Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ramaswamy Murugavel' _publ_contact_author_address ; Department of Chemistry IIT-Bombay Powai Mumbai 400076 INDIA ; _publ_contact_author_email RMV@CHEM.IITB.AC.IN _publ_section_title ; Sterically Encumbered Acyclic Diphosphazanes: Synthesis, Conformations, and Co-ordination Behavior ; loop_ _publ_author_name 'Ramaswamy Murugavel' 'R. Butcher' 'Ganesan Prabusankar' # Attachment '289829.cif' data_gp299m #(compound 5) _database_code_depnum_ccdc_archive 'CCDC 289829' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H41 Mo N O8 P2' _chemical_formula_weight 797.60 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' O O 0.0106 0.0060 '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' Mo Mo -1.6832 0.6857 '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)/c 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 12.4493(8) _cell_length_b 14.5027(10) _cell_length_c 21.6089(15) _cell_angle_alpha 90.00 _cell_angle_beta 102.0870(10) _cell_angle_gamma 90.00 _cell_volume 3815.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.6 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.714639 _exptl_absorpt_correction_T_max 0.928081 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30043 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 29.14 _reflns_number_total 9679 _reflns_number_gt 7790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0334P)^2^+3.3953P] 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 9679 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.135 _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 Mo Mo 0.24841(2) 0.353698(16) 0.354834(11) 0.03654(7) Uani 1 1 d . . . P1 P 0.36245(6) 0.21290(5) 0.38116(3) 0.03219(14) Uani 1 1 d . . . P2 P 0.14505(5) 0.20961(5) 0.36348(3) 0.03196(14) Uani 1 1 d . . . O1 O 0.4316(2) 0.50224(19) 0.35318(15) 0.0835(9) Uani 1 1 d . . . O2 O 0.0516(2) 0.4933(2) 0.31858(15) 0.0819(9) Uani 1 1 d . . . O3 O 0.2335(2) 0.34527(18) 0.20686(11) 0.0653(7) Uani 1 1 d . . . O4 O 0.2608(2) 0.4292(2) 0.49431(13) 0.0807(8) Uani 1 1 d . . . O11 O 0.43447(15) 0.16934(13) 0.33383(9) 0.0385(4) Uani 1 1 d . . . O12 O 0.43970(15) 0.17908(14) 0.44751(9) 0.0414(4) Uani 1 1 d . . . O21 O 0.07201(15) 0.14509(14) 0.30924(9) 0.0417(4) Uani 1 1 d . . . O22 O 0.07378(15) 0.19232(13) 0.41711(8) 0.0367(4) Uani 1 1 d . . . N N 0.25649(17) 0.14081(14) 0.38224(10) 0.0335(4) Uani 1 1 d . . . C1 C 0.3639(3) 0.4492(2) 0.35362(15) 0.0519(8) Uani 1 1 d . . . C2 C 0.1243(3) 0.4442(2) 0.33196(16) 0.0536(8) Uani 1 1 d . . . C3 C 0.2408(3) 0.3421(2) 0.26023(15) 0.0454(7) Uani 1 1 d . . . C4 C 0.2551(3) 0.3954(2) 0.44639(15) 0.0522(8) Uani 1 1 d . . . C11 C 0.2584(2) 0.04446(18) 0.40483(13) 0.0398(6) Uani 1 1 d . . . H11J H 0.1926 0.0336 0.4211 0.048 Uiso 1 1 calc R . . H11K H 0.3209 0.0370 0.4397 0.048 Uiso 1 1 calc R . . C12 C 0.2650(3) -0.0280(2) 0.35556(18) 0.0617(9) Uani 1 1 d . . . H12J H 0.2660 -0.0881 0.3743 0.093 Uiso 1 1 calc R . . H12K H 0.3309 -0.0192 0.3398 0.093 Uiso 1 1 calc R . . H12L H 0.2023 -0.0228 0.3213 0.093 Uiso 1 1 calc R . . C111 C 0.4481(2) 0.21074(19) 0.27675(12) 0.0373(6) Uani 1 1 d . . . C112 C 0.3934(3) 0.1707(2) 0.22027(14) 0.0457(7) Uani 1 1 d . . . C113 C 0.3173(3) 0.0904(3) 0.21896(17) 0.0669(10) Uani 1 1 d . . . H11A H 0.2860 0.0744 0.1759 0.100 Uiso 1 1 calc R . . H11B H 0.2597 0.1067 0.2403 0.100 Uiso 1 1 calc R . . H11C H 0.3575 0.0388 0.2399 0.100 Uiso 1 1 calc R . . C114 C 0.4140(3) 0.2077(3) 0.16445(15) 0.0577(9) Uani 1 1 d . . . H11D H 0.3812 0.1812 0.1259 0.069 Uiso 1 1 calc R . . C115 C 0.4817(3) 0.2822(3) 0.16510(17) 0.0665(10) Uani 1 1 d . . . H11E H 0.4915 0.3076 0.1272 0.080 Uiso 1 1 calc R . . C116 C 0.5352(3) 0.3195(3) 0.22166(17) 0.0590(9) Uani 1 1 d . . . H11F H 0.5811 0.3700 0.2215 0.071 Uiso 1 1 calc R . . C117 C 0.5218(2) 0.2830(2) 0.27940(15) 0.0473(7) Uani 1 1 d . . . C118 C 0.5907(3) 0.3172(3) 0.34056(16) 0.0593(9) Uani 1 1 d . . . H11G H 0.5440 0.3318 0.3694 0.089 Uiso 1 1 calc R . . H11H H 0.6300 0.3714 0.3327 0.089 Uiso 1 1 calc R . . H11I H 0.6420 0.2702 0.3587 0.089 Uiso 1 1 calc R . . C121 C 0.5549(2) 0.1855(2) 0.46624(13) 0.0435(7) Uani 1 1 d . . . C122 C 0.6185(3) 0.1117(2) 0.45432(15) 0.0502(7) Uani 1 1 d . . . C123 C 0.5707(3) 0.0247(2) 0.42187(18) 0.0623(9) Uani 1 1 d . . . H12A H 0.6275 -0.0209 0.4247 0.093 Uiso 1 1 calc R . . H12B H 0.5399 0.0375 0.3782 0.093 Uiso 1 1 calc R . . H12C H 0.5143 0.0019 0.4421 0.093 Uiso 1 1 calc R . . C124 C 0.7324(3) 0.1194(3) 0.47496(18) 0.0640(10) Uani 1 1 d . . . H12D H 0.7776 0.0722 0.4664 0.077 Uiso 1 1 calc R . . C125 C 0.7783(3) 0.1958(3) 0.5077(2) 0.0739(12) Uani 1 1 d . . . H12E H 0.8542 0.1998 0.5211 0.089 Uiso 1 1 calc R . . C126 C 0.7129(3) 0.2663(3) 0.52078(18) 0.0688(11) Uani 1 1 d . . . H12F H 0.7452 0.3171 0.5437 0.083 Uiso 1 1 calc R . . C127 C 0.5992(3) 0.2632(3) 0.50036(15) 0.0549(8) Uani 1 1 d . . . C128 C 0.5286(4) 0.3412(3) 0.51391(19) 0.0738(11) Uani 1 1 d . . . H12G H 0.5672 0.3755 0.5497 0.111 Uiso 1 1 calc R . . H12H H 0.4618 0.3171 0.5230 0.111 Uiso 1 1 calc R . . H12I H 0.5115 0.3810 0.4777 0.111 Uiso 1 1 calc R . . C211 C -0.0439(2) 0.1450(2) 0.29122(14) 0.0443(7) Uani 1 1 d . . . C212 C -0.0933(3) 0.2029(2) 0.24236(15) 0.0530(8) Uani 1 1 d . . . C213 C -0.0279(3) 0.2666(3) 0.21004(18) 0.0745(11) Uani 1 1 d . . . H21A H 0.0380 0.2362 0.2048 0.112 Uiso 1 1 calc R . . H21B H -0.0092 0.3210 0.2353 0.112 Uiso 1 1 calc R . . H21C H -0.0707 0.2836 0.1693 0.112 Uiso 1 1 calc R . . C214 C -0.2070(3) 0.1985(3) 0.22367(19) 0.0674(10) Uani 1 1 d . . . H21D H -0.2427 0.2368 0.1913 0.081 Uiso 1 1 calc R . . C215 C -0.2676(3) 0.1393(3) 0.2518(2) 0.0745(12) Uani 1 1 d . . . H21E H -0.3437 0.1386 0.2390 0.089 Uiso 1 1 calc R . . C216 C -0.2165(3) 0.0810(3) 0.2986(2) 0.0685(11) Uani 1 1 d . . . H21F H -0.2585 0.0406 0.3171 0.082 Uiso 1 1 calc R . . C217 C -0.1018(3) 0.0812(2) 0.31929(16) 0.0529(8) Uani 1 1 d . . . C218 C -0.0471(3) 0.0124(3) 0.36750(19) 0.0675(10) Uani 1 1 d . . . H21G H -0.0989 -0.0346 0.3726 0.101 Uiso 1 1 calc R . . H21H H -0.0211 0.0429 0.4072 0.101 Uiso 1 1 calc R . . H21I H 0.0138 -0.0153 0.3535 0.101 Uiso 1 1 calc R . . C221 C 0.0615(2) 0.25603(19) 0.46454(13) 0.0384(6) Uani 1 1 d . . . C222 C -0.0189(2) 0.3232(2) 0.45044(15) 0.0456(7) Uani 1 1 d . . . C223 C -0.0938(3) 0.3307(3) 0.38642(18) 0.0615(9) Uani 1 1 d . . . H22A H -0.0506 0.3363 0.3546 0.092 Uiso 1 1 calc R . . H22B H -0.1398 0.3840 0.3853 0.092 Uiso 1 1 calc R . . H22C H -0.1387 0.2765 0.3784 0.092 Uiso 1 1 calc R . . C224 C -0.0309(3) 0.3808(2) 0.50054(19) 0.0593(9) Uani 1 1 d . . . H22D H -0.0829 0.4277 0.4931 0.071 Uiso 1 1 calc R . . C225 C 0.0319(3) 0.3699(3) 0.56015(18) 0.0664(10) Uani 1 1 d . . . H22E H 0.0224 0.4096 0.5924 0.080 Uiso 1 1 calc R . . C226 C 0.1088(3) 0.3008(3) 0.57269(16) 0.0602(9) Uani 1 1 d . . . H22F H 0.1497 0.2932 0.6136 0.072 Uiso 1 1 calc R . . C227 C 0.1262(3) 0.2420(2) 0.52501(13) 0.0449(7) Uani 1 1 d . . . C228 C 0.2101(3) 0.1671(2) 0.53827(15) 0.0565(8) Uani 1 1 d . . . H22G H 0.2386 0.1631 0.5830 0.085 Uiso 1 1 calc R . . H22H H 0.2689 0.1805 0.5172 0.085 Uiso 1 1 calc R . . H22I H 0.1767 0.1094 0.5231 0.085 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 Mo 0.04621(14) 0.03127(12) 0.03462(12) 0.00155(9) 0.01415(9) 0.00169(10) P1 0.0347(3) 0.0347(3) 0.0280(3) 0.0021(2) 0.0085(2) -0.0005(3) P2 0.0346(3) 0.0335(3) 0.0287(3) -0.0006(2) 0.0087(2) 0.0013(3) O1 0.085(2) 0.0592(16) 0.106(2) 0.0083(15) 0.0188(17) -0.0250(15) O2 0.086(2) 0.0711(17) 0.098(2) 0.0290(15) 0.0428(16) 0.0405(16) O3 0.0814(17) 0.0799(17) 0.0364(12) 0.0087(11) 0.0162(11) 0.0271(14) O4 0.103(2) 0.087(2) 0.0599(16) -0.0291(15) 0.0350(15) -0.0214(17) O11 0.0421(11) 0.0428(10) 0.0335(10) 0.0087(8) 0.0145(8) 0.0081(8) O12 0.0366(10) 0.0545(12) 0.0319(10) 0.0065(8) 0.0040(8) -0.0010(9) O21 0.0377(10) 0.0512(11) 0.0353(10) -0.0109(8) 0.0059(8) -0.0014(9) O22 0.0402(10) 0.0391(10) 0.0343(10) -0.0050(7) 0.0155(8) -0.0028(8) N 0.0349(11) 0.0317(11) 0.0355(11) 0.0040(9) 0.0113(9) 0.0022(9) C1 0.065(2) 0.0416(16) 0.0511(18) 0.0012(13) 0.0176(15) -0.0043(15) C2 0.067(2) 0.0462(17) 0.0553(19) 0.0067(14) 0.0300(16) 0.0086(16) C3 0.0500(17) 0.0394(15) 0.0487(17) 0.0048(12) 0.0146(13) 0.0108(13) C4 0.064(2) 0.0480(17) 0.0485(18) -0.0078(14) 0.0220(15) -0.0066(15) C11 0.0458(16) 0.0334(13) 0.0427(15) 0.0065(11) 0.0149(12) 0.0010(12) C12 0.084(3) 0.0309(15) 0.077(2) -0.0021(15) 0.033(2) -0.0004(15) C111 0.0389(14) 0.0439(15) 0.0327(13) 0.0084(11) 0.0157(11) 0.0102(12) C112 0.0548(18) 0.0473(16) 0.0382(15) 0.0034(12) 0.0170(13) 0.0127(14) C113 0.090(3) 0.061(2) 0.0463(19) -0.0010(16) 0.0064(18) -0.007(2) C114 0.076(2) 0.066(2) 0.0342(16) 0.0058(14) 0.0183(15) 0.0156(19) C115 0.080(3) 0.079(3) 0.048(2) 0.0228(18) 0.0315(18) 0.014(2) C116 0.061(2) 0.060(2) 0.064(2) 0.0209(17) 0.0295(17) 0.0027(16) C117 0.0456(17) 0.0525(18) 0.0473(17) 0.0118(13) 0.0174(13) 0.0070(14) C118 0.052(2) 0.068(2) 0.058(2) 0.0107(17) 0.0116(16) -0.0108(17) C121 0.0394(15) 0.0563(17) 0.0329(14) 0.0125(12) 0.0032(11) -0.0052(13) C122 0.0461(17) 0.0602(19) 0.0437(17) 0.0211(14) 0.0078(13) 0.0024(15) C123 0.058(2) 0.057(2) 0.069(2) 0.0117(17) 0.0068(17) 0.0155(16) C124 0.0442(19) 0.079(3) 0.067(2) 0.0325(19) 0.0080(16) 0.0055(17) C125 0.043(2) 0.099(3) 0.073(3) 0.033(2) -0.0024(18) -0.014(2) C126 0.063(2) 0.082(3) 0.055(2) 0.0102(19) -0.0021(17) -0.026(2) C127 0.059(2) 0.067(2) 0.0362(16) 0.0049(14) 0.0050(14) -0.0116(17) C128 0.086(3) 0.079(3) 0.055(2) -0.0208(19) 0.009(2) -0.009(2) C211 0.0379(15) 0.0520(17) 0.0418(15) -0.0174(13) 0.0055(12) -0.0009(13) C212 0.0469(18) 0.062(2) 0.0467(17) -0.0136(15) 0.0011(14) 0.0072(15) C213 0.070(3) 0.095(3) 0.053(2) 0.013(2) 0.0011(18) 0.008(2) C214 0.054(2) 0.070(2) 0.068(2) -0.0173(19) -0.0097(18) 0.0120(19) C215 0.045(2) 0.075(3) 0.098(3) -0.031(2) 0.002(2) 0.0014(19) C216 0.052(2) 0.063(2) 0.095(3) -0.030(2) 0.026(2) -0.0182(18) C217 0.0500(18) 0.0493(18) 0.060(2) -0.0189(15) 0.0128(15) -0.0094(15) C218 0.070(2) 0.055(2) 0.079(3) -0.0029(18) 0.019(2) -0.0217(18) C221 0.0428(15) 0.0383(14) 0.0391(15) -0.0054(11) 0.0200(12) -0.0054(12) C222 0.0424(16) 0.0435(15) 0.0558(18) -0.0020(13) 0.0217(14) -0.0034(12) C223 0.0467(19) 0.062(2) 0.075(2) 0.0009(17) 0.0096(17) 0.0122(16) C224 0.061(2) 0.0436(17) 0.083(3) -0.0100(16) 0.0353(19) 0.0048(15) C225 0.087(3) 0.061(2) 0.061(2) -0.0237(17) 0.037(2) -0.0063(19) C226 0.080(2) 0.065(2) 0.0413(17) -0.0126(15) 0.0244(16) -0.0065(19) C227 0.0544(18) 0.0487(16) 0.0357(15) -0.0045(12) 0.0186(13) -0.0060(14) C228 0.068(2) 0.067(2) 0.0340(16) 0.0023(14) 0.0095(15) 0.0056(17) _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 Mo C1 2.000(3) . ? Mo C2 2.009(3) . ? Mo C3 2.034(3) . ? Mo C4 2.054(3) . ? Mo P2 2.4815(7) . ? Mo P1 2.4841(7) . ? P1 O11 1.6225(19) . ? P1 O12 1.6260(19) . ? P1 N 1.687(2) . ? P1 P2 2.6534(10) . ? P2 O22 1.6198(18) . ? P2 O21 1.6216(19) . ? P2 N 1.688(2) . ? O1 C1 1.143(4) . ? O2 C2 1.140(4) . ? O3 C3 1.139(4) . ? O4 C4 1.134(4) . ? O11 C111 1.413(3) . ? O12 C121 1.409(3) . ? O21 C211 1.414(3) . ? O22 C221 1.412(3) . ? N C11 1.479(3) . ? C11 C12 1.510(4) . ? C11 H11J 0.9700 . ? C11 H11K 0.9700 . ? C12 H12J 0.9600 . ? C12 H12K 0.9600 . ? C12 H12L 0.9600 . ? C111 C117 1.387(4) . ? C111 C112 1.393(4) . ? C112 C114 1.392(4) . ? C112 C113 1.497(5) . ? C113 H11A 0.9600 . ? C113 H11B 0.9600 . ? C113 H11C 0.9600 . ? C114 C115 1.368(5) . ? C114 H11D 0.9300 . ? C115 C116 1.375(5) . ? C115 H11E 0.9300 . ? C116 C117 1.397(4) . ? C116 H11F 0.9300 . ? C117 C118 1.501(5) . ? C118 H11G 0.9600 . ? C118 H11H 0.9600 . ? C118 H11I 0.9600 . ? C121 C122 1.387(5) . ? C121 C127 1.396(5) . ? C122 C124 1.398(4) . ? C122 C123 1.505(5) . ? C123 H12A 0.9600 . ? C123 H12B 0.9600 . ? C123 H12C 0.9600 . ? C124 C125 1.373(6) . ? C124 H12D 0.9300 . ? C125 C126 1.373(6) . ? C125 H12E 0.9300 . ? C126 C127 1.392(5) . ? C126 H12F 0.9300 . ? C127 C128 1.499(5) . ? C128 H12G 0.9600 . ? C128 H12H 0.9600 . ? C128 H12I 0.9600 . ? C211 C212 1.388(5) . ? C211 C217 1.388(5) . ? C212 C214 1.390(5) . ? C212 C213 1.498(5) . ? C213 H21A 0.9600 . ? C213 H21B 0.9600 . ? C213 H21C 0.9600 . ? C214 C215 1.366(6) . ? C214 H21D 0.9300 . ? C215 C216 1.369(6) . ? C215 H21E 0.9300 . ? C216 C217 1.404(5) . ? C216 H21F 0.9300 . ? C217 C218 1.500(5) . ? C218 H21G 0.9600 . ? C218 H21H 0.9600 . ? C218 H21I 0.9600 . ? C221 C222 1.385(4) . ? C221 C227 1.398(4) . ? C222 C224 1.399(4) . ? C222 C223 1.501(5) . ? C223 H22A 0.9600 . ? C223 H22B 0.9600 . ? C223 H22C 0.9600 . ? C224 C225 1.369(5) . ? C224 H22D 0.9300 . ? C225 C226 1.373(5) . ? C225 H22E 0.9300 . ? C226 C227 1.388(4) . ? C226 H22F 0.9300 . ? C227 C228 1.493(4) . ? C228 H22G 0.9600 . ? C228 H22H 0.9600 . ? C228 H22I 0.9600 . ? 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 C1 Mo C2 93.61(14) . . ? C1 Mo C3 85.79(13) . . ? C2 Mo C3 86.27(12) . . ? C1 Mo C4 85.67(13) . . ? C2 Mo C4 85.33(14) . . ? C3 Mo C4 167.62(12) . . ? C1 Mo P2 165.78(10) . . ? C2 Mo P2 100.62(10) . . ? C3 Mo P2 95.17(9) . . ? C4 Mo P2 95.31(9) . . ? C1 Mo P1 101.18(10) . . ? C2 Mo P1 165.18(10) . . ? C3 Mo P1 93.81(8) . . ? C4 Mo P1 96.64(10) . . ? P2 Mo P1 64.60(2) . . ? O11 P1 O12 97.79(10) . . ? O11 P1 N 107.72(11) . . ? O12 P1 N 96.93(10) . . ? O11 P1 Mo 122.71(7) . . ? O12 P1 Mo 130.84(8) . . ? N P1 Mo 95.83(8) . . ? O11 P1 P2 125.72(8) . . ? O12 P1 P2 121.24(7) . . ? N P1 P2 38.19(7) . . ? Mo P1 P2 57.65(2) . . ? O22 P2 O21 96.86(10) . . ? O22 P2 N 106.41(10) . . ? O21 P2 N 98.09(11) . . ? O22 P2 Mo 123.68(7) . . ? O21 P2 Mo 130.74(8) . . ? N P2 Mo 95.90(8) . . ? O22 P2 P1 126.50(8) . . ? O21 P2 P1 121.01(8) . . ? N P2 P1 38.16(7) . . ? Mo P2 P1 57.75(2) . . ? C111 O11 P1 124.58(16) . . ? C121 O12 P1 127.73(17) . . ? C211 O21 P2 125.81(17) . . ? C221 O22 P2 125.22(16) . . ? C11 N P1 129.17(18) . . ? C11 N P2 126.41(18) . . ? P1 N P2 103.65(11) . . ? O1 C1 Mo 178.5(3) . . ? O2 C2 Mo 177.9(3) . . ? O3 C3 Mo 172.7(3) . . ? O4 C4 Mo 171.4(3) . . ? N C11 C12 115.1(2) . . ? N C11 H11J 108.5 . . ? C12 C11 H11J 108.5 . . ? N C11 H11K 108.5 . . ? C12 C11 H11K 108.5 . . ? H11J C11 H11K 107.5 . . ? C11 C12 H12J 109.5 . . ? C11 C12 H12K 109.5 . . ? H12J C12 H12K 109.5 . . ? C11 C12 H12L 109.5 . . ? H12J C12 H12L 109.5 . . ? H12K C12 H12L 109.5 . . ? C117 C111 C112 123.3(3) . . ? C117 C111 O11 119.0(2) . . ? C112 C111 O11 117.5(3) . . ? C114 C112 C111 117.0(3) . . ? C114 C112 C113 120.9(3) . . ? C111 C112 C113 122.1(3) . . ? C112 C113 H11A 109.5 . . ? C112 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? C112 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 109.5 . . ? C115 C114 C112 121.4(3) . . ? C115 C114 H11D 119.3 . . ? C112 C114 H11D 119.3 . . ? C114 C115 C116 120.2(3) . . ? C114 C115 H11E 119.9 . . ? C116 C115 H11E 119.9 . . ? C115 C116 C117 121.3(3) . . ? C115 C116 H11F 119.4 . . ? C117 C116 H11F 119.4 . . ? C111 C117 C116 116.8(3) . . ? C111 C117 C118 122.5(3) . . ? C116 C117 C118 120.6(3) . . ? C117 C118 H11G 109.5 . . ? C117 C118 H11H 109.5 . . ? H11G C118 H11H 109.5 . . ? C117 C118 H11I 109.5 . . ? H11G C118 H11I 109.5 . . ? H11H C118 H11I 109.5 . . ? C122 C121 C127 122.8(3) . . ? C122 C121 O12 118.9(3) . . ? C127 C121 O12 118.1(3) . . ? C121 C122 C124 117.4(3) . . ? C121 C122 C123 123.2(3) . . ? C124 C122 C123 119.4(3) . . ? C122 C123 H12A 109.5 . . ? C122 C123 H12B 109.5 . . ? H12A C123 H12B 109.5 . . ? C122 C123 H12C 109.5 . . ? H12A C123 H12C 109.5 . . ? H12B C123 H12C 109.5 . . ? C125 C124 C122 120.9(4) . . ? C125 C124 H12D 119.5 . . ? C122 C124 H12D 119.5 . . ? C126 C125 C124 120.4(3) . . ? C126 C125 H12E 119.8 . . ? C124 C125 H12E 119.8 . . ? C125 C126 C127 121.2(4) . . ? C125 C126 H12F 119.4 . . ? C127 C126 H12F 119.4 . . ? C126 C127 C121 117.2(4) . . ? C126 C127 C128 120.8(3) . . ? C121 C127 C128 122.0(3) . . ? C127 C128 H12G 109.5 . . ? C127 C128 H12H 109.5 . . ? H12G C128 H12H 109.5 . . ? C127 C128 H12I 109.5 . . ? H12G C128 H12I 109.5 . . ? H12H C128 H12I 109.5 . . ? C212 C211 C217 123.2(3) . . ? C212 C211 O21 118.3(3) . . ? C217 C211 O21 118.3(3) . . ? C211 C212 C214 117.1(3) . . ? C211 C212 C213 122.0(3) . . ? C214 C212 C213 120.9(3) . . ? C212 C213 H21A 109.5 . . ? C212 C213 H21B 109.5 . . ? H21A C213 H21B 109.5 . . ? C212 C213 H21C 109.5 . . ? H21A C213 H21C 109.5 . . ? H21B C213 H21C 109.5 . . ? C215 C214 C212 121.5(4) . . ? C215 C214 H21D 119.2 . . ? C212 C214 H21D 119.2 . . ? C214 C215 C216 120.2(4) . . ? C214 C215 H21E 119.9 . . ? C216 C215 H21E 119.9 . . ? C215 C216 C217 121.2(4) . . ? C215 C216 H21F 119.4 . . ? C217 C216 H21F 119.4 . . ? C211 C217 C216 116.7(3) . . ? C211 C217 C218 123.0(3) . . ? C216 C217 C218 120.2(3) . . ? C217 C218 H21G 109.5 . . ? C217 C218 H21H 109.5 . . ? H21G C218 H21H 109.5 . . ? C217 C218 H21I 109.5 . . ? H21G C218 H21I 109.5 . . ? H21H C218 H21I 109.5 . . ? C222 C221 C227 123.8(3) . . ? C222 C221 O22 118.9(3) . . ? C227 C221 O22 117.1(2) . . ? C221 C222 C224 116.0(3) . . ? C221 C222 C223 122.3(3) . . ? C224 C222 C223 121.6(3) . . ? C222 C223 H22A 109.5 . . ? C222 C223 H22B 109.5 . . ? H22A C223 H22B 109.5 . . ? C222 C223 H22C 109.5 . . ? H22A C223 H22C 109.5 . . ? H22B C223 H22C 109.5 . . ? C225 C224 C222 121.8(3) . . ? C225 C224 H22D 119.1 . . ? C222 C224 H22D 119.1 . . ? C224 C225 C226 120.4(3) . . ? C224 C225 H22E 119.8 . . ? C226 C225 H22E 119.8 . . ? C225 C226 C227 120.8(3) . . ? C225 C226 H22F 119.6 . . ? C227 C226 H22F 119.6 . . ? C226 C227 C221 117.1(3) . . ? C226 C227 C228 121.1(3) . . ? C221 C227 C228 121.8(3) . . ? C227 C228 H22G 109.5 . . ? C227 C228 H22H 109.5 . . ? H22G C228 H22H 109.5 . . ? C227 C228 H22I 109.5 . . ? H22G C228 H22I 109.5 . . ? H22H C228 H22I 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 Mo P1 O11 -65.88(13) . . . . ? C2 Mo P1 O11 110.4(4) . . . . ? C3 Mo P1 O11 20.58(13) . . . . ? C4 Mo P1 O11 -152.76(13) . . . . ? P2 Mo P1 O11 114.49(9) . . . . ? C1 Mo P1 O12 74.32(14) . . . . ? C2 Mo P1 O12 -109.4(4) . . . . ? C3 Mo P1 O12 160.77(13) . . . . ? C4 Mo P1 O12 -12.56(14) . . . . ? P2 Mo P1 O12 -105.31(10) . . . . ? C1 Mo P1 N 178.71(12) . . . . ? C2 Mo P1 N -5.0(4) . . . . ? C3 Mo P1 N -94.84(12) . . . . ? C4 Mo P1 N 91.83(12) . . . . ? P2 Mo P1 N -0.92(8) . . . . ? C1 Mo P1 P2 179.63(10) . . . . ? C2 Mo P1 P2 -4.1(4) . . . . ? C3 Mo P1 P2 -93.92(9) . . . . ? C4 Mo P1 P2 92.75(9) . . . . ? C1 Mo P2 O22 113.6(4) . . . . ? C2 Mo P2 O22 -65.93(13) . . . . ? C3 Mo P2 O22 -153.10(12) . . . . ? C4 Mo P2 O22 20.29(13) . . . . ? P1 Mo P2 O22 115.13(9) . . . . ? C1 Mo P2 O21 -106.6(4) . . . . ? C2 Mo P2 O21 73.84(14) . . . . ? C3 Mo P2 O21 -13.33(13) . . . . ? C4 Mo P2 O21 160.07(14) . . . . ? P1 Mo P2 O21 -105.09(10) . . . . ? C1 Mo P2 N -0.6(4) . . . . ? C2 Mo P2 N 179.85(12) . . . . ? C3 Mo P2 N 92.69(11) . . . . ? C4 Mo P2 N -93.92(13) . . . . ? P1 Mo P2 N 0.92(8) . . . . ? C1 Mo P2 P1 -1.5(4) . . . . ? C2 Mo P2 P1 178.93(10) . . . . ? C3 Mo P2 P1 91.77(8) . . . . ? C4 Mo P2 P1 -94.84(10) . . . . ? O11 P1 P2 O22 140.17(12) . . . . ? O12 P1 P2 O22 11.00(14) . . . . ? N P1 P2 O22 68.10(15) . . . . ? Mo P1 P2 O22 -110.41(9) . . . . ? O11 P1 P2 O21 11.99(13) . . . . ? O12 P1 P2 O21 -117.18(13) . . . . ? N P1 P2 O21 -60.07(15) . . . . ? Mo P1 P2 O21 121.41(9) . . . . ? O11 P1 P2 N 72.06(15) . . . . ? O12 P1 P2 N -57.10(15) . . . . ? Mo P1 P2 N -178.52(12) . . . . ? O11 P1 P2 Mo -109.42(9) . . . . ? O12 P1 P2 Mo 121.41(10) . . . . ? N P1 P2 Mo 178.52(12) . . . . ? O12 P1 O11 C111 -144.5(2) . . . . ? N P1 O11 C111 115.6(2) . . . . ? Mo P1 O11 C111 6.3(2) . . . . ? P2 P1 O11 C111 77.5(2) . . . . ? O11 P1 O12 C121 46.5(3) . . . . ? N P1 O12 C121 155.5(2) . . . . ? Mo P1 O12 C121 -100.6(2) . . . . ? P2 P1 O12 C121 -173.0(2) . . . . ? O22 P2 O21 C211 46.6(2) . . . . ? N P2 O21 C211 154.3(2) . . . . ? Mo P2 O21 C211 -100.6(2) . . . . ? P1 P2 O21 C211 -172.9(2) . . . . ? O21 P2 O22 C221 -150.2(2) . . . . ? N P2 O22 C221 109.2(2) . . . . ? Mo P2 O22 C221 0.2(2) . . . . ? P1 P2 O22 C221 72.5(2) . . . . ? O11 P1 N C11 63.9(2) . . . . ? O12 P1 N C11 -36.6(2) . . . . ? Mo P1 N C11 -169.0(2) . . . . ? P2 P1 N C11 -170.3(3) . . . . ? O11 P1 N P2 -125.82(11) . . . . ? O12 P1 N P2 133.68(12) . . . . ? Mo P1 N P2 1.26(11) . . . . ? O22 P2 N C11 41.7(2) . . . . ? O21 P2 N C11 -58.0(2) . . . . ? Mo P2 N C11 169.4(2) . . . . ? P1 P2 N C11 170.6(3) . . . . ? O22 P2 N P1 -128.97(11) . . . . ? O21 P2 N P1 131.38(12) . . . . ? Mo P2 N P1 -1.26(11) . . . . ? C2 Mo C1 O1 -177(100) . . . . ? C3 Mo C1 O1 -91(12) . . . . ? C4 Mo C1 O1 98(12) . . . . ? P2 Mo C1 O1 4(12) . . . . ? P1 Mo C1 O1 2(12) . . . . ? C1 Mo C2 O2 166(8) . . . . ? C3 Mo C2 O2 81(8) . . . . ? C4 Mo C2 O2 -108(8) . . . . ? P2 Mo C2 O2 -14(8) . . . . ? P1 Mo C2 O2 -10(8) . . . . ? C1 Mo C3 O3 -60(2) . . . . ? C2 Mo C3 O3 34(2) . . . . ? C4 Mo C3 O3 -13(3) . . . . ? P2 Mo C3 O3 134(2) . . . . ? P1 Mo C3 O3 -161(2) . . . . ? C1 Mo C4 O4 36(2) . . . . ? C2 Mo C4 O4 -58(2) . . . . ? C3 Mo C4 O4 -10(3) . . . . ? P2 Mo C4 O4 -158(2) . . . . ? P1 Mo C4 O4 137(2) . . . . ? P1 N C11 C12 -89.6(3) . . . . ? P2 N C11 C12 102.1(3) . . . . ? P1 O11 C111 C117 78.3(3) . . . . ? P1 O11 C111 C112 -107.4(3) . . . . ? C117 C111 C112 C114 -1.1(4) . . . . ? O11 C111 C112 C114 -175.2(2) . . . . ? C117 C111 C112 C113 177.7(3) . . . . ? O11 C111 C112 C113 3.6(4) . . . . ? C111 C112 C114 C115 -2.5(5) . . . . ? C113 C112 C114 C115 178.7(3) . . . . ? C112 C114 C115 C116 3.2(5) . . . . ? C114 C115 C116 C117 -0.2(6) . . . . ? C112 C111 C117 C116 3.9(4) . . . . ? O11 C111 C117 C116 177.8(3) . . . . ? C112 C111 C117 C118 -172.0(3) . . . . ? O11 C111 C117 C118 2.0(4) . . . . ? C115 C116 C117 C111 -3.2(5) . . . . ? C115 C116 C117 C118 172.8(3) . . . . ? P1 O12 C121 C122 -92.4(3) . . . . ? P1 O12 C121 C127 92.4(3) . . . . ? C127 C121 C122 C124 -3.4(4) . . . . ? O12 C121 C122 C124 -178.4(3) . . . . ? C127 C121 C122 C123 175.3(3) . . . . ? O12 C121 C122 C123 0.3(4) . . . . ? C121 C122 C124 C125 2.3(5) . . . . ? C123 C122 C124 C125 -176.5(3) . . . . ? C122 C124 C125 C126 0.0(6) . . . . ? C124 C125 C126 C127 -1.2(6) . . . . ? C125 C126 C127 C121 0.1(5) . . . . ? C125 C126 C127 C128 -179.0(4) . . . . ? C122 C121 C127 C126 2.3(5) . . . . ? O12 C121 C127 C126 177.3(3) . . . . ? C122 C121 C127 C128 -178.7(3) . . . . ? O12 C121 C127 C128 -3.6(4) . . . . ? P2 O21 C211 C212 91.3(3) . . . . ? P2 O21 C211 C217 -94.5(3) . . . . ? C217 C211 C212 C214 3.2(5) . . . . ? O21 C211 C212 C214 177.2(3) . . . . ? C217 C211 C212 C213 -175.8(3) . . . . ? O21 C211 C212 C213 -1.9(5) . . . . ? C211 C212 C214 C215 -0.5(5) . . . . ? C213 C212 C214 C215 178.6(4) . . . . ? C212 C214 C215 C216 -1.4(6) . . . . ? C214 C215 C216 C217 0.6(6) . . . . ? C212 C211 C217 C216 -3.9(5) . . . . ? O21 C211 C217 C216 -177.8(3) . . . . ? C212 C211 C217 C218 173.7(3) . . . . ? O21 C211 C217 C218 -0.3(4) . . . . ? C215 C216 C217 C211 1.9(5) . . . . ? C215 C216 C217 C218 -175.8(4) . . . . ? P2 O22 C221 C222 84.7(3) . . . . ? P2 O22 C221 C227 -100.7(3) . . . . ? C227 C221 C222 C224 2.2(4) . . . . ? O22 C221 C222 C224 176.5(2) . . . . ? C227 C221 C222 C223 -174.2(3) . . . . ? O22 C221 C222 C223 0.0(4) . . . . ? C221 C222 C224 C225 -1.3(5) . . . . ? C223 C222 C224 C225 175.2(3) . . . . ? C222 C224 C225 C226 -0.5(6) . . . . ? C224 C225 C226 C227 1.5(6) . . . . ? C225 C226 C227 C221 -0.6(5) . . . . ? C225 C226 C227 C228 179.6(3) . . . . ? C222 C221 C227 C226 -1.3(4) . . . . ? O22 C221 C227 C226 -175.6(3) . . . . ? C222 C221 C227 C228 178.4(3) . . . . ? O22 C221 C227 C228 4.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 29.14 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.368 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.064 # Attachment '289830.cif' data_mur11a #(compound 1) _database_code_depnum_ccdc_archive 'CCDC 289830' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H76 N O4 P2' _chemical_formula_weight 817.06 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' 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 25.910(5) _cell_length_b 8.8881(18) _cell_length_c 22.878(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.65(3) _cell_angle_gamma 90.00 _cell_volume 5047.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 0.126 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2326 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 20.00 _reflns_number_total 2291 _reflns_number_gt 1601 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0962P)^2^+41.1367P] 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 SHELXL _refine_ls_extinction_coef 0.0023(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2291 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1415 _refine_ls_R_factor_gt 0.0985 _refine_ls_wR_factor_ref 0.2623 _refine_ls_wR_factor_gt 0.2365 _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 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 0.04908(8) 0.1299(3) 0.79300(10) 0.0522(8) Uani 1 1 d . . . O1 O 0.1049(2) 0.0570(6) 0.7833(2) 0.0646(17) Uani 1 1 d . . . O2 O 0.0544(2) 0.0473(6) 0.8587(2) 0.0564(16) Uani 1 1 d . . . N1 N 0.0000 0.0212(9) 0.7500 0.048(2) Uani 1 2 d S . . C7 C 0.0000 -0.145(2) 0.7500 0.131(9) Uani 1 2 d S . . H7A H -0.0274 -0.0823 0.7592 0.157 Uiso 0.50 1 calc PR . . H7B H 0.0274 -0.0823 0.7408 0.157 Uiso 0.50 1 calc PR . . C8 C 0.0175(8) -0.234(2) 0.7868(9) 0.092(7) Uani 0.50 1 d P . . H8A H 0.0108 -0.3347 0.7717 0.080 Uiso 1 1 d R . . H8B H 0.0556 -0.2179 0.8029 0.080 Uiso 1 1 d R . . H8C H 0.0005 -0.2179 0.8185 0.080 Uiso 1 1 d R . . C1 C 0.1301(4) 0.1309(14) 0.7446(5) 0.078(3) Uani 1 1 d . . . C2 C 0.1565(4) 0.2685(14) 0.7636(5) 0.084(3) Uani 1 1 d . . . C3 C 0.1816(4) 0.3358(15) 0.7221(6) 0.107(4) Uani 1 1 d . . . H3A H 0.1994 0.4307 0.7333 0.080 Uiso 1 1 d R . . C4 C 0.1818(5) 0.265(2) 0.6684(6) 0.116(4) Uani 1 1 d . . . H4A H 0.1989 0.3135 0.6413 0.080 Uiso 1 1 d R . . C5 C 0.1568(5) 0.1303(18) 0.6544(6) 0.112(4) Uani 1 1 d . . . H5A H 0.1570 0.0831 0.6167 0.080 Uiso 1 1 d R . . C6 C 0.1313(4) 0.0589(14) 0.6920(5) 0.083(3) Uani 1 1 d . . . C21 C 0.1577(4) 0.3510(15) 0.8228(5) 0.092(3) Uani 1 1 d . . . H21A H 0.1387 0.2885 0.8440 0.080 Uiso 1 1 d R . . C22 C 0.2134(5) 0.367(2) 0.8607(6) 0.164(7) Uani 1 1 d . . . H22A H 0.2146 0.4173 0.8982 0.080 Uiso 1 1 d R . . H22B H 0.2281 0.2677 0.8695 0.080 Uiso 1 1 d R . . H22C H 0.2341 0.4228 0.8394 0.080 Uiso 1 1 d R . . C23 C 0.1280(7) 0.4984(17) 0.8115(7) 0.153(6) Uani 1 1 d . . . H23A H 0.0918 0.4821 0.7864 0.080 Uiso 1 1 d R . . H23B H 0.1273 0.5435 0.8494 0.080 Uiso 1 1 d R . . H23C H 0.1463 0.5643 0.7908 0.080 Uiso 1 1 d R . . C61 C 0.1065(5) -0.0955(15) 0.6740(5) 0.095(4) Uani 1 1 d . . . H61A H 0.0862 -0.1200 0.7018 0.080 Uiso 1 1 d R . . C62 C 0.0695(6) -0.1106(15) 0.6115(6) 0.139(5) Uani 1 1 d . . . H62A H 0.0411 -0.0377 0.6060 0.080 Uiso 1 1 d R . . H62B H 0.0894 -0.0916 0.5828 0.080 Uiso 1 1 d R . . H62C H 0.0542 -0.2098 0.6050 0.080 Uiso 1 1 d R . . C63 C 0.1489(6) -0.2152(17) 0.6848(8) 0.173(7) Uani 1 1 d . . . H63A H 0.1334 -0.3132 0.6741 0.080 Uiso 1 1 d R . . H63B H 0.1710 -0.1901 0.6590 0.080 Uiso 1 1 d R . . H63C H 0.1705 -0.2155 0.7266 0.080 Uiso 1 1 d R . . C11 C 0.0853(3) 0.1274(11) 0.9100(4) 0.061(2) Uani 1 1 d . . . C12 C 0.1369(4) 0.0745(13) 0.9415(4) 0.073(3) Uani 1 1 d . . . C13 C 0.1665(4) 0.157(2) 0.9896(5) 0.107(4) Uani 1 1 d . . . H13A H 0.2018 0.1232 1.0119 0.080 Uiso 1 1 d R . . C14 C 0.1483(6) 0.2903(18) 1.0061(5) 0.102(4) Uani 1 1 d . . . H14A H 0.1703 0.3515 1.0383 0.080 Uiso 1 1 d R . . C15 C 0.0982(5) 0.3337(13) 0.9775(5) 0.091(3) Uani 1 1 d . . . H15A H 0.0841 0.4249 0.9894 0.080 Uiso 1 1 d R . . C16 C 0.0647(4) 0.2552(12) 0.9304(4) 0.075(3) Uani 1 1 d . . . C121 C 0.1552(4) -0.0794(15) 0.9238(4) 0.094(4) Uani 1 1 d . . . H12A H 0.1327 -0.1066 0.8841 0.080 Uiso 1 1 d R . . C122 C 0.2108(5) -0.0881(18) 0.9216(9) 0.189(8) Uani 1 1 d . . . H12B H 0.2214 -0.1846 0.9100 0.080 Uiso 1 1 d R . . H12C H 0.2151 -0.0133 0.8931 0.080 Uiso 1 1 d R . . H12D H 0.2330 -0.0628 0.9617 0.080 Uiso 1 1 d R . . C123 C 0.1497(7) -0.1977(17) 0.9678(7) 0.174(7) Uani 1 1 d . . . H12E H 0.1599 -0.2955 0.9572 0.080 Uiso 1 1 d R . . H12F H 0.1724 -0.1697 1.0073 0.080 Uiso 1 1 d R . . H12G H 0.1128 -0.2000 0.9687 0.080 Uiso 1 1 d R . . C161 C 0.0059(4) 0.2983(13) 0.9031(5) 0.090(3) Uani 1 1 d . . . H16A H -0.0100 0.2287 0.8709 0.080 Uiso 1 1 d R . . C162 C -0.0246(4) 0.2899(15) 0.9515(6) 0.122(5) Uani 1 1 d . . . H16B H -0.0214 0.1893 0.9674 0.080 Uiso 1 1 d R . . H16C H -0.0092 0.3593 0.9840 0.080 Uiso 1 1 d R . . H16D H -0.0620 0.3136 0.9337 0.080 Uiso 1 1 d R . . C163 C -0.0006(5) 0.4520(16) 0.8740(6) 0.140(5) Uani 1 1 d . . . H16E H 0.0184 0.4560 0.8437 0.080 Uiso 1 1 d R . . H16F H -0.0378 0.4769 0.8557 0.080 Uiso 1 1 d R . . H16G H 0.0150 0.5227 0.9059 0.080 Uiso 1 1 d 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 0.0463(13) 0.0616(15) 0.0488(14) 0.0002(12) 0.0138(10) 0.0032(11) O1 0.057(3) 0.087(4) 0.059(4) 0.014(3) 0.032(3) 0.014(3) O2 0.058(3) 0.081(4) 0.029(3) 0.000(3) 0.010(3) 0.014(3) N1 0.055(6) 0.038(6) 0.055(6) 0.000 0.020(5) 0.000 C7 0.19(2) 0.036(11) 0.23(3) 0.000 0.17(2) 0.000 C8 0.126(18) 0.041(13) 0.089(16) -0.002(12) -0.002(13) -0.023(12) C1 0.049(6) 0.106(8) 0.084(8) 0.011(7) 0.029(6) 0.012(6) C2 0.061(6) 0.111(9) 0.092(8) 0.008(7) 0.043(6) -0.006(6) C3 0.083(8) 0.115(10) 0.128(11) 0.007(9) 0.041(8) -0.009(7) C4 0.111(10) 0.159(14) 0.101(10) 0.026(10) 0.067(8) -0.009(10) C5 0.121(10) 0.149(12) 0.099(9) -0.009(9) 0.082(8) -0.001(9) C6 0.072(7) 0.122(10) 0.071(7) 0.005(7) 0.046(6) 0.007(7) C21 0.076(7) 0.120(10) 0.082(8) 0.009(7) 0.025(6) -0.025(7) C22 0.116(11) 0.26(2) 0.107(10) 0.020(12) 0.017(9) -0.041(12) C23 0.205(16) 0.131(12) 0.142(13) -0.029(11) 0.082(12) -0.031(13) C61 0.104(8) 0.134(11) 0.063(7) -0.011(7) 0.049(6) -0.002(9) C62 0.185(14) 0.107(10) 0.135(13) -0.031(9) 0.064(11) 0.015(10) C63 0.158(14) 0.129(12) 0.220(19) 0.067(13) 0.034(13) 0.003(12) C11 0.064(6) 0.085(7) 0.040(5) 0.001(5) 0.024(5) 0.006(5) C12 0.054(6) 0.122(9) 0.042(6) 0.014(6) 0.010(5) 0.012(6) C13 0.066(7) 0.182(14) 0.058(8) 0.003(9) -0.006(6) -0.016(9) C14 0.097(10) 0.141(12) 0.054(7) -0.041(8) 0.000(7) -0.041(9) C15 0.108(10) 0.097(8) 0.071(8) -0.019(7) 0.028(7) -0.021(8) C16 0.081(7) 0.092(8) 0.062(6) -0.012(6) 0.038(6) -0.001(6) C121 0.070(7) 0.151(11) 0.055(6) 0.014(7) 0.009(5) 0.038(7) C122 0.121(12) 0.153(15) 0.31(2) 0.019(15) 0.080(14) 0.040(11) C123 0.28(2) 0.130(13) 0.151(15) -0.005(12) 0.121(15) 0.030(13) C161 0.083(8) 0.092(8) 0.094(8) -0.020(7) 0.022(6) 0.015(6) C162 0.101(8) 0.140(11) 0.132(10) -0.064(9) 0.043(8) 0.006(8) C163 0.137(12) 0.151(13) 0.133(11) -0.001(11) 0.039(9) 0.053(10) _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 P1 O2 1.642(5) . ? P1 O1 1.658(5) . ? P1 N1 1.674(5) . ? O1 C1 1.404(11) . ? O2 C11 1.410(10) . ? N1 C7 1.473(19) . ? N1 P1 1.674(5) 2_556 ? C7 C8 1.151(16) 2_556 ? C7 C8 1.151(16) . ? C8 C8 1.67(4) 2_556 ? C1 C6 1.371(14) . ? C1 C2 1.408(14) . ? C2 C3 1.426(14) . ? C2 C21 1.534(15) . ? C3 C4 1.382(16) . ? C4 C5 1.355(17) . ? C5 C6 1.380(15) . ? C6 C61 1.521(15) . ? C21 C22 1.462(14) . ? C21 C23 1.503(17) . ? C61 C62 1.483(15) . ? C61 C63 1.497(16) . ? C11 C16 1.391(12) . ? C11 C12 1.407(12) . ? C12 C13 1.361(15) . ? C12 C121 1.539(14) . ? C13 C14 1.369(16) . ? C14 C15 1.333(15) . ? C15 C16 1.364(13) . ? C16 C161 1.522(13) . ? C121 C122 1.459(14) . ? C121 C123 1.491(16) . ? C161 C163 1.508(16) . ? C161 C162 1.535(14) . ? 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 O2 P1 O1 95.8(3) . . ? O2 P1 N1 97.5(3) . . ? O1 P1 N1 103.9(3) . . ? C1 O1 P1 118.8(5) . . ? C11 O2 P1 114.5(5) . . ? C7 N1 P1 125.3(2) . . ? C7 N1 P1 125.3(2) . 2_556 ? P1 N1 P1 109.5(5) . 2_556 ? C8 C7 C8 93(2) 2_556 . ? C8 C7 N1 133.5(11) 2_556 . ? C8 C7 N1 133.5(11) . . ? C7 C8 C8 43.5(11) . 2_556 ? C6 C1 O1 117.8(10) . . ? C6 C1 C2 123.0(10) . . ? O1 C1 C2 119.0(9) . . ? C1 C2 C3 115.7(11) . . ? C1 C2 C21 124.9(9) . . ? C3 C2 C21 119.3(11) . . ? C4 C3 C2 121.3(12) . . ? C5 C4 C3 119.3(12) . . ? C4 C5 C6 122.7(12) . . ? C1 C6 C5 117.9(12) . . ? C1 C6 C61 123.0(9) . . ? C5 C6 C61 119.1(11) . . ? C22 C21 C23 112.7(13) . . ? C22 C21 C2 109.7(10) . . ? C23 C21 C2 112.6(10) . . ? C62 C61 C63 109.7(11) . . ? C62 C61 C6 116.6(11) . . ? C63 C61 C6 111.4(10) . . ? C16 C11 C12 120.1(9) . . ? C16 C11 O2 120.8(8) . . ? C12 C11 O2 119.1(9) . . ? C13 C12 C11 117.8(11) . . ? C13 C12 C121 123.1(10) . . ? C11 C12 C121 118.8(9) . . ? C12 C13 C14 122.1(11) . . ? C15 C14 C13 118.6(10) . . ? C14 C15 C16 123.4(11) . . ? C15 C16 C11 117.7(10) . . ? C15 C16 C161 122.1(10) . . ? C11 C16 C161 120.2(9) . . ? C122 C121 C123 105.9(11) . . ? C122 C121 C12 116.0(11) . . ? C123 C121 C12 110.7(9) . . ? C163 C161 C16 112.4(10) . . ? C163 C161 C162 110.3(10) . . ? C16 C161 C162 110.7(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 O2 P1 O1 C1 -157.5(7) . . . . ? N1 P1 O1 C1 103.3(7) . . . . ? O1 P1 O2 C11 87.4(5) . . . . ? N1 P1 O2 C11 -167.7(5) . . . . ? O2 P1 N1 C7 -49.8(2) . . . . ? O1 P1 N1 C7 48.0(2) . . . . ? O2 P1 N1 P1 130.2(2) . . . 2_556 ? O1 P1 N1 P1 -132.0(2) . . . 2_556 ? P1 N1 C7 C8 -148.3(16) . . . 2_556 ? P1 N1 C7 C8 31.7(16) 2_556 . . 2_556 ? P1 N1 C7 C8 31.7(16) . . . . ? P1 N1 C7 C8 -148.3(16) 2_556 . . . ? N1 C7 C8 C8 180.000(13) . . . 2_556 ? P1 O1 C1 C6 -114.0(8) . . . . ? P1 O1 C1 C2 71.1(9) . . . . ? C6 C1 C2 C3 4.7(15) . . . . ? O1 C1 C2 C3 179.4(8) . . . . ? C6 C1 C2 C21 -178.2(10) . . . . ? O1 C1 C2 C21 -3.6(14) . . . . ? C1 C2 C3 C4 -3.2(16) . . . . ? C21 C2 C3 C4 179.5(11) . . . . ? C2 C3 C4 C5 1.3(19) . . . . ? C3 C4 C5 C6 -1(2) . . . . ? O1 C1 C6 C5 -178.9(9) . . . . ? C2 C1 C6 C5 -4.2(15) . . . . ? O1 C1 C6 C61 0.3(14) . . . . ? C2 C1 C6 C61 175.0(9) . . . . ? C4 C5 C6 C1 2.1(18) . . . . ? C4 C5 C6 C61 -177.1(12) . . . . ? C1 C2 C21 C22 119.9(12) . . . . ? C3 C2 C21 C22 -63.1(14) . . . . ? C1 C2 C21 C23 -113.7(12) . . . . ? C3 C2 C21 C23 63.3(13) . . . . ? C1 C6 C61 C62 129.2(11) . . . . ? C5 C6 C61 C62 -51.6(14) . . . . ? C1 C6 C61 C63 -103.9(12) . . . . ? C5 C6 C61 C63 75.3(14) . . . . ? P1 O2 C11 C16 74.4(8) . . . . ? P1 O2 C11 C12 -107.1(7) . . . . ? C16 C11 C12 C13 -3.6(13) . . . . ? O2 C11 C12 C13 177.9(8) . . . . ? C16 C11 C12 C121 170.9(8) . . . . ? O2 C11 C12 C121 -7.6(12) . . . . ? C11 C12 C13 C14 -2.7(16) . . . . ? C121 C12 C13 C14 -177.0(10) . . . . ? C12 C13 C14 C15 6.1(18) . . . . ? C13 C14 C15 C16 -3.1(18) . . . . ? C14 C15 C16 C11 -3.0(16) . . . . ? C14 C15 C16 C161 173.3(11) . . . . ? C12 C11 C16 C15 6.4(13) . . . . ? O2 C11 C16 C15 -175.1(8) . . . . ? C12 C11 C16 C161 -170.0(9) . . . . ? O2 C11 C16 C161 8.5(13) . . . . ? C13 C12 C121 C122 -46.9(15) . . . . ? C11 C12 C121 C122 138.9(11) . . . . ? C13 C12 C121 C123 73.7(14) . . . . ? C11 C12 C121 C123 -100.5(12) . . . . ? C15 C16 C161 C163 63.3(13) . . . . ? C11 C16 C161 C163 -120.4(10) . . . . ? C15 C16 C161 C162 -60.5(13) . . . . ? C11 C16 C161 C162 115.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.267 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.063 # Attachment '289831.cif' data_rm102a #(compound 4) _database_code_depnum_ccdc_archive 'CCDC 289831' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H51 Cl2 N O2 P2' _chemical_formula_weight 614.58 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3484(10) _cell_length_b 12.2160(9) _cell_length_c 15.4244(11) _cell_angle_alpha 97.828(6) _cell_angle_beta 96.701(7) _cell_angle_gamma 90.327(7) _cell_volume 1732.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6502 _diffrn_reflns_av_R_equivalents 0.0096 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6088 _reflns_number_gt 4695 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0458P)^2^+1.4769P] 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 6088 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1311 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 P1 P 0.80503(8) 0.29839(7) 0.08216(4) 0.0515(2) Uani 1 1 d . . . P2 P 0.76623(8) 0.19806(7) -0.09022(5) 0.0512(2) Uani 1 1 d . . . N1 N 0.8879(2) 0.2480(3) -0.00505(15) 0.0661(8) Uani 1 1 d . . . O1 O 0.89420(18) 0.23822(15) 0.15938(11) 0.0456(4) Uani 1 1 d . . . O2 O 0.82024(18) 0.26129(15) -0.16792(11) 0.0448(4) Uani 1 1 d . . . Cl1 Cl 0.89595(11) 0.45828(8) 0.11260(6) 0.0787(3) Uani 1 1 d . . . Cl2 Cl 0.84389(12) 0.04001(8) -0.12537(6) 0.0814(3) Uani 1 1 d . . . C1 C 0.8356(3) 0.2570(2) 0.24095(15) 0.0405(6) Uani 1 1 d . . . C2 C 0.7013(3) 0.2085(2) 0.24787(17) 0.0453(6) Uani 1 1 d . . . C3 C 0.6337(3) 0.2524(3) 0.32080(18) 0.0538(7) Uani 1 1 d . . . H3 H 0.5422 0.2256 0.3259 0.065 Uiso 1 1 calc R . . C4 C 0.6957(3) 0.3332(3) 0.38539(18) 0.0542(7) Uani 1 1 d . . . C5 C 0.8363(3) 0.3646(2) 0.38117(17) 0.0524(7) Uani 1 1 d . . . H5 H 0.8825 0.4134 0.4277 0.063 Uiso 1 1 calc R . . C6 C 0.9132(3) 0.3272(2) 0.31081(16) 0.0427(6) Uani 1 1 d . . . C7 C 0.6251(3) 0.1086(2) 0.18656(19) 0.0559(7) Uani 1 1 d . . . C8 C 0.4944(4) 0.1473(3) 0.1292(2) 0.0812(11) Uani 1 1 d . . . H8A H 0.5264 0.1972 0.0921 0.122 Uiso 1 1 calc R . . H8B H 0.4292 0.1843 0.1665 0.122 Uiso 1 1 calc R . . H8C H 0.4462 0.0844 0.0933 0.122 Uiso 1 1 calc R . . C9 C 0.5726(5) 0.0270(3) 0.2442(3) 0.0904(12) Uani 1 1 d . . . H9A H 0.6514 0.0096 0.2854 0.136 Uiso 1 1 calc R . . H9B H 0.5361 -0.0394 0.2074 0.136 Uiso 1 1 calc R . . H9C H 0.4974 0.0600 0.2757 0.136 Uiso 1 1 calc R . . C10 C 0.7228(4) 0.0419(3) 0.1261(3) 0.0797(10) Uani 1 1 d . . . H10A H 0.7391 0.0822 0.0788 0.119 Uiso 1 1 calc R . . H10B H 0.6770 -0.0281 0.1024 0.119 Uiso 1 1 calc R . . H10C H 0.8133 0.0299 0.1595 0.119 Uiso 1 1 calc R . . C11 C 0.6150(4) 0.3840(3) 0.4597(2) 0.0803(11) Uani 1 1 d . . . H11A H 0.5207 0.3503 0.4535 0.120 Uiso 1 1 calc R . . H11B H 0.6064 0.4619 0.4578 0.120 Uiso 1 1 calc R . . H11C H 0.6666 0.3721 0.5150 0.120 Uiso 1 1 calc R . . C12 C 1.0745(3) 0.3604(2) 0.32122(17) 0.0494(6) Uani 1 1 d . . . C13 C 1.0934(4) 0.4868(3) 0.3306(2) 0.0698(9) Uani 1 1 d . . . H13A H 1.1942 0.5064 0.3414 0.105 Uiso 1 1 calc R . . H13B H 1.0456 0.5203 0.3790 0.105 Uiso 1 1 calc R . . H13C H 1.0523 0.5125 0.2772 0.105 Uiso 1 1 calc R . . C14 C 1.1438(3) 0.3211(3) 0.4072(2) 0.0715(9) Uani 1 1 d . . . H14A H 1.2446 0.3405 0.4164 0.107 Uiso 1 1 calc R . . H14B H 1.1319 0.2423 0.4028 0.107 Uiso 1 1 calc R . . H14C H 1.0979 0.3560 0.4560 0.107 Uiso 1 1 calc R . . C15 C 1.1598(3) 0.3082(3) 0.2481(2) 0.0619(8) Uani 1 1 d . . . H15A H 1.2605 0.3253 0.2645 0.093 Uiso 1 1 calc R . . H15B H 1.1278 0.3369 0.1944 0.093 Uiso 1 1 calc R . . H15C H 1.1447 0.2294 0.2395 0.093 Uiso 1 1 calc R . . C16 C 0.7243(3) 0.2471(2) -0.24706(15) 0.0406(6) Uani 1 1 d . . . C17 C 0.7674(3) 0.1814(2) -0.32117(16) 0.0453(6) Uani 1 1 d . . . C18 C 0.6584(3) 0.1501(2) -0.38998(18) 0.0558(7) Uani 1 1 d . . . H18 H 0.6819 0.1044 -0.4394 0.067 Uiso 1 1 calc R . . C19 C 0.5181(3) 0.1830(3) -0.38877(19) 0.0574(7) Uani 1 1 d . . . C20 C 0.4875(3) 0.2592(3) -0.31967(19) 0.0555(7) Uani 1 1 d . . . H20 H 0.3949 0.2868 -0.3208 0.067 Uiso 1 1 calc R . . C21 C 0.5887(3) 0.2972(2) -0.24780(17) 0.0451(6) Uani 1 1 d . . . C22 C 0.9217(3) 0.1460(2) -0.33769(18) 0.0519(7) Uani 1 1 d . . . C23 C 1.0422(3) 0.1929(3) -0.2661(2) 0.0617(8) Uani 1 1 d . . . H23A H 1.1340 0.1757 -0.2860 0.093 Uiso 1 1 calc R . . H23B H 1.0342 0.1608 -0.2133 0.093 Uiso 1 1 calc R . . H23C H 1.0339 0.2716 -0.2540 0.093 Uiso 1 1 calc R . . C24 C 0.9540(4) 0.1892(3) -0.4232(2) 0.0768(10) Uani 1 1 d . . . H24A H 0.8853 0.1576 -0.4714 0.115 Uiso 1 1 calc R . . H24B H 1.0494 0.1687 -0.4354 0.115 Uiso 1 1 calc R . . H24C H 0.9475 0.2683 -0.4160 0.115 Uiso 1 1 calc R . . C25 C 0.9300(4) 0.0190(3) -0.3512(2) 0.0757(10) Uani 1 1 d . . . H25A H 0.8601 -0.0111 -0.3992 0.114 Uiso 1 1 calc R . . H25B H 0.9105 -0.0088 -0.2984 0.114 Uiso 1 1 calc R . . H25C H 1.0247 -0.0021 -0.3644 0.114 Uiso 1 1 calc R . . C26 C 0.4016(4) 0.1402(3) -0.4628(2) 0.0872(12) Uani 1 1 d . . . H26A H 0.4436 0.1235 -0.5168 0.131 Uiso 1 1 calc R . . H26B H 0.3300 0.1955 -0.4691 0.131 Uiso 1 1 calc R . . H26C H 0.3574 0.0744 -0.4492 0.131 Uiso 1 1 calc R . . C27 C 0.5427(3) 0.3929(2) -0.18081(19) 0.0550(7) Uani 1 1 d . . . C28 C 0.4678(4) 0.4800(3) -0.2333(3) 0.0828(11) Uani 1 1 d . . . H28A H 0.3791 0.4492 -0.2652 0.124 Uiso 1 1 calc R . . H28B H 0.5297 0.5010 -0.2739 0.124 Uiso 1 1 calc R . . H28C H 0.4479 0.5439 -0.1932 0.124 Uiso 1 1 calc R . . C29 C 0.6667(4) 0.4557(3) -0.1201(2) 0.0713(9) Uani 1 1 d . . . H29A H 0.7430 0.4697 -0.1540 0.107 Uiso 1 1 calc R . . H29B H 0.7020 0.4120 -0.0752 0.107 Uiso 1 1 calc R . . H29C H 0.6327 0.5246 -0.0931 0.107 Uiso 1 1 calc R . . C30 C 0.4342(4) 0.3492(3) -0.1247(2) 0.0819(11) Uani 1 1 d . . . H30A H 0.3542 0.3132 -0.1628 0.123 Uiso 1 1 calc R . . H30B H 0.4003 0.4099 -0.0867 0.123 Uiso 1 1 calc R . . H30C H 0.4808 0.2975 -0.0897 0.123 Uiso 1 1 calc R . . C31 C 1.0723(8) 0.2875(4) -0.0177(3) 0.143(3) Uani 1 1 d . . . H31A H 1.0894 0.2916 -0.0780 0.172 Uiso 1 1 calc R . . H31B H 1.1104 0.3524 0.0217 0.172 Uiso 1 1 calc R . . C32 C 1.1047(9) 0.1979(4) 0.0088(3) 0.173(3) Uani 1 1 d . . . H32A H 1.0885 0.2014 0.0694 0.260 Uiso 1 1 calc R . . H32B H 1.2045 0.1839 0.0034 0.260 Uiso 1 1 calc R . . H32C H 1.0462 0.1394 -0.0261 0.260 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 0.0415(4) 0.0784(5) 0.0353(4) 0.0093(3) 0.0055(3) 0.0118(4) P2 0.0407(4) 0.0762(5) 0.0370(4) 0.0103(3) 0.0023(3) -0.0023(3) N1 0.0347(12) 0.124(2) 0.0358(12) -0.0016(13) 0.0039(10) 0.0055(14) O1 0.0412(10) 0.0619(11) 0.0329(9) 0.0021(8) 0.0053(7) 0.0076(8) O2 0.0385(9) 0.0610(11) 0.0332(9) 0.0029(8) 0.0018(7) -0.0019(8) Cl1 0.0995(7) 0.0712(5) 0.0647(5) 0.0179(4) -0.0025(5) 0.0062(5) Cl2 0.1083(7) 0.0688(5) 0.0709(6) 0.0180(4) 0.0162(5) 0.0070(5) C1 0.0402(13) 0.0486(15) 0.0325(12) 0.0045(11) 0.0047(10) 0.0094(11) C2 0.0409(14) 0.0540(16) 0.0408(14) 0.0072(12) 0.0032(11) 0.0053(12) C3 0.0418(15) 0.0698(19) 0.0510(16) 0.0079(14) 0.0103(12) 0.0030(13) C4 0.0513(17) 0.0713(19) 0.0404(14) 0.0041(14) 0.0109(12) 0.0113(14) C5 0.0548(17) 0.0617(18) 0.0373(14) -0.0029(12) 0.0027(12) 0.0040(14) C6 0.0435(14) 0.0483(15) 0.0362(13) 0.0068(11) 0.0028(11) 0.0049(11) C7 0.0523(17) 0.0581(18) 0.0545(17) 0.0012(14) 0.0033(13) -0.0053(14) C8 0.060(2) 0.095(3) 0.079(2) 0.001(2) -0.0146(18) -0.0110(19) C9 0.105(3) 0.079(3) 0.088(3) 0.010(2) 0.014(2) -0.027(2) C10 0.084(3) 0.061(2) 0.087(3) -0.0184(18) 0.016(2) -0.0038(18) C11 0.070(2) 0.110(3) 0.059(2) -0.0129(19) 0.0252(17) 0.008(2) C12 0.0457(15) 0.0561(17) 0.0443(14) 0.0058(12) -0.0015(12) -0.0041(12) C13 0.077(2) 0.064(2) 0.065(2) 0.0019(16) 0.0053(17) -0.0125(17) C14 0.0537(19) 0.097(3) 0.061(2) 0.0185(18) -0.0115(15) -0.0037(17) C15 0.0374(15) 0.080(2) 0.0664(19) 0.0020(16) 0.0063(14) -0.0015(14) C16 0.0399(13) 0.0471(15) 0.0337(12) 0.0055(11) -0.0002(10) -0.0012(11) C17 0.0490(15) 0.0484(15) 0.0374(13) 0.0039(11) 0.0022(11) 0.0044(12) C18 0.0612(18) 0.0632(18) 0.0385(14) -0.0026(13) -0.0021(13) 0.0045(14) C19 0.0527(17) 0.068(2) 0.0462(16) 0.0048(14) -0.0109(13) -0.0007(14) C20 0.0438(16) 0.0668(19) 0.0552(17) 0.0115(15) -0.0012(13) 0.0059(14) C21 0.0425(14) 0.0516(16) 0.0421(14) 0.0087(12) 0.0056(11) 0.0025(12) C22 0.0520(16) 0.0584(17) 0.0447(15) 0.0015(13) 0.0092(13) 0.0106(13) C23 0.0402(15) 0.081(2) 0.0629(19) -0.0002(16) 0.0112(13) 0.0077(14) C24 0.075(2) 0.104(3) 0.0568(19) 0.0140(19) 0.0248(17) 0.014(2) C25 0.080(2) 0.069(2) 0.073(2) -0.0071(17) 0.0057(18) 0.0196(18) C26 0.075(2) 0.103(3) 0.070(2) -0.005(2) -0.0263(19) 0.001(2) C27 0.0523(17) 0.0599(18) 0.0533(17) 0.0046(14) 0.0114(13) 0.0112(14) C28 0.089(3) 0.074(2) 0.083(3) 0.0076(19) 0.006(2) 0.030(2) C29 0.079(2) 0.061(2) 0.068(2) -0.0109(16) 0.0067(18) 0.0092(17) C30 0.074(2) 0.096(3) 0.081(2) 0.009(2) 0.036(2) 0.017(2) C31 0.296(8) 0.069(3) 0.052(2) 0.005(2) -0.029(3) 0.008(4) C32 0.382(11) 0.078(3) 0.063(3) -0.003(2) 0.053(4) 0.010(5) _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 P1 O1 1.6333(18) . ? P1 N1 1.677(2) . ? P1 Cl1 2.0966(13) . ? P2 O2 1.6361(19) . ? P2 N1 1.678(2) . ? P2 Cl2 2.0908(13) . ? N1 C31 1.826(7) . ? O1 C1 1.421(3) . ? O2 C16 1.418(3) . ? C1 C2 1.406(4) . ? C1 C6 1.408(3) . ? C2 C3 1.399(4) . ? C2 C7 1.553(4) . ? C3 C4 1.376(4) . ? C4 C5 1.378(4) . ? C4 C11 1.510(4) . ? C5 C6 1.398(4) . ? C6 C12 1.544(4) . ? C7 C9 1.536(5) . ? C7 C8 1.538(4) . ? C7 C10 1.539(4) . ? C12 C15 1.528(4) . ? C12 C13 1.538(4) . ? C12 C14 1.545(4) . ? C16 C17 1.405(3) . ? C16 C21 1.409(4) . ? C17 C18 1.394(4) . ? C17 C22 1.548(4) . ? C18 C19 1.376(4) . ? C19 C20 1.374(4) . ? C19 C26 1.518(4) . ? C20 C21 1.397(4) . ? C21 C27 1.550(4) . ? C22 C23 1.532(4) . ? C22 C25 1.540(4) . ? C22 C24 1.547(4) . ? C27 C29 1.533(4) . ? C27 C28 1.545(4) . ? C27 C30 1.545(4) . ? C31 C32 1.246(6) . ? 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 O1 P1 N1 100.72(11) . . ? O1 P1 Cl1 100.22(8) . . ? N1 P1 Cl1 101.36(11) . . ? O2 P2 N1 100.34(12) . . ? O2 P2 Cl2 100.05(8) . . ? N1 P2 Cl2 101.57(11) . . ? P1 N1 P2 110.35(13) . . ? P1 N1 C31 123.0(2) . . ? P2 N1 C31 123.23(19) . . ? C1 O1 P1 113.15(15) . . ? C16 O2 P2 113.57(15) . . ? C2 C1 C6 122.8(2) . . ? C2 C1 O1 119.2(2) . . ? C6 C1 O1 118.0(2) . . ? C3 C2 C1 115.7(2) . . ? C3 C2 C7 117.1(2) . . ? C1 C2 C7 127.1(2) . . ? C4 C3 C2 123.4(3) . . ? C3 C4 C5 117.5(2) . . ? C3 C4 C11 121.7(3) . . ? C5 C4 C11 120.8(3) . . ? C4 C5 C6 123.6(3) . . ? C5 C6 C1 115.5(2) . . ? C5 C6 C12 116.9(2) . . ? C1 C6 C12 127.5(2) . . ? C9 C7 C8 108.9(3) . . ? C9 C7 C10 105.7(3) . . ? C8 C7 C10 108.7(3) . . ? C9 C7 C2 108.5(3) . . ? C8 C7 C2 110.3(3) . . ? C10 C7 C2 114.5(2) . . ? C15 C12 C13 108.7(3) . . ? C15 C12 C6 115.8(2) . . ? C13 C12 C6 110.5(2) . . ? C15 C12 C14 106.4(2) . . ? C13 C12 C14 108.4(2) . . ? C6 C12 C14 106.8(2) . . ? C17 C16 C21 122.7(2) . . ? C17 C16 O2 118.4(2) . . ? C21 C16 O2 118.9(2) . . ? C18 C17 C16 115.5(2) . . ? C18 C17 C22 116.4(2) . . ? C16 C17 C22 127.9(2) . . ? C19 C18 C17 123.6(3) . . ? C20 C19 C18 117.8(3) . . ? C20 C19 C26 120.8(3) . . ? C18 C19 C26 121.4(3) . . ? C19 C20 C21 123.2(3) . . ? C20 C21 C16 115.7(2) . . ? C20 C21 C27 116.8(2) . . ? C16 C21 C27 127.4(2) . . ? C23 C22 C25 108.7(3) . . ? C23 C22 C24 106.2(3) . . ? C25 C22 C24 108.7(3) . . ? C23 C22 C17 115.6(2) . . ? C25 C22 C17 110.1(3) . . ? C24 C22 C17 107.3(2) . . ? C29 C27 C28 105.3(3) . . ? C29 C27 C30 109.6(3) . . ? C28 C27 C30 108.6(3) . . ? C29 C27 C21 115.2(2) . . ? C28 C27 C21 108.0(2) . . ? C30 C27 C21 109.9(3) . . ? C32 C31 N1 84.8(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.696 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.046 # Attachment '289832.cif' data_rm91 #(compound 2) _database_code_depnum_ccdc_archive 'CCDC 289832' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H41 N1 O4 P2' _chemical_formula_sum 'C34 H41 N O4 P2' _chemical_formula_weight 589.62 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.1004(7) _cell_length_b 10.9409(9) _cell_length_c 12.6202(13) _cell_angle_alpha 90.00 _cell_angle_beta 102.384(7) _cell_angle_gamma 90.00 _cell_volume 1631.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.170 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 2990 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 24.95 _reflns_number_total 2855 _reflns_number_gt 1825 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0851P)^2^+0.2478P] 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 2855 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1519 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 P1 P 0.76257(7) 0.23312(7) 0.64126(6) 0.0519(3) Uani 1 1 d . . . N1 N 0.7500 0.1478(3) 0.7500 0.0628(10) Uani 1 2 d S . . O1 O 0.86730(16) 0.15361(17) 0.61194(14) 0.0570(5) Uani 1 1 d . . . O2 O 0.66254(17) 0.17926(18) 0.54222(15) 0.0599(5) Uani 1 1 d . . . C1 C 0.7096(6) 0.0121(7) 0.7302(6) 0.070(2) Uani 0.50 1 d P . . C2 C 0.7995(8) -0.0677(8) 0.7906(9) 0.115(3) Uani 0.50 1 d P . . C3 C 0.9224(2) 0.1929(3) 0.5307(2) 0.0533(7) Uani 1 1 d . . . C4 C 0.9040(2) 0.1252(3) 0.4351(2) 0.0645(8) Uani 1 1 d . . . C5 C 0.9627(4) 0.1642(5) 0.3561(3) 0.0892(13) Uani 1 1 d . . . C6 C 1.0346(4) 0.2610(5) 0.3735(4) 0.1011(16) Uani 1 1 d . . . C7 C 1.0528(3) 0.3246(4) 0.4705(4) 0.0883(12) Uani 1 1 d . . . C8 C 0.9972(3) 0.2907(3) 0.5511(3) 0.0665(8) Uani 1 1 d . . . C9 C 0.5677(3) 0.2526(3) 0.5010(2) 0.0635(8) Uani 1 1 d . . . C10 C 0.5768(3) 0.3446(3) 0.4272(3) 0.0746(9) Uani 1 1 d . . . C11 C 0.4774(4) 0.4111(5) 0.3852(4) 0.0938(13) Uani 1 1 d . . . C12 C 0.3778(4) 0.3843(6) 0.4155(5) 0.1084(17) Uani 1 1 d . . . C13 C 0.3715(4) 0.2920(5) 0.4872(4) 0.0997(13) Uani 1 1 d . . . C14 C 0.4661(3) 0.2249(4) 0.5322(3) 0.0778(10) Uani 1 1 d . . . C21 C 0.8259(4) 0.0170(4) 0.4171(4) 0.0833(11) Uani 1 1 d . . . C22 C 1.0222(5) 0.3583(5) 0.6582(5) 0.0980(14) Uani 1 1 d . . . C23 C 0.6842(4) 0.3720(6) 0.3916(4) 0.0916(13) Uani 1 1 d . . . C24 C 0.4583(4) 0.1226(5) 0.6089(5) 0.0955(14) Uani 1 1 d . . . H5 H 0.945(3) 0.115(3) 0.292(3) 0.082(11) Uiso 1 1 d . . . H6 H 1.072(4) 0.288(4) 0.321(4) 0.133(16) Uiso 1 1 d . . . H7 H 1.108(4) 0.403(4) 0.485(4) 0.136(16) Uiso 1 1 d . . . H11 H 0.493(3) 0.475(3) 0.347(3) 0.075(12) Uiso 1 1 d . . . H12 H 0.313(4) 0.426(4) 0.386(3) 0.111(14) Uiso 1 1 d . . . H13 H 0.292(4) 0.276(4) 0.513(3) 0.128(15) Uiso 1 1 d . . . H21A H 0.833(4) -0.035(4) 0.476(4) 0.119(17) Uiso 1 1 d . . . H21B H 0.736(5) 0.042(5) 0.413(4) 0.163(19) Uiso 1 1 d . . . H21C H 0.835(4) -0.017(4) 0.348(4) 0.126(15) Uiso 1 1 d . . . H22A H 1.076(5) 0.420(6) 0.654(5) 0.18(2) Uiso 1 1 d . . . H22B H 0.951(5) 0.410(5) 0.655(4) 0.15(2) Uiso 1 1 d . . . H22C H 1.024(4) 0.312(5) 0.714(4) 0.126(19) Uiso 1 1 d . . . H23A H 0.688(4) 0.437(5) 0.340(5) 0.148(18) Uiso 1 1 d . . . H23B H 0.747(4) 0.389(4) 0.452(4) 0.108(15) Uiso 1 1 d . . . H23C H 0.718(4) 0.306(5) 0.370(3) 0.115(17) Uiso 1 1 d . . . H24A H 0.482(4) 0.041(5) 0.576(4) 0.131(16) Uiso 1 1 d . . . H24B H 0.513(4) 0.129(4) 0.675(4) 0.125(17) Uiso 1 1 d . . . H24C H 0.396(4) 0.123(4) 0.635(4) 0.120(16) 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 P1 0.0609(5) 0.0557(5) 0.0435(4) -0.0005(3) 0.0209(3) -0.0026(4) N1 0.098(3) 0.0500(19) 0.0511(19) 0.000 0.0390(19) 0.000 O1 0.0625(12) 0.0647(12) 0.0487(11) 0.0030(9) 0.0225(9) 0.0021(10) O2 0.0616(12) 0.0680(12) 0.0530(11) -0.0107(10) 0.0187(9) -0.0001(11) C1 0.095(6) 0.053(3) 0.066(5) -0.006(4) 0.031(5) -0.004(3) C2 0.135(9) 0.069(5) 0.144(10) 0.034(6) 0.038(6) 0.031(5) C3 0.0499(16) 0.0681(18) 0.0457(15) 0.0071(13) 0.0186(12) 0.0062(14) C4 0.0545(18) 0.091(2) 0.0503(17) 0.0010(16) 0.0158(14) 0.0142(17) C5 0.080(3) 0.138(4) 0.056(2) 0.005(2) 0.0288(19) 0.025(3) C6 0.085(3) 0.139(4) 0.093(3) 0.046(3) 0.050(3) 0.019(3) C7 0.070(2) 0.095(3) 0.107(3) 0.033(3) 0.034(2) 0.003(2) C8 0.0577(18) 0.071(2) 0.072(2) 0.0125(17) 0.0175(16) 0.0019(16) C9 0.0593(19) 0.078(2) 0.0522(16) -0.0172(16) 0.0103(14) 0.0042(16) C10 0.076(2) 0.092(2) 0.0550(18) -0.0107(18) 0.0109(17) 0.016(2) C11 0.105(4) 0.098(3) 0.074(3) -0.006(2) 0.008(2) 0.024(3) C12 0.070(3) 0.146(5) 0.100(3) -0.035(3) -0.001(3) 0.031(3) C13 0.070(3) 0.124(4) 0.104(3) -0.030(3) 0.017(3) 0.002(3) C14 0.059(2) 0.100(3) 0.073(2) -0.034(2) 0.0112(17) -0.0033(19) C21 0.079(3) 0.102(3) 0.069(2) -0.029(2) 0.018(2) 0.000(2) C22 0.106(4) 0.087(3) 0.098(3) -0.010(3) 0.014(3) -0.030(3) C23 0.096(3) 0.109(4) 0.076(3) 0.028(3) 0.034(3) 0.023(3) C24 0.073(3) 0.112(4) 0.108(4) -0.018(3) 0.035(3) -0.027(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 P1 O1 1.643(2) . ? P1 O2 1.651(2) . ? P1 N1 1.6930(19) . ? N1 C1 1.567(8) . ? N1 C1 1.567(8) 2_656 ? N1 P1 1.6930(19) 2_656 ? O1 C3 1.405(3) . ? O2 C9 1.405(4) . ? C1 C2 0.911(8) 2_656 ? C1 C1 0.998(13) 2_656 ? C1 C2 1.473(9) . ? C2 C1 0.911(8) 2_656 ? C2 C2 1.40(2) 2_656 ? C3 C8 1.390(4) . ? C3 C4 1.391(4) . ? C4 C5 1.409(5) . ? C4 C21 1.502(5) . ? C5 C6 1.359(7) . ? C6 C7 1.383(7) . ? C7 C8 1.386(5) . ? C8 C22 1.512(6) . ? C9 C10 1.392(5) . ? C9 C14 1.401(5) . ? C10 C11 1.408(5) . ? C10 C23 1.494(6) . ? C11 C12 1.373(7) . ? C12 C13 1.369(7) . ? C13 C14 1.376(6) . ? C14 C24 1.496(6) . ? 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 O1 P1 O2 96.67(10) . . ? O1 P1 N1 95.65(10) . . ? O2 P1 N1 103.78(9) . . ? C1 N1 C1 37.1(5) . 2_656 ? C1 N1 P1 118.2(3) . . ? C1 N1 P1 124.9(3) 2_656 . ? C1 N1 P1 124.9(3) . 2_656 ? C1 N1 P1 118.2(3) 2_656 2_656 ? P1 N1 P1 113.11(19) . 2_656 ? C3 O1 P1 120.80(17) . . ? C9 O2 P1 118.96(17) . . ? C2 C1 C1 100.9(9) 2_656 2_656 ? C2 C1 C2 67.2(11) 2_656 . ? C1 C1 C2 37.4(4) 2_656 . ? C2 C1 N1 165.5(11) 2_656 . ? C1 C1 N1 71.4(2) 2_656 . ? C2 C1 N1 108.0(5) . . ? C1 C2 C2 76.0(8) 2_656 2_656 ? C1 C2 C1 41.7(7) 2_656 . ? C2 C2 C1 36.9(4) 2_656 . ? C8 C3 C4 123.2(3) . . ? C8 C3 O1 119.5(2) . . ? C4 C3 O1 117.2(3) . . ? C3 C4 C5 116.2(3) . . ? C3 C4 C21 122.0(3) . . ? C5 C4 C21 121.8(4) . . ? C6 C5 C4 121.6(4) . . ? C5 C6 C7 120.7(4) . . ? C6 C7 C8 120.3(4) . . ? C7 C8 C3 118.0(3) . . ? C7 C8 C22 119.3(4) . . ? C3 C8 C22 122.7(3) . . ? C10 C9 C14 122.9(3) . . ? C10 C9 O2 119.0(3) . . ? C14 C9 O2 118.0(3) . . ? C9 C10 C11 116.2(4) . . ? C9 C10 C23 123.1(3) . . ? C11 C10 C23 120.7(4) . . ? C12 C11 C10 121.0(5) . . ? C13 C12 C11 121.2(5) . . ? C12 C13 C14 120.5(5) . . ? C13 C14 C9 118.1(4) . . ? C13 C14 C24 120.2(4) . . ? C9 C14 C24 121.6(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.328 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.049