# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Peter Hofmann' 'Frank Eisentrager' 'Alexander Gothlich' 'Irene Gruber' 'Helmut Heiss' 'Christoph A. Kiener' 'Carl Kruger' 'J. Ulrich Notheis' 'Frank Rominger' 'Gunter Scherhag' 'Madeleine Schultz' 'Bernd F. Straub' 'Martin A. O. Volland' _publ_contact_author_name 'Prof Peter Hofmann' _publ_contact_author_address ; Organisch-Chemisches Institut Ruprecht-Karls-Universitat Heidelberg Im Neuenheimer Feld 270 Heidelberg D-69120 GERMANY ; _publ_contact_author_email PH@PHINDIGO.OCI.UNI-HEIDELBERG.DE _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Sterically Crowded Diphosphinomethane Ligands: Molecular Structures, UV-Photoelectron Spectroscopy and a Convenient General Synthesis of tBu2PCH2PtBu2 and Related Species ; data_ig1_dtbpm_1 _database_code_CSD 199933 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common dtbpm _chemical_formula_moiety 'C17 H38 P2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H38 P2' _chemical_formula_weight 304.41 _chemical_melting_point ? _chemical_compound_source ? 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 9.35650(10) _cell_length_b 17.3925(2) _cell_length_c 12.5085(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2035.54(5) _cell_formula_units_Z 4 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max .55 _exptl_crystal_size_mid .50 _exptl_crystal_size_min .16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.993 _exptl_crystal_density_method ? _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(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 'Siemens Smart CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16625 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.57 _reflns_number_total 3534 _reflns_number_observed 2874 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 10 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+0.3058P] 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 0.14(29) _refine_ls_number_reflns 3524 _refine_ls_number_parameters 368 _refine_ls_number_restraints 931 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_obs 0.0405 _refine_ls_wR_factor_all 0.1299 _refine_ls_wR_factor_obs 0.1103 _refine_ls_goodness_of_fit_all 1.083 _refine_ls_goodness_of_fit_obs 1.058 _refine_ls_restrained_S_all 1.416 _refine_ls_restrained_S_obs 1.440 _refine_ls_shift/esd_max 2.125 _refine_ls_shift/esd_mean 0.241 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P1A P 0.7962(5) 0.1252(3) 0.4906(11) 0.089(2) Uani 0.540(7) d PD 1 C11A C 0.9099(16) 0.1313(8) 0.3675(13) 0.081(5) Uani 0.540(7) d PD 1 C12A C 0.9779(22) 0.2109(8) 0.3530(14) 0.137(8) Uani 0.540(7) d PD 1 H12A H 1.0550(75) 0.2169(25) 0.4029(61) 0.205 Uiso 0.540(7) calc PR 1 H12B H 0.9073(34) 0.2499(8) 0.3656(83) 0.205 Uiso 0.540(7) calc PR 1 H12C H 1.0139(107) 0.2156(24) 0.2814(31) 0.205 Uiso 0.540(7) calc PR 1 C13A C 1.0247(14) 0.0683(7) 0.3476(14) 0.098(5) Uani 0.540(7) d PD 1 H13A H 0.9785(14) 0.0196(13) 0.3369(78) 0.147 Uiso 0.540(7) calc PR 1 H13B H 1.0870(64) 0.0652(40) 0.4084(36) 0.147 Uiso 0.540(7) calc PR 1 H13C H 1.0793(71) 0.0813(30) 0.2852(48) 0.147 Uiso 0.540(7) calc PR 1 C14A C 0.8001(22) 0.1228(13) 0.2745(16) 0.113(10) Uani 0.540(7) d PD 1 H14A H 0.7362(84) 0.1660(37) 0.2747(61) 0.169 Uiso 0.540(7) calc PR 1 H14B H 0.7463(89) 0.0763(37) 0.2839(54) 0.169 Uiso 0.540(7) calc PR 1 H14C H 0.8500(24) 0.1209(70) 0.2075(17) 0.169 Uiso 0.540(7) calc PR 1 C15A C 0.9081(17) 0.1511(11) 0.6111(14) 0.074(6) Uani 0.540(7) d PD 1 C16A C 0.8164(29) 0.1297(16) 0.7112(19) 0.143(14) Uani 0.540(7) d PD 1 H16A H 0.7254(97) 0.1550(105) 0.7070(91) 0.215 Uiso 0.540(7) calc PR 1 H16B H 0.8652(117) 0.1458(119) 0.7749(20) 0.215 Uiso 0.540(7) calc PR 1 H16C H 0.8022(206) 0.0750(21) 0.7132(102) 0.215 Uiso 0.540(7) calc PR 1 C17A C 1.0495(22) 0.1057(19) 0.6236(19) 0.158(13) Uani 0.540(7) d PD 1 H17A H 1.0315(37) 0.0519(22) 0.6129(116) 0.236 Uiso 0.540(7) calc PR 1 H17B H 1.0873(82) 0.1137(69) 0.6941(43) 0.236 Uiso 0.540(7) calc PR 1 H17C H 1.1174(57) 0.1234(61) 0.5715(79) 0.236 Uiso 0.540(7) calc PR 1 C18A C 0.9364(28) 0.2381(12) 0.6169(18) 0.134(11) Uani 0.540(7) d PD 1 H18A H 0.8506(47) 0.2655(12) 0.5989(95) 0.201 Uiso 0.540(7) calc PR 1 H18B H 1.0106(98) 0.2515(17) 0.5673(77) 0.201 Uiso 0.540(7) calc PR 1 H18C H 0.9656(130) 0.2516(16) 0.6880(34) 0.201 Uiso 0.540(7) calc PR 1 C10A C 0.7854(11) 0.0215(5) 0.5153(9) 0.070(3) Uani 0.540(7) d PD 1 H10A H 0.7492(11) 0.0143(5) 0.5872(9) 0.084 Uiso 0.540(7) calc PR 1 H10B H 0.8819(11) 0.0012(5) 0.5138(9) 0.084 Uiso 0.540(7) calc PR 1 P2A P 0.6761(4) -0.0372(2) 0.4250(2) 0.0665(14) Uani 0.540(7) d PD 1 C21A C 0.7256(18) -0.1369(5) 0.4751(15) 0.082(11) Uani 0.540(7) d PD 1 C22A C 0.8924(16) -0.1401(11) 0.4759(31) 0.168(12) Uani 0.540(7) d PD 1 H22A H 0.9295(17) -0.1026(76) 0.4268(117) 0.252 Uiso 0.540(7) calc PR 1 H22B H 0.9236(17) -0.1904(34) 0.4549(147) 0.252 Uiso 0.540(7) calc PR 1 H22C H 0.9268(18) -0.1290(106) 0.5466(47) 0.252 Uiso 0.540(7) calc PR 1 C23A C 0.6771(20) -0.1566(10) 0.5895(12) 0.108(6) Uani 0.540(7) d PD 1 H23A H 0.5782(41) -0.1713(68) 0.5886(19) 0.161 Uiso 0.540(7) calc PR 1 H23B H 0.6893(122) -0.1125(23) 0.6346(25) 0.161 Uiso 0.540(7) calc PR 1 H23C H 0.7335(90) -0.1984(47) 0.6165(38) 0.161 Uiso 0.540(7) calc PR 1 C24A C 0.6689(28) -0.1971(10) 0.3964(20) 0.181(12) Uani 0.540(7) d PD 1 H24A H 0.5682(43) -0.1895(58) 0.3860(100) 0.272 Uiso 0.540(7) calc PR 1 H24B H 0.6855(152) -0.2476(11) 0.4246(59) 0.272 Uiso 0.540(7) calc PR 1 H24C H 0.7175(122) -0.1918(58) 0.3292(42) 0.272 Uiso 0.540(7) calc PR 1 C25A C 0.4870(12) -0.0130(9) 0.4632(14) 0.080(6) Uani 0.540(7) d PD 1 C26A C 0.4511(18) 0.0587(11) 0.3944(17) 0.139(10) Uani 0.540(7) d PD 1 H26A H 0.3515(45) 0.0709(59) 0.4020(106) 0.209 Uiso 0.540(7) calc PR 1 H26B H 0.4716(168) 0.0480(35) 0.3207(25) 0.209 Uiso 0.540(7) calc PR 1 H26C H 0.5078(134) 0.1015(27) 0.4178(91) 0.209 Uiso 0.540(7) calc PR 1 C27A C 0.4655(14) 0.0127(10) 0.5801(10) 0.091(5) Uani 0.540(7) d PD 1 H27A H 0.5301(64) 0.0540(33) 0.5962(22) 0.137 Uiso 0.540(7) calc PR 1 H27B H 0.4842(88) -0.0298(16) 0.6271(11) 0.137 Uiso 0.540(7) calc PR 1 H27C H 0.3689(28) 0.0299(47) 0.5899(20) 0.137 Uiso 0.540(7) calc PR 1 C28A C 0.3841(13) -0.0787(10) 0.4390(17) 0.133(7) Uani 0.540(7) d PD 1 H28A H 0.4154(99) -0.1243(25) 0.4754(110) 0.199 Uiso 0.540(7) calc PR 1 H28B H 0.3823(138) -0.0880(66) 0.3634(22) 0.199 Uiso 0.540(7) calc PR 1 H28C H 0.2900(36) -0.0651(39) 0.4630(121) 0.199 Uiso 0.540(7) calc PR 1 P1B P 0.8028(4) 0.12850(14) 0.4749(7) 0.0357(8) Uani 0.460(7) d PD 2 C11B C 0.9129(15) 0.1567(8) 0.3517(12) 0.062(5) Uani 0.460(7) d PD 2 C12B C 0.9280(17) 0.2449(7) 0.3528(15) 0.085(5) Uani 0.460(7) d PD 2 H12D H 0.8349(19) 0.2680(7) 0.3492(65) 0.128 Uiso 0.460(7) calc PR 2 H12E H 0.9836(77) 0.2610(8) 0.2923(39) 0.128 Uiso 0.460(7) calc PR 2 H12F H 0.9747(74) 0.2607(7) 0.4174(34) 0.128 Uiso 0.460(7) calc PR 2 C13B C 1.0618(11) 0.1202(9) 0.3483(15) 0.092(5) Uani 0.460(7) d PD 2 H13D H 1.0537(16) 0.0657(12) 0.3592(89) 0.139 Uiso 0.460(7) calc PR 2 H13E H 1.1202(38) 0.1421(45) 0.4035(54) 0.139 Uiso 0.460(7) calc PR 2 H13F H 1.1047(47) 0.1299(53) 0.2799(32) 0.139 Uiso 0.460(7) calc PR 2 C14B C 0.8246(20) 0.1329(10) 0.2544(14) 0.058(4) Uani 0.460(7) d PD 2 H14D H 0.7284(28) 0.1512(45) 0.2624(35) 0.087 Uiso 0.460(7) calc PR 2 H14E H 0.8239(80) 0.0778(9) 0.2487(40) 0.087 Uiso 0.460(7) calc PR 2 H14F H 0.8660(53) 0.1545(39) 0.1910(16) 0.087 Uiso 0.460(7) calc PR 2 C15B C 0.9150(19) 0.1368(12) 0.6007(11) 0.064(6) Uani 0.460(7) d PD 2 C16B C 0.8134(24) 0.1316(13) 0.6963(15) 0.078(8) Uani 0.460(7) d PD 2 H16D H 0.7341(88) 0.1657(69) 0.6855(59) 0.117 Uiso 0.460(7) calc PR 2 H16E H 0.8634(51) 0.1459(85) 0.7603(23) 0.117 Uiso 0.460(7) calc PR 2 H16F H 0.7790(130) 0.0798(25) 0.7031(76) 0.117 Uiso 0.460(7) calc PR 2 C17B C 1.0382(28) 0.0791(22) 0.6103(21) 0.209(25) Uani 0.460(7) d PD 2 H17D H 1.1269(44) 0.1064(22) 0.6170(244) 0.314 Uiso 0.460(7) calc PR 2 H17E H 1.0409(203) 0.0473(117) 0.5477(110) 0.314 Uiso 0.460(7) calc PR 2 H17F H 1.0239(170) 0.0475(117) 0.6723(138) 0.314 Uiso 0.460(7) calc PR 2 C18B C 0.9763(27) 0.2205(15) 0.6035(18) 0.140(13) Uani 0.460(7) d PD 2 H18D H 1.0061(147) 0.2327(34) 0.6749(29) 0.210 Uiso 0.460(7) calc PR 2 H18E H 0.9037(50) 0.2560(16) 0.5812(110) 0.210 Uiso 0.460(7) calc PR 2 H18F H 1.0567(94) 0.2240(25) 0.5561(88) 0.210 Uiso 0.460(7) calc PR 2 C10B C 0.7921(10) 0.0236(4) 0.4521(11) 0.048(3) Uani 0.460(7) d PD 2 H10C H 0.7628(10) 0.0160(4) 0.3785(11) 0.058 Uiso 0.460(7) calc PR 2 H10D H 0.8883(10) 0.0033(4) 0.4585(11) 0.058 Uiso 0.460(7) calc PR 2 P2B P 0.6747(4) -0.0370(2) 0.5365(2) 0.0537(14) Uani 0.460(7) d PD 2 C21B C 0.7163(20) -0.1354(7) 0.4857(15) 0.091(11) Uani 0.460(7) d PD 2 C22B C 0.8808(17) -0.1465(9) 0.4871(26) 0.098(8) Uani 0.460(7) d PD 2 H22D H 0.9178(31) -0.1311(108) 0.5554(57) 0.147 Uiso 0.460(7) calc PR 2 H22E H 0.9233(25) -0.1156(89) 0.4320(103) 0.147 Uiso 0.460(7) calc PR 2 H22F H 0.9031(18) -0.1996(22) 0.4747(165) 0.147 Uiso 0.460(7) calc PR 2 C23B C 0.6527(25) -0.1968(8) 0.5597(15) 0.118(7) Uani 0.460(7) d PD 2 H23D H 0.5505(25) -0.1969(49) 0.5528(74) 0.176 Uiso 0.460(7) calc PR 2 H23E H 0.6783(117) -0.1856(41) 0.6324(19) 0.176 Uiso 0.460(7) calc PR 2 H23F H 0.6895(103) -0.2464(12) 0.5402(67) 0.176 Uiso 0.460(7) calc PR 2 C24B C 0.6694(29) -0.1530(13) 0.3688(16) 0.152(13) Uani 0.460(7) d PD 2 H24D H 0.7134(187) -0.1999(65) 0.3453(63) 0.228 Uiso 0.460(7) calc PR 2 H24E H 0.6985(204) -0.1115(59) 0.3230(32) 0.228 Uiso 0.460(7) calc PR 2 H24F H 0.5673(36) -0.1583(125) 0.3660(35) 0.228 Uiso 0.460(7) calc PR 2 C25B C 0.4898(12) -0.0072(9) 0.4939(13) 0.054(4) Uani 0.460(7) d PD 2 C26B C 0.4754(17) 0.0135(14) 0.3746(11) 0.102(7) Uani 0.460(7) d PD 2 H26D H 0.3769(23) 0.0099(62) 0.3536(24) 0.153 Uiso 0.460(7) calc PR 2 H26E H 0.5313(91) -0.0216(38) 0.3326(13) 0.153 Uiso 0.460(7) calc PR 2 H26F H 0.5089(106) 0.0650(24) 0.3631(18) 0.153 Uiso 0.460(7) calc PR 2 C27B C 0.4496(13) 0.0628(9) 0.5617(12) 0.079(4) Uani 0.460(7) d PD 2 H27D H 0.5252(55) 0.1001(29) 0.5586(74) 0.118 Uiso 0.460(7) calc PR 2 H27E H 0.4352(118) 0.0471(14) 0.6345(21) 0.118 Uiso 0.460(7) calc PR 2 H27F H 0.3631(67) 0.0852(40) 0.5345(56) 0.118 Uiso 0.460(7) calc PR 2 C28B C 0.3811(18) -0.0713(10) 0.5190(21) 0.116(9) Uani 0.460(7) d PD 2 H28D H 0.4090(123) -0.0975(79) 0.5832(95) 0.174 Uiso 0.460(7) calc PR 2 H28E H 0.3784(166) -0.1073(66) 0.4608(78) 0.174 Uiso 0.460(7) calc PR 2 H28F H 0.2880(43) -0.0491(17) 0.5286(167) 0.174 Uiso 0.460(7) calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1A 0.066(3) 0.098(3) 0.102(5) 0.007(2) 0.014(2) 0.002(2) C11A 0.081(10) 0.063(9) 0.100(11) 0.025(7) 0.013(8) 0.002(8) C12A 0.239(21) 0.062(9) 0.109(11) -0.016(9) 0.067(14) -0.054(12) C13A 0.092(9) 0.090(8) 0.111(11) -0.006(7) 0.028(8) -0.003(7) C14A 0.133(18) 0.122(19) 0.083(11) 0.019(9) 0.033(10) -0.028(10) C15A 0.053(10) 0.081(12) 0.087(13) -0.013(10) -0.007(9) -0.023(8) C16A 0.112(20) 0.197(30) 0.121(18) 0.002(15) 0.034(13) -0.029(16) C17A 0.095(14) 0.282(35) 0.096(13) -0.028(16) 0.010(10) 0.061(16) C18A 0.160(22) 0.126(16) 0.116(15) -0.048(12) 0.061(14) -0.085(16) C10A 0.068(6) 0.077(7) 0.067(7) 0.006(7) 0.027(6) 0.000(5) P2A 0.067(2) 0.064(2) 0.069(3) -0.003(2) -0.0116(15) -0.007(2) C21A 0.105(20) 0.036(9) 0.105(22) 0.009(10) 0.022(13) -0.005(8) C22A 0.123(15) 0.103(13) 0.277(31) -0.026(27) -0.008(32) 0.067(10) C23A 0.134(15) 0.067(11) 0.122(17) 0.026(10) -0.012(12) -0.014(9) C24A 0.153(19) 0.102(16) 0.290(34) -0.083(18) -0.032(18) -0.005(14) C25A 0.059(10) 0.107(11) 0.074(13) -0.006(9) -0.016(6) -0.003(8) C26A 0.089(12) 0.141(17) 0.188(21) 0.055(15) -0.035(11) 0.044(10) C27A 0.054(7) 0.093(11) 0.126(14) 0.003(9) -0.006(6) 0.003(7) C28A 0.057(8) 0.173(16) 0.167(15) -0.025(14) 0.008(9) -0.052(9) P1B 0.0284(13) 0.0202(10) 0.058(2) 0.0024(15) 0.000(2) 0.0007(9) C11B 0.050(9) 0.066(12) 0.071(9) 0.021(8) 0.003(7) 0.008(7) C12B 0.095(12) 0.044(7) 0.117(13) 0.019(8) -0.011(10) -0.030(7) C13B 0.042(7) 0.094(11) 0.141(14) 0.044(8) 0.033(8) 0.002(6) C14B 0.064(8) 0.038(6) 0.072(11) 0.009(6) 0.007(8) -0.016(6) C15B 0.056(12) 0.086(13) 0.051(10) 0.013(8) 0.005(8) 0.013(10) C16B 0.099(17) 0.081(13) 0.054(9) -0.004(8) 0.002(8) 0.028(11) C17B 0.161(24) 0.360(54) 0.107(16) -0.033(23) -0.068(15) 0.197(32) C18B 0.094(15) 0.237(31) 0.090(13) -0.065(15) -0.013(13) -0.074(16) C10B 0.042(5) 0.038(5) 0.065(8) -0.002(6) 0.034(6) -0.004(4) P2B 0.057(2) 0.048(2) 0.057(3) 0.003(2) -0.0078(14) -0.010(2) C21B 0.086(15) 0.073(17) 0.114(20) -0.010(12) -0.022(13) -0.003(10) C22B 0.101(13) 0.041(6) 0.151(18) 0.016(13) -0.014(17) 0.001(7) C23B 0.181(19) 0.038(8) 0.134(17) 0.019(8) -0.028(14) -0.030(9) C24B 0.163(23) 0.119(18) 0.175(25) -0.102(17) -0.028(19) 0.057(17) C25B 0.044(8) 0.069(8) 0.050(9) -0.009(7) 0.008(6) -0.020(6) C26B 0.052(8) 0.165(22) 0.089(11) 0.038(12) -0.036(7) -0.013(11) C27B 0.046(7) 0.086(10) 0.104(11) -0.012(8) 0.013(6) -0.012(7) C28B 0.096(13) 0.097(10) 0.155(22) -0.017(12) 0.056(15) -0.036(9) _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 P1A C10A 1.832(9) . ? P1A C11A 1.874(13) . ? P1A C15A 1.890(13) . ? C11A C14A 1.559(15) . ? C11A C12A 1.534(13) . ? C11A C13A 1.554(14) . ? C15A C16A 1.563(15) . ? C15A C18A 1.537(15) . ? C15A C17A 1.549(15) . ? C10A P2A 1.834(9) . ? P2A C25A 1.881(12) . ? P2A C21A 1.902(11) . ? C21A C24A 1.531(14) . ? C21A C23A 1.54(2) . ? C21A C22A 1.562(14) . ? C25A C28A 1.524(13) . ? C25A C26A 1.551(15) . ? C25A C27A 1.54(2) . ? P1B C10B 1.849(8) . ? P1B C11B 1.917(13) . ? P1B C15B 1.898(13) . ? C11B C13B 1.531(14) . ? C11B C12B 1.540(13) . ? C11B C14B 1.529(14) . ? C15B C17B 1.533(15) . ? C15B C16B 1.530(15) . ? C15B C18B 1.56(2) . ? C10B P2B 1.852(9) . ? P2B C21B 1.865(13) . ? P2B C25B 1.883(12) . ? C21B C23B 1.534(15) . ? C21B C24B 1.56(2) . ? C21B C22B 1.552(14) . ? C25B C27B 1.531(14) . ? C25B C26B 1.541(14) . ? C25B C28B 1.542(13) . ? 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 C10A P1A C11A 103.0(6) . . ? C10A P1A C15A 97.5(8) . . ? C11A P1A C15A 109.1(7) . . ? C14A C11A C12A 105.7(12) . . ? C14A C11A C13A 105.6(13) . . ? C12A C11A C13A 109.3(11) . . ? C14A C11A P1A 103.5(11) . . ? C12A C11A P1A 112.5(11) . . ? C13A C11A P1A 119.0(9) . . ? C16A C15A C18A 107.0(14) . . ? C16A C15A C17A 105.4(14) . . ? C18A C15A C17A 110.5(13) . . ? C16A C15A P1A 106.1(12) . . ? C18A C15A P1A 111.5(12) . . ? C17A C15A P1A 115.6(12) . . ? P1A C10A P2A 118.4(7) . . ? C10A P2A C25A 104.1(6) . . ? C10A P2A C21A 99.7(6) . . ? C25A P2A C21A 110.5(7) . . ? C24A C21A C23A 110.1(12) . . ? C24A C21A C22A 109.1(14) . . ? C23A C21A C22A 106.3(15) . . ? C24A C21A P2A 109.0(12) . . ? C23A C21A P2A 115.9(10) . . ? C22A C21A P2A 106.1(10) . . ? C28A C25A C26A 110.8(13) . . ? C28A C25A C27A 108.8(12) . . ? C26A C25A C27A 105.4(12) . . ? C28A C25A P2A 112.1(10) . . ? C26A C25A P2A 104.1(10) . . ? C27A C25A P2A 115.4(10) . . ? C10B P1B C11B 99.1(6) . . ? C10B P1B C15B 103.5(7) . . ? C11B P1B C15B 110.5(6) . . ? C13B C11B C12B 109.3(11) . . ? C13B C11B C14B 110.9(13) . . ? C12B C11B C14B 109.0(12) . . ? C13B C11B P1B 113.9(9) . . ? C12B C11B P1B 107.3(10) . . ? C14B C11B P1B 106.3(11) . . ? C17B C15B C16B 111.5(14) . . ? C17B C15B C18B 109.3(16) . . ? C16B C15B C18B 105.4(14) . . ? C17B C15B P1B 115.5(12) . . ? C16B C15B P1B 107.5(12) . . ? C18B C15B P1B 107.0(10) . . ? P2B C10B P1B 120.4(6) . . ? C10B P2B C21B 101.8(6) . . ? C10B P2B C25B 103.1(6) . . ? C21B P2B C25B 110.3(8) . . ? C23B C21B C24B 108.7(13) . . ? C23B C21B C22B 106.9(13) . . ? C24B C21B C22B 105.4(15) . . ? C23B C21B P2B 110.6(12) . . ? C24B C21B P2B 116.2(11) . . ? C22B C21B P2B 108.5(10) . . ? C27B C25B C26B 109.2(13) . . ? C27B C25B C28B 107.4(11) . . ? C26B C25B C28B 107.9(12) . . ? C27B C25B P2B 106.8(9) . . ? C26B C25B P2B 114.8(10) . . ? C28B C25B P2B 110.5(11) . . ? _refine_diff_density_max 0.410 _refine_diff_density_min -0.146 _refine_diff_density_rms 0.026 #===END data_1312_dcpm_2 _database_code_CSD 199934 _chemical_name_systematic ; ? ; _chemical_name_common dcpm _chemical_melting_point ? _chemical_compound_source 'see paper' _chemical_formula_moiety 'C25 H46 P2' _chemical_formula_sum 'C25 H46 P2' _chemical_formula_weight 408.56 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' P P 0.1023 0.0942 '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 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.718(2) _cell_length_b 10.423(2) _cell_length_c 12.7750(10) _cell_angle_alpha 98.210(10) _cell_angle_beta 96.840(10) _cell_angle_gamma 105.230(10) _cell_volume 1219.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 75 _cell_measurement_theta_min 9.09 _cell_measurement_theta_max 25.83 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method none _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 0.186 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min 0 _exptl_absorpt_correction_T_max 0 _diffrn_ambient_temperature 100 _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 CAD4' _diffrn_measurement_method '\w-2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 5.66 _diffrn_reflns_number 31999 _diffrn_reflns_av_R_equivalents 0.0868 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5611 _reflns_number_gt 4742 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'EXPRESS / CAD4 software (Enraf-Nonius, 1995)' _computing_cell_refinement 'EXPRESS / CAD4 software (Enraf-Nonius, 1995)' _computing_data_reduction 'DATAP (Coppens,Leiserowitz & Rabinovich, 1965)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _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^)+(0.0897P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 5611 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1294 _refine_ls_goodness_of_fit_ref 1.182 _refine_ls_restrained_S_all 1.182 _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 0.66553(18) 0.91821(16) 0.31097(12) 0.0168(3) Uani 1 1 d . . . C2 C 0.40379(17) 0.72277(15) 0.34513(12) 0.0153(3) Uani 1 1 d . . . C3 C 0.36277(17) 0.84231(16) 0.40329(13) 0.0190(3) Uani 1 1 d . . . C4 C 0.20029(19) 0.80663(19) 0.40656(14) 0.0236(4) Uani 1 1 d . . . C5 C 0.11371(19) 0.76039(18) 0.29355(14) 0.0240(4) Uani 1 1 d . . . C6 C 0.15225(18) 0.64021(17) 0.23434(14) 0.0218(4) Uani 1 1 d . . . C7 C 0.31423(18) 0.67331(17) 0.23213(13) 0.0186(3) Uani 1 1 d . . . C8 C 0.68259(16) 0.78565(15) 0.48508(12) 0.0142(3) Uani 1 1 d . . . C9 C 0.84564(17) 0.80678(19) 0.49349(13) 0.0204(3) Uani 1 1 d . . . C10 C 0.92209(19) 0.8331(2) 0.60940(14) 0.0258(4) Uani 1 1 d . . . C11 C 0.8568(2) 0.7200(2) 0.66734(15) 0.0272(4) Uani 1 1 d . . . C12 C 0.6951(2) 0.6994(2) 0.66125(14) 0.0248(4) Uani 1 1 d . . . C13 C 0.61839(18) 0.67332(17) 0.54559(13) 0.0192(3) Uani 1 1 d . . . C14 C 0.71145(17) 1.13683(15) 0.20057(12) 0.0138(3) Uani 1 1 d . . . C15 C 0.70826(19) 1.18941(16) 0.09460(13) 0.0193(3) Uani 1 1 d . . . C16 C 0.7940(2) 1.33872(17) 0.10941(15) 0.0232(4) Uani 1 1 d . . . C17 C 0.7427(2) 1.42703(17) 0.19280(15) 0.0246(4) Uani 1 1 d . . . C18 C 0.7470(2) 1.37605(17) 0.29875(15) 0.0271(4) Uani 1 1 d . . . C19 C 0.6592(2) 1.22768(17) 0.28289(15) 0.0255(4) Uani 1 1 d . . . C20 C 0.68471(17) 0.87026(15) 0.08270(12) 0.0151(3) Uani 1 1 d . . . C21 C 0.84821(18) 0.89456(17) 0.10929(14) 0.0214(4) Uani 1 1 d . . . C22 C 0.9051(2) 0.82625(18) 0.01647(16) 0.0263(4) Uani 1 1 d . . . C23 C 0.8278(2) 0.67454(18) -0.01279(16) 0.0268(4) Uani 1 1 d . . . C24 C 0.6647(2) 0.64883(17) -0.03628(14) 0.0229(4) Uani 1 1 d . . . C25 C 0.60870(18) 0.71748(15) 0.05638(12) 0.0161(3) Uani 1 1 d . . . H1A H 0.772(2) 0.932(2) 0.3171(18) 0.036(6) Uiso 1 1 d . . . H1B H 0.643(2) 0.986(2) 0.3717(16) 0.027(5) Uiso 1 1 d . . . H2 H 0.380(2) 0.647(2) 0.3857(16) 0.025(5) Uiso 1 1 d . . . H3A H 0.420(2) 0.873(2) 0.4764(17) 0.024(5) Uiso 1 1 d . . . H3B H 0.386(2) 0.9170(19) 0.3622(15) 0.020(5) Uiso 1 1 d . . . H4A H 0.176(2) 0.737(2) 0.4471(16) 0.025(5) Uiso 1 1 d . . . H4B H 0.176(2) 0.883(2) 0.4432(17) 0.032(5) Uiso 1 1 d . . . H5A H 0.014(2) 0.735(2) 0.2985(16) 0.027(5) Uiso 1 1 d . . . H5B H 0.132(2) 0.836(2) 0.2508(16) 0.027(5) Uiso 1 1 d . . . H6A H 0.101(2) 0.610(2) 0.1586(17) 0.024(5) Uiso 1 1 d . . . H6B H 0.120(2) 0.569(2) 0.2733(17) 0.030(5) Uiso 1 1 d . . . H7A H 0.337(2) 0.7397(19) 0.1907(15) 0.020(5) Uiso 1 1 d . . . H7B H 0.340(2) 0.594(2) 0.2013(15) 0.020(5) Uiso 1 1 d . . . H8 H 0.670(2) 0.868(2) 0.5176(16) 0.022(5) Uiso 1 1 d . . . H9A H 0.890(2) 0.884(2) 0.4620(16) 0.023(5) Uiso 1 1 d . . . H9B H 0.861(2) 0.727(2) 0.4583(16) 0.026(5) Uiso 1 1 d . . . H10A H 1.022(3) 0.846(2) 0.6112(18) 0.038(6) Uiso 1 1 d . . . H10B H 0.914(2) 0.918(2) 0.6479(18) 0.039(6) Uiso 1 1 d . . . H11A H 0.877(2) 0.638(2) 0.6362(18) 0.036(6) Uiso 1 1 d . . . H11B H 0.906(3) 0.741(2) 0.740(2) 0.043(6) Uiso 1 1 d . . . H12A H 0.650(2) 0.627(2) 0.6984(17) 0.033(5) Uiso 1 1 d . . . H12B H 0.682(2) 0.786(2) 0.6971(16) 0.026(5) Uiso 1 1 d . . . H13A H 0.520(2) 0.664(2) 0.5453(16) 0.031(5) Uiso 1 1 d . . . H13B H 0.626(2) 0.584(2) 0.5088(16) 0.023(5) Uiso 1 1 d . . . H14 H 0.806(2) 1.1395(18) 0.2275(15) 0.017(4) Uiso 1 1 d . . . H15A H 0.749(2) 1.138(2) 0.0456(17) 0.029(5) Uiso 1 1 d . . . H15B H 0.609(2) 1.1818(19) 0.0646(16) 0.022(5) Uiso 1 1 d . . . H16A H 0.886(2) 1.3429(18) 0.1365(15) 0.015(4) Uiso 1 1 d . . . H16B H 0.792(2) 1.368(2) 0.0440(18) 0.030(5) Uiso 1 1 d . . . H17A H 0.652(2) 1.431(2) 0.1643(17) 0.029(5) Uiso 1 1 d . . . H17B H 0.807(2) 1.518(2) 0.2025(18) 0.039(6) Uiso 1 1 d . . . H18A H 0.712(2) 1.434(2) 0.3521(18) 0.041(6) Uiso 1 1 d . . . H18B H 0.851(2) 1.385(2) 0.3317(18) 0.035(6) Uiso 1 1 d . . . H19A H 0.661(3) 1.195(3) 0.351(2) 0.048(7) Uiso 1 1 d . . . H19B H 0.557(2) 1.2185(18) 0.2492(15) 0.019(5) Uiso 1 1 d . . . H20 H 0.6676(18) 0.9076(18) 0.0160(14) 0.012(4) Uiso 1 1 d . . . H21A H 0.868(2) 0.853(2) 0.1729(16) 0.025(5) Uiso 1 1 d . . . H21B H 0.900(2) 0.990(2) 0.1280(16) 0.028(5) Uiso 1 1 d . . . H22A H 0.997(2) 0.840(2) 0.0353(16) 0.024(5) Uiso 1 1 d . . . H22B H 0.892(2) 0.870(2) -0.0471(19) 0.038(6) Uiso 1 1 d . . . H23A H 0.856(2) 0.632(2) 0.0451(18) 0.029(5) Uiso 1 1 d . . . H23B H 0.864(2) 0.6312(19) -0.0775(16) 0.023(5) Uiso 1 1 d . . . H24A H 0.615(2) 0.551(2) -0.0564(17) 0.030(5) Uiso 1 1 d . . . H24B H 0.641(2) 0.681(2) -0.1027(19) 0.039(6) Uiso 1 1 d . . . H25A H 0.6246(18) 0.6787(17) 0.1173(14) 0.011(4) Uiso 1 1 d . . . H25B H 0.503(2) 0.6990(18) 0.0396(15) 0.018(4) Uiso 1 1 d . . . P1 P 0.59952(4) 0.74492(4) 0.34025(3) 0.01377(13) Uani 1 1 d . . . P2 P 0.59720(4) 0.95828(4) 0.18099(3) 0.01366(13) 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 0.0204(8) 0.0162(7) 0.0119(7) 0.0032(6) 0.0020(6) 0.0022(6) C2 0.0187(7) 0.0138(7) 0.0119(7) 0.0020(6) 0.0017(6) 0.0027(6) C3 0.0198(8) 0.0179(8) 0.0166(8) -0.0022(6) 0.0021(6) 0.0042(6) C4 0.0233(8) 0.0245(9) 0.0220(9) -0.0027(7) 0.0052(7) 0.0079(7) C5 0.0201(8) 0.0262(9) 0.0244(9) 0.0011(7) 0.0006(7) 0.0075(7) C6 0.0208(8) 0.0205(8) 0.0190(8) -0.0004(7) -0.0015(7) 0.0011(7) C7 0.0211(8) 0.0175(8) 0.0140(8) -0.0014(6) 0.0003(6) 0.0033(6) C8 0.0195(7) 0.0118(7) 0.0114(7) 0.0023(6) 0.0027(6) 0.0043(6) C9 0.0176(8) 0.0260(9) 0.0178(8) 0.0093(7) 0.0022(6) 0.0038(7) C10 0.0198(8) 0.0347(10) 0.0214(9) 0.0099(8) -0.0020(7) 0.0049(8) C11 0.0288(9) 0.0378(11) 0.0192(9) 0.0138(8) 0.0019(7) 0.0127(8) C12 0.0283(9) 0.0308(10) 0.0158(8) 0.0115(7) 0.0042(7) 0.0053(8) C13 0.0211(8) 0.0198(8) 0.0159(8) 0.0074(6) 0.0028(6) 0.0021(7) C14 0.0165(7) 0.0115(7) 0.0135(7) 0.0031(6) 0.0017(6) 0.0042(6) C15 0.0276(9) 0.0146(7) 0.0154(8) 0.0058(6) 0.0022(7) 0.0044(7) C16 0.0309(10) 0.0167(8) 0.0212(9) 0.0069(7) 0.0047(7) 0.0030(7) C17 0.0300(9) 0.0136(8) 0.0312(10) 0.0049(7) 0.0053(8) 0.0072(7) C18 0.0405(11) 0.0164(8) 0.0242(9) -0.0009(7) 0.0095(8) 0.0086(8) C19 0.0406(11) 0.0154(8) 0.0232(9) 0.0028(7) 0.0154(8) 0.0086(7) C20 0.0194(8) 0.0138(7) 0.0122(7) 0.0026(6) 0.0030(6) 0.0048(6) C21 0.0201(8) 0.0181(8) 0.0247(9) 0.0008(7) 0.0048(7) 0.0041(7) C22 0.0241(9) 0.0210(9) 0.0352(10) 0.0027(8) 0.0140(8) 0.0058(7) C23 0.0361(10) 0.0188(8) 0.0299(10) 0.0036(7) 0.0168(8) 0.0107(7) C24 0.0338(9) 0.0150(8) 0.0178(8) -0.0008(6) 0.0082(7) 0.0037(7) C25 0.0218(8) 0.0135(7) 0.0124(7) 0.0025(6) 0.0031(6) 0.0037(6) P1 0.0178(2) 0.0124(2) 0.0111(2) 0.00212(15) 0.00235(15) 0.00410(16) P2 0.0168(2) 0.0124(2) 0.0120(2) 0.00287(15) 0.00167(15) 0.00426(16) _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 P2 1.8584(16) . ? C1 P1 1.8588(16) . ? C1 H1A 0.99(2) . ? C1 H1B 1.05(2) . ? C2 C3 1.527(2) . ? C2 C7 1.536(2) . ? C2 P1 1.8647(16) . ? C2 H2 1.00(2) . ? C3 C4 1.531(2) . ? C3 H3A 0.99(2) . ? C3 H3B 0.99(2) . ? C4 C5 1.524(2) . ? C4 H4A 0.94(2) . ? C4 H4B 0.96(2) . ? C5 C6 1.525(2) . ? C5 H5A 0.95(2) . ? C5 H5B 1.01(2) . ? C6 C7 1.525(2) . ? C6 H6A 1.00(2) . ? C6 H6B 0.95(2) . ? C7 H7A 0.93(2) . ? C7 H7B 0.97(2) . ? C8 C9 1.530(2) . ? C8 C13 1.532(2) . ? C8 P1 1.8694(15) . ? C8 H8 0.94(2) . ? C9 C10 1.528(2) . ? C9 H9A 0.97(2) . ? C9 H9B 0.94(2) . ? C10 C11 1.519(3) . ? C10 H10A 0.94(2) . ? C10 H10B 0.97(2) . ? C11 C12 1.520(3) . ? C11 H11A 0.97(2) . ? C11 H11B 0.95(2) . ? C12 C13 1.526(2) . ? C12 H12A 0.98(2) . ? C12 H12B 1.00(2) . ? C13 H13A 0.94(2) . ? C13 H13B 1.01(2) . ? C14 C15 1.531(2) . ? C14 C19 1.535(2) . ? C14 P2 1.8638(15) . ? C14 H14 0.929(19) . ? C15 C16 1.533(2) . ? C15 H15A 0.95(2) . ? C15 H15B 0.97(2) . ? C16 C17 1.522(3) . ? C16 H16A 0.911(19) . ? C16 H16B 0.93(2) . ? C17 C18 1.523(3) . ? C17 H17A 0.92(2) . ? C17 H17B 0.97(2) . ? C18 C19 1.528(2) . ? C18 H18A 1.00(2) . ? C18 H18B 1.02(2) . ? C19 H19A 0.97(3) . ? C19 H19B 1.009(19) . ? C20 C21 1.530(2) . ? C20 C25 1.538(2) . ? C20 P2 1.8647(16) . ? C20 H20 1.001(18) . ? C21 C22 1.530(2) . ? C21 H21A 1.00(2) . ? C21 H21B 0.97(2) . ? C22 C23 1.531(2) . ? C22 H22A 0.86(2) . ? C22 H22B 1.00(2) . ? C23 C24 1.521(3) . ? C23 H23A 0.96(2) . ? C23 H23B 1.03(2) . ? C24 C25 1.525(2) . ? C24 H24A 0.99(2) . ? C24 H24B 0.98(2) . ? C25 H25A 0.942(18) . ? C25 H25B 0.981(19) . ? 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 P2 C1 P1 120.29(8) . . ? P2 C1 H1A 109.0(13) . . ? P1 C1 H1A 102.7(13) . . ? P2 C1 H1B 106.7(11) . . ? P1 C1 H1B 107.8(11) . . ? H1A C1 H1B 110.2(17) . . ? C3 C2 C7 110.39(13) . . ? C3 C2 P1 117.17(11) . . ? C7 C2 P1 110.66(11) . . ? C3 C2 H2 108.3(11) . . ? C7 C2 H2 107.7(11) . . ? P1 C2 H2 101.9(11) . . ? C2 C3 C4 111.29(13) . . ? C2 C3 H3A 109.9(11) . . ? C4 C3 H3A 111.1(11) . . ? C2 C3 H3B 107.9(11) . . ? C4 C3 H3B 107.4(11) . . ? H3A C3 H3B 109.2(15) . . ? C5 C4 C3 110.68(14) . . ? C5 C4 H4A 110.0(12) . . ? C3 C4 H4A 108.9(12) . . ? C5 C4 H4B 110.5(13) . . ? C3 C4 H4B 110.3(13) . . ? H4A C4 H4B 106.3(17) . . ? C4 C5 C6 110.91(15) . . ? C4 C5 H5A 108.6(12) . . ? C6 C5 H5A 109.5(12) . . ? C4 C5 H5B 111.3(11) . . ? C6 C5 H5B 108.9(12) . . ? H5A C5 H5B 107.6(17) . . ? C5 C6 C7 111.13(14) . . ? C5 C6 H6A 113.2(12) . . ? C7 C6 H6A 107.8(11) . . ? C5 C6 H6B 104.3(12) . . ? C7 C6 H6B 112.1(13) . . ? H6A C6 H6B 108.3(16) . . ? C6 C7 C2 112.02(13) . . ? C6 C7 H7A 107.5(12) . . ? C2 C7 H7A 110.1(12) . . ? C6 C7 H7B 111.1(11) . . ? C2 C7 H7B 106.5(11) . . ? H7A C7 H7B 109.8(16) . . ? C9 C8 C13 109.55(13) . . ? C9 C8 P1 108.85(10) . . ? C13 C8 P1 112.00(11) . . ? C9 C8 H8 106.5(12) . . ? C13 C8 H8 109.7(12) . . ? P1 C8 H8 110.1(12) . . ? C10 C9 C8 112.65(14) . . ? C10 C9 H9A 107.2(12) . . ? C8 C9 H9A 110.7(12) . . ? C10 C9 H9B 107.2(12) . . ? C8 C9 H9B 108.2(12) . . ? H9A C9 H9B 110.9(17) . . ? C11 C10 C9 111.32(15) . . ? C11 C10 H10A 111.6(14) . . ? C9 C10 H10A 110.1(14) . . ? C11 C10 H10B 108.6(14) . . ? C9 C10 H10B 110.0(14) . . ? H10A C10 H10B 105.1(19) . . ? C10 C11 C12 110.57(15) . . ? C10 C11 H11A 109.1(14) . . ? C12 C11 H11A 111.3(13) . . ? C10 C11 H11B 108.7(14) . . ? C12 C11 H11B 111.7(14) . . ? H11A C11 H11B 105.3(19) . . ? C11 C12 C13 111.71(15) . . ? C11 C12 H12A 112.3(13) . . ? C13 C12 H12A 110.4(13) . . ? C11 C12 H12B 107.0(12) . . ? C13 C12 H12B 106.6(11) . . ? H12A C12 H12B 108.5(16) . . ? C12 C13 C8 112.39(14) . . ? C12 C13 H13A 109.1(13) . . ? C8 C13 H13A 110.3(13) . . ? C12 C13 H13B 107.8(11) . . ? C8 C13 H13B 110.3(11) . . ? H13A C13 H13B 106.6(17) . . ? C15 C14 C19 109.52(13) . . ? C15 C14 P2 110.99(11) . . ? C19 C14 P2 110.39(11) . . ? C15 C14 H14 109.8(12) . . ? C19 C14 H14 108.2(11) . . ? P2 C14 H14 107.9(11) . . ? C14 C15 C16 112.15(14) . . ? C14 C15 H15A 109.4(13) . . ? C16 C15 H15A 108.6(12) . . ? C14 C15 H15B 109.7(12) . . ? C16 C15 H15B 107.2(11) . . ? H15A C15 H15B 109.8(16) . . ? C17 C16 C15 111.77(15) . . ? C17 C16 H16A 106.6(11) . . ? C15 C16 H16A 105.5(11) . . ? C17 C16 H16B 112.5(13) . . ? C15 C16 H16B 110.7(13) . . ? H16A C16 H16B 109.5(17) . . ? C16 C17 C18 111.00(14) . . ? C16 C17 H17A 108.1(13) . . ? C18 C17 H17A 113.7(13) . . ? C16 C17 H17B 107.0(13) . . ? C18 C17 H17B 110.1(14) . . ? H17A C17 H17B 106.7(18) . . ? C17 C18 C19 110.94(15) . . ? C17 C18 H18A 110.0(13) . . ? C19 C18 H18A 111.4(13) . . ? C17 C18 H18B 110.7(13) . . ? C19 C18 H18B 108.8(12) . . ? H18A C18 H18B 104.9(17) . . ? C18 C19 C14 112.15(14) . . ? C18 C19 H19A 111.1(15) . . ? C14 C19 H19A 110.0(15) . . ? C18 C19 H19B 108.6(11) . . ? C14 C19 H19B 103.7(10) . . ? H19A C19 H19B 111.1(19) . . ? C21 C20 C25 109.74(13) . . ? C21 C20 P2 117.38(11) . . ? C25 C20 P2 110.98(10) . . ? C21 C20 H20 106.2(10) . . ? C25 C20 H20 107.4(10) . . ? P2 C20 H20 104.4(10) . . ? C20 C21 C22 110.92(14) . . ? C20 C21 H21A 107.8(11) . . ? C22 C21 H21A 107.8(11) . . ? C20 C21 H21B 112.1(12) . . ? C22 C21 H21B 110.4(12) . . ? H21A C21 H21B 107.6(16) . . ? C21 C22 C23 111.40(15) . . ? C21 C22 H22A 108.0(14) . . ? C23 C22 H22A 110.9(14) . . ? C21 C22 H22B 109.3(13) . . ? C23 C22 H22B 110.0(13) . . ? H22A C22 H22B 107.2(19) . . ? C24 C23 C22 111.05(15) . . ? C24 C23 H23A 111.6(13) . . ? C22 C23 H23A 108.4(13) . . ? C24 C23 H23B 110.4(11) . . ? C22 C23 H23B 110.3(11) . . ? H23A C23 H23B 104.9(16) . . ? C23 C24 C25 111.63(14) . . ? C23 C24 H24A 110.9(12) . . ? C25 C24 H24A 112.5(12) . . ? C23 C24 H24B 108.2(13) . . ? C25 C24 H24B 111.4(13) . . ? H24A C24 H24B 101.8(18) . . ? C24 C25 C20 110.95(13) . . ? C24 C25 H25A 109.5(10) . . ? C20 C25 H25A 109.6(10) . . ? C24 C25 H25B 110.1(11) . . ? C20 C25 H25B 111.4(11) . . ? H25A C25 H25B 105.1(15) . . ? C1 P1 C2 103.97(7) . . ? C1 P1 C8 96.98(7) . . ? C2 P1 C8 103.04(7) . . ? C1 P2 C14 98.19(7) . . ? C1 P2 C20 103.52(7) . . ? C14 P2 C20 101.93(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.592 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.069 #===END data_ig5_ctbpm_3 _database_code_CSD 199935 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ctbpm _chemical_melting_point ? _chemical_formula_moiety 'C21 H42 P2' _chemical_formula_sum 'C21 H42 P2' _chemical_formula_weight 356.49 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' 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 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 11.1753(5) _cell_length_b 9.8062(4) _cell_length_c 20.3041(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.6330(10) _cell_angle_gamma 90.00 _cell_volume 2217.80(16) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max .20 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 18216 _diffrn_reflns_av_R_equivalents 0.1198 _diffrn_reflns_av_sigmaI/netI 0.0886 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3913 _reflns_number_gt 2341 _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^)+(0.0441P)^2^+0.3229P] 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 3913 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _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 0.66130(7) 0.41331(8) 0.15699(4) 0.0326(2) Uani 1 1 d . . . P2 P 0.39165(7) 0.38333(8) 0.20090(4) 0.0316(2) Uani 1 1 d . . . C1 C 0.6421(2) 0.5957(3) 0.13228(13) 0.0319(7) Uani 1 1 d . . . H1 H 0.7240 0.6293 0.1239 0.038 Uiso 1 1 calc R . . C2 C 0.6023(3) 0.6816(3) 0.18996(16) 0.0450(9) Uani 1 1 d . . . H2A H 0.5216 0.6515 0.2007 0.054 Uiso 1 1 calc R . . H2B H 0.6587 0.6663 0.2294 0.054 Uiso 1 1 calc R . . C3 C 0.5985(3) 0.8329(3) 0.17366(18) 0.0546(10) Uani 1 1 d . . . H3A H 0.6809 0.8657 0.1681 0.065 Uiso 1 1 calc R . . H3B H 0.5676 0.8838 0.2108 0.065 Uiso 1 1 calc R . . C4 C 0.5191(3) 0.8614(3) 0.1108(2) 0.0589(11) Uani 1 1 d . . . H4A H 0.4350 0.8372 0.1177 0.071 Uiso 1 1 calc R . . H4B H 0.5218 0.9599 0.1003 0.071 Uiso 1 1 calc R . . C5 C 0.5606(3) 0.7793(3) 0.05334(17) 0.0511(10) Uani 1 1 d . . . H5A H 0.6423 0.8090 0.0441 0.061 Uiso 1 1 calc R . . H5B H 0.5060 0.7964 0.0133 0.061 Uiso 1 1 calc R . . C6 C 0.5620(3) 0.6267(3) 0.06936(15) 0.0411(8) Uani 1 1 d . . . H6A H 0.4792 0.5957 0.0751 0.049 Uiso 1 1 calc R . . H6B H 0.5917 0.5755 0.0319 0.049 Uiso 1 1 calc R . . C10 C 0.5062(2) 0.3441(3) 0.14242(15) 0.0336(8) Uani 1 1 d . . . H10A H 0.4739 0.3755 0.0982 0.040 Uiso 1 1 calc R . . H10B H 0.5130 0.2436 0.1401 0.040 Uiso 1 1 calc R . . C11 C 0.7244(2) 0.3343(3) 0.08350(14) 0.0299(7) Uani 1 1 d . . . H11 H 0.6637 0.3438 0.0448 0.036 Uiso 1 1 calc R . . C12 C 0.7465(3) 0.1819(3) 0.09606(17) 0.0466(9) Uani 1 1 d . . . H12A H 0.8040 0.1708 0.1354 0.056 Uiso 1 1 calc R . . H12B H 0.6701 0.1379 0.1057 0.056 Uiso 1 1 calc R . . C13 C 0.7961(3) 0.1104(3) 0.03743(16) 0.0462(9) Uani 1 1 d . . . H13A H 0.8121 0.0135 0.0486 0.055 Uiso 1 1 calc R . . H13B H 0.7357 0.1137 -0.0010 0.055 Uiso 1 1 calc R . . C14 C 0.9114(3) 0.1782(3) 0.01951(16) 0.0430(9) Uani 1 1 d . . . H14A H 0.9749 0.1647 0.0558 0.052 Uiso 1 1 calc R . . H14B H 0.9385 0.1354 -0.0209 0.052 Uiso 1 1 calc R . . C15 C 0.8918(3) 0.3299(3) 0.00768(16) 0.0436(9) Uani 1 1 d . . . H15A H 0.8358 0.3426 -0.0322 0.052 Uiso 1 1 calc R . . H15B H 0.9693 0.3726 -0.0010 0.052 Uiso 1 1 calc R . . C16 C 0.8411(2) 0.4021(3) 0.06591(14) 0.0349(7) Uani 1 1 d . . . H16A H 0.8254 0.4989 0.0545 0.042 Uiso 1 1 calc R . . H16B H 0.9008 0.3990 0.1047 0.042 Uiso 1 1 calc R . . C21 C 0.4529(3) 0.2893(3) 0.27798(15) 0.0350(8) Uani 1 1 d . . . C22 C 0.3508(3) 0.2518(3) 0.32100(15) 0.0494(9) Uani 1 1 d . . . H22A H 0.3018 0.1792 0.2994 0.074 Uiso 1 1 calc R . . H22B H 0.3007 0.3322 0.3268 0.074 Uiso 1 1 calc R . . H22C H 0.3849 0.2201 0.3643 0.074 Uiso 1 1 calc R . . C23 C 0.5271(3) 0.1614(3) 0.26629(16) 0.0506(9) Uani 1 1 d . . . H23A H 0.5514 0.1181 0.3088 0.076 Uiso 1 1 calc R . . H23B H 0.5987 0.1870 0.2443 0.076 Uiso 1 1 calc R . . H23C H 0.4786 0.0974 0.2383 0.076 Uiso 1 1 calc R . . C24 C 0.5330(3) 0.3933(3) 0.31722(15) 0.0489(9) Uani 1 1 d . . . H24A H 0.4848 0.4725 0.3279 0.073 Uiso 1 1 calc R . . H24B H 0.5977 0.4226 0.2906 0.073 Uiso 1 1 calc R . . H24C H 0.5676 0.3510 0.3582 0.073 Uiso 1 1 calc R . . C25 C 0.2589(3) 0.2871(3) 0.15899(15) 0.0352(8) Uani 1 1 d . . . C26 C 0.2336(3) 0.3566(4) 0.09131(16) 0.0551(10) Uani 1 1 d . . . H26A H 0.2961 0.3310 0.0624 0.083 Uiso 1 1 calc R . . H26B H 0.2336 0.4558 0.0971 0.083 Uiso 1 1 calc R . . H26C H 0.1551 0.3272 0.0713 0.083 Uiso 1 1 calc R . . C27 C 0.1479(3) 0.3108(3) 0.19736(17) 0.0503(10) Uani 1 1 d . . . H27A H 0.1395 0.4085 0.2061 0.075 Uiso 1 1 calc R . . H27B H 0.1572 0.2611 0.2393 0.075 Uiso 1 1 calc R . . H27C H 0.0762 0.2780 0.1711 0.075 Uiso 1 1 calc R . . C28 C 0.2755(3) 0.1336(3) 0.14796(17) 0.0494(9) Uani 1 1 d . . . H28A H 0.2047 0.0972 0.1221 0.074 Uiso 1 1 calc R . . H28B H 0.2852 0.0870 0.1908 0.074 Uiso 1 1 calc R . . H28C H 0.3470 0.1185 0.1240 0.074 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 0.0301(4) 0.0378(5) 0.0305(5) -0.0002(4) 0.0054(3) -0.0010(4) P2 0.0311(5) 0.0294(5) 0.0352(5) 0.0028(4) 0.0083(3) 0.0000(4) C1 0.0311(17) 0.0292(18) 0.0357(18) -0.0066(14) 0.0049(14) -0.0034(15) C2 0.046(2) 0.047(2) 0.042(2) -0.0166(16) 0.0107(17) -0.0039(17) C3 0.054(2) 0.039(2) 0.072(3) -0.0239(19) 0.019(2) -0.0055(18) C4 0.041(2) 0.031(2) 0.105(3) -0.008(2) 0.010(2) 0.0030(17) C5 0.054(2) 0.033(2) 0.065(3) 0.0015(18) -0.0038(19) -0.0008(17) C6 0.046(2) 0.034(2) 0.042(2) -0.0063(16) -0.0007(16) -0.0015(16) C10 0.0349(18) 0.0345(19) 0.0321(19) 0.0031(14) 0.0067(14) -0.0042(15) C11 0.0286(17) 0.0290(18) 0.0320(18) -0.0008(13) 0.0005(14) 0.0011(14) C12 0.047(2) 0.0319(19) 0.064(3) 0.0031(16) 0.0194(18) -0.0012(16) C13 0.047(2) 0.0314(19) 0.061(2) -0.0075(17) 0.0087(17) 0.0040(17) C14 0.044(2) 0.043(2) 0.043(2) -0.0036(16) 0.0111(16) 0.0090(17) C15 0.048(2) 0.042(2) 0.043(2) 0.0002(16) 0.0175(16) 0.0042(17) C16 0.0324(17) 0.0322(18) 0.0408(19) -0.0007(15) 0.0071(14) -0.0001(15) C21 0.0396(19) 0.0348(19) 0.0312(19) 0.0022(14) 0.0061(15) 0.0001(15) C22 0.059(2) 0.060(2) 0.032(2) 0.0077(17) 0.0118(17) -0.0058(19) C23 0.050(2) 0.053(2) 0.048(2) 0.0131(17) 0.0012(17) 0.0121(18) C24 0.053(2) 0.060(2) 0.034(2) -0.0015(18) 0.0037(16) -0.0042(19) C25 0.0284(18) 0.0325(19) 0.045(2) 0.0047(15) 0.0054(15) -0.0008(14) C26 0.040(2) 0.071(3) 0.053(2) 0.0160(19) -0.0071(17) -0.0074(19) C27 0.0273(18) 0.056(2) 0.069(3) -0.0027(19) 0.0137(17) -0.0053(17) C28 0.043(2) 0.040(2) 0.065(2) -0.0086(18) 0.0031(18) -0.0037(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 P1 C10 1.863(3) . ? P1 C1 1.866(3) . ? P1 C11 1.869(3) . ? P2 C10 1.855(3) . ? P2 C21 1.896(3) . ? P2 C25 1.900(3) . ? C1 C6 1.530(4) . ? C1 C2 1.537(4) . ? C2 C3 1.520(4) . ? C3 C4 1.521(5) . ? C4 C5 1.520(4) . ? C5 C6 1.532(4) . ? C11 C16 1.531(4) . ? C11 C12 1.532(4) . ? C12 C13 1.524(4) . ? C13 C14 1.520(4) . ? C14 C15 1.519(4) . ? C15 C16 1.526(4) . ? C21 C23 1.532(4) . ? C21 C22 1.536(4) . ? C21 C24 1.536(4) . ? C25 C27 1.535(4) . ? C25 C28 1.536(4) . ? C25 C26 1.539(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 P1 C1 102.79(13) . . ? C10 P1 C11 97.37(13) . . ? C1 P1 C11 103.04(13) . . ? C10 P2 C21 101.88(13) . . ? C10 P2 C25 99.46(13) . . ? C21 P2 C25 110.17(14) . . ? C6 C1 C2 110.0(2) . . ? C6 C1 P1 117.48(19) . . ? C2 C1 P1 110.8(2) . . ? C3 C2 C1 111.9(3) . . ? C2 C3 C4 111.5(3) . . ? C5 C4 C3 110.7(3) . . ? C4 C5 C6 110.7(3) . . ? C1 C6 C5 111.5(2) . . ? P2 C10 P1 120.26(16) . . ? C16 C11 C12 109.4(2) . . ? C16 C11 P1 112.91(19) . . ? C12 C11 P1 109.7(2) . . ? C13 C12 C11 112.5(3) . . ? C14 C13 C12 110.7(3) . . ? C15 C14 C13 110.6(3) . . ? C14 C15 C16 112.9(3) . . ? C15 C16 C11 110.8(2) . . ? C23 C21 C22 109.1(3) . . ? C23 C21 C24 108.9(3) . . ? C22 C21 C24 107.0(2) . . ? C23 C21 P2 115.7(2) . . ? C22 C21 P2 110.5(2) . . ? C24 C21 P2 105.2(2) . . ? C27 C25 C28 109.5(2) . . ? C27 C25 C26 106.8(3) . . ? C28 C25 C26 108.6(3) . . ? C27 C25 P2 109.3(2) . . ? C28 C25 P2 116.9(2) . . ? C26 C25 P2 105.1(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.228 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.052 #===END data_fe20_ptbpm_5 _database_code_CSD 199936 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ptbpm _chemical_melting_point ? _chemical_formula_moiety 'C21 H30 P2' _chemical_formula_sum 'C21 H30 P2' _chemical_formula_weight 344.39 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' 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 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 6.2975(2) _cell_length_b 33.5911(4) _cell_length_c 10.2346(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.3140(10) _cell_angle_gamma 90.00 _cell_volume 2088.15(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max .154 _exptl_crystal_size_mid .08 _exptl_crystal_size_min .08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.095 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 15312 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 25.46 _reflns_number_total 3599 _reflns_number_gt 2435 _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^)+(0.0507P)^2^+0.0370P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3599 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.321 _refine_ls_shift/su_mean 0.046 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 0.15491(10) 0.389932(19) 0.23081(6) 0.0365(2) Uani 1 1 d . . . P2 P 0.22924(10) 0.339096(18) 0.48416(6) 0.0356(2) Uani 1 1 d . . . C10 C 0.3610(4) 0.36073(8) 0.3587(2) 0.0361(6) Uani 1 1 d . . . C11 C 0.1187(4) 0.35714(8) 0.0766(2) 0.0474(7) Uani 1 1 d . . . C12 C 0.3224(7) 0.34691(14) 0.0302(4) 0.0803(11) Uani 1 1 d . . . H12A H 0.452(5) 0.3390(8) 0.099(3) 0.067(10) Uiso 1 1 d . . . H12B H 0.285(5) 0.3247(10) -0.038(3) 0.098(11) Uiso 1 1 d . . . H12C H 0.372(6) 0.3703(10) -0.022(4) 0.114(14) Uiso 1 1 d . . . C13 C -0.0557(7) 0.37525(12) -0.0414(3) 0.0720(10) Uani 1 1 d . . . H13A H -0.100(5) 0.3565(8) -0.116(3) 0.074(9) Uiso 1 1 d . . . H13B H -0.007(5) 0.3999(9) -0.075(3) 0.083(11) Uiso 1 1 d . . . H13C H -0.196(6) 0.3850(11) -0.017(4) 0.119(16) Uiso 1 1 d . . . C14 C 0.0203(8) 0.31841(11) 0.1167(4) 0.0730(11) Uani 1 1 d . . . H14B H -0.015(5) 0.3023(8) 0.040(3) 0.075(10) Uiso 1 1 d . . . H14C H 0.132(5) 0.3023(8) 0.190(3) 0.078(9) Uiso 1 1 d . . . H14A H -0.115(6) 0.3249(11) 0.145(4) 0.111(16) Uiso 1 1 d . . . C15 C 0.3153(4) 0.43648(7) 0.2150(2) 0.0432(6) Uani 1 1 d . . . C16 C 0.1713(7) 0.46278(10) 0.1050(4) 0.0636(9) Uani 1 1 d . . . H16A H 0.026(5) 0.4658(9) 0.118(3) 0.088(12) Uiso 1 1 d . . . H16B H 0.239(4) 0.4902(9) 0.108(3) 0.074(9) Uiso 1 1 d . . . H16C H 0.157(5) 0.4509(9) 0.015(3) 0.081(10) Uiso 1 1 d . . . C17 C 0.5402(6) 0.43086(12) 0.1887(5) 0.0727(10) Uani 1 1 d . . . H17A H 0.603(5) 0.4556(9) 0.190(3) 0.079(10) Uiso 1 1 d . . . H17C H 0.527(5) 0.4209(9) 0.100(3) 0.086(13) Uiso 1 1 d . . . H17B H 0.641(5) 0.4086(10) 0.249(3) 0.091(10) Uiso 1 1 d . . . C18 C 0.3452(8) 0.45817(10) 0.3511(3) 0.0679(10) Uani 1 1 d . . . H18A H 0.414(4) 0.4846(9) 0.350(3) 0.079(10) Uiso 1 1 d . . . H18C H 0.208(5) 0.4621(9) 0.369(3) 0.084(13) Uiso 1 1 d . . . H18B H 0.440(5) 0.4431(9) 0.425(3) 0.075(10) Uiso 1 1 d . . . C21 C 0.2176(4) 0.38375(7) 0.5863(2) 0.0363(6) Uani 1 1 d . . . C22 C 0.0170(5) 0.40339(8) 0.5659(3) 0.0499(7) Uani 1 1 d . . . H22 H -0.104(4) 0.3926(7) 0.507(3) 0.051(8) Uiso 1 1 d . . . C23 C -0.0004(6) 0.43849(9) 0.6316(3) 0.0650(9) Uani 1 1 d . . . H23 H -0.135(5) 0.4527(8) 0.616(3) 0.078(10) Uiso 1 1 d . . . C24 C 0.1819(6) 0.45444(9) 0.7207(3) 0.0625(9) Uani 1 1 d . . . H24 H 0.172(4) 0.4784(8) 0.765(3) 0.063(8) Uiso 1 1 d . . . C25 C 0.3825(6) 0.43532(8) 0.7450(3) 0.0564(8) Uani 1 1 d . . . H25 H 0.507(4) 0.4449(7) 0.802(3) 0.053(8) Uiso 1 1 d . . . C26 C 0.4006(5) 0.40008(8) 0.6780(3) 0.0435(7) Uani 1 1 d . . . H26 H 0.535(4) 0.3872(6) 0.695(2) 0.035(7) Uiso 1 1 d . . . C27 C 0.4541(4) 0.31144(6) 0.5985(2) 0.0355(6) Uani 1 1 d . . . C28 C 0.4146(5) 0.29560(8) 0.7164(3) 0.0507(7) Uani 1 1 d . . . H28 H 0.288(4) 0.3003(7) 0.736(2) 0.036(7) Uiso 1 1 d . . . C29 C 0.5657(6) 0.27103(9) 0.8018(3) 0.0620(9) Uani 1 1 d . . . H29 H 0.530(5) 0.2612(8) 0.877(3) 0.074(10) Uiso 1 1 d . . . C30 C 0.7582(6) 0.26129(9) 0.7712(3) 0.0584(9) Uani 1 1 d . . . H30 H 0.855(4) 0.2430(8) 0.828(3) 0.057(8) Uiso 1 1 d . . . C31 C 0.8028(5) 0.27656(8) 0.6562(3) 0.0531(8) Uani 1 1 d . . . H31 H 0.937(4) 0.2705(7) 0.636(3) 0.054(8) Uiso 1 1 d . . . C32 C 0.6535(4) 0.30199(7) 0.5707(3) 0.0419(6) Uani 1 1 d . . . H32 H 0.691(4) 0.3130(7) 0.494(2) 0.044(7) Uiso 1 1 d . . . H10A H 0.417(4) 0.3395(7) 0.318(2) 0.041(7) Uiso 1 1 d . . . H10B H 0.486(4) 0.3783(7) 0.404(2) 0.040(7) 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 0.0336(4) 0.0458(4) 0.0302(4) 0.0047(3) 0.0086(3) 0.0047(3) P2 0.0373(4) 0.0386(4) 0.0297(4) 0.0005(3) 0.0070(3) -0.0001(3) C10 0.0386(16) 0.0394(15) 0.0314(14) 0.0019(12) 0.0109(12) 0.0044(13) C11 0.0551(18) 0.0532(17) 0.0312(14) -0.0002(12) 0.0066(13) -0.0053(13) C12 0.089(3) 0.107(3) 0.049(2) -0.020(2) 0.025(2) 0.013(3) C13 0.086(3) 0.080(3) 0.0363(19) 0.0063(18) -0.0076(19) -0.014(2) C14 0.106(3) 0.057(2) 0.045(2) -0.0044(17) 0.000(2) -0.022(2) C15 0.0475(16) 0.0393(15) 0.0429(15) 0.0065(12) 0.0118(13) 0.0035(12) C16 0.084(3) 0.047(2) 0.057(2) 0.0123(16) 0.014(2) 0.0099(18) C17 0.062(2) 0.065(3) 0.102(3) 0.013(2) 0.039(2) -0.010(2) C18 0.099(3) 0.046(2) 0.057(2) -0.0032(16) 0.018(2) -0.012(2) C21 0.0426(16) 0.0394(14) 0.0289(13) 0.0043(11) 0.0131(12) 0.0002(12) C22 0.0454(19) 0.0538(18) 0.0532(19) -0.0011(15) 0.0176(16) 0.0042(15) C23 0.065(2) 0.061(2) 0.077(2) -0.0017(18) 0.034(2) 0.0165(19) C24 0.096(3) 0.0423(18) 0.063(2) -0.0035(16) 0.045(2) 0.0087(19) C25 0.080(3) 0.0459(18) 0.0418(17) -0.0043(14) 0.0137(17) -0.0114(18) C26 0.0500(18) 0.0409(16) 0.0384(16) 0.0026(12) 0.0098(14) 0.0034(14) C27 0.0438(16) 0.0327(13) 0.0274(13) -0.0036(10) 0.0047(12) -0.0014(11) C28 0.059(2) 0.0559(18) 0.0379(17) 0.0038(13) 0.0139(16) 0.0087(16) C29 0.085(3) 0.060(2) 0.0390(18) 0.0097(15) 0.0120(18) 0.0166(18) C30 0.077(2) 0.0451(17) 0.0417(18) 0.0012(14) -0.0048(18) 0.0198(16) C31 0.054(2) 0.0475(17) 0.0537(19) -0.0059(14) 0.0064(16) 0.0126(15) C32 0.0495(18) 0.0379(15) 0.0369(15) -0.0026(12) 0.0090(14) 0.0035(13) _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 C10 1.861(2) . ? P1 C11 1.888(3) . ? P1 C15 1.892(3) . ? P2 C27 1.834(2) . ? P2 C21 1.841(2) . ? P2 C10 1.852(3) . ? C11 C12 1.520(4) . ? C11 C13 1.528(4) . ? C11 C14 1.542(4) . ? C15 C17 1.522(4) . ? C15 C16 1.527(4) . ? C15 C18 1.538(4) . ? C21 C22 1.391(3) . ? C21 C26 1.392(3) . ? C22 C23 1.376(4) . ? C23 C24 1.372(4) . ? C24 C25 1.380(4) . ? C25 C26 1.387(4) . ? C27 C32 1.395(3) . ? C27 C28 1.400(4) . ? C28 C29 1.382(4) . ? C29 C30 1.370(4) . ? C30 C31 1.380(4) . ? C31 C32 1.394(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 P1 C11 100.84(12) . . ? C10 P1 C15 101.94(12) . . ? C11 P1 C15 111.11(12) . . ? C27 P2 C21 100.98(10) . . ? C27 P2 C10 103.26(11) . . ? C21 P2 C10 99.58(12) . . ? P2 C10 P1 109.74(13) . . ? C12 C11 C13 109.4(3) . . ? C12 C11 C14 108.9(3) . . ? C13 C11 C14 106.9(3) . . ? C12 C11 P1 117.9(2) . . ? C13 C11 P1 109.4(2) . . ? C14 C11 P1 103.8(2) . . ? C17 C15 C16 109.9(3) . . ? C17 C15 C18 108.8(3) . . ? C16 C15 C18 107.5(3) . . ? C17 C15 P1 117.1(2) . . ? C16 C15 P1 108.3(2) . . ? C18 C15 P1 104.7(2) . . ? C22 C21 C26 118.1(2) . . ? C22 C21 P2 118.2(2) . . ? C26 C21 P2 123.64(19) . . ? C23 C22 C21 121.3(3) . . ? C24 C23 C22 119.9(3) . . ? C23 C24 C25 120.2(3) . . ? C24 C25 C26 119.9(3) . . ? C25 C26 C21 120.5(3) . . ? C32 C27 C28 117.6(2) . . ? C32 C27 P2 124.78(19) . . ? C28 C27 P2 117.4(2) . . ? C29 C28 C27 121.5(3) . . ? C30 C29 C28 120.1(3) . . ? C29 C30 C31 119.9(3) . . ? C30 C31 C32 120.5(3) . . ? C31 C32 C27 120.4(3) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.198 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.041 #===END data_ig4_dtbpe_6 _database_code_CSD 199937 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common dtbpe _chemical_melting_point ? _chemical_formula_moiety 'C18 H40 P2' _chemical_formula_sum 'C18 H40 P2' _chemical_formula_weight 318.44 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' 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 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 8.500 _cell_length_b 10.1304(2) _cell_length_c 12.9111(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.18 _cell_angle_gamma 90.00 _cell_volume 1067.75(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max .43 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.990 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 356 _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 10678 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2444 _reflns_number_gt 1954 _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^)+(0.0493P)^2^+0.1813P] 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 2444 _refine_ls_number_parameters 97 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 0.12113(4) 0.12258(3) 0.64785(2) 0.02836(12) Uani 1 1 d . . . C1 C -0.01776(18) 0.07045(13) 0.51579(10) 0.0350(3) Uani 1 1 d . . . H1A H -0.1325 0.0753 0.5192 0.042 Uiso 1 1 calc R . . H1B H -0.0059 0.1326 0.4592 0.042 Uiso 1 1 calc R . . C11 C 0.27561(18) 0.23119(14) 0.60817(11) 0.0375(3) Uani 1 1 d . . . C12 C 0.41596(19) 0.25779(18) 0.71044(14) 0.0514(4) Uani 1 1 d . . . H12A H 0.4531 0.1741 0.7473 0.077 Uiso 1 1 calc R . . H12B H 0.3771 0.3162 0.7587 0.077 Uiso 1 1 calc R . . H12C H 0.5072 0.3000 0.6906 0.077 Uiso 1 1 calc R . . C13 C 0.2142(2) 0.36233(16) 0.55229(15) 0.0554(4) Uani 1 1 d . . . H13A H 0.1863 0.4224 0.6040 0.083 Uiso 1 1 calc R . . H13B H 0.1168 0.3464 0.4919 0.083 Uiso 1 1 calc R . . H13C H 0.3003 0.4021 0.5253 0.083 Uiso 1 1 calc R . . C14 C 0.3461(2) 0.14771(17) 0.53192(14) 0.0516(4) Uani 1 1 d . . . H14A H 0.4396 0.1939 0.5181 0.077 Uiso 1 1 calc R . . H14B H 0.2614 0.1341 0.4637 0.077 Uiso 1 1 calc R . . H14C H 0.3822 0.0621 0.5655 0.077 Uiso 1 1 calc R . . C15 C -0.02235(17) 0.22626(14) 0.70279(11) 0.0360(3) Uani 1 1 d . . . C16 C 0.0776(2) 0.30249(19) 0.80175(13) 0.0553(5) Uani 1 1 d . . . H16A H 0.0037 0.3403 0.8401 0.083 Uiso 1 1 calc R . . H16B H 0.1384 0.3736 0.7786 0.083 Uiso 1 1 calc R . . H16C H 0.1548 0.2424 0.8499 0.083 Uiso 1 1 calc R . . C17 C -0.1358(2) 0.32226(17) 0.62501(15) 0.0546(4) Uani 1 1 d . . . H17A H -0.2023 0.2735 0.5625 0.082 Uiso 1 1 calc R . . H17B H -0.0699 0.3887 0.6009 0.082 Uiso 1 1 calc R . . H17C H -0.2078 0.3660 0.6619 0.082 Uiso 1 1 calc R . . C18 C -0.1279(2) 0.12481(17) 0.74200(15) 0.0519(4) Uani 1 1 d . . . H18A H -0.0568 0.0668 0.7959 0.078 Uiso 1 1 calc R . . H18B H -0.1903 0.0720 0.6807 0.078 Uiso 1 1 calc R . . H18C H -0.2037 0.1711 0.7744 0.078 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 0.03257(19) 0.02808(19) 0.02277(18) -0.00167(13) 0.00499(12) -0.00023(14) C1 0.0421(7) 0.0310(7) 0.0265(6) -0.0043(5) 0.0007(5) 0.0022(6) C11 0.0436(8) 0.0354(7) 0.0369(7) -0.0045(6) 0.0169(6) -0.0043(6) C12 0.0372(8) 0.0606(11) 0.0569(10) -0.0152(8) 0.0141(7) -0.0112(7) C13 0.0722(12) 0.0378(9) 0.0612(11) 0.0058(8) 0.0269(9) -0.0068(8) C14 0.0629(11) 0.0503(10) 0.0541(10) -0.0106(8) 0.0370(8) -0.0104(8) C15 0.0379(7) 0.0370(8) 0.0352(7) -0.0080(6) 0.0137(6) -0.0020(6) C16 0.0575(10) 0.0683(12) 0.0467(9) -0.0285(9) 0.0256(8) -0.0137(9) C17 0.0554(10) 0.0452(10) 0.0656(11) -0.0019(8) 0.0208(9) 0.0161(8) C18 0.0482(9) 0.0517(10) 0.0640(11) -0.0066(8) 0.0292(8) -0.0078(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 P1 C1 1.8597(13) . ? P1 C11 1.8900(14) . ? P1 C15 1.8910(14) . ? C1 C1 1.537(3) 3_556 ? C11 C13 1.532(2) . ? C11 C12 1.537(2) . ? C11 C14 1.540(2) . ? C15 C17 1.531(2) . ? C15 C16 1.5317(19) . ? C15 C18 1.540(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 C1 P1 C11 103.19(7) . . ? C1 P1 C15 100.99(6) . . ? C11 P1 C15 110.35(6) . . ? C1 C1 P1 112.67(12) 3_556 . ? C13 C11 C12 109.48(13) . . ? C13 C11 C14 108.50(13) . . ? C12 C11 C14 107.36(13) . . ? C13 C11 P1 117.46(11) . . ? C12 C11 P1 107.50(10) . . ? C14 C11 P1 106.08(10) . . ? C17 C15 C16 109.19(14) . . ? C17 C15 C18 108.75(13) . . ? C16 C15 C18 107.52(12) . . ? C17 C15 P1 117.45(10) . . ? C16 C15 P1 109.08(10) . . ? C18 C15 P1 104.38(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.286 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.037 #===END data_ck1_dtbpmO2_7 _database_code_CSD 199938 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common dtbpmO2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H38 O2 P2' _chemical_formula_weight 336.41 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' 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 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 9.5711(2) _cell_length_b 25.0934(4) _cell_length_c 17.63570(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.0610(10) _cell_angle_gamma 90.00 _cell_volume 4090.10(11) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max .5 _exptl_crystal_size_mid .31 _exptl_crystal_size_min .31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 30348 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.62 _reflns_number_total 7114 _reflns_number_gt 5422 _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^)+(0.0478P)^2^+2.1791P] 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 7114 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.003 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 0.39308(6) 0.51788(2) 0.70241(3) 0.03265(15) Uani 1 1 d . . . P2 P 0.16950(6) 0.52561(2) 0.81639(4) 0.03595(15) Uani 1 1 d . . . P3 P 0.58888(6) 0.27032(2) 0.71085(3) 0.03024(14) Uani 1 1 d . . . P4 P 0.34336(6) 0.28131(2) 0.54543(3) 0.03218(15) Uani 1 1 d . . . O1 O 0.38801(17) 0.45905(6) 0.69173(9) 0.0427(4) Uani 1 1 d . . . O2 O 0.03693(17) 0.54499(7) 0.75938(10) 0.0512(4) Uani 1 1 d . . . O3 O 0.58635(17) 0.21108(6) 0.70966(9) 0.0416(4) Uani 1 1 d . . . O4 O 0.44455(18) 0.27502(7) 0.49504(9) 0.0534(5) Uani 1 1 d . . . C10 C 0.3386(2) 0.53988(9) 0.78992(13) 0.0383(5) Uani 1 1 d . . . H10A H 0.4165 0.5274 0.8351 0.046 Uiso 1 1 calc R . . H10B H 0.3461 0.5792 0.7899 0.046 Uiso 1 1 calc R . . C11 C 0.2727(3) 0.55305(9) 0.61814(14) 0.0447(6) Uani 1 1 d . . . C12 C 0.3367(3) 0.55224(13) 0.54730(16) 0.0712(9) Uani 1 1 d . . . H12A H 0.2634 0.5641 0.5005 0.107 Uiso 1 1 calc R . . H12B H 0.3675 0.5159 0.5391 0.107 Uiso 1 1 calc R . . H12C H 0.4203 0.5762 0.5569 0.107 Uiso 1 1 calc R . . C13 C 0.2384(3) 0.61033(10) 0.63919(19) 0.0674(9) Uani 1 1 d . . . H13A H 0.3288 0.6290 0.6639 0.101 Uiso 1 1 calc R . . H13B H 0.1769 0.6092 0.6758 0.101 Uiso 1 1 calc R . . H13C H 0.1877 0.6293 0.5913 0.101 Uiso 1 1 calc R . . C14 C 0.1301(3) 0.52182(10) 0.59542(15) 0.0542(7) Uani 1 1 d . . . H14A H 0.0643 0.5386 0.5497 0.081 Uiso 1 1 calc R . . H14B H 0.0855 0.5219 0.6395 0.081 Uiso 1 1 calc R . . H14C H 0.1494 0.4850 0.5825 0.081 Uiso 1 1 calc R . . C15 C 0.5849(2) 0.54048(9) 0.72308(14) 0.0390(5) Uani 1 1 d . . . C16 C 0.6554(3) 0.51396(11) 0.66330(17) 0.0570(7) Uani 1 1 d . . . H16A H 0.6105 0.5278 0.6106 0.086 Uiso 1 1 calc R . . H16B H 0.6413 0.4753 0.6639 0.086 Uiso 1 1 calc R . . H16C H 0.7592 0.5220 0.6773 0.086 Uiso 1 1 calc R . . C17 C 0.6068(3) 0.60099(10) 0.72227(17) 0.0523(7) Uani 1 1 d . . . H17A H 0.5592 0.6179 0.7590 0.078 Uiso 1 1 calc R . . H17B H 0.5648 0.6147 0.6692 0.078 Uiso 1 1 calc R . . H17C H 0.7106 0.6091 0.7381 0.078 Uiso 1 1 calc R . . C18 C 0.6646(3) 0.51896(12) 0.80433(16) 0.0571(7) Uani 1 1 d . . . H18A H 0.7692 0.5223 0.8115 0.086 Uiso 1 1 calc R . . H18B H 0.6396 0.4814 0.8083 0.086 Uiso 1 1 calc R . . H18C H 0.6358 0.5395 0.8451 0.086 Uiso 1 1 calc R . . C21 C 0.1954(3) 0.56351(10) 0.91001(15) 0.0483(6) Uani 1 1 d . . . C22 C 0.0509(4) 0.56451(12) 0.9330(2) 0.0759(10) Uani 1 1 d . . . H22A H 0.0592 0.5883 0.9780 0.114 Uiso 1 1 calc R . . H22B H 0.0274 0.5284 0.9471 0.114 Uiso 1 1 calc R . . H22C H -0.0259 0.5774 0.8885 0.114 Uiso 1 1 calc R . . C23 C 0.3135(4) 0.54243(17) 0.97894(19) 0.1067(15) Uani 1 1 d . . . H23A H 0.4064 0.5428 0.9653 0.160 Uiso 1 1 calc R . . H23B H 0.2902 0.5058 0.9908 0.160 Uiso 1 1 calc R . . H23C H 0.3197 0.5650 1.0250 0.160 Uiso 1 1 calc R . . C24 C 0.2258(4) 0.62106(11) 0.8933(2) 0.0849(11) Uani 1 1 d . . . H24A H 0.2146 0.6436 0.9367 0.127 Uiso 1 1 calc R . . H24B H 0.1576 0.6326 0.8445 0.127 Uiso 1 1 calc R . . H24C H 0.3250 0.6242 0.8881 0.127 Uiso 1 1 calc R . . C25 C 0.1611(3) 0.45253(9) 0.83079(14) 0.0415(6) Uani 1 1 d . . . C26 C 0.0526(3) 0.43887(11) 0.8781(2) 0.0698(9) Uani 1 1 d . . . H26A H 0.0352 0.4003 0.8760 0.105 Uiso 1 1 calc R . . H26B H -0.0387 0.4576 0.8557 0.105 Uiso 1 1 calc R . . H26C H 0.0916 0.4499 0.9328 0.105 Uiso 1 1 calc R . . C27 C 0.1046(4) 0.42802(11) 0.74887(18) 0.0698(9) Uani 1 1 d . . . H27A H 0.1731 0.4354 0.7174 0.105 Uiso 1 1 calc R . . H27B H 0.0103 0.4436 0.7231 0.105 Uiso 1 1 calc R . . H27C H 0.0943 0.3894 0.7537 0.105 Uiso 1 1 calc R . . C28 C 0.3075(3) 0.42798(11) 0.8685(2) 0.0681(8) Uani 1 1 d . . . H28A H 0.3466 0.4436 0.9207 0.102 Uiso 1 1 calc R . . H28B H 0.3739 0.4351 0.8358 0.102 Uiso 1 1 calc R . . H28C H 0.2967 0.3894 0.8735 0.102 Uiso 1 1 calc R . . C30 C 0.4291(2) 0.30204(8) 0.64636(11) 0.0293(5) Uani 1 1 d . . . H30A H 0.3526 0.3006 0.6748 0.035 Uiso 1 1 calc R . . H30B H 0.4541 0.3401 0.6435 0.035 Uiso 1 1 calc R . . C31 C 0.5828(3) 0.29389(10) 0.80993(13) 0.0436(6) Uani 1 1 d . . . C32 C 0.4333(3) 0.27837(13) 0.82112(15) 0.0654(8) Uani 1 1 d . . . H32A H 0.4341 0.2824 0.8765 0.098 Uiso 1 1 calc R . . H32B H 0.4120 0.2412 0.8051 0.098 Uiso 1 1 calc R . . H32C H 0.3589 0.3016 0.7889 0.098 Uiso 1 1 calc R . . C33 C 0.6965(3) 0.26344(12) 0.87289(15) 0.0673(8) Uani 1 1 d . . . H33A H 0.7934 0.2763 0.8734 0.101 Uiso 1 1 calc R . . H33B H 0.6896 0.2253 0.8608 0.101 Uiso 1 1 calc R . . H33C H 0.6788 0.2694 0.9245 0.101 Uiso 1 1 calc R . . C34 C 0.6064(3) 0.35412(10) 0.82251(15) 0.0597(8) Uani 1 1 d . . . H34A H 0.5367 0.3735 0.7811 0.090 Uiso 1 1 calc R . . H34B H 0.7050 0.3633 0.8206 0.090 Uiso 1 1 calc R . . H34C H 0.5927 0.3640 0.8738 0.090 Uiso 1 1 calc R . . C35 C 0.7472(2) 0.29657(9) 0.67980(14) 0.0412(6) Uani 1 1 d . . . C36 C 0.7338(3) 0.35559(11) 0.6558(2) 0.0664(8) Uani 1 1 d . . . H36A H 0.7151 0.3769 0.6986 0.100 Uiso 1 1 calc R . . H36B H 0.6537 0.3600 0.6086 0.100 Uiso 1 1 calc R . . H36C H 0.8241 0.3675 0.6448 0.100 Uiso 1 1 calc R . . C37 C 0.8871(3) 0.28763(13) 0.74444(19) 0.0679(8) Uani 1 1 d . . . H37A H 0.9706 0.2957 0.7239 0.102 Uiso 1 1 calc R . . H37B H 0.8922 0.2504 0.7617 0.102 Uiso 1 1 calc R . . H37C H 0.8881 0.3110 0.7890 0.102 Uiso 1 1 calc R . . C38 C 0.7566(3) 0.26355(12) 0.60835(17) 0.0628(8) Uani 1 1 d . . . H38A H 0.8403 0.2752 0.5904 0.094 Uiso 1 1 calc R . . H38B H 0.6681 0.2686 0.5661 0.094 Uiso 1 1 calc R . . H38C H 0.7672 0.2258 0.6229 0.094 Uiso 1 1 calc R . . C41 C 0.2466(3) 0.21787(9) 0.55203(15) 0.0468(6) Uani 1 1 d . . . C42 C 0.1196(3) 0.20942(11) 0.47882(18) 0.0730(9) Uani 1 1 d . . . H42A H 0.0806 0.1734 0.4798 0.110 Uiso 1 1 calc R . . H42B H 0.1539 0.2139 0.4314 0.110 Uiso 1 1 calc R . . H42C H 0.0436 0.2356 0.4787 0.110 Uiso 1 1 calc R . . C43 C 0.1917(3) 0.21392(11) 0.62604(18) 0.0628(8) Uani 1 1 d . . . H43A H 0.1349 0.1812 0.6241 0.094 Uiso 1 1 calc R . . H43B H 0.1307 0.2448 0.6289 0.094 Uiso 1 1 calc R . . H43C H 0.2743 0.2132 0.6725 0.094 Uiso 1 1 calc R . . C44 C 0.3574(3) 0.17294(10) 0.55371(18) 0.0666(9) Uani 1 1 d . . . H44A H 0.4395 0.1773 0.5999 0.100 Uiso 1 1 calc R . . H44B H 0.3918 0.1747 0.5061 0.100 Uiso 1 1 calc R . . H44C H 0.3114 0.1383 0.5562 0.100 Uiso 1 1 calc R . . C45 C 0.2184(2) 0.33782(9) 0.50727(12) 0.0362(5) Uani 1 1 d . . . C46 C 0.1013(3) 0.34628(10) 0.55054(15) 0.0504(6) Uani 1 1 d . . . H46A H 0.0465 0.3786 0.5308 0.076 Uiso 1 1 calc R . . H46B H 0.1465 0.3501 0.6069 0.076 Uiso 1 1 calc R . . H46C H 0.0359 0.3156 0.5417 0.076 Uiso 1 1 calc R . . C47 C 0.3128(3) 0.38851(10) 0.51614(16) 0.0535(7) Uani 1 1 d . . . H47A H 0.2564 0.4176 0.4858 0.080 Uiso 1 1 calc R . . H47B H 0.3980 0.3814 0.4967 0.080 Uiso 1 1 calc R . . H47C H 0.3438 0.3987 0.5716 0.080 Uiso 1 1 calc R . . C48 C 0.1516(3) 0.33002(11) 0.41848(14) 0.0556(7) Uani 1 1 d . . . H48A H 0.0784 0.3018 0.4103 0.083 Uiso 1 1 calc R . . H48B H 0.2277 0.3199 0.3932 0.083 Uiso 1 1 calc R . . H48C H 0.1064 0.3634 0.3955 0.083 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 0.0345(3) 0.0297(3) 0.0310(3) 0.0005(2) 0.0035(2) -0.0026(2) P2 0.0317(3) 0.0316(3) 0.0438(3) -0.0008(3) 0.0086(3) -0.0016(2) P3 0.0309(3) 0.0262(3) 0.0312(3) -0.0019(2) 0.0036(2) 0.0005(2) P4 0.0319(3) 0.0366(3) 0.0269(3) -0.0059(2) 0.0056(2) 0.0010(2) O1 0.0520(10) 0.0301(8) 0.0437(9) 0.0001(7) 0.0084(8) -0.0038(7) O2 0.0346(9) 0.0516(10) 0.0621(11) 0.0074(8) 0.0030(8) 0.0031(8) O3 0.0466(10) 0.0274(8) 0.0469(9) 0.0000(7) 0.0053(8) -0.0001(7) O4 0.0471(10) 0.0811(13) 0.0358(9) -0.0127(9) 0.0172(8) 0.0083(9) C10 0.0315(12) 0.0428(13) 0.0385(13) -0.0045(10) 0.0051(10) -0.0059(10) C11 0.0500(15) 0.0375(13) 0.0386(13) 0.0047(10) -0.0031(11) -0.0020(11) C12 0.082(2) 0.084(2) 0.0420(16) 0.0185(15) 0.0056(15) -0.0127(17) C13 0.0649(19) 0.0393(15) 0.079(2) 0.0072(14) -0.0154(16) 0.0062(13) C14 0.0534(16) 0.0521(16) 0.0430(15) 0.0035(12) -0.0127(12) -0.0040(12) C15 0.0355(13) 0.0394(13) 0.0432(14) 0.0004(10) 0.0119(11) -0.0021(10) C16 0.0559(17) 0.0540(16) 0.0683(19) -0.0023(14) 0.0290(15) 0.0029(13) C17 0.0464(15) 0.0434(14) 0.0693(18) -0.0074(13) 0.0191(14) -0.0144(12) C18 0.0331(14) 0.0731(19) 0.0595(17) 0.0090(14) 0.0019(12) -0.0010(13) C21 0.0531(16) 0.0422(14) 0.0521(15) -0.0107(12) 0.0183(13) -0.0015(12) C22 0.093(2) 0.0582(19) 0.096(2) -0.0192(17) 0.060(2) -0.0069(17) C23 0.119(3) 0.132(3) 0.0494(19) -0.038(2) -0.014(2) 0.043(3) C24 0.121(3) 0.0504(18) 0.107(3) -0.0331(17) 0.072(2) -0.0269(18) C25 0.0433(14) 0.0302(12) 0.0545(15) -0.0004(11) 0.0190(12) -0.0017(10) C26 0.083(2) 0.0383(15) 0.108(3) 0.0073(15) 0.060(2) -0.0020(14) C27 0.090(2) 0.0450(16) 0.078(2) -0.0161(15) 0.0290(18) -0.0315(15) C28 0.071(2) 0.0446(16) 0.090(2) 0.0135(15) 0.0236(18) 0.0173(14) C30 0.0304(11) 0.0294(11) 0.0276(11) -0.0034(9) 0.0069(9) -0.0004(9) C31 0.0529(15) 0.0459(14) 0.0275(12) -0.0004(10) 0.0025(11) 0.0085(11) C32 0.074(2) 0.095(2) 0.0320(14) 0.0054(14) 0.0219(14) 0.0035(17) C33 0.087(2) 0.0655(19) 0.0370(15) 0.0051(13) -0.0071(15) 0.0190(16) C34 0.079(2) 0.0516(16) 0.0421(15) -0.0164(12) 0.0032(14) 0.0154(14) C35 0.0295(12) 0.0394(13) 0.0533(15) -0.0039(11) 0.0081(11) -0.0038(10) C36 0.0575(18) 0.0489(16) 0.097(2) 0.0142(16) 0.0275(17) -0.0106(13) C37 0.0341(15) 0.078(2) 0.083(2) -0.0021(17) 0.0000(15) -0.0018(14) C38 0.0441(16) 0.081(2) 0.0708(19) -0.0206(16) 0.0283(14) -0.0080(14) C41 0.0475(15) 0.0333(13) 0.0499(15) -0.0050(11) -0.0047(12) -0.0031(11) C42 0.070(2) 0.0476(16) 0.077(2) -0.0077(15) -0.0240(17) -0.0159(14) C43 0.0601(18) 0.0468(16) 0.080(2) 0.0116(14) 0.0151(16) -0.0186(13) C44 0.078(2) 0.0375(14) 0.0685(19) -0.0164(13) -0.0091(16) 0.0095(14) C45 0.0390(13) 0.0386(13) 0.0291(12) 0.0036(9) 0.0054(10) 0.0016(10) C46 0.0450(15) 0.0551(16) 0.0510(16) 0.0093(12) 0.0124(12) 0.0174(12) C47 0.0644(18) 0.0421(14) 0.0494(16) 0.0127(12) 0.0069(13) -0.0052(12) C48 0.0602(17) 0.0659(18) 0.0339(14) 0.0038(12) -0.0001(12) 0.0035(14) _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 1.4875(16) . ? P1 C10 1.837(2) . ? P1 C11 1.851(2) . ? P1 C15 1.865(2) . ? P2 O2 1.4813(17) . ? P2 C10 1.833(2) . ? P2 C25 1.856(2) . ? P2 C21 1.865(2) . ? P3 O3 1.4869(15) . ? P3 C30 1.833(2) . ? P3 C31 1.860(2) . ? P3 C35 1.861(2) . ? P4 O4 1.4832(16) . ? P4 C30 1.831(2) . ? P4 C41 1.861(2) . ? P4 C45 1.864(2) . ? C11 C12 1.528(4) . ? C11 C14 1.534(3) . ? C11 C13 1.541(3) . ? C15 C17 1.533(3) . ? C15 C18 1.536(3) . ? C15 C16 1.542(3) . ? C21 C24 1.517(4) . ? C21 C23 1.523(4) . ? C21 C22 1.540(4) . ? C25 C28 1.517(4) . ? C25 C26 1.530(3) . ? C25 C27 1.534(4) . ? C31 C34 1.536(3) . ? C31 C33 1.540(3) . ? C31 C32 1.544(4) . ? C35 C38 1.530(3) . ? C35 C37 1.533(3) . ? C35 C36 1.537(3) . ? C41 C43 1.531(4) . ? C41 C42 1.540(3) . ? C41 C44 1.543(3) . ? C45 C46 1.525(3) . ? C45 C48 1.542(3) . ? C45 C47 1.544(3) . ? 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 C10 113.42(10) . . ? O1 P1 C11 112.24(10) . . ? C10 P1 C11 106.14(11) . . ? O1 P1 C15 108.94(10) . . ? C10 P1 C15 102.96(10) . . ? C11 P1 C15 112.83(11) . . ? O2 P2 C10 114.86(11) . . ? O2 P2 C25 110.95(11) . . ? C10 P2 C25 107.47(11) . . ? O2 P2 C21 109.08(11) . . ? C10 P2 C21 101.69(11) . . ? C25 P2 C21 112.53(11) . . ? O3 P3 C30 114.67(9) . . ? O3 P3 C31 109.08(10) . . ? C30 P3 C31 102.72(10) . . ? O3 P3 C35 111.18(10) . . ? C30 P3 C35 105.99(10) . . ? C31 P3 C35 113.00(11) . . ? O4 P4 C30 114.53(10) . . ? O4 P4 C41 111.08(11) . . ? C30 P4 C41 106.68(10) . . ? O4 P4 C45 108.80(10) . . ? C30 P4 C45 102.61(10) . . ? C41 P4 C45 112.96(11) . . ? P2 C10 P1 128.12(12) . . ? C12 C11 C14 107.4(2) . . ? C12 C11 C13 111.4(2) . . ? C14 C11 C13 108.0(2) . . ? C12 C11 P1 110.60(19) . . ? C14 C11 P1 107.00(16) . . ? C13 C11 P1 112.23(17) . . ? C17 C15 C18 108.7(2) . . ? C17 C15 C16 109.6(2) . . ? C18 C15 C16 106.7(2) . . ? C17 C15 P1 115.43(16) . . ? C18 C15 P1 107.48(16) . . ? C16 C15 P1 108.57(17) . . ? C24 C21 C23 110.2(3) . . ? C24 C21 C22 105.4(2) . . ? C23 C21 C22 109.0(3) . . ? C24 C21 P2 107.58(19) . . ? C23 C21 P2 115.45(19) . . ? C22 C21 P2 108.63(19) . . ? C28 C25 C26 110.5(2) . . ? C28 C25 C27 108.1(2) . . ? C26 C25 C27 107.5(2) . . ? C28 C25 P2 113.18(17) . . ? C26 C25 P2 110.82(16) . . ? C27 C25 P2 106.53(17) . . ? P4 C30 P3 124.79(11) . . ? C34 C31 C33 109.5(2) . . ? C34 C31 C32 109.6(2) . . ? C33 C31 C32 106.7(2) . . ? C34 C31 P3 114.16(17) . . ? C33 C31 P3 109.32(17) . . ? C32 C31 P3 107.23(17) . . ? C38 C35 C37 107.9(2) . . ? C38 C35 C36 108.3(2) . . ? C37 C35 C36 109.9(2) . . ? C38 C35 P3 106.08(16) . . ? C37 C35 P3 110.49(18) . . ? C36 C35 P3 113.97(17) . . ? C43 C41 C42 109.6(2) . . ? C43 C41 C44 108.8(2) . . ? C42 C41 C44 107.7(2) . . ? C43 C41 P4 113.28(17) . . ? C42 C41 P4 111.24(18) . . ? C44 C41 P4 105.98(19) . . ? C46 C45 C48 111.2(2) . . ? C46 C45 C47 108.7(2) . . ? C48 C45 C47 106.52(19) . . ? C46 C45 P4 114.27(15) . . ? C48 C45 P4 109.12(16) . . ? C47 C45 P4 106.63(16) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 25.62 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.425 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.042 #===END data_ig7_dtbpmH+_8 _database_code_CSD 199939 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common dtbpmH+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H51 B F24 P2' _chemical_formula_weight 1168.65 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 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 16.79070(10) _cell_length_b 19.1459(2) _cell_length_c 18.2699(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.5520(10) _cell_angle_gamma 90.00 _cell_volume 5384.02(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9431 _exptl_absorpt_correction_T_max 0.9863 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 47177 _diffrn_reflns_av_R_equivalents 0.0671 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.33 _reflns_number_total 9828 _reflns_number_gt 5980 _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^)+(0.0464P)^2^+2.5364P] 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 9828 _refine_ls_number_parameters 813 _refine_ls_number_restraints 1990 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0470 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 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 0.22878(5) 0.36989(4) 0.49209(4) 0.03398(18) Uani 1 1 d . . . H1 H 0.1772(15) 0.4143(12) 0.5092(14) 0.036(7) Uiso 1 1 d . . . P2 P 0.08312(5) 0.37367(4) 0.31611(4) 0.0385(2) Uani 1 1 d . . . C10 C 0.20104(16) 0.37499(15) 0.38603(15) 0.0345(6) Uani 1 1 d . . . H10A H 0.2299 0.3355 0.3715 0.041 Uiso 1 1 calc R . . H10B H 0.2268 0.4185 0.3758 0.041 Uiso 1 1 calc R . . C11 C 0.20481(19) 0.28307(15) 0.52175(17) 0.0406(7) Uani 1 1 d . . . C12 C 0.2351(3) 0.22534(16) 0.4802(2) 0.0686(11) Uani 1 1 d . . . H12A H 0.2256 0.1796 0.4993 0.103 Uiso 1 1 calc R . . H12B H 0.2971 0.2313 0.4925 0.103 Uiso 1 1 calc R . . H12C H 0.2020 0.2283 0.4224 0.103 Uiso 1 1 calc R . . C13 C 0.2489(2) 0.27302(18) 0.61280(19) 0.0651(10) Uani 1 1 d . . . H13A H 0.2342 0.3123 0.6395 0.098 Uiso 1 1 calc R . . H13B H 0.3120 0.2710 0.6294 0.098 Uiso 1 1 calc R . . H13C H 0.2286 0.2294 0.6275 0.098 Uiso 1 1 calc R . . C14 C 0.1070(2) 0.2792(2) 0.4969(2) 0.0720(11) Uani 1 1 d . . . H14A H 0.0777 0.2840 0.4388 0.108 Uiso 1 1 calc R . . H14B H 0.0885 0.3170 0.5227 0.108 Uiso 1 1 calc R . . H14C H 0.0919 0.2341 0.5133 0.108 Uiso 1 1 calc R . . C15 C 0.33899(18) 0.40515(15) 0.54697(16) 0.0388(7) Uani 1 1 d . . . C16 C 0.3515(2) 0.4220(2) 0.63303(19) 0.0656(10) Uani 1 1 d . . . H16A H 0.3553 0.3784 0.6624 0.098 Uiso 1 1 calc R . . H16B H 0.3021 0.4495 0.6325 0.098 Uiso 1 1 calc R . . H16C H 0.4052 0.4489 0.6592 0.098 Uiso 1 1 calc R . . C17 C 0.4086(2) 0.35538(19) 0.5452(2) 0.0696(11) Uani 1 1 d . . . H17A H 0.4657 0.3775 0.5707 0.104 Uiso 1 1 calc R . . H17B H 0.3976 0.3440 0.4897 0.104 Uiso 1 1 calc R . . H17C H 0.4074 0.3125 0.5740 0.104 Uiso 1 1 calc R . . C18 C 0.3450(2) 0.47457(18) 0.5079(2) 0.0728(11) Uani 1 1 d . . . H18A H 0.2946 0.5036 0.5015 0.109 Uiso 1 1 calc R . . H18B H 0.3459 0.4656 0.4554 0.109 Uiso 1 1 calc R . . H18C H 0.3984 0.4990 0.5417 0.109 Uiso 1 1 calc R . . C21 C 0.09291(19) 0.33424(16) 0.22549(17) 0.0441(8) Uani 1 1 d . . . C22 C 0.0075(2) 0.3455(2) 0.15238(19) 0.0757(11) Uani 1 1 d . . . H22A H 0.0066 0.3156 0.1085 0.113 Uiso 1 1 calc R . . H22B H 0.0029 0.3946 0.1358 0.113 Uiso 1 1 calc R . . H22C H -0.0416 0.3335 0.1661 0.113 Uiso 1 1 calc R . . C23 C 0.1685(2) 0.35930(19) 0.2053(2) 0.0621(10) Uani 1 1 d . . . H23A H 0.1682 0.3336 0.1588 0.093 Uiso 1 1 calc R . . H23B H 0.2235 0.3509 0.2510 0.093 Uiso 1 1 calc R . . H23C H 0.1621 0.4094 0.1932 0.093 Uiso 1 1 calc R . . C24 C 0.1046(3) 0.25550(18) 0.2419(2) 0.0700(11) Uani 1 1 d . . . H24A H 0.0572 0.2378 0.2551 0.105 Uiso 1 1 calc R . . H24B H 0.1603 0.2469 0.2867 0.105 Uiso 1 1 calc R . . H24C H 0.1039 0.2315 0.1942 0.105 Uiso 1 1 calc R . . C25 C 0.0550(2) 0.46924(16) 0.29924(19) 0.0492(8) Uani 1 1 d . . . C26 C 0.0990(2) 0.51163(18) 0.2550(2) 0.0727(11) Uani 1 1 d . . . H26A H 0.0847 0.5612 0.2559 0.109 Uiso 1 1 calc R . . H26B H 0.0784 0.4955 0.1996 0.109 Uiso 1 1 calc R . . H26C H 0.1621 0.5054 0.2813 0.109 Uiso 1 1 calc R . . C27 C 0.0772(2) 0.50186(18) 0.3816(2) 0.0707(11) Uani 1 1 d . . . H27A H 0.1403 0.5068 0.4093 0.106 Uiso 1 1 calc R . . H27B H 0.0555 0.4717 0.4130 0.106 Uiso 1 1 calc R . . H27C H 0.0498 0.5479 0.3753 0.106 Uiso 1 1 calc R . . C28 C -0.0442(2) 0.4738(2) 0.2536(2) 0.0709(11) Uani 1 1 d . . . H28A H -0.0625 0.5228 0.2498 0.106 Uiso 1 1 calc R . . H28B H -0.0726 0.4470 0.2821 0.106 Uiso 1 1 calc R . . H28C H -0.0607 0.4546 0.1998 0.106 Uiso 1 1 calc R . . B1 B 0.40382(18) 0.32130(15) 0.10182(17) 0.0255(7) Uani 1 1 d . . . C31 C 0.33809(16) 0.26273(13) 0.04239(14) 0.0277(6) Uani 1 1 d . . . C32 C 0.36760(17) 0.21556(13) 0.00016(15) 0.0313(6) Uani 1 1 d . . . H32 H 0.4250 0.2206 0.0029 0.038 Uiso 1 1 calc R . . C33 C 0.31635(18) 0.16186(14) -0.04540(16) 0.0367(7) Uani 1 1 d D A . C34 C 0.23254(19) 0.15217(14) -0.05012(16) 0.0402(7) Uani 1 1 d . . . H34 H 0.1966 0.1162 -0.0824 0.048 Uiso 1 1 calc R . . C35 C 0.20268(16) 0.19597(14) -0.00684(16) 0.0333(6) Uani 1 1 d D . . C36 C 0.25419(16) 0.25034(13) 0.03790(15) 0.0306(6) Uani 1 1 d . . . H36 H 0.2315 0.2802 0.0665 0.037 Uiso 1 1 calc R . . C37 C 0.3517(2) 0.11450(18) -0.0901(2) 0.0580(9) Uani 1 1 d DU . . F31 F 0.3192(5) 0.0508(2) -0.0986(6) 0.087(2) Uani 0.675(17) 1 d PDU A 1 F32 F 0.3386(8) 0.1364(6) -0.1611(4) 0.129(4) Uani 0.675(17) 1 d PDU A 1 F33 F 0.4360(3) 0.1043(4) -0.0527(5) 0.100(3) Uani 0.675(17) 1 d PDU A 1 C38 C 0.11652(19) 0.18217(16) -0.00435(19) 0.0478(8) Uani 1 1 d DU . . F34 F 0.12204(12) 0.13924(12) 0.05435(13) 0.0866(7) Uani 1 1 d DU . . F35 F 0.05957(12) 0.15272(11) -0.07084(13) 0.0750(6) Uani 1 1 d DU . . F36 F 0.07738(11) 0.23998(10) 0.00541(13) 0.0709(6) Uani 1 1 d DU . . C41 C 0.35206(15) 0.38783(13) 0.11884(14) 0.0250(6) Uani 1 1 d . . . C42 C 0.27822(16) 0.41691(13) 0.05888(15) 0.0268(6) Uani 1 1 d . . . H42 H 0.2555 0.3957 0.0076 0.032 Uiso 1 1 calc R . . C43 C 0.23690(16) 0.47570(13) 0.07163(15) 0.0283(6) Uani 1 1 d D B . C44 C 0.26892(16) 0.50895(13) 0.14503(15) 0.0307(6) Uani 1 1 d . . . H44 H 0.2411 0.5493 0.1539 0.037 Uiso 1 1 calc R . . C45 C 0.34248(16) 0.48182(13) 0.20509(14) 0.0282(6) Uani 1 1 d D C . C46 C 0.38275(16) 0.42248(13) 0.19241(15) 0.0274(6) Uani 1 1 d . . . H46 H 0.4327 0.4048 0.2350 0.033 Uiso 1 1 calc R . . C47 C 0.15572(19) 0.50304(16) 0.00760(17) 0.0446(7) Uani 1 1 d DU . . F41 F 0.1570(10) 0.5690(4) -0.0065(8) 0.114(4) Uani 0.49(2) 1 d PDU B 1 F42 F 0.0876(7) 0.4953(11) 0.0251(9) 0.134(6) Uani 0.49(2) 1 d PDU B 1 F43 F 0.1345(9) 0.4696(7) -0.0598(5) 0.067(3) Uani 0.49(2) 1 d PDU B 1 C48 C 0.37641(19) 0.51676(16) 0.28471(17) 0.0416(7) Uani 1 1 d DU . . F44 F 0.4128(5) 0.5781(4) 0.2841(5) 0.077(2) Uani 0.577(17) 1 d PDU C 1 F45 F 0.4373(6) 0.4824(4) 0.3425(4) 0.081(3) Uani 0.577(17) 1 d PDU C 1 F46 F 0.3173(4) 0.5315(5) 0.3116(5) 0.074(2) Uani 0.577(17) 1 d PDU C 1 C51 C 0.45578(15) 0.27660(12) 0.18376(14) 0.0256(6) Uani 1 1 d . . . C52 C 0.41286(16) 0.25831(13) 0.23349(15) 0.0299(6) Uani 1 1 d . . . H52 H 0.3563 0.2764 0.2212 0.036 Uiso 1 1 calc R . . C54 C 0.53247(17) 0.18812(13) 0.32003(15) 0.0326(6) Uani 1 1 d . . . H54 H 0.5582 0.1590 0.3655 0.039 Uiso 1 1 calc R . . C55 C 0.57648(16) 0.20482(13) 0.27260(15) 0.0303(6) Uani 1 1 d D . . C56 C 0.53825(16) 0.24763(13) 0.20590(15) 0.0287(6) Uani 1 1 d . . . H56 H 0.5699 0.2575 0.1741 0.034 Uiso 1 1 calc R . . C53 C 0.44941(17) 0.21520(13) 0.29930(15) 0.0311(6) Uani 1 1 d D . . C57 C 0.3974(2) 0.19802(16) 0.34663(18) 0.0433(7) Uani 1 1 d DU . . F51 F 0.43871(13) 0.15858(11) 0.40963(12) 0.0803(7) Uani 1 1 d DU . . F52 F 0.32370(12) 0.16475(10) 0.30342(12) 0.0699(6) Uani 1 1 d DU . . F53 F 0.37225(13) 0.25522(10) 0.37378(12) 0.0682(6) Uani 1 1 d DU . . C58 C 0.66542(19) 0.17671(15) 0.29119(17) 0.0421(7) Uani 1 1 d DU . . F54 F 0.72194(11) 0.22636(10) 0.29279(12) 0.0659(5) Uani 1 1 d DU . . F55 F 0.69928(13) 0.14360(12) 0.36067(11) 0.0829(7) Uani 1 1 d DU . . F56 F 0.66682(11) 0.13149(9) 0.23629(11) 0.0633(5) Uani 1 1 d DU . . C61 C 0.46832(16) 0.35624(12) 0.06433(14) 0.0260(6) Uani 1 1 d . . . C62 C 0.54725(16) 0.38769(13) 0.11246(16) 0.0315(6) Uani 1 1 d . . . H62 H 0.5654 0.3859 0.1688 0.038 Uiso 1 1 calc R . . C63 C 0.60037(17) 0.42144(13) 0.08139(17) 0.0344(7) Uani 1 1 d D . . C64 C 0.57571(19) 0.42520(14) -0.00040(17) 0.0388(7) Uani 1 1 d . . . H64 H 0.6115 0.4482 -0.0221 0.047 Uiso 1 1 calc R . . C65 C 0.49833(18) 0.39506(14) -0.04985(15) 0.0339(7) Uani 1 1 d D D . C66 C 0.44546(16) 0.36192(13) -0.01794(15) 0.0288(6) Uani 1 1 d . . . H66 H 0.3919 0.3425 -0.0534 0.035 Uiso 1 1 calc R . . C67 C 0.6859(2) 0.45059(16) 0.1360(2) 0.0502(8) Uani 1 1 d DU . . F61 F 0.69090(13) 0.46433(12) 0.20887(13) 0.0862(7) Uani 1 1 d DU . . F62 F 0.75086(12) 0.40670(11) 0.14721(16) 0.0965(8) Uani 1 1 d DU . . F63 F 0.70564(14) 0.50977(11) 0.10994(13) 0.0895(7) Uani 1 1 d DU . . C68 C 0.4741(2) 0.39483(17) -0.13798(18) 0.0490(8) Uani 1 1 d DU . . F64 F 0.5063(14) 0.3428(10) -0.1629(12) 0.107(5) Uani 0.45(3) 1 d PDU D 1 F65 F 0.3872(4) 0.3891(8) -0.1784(6) 0.071(3) Uani 0.45(3) 1 d PDU D 1 F66 F 0.4956(13) 0.4511(7) -0.1652(9) 0.099(5) Uani 0.45(3) 1 d PDU D 1 F41B F 0.1151(10) 0.4621(7) -0.0515(7) 0.105(5) Uani 0.51(2) 1 d PDU B 2 F42B F 0.1713(8) 0.5607(6) -0.0236(8) 0.119(4) Uani 0.51(2) 1 d PDU B 2 F43B F 0.0978(7) 0.5198(7) 0.0354(7) 0.088(3) Uani 0.51(2) 1 d PDU B 2 F44B F 0.3397(12) 0.4905(12) 0.3292(7) 0.133(7) Uani 0.423(17) 1 d PDU C 2 F45B F 0.3643(18) 0.5831(5) 0.2820(7) 0.167(8) Uani 0.423(17) 1 d PDU C 2 F46B F 0.4569(5) 0.5057(10) 0.3241(8) 0.106(5) Uani 0.423(17) 1 d PDU C 2 F31B F 0.3785(16) 0.1512(8) -0.1362(13) 0.101(6) Uani 0.325(17) 1 d PDU A 2 F32B F 0.4194(15) 0.0793(13) -0.0467(8) 0.177(9) Uani 0.325(17) 1 d PDU A 2 F33B F 0.2957(12) 0.0731(15) -0.1406(16) 0.170(10) Uani 0.325(17) 1 d PDU A 2 F64B F 0.4748(9) 0.4570(4) -0.1680(6) 0.068(3) Uani 0.55(3) 1 d PDU D 2 F65B F 0.5347(12) 0.3612(11) -0.1540(10) 0.128(6) Uani 0.55(3) 1 d PDU D 2 F66B F 0.4025(10) 0.3649(10) -0.1808(6) 0.131(5) Uani 0.55(3) 1 d PDU D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0318(4) 0.0388(4) 0.0302(4) 0.0040(3) 0.0112(3) -0.0009(3) P2 0.0297(4) 0.0494(5) 0.0334(4) 0.0084(4) 0.0094(3) -0.0012(4) C10 0.0322(15) 0.0376(16) 0.0343(16) 0.0035(13) 0.0140(13) -0.0012(13) C11 0.0439(18) 0.0415(18) 0.0414(18) 0.0096(14) 0.0223(15) -0.0010(14) C12 0.108(3) 0.041(2) 0.075(3) 0.0062(18) 0.056(2) -0.003(2) C13 0.085(3) 0.067(2) 0.048(2) 0.0201(18) 0.031(2) 0.002(2) C14 0.053(2) 0.077(3) 0.085(3) 0.029(2) 0.027(2) -0.0160(19) C15 0.0353(17) 0.0471(18) 0.0307(16) -0.0024(13) 0.0097(13) -0.0068(14) C16 0.057(2) 0.092(3) 0.040(2) -0.0155(19) 0.0109(17) -0.013(2) C17 0.0337(19) 0.087(3) 0.085(3) -0.031(2) 0.0204(19) -0.0043(18) C18 0.069(3) 0.067(2) 0.062(2) 0.0001(19) 0.0045(19) -0.035(2) C21 0.0453(19) 0.050(2) 0.0326(17) 0.0008(14) 0.0112(14) -0.0090(15) C22 0.067(3) 0.102(3) 0.040(2) -0.003(2) 0.0034(18) -0.011(2) C23 0.072(2) 0.076(3) 0.050(2) -0.0019(18) 0.0377(19) -0.0071(19) C24 0.098(3) 0.059(2) 0.051(2) -0.0079(18) 0.029(2) -0.010(2) C25 0.0423(18) 0.054(2) 0.051(2) 0.0141(16) 0.0175(16) 0.0103(15) C26 0.079(3) 0.051(2) 0.096(3) 0.029(2) 0.043(2) 0.0104(19) C27 0.078(3) 0.053(2) 0.074(3) 0.0066(19) 0.023(2) 0.0264(19) C28 0.046(2) 0.097(3) 0.067(2) 0.031(2) 0.0206(18) 0.029(2) B1 0.0234(16) 0.0306(17) 0.0234(16) 0.0008(13) 0.0105(13) 0.0028(13) C31 0.0291(15) 0.0305(15) 0.0232(14) 0.0048(11) 0.0102(12) 0.0024(12) C32 0.0287(15) 0.0347(16) 0.0329(16) -0.0015(13) 0.0148(13) 0.0006(12) C33 0.0415(18) 0.0338(16) 0.0389(17) -0.0063(13) 0.0204(14) -0.0035(13) C34 0.0441(19) 0.0362(17) 0.0389(17) -0.0065(13) 0.0152(15) -0.0111(14) C35 0.0306(16) 0.0352(16) 0.0329(16) 0.0035(13) 0.0114(13) -0.0027(13) C36 0.0327(15) 0.0299(15) 0.0309(15) 0.0024(12) 0.0145(12) 0.0035(12) C37 0.068(3) 0.055(2) 0.063(2) -0.0219(19) 0.040(2) -0.0108(19) F31 0.108(4) 0.044(3) 0.139(5) -0.049(3) 0.082(4) -0.024(2) F32 0.237(11) 0.104(6) 0.081(4) -0.005(4) 0.100(5) 0.044(6) F33 0.052(3) 0.095(4) 0.167(6) -0.083(4) 0.056(3) -0.011(3) C38 0.0375(18) 0.048(2) 0.057(2) -0.0007(16) 0.0177(16) -0.0056(15) F34 0.0561(13) 0.1141(18) 0.1008(17) 0.0519(14) 0.0430(12) -0.0013(12) F35 0.0406(11) 0.0859(15) 0.0900(15) -0.0240(12) 0.0171(11) -0.0231(10) F36 0.0433(11) 0.0645(13) 0.1148(17) -0.0171(11) 0.0418(11) -0.0041(9) C41 0.0229(14) 0.0280(14) 0.0257(14) 0.0031(11) 0.0114(12) -0.0027(11) C42 0.0291(15) 0.0292(15) 0.0227(14) -0.0021(11) 0.0110(12) -0.0021(12) C43 0.0269(14) 0.0296(15) 0.0284(15) 0.0024(12) 0.0111(12) 0.0020(12) C44 0.0333(16) 0.0259(15) 0.0391(16) -0.0040(12) 0.0209(13) -0.0011(12) C45 0.0271(15) 0.0310(15) 0.0278(15) -0.0062(12) 0.0124(12) -0.0082(12) C46 0.0235(14) 0.0331(15) 0.0242(14) 0.0000(12) 0.0079(11) -0.0014(11) C47 0.0404(19) 0.048(2) 0.0394(19) 0.0001(16) 0.0100(15) 0.0099(16) F41 0.114(9) 0.028(4) 0.120(7) -0.005(4) -0.036(5) 0.028(4) F42 0.035(4) 0.286(17) 0.076(7) 0.048(9) 0.018(4) 0.025(7) F43 0.060(5) 0.093(5) 0.022(3) -0.004(3) -0.012(3) 0.041(4) C48 0.0380(18) 0.0449(19) 0.0405(18) -0.0114(15) 0.0140(15) -0.0013(15) F44 0.110(5) 0.060(4) 0.064(3) -0.030(3) 0.038(4) -0.052(3) F45 0.106(6) 0.075(4) 0.031(2) -0.009(2) -0.004(3) 0.038(4) F46 0.046(3) 0.131(6) 0.048(4) -0.045(4) 0.024(2) -0.002(3) C51 0.0256(14) 0.0250(14) 0.0262(14) -0.0016(11) 0.0102(11) -0.0008(11) C52 0.0266(14) 0.0328(15) 0.0317(15) -0.0012(12) 0.0130(12) 0.0021(12) C54 0.0410(17) 0.0286(15) 0.0267(15) 0.0051(12) 0.0120(13) 0.0032(13) C55 0.0312(15) 0.0298(15) 0.0286(15) 0.0004(12) 0.0105(13) 0.0023(12) C56 0.0289(15) 0.0321(15) 0.0270(14) 0.0003(12) 0.0132(12) -0.0002(12) C53 0.0344(16) 0.0311(15) 0.0308(15) -0.0012(12) 0.0162(13) -0.0019(12) C57 0.049(2) 0.0457(19) 0.0421(19) 0.0073(15) 0.0256(16) -0.0012(15) F51 0.0802(15) 0.1054(17) 0.0714(14) 0.0529(13) 0.0474(12) 0.0166(12) F52 0.0623(13) 0.0863(15) 0.0734(13) -0.0113(11) 0.0401(11) -0.0346(11) F53 0.0957(15) 0.0635(13) 0.0785(14) -0.0078(10) 0.0695(13) -0.0026(11) C58 0.0417(18) 0.0445(19) 0.0393(18) 0.0103(15) 0.0153(15) 0.0109(15) F54 0.0331(10) 0.0619(12) 0.0957(15) 0.0039(11) 0.0184(10) 0.0003(9) F55 0.0633(13) 0.1282(19) 0.0619(13) 0.0540(13) 0.0299(11) 0.0543(13) F56 0.0558(12) 0.0623(12) 0.0768(13) -0.0130(10) 0.0318(10) 0.0164(9) C61 0.0253(14) 0.0257(14) 0.0260(14) -0.0005(11) 0.0093(12) 0.0047(11) C62 0.0326(16) 0.0300(15) 0.0315(15) -0.0006(12) 0.0124(13) 0.0026(12) C63 0.0306(16) 0.0265(15) 0.0480(19) -0.0007(13) 0.0175(14) -0.0014(12) C64 0.0431(18) 0.0352(17) 0.0486(19) 0.0024(14) 0.0295(16) -0.0020(14) C65 0.0444(18) 0.0316(15) 0.0325(16) 0.0027(12) 0.0226(14) 0.0048(13) C66 0.0280(14) 0.0276(15) 0.0302(15) -0.0006(12) 0.0111(12) 0.0025(11) C67 0.0397(19) 0.0438(19) 0.065(2) -0.0050(17) 0.0194(17) -0.0109(15) F61 0.0605(14) 0.1188(19) 0.0666(14) -0.0276(13) 0.0119(11) -0.0369(13) F62 0.0348(12) 0.0781(15) 0.151(2) -0.0289(14) 0.0101(13) -0.0022(11) F63 0.0791(15) 0.0686(14) 0.1014(17) 0.0078(12) 0.0156(13) -0.0426(12) C68 0.070(2) 0.046(2) 0.0429(19) 0.0041(16) 0.0354(19) -0.0003(18) F64 0.166(10) 0.103(7) 0.051(5) -0.010(5) 0.042(7) 0.069(7) F65 0.050(4) 0.134(7) 0.023(4) 0.010(4) 0.008(3) 0.008(5) F66 0.133(9) 0.111(8) 0.070(7) 0.022(6) 0.058(6) -0.055(8) F41B 0.065(6) 0.085(6) 0.102(8) -0.055(6) -0.034(5) 0.031(4) F42B 0.072(5) 0.120(7) 0.125(7) 0.101(7) -0.004(5) 0.001(5) F43B 0.038(4) 0.138(7) 0.072(5) -0.029(4) 0.005(3) 0.048(4) F44B 0.138(11) 0.235(15) 0.053(6) -0.065(8) 0.066(8) -0.120(10) F45B 0.32(2) 0.053(5) 0.066(6) -0.032(4) 0.005(10) 0.054(8) F46B 0.035(4) 0.193(13) 0.065(8) -0.087(7) -0.007(4) -0.009(5) F31B 0.164(15) 0.075(7) 0.138(13) -0.023(7) 0.138(13) -0.005(7) F32B 0.275(18) 0.149(15) 0.078(9) 0.003(8) 0.041(10) 0.153(14) F33B 0.156(12) 0.23(2) 0.183(17) -0.182(15) 0.131(11) -0.133(13) F64B 0.121(6) 0.047(4) 0.037(4) 0.012(3) 0.031(4) 0.021(4) F65B 0.197(10) 0.156(10) 0.067(8) 0.026(6) 0.092(8) 0.101(8) F66B 0.188(9) 0.172(10) 0.044(4) -0.039(6) 0.059(6) -0.129(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 P1 C10 1.806(3) . ? P1 C11 1.842(3) . ? P1 C15 1.845(3) . ? P1 H1 1.34(2) . ? P2 C10 1.879(3) . ? P2 C25 1.884(3) . ? P2 C21 1.886(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C14 1.520(4) . ? C11 C12 1.538(4) . ? C11 C13 1.539(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.519(4) . ? C15 C18 1.531(4) . ? C15 C16 1.535(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 C23 1.533(4) . ? C21 C24 1.534(4) . ? C21 C22 1.535(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.527(4) . ? C25 C27 1.532(4) . ? C25 C28 1.539(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? B1 C61 1.638(4) . ? B1 C41 1.640(4) . ? B1 C51 1.640(4) . ? B1 C31 1.642(4) . ? C31 C36 1.398(3) . ? C31 C32 1.401(3) . ? C32 C33 1.385(4) . ? C32 H32 0.9500 . ? C33 C34 1.388(4) . ? C33 C37 1.494(4) . ? C34 C35 1.377(4) . ? C34 H34 0.9500 . ? C35 C36 1.391(4) . ? C35 C38 1.489(4) . ? C36 H36 0.9500 . ? C37 F32B 1.285(10) . ? C37 F33B 1.293(10) . ? C37 F32 1.294(7) . ? C37 F31B 1.306(10) . ? C37 F33 1.316(6) . ? C37 F31 1.320(6) . ? C38 F34 1.325(3) . ? C38 F35 1.334(3) . ? C38 F36 1.335(3) . ? C41 C46 1.399(3) . ? C41 C42 1.401(3) . ? C42 C43 1.390(3) . ? C42 H42 0.9500 . ? C43 C44 1.384(3) . ? C43 C47 1.492(4) . ? C44 C45 1.384(3) . ? C44 H44 0.9500 . ? C45 C46 1.388(3) . ? C45 C48 1.492(4) . ? C46 H46 0.9500 . ? C47 F41B 1.287(9) . ? C47 F41 1.291(8) . ? C47 F43B 1.304(8) . ? C47 F43 1.305(8) . ? C47 F42 1.313(9) . ? C47 F42B 1.315(7) . ? C48 F46B 1.270(8) . ? C48 F45B 1.283(8) . ? C48 F44B 1.301(8) . ? C48 F46 1.303(6) . ? C48 F45 1.316(6) . ? C48 F44 1.326(6) . ? C51 C56 1.393(3) . ? C51 C52 1.411(3) . ? C52 C53 1.383(3) . ? C52 H52 0.9500 . ? C54 C55 1.382(3) . ? C54 C53 1.391(4) . ? C54 H54 0.9500 . ? C55 C56 1.394(3) . ? C55 C58 1.493(4) . ? C56 H56 0.9500 . ? C53 C57 1.490(4) . ? C57 F51 1.318(3) . ? C57 F52 1.334(3) . ? C57 F53 1.339(3) . ? C58 F55 1.326(3) . ? C58 F56 1.332(3) . ? C58 F54 1.335(3) . ? C61 C66 1.399(3) . ? C61 C62 1.400(3) . ? C62 C63 1.393(4) . ? C62 H62 0.9500 . ? C63 C64 1.384(4) . ? C63 C67 1.491(4) . ? C64 C65 1.378(4) . ? C64 H64 0.9500 . ? C65 C66 1.394(3) . ? C65 C68 1.495(4) . ? C66 H66 0.9500 . ? C67 F63 1.322(3) . ? C67 F61 1.326(4) . ? C67 F62 1.327(3) . ? C68 F66B 1.278(8) . ? C68 F66 1.296(9) . ? C68 F64 1.300(10) . ? C68 F64B 1.313(7) . ? C68 F65B 1.333(9) . ? C68 F65 1.350(8) . ? 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 C10 P1 C11 111.81(13) . . ? C10 P1 C15 109.64(12) . . ? C11 P1 C15 117.39(13) . . ? C10 P1 H1 107.6(10) . . ? C11 P1 H1 105.5(10) . . ? C15 P1 H1 104.1(10) . . ? C10 P2 C25 103.02(13) . . ? C10 P2 C21 99.47(13) . . ? C25 P2 C21 110.44(14) . . ? P1 C10 P2 118.60(14) . . ? P1 C10 H10A 107.7 . . ? P2 C10 H10A 107.7 . . ? P1 C10 H10B 107.7 . . ? P2 C10 H10B 107.7 . . ? H10A C10 H10B 107.1 . . ? C14 C11 C12 110.4(3) . . ? C14 C11 C13 108.2(3) . . ? C12 C11 C13 109.4(3) . . ? C14 C11 P1 107.1(2) . . ? C12 C11 P1 110.4(2) . . ? C13 C11 P1 111.3(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C18 109.9(3) . . ? C17 C15 C16 111.3(3) . . ? C18 C15 C16 106.7(3) . . ? C17 C15 P1 111.9(2) . . ? C18 C15 P1 107.6(2) . . ? C16 C15 P1 109.3(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C23 C21 C24 107.5(3) . . ? C23 C21 C22 108.8(3) . . ? C24 C21 C22 108.1(3) . . ? C23 C21 P2 117.2(2) . . ? C24 C21 P2 105.8(2) . . ? C22 C21 P2 109.2(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C27 108.9(3) . . ? C26 C25 C28 109.3(3) . . ? C27 C25 C28 107.1(3) . . ? C26 C25 P2 117.4(2) . . ? C27 C25 P2 106.8(2) . . ? C28 C25 P2 106.9(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C61 B1 C41 104.5(2) . . ? C61 B1 C51 113.3(2) . . ? C41 B1 C51 111.2(2) . . ? C61 B1 C31 112.6(2) . . ? C41 B1 C31 112.9(2) . . ? C51 B1 C31 102.7(2) . . ? C36 C31 C32 115.4(2) . . ? C36 C31 B1 123.4(2) . . ? C32 C31 B1 120.8(2) . . ? C33 C32 C31 122.6(2) . . ? C33 C32 H32 118.7 . . ? C31 C32 H32 118.7 . . ? C32 C33 C34 120.5(2) . . ? C32 C33 C37 119.5(3) . . ? C34 C33 C37 120.0(3) . . ? C35 C34 C33 118.4(2) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? C34 C35 C36 120.6(2) . . ? C34 C35 C38 119.4(3) . . ? C36 C35 C38 119.9(2) . . ? C35 C36 C31 122.5(2) . . ? C35 C36 H36 118.8 . . ? C31 C36 H36 118.8 . . ? F32B C37 F33B 109.3(11) . . ? F32B C37 F32 122.9(10) . . ? F33B C37 F32 72.5(12) . . ? F32B C37 F31B 103.5(11) . . ? F33B C37 F31B 102.1(10) . . ? F32 C37 F31B 31.3(10) . . ? F32B C37 F33 26.0(14) . . ? F33B C37 F33 127.2(13) . . ? F32 C37 F33 106.6(6) . . ? F31B C37 F33 80.8(11) . . ? F32B C37 F31 79.1(13) . . ? F33B C37 F31 36.9(15) . . ? F32 C37 F31 106.5(5) . . ? F31B C37 F31 130.9(8) . . ? F33 C37 F31 103.4(5) . . ? F32B C37 C33 115.3(7) . . ? F33B C37 C33 115.3(8) . . ? F32 C37 C33 113.9(5) . . ? F31B C37 C33 109.9(8) . . ? F33 C37 C33 112.7(4) . . ? F31 C37 C33 112.9(4) . . ? F34 C38 F35 105.5(3) . . ? F34 C38 F36 106.6(3) . . ? F35 C38 F36 105.1(2) . . ? F34 C38 C35 112.4(2) . . ? F35 C38 C35 113.5(3) . . ? F36 C38 C35 113.1(2) . . ? C46 C41 C42 115.7(2) . . ? C46 C41 B1 122.0(2) . . ? C42 C41 B1 122.1(2) . . ? C43 C42 C41 122.4(2) . . ? C43 C42 H42 118.8 . . ? C41 C42 H42 118.8 . . ? C44 C43 C42 120.5(2) . . ? C44 C43 C47 118.5(2) . . ? C42 C43 C47 120.9(2) . . ? C43 C44 C45 118.3(2) . . ? C43 C44 H44 120.9 . . ? C45 C44 H44 120.9 . . ? C44 C45 C46 121.0(2) . . ? C44 C45 C48 118.5(2) . . ? C46 C45 C48 120.5(2) . . ? C45 C46 C41 122.1(2) . . ? C45 C46 H46 119.0 . . ? C41 C46 H46 119.0 . . ? F41B C47 F41 118.3(9) . . ? F41B C47 F43B 104.4(9) . . ? F41 C47 F43B 84.9(9) . . ? F41B C47 F43 19.3(13) . . ? F41 C47 F43 108.2(8) . . ? F43B C47 F43 121.6(8) . . ? F41B C47 F42 85.1(10) . . ? F41 C47 F42 104.1(8) . . ? F43B C47 F42 22.5(11) . . ? F43 C47 F42 103.8(9) . . ? F41B C47 F42B 106.1(8) . . ? F41 C47 F42B 21.7(10) . . ? F43B C47 F42B 105.7(7) . . ? F43 C47 F42B 91.7(9) . . ? F42 C47 F42B 122.9(9) . . ? F41B C47 C43 117.1(6) . . ? F41 C47 C43 114.6(6) . . ? F43B C47 C43 111.7(6) . . ? F43 C47 C43 112.8(6) . . ? F42 C47 C43 112.4(7) . . ? F42B C47 C43 110.9(6) . . ? F46B C48 F45B 107.6(9) . . ? F46B C48 F44B 104.1(7) . . ? F45B C48 F44B 107.4(8) . . ? F46B C48 F46 128.4(7) . . ? F45B C48 F46 70.6(11) . . ? F44B C48 F46 39.2(9) . . ? F46B C48 F45 31.9(8) . . ? F45B C48 F45 125.9(8) . . ? F44B C48 F45 73.5(9) . . ? F46 C48 F45 105.7(5) . . ? F46B C48 F44 76.3(8) . . ? F45B C48 F44 35.9(12) . . ? F44B C48 F44 133.0(8) . . ? F46 C48 F44 103.6(5) . . ? F45 C48 F44 103.7(5) . . ? F46B C48 C45 112.6(6) . . ? F45B C48 C45 114.4(6) . . ? F44B C48 C45 110.1(5) . . ? F46 C48 C45 114.4(4) . . ? F45 C48 C45 115.5(4) . . ? F44 C48 C45 112.7(4) . . ? C56 C51 C52 114.7(2) . . ? C56 C51 B1 125.2(2) . . ? C52 C51 B1 119.7(2) . . ? C53 C52 C51 123.0(2) . . ? C53 C52 H52 118.5 . . ? C51 C52 H52 118.5 . . ? C55 C54 C53 118.2(2) . . ? C55 C54 H54 120.9 . . ? C53 C54 H54 120.9 . . ? C54 C55 C56 120.6(2) . . ? C54 C55 C58 120.7(2) . . ? C56 C55 C58 118.7(2) . . ? C51 C56 C55 123.0(2) . . ? C51 C56 H56 118.5 . . ? C55 C56 H56 118.5 . . ? C52 C53 C54 120.5(2) . . ? C52 C53 C57 118.5(2) . . ? C54 C53 C57 121.0(2) . . ? F51 C57 F52 106.4(2) . . ? F51 C57 F53 106.2(2) . . ? F52 C57 F53 104.7(2) . . ? F51 C57 C53 114.1(2) . . ? F52 C57 C53 112.5(2) . . ? F53 C57 C53 112.3(2) . . ? F55 C58 F56 106.3(2) . . ? F55 C58 F54 106.9(2) . . ? F56 C58 F54 104.6(2) . . ? F55 C58 C55 113.4(2) . . ? F56 C58 C55 112.3(2) . . ? F54 C58 C55 112.7(2) . . ? C66 C61 C62 115.2(2) . . ? C66 C61 B1 122.5(2) . . ? C62 C61 B1 122.1(2) . . ? C63 C62 C61 122.9(2) . . ? C63 C62 H62 118.6 . . ? C61 C62 H62 118.6 . . ? C64 C63 C62 120.0(2) . . ? C64 C63 C67 119.7(3) . . ? C62 C63 C67 120.2(3) . . ? C65 C64 C63 118.9(2) . . ? C65 C64 H64 120.6 . . ? C63 C64 H64 120.6 . . ? C64 C65 C66 120.5(2) . . ? C64 C65 C68 119.2(3) . . ? C66 C65 C68 120.3(3) . . ? C65 C66 C61 122.5(2) . . ? C65 C66 H66 118.7 . . ? C61 C66 H66 118.7 . . ? F63 C67 F61 105.5(3) . . ? F63 C67 F62 106.8(3) . . ? F61 C67 F62 104.6(3) . . ? F63 C67 C63 113.1(3) . . ? F61 C67 C63 113.9(3) . . ? F62 C67 C63 112.3(3) . . ? F66B C68 F66 118.4(10) . . ? F66B C68 F64 82.1(11) . . ? F66 C68 F64 106.5(11) . . ? F66B C68 F64B 108.4(8) . . ? F66 C68 F64B 15.5(12) . . ? F64 C68 F64B 118.3(12) . . ? F66B C68 F65B 105.3(9) . . ? F66 C68 F65B 87.8(12) . . ? F64 C68 F65B 24.7(15) . . ? F64B C68 F65B 102.2(9) . . ? F66B C68 F65 23.5(11) . . ? F66 C68 F65 105.2(9) . . ? F64 C68 F65 104.8(10) . . ? F64B C68 F65 91.9(9) . . ? F65B C68 F65 126.5(10) . . ? F66B C68 C65 116.4(6) . . ? F66 C68 C65 114.4(8) . . ? F64 C68 C65 114.0(10) . . ? F64B C68 C65 113.8(5) . . ? F65B C68 C65 109.5(8) . . ? F65 C68 C65 111.1(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.324 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.048 #===END data_mv15_dtbpmCl+_9 _database_code_CSD 199940 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common dtbpmCl+ _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H40 Cl6 Fe P2' _chemical_formula_weight 586.99 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' 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' Fe Fe 0.3463 0.8444 '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 18.2861(3) _cell_length_b 9.9887(2) _cell_length_c 17.3272(3) _cell_angle_alpha 90.00 _cell_angle_beta 113.8570(10) _cell_angle_gamma 90.00 _cell_volume 2894.47(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max .38 _exptl_crystal_size_mid .17 _exptl_crystal_size_min .07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.190 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 28351 _diffrn_reflns_av_R_equivalents 0.1251 _diffrn_reflns_av_sigmaI/netI 0.0879 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.65 _reflns_number_total 6617 _reflns_number_gt 3776 _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^)+(0.0824P)^2^+19.1108P] 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 6617 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1835 _refine_ls_R_factor_gt 0.1019 _refine_ls_wR_factor_ref 0.2771 _refine_ls_wR_factor_gt 0.2307 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.132 _refine_ls_shift/su_max 0.877 _refine_ls_shift/su_mean 0.141 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 Fe1 Fe 0.40141(7) 0.44757(12) 0.45280(9) 0.0469(4) Uani 1 1 d . . . Cl1 Cl 0.36557(16) 0.2569(3) 0.3755(2) 0.0750(9) Uani 1 1 d . . . Cl2 Cl 0.29938(13) 0.5603(2) 0.46493(16) 0.0545(6) Uani 1 1 d . . . Cl3 Cl 0.48813(13) 0.5917(3) 0.41502(18) 0.0650(7) Uani 1 1 d . . . P1 P 0.17954(12) 0.7968(2) 0.63583(14) 0.0390(5) Uani 1 1 d . . . P2 P 0.32402(12) 0.95910(19) 0.62167(13) 0.0349(5) Uani 1 1 d . . . Cl4 Cl 0.3467(2) 1.0071(4) 0.7363(2) 0.1028(12) Uani 1 1 d . . . C10 C 0.2564(4) 0.8187(7) 0.5884(5) 0.0339(16) Uani 1 1 d . . . H10A H 0.2891 0.7362 0.6004 0.041 Uiso 1 1 calc R . . H10B H 0.2270 0.8245 0.5264 0.041 Uiso 1 1 calc R . . C11 C 0.0894(5) 0.7397(10) 0.5402(7) 0.059(3) Uani 1 1 d . . . C12 C 0.0642(8) 0.8590(19) 0.4770(11) 0.169(10) Uani 1 1 d . . . H12A H 0.1007 0.8647 0.4484 0.254 Uiso 1 1 calc R . . H12B H 0.0667 0.9424 0.5078 0.254 Uiso 1 1 calc R . . H12C H 0.0095 0.8449 0.4352 0.254 Uiso 1 1 calc R . . C13 C 0.0992(8) 0.6198(18) 0.4902(9) 0.128(7) Uani 1 1 d . . . H13A H 0.1155 0.5410 0.5270 0.191 Uiso 1 1 calc R . . H13B H 0.1402 0.6400 0.4690 0.191 Uiso 1 1 calc R . . H13C H 0.0483 0.6015 0.4426 0.191 Uiso 1 1 calc R . . C14 C 0.0204(7) 0.7155(16) 0.5645(10) 0.109(5) Uani 1 1 d . . . H14A H -0.0277 0.6960 0.5138 0.163 Uiso 1 1 calc R . . H14B H 0.0114 0.7955 0.5923 0.163 Uiso 1 1 calc R . . H14C H 0.0327 0.6393 0.6033 0.163 Uiso 1 1 calc R . . C15 C 0.2224(5) 0.6495(9) 0.7100(6) 0.049(2) Uani 1 1 d . . . C16 C 0.1654(9) 0.6192(16) 0.7526(11) 0.127(7) Uani 1 1 d . . . H16A H 0.1900 0.5531 0.7976 0.190 Uiso 1 1 calc R . . H16B H 0.1151 0.5833 0.7108 0.190 Uiso 1 1 calc R . . H16C H 0.1546 0.7017 0.7768 0.190 Uiso 1 1 calc R . . C17 C 0.2405(9) 0.5212(11) 0.6726(8) 0.097(4) Uani 1 1 d . . . H17A H 0.2722 0.5432 0.6402 0.145 Uiso 1 1 calc R . . H17B H 0.1902 0.4790 0.6354 0.145 Uiso 1 1 calc R . . H17C H 0.2708 0.4593 0.7183 0.145 Uiso 1 1 calc R . . C18 C 0.3012(7) 0.6999(12) 0.7791(7) 0.080(3) Uani 1 1 d . . . H18A H 0.2920 0.7859 0.8009 0.120 Uiso 1 1 calc R . . H18B H 0.3411 0.7114 0.7552 0.120 Uiso 1 1 calc R . . H18C H 0.3208 0.6345 0.8251 0.120 Uiso 1 1 calc R . . C21 C 0.2750(6) 1.1149(9) 0.5666(7) 0.060(3) Uani 1 1 d . . . C22 C 0.3379(7) 1.2314(9) 0.5937(10) 0.090(4) Uani 1 1 d . . . H22A H 0.3781 1.2149 0.5708 0.136 Uiso 1 1 calc R . . H22B H 0.3641 1.2354 0.6554 0.136 Uiso 1 1 calc R . . H22C H 0.3109 1.3165 0.5719 0.136 Uiso 1 1 calc R . . C23 C 0.2378(7) 1.0939(13) 0.4701(8) 0.094(5) Uani 1 1 d . . . H23A H 0.1923 1.0325 0.4546 0.142 Uiso 1 1 calc R . . H23B H 0.2781 1.0558 0.4525 0.142 Uiso 1 1 calc R . . H23C H 0.2196 1.1801 0.4418 0.142 Uiso 1 1 calc R . . C24 C 0.2089(7) 1.1512(10) 0.6001(9) 0.082(4) Uani 1 1 d . . . H24A H 0.1827 1.2351 0.5743 0.123 Uiso 1 1 calc R . . H24B H 0.2340 1.1616 0.6616 0.123 Uiso 1 1 calc R . . H24C H 0.1691 1.0793 0.5854 0.123 Uiso 1 1 calc R . . C25 C 0.4212(5) 0.9115(8) 0.6181(5) 0.0407(18) Uani 1 1 d . . . C26 C 0.4464(5) 0.7750(8) 0.6622(6) 0.046(2) Uani 1 1 d . . . H26A H 0.4073 0.7068 0.6305 0.069 Uiso 1 1 calc R . . H26B H 0.4488 0.7808 0.7196 0.069 Uiso 1 1 calc R . . H26C H 0.4992 0.7505 0.6646 0.069 Uiso 1 1 calc R . . C27 C 0.4100(6) 0.8981(9) 0.5246(6) 0.054(2) Uani 1 1 d . . . H27A H 0.3989 0.9864 0.4977 0.081 Uiso 1 1 calc R . . H27B H 0.3652 0.8377 0.4947 0.081 Uiso 1 1 calc R . . H27C H 0.4590 0.8618 0.5225 0.081 Uiso 1 1 calc R . . C28 C 0.4884(5) 1.0131(9) 0.6661(7) 0.063(3) Uani 1 1 d . . . H28A H 0.4757 1.1000 0.6376 0.094 Uiso 1 1 calc R . . H28B H 0.5394 0.9806 0.6671 0.094 Uiso 1 1 calc R . . H28C H 0.4928 1.0229 0.7241 0.094 Uiso 1 1 calc R . . C30 C 0.1313(7) 0.4286(13) 0.2790(8) 0.086(4) Uani 1 1 d . . . H30A H 0.1665 0.4355 0.3398 0.103 Uiso 1 1 calc R . . H30B H 0.1601 0.4682 0.2469 0.103 Uiso 1 1 calc R . . Cl5 Cl 0.0442(3) 0.5201(4) 0.2586(3) 0.1151(13) Uani 1 1 d . . . Cl6 Cl 0.1123(2) 0.2584(3) 0.2517(2) 0.1038(12) 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 Fe1 0.0390(6) 0.0337(6) 0.0745(9) -0.0046(6) 0.0297(6) -0.0048(5) Cl1 0.0694(16) 0.0504(14) 0.127(2) -0.0354(15) 0.0622(17) -0.0228(12) Cl2 0.0439(11) 0.0437(11) 0.0774(16) -0.0139(11) 0.0262(11) 0.0007(9) Cl3 0.0452(12) 0.0581(14) 0.0901(18) 0.0195(13) 0.0256(12) -0.0117(11) P1 0.0371(11) 0.0312(10) 0.0525(12) 0.0005(9) 0.0221(10) -0.0032(8) P2 0.0389(11) 0.0241(9) 0.0459(11) -0.0035(8) 0.0216(9) -0.0047(8) Cl4 0.127(3) 0.100(3) 0.082(2) -0.0148(19) 0.043(2) -0.022(2) C10 0.033(4) 0.029(4) 0.039(4) -0.004(3) 0.014(3) -0.006(3) C11 0.035(5) 0.063(6) 0.072(7) 0.000(5) 0.015(5) -0.009(4) C12 0.080(10) 0.164(17) 0.152(15) 0.080(13) -0.068(10) -0.062(11) C13 0.070(8) 0.183(16) 0.116(12) -0.100(12) 0.023(8) -0.021(9) C14 0.050(7) 0.138(13) 0.142(13) -0.030(10) 0.042(8) -0.026(8) C15 0.061(5) 0.039(4) 0.059(6) 0.008(4) 0.035(5) -0.004(4) C16 0.124(11) 0.121(12) 0.187(16) 0.103(12) 0.116(12) 0.038(10) C17 0.157(13) 0.044(6) 0.082(8) 0.011(6) 0.041(9) 0.022(7) C18 0.090(8) 0.076(8) 0.056(6) 0.036(6) 0.013(6) -0.002(6) C21 0.061(6) 0.032(4) 0.100(8) 0.019(5) 0.047(6) 0.002(4) C22 0.083(8) 0.028(5) 0.181(14) 0.012(6) 0.075(9) 0.000(5) C23 0.065(7) 0.097(9) 0.113(10) 0.076(8) 0.027(7) 0.012(6) C24 0.071(7) 0.034(5) 0.162(12) 0.016(6) 0.069(8) 0.013(5) C25 0.039(4) 0.033(4) 0.056(5) -0.005(4) 0.025(4) -0.006(3) C26 0.034(4) 0.046(5) 0.058(5) 0.011(4) 0.019(4) 0.004(4) C27 0.069(6) 0.044(5) 0.069(6) 0.001(4) 0.050(5) -0.002(4) C28 0.038(5) 0.048(5) 0.097(8) -0.013(5) 0.022(5) -0.014(4) C30 0.084(8) 0.086(9) 0.078(8) -0.008(7) 0.023(7) -0.026(7) Cl5 0.134(3) 0.115(3) 0.135(3) -0.003(2) 0.095(3) 0.008(3) Cl6 0.111(3) 0.070(2) 0.103(3) 0.0013(18) 0.015(2) -0.0175(19) _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 Fe1 Cl2 2.261(2) . ? Fe1 Cl1 2.267(3) . ? Fe1 Cl3 2.395(3) 3_666 ? Fe1 Cl3 2.420(2) . ? Cl3 Fe1 2.395(3) 3_666 ? P1 C11 1.891(10) . ? P1 C15 1.902(9) . ? P1 C10 1.906(7) . ? P2 C10 1.803(7) . ? P2 C21 1.856(9) . ? P2 C25 1.865(8) . ? P2 Cl4 1.918(4) . ? C11 C14 1.502(14) . ? C11 C13 1.531(16) . ? C11 C12 1.556(17) . ? C15 C16 1.532(14) . ? C15 C18 1.538(14) . ? C15 C17 1.532(14) . ? C21 C23 1.544(17) . ? C21 C22 1.569(13) . ? C21 C24 1.580(14) . ? C25 C26 1.539(11) . ? C25 C28 1.551(11) . ? C25 C27 1.554(12) . ? C30 Cl5 1.745(14) . ? C30 Cl6 1.761(13) . ? 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 Cl2 Fe1 Cl1 114.91(10) . . ? Cl2 Fe1 Cl3 113.65(11) . 3_666 ? Cl1 Fe1 Cl3 110.96(12) . 3_666 ? Cl2 Fe1 Cl3 112.61(10) . . ? Cl1 Fe1 Cl3 113.86(11) . . ? Cl3 Fe1 Cl3 87.98(9) 3_666 . ? Fe1 Cl3 Fe1 92.02(9) 3_666 . ? C11 P1 C15 109.5(4) . . ? C11 P1 C10 101.0(4) . . ? C15 P1 C10 101.9(4) . . ? C10 P2 C21 111.2(4) . . ? C10 P2 C25 109.3(3) . . ? C21 P2 C25 117.8(4) . . ? C10 P2 Cl4 111.0(3) . . ? C21 P2 Cl4 100.4(4) . . ? C25 P2 Cl4 106.8(3) . . ? P2 C10 P1 118.8(4) . . ? C14 C11 C13 109.7(10) . . ? C14 C11 C12 106.1(11) . . ? C13 C11 C12 105.6(13) . . ? C14 C11 P1 109.7(8) . . ? C13 C11 P1 118.1(8) . . ? C12 C11 P1 106.9(7) . . ? C16 C15 C18 107.2(10) . . ? C16 C15 C17 110.1(10) . . ? C18 C15 C17 107.9(9) . . ? C16 C15 P1 107.7(7) . . ? C18 C15 P1 105.9(6) . . ? C17 C15 P1 117.5(7) . . ? C23 C21 C22 111.9(9) . . ? C23 C21 C24 111.3(9) . . ? C22 C21 C24 107.3(9) . . ? C23 C21 P2 110.7(7) . . ? C22 C21 P2 108.9(7) . . ? C24 C21 P2 106.6(6) . . ? C26 C25 C28 107.5(7) . . ? C26 C25 C27 109.2(7) . . ? C28 C25 C27 110.9(7) . . ? C26 C25 P2 107.9(5) . . ? C28 C25 P2 112.0(6) . . ? C27 C25 P2 109.3(6) . . ? Cl5 C30 Cl6 112.7(7) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.261 _refine_diff_density_min -1.436 _refine_diff_density_rms 0.121 #===END #_eof End of Crystallographic Information File