#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:50:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179131 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/93/4309352.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_4309352
loop_
_publ_author_name
'Neil Burford'
'Jeff C. Landry'
'Michael J. Ferguson'
'Robert McDonald'
_publ_contact_author_address
;Department of Chemistry
Dalhousie University
Halifax, NS. CANADA
B3H 4J3
;
_publ_contact_author_email       neil.burford@dal.ca
_publ_contact_author_fax         902-494-1310
_publ_contact_author_name        'Neil Burford'
_publ_contact_author_phone       902-494-3190
_publ_section_title
;
Synthesis of cyclo-2,4,6-Triarsa-1,3,5-triazanes
from cyclo-2,4-Diarsa-1,3-diazanes Demonstrating the General Influence of
Substituent Steric Strain on the Relative Stability of Pnictazane Oligomers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5897
_journal_page_last               5902
_journal_paper_doi               10.1021/ic050532m
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C36 H46 As2 Cl2 N2'
_chemical_formula_sum            'C36 H46 As2 Cl2 N2'
_chemical_formula_weight         727.49
_chemical_melting_point          505.5(15)
_chemical_name_common            'DippNAsCl Dimer'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.8454(16)
_cell_length_b                   10.2167(7)
_cell_length_c                   15.6939(11)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.414
_cell_measurement_theta_min      2.378
_cell_volume                     3663.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27542
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.996
_exptl_absorpt_correction_T_max  0.5858
_exptl_absorpt_correction_T_min  0.4413
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   empirical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0348P)²+1.1181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                3316
_reflns_number_total             3983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050532msi20050407_085836_1.cif
_cod_data_source_block           dal0458
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value '504-507' changed to '505.5(15)' - took
average value and fixed precision.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 
;
_cod_database_code               4309352
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
As As 0.366228(8) 0.113034(16) -0.024303(10) 0.03009(7) Uani 1 1 d . . .
Cl Cl 0.32844(2) 0.02292(5) -0.14216(3) 0.04525(12) Uani 1 1 d . . .
N1 N 0.31542(9) 0.2500 -0.00424(13) 0.0298(4) Uani 1 2 d S . .
N2 N 0.40962(9) 0.2500 -0.06735(13) 0.0309(4) Uani 1 2 d S . .
C11 C 0.26578(11) 0.2500 0.05137(15) 0.0312(5) Uani 1 2 d S . .
C12 C 0.20958(12) 0.2500 0.01428(17) 0.0392(6) Uani 1 2 d S . .
C13 C 0.16153(13) 0.2500 0.0690(2) 0.0591(8) Uani 1 2 d S . .
H13 H 0.1232 0.2500 0.0456 0.071 Uiso 1 2 calc SR . .
C14 C 0.16826(15) 0.2500 0.1555(2) 0.0682(10) Uani 1 2 d S . .
H14 H 0.1347 0.2500 0.1912 0.082 Uiso 1 2 calc SR . .
C15 C 0.22299(15) 0.2500 0.19135(19) 0.0556(8) Uani 1 2 d S . .
H15 H 0.2267 0.2500 0.2516 0.067 Uiso 1 2 calc SR . .
C16 C 0.27342(12) 0.2500 0.14083(16) 0.0387(6) Uani 1 2 d S . .
C17 C 0.20068(12) 0.2500 -0.08117(18) 0.0415(6) Uani 1 2 d S . .
H17 H 0.2402 0.2500 -0.1084 0.050 Uiso 1 2 calc SR . .
C18 C 0.16860(13) 0.1286(2) -0.11148(18) 0.0692(7) Uani 1 1 d . . .
H18A H 0.1643 0.1317 -0.1736 0.083 Uiso 1 1 calc R . .
H18B H 0.1298 0.1251 -0.0849 0.083 Uiso 1 1 calc R . .
H18C H 0.1910 0.0505 -0.0955 0.083 Uiso 1 1 calc R . .
C19 C 0.33287(13) 0.2500 0.18287(17) 0.0465(7) Uani 1 2 d S . .
H19 H 0.3629 0.2500 0.1365 0.056 Uiso 1 2 calc SR . .
C20 C 0.34242(15) 0.1276(3) 0.2358(2) 0.0885(9) Uani 1 1 d . . .
H20A H 0.3813 0.1307 0.2619 0.106 Uiso 1 1 calc R . .
H20B H 0.3395 0.0503 0.1991 0.106 Uiso 1 1 calc R . .
H20C H 0.3126 0.1228 0.2805 0.106 Uiso 1 1 calc R . .
C21 C 0.47142(11) 0.2500 -0.08447(16) 0.0325(5) Uani 1 2 d S . .
C22 C 0.48940(12) 0.2500 -0.17025(17) 0.0417(6) Uani 1 2 d S . .
C23 C 0.54961(14) 0.2500 -0.1861(2) 0.0580(8) Uani 1 2 d S . .
H23 H 0.5631 0.2500 -0.2434 0.070 Uiso 1 2 calc SR . .
C24 C 0.58965(14) 0.2500 -0.1212(2) 0.0630(9) Uani 1 2 d S . .
H24 H 0.6303 0.2500 -0.1339 0.076 Uiso 1 2 calc SR . .
C25 C 0.57140(13) 0.2500 -0.0375(2) 0.0525(8) Uani 1 2 d S . .
H25 H 0.5997 0.2500 0.0069 0.063 Uiso 1 2 calc SR . .
C26 C 0.51191(12) 0.2500 -0.01707(17) 0.0382(6) Uani 1 2 d S . .
C27 C 0.44603(14) 0.2500 -0.24304(17) 0.0464(7) Uani 1 2 d S . .
H27 H 0.4060 0.2500 -0.2174 0.056 Uiso 1 2 calc SR . .
C28 C 0.45111(13) 0.1270(2) -0.29721(16) 0.0687(7) Uani 1 1 d . . .
H28A H 0.4222 0.1301 -0.3433 0.082 Uiso 1 1 calc R . .
H28B H 0.4439 0.0498 -0.2616 0.082 Uiso 1 1 calc R . .
H28C H 0.4905 0.1217 -0.3216 0.082 Uiso 1 1 calc R . .
C29 C 0.49358(12) 0.2500 0.07582(17) 0.0406(6) Uani 1 2 d S . .
H29 H 0.4498 0.2500 0.0765 0.049 Uiso 1 2 calc SR . .
C30 C 0.51284(15) 0.1275(3) 0.12219(18) 0.0882(10) Uani 1 1 d . . .
H30A H 0.4999 0.1317 0.1817 0.106 Uiso 1 1 calc R . .
H30B H 0.5556 0.1207 0.1203 0.106 Uiso 1 1 calc R . .
H30C H 0.4955 0.0506 0.0947 0.106 Uiso 1 1 calc R . .
C11S C 0.22113(16) -0.2500 0.1774(2) 0.0682(10) Uani 1 2 d S . .
H11S H 0.2087 -0.2500 0.2352 0.082 Uiso 1 2 calc SR . .
C12S C 0.22994(11) -0.1355(3) 0.13628(19) 0.0693(7) Uani 1 1 d . . .
H12S H 0.2231 -0.0551 0.1651 0.083 Uiso 1 1 calc R . .
C13S C 0.24858(11) -0.1345(3) 0.0539(2) 0.0705(8) Uani 1 1 d . . .
H13S H 0.2548 -0.0535 0.0255 0.085 Uiso 1 1 calc R . .
C14S C 0.25846(15) -0.2500 0.0117(2) 0.0701(11) Uani 1 2 d S . .
H14S H 0.2719 -0.2500 -0.0456 0.084 Uiso 1 2 calc SR . .
C21S C 0.49871(10) -0.1843(3) 0.59920(18) 0.0697(7) Uani 1 1 d . . .
H21S H 0.4666 -0.1379 0.6229 0.084 Uiso 1 1 calc R . .
C22S C 0.54499(13) -0.1173(3) 0.5651(2) 0.0840(9) Uani 1 1 d . . .
H22S H 0.5447 -0.0243 0.5646 0.101 Uiso 1 1 calc R . .
C23S C 0.59185(11) -0.1840(3) 0.53158(15) 0.0751(8) Uani 1 1 d . . .
H23S H 0.6241 -0.1373 0.5085 0.090 Uiso 1 1 calc R . .
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'
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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 As N1 79.93(7) . . ?
N2 As Cl 102.52(6) . . ?
N1 As Cl 102.14(6) . . ?
N2 As As 40.61(5) . 7_565 ?
N1 As As 40.68(5) . 7_565 ?
Cl As As 114.277(14) . 7_565 ?
C11 N1 As 127.06(7) . 7_565 ?
C11 N1 As 127.06(7) . . ?
As N1 As 98.65(9) 7_565 . ?
C21 N2 As 126.65(7) . . ?
C21 N2 As 126.65(7) . 7_565 ?
As N2 As 98.79(9) . 7_565 ?
C12 C11 C16 121.5(2) . . ?
C12 C11 N1 118.0(2) . . ?
C16 C11 N1 120.5(2) . . ?
C13 C12 C11 117.6(3) . . ?
C13 C12 C17 120.3(3) . . ?
C11 C12 C17 122.1(2) . . ?
C14 C13 C12 121.6(3) . . ?
C13 C14 C15 120.7(3) . . ?
C14 C15 C16 121.3(3) . . ?
C15 C16 C11 117.5(3) . . ?
C15 C16 C19 119.6(2) . . ?
C11 C16 C19 123.0(2) . . ?
C12 C17 C18 112.06(17) . . ?
C12 C17 C18 112.06(17) . 7_565 ?
C18 C17 C18 109.7(3) . 7_565 ?
C16 C19 C20 111.62(19) . . ?
C16 C19 C20 111.62(19) . 7_565 ?
C20 C19 C20 111.1(3) . 7_565 ?
C26 C21 C22 121.9(2) . . ?
C26 C21 N2 120.4(2) . . ?
C22 C21 N2 117.7(2) . . ?
C23 C22 C21 117.2(3) . . ?
C23 C22 C27 120.7(3) . . ?
C21 C22 C27 122.1(2) . . ?
C24 C23 C22 121.6(3) . . ?
C23 C24 C25 120.5(3) . . ?
C24 C25 C26 120.9(3) . . ?
C25 C26 C21 117.9(2) . . ?
C25 C26 C29 119.3(2) . . ?
C21 C26 C29 122.8(2) . . ?
C22 C27 C28 111.84(18) . 7_565 ?
C22 C27 C28 111.84(18) . . ?
C28 C27 C28 111.4(3) 7_565 . ?
C30 C29 C30 111.6(3) 7_565 . ?
C30 C29 C26 112.45(17) 7_565 . ?
C30 C29 C26 112.45(17) . . ?
C12S C11S C12S 120.0(3) 7 . ?
C11S C12S C13S 120.4(3) . . ?
C12S C13S C14S 120.2(3) . . ?
C13S C14S C13S 118.7(3) . 7 ?
C21S C21S C22S 120.04(17) 7 . ?
C21S C22S C23S 120.2(3) . . ?
C23S C23S C22S 119.75(18) 7 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As N2 1.8432(13) . ?
As N1 1.8451(13) . ?
As Cl 2.2392(5) . ?
As As 2.7987(4) 7_565 ?
N1 C11 1.431(3) . ?
N1 As 1.8451(13) 7_565 ?
N2 C21 1.437(3) . ?
N2 As 1.8432(13) 7_565 ?
C11 C12 1.410(4) . ?
C11 C16 1.415(3) . ?
C12 C13 1.394(4) . ?
C12 C17 1.512(4) . ?
C13 C14 1.367(5) . ?
C14 C15 1.371(5) . ?
C15 C16 1.398(4) . ?
C16 C19 1.510(4) . ?
C17 C18 1.517(3) . ?
C17 C18 1.517(3) 7_565 ?
C19 C20 1.517(3) . ?
C19 C20 1.517(3) 7_565 ?
C21 C26 1.405(4) . ?
C21 C22 1.407(4) . ?
C22 C23 1.398(4) . ?
C22 C27 1.512(4) . ?
C23 C24 1.370(5) . ?
C24 C25 1.378(5) . ?
C25 C26 1.396(4) . ?
C26 C29 1.517(4) . ?
C27 C28 1.522(3) 7_565 ?
C27 C28 1.522(3) . ?
C29 C30 1.514(3) 7_565 ?
C29 C30 1.514(3) . ?
C11S C12S 1.351(3) 7 ?
C11S C12S 1.351(3) . ?
C12S C13S 1.361(4) . ?
C13S C14S 1.372(3) . ?
C14S C13S 1.372(3) 7 ?
C21S C21S 1.342(5) 7 ?
C21S C22S 1.369(4) . ?
C22S C23S 1.374(4) . ?
C23S C23S 1.349(6) 7 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 As N1 C11 -164.0(2) . . . . ?
Cl As N1 C11 95.26(19) . . . . ?
As As N1 C11 -151.5(2) 7_565 . . . ?
N2 As N1 As -12.49(9) . . . 7_565 ?
Cl As N1 As -113.27(7) . . . 7_565 ?
N1 As N2 C21 162.7(2) . . . . ?
Cl As N2 C21 -96.96(18) . . . . ?
As As N2 C21 150.2(2) 7_565 . . . ?
N1 As N2 As 12.51(9) . . . 7_565 ?
Cl As N2 As 112.83(7) . . . 7_565 ?
As N1 C11 C12 108.14(15) 7_565 . . . ?
As N1 C11 C12 -108.14(15) . . . . ?
As N1 C11 C16 -71.86(15) 7_565 . . . ?
As N1 C11 C16 71.86(15) . . . . ?
C16 C11 C12 C13 0.0 . . . . ?
N1 C11 C12 C13 180.0 . . . . ?
C16 C11 C12 C17 180.0 . . . . ?
N1 C11 C12 C17 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C17 C12 C13 C14 180.0 . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C14 C15 C16 C11 0.0 . . . . ?
C14 C15 C16 C19 180.0 . . . . ?
C12 C11 C16 C15 0.0 . . . . ?
N1 C11 C16 C15 180.0 . . . . ?
C12 C11 C16 C19 180.0 . . . . ?
N1 C11 C16 C19 0.0 . . . . ?
C13 C12 C17 C18 -61.90(19) . . . . ?
C11 C12 C17 C18 118.10(19) . . . . ?
C13 C12 C17 C18 61.90(19) . . . 7_565 ?
C11 C12 C17 C18 -118.10(19) . . . 7_565 ?
C15 C16 C19 C20 62.5(2) . . . . ?
C11 C16 C19 C20 -117.5(2) . . . . ?
C15 C16 C19 C20 -62.5(2) . . . 7_565 ?
C11 C16 C19 C20 117.5(2) . . . 7_565 ?
As N2 C21 C26 -71.13(15) . . . . ?
As N2 C21 C26 71.13(15) 7_565 . . . ?
As N2 C21 C22 108.87(15) . . . . ?
As N2 C21 C22 -108.87(15) 7_565 . . . ?
C26 C21 C22 C23 0.0 . . . . ?
N2 C21 C22 C23 180.0 . . . . ?
C26 C21 C22 C27 180.0 . . . . ?
N2 C21 C22 C27 0.0 . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C27 C22 C23 C24 180.0 . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
C24 C25 C26 C21 0.0 . . . . ?
C24 C25 C26 C29 180.0 . . . . ?
C22 C21 C26 C25 0.0 . . . . ?
N2 C21 C26 C25 180.0 . . . . ?
C22 C21 C26 C29 180.0 . . . . ?
N2 C21 C26 C29 0.0 . . . . ?
C23 C22 C27 C28 -62.85(19) . . . 7_565 ?
C21 C22 C27 C28 117.15(19) . . . 7_565 ?
C23 C22 C27 C28 62.85(19) . . . . ?
C21 C22 C27 C28 -117.15(19) . . . . ?
C25 C26 C29 C30 63.5(2) . . . 7_565 ?
C21 C26 C29 C30 -116.5(2) . . . 7_565 ?
C25 C26 C29 C30 -63.5(2) . . . . ?
C21 C26 C29 C30 116.5(2) . . . . ?
C12S C11S C12S C13S -1.0(6) 7 . . . ?
C11S C12S C13S C14S 0.2(5) . . . . ?
C12S C13S C14S C13S 0.7(5) . . . 7 ?
C21S C21S C22S C23S -0.7(4) 7 . . . ?
C21S C22S C23S C23S 0.7(4) . . . 7 ?
