#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/93/4309355.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_4309355
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         'C24 H27 As3 Cl3 N3'
_chemical_formula_sum            'C24 H27 As3 Cl3 N3'
_chemical_formula_weight         688.60
_chemical_melting_point          489.0(10)
_chemical_name_common            'DmpNAsCl Trimer'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 96.3590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.883(3)
_cell_length_b                   9.2627(8)
_cell_length_c                   18.7383(15)
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.230
_cell_measurement_theta_min      2.291
_cell_volume                     5499.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13754
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.29
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.934
_exptl_absorpt_correction_T_max  0.3950
_exptl_absorpt_correction_T_min  0.2764
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   emperical
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.344
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5605
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0648P)²+1.2912P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                4196
_reflns_number_total             5605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050532msi20050407_085836_4.cif
_cod_data_source_block           dal04a1
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value '488-490' changed to '489.0(10)' - took
average value and fixed precision.
Automatic conversion script
Id: cif_fix_values 1391 2010-09-07 12:51:13Z saulius 
;
_cod_original_cell_volume        5499.9(8)
_cod_database_code               4309355
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
As3 As 0.174086(13) 0.09811(5) -0.01462(2) 0.02986(13) Uani 1 1 d . . .
As1 As 0.135639(13) 0.20892(5) 0.13341(2) 0.02753(13) Uani 1 1 d . . .
As2 As 0.073284(14) 0.02806(5) 0.00709(2) 0.03504(14) Uani 1 1 d . . .
Cl3 Cl 0.08872(5) -0.17625(14) 0.06750(8) 0.0610(4) Uani 1 1 d . . .
Cl1 Cl 0.13684(4) 0.05510(14) 0.22617(6) 0.0458(3) Uani 1 1 d . . .
Cl2 Cl 0.16719(4) 0.33206(13) -0.04715(6) 0.0417(3) Uani 1 1 d . . .
N3 N 0.17318(10) 0.1106(4) 0.08288(17) 0.0287(8) Uani 1 1 d . . .
N1 N 0.08690(10) 0.1614(4) 0.07781(17) 0.0279(8) Uani 1 1 d . . .
N2 N 0.11971(10) 0.0391(4) -0.04194(17) 0.0284(8) Uani 1 1 d . . .
C11 C 0.21508(14) 0.0946(5) 0.1224(2) 0.0366(11) Uani 1 1 d . . .
C12 C 0.24031(13) 0.2157(6) 0.1409(2) 0.0395(12) Uani 1 1 d . . .
C13 C 0.27894(15) 0.1930(7) 0.1813(3) 0.0511(15) Uani 1 1 d . . .
H13 H 0.2964 0.2735 0.1955 0.061 Uiso 1 1 calc R . .
C14 C 0.29269(17) 0.0550(8) 0.2015(3) 0.0652(19) Uani 1 1 d . . .
H14 H 0.3193 0.0417 0.2288 0.078 Uiso 1 1 calc R . .
C15 C 0.26779(18) -0.0610(7) 0.1820(3) 0.0581(16) Uani 1 1 d . . .
H15 H 0.2775 -0.1550 0.1958 0.070 Uiso 1 1 calc R . .
C16 C 0.22853(16) -0.0450(6) 0.1423(3) 0.0457(13) Uani 1 1 d . . .
C17 C 0.22876(14) 0.3665(6) 0.1195(3) 0.0454(13) Uani 1 1 d . . .
H17A H 0.2431 0.4338 0.1544 0.055 Uiso 1 1 calc R . .
H17B H 0.1982 0.3789 0.1181 0.055 Uiso 1 1 calc R . .
H17C H 0.2374 0.3860 0.0718 0.055 Uiso 1 1 calc R . .
C18 C 0.20196(19) -0.1753(6) 0.1229(3) 0.0627(16) Uani 1 1 d . . .
H18A H 0.2038 -0.2004 0.0725 0.075 Uiso 1 1 calc R . .
H18B H 0.1725 -0.1545 0.1297 0.075 Uiso 1 1 calc R . .
H18C H 0.2121 -0.2565 0.1536 0.075 Uiso 1 1 calc R . .
C21 C 0.05058(12) 0.2464(5) 0.0972(2) 0.0299(10) Uani 1 1 d . . .
C22 C 0.04713(13) 0.3885(5) 0.0738(2) 0.0346(10) Uani 1 1 d . . .
C23 C 0.01319(15) 0.4711(6) 0.0938(2) 0.0446(12) Uani 1 1 d . . .
H23 H 0.0105 0.5697 0.0801 0.054 Uiso 1 1 calc R . .
C24 C -0.01625(16) 0.4090(7) 0.1333(3) 0.0560(15) Uani 1 1 d . . .
H24 H -0.0395 0.4645 0.1455 0.067 Uiso 1 1 calc R . .
C25 C -0.01218(14) 0.2691(7) 0.1549(3) 0.0494(14) Uani 1 1 d . . .
H25 H -0.0326 0.2294 0.1825 0.059 Uiso 1 1 calc R . .
C26 C 0.02108(13) 0.1815(6) 0.1380(2) 0.0388(11) Uani 1 1 d . . .
C27 C 0.07804(15) 0.4580(5) 0.0302(2) 0.0402(11) Uani 1 1 d . . .
H27A H 0.0833 0.3940 -0.0095 0.048 Uiso 1 1 calc R . .
H27B H 0.1046 0.4758 0.0606 0.048 Uiso 1 1 calc R . .
H27C H 0.0665 0.5499 0.0108 0.048 Uiso 1 1 calc R . .
C28 C 0.02437(15) 0.0292(6) 0.1631(3) 0.0512(14) Uani 1 1 d . . .
H28A H 0.0086 0.0174 0.2048 0.061 Uiso 1 1 calc R . .
H28B H 0.0541 0.0048 0.1767 0.061 Uiso 1 1 calc R . .
H28C H 0.0125 -0.0350 0.1244 0.061 Uiso 1 1 calc R . .
C31 C 0.11217(13) -0.0121(5) -0.1160(2) 0.0320(10) Uani 1 1 d . . .
C32 C 0.08899(13) 0.0764(5) -0.1668(2) 0.0351(11) Uani 1 1 d . . .
C33 C 0.08258(15) 0.0260(6) -0.2377(2) 0.0448(13) Uani 1 1 d . . .
H33 H 0.0669 0.0832 -0.2733 0.054 Uiso 1 1 calc R . .
C34 C 0.09847(16) -0.1047(6) -0.2567(3) 0.0517(15) Uani 1 1 d . . .
H34 H 0.0939 -0.1366 -0.3051 0.062 Uiso 1 1 calc R . .
C35 C 0.12076(16) -0.1886(6) -0.2060(3) 0.0496(14) Uani 1 1 d . . .
H35 H 0.1316 -0.2786 -0.2198 0.059 Uiso 1 1 calc R . .
C36 C 0.12811(14) -0.1452(5) -0.1340(2) 0.0377(11) Uani 1 1 d . . .
C37 C 0.07158(15) 0.2209(5) -0.1503(3) 0.0424(12) Uani 1 1 d . . .
H37A H 0.0941 0.2809 -0.1261 0.051 Uiso 1 1 calc R . .
H37B H 0.0492 0.2088 -0.1190 0.051 Uiso 1 1 calc R . .
H37C H 0.0600 0.2678 -0.1951 0.051 Uiso 1 1 calc R . .
C38 C 0.15262(19) -0.2435(6) -0.0807(3) 0.0573(15) Uani 1 1 d . . .
H38A H 0.1805 -0.2015 -0.0661 0.069 Uiso 1 1 calc R . .
H38B H 0.1560 -0.3380 -0.1029 0.069 Uiso 1 1 calc R . .
H38C H 0.1373 -0.2551 -0.0385 0.069 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
N3 As3 N2 100.25(14) . . ?
N3 As3 Cl2 101.35(12) . . ?
N2 As3 Cl2 98.63(12) . . ?
N1 As1 N3 98.49(15) . . ?
N1 As1 Cl1 103.26(11) . . ?
N3 As1 Cl1 97.33(11) . . ?
N1 As2 N2 100.72(14) . . ?
N1 As2 Cl3 100.60(12) . . ?
N2 As2 Cl3 99.02(12) . . ?
C11 N3 As3 112.6(3) . . ?
C11 N3 As1 113.5(3) . . ?
As3 N3 As1 128.65(19) . . ?
C21 N1 As1 111.8(2) . . ?
C21 N1 As2 114.1(2) . . ?
As1 N1 As2 134.0(2) . . ?
C31 N2 As2 113.7(2) . . ?
C31 N2 As3 114.4(2) . . ?
As2 N2 As3 131.93(19) . . ?
C16 C11 C12 121.5(4) . . ?
C16 C11 N3 117.7(4) . . ?
C12 C11 N3 120.8(4) . . ?
C13 C12 C11 117.6(5) . . ?
C13 C12 C17 117.9(5) . . ?
C11 C12 C17 124.5(4) . . ?
C12 C13 C14 121.4(5) . . ?
C15 C14 C13 119.7(5) . . ?
C14 C15 C16 121.5(6) . . ?
C15 C16 C11 118.2(5) . . ?
C15 C16 C18 119.7(5) . . ?
C11 C16 C18 122.1(5) . . ?
C22 C21 C26 122.8(4) . . ?
C22 C21 N1 117.6(4) . . ?
C26 C21 N1 119.6(4) . . ?
C21 C22 C23 117.9(4) . . ?
C21 C22 C27 123.2(4) . . ?
C23 C22 C27 118.9(5) . . ?
C24 C23 C22 120.1(5) . . ?
C25 C24 C23 120.5(5) . . ?
C24 C25 C26 122.3(5) . . ?
C25 C26 C21 116.3(5) . . ?
C25 C26 C28 120.5(4) . . ?
C21 C26 C28 123.2(4) . . ?
C36 C31 C32 122.2(4) . . ?
C36 C31 N2 119.5(4) . . ?
C32 C31 N2 118.3(4) . . ?
C33 C32 C31 117.3(5) . . ?
C33 C32 C37 118.4(4) . . ?
C31 C32 C37 124.3(4) . . ?
C34 C33 C32 121.3(5) . . ?
C35 C34 C33 120.0(5) . . ?
C34 C35 C36 121.7(5) . . ?
C31 C36 C35 117.5(5) . . ?
C31 C36 C38 123.6(4) . . ?
C35 C36 C38 118.9(4) . . ?
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
As3 N3 1.834(3) . ?
As3 N2 1.836(3) . ?
As3 Cl2 2.2553(13) . ?
As1 N1 1.826(3) . ?
As1 N3 1.846(3) . ?
As1 Cl1 2.2446(12) . ?
As2 N1 1.828(3) . ?
As2 N2 1.829(3) . ?
As2 Cl3 2.2320(15) . ?
N3 C11 1.462(5) . ?
N1 C21 1.478(5) . ?
N2 C31 1.461(5) . ?
C11 C16 1.400(7) . ?
C11 C12 1.401(7) . ?
C12 C13 1.389(7) . ?
C12 C17 1.488(7) . ?
C13 C14 1.390(8) . ?
C14 C15 1.362(9) . ?
C15 C16 1.391(7) . ?
C16 C18 1.496(8) . ?
C21 C22 1.388(6) . ?
C21 C26 1.411(6) . ?
C22 C23 1.410(6) . ?
C22 C27 1.494(6) . ?
C23 C24 1.384(7) . ?
C24 C25 1.360(8) . ?
C25 C26 1.399(7) . ?
C26 C28 1.487(7) . ?
C31 C36 1.389(6) . ?
C31 C32 1.404(6) . ?
C32 C33 1.401(6) . ?
C32 C37 1.494(7) . ?
C33 C34 1.374(8) . ?
C34 C35 1.364(8) . ?
C35 C36 1.403(7) . ?
C36 C38 1.504(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 As3 N3 C11 155.2(3) . . . . ?
Cl2 As3 N3 C11 -103.8(3) . . . . ?
N2 As3 N3 As1 -52.6(3) . . . . ?
Cl2 As3 N3 As1 48.5(2) . . . . ?
N1 As1 N3 C11 -165.4(3) . . . . ?
Cl1 As1 N3 C11 -60.8(3) . . . . ?
N1 As1 N3 As3 42.5(3) . . . . ?
Cl1 As1 N3 As3 147.2(2) . . . . ?
N3 As1 N1 C21 -169.8(3) . . . . ?
Cl1 As1 N1 C21 90.6(3) . . . . ?
N3 As1 N1 As2 13.3(3) . . . . ?
Cl1 As1 N1 As2 -86.3(2) . . . . ?
N2 As2 N1 C21 143.1(3) . . . . ?
Cl3 As2 N1 C21 -115.5(3) . . . . ?
N2 As2 N1 As1 -40.0(3) . . . . ?
Cl3 As2 N1 As1 61.4(3) . . . . ?
N1 As2 N2 C31 -157.9(3) . . . . ?
Cl3 As2 N2 C31 99.4(3) . . . . ?
N1 As2 N2 As3 23.8(3) . . . . ?
Cl3 As2 N2 As3 -78.8(3) . . . . ?
N3 As3 N2 C31 -167.2(3) . . . . ?
Cl2 As3 N2 C31 89.5(3) . . . . ?
N3 As3 N2 As2 11.0(3) . . . . ?
Cl2 As3 N2 As2 -92.3(3) . . . . ?
As3 N3 C11 C16 -89.4(4) . . . . ?
As1 N3 C11 C16 114.0(4) . . . . ?
As3 N3 C11 C12 92.1(4) . . . . ?
As1 N3 C11 C12 -64.6(5) . . . . ?
C16 C11 C12 C13 -1.4(6) . . . . ?
N3 C11 C12 C13 177.1(4) . . . . ?
C16 C11 C12 C17 177.8(4) . . . . ?
N3 C11 C12 C17 -3.7(6) . . . . ?
C11 C12 C13 C14 1.4(7) . . . . ?
C17 C12 C13 C14 -177.9(4) . . . . ?
C12 C13 C14 C15 -0.6(8) . . . . ?
C13 C14 C15 C16 -0.3(8) . . . . ?
C14 C15 C16 C11 0.3(8) . . . . ?
C14 C15 C16 C18 -179.2(5) . . . . ?
C12 C11 C16 C15 0.6(7) . . . . ?
N3 C11 C16 C15 -177.9(4) . . . . ?
C12 C11 C16 C18 -179.9(5) . . . . ?
N3 C11 C16 C18 1.6(7) . . . . ?
As1 N1 C21 C22 76.8(4) . . . . ?
As2 N1 C21 C22 -105.6(4) . . . . ?
As1 N1 C21 C26 -103.3(4) . . . . ?
As2 N1 C21 C26 74.2(4) . . . . ?
C26 C21 C22 C23 1.8(6) . . . . ?
N1 C21 C22 C23 -178.4(4) . . . . ?
C26 C21 C22 C27 -179.6(4) . . . . ?
N1 C21 C22 C27 0.3(6) . . . . ?
C21 C22 C23 C24 -2.2(7) . . . . ?
C27 C22 C23 C24 179.1(4) . . . . ?
C22 C23 C24 C25 1.7(8) . . . . ?
C23 C24 C25 C26 -0.7(8) . . . . ?
C24 C25 C26 C21 0.2(7) . . . . ?
C24 C25 C26 C28 179.7(5) . . . . ?
C22 C21 C26 C25 -0.8(6) . . . . ?
N1 C21 C26 C25 179.4(4) . . . . ?
C22 C21 C26 C28 179.7(4) . . . . ?
N1 C21 C26 C28 -0.1(6) . . . . ?
As2 N2 C31 C36 -105.5(4) . . . . ?
As3 N2 C31 C36 73.1(4) . . . . ?
As2 N2 C31 C32 74.8(4) . . . . ?
As3 N2 C31 C32 -106.6(4) . . . . ?
C36 C31 C32 C33 -0.5(6) . . . . ?
N2 C31 C32 C33 179.2(4) . . . . ?
C36 C31 C32 C37 -179.3(4) . . . . ?
N2 C31 C32 C37 0.4(6) . . . . ?
C31 C32 C33 C34 -0.2(6) . . . . ?
C37 C32 C33 C34 178.7(4) . . . . ?
C32 C33 C34 C35 0.4(7) . . . . ?
C33 C34 C35 C36 0.0(7) . . . . ?
C32 C31 C36 C35 0.9(6) . . . . ?
N2 C31 C36 C35 -178.8(4) . . . . ?
C32 C31 C36 C38 -179.3(4) . . . . ?
N2 C31 C36 C38 1.0(6) . . . . ?
C34 C35 C36 C31 -0.7(7) . . . . ?
C34 C35 C36 C38 179.5(5) . . . . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30660859
