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_7120008
_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         'C21 H25 As N2'
_chemical_formula_sum            'C21 H25 As N2'
_chemical_formula_weight         380.35
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Light-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 102.690(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2857(2)
_cell_length_b                   14.8334(2)
_cell_length_c                   16.1781(4)
_cell_measurement_reflns_used    6785
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.8230
_cell_measurement_theta_min      4.0630
_cell_volume                     1939.80(7)
_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 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.959
_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     21.00 113.00   1.00   12.50    --   44.92  57.00-120.00   92
  2  \w    -20.00  84.00   1.00   12.50    --   44.92 -99.00  90.00  104
  3  \w     33.00 135.00   1.00   42.50    --  104.50 -77.00-120.00  102
  4  \w     32.00 128.00   1.00   42.50    --  104.50 -30.00 150.00   96
  5  \w     82.00 173.00   1.00   42.50    --  104.50  45.00 150.00   91
  6  \w     74.00 176.00   1.00   42.50    --  104.50  77.00  90.00  102
  7  \w   -117.00 -15.00   1.00   12.50    --  -44.92 -77.00  30.00  102
  8  \w     22.00 116.00   1.00   12.50    --   44.92  37.00 150.00   94
  9  \w     82.00 165.00   1.00   42.50    --  104.50  45.00 -60.00   83
;
_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      -0.1769972000
_diffrn_orient_matrix_UB_12      0.0337180000
_diffrn_orient_matrix_UB_13      -0.0370653000
_diffrn_orient_matrix_UB_21      -0.0431688000
_diffrn_orient_matrix_UB_22      -0.0914755000
_diffrn_orient_matrix_UB_23      -0.0444879000
_diffrn_orient_matrix_UB_31      -0.0562050000
_diffrn_orient_matrix_UB_32      -0.0357432000
_diffrn_orient_matrix_UB_33      0.0785274000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11051
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.896
_diffrn_reflns_theta_min         4.090
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.380
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.714
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_recrystallization_method 'from saturated hexanes solution'
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.699
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0680P)^2^+2.2713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3455
_reflns_number_total             3778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02628e2.cif
_cod_data_source_block           mw57_abs
_cod_database_code               7120008
_chemical_oxdiff_formula         'C21 H25 N2 As1'
_chemical_oxdiff_usercomment     'colorless needle'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Aromatic/amide H refined with riding coordinates:
 C6(H6), C18(H18), C8(H8), C2(H2), C3(H3), C15(H15)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C17(H17A,H17B,H17C)
;
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.753