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_7120009
_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         'C69 H57 As N2, C7 H8'
_chemical_formula_sum            'C76 H65 As N2'
_chemical_formula_weight         1081.22
_chemical_name_systematic
;
 HAs{C[N(2,6-CHPh2,4-Me-C6H2)CH]2}*tol
;
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Light-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-02-24 deposited with the CCDC.
2017-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3683(2)
_cell_length_b                   14.8549(2)
_cell_length_c                   20.2018(3)
_cell_measurement_reflns_used    11473
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75.9223
_cell_measurement_theta_min      2.9723
_cell_volume                     5812.34(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4102
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21416
_diffrn_reflns_point_group_measured_fraction_full 0.785
_diffrn_reflns_point_group_measured_fraction_max 0.774
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.113
_diffrn_reflns_theta_min         3.693
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 2713 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.035(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         9425
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0939P)^2^+2.7498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.519
_reflns_Friedel_fraction_full    0.556
_reflns_Friedel_fraction_max     0.545
_reflns_number_gt                8702
_reflns_number_total             9425
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02628e2.cif
_cod_data_source_block           MW083
_cod_database_code               7120009
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.915
_shelxl_version_number           2013-4
_shelx_res_checksum              59539
_shelx_hkl_checksum              16291