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_7126045
_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'
_chemical_formula_sum            'C54 H72 As N3'
_chemical_formula_weight         838.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2019-08-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2019-11-19 deposited with the CCDC.	2020-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.2310(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.59029(7)
_cell_length_b                   15.93625(8)
_cell_length_c                   23.78509(12)
_cell_measurement_reflns_used    64139
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.3860
_cell_measurement_theta_min      3.6930
_cell_volume                     4764.70(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -64.00  30.00   1.00    2.00    --  -38.50  57.00 -30.00   94
  2  \w    -59.00  33.00   1.00    2.00    --  -38.50  38.00  90.00   92
  3  \w    -72.00  39.00   1.00    2.00    --  -38.50  19.00-180.00  111
  4  \w    -87.00  -6.00   1.00    2.00    --  -38.50 125.00 120.00   81
  5  \w    -59.00  33.00   1.00    2.00    --  -38.50  38.00-120.00   92
  6  \w     13.00  42.00   1.00    2.00    --   42.89  76.00  76.43   29
  7  \w     12.00  42.00   1.00    2.00    --   42.89  78.00 -63.98   30
  8  \w     12.00  42.00   1.00    2.00    --   42.89  81.00-132.38   30
  9  \w     18.00 111.00   1.00    2.00    --   42.89  57.00-180.00   93
 10  \w     22.00 114.00   1.00    2.00    --   42.89  38.00  60.00   92
 11  \w     18.00 111.00   1.00    2.00    --   42.89  57.00 -60.00   93
 12  \w     11.00  42.00   1.00    2.00    --   42.89  82.00  27.72   31
 13  \w     12.00  42.00   1.00    2.00    --   42.89  79.00 125.64   30
 14  \w     27.00  97.00   1.00    2.00    --   42.89-125.00  60.00   70
 15  \w     11.00  42.00   1.00    2.00    --   42.89  82.00 145.98   31
 16  \w     18.00 111.00   1.00    2.00    --   42.89  57.00-120.00   93
 17  \w     13.00  42.00   1.00    2.00    --   42.89  76.00  -0.28   29
 18  \w     18.00 111.00   1.00    2.00    --   42.89  57.00  90.00   93
 19  \w     83.00 178.00   1.00    8.00    --  111.00  67.00  30.93   95
 20  \w     85.00 178.00   1.00    8.00    --  111.00  61.00  14.87   93
 21  \w     85.00 178.00   1.00    8.00    --  111.00  59.00 -37.27   93
 22  \w     83.00 178.00   1.00    8.00    --  111.00  68.00  64.49   95
 23  \w     82.00 178.00   1.00    8.00    --  111.00  71.00 163.92   96
 24  \w     84.00 178.00   1.00    8.00    --  111.00  63.00-157.89   94
 25  \w     85.00 178.00   1.00    8.00    --  111.00  61.00  48.05   93
 26  \w     83.00 178.00   1.00    8.00    --  111.00  67.00 135.45   95
 27  \w     82.00 178.00   1.00    8.00    --  111.00  74.00 146.71   96
 28  \w     84.00 178.00   1.00    8.00    --  111.00  64.00-108.68   94
 29  \w     41.00 113.00   1.00    8.00    --  111.00-125.00 120.00   72
 30  \w     82.00 178.00   1.00    8.00    --  111.00  74.00  11.96   96
 31  \w     83.00 178.00   1.00    8.00    --  111.00  69.00  90.77   95
 32  \w     86.00 178.00   1.00    8.00    --  111.00  57.00-134.44   92
 33  \w     83.00 178.00   1.00    8.00    --  111.00  67.00 127.06   95
 34  \w     84.00 178.00   1.00    8.00    --  111.00  63.00-132.10   94
 35  \w     82.00 178.00   1.00    8.00    --  111.00  72.00  66.12   96
 36  \w     85.00 178.00   1.00    8.00    --  111.00  60.00 127.00   93
 37  \w     82.00 178.00   1.00    8.00    --  111.00  73.00 -32.21   96
 38  \w     84.00 178.00   1.00    8.00    --  111.00  63.00 -54.44   94
 39  \w     84.00 178.00   1.00    8.00    --  111.00  63.00 -98.26   94
 40  \w     31.00 107.00   1.00    8.00    --  111.00 -94.00 -30.00   76
 41  \w     43.00 137.00   1.00    8.00    --  111.00 -61.00 150.00   94
 42  \w     85.00 178.00   1.00    8.00    --  111.00  61.00  60.00   93
 43  \w     85.00 178.00   1.00    8.00    --  111.00  61.00   0.00   93
 44  \w     41.00 113.00   1.00    8.00    --  111.00-125.00 -30.00   72
 45  \w     31.00 107.00   1.00    8.00    --  111.00 -94.00 150.00   76
 46  \w     82.00 178.00   1.00    8.00    --  111.00  72.00 -94.04   96
 47  \w     86.00 160.00   1.00    8.00    --  111.00  61.00 -90.00   74
 48  \w     63.00 137.00   1.00    8.00    --  111.00 -61.00 -60.00   74
 49  \w     85.00 111.00   1.00    8.00    --  111.00  61.00 -60.00   26
 50  \w     85.00 136.00   1.00    8.00    --  111.00  61.00 -30.00   51
 51  \w     85.00 111.00   1.00    8.00    --  111.00  61.00-120.00   26
 52  \w     82.00 178.00   1.00    8.00    --  111.00  72.00 104.15   96
 53  \w     80.00 107.00   1.00    8.00    --  111.00 -94.00   0.00   27
 54  \w     85.00 113.00   1.00    8.00    --  111.00-125.00 -90.00   28
 55  \w     86.00 111.00   1.00    8.00    --  111.00  61.00-180.00   25
 56  \w    124.00 174.00   1.00    8.00    --  111.00  61.00-180.00   50
 57  \w     85.00 111.00   1.00    8.00    --  111.00  61.00  90.00   26
 58  \w     85.00 127.00   1.00    8.00    --  111.00  61.00 150.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0851184000
_diffrn_orient_matrix_UB_12      -0.0695611000
_diffrn_orient_matrix_UB_13      -0.0021580000
_diffrn_orient_matrix_UB_21      -0.0523311000
_diffrn_orient_matrix_UB_22      0.0392182000
_diffrn_orient_matrix_UB_23      -0.0539035000
_diffrn_orient_matrix_UB_31      0.0709539000
_diffrn_orient_matrix_UB_32      -0.0544646000
_diffrn_orient_matrix_UB_33      -0.0360497000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            132664
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.519
_diffrn_reflns_theta_min         3.340
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.235
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     811
_refine_ls_number_reflns         9986
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+1.7124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9089
_reflns_number_total             9986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00624f2.cif
_cod_data_source_block           compound2a
_cod_depositor_comments
'Adding full bibliography for 7126045--7126050.cif.'
_cod_database_code               7126045
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C54H72AsN3
_diffrn_oxdiff_digest_frames
;
019223a95fb45029279e3dbc28c5f819a704322bf47
;
_diffrn_oxdiff_digest_hkl
;
01a17ea13ec9f4be8e839dd472fb491e19d1bd
;
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
;
_shelx_res_checksum              32505
_olex2_date_sample_data_collection 2019-08-15
_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 1.760
_oxdiff_exptl_absorpt_empirical_full_min 0.445