# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Harry R Allcock' _publ_contact_author_email HRA@CHEM.PSU.EDU _publ_section_title ; Synthesis and Optical Properties of Sulfur-Containing Monomers and Cyclomatrix Polyphosphazenes ; loop_ _publ_author_name 'Harry R Allcock' 'Toshiki Fushimi' #===END data_tuf7s _database_code_depnum_ccdc_archive 'CCDC 760670' #TrackingRef 'SulfurContainingCyclomatrixPhosphazenes2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic cis-N3P3Cl2(NHCH2CH2S)2 _chemical_name_common cis-N3P3Cl2(NHCH2CH2S)2 _chemical_melting_point ? _chemical_formula_moiety '2(C4 H10 Cl2 N5 P3 S2)' _chemical_formula_sum 'C8 H20 Cl4 N10 P6 S4' _chemical_formula_weight 712.20 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1908(6) _cell_length_b 13.5389(9) _cell_length_c 21.8660(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.6750(10) _cell_angle_gamma 90.00 _cell_volume 2711.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 9500 _cell_measurement_theta_min 2.341 _cell_measurement_theta_max 28.292 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.121 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8237 _exptl_absorpt_correction_T_max 0.8588 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 17485 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.33 _reflns_number_total 6672 _reflns_number_gt 5536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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^ > 2sigma(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^)+(0.0551P)^2^+1.1611P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6672 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.9647(3) 0.3517(2) 0.15137(14) 0.0459(6) Uani 1 1 d . . . H1A H 1.0693 0.3416 0.1578 0.055 Uiso 1 1 calc R . . H1B H 0.9165 0.3034 0.1755 0.055 Uiso 1 1 calc R . . C2 C 0.9144(3) 0.3399(2) 0.08347(13) 0.0423(6) Uani 1 1 d . . . H2A H 0.9819 0.3736 0.0587 0.051 Uiso 1 1 calc R . . H2B H 0.9132 0.2705 0.0725 0.051 Uiso 1 1 calc R . . C3 C 0.2480(3) 0.6740(3) 0.15172(16) 0.0632(9) Uani 1 1 d . . . H3A H 0.1843 0.6631 0.1844 0.076 Uiso 1 1 calc R . . H3B H 0.2244 0.7376 0.1331 0.076 Uiso 1 1 calc R . . C4 C 0.2271(3) 0.5948(3) 0.10531(16) 0.0628(9) Uani 1 1 d . . . H4A H 0.2214 0.5312 0.1254 0.075 Uiso 1 1 calc R . . H4B H 0.1368 0.6054 0.0800 0.075 Uiso 1 1 calc R . . C5 C 0.7379(4) 0.5327(2) 0.48538(14) 0.0576(8) Uani 1 1 d . . . H5A H 0.6408 0.5195 0.4978 0.069 Uiso 1 1 calc R . . H5B H 0.8003 0.4774 0.4980 0.069 Uiso 1 1 calc R . . C6 C 0.7965(3) 0.6254(2) 0.51499(13) 0.0468(6) Uani 1 1 d . . . H6A H 0.7191 0.6740 0.5159 0.056 Uiso 1 1 calc R . . H6B H 0.8340 0.6119 0.5569 0.056 Uiso 1 1 calc R . . C7 C 0.7969(4) 0.8441(2) 0.20814(13) 0.0528(7) Uani 1 1 d . . . H7A H 0.7715 0.8566 0.1649 0.063 Uiso 1 1 calc R . . H7B H 0.7176 0.8670 0.2312 0.063 Uiso 1 1 calc R . . C8 C 0.9359(4) 0.8961(2) 0.22912(14) 0.0593(8) Uani 1 1 d . . . H8A H 1.0073 0.8863 0.1994 0.071 Uiso 1 1 calc R . . H8B H 0.9179 0.9664 0.2324 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.70588(8) 0.67135(6) -0.05774(3) 0.05188(18) Uani 1 1 d . . . Cl2 Cl 0.88046(8) 0.78297(5) 0.04679(4) 0.05391(19) Uani 1 1 d . . . Cl3 Cl 1.36434(7) 0.60432(6) 0.37069(4) 0.0569(2) Uani 1 1 d . . . Cl4 Cl 1.16557(10) 0.45764(7) 0.29854(4) 0.0713(3) Uani 1 1 d . . . N1 N 0.6030(2) 0.51775(15) 0.11914(10) 0.0351(4) Uani 1 1 d . . . N2 N 0.5964(2) 0.69443(16) 0.06294(11) 0.0421(5) Uani 1 1 d . . . N3 N 0.8281(2) 0.57151(15) 0.05349(9) 0.0342(4) Uani 1 1 d . . . N4 N 0.7673(2) 0.38189(14) 0.07130(9) 0.0341(4) Uani 1 1 d . . . H4 H 0.6945 0.3523 0.0520 0.041 Uiso 1 1 calc R . . N5 N 0.3500(2) 0.5962(2) 0.06752(10) 0.0483(6) Uani 1 1 d . . . H5 H 0.3384 0.5872 0.0285 0.058 Uiso 1 1 calc R . . N6 N 0.8943(2) 0.72707(14) 0.36392(9) 0.0344(4) Uani 1 1 d . . . N7 N 1.0631(2) 0.57288(18) 0.39895(11) 0.0457(5) Uani 1 1 d . . . N8 N 1.1077(3) 0.67095(19) 0.29427(11) 0.0510(6) Uani 1 1 d . . . N9 N 0.9928(3) 0.85720(16) 0.28896(10) 0.0447(5) Uani 1 1 d . . . H9 H 1.0374 0.8942 0.3165 0.054 Uiso 1 1 calc R . . N10 N 0.9113(2) 0.66335(17) 0.48083(10) 0.0432(5) Uani 1 1 d . . . H10 H 0.9767 0.7015 0.4985 0.052 Uiso 1 1 calc R . . P1 P 0.51059(6) 0.61550(5) 0.10234(3) 0.03006(13) Uani 1 1 d . . . P2 P 0.74318(6) 0.66744(4) 0.03451(3) 0.03153(14) Uani 1 1 d . . . P3 P 0.76280(6) 0.49464(4) 0.10029(3) 0.02680(13) Uani 1 1 d . . . P4 P 0.91817(6) 0.63441(4) 0.40895(3) 0.02970(13) Uani 1 1 d . . . P5 P 1.15196(7) 0.58835(5) 0.34175(3) 0.03774(15) Uani 1 1 d . . . P6 P 0.96656(7) 0.73920(5) 0.30028(3) 0.03244(14) Uani 1 1 d . . . S1 S 0.91769(7) 0.47650(5) 0.17448(3) 0.03822(15) Uani 1 1 d . . . S2 S 0.43910(8) 0.67206(6) 0.18275(3) 0.04890(18) Uani 1 1 d . . . S3 S 0.82897(9) 0.71377(5) 0.22133(3) 0.05270(19) Uani 1 1 d . . . S4 S 0.73106(7) 0.54773(5) 0.40293(3) 0.04515(16) Uani 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 C1 0.0416(14) 0.0406(14) 0.0550(17) 0.0060(12) 0.0004(12) 0.0150(11) C2 0.0381(13) 0.0377(13) 0.0520(16) -0.0046(11) 0.0088(11) 0.0105(10) C3 0.0438(16) 0.089(2) 0.060(2) 0.0099(17) 0.0253(15) 0.0191(16) C4 0.0259(13) 0.100(3) 0.064(2) 0.0074(19) 0.0112(13) -0.0005(14) C5 0.0623(18) 0.063(2) 0.0469(17) 0.0130(14) 0.0025(14) -0.0248(15) C6 0.0546(16) 0.0519(16) 0.0352(14) 0.0015(11) 0.0105(12) -0.0038(13) C7 0.073(2) 0.0486(16) 0.0366(15) 0.0077(12) 0.0032(13) 0.0250(15) C8 0.095(3) 0.0437(16) 0.0401(16) 0.0135(12) 0.0127(16) -0.0006(16) Cl1 0.0481(4) 0.0718(5) 0.0359(3) 0.0136(3) 0.0044(3) 0.0152(3) Cl2 0.0551(4) 0.0389(4) 0.0701(5) 0.0009(3) 0.0197(4) -0.0085(3) Cl3 0.0313(3) 0.0731(5) 0.0655(5) -0.0049(4) -0.0007(3) 0.0048(3) Cl4 0.0781(6) 0.0622(5) 0.0684(5) -0.0237(4) -0.0247(4) 0.0264(4) N1 0.0282(9) 0.0359(11) 0.0423(12) 0.0110(8) 0.0104(8) 0.0036(8) N2 0.0353(10) 0.0415(11) 0.0519(13) 0.0180(10) 0.0188(10) 0.0150(9) N3 0.0266(9) 0.0363(10) 0.0412(11) 0.0121(9) 0.0109(8) 0.0066(8) N4 0.0295(9) 0.0328(10) 0.0398(11) -0.0052(8) 0.0012(8) -0.0020(8) N5 0.0288(10) 0.0802(17) 0.0356(12) 0.0017(11) 0.0014(9) 0.0025(10) N6 0.0376(10) 0.0329(10) 0.0334(11) 0.0022(8) 0.0076(8) 0.0075(8) N7 0.0375(11) 0.0522(13) 0.0480(13) 0.0187(10) 0.0063(10) 0.0158(10) N8 0.0502(13) 0.0657(16) 0.0396(13) 0.0133(11) 0.0175(10) 0.0265(12) N9 0.0607(14) 0.0367(11) 0.0375(12) 0.0018(9) 0.0083(10) -0.0082(10) N10 0.0483(12) 0.0503(13) 0.0310(11) -0.0053(9) 0.0034(9) -0.0213(10) P1 0.0241(3) 0.0373(3) 0.0295(3) 0.0052(2) 0.0065(2) 0.0050(2) P2 0.0280(3) 0.0328(3) 0.0349(3) 0.0101(2) 0.0096(2) 0.0056(2) P3 0.0233(2) 0.0278(3) 0.0295(3) 0.0042(2) 0.0034(2) 0.0017(2) P4 0.0283(3) 0.0314(3) 0.0291(3) 0.0008(2) -0.0001(2) -0.0005(2) P5 0.0313(3) 0.0457(4) 0.0357(3) 0.0007(3) -0.0006(2) 0.0120(3) P6 0.0358(3) 0.0333(3) 0.0284(3) 0.0016(2) 0.0040(2) 0.0059(2) S1 0.0377(3) 0.0407(3) 0.0349(3) 0.0017(2) -0.0055(2) 0.0037(2) S2 0.0509(4) 0.0608(4) 0.0364(4) -0.0054(3) 0.0120(3) 0.0094(3) S3 0.0715(5) 0.0426(4) 0.0408(4) -0.0022(3) -0.0154(3) 0.0078(3) S4 0.0404(3) 0.0465(4) 0.0472(4) -0.0055(3) -0.0046(3) -0.0135(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 1.527(4) . ? C1 S1 1.825(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N4 1.471(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.478(5) . ? C3 S2 1.831(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N5 1.453(3) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.492(4) . ? C5 S4 1.810(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N10 1.436(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.497(5) . ? C7 S3 1.808(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N9 1.467(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? Cl1 P2 2.0190(9) . ? Cl2 P2 2.0139(9) . ? Cl3 P5 2.0139(9) . ? Cl4 P5 2.0148(10) . ? N1 P3 1.5881(18) . ? N1 P1 1.599(2) . ? N2 P2 1.5734(19) . ? N2 P1 1.618(2) . ? N3 P2 1.5542(19) . ? N3 P3 1.6096(19) . ? N4 P3 1.655(2) . ? N4 H4 0.8600 . ? N5 P1 1.626(2) . ? N5 H5 0.8600 . ? N6 P6 1.599(2) . ? N6 P4 1.599(2) . ? N7 P5 1.562(2) . ? N7 P4 1.601(2) . ? N8 P5 1.557(2) . ? N8 P6 1.606(2) . ? N9 P6 1.638(2) . ? N9 H9 0.8600 . ? N10 P4 1.626(2) . ? N10 H10 0.8600 . ? P1 S2 2.0731(9) . ? P3 S1 2.0837(8) . ? P4 S4 2.0773(9) . ? P6 S3 2.0838(10) . ? 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 S1 107.83(17) . . ? C2 C1 H1A 110.1 . . ? S1 C1 H1A 110.1 . . ? C2 C1 H1B 110.1 . . ? S1 C1 H1B 110.1 . . ? H1A C1 H1B 108.5 . . ? N4 C2 C1 109.6(2) . . ? N4 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N4 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 S2 108.1(2) . . ? C4 C3 H3A 110.1 . . ? S2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? S2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? N5 C4 C3 108.5(3) . . ? N5 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? N5 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? C6 C5 S4 108.65(19) . . ? C6 C5 H5A 110.0 . . ? S4 C5 H5A 110.0 . . ? C6 C5 H5B 110.0 . . ? S4 C5 H5B 110.0 . . ? H5A C5 H5B 108.3 . . ? N10 C6 C5 109.3(2) . . ? N10 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N10 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C8 C7 S3 106.6(2) . . ? C8 C7 H7A 110.4 . . ? S3 C7 H7A 110.4 . . ? C8 C7 H7B 110.4 . . ? S3 C7 H7B 110.4 . . ? H7A C7 H7B 108.6 . . ? N9 C8 C7 109.8(2) . . ? N9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? N9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? P3 N1 P1 126.05(12) . . ? P2 N2 P1 121.87(13) . . ? P2 N3 P3 120.32(11) . . ? C2 N4 P3 109.76(16) . . ? C2 N4 H4 125.1 . . ? P3 N4 H4 125.1 . . ? C4 N5 P1 117.0(2) . . ? C4 N5 H5 121.5 . . ? P1 N5 H5 121.5 . . ? P6 N6 P4 124.79(12) . . ? P5 N7 P4 122.30(14) . . ? P5 N8 P6 121.83(14) . . ? C8 N9 P6 116.0(2) . . ? C8 N9 H9 122.0 . . ? P6 N9 H9 122.0 . . ? C6 N10 P4 120.30(18) . . ? C6 N10 H10 119.9 . . ? P4 N10 H10 119.9 . . ? N1 P1 N2 113.32(10) . . ? N1 P1 N5 114.80(13) . . ? N2 P1 N5 108.68(12) . . ? N1 P1 S2 108.06(8) . . ? N2 P1 S2 114.19(9) . . ? N5 P1 S2 96.80(9) . . ? N3 P2 N2 121.11(10) . . ? N3 P2 Cl2 108.53(8) . . ? N2 P2 Cl2 108.35(10) . . ? N3 P2 Cl1 109.23(9) . . ? N2 P2 Cl1 107.90(9) . . ? Cl2 P2 Cl1 99.57(4) . . ? N1 P3 N3 116.00(10) . . ? N1 P3 N4 109.48(11) . . ? N3 P3 N4 109.31(10) . . ? N1 P3 S1 114.11(8) . . ? N3 P3 S1 107.73(8) . . ? N4 P3 S1 98.79(8) . . ? N6 P4 N7 113.47(11) . . ? N6 P4 N10 113.08(11) . . ? N7 P4 N10 110.83(13) . . ? N6 P4 S4 109.44(8) . . ? N7 P4 S4 113.02(10) . . ? N10 P4 S4 95.75(8) . . ? N8 P5 N7 120.31(11) . . ? N8 P5 Cl3 109.05(11) . . ? N7 P5 Cl3 108.61(10) . . ? N8 P5 Cl4 109.93(10) . . ? N7 P5 Cl4 108.31(11) . . ? Cl3 P5 Cl4 98.39(4) . . ? N6 P6 N8 114.07(11) . . ? N6 P6 N9 107.97(11) . . ? N8 P6 N9 114.76(13) . . ? N6 P6 S3 115.91(9) . . ? N8 P6 S3 106.06(10) . . ? N9 P6 S3 97.06(9) . . ? C1 S1 P3 93.19(10) . . ? C3 S2 P1 92.96(11) . . ? C7 S3 P6 92.93(11) . . ? C5 S4 P4 92.24(10) . . ? 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 S1 C1 C2 N4 -44.0(3) . . . . ? S2 C3 C4 N5 -43.4(3) . . . . ? S4 C5 C6 N10 -38.9(3) . . . . ? S3 C7 C8 N9 -45.6(3) . . . . ? C1 C2 N4 P3 50.2(2) . . . . ? C3 C4 N5 P1 40.3(4) . . . . ? C7 C8 N9 P6 35.0(3) . . . . ? C5 C6 N10 P4 23.6(3) . . . . ? P3 N1 P1 N2 -0.5(2) . . . . ? P3 N1 P1 N5 125.19(17) . . . . ? P3 N1 P1 S2 -128.08(15) . . . . ? P2 N2 P1 N1 10.5(2) . . . . ? P2 N2 P1 N5 -118.44(18) . . . . ? P2 N2 P1 S2 134.77(15) . . . . ? C4 N5 P1 N1 96.5(3) . . . . ? C4 N5 P1 N2 -135.4(2) . . . . ? C4 N5 P1 S2 -17.0(3) . . . . ? P3 N3 P2 N2 3.2(2) . . . . ? P3 N3 P2 Cl2 129.36(13) . . . . ? P3 N3 P2 Cl1 -123.01(13) . . . . ? P1 N2 P2 N3 -12.2(2) . . . . ? P1 N2 P2 Cl2 -138.45(15) . . . . ? P1 N2 P2 Cl1 114.62(16) . . . . ? P1 N1 P3 N3 -7.6(2) . . . . ? P1 N1 P3 N4 -131.84(16) . . . . ? P1 N1 P3 S1 118.53(15) . . . . ? P2 N3 P3 N1 6.2(2) . . . . ? P2 N3 P3 N4 130.52(15) . . . . ? P2 N3 P3 S1 -123.10(13) . . . . ? C2 N4 P3 N1 -150.50(17) . . . . ? C2 N4 P3 N3 81.44(18) . . . . ? C2 N4 P3 S1 -30.95(17) . . . . ? P6 N6 P4 N7 21.2(2) . . . . ? P6 N6 P4 N10 148.56(15) . . . . ? P6 N6 P4 S4 -106.02(15) . . . . ? P5 N7 P4 N6 -12.7(2) . . . . ? P5 N7 P4 N10 -141.17(17) . . . . ? P5 N7 P4 S4 112.68(17) . . . . ? C6 N10 P4 N6 114.8(2) . . . . ? C6 N10 P4 N7 -116.5(2) . . . . ? C6 N10 P4 S4 0.8(2) . . . . ? P6 N8 P5 N7 -2.9(3) . . . . ? P6 N8 P5 Cl3 -129.30(17) . . . . ? P6 N8 P5 Cl4 123.87(17) . . . . ? P4 N7 P5 N8 4.5(3) . . . . ? P4 N7 P5 Cl3 131.10(16) . . . . ? P4 N7 P5 Cl4 -123.02(16) . . . . ? P4 N6 P6 N8 -19.9(2) . . . . ? P4 N6 P6 N9 -148.76(16) . . . . ? P4 N6 P6 S3 103.70(15) . . . . ? P5 N8 P6 N6 9.8(3) . . . . ? P5 N8 P6 N9 135.11(19) . . . . ? P5 N8 P6 S3 -119.00(18) . . . . ? C8 N9 P6 N6 -128.7(2) . . . . ? C8 N9 P6 N8 102.8(2) . . . . ? C8 N9 P6 S3 -8.5(2) . . . . ? C2 C1 S1 P3 19.67(18) . . . . ? N1 P3 S1 C1 121.49(12) . . . . ? N3 P3 S1 C1 -108.17(12) . . . . ? N4 P3 S1 C1 5.45(12) . . . . ? C4 C3 S2 P1 28.5(2) . . . . ? N1 P1 S2 C3 -125.88(14) . . . . ? N2 P1 S2 C3 107.04(15) . . . . ? N5 P1 S2 C3 -6.98(15) . . . . ? C8 C7 S3 P6 34.2(2) . . . . ? N6 P6 S3 C7 99.15(13) . . . . ? N8 P6 S3 C7 -133.15(14) . . . . ? N9 P6 S3 C7 -14.79(13) . . . . ? C6 C5 S4 P4 34.2(2) . . . . ? N6 P4 S4 C5 -136.21(14) . . . . ? N7 P4 S4 C5 96.29(15) . . . . ? N10 P4 S4 C5 -19.25(15) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.620 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.071 # Attachment 'SulfurContainingCyclomatrixPhosphazenes2.cif' data_tuf6s _database_code_depnum_ccdc_archive 'CCDC 760671' #TrackingRef 'SulfurContainingCyclomatrixPhosphazenes2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic N3P3Cl4(NHCH2CH2S) _chemical_name_common N3P3Cl4(NHCH2CH2S) _chemical_melting_point ? _chemical_formula_moiety 'C2 H5 Cl4 N4 P3 S' _chemical_formula_sum 'C2 H5 Cl4 N4 P3 S' _chemical_formula_weight 351.87 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.2552(13) _cell_length_b 6.0436(6) _cell_length_c 15.5469(14) _cell_angle_alpha 90.00 _cell_angle_beta 113.376(2) _cell_angle_gamma 90.00 _cell_volume 1229.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2711 _cell_measurement_theta_min 2.494 _cell_measurement_theta_max 26.436 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.901 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.490 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7650 _exptl_absorpt_correction_T_max 0.9029 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 10107 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.25 _reflns_number_total 3006 _reflns_number_gt 2339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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^ > 2sigma(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^)+(0.1058P)^2^+2.3344P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3006 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0842 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.2031 _refine_ls_wR_factor_gt 0.1899 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.5614(5) 0.7768(15) 0.1352(6) 0.085(2) Uani 1 1 d . . . H1A H 0.5729 0.8814 0.1857 0.102 Uiso 1 1 calc R . . H1B H 0.4897 0.7854 0.0936 0.102 Uiso 1 1 calc R . . C2 C 0.5819(7) 0.561(2) 0.1738(7) 0.124(4) Uani 1 1 d . . . H2A H 0.5184 0.4782 0.1483 0.149 Uiso 1 1 calc R . . H2B H 0.6002 0.5743 0.2407 0.149 Uiso 1 1 calc R . . Cl1 Cl 0.74749(13) 0.0991(2) -0.09189(11) 0.0702(5) Uani 1 1 d . . . Cl2 Cl 0.70303(13) 0.5552(3) -0.18260(11) 0.0742(5) Uani 1 1 d . . . Cl3 Cl 0.97693(12) 0.8783(2) 0.09335(11) 0.0658(4) Uani 1 1 d . . . Cl4 Cl 1.03077(10) 0.4223(2) 0.18352(9) 0.0575(4) Uani 1 1 d . . . N1 N 0.8723(3) 0.4829(9) -0.0032(3) 0.0536(11) Uani 1 1 d . . . N2 N 0.6816(3) 0.4604(12) -0.0078(4) 0.090(2) Uani 1 1 d . . . N3 N 0.8332(3) 0.6233(9) 0.1445(3) 0.0601(13) Uani 1 1 d . . . N4 N 0.6620(3) 0.4249(7) 0.1605(3) 0.0457(10) Uani 1 1 d . . . H4 H 0.6804 0.2938 0.1821 0.055 Uiso 1 1 calc R . . P1 P 0.91054(8) 0.5916(2) 0.09682(8) 0.0391(3) Uani 1 1 d . . . P2 P 0.75670(9) 0.4171(2) -0.05515(8) 0.0476(4) Uani 1 1 d . . . P3 P 0.71308(9) 0.5810(2) 0.09192(9) 0.0494(4) Uani 1 1 d . . . S1 S 0.63266(19) 0.8554(4) 0.07482(18) 0.0997(7) Uani 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 C1 0.060(4) 0.107(6) 0.097(5) -0.027(5) 0.041(4) 0.011(4) C2 0.081(5) 0.202(12) 0.118(7) 0.072(7) 0.070(5) 0.030(6) Cl1 0.0730(10) 0.0578(8) 0.0650(9) -0.0075(6) 0.0117(7) -0.0068(7) Cl2 0.0751(10) 0.0703(10) 0.0534(8) 0.0019(6) 0.0001(7) 0.0035(7) Cl3 0.0720(9) 0.0475(7) 0.0704(9) 0.0045(6) 0.0203(7) -0.0093(6) Cl4 0.0482(7) 0.0669(8) 0.0511(7) 0.0146(6) 0.0129(5) 0.0057(5) N1 0.0358(19) 0.088(3) 0.039(2) -0.024(2) 0.0162(16) -0.011(2) N2 0.034(2) 0.160(6) 0.076(4) -0.068(4) 0.022(2) -0.027(3) N3 0.037(2) 0.104(4) 0.040(2) -0.027(2) 0.0156(17) -0.008(2) N4 0.050(2) 0.056(2) 0.048(2) 0.0224(17) 0.0369(19) 0.0178(17) P1 0.0300(5) 0.0520(7) 0.0319(5) -0.0076(4) 0.0086(4) -0.0050(4) P2 0.0338(6) 0.0677(8) 0.0370(6) -0.0186(5) 0.0095(5) -0.0052(5) P3 0.0340(6) 0.0742(9) 0.0410(6) -0.0148(6) 0.0160(5) -0.0039(5) S1 0.1067(15) 0.0894(14) 0.1245(18) 0.0193(12) 0.0688(14) 0.0326(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 1.416(12) . ? C1 S1 1.702(8) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N4 1.487(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? Cl1 P2 1.994(2) . ? Cl2 P2 2.001(2) . ? Cl3 P1 1.9854(18) . ? Cl4 P1 1.9919(17) . ? N1 P2 1.571(4) . ? N1 P1 1.573(4) . ? N2 P2 1.543(5) . ? N2 P3 1.608(5) . ? N3 P1 1.566(4) . ? N3 P3 1.598(4) . ? N4 P3 1.781(4) . ? N4 H4 0.8600 . ? P3 S1 1.973(2) . ? 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 S1 115.0(5) . . ? C2 C1 H1A 108.5 . . ? S1 C1 H1A 108.5 . . ? C2 C1 H1B 108.5 . . ? S1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C1 C2 N4 119.4(6) . . ? C1 C2 H2A 107.5 . . ? N4 C2 H2A 107.5 . . ? C1 C2 H2B 107.5 . . ? N4 C2 H2B 107.5 . . ? H2A C2 H2B 107.0 . . ? P2 N1 P1 119.7(2) . . ? P2 N2 P3 123.8(3) . . ? P1 N3 P3 123.4(3) . . ? C2 N4 P3 108.0(4) . . ? C2 N4 H4 126.0 . . ? P3 N4 H4 126.0 . . ? N3 P1 N1 119.1(2) . . ? N3 P1 Cl3 109.8(2) . . ? N1 P1 Cl3 108.62(19) . . ? N3 P1 Cl4 108.7(2) . . ? N1 P1 Cl4 108.81(19) . . ? Cl3 P1 Cl4 100.08(8) . . ? N2 P2 N1 119.8(2) . . ? N2 P2 Cl1 108.7(3) . . ? N1 P2 Cl1 109.1(2) . . ? N2 P2 Cl2 109.6(3) . . ? N1 P2 Cl2 108.28(19) . . ? Cl1 P2 Cl2 99.36(8) . . ? N3 P3 N2 113.5(2) . . ? N3 P3 N4 112.8(2) . . ? N2 P3 N4 108.2(3) . . ? N3 P3 S1 112.4(2) . . ? N2 P3 S1 109.0(3) . . ? N4 P3 S1 99.92(14) . . ? C1 S1 P3 97.7(3) . . ? 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 S1 C1 C2 N4 0.8(12) . . . . ? C1 C2 N4 P3 -1.2(11) . . . . ? P3 N3 P1 N1 -8.4(6) . . . . ? P3 N3 P1 Cl3 117.7(4) . . . . ? P3 N3 P1 Cl4 -133.8(3) . . . . ? P2 N1 P1 N3 2.4(5) . . . . ? P2 N1 P1 Cl3 -124.2(3) . . . . ? P2 N1 P1 Cl4 127.7(3) . . . . ? P3 N2 P2 N1 2.7(8) . . . . ? P3 N2 P2 Cl1 129.1(5) . . . . ? P3 N2 P2 Cl2 -123.3(5) . . . . ? P1 N1 P2 N2 0.3(6) . . . . ? P1 N1 P2 Cl1 -125.9(3) . . . . ? P1 N1 P2 Cl2 126.9(3) . . . . ? P1 N3 P3 N2 10.7(6) . . . . ? P1 N3 P3 N4 134.3(4) . . . . ? P1 N3 P3 S1 -113.7(4) . . . . ? P2 N2 P3 N3 -7.8(7) . . . . ? P2 N2 P3 N4 -133.9(5) . . . . ? P2 N2 P3 S1 118.3(5) . . . . ? C2 N4 P3 N3 120.6(6) . . . . ? C2 N4 P3 N2 -113.0(6) . . . . ? C2 N4 P3 S1 1.0(6) . . . . ? C2 C1 S1 P3 0.0(8) . . . . ? N3 P3 S1 C1 -120.4(3) . . . . ? N2 P3 S1 C1 112.8(4) . . . . ? N4 P3 S1 C1 -0.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.158 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.137 #===END data_tuf3o _database_code_depnum_ccdc_archive 'CCDC 760672' #TrackingRef 'SulfurContainingCyclomatrixPhosphazenes2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-N3P3(NHCH2CH2S)3 _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 N6 P3 S3' _chemical_formula_sum 'C6 H15 N6 P3 S3' _chemical_formula_weight 360.31 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.316(2) _cell_length_b 16.802(4) _cell_length_c 15.148(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2880.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 7501 _cell_measurement_theta_min 2.170 _cell_measurement_theta_max 28.205 _exptl_crystal_description pyramid _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.859 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 25831 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.30 _reflns_number_total 3584 _reflns_number_gt 3309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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^ > 2sigma(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^)+(0.0384P)^2^+7.4432P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3584 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1287 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.268 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.002 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 0.9218(9) 0.4254(6) -0.1504(7) 0.0370(19) Uani 0.643(8) 1 d P A 1 H1A H 0.9657 0.4759 -0.1423 0.044 Uiso 0.643(8) 1 calc PR A 1 H1B H 0.8953 0.4226 -0.2126 0.044 Uiso 0.643(8) 1 calc PR A 1 C2 C 0.8159(17) 0.4245(13) -0.0904(14) 0.056(5) Uani 0.643(8) 1 d P A 1 H2A H 0.7654 0.4720 -0.0989 0.067 Uiso 0.643(8) 1 calc PR A 1 H2B H 0.7680 0.3757 -0.0982 0.067 Uiso 0.643(8) 1 calc PR A 1 C3 C 0.8473(5) 0.0617(3) 0.0723(4) 0.0355(16) Uani 0.761(15) 1 d P A 1 H3A H 0.7833 0.0839 0.0352 0.043 Uiso 0.761(15) 1 calc PR A 1 H3B H 0.8440 0.0029 0.0685 0.043 Uiso 0.761(15) 1 calc PR A 1 C4 C 0.8318(4) 0.0878(2) 0.1663(3) 0.0388(9) Uani 1 1 d . A 1 H4A H 0.7482 0.0825 0.1833 0.046 Uiso 1 1 calc R A 1 H4B H 0.8806 0.0550 0.2058 0.046 Uiso 1 1 calc R A 1 C5 C 1.3013(3) 0.3515(3) 0.2754(2) 0.0355(8) Uani 1 1 d . A 1 H5A H 1.3408 0.3892 0.3161 0.043 Uiso 1 1 calc R A 1 H5B H 1.3036 0.2977 0.3019 0.043 Uiso 1 1 calc R A 1 C6 C 1.3625(3) 0.3515(3) 0.1861(3) 0.0365(9) Uani 1 1 d . A 1 H6A H 1.3771 0.4068 0.1663 0.044 Uiso 1 1 calc R A 1 H6B H 1.4393 0.3236 0.1900 0.044 Uiso 1 1 calc R A 1 C3A C 0.9190(17) 0.0423(8) 0.1238(11) 0.039(5) Uani 0.249(14) 1 d P A 1 H3A1 H 0.8826 -0.0068 0.0999 0.047 Uiso 0.249(14) 1 calc PR A 1 H3A2 H 0.9798 0.0264 0.1673 0.047 Uiso 0.249(14) 1 calc PR A 1 N1 N 1.0818(3) 0.3756(2) 0.0618(2) 0.0342(7) Uani 1 1 d . A 1 N2 N 0.9060(3) 0.26810(19) 0.0335(2) 0.0334(7) Uani 1 1 d . A 1 N3 N 1.0842(2) 0.23392(17) 0.14601(18) 0.0251(6) Uani 1 1 d . A 1 N4 N 1.2854(3) 0.3111(2) 0.1245(2) 0.0347(7) Uani 1 1 d . A 1 H4C H 1.3152 0.2820 0.0816 0.042 Uiso 1 1 calc R A 1 N5 N 0.8764(7) 0.4258(4) -0.0045(5) 0.0341(16) Uani 0.643(8) 1 d P A 1 H5 H 0.8649 0.4626 0.0360 0.041 Uiso 0.643(8) 1 calc PR A 1 N6 N 0.8684(3) 0.17164(17) 0.17289(19) 0.0274(6) Uani 1 1 d . A 1 H6 H 0.8399 0.2028 0.2144 0.033 Uiso 1 1 calc R A 1 P1 P 0.96860(8) 0.34981(5) 0.00743(5) 0.0245(2) Uani 1 1 d . A 1 P2 P 0.96388(7) 0.20536(5) 0.10037(5) 0.02238(19) Uani 1 1 d . A 1 P3 P 1.14228(7) 0.32027(5) 0.13529(5) 0.0229(2) Uani 1 1 d . A 1 S1 S 1.01719(17) 0.34308(12) -0.12679(13) 0.0317(6) Uani 0.643(8) 1 d P A 1 S2 S 0.98927(9) 0.09721(6) 0.03408(6) 0.0347(2) Uani 1 1 d . A 1 S3 S 1.14919(7) 0.38209(5) 0.25563(6) 0.02593(19) Uani 1 1 d . A 1 S1A S 0.8434(4) 0.4365(2) 0.0265(3) 0.0338(11) Uani 0.376(8) 1 d P A 1 N5A N 0.9706(15) 0.3563(7) -0.1013(8) 0.046(3) Uani 0.376(8) 1 d P A 1 H5A1 H 1.0274 0.3296 -0.1276 0.056 Uiso 0.376(8) 1 calc PR A 1 C1A C 0.8106(18) 0.4421(19) -0.0868(16) 0.037(6) Uani 0.376(8) 1 d P A 1 H1A1 H 0.7297 0.4207 -0.0939 0.044 Uiso 0.376(8) 1 calc PR A 1 H1A2 H 0.8063 0.4994 -0.1016 0.044 Uiso 0.376(8) 1 calc PR A 1 C2A C 0.8893(17) 0.4014(14) -0.1617(14) 0.053(5) Uani 0.376(8) 1 d P A 1 H2A1 H 0.8425 0.3656 -0.2001 0.064 Uiso 0.376(8) 1 calc PR A 1 H2A2 H 0.9319 0.4410 -0.1981 0.064 Uiso 0.376(8) 1 calc PR A 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.030(5) 0.041(5) 0.041(5) 0.008(4) -0.008(4) -0.001(3) C2 0.056(8) 0.060(8) 0.050(7) -0.011(5) -0.015(5) 0.024(5) C3 0.039(3) 0.032(3) 0.035(3) -0.009(2) -0.007(2) -0.001(2) C4 0.047(2) 0.0341(19) 0.035(2) -0.0054(16) 0.0051(18) -0.0134(17) C5 0.0265(17) 0.052(2) 0.0277(18) -0.0058(16) -0.0068(15) 0.0004(16) C6 0.0185(16) 0.058(2) 0.0324(19) -0.0049(18) -0.0021(14) -0.0041(16) C3A 0.060(12) 0.021(7) 0.036(9) 0.002(6) 0.015(8) -0.007(7) N1 0.0297(16) 0.0445(18) 0.0283(15) 0.0124(14) -0.0061(13) -0.0139(14) N2 0.0287(15) 0.0408(17) 0.0308(16) 0.0090(13) -0.0139(13) -0.0089(13) N3 0.0218(13) 0.0343(15) 0.0192(13) -0.0002(11) -0.0035(11) 0.0009(12) N4 0.0181(13) 0.061(2) 0.0249(14) -0.0148(14) 0.0024(11) -0.0028(14) N5 0.037(4) 0.037(3) 0.028(3) -0.004(3) 0.007(3) 0.002(3) N6 0.0280(15) 0.0307(15) 0.0235(14) -0.0050(11) 0.0035(12) -0.0028(12) P1 0.0249(4) 0.0312(4) 0.0173(4) 0.0015(3) -0.0033(3) 0.0001(3) P2 0.0209(4) 0.0294(4) 0.0169(4) -0.0021(3) -0.0025(3) -0.0012(3) P3 0.0172(4) 0.0358(5) 0.0158(4) -0.0009(3) -0.0005(3) -0.0027(3) S1 0.0284(10) 0.0474(10) 0.0193(9) 0.0039(7) 0.0003(7) 0.0051(7) S2 0.0334(5) 0.0396(5) 0.0312(5) -0.0131(4) 0.0009(4) 0.0019(4) S3 0.0230(4) 0.0344(4) 0.0203(4) -0.0041(3) 0.0006(3) -0.0001(3) S1A 0.039(2) 0.0348(16) 0.028(2) 0.0051(13) -0.0063(14) 0.0067(13) N5A 0.051(7) 0.063(7) 0.026(5) -0.012(5) 0.007(5) 0.020(6) C1A 0.021(8) 0.072(15) 0.017(7) 0.013(8) -0.004(6) -0.019(9) C2A 0.039(10) 0.076(15) 0.045(8) 0.000(9) -0.026(7) 0.006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 1.50(2) . ? C1 S1 1.791(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N5 1.47(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.500(6) . ? C3 S2 1.810(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C3A 1.404(17) . ? C4 N6 1.472(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.520(5) . ? C5 S3 1.821(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N4 1.447(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C3A S2 1.826(15) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? N1 P1 1.584(3) . ? N1 P3 1.603(3) . ? N2 P1 1.595(3) . ? N2 P2 1.602(3) . ? N3 P2 1.601(3) . ? N3 P3 1.601(3) . ? N4 P3 1.635(3) . ? N4 H4C 0.8800 . ? N5 P1 1.658(7) . ? N5 H5 0.8800 . ? N6 P2 1.642(3) . ? N6 H6 0.8800 . ? P1 N5A 1.651(13) . ? P1 S1A 2.052(4) . ? P1 S1 2.109(2) . ? P2 S2 2.0959(13) . ? P3 S3 2.0995(12) . ? S1A C1A 1.76(2) . ? N5A C2A 1.50(2) . ? N5A H5A1 0.8800 . ? C1A C2A 1.60(4) . ? C1A H1A1 0.9900 . ? C1A H1A2 0.9900 . ? C2A H2A1 0.9900 . ? C2A H2A2 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 C2 C1 S1 110.6(10) . . ? C2 C1 H1A 109.5 . . ? S1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? S1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? N5 C2 C1 99.5(13) . . ? N5 C2 H2A 111.9 . . ? C1 C2 H2A 111.9 . . ? N5 C2 H2B 111.9 . . ? C1 C2 H2B 111.9 . . ? H2A C2 H2B 109.6 . . ? C4 C3 S2 108.1(3) . . ? C4 C3 H3A 110.1 . . ? S2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? S2 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C3A C4 N6 110.8(7) . . ? C3A C4 C3 47.4(8) . . ? N6 C4 C3 108.1(3) . . ? N6 C4 H4A 109.7 . . ? C3 C4 H4A 109.8 . . ? N6 C4 H4B 109.9 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? C6 C5 S3 106.5(3) . . ? C6 C5 H5A 110.4 . . ? S3 C5 H5A 110.4 . . ? C6 C5 H5B 110.4 . . ? S3 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? N4 C6 C5 107.4(3) . . ? N4 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? N4 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C4 C3A S2 111.9(9) . . ? C4 C3A H3A1 109.2 . . ? S2 C3A H3A1 109.2 . . ? C4 C3A H3A2 109.2 . . ? S2 C3A H3A2 109.2 . . ? H3A1 C3A H3A2 107.9 . . ? P1 N1 P3 123.2(2) . . ? P1 N2 P2 122.83(19) . . ? P2 N3 P3 125.25(18) . . ? C6 N4 P3 119.2(2) . . ? C6 N4 H4C 120.4 . . ? P3 N4 H4C 120.4 . . ? C2 N5 P1 112.2(9) . . ? C2 N5 H5 123.9 . . ? P1 N5 H5 123.9 . . ? C4 N6 P2 118.0(2) . . ? C4 N6 H6 121.0 . . ? P2 N6 H6 121.0 . . ? N1 P1 N2 117.76(16) . . ? N1 P1 N5A 119.4(6) . . ? N2 P1 N5A 108.1(5) . . ? N1 P1 N5 110.8(3) . . ? N2 P1 N5 114.2(3) . . ? N1 P1 S1A 106.90(17) . . ? N2 P1 S1A 105.67(17) . . ? N5A P1 S1A 95.9(5) . . ? N1 P1 S1 107.79(13) . . ? N2 P1 S1 107.97(14) . . ? N5 P1 S1 95.8(3) . . ? S1A P1 S1 110.71(12) . . ? N3 P2 N2 115.04(16) . . ? N3 P2 N6 111.99(15) . . ? N2 P2 N6 112.41(17) . . ? N3 P2 S2 110.51(11) . . ? N2 P2 S2 108.89(13) . . ? N6 P2 S2 96.41(11) . . ? N3 P3 N1 114.87(16) . . ? N3 P3 N4 109.38(17) . . ? N1 P3 N4 114.05(18) . . ? N3 P3 S3 112.06(11) . . ? N1 P3 S3 109.36(14) . . ? N4 P3 S3 95.55(11) . . ? C1 S1 P1 89.6(4) . . ? C3 S2 P2 90.62(16) . . ? C3A S2 P2 91.3(5) . . ? C5 S3 P3 92.22(13) . . ? C1A S1A P1 92.6(10) . . ? C2A N5A P1 129.3(15) . . ? C2A N5A H5A1 115.4 . . ? P1 N5A H5A1 115.4 . . ? C2A C1A S1A 123.6(17) . . ? C2A C1A H1A1 106.4 . . ? S1A C1A H1A1 106.4 . . ? C2A C1A H1A2 106.4 . . ? S1A C1A H1A2 106.4 . . ? H1A1 C1A H1A2 106.5 . . ? N5A C2A C1A 97.2(16) . . ? N5A C2A H2A1 112.3 . . ? C1A C2A H2A1 112.3 . . ? N5A C2A H2A2 112.3 . . ? C1A C2A H2A2 112.3 . . ? H2A1 C2A H2A2 109.9 . . ? 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 S1 C1 C2 N5 57.0(13) . . . . ? S2 C3 C4 C3A -57.1(8) . . . . ? S2 C3 C4 N6 44.8(4) . . . . ? S3 C5 C6 N4 -46.6(4) . . . . ? N6 C4 C3A S2 -37.5(13) . . . . ? C3 C4 C3A S2 58.4(9) . . . . ? C5 C6 N4 P3 34.4(5) . . . . ? C1 C2 N5 P1 -57.6(13) . . . . ? C3A C4 N6 P2 24.9(9) . . . . ? C3 C4 N6 P2 -25.5(5) . . . . ? P3 N1 P1 N2 5.5(3) . . . . ? P3 N1 P1 N5A -128.8(6) . . . . ? P3 N1 P1 N5 139.6(4) . . . . ? P3 N1 P1 S1A 124.1(3) . . . . ? P3 N1 P1 S1 -116.8(2) . . . . ? P2 N2 P1 N1 -10.2(3) . . . . ? P2 N2 P1 N5A 128.8(6) . . . . ? P2 N2 P1 N5 -142.7(4) . . . . ? P2 N2 P1 S1A -129.4(2) . . . . ? P2 N2 P1 S1 112.1(2) . . . . ? C2 N5 P1 N1 144.8(9) . . . . ? C2 N5 P1 N2 -79.4(10) . . . . ? C2 N5 P1 N5A 26.6(11) . . . . ? C2 N5 P1 S1A -137.5(16) . . . . ? C2 N5 P1 S1 33.2(9) . . . . ? P3 N3 P2 N2 4.9(3) . . . . ? P3 N3 P2 N6 -125.0(2) . . . . ? P3 N3 P2 S2 128.73(18) . . . . ? P1 N2 P2 N3 5.2(3) . . . . ? P1 N2 P2 N6 134.9(2) . . . . ? P1 N2 P2 S2 -119.5(2) . . . . ? C4 N6 P2 N3 -117.6(3) . . . . ? C4 N6 P2 N2 111.1(3) . . . . ? C4 N6 P2 S2 -2.4(3) . . . . ? P2 N3 P3 N1 -9.1(3) . . . . ? P2 N3 P3 N4 -138.8(2) . . . . ? P2 N3 P3 S3 116.55(19) . . . . ? P1 N1 P3 N3 3.5(3) . . . . ? P1 N1 P3 N4 130.9(2) . . . . ? P1 N1 P3 S3 -123.5(2) . . . . ? C6 N4 P3 N3 -122.7(3) . . . . ? C6 N4 P3 N1 107.1(3) . . . . ? C6 N4 P3 S3 -7.0(3) . . . . ? C2 C1 S1 P1 -32.7(11) . . . . ? N1 P1 S1 C1 -113.7(3) . . . . ? N2 P1 S1 C1 118.2(3) . . . . ? N5A P1 S1 C1 25.1(16) . . . . ? N5 P1 S1 C1 0.4(4) . . . . ? S1A P1 S1 C1 2.9(3) . . . . ? C4 C3 S2 C3A 51.2(8) . . . . ? C4 C3 S2 P2 -40.0(3) . . . . ? C4 C3A S2 C3 -58.5(10) . . . . ? C4 C3A S2 P2 30.9(11) . . . . ? N3 P2 S2 C3 139.5(2) . . . . ? N2 P2 S2 C3 -93.2(2) . . . . ? N6 P2 S2 C3 23.1(2) . . . . ? N3 P2 S2 C3A 101.9(7) . . . . ? N2 P2 S2 C3A -130.8(7) . . . . ? N6 P2 S2 C3A -14.5(7) . . . . ? C6 C5 S3 P3 36.8(3) . . . . ? N3 P3 S3 C5 96.28(18) . . . . ? N1 P3 S3 C5 -135.15(18) . . . . ? N4 P3 S3 C5 -17.24(19) . . . . ? N1 P1 S1A C1A 132.9(8) . . . . ? N2 P1 S1A C1A -100.9(8) . . . . ? N5A P1 S1A C1A 9.8(9) . . . . ? N5 P1 S1A C1A 25.6(13) . . . . ? S1 P1 S1A C1A 15.8(8) . . . . ? N1 P1 N5A C2A -122.7(13) . . . . ? N2 P1 N5A C2A 99.1(14) . . . . ? N5 P1 N5A C2A -13.6(14) . . . . ? S1A P1 N5A C2A -9.5(14) . . . . ? S1 P1 N5A C2A -169(3) . . . . ? P1 S1A C1A C2A -12(2) . . . . ? P1 N5A C2A C1A 3(2) . . . . ? S1A C1A C2A N5A 8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.545 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.094 #===END #===END data_tuf5s _database_code_depnum_ccdc_archive 'CCDC 760673' #TrackingRef 'SulfurContainingCyclomatrixPhosphazenes2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common trans-N3P3Cl2(NHCH2CH2S)2 _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Cl2 N5 P3 S2' _chemical_formula_sum 'C4 H10 Cl2 N5 P3 S2' _chemical_formula_weight 356.10 _chemical_absolute_configuration unk 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.850(2) _cell_length_b 11.225(2) _cell_length_c 12.684(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.897(3) _cell_angle_gamma 90.00 _cell_volume 1377.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 5032 _cell_measurement_theta_min 2.408 _cell_measurement_theta_max 28.319 _exptl_crystal_description pyramid _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.751 _exptl_absorpt_correction_T_max 0.799 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 13157 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0287 _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 -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6658 _reflns_number_gt 6548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; 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^ > 2sigma(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^)+(0.0435P)^2^+0.8372P] 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 noref _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 0.04(6) _refine_ls_number_reflns 6658 _refine_ls_number_parameters 289 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0753 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 N10 N 0.2726(2) -0.0726(2) 0.61790(16) 0.0202(4) Uani 1 1 d . . . H10 H 0.2708 -0.1026 0.6817 0.024 Uiso 1 1 calc R . . S2 S 0.05612(5) 0.89194(5) 0.83447(5) 0.01718(11) Uani 1 1 d . . . P4 P 0.16191(6) 0.02965(6) 0.56468(5) 0.01683(11) Uani 1 1 d . . . P1 P 0.45682(6) 1.07499(6) 0.88102(5) 0.01555(11) Uani 1 1 d . . . P5 P -0.12274(6) 0.02698(6) 0.55605(5) 0.01864(12) Uani 1 1 d . . . P2 P 0.26148(6) 0.89698(6) 0.91582(4) 0.01540(11) Uani 1 1 d . . . P3 P 0.35630(6) 1.06674(6) 1.07139(5) 0.01856(12) Uani 1 1 d . . . S3 S 0.06319(6) 0.18100(5) 0.85522(4) 0.01819(11) Uani 1 1 d . . . P6 P 0.03545(6) 0.19393(5) 0.68808(4) 0.01523(11) Uani 1 1 d . . . Cl4 Cl -0.22878(6) -0.10634(6) 0.60904(6) 0.02903(13) Uani 1 1 d . . . Cl3 Cl -0.25819(7) 0.07031(7) 0.42087(5) 0.03110(14) Uani 1 1 d . . . Cl2 Cl 0.48775(7) 1.02474(8) 1.20930(5) 0.03698(17) Uani 1 1 d . . . Cl1 Cl 0.24042(7) 1.19013(7) 1.12849(6) 0.03303(15) Uani 1 1 d . . . S9 S 0.24903(7) 0.06629(7) 0.43059(5) 0.02551(13) Uani 1 1 d . . . C6 C -0.0051(3) 0.4000(2) 0.7761(2) 0.0244(5) Uani 1 1 d . . . H6A H -0.1054 0.3914 0.7746 0.029 Uiso 1 1 calc R . . H6B H 0.0172 0.4859 0.7748 0.029 Uiso 1 1 calc R . . N4 N 0.2860(2) 0.75375(19) 0.91749(19) 0.0219(4) Uani 1 1 d . . . H4 H 0.3669 0.7239 0.9468 0.026 Uiso 1 1 calc R . . N1 N 0.4423(2) 1.13094(19) 0.99602(17) 0.0189(4) Uani 1 1 d . . . N9 N 0.0331(2) 0.3396(2) 0.68387(17) 0.0215(4) Uani 1 1 d . . . H9 H 0.0537 0.3793 0.6292 0.026 Uiso 1 1 calc R . . N7 N -0.1116(2) 0.1357(2) 0.63490(17) 0.0201(4) Uani 1 1 d . . . N2 N 0.3631(2) 0.95991(18) 0.84862(16) 0.0178(4) Uani 1 1 d . . . N3 N 0.2650(2) 0.9543(2) 1.03309(16) 0.0199(4) Uani 1 1 d . . . C5 C 0.0771(3) 0.3420(2) 0.8759(2) 0.0279(6) Uani 1 1 d . . . H5A H 0.0392 0.3651 0.9399 0.033 Uiso 1 1 calc R . . H5B H 0.1751 0.3672 0.8869 0.033 Uiso 1 1 calc R . . N6 N 0.1633(2) 0.14279(19) 0.64114(17) 0.0189(4) Uani 1 1 d . . . C3 C 0.1728(2) 0.6750(2) 0.8700(2) 0.0231(5) Uani 1 1 d . . . H3A H 0.1192 0.6503 0.9249 0.028 Uiso 1 1 calc R . . H3B H 0.2097 0.6027 0.8406 0.028 Uiso 1 1 calc R . . N8 N 0.0103(2) -0.0274(2) 0.52266(19) 0.0250(5) Uani 1 1 d . . . C4 C 0.0807(2) 0.7442(2) 0.7803(2) 0.0197(5) Uani 1 1 d . . . H4C H -0.0093 0.7034 0.7584 0.024 Uiso 1 1 calc R . . H4D H 0.1255 0.7507 0.7170 0.024 Uiso 1 1 calc R . . S1 S 0.66123(6) 1.03566(8) 0.87645(6) 0.03038(15) Uani 1 1 d . . . N5 N 0.4334(2) 1.1793(2) 0.78868(17) 0.0233(4) Uani 1 1 d . . . H5 H 0.3559 1.2203 0.7738 0.028 Uiso 1 1 calc R . . C1 C 0.6807(3) 1.1763(3) 0.8100(2) 0.0372(7) Uani 1 1 d . . . H1A H 0.7000 1.2412 0.8636 0.045 Uiso 1 1 calc R . . H1B H 0.7587 1.1715 0.7711 0.045 Uiso 1 1 calc R . . C2 C 0.5480(3) 1.2009(3) 0.7324(2) 0.0342(7) Uani 1 1 d . . . H2A H 0.5462 1.2845 0.7072 0.041 Uiso 1 1 calc R . . H2B H 0.5401 1.1477 0.6692 0.041 Uiso 1 1 calc R . . C8 C 0.3745(4) -0.1120(4) 0.5551(3) 0.0468(9) Uani 1 1 d . . . H8A H 0.4681 -0.1038 0.5996 0.056 Uiso 1 1 calc R . . H8B H 0.3591 -0.1975 0.5377 0.056 Uiso 1 1 calc R . . C7 C 0.3694(8) -0.0501(7) 0.4623(5) 0.142(4) Uani 1 1 d . . . H7A H 0.3518 -0.1081 0.4025 0.170 Uiso 1 1 calc R . . H7B H 0.4625 -0.0162 0.4635 0.170 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 N10 0.0189(9) 0.0259(11) 0.0163(9) -0.0011(8) 0.0042(8) 0.0015(8) S2 0.0125(2) 0.0181(3) 0.0192(2) 0.0017(2) -0.00138(18) -0.0010(2) P4 0.0146(2) 0.0227(3) 0.0134(2) -0.0029(2) 0.00321(19) -0.0002(2) P1 0.0121(2) 0.0199(3) 0.0145(2) -0.0013(2) 0.00221(19) -0.0037(2) P5 0.0133(2) 0.0259(3) 0.0158(3) -0.0047(2) 0.0006(2) 0.0006(2) P2 0.0128(2) 0.0169(3) 0.0151(3) 0.0033(2) -0.00115(19) -0.0026(2) P3 0.0166(3) 0.0265(3) 0.0119(2) 0.0002(2) 0.0010(2) -0.0045(2) S3 0.0227(3) 0.0204(3) 0.0107(2) -0.0004(2) 0.00109(19) 0.0024(2) P6 0.0151(2) 0.0192(3) 0.0110(2) -0.0009(2) 0.00161(19) 0.0008(2) Cl4 0.0198(3) 0.0314(3) 0.0350(3) 0.0004(3) 0.0028(2) -0.0050(3) Cl3 0.0269(3) 0.0434(4) 0.0184(3) -0.0028(3) -0.0074(2) 0.0022(3) Cl2 0.0348(3) 0.0517(4) 0.0187(3) 0.0085(3) -0.0097(2) -0.0137(3) Cl1 0.0331(3) 0.0410(4) 0.0290(3) -0.0113(3) 0.0158(3) -0.0029(3) S9 0.0297(3) 0.0312(3) 0.0177(3) 0.0013(2) 0.0098(2) 0.0016(3) C6 0.0340(13) 0.0181(11) 0.0203(11) -0.0016(10) 0.0030(10) 0.0021(11) N4 0.0132(9) 0.0178(10) 0.0311(12) 0.0030(9) -0.0051(8) -0.0013(8) N1 0.0174(9) 0.0218(10) 0.0174(10) -0.0023(8) 0.0032(8) -0.0048(8) N9 0.0292(11) 0.0198(10) 0.0160(9) 0.0038(8) 0.0060(8) 0.0027(8) N7 0.0137(9) 0.0281(11) 0.0177(10) -0.0056(8) 0.0010(7) 0.0020(8) N2 0.0173(9) 0.0208(10) 0.0147(9) -0.0005(7) 0.0020(7) -0.0046(7) N3 0.0166(9) 0.0286(11) 0.0143(9) 0.0018(8) 0.0022(7) -0.0066(8) C5 0.0430(16) 0.0222(12) 0.0167(11) -0.0068(10) 0.0014(10) -0.0045(11) N6 0.0153(9) 0.0248(10) 0.0167(9) -0.0042(8) 0.0031(7) 0.0006(8) C3 0.0175(11) 0.0175(11) 0.0321(13) 0.0055(10) -0.0009(9) -0.0022(9) N8 0.0136(9) 0.0320(12) 0.0288(12) -0.0164(9) 0.0029(8) -0.0026(8) C4 0.0169(11) 0.0171(11) 0.0235(12) -0.0025(9) -0.0001(9) -0.0022(8) S1 0.0134(2) 0.0424(4) 0.0358(3) -0.0168(3) 0.0057(2) -0.0026(3) N5 0.0258(10) 0.0243(10) 0.0198(10) 0.0043(9) 0.0045(8) -0.0073(9) C1 0.0299(14) 0.0532(19) 0.0341(15) -0.0230(14) 0.0199(12) -0.0254(14) C2 0.0474(17) 0.0373(16) 0.0224(13) -0.0076(12) 0.0178(12) -0.0225(14) C8 0.0483(19) 0.057(2) 0.0421(17) 0.0149(17) 0.0263(16) 0.0347(18) C7 0.205(8) 0.155(6) 0.108(4) 0.096(5) 0.136(5) 0.151(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N10 C8 1.462(3) . ? N10 P4 1.638(2) . ? N10 H10 0.8800 . ? S2 C4 1.829(3) . ? S2 P2 2.0906(8) . ? P4 N6 1.596(2) . ? P4 N8 1.620(2) . ? P4 S9 2.0857(9) . ? P1 N2 1.596(2) . ? P1 N1 1.619(2) . ? P1 N5 1.642(2) . ? P1 S1 2.0728(9) . ? P5 N7 1.568(2) . ? P5 N8 1.575(2) . ? P5 Cl4 2.0119(10) . ? P5 Cl3 2.0229(9) . ? P2 N2 1.597(2) . ? P2 N3 1.615(2) . ? P2 N4 1.625(2) . ? P3 N1 1.567(2) . ? P3 N3 1.573(2) . ? P3 Cl1 2.0145(10) . ? P3 Cl2 2.0254(9) . ? S3 C5 1.827(3) . ? S3 P6 2.0907(9) . ? P6 N6 1.598(2) . ? P6 N7 1.616(2) . ? P6 N9 1.636(2) . ? S9 C7 1.759(5) . ? C6 N9 1.461(3) . ? C6 C5 1.515(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N4 C3 1.461(3) . ? N4 H4 0.8800 . ? N9 H9 0.8800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C3 C4 1.526(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? S1 C1 1.817(4) . ? N5 C2 1.466(3) . ? N5 H5 0.8800 . ? C1 C2 1.506(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C8 C7 1.360(5) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 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 C8 N10 P4 117.35(19) . . ? C8 N10 H10 121.3 . . ? P4 N10 H10 121.3 . . ? C4 S2 P2 91.45(8) . . ? N6 P4 N8 114.58(11) . . ? N6 P4 N10 112.24(11) . . ? N8 P4 N10 111.03(13) . . ? N6 P4 S9 112.40(9) . . ? N8 P4 S9 107.79(9) . . ? N10 P4 S9 97.46(8) . . ? N2 P1 N1 113.62(11) . . ? N2 P1 N5 113.42(11) . . ? N1 P1 N5 109.97(12) . . ? N2 P1 S1 109.76(8) . . ? N1 P1 S1 111.08(8) . . ? N5 P1 S1 97.95(9) . . ? N7 P5 N8 120.79(11) . . ? N7 P5 Cl4 110.10(9) . . ? N8 P5 Cl4 108.21(10) . . ? N7 P5 Cl3 107.99(9) . . ? N8 P5 Cl3 108.33(10) . . ? Cl4 P5 Cl3 99.27(4) . . ? N2 P2 N3 114.15(11) . . ? N2 P2 N4 109.75(12) . . ? N3 P2 N4 113.87(12) . . ? N2 P2 S2 113.22(8) . . ? N3 P2 S2 108.40(8) . . ? N4 P2 S2 96.15(8) . . ? N1 P3 N3 121.60(11) . . ? N1 P3 Cl1 108.14(9) . . ? N3 P3 Cl1 109.46(9) . . ? N1 P3 Cl2 107.63(9) . . ? N3 P3 Cl2 108.35(9) . . ? Cl1 P3 Cl2 99.37(4) . . ? C5 S3 P6 93.96(9) . . ? N6 P6 N7 113.97(11) . . ? N6 P6 N9 110.74(12) . . ? N7 P6 N9 112.64(12) . . ? N6 P6 S3 113.07(8) . . ? N7 P6 S3 109.28(8) . . ? N9 P6 S3 95.79(8) . . ? C7 S9 P4 91.75(14) . . ? N9 C6 C5 107.0(2) . . ? N9 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? N9 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? C3 N4 P2 119.58(17) . . ? C3 N4 H4 120.2 . . ? P2 N4 H4 120.2 . . ? P3 N1 P1 121.42(13) . . ? C6 N9 P6 116.20(17) . . ? C6 N9 H9 121.9 . . ? P6 N9 H9 121.9 . . ? P5 N7 P6 122.01(13) . . ? P1 N2 P2 127.67(13) . . ? P3 N3 P2 121.03(13) . . ? C6 C5 S3 106.92(18) . . ? C6 C5 H5A 110.3 . . ? S3 C5 H5A 110.3 . . ? C6 C5 H5B 110.3 . . ? S3 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? P4 N6 P6 126.55(13) . . ? N4 C3 C4 107.4(2) . . ? N4 C3 H3A 110.2 . . ? C4 C3 H3A 110.2 . . ? N4 C3 H3B 110.2 . . ? C4 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? P5 N8 P4 121.36(14) . . ? C3 C4 S2 106.51(17) . . ? C3 C4 H4C 110.4 . . ? S2 C4 H4C 110.4 . . ? C3 C4 H4D 110.4 . . ? S2 C4 H4D 110.4 . . ? H4C C4 H4D 108.6 . . ? C1 S1 P1 90.94(11) . . ? C2 N5 P1 116.6(2) . . ? C2 N5 H5 121.7 . . ? P1 N5 H5 121.7 . . ? C2 C1 S1 107.92(19) . . ? C2 C1 H1A 110.1 . . ? S1 C1 H1A 110.1 . . ? C2 C1 H1B 110.1 . . ? S1 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N5 C2 C1 107.7(2) . . ? N5 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? N5 C2 H2B 110.2 . . ? C1 C2 H2B 110.2 . . ? H2A C2 H2B 108.5 . . ? C7 C8 N10 113.6(3) . . ? C7 C8 H8A 108.8 . . ? N10 C8 H8A 108.8 . . ? C7 C8 H8B 108.8 . . ? N10 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C7 S9 119.4(3) . . ? C8 C7 H7A 107.5 . . ? S9 C7 H7A 107.5 . . ? C8 C7 H7B 107.5 . . ? S9 C7 H7B 107.5 . . ? H7A C7 H7B 107.0 . . ? 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 C8 N10 P4 N6 -124.8(3) . . . . ? C8 N10 P4 N8 105.5(3) . . . . ? C8 N10 P4 S9 -6.9(3) . . . . ? C4 S2 P2 N2 93.11(12) . . . . ? C4 S2 P2 N3 -139.17(12) . . . . ? C4 S2 P2 N4 -21.48(12) . . . . ? C5 S3 P6 N6 111.66(14) . . . . ? C5 S3 P6 N7 -120.26(13) . . . . ? C5 S3 P6 N9 -3.81(13) . . . . ? N6 P4 S9 C7 123.7(4) . . . . ? N8 P4 S9 C7 -109.1(4) . . . . ? N10 P4 S9 C7 5.9(4) . . . . ? N2 P2 N4 C3 -118.2(2) . . . . ? N3 P2 N4 C3 112.4(2) . . . . ? S2 P2 N4 C3 -0.8(2) . . . . ? N3 P3 N1 P1 -7.9(2) . . . . ? Cl1 P3 N1 P1 -135.75(13) . . . . ? Cl2 P3 N1 P1 117.76(13) . . . . ? N2 P1 N1 P3 6.5(2) . . . . ? N5 P1 N1 P3 134.88(15) . . . . ? S1 P1 N1 P3 -117.80(13) . . . . ? C5 C6 N9 P6 46.8(3) . . . . ? N6 P6 N9 C6 -140.66(19) . . . . ? N7 P6 N9 C6 90.4(2) . . . . ? S3 P6 N9 C6 -23.31(19) . . . . ? N8 P5 N7 P6 -1.9(2) . . . . ? Cl4 P5 N7 P6 125.33(14) . . . . ? Cl3 P5 N7 P6 -127.26(14) . . . . ? N6 P6 N7 P5 7.8(2) . . . . ? N9 P6 N7 P5 135.04(15) . . . . ? S3 P6 N7 P5 -119.79(14) . . . . ? N1 P1 N2 P2 -0.3(2) . . . . ? N5 P1 N2 P2 -126.86(17) . . . . ? S1 P1 N2 P2 124.73(15) . . . . ? N3 P2 N2 P1 -4.4(2) . . . . ? N4 P2 N2 P1 -133.59(16) . . . . ? S2 P2 N2 P1 120.27(15) . . . . ? N1 P3 N3 P2 2.7(2) . . . . ? Cl1 P3 N3 P2 129.90(13) . . . . ? Cl2 P3 N3 P2 -122.70(13) . . . . ? N2 P2 N3 P3 3.2(2) . . . . ? N4 P2 N3 P3 130.28(15) . . . . ? S2 P2 N3 P3 -124.02(13) . . . . ? N9 C6 C5 S3 -46.1(3) . . . . ? P6 S3 C5 C6 27.8(2) . . . . ? N8 P4 N6 P6 6.8(2) . . . . ? N10 P4 N6 P6 -120.98(17) . . . . ? S9 P4 N6 P6 130.35(14) . . . . ? N7 P6 N6 P4 -10.6(2) . . . . ? N9 P6 N6 P4 -138.87(16) . . . . ? S3 P6 N6 P4 114.96(15) . . . . ? P2 N4 C3 C4 28.9(3) . . . . ? N7 P5 N8 P4 -2.4(3) . . . . ? Cl4 P5 N8 P4 -130.46(15) . . . . ? Cl3 P5 N8 P4 122.83(16) . . . . ? N6 P4 N8 P5 0.1(2) . . . . ? N10 P4 N8 P5 128.59(17) . . . . ? S9 P4 N8 P5 -125.79(16) . . . . ? N4 C3 C4 S2 -45.2(2) . . . . ? P2 S2 C4 C3 39.02(16) . . . . ? N2 P1 S1 C1 136.72(12) . . . . ? N1 P1 S1 C1 -96.79(13) . . . . ? N5 P1 S1 C1 18.26(12) . . . . ? N2 P1 N5 C2 -110.8(2) . . . . ? N1 P1 N5 C2 120.7(2) . . . . ? S1 P1 N5 C2 4.8(2) . . . . ? P1 S1 C1 C2 -37.61(18) . . . . ? P1 N5 C2 C1 -32.1(3) . . . . ? S1 C1 C2 N5 46.7(3) . . . . ? P4 N10 C8 C7 4.8(7) . . . . ? N10 C8 C7 S9 1.0(9) . . . . ? P4 S9 C7 C8 -4.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.946 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.077