#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:48:43 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178964 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/93/4119377.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4119377
loop_
_publ_author_name
'Mariham Y. Abraham'
'Yuzhong Wang'
'Yaoming Xie'
'Robert J. Gilliard'
'Pingrong Wei'
'Brian J. Vaccaro'
'Michael K. Johnson'
'Henry F. Schaefer'
'Paul v. R. Schleyer'
'Gregory H. Robinson'
_publ_section_title
;
 Oxidation of Carbene-Stabilized Diarsenic: Diarsene Dications and
 Diarsenic Radical Cations
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2486
_journal_page_last               2488
_journal_paper_doi               10.1021/ja400219d
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C58 H78 As2 Cl8 Ga2 N6'
_chemical_formula_weight         1432.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.9530(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.2173(10)
_cell_length_b                   18.3240(12)
_cell_length_c                   13.9424(9)
_cell_measurement_reflns_used    9943
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.134
_cell_measurement_theta_min      2.675
_cell_volume                     3495.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER SMART APEX II'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43129
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    2.054
_exptl_absorpt_correction_T_max  0.7619
_exptl_absorpt_correction_T_min  0.4938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7634
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0474P)²+2.9500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1045
_reflns_number_gt                6058
_reflns_number_total             7634
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja400219d_si_003.cif
_cod_data_source_block           j1
_cod_database_code               4119377
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
As1 As 0.428213(18) 0.475142(15) 0.44008(2) 0.04150(9) Uani 1 1 d .
N1 N 0.34218(15) 0.57840(11) 0.55272(16) 0.0375(4) Uani 1 1 d .
N2 N 0.23832(14) 0.51646(11) 0.42021(16) 0.0353(4) Uani 1 1 d .
C1 C 0.33498(16) 0.52900(13) 0.47753(18) 0.0331(5) Uani 1 1 d .
C2 C 0.25062(19) 0.59605(16) 0.5421(2) 0.0459(6) Uani 1 1 d .
H2A H 0.2361 0.6288 0.5840 0.055 Uiso 1 1 calc R
C3 C 0.18587(18) 0.55691(16) 0.4597(2) 0.0435(6) Uani 1 1 d .
H3A H 0.1183 0.5573 0.4343 0.052 Uiso 1 1 calc R
C4 C 0.19651(17) 0.46663(15) 0.33005(19) 0.0392(5) Uani 1 1 d .
C5 C 0.16981(19) 0.49525(17) 0.2281(2) 0.0465(6) Uani 1 1 d .
C6 C 0.1361(2) 0.4449(2) 0.1447(2) 0.0640(9) Uani 1 1 d .
H6A H 0.1184 0.4611 0.0754 0.077 Uiso 1 1 calc R
C7 C 0.1284(3) 0.3725(2) 0.1622(3) 0.0707(10) Uani 1 1 d .
H7A H 0.1074 0.3400 0.1052 0.085 Uiso 1 1 calc R
C8 C 0.1512(2) 0.34713(19) 0.2624(3) 0.0636(9) Uani 1 1 d .
H8A H 0.1441 0.2977 0.2723 0.076 Uiso 1 1 calc R
C9 C 0.1849(2) 0.39392(16) 0.3506(2) 0.0480(6) Uani 1 1 d .
C10 C 0.2035(2) 0.36538(18) 0.4597(3) 0.0584(8) Uani 1 1 d .
H10A H 0.2260 0.4065 0.5096 0.070 Uiso 1 1 calc R
C11 C 0.1097(3) 0.3365(3) 0.4601(4) 0.0976(14) Uani 1 1 d .
H11A H 0.0608 0.3741 0.4360 0.146 Uiso 1 1 calc R
H11B H 0.1224 0.3222 0.5312 0.146 Uiso 1 1 calc R
H11C H 0.0869 0.2951 0.4134 0.146 Uiso 1 1 calc R
C12 C 0.2831(4) 0.3084(3) 0.4986(5) 0.125(2) Uani 1 1 d .
H12A H 0.3413 0.3282 0.4981 0.187 Uiso 1 1 calc R
H12B H 0.2622 0.2666 0.4526 0.187 Uiso 1 1 calc R
H12C H 0.2964 0.2941 0.5699 0.187 Uiso 1 1 calc R
C13 C 0.1769(2) 0.57602(19) 0.2073(2) 0.0565(7) Uani 1 1 d .
H13A H 0.1779 0.6033 0.2681 0.068 Uiso 1 1 calc R
C14 C 0.2714(3) 0.5928(3) 0.1989(4) 0.0879(13) Uani 1 1 d .
H14A H 0.3261 0.5765 0.2625 0.132 Uiso 1 1 calc R
H14B H 0.2764 0.6444 0.1909 0.132 Uiso 1 1 calc R
H14C H 0.2712 0.5680 0.1382 0.132 Uiso 1 1 calc R
C15 C 0.0900(3) 0.6029(3) 0.1069(3) 0.0856(12) Uani 1 1 d .
H15A H 0.0305 0.5928 0.1124 0.128 Uiso 1 1 calc R
H15B H 0.0891 0.5784 0.0457 0.128 Uiso 1 1 calc R
H15C H 0.0958 0.6546 0.0996 0.128 Uiso 1 1 calc R
C16 C 0.43280(18) 0.61012(14) 0.6299(2) 0.0411(6) Uani 1 1 d .
C17 C 0.4672(2) 0.67242(15) 0.5995(2) 0.0509(7) Uani 1 1 d .
C18 C 0.5582(2) 0.69791(18) 0.6725(3) 0.0676(9) Uani 1 1 d .
H18A H 0.5848 0.7389 0.6558 0.081 Uiso 1 1 calc R
C19 C 0.6092(2) 0.6637(2) 0.7685(3) 0.0728(11) Uani 1 1 d .
H19A H 0.6710 0.6807 0.8146 0.087 Uiso 1 1 calc R
C20 C 0.5710(2) 0.6052(2) 0.7978(3) 0.0664(9) Uani 1 1 d .
H20A H 0.6062 0.5843 0.8646 0.080 Uiso 1 1 calc R
C21 C 0.4797(2) 0.57594(17) 0.7293(2) 0.0498(7) Uani 1 1 d .
C22 C 0.4337(2) 0.51491(19) 0.7645(2) 0.0580(8) Uani 1 1 d .
H22A H 0.3745 0.4996 0.7022 0.070 Uiso 1 1 calc R
C23 C 0.4025(4) 0.5436(3) 0.8475(4) 0.1076(16) Uani 1 1 d .
H23A H 0.3613 0.5856 0.8196 0.161 Uiso 1 1 calc R
H23B H 0.4594 0.5571 0.9110 0.161 Uiso 1 1 calc R
H23C H 0.3672 0.5063 0.8643 0.161 Uiso 1 1 calc R
C24 C 0.4988(4) 0.4485(3) 0.8058(5) 0.1110(18) Uani 1 1 d .
H24A H 0.5164 0.4309 0.7517 0.166 Uiso 1 1 calc R
H24B H 0.4643 0.4110 0.8236 0.166 Uiso 1 1 calc R
H24C H 0.5568 0.4616 0.8682 0.166 Uiso 1 1 calc R
C25 C 0.4067(2) 0.71395(17) 0.4981(3) 0.0629(8) Uani 1 1 d .
H25A H 0.3509 0.6830 0.4544 0.075 Uiso 1 1 calc R
C26 C 0.3659(4) 0.7828(2) 0.5259(5) 0.1172(19) Uani 1 1 d .
H26A H 0.3329 0.7699 0.5685 0.176 Uiso 1 1 calc R
H26B H 0.3206 0.8060 0.4614 0.176 Uiso 1 1 calc R
H26C H 0.4185 0.8157 0.5652 0.176 Uiso 1 1 calc R
C27 C 0.4604(4) 0.7323(3) 0.4311(4) 0.1073(17) Uani 1 1 d .
H27A H 0.4854 0.6883 0.4149 0.161 Uiso 1 1 calc R
H27B H 0.5136 0.7648 0.4703 0.161 Uiso 1 1 calc R
H27C H 0.4161 0.7553 0.3660 0.161 Uiso 1 1 calc R
Ga1 Ga 1.14815(3) 0.40942(2) 0.76642(3) 0.06579(13) Uani 1 1 d .
Cl1 Cl 1.10248(11) 0.49719(6) 0.65224(10) 0.1022(4) Uani 1 1 d .
Cl2 Cl 1.26827(9) 0.35007(7) 0.76059(12) 0.1055(4) Uani 1 1 d .
Cl3 Cl 1.02433(9) 0.33619(7) 0.72042(14) 0.1146(5) Uani 1 1 d .
Cl4 Cl 1.19443(13) 0.45268(13) 0.92445(11) 0.1492(7) Uani 1 1 d .
C28 C 1.1134(4) 0.6600(3) 0.8211(5) 0.1223(19) Uani 1 1 d .
H28A H 1.0468 0.6485 0.7740 0.183 Uiso 1 1 calc R
H28B H 1.1150 0.6969 0.8707 0.183 Uiso 1 1 calc R
H28C H 1.1460 0.6170 0.8595 0.183 Uiso 1 1 calc R
C29 C 1.1623(4) 0.6865(3) 0.7598(5) 0.1002(15) Uani 1 1 d .
N3 N 1.2007(4) 0.7056(3) 0.7115(5) 0.1289(17) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_3
C1 As1 As1 100.10(7) 3_666
C1 N1 C2 109.9(2) .
C1 N1 C16 124.9(2) .
C2 N1 C16 125.2(2) .
C1 N2 C3 110.2(2) .
C1 N2 C4 124.7(2) .
C3 N2 C4 125.1(2) .
N2 C1 N1 105.7(2) .
N2 C1 As1 118.70(17) .
N1 C1 As1 135.61(17) .
C3 C2 N1 107.1(2) .
C2 C3 N2 107.1(2) .
C9 C4 C5 124.2(2) .
C9 C4 N2 118.1(2) .
C5 C4 N2 117.7(2) .
C6 C5 C4 115.9(3) .
C6 C5 C13 121.0(3) .
C4 C5 C13 123.0(2) .
C7 C6 C5 121.5(3) .
C8 C7 C6 120.8(3) .
C7 C8 C9 121.4(3) .
C4 C9 C8 115.9(3) .
C4 C9 C10 123.6(3) .
C8 C9 C10 120.4(3) .
C9 C10 C12 111.6(3) .
C9 C10 C11 111.1(3) .
C12 C10 C11 111.3(4) .
C5 C13 C14 111.0(3) .
C5 C13 C15 112.5(3) .
C14 C13 C15 109.4(3) .
C21 C16 C17 124.8(2) .
C21 C16 N1 117.6(2) .
C17 C16 N1 117.6(2) .
C16 C17 C18 115.9(3) .
C16 C17 C25 122.7(3) .
C18 C17 C25 121.2(3) .
C19 C18 C17 121.2(3) .
C18 C19 C20 121.2(3) .
C19 C20 C21 121.5(3) .
C16 C21 C20 115.2(3) .
C16 C21 C22 123.1(3) .
C20 C21 C22 121.6(3) .
C21 C22 C23 109.5(3) .
C21 C22 C24 113.6(3) .
C23 C22 C24 111.0(4) .
C17 C25 C26 109.1(3) .
C17 C25 C27 114.4(3) .
C26 C25 C27 111.1(4) .
Cl4 Ga1 Cl1 109.72(7) .
Cl4 Ga1 Cl2 108.74(7) .
Cl1 Ga1 Cl2 110.68(6) .
Cl4 Ga1 Cl3 112.57(7) .
Cl1 Ga1 Cl3 106.61(6) .
Cl2 Ga1 Cl3 108.52(5) .
N3 C29 C28 178.5(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As1 C1 1.977(2) .
As1 As1 2.2803(5) 3_666
N1 C1 1.353(3) .
N1 C2 1.374(3) .
N1 C16 1.449(3) .
N2 C1 1.351(3) .
N2 C3 1.369(3) .
N2 C4 1.456(3) .
C2 C3 1.348(4) .
C4 C9 1.390(4) .
C4 C5 1.399(4) .
C5 C6 1.394(4) .
C5 C13 1.521(5) .
C6 C7 1.364(5) .
C7 C8 1.366(5) .
C8 C9 1.399(4) .
C9 C10 1.514(4) .
C10 C12 1.509(5) .
C10 C11 1.525(5) .
C13 C14 1.523(5) .
C13 C15 1.527(4) .
C16 C21 1.399(4) .
C16 C17 1.396(4) .
C17 C18 1.393(4) .
C17 C25 1.512(5) .
C18 C19 1.370(6) .
C19 C20 1.364(6) .
C20 C21 1.403(4) .
C21 C22 1.510(5) .
C22 C23 1.524(5) .
C22 C24 1.514(5) .
C25 C26 1.528(5) .
C25 C27 1.524(6) .
Ga1 Cl4 2.1496(15) .
Ga1 Cl1 2.1530(11) .
Ga1 Cl2 2.1588(11) .
Ga1 Cl3 2.1689(13) .
C28 C29 1.440(8) .
C29 N3 1.125(7) .
