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_7120007
_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         'C24 H33 As N2 Si, 0.5(C3 H6)'
_chemical_formula_sum            'C25.5 H36 As N2 Si'
_chemical_formula_weight         473.57
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.949(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8764(6)
_cell_length_b                   9.1798(3)
_cell_length_c                   38.5234(13)
_cell_measurement_reflns_used    10816
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.5260
_cell_measurement_theta_min      5.5610
_cell_volume                     5492.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    -50.00  26.00   1.00    5.00    --  -44.93  38.00 -90.00   76
  2  \w   -124.00 -79.00   1.00    5.00    --  -44.93 -99.00-150.00   45
  3  \w     21.00 114.00   1.00    5.00    --   44.93  57.00 -60.00   93
  4  \w    -24.00  69.00   1.00    5.00    --   44.93 -57.00  90.00   93
  5  \w     21.00 114.00   1.00    5.00    --   44.93  57.00-120.00   93
  6  \w     21.00 114.00   1.00    5.00    --   44.93  57.00-180.00   93
  7  \w     74.00 176.00   1.00   20.00    --  104.50  77.00 150.00  102
  8  \w     79.00 174.00   1.00   20.00    --  104.50  61.00-120.00   95
  9  \w     36.00  98.00   1.00   20.00    --  104.50 -45.00 120.00   62
 10  \w     74.00 176.00   1.00   20.00    --  104.50  77.00 -90.00  102
 11  \w     74.00 100.00   1.00   20.00    --  104.50  77.00-150.00   26
 12  \w    114.00 171.00   1.00   20.00    --  104.50  77.00-150.00   57
 13  \w     81.00 115.00   1.00   20.00    --  104.50  61.00 -90.00   34
 14  \w     58.00 109.00   1.00   20.00    --  104.50 -94.00-120.00   51
 15  \w     35.00  84.00   1.00   20.00    --  104.50 -30.00 150.00   49
 16  \w     38.00 115.00   1.00   20.00    --  104.50-125.00-180.00   77
 17  \w     79.00 114.00   1.00   20.00    --  104.50  61.00-150.00   35
 18  \w    128.00 176.00   1.00   20.00    --  104.50  77.00 165.44   48
 19  \w     75.00 100.00   1.00   20.00    --  104.50  77.00-120.00   25
 20  \w    121.00 174.00   1.00   20.00    --  104.50  77.00-120.00   53
 21  \w     81.00 109.00   1.00   20.00    --  104.50  77.00 165.44   28
 22  \w     74.00 101.00   1.00   20.00    --  104.50  77.00-180.00   27
 23  \w     55.00  82.00   1.00   20.00    --  104.50 -30.00 -90.00   27
 24  \w     83.00 111.00   1.00   20.00    --  104.50  45.00-120.00   28
 25  \w     84.00 169.00   1.00   20.00    --  104.50  45.00 -60.00   85
 26  \w     80.00 106.00   1.00   20.00    --  104.50  61.00-180.00   26
 27  \w     86.00 113.00   1.00   20.00    --  104.50  45.00 -90.00   27
 28  \w    114.00 163.00   1.00   20.00    --  104.50  61.00  42.78   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0954111000
_diffrn_orient_matrix_UB_12      0.0392931000
_diffrn_orient_matrix_UB_13      0.0137674000
_diffrn_orient_matrix_UB_21      -0.0216244000
_diffrn_orient_matrix_UB_22      0.0576172000
_diffrn_orient_matrix_UB_23      0.0346636000
_diffrn_orient_matrix_UB_31      0.0166902000
_diffrn_orient_matrix_UB_32      -0.1526447000
_diffrn_orient_matrix_UB_33      0.0166287000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            29510
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.642
_diffrn_reflns_theta_min         2.345
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.145
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_recrystallization_method 'from saturated hexanes solution'
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0568
_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^)+(0.1216P)^2^+3.8945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1853
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4609
_reflns_number_total             5569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02628e2.cif
_cod_data_source_block           mw41_abs
_cod_original_formula_sum        'C25.50 H36 As N2 Si'
_cod_database_code               7120007
_chemical_oxdiff_formula         'C25.5 H36 N2 Si As1'
_chemical_oxdiff_usercomment     'yellow block'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 Fixed Sof: C0AA(0.5) H0AA(0.5) H0AB(0.5) C1AA(0.5) H1AA(0.5) H1AB(0.5)
 C2AA(0.5) H2AA(0.5) H2AB(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C18(H18), C20(H20), C6(H6), C3(H3), C2(H2)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C23(H23A,H23B,H23C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C13(H13A,
 H13B,H13C), C24(H24A,H24B,H24C)
;
_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 3.398
_oxdiff_exptl_absorpt_empirical_full_min 0.684