N-Heterocyclic Carbene-Stabilised Arsinidene (AsH)
Doddi, Adinarayana; Weinhart, Michael; Hinz, Alexander; Bockfeld, Dirk; Goicoechea, Jose M.; Scheer, Manfred; Tamm, Matthias; Chem. Commun.  (2017) –; doi:10.1039/C7CC02628E

data_7120010
_publ_section_title
;
 N-Heterocyclic Carbene-Stabilised Arsinidene (AsH)
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02628E
_journal_year                    2017
_chemical_formula_moiety         '1(C27 H37 As N2)'
_chemical_formula_sum            'C27 H37 As N2'
_chemical_formula_weight         464.51
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Light-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.303(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0571(5)
_cell_length_b                   7.0854(2)
_cell_length_c                   39.0742(10)
_cell_measurement_reflns_used    7381
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.1920
_cell_measurement_theta_min      4.5640
_cell_volume                     5301.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9887
_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     95.00 135.00   1.00   16.00    --  111.00 -61.00 120.00   40
  2  \w     63.00  91.00   1.00   16.00    --  111.00 -61.00 120.00   28
  3  \w     44.00  90.00   1.00   16.00    --  111.00 -45.00 120.00   46
  4  \w     31.00 109.00   1.00   16.00    --  111.00 -94.00  60.00   78
  5  \w     32.00  83.00   1.00    4.00    --   41.90-125.00  90.00   51
  6  \w     38.00  76.00   1.00   16.00    --  111.00 -30.00-120.00   38
  7  \w     57.00  83.00   1.00   16.00    --  111.00 -45.00-150.00   26
  8  \w     47.00  80.00   1.00   16.00    --  111.00 -15.00-120.00   33
  9  \w    124.00 156.00   1.00   16.00    --  111.00 -15.00-120.00   32
 10  \w    142.00 175.00   1.00   16.00    --  111.00  61.00   0.00   33
 11  \w    149.00 176.00   1.00   16.00    --  111.00 111.00  60.00   27
 12  \w    153.00 178.00   1.00   16.00    --  111.00 111.00  90.00   25
 13  \w    112.00 137.00   1.00   16.00    --  111.00 111.00  90.00   25
 14  \w    102.00 133.00   1.00   16.00    --  111.00 111.00  60.00   31
 15  \w    102.00 178.00   1.00   16.00    --  111.00 111.00  30.00   76
 16  \w     86.00 136.00   1.00   16.00    --  111.00  61.00   0.00   50
 17  \w     84.00 145.00   1.00   16.00    --  111.00  61.00 -30.00   61
 18  \w     57.00 123.00   1.00   16.00    --  111.00 178.00-180.00   66
 19  \w      6.00  31.00   1.00    4.00    --  -41.90  37.00  90.00   25
 20  \w    -48.00  25.00   1.00    4.00    --  -41.90  37.00 -30.00   73
 21  \w   -118.00 -16.00   1.00    4.00    --  -41.90 -19.00 150.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0575612000
_diffrn_orient_matrix_UB_12      -0.0437583000
_diffrn_orient_matrix_UB_13      0.0175931000
_diffrn_orient_matrix_UB_21      0.0265841000
_diffrn_orient_matrix_UB_22      0.1621365000
_diffrn_orient_matrix_UB_23      0.0268586000
_diffrn_orient_matrix_UB_31      -0.0495531000
_diffrn_orient_matrix_UB_32      0.1380172000
_diffrn_orient_matrix_UB_33      -0.0259690000
_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  0.0267
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            15093
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.340
_diffrn_reflns_theta_min         4.618
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41h (Rigaku Oxford Diffraction, 2015)
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    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method
'crystallisation in a saturated n-hexane solution'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         5494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0880P)^2^+6.7580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1425
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4981
_reflns_number_total             5494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02628e2.cif
_cod_data_source_block           mw078_abs
_cod_original_formula_sum        'C27 H37 As1 N2'
_cod_database_code               7120010
_chemical_oxdiff_formula         'C27 H37 As1 N2'
_chemical_oxdiff_usercomment     ' '
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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 Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C7(H7), C3(H3), C6(H6), C18(H18), C20(H20), C19(H19)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C24(H24A,H24B,
 H24C), C15(H15A,H15B,H15C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C26(H26A,
 H26B,H26C)
;
_shelx_shelxl_version_number     2014/7
_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 1.573
_oxdiff_exptl_absorpt_empirical_full_min 0.696