344
_refine_ls_number_reflns         29076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0599P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1308
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19032
_reflns_number_total             29076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00624f2.cif
_cod_data_source_block           compound4b
_cod_depositor_comments
'Adding full bibliography for 7126045--7126050.cif.'
_cod_database_code               7126048
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C78 H72 As F2 Ga2 N2 Cl4'
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.801
_diffrn_oxdiff_digest_frames
;
011700a3cad12e076606fc4cc3b941148b000276cfc
;
_diffrn_oxdiff_digest_hkl
;
019dad25ea5d368dfc5d5b88c1d0edde42ea54
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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. Others
 Sof(Ga4B)=Sof(Cl17)=Sof(Cl18)=Sof(Cl19)=1-FVAR(1)
 Sof(Ga4)=Sof(Cl14)=Sof(Cl15)=Sof(Cl16)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C52(H52), C55(H55), C67(H67),
 C70(H70), C79(H79), C82(H82), C109(H109), C112(H112)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C94(H94A,H94B), C96(H96A,H96B), C97(H97A,H97B),
 C98(H98A,H98B), C99(H99A,H99B), C100(H10A,H10B)
3.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), C48(H48), C49(H49), C50(H50),
  C59(H59), C60(H60), C63(H63), C64(H64), C65(H65), C75(H75), C76(H76),
 C77(H77), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C105(H105),
 C106(H106), C107(H107)
3.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), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C80(H80A,
 H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C),
 C101(H10C,H10D,H10E), C102(H10F,H10G,H10H), C110(H11D,H11E,H11F), C111(H11G,
 H11H,H11I), C113(H11J,H11K,H11L), C114(H11M,H11N,H11O)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32762
_shelx_fab_checksum              40326
_olex2_date_sample_data_collection 2019-06-25
_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 1.234
_oxdiff_exptl_absorpt_empirical_full_min 0.837