# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010


data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Schulz, A.'
'Villinger, Alexander'

_publ_contact_author_name        'Schulz, Axel'
_publ_contact_author_email       axel.schulz@uni-rostock.de

_publ_section_title              
;
Synthesis of Sterically Encumbered 2,4-Bis-m-Terphenyl-1,3-Dichloro-2,4-
cyclo-Dipnictadiazanes [m-TerNPnCl]2, (Pn = P, As)
;

# Attachment '- TerN2Pn2Cl2_submitted.cif'

data_ter_n3
_database_code_depnum_ccdc_archive 'CCDC 781907'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
2,6-(2,4,6-trimethylphenyl)azidobenzene
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H25 N3'
_chemical_formula_sum            'C24 H25 N3'
_chemical_formula_weight         355.47

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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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'

_cell_length_a                   7.6300(15)
_cell_length_b                   29.310(6)
_cell_length_c                   8.9600(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.57(3)
_cell_angle_gamma                90.00
_cell_volume                     1999.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5426
_cell_measurement_theta_min      4.760
_cell_measurement_theta_max      59.497

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9712
_exptl_absorpt_correction_T_max  0.9909
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38641
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.38
_diffrn_reflns_theta_max         29.00
_reflns_number_total             5323
_reflns_number_gt                3846
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.2408P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5323
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0504
_refine_ls_wR_factor_ref         0.1460
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
N1 N 0.55537(15) 0.12700(5) 0.82804(14) 0.0389(3) Uani 1 1 d . . .
N2 N 0.51786(14) 0.11766(4) 0.95523(13) 0.0310(3) Uani 1 1 d . . .
N3 N 0.45546(19) 0.11065(5) 1.06379(16) 0.0499(4) Uani 1 1 d . . .
C1 C 0.73295(16) 0.12784(4) 0.78562(14) 0.0256(3) Uani 1 1 d . . .
C2 C 0.75929(16) 0.15528(4) 0.66159(14) 0.0259(3) Uani 1 1 d . . .
C3 C 0.92652(17) 0.15715(5) 0.60840(15) 0.0298(3) Uani 1 1 d . . .
H3 H 0.9468 0.1758 0.5244 0.036 Uiso 1 1 calc R . .
C4 C 1.06362(18) 0.13236(5) 0.67578(16) 0.0336(3) Uani 1 1 d . . .
H4 H 1.1771 0.1337 0.6379 0.040 Uiso 1 1 calc R . .
C5 C 1.03443(18) 0.10566(5) 0.79846(16) 0.0314(3) Uani 1 1 d . . .
H5 H 1.1296 0.0890 0.8451 0.038 Uiso 1 1 calc R . .
C6 C 0.86980(17) 0.10243(4) 0.85591(14) 0.0262(3) Uani 1 1 d . . .
C7 C 0.61498(16) 0.18403(4) 0.59226(13) 0.0259(3) Uani 1 1 d . . .
C8 C 0.48936(17) 0.16517(5) 0.48953(14) 0.0295(3) Uani 1 1 d . . .
C9 C 0.36081(18) 0.19369(5) 0.42401(15) 0.0349(3) Uani 1 1 d . . .
H9 H 0.2758 0.1812 0.3536 0.042 Uiso 1 1 calc R . .
C10 C 0.35241(19) 0.23977(5) 0.45796(17) 0.0382(3) Uani 1 1 d . . .
C11 C 0.47609(19) 0.25732(5) 0.56172(17) 0.0361(3) Uani 1 1 d . . .
H11 H 0.4707 0.2887 0.5876 0.043 Uiso 1 1 calc R . .
C12 C 0.60791(17) 0.23034(5) 0.62920(14) 0.0294(3) Uani 1 1 d . . .
C13 C 0.84371(16) 0.07334(4) 0.98965(14) 0.0261(3) Uani 1 1 d . . .
C14 C 0.76809(17) 0.03011(4) 0.97277(15) 0.0284(3) Uani 1 1 d . . .
C15 C 0.73850(18) 0.00480(5) 1.10008(16) 0.0329(3) Uani 1 1 d . . .
H15 H 0.6845 -0.0243 1.0889 0.039 Uiso 1 1 calc R . .
C16 C 0.78529(19) 0.02070(5) 1.24253(16) 0.0356(3) Uani 1 1 d . . .
C17 C 0.86553(19) 0.06291(5) 1.25612(15) 0.0356(3) Uani 1 1 d . . .
H17 H 0.9016 0.0739 1.3530 0.043 Uiso 1 1 calc R . .
C18 C 0.89500(18) 0.08983(5) 1.13236(15) 0.0311(3) Uani 1 1 d . . .
C19 C 0.4927(2) 0.11554(5) 0.44979(17) 0.0399(3) Uani 1 1 d . . .
H19A H 0.3887 0.1081 0.3848 0.060 Uiso 1 1 calc R . .
H19B H 0.4930 0.0972 0.5412 0.060 Uiso 1 1 calc R . .
H19C H 0.5988 0.1089 0.3973 0.060 Uiso 1 1 calc R . .
C20 C 0.2143(3) 0.27012(7) 0.3837(2) 0.0609(5) Uani 1 1 d . . .
H20A H 0.1094 0.2698 0.4415 0.091 Uiso 1 1 calc R . .
H20B H 0.1839 0.2590 0.2822 0.091 Uiso 1 1 calc R . .
H20C H 0.2594 0.3014 0.3790 0.091 Uiso 1 1 calc R . .
C21 C 0.7405(2) 0.25125(5) 0.73970(18) 0.0399(4) Uani 1 1 d . . .
H21A H 0.8528 0.2547 0.6933 0.060 Uiso 1 1 calc R . .
H21B H 0.7566 0.2314 0.8276 0.060 Uiso 1 1 calc R . .
H21C H 0.6988 0.2813 0.7703 0.060 Uiso 1 1 calc R . .
C22 C 0.7224(2) 0.01041(5) 0.82009(16) 0.0376(3) Uani 1 1 d . . .
H22A H 0.8303 0.0048 0.7692 0.056 Uiso 1 1 calc R . .
H22B H 0.6482 0.0320 0.7614 0.056 Uiso 1 1 calc R . .
H22C H 0.6588 -0.0184 0.8303 0.056 Uiso 1 1 calc R . .
C23 C 0.7494(3) -0.00697(7) 1.37917(19) 0.0531(5) Uani 1 1 d . . .
H23A H 0.6778 0.0110 1.4447 0.080 Uiso 1 1 calc R . .
H23B H 0.8608 -0.0150 1.4330 0.080 Uiso 1 1 calc R . .
H23C H 0.6861 -0.0349 1.3486 0.080 Uiso 1 1 calc R . .
C24 C 0.9787(2) 0.13602(6) 1.15315(19) 0.0468(4) Uani 1 1 d . . .
H24A H 0.9791 0.1449 1.2587 0.070 Uiso 1 1 calc R . .
H24B H 0.9118 0.1585 1.0919 0.070 Uiso 1 1 calc R . .
H24C H 1.0997 0.1348 1.1225 0.070 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0247(6) 0.0594(8) 0.0330(6) 0.0166(6) 0.0044(5) 0.0068(5)
N2 0.0261(6) 0.0350(6) 0.0322(6) 0.0038(5) 0.0030(5) 0.0026(5)
N3 0.0397(8) 0.0729(10) 0.0386(8) 0.0116(7) 0.0134(6) 0.0097(7)
C1 0.0206(6) 0.0302(6) 0.0262(6) 0.0018(5) 0.0029(5) 0.0012(5)
C2 0.0251(6) 0.0285(6) 0.0241(6) 0.0006(5) 0.0016(5) 0.0021(5)
C3 0.0293(7) 0.0327(7) 0.0281(6) 0.0030(5) 0.0060(5) 0.0002(5)
C4 0.0241(6) 0.0398(8) 0.0378(7) 0.0022(6) 0.0099(6) 0.0030(5)
C5 0.0247(6) 0.0333(7) 0.0364(7) 0.0024(5) 0.0019(5) 0.0058(5)
C6 0.0251(6) 0.0273(6) 0.0259(6) 0.0005(5) 0.0002(5) 0.0023(5)
C7 0.0242(6) 0.0311(6) 0.0226(6) 0.0043(5) 0.0037(5) 0.0006(5)
C8 0.0273(6) 0.0372(7) 0.0241(6) 0.0034(5) 0.0042(5) -0.0024(5)
C9 0.0251(7) 0.0499(8) 0.0293(7) 0.0032(6) -0.0019(5) -0.0022(6)
C10 0.0292(7) 0.0486(8) 0.0367(8) 0.0104(6) 0.0012(6) 0.0086(6)
C11 0.0361(8) 0.0336(7) 0.0389(8) 0.0036(6) 0.0045(6) 0.0067(6)
C12 0.0277(7) 0.0331(7) 0.0277(6) 0.0031(5) 0.0031(5) 0.0006(5)
C13 0.0229(6) 0.0291(6) 0.0262(6) 0.0023(5) 0.0009(5) 0.0059(5)
C14 0.0247(6) 0.0299(6) 0.0307(7) 0.0011(5) 0.0019(5) 0.0063(5)
C15 0.0311(7) 0.0295(6) 0.0385(7) 0.0072(5) 0.0053(6) 0.0053(5)
C16 0.0317(7) 0.0448(8) 0.0310(7) 0.0106(6) 0.0054(6) 0.0112(6)
C17 0.0317(7) 0.0501(8) 0.0248(6) 0.0008(6) -0.0008(5) 0.0086(6)
C18 0.0262(6) 0.0372(7) 0.0297(7) -0.0014(5) -0.0002(5) 0.0045(5)
C19 0.0414(9) 0.0408(8) 0.0372(8) -0.0043(6) 0.0008(6) -0.0039(6)
C20 0.0464(10) 0.0688(12) 0.0659(12) 0.0107(10) -0.0104(9) 0.0238(9)
C21 0.0381(8) 0.0379(8) 0.0429(8) -0.0070(6) -0.0029(7) -0.0006(6)
C22 0.0399(8) 0.0376(7) 0.0351(7) -0.0041(6) 0.0009(6) -0.0028(6)
C23 0.0598(11) 0.0618(11) 0.0383(9) 0.0188(8) 0.0089(8) 0.0070(9)
C24 0.0532(10) 0.0459(9) 0.0409(8) -0.0097(7) -0.0007(7) -0.0095(7)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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
N1 N2 1.2232(16) . ?
N1 C1 1.4300(17) . ?
N2 N3 1.1282(17) . ?
C1 C2 1.3965(17) . ?
C1 C6 1.4000(17) . ?
C2 C3 1.3907(18) . ?
C2 C7 1.4911(17) . ?
C3 C4 1.3814(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3900(19) . ?
C5 H5 0.9500 . ?
C6 C13 1.4940(17) . ?
C7 C12 1.3989(19) . ?
C7 C8 1.4007(18) . ?
C8 C9 1.3908(19) . ?
C8 C19 1.498(2) . ?
C9 C10 1.387(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(2) . ?
C10 C20 1.502(2) . ?
C11 C12 1.3880(19) . ?
C11 H11 0.9500 . ?
C12 C21 1.502(2) . ?
C13 C14 1.3965(19) . ?
C13 C18 1.3998(18) . ?
C14 C15 1.3908(19) . ?
C14 C22 1.5057(19) . ?
C15 C16 1.385(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.382(2) . ?
C16 C23 1.508(2) . ?
C17 C18 1.391(2) . ?
C17 H17 0.9500 . ?
C18 C24 1.503(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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 N1 C1 122.14(12) . . ?
N3 N2 N1 168.48(14) . . ?
C2 C1 C6 121.61(12) . . ?
C2 C1 N1 114.03(11) . . ?
C6 C1 N1 124.31(11) . . ?
C3 C2 C1 118.43(12) . . ?
C3 C2 C7 120.29(11) . . ?
C1 C2 C7 121.19(11) . . ?
C4 C3 C2 121.02(12) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 119.44(12) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.90(12) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C5 C6 C1 117.58(12) . . ?
C5 C6 C13 120.30(11) . . ?
C1 C6 C13 122.11(11) . . ?
C12 C7 C8 120.24(12) . . ?
C12 C7 C2 119.22(11) . . ?
C8 C7 C2 120.53(12) . . ?
C9 C8 C7 118.41(13) . . ?
C9 C8 C19 120.37(13) . . ?
C7 C8 C19 121.22(12) . . ?
C10 C9 C8 122.28(13) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C11 C10 C9 118.09(13) . . ?
C11 C10 C20 120.56(15) . . ?
C9 C10 C20 121.35(15) . . ?
C10 C11 C12 121.81(14) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C7 119.15(12) . . ?
C11 C12 C21 119.67(13) . . ?
C7 C12 C21 121.17(12) . . ?
C14 C13 C18 120.15(12) . . ?
C14 C13 C6 120.38(11) . . ?
C18 C13 C6 119.48(12) . . ?
C15 C14 C13 118.83(12) . . ?
C15 C14 C22 120.02(12) . . ?
C13 C14 C22 121.14(12) . . ?
C16 C15 C14 122.07(13) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C17 C16 C15 118.02(13) . . ?
C17 C16 C23 120.77(14) . . ?
C15 C16 C23 121.21(15) . . ?
C16 C17 C18 122.02(13) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C17 C18 C13 118.86(13) . . ?
C17 C18 C24 120.04(13) . . ?
C13 C18 C24 121.10(13) . . ?
C8 C19 H19A 109.5 . . ?
C8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 H23A 109.5 . . ?
C16 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C16 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

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
C1 N1 N2 N3 176.2(7) . . . . ?
N2 N1 C1 C2 -156.13(13) . . . . ?
N2 N1 C1 C6 26.3(2) . . . . ?
C6 C1 C2 C3 -0.24(19) . . . . ?
N1 C1 C2 C3 -177.85(12) . . . . ?
C6 C1 C2 C7 -176.87(12) . . . . ?
N1 C1 C2 C7 5.52(18) . . . . ?
C1 C2 C3 C4 0.30(19) . . . . ?
C7 C2 C3 C4 176.96(12) . . . . ?
C2 C3 C4 C5 -0.6(2) . . . . ?
C3 C4 C5 C6 0.8(2) . . . . ?
C4 C5 C6 C1 -0.7(2) . . . . ?
C4 C5 C6 C13 -179.62(13) . . . . ?
C2 C1 C6 C5 0.44(19) . . . . ?
N1 C1 C6 C5 177.80(13) . . . . ?
C2 C1 C6 C13 179.33(12) . . . . ?
N1 C1 C6 C13 -3.3(2) . . . . ?
C3 C2 C7 C12 -78.24(16) . . . . ?
C1 C2 C7 C12 98.33(15) . . . . ?
C3 C2 C7 C8 100.77(15) . . . . ?
C1 C2 C7 C8 -82.66(16) . . . . ?
C12 C7 C8 C9 1.17(18) . . . . ?
C2 C7 C8 C9 -177.83(12) . . . . ?
C12 C7 C8 C19 -179.15(12) . . . . ?
C2 C7 C8 C19 1.85(19) . . . . ?
C7 C8 C9 C10 -0.6(2) . . . . ?
C19 C8 C9 C10 179.76(13) . . . . ?
C8 C9 C10 C11 -0.6(2) . . . . ?
C8 C9 C10 C20 178.90(14) . . . . ?
C9 C10 C11 C12 1.2(2) . . . . ?
C20 C10 C11 C12 -178.33(15) . . . . ?
C10 C11 C12 C7 -0.6(2) . . . . ?
C10 C11 C12 C21 179.16(14) . . . . ?
C8 C7 C12 C11 -0.63(19) . . . . ?
C2 C7 C12 C11 178.39(12) . . . . ?
C8 C7 C12 C21 179.64(12) . . . . ?
C2 C7 C12 C21 -1.35(19) . . . . ?
C5 C6 C13 C14 -101.10(15) . . . . ?
C1 C6 C13 C14 80.04(16) . . . . ?
C5 C6 C13 C18 79.18(16) . . . . ?
C1 C6 C13 C18 -99.68(15) . . . . ?
C18 C13 C14 C15 2.59(19) . . . . ?
C6 C13 C14 C15 -177.13(11) . . . . ?
C18 C13 C14 C22 -176.09(12) . . . . ?
C6 C13 C14 C22 4.19(19) . . . . ?
C13 C14 C15 C16 -1.5(2) . . . . ?
C22 C14 C15 C16 177.20(13) . . . . ?
C14 C15 C16 C17 -0.7(2) . . . . ?
C14 C15 C16 C23 179.00(14) . . . . ?
C15 C16 C17 C18 1.9(2) . . . . ?
C23 C16 C17 C18 -177.82(14) . . . . ?
C16 C17 C18 C13 -0.8(2) . . . . ?
C16 C17 C18 C24 178.47(14) . . . . ?
C14 C13 C18 C17 -1.47(19) . . . . ?
C6 C13 C18 C17 178.25(12) . . . . ?
C14 C13 C18 C24 179.25(13) . . . . ?
C6 C13 C18 C24 -1.0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        29.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.044

#=============================================================================

data_ter_h
_database_code_depnum_ccdc_archive 'CCDC 781908'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
2,6-(2,4,6-trimethylphenyl)benzene
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26'
_chemical_formula_sum            'C24 H26'
_chemical_formula_weight         314.45

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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.958(17)
_cell_length_b                   11.54(2)
_cell_length_c                   17.99(5)
_cell_angle_alpha                98.22(12)
_cell_angle_beta                 96.31(15)
_cell_angle_gamma                106.77(8)
_cell_volume                     1739(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3152
_cell_measurement_theta_min      4.708
_cell_measurement_theta_max      40.976

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             680
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9769
_exptl_absorpt_correction_T_max  0.9887
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            36100
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0210
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.16
_diffrn_reflns_theta_max         28.50
_reflns_number_total             8672
_reflns_number_gt                6794
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.2466P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8672
_refine_ls_number_parameters     446
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1395
_refine_ls_wR_factor_gt          0.1312
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
C1 C 0.69276(13) 0.54005(10) 0.32084(6) 0.0335(2) Uani 1 1 d . . .
H1 H 0.6491 0.5908 0.2939 0.040 Uiso 1 1 calc R . .
C2 C 0.59766(13) 0.42704(10) 0.32705(6) 0.0321(2) Uani 1 1 d . . .
C3 C 0.66122(14) 0.35543(11) 0.36591(7) 0.0377(3) Uani 1 1 d . . .
H3 H 0.5975 0.2760 0.3705 0.045 Uiso 1 1 calc R . .
C4 C 0.81618(15) 0.39726(12) 0.39829(7) 0.0416(3) Uani 1 1 d . . .
H4 H 0.8594 0.3471 0.4260 0.050 Uiso 1 1 calc R . .
C5 C 0.90913(14) 0.50935(11) 0.39148(7) 0.0387(3) Uani 1 1 d . . .
H5 H 1.0171 0.5372 0.4142 0.046 Uiso 1 1 calc R . .
C6 C 0.84888(13) 0.58248(10) 0.35222(7) 0.0338(2) Uani 1 1 d . . .
C7 C 0.43005(12) 0.38409(10) 0.29324(6) 0.0307(2) Uani 1 1 d . . .
C8 C 0.31401(14) 0.38636(11) 0.33731(7) 0.0347(2) Uani 1 1 d . . .
C9 C 0.15904(14) 0.34761(11) 0.30468(7) 0.0378(3) Uani 1 1 d . . .
H9 H 0.0804 0.3486 0.3359 0.045 Uiso 1 1 calc R . .
C10 C 0.11555(13) 0.30831(10) 0.22967(7) 0.0358(2) Uani 1 1 d . . .
C11 C 0.23221(14) 0.30672(10) 0.18689(7) 0.0362(2) Uani 1 1 d . . .
H11 H 0.2033 0.2795 0.1334 0.043 Uiso 1 1 calc R . .
C12 C 0.38858(13) 0.34258(11) 0.21752(6) 0.0340(2) Uani 1 1 d . . .
C13 C 0.95072(13) 0.70329(10) 0.34438(7) 0.0361(3) Uani 1 1 d . . .
C14 C 1.01072(14) 0.72085(11) 0.27896(8) 0.0385(3) Uani 1 1 d . . .
C15 C 1.11060(15) 0.83330(12) 0.27431(9) 0.0457(3) Uani 1 1 d . . .
H15 H 1.1511 0.8445 0.2283 0.055 Uiso 1 1 calc R . .
C16 C 1.15301(16) 0.92825(12) 0.33290(10) 0.0518(4) Uani 1 1 d . . .
C17 C 1.09060(17) 0.90955(12) 0.39665(10) 0.0546(4) Uani 1 1 d . . .
H17 H 1.1186 0.9762 0.4385 0.066 Uiso 1 1 calc R . .
C18 C 0.98866(15) 0.79907(12) 0.40403(8) 0.0447(3) Uani 1 1 d . . .
C19 C 0.35566(17) 0.43009(16) 0.41898(7) 0.0513(3) Uani 1 1 d . . .
H19A H 0.2645 0.4450 0.4393 0.077 Uiso 1 1 calc R . .
H19B H 0.4439 0.5069 0.4295 0.077 Uiso 1 1 calc R . .
H19C H 0.3867 0.3679 0.4432 0.077 Uiso 1 1 calc R . .
C20 C -0.05370(15) 0.26704(14) 0.19598(9) 0.0510(3) Uani 1 1 d . . .
H20A H -0.0641 0.2787 0.1430 0.076 Uiso 0.702(19) 1 calc PR A 1
H20B H -0.1090 0.3155 0.2248 0.076 Uiso 0.702(19) 1 calc PR A 1
H20C H -0.1000 0.1797 0.1978 0.076 Uiso 0.702(19) 1 calc PR A 1
H20D H -0.1185 0.2371 0.2340 0.076 Uiso 0.298(19) 1 d PR A 2
H20E H -0.0736 0.2002 0.1521 0.076 Uiso 0.298(19) 1 d PR A 2
H20F H -0.0825 0.3362 0.1792 0.076 Uiso 0.298(19) 1 d PR A 2
C21 C 0.51042(16) 0.33444(15) 0.16888(8) 0.0512(3) Uani 1 1 d . . .
H21A H 0.5694 0.4173 0.1624 0.077 Uiso 1 1 calc R . .
H21B H 0.4590 0.2840 0.1190 0.077 Uiso 1 1 calc R . .
H21C H 0.5832 0.2967 0.1932 0.077 Uiso 1 1 calc R . .
C22 C 0.9200(2) 0.78379(15) 0.47362(9) 0.0608(4) Uani 1 1 d . . .
H22A H 0.8055 0.7675 0.4623 0.091 Uiso 1 1 calc R . .
H22B H 0.9664 0.8592 0.5119 0.091 Uiso 1 1 calc R . .
H22C H 0.9421 0.7145 0.4933 0.091 Uiso 1 1 calc R . .
C23 C 0.97146(17) 0.61963(12) 0.21409(8) 0.0472(3) Uani 1 1 d . . .
H23A H 1.0127 0.5544 0.2281 0.071 Uiso 1 1 calc R . .
H23B H 1.0188 0.6498 0.1712 0.071 Uiso 1 1 calc R . .
H23C H 0.8565 0.5868 0.1995 0.071 Uiso 1 1 calc R . .
C24 C 1.2661(2) 1.04837(14) 0.32796(13) 0.0737(5) Uani 1 1 d . . .
H24A H 1.2864 1.1048 0.3767 0.111 Uiso 1 1 calc R . .
H24B H 1.2212 1.0834 0.2878 0.111 Uiso 1 1 calc R . .
H24C H 1.3653 1.0363 0.3161 0.111 Uiso 1 1 calc R . .
C25 C 0.73095(13) 0.83859(10) 0.16545(7) 0.0331(2) Uani 1 1 d . . .
H25 H 0.7732 0.7852 0.1905 0.040 Uiso 1 1 calc R . .
C26 C 0.62506(13) 0.88717(10) 0.19776(7) 0.0323(2) Uani 1 1 d . . .
C27 C 0.56639(13) 0.96474(11) 0.16205(7) 0.0358(2) Uani 1 1 d . . .
H27 H 0.4938 0.9999 0.1838 0.043 Uiso 1 1 calc R . .
C28 C 0.61114(14) 0.99171(11) 0.09602(7) 0.0388(3) Uani 1 1 d . . .
H28 H 0.5701 1.0460 0.0712 0.047 Uiso 1 1 calc R . .
C29 C 0.71542(14) 0.94141(11) 0.06436(7) 0.0373(3) Uani 1 1 d . . .
H29 H 0.7454 0.9605 0.0174 0.045 Uiso 1 1 calc R . .
C30 C 0.77666(12) 0.86461(10) 0.09908(7) 0.0319(2) Uani 1 1 d . . .
C31 C 0.57444(13) 0.85615(11) 0.26843(7) 0.0338(2) Uani 1 1 d . . .
C32 C 0.64079(16) 0.93600(12) 0.33471(7) 0.0436(3) Uani 1 1 d . . .
C33 C 0.5853(2) 0.90616(15) 0.39898(8) 0.0526(4) Uani 1 1 d . . .
H33 H 0.6307 0.9615 0.4458 0.063 Uiso 1 1 calc R . .
C34 C 0.46838(18) 0.80133(14) 0.39963(8) 0.0493(3) Uani 1 1 d . . .
C35 C 0.40781(16) 0.72242(13) 0.33403(8) 0.0442(3) Uani 1 1 d . . .
H35 H 0.3276 0.6473 0.3334 0.053 Uiso 1 1 calc R . .
C36 C 0.45906(14) 0.74789(11) 0.26822(7) 0.0373(3) Uani 1 1 d . . .
C37 C 0.89303(12) 0.81272(10) 0.06660(6) 0.0314(2) Uani 1 1 d . . .
C38 C 0.84633(13) 0.69600(10) 0.02603(7) 0.0330(2) Uani 1 1 d . . .
C39 C 0.95779(14) 0.65023(11) -0.00338(7) 0.0360(2) Uani 1 1 d . . .
H39 H 0.9247 0.5695 -0.0329 0.043 Uiso 1 1 calc R . .
C40 C 1.11454(14) 0.71687(11) 0.00840(7) 0.0355(2) Uani 1 1 d . . .
C41 C 1.15820(13) 0.83173(11) 0.04946(7) 0.0370(3) Uani 1 1 d . . .
H41 H 1.2666 0.8792 0.0590 0.044 Uiso 1 1 calc R . .
C42 C 1.05026(13) 0.88187(10) 0.07782(7) 0.0356(2) Uani 1 1 d . . .
C43 C 0.7689(2) 1.05086(14) 0.33666(10) 0.0626(4) Uani 1 1 d . . .
H43A H 0.8053 1.0946 0.3894 0.094 Uiso 1 1 calc R . .
H43B H 0.7296 1.1032 0.3063 0.094 Uiso 1 1 calc R . .
H43C H 0.8568 1.0312 0.3156 0.094 Uiso 1 1 calc R . .
C44 C 0.4055(3) 0.77444(19) 0.46958(9) 0.0713(5) Uani 1 1 d . . .
H44A H 0.3007 0.7853 0.4674 0.107 Uiso 1 1 calc R . .
H44B H 0.4766 0.8308 0.5137 0.107 Uiso 1 1 calc R . .
H44C H 0.3974 0.6893 0.4742 0.107 Uiso 1 1 calc R . .
C45 C 0.38785(17) 0.65971(13) 0.19796(8) 0.0488(3) Uani 1 1 d . . .
H45A H 0.3313 0.6970 0.1634 0.073 Uiso 1 1 calc R . .
H45B H 0.3136 0.5860 0.2094 0.073 Uiso 1 1 calc R . .
H45C H 0.4707 0.6368 0.1738 0.073 Uiso 1 1 calc R . .
C46 C 1.10213(15) 1.00933(12) 0.11883(9) 0.0498(3) Uani 1 1 d . . .
H46A H 1.2177 1.0392 0.1300 0.075 Uiso 1 1 calc R . .
H46B H 1.0589 1.0131 0.1665 0.075 Uiso 1 1 calc R . .
H46C H 1.0644 1.0610 0.0874 0.075 Uiso 1 1 calc R . .
C47 C 0.67818(14) 0.61902(12) 0.01394(8) 0.0433(3) Uani 1 1 d . . .
H47A H 0.6563 0.5811 0.0586 0.065 Uiso 1 1 calc R . .
H47B H 0.6571 0.5545 -0.0311 0.065 Uiso 1 1 calc R . .
H47C H 0.6102 0.6707 0.0064 0.065 Uiso 1 1 calc R . .
C48 C 1.23508(16) 0.66725(13) -0.02268(9) 0.0473(3) Uani 1 1 d . . .
H48A H 1.2922 0.7229 -0.0537 0.071 Uiso 1 1 calc R . .
H48B H 1.1830 0.5857 -0.0542 0.071 Uiso 1 1 calc R . .
H48C H 1.3096 0.6604 0.0193 0.071 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0312(5) 0.0376(6) 0.0340(6) 0.0070(4) 0.0024(4) 0.0147(4)
C2 0.0300(5) 0.0383(6) 0.0292(5) 0.0048(4) 0.0054(4) 0.0126(4)
C3 0.0380(6) 0.0416(6) 0.0378(6) 0.0131(5) 0.0085(5) 0.0152(5)
C4 0.0409(6) 0.0490(7) 0.0431(7) 0.0177(5) 0.0055(5) 0.0223(5)
C5 0.0310(5) 0.0459(6) 0.0407(6) 0.0064(5) -0.0003(5) 0.0173(5)
C6 0.0312(5) 0.0365(6) 0.0345(6) 0.0027(4) 0.0025(4) 0.0145(4)
C7 0.0293(5) 0.0320(5) 0.0310(5) 0.0063(4) 0.0051(4) 0.0093(4)
C8 0.0355(6) 0.0398(6) 0.0310(6) 0.0063(4) 0.0072(4) 0.0144(5)
C9 0.0318(5) 0.0420(6) 0.0423(7) 0.0090(5) 0.0112(5) 0.0131(5)
C10 0.0303(5) 0.0309(5) 0.0429(6) 0.0076(5) 0.0019(5) 0.0054(4)
C11 0.0370(6) 0.0342(5) 0.0318(6) 0.0036(4) 0.0015(5) 0.0054(5)
C12 0.0334(5) 0.0359(6) 0.0315(6) 0.0057(4) 0.0074(4) 0.0084(4)
C13 0.0276(5) 0.0339(5) 0.0456(7) 0.0036(5) -0.0034(5) 0.0130(4)
C14 0.0313(5) 0.0345(6) 0.0495(7) 0.0064(5) 0.0010(5) 0.0126(4)
C15 0.0366(6) 0.0373(6) 0.0645(9) 0.0136(6) 0.0029(6) 0.0130(5)
C16 0.0390(7) 0.0338(6) 0.0784(11) 0.0094(6) -0.0058(7) 0.0108(5)
C17 0.0502(8) 0.0352(6) 0.0696(10) -0.0081(6) -0.0140(7) 0.0165(6)
C18 0.0412(6) 0.0400(6) 0.0507(8) -0.0021(5) -0.0056(5) 0.0188(5)
C19 0.0502(7) 0.0761(10) 0.0314(6) 0.0036(6) 0.0098(5) 0.0271(7)
C20 0.0318(6) 0.0538(8) 0.0595(9) 0.0091(6) -0.0015(6) 0.0049(5)
C21 0.0431(7) 0.0723(9) 0.0350(7) 0.0019(6) 0.0123(5) 0.0144(7)
C22 0.0723(10) 0.0582(9) 0.0504(9) -0.0077(7) 0.0006(7) 0.0298(8)
C23 0.0524(7) 0.0402(6) 0.0478(7) 0.0070(6) 0.0122(6) 0.0116(6)
C24 0.0589(10) 0.0362(7) 0.1121(15) 0.0121(8) -0.0087(10) 0.0021(7)
C25 0.0306(5) 0.0334(5) 0.0389(6) 0.0101(4) 0.0069(4) 0.0132(4)
C26 0.0286(5) 0.0330(5) 0.0357(6) 0.0062(4) 0.0050(4) 0.0102(4)
C27 0.0307(5) 0.0378(6) 0.0426(6) 0.0085(5) 0.0065(5) 0.0156(4)
C28 0.0364(6) 0.0386(6) 0.0467(7) 0.0155(5) 0.0058(5) 0.0162(5)
C29 0.0360(6) 0.0381(6) 0.0412(6) 0.0148(5) 0.0099(5) 0.0120(5)
C30 0.0268(5) 0.0303(5) 0.0390(6) 0.0080(4) 0.0080(4) 0.0078(4)
C31 0.0342(5) 0.0398(6) 0.0348(6) 0.0092(5) 0.0076(4) 0.0209(5)
C32 0.0511(7) 0.0438(7) 0.0400(7) 0.0055(5) 0.0031(5) 0.0238(6)
C33 0.0728(10) 0.0608(9) 0.0347(7) 0.0050(6) 0.0040(6) 0.0401(8)
C34 0.0642(9) 0.0638(9) 0.0407(7) 0.0210(6) 0.0182(6) 0.0430(8)
C35 0.0457(7) 0.0536(7) 0.0458(7) 0.0216(6) 0.0159(6) 0.0254(6)
C36 0.0362(6) 0.0436(6) 0.0392(6) 0.0129(5) 0.0102(5) 0.0192(5)
C37 0.0285(5) 0.0334(5) 0.0352(6) 0.0108(4) 0.0091(4) 0.0106(4)
C38 0.0293(5) 0.0345(5) 0.0361(6) 0.0097(4) 0.0068(4) 0.0089(4)
C39 0.0374(6) 0.0348(6) 0.0378(6) 0.0076(5) 0.0094(5) 0.0127(5)
C40 0.0348(6) 0.0411(6) 0.0387(6) 0.0156(5) 0.0141(5) 0.0170(5)
C41 0.0277(5) 0.0391(6) 0.0462(7) 0.0142(5) 0.0106(5) 0.0085(4)
C42 0.0310(5) 0.0334(5) 0.0423(6) 0.0091(5) 0.0091(5) 0.0077(4)
C43 0.0706(10) 0.0487(8) 0.0556(9) -0.0014(7) -0.0075(8) 0.0101(7)
C44 0.1043(14) 0.0940(13) 0.0462(9) 0.0325(9) 0.0325(9) 0.0609(12)
C45 0.0478(7) 0.0461(7) 0.0470(8) 0.0100(6) 0.0089(6) 0.0051(6)
C46 0.0362(6) 0.0378(6) 0.0683(9) 0.0001(6) 0.0089(6) 0.0048(5)
C47 0.0302(6) 0.0387(6) 0.0564(8) 0.0038(5) 0.0057(5) 0.0065(5)
C48 0.0429(7) 0.0547(8) 0.0564(8) 0.0174(6) 0.0223(6) 0.0251(6)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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
C1 C2 1.364(3) . ?
C1 C6 1.366(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.358(3) . ?
C2 C7 1.468(3) . ?
C3 C4 1.362(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.351(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.361(3) . ?
C5 H5 0.9500 . ?
C6 C13 1.465(3) . ?
C7 C12 1.350(4) . ?
C7 C8 1.379(3) . ?
C8 C9 1.364(3) . ?
C8 C19 1.453(4) . ?
C9 C10 1.337(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.367(3) . ?
C10 C20 1.480(4) . ?
C11 C12 1.367(3) . ?
C11 H11 0.9500 . ?
C12 C21 1.487(3) . ?
C13 C18 1.361(4) . ?
C13 C14 1.364(4) . ?
C14 C15 1.367(3) . ?
C14 C23 1.460(4) . ?
C15 C16 1.340(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.348(4) . ?
C16 C24 1.483(3) . ?
C17 C18 1.371(3) . ?
C17 H17 0.9500 . ?
C18 C22 1.465(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 H20D 0.9821 . ?
C20 H20E 0.9821 . ?
C20 H20F 0.9821 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.350(4) . ?
C25 C26 1.374(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.361(3) . ?
C26 C31 1.454(4) . ?
C27 C28 1.344(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.367(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.356(3) . ?
C29 H29 0.9500 . ?
C30 C37 1.477(3) . ?
C31 C32 1.356(4) . ?
C31 C36 1.371(3) . ?
C32 C33 1.358(4) . ?
C32 C43 1.474(3) . ?
C33 C34 1.355(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.335(4) . ?
C34 C44 1.471(4) . ?
C35 C36 1.356(4) . ?
C35 H35 0.9500 . ?
C36 C45 1.456(4) . ?
C37 C38 1.359(3) . ?
C37 C42 1.380(3) . ?
C38 C39 1.377(3) . ?
C38 C47 1.485(3) . ?
C39 C40 1.368(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.346(3) . ?
C40 C48 1.485(3) . ?
C41 C42 1.370(3) . ?
C41 H41 0.9500 . ?
C42 C46 1.464(4) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?

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
C2 C1 C6 121.99(14) . . ?
C2 C1 H1 119.0 . . ?
C6 C1 H1 119.0 . . ?
C3 C2 C1 118.48(18) . . ?
C3 C2 C7 120.66(16) . . ?
C1 C2 C7 120.86(14) . . ?
C2 C3 C4 120.12(17) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 120.74(15) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 120.35(18) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 118.31(16) . . ?
C5 C6 C13 120.05(18) . . ?
C1 C6 C13 121.64(14) . . ?
C12 C7 C8 119.31(19) . . ?
C12 C7 C2 119.49(17) . . ?
C8 C7 C2 121.20(19) . . ?
C9 C8 C7 120.3(2) . . ?
C9 C8 C19 119.36(18) . . ?
C7 C8 C19 120.32(19) . . ?
C10 C9 C8 121.37(18) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C9 C10 C11 117.48(19) . . ?
C9 C10 C20 120.05(18) . . ?
C11 C10 C20 122.5(2) . . ?
C12 C11 C10 123.0(2) . . ?
C12 C11 H11 118.5 . . ?
C10 C11 H11 118.5 . . ?
C7 C12 C11 118.51(18) . . ?
C7 C12 C21 120.59(19) . . ?
C11 C12 C21 120.9(2) . . ?
C18 C13 C14 119.45(19) . . ?
C18 C13 C6 119.4(2) . . ?
C14 C13 C6 121.18(16) . . ?
C13 C14 C15 119.94(18) . . ?
C13 C14 C23 120.50(19) . . ?
C15 C14 C23 119.6(2) . . ?
C16 C15 C14 121.8(2) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 117.4(2) . . ?
C15 C16 C24 121.1(2) . . ?
C17 C16 C24 121.5(2) . . ?
C16 C17 C18 123.20(18) . . ?
C16 C17 H17 118.4 . . ?
C18 C17 H17 118.4 . . ?
C13 C18 C17 118.2(2) . . ?
C13 C18 C22 120.37(19) . . ?
C17 C18 C22 121.39(18) . . ?
C8 C19 H19A 109.5 . . ?
C8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
C10 C20 H20D 109.7 . . ?
C10 C20 H20E 109.7 . . ?
H20D C20 H20E 109.3 . . ?
C10 C20 H20F 109.7 . . ?
H20D C20 H20F 109.3 . . ?
H20E C20 H20F 109.3 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C14 C23 H23A 109.5 . . ?
C14 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C14 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C16 C24 H24A 109.5 . . ?
C16 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C16 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 121.84(15) . . ?
C30 C25 H25 119.1 . . ?
C26 C25 H25 119.1 . . ?
C27 C26 C25 118.79(18) . . ?
C27 C26 C31 120.04(15) . . ?
C25 C26 C31 121.17(15) . . ?
C28 C27 C26 120.02(16) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.32(16) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C30 C29 C28 120.86(18) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C25 C30 C29 118.17(16) . . ?
C25 C30 C37 120.49(15) . . ?
C29 C30 C37 121.33(17) . . ?
C32 C31 C36 120.05(19) . . ?
C32 C31 C26 119.4(2) . . ?
C36 C31 C26 120.50(18) . . ?
C31 C32 C33 117.6(2) . . ?
C31 C32 C43 121.0(2) . . ?
C33 C32 C43 121.39(19) . . ?
C34 C33 C32 123.20(19) . . ?
C34 C33 H33 118.4 . . ?
C32 C33 H33 118.4 . . ?
C35 C34 C33 118.1(2) . . ?
C35 C34 C44 119.9(2) . . ?
C33 C34 C44 121.9(2) . . ?
C34 C35 C36 121.0(2) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C35 C36 C31 119.98(18) . . ?
C35 C36 C45 118.9(2) . . ?
C31 C36 C45 121.08(19) . . ?
C38 C37 C42 119.47(15) . . ?
C38 C37 C30 120.24(15) . . ?
C42 C37 C30 120.28(17) . . ?
C37 C38 C39 118.83(16) . . ?
C37 C38 C47 120.57(15) . . ?
C39 C38 C47 120.60(18) . . ?
C40 C39 C38 122.38(18) . . ?
C40 C39 H39 118.8 . . ?
C38 C39 H39 118.8 . . ?
C41 C40 C39 117.70(15) . . ?
C41 C40 C48 119.84(16) . . ?
C39 C40 C48 122.45(18) . . ?
C40 C41 C42 121.68(16) . . ?
C40 C41 H41 119.2 . . ?
C42 C41 H41 119.2 . . ?
C41 C42 C37 119.90(18) . . ?
C41 C42 C46 119.73(16) . . ?
C37 C42 C46 120.36(15) . . ?
C32 C43 H43A 109.5 . . ?
C32 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C32 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C34 C44 H44A 109.5 . . ?
C34 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C34 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C36 C45 H45A 109.5 . . ?
C36 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C36 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C42 C46 H46A 109.5 . . ?
C42 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C42 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C38 C47 H47A 109.5 . . ?
C38 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C38 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C40 C48 H48A 109.5 . . ?
C40 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C40 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?

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
C6 C1 C2 C3 0.20(17) . . . . ?
C6 C1 C2 C7 179.57(10) . . . . ?
C1 C2 C3 C4 0.64(17) . . . . ?
C7 C2 C3 C4 -178.73(11) . . . . ?
C2 C3 C4 C5 -0.85(19) . . . . ?
C3 C4 C5 C6 0.20(19) . . . . ?
C4 C5 C6 C1 0.62(18) . . . . ?
C4 C5 C6 C13 -179.34(12) . . . . ?
C2 C1 C6 C5 -0.83(17) . . . . ?
C2 C1 C6 C13 179.13(11) . . . . ?
C3 C2 C7 C12 -103.4(2) . . . . ?
C1 C2 C7 C12 77.3(2) . . . . ?
C3 C2 C7 C8 77.2(2) . . . . ?
C1 C2 C7 C8 -102.1(2) . . . . ?
C12 C7 C8 C9 -0.30(18) . . . . ?
C2 C7 C8 C9 179.11(10) . . . . ?
C12 C7 C8 C19 179.71(12) . . . . ?
C2 C7 C8 C19 -0.88(18) . . . . ?
C7 C8 C9 C10 -0.95(19) . . . . ?
C19 C8 C9 C10 179.04(12) . . . . ?
C8 C9 C10 C11 0.92(18) . . . . ?
C8 C9 C10 C20 -179.89(12) . . . . ?
C9 C10 C11 C12 0.33(18) . . . . ?
C20 C10 C11 C12 -178.84(12) . . . . ?
C8 C7 C12 C11 1.48(17) . . . . ?
C2 C7 C12 C11 -177.94(10) . . . . ?
C8 C7 C12 C21 -177.63(12) . . . . ?
C2 C7 C12 C21 2.95(18) . . . . ?
C10 C11 C12 C7 -1.54(18) . . . . ?
C10 C11 C12 C21 177.57(12) . . . . ?
C5 C6 C13 C18 -77.5(2) . . . . ?
C1 C6 C13 C18 102.5(2) . . . . ?
C5 C6 C13 C14 101.2(2) . . . . ?
C1 C6 C13 C14 -78.8(2) . . . . ?
C18 C13 C14 C15 1.33(17) . . . . ?
C6 C13 C14 C15 -177.34(10) . . . . ?
C18 C13 C14 C23 -179.84(11) . . . . ?
C6 C13 C14 C23 1.49(17) . . . . ?
C13 C14 C15 C16 0.38(18) . . . . ?
C23 C14 C15 C16 -178.47(12) . . . . ?
C14 C15 C16 C17 -1.33(19) . . . . ?
C14 C15 C16 C24 177.73(13) . . . . ?
C15 C16 C17 C18 0.6(2) . . . . ?
C24 C16 C17 C18 -178.43(13) . . . . ?
C14 C13 C18 C17 -1.97(17) . . . . ?
C6 C13 C18 C17 176.72(11) . . . . ?
C14 C13 C18 C22 177.26(12) . . . . ?
C6 C13 C18 C22 -4.05(17) . . . . ?
C16 C17 C18 C13 1.0(2) . . . . ?
C16 C17 C18 C22 -178.20(13) . . . . ?
C30 C25 C26 C27 -0.76(17) . . . . ?
C30 C25 C26 C31 178.66(11) . . . . ?
C25 C26 C27 C28 0.59(17) . . . . ?
C31 C26 C27 C28 -178.84(11) . . . . ?
C26 C27 C28 C29 0.09(18) . . . . ?
C27 C28 C29 C30 -0.62(19) . . . . ?
C26 C25 C30 C29 0.24(17) . . . . ?
C26 C25 C30 C37 178.84(10) . . . . ?
C28 C29 C30 C25 0.45(17) . . . . ?
C28 C29 C30 C37 -178.13(11) . . . . ?
C27 C26 C31 C32 -80.5(2) . . . . ?
C25 C26 C31 C32 100.0(2) . . . . ?
C27 C26 C31 C36 98.6(2) . . . . ?
C25 C26 C31 C36 -80.8(2) . . . . ?
C36 C31 C32 C33 -2.01(17) . . . . ?
C26 C31 C32 C33 177.12(11) . . . . ?
C36 C31 C32 C43 177.85(12) . . . . ?
C26 C31 C32 C43 -3.03(18) . . . . ?
C31 C32 C33 C34 0.2(2) . . . . ?
C43 C32 C33 C34 -179.70(13) . . . . ?
C32 C33 C34 C35 1.7(2) . . . . ?
C32 C33 C34 C44 -176.96(13) . . . . ?
C33 C34 C35 C36 -1.64(19) . . . . ?
C44 C34 C35 C36 177.02(12) . . . . ?
C34 C35 C36 C31 -0.17(18) . . . . ?
C34 C35 C36 C45 -179.17(12) . . . . ?
C32 C31 C36 C35 2.05(17) . . . . ?
C26 C31 C36 C35 -177.07(10) . . . . ?
C32 C31 C36 C45 -178.97(11) . . . . ?
C26 C31 C36 C45 1.91(17) . . . . ?
C25 C30 C37 C38 81.7(2) . . . . ?
C29 C30 C37 C38 -99.8(2) . . . . ?
C25 C30 C37 C42 -97.7(2) . . . . ?
C29 C30 C37 C42 80.9(2) . . . . ?
C42 C37 C38 C39 -0.50(17) . . . . ?
C30 C37 C38 C39 -179.86(10) . . . . ?
C42 C37 C38 C47 179.22(11) . . . . ?
C30 C37 C38 C47 -0.15(18) . . . . ?
C37 C38 C39 C40 1.70(18) . . . . ?
C47 C38 C39 C40 -178.01(12) . . . . ?
C38 C39 C40 C41 -0.98(18) . . . . ?
C38 C39 C40 C48 179.45(11) . . . . ?
C39 C40 C41 C42 -0.94(19) . . . . ?
C48 C40 C41 C42 178.64(12) . . . . ?
C40 C41 C42 C37 2.12(19) . . . . ?
C40 C41 C42 C46 -176.89(13) . . . . ?
C38 C37 C42 C41 -1.35(18) . . . . ?
C30 C37 C42 C41 178.01(11) . . . . ?
C38 C37 C42 C46 177.65(12) . . . . ?
C30 C37 C42 C46 -2.98(18) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        28.50
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.041

#=============================================================================

data_ter_npcl22
_database_code_depnum_ccdc_archive 'CCDC 781909'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
N,N-bis-dichlorophosphino-2,6-bis-(2,4,6-trimethylphenyl)aniline
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H25 Cl4 N P2'
_chemical_formula_sum            'C24 H25 Cl4 N P2'
_chemical_formula_weight         531.19

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'
P P 0.1023 0.0942 '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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_Int_Tables_number      61

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   16.571(3)
_cell_length_b                   17.535(4)
_cell_length_c                   17.726(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5150.7(18)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9179
_cell_measurement_theta_min      4.646
_cell_measurement_theta_max      62.181

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2192
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_T_max  0.9482
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42834
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.61
_diffrn_reflns_theta_max         30.00
_reflns_number_total             7492
_reflns_number_gt                5347
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+1.3097P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7492
_refine_ls_number_parameters     286
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_ref         0.1265
_refine_ls_wR_factor_gt          0.1151
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
P1 P -0.03181(3) 0.28467(3) 0.28433(3) 0.03081(12) Uani 1 1 d . . .
P2 P 0.04110(3) 0.17017(3) 0.40655(3) 0.03047(12) Uani 1 1 d . . .
Cl1 Cl 0.07960(4) 0.30418(4) 0.23919(4) 0.06185(19) Uani 1 1 d . . .
Cl2 Cl -0.06256(5) 0.19561(3) 0.21429(3) 0.05612(18) Uani 1 1 d . . .
Cl3 Cl 0.15588(3) 0.19037(4) 0.36594(4) 0.05934(19) Uani 1 1 d . . .
Cl4 Cl 0.01603(4) 0.07803(3) 0.33991(3) 0.04489(14) Uani 1 1 d . . .
N N -0.01486(8) 0.24338(8) 0.37043(8) 0.0236(3) Uani 1 1 d . . .
C1 C -0.06163(10) 0.28187(9) 0.43003(9) 0.0222(3) Uani 1 1 d . . .
C2 C -0.12298(10) 0.24193(9) 0.46763(9) 0.0244(3) Uani 1 1 d . . .
C3 C -0.16694(11) 0.28012(11) 0.52303(11) 0.0306(4) Uani 1 1 d . . .
H3 H -0.2080 0.2537 0.5497 0.037 Uiso 1 1 calc R . .
C4 C -0.15186(12) 0.35554(11) 0.53976(11) 0.0323(4) Uani 1 1 d . . .
H4 H -0.1838 0.3811 0.5764 0.039 Uiso 1 1 calc R . .
C5 C -0.09020(11) 0.39415(10) 0.50326(11) 0.0294(4) Uani 1 1 d . . .
H5 H -0.0798 0.4460 0.5155 0.035 Uiso 1 1 calc R . .
C6 C -0.04327(10) 0.35787(9) 0.44892(10) 0.0233(3) Uani 1 1 d . . .
C7 C -0.14136(10) 0.16004(10) 0.45248(10) 0.0251(3) Uani 1 1 d . . .
C8 C -0.11185(11) 0.10323(10) 0.50128(11) 0.0289(4) Uani 1 1 d . . .
C9 C -0.12902(12) 0.02700(10) 0.48547(12) 0.0343(4) Uani 1 1 d . . .
H9 H -0.1078 -0.0115 0.5175 0.041 Uiso 1 1 calc R . .
C10 C -0.17608(13) 0.00594(11) 0.42436(12) 0.0372(5) Uani 1 1 d . . .
C11 C -0.20843(12) 0.06336(11) 0.37939(11) 0.0356(4) Uani 1 1 d . . .
H11 H -0.2430 0.0497 0.3388 0.043 Uiso 1 1 calc R . .
C12 C -0.19188(11) 0.14009(11) 0.39176(10) 0.0295(4) Uani 1 1 d . . .
C13 C -0.06428(14) 0.12230(12) 0.57154(12) 0.0399(5) Uani 1 1 d . . .
H13A H -0.1012 0.1274 0.6144 0.060 Uiso 1 1 calc R . .
H13B H -0.0353 0.1704 0.5640 0.060 Uiso 1 1 calc R . .
H13C H -0.0254 0.0815 0.5818 0.060 Uiso 1 1 calc R . .
C14 C -0.19203(16) -0.07711(12) 0.40701(16) 0.0526(6) Uani 1 1 d . . .
H14A H -0.1720 -0.1088 0.4486 0.079 Uiso 1 1 calc R . .
H14B H -0.1642 -0.0912 0.3603 0.079 Uiso 1 1 calc R . .
H14C H -0.2502 -0.0852 0.4010 0.079 Uiso 1 1 calc R . .
C15 C -0.23011(13) 0.20020(13) 0.34261(12) 0.0400(5) Uani 1 1 d . . .
H15A H -0.2549 0.1759 0.2985 0.060 Uiso 1 1 calc R . .
H15B H -0.1887 0.2364 0.3259 0.060 Uiso 1 1 calc R . .
H15C H -0.2715 0.2274 0.3715 0.060 Uiso 1 1 calc R . .
C16 C 0.02865(10) 0.39741(9) 0.41710(10) 0.0248(3) Uani 1 1 d . . .
C17 C 0.10441(11) 0.37984(10) 0.44767(10) 0.0271(4) Uani 1 1 d . . .
C18 C 0.17268(11) 0.41374(11) 0.41698(11) 0.0323(4) Uani 1 1 d . . .
H18 H 0.2241 0.4015 0.4373 0.039 Uiso 1 1 calc R . .
C19 C 0.16795(12) 0.46469(11) 0.35776(11) 0.0331(4) Uani 1 1 d . . .
C20 C 0.09226(12) 0.48500(11) 0.33148(11) 0.0341(4) Uani 1 1 d . . .
H20 H 0.0882 0.5219 0.2924 0.041 Uiso 1 1 calc R . .
C21 C 0.02201(11) 0.45299(10) 0.36054(11) 0.0300(4) Uani 1 1 d . . .
C22 C 0.11287(12) 0.32855(12) 0.51560(11) 0.0358(4) Uani 1 1 d . . .
H22A H 0.1700 0.3166 0.5237 0.054 Uiso 1 1 calc R . .
H22B H 0.0828 0.2812 0.5070 0.054 Uiso 1 1 calc R . .
H22C H 0.0913 0.3545 0.5602 0.054 Uiso 1 1 calc R . .
C23 C 0.24385(14) 0.49771(14) 0.32382(13) 0.0469(5) Uani 1 1 d . . .
H23A H 0.2835 0.5070 0.3638 0.070 Uiso 1 1 calc R . .
H23B H 0.2311 0.5459 0.2985 0.070 Uiso 1 1 calc R . .
H23C H 0.2663 0.4617 0.2871 0.070 Uiso 1 1 calc R . .
C24 C -0.05967(13) 0.47927(13) 0.33226(15) 0.0457(5) Uani 1 1 d . . .
H24A H -0.0611 0.5351 0.3309 0.069 Uiso 1 1 calc R . .
H24B H -0.1019 0.4605 0.3662 0.069 Uiso 1 1 calc R . .
H24C H -0.0688 0.4592 0.2814 0.069 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0425(3) 0.0264(2) 0.0235(2) 0.00350(18) 0.00251(19) 0.00139(19)
P2 0.0363(3) 0.0267(2) 0.0283(2) -0.00354(19) -0.00465(19) 0.00944(18)
Cl1 0.0614(4) 0.0798(5) 0.0443(3) 0.0032(3) 0.0227(3) -0.0160(3)
Cl2 0.0958(5) 0.0449(3) 0.0277(3) -0.0035(2) -0.0132(3) -0.0131(3)
Cl3 0.0300(3) 0.0598(4) 0.0882(5) -0.0071(3) 0.0017(3) 0.0099(2)
Cl4 0.0615(3) 0.0271(2) 0.0460(3) -0.0118(2) -0.0051(2) 0.0103(2)
N 0.0279(7) 0.0202(7) 0.0226(7) -0.0008(5) 0.0003(5) 0.0019(5)
C1 0.0250(8) 0.0209(7) 0.0206(8) -0.0002(6) -0.0031(6) 0.0028(6)
C2 0.0281(8) 0.0211(8) 0.0241(8) 0.0022(6) -0.0026(6) -0.0008(6)
C3 0.0327(9) 0.0290(9) 0.0300(9) 0.0009(7) 0.0049(7) -0.0016(7)
C4 0.0346(9) 0.0294(9) 0.0329(10) -0.0051(8) 0.0059(7) 0.0030(7)
C5 0.0357(9) 0.0212(8) 0.0313(9) -0.0032(7) 0.0000(7) 0.0013(7)
C6 0.0274(8) 0.0188(7) 0.0237(8) 0.0026(6) -0.0028(6) 0.0007(6)
C7 0.0276(8) 0.0230(8) 0.0246(8) 0.0003(7) 0.0024(6) -0.0018(6)
C8 0.0342(9) 0.0241(8) 0.0283(9) 0.0010(7) 0.0021(7) -0.0010(7)
C9 0.0411(10) 0.0226(8) 0.0390(11) 0.0045(8) 0.0079(8) -0.0001(7)
C10 0.0423(11) 0.0273(9) 0.0419(11) -0.0079(8) 0.0123(9) -0.0085(8)
C11 0.0367(10) 0.0370(10) 0.0332(10) -0.0069(8) 0.0018(8) -0.0107(8)
C12 0.0292(9) 0.0321(9) 0.0272(9) 0.0000(7) 0.0018(7) -0.0052(7)
C13 0.0526(12) 0.0353(11) 0.0319(11) 0.0047(8) -0.0074(9) 0.0014(9)
C14 0.0630(15) 0.0293(10) 0.0654(16) -0.0134(11) 0.0119(12) -0.0121(10)
C15 0.0376(11) 0.0471(12) 0.0353(11) 0.0087(9) -0.0069(8) -0.0050(9)
C16 0.0300(8) 0.0178(7) 0.0267(8) -0.0027(6) -0.0002(6) -0.0014(6)
C17 0.0310(9) 0.0225(8) 0.0278(9) -0.0014(7) -0.0035(7) -0.0012(6)
C18 0.0310(9) 0.0310(9) 0.0349(10) -0.0034(8) -0.0010(7) -0.0022(7)
C19 0.0386(10) 0.0285(9) 0.0321(10) -0.0051(8) 0.0034(7) -0.0089(7)
C20 0.0473(11) 0.0263(9) 0.0288(9) 0.0051(8) -0.0010(8) -0.0083(8)
C21 0.0364(10) 0.0217(8) 0.0318(10) 0.0015(7) -0.0046(7) -0.0001(7)
C22 0.0363(10) 0.0359(10) 0.0352(10) 0.0081(9) -0.0095(8) -0.0026(8)
C23 0.0479(12) 0.0482(13) 0.0445(12) -0.0007(10) 0.0089(10) -0.0172(10)
C24 0.0434(12) 0.0365(11) 0.0572(14) 0.0191(10) -0.0105(10) 0.0005(9)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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
P1 N 1.7125(15) . ?
P1 Cl1 2.0411(9) . ?
P1 Cl2 2.0592(8) . ?
P2 N 1.7082(15) . ?
P2 Cl4 2.0440(8) . ?
P2 Cl3 2.0643(9) . ?
N C1 1.474(2) . ?
C1 C2 1.403(2) . ?
C1 C6 1.407(2) . ?
C2 C3 1.394(2) . ?
C2 C7 1.492(2) . ?
C3 C4 1.378(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(2) . ?
C5 H5 0.9500 . ?
C6 C16 1.490(2) . ?
C7 C8 1.407(3) . ?
C7 C12 1.408(3) . ?
C8 C9 1.395(3) . ?
C8 C13 1.512(3) . ?
C9 C10 1.385(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(3) . ?
C10 C14 1.512(3) . ?
C11 C12 1.390(3) . ?
C11 H11 0.9500 . ?
C12 C15 1.507(3) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.402(2) . ?
C16 C21 1.403(3) . ?
C17 C18 1.389(3) . ?
C17 C22 1.509(3) . ?
C18 C19 1.381(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(3) . ?
C19 C23 1.510(3) . ?
C20 C21 1.391(3) . ?
C20 H20 0.9500 . ?
C21 C24 1.515(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
N P1 Cl1 105.78(6) . . ?
N P1 Cl2 104.91(6) . . ?
Cl1 P1 Cl2 96.58(4) . . ?
N P2 Cl4 105.49(6) . . ?
N P2 Cl3 103.92(6) . . ?
Cl4 P2 Cl3 96.97(3) . . ?
C1 N P2 111.16(11) . . ?
C1 N P1 111.03(10) . . ?
P2 N P1 137.80(9) . . ?
C2 C1 C6 121.09(15) . . ?
C2 C1 N 119.53(14) . . ?
C6 C1 N 119.37(15) . . ?
C3 C2 C1 118.26(16) . . ?
C3 C2 C7 118.84(15) . . ?
C1 C2 C7 122.88(15) . . ?
C4 C3 C2 121.18(17) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 120.13(17) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.78(17) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 118.46(16) . . ?
C5 C6 C16 119.76(15) . . ?
C1 C6 C16 121.57(15) . . ?
C8 C7 C12 120.04(16) . . ?
C8 C7 C2 119.99(16) . . ?
C12 C7 C2 119.88(16) . . ?
C9 C8 C7 118.96(18) . . ?
C9 C8 C13 118.94(17) . . ?
C7 C8 C13 122.08(16) . . ?
C10 C9 C8 121.83(18) . . ?
C10 C9 H9 119.1 . . ?
C8 C9 H9 119.1 . . ?
C9 C10 C11 118.17(17) . . ?
C9 C10 C14 121.0(2) . . ?
C11 C10 C14 120.9(2) . . ?
C12 C11 C10 122.26(18) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 C7 118.59(17) . . ?
C11 C12 C15 120.17(18) . . ?
C7 C12 C15 121.21(17) . . ?
C8 C13 H13A 109.5 . . ?
C8 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C8 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C21 119.96(16) . . ?
C17 C16 C6 117.90(15) . . ?
C21 C16 C6 122.10(16) . . ?
C18 C17 C16 118.95(17) . . ?
C18 C17 C22 119.46(16) . . ?
C16 C17 C22 121.50(16) . . ?
C19 C18 C17 121.91(18) . . ?
C19 C18 H18 119.0 . . ?
C17 C18 H18 119.0 . . ?
C18 C19 C20 118.27(17) . . ?
C18 C19 C23 120.27(19) . . ?
C20 C19 C23 121.46(19) . . ?
C19 C20 C21 121.98(18) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C20 C21 C16 118.64(17) . . ?
C20 C21 C24 120.15(17) . . ?
C16 C21 C24 121.19(17) . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

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
Cl4 P2 N C1 129.60(10) . . . . ?
Cl3 P2 N C1 -128.95(10) . . . . ?
Cl4 P2 N P1 -50.47(14) . . . . ?
Cl3 P2 N P1 50.98(14) . . . . ?
Cl1 P1 N C1 130.41(10) . . . . ?
Cl2 P1 N C1 -128.14(10) . . . . ?
Cl1 P1 N P2 -49.51(14) . . . . ?
Cl2 P1 N P2 51.93(14) . . . . ?
P2 N C1 C2 -65.40(17) . . . . ?
P1 N C1 C2 114.65(15) . . . . ?
P2 N C1 C6 113.80(14) . . . . ?
P1 N C1 C6 -66.15(17) . . . . ?
C6 C1 C2 C3 1.7(2) . . . . ?
N C1 C2 C3 -179.14(15) . . . . ?
C6 C1 C2 C7 -176.44(15) . . . . ?
N C1 C2 C7 2.7(2) . . . . ?
C1 C2 C3 C4 1.2(3) . . . . ?
C7 C2 C3 C4 179.36(17) . . . . ?
C2 C3 C4 C5 -2.3(3) . . . . ?
C3 C4 C5 C6 0.6(3) . . . . ?
C4 C5 C6 C1 2.1(3) . . . . ?
C4 C5 C6 C16 -172.75(17) . . . . ?
C2 C1 C6 C5 -3.3(2) . . . . ?
N C1 C6 C5 177.51(15) . . . . ?
C2 C1 C6 C16 171.49(16) . . . . ?
N C1 C6 C16 -7.7(2) . . . . ?
C3 C2 C7 C8 -78.4(2) . . . . ?
C1 C2 C7 C8 99.7(2) . . . . ?
C3 C2 C7 C12 98.1(2) . . . . ?
C1 C2 C7 C12 -83.8(2) . . . . ?
C12 C7 C8 C9 4.2(3) . . . . ?
C2 C7 C8 C9 -179.25(16) . . . . ?
C12 C7 C8 C13 -173.89(18) . . . . ?
C2 C7 C8 C13 2.6(3) . . . . ?
C7 C8 C9 C10 -1.8(3) . . . . ?
C13 C8 C9 C10 176.37(18) . . . . ?
C8 C9 C10 C11 -1.8(3) . . . . ?
C8 C9 C10 C14 178.29(19) . . . . ?
C9 C10 C11 C12 3.1(3) . . . . ?
C14 C10 C11 C12 -176.97(19) . . . . ?
C10 C11 C12 C7 -0.7(3) . . . . ?
C10 C11 C12 C15 -178.46(19) . . . . ?
C8 C7 C12 C11 -3.0(3) . . . . ?
C2 C7 C12 C11 -179.51(16) . . . . ?
C8 C7 C12 C15 174.71(17) . . . . ?
C2 C7 C12 C15 -1.8(3) . . . . ?
C5 C6 C16 C17 97.6(2) . . . . ?
C1 C6 C16 C17 -77.2(2) . . . . ?
C5 C6 C16 C21 -79.8(2) . . . . ?
C1 C6 C16 C21 105.5(2) . . . . ?
C21 C16 C17 C18 -5.1(3) . . . . ?
C6 C16 C17 C18 177.53(16) . . . . ?
C21 C16 C17 C22 171.51(17) . . . . ?
C6 C16 C17 C22 -5.9(3) . . . . ?
C16 C17 C18 C19 0.6(3) . . . . ?
C22 C17 C18 C19 -176.05(18) . . . . ?
C17 C18 C19 C20 3.4(3) . . . . ?
C17 C18 C19 C23 -177.37(18) . . . . ?
C18 C19 C20 C21 -3.1(3) . . . . ?
C23 C19 C20 C21 177.74(19) . . . . ?
C19 C20 C21 C16 -1.3(3) . . . . ?
C19 C20 C21 C24 177.5(2) . . . . ?
C17 C16 C21 C20 5.4(3) . . . . ?
C6 C16 C21 C20 -177.31(17) . . . . ?
C17 C16 C21 C24 -173.42(18) . . . . ?
C6 C16 C21 C24 3.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.067

#=============================================================================

data_ter_nhpcl2
_database_code_depnum_ccdc_archive 'CCDC 781910'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
[2,6-bis-(2,4,6-trimethylphenyl)phenyl]amino(dichloro)phosphane
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 Cl2 N P'
_chemical_formula_sum            'C24 H26 Cl2 N P'
_chemical_formula_weight         430.33

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'
P P 0.1023 0.0942 '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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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'

_cell_length_a                   9.2270(18)
_cell_length_b                   28.933(6)
_cell_length_c                   9.3780(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.25(3)
_cell_angle_gamma                90.00
_cell_volume                     2264.4(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7614
_cell_measurement_theta_min      4.875
_cell_measurement_theta_max      70.955

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7678
_exptl_absorpt_correction_T_max  0.9470
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            82257
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         32.50
_reflns_number_total             8171
_reflns_number_gt                6390
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
The H atom at N was refined freely. All other H atoms were positioned
geometrically and refined using a riding model , with C---H = 0.98
(methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+1.0654P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8171
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1188
_refine_ls_wR_factor_gt          0.1125
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.050
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
P P 0.45927(4) 0.089952(13) 0.78686(4) 0.02804(8) Uani 1 1 d . . .
Cl1 Cl 0.23165(4) 0.105407(17) 0.76580(5) 0.04442(11) Uani 1 1 d . . .
Cl2 Cl 0.41786(5) 0.107962(17) 0.55931(4) 0.04310(11) Uani 1 1 d . . .
N N 0.55832(13) 0.13601(4) 0.88563(13) 0.0286(2) Uani 1 1 d . . .
H1 H 0.506(3) 0.1594(8) 0.875(3) 0.059(7) Uiso 1 1 d . . .
C1 C 0.69975(14) 0.13283(5) 1.02981(14) 0.0241(2) Uani 1 1 d . . .
C2 C 0.82842(15) 0.10521(5) 1.04021(15) 0.0261(2) Uani 1 1 d . . .
C3 C 0.96401(16) 0.10405(6) 1.18439(17) 0.0352(3) Uani 1 1 d . . .
H3 H 1.0519 0.0850 1.1952 0.042 Uiso 1 1 calc R . .
C4 C 0.97330(17) 0.13007(7) 1.31173(17) 0.0404(4) Uani 1 1 d . . .
H4 H 1.0673 0.1291 1.4083 0.049 Uiso 1 1 calc R . .
C5 C 0.84498(17) 0.15744(6) 1.29778(16) 0.0348(3) Uani 1 1 d . . .
H5 H 0.8521 0.1756 1.3850 0.042 Uiso 1 1 calc R . .
C6 C 0.70563(15) 0.15880(5) 1.15780(14) 0.0253(2) Uani 1 1 d . . .
C7 C 0.82285(14) 0.07958(5) 0.89990(16) 0.0259(2) Uani 1 1 d . . .
C8 C 0.78682(17) 0.03216(5) 0.87920(19) 0.0336(3) Uani 1 1 d . . .
C9 C 0.77300(19) 0.01099(6) 0.7406(2) 0.0393(3) Uani 1 1 d . . .
H9 H 0.7460 -0.0209 0.7251 0.047 Uiso 1 1 calc R . .
C10 C 0.79723(18) 0.03482(6) 0.62449(19) 0.0375(3) Uani 1 1 d . . .
C11 C 0.83908(16) 0.08116(6) 0.65022(17) 0.0320(3) Uani 1 1 d . . .
H11 H 0.8592 0.0978 0.5731 0.038 Uiso 1 1 calc R . .
C12 C 0.85235(15) 0.10393(5) 0.78582(16) 0.0269(2) Uani 1 1 d . . .
C13 C 0.56212(15) 0.18527(5) 1.14564(14) 0.0256(2) Uani 1 1 d . . .
C14 C 0.44784(16) 0.16265(5) 1.18228(15) 0.0280(3) Uani 1 1 d . . .
C15 C 0.31617(18) 0.18741(6) 1.17633(18) 0.0365(3) Uani 1 1 d . . .
H15 H 0.2395 0.1722 1.2025 0.044 Uiso 1 1 calc R . .
C16 C 0.2937(2) 0.23343(7) 1.1335(2) 0.0435(4) Uani 1 1 d . . .
C17 C 0.4048(2) 0.25486(6) 1.0920(2) 0.0422(4) Uani 1 1 d . . .
H17 H 0.3888 0.2863 1.0592 0.051 Uiso 1 1 calc R . .
C18 C 0.53933(18) 0.23150(5) 1.09716(16) 0.0327(3) Uani 1 1 d . . .
C19 C 0.7616(2) 0.00440(6) 1.0028(2) 0.0476(4) Uani 1 1 d . . .
H19A H 0.7040 -0.0242 0.9556 0.071 Uiso 1 1 calc R . .
H19B H 0.6986 0.0226 1.0445 0.071 Uiso 1 1 calc R . .
H19C H 0.8657 -0.0032 1.0887 0.071 Uiso 1 1 calc R . .
C20 C 0.7768(3) 0.01157(8) 0.4729(3) 0.0574(5) Uani 1 1 d . . .
H20A H 0.6624 0.0083 0.4037 0.086 Uiso 1 1 calc R . .
H20B H 0.8270 -0.0190 0.4965 0.086 Uiso 1 1 calc R . .
H20C H 0.8279 0.0304 0.4203 0.086 Uiso 1 1 calc R . .
C21 C 0.8973(2) 0.15431(5) 0.80865(19) 0.0367(3) Uani 1 1 d . . .
H21A H 0.9192 0.1651 0.7208 0.055 Uiso 1 1 calc R . .
H21B H 0.9932 0.1584 0.9079 0.055 Uiso 1 1 calc R . .
H21C H 0.8087 0.1722 0.8121 0.055 Uiso 1 1 calc R . .
C22 C 0.4663(2) 0.11213(5) 1.22387(19) 0.0366(3) Uani 1 1 d . . .
H22A H 0.5590 0.1077 1.3255 0.055 Uiso 1 1 calc R . .
H22B H 0.4825 0.0948 1.1421 0.055 Uiso 1 1 calc R . .
H22C H 0.3694 0.1009 1.2311 0.055 Uiso 1 1 calc R . .
C23 C 0.1502(3) 0.25930(9) 1.1302(3) 0.0706(7) Uani 1 1 d . . .
H23A H 0.1576 0.2614 1.2374 0.106 Uiso 1 1 calc R . .
H23B H 0.0520 0.2428 1.0627 0.106 Uiso 1 1 calc R . .
H23C H 0.1479 0.2905 1.0883 0.106 Uiso 1 1 calc R . .
C24 C 0.6550(2) 0.25534(6) 1.0467(2) 0.0467(4) Uani 1 1 d . . .
H24A H 0.7642 0.2521 1.1295 0.070 Uiso 1 1 calc R . .
H24B H 0.6276 0.2882 1.0286 0.070 Uiso 1 1 calc R . .
H24C H 0.6484 0.2413 0.9491 0.070 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P 0.01998(14) 0.03514(19) 0.02502(16) -0.00256(13) 0.00579(12) -0.00019(12)
Cl1 0.02110(15) 0.0736(3) 0.0389(2) 0.00028(18) 0.01314(13) -0.00006(15)
Cl2 0.03455(18) 0.0716(3) 0.02183(15) -0.00881(16) 0.01076(13) -0.00460(17)
N 0.0227(5) 0.0332(6) 0.0212(5) -0.0043(4) 0.0010(4) 0.0057(4)
C1 0.0191(5) 0.0312(6) 0.0188(5) 0.0006(4) 0.0050(4) -0.0009(4)
C2 0.0199(5) 0.0327(7) 0.0248(6) 0.0034(5) 0.0086(4) 0.0006(4)
C3 0.0209(6) 0.0489(9) 0.0301(7) 0.0078(6) 0.0054(5) 0.0057(5)
C4 0.0236(6) 0.0632(11) 0.0243(6) 0.0031(6) 0.0004(5) 0.0000(6)
C5 0.0272(6) 0.0523(9) 0.0197(6) -0.0031(6) 0.0050(5) -0.0047(6)
C6 0.0213(5) 0.0336(7) 0.0192(5) -0.0008(5) 0.0068(4) -0.0036(4)
C7 0.0184(5) 0.0299(6) 0.0288(6) 0.0016(5) 0.0093(4) 0.0034(4)
C8 0.0264(6) 0.0304(7) 0.0434(8) 0.0040(6) 0.0144(6) 0.0027(5)
C9 0.0338(7) 0.0289(7) 0.0545(10) -0.0066(7) 0.0182(7) 0.0003(6)
C10 0.0286(6) 0.0423(8) 0.0416(8) -0.0114(7) 0.0149(6) 0.0027(6)
C11 0.0239(6) 0.0410(8) 0.0328(7) -0.0016(6) 0.0137(5) 0.0023(5)
C12 0.0199(5) 0.0301(6) 0.0303(6) 0.0007(5) 0.0104(5) 0.0023(4)
C13 0.0257(5) 0.0313(6) 0.0181(5) -0.0047(4) 0.0076(4) -0.0029(5)
C14 0.0277(6) 0.0341(7) 0.0225(5) -0.0043(5) 0.0112(5) -0.0018(5)
C15 0.0301(7) 0.0486(9) 0.0330(7) -0.0069(6) 0.0154(6) -0.0003(6)
C16 0.0377(8) 0.0482(9) 0.0399(8) -0.0059(7) 0.0119(7) 0.0115(7)
C17 0.0475(9) 0.0321(8) 0.0382(8) -0.0019(6) 0.0099(7) 0.0059(6)
C18 0.0369(7) 0.0323(7) 0.0246(6) -0.0033(5) 0.0088(5) -0.0054(6)
C19 0.0492(9) 0.0372(9) 0.0566(11) 0.0128(8) 0.0228(8) -0.0018(7)
C20 0.0589(12) 0.0607(12) 0.0567(11) -0.0260(10) 0.0286(10) -0.0045(9)
C21 0.0434(8) 0.0326(7) 0.0387(8) 0.0021(6) 0.0218(7) -0.0020(6)
C22 0.0426(8) 0.0370(8) 0.0373(7) 0.0010(6) 0.0239(6) -0.0052(6)
C23 0.0550(12) 0.0734(15) 0.0823(16) -0.0020(13) 0.0282(12) 0.0292(11)
C24 0.0539(10) 0.0411(9) 0.0438(9) 0.0009(7) 0.0194(8) -0.0167(8)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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
P N 1.6574(13) . ?
P Cl2 2.0678(7) . ?
P Cl1 2.0726(6) . ?
N C1 1.4263(17) . ?
N H1 0.81(2) . ?
C1 C6 1.3974(18) . ?
C1 C2 1.3996(18) . ?
C2 C3 1.3969(19) . ?
C2 C7 1.4921(19) . ?
C3 C4 1.383(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3922(19) . ?
C5 H5 0.9500 . ?
C6 C13 1.4913(19) . ?
C7 C12 1.4014(19) . ?
C7 C8 1.406(2) . ?
C8 C9 1.393(2) . ?
C8 C19 1.508(2) . ?
C9 C10 1.385(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(2) . ?
C10 C20 1.510(2) . ?
C11 C12 1.390(2) . ?
C11 H11 0.9500 . ?
C12 C21 1.505(2) . ?
C13 C18 1.400(2) . ?
C13 C14 1.4026(19) . ?
C14 C15 1.391(2) . ?
C14 C22 1.504(2) . ?
C15 C16 1.381(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(3) . ?
C16 C23 1.510(3) . ?
C17 C18 1.396(2) . ?
C17 H17 0.9500 . ?
C18 C24 1.507(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
N P Cl2 100.91(5) . . ?
N P Cl1 100.05(5) . . ?
Cl2 P Cl1 96.53(4) . . ?
C1 N P 122.77(10) . . ?
C1 N H1 115.3(16) . . ?
P N H1 116.5(16) . . ?
C6 C1 C2 121.75(11) . . ?
C6 C1 N 117.65(11) . . ?
C2 C1 N 120.59(12) . . ?
C3 C2 C1 117.65(13) . . ?
C3 C2 C7 121.42(12) . . ?
C1 C2 C7 120.88(11) . . ?
C4 C3 C2 121.52(14) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C3 C4 C5 119.64(13) . . ?
C3 C4 H4 120.2 . . ?
C5 C4 H4 120.2 . . ?
C4 C5 C6 120.95(14) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 118.46(13) . . ?
C5 C6 C13 121.29(12) . . ?
C1 C6 C13 120.17(11) . . ?
C12 C7 C8 119.80(13) . . ?
C12 C7 C2 118.59(12) . . ?
C8 C7 C2 121.61(13) . . ?
C9 C8 C7 118.70(14) . . ?
C9 C8 C19 120.05(15) . . ?
C7 C8 C19 121.24(15) . . ?
C10 C9 C8 122.25(15) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C9 C10 C11 118.07(14) . . ?
C9 C10 C20 121.40(16) . . ?
C11 C10 C20 120.53(16) . . ?
C10 C11 C12 121.76(14) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C7 119.34(13) . . ?
C11 C12 C21 120.02(13) . . ?
C7 C12 C21 120.64(13) . . ?
C18 C13 C14 120.06(13) . . ?
C18 C13 C6 121.41(12) . . ?
C14 C13 C6 118.52(12) . . ?
C15 C14 C13 119.02(14) . . ?
C15 C14 C22 120.76(13) . . ?
C13 C14 C22 120.21(12) . . ?
C16 C15 C14 121.88(15) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 C17 118.41(15) . . ?
C15 C16 C23 120.35(19) . . ?
C17 C16 C23 121.23(19) . . ?
C16 C17 C18 121.72(16) . . ?
C16 C17 H17 119.1 . . ?
C18 C17 H17 119.1 . . ?
C17 C18 C13 118.83(14) . . ?
C17 C18 C24 120.41(15) . . ?
C13 C18 C24 120.74(14) . . ?
C8 C19 H19A 109.5 . . ?
C8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 H23A 109.5 . . ?
C16 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C16 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

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
Cl2 P N C1 -134.99(10) . . . . ?
Cl1 P N C1 126.28(11) . . . . ?
P N C1 C6 -129.26(12) . . . . ?
P N C1 C2 51.92(17) . . . . ?
C6 C1 C2 C3 0.5(2) . . . . ?
N C1 C2 C3 179.29(13) . . . . ?
C6 C1 C2 C7 -176.95(12) . . . . ?
N C1 C2 C7 1.82(19) . . . . ?
C1 C2 C3 C4 -1.6(2) . . . . ?
C7 C2 C3 C4 175.88(14) . . . . ?
C2 C3 C4 C5 1.0(3) . . . . ?
C3 C4 C5 C6 0.7(3) . . . . ?
C4 C5 C6 C1 -1.8(2) . . . . ?
C4 C5 C6 C13 175.13(14) . . . . ?
C2 C1 C6 C5 1.1(2) . . . . ?
N C1 C6 C5 -177.69(13) . . . . ?
C2 C1 C6 C13 -175.81(12) . . . . ?
N C1 C6 C13 5.38(19) . . . . ?
C3 C2 C7 C12 -98.91(16) . . . . ?
C1 C2 C7 C12 78.47(16) . . . . ?
C3 C2 C7 C8 81.97(17) . . . . ?
C1 C2 C7 C8 -100.65(16) . . . . ?
C12 C7 C8 C9 -3.36(19) . . . . ?
C2 C7 C8 C9 175.75(12) . . . . ?
C12 C7 C8 C19 177.27(13) . . . . ?
C2 C7 C8 C19 -3.6(2) . . . . ?
C7 C8 C9 C10 1.5(2) . . . . ?
C19 C8 C9 C10 -179.08(15) . . . . ?
C8 C9 C10 C11 1.0(2) . . . . ?
C8 C9 C10 C20 -178.16(16) . . . . ?
C9 C10 C11 C12 -1.8(2) . . . . ?
C20 C10 C11 C12 177.37(15) . . . . ?
C10 C11 C12 C7 0.0(2) . . . . ?
C10 C11 C12 C21 -179.70(13) . . . . ?
C8 C7 C12 C11 2.61(18) . . . . ?
C2 C7 C12 C11 -176.52(11) . . . . ?
C8 C7 C12 C21 -177.67(13) . . . . ?
C2 C7 C12 C21 3.19(18) . . . . ?
C5 C6 C13 C18 91.02(17) . . . . ?
C1 C6 C13 C18 -92.14(16) . . . . ?
C5 C6 C13 C14 -89.72(16) . . . . ?
C1 C6 C13 C14 87.11(15) . . . . ?
C18 C13 C14 C15 -2.81(19) . . . . ?
C6 C13 C14 C15 177.93(12) . . . . ?
C18 C13 C14 C22 175.88(12) . . . . ?
C6 C13 C14 C22 -3.38(18) . . . . ?
C13 C14 C15 C16 0.8(2) . . . . ?
C22 C14 C15 C16 -177.84(14) . . . . ?
C14 C15 C16 C17 1.5(2) . . . . ?
C14 C15 C16 C23 -179.29(17) . . . . ?
C15 C16 C17 C18 -1.9(2) . . . . ?
C23 C16 C17 C18 178.89(17) . . . . ?
C16 C17 C18 C13 0.0(2) . . . . ?
C16 C17 C18 C24 178.14(15) . . . . ?
C14 C13 C18 C17 2.41(19) . . . . ?
C6 C13 C18 C17 -178.35(12) . . . . ?
C14 C13 C18 C24 -175.77(13) . . . . ?
C6 C13 C18 C24 3.5(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        32.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.055

#=============================================================================

data_ter_npnn
_database_code_depnum_ccdc_archive 'CCDC 781911'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

# start Validation Reply Form
_vrf_PLAT374_ter_npnn            
;
PROBLEM: Long N - N Bond N2 - N3 ... 1.47 Ang.
RESPONSE: Can be considered as normal in this compound.
;
# end Validation Reply Form

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
N,N',N'-[Tris-(trimethylsilyl)]hydrazino-
[2,6-bis-(2,4,6-(trimethylphenyl)phenyl]imino-phosphane
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H52 N3 P Si3'
_chemical_formula_sum            'C33 H52 N3 P Si3'
_chemical_formula_weight         606.02

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.684(2)
_cell_length_b                   11.033(2)
_cell_length_c                   16.094(3)
_cell_angle_alpha                86.43(3)
_cell_angle_beta                 82.08(3)
_cell_angle_gamma                75.71(3)
_cell_volume                     1820.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6478
_cell_measurement_theta_min      4.647
_cell_measurement_theta_max      60.541

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9318
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18998
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.33
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7942
_reflns_number_gt                6071
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.1990P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7942
_refine_ls_number_parameters     376
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0426
_refine_ls_wR_factor_ref         0.1193
_refine_ls_wR_factor_gt          0.1117
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
P P 0.22165(4) 0.80871(4) 0.27332(3) 0.02624(12) Uani 1 1 d . . .
Si1 Si 0.47221(5) 0.71538(5) 0.14948(3) 0.03304(14) Uani 1 1 d . . .
Si2 Si 0.33128(5) 1.07244(5) 0.20072(4) 0.03735(14) Uani 1 1 d . . .
Si3 Si 0.48104(5) 0.91158(5) 0.33941(3) 0.03113(13) Uani 1 1 d . . .
N1 N 0.19524(13) 0.69203(14) 0.23538(8) 0.0267(3) Uani 1 1 d . . .
N2 N 0.36518(13) 0.82005(13) 0.22334(8) 0.0243(3) Uani 1 1 d . . .
N3 N 0.40462(13) 0.93023(13) 0.24790(8) 0.0250(3) Uani 1 1 d . . .
C1 C 0.62504(18) 0.7694(2) 0.13050(12) 0.0388(5) Uani 1 1 d . . .
H1A H 0.6057 0.8574 0.1115 0.058 Uiso 1 1 calc R . .
H1B H 0.6856 0.7187 0.0873 0.058 Uiso 1 1 calc R . .
H1C H 0.6647 0.7607 0.1826 0.058 Uiso 1 1 calc R . .
C2 C 0.4025(2) 0.7195(3) 0.04972(13) 0.0578(7) Uani 1 1 d . . .
H2A H 0.3115 0.7142 0.0620 0.087 Uiso 1 1 calc R . .
H2B H 0.4524 0.6487 0.0159 0.087 Uiso 1 1 calc R . .
H2C H 0.4066 0.7980 0.0186 0.087 Uiso 1 1 calc R . .
C3 C 0.5041(2) 0.5530(2) 0.19447(17) 0.0600(7) Uani 1 1 d . . .
H3A H 0.5429 0.5500 0.2466 0.090 Uiso 1 1 calc R . .
H3B H 0.5643 0.4965 0.1542 0.090 Uiso 1 1 calc R . .
H3C H 0.4220 0.5269 0.2064 0.090 Uiso 1 1 calc R . .
C4 C 0.3113(3) 1.0489(3) 0.09094(15) 0.0659(7) Uani 1 1 d . . .
H4A H 0.3972 1.0199 0.0585 0.099 Uiso 1 1 calc R . .
H4B H 0.2655 1.1281 0.0663 0.099 Uiso 1 1 calc R . .
H4C H 0.2607 0.9861 0.0899 0.099 Uiso 1 1 calc R . .
C5 C 0.1674(2) 1.1451(2) 0.25580(19) 0.0649(7) Uani 1 1 d . . .
H5A H 0.1075 1.0924 0.2504 0.097 Uiso 1 1 calc R . .
H5B H 0.1348 1.2282 0.2307 0.097 Uiso 1 1 calc R . .
H5C H 0.1736 1.1530 0.3153 0.097 Uiso 1 1 calc R . .
C6 C 0.4380(3) 1.1823(2) 0.2031(2) 0.0671(8) Uani 1 1 d . . .
H6A H 0.4460 1.1961 0.2615 0.101 Uiso 1 1 calc R . .
H6B H 0.3997 1.2621 0.1758 0.101 Uiso 1 1 calc R . .
H6C H 0.5243 1.1463 0.1733 0.101 Uiso 1 1 calc R . .
C7 C 0.6361(2) 0.9637(2) 0.32117(14) 0.0509(6) Uani 1 1 d . . .
H7A H 0.6914 0.9212 0.2726 0.076 Uiso 1 1 calc R . .
H7B H 0.6816 0.9429 0.3710 0.076 Uiso 1 1 calc R . .
H7C H 0.6168 1.0544 0.3103 0.076 Uiso 1 1 calc R . .
C8 C 0.5217(2) 0.7452(2) 0.37437(14) 0.0552(6) Uani 1 1 d . . .
H8A H 0.4418 0.7152 0.3859 0.083 Uiso 1 1 calc R . .
H8B H 0.5637 0.7367 0.4255 0.083 Uiso 1 1 calc R . .
H8C H 0.5810 0.6955 0.3302 0.083 Uiso 1 1 calc R . .
C9 C 0.3686(2) 1.0035(3) 0.42440(15) 0.0709(9) Uani 1 1 d . . .
H9A H 0.3540 1.0929 0.4095 0.106 Uiso 1 1 calc R . .
H9B H 0.4073 0.9867 0.4770 0.106 Uiso 1 1 calc R . .
H9C H 0.2854 0.9793 0.4315 0.106 Uiso 1 1 calc R . .
C10 C 0.08700(16) 0.64108(16) 0.26036(10) 0.0246(3) Uani 1 1 d . . .
C11 C 0.01844(16) 0.61711(16) 0.19747(10) 0.0257(4) Uani 1 1 d . . .
C12 C -0.08383(19) 0.55926(19) 0.21903(12) 0.0357(4) Uani 1 1 d . . .
H12 H -0.1304 0.5430 0.1765 0.043 Uiso 1 1 calc R . .
C13 C -0.1188(2) 0.5250(2) 0.30149(12) 0.0432(5) Uani 1 1 d . . .
H13 H -0.1888 0.4855 0.3155 0.052 Uiso 1 1 calc R . .
C14 C -0.05112(19) 0.5488(2) 0.36332(11) 0.0374(5) Uani 1 1 d . . .
H14 H -0.0749 0.5247 0.4199 0.045 Uiso 1 1 calc R . .
C15 C 0.05075(16) 0.60711(17) 0.34466(10) 0.0276(4) Uani 1 1 d . . .
C16 C 0.12074(16) 0.63049(17) 0.41404(10) 0.0265(4) Uani 1 1 d . . .
C17 C 0.23289(17) 0.54253(17) 0.43334(11) 0.0305(4) Uani 1 1 d . . .
C18 C 0.29769(19) 0.5662(2) 0.49712(11) 0.0361(4) Uani 1 1 d . . .
H18 H 0.3737 0.5063 0.5099 0.043 Uiso 1 1 calc R . .
C19 C 0.2556(2) 0.6739(2) 0.54267(11) 0.0389(5) Uani 1 1 d . . .
C20 C 0.1427(2) 0.7579(2) 0.52454(11) 0.0418(5) Uani 1 1 d . . .
H20 H 0.1109 0.8313 0.5564 0.050 Uiso 1 1 calc R . .
C21 C 0.07385(18) 0.73852(18) 0.46096(11) 0.0332(4) Uani 1 1 d . . .
C22 C 0.05473(16) 0.65157(16) 0.10749(10) 0.0250(4) Uani 1 1 d . . .
C23 C 0.13173(17) 0.55970(16) 0.05313(10) 0.0270(4) Uani 1 1 d . . .
C24 C 0.16505(17) 0.59272(17) -0.03019(10) 0.0296(4) Uani 1 1 d . . .
H24 H 0.2182 0.5305 -0.0666 0.036 Uiso 1 1 calc R . .
C25 C 0.12338(18) 0.71315(18) -0.06192(10) 0.0307(4) Uani 1 1 d . . .
C26 C 0.04530(18) 0.80234(17) -0.00752(11) 0.0320(4) Uani 1 1 d . . .
H26 H 0.0142 0.8852 -0.0285 0.038 Uiso 1 1 calc R . .
C27 C 0.01117(17) 0.77406(16) 0.07683(11) 0.0279(4) Uani 1 1 d . . .
C28 C 0.2799(2) 0.4223(2) 0.38668(14) 0.0474(5) Uani 1 1 d . . .
H28A H 0.3596 0.3727 0.4072 0.071 Uiso 1 1 calc R . .
H28B H 0.2979 0.4413 0.3266 0.071 Uiso 1 1 calc R . .
H28C H 0.2127 0.3747 0.3959 0.071 Uiso 1 1 calc R . .
C29 C 0.3307(3) 0.7001(3) 0.60930(14) 0.0603(7) Uani 1 1 d . . .
H29A H 0.3768 0.6208 0.6338 0.090 Uiso 1 1 calc R . .
H29B H 0.2704 0.7493 0.6533 0.090 Uiso 1 1 calc R . .
H29C H 0.3939 0.7472 0.5842 0.090 Uiso 1 1 calc R . .
C30 C -0.0487(2) 0.8330(2) 0.44355(15) 0.0526(6) Uani 1 1 d . . .
H30A H -0.0372 0.8665 0.3859 0.079 Uiso 1 1 calc R . .
H30B H -0.0670 0.9014 0.4829 0.079 Uiso 1 1 calc R . .
H30C H -0.1216 0.7925 0.4505 0.079 Uiso 1 1 calc R . .
C31 C 0.1807(2) 0.42755(18) 0.08440(13) 0.0433(5) Uani 1 1 d . . .
H31A H 0.1145 0.3805 0.0821 0.065 Uiso 1 1 calc R . .
H31B H 0.1985 0.4280 0.1425 0.065 Uiso 1 1 calc R . .
H31C H 0.2608 0.3879 0.0490 0.065 Uiso 1 1 calc R . .
C32 C 0.1632(2) 0.7470(2) -0.15262(11) 0.0439(5) Uani 1 1 d . . .
H32A H 0.2584 0.7252 -0.1646 0.066 Uiso 1 1 calc R . .
H32B H 0.1300 0.8370 -0.1626 0.066 Uiso 1 1 calc R . .
H32C H 0.1269 0.7006 -0.1894 0.066 Uiso 1 1 calc R . .
C33 C -0.0689(2) 0.87579(18) 0.13375(12) 0.0382(5) Uani 1 1 d . . .
H33A H -0.0111 0.9172 0.1573 0.057 Uiso 1 1 calc R . .
H33B H -0.1198 0.8391 0.1794 0.057 Uiso 1 1 calc R . .
H33C H -0.1280 0.9372 0.1016 0.057 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P 0.0235(2) 0.0278(3) 0.0281(2) -0.00105(17) -0.00022(16) -0.00910(18)
Si1 0.0325(3) 0.0345(3) 0.0329(3) -0.0092(2) 0.0044(2) -0.0124(2)
Si2 0.0352(3) 0.0277(3) 0.0489(3) 0.0084(2) -0.0085(2) -0.0076(2)
Si3 0.0265(3) 0.0434(3) 0.0246(2) -0.0049(2) -0.00291(18) -0.0096(2)
N1 0.0271(7) 0.0336(8) 0.0225(7) 0.0003(6) -0.0019(5) -0.0139(6)
N2 0.0248(7) 0.0253(8) 0.0247(7) -0.0009(6) -0.0028(5) -0.0098(6)
N3 0.0263(7) 0.0230(7) 0.0279(7) -0.0003(6) -0.0047(6) -0.0096(6)
C1 0.0315(10) 0.0447(12) 0.0386(10) -0.0097(9) 0.0052(8) -0.0096(9)
C2 0.0565(14) 0.0881(19) 0.0387(11) -0.0245(12) 0.0030(10) -0.0351(13)
C3 0.0567(14) 0.0306(12) 0.0843(18) -0.0092(11) 0.0175(13) -0.0075(11)
C4 0.0814(19) 0.0591(16) 0.0523(14) 0.0230(12) -0.0251(13) -0.0042(14)
C5 0.0435(13) 0.0415(14) 0.098(2) 0.0097(13) -0.0051(13) 0.0056(11)
C6 0.0586(16) 0.0358(13) 0.111(2) 0.0176(14) -0.0191(15) -0.0189(12)
C7 0.0418(12) 0.0732(17) 0.0464(12) -0.0079(11) -0.0110(9) -0.0261(12)
C8 0.0581(15) 0.0680(17) 0.0419(12) 0.0210(11) -0.0201(10) -0.0175(13)
C9 0.0505(14) 0.115(2) 0.0409(12) -0.0341(14) -0.0010(10) -0.0032(15)
C10 0.0239(8) 0.0245(9) 0.0253(8) 0.0002(6) -0.0010(6) -0.0070(7)
C11 0.0270(9) 0.0258(9) 0.0256(8) 0.0014(7) -0.0036(6) -0.0093(7)
C12 0.0382(10) 0.0442(12) 0.0326(9) 0.0054(8) -0.0116(8) -0.0225(9)
C13 0.0413(11) 0.0619(14) 0.0369(10) 0.0115(9) -0.0066(8) -0.0346(11)
C14 0.0379(10) 0.0517(13) 0.0277(9) 0.0073(8) -0.0033(7) -0.0231(9)
C15 0.0263(9) 0.0323(10) 0.0249(8) 0.0001(7) -0.0017(6) -0.0090(7)
C16 0.0267(9) 0.0334(10) 0.0207(7) 0.0023(7) 0.0001(6) -0.0122(7)
C17 0.0302(9) 0.0331(10) 0.0282(8) 0.0059(7) -0.0017(7) -0.0107(8)
C18 0.0312(10) 0.0471(12) 0.0329(9) 0.0127(8) -0.0086(7) -0.0159(9)
C19 0.0443(11) 0.0551(13) 0.0263(9) 0.0072(8) -0.0067(8) -0.0300(10)
C20 0.0562(13) 0.0451(12) 0.0277(9) -0.0090(8) 0.0046(9) -0.0225(10)
C21 0.0338(10) 0.0354(11) 0.0282(9) -0.0020(7) 0.0030(7) -0.0078(8)
C22 0.0268(8) 0.0269(9) 0.0244(8) 0.0004(6) -0.0060(6) -0.0110(7)
C23 0.0313(9) 0.0243(9) 0.0273(8) -0.0011(7) -0.0092(7) -0.0071(7)
C24 0.0340(10) 0.0290(10) 0.0260(8) -0.0054(7) -0.0051(7) -0.0061(8)
C25 0.0362(10) 0.0342(10) 0.0242(8) 0.0012(7) -0.0055(7) -0.0129(8)
C26 0.0355(10) 0.0270(10) 0.0337(9) 0.0052(7) -0.0053(7) -0.0090(8)
C27 0.0281(9) 0.0245(9) 0.0316(9) 0.0001(7) -0.0020(7) -0.0086(7)
C28 0.0455(12) 0.0382(12) 0.0542(13) -0.0015(10) -0.0071(10) -0.0014(10)
C29 0.0741(17) 0.088(2) 0.0376(11) 0.0093(12) -0.0197(11) -0.0504(15)
C30 0.0452(13) 0.0489(14) 0.0546(13) -0.0107(11) 0.0018(10) 0.0040(10)
C31 0.0539(13) 0.0296(11) 0.0404(11) 0.0021(8) -0.0058(9) 0.0003(9)
C32 0.0586(13) 0.0436(12) 0.0273(9) 0.0044(8) -0.0023(9) -0.0113(10)
C33 0.0426(11) 0.0291(10) 0.0385(10) -0.0011(8) 0.0050(8) -0.0059(9)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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
P N1 1.5601(15) . ?
P N2 1.6603(14) . ?
Si1 N2 1.7886(16) . ?
Si1 C1 1.854(2) . ?
Si1 C2 1.854(2) . ?
Si1 C3 1.859(2) . ?
Si2 N3 1.7495(17) . ?
Si2 C4 1.850(3) . ?
Si2 C5 1.861(3) . ?
Si2 C6 1.862(2) . ?
Si3 N3 1.7574(16) . ?
Si3 C8 1.849(3) . ?
Si3 C9 1.861(2) . ?
Si3 C7 1.865(2) . ?
N1 C10 1.407(2) . ?
N2 N3 1.4731(19) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.401(2) . ?
C10 C15 1.412(2) . ?
C11 C12 1.391(2) . ?
C11 C22 1.497(2) . ?
C12 C13 1.383(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(2) . ?
C14 H14 0.9500 . ?
C15 C16 1.495(2) . ?
C16 C21 1.398(2) . ?
C16 C17 1.402(3) . ?
C17 C18 1.385(3) . ?
C17 C28 1.506(3) . ?
C18 C19 1.380(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(3) . ?
C19 C29 1.506(3) . ?
C20 C21 1.395(3) . ?
C20 H20 0.9500 . ?
C21 C30 1.507(3) . ?
C22 C27 1.399(2) . ?
C22 C23 1.404(2) . ?
C23 C24 1.389(2) . ?
C23 C31 1.502(3) . ?
C24 C25 1.382(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(3) . ?
C25 C32 1.513(2) . ?
C26 C27 1.393(2) . ?
C26 H26 0.9500 . ?
C27 C33 1.506(2) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

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
N1 P N2 104.22(8) . . ?
N2 Si1 C1 105.88(8) . . ?
N2 Si1 C2 111.39(10) . . ?
C1 Si1 C2 110.08(10) . . ?
N2 Si1 C3 109.94(9) . . ?
C1 Si1 C3 110.29(11) . . ?
C2 Si1 C3 109.21(13) . . ?
N3 Si2 C4 110.25(10) . . ?
N3 Si2 C5 112.77(10) . . ?
C4 Si2 C5 107.48(14) . . ?
N3 Si2 C6 108.03(10) . . ?
C4 Si2 C6 109.96(14) . . ?
C5 Si2 C6 108.31(13) . . ?
N3 Si3 C8 110.63(9) . . ?
N3 Si3 C9 109.21(10) . . ?
C8 Si3 C9 108.52(13) . . ?
N3 Si3 C7 111.35(9) . . ?
C8 Si3 C7 107.31(12) . . ?
C9 Si3 C7 109.76(12) . . ?
C10 N1 P 125.73(11) . . ?
N3 N2 P 112.41(10) . . ?
N3 N2 Si1 119.41(10) . . ?
P N2 Si1 128.15(8) . . ?
N2 N3 Si2 115.26(10) . . ?
N2 N3 Si3 116.02(11) . . ?
Si2 N3 Si3 126.19(9) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si3 C7 H7A 109.5 . . ?
Si3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si3 C8 H8A 109.5 . . ?
Si3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si3 C9 H9A 109.5 . . ?
Si3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 N1 117.66(14) . . ?
C11 C10 C15 119.64(15) . . ?
N1 C10 C15 122.58(15) . . ?
C12 C11 C10 119.39(15) . . ?
C12 C11 C22 119.65(15) . . ?
C10 C11 C22 120.95(14) . . ?
C13 C12 C11 121.04(17) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C12 119.44(17) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 121.39(17) . . ?
C13 C14 H14 119.3 . . ?
C15 C14 H14 119.3 . . ?
C14 C15 C10 119.09(16) . . ?
C14 C15 C16 119.15(15) . . ?
C10 C15 C16 121.75(15) . . ?
C21 C16 C17 119.65(16) . . ?
C21 C16 C15 120.47(17) . . ?
C17 C16 C15 119.87(16) . . ?
C18 C17 C16 119.22(17) . . ?
C18 C17 C28 120.59(18) . . ?
C16 C17 C28 120.17(17) . . ?
C19 C18 C17 122.22(19) . . ?
C19 C18 H18 118.9 . . ?
C17 C18 H18 118.9 . . ?
C18 C19 C20 117.83(18) . . ?
C18 C19 C29 121.3(2) . . ?
C20 C19 C29 120.9(2) . . ?
C19 C20 C21 122.17(18) . . ?
C19 C20 H20 118.9 . . ?
C21 C20 H20 118.9 . . ?
C20 C21 C16 118.86(18) . . ?
C20 C21 C30 120.17(18) . . ?
C16 C21 C30 120.98(18) . . ?
C27 C22 C23 119.70(15) . . ?
C27 C22 C11 120.62(15) . . ?
C23 C22 C11 119.68(16) . . ?
C24 C23 C22 119.21(16) . . ?
C24 C23 C31 119.88(16) . . ?
C22 C23 C31 120.89(16) . . ?
C25 C24 C23 122.15(16) . . ?
C25 C24 H24 118.9 . . ?
C23 C24 H24 118.9 . . ?
C24 C25 C26 117.81(16) . . ?
C24 C25 C32 120.99(17) . . ?
C26 C25 C32 121.19(17) . . ?
C25 C26 C27 122.06(17) . . ?
C25 C26 H26 119.0 . . ?
C27 C26 H26 119.0 . . ?
C26 C27 C22 119.05(16) . . ?
C26 C27 C33 119.76(16) . . ?
C22 C27 C33 121.18(15) . . ?
C17 C28 H28A 109.5 . . ?
C17 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C17 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C19 C29 H29A 109.5 . . ?
C19 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C19 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C21 C30 H30A 109.5 . . ?
C21 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C21 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C23 C31 H31A 109.5 . . ?
C23 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C23 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C25 C32 H32A 109.5 . . ?
C25 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C25 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C27 C33 H33A 109.5 . . ?
C27 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C27 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

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 P N1 C10 177.17(14) . . . . ?
N1 P N2 N3 177.12(11) . . . . ?
N1 P N2 Si1 -4.83(13) . . . . ?
C1 Si1 N2 N3 6.37(14) . . . . ?
C2 Si1 N2 N3 -113.29(14) . . . . ?
C3 Si1 N2 N3 125.50(14) . . . . ?
C1 Si1 N2 P -171.57(11) . . . . ?
C2 Si1 N2 P 68.77(14) . . . . ?
C3 Si1 N2 P -52.44(15) . . . . ?
P N2 N3 Si2 -79.19(12) . . . . ?
Si1 N2 N3 Si2 102.57(12) . . . . ?
P N2 N3 Si3 83.93(12) . . . . ?
Si1 N2 N3 Si3 -94.32(12) . . . . ?
C4 Si2 N3 N2 -36.78(15) . . . . ?
C5 Si2 N3 N2 83.36(14) . . . . ?
C6 Si2 N3 N2 -156.96(13) . . . . ?
C4 Si2 N3 Si3 162.09(13) . . . . ?
C5 Si2 N3 Si3 -77.76(14) . . . . ?
C6 Si2 N3 Si3 41.91(14) . . . . ?
C8 Si3 N3 N2 10.32(14) . . . . ?
C9 Si3 N3 N2 -109.06(15) . . . . ?
C7 Si3 N3 N2 129.56(12) . . . . ?
C8 Si3 N3 Si2 171.32(11) . . . . ?
C9 Si3 N3 Si2 51.94(15) . . . . ?
C7 Si3 N3 Si2 -69.44(13) . . . . ?
P N1 C10 C11 130.24(15) . . . . ?
P N1 C10 C15 -53.6(2) . . . . ?
N1 C10 C11 C12 175.83(16) . . . . ?
C15 C10 C11 C12 -0.5(3) . . . . ?
N1 C10 C11 C22 -3.5(2) . . . . ?
C15 C10 C11 C22 -179.79(15) . . . . ?
C10 C11 C12 C13 0.0(3) . . . . ?
C22 C11 C12 C13 179.30(19) . . . . ?
C11 C12 C13 C14 0.0(3) . . . . ?
C12 C13 C14 C15 0.4(3) . . . . ?
C13 C14 C15 C10 -0.9(3) . . . . ?
C13 C14 C15 C16 -179.96(19) . . . . ?
C11 C10 C15 C14 1.0(3) . . . . ?
N1 C10 C15 C14 -175.17(17) . . . . ?
C11 C10 C15 C16 179.94(16) . . . . ?
N1 C10 C15 C16 3.8(3) . . . . ?
C14 C15 C16 C21 -86.0(2) . . . . ?
C10 C15 C16 C21 95.0(2) . . . . ?
C14 C15 C16 C17 92.8(2) . . . . ?
C10 C15 C16 C17 -86.2(2) . . . . ?
C21 C16 C17 C18 -2.0(2) . . . . ?
C15 C16 C17 C18 179.19(15) . . . . ?
C21 C16 C17 C28 176.39(17) . . . . ?
C15 C16 C17 C28 -2.5(2) . . . . ?
C16 C17 C18 C19 0.0(3) . . . . ?
C28 C17 C18 C19 -178.32(18) . . . . ?
C17 C18 C19 C20 1.9(3) . . . . ?
C17 C18 C19 C29 -177.43(17) . . . . ?
C18 C19 C20 C21 -1.9(3) . . . . ?
C29 C19 C20 C21 177.43(18) . . . . ?
C19 C20 C21 C16 0.0(3) . . . . ?
C19 C20 C21 C30 -179.94(18) . . . . ?
C17 C16 C21 C20 2.0(3) . . . . ?
C15 C16 C21 C20 -179.21(16) . . . . ?
C17 C16 C21 C30 -178.13(17) . . . . ?
C15 C16 C21 C30 0.7(3) . . . . ?
C12 C11 C22 C27 98.9(2) . . . . ?
C10 C11 C22 C27 -81.8(2) . . . . ?
C12 C11 C22 C23 -80.2(2) . . . . ?
C10 C11 C22 C23 99.1(2) . . . . ?
C27 C22 C23 C24 1.0(2) . . . . ?
C11 C22 C23 C24 -179.87(15) . . . . ?
C27 C22 C23 C31 179.59(17) . . . . ?
C11 C22 C23 C31 -1.3(2) . . . . ?
C22 C23 C24 C25 -0.9(3) . . . . ?
C31 C23 C24 C25 -179.52(18) . . . . ?
C23 C24 C25 C26 -0.2(3) . . . . ?
C23 C24 C25 C32 178.91(18) . . . . ?
C24 C25 C26 C27 1.3(3) . . . . ?
C32 C25 C26 C27 -177.83(18) . . . . ?
C25 C26 C27 C22 -1.2(3) . . . . ?
C25 C26 C27 C33 177.35(17) . . . . ?
C23 C22 C27 C26 0.1(2) . . . . ?
C11 C22 C27 C26 -179.09(16) . . . . ?
C23 C22 C27 C33 -178.51(16) . . . . ?
C11 C22 C27 C33 2.3(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.949
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.949
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.050

#=============================================================================

data_ter2n2p2cl2
_database_code_depnum_ccdc_archive 'CCDC 781912'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
1,3-dichloro-2,4-bis[2,6-bis-(2,4,6-trimethylphenyl)phenyl]-cyclo-1,3-
diphospha-2,4-diazane
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C48 H50 Cl2 N2 P2'
_chemical_formula_sum            'C48 H50 Cl2 N2 P2'
_chemical_formula_weight         787.74

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'
P P 0.1023 0.0942 '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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.912(4)
_cell_length_b                   8.8080(18)
_cell_length_c                   24.420(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.56(3)
_cell_angle_gamma                90.00
_cell_volume                     4180.5(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9294
_cell_measurement_theta_min      5.065
_cell_measurement_theta_max      49.623

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1664
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8890
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31428
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         24.95
_reflns_number_total             3656
_reflns_number_gt                3041
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
All H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+6.1046P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3656
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0383
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
P P 0.03446(2) 0.86689(6) 0.302028(19) 0.02370(14) Uani 1 1 d . . .
Cl Cl 0.06301(3) 0.63493(7) 0.31485(3) 0.04975(19) Uani 1 1 d . . .
N N 0.04892(8) 0.87584(17) 0.23473(6) 0.0208(3) Uani 1 1 d . . .
C1 C 0.11306(9) 0.8913(2) 0.21789(7) 0.0207(4) Uani 1 1 d . . .
C2 C 0.11945(10) 0.8457(2) 0.16424(8) 0.0243(4) Uani 1 1 d . . .
C3 C 0.18338(10) 0.8601(2) 0.14997(9) 0.0314(5) Uani 1 1 d . . .
H3 H 0.1884 0.8270 0.1141 0.038 Uiso 1 1 calc R . .
C4 C 0.23922(10) 0.9210(3) 0.18668(9) 0.0351(5) Uani 1 1 d . . .
H4 H 0.2824 0.9289 0.1763 0.042 Uiso 1 1 calc R . .
C5 C 0.23189(10) 0.9704(2) 0.23851(9) 0.0321(5) Uani 1 1 d . . .
H5 H 0.2701 1.0149 0.2635 0.038 Uiso 1 1 calc R . .
C6 C 0.16936(9) 0.9566(2) 0.25514(8) 0.0252(4) Uani 1 1 d . . .
C7 C 0.16502(9) 1.0223(2) 0.31086(8) 0.0257(4) Uani 1 1 d . . .
C8 C 0.19661(10) 0.9493(2) 0.36077(8) 0.0299(5) Uani 1 1 d . . .
C9 C 0.19221(11) 1.0163(3) 0.41168(9) 0.0363(5) Uani 1 1 d . . .
H9 H 0.2133 0.9670 0.4457 0.044 Uiso 1 1 calc R . .
C10 C 0.15809(11) 1.1522(3) 0.41428(9) 0.0362(5) Uani 1 1 d . . .
C11 C 0.12804(11) 1.2234(2) 0.36413(9) 0.0334(5) Uani 1 1 d . . .
H11 H 0.1046 1.3170 0.3652 0.040 Uiso 1 1 calc R . .
C12 C 0.13129(10) 1.1616(2) 0.31243(8) 0.0281(5) Uani 1 1 d . . .
C13 C 0.06004(10) 0.7948(2) 0.11980(8) 0.0243(4) Uani 1 1 d . . .
C14 C 0.04800(11) 0.6409(2) 0.10813(8) 0.0294(5) Uani 1 1 d . . .
C15 C -0.00748(11) 0.5983(3) 0.06568(8) 0.0336(5) Uani 1 1 d . . .
H15 H -0.0152 0.4936 0.0573 0.040 Uiso 1 1 calc R . .
C16 C -0.05187(11) 0.7052(3) 0.03525(8) 0.0328(5) Uani 1 1 d . . .
C17 C -0.03752(10) 0.8574(2) 0.04628(8) 0.0315(5) Uani 1 1 d . . .
H17 H -0.0665 0.9317 0.0249 0.038 Uiso 1 1 calc R . .
C18 C 0.01788(10) 0.9049(2) 0.08752(8) 0.0267(4) Uani 1 1 d . . .
C19 C 0.09947(12) 1.2439(2) 0.25912(9) 0.0359(5) Uani 1 1 d . . .
H19A H 0.0826 1.3432 0.2683 0.054 Uiso 1 1 calc R . .
H19B H 0.0610 1.1841 0.2379 0.054 Uiso 1 1 calc R . .
H19C H 0.1341 1.2579 0.2365 0.054 Uiso 1 1 calc R . .
C20 C 0.15399(14) 1.2221(3) 0.47006(10) 0.0530(7) Uani 1 1 d . . .
H20A H 0.1738 1.1519 0.5004 0.080 Uiso 1 1 calc R . .
H20B H 0.1058 1.2419 0.4708 0.080 Uiso 1 1 calc R . .
H20C H 0.1798 1.3177 0.4751 0.080 Uiso 1 1 calc R . .
C21 C 0.23332(12) 0.8002(3) 0.36072(10) 0.0404(5) Uani 1 1 d . . .
H21A H 0.2080 0.7361 0.3303 0.061 Uiso 1 1 calc R . .
H21B H 0.2360 0.7489 0.3968 0.061 Uiso 1 1 calc R . .
H21C H 0.2799 0.8182 0.3550 0.061 Uiso 1 1 calc R . .
C22 C 0.03127(11) 1.0718(2) 0.09824(9) 0.0348(5) Uani 1 1 d . . .
H22A H 0.0078 1.1300 0.0654 0.052 Uiso 1 1 calc R . .
H22B H 0.0809 1.0912 0.1051 0.052 Uiso 1 1 calc R . .
H22C H 0.0138 1.1028 0.1311 0.052 Uiso 1 1 calc R . .
C23 C -0.11556(12) 0.6570(3) -0.00653(10) 0.0470(6) Uani 1 1 d . . .
H23A H -0.1068 0.5608 -0.0239 0.071 Uiso 1 1 calc R . .
H23B H -0.1278 0.7350 -0.0356 0.071 Uiso 1 1 calc R . .
H23C H -0.1536 0.6438 0.0127 0.071 Uiso 1 1 calc R . .
C24 C 0.09246(13) 0.5223(3) 0.14280(9) 0.0420(6) Uani 1 1 d . . .
H24A H 0.1394 0.5293 0.1366 0.063 Uiso 1 1 calc R . .
H24B H 0.0737 0.4213 0.1318 0.063 Uiso 1 1 calc R . .
H24C H 0.0932 0.5392 0.1826 0.063 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P 0.0221(3) 0.0327(3) 0.0158(3) 0.0002(2) 0.0030(2) 0.0022(2)
Cl 0.0605(4) 0.0481(4) 0.0472(4) 0.0249(3) 0.0260(3) 0.0289(3)
N 0.0213(8) 0.0252(8) 0.0155(8) -0.0009(6) 0.0034(6) -0.0013(7)
C1 0.0206(9) 0.0206(9) 0.0207(10) 0.0027(7) 0.0040(7) 0.0022(7)
C2 0.0260(10) 0.0259(10) 0.0208(10) 0.0013(8) 0.0050(8) 0.0039(8)
C3 0.0305(11) 0.0393(12) 0.0270(11) -0.0007(9) 0.0124(9) 0.0058(9)
C4 0.0238(10) 0.0442(13) 0.0402(13) 0.0023(10) 0.0137(9) 0.0050(9)
C5 0.0217(10) 0.0369(12) 0.0358(12) -0.0014(10) 0.0023(9) -0.0009(9)
C6 0.0230(10) 0.0274(10) 0.0243(10) 0.0003(8) 0.0028(8) 0.0017(8)
C7 0.0214(10) 0.0290(10) 0.0256(10) -0.0040(8) 0.0026(8) -0.0062(8)
C8 0.0242(10) 0.0337(11) 0.0285(11) -0.0034(9) -0.0016(8) -0.0043(9)
C9 0.0329(11) 0.0466(13) 0.0253(11) -0.0015(10) -0.0023(9) -0.0058(10)
C10 0.0346(12) 0.0441(13) 0.0295(12) -0.0128(10) 0.0061(9) -0.0120(10)
C11 0.0343(11) 0.0264(11) 0.0396(13) -0.0087(9) 0.0082(10) -0.0061(9)
C12 0.0267(10) 0.0267(11) 0.0301(11) -0.0030(8) 0.0046(9) -0.0067(8)
C13 0.0267(10) 0.0327(11) 0.0149(9) -0.0018(8) 0.0074(8) 0.0020(8)
C14 0.0353(11) 0.0326(11) 0.0205(10) -0.0032(9) 0.0065(9) 0.0037(9)
C15 0.0433(12) 0.0348(12) 0.0221(11) -0.0068(9) 0.0060(9) -0.0006(10)
C16 0.0336(11) 0.0474(13) 0.0173(10) -0.0022(9) 0.0052(9) -0.0015(10)
C17 0.0338(11) 0.0430(12) 0.0179(10) 0.0038(9) 0.0063(9) 0.0071(10)
C18 0.0312(11) 0.0331(11) 0.0178(9) 0.0023(8) 0.0096(8) 0.0022(9)
C19 0.0409(12) 0.0258(11) 0.0392(13) -0.0004(9) 0.0045(10) 0.0001(9)
C20 0.0575(16) 0.0615(17) 0.0391(14) -0.0200(12) 0.0084(12) -0.0107(13)
C21 0.0361(12) 0.0438(13) 0.0353(12) 0.0014(10) -0.0051(10) 0.0043(11)
C22 0.0428(13) 0.0348(12) 0.0267(11) 0.0087(9) 0.0074(9) 0.0026(10)
C23 0.0432(14) 0.0609(16) 0.0319(13) -0.0036(11) -0.0030(11) -0.0061(12)
C24 0.0552(15) 0.0328(12) 0.0324(12) -0.0038(10) -0.0024(11) 0.0096(11)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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
P N 1.7091(16) 2 ?
P N 1.7307(16) . ?
P Cl 2.1256(9) . ?
P P 2.6123(12) 2 ?
N C1 1.431(2) . ?
N P 1.7091(16) 2 ?
C1 C2 1.402(3) . ?
C1 C6 1.404(3) . ?
C2 C3 1.397(3) . ?
C2 C13 1.490(3) . ?
C3 C4 1.376(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.396(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.498(3) . ?
C7 C8 1.400(3) . ?
C7 C12 1.403(3) . ?
C8 C9 1.396(3) . ?
C8 C21 1.504(3) . ?
C9 C10 1.385(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(3) . ?
C10 C20 1.513(3) . ?
C11 C12 1.390(3) . ?
C11 H11 0.9500 . ?
C12 C19 1.504(3) . ?
C13 C14 1.395(3) . ?
C13 C18 1.407(3) . ?
C14 C15 1.392(3) . ?
C14 C24 1.505(3) . ?
C15 C16 1.391(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(3) . ?
C16 C23 1.506(3) . ?
C17 C18 1.387(3) . ?
C17 H17 0.9500 . ?
C18 C22 1.507(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
N P N 80.93(8) 2 . ?
N P Cl 108.66(6) 2 . ?
N P Cl 95.12(6) . . ?
N P P 40.90(6) 2 2 ?
N P P 40.28(5) . 2 ?
Cl P P 102.15(2) . 2 ?
C1 N P 132.79(12) . 2 ?
C1 N P 128.35(12) . . ?
P N P 98.83(8) 2 . ?
C2 C1 C6 120.05(17) . . ?
C2 C1 N 120.62(16) . . ?
C6 C1 N 119.32(16) . . ?
C3 C2 C1 118.68(18) . . ?
C3 C2 C13 117.90(17) . . ?
C1 C2 C13 123.21(17) . . ?
C4 C3 C2 121.59(19) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C5 C4 C3 119.35(19) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.29(19) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C1 118.97(18) . . ?
C5 C6 C7 117.48(17) . . ?
C1 C6 C7 123.43(16) . . ?
C8 C7 C12 120.30(18) . . ?
C8 C7 C6 120.64(18) . . ?
C12 C7 C6 119.00(17) . . ?
C9 C8 C7 118.57(19) . . ?
C9 C8 C21 119.63(19) . . ?
C7 C8 C21 121.78(18) . . ?
C10 C9 C8 122.2(2) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C9 C10 C11 118.13(19) . . ?
C9 C10 C20 121.1(2) . . ?
C11 C10 C20 120.8(2) . . ?
C12 C11 C10 121.8(2) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C7 118.99(19) . . ?
C11 C12 C19 120.22(19) . . ?
C7 C12 C19 120.78(18) . . ?
C14 C13 C18 120.00(18) . . ?
C14 C13 C2 121.02(17) . . ?
C18 C13 C2 118.90(18) . . ?
C15 C14 C13 119.16(19) . . ?
C15 C14 C24 120.43(19) . . ?
C13 C14 C24 120.34(18) . . ?
C16 C15 C14 121.6(2) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C17 C16 C15 118.12(19) . . ?
C17 C16 C23 120.8(2) . . ?
C15 C16 C23 121.0(2) . . ?
C16 C17 C18 122.06(19) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C17 C18 C13 118.89(19) . . ?
C17 C18 C22 120.19(18) . . ?
C13 C18 C22 120.91(18) . . ?
C12 C19 H19A 109.5 . . ?
C12 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C12 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 H23A 109.5 . . ?
C16 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C16 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C14 C24 H24A 109.5 . . ?
C14 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C14 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

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
N P N C1 172.82(12) 2 . . . ?
Cl P N C1 -79.06(15) . . . . ?
P P N C1 178.2(2) 2 . . . ?
N P N P -5.35(11) 2 . . 2 ?
Cl P N P 102.77(7) . . . 2 ?
P N C1 C2 -24.5(3) 2 . . . ?
P N C1 C2 157.98(14) . . . . ?
P N C1 C6 153.85(15) 2 . . . ?
P N C1 C6 -23.7(2) . . . . ?
C6 C1 C2 C3 2.9(3) . . . . ?
N C1 C2 C3 -178.74(17) . . . . ?
C6 C1 C2 C13 -171.67(18) . . . . ?
N C1 C2 C13 6.7(3) . . . . ?
C1 C2 C3 C4 -1.6(3) . . . . ?
C13 C2 C3 C4 173.29(19) . . . . ?
C2 C3 C4 C5 -0.7(3) . . . . ?
C3 C4 C5 C6 1.6(3) . . . . ?
C4 C5 C6 C1 -0.3(3) . . . . ?
C4 C5 C6 C7 -176.29(19) . . . . ?
C2 C1 C6 C5 -2.0(3) . . . . ?
N C1 C6 C5 179.62(17) . . . . ?
C2 C1 C6 C7 173.74(18) . . . . ?
N C1 C6 C7 -4.6(3) . . . . ?
C5 C6 C7 C8 -74.6(2) . . . . ?
C1 C6 C7 C8 109.5(2) . . . . ?
C5 C6 C7 C12 102.6(2) . . . . ?
C1 C6 C7 C12 -73.2(2) . . . . ?
C12 C7 C8 C9 1.6(3) . . . . ?
C6 C7 C8 C9 178.87(18) . . . . ?
C12 C7 C8 C21 -179.89(18) . . . . ?
C6 C7 C8 C21 -2.6(3) . . . . ?
C7 C8 C9 C10 -0.4(3) . . . . ?
C21 C8 C9 C10 -178.9(2) . . . . ?
C8 C9 C10 C11 -0.5(3) . . . . ?
C8 C9 C10 C20 179.9(2) . . . . ?
C9 C10 C11 C12 0.3(3) . . . . ?
C20 C10 C11 C12 179.8(2) . . . . ?
C10 C11 C12 C7 0.9(3) . . . . ?
C10 C11 C12 C19 -178.63(19) . . . . ?
C8 C7 C12 C11 -1.9(3) . . . . ?
C6 C7 C12 C11 -179.19(17) . . . . ?
C8 C7 C12 C19 177.68(18) . . . . ?
C6 C7 C12 C19 0.4(3) . . . . ?
C3 C2 C13 C14 84.1(2) . . . . ?
C1 C2 C13 C14 -101.3(2) . . . . ?
C3 C2 C13 C18 -92.7(2) . . . . ?
C1 C2 C13 C18 81.9(2) . . . . ?
C18 C13 C14 C15 -2.3(3) . . . . ?
C2 C13 C14 C15 -179.02(18) . . . . ?
C18 C13 C14 C24 -179.44(19) . . . . ?
C2 C13 C14 C24 3.8(3) . . . . ?
C13 C14 C15 C16 -1.1(3) . . . . ?
C24 C14 C15 C16 176.1(2) . . . . ?
C14 C15 C16 C17 3.2(3) . . . . ?
C14 C15 C16 C23 -173.9(2) . . . . ?
C15 C16 C17 C18 -2.1(3) . . . . ?
C23 C16 C17 C18 175.04(19) . . . . ?
C16 C17 C18 C13 -1.2(3) . . . . ?
C16 C17 C18 C22 -179.67(19) . . . . ?
C14 C13 C18 C17 3.4(3) . . . . ?
C2 C13 C18 C17 -179.81(17) . . . . ?
C14 C13 C18 C22 -178.13(18) . . . . ?
C2 C13 C18 C22 -1.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.95
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.044

#=============================================================================

data_ter_nhascl2
_database_code_depnum_ccdc_archive 'CCDC 781913'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
[2,6-bis-(2,4,6-trimethylphenyl)phenyl]amino(dichloro)arsane
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 As Cl2 N'
_chemical_formula_sum            'C24 H26 As Cl2 N'
_chemical_formula_weight         474.28

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'
As As 0.0499 2.0058 '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'
N N 0.0061 0.0033 '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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_Int_Tables_number      33

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   24.301(5)
_cell_length_b                   10.580(2)
_cell_length_c                   8.8420(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2273.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9680
_cell_measurement_theta_min      4.190
_cell_measurement_theta_max      70.475

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    1.740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5429
_exptl_absorpt_correction_T_max  0.5429
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49272
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.85
_diffrn_reflns_theta_max         36.03
_reflns_number_total             10714
_reflns_number_gt                9203
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
The H atom at N was refined freely. All other H atoms were positioned
geometrically and refined using a riding model , with C---H = 0.98
(methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.1434P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.310(4)
_refine_ls_number_reflns         10714
_refine_ls_number_parameters     264
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0251
_refine_ls_wR_factor_ref         0.0608
_refine_ls_wR_factor_gt          0.0578
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.189502(4) 0.442706(9) 0.127128(14) 0.02242(3) Uani 1 1 d . . .
Cl1 Cl 0.189155(14) 0.43491(4) -0.12519(4) 0.03910(8) Uani 1 1 d . . .
Cl2 Cl 0.138523(12) 0.61728(2) 0.14012(5) 0.03447(6) Uani 1 1 d . . .
N N 0.12999(4) 0.34554(9) 0.17260(12) 0.02450(18) Uani 1 1 d . . .
C1 C 0.12531(4) 0.21354(10) 0.18755(12) 0.02113(17) Uani 1 1 d . . .
C2 C 0.07209(4) 0.16064(11) 0.18006(14) 0.02479(19) Uani 1 1 d . . .
C3 C 0.06622(5) 0.03039(12) 0.20266(19) 0.0346(3) Uani 1 1 d . . .
H3 H 0.0306 -0.0066 0.1983 0.042 Uiso 1 1 calc R . .
C4 C 0.11170(7) -0.04556(13) 0.2314(2) 0.0396(3) Uani 1 1 d . . .
H4 H 0.1070 -0.1337 0.2473 0.048 Uiso 1 1 calc R . .
C5 C 0.16389(6) 0.00734(12) 0.23679(17) 0.0328(3) Uani 1 1 d . . .
H5 H 0.1948 -0.0452 0.2558 0.039 Uiso 1 1 calc R . .
C6 C 0.17160(5) 0.13699(10) 0.21462(13) 0.02342(18) Uani 1 1 d . . .
C7 C 0.02395(4) 0.24436(10) 0.14745(14) 0.0242(2) Uani 1 1 d . . .
C8 C 0.01243(5) 0.27777(12) -0.00242(15) 0.0278(2) Uani 1 1 d . . .
C9 C -0.03058(5) 0.36225(13) -0.03227(14) 0.0307(2) Uani 1 1 d . . .
H9 H -0.0385 0.3847 -0.1340 0.037 Uiso 1 1 calc R . .
C10 C -0.06190(5) 0.41392(12) 0.08406(15) 0.0286(2) Uani 1 1 d . . .
C11 C -0.05037(5) 0.37855(13) 0.23164(15) 0.0297(2) Uani 1 1 d . . .
H11 H -0.0720 0.4123 0.3115 0.036 Uiso 1 1 calc R . .
C12 C -0.00795(5) 0.29491(12) 0.26621(13) 0.0261(2) Uani 1 1 d . . .
C13 C 0.22703(4) 0.19815(10) 0.21926(14) 0.02403(19) Uani 1 1 d . . .
C14 C 0.24654(5) 0.25100(12) 0.35524(14) 0.0300(2) Uani 1 1 d . . .
C15 C 0.29612(6) 0.31843(13) 0.35342(19) 0.0379(3) Uani 1 1 d . . .
H15 H 0.3095 0.3536 0.4452 0.045 Uiso 1 1 calc R . .
C16 C 0.32636(6) 0.33545(13) 0.2213(2) 0.0389(3) Uani 1 1 d . . .
C17 C 0.30804(5) 0.27698(13) 0.08987(17) 0.0337(3) Uani 1 1 d . . .
H17 H 0.3291 0.2847 -0.0001 0.040 Uiso 1 1 calc R . .
C18 C 0.25901(5) 0.20665(11) 0.08705(14) 0.0269(2) Uani 1 1 d . . .
C19 C 0.04593(6) 0.22563(17) -0.13287(16) 0.0414(3) Uani 1 1 d . . .
H19A H 0.0294 0.2523 -0.2288 0.062 Uiso 1 1 calc R . .
H19B H 0.0464 0.1331 -0.1276 0.062 Uiso 1 1 calc R . .
H19C H 0.0837 0.2577 -0.1266 0.062 Uiso 1 1 calc R . .
C20 C -0.10799(6) 0.50564(15) 0.04954(18) 0.0390(3) Uani 1 1 d . . .
H20A H -0.1434 0.4657 0.0720 0.059 Uiso 1 1 calc R . .
H20B H -0.1067 0.5291 -0.0576 0.059 Uiso 1 1 calc R . .
H20C H -0.1037 0.5816 0.1119 0.059 Uiso 1 1 calc R . .
C21 C 0.00220(6) 0.25782(16) 0.42846(15) 0.0393(3) Uani 1 1 d . . .
H21A H -0.0146 0.3205 0.4957 0.059 Uiso 1 1 calc R . .
H21B H 0.0419 0.2543 0.4473 0.059 Uiso 1 1 calc R . .
H21C H -0.0141 0.1746 0.4478 0.059 Uiso 1 1 calc R . .
C22 C 0.21473(7) 0.23617(16) 0.49952(17) 0.0435(3) Uani 1 1 d . . .
H22A H 0.2324 0.2857 0.5796 0.065 Uiso 1 1 calc R . .
H22B H 0.2140 0.1468 0.5287 0.065 Uiso 1 1 calc R . .
H22C H 0.1770 0.2663 0.4845 0.065 Uiso 1 1 calc R . .
C23 C 0.37762(7) 0.41691(18) 0.2193(3) 0.0612(6) Uani 1 1 d . . .
H23A H 0.3683 0.5014 0.1817 0.092 Uiso 1 1 calc R . .
H23B H 0.4052 0.3784 0.1529 0.092 Uiso 1 1 calc R . .
H23C H 0.3925 0.4236 0.3220 0.092 Uiso 1 1 calc R . .
C24 C 0.24259(6) 0.13986(14) -0.05635(16) 0.0367(3) Uani 1 1 d . . .
H24A H 0.2510 0.0496 -0.0473 0.055 Uiso 1 1 calc R . .
H24B H 0.2631 0.1756 -0.1418 0.055 Uiso 1 1 calc R . .
H24C H 0.2030 0.1509 -0.0734 0.055 Uiso 1 1 calc R . .
H1 H 0.1004(7) 0.3772(15) 0.1598(19) 0.030(4) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As 0.02063(4) 0.02012(4) 0.02650(5) -0.00095(5) -0.00222(5) -0.00089(3)
Cl1 0.04003(16) 0.0505(2) 0.02681(14) 0.00261(13) 0.00420(12) 0.00210(13)
Cl2 0.03685(12) 0.02069(10) 0.04586(17) 0.00212(13) 0.00316(14) 0.00471(9)
N 0.0193(3) 0.0207(4) 0.0334(5) 0.0015(3) -0.0002(3) 0.0022(3)
C1 0.0221(4) 0.0196(4) 0.0217(4) -0.0002(3) 0.0007(3) 0.0017(3)
C2 0.0227(4) 0.0231(5) 0.0286(5) 0.0010(4) 0.0006(4) -0.0010(4)
C3 0.0297(5) 0.0241(5) 0.0500(8) 0.0013(5) 0.0008(5) -0.0047(4)
C4 0.0385(7) 0.0193(5) 0.0610(9) 0.0034(5) -0.0001(6) -0.0006(5)
C5 0.0332(6) 0.0206(5) 0.0446(7) 0.0003(5) -0.0010(5) 0.0051(5)
C6 0.0237(4) 0.0212(4) 0.0254(5) -0.0013(4) -0.0004(4) 0.0032(4)
C7 0.0200(3) 0.0240(4) 0.0285(6) 0.0012(4) -0.0006(4) -0.0018(3)
C8 0.0251(4) 0.0322(5) 0.0260(5) -0.0027(5) -0.0014(4) -0.0003(4)
C9 0.0279(5) 0.0377(6) 0.0264(5) 0.0020(4) -0.0022(4) 0.0021(5)
C10 0.0246(5) 0.0302(5) 0.0310(6) 0.0014(4) -0.0016(4) 0.0028(4)
C11 0.0260(5) 0.0351(6) 0.0281(5) 0.0008(5) 0.0024(4) 0.0045(5)
C12 0.0230(5) 0.0307(6) 0.0247(5) 0.0021(4) 0.0011(4) 0.0005(4)
C13 0.0235(4) 0.0208(4) 0.0278(5) -0.0039(4) -0.0044(4) 0.0051(4)
C14 0.0349(5) 0.0248(5) 0.0303(6) -0.0043(4) -0.0111(4) 0.0107(4)
C15 0.0384(6) 0.0250(6) 0.0504(8) -0.0097(5) -0.0239(6) 0.0088(5)
C16 0.0247(5) 0.0257(6) 0.0663(9) -0.0060(6) -0.0130(6) 0.0028(5)
C17 0.0230(4) 0.0281(6) 0.0501(8) -0.0044(5) 0.0029(4) 0.0010(4)
C18 0.0236(4) 0.0223(5) 0.0350(6) -0.0061(4) 0.0007(4) 0.0016(4)
C19 0.0391(6) 0.0567(9) 0.0283(6) -0.0081(6) 0.0013(5) 0.0090(6)
C20 0.0325(6) 0.0429(8) 0.0416(7) 0.0041(6) -0.0032(5) 0.0111(6)
C21 0.0387(6) 0.0544(9) 0.0248(6) 0.0057(6) 0.0013(5) 0.0064(6)
C22 0.0573(8) 0.0459(8) 0.0272(5) -0.0048(6) -0.0071(6) 0.0133(7)
C23 0.0329(7) 0.0380(8) 0.1128(17) -0.0045(10) -0.0222(9) -0.0059(6)
C24 0.0400(7) 0.0358(6) 0.0342(6) -0.0122(5) 0.0070(5) -0.0040(5)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 N 1.8194(10) . ?
As Cl2 2.2270(4) . ?
As Cl1 2.2325(6) . ?
N C1 1.4074(14) . ?
N H1 0.802(16) . ?
C1 C6 1.4067(15) . ?
C1 C2 1.4107(15) . ?
C2 C3 1.3998(17) . ?
C2 C7 1.4955(15) . ?
C3 C4 1.390(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.387(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3983(18) . ?
C5 H5 0.9500 . ?
C6 C13 1.4948(16) . ?
C7 C8 1.3997(18) . ?
C7 C12 1.4105(17) . ?
C8 C9 1.4005(18) . ?
C8 C19 1.5157(19) . ?
C9 C10 1.3914(19) . ?
C9 H9 0.9500 . ?
C10 C11 1.3861(19) . ?
C10 C20 1.5132(18) . ?
C11 C12 1.3924(18) . ?
C11 H11 0.9500 . ?
C12 C21 1.5077(18) . ?
C13 C18 1.4068(17) . ?
C13 C14 1.4082(17) . ?
C14 C15 1.400(2) . ?
C14 C22 1.500(2) . ?
C15 C16 1.392(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.390(2) . ?
C16 C23 1.515(2) . ?
C17 C18 1.4049(17) . ?
C17 H17 0.9500 . ?
C18 C24 1.5055(18) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
N As Cl2 90.86(3) . . ?
N As Cl1 101.36(3) . . ?
Cl2 As Cl1 94.593(15) . . ?
C1 N As 130.21(7) . . ?
C1 N H1 110.8(12) . . ?
As N H1 116.5(12) . . ?
C6 C1 N 121.51(10) . . ?
C6 C1 C2 120.85(10) . . ?
N C1 C2 117.60(9) . . ?
C3 C2 C1 118.52(10) . . ?
C3 C2 C7 122.06(10) . . ?
C1 C2 C7 119.42(10) . . ?
C4 C3 C2 120.94(12) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 120.01(12) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.89(12) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 118.78(11) . . ?
C5 C6 C13 122.79(10) . . ?
C1 C6 C13 118.43(10) . . ?
C8 C7 C12 119.94(10) . . ?
C8 C7 C2 119.24(10) . . ?
C12 C7 C2 120.73(11) . . ?
C7 C8 C9 119.26(11) . . ?
C7 C8 C19 121.41(11) . . ?
C9 C8 C19 119.32(12) . . ?
C10 C9 C8 121.31(12) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C11 C10 C9 118.64(11) . . ?
C11 C10 C20 120.85(12) . . ?
C9 C10 C20 120.51(12) . . ?
C10 C11 C12 121.86(12) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C7 118.97(11) . . ?
C11 C12 C21 119.70(12) . . ?
C7 C12 C21 121.31(11) . . ?
C18 C13 C14 119.87(11) . . ?
C18 C13 C6 120.18(10) . . ?
C14 C13 C6 119.92(11) . . ?
C15 C14 C13 118.83(13) . . ?
C15 C14 C22 120.43(12) . . ?
C13 C14 C22 120.74(12) . . ?
C16 C15 C14 122.00(12) . . ?
C16 C15 H15 119.0 . . ?
C14 C15 H15 119.0 . . ?
C17 C16 C15 118.37(12) . . ?
C17 C16 C23 120.45(18) . . ?
C15 C16 C23 121.18(16) . . ?
C16 C17 C18 121.48(13) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C17 C18 C13 119.19(11) . . ?
C17 C18 C24 119.24(11) . . ?
C13 C18 C24 121.56(11) . . ?
C8 C19 H19A 109.5 . . ?
C8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 H23A 109.5 . . ?
C16 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C16 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

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
Cl2 As N C1 179.47(10) . . . . ?
Cl1 As N C1 84.61(10) . . . . ?
As N C1 C6 20.38(16) . . . . ?
As N C1 C2 -161.94(9) . . . . ?
C6 C1 C2 C3 1.04(18) . . . . ?
N C1 C2 C3 -176.66(12) . . . . ?
C6 C1 C2 C7 -178.56(11) . . . . ?
N C1 C2 C7 3.74(16) . . . . ?
C1 C2 C3 C4 -0.2(2) . . . . ?
C7 C2 C3 C4 179.38(14) . . . . ?
C2 C3 C4 C5 -0.5(3) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C4 C5 C6 C1 0.4(2) . . . . ?
C4 C5 C6 C13 -179.94(14) . . . . ?
N C1 C6 C5 176.47(11) . . . . ?
C2 C1 C6 C5 -1.14(17) . . . . ?
N C1 C6 C13 -3.20(16) . . . . ?
C2 C1 C6 C13 179.19(10) . . . . ?
C3 C2 C7 C8 -98.09(15) . . . . ?
C1 C2 C7 C8 81.49(14) . . . . ?
C3 C2 C7 C12 85.25(16) . . . . ?
C1 C2 C7 C12 -95.17(14) . . . . ?
C12 C7 C8 C9 0.53(17) . . . . ?
C2 C7 C8 C9 -176.16(11) . . . . ?
C12 C7 C8 C19 179.82(12) . . . . ?
C2 C7 C8 C19 3.14(17) . . . . ?
C7 C8 C9 C10 0.26(19) . . . . ?
C19 C8 C9 C10 -179.05(13) . . . . ?
C8 C9 C10 C11 -1.1(2) . . . . ?
C8 C9 C10 C20 179.64(13) . . . . ?
C9 C10 C11 C12 1.1(2) . . . . ?
C20 C10 C11 C12 -179.60(13) . . . . ?
C10 C11 C12 C7 -0.3(2) . . . . ?
C10 C11 C12 C21 -178.94(13) . . . . ?
C8 C7 C12 C11 -0.49(17) . . . . ?
C2 C7 C12 C11 176.14(11) . . . . ?
C8 C7 C12 C21 178.09(12) . . . . ?
C2 C7 C12 C21 -5.28(18) . . . . ?
C5 C6 C13 C18 88.50(15) . . . . ?
C1 C6 C13 C18 -91.84(13) . . . . ?
C5 C6 C13 C14 -93.53(15) . . . . ?
C1 C6 C13 C14 86.13(14) . . . . ?
C18 C13 C14 C15 4.10(17) . . . . ?
C6 C13 C14 C15 -173.87(10) . . . . ?
C18 C13 C14 C22 -176.25(11) . . . . ?
C6 C13 C14 C22 5.78(17) . . . . ?
C13 C14 C15 C16 0.48(19) . . . . ?
C22 C14 C15 C16 -179.17(12) . . . . ?
C14 C15 C16 C17 -3.87(19) . . . . ?
C14 C15 C16 C23 175.35(13) . . . . ?
C15 C16 C17 C18 2.73(19) . . . . ?
C23 C16 C17 C18 -176.49(13) . . . . ?
C16 C17 C18 C13 1.74(18) . . . . ?
C16 C17 C18 C24 -176.94(13) . . . . ?
C14 C13 C18 C17 -5.19(17) . . . . ?
C6 C13 C18 C17 172.78(11) . . . . ?
C14 C13 C18 C24 173.46(12) . . . . ?
C6 C13 C18 C24 -8.57(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        36.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.051

#=============================================================================

data_ter_nhascl2_2
_database_code_depnum_ccdc_archive 'CCDC 781914'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

# start Validation Reply Form
_vrf_PLAT432_ternhascl2_2        
;
PROBLEM: Short Inter X...Y Contact C23 .. Cl2B .. 2.94 Ang.
RESPONSE: Cl2b belongs to the minor part of a disordered AsCl2 unit. For the
mesityl unit involving C23 no split model could be applied.
;
# end Validation Reply Form

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
[2,6-bis-(2,4,6-trimethylphenyl)phenyl]amino(dichloro)arsane
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 As Cl2 N'
_chemical_formula_sum            'C24 H26 As Cl2 N'
_chemical_formula_weight         474.28

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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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'

_cell_length_a                   9.0170(18)
_cell_length_b                   29.293(6)
_cell_length_c                   9.3090(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.09(3)
_cell_angle_gamma                90.00
_cell_volume                     2337.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6094
_cell_measurement_theta_min      5.672
_cell_measurement_theta_max      67.763

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             976
_exptl_absorpt_coefficient_mu    1.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3796
_exptl_absorpt_correction_T_max  0.8357
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42147
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         32.50
_reflns_number_total             8395
_reflns_number_gt                6382
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
The H atom H1a at N was refined freely. All other H atoms were positioned
geometrically and refined using a riding model , with C---H = 0.98
(methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.7970P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8395
_refine_ls_number_parameters     273
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
As1A As 0.62033(2) 0.145322(6) 0.704140(19) 0.02766(6) Uani 0.9785(5) 1 d P A 1
Cl1A Cl 0.68669(7) 0.12540(2) 0.94607(5) 0.04203(13) Uani 0.9785(5) 1 d P A 1
Cl2A Cl 0.68775(7) 0.079977(19) 0.62267(6) 0.04821(14) Uani 0.9785(5) 1 d P A 1
As1B As 0.4656(9) 0.0873(3) 0.8123(8) 0.02766(6) Uani 0.0215(5) 1 d P A 2
Cl2B Cl 0.539(3) 0.0382(9) 0.665(3) 0.04821(14) Uani 0.0215(5) 1 d P A 2
Cl1B Cl 0.695(4) 0.1088(11) 0.920(3) 0.04203(13) Uani 0.0215(5) 1 d P A 2
N N 0.41522(17) 0.13582(6) 0.68334(15) 0.0286(3) Uani 1 1 d . . .
H1B H 0.4707 0.1610 0.7053 0.034 Uiso 0.0215(5) 1 calc PR A 2
C1 C 0.28879(18) 0.13336(6) 0.54920(16) 0.0237(3) Uani 1 1 d . A .
C2 C 0.29047(19) 0.15721(6) 0.41840(16) 0.0256(3) Uani 1 1 d . . .
C3 C 0.1585(2) 0.15482(7) 0.29092(18) 0.0347(4) Uani 1 1 d . A .
H3 H 0.1573 0.1710 0.2021 0.042 Uiso 1 1 calc R . .
C4 C 0.0295(2) 0.12930(8) 0.2916(2) 0.0416(5) Uani 1 1 d . . .
H4 H -0.0590 0.1280 0.2037 0.050 Uiso 1 1 calc R A .
C5 C 0.0296(2) 0.10558(7) 0.4209(2) 0.0370(4) Uani 1 1 d . A .
H5 H -0.0591 0.0881 0.4207 0.044 Uiso 1 1 calc R . .
C6 C 0.1581(2) 0.10722(6) 0.55055(18) 0.0276(3) Uani 1 1 d . . .
C7 C 0.43235(19) 0.18294(6) 0.41777(16) 0.0260(3) Uani 1 1 d . A .
C8 C 0.4641(2) 0.22648(6) 0.48720(18) 0.0303(3) Uani 1 1 d . . .
C9 C 0.6034(2) 0.24809(7) 0.4948(2) 0.0374(4) Uani 1 1 d . A .
H9 H 0.6250 0.2773 0.5410 0.045 Uiso 1 1 calc R . .
C10 C 0.7124(2) 0.22798(7) 0.4361(2) 0.0408(4) Uani 1 1 d . . .
C11 C 0.6765(2) 0.18625(7) 0.3633(2) 0.0377(4) Uani 1 1 d . A .
H11 H 0.7492 0.1728 0.3209 0.045 Uiso 1 1 calc R . .
C12 C 0.5381(2) 0.16338(7) 0.35026(18) 0.0307(3) Uani 1 1 d . . .
C13 C 0.1622(2) 0.08178(6) 0.69130(19) 0.0301(3) Uani 1 1 d . A .
C14 C 0.1195(2) 0.10410(7) 0.80575(19) 0.0320(4) Uani 1 1 d . . .
C15 C 0.1333(3) 0.08077(8) 0.9401(2) 0.0427(5) Uani 1 1 d . A .
H15 H 0.1020 0.0955 1.0169 0.051 Uiso 1 1 calc R . .
C16 C 0.1915(3) 0.03655(9) 0.9643(3) 0.0552(6) Uani 1 1 d . . .
C17 C 0.2322(4) 0.01528(8) 0.8503(3) 0.0597(7) Uani 1 1 d . A .
H17 H 0.2703 -0.0152 0.8652 0.072 Uiso 1 1 calc R . .
C18 C 0.2194(3) 0.03686(7) 0.7133(2) 0.0455(5) Uani 1 1 d . . .
C19 C 0.3493(3) 0.24868(7) 0.5537(2) 0.0403(4) Uani 1 1 d . A .
H19A H 0.3497 0.2324 0.6459 0.060 Uiso 1 1 calc R . .
H19B H 0.2445 0.2474 0.4803 0.060 Uiso 1 1 calc R . .
H19C H 0.3791 0.2806 0.5782 0.060 Uiso 1 1 calc R . .
C20 C 0.8667(3) 0.25107(9) 0.4495(4) 0.0635(7) Uani 1 1 d . A .
H20A H 0.9518 0.2290 0.4859 0.095 Uiso 1 1 calc R . .
H20B H 0.8828 0.2765 0.5209 0.095 Uiso 1 1 calc R . .
H20C H 0.8653 0.2626 0.3502 0.095 Uiso 1 1 calc R . .
C21 C 0.5010(3) 0.11889(8) 0.2642(2) 0.0398(4) Uani 1 1 d . A .
H21A H 0.4224 0.1242 0.1660 0.060 Uiso 1 1 calc R . .
H21B H 0.4605 0.0969 0.3221 0.060 Uiso 1 1 calc R . .
H21C H 0.5960 0.1067 0.2487 0.060 Uiso 1 1 calc R . .
C22 C 0.0623(3) 0.15263(8) 0.7858(3) 0.0450(5) Uani 1 1 d . A .
H22A H 0.1450 0.1726 0.7739 0.067 Uiso 1 1 calc R . .
H22B H 0.0341 0.1621 0.8748 0.067 Uiso 1 1 calc R . .
H22C H -0.0294 0.1548 0.6957 0.067 Uiso 1 1 calc R . .
C23 C 0.2106(5) 0.01266(12) 1.1140(3) 0.0851(11) Uani 1 1 d . A .
H23A H 0.3215 0.0115 1.1728 0.128 Uiso 1 1 calc R . .
H23B H 0.1695 -0.0185 1.0949 0.128 Uiso 1 1 calc R . .
H23C H 0.1533 0.0295 1.1707 0.128 Uiso 1 1 calc R . .
C24 C 0.2680(4) 0.01259(9) 0.5916(3) 0.0731(9) Uani 1 1 d . A .
H24A H 0.1778 0.0097 0.5004 0.110 Uiso 1 1 calc R . .
H24B H 0.3079 -0.0178 0.6274 0.110 Uiso 1 1 calc R . .
H24C H 0.3499 0.0302 0.5680 0.110 Uiso 1 1 calc R . .
H1A H 0.407(3) 0.1191(9) 0.746(3) 0.049(7) Uiso 0.9785(5) 1 d P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As1A 0.02218(9) 0.03209(10) 0.02494(8) 0.00222(6) 0.00180(6) 0.00058(7)
Cl1A 0.0396(3) 0.0548(4) 0.0225(2) 0.00142(19) -0.00381(17) 0.0052(3)
Cl2A 0.0633(4) 0.0434(3) 0.0395(2) 0.0033(2) 0.0181(2) 0.0198(3)
As1B 0.02218(9) 0.03209(10) 0.02494(8) 0.00222(6) 0.00180(6) 0.00058(7)
Cl2B 0.0633(4) 0.0434(3) 0.0395(2) 0.0033(2) 0.0181(2) 0.0198(3)
Cl1B 0.0396(3) 0.0548(4) 0.0225(2) 0.00142(19) -0.00381(17) 0.0052(3)
N 0.0254(7) 0.0394(8) 0.0183(5) 0.0046(5) 0.0027(5) -0.0031(6)
C1 0.0212(7) 0.0289(8) 0.0195(6) -0.0026(5) 0.0040(5) 0.0014(6)
C2 0.0246(7) 0.0316(8) 0.0196(6) -0.0012(5) 0.0054(5) 0.0020(6)
C3 0.0312(9) 0.0505(11) 0.0197(6) 0.0016(7) 0.0040(6) 0.0044(8)
C4 0.0261(9) 0.0675(14) 0.0250(7) -0.0054(8) -0.0013(6) -0.0023(9)
C5 0.0248(8) 0.0528(12) 0.0317(8) -0.0094(8) 0.0063(7) -0.0077(8)
C6 0.0259(8) 0.0312(8) 0.0259(7) -0.0053(6) 0.0084(6) -0.0019(6)
C7 0.0259(7) 0.0311(8) 0.0197(6) 0.0051(6) 0.0052(5) 0.0020(6)
C8 0.0318(9) 0.0308(9) 0.0264(7) 0.0055(6) 0.0061(6) 0.0035(7)
C9 0.0388(10) 0.0300(9) 0.0391(9) 0.0056(7) 0.0060(8) -0.0033(8)
C10 0.0312(9) 0.0414(11) 0.0490(10) 0.0160(9) 0.0114(8) -0.0040(8)
C11 0.0339(9) 0.0432(11) 0.0410(9) 0.0127(8) 0.0192(8) 0.0062(8)
C12 0.0339(9) 0.0351(9) 0.0245(7) 0.0060(6) 0.0113(6) 0.0042(7)
C13 0.0322(8) 0.0294(9) 0.0303(7) -0.0037(6) 0.0121(6) -0.0075(7)
C14 0.0293(8) 0.0379(10) 0.0313(8) -0.0047(7) 0.0130(7) -0.0062(7)
C15 0.0470(12) 0.0520(12) 0.0331(9) -0.0042(8) 0.0181(8) -0.0147(10)
C16 0.0737(17) 0.0483(13) 0.0429(11) 0.0099(9) 0.0174(11) -0.0193(12)
C17 0.086(2) 0.0317(11) 0.0613(14) 0.0105(10) 0.0219(14) -0.0035(12)
C18 0.0621(14) 0.0301(10) 0.0474(11) -0.0022(8) 0.0216(10) -0.0018(10)
C19 0.0417(11) 0.0365(10) 0.0417(10) -0.0067(8) 0.0117(8) 0.0056(9)
C20 0.0388(12) 0.0576(15) 0.095(2) 0.0187(14) 0.0216(13) -0.0092(11)
C21 0.0434(11) 0.0465(11) 0.0326(8) -0.0055(8) 0.0161(8) 0.0045(9)
C22 0.0488(12) 0.0479(12) 0.0445(11) -0.0069(9) 0.0237(10) 0.0071(10)
C23 0.121(3) 0.079(2) 0.0517(15) 0.0268(14) 0.0213(17) -0.023(2)
C24 0.122(3) 0.0376(13) 0.0709(17) -0.0082(12) 0.0456(18) 0.0151(15)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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
As1A Cl2A 2.2124(7) . ?
As1A Cl1A 2.2212(7) . ?
As1B N 1.825(8) . ?
As1B Cl1B 2.10(3) . ?
As1B Cl2B 2.22(2) . ?
As1B H1A 1.15(3) . ?
N C1 1.407(2) . ?
N H1B 0.8800 . ?
N H1A 0.78(3) . ?
C1 C2 1.408(2) . ?
C1 C6 1.409(2) . ?
C2 C3 1.397(2) . ?
C2 C7 1.486(2) . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.390(2) . ?
C5 H5 0.9500 . ?
C6 C13 1.498(2) . ?
C7 C12 1.416(2) . ?
C7 C8 1.418(3) . ?
C8 C9 1.389(3) . ?
C8 C19 1.509(3) . ?
C9 C10 1.394(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(3) . ?
C10 C20 1.517(3) . ?
C11 C12 1.388(3) . ?
C11 H11 0.9500 . ?
C12 C21 1.512(3) . ?
C13 C14 1.402(2) . ?
C13 C18 1.405(3) . ?
C14 C15 1.396(3) . ?
C14 C22 1.504(3) . ?
C15 C16 1.390(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.375(4) . ?
C16 C23 1.520(3) . ?
C17 C18 1.395(3) . ?
C17 H17 0.9500 . ?
C18 C24 1.514(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
Cl2A As1A Cl1A 95.98(2) . . ?
N As1B Cl1B 95.0(9) . . ?
N As1B Cl2B 99.1(7) . . ?
Cl1B As1B Cl2B 93.1(12) . . ?
N As1B H1A 15.9(13) . . ?
Cl1B As1B H1A 103.5(17) . . ?
Cl2B As1B H1A 111.5(15) . . ?
C1 N As1B 120.8(3) . . ?
C1 N H1B 119.6 . . ?
As1B N H1B 119.6 . . ?
C1 N H1A 113(2) . . ?
As1B N H1A 24(2) . . ?
H1B N H1A 122.1 . . ?
N C1 C2 121.25(15) . . ?
N C1 C6 118.00(14) . . ?
C2 C1 C6 120.73(15) . . ?
C3 C2 C1 118.35(16) . . ?
C3 C2 C7 121.94(15) . . ?
C1 C2 C7 119.69(14) . . ?
C4 C3 C2 121.21(17) . . ?
C4 C3 H3 119.4 . . ?
C2 C3 H3 119.4 . . ?
C3 C4 C5 119.97(17) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.72(18) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.01(16) . . ?
C5 C6 C13 122.01(16) . . ?
C1 C6 C13 118.98(15) . . ?
C12 C7 C8 119.86(16) . . ?
C12 C7 C2 119.71(16) . . ?
C8 C7 C2 120.42(15) . . ?
C9 C8 C7 118.96(17) . . ?
C9 C8 C19 120.52(17) . . ?
C7 C8 C19 120.51(17) . . ?
C8 C9 C10 121.60(18) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C11 C10 C9 118.54(18) . . ?
C11 C10 C20 120.1(2) . . ?
C9 C10 C20 121.3(2) . . ?
C10 C11 C12 122.39(18) . . ?
C10 C11 H11 118.8 . . ?
C12 C11 H11 118.8 . . ?
C11 C12 C7 118.47(17) . . ?
C11 C12 C21 120.49(17) . . ?
C7 C12 C21 121.03(17) . . ?
C14 C13 C18 120.05(17) . . ?
C14 C13 C6 119.65(16) . . ?
C18 C13 C6 120.14(16) . . ?
C15 C14 C13 118.90(19) . . ?
C15 C14 C22 120.32(17) . . ?
C13 C14 C22 120.76(16) . . ?
C16 C15 C14 121.70(19) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C17 C16 C15 118.4(2) . . ?
C17 C16 C23 121.1(3) . . ?
C15 C16 C23 120.5(2) . . ?
C16 C17 C18 122.3(2) . . ?
C16 C17 H17 118.9 . . ?
C18 C17 H17 118.9 . . ?
C17 C18 C13 118.7(2) . . ?
C17 C18 C24 120.7(2) . . ?
C13 C18 C24 120.60(19) . . ?
C8 C19 H19A 109.5 . . ?
C8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 H23A 109.5 . . ?
C16 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C16 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

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
Cl1B As1B N C1 159.8(8) . . . . ?
Cl2B As1B N C1 65.8(9) . . . . ?
As1B N C1 C2 -148.0(3) . . . . ?
As1B N C1 C6 33.7(4) . . . . ?
N C1 C2 C3 -177.40(16) . . . . ?
C6 C1 C2 C3 0.9(2) . . . . ?
N C1 C2 C7 4.3(2) . . . . ?
C6 C1 C2 C7 -177.40(15) . . . . ?
C1 C2 C3 C4 -0.7(3) . . . . ?
C7 C2 C3 C4 177.53(18) . . . . ?
C2 C3 C4 C5 0.2(3) . . . . ?
C3 C4 C5 C6 0.1(3) . . . . ?
C4 C5 C6 C1 0.0(3) . . . . ?
C4 C5 C6 C13 -179.55(18) . . . . ?
N C1 C6 C5 177.80(16) . . . . ?
C2 C1 C6 C5 -0.6(3) . . . . ?
N C1 C6 C13 -2.6(2) . . . . ?
C2 C1 C6 C13 179.02(15) . . . . ?
C3 C2 C7 C12 -78.5(2) . . . . ?
C1 C2 C7 C12 99.71(18) . . . . ?
C3 C2 C7 C8 102.8(2) . . . . ?
C1 C2 C7 C8 -78.9(2) . . . . ?
C12 C7 C8 C9 -3.5(2) . . . . ?
C2 C7 C8 C9 175.15(15) . . . . ?
C12 C7 C8 C19 177.36(15) . . . . ?
C2 C7 C8 C19 -4.0(2) . . . . ?
C7 C8 C9 C10 -0.1(3) . . . . ?
C19 C8 C9 C10 179.04(17) . . . . ?
C8 C9 C10 C11 2.7(3) . . . . ?
C8 C9 C10 C20 -177.9(2) . . . . ?
C9 C10 C11 C12 -1.7(3) . . . . ?
C20 C10 C11 C12 178.9(2) . . . . ?
C10 C11 C12 C7 -1.9(3) . . . . ?
C10 C11 C12 C21 177.44(18) . . . . ?
C8 C7 C12 C11 4.4(2) . . . . ?
C2 C7 C12 C11 -174.20(15) . . . . ?
C8 C7 C12 C21 -174.87(16) . . . . ?
C2 C7 C12 C21 6.5(2) . . . . ?
C5 C6 C13 C14 -94.8(2) . . . . ?
C1 C6 C13 C14 85.6(2) . . . . ?
C5 C6 C13 C18 89.8(2) . . . . ?
C1 C6 C13 C18 -89.8(2) . . . . ?
C18 C13 C14 C15 -0.7(3) . . . . ?
C6 C13 C14 C15 -176.06(17) . . . . ?
C18 C13 C14 C22 178.3(2) . . . . ?
C6 C13 C14 C22 2.9(3) . . . . ?
C13 C14 C15 C16 1.5(3) . . . . ?
C22 C14 C15 C16 -177.4(2) . . . . ?
C14 C15 C16 C17 -1.8(4) . . . . ?
C14 C15 C16 C23 177.8(2) . . . . ?
C15 C16 C17 C18 1.1(4) . . . . ?
C23 C16 C17 C18 -178.4(3) . . . . ?
C16 C17 C18 C13 -0.3(4) . . . . ?
C16 C17 C18 C24 178.9(3) . . . . ?
C14 C13 C18 C17 0.1(3) . . . . ?
C6 C13 C18 C17 175.4(2) . . . . ?
C14 C13 C18 C24 -179.1(2) . . . . ?
C6 C13 C18 C24 -3.8(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        32.50
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.068

#=============================================================================

data_ter_nhasclnipr2
_database_code_depnum_ccdc_archive 'CCDC 781915'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
[2,6-bis-(2,4,6-trimethylphenyl)phenyl]amino-diisopropylamino(chloro)arsane
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H40 As Cl N2'
_chemical_formula_sum            'C30 H40 As Cl N2'
_chemical_formula_weight         539.01

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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.960(2)
_cell_length_b                   11.400(2)
_cell_length_c                   11.530(2)
_cell_angle_alpha                86.53(3)
_cell_angle_beta                 87.06(3)
_cell_angle_gamma                83.06(3)
_cell_volume                     1426.0(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6872
_cell_measurement_theta_min      4.845
_cell_measurement_theta_max      45.413

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             568
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6726
_exptl_absorpt_correction_T_max  0.8916
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            24284
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         23.63
_reflns_number_total             4136
_reflns_number_gt                3336
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
The positions of the H atoms at N were refined freely, but are refined using
a riding model with <i>U</i>~iso~(H) = 1.2 times <i>U</i>~eq~(N). All other
H atoms were positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+1.0086P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4136
_refine_ls_number_parameters     404
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0375
_refine_ls_wR_factor_ref         0.0921
_refine_ls_wR_factor_gt          0.0862
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
As1A As 0.27655(4) 0.79318(4) 0.36373(3) 0.04538(18) Uani 0.7144(9) 1 d P A 1
Cl1A Cl 0.2293(4) 0.9897(4) 0.2963(2) 0.0534(7) Uani 0.7144(9) 1 d P A 1
N2A N 0.1220(14) 0.7439(11) 0.3835(9) 0.0494(19) Uani 0.7144(9) 1 d P A 1
C26A C -0.0069(9) 0.6538(9) 0.2566(8) 0.128(4) Uani 0.7144(9) 1 d P A 1
H26A H 0.0643 0.6025 0.2262 0.192 Uiso 0.7144(9) 1 calc PR A 1
H26B H -0.0681 0.6700 0.1969 0.192 Uiso 0.7144(9) 1 calc PR A 1
H26C H -0.0433 0.6142 0.3255 0.192 Uiso 0.7144(9) 1 calc PR A 1
C25A C 0.0339(5) 0.7690(5) 0.2895(5) 0.0638(13) Uani 0.7144(9) 1 d P A 1
H25 H 0.0804 0.8008 0.2201 0.077 Uiso 0.7144(9) 1 calc PR A 1
C27A C -0.0735(8) 0.8614(9) 0.3160(7) 0.085(2) Uani 0.7144(9) 1 d P A 1
H27A H -0.1221 0.8334 0.3836 0.128 Uiso 0.7144(9) 1 calc PR A 1
H27B H -0.1254 0.8753 0.2486 0.128 Uiso 0.7144(9) 1 calc PR A 1
H27C H -0.0426 0.9354 0.3330 0.128 Uiso 0.7144(9) 1 calc PR A 1
C28A C 0.0795(7) 0.7300(5) 0.5021(5) 0.0817(19) Uani 0.7144(9) 1 d P A 1
H28 H -0.0088 0.7170 0.4988 0.098 Uiso 0.7144(9) 1 calc PR A 1
C29A C 0.0784(9) 0.8295(7) 0.5696(5) 0.113(3) Uani 0.7144(9) 1 d P A 1
H29A H 0.1631 0.8457 0.5788 0.169 Uiso 0.7144(9) 1 calc PR A 1
H29B H 0.0392 0.8135 0.6462 0.169 Uiso 0.7144(9) 1 calc PR A 1
H29C H 0.0323 0.8984 0.5304 0.169 Uiso 0.7144(9) 1 calc PR A 1
C30A C 0.1470(11) 0.6077(11) 0.5394(11) 0.145(6) Uani 0.7144(9) 1 d P A 1
H30A H 0.2322 0.6161 0.5560 0.218 Uiso 0.7144(9) 1 calc PR A 1
H30B H 0.1463 0.5537 0.4766 0.218 Uiso 0.7144(9) 1 calc PR A 1
H30C H 0.1052 0.5757 0.6094 0.218 Uiso 0.7144(9) 1 calc PR A 1
As1B As 0.16679(9) 0.81468(9) 0.23791(9) 0.0397(4) Uani 0.2856(9) 1 d P A 2
Cl1B Cl 0.2231(13) 0.9761(13) 0.2959(11) 0.109(5) Uani 0.2856(9) 1 d P A 2
N2B N 0.112(4) 0.763(3) 0.357(3) 0.0494(19) Uani 0.2856(9) 1 d P A 2
C25B C -0.0341(11) 0.7652(13) 0.3773(10) 0.063(3) Uani 0.2856(9) 1 d P A 2
H25B H -0.0515 0.7318 0.4578 0.075 Uiso 0.2856(9) 1 calc PR A 2
C28B C 0.1694(15) 0.7138(14) 0.4682(16) 0.078(4) Uani 0.2856(9) 1 d P A 2
H28B H 0.2536 0.6745 0.4476 0.093 Uiso 0.2856(9) 1 calc PR A 2
C29B C 0.1776(19) 0.7810(17) 0.5836(17) 0.115(8) Uani 0.2856(9) 1 d P A 2
H29D H 0.1660 0.8666 0.5656 0.173 Uiso 0.2856(9) 1 calc PR A 2
H29E H 0.2586 0.7584 0.6160 0.173 Uiso 0.2856(9) 1 calc PR A 2
H29F H 0.1134 0.7594 0.6405 0.173 Uiso 0.2856(9) 1 calc PR A 2
C26B C -0.0815(16) 0.6912(19) 0.2950(17) 0.092(6) Uani 0.2856(9) 1 d P A 2
H26D H -0.0708 0.7259 0.2158 0.138 Uiso 0.2856(9) 1 calc PR A 2
H26E H -0.1692 0.6866 0.3134 0.138 Uiso 0.2856(9) 1 calc PR A 2
H26F H -0.0365 0.6116 0.3007 0.138 Uiso 0.2856(9) 1 calc PR A 2
C30B C 0.098(4) 0.617(2) 0.559(2) 0.144(16) Uani 0.2856(9) 1 d P A 2
H30D H 0.0125 0.6179 0.5357 0.215 Uiso 0.2856(9) 1 calc PR A 2
H30E H 0.0974 0.6414 0.6388 0.215 Uiso 0.2856(9) 1 calc PR A 2
H30F H 0.1412 0.5376 0.5532 0.215 Uiso 0.2856(9) 1 calc PR A 2
C27B C -0.080(2) 0.8944(17) 0.3724(16) 0.068(5) Uani 0.2856(9) 1 d P A 2
H27D H -0.0480 0.9315 0.4374 0.102 Uiso 0.2856(9) 1 calc PR A 2
H27E H -0.1698 0.9049 0.3778 0.102 Uiso 0.2856(9) 1 calc PR A 2
H27F H -0.0509 0.9316 0.2988 0.102 Uiso 0.2856(9) 1 calc PR A 2
N1 N 0.3153(2) 0.7276(2) 0.2276(2) 0.0409(6) Uani 1 1 d . . .
C1 C 0.4052(2) 0.7566(2) 0.1444(2) 0.0313(6) Uani 1 1 d . A .
C2 C 0.5227(2) 0.7704(2) 0.1770(2) 0.0337(6) Uani 1 1 d . . .
C3 C 0.6084(2) 0.7983(2) 0.0915(2) 0.0390(7) Uani 1 1 d . A .
H3 H 0.6888 0.8090 0.1128 0.047 Uiso 1 1 calc R . .
C4 C 0.5809(3) 0.8110(2) -0.0239(2) 0.0415(7) Uani 1 1 d . . .
H4 H 0.6408 0.8319 -0.0814 0.050 Uiso 1 1 calc R A .
C5 C 0.4655(2) 0.7929(2) -0.0547(2) 0.0388(7) Uani 1 1 d . A .
H5 H 0.4466 0.8000 -0.1345 0.047 Uiso 1 1 calc R . .
C6 C 0.3772(2) 0.7648(2) 0.0271(2) 0.0337(6) Uani 1 1 d . . .
C7 C 0.2552(2) 0.7434(2) -0.0123(2) 0.0359(6) Uani 1 1 d . A .
C8 C 0.2281(2) 0.6279(2) -0.0196(2) 0.0391(7) Uani 1 1 d . . .
C9 C 0.1170(3) 0.6099(3) -0.0629(3) 0.0496(8) Uani 1 1 d . A .
H9 H 0.0982 0.5313 -0.0684 0.060 Uiso 1 1 calc R . .
C10 C 0.0323(3) 0.7038(3) -0.0984(3) 0.0537(8) Uani 1 1 d . . .
C11 C 0.0603(3) 0.8167(3) -0.0897(3) 0.0505(8) Uani 1 1 d . A .
H11 H 0.0024 0.8814 -0.1137 0.061 Uiso 1 1 calc R . .
C12 C 0.1699(3) 0.8395(3) -0.0473(2) 0.0419(7) Uani 1 1 d . . .
C13 C 0.5591(2) 0.7545(2) 0.3003(2) 0.0357(6) Uani 1 1 d . A .
C14 C 0.5748(3) 0.6407(3) 0.3536(2) 0.0431(7) Uani 1 1 d . . .
C15 C 0.6063(3) 0.6276(3) 0.4693(2) 0.0513(8) Uani 1 1 d . A .
H15 H 0.6147 0.5508 0.5069 0.062 Uiso 1 1 calc R . .
C16 C 0.6259(3) 0.7233(3) 0.5311(3) 0.0531(8) Uani 1 1 d . . .
C17 C 0.6135(3) 0.8338(3) 0.4754(2) 0.0476(8) Uani 1 1 d . A .
H17 H 0.6283 0.8998 0.5168 0.057 Uiso 1 1 calc R . .
C18 C 0.5801(2) 0.8523(3) 0.3613(2) 0.0408(7) Uani 1 1 d . . .
C19 C 0.3179(3) 0.5236(3) 0.0185(3) 0.0504(8) Uani 1 1 d . A .
H19A H 0.3170 0.5159 0.1037 0.076 Uiso 1 1 calc R . .
H19B H 0.4008 0.5358 -0.0119 0.076 Uiso 1 1 calc R . .
H19C H 0.2943 0.4513 -0.0114 0.076 Uiso 1 1 calc R . .
C20 C -0.0880(3) 0.6828(4) -0.1457(4) 0.0844(13) Uani 1 1 d . A .
H20A H -0.0807 0.6030 -0.1746 0.127 Uiso 0.62(5) 1 calc PR B 1
H20B H -0.1089 0.7413 -0.2096 0.127 Uiso 0.62(5) 1 calc PR B 1
H20C H -0.1527 0.6905 -0.0839 0.127 Uiso 0.62(5) 1 calc PR B 1
H20D H -0.1481 0.7535 -0.1376 0.127 Uiso 0.38(5) 1 d PR B 2
H20E H -0.1197 0.6151 -0.1025 0.127 Uiso 0.38(5) 1 d PR B 2
H20F H -0.0759 0.6660 -0.2284 0.127 Uiso 0.38(5) 1 d PR B 2
C21 C 0.1953(3) 0.9646(3) -0.0365(3) 0.0603(9) Uani 1 1 d . A .
H21A H 0.1248 1.0191 -0.0628 0.090 Uiso 1 1 calc R . .
H21B H 0.2688 0.9793 -0.0847 0.090 Uiso 1 1 calc R . .
H21C H 0.2090 0.9771 0.0449 0.090 Uiso 1 1 calc R . .
C22 C 0.5612(3) 0.5324(3) 0.2885(3) 0.0554(8) Uani 1 1 d . A .
H22A H 0.5677 0.4624 0.3426 0.083 Uiso 1 1 calc R . .
H22B H 0.6263 0.5226 0.2272 0.083 Uiso 1 1 calc R . .
H22C H 0.4807 0.5419 0.2536 0.083 Uiso 1 1 calc R . .
C23 C 0.6624(4) 0.7050(4) 0.6564(3) 0.0772(11) Uani 1 1 d . A .
H23A H 0.6968 0.7752 0.6793 0.116 Uiso 1 1 calc R . .
H23B H 0.7243 0.6357 0.6643 0.116 Uiso 1 1 calc R . .
H23C H 0.5899 0.6923 0.7067 0.116 Uiso 1 1 calc R . .
C24 C 0.5687(3) 0.9751(3) 0.3061(3) 0.0509(8) Uani 1 1 d . A .
H24A H 0.6392 0.9836 0.2516 0.076 Uiso 1 1 calc R . .
H24B H 0.5670 1.0323 0.3664 0.076 Uiso 1 1 calc R . .
H24C H 0.4925 0.9899 0.2639 0.076 Uiso 1 1 calc R . .
H1A H 0.260(4) 0.713(4) 0.205(4) 0.061 Uiso 0.7144(9) 1 d P A 1
H1B H 0.347(12) 0.732(11) 0.278(11) 0.061 Uiso 0.2856(9) 1 d P A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As1A 0.0463(3) 0.0603(3) 0.0268(2) -0.00531(19) 0.00410(18) 0.0038(2)
Cl1A 0.0628(16) 0.0416(13) 0.0576(13) -0.0061(9) 0.0030(11) -0.0139(10)
N2A 0.058(3) 0.050(5) 0.031(6) 0.027(3) 0.018(5) 0.009(3)
C26A 0.169(10) 0.129(7) 0.102(6) -0.041(5) 0.033(7) -0.085(7)
C25A 0.053(3) 0.079(4) 0.061(3) -0.007(3) 0.004(3) -0.015(3)
C27A 0.052(4) 0.122(8) 0.079(6) -0.009(5) -0.006(4) 0.005(4)
C28A 0.081(4) 0.084(4) 0.063(4) 0.034(3) 0.040(4) 0.024(3)
C29A 0.182(9) 0.104(6) 0.042(3) -0.003(3) 0.023(4) 0.017(5)
C30A 0.112(6) 0.157(10) 0.130(10) 0.108(7) 0.050(6) 0.049(6)
As1B 0.0304(6) 0.0521(7) 0.0349(6) 0.0039(5) 0.0024(4) -0.0023(5)
Cl1B 0.098(7) 0.060(5) 0.169(9) -0.025(4) 0.043(5) -0.016(4)
N2B 0.058(3) 0.050(5) 0.031(6) 0.027(3) 0.018(5) 0.009(3)
C25B 0.039(6) 0.105(11) 0.043(7) 0.009(7) 0.024(6) -0.024(7)
C28B 0.055(10) 0.103(12) 0.066(11) 0.009(9) 0.024(9) 0.011(8)
C29B 0.123(16) 0.096(13) 0.109(15) 0.001(11) 0.093(14) 0.016(12)
C26B 0.082(13) 0.122(16) 0.083(14) 0.001(11) -0.009(10) -0.059(12)
C30B 0.32(5) 0.080(16) 0.042(10) 0.002(10) 0.04(2) -0.08(2)
C27B 0.053(9) 0.069(11) 0.078(14) -0.005(10) -0.002(11) 0.009(7)
N1 0.0355(16) 0.0557(16) 0.0310(15) -0.0026(13) 0.0049(12) -0.0054(13)
C1 0.0319(15) 0.0325(14) 0.0288(15) -0.0002(11) 0.0021(12) -0.0027(11)
C2 0.0345(15) 0.0345(15) 0.0316(15) -0.0042(12) -0.0008(12) -0.0015(12)
C3 0.0326(15) 0.0422(16) 0.0430(17) -0.0045(13) -0.0025(13) -0.0053(12)
C4 0.0379(17) 0.0521(18) 0.0338(16) 0.0001(13) 0.0065(13) -0.0071(13)
C5 0.0408(17) 0.0482(17) 0.0265(14) 0.0021(12) -0.0004(13) -0.0048(13)
C6 0.0320(15) 0.0376(15) 0.0311(15) -0.0014(12) -0.0002(12) -0.0028(12)
C7 0.0318(15) 0.0502(18) 0.0239(14) -0.0005(12) 0.0020(12) 0.0000(13)
C8 0.0328(16) 0.0484(18) 0.0355(16) -0.0008(13) -0.0032(13) -0.0028(13)
C9 0.0385(17) 0.060(2) 0.0512(19) -0.0017(15) -0.0047(15) -0.0102(15)
C10 0.0340(17) 0.080(2) 0.0468(19) 0.0067(17) -0.0074(15) -0.0080(16)
C11 0.0362(17) 0.068(2) 0.0425(18) 0.0076(15) -0.0034(14) 0.0076(15)
C12 0.0386(17) 0.0522(18) 0.0320(16) 0.0020(13) 0.0008(13) 0.0028(14)
C13 0.0315(15) 0.0475(17) 0.0281(14) -0.0059(13) 0.0005(12) -0.0037(12)
C14 0.0467(17) 0.0508(18) 0.0314(16) -0.0046(13) -0.0040(13) -0.0019(14)
C15 0.061(2) 0.057(2) 0.0349(17) 0.0022(15) -0.0099(15) -0.0020(15)
C16 0.052(2) 0.076(2) 0.0326(17) -0.0101(16) -0.0085(15) -0.0082(16)
C17 0.0462(18) 0.061(2) 0.0379(17) -0.0160(15) -0.0033(14) -0.0104(15)
C18 0.0331(16) 0.0543(19) 0.0352(16) -0.0092(14) 0.0028(13) -0.0045(13)
C19 0.0418(17) 0.0504(19) 0.059(2) -0.0030(15) -0.0089(15) -0.0028(14)
C20 0.043(2) 0.112(3) 0.100(3) 0.016(3) -0.028(2) -0.016(2)
C21 0.058(2) 0.051(2) 0.066(2) 0.0019(17) -0.0069(18) 0.0116(16)
C22 0.080(2) 0.0464(18) 0.0391(17) -0.0027(14) -0.0110(17) -0.0014(16)
C23 0.100(3) 0.096(3) 0.040(2) -0.0037(19) -0.025(2) -0.020(2)
C24 0.0542(19) 0.0521(19) 0.0482(19) -0.0133(15) 0.0009(15) -0.0094(15)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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
As1A N1 1.789(3) . ?
As1A N2A 1.848(16) . ?
As1A Cl1A 2.333(4) . ?
As1A H1B 1.39(13) . ?
N2A C28A 1.427(11) . ?
N2A C25A 1.480(14) . ?
C26A C25A 1.513(9) . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
C25A C27A 1.514(10) . ?
C25A H25 1.0000 . ?
C27A H27A 0.9800 . ?
C27A H27B 0.9800 . ?
C27A H27C 0.9800 . ?
C28A C29A 1.413(10) . ?
C28A C30A 1.545(12) . ?
C28A H28 1.0000 . ?
C29A H29A 0.9800 . ?
C29A H29B 0.9800 . ?
C29A H29C 0.9800 . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
As1B N2B 1.58(3) . ?
As1B N1 1.803(3) . ?
As1B Cl1B 2.163(14) . ?
As1B H1A 1.50(5) . ?
N2B C28B 1.50(3) . ?
N2B C25B 1.61(5) . ?
C25B C26B 1.46(2) . ?
C25B C27B 1.50(2) . ?
C25B H25B 1.0000 . ?
C28B C29B 1.59(3) . ?
C28B C30B 1.70(3) . ?
C28B H28B 1.0000 . ?
C29B H29D 0.9800 . ?
C29B H29E 0.9800 . ?
C29B H29F 0.9800 . ?
C26B H26D 0.9800 . ?
C26B H26E 0.9800 . ?
C26B H26F 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C27B H27D 0.9800 . ?
C27B H27E 0.9800 . ?
C27B H27F 0.9800 . ?
N1 C1 1.395(4) . ?
N1 H1A 0.72(5) . ?
N1 H1B 0.70(12) . ?
C1 C2 1.390(4) . ?
C1 C6 1.397(4) . ?
C2 C3 1.376(4) . ?
C2 C13 1.491(4) . ?
C3 C4 1.375(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.369(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.485(4) . ?
C7 C8 1.393(4) . ?
C7 C12 1.405(4) . ?
C8 C9 1.381(4) . ?
C8 C19 1.508(4) . ?
C9 C10 1.386(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.370(4) . ?
C10 C20 1.502(4) . ?
C11 C12 1.378(4) . ?
C11 H11 0.9500 . ?
C12 C21 1.500(4) . ?
C13 C14 1.397(4) . ?
C13 C18 1.401(4) . ?
C14 C15 1.390(4) . ?
C14 C22 1.509(4) . ?
C15 C16 1.382(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.374(4) . ?
C16 C23 1.515(4) . ?
C17 C18 1.380(4) . ?
C17 H17 0.9500 . ?
C18 C24 1.497(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 H20D 0.9829 . ?
C20 H20E 0.9829 . ?
C20 H20F 0.9830 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?

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
N1 As1A N2A 96.0(4) . . ?
N1 As1A Cl1A 99.16(12) . . ?
N2A As1A Cl1A 101.6(3) . . ?
N1 As1A H1B 21(5) . . ?
N2A As1A H1B 111(5) . . ?
Cl1A As1A H1B 109(5) . . ?
C28A N2A C25A 120.8(10) . . ?
C28A N2A As1A 114.2(9) . . ?
C25A N2A As1A 119.8(5) . . ?
N2A C25A C26A 109.0(8) . . ?
N2A C25A C27A 114.5(7) . . ?
C26A C25A C27A 112.5(6) . . ?
N2A C25A H25 106.8 . . ?
C26A C25A H25 106.8 . . ?
C27A C25A H25 106.8 . . ?
C29A C28A N2A 116.3(8) . . ?
C29A C28A C30A 122.1(8) . . ?
N2A C28A C30A 101.8(7) . . ?
C29A C28A H28 105.0 . . ?
N2A C28A H28 105.0 . . ?
C30A C28A H28 105.0 . . ?
N2B As1B N1 101.3(14) . . ?
N2B As1B Cl1B 99.3(18) . . ?
N1 As1B Cl1B 99.1(4) . . ?
N2B As1B H1A 101(2) . . ?
N1 As1B H1A 22.9(18) . . ?
Cl1B As1B H1A 121.4(19) . . ?
C28B N2B As1B 133(3) . . ?
C28B N2B C25B 107(2) . . ?
As1B N2B C25B 119(2) . . ?
C26B C25B C27B 118.1(15) . . ?
C26B C25B N2B 110(2) . . ?
C27B C25B N2B 103.3(17) . . ?
C26B C25B H25B 108.3 . . ?
C27B C25B H25B 108.3 . . ?
N2B C25B H25B 108.3 . . ?
N2B C28B C29B 127(2) . . ?
N2B C28B C30B 120(2) . . ?
C29B C28B C30B 83.6(13) . . ?
N2B C28B H28B 107.6 . . ?
C29B C28B H28B 107.6 . . ?
C30B C28B H28B 107.6 . . ?
C28B C29B H29D 109.5 . . ?
C28B C29B H29E 109.5 . . ?
H29D C29B H29E 109.5 . . ?
C28B C29B H29F 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C25B C26B H26D 109.5 . . ?
C25B C26B H26E 109.5 . . ?
H26D C26B H26E 109.5 . . ?
C25B C26B H26F 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C28B C30B H30D 109.5 . . ?
C28B C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C28B C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C25B C27B H27D 109.5 . . ?
C25B C27B H27E 109.5 . . ?
H27D C27B H27E 109.5 . . ?
C25B C27B H27F 109.5 . . ?
H27D C27B H27F 109.5 . . ?
H27E C27B H27F 109.5 . . ?
C1 N1 As1A 127.4(2) . . ?
C1 N1 As1B 121.3(2) . . ?
As1A N1 As1B 64.52(10) . . ?
C1 N1 H1A 115(4) . . ?
As1A N1 H1A 108(4) . . ?
As1B N1 H1A 54(4) . . ?
C1 N1 H1B 99(10) . . ?
As1A N1 H1B 46(10) . . ?
As1B N1 H1B 110(10) . . ?
H1A N1 H1B 145(10) . . ?
C2 C1 N1 120.6(2) . . ?
C2 C1 C6 120.6(2) . . ?
N1 C1 C6 118.8(2) . . ?
C3 C2 C1 118.3(2) . . ?
C3 C2 C13 119.3(2) . . ?
C1 C2 C13 122.4(2) . . ?
C4 C3 C2 121.8(3) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C6 C5 C4 121.4(3) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C1 118.9(2) . . ?
C5 C6 C7 118.7(2) . . ?
C1 C6 C7 122.5(2) . . ?
C8 C7 C12 120.2(3) . . ?
C8 C7 C6 119.8(2) . . ?
C12 C7 C6 120.0(2) . . ?
C9 C8 C7 118.8(3) . . ?
C9 C8 C19 120.1(3) . . ?
C7 C8 C19 121.0(2) . . ?
C8 C9 C10 121.6(3) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C11 C10 C9 118.6(3) . . ?
C11 C10 C20 120.4(3) . . ?
C9 C10 C20 121.0(3) . . ?
C10 C11 C12 122.0(3) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C11 C12 C7 118.7(3) . . ?
C11 C12 C21 120.2(3) . . ?
C7 C12 C21 121.1(3) . . ?
C14 C13 C18 120.3(2) . . ?
C14 C13 C2 119.3(2) . . ?
C18 C13 C2 120.4(2) . . ?
C15 C14 C13 118.6(3) . . ?
C15 C14 C22 119.5(3) . . ?
C13 C14 C22 121.9(2) . . ?
C16 C15 C14 121.8(3) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C17 C16 C15 118.3(3) . . ?
C17 C16 C23 121.5(3) . . ?
C15 C16 C23 120.2(3) . . ?
C16 C17 C18 122.3(3) . . ?
C16 C17 H17 118.8 . . ?
C18 C17 H17 118.8 . . ?
C17 C18 C13 118.6(3) . . ?
C17 C18 C24 119.4(3) . . ?
C13 C18 C24 122.0(2) . . ?
C8 C19 H19A 109.5 . . ?
C8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
C10 C20 H20D 109.8 . . ?
C10 C20 H20E 109.8 . . ?
H20D C20 H20E 109.2 . . ?
C10 C20 H20F 109.8 . . ?
H20D C20 H20F 109.2 . . ?
H20E C20 H20F 109.2 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 H23A 109.5 . . ?
C16 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C16 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

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
N1 As1A N2A C28A 152.8(7) . . . . ?
Cl1A As1A N2A C28A -106.5(7) . . . . ?
N1 As1A N2A C25A -52.4(9) . . . . ?
Cl1A As1A N2A C25A 48.2(10) . . . . ?
C28A N2A C25A C26A -83.0(12) . . . . ?
As1A N2A C25A C26A 123.9(8) . . . . ?
C28A N2A C25A C27A 43.9(13) . . . . ?
As1A N2A C25A C27A -109.1(9) . . . . ?
C25A N2A C28A C29A -99.4(13) . . . . ?
As1A N2A C28A C29A 55.0(10) . . . . ?
C25A N2A C28A C30A 125.4(11) . . . . ?
As1A N2A C28A C30A -80.1(10) . . . . ?
N1 As1B N2B C28B 33(4) . . . . ?
Cl1B As1B N2B C28B -69(4) . . . . ?
N1 As1B N2B C25B -151(3) . . . . ?
Cl1B As1B N2B C25B 107(3) . . . . ?
C28B N2B C25B C26B -119(3) . . . . ?
As1B N2B C25B C26B 64(3) . . . . ?
C28B N2B C25B C27B 113(2) . . . . ?
As1B N2B C25B C27B -64(3) . . . . ?
As1B N2B C28B C29B 98(4) . . . . ?
C25B N2B C28B C29B -78(3) . . . . ?
As1B N2B C28B C30B -155(3) . . . . ?
C25B N2B C28B C30B 28(4) . . . . ?
N2A As1A N1 C1 160.1(3) . . . . ?
Cl1A As1A N1 C1 57.3(3) . . . . ?
N2A As1A N1 As1B 49.0(2) . . . . ?
Cl1A As1A N1 As1B -53.80(13) . . . . ?
N2B As1B N1 C1 -168.9(19) . . . . ?
Cl1B As1B N1 C1 -67.4(4) . . . . ?
N2B As1B N1 As1A -49.0(19) . . . . ?
Cl1B As1B N1 As1A 52.5(4) . . . . ?
As1A N1 C1 C2 46.7(4) . . . . ?
As1B N1 C1 C2 127.0(2) . . . . ?
As1A N1 C1 C6 -137.0(2) . . . . ?
As1B N1 C1 C6 -56.7(3) . . . . ?
N1 C1 C2 C3 179.6(2) . . . . ?
C6 C1 C2 C3 3.3(4) . . . . ?
N1 C1 C2 C13 0.4(4) . . . . ?
C6 C1 C2 C13 -175.8(2) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
C13 C2 C3 C4 178.3(3) . . . . ?
C2 C3 C4 C5 -1.4(4) . . . . ?
C3 C4 C5 C6 1.3(4) . . . . ?
C4 C5 C6 C1 1.1(4) . . . . ?
C4 C5 C6 C7 -178.5(2) . . . . ?
C2 C1 C6 C5 -3.4(4) . . . . ?
N1 C1 C6 C5 -179.8(2) . . . . ?
C2 C1 C6 C7 176.1(2) . . . . ?
N1 C1 C6 C7 -0.2(4) . . . . ?
C5 C6 C7 C8 100.2(3) . . . . ?
C1 C6 C7 C8 -79.4(3) . . . . ?
C5 C6 C7 C12 -76.8(3) . . . . ?
C1 C6 C7 C12 103.6(3) . . . . ?
C12 C7 C8 C9 0.8(4) . . . . ?
C6 C7 C8 C9 -176.3(3) . . . . ?
C12 C7 C8 C19 -179.4(3) . . . . ?
C6 C7 C8 C19 3.5(4) . . . . ?
C7 C8 C9 C10 -0.3(4) . . . . ?
C19 C8 C9 C10 179.8(3) . . . . ?
C8 C9 C10 C11 -0.2(5) . . . . ?
C8 C9 C10 C20 179.8(3) . . . . ?
C9 C10 C11 C12 0.3(5) . . . . ?
C20 C10 C11 C12 -179.7(3) . . . . ?
C10 C11 C12 C7 0.2(4) . . . . ?
C10 C11 C12 C21 -178.4(3) . . . . ?
C8 C7 C12 C11 -0.7(4) . . . . ?
C6 C7 C12 C11 176.3(2) . . . . ?
C8 C7 C12 C21 177.9(3) . . . . ?
C6 C7 C12 C21 -5.0(4) . . . . ?
C3 C2 C13 C14 -107.0(3) . . . . ?
C1 C2 C13 C14 72.1(3) . . . . ?
C3 C2 C13 C18 71.6(3) . . . . ?
C1 C2 C13 C18 -109.3(3) . . . . ?
C18 C13 C14 C15 2.7(4) . . . . ?
C2 C13 C14 C15 -178.7(3) . . . . ?
C18 C13 C14 C22 -175.9(3) . . . . ?
C2 C13 C14 C22 2.7(4) . . . . ?
C13 C14 C15 C16 -1.9(5) . . . . ?
C22 C14 C15 C16 176.7(3) . . . . ?
C14 C15 C16 C17 0.0(5) . . . . ?
C14 C15 C16 C23 -178.9(3) . . . . ?
C15 C16 C17 C18 1.2(5) . . . . ?
C23 C16 C17 C18 -180.0(3) . . . . ?
C16 C17 C18 C13 -0.5(4) . . . . ?
C16 C17 C18 C24 -179.8(3) . . . . ?
C14 C13 C18 C17 -1.5(4) . . . . ?
C2 C13 C18 C17 179.9(2) . . . . ?
C14 C13 C18 C24 177.8(3) . . . . ?
C2 C13 C18 C24 -0.7(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.965
_diffrn_reflns_theta_full        23.63
_diffrn_measured_fraction_theta_full 0.965
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.039

#=============================================================================

data_ter_nhascldbu
_database_code_depnum_ccdc_archive 'CCDC 781916'
#TrackingRef '- TerN2Pn2Cl2_submitted.cif'

# start Validation Reply Form
_vrf_PLAT432_ter_nhascldbu       
;
PROBLEM: Short Inter X...Y Contact As .. Cl .. 2.61 Ang.
RESPONSE: Can be considered as normal in this type of compound.
;
# end Validation Reply Form

_audit_author_name               'Villinger, A.'
_audit_creation_method           SHELXL-97

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
2-[2,6-bis-(2,4,6-trimethylphenyl)phenyl]amino-2-arsa-3,7-diaza-
tricyclo[5.4.1.03,12]dodec-3(12)-enylium chloride
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H41 As N3 +, Cl -'
_chemical_formula_sum            'C33 H41 As Cl N3'
_chemical_formula_weight         590.06

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'
As As 0.0499 2.0058 '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'
N N 0.0061 0.0033 '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'

#==============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.158(2)
_cell_length_b                   11.122(2)
_cell_length_c                   14.580(3)
_cell_angle_alpha                96.83(3)
_cell_angle_beta                 100.13(3)
_cell_angle_gamma                110.10(3)
_cell_volume                     1493.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8298
_cell_measurement_theta_min      4.432
_cell_measurement_theta_max      65.646

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             620
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6825
_exptl_absorpt_correction_T_max  0.8152
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius Apex-X8-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            48634
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         35.00
_reflns_number_total             12631
_reflns_number_gt                9234
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Bruker Apex v7.51a'
_computing_cell_refinement       'Bruker Apex v7.51a'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-97

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
The H atom2 at N and C26 were refined freely. All other H atoms were
positioned geometrically and refined using a riding model,
with C---H = 0.98 (methyl groups), 0.99\%A (methylene groups),
1.00\%A (methine groups) or 0.95 \%A (aryl CH) and with <i>U</i>~iso~(H) =
1.5 times <i>U</i>~eq~(C) (methyl groups) or with <i>U</i>~iso~(H) = 1.2 times
<i>U</i>~eq~(C) (methylene groups, aryl CH, methine groups). Torsion angles
of all methyl groups were allowed to refine.

Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12631
_refine_ls_number_parameters     357
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0915
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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 0.406514(13) 0.343262(12) 0.351537(9) 0.02137(4) Uani 1 1 d . . .
Cl Cl 0.26780(4) 0.48459(4) 0.40969(2) 0.03187(7) Uani 1 1 d . . .
N1 N 0.31440(11) 0.31504(11) 0.22455(7) 0.0231(2) Uani 1 1 d . . .
N2 N 0.58531(12) 0.30885(11) 0.32150(8) 0.0276(2) Uani 1 1 d . . .
N3 N 0.80643(12) 0.48468(12) 0.34737(9) 0.0312(3) Uani 1 1 d . . .
C1 C 0.16505(13) 0.24785(12) 0.19231(8) 0.0208(2) Uani 1 1 d . . .
C2 C 0.09472(14) 0.12902(12) 0.21960(9) 0.0239(2) Uani 1 1 d . . .
C3 C -0.05468(15) 0.06915(13) 0.18815(9) 0.0283(3) Uani 1 1 d . . .
H3 H -0.1035 -0.0086 0.2087 0.034 Uiso 1 1 calc R . .
C4 C -0.13363(15) 0.11960(14) 0.12806(10) 0.0329(3) Uani 1 1 d . . .
H4 H -0.2356 0.0786 0.1092 0.040 Uiso 1 1 calc R . .
C5 C -0.06237(15) 0.23099(14) 0.09548(10) 0.0304(3) Uani 1 1 d . . .
H5 H -0.1158 0.2638 0.0518 0.036 Uiso 1 1 calc R . .
C6 C 0.08622(14) 0.29510(12) 0.12592(9) 0.0235(2) Uani 1 1 d . . .
C7 C 0.16478(14) 0.40705(13) 0.08305(9) 0.0249(2) Uani 1 1 d . . .
C8 C 0.17844(15) 0.53531(13) 0.11632(9) 0.0274(3) Uani 1 1 d . . .
C9 C 0.26034(15) 0.63562(14) 0.07684(10) 0.0322(3) Uani 1 1 d . . .
H9 H 0.2703 0.7227 0.0997 0.039 Uiso 1 1 calc R . .
C10 C 0.32739(16) 0.61248(16) 0.00569(11) 0.0367(3) Uani 1 1 d . . .
C11 C 0.30874(17) 0.48485(17) -0.02825(11) 0.0388(3) Uani 1 1 d . . .
H11 H 0.3531 0.4673 -0.0777 0.047 Uiso 1 1 calc R . .
C12 C 0.22660(16) 0.38111(15) 0.00803(10) 0.0320(3) Uani 1 1 d . . .
C13 C 0.17516(14) 0.06012(12) 0.27471(9) 0.0240(2) Uani 1 1 d . . .
C14 C 0.15986(14) 0.04342(12) 0.36699(9) 0.0250(2) Uani 1 1 d . . .
C15 C 0.22973(15) -0.02749(13) 0.41425(10) 0.0293(3) Uani 1 1 d . . .
H15 H 0.2191 -0.0383 0.4765 0.035 Uiso 1 1 calc R . .
C16 C 0.31411(16) -0.08262(13) 0.37363(10) 0.0307(3) Uani 1 1 d . . .
C17 C 0.32811(16) -0.06502(13) 0.28272(10) 0.0318(3) Uani 1 1 d . . .
H17 H 0.3862 -0.1016 0.2539 0.038 Uiso 1 1 calc R . .
C18 C 0.25974(16) 0.00474(13) 0.23205(10) 0.0283(3) Uani 1 1 d . . .
C19 C 0.10386(18) 0.56539(14) 0.19094(11) 0.0365(3) Uani 1 1 d . . .
H19A H 0.1308 0.6600 0.2078 0.055 Uiso 1 1 calc R . .
H19B H 0.1328 0.5324 0.2474 0.055 Uiso 1 1 calc R . .
H19C H -0.0007 0.5234 0.1664 0.055 Uiso 1 1 calc R . .
C20 C 0.4148(2) 0.7222(2) -0.03701(15) 0.0568(5) Uani 1 1 d . . .
H20A H 0.4880 0.6981 -0.0615 0.085 Uiso 1 1 calc R . .
H20B H 0.4621 0.8018 0.0119 0.085 Uiso 1 1 calc R . .
H20C H 0.3509 0.7376 -0.0890 0.085 Uiso 1 1 calc R . .
C21 C 0.2011(2) 0.24371(17) -0.03590(12) 0.0465(4) Uani 1 1 d . . .
H21A H 0.2271 0.1983 0.0137 0.070 Uiso 1 1 calc R . .
H21B H 0.2604 0.2449 -0.0823 0.070 Uiso 1 1 calc R . .
H21C H 0.0991 0.1982 -0.0678 0.070 Uiso 1 1 calc R . .
C22 C 0.07430(16) 0.10512(14) 0.41556(10) 0.0320(3) Uani 1 1 d . . .
H22A H -0.0288 0.0566 0.3880 0.048 Uiso 1 1 calc R . .
H22B H 0.1000 0.1957 0.4069 0.048 Uiso 1 1 calc R . .
H22C H 0.0956 0.1034 0.4835 0.048 Uiso 1 1 calc R . .
C23 C 0.3897(2) -0.15927(16) 0.42493(12) 0.0431(4) Uani 1 1 d . . .
H23A H 0.4118 -0.1271 0.4936 0.065 Uiso 1 1 calc R . .
H23B H 0.4794 -0.1486 0.4047 0.065 Uiso 1 1 calc R . .
H23C H 0.3270 -0.2519 0.4099 0.065 Uiso 1 1 calc R . .
C24 C 0.2800(2) 0.01979(16) 0.13384(11) 0.0397(4) Uani 1 1 d . . .
H24A H 0.3421 0.1100 0.1352 0.060 Uiso 1 1 calc R . .
H24B H 0.1861 -0.0012 0.0907 0.060 Uiso 1 1 calc R . .
H24C H 0.3251 -0.0396 0.1115 0.060 Uiso 1 1 calc R . .
C25 C 0.66506(13) 0.43360(13) 0.34116(9) 0.0248(2) Uani 1 1 d . . .
C26 C 0.57187(13) 0.50836(13) 0.35599(9) 0.0234(2) Uani 1 1 d . . .
C27 C 0.55968(14) 0.59659(13) 0.28549(10) 0.0295(3) Uani 1 1 d . . .
H27A H 0.4748 0.6203 0.2882 0.035 Uiso 1 1 calc R . .
H27B H 0.5449 0.5488 0.2204 0.035 Uiso 1 1 calc R . .
C28 C 0.69582(17) 0.72172(15) 0.30703(13) 0.0402(4) Uani 1 1 d . . .
H28A H 0.6803 0.7784 0.2621 0.048 Uiso 1 1 calc R . .
H28B H 0.7084 0.7691 0.3718 0.048 Uiso 1 1 calc R . .
C29 C 0.83474(16) 0.70076(16) 0.30062(12) 0.0399(4) Uani 1 1 d . . .
H29A H 0.8218 0.6533 0.2357 0.048 Uiso 1 1 calc R . .
H29B H 0.9125 0.7873 0.3092 0.048 Uiso 1 1 calc R . .
C30 C 0.88476(15) 0.62625(15) 0.37138(11) 0.0367(3) Uani 1 1 d . . .
H30A H 0.9885 0.6447 0.3759 0.044 Uiso 1 1 calc R . .
H30B H 0.8743 0.6593 0.4347 0.044 Uiso 1 1 calc R . .
C31 C 0.88380(18) 0.39571(18) 0.33965(15) 0.0485(4) Uani 1 1 d . . .
H31A H 0.9827 0.4380 0.3802 0.058 Uiso 1 1 calc R . .
H31B H 0.8912 0.3762 0.2731 0.058 Uiso 1 1 calc R . .
C32 C 0.80561(18) 0.27001(18) 0.37023(15) 0.0498(4) Uani 1 1 d . . .
H32A H 0.8535 0.2076 0.3589 0.060 Uiso 1 1 calc R . .
H32B H 0.8097 0.2879 0.4390 0.060 Uiso 1 1 calc R . .
C33 C 0.65014(17) 0.21077(15) 0.31525(12) 0.0365(3) Uani 1 1 d . . .
H33A H 0.6451 0.1787 0.2479 0.044 Uiso 1 1 calc R . .
H33B H 0.5965 0.1357 0.3417 0.044 Uiso 1 1 calc R . .
H1 H 0.3412(19) 0.3832(17) 0.1997(13) 0.040(5) Uiso 1 1 d . . .
H2 H 0.5970(18) 0.5538(15) 0.4198(12) 0.032(4) Uiso 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As 0.01924(6) 0.02457(7) 0.02066(6) 0.00792(5) 0.00391(4) 0.00781(5)
Cl 0.02951(15) 0.03946(18) 0.03236(17) 0.01155(14) 0.00848(12) 0.01776(15)
N1 0.0206(5) 0.0240(5) 0.0221(5) 0.0082(4) 0.0029(4) 0.0048(4)
N2 0.0242(5) 0.0317(6) 0.0295(6) 0.0089(5) 0.0066(4) 0.0125(5)
N3 0.0195(5) 0.0391(7) 0.0353(6) 0.0094(5) 0.0081(4) 0.0099(5)
C1 0.0214(5) 0.0214(5) 0.0183(5) 0.0040(4) 0.0031(4) 0.0071(5)
C2 0.0266(6) 0.0214(6) 0.0200(5) 0.0039(4) 0.0024(4) 0.0059(5)
C3 0.0276(6) 0.0226(6) 0.0288(6) 0.0068(5) 0.0034(5) 0.0028(5)
C4 0.0233(6) 0.0325(7) 0.0340(7) 0.0064(6) -0.0009(5) 0.0031(6)
C5 0.0267(6) 0.0316(7) 0.0278(6) 0.0083(5) -0.0022(5) 0.0080(6)
C6 0.0259(6) 0.0226(6) 0.0202(5) 0.0054(4) 0.0024(4) 0.0082(5)
C7 0.0248(6) 0.0280(6) 0.0207(5) 0.0094(5) 0.0015(4) 0.0086(5)
C8 0.0286(6) 0.0281(6) 0.0237(6) 0.0102(5) 0.0012(5) 0.0092(5)
C9 0.0325(7) 0.0280(7) 0.0332(7) 0.0138(6) 0.0027(6) 0.0075(6)
C10 0.0308(7) 0.0435(9) 0.0371(8) 0.0230(7) 0.0081(6) 0.0103(7)
C11 0.0394(8) 0.0533(10) 0.0317(7) 0.0202(7) 0.0139(6) 0.0202(8)
C12 0.0349(7) 0.0383(8) 0.0260(6) 0.0123(6) 0.0070(5) 0.0156(6)
C13 0.0273(6) 0.0183(5) 0.0235(6) 0.0054(4) 0.0034(5) 0.0057(5)
C14 0.0264(6) 0.0195(6) 0.0263(6) 0.0068(5) 0.0050(5) 0.0050(5)
C15 0.0337(7) 0.0236(6) 0.0276(6) 0.0096(5) 0.0046(5) 0.0069(5)
C16 0.0331(7) 0.0207(6) 0.0346(7) 0.0076(5) 0.0013(6) 0.0079(6)
C17 0.0374(7) 0.0237(6) 0.0354(7) 0.0046(5) 0.0080(6) 0.0133(6)
C18 0.0355(7) 0.0215(6) 0.0262(6) 0.0040(5) 0.0062(5) 0.0092(5)
C19 0.0471(9) 0.0296(7) 0.0348(8) 0.0098(6) 0.0123(6) 0.0144(7)
C20 0.0493(10) 0.0600(12) 0.0707(13) 0.0418(10) 0.0273(9) 0.0158(9)
C21 0.0656(12) 0.0480(10) 0.0345(8) 0.0084(7) 0.0192(8) 0.0276(9)
C22 0.0391(8) 0.0320(7) 0.0297(7) 0.0123(6) 0.0134(6) 0.0145(6)
C23 0.0529(10) 0.0361(8) 0.0462(9) 0.0159(7) 0.0053(7) 0.0241(8)
C24 0.0581(10) 0.0362(8) 0.0325(8) 0.0074(6) 0.0175(7) 0.0234(8)
C25 0.0199(5) 0.0331(7) 0.0205(5) 0.0066(5) 0.0035(4) 0.0088(5)
C26 0.0206(5) 0.0264(6) 0.0221(6) 0.0052(5) 0.0044(4) 0.0075(5)
C27 0.0250(6) 0.0288(7) 0.0308(7) 0.0094(5) 0.0030(5) 0.0057(5)
C28 0.0356(8) 0.0275(7) 0.0482(9) 0.0117(6) 0.0042(7) 0.0015(6)
C29 0.0298(7) 0.0346(8) 0.0433(9) 0.0109(7) 0.0057(6) -0.0026(6)
C30 0.0214(6) 0.0414(8) 0.0372(8) 0.0051(6) 0.0030(5) 0.0023(6)
C31 0.0289(7) 0.0551(10) 0.0726(12) 0.0212(9) 0.0209(8) 0.0220(8)
C32 0.0322(8) 0.0551(10) 0.0735(13) 0.0256(9) 0.0121(8) 0.0260(8)
C33 0.0362(8) 0.0362(8) 0.0464(9) 0.0128(7) 0.0134(6) 0.0214(7)

#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;

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 N1 1.8581(12) . ?
As C26 2.0026(15) . ?
As N2 2.0867(12) . ?
As Cl 2.6078(7) . ?
N1 C1 1.4026(16) . ?
N1 H1 0.859(18) . ?
N2 C25 1.3095(18) . ?
N2 C33 1.4572(18) . ?
N3 C25 1.3321(17) . ?
N3 C30 1.465(2) . ?
N3 C31 1.466(2) . ?
C1 C2 1.4112(18) . ?
C1 C6 1.4113(17) . ?
C2 C3 1.3946(19) . ?
C2 C13 1.4988(18) . ?
C3 C4 1.3802(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.389(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.3903(19) . ?
C5 H5 0.9500 . ?
C6 C7 1.5018(18) . ?
C7 C12 1.402(2) . ?
C7 C8 1.4019(19) . ?
C8 C9 1.3969(19) . ?
C8 C19 1.499(2) . ?
C9 C10 1.383(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(2) . ?
C10 C20 1.515(2) . ?
C11 C12 1.395(2) . ?
C11 H11 0.9500 . ?
C12 C21 1.500(2) . ?
C13 C18 1.402(2) . ?
C13 C14 1.4077(18) . ?
C14 C15 1.3938(18) . ?
C14 C22 1.496(2) . ?
C15 C16 1.384(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.387(2) . ?
C16 C23 1.5085(19) . ?
C17 C18 1.3987(19) . ?
C17 H17 0.9500 . ?
C18 C24 1.503(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.4847(19) . ?
C26 C27 1.5211(18) . ?
C26 H2 0.950(16) . ?
C27 C28 1.539(2) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.524(2) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.522(2) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.515(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.511(2) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?

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
N1 As C26 98.23(6) . . ?
N1 As N2 94.09(5) . . ?
C26 As N2 67.47(5) . . ?
N1 As Cl 93.94(4) . . ?
C26 As Cl 88.63(4) . . ?
N2 As Cl 155.64(4) . . ?
C1 N1 As 121.64(9) . . ?
C1 N1 H1 109.8(12) . . ?
As N1 H1 113.4(12) . . ?
C25 N2 C33 121.06(12) . . ?
C25 N2 As 92.34(9) . . ?
C33 N2 As 143.36(10) . . ?
C25 N3 C30 120.65(13) . . ?
C25 N3 C31 118.29(13) . . ?
C30 N3 C31 120.74(12) . . ?
N1 C1 C2 121.03(11) . . ?
N1 C1 C6 119.16(11) . . ?
C2 C1 C6 119.64(11) . . ?
C3 C2 C1 118.43(11) . . ?
C3 C2 C13 118.85(11) . . ?
C1 C2 C13 122.55(11) . . ?
C4 C3 C2 121.90(12) . . ?
C4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
C3 C4 C5 119.29(13) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C4 C5 C6 120.83(12) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 119.49(12) . . ?
C5 C6 C7 120.65(11) . . ?
C1 C6 C7 119.66(11) . . ?
C12 C7 C8 119.70(12) . . ?
C12 C7 C6 118.33(12) . . ?
C8 C7 C6 121.96(12) . . ?
C9 C8 C7 118.79(13) . . ?
C9 C8 C19 119.96(13) . . ?
C7 C8 C19 121.23(12) . . ?
C10 C9 C8 122.22(14) . . ?
C10 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C11 C10 C9 118.08(14) . . ?
C11 C10 C20 120.29(16) . . ?
C9 C10 C20 121.60(16) . . ?
C10 C11 C12 121.88(15) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C7 119.21(14) . . ?
C11 C12 C21 119.75(14) . . ?
C7 C12 C21 121.00(13) . . ?
C18 C13 C14 119.43(12) . . ?
C18 C13 C2 119.78(11) . . ?
C14 C13 C2 120.68(12) . . ?
C15 C14 C13 119.25(13) . . ?
C15 C14 C22 120.10(12) . . ?
C13 C14 C22 120.61(12) . . ?
C16 C15 C14 122.29(13) . . ?
C16 C15 H15 118.9 . . ?
C14 C15 H15 118.9 . . ?
C15 C16 C17 117.66(12) . . ?
C15 C16 C23 122.21(14) . . ?
C17 C16 C23 120.14(14) . . ?
C16 C17 C18 122.32(14) . . ?
C16 C17 H17 118.8 . . ?
C18 C17 H17 118.8 . . ?
C17 C18 C13 119.05(13) . . ?
C17 C18 C24 119.30(14) . . ?
C13 C18 C24 121.65(13) . . ?
C8 C19 H19A 109.5 . . ?
C8 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C8 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C10 C20 H20A 109.5 . . ?
C10 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C10 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C12 C21 H21A 109.5 . . ?
C12 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C12 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C16 C23 H23A 109.5 . . ?
C16 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C16 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N2 C25 N3 125.58(13) . . ?
N2 C25 C26 108.64(11) . . ?
N3 C25 C26 125.77(13) . . ?
C25 C26 C27 115.59(12) . . ?
C25 C26 As 90.74(8) . . ?
C27 C26 As 120.82(9) . . ?
C25 C26 H2 111.3(10) . . ?
C27 C26 H2 111.8(10) . . ?
As C26 H2 104.6(10) . . ?
C26 C27 C28 111.42(12) . . ?
C26 C27 H27A 109.3 . . ?
C28 C27 H27A 109.3 . . ?
C26 C27 H27B 109.3 . . ?
C28 C27 H27B 109.3 . . ?
H27A C27 H27B 108.0 . . ?
C29 C28 C27 115.31(13) . . ?
C29 C28 H28A 108.4 . . ?
C27 C28 H28A 108.4 . . ?
C29 C28 H28B 108.4 . . ?
C27 C28 H28B 108.4 . . ?
H28A C28 H28B 107.5 . . ?
C30 C29 C28 116.31(14) . . ?
C30 C29 H29A 108.2 . . ?
C28 C29 H29A 108.2 . . ?
C30 C29 H29B 108.2 . . ?
C28 C29 H29B 108.2 . . ?
H29A C29 H29B 107.4 . . ?
N3 C30 C29 114.43(12) . . ?
N3 C30 H30A 108.7 . . ?
C29 C30 H30A 108.7 . . ?
N3 C30 H30B 108.7 . . ?
C29 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
N3 C31 C32 110.37(13) . . ?
N3 C31 H31A 109.6 . . ?
C32 C31 H31A 109.6 . . ?
N3 C31 H31B 109.6 . . ?
C32 C31 H31B 109.6 . . ?
H31A C31 H31B 108.1 . . ?
C33 C32 C31 110.27(14) . . ?
C33 C32 H32A 109.6 . . ?
C31 C32 H32A 109.6 . . ?
C33 C32 H32B 109.6 . . ?
C31 C32 H32B 109.6 . . ?
H32A C32 H32B 108.1 . . ?
N2 C33 C32 109.49(13) . . ?
N2 C33 H33A 109.8 . . ?
C32 C33 H33A 109.8 . . ?
N2 C33 H33B 109.8 . . ?
C32 C33 H33B 109.8 . . ?
H33A C33 H33B 108.2 . . ?

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
C26 As N1 C1 -151.84(10) . . . . ?
N2 As N1 C1 140.36(10) . . . . ?
Cl As N1 C1 -62.66(10) . . . . ?
N1 As N2 C25 103.27(9) . . . . ?
C26 As N2 C25 6.05(8) . . . . ?
Cl As N2 C25 -5.70(13) . . . . ?
N1 As N2 C33 -99.79(17) . . . . ?
C26 As N2 C33 163.00(17) . . . . ?
Cl As N2 C33 151.24(13) . . . . ?
As N1 C1 C2 -46.87(16) . . . . ?
As N1 C1 C6 137.98(10) . . . . ?
N1 C1 C2 C3 177.65(12) . . . . ?
C6 C1 C2 C3 -7.23(19) . . . . ?
N1 C1 C2 C13 -7.01(19) . . . . ?
C6 C1 C2 C13 168.12(12) . . . . ?
C1 C2 C3 C4 3.1(2) . . . . ?
C13 C2 C3 C4 -172.46(13) . . . . ?
C2 C3 C4 C5 2.0(2) . . . . ?
C3 C4 C5 C6 -2.8(2) . . . . ?
C4 C5 C6 C1 -1.4(2) . . . . ?
C4 C5 C6 C7 173.62(13) . . . . ?
N1 C1 C6 C5 -178.34(12) . . . . ?
C2 C1 C6 C5 6.44(19) . . . . ?
N1 C1 C6 C7 6.62(18) . . . . ?
C2 C1 C6 C7 -168.59(12) . . . . ?
C5 C6 C7 C12 -95.07(16) . . . . ?
C1 C6 C7 C12 79.91(16) . . . . ?
C5 C6 C7 C8 85.40(17) . . . . ?
C1 C6 C7 C8 -99.63(15) . . . . ?
C12 C7 C8 C9 -3.33(18) . . . . ?
C6 C7 C8 C9 176.20(11) . . . . ?
C12 C7 C8 C19 174.99(13) . . . . ?
C6 C7 C8 C19 -5.47(18) . . . . ?
C7 C8 C9 C10 0.5(2) . . . . ?
C19 C8 C9 C10 -177.87(13) . . . . ?
C8 C9 C10 C11 1.6(2) . . . . ?
C8 C9 C10 C20 179.47(15) . . . . ?
C9 C10 C11 C12 -0.8(2) . . . . ?
C20 C10 C11 C12 -178.71(15) . . . . ?
C10 C11 C12 C7 -2.0(2) . . . . ?
C10 C11 C12 C21 175.68(15) . . . . ?
C8 C7 C12 C11 4.09(19) . . . . ?
C6 C7 C12 C11 -175.46(12) . . . . ?
C8 C7 C12 C21 -173.59(13) . . . . ?
C6 C7 C12 C21 6.87(19) . . . . ?
C3 C2 C13 C18 107.40(16) . . . . ?
C1 C2 C13 C18 -67.93(17) . . . . ?
C3 C2 C13 C14 -68.72(17) . . . . ?
C1 C2 C13 C14 115.95(15) . . . . ?
C18 C13 C14 C15 0.27(19) . . . . ?
C2 C13 C14 C15 176.40(12) . . . . ?
C18 C13 C14 C22 177.96(12) . . . . ?
C2 C13 C14 C22 -5.92(18) . . . . ?
C13 C14 C15 C16 -0.1(2) . . . . ?
C22 C14 C15 C16 -177.76(13) . . . . ?
C14 C15 C16 C17 0.1(2) . . . . ?
C14 C15 C16 C23 179.97(13) . . . . ?
C15 C16 C17 C18 -0.4(2) . . . . ?
C23 C16 C17 C18 179.72(14) . . . . ?
C16 C17 C18 C13 0.7(2) . . . . ?
C16 C17 C18 C24 179.97(14) . . . . ?
C14 C13 C18 C17 -0.56(19) . . . . ?
C2 C13 C18 C17 -176.72(12) . . . . ?
C14 C13 C18 C24 -179.86(13) . . . . ?
C2 C13 C18 C24 4.0(2) . . . . ?
C33 N2 C25 N3 7.5(2) . . . . ?
As N2 C25 N3 171.64(12) . . . . ?
C33 N2 C25 C26 -172.14(12) . . . . ?
As N2 C25 C26 -7.97(10) . . . . ?
C30 N3 C25 N2 -179.04(13) . . . . ?
C31 N3 C25 N2 -5.4(2) . . . . ?
C30 N3 C25 C26 0.5(2) . . . . ?
C31 N3 C25 C26 174.11(14) . . . . ?
N2 C25 C26 C27 -116.75(13) . . . . ?
N3 C25 C26 C27 63.64(17) . . . . ?
N2 C25 C26 As 8.30(10) . . . . ?
N3 C25 C26 As -171.31(12) . . . . ?
N1 As C26 C25 -96.37(8) . . . . ?
N2 As C26 C25 -5.33(7) . . . . ?
Cl As C26 C25 169.85(7) . . . . ?
N1 As C26 C27 24.34(12) . . . . ?
N2 As C26 C27 115.38(12) . . . . ?
Cl As C26 C27 -69.44(11) . . . . ?
C25 C26 C27 C28 -76.31(16) . . . . ?
As C26 C27 C28 176.08(10) . . . . ?
C26 C27 C28 C29 61.87(18) . . . . ?
C27 C28 C29 C30 -63.79(19) . . . . ?
C25 N3 C30 C29 -61.39(18) . . . . ?
C31 N3 C30 C29 125.16(16) . . . . ?
C28 C29 C30 N3 77.77(18) . . . . ?
C25 N3 C31 C32 -26.0(2) . . . . ?
C30 N3 C31 C32 147.62(15) . . . . ?
N3 C31 C32 C33 53.9(2) . . . . ?
C25 N2 C33 C32 22.28(19) . . . . ?
As N2 C33 C32 -130.54(15) . . . . ?
C31 C32 C33 N2 -51.6(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        35.00
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.072

#===================== End of CIF submission =================================