data_2100431
_journal_coeditor_code         DE5025
_journal_date_accepted         2006-01-08
_journal_date_recd_electronic  2005-11-02
_journal_issue                 2
_journal_name_full             'Acta Crystallographica, Section B'
_journal_page_first            321
_journal_page_last             329
_journal_paper_category        FA
_journal_volume                62
_journal_year                  2006
_chemical_formula_moiety       ?
_chemical_formula_sum          'C4 H10 Cl5 N4 P3'
_chemical_formula_weight       384.32
_chemical_melting_point        46\%C
_chemical_name_common          ?
_chemical_name_systematic
;
 1-tert-butylamino-1,3,3,5,5-pentachlorocyclotriphosphazatriene
;
_symmetry_cell_setting         Monoclinic
_symmetry_space_group_name_H-M P2(1)/c
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary   direct
_atom_sites_solution_secondary difmap
_audit_creation_method         SHELXL-97
_cell_angle_alpha              90.00
_cell_angle_beta               104.132(7)
_cell_angle_gamma              90.00
_cell_formula_units_Z          8
_cell_length_a                 13.8045(14)
_cell_length_b                 10.7964(16)
_cell_length_c                 20.7719(12)
_cell_measurement_reflns_used  6816
_cell_measurement_temperature  120(2)
_cell_measurement_theta_max    27.48
_cell_measurement_theta_min    2.91
_cell_volume                   3002.1(6)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_data_collection     'COLLECT (Hooft, 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)'
_computing_molecular_graphics  ?
_computing_publication_material ?
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution  ?
_diffrn_ambient_temperature    120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method     '\F & \w scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source       'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type         MoK\a
_diffrn_radiation_wavelength   0.71073
_diffrn_reflns_av_R_equivalents 0.0437
_diffrn_reflns_av_sigmaI/netI  0.0371
_diffrn_reflns_limit_h_max     17
_diffrn_reflns_limit_h_min     -17
_diffrn_reflns_limit_k_max     14
_diffrn_reflns_limit_k_min     -14
_diffrn_reflns_limit_l_max     26
_diffrn_reflns_limit_l_min     -26
_diffrn_reflns_number          40456
_diffrn_reflns_theta_full      27.50
_diffrn_reflns_theta_max       27.50
_diffrn_reflns_theta_min       3.04
_diffrn_standards_decay_%      ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_number       ?
_exptl_absorpt_coefficient_mu  1.266
_exptl_absorpt_correction_T_max 0.9751
_exptl_absorpt_correction_T_min 0.8042
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SORTAV (Blessing, 1997)'
_exptl_crystal_colour          colourless
_exptl_crystal_density_diffrn  1.701
_exptl_crystal_density_meas    ?
_exptl_crystal_density_method  'not measured'
_exptl_crystal_description     'cut plate'
_exptl_crystal_F_000           1536
_exptl_crystal_size_max        0.18
_exptl_crystal_size_mid        0.10
_exptl_crystal_size_min        0.02
_refine_diff_density_max       0.486
_refine_diff_density_min       -0.498
_refine_ls_extinction_coef     0.0021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method   SHELXL
_refine_ls_goodness_of_fit_ref 1.072
_refine_ls_hydrogen_treatment  difmap
_refine_ls_matrix_type         full
_refine_ls_number_parameters   370
_refine_ls_number_reflns       6867
_refine_ls_number_restraints   0
_refine_ls_restrained_S_all    1.072
_refine_ls_R_factor_all        0.0492
_refine_ls_R_factor_gt         0.0339
_refine_ls_shift/su_max        0.001
_refine_ls_shift/su_mean       0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+1.5716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme    calc
_refine_ls_wR_factor_gt        0.0787
_refine_ls_wR_factor_ref       0.0862
_reflns_number_gt              5549
_reflns_number_total           6867
_reflns_threshold_expression   >2sigma(I)
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C1 0.17129(17) 1.3566(2) 0.02067(11) 0.0200(5) Uani d . 1 . .
C C2 0.06088(19) 1.3307(3) -0.01014(13) 0.0267(5) Uani d . 1 . .
C C3 0.1898(2) 1.4958(2) 0.02625(14) 0.0281(5) Uani d . 1 . .
C C4 0.2045(2) 1.2962(2) 0.08855(12) 0.0258(5) Uani d . 1 . .
N N1 0.19717(16) 0.94770(19) -0.13223(10) 0.0262(5) Uani d . 1 . .
N N2 0.19499(15) 1.06715(17) -0.01843(9) 0.0221(4) Uani d . 1 . .
N N3 0.29851(14) 1.16389(18) -0.10223(9) 0.0203(4) Uani d . 1 . .
N N4 0.23111(15) 1.30907(17) -0.02485(10) 0.0190(4) Uani d . 1 . .
P P1 0.27037(4) 1.04750(5) -0.14864(3) 0.01853(13) Uani d . 1 . .
P P2 0.16093(4) 0.95511(5) -0.06614(3) 0.01894(13) Uani d . 1 . .
P P3 0.26885(4) 1.17078(5) -0.03256(3) 0.01697(13) Uani d . 1 . .
Cl Cl1 0.21669(5) 1.10893(6) -0.24080(3) 0.03175(15) Uani d . 1 . .
Cl Cl2 0.39452(5) 0.96200(6) -0.15753(3) 0.02996(15) Uani d . 1 . .
Cl Cl3 0.19861(5) 0.79780(5) -0.01638(3) 0.03274(15) Uani d . 1 . .
Cl Cl4 0.01293(4) 0.94518(6) -0.08895(3) 0.03296(15) Uani d . 1 . .
Cl Cl5 0.39640(5) 1.14713(6) 0.03862(3) 0.03337(16) Uani d . 1 . .
H H2A 0.0431(18) 1.365(2) -0.0526(13) 0.022(6) Uiso d . 1 . .
H H2B 0.023(2) 1.364(3) 0.0177(14) 0.036(8) Uiso d . 1 . .
H H2C 0.046(2) 1.242(3) -0.0130(13) 0.036(8) Uiso d . 1 . .
H H3A 0.257(2) 1.505(3) 0.0443(13) 0.027(7) Uiso d . 1 . .
H H3B 0.172(2) 1.533(2) -0.0176(14) 0.027(7) Uiso d . 1 . .
H H3C 0.151(2) 1.530(3) 0.0543(14) 0.035(8) Uiso d . 1 . .
H H4A 0.165(2) 1.333(3) 0.1171(15) 0.043(8) Uiso d . 1 . .
H H4B 0.276(2) 1.310(3) 0.1100(13) 0.028(7) Uiso d . 1 . .
H H4C 0.191(2) 1.208(3) 0.0842(14) 0.038(8) Uiso d . 1 . .
H H4N 0.2283(18) 1.349(2) -0.0552(12) 0.016(6) Uiso d . 1 . .
C C5 0.49140(17) 1.1284(2) 0.33533(12) 0.0232(5) Uani d . 1 . .
C C6 0.4741(2) 1.1961(3) 0.26974(15) 0.0363(7) Uani d . 1 . .
C C7 0.5492(2) 1.2093(3) 0.39132(16) 0.0383(7) Uani d . 1 . .
C C8 0.5476(2) 1.0082(3) 0.3331(2) 0.0404(7) Uani d . 1 . .
N N5 0.12289(14) 0.9223(2) 0.23559(9) 0.0255(4) Uani d . 1 . .
N N6 0.21928(13) 1.02251(18) 0.35386(9) 0.0199(4) Uani d . 1 . .
N N7 0.32415(14) 0.9041(2) 0.27736(10) 0.0295(5) Uani d . 1 . .
N N8 0.39181(15) 1.1045(2) 0.34894(11) 0.0264(5) Uani d . 1 . .
P P4 0.22630(4) 0.88148(6) 0.22243(3) 0.01944(13) Uani d . 1 . .
P P5 0.11899(4) 0.98830(6) 0.30245(3) 0.01815(13) Uani d . 1 . .
P P6 0.32529(4) 0.98200(5) 0.34220(3) 0.01789(13) Uani d . 1 . .
Cl Cl6 0.21650(5) 0.70290(6) 0.19752(3) 0.02974(15) Uani d . 1 . .
Cl Cl7 0.23985(5) 0.95840(6) 0.13795(3) 0.03634(17) Uani d . 1 . .
Cl Cl8 0.03513(5) 1.13916(6) 0.28189(3) 0.03327(16) Uani d . 1 . .
Cl Cl9 0.03580(4) 0.88348(6) 0.34766(3) 0.02836(14) Uani d . 1 . .
Cl Cl10 0.38806(5) 0.86825(7) 0.41762(3) 0.03675(17) Uani d . 1 . .
H H6A 0.435(2) 1.148(3) 0.2370(15) 0.040(9) Uiso d . 1 . .
H H6B 0.537(2) 1.217(3) 0.2576(14) 0.044(8) Uiso d . 1 . .
H H6C 0.438(3) 1.276(3) 0.2701(17) 0.063(11) Uiso d . 1 . .
H H7A 0.615(2) 1.231(3) 0.3834(15) 0.050(9) Uiso d . 1 . .
H H7B 0.515(2) 1.288(3) 0.3950(15) 0.047(9) Uiso d . 1 . .
H H7C 0.562(3) 1.160(3) 0.4311(18) 0.058(10) Uiso d . 1 . .
H H8A 0.610(2) 1.026(3) 0.3230(14) 0.039(8) Uiso d . 1 . .
H H8B 0.515(2) 0.955(3) 0.2961(15) 0.042(9) Uiso d . 1 . .
H H8C 0.558(3) 0.963(4) 0.376(2) 0.071(12) Uiso d . 1 . .
H H8N 0.366(2) 1.166(3) 0.3608(13) 0.026(7) Uiso d . 1 . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
C1 0.0267(12) 0.0161(12) 0.0190(11) 0.0017(9) 0.0092(10) -0.0025(9)
C2 0.0273(13) 0.0306(15) 0.0251(13) 0.0023(11) 0.0121(11) 0.0016(11)
C3 0.0371(16) 0.0185(13) 0.0300(14) 0.0025(11) 0.0104(13) -0.0027(10)
C4 0.0351(15) 0.0252(14) 0.0191(11) 0.0033(11) 0.0110(11) 0.0014(10)
N1 0.0335(12) 0.0238(11) 0.0245(10) -0.0090(9) 0.0133(9) -0.0085(8)
N2 0.0315(11) 0.0152(10) 0.0231(10) -0.0039(8) 0.0135(9) -0.0009(8)
N3 0.0232(10) 0.0181(10) 0.0228(10) -0.0026(8) 0.0117(8) -0.0018(8)
N4 0.0272(11) 0.0132(10) 0.0189(10) 0.0014(8) 0.0097(9) 0.0029(8)
P1 0.0213(3) 0.0177(3) 0.0178(3) 0.0012(2) 0.0071(2) -0.0008(2)
P2 0.0222(3) 0.0148(3) 0.0204(3) -0.0024(2) 0.0064(2) 0.0002(2)
P3 0.0197(3) 0.0141(3) 0.0179(3) -0.0009(2) 0.0061(2) -0.0003(2)
Cl1 0.0399(4) 0.0327(4) 0.0203(3) 0.0059(3) 0.0029(3) 0.0040(2)
Cl2 0.0280(3) 0.0291(3) 0.0342(3) 0.0092(3) 0.0104(3) -0.0037(2)
Cl3 0.0450(4) 0.0155(3) 0.0345(3) 0.0012(3) 0.0035(3) 0.0038(2)
Cl4 0.0221(3) 0.0410(4) 0.0352(3) -0.0039(3) 0.0059(3) 0.0008(3)
Cl5 0.0248(3) 0.0396(4) 0.0313(3) 0.0065(3) -0.0016(3) 0.0024(3)
C5 0.0164(11) 0.0228(13) 0.0327(13) -0.0002(9) 0.0108(10) -0.0009(10)
C6 0.0265(14) 0.0481(19) 0.0379(16) 0.0022(14) 0.0150(13) 0.0100(14)
C7 0.0253(14) 0.0468(19) 0.0432(17) -0.0061(13) 0.0092(13) -0.0141(15)
C8 0.0273(15) 0.0286(16) 0.073(2) 0.0020(12) 0.0282(16) -0.0028(16)
N5 0.0199(10) 0.0361(12) 0.0189(9) 0.0058(9) 0.0019(8) -0.0050(9)
N6 0.0175(9) 0.0237(11) 0.0199(9) -0.0012(8) 0.0073(8) -0.0047(8)
N7 0.0164(10) 0.0430(13) 0.0296(11) 0.0030(9) 0.0064(9) -0.0163(10)
N8 0.0198(10) 0.0185(11) 0.0462(13) -0.0002(8) 0.0184(10) -0.0029(9)
P4 0.0195(3) 0.0222(3) 0.0176(3) 0.0022(2) 0.0064(2) -0.0023(2)
P5 0.0166(3) 0.0213(3) 0.0179(3) 0.0020(2) 0.0068(2) -0.0001(2)
P6 0.0163(3) 0.0197(3) 0.0184(3) 0.0001(2) 0.0058(2) -0.0017(2)
Cl6 0.0296(3) 0.0221(3) 0.0383(3) -0.0009(2) 0.0096(3) -0.0046(2)
Cl7 0.0490(4) 0.0354(4) 0.0314(3) 0.0103(3) 0.0228(3) 0.0111(3)
Cl8 0.0320(3) 0.0288(3) 0.0396(3) 0.0128(3) 0.0099(3) 0.0048(3)
Cl9 0.0254(3) 0.0350(4) 0.0254(3) -0.0095(3) 0.0076(2) 0.0017(2)
Cl10 0.0366(4) 0.0386(4) 0.0366(3) 0.0096(3) 0.0119(3) 0.0178(3)
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N4 C1 C4 . . 110.64(19) ?
N4 C1 C3 . . 106.22(19) ?
C4 C1 C3 . . 110.2(2) ?
N4 C1 C2 . . 108.78(18) ?
C4 C1 C2 . . 110.8(2) ?
C3 C1 C2 . . 110.1(2) ?
C1 C2 H2A . . 109.3(15) ?
C1 C2 H2B . . 108.9(17) ?
H2A C2 H2B . . 112(2) ?
C1 C2 H2C . . 112.4(17) ?
H2A C2 H2C . . 109(2) ?
H2B C2 H2C . . 105(2) ?
C1 C3 H3A . . 105.9(17) ?
C1 C3 H3B . . 109.8(16) ?
H3A C3 H3B . . 110(2) ?
C1 C3 H3C . . 108.4(17) ?
H3A C3 H3C . . 111(2) ?
H3B C3 H3C . . 111(2) ?
C1 C4 H4A . . 107.4(17) ?
C1 C4 H4B . . 113.3(15) ?
H4A C4 H4B . . 108(2) ?
C1 C4 H4C . . 109.1(17) ?
H4A C4 H4C . . 109(2) ?
H4B C4 H4C . . 110(2) ?
P1 N1 P2 . . 120.85(13) ?
P2 N2 P3 . . 122.38(12) ?
P1 N3 P3 . . 120.80(12) ?
C1 N4 P3 . . 128.93(16) ?
C1 N4 H4N . . 113.9(19) ?
P3 N4 H4N . . 113.8(19) ?
N1 P1 N3 . . 119.38(10) ?
N1 P1 Cl1 . . 109.22(8) ?
N3 P1 Cl1 . . 107.54(8) ?
N1 P1 Cl2 . . 108.39(9) ?
N3 P1 Cl2 . . 109.70(8) ?
Cl1 P1 Cl2 . . 101.05(4) ?
N2 P2 N1 . . 118.84(10) ?
N2 P2 Cl4 . . 109.04(8) ?
N1 P2 Cl4 . . 108.49(9) ?
N2 P2 Cl3 . . 109.35(8) ?
N1 P2 Cl3 . . 108.14(9) ?
Cl4 P2 Cl3 . . 101.60(4) ?
N2 P3 N3 . . 116.88(10) ?
N2 P3 N4 . . 113.50(10) ?
N3 P3 N4 . . 107.17(10) ?
N2 P3 Cl5 . . 105.06(8) ?
N3 P3 Cl5 . . 106.65(8) ?
N4 P3 Cl5 . . 106.93(8) ?
N8 C5 C6 . . 107.7(2) ?
N8 C5 C7 . . 106.9(2) ?
C6 C5 C7 . . 110.5(2) ?
N8 C5 C8 . . 111.1(2) ?
C6 C5 C8 . . 110.8(2) ?
C7 C5 C8 . . 109.8(2) ?
C5 C6 H6A . . 109.2(19) ?
C5 C6 H6B . . 112.5(18) ?
H6A C6 H6B . . 110(2) ?
C5 C6 H6C . . 112(2) ?
H6A C6 H6C . . 107(3) ?
H6B C6 H6C . . 106(3) ?
C5 C7 H7A . . 110.1(19) ?
C5 C7 H7B . . 112.7(19) ?
H7A C7 H7B . . 106(3) ?
C5 C7 H7C . . 107(2) ?
H7A C7 H7C . . 107(3) ?
H7B C7 H7C . . 114(3) ?
C5 C8 H8A . . 109.3(18) ?
C5 C8 H8B . . 112.6(18) ?
H8A C8 H8B . . 102(2) ?
C5 C8 H8C . . 111(2) ?
H8A C8 H8C . . 110(3) ?
H8B C8 H8C . . 111(3) ?
P5 N5 P4 . . 120.40(12) ?
P5 N6 P6 . . 121.25(11) ?
P4 N7 P6 . . 122.14(12) ?
C5 N8 P6 . . 131.54(17) ?
C5 N8 H8N . . 114.4(19) ?
P6 N8 H8N . . 114.0(19) ?
N7 P4 N5 . . 119.15(10) ?
N7 P4 Cl7 . . 109.17(9) ?
N5 P4 Cl7 . . 108.62(8) ?
N7 P4 Cl6 . . 109.47(9) ?
N5 P4 Cl6 . . 107.94(9) ?
Cl7 P4 Cl6 . . 100.94(4) ?
N6 P5 N5 . . 119.46(10) ?
N6 P5 Cl8 . . 108.91(8) ?
N5 P5 Cl8 . . 109.00(8) ?
N6 P5 Cl9 . . 108.97(8) ?
N5 P5 Cl9 . . 107.78(9) ?
Cl8 P5 Cl9 . . 101.17(4) ?
N7 P6 N8 . . 113.58(12) ?
N7 P6 N6 . . 116.98(10) ?
N8 P6 N6 . . 106.72(11) ?
N7 P6 Cl10 . . 104.53(9) ?
N8 P6 Cl10 . . 107.95(9) ?
N6 P6 Cl10 . . 106.54(7) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 N4 . 1.490(3) ?
C1 C4 . 1.519(3) ?
C1 C3 . 1.524(3) ?
C1 C2 . 1.528(3) ?
C2 H2A . 0.93(3) ?
C2 H2B . 0.94(3) ?
C2 H2C . 0.98(3) ?
C3 H3A . 0.91(3) ?
C3 H3B . 0.97(3) ?
C3 H3C . 0.95(3) ?
C4 H4A . 0.99(3) ?
C4 H4B . 0.99(3) ?
C4 H4C . 0.97(3) ?
N1 P1 . 1.570(2) ?
N1 P2 . 1.5737(19) ?
N2 P2 . 1.562(2) ?
N2 P3 . 1.5886(19) ?
N3 P1 . 1.5736(19) ?
N3 P3 . 1.5991(18) ?
N4 P3 . 1.6021(19) ?
N4 H4N . 0.76(3) ?
P1 Cl1 . 1.9902(8) ?
P1 Cl2 . 1.9946(8) ?
P2 Cl4 . 1.9844(9) ?
P2 Cl3 . 1.9901(9) ?
P3 Cl5 . 2.0200(9) ?
C5 N8 . 1.492(3) ?
C5 C6 . 1.513(4) ?
C5 C7 . 1.516(4) ?
C5 C8 . 1.518(4) ?
C6 H6A . 0.92(3) ?
C6 H6B . 0.99(3) ?
C6 H6C . 1.00(4) ?
C7 H7A . 0.99(3) ?
C7 H7B . 0.98(3) ?
C7 H7C . 0.96(4) ?
C8 H8A . 0.96(3) ?
C8 H8B . 0.98(3) ?
C8 H8C . 1.00(4) ?
N5 P5 . 1.5733(19) ?
N5 P4 . 1.581(2) ?
N6 P5 . 1.5722(19) ?
N6 P6 . 1.6014(18) ?
N7 P4 . 1.560(2) ?
N7 P6 . 1.585(2) ?
N8 P6 . 1.597(2) ?
N8 H8N . 0.82(3) ?
P4 Cl7 . 1.9909(8) ?
P4 Cl6 . 1.9922(9) ?
P5 Cl8 . 1.9834(9) ?
P5 Cl9 . 2.0020(8) ?
P6 Cl10 . 2.0125(9) ?