# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Michael Hill' 'Peter B. Hitchcock' _publ_contact_author_name 'Dr Michael Hill' _publ_contact_author_address ; Chemistry Imperial College London Exhibition Road South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email MIKE.HILL@IMPERIAL.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Bis(phosphinimino)methyl derivatives of Ca, Sr and Ba: facile access to heavier alkaline earth organometallic chemistry. ; data_feb2703 _database_code_CSD 211013 _audit_creation_date 2003-02-25T15:53:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Ca(thf){N(SiMe3)2}(MesNPPh2CHPPh2NMes)]' ; _chemical_formula_moiety 'C53 H69 Ca1 N3 O1 P2 Si2' _chemical_formula_sum 'C53 H69 Ca1 N3 O1 P2 Si2' _chemical_formula_weight 922.31 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6861(6) _cell_length_b 22.9406(11) _cell_length_c 18.2982(10) _cell_angle_alpha 90 _cell_angle_beta 104.334(2) _cell_angle_gamma 90 _cell_volume 5159.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 34842 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_special_details ; Very weak diffraction ; essentially nothing above 20 degrees in theta. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.985 _exptl_absorpt_correction_T_max 0.867 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.2264 _diffrn_reflns_av_unetI/netI 0.1598 _diffrn_reflns_number 28754 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 23.03 _diffrn_reflns_theta_full 23.03 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 7073 _reflns_number_gt 4054 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There is disorder in the thf group, with alternative lower occupancy atom positions for three of the carbons (these were left isotropic), and SADI bond constraints were applied to this ligand. 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^)+(0.0000P)^2^+17.8430P] 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_number_reflns 7073 _refine_ls_number_parameters 575 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1741 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.1 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.333 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.078 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ca Ca 0.69808(11) 0.14260(6) 0.24563(8) 0.0263(4) Uani 1 1 d . B . P1 P 0.69845(14) 0.01428(8) 0.30799(10) 0.0222(4) Uani 1 1 d . B . P2 P 0.91871(14) 0.08407(8) 0.33368(10) 0.0215(4) Uani 1 1 d . B . Si1 Si 0.73979(18) 0.28413(9) 0.27175(12) 0.0353(6) Uani 1 1 d . B . Si2 Si 0.62909(17) 0.23709(9) 0.38490(12) 0.0362(6) Uani 1 1 d . B . O O 0.5434(5) 0.1662(2) 0.1416(3) 0.067(2) Uani 1 1 d D . . N1 N 0.6125(4) 0.0485(2) 0.2427(3) 0.0229(14) Uani 1 1 d . . . N2 N 0.8903(4) 0.1181(2) 0.2549(3) 0.0238(14) Uani 1 1 d . . . N3 N 0.6880(4) 0.2282(2) 0.3122(3) 0.0277(14) Uani 1 1 d . . . C1 C 0.7979(5) 0.0638(3) 0.3507(4) 0.0189(16) Uani 1 1 d . . . H1 H 0.797(5) 0.075(3) 0.394(4) 0.028 Uiso 1 1 d . . . C2 C 0.7565(6) -0.0489(3) 0.2710(4) 0.0253(18) Uani 1 1 d . . . C3 C 0.8253(6) -0.0410(3) 0.2240(4) 0.0327(19) Uani 1 1 d . B . H3 H 0.8444 -0.0025 0.2132 0.039 Uiso 1 1 calc R . . C4 C 0.8674(6) -0.0876(4) 0.1923(4) 0.043(2) Uani 1 1 d . . . H4 H 0.9163 -0.0811 0.1614 0.052 Uiso 1 1 calc R B . C5 C 0.8380(7) -0.1428(4) 0.2060(5) 0.051(2) Uani 1 1 d . B . H5 H 0.8661 -0.1748 0.184 0.061 Uiso 1 1 calc R . . C6 C 0.7679(7) -0.1528(3) 0.2516(5) 0.044(2) Uani 1 1 d . . . H6 H 0.7471 -0.1915 0.2602 0.053 Uiso 1 1 calc R B . C7 C 0.7279(6) -0.1060(3) 0.2847(4) 0.036(2) Uani 1 1 d . B . H7 H 0.6808 -0.1129 0.3169 0.044 Uiso 1 1 calc R . . C8 C 0.6410(5) -0.0160(3) 0.3807(4) 0.0251(17) Uani 1 1 d . . . C9 C 0.6946(6) -0.0134(3) 0.4565(4) 0.0297(18) Uani 1 1 d . B . H9 H 0.7625 0.0063 0.4708 0.036 Uiso 1 1 calc R . . C10 C 0.6528(6) -0.0385(3) 0.5118(4) 0.0346(19) Uani 1 1 d . . . H10 H 0.6908 -0.0352 0.5634 0.042 Uiso 1 1 calc R B . C11 C 0.5558(6) -0.0683(3) 0.4920(4) 0.044(2) Uani 1 1 d . B . H11 H 0.528 -0.087 0.5296 0.053 Uiso 1 1 calc R . . C12 C 0.4994(6) -0.0711(3) 0.4178(4) 0.041(2) Uani 1 1 d . . . H12 H 0.4312 -0.0906 0.4044 0.05 Uiso 1 1 calc R B . C13 C 0.5412(6) -0.0456(3) 0.3617(4) 0.0332(19) Uani 1 1 d . B . H13 H 0.5019 -0.0483 0.3104 0.04 Uiso 1 1 calc R . . C14 C 1.0116(5) 0.0228(3) 0.3385(3) 0.0182(16) Uani 1 1 d . . . C15 C 1.0093(5) -0.0211(3) 0.3923(4) 0.0290(18) Uani 1 1 d . B . H15 H 0.9588 -0.0184 0.4227 0.035 Uiso 1 1 calc R . . C16 C 1.0805(6) -0.0681(3) 0.4010(4) 0.0332(19) Uani 1 1 d . . . H16 H 1.079 -0.0972 0.4376 0.04 Uiso 1 1 calc R B . C17 C 1.1517(6) -0.0722(3) 0.3573(4) 0.036(2) Uani 1 1 d . B . H17 H 1.1997 -0.1046 0.3631 0.043 Uiso 1 1 calc R . . C18 C 1.1561(6) -0.0303(3) 0.3044(4) 0.036(2) Uani 1 1 d . . . H18 H 1.2071 -0.0336 0.2744 0.044 Uiso 1 1 calc R B . C19 C 1.0852(5) 0.0171(3) 0.2950(4) 0.0292(18) Uani 1 1 d . B . H19 H 1.0878 0.0459 0.2582 0.035 Uiso 1 1 calc R . . C20 C 0.9842(5) 0.1263(3) 0.4166(4) 0.0235(17) Uani 1 1 d . . . C21 C 1.0853(6) 0.1118(3) 0.4648(4) 0.0318(19) Uani 1 1 d . B . H21 H 1.1232 0.0783 0.4545 0.038 Uiso 1 1 calc R . . C22 C 1.1296(6) 0.1457(4) 0.5265(4) 0.041(2) Uani 1 1 d . . . H22 H 1.1985 0.1354 0.558 0.049 Uiso 1 1 calc R B . C23 C 1.0780(7) 0.1931(3) 0.5436(4) 0.045(2) Uani 1 1 d . B . H23 H 1.1103 0.2157 0.5869 0.054 Uiso 1 1 calc R . . C24 C 0.9789(7) 0.2089(3) 0.4987(4) 0.043(2) Uani 1 1 d . . . H24 H 0.9418 0.2419 0.5113 0.052 Uiso 1 1 calc R B . C25 C 0.9326(6) 0.1764(3) 0.4346(4) 0.0276(18) Uani 1 1 d . B . H25 H 0.8652 0.1884 0.4025 0.033 Uiso 1 1 calc R . . C26 C 0.5040(5) 0.0297(3) 0.2049(4) 0.0236(17) Uani 1 1 d . B . C27 C 0.4829(5) -0.0075(3) 0.1412(4) 0.0271(18) Uani 1 1 d . . . C28 C 0.3728(6) -0.0194(3) 0.1057(4) 0.035(2) Uani 1 1 d . B . H28 H 0.3577 -0.0453 0.0639 0.042 Uiso 1 1 calc R . . C29 C 0.2858(6) 0.0044(3) 0.1281(4) 0.0320(19) Uani 1 1 d . . . C30 C 0.3113(6) 0.0418(3) 0.1892(4) 0.037(2) Uani 1 1 d . B . H30 H 0.2532 0.0595 0.2054 0.044 Uiso 1 1 calc R . . C31 C 0.4164(5) 0.0549(3) 0.2280(4) 0.0251(17) Uani 1 1 d . . . C32 C 0.5707(6) -0.0327(3) 0.1098(4) 0.040(2) Uani 1 1 d . B . H32A H 0.6418 -0.0204 0.1407 0.06 Uiso 0.5 1 calc PR . . H32B H 0.562 -0.019 0.0579 0.06 Uiso 0.5 1 calc PR . . H32C H 0.566 -0.0754 0.1101 0.06 Uiso 0.5 1 calc PR . . H32D H 0.5381 -0.0561 0.0651 0.06 Uiso 0.5 1 calc PR . . H32E H 0.6178 -0.0575 0.1479 0.06 Uiso 0.5 1 calc PR . . H32F H 0.6139 -0.0012 0.0957 0.06 Uiso 0.5 1 calc PR . . C33 C 0.1704(6) -0.0102(4) 0.0876(5) 0.056(3) Uani 1 1 d . B . H33A H 0.1705 -0.0373 0.0462 0.085 Uiso 0.5 1 calc PR . . H33B H 0.1319 0.0256 0.0673 0.085 Uiso 0.5 1 calc PR . . H33C H 0.1336 -0.0284 0.123 0.085 Uiso 0.5 1 calc PR . . H33D H 0.1201 0.0106 0.1115 0.085 Uiso 0.5 1 calc PR . . H33E H 0.1588 -0.0523 0.0904 0.085 Uiso 0.5 1 calc PR . . H33F H 0.157 0.0017 0.0347 0.085 Uiso 0.5 1 calc PR . . C34 C 0.4357(6) 0.0954(3) 0.2933(4) 0.039(2) Uani 1 1 d . B . H34A H 0.5141 0.1001 0.3143 0.058 Uiso 0.5 1 calc PR . . H34B H 0.4025 0.0795 0.332 0.058 Uiso 0.5 1 calc PR . . H34C H 0.4032 0.1334 0.2767 0.058 Uiso 0.5 1 calc PR . . H34D H 0.3657 0.1086 0.301 0.058 Uiso 0.5 1 calc PR . . H34E H 0.4774 0.1292 0.2833 0.058 Uiso 0.5 1 calc PR . . H34F H 0.4767 0.0752 0.3387 0.058 Uiso 0.5 1 calc PR . . C35 C 0.9511(5) 0.1291(3) 0.2011(4) 0.0212(16) Uani 1 1 d . B . C36 C 1.0555(5) 0.1553(3) 0.2173(4) 0.0261(17) Uani 1 1 d . . . C37 C 1.1085(6) 0.1627(3) 0.1597(4) 0.038(2) Uani 1 1 d . B . H37 H 1.1788 0.1798 0.1718 0.045 Uiso 1 1 calc R . . C38 C 1.0635(6) 0.1461(3) 0.0852(5) 0.040(2) Uani 1 1 d . . . C39 C 0.9577(7) 0.1245(3) 0.0697(4) 0.038(2) Uani 1 1 d . B . H39 H 0.9226 0.115 0.0189 0.046 Uiso 1 1 calc R . . C40 C 0.9019(6) 0.1162(3) 0.1241(4) 0.0327(19) Uani 1 1 d . . . C41 C 1.1107(6) 0.1765(3) 0.2952(4) 0.041(2) Uani 1 1 d . B . H41A H 1.064 0.1686 0.3295 0.061 Uiso 0.5 1 calc PR . . H41B H 1.1237 0.2185 0.2937 0.061 Uiso 0.5 1 calc PR . . H41C H 1.1802 0.1562 0.3132 0.061 Uiso 0.5 1 calc PR . . H41D H 1.1813 0.1936 0.2948 0.061 Uiso 0.5 1 calc PR . . H41E H 1.1216 0.1437 0.3306 0.061 Uiso 0.5 1 calc PR . . H41F H 1.065 0.206 0.3111 0.061 Uiso 0.5 1 calc PR . . C42 C 1.1242(8) 0.1509(4) 0.0244(5) 0.069(3) Uani 1 1 d . B . H42A H 1.0777 0.1373 -0.0235 0.104 Uiso 0.5 1 calc PR . . H42B H 1.1901 0.1269 0.0379 0.104 Uiso 0.5 1 calc PR . . H42C H 1.1444 0.1917 0.0194 0.104 Uiso 0.5 1 calc PR . . H42D H 1.1971 0.1666 0.0461 0.104 Uiso 0.5 1 calc PR . . H42E H 1.0847 0.177 -0.0154 0.104 Uiso 0.5 1 calc PR . . H42F H 1.1304 0.1123 0.0031 0.104 Uiso 0.5 1 calc PR . . C43 C 0.7856(6) 0.0957(4) 0.1014(4) 0.047(2) Uani 1 1 d . B . H43A H 0.7573 0.0921 0.1464 0.071 Uiso 0.5 1 calc PR . . H43B H 0.7821 0.0578 0.0763 0.071 Uiso 0.5 1 calc PR . . H43C H 0.7416 0.1241 0.0667 0.071 Uiso 0.5 1 calc PR . . H43D H 0.7634 0.0905 0.0466 0.071 Uiso 0.5 1 calc PR . . H43E H 0.7386 0.1248 0.1167 0.071 Uiso 0.5 1 calc PR . . H43F H 0.7791 0.0585 0.1263 0.071 Uiso 0.5 1 calc PR . . C44 C 0.8731(6) 0.3145(4) 0.3280(5) 0.051(2) Uani 1 1 d . . . H44A H 0.8645 0.3287 0.3767 0.077 Uiso 1 1 calc R B . H44B H 0.8955 0.3468 0.3002 0.077 Uiso 1 1 calc R . . H44C H 0.9286 0.2839 0.3363 0.077 Uiso 1 1 calc R . . C45 C 0.7681(7) 0.2589(4) 0.1812(5) 0.054(2) Uani 1 1 d . . . H45A H 0.7018 0.2422 0.1487 0.081 Uiso 1 1 calc R B . H45B H 0.8254 0.2292 0.1919 0.081 Uiso 1 1 calc R . . H45C H 0.792 0.292 0.1555 0.081 Uiso 1 1 calc R . . C46 C 0.6445(6) 0.3480(3) 0.2490(5) 0.049(2) Uani 1 1 d . . . H46A H 0.6279 0.3623 0.2954 0.073 Uiso 1 1 calc R B . H46B H 0.577 0.3358 0.2133 0.073 Uiso 1 1 calc R . . H46C H 0.6789 0.3792 0.2264 0.073 Uiso 1 1 calc R . . C47 C 0.6899(7) 0.2981(4) 0.4514(5) 0.057(3) Uani 1 1 d . . . H47A H 0.6854 0.3347 0.4232 0.085 Uiso 1 1 calc R B . H47B H 0.7663 0.2892 0.4752 0.085 Uiso 1 1 calc R . . H47C H 0.6496 0.302 0.4905 0.085 Uiso 1 1 calc R . . C48 C 0.6444(7) 0.1716(3) 0.4474(4) 0.048(2) Uani 1 1 d . . . H48A H 0.7217 0.1618 0.4653 0.072 Uiso 1 1 calc R B . H48B H 0.6053 0.1387 0.419 0.072 Uiso 1 1 calc R . . H48C H 0.6142 0.1801 0.4906 0.072 Uiso 1 1 calc R . . C49 C 0.4801(7) 0.2537(4) 0.3532(6) 0.066(3) Uani 1 1 d . . . H49A H 0.469 0.2878 0.3199 0.099 Uiso 1 1 calc R B . H49B H 0.4516 0.2618 0.3973 0.099 Uiso 1 1 calc R . . H49C H 0.4418 0.2201 0.3258 0.099 Uiso 1 1 calc R . . C50 C 0.4944(9) 0.1338(4) 0.0720(4) 0.069(3) Uani 1 1 d D B . H50A H 0.5515 0.1196 0.0481 0.083 Uiso 1 1 calc R A 1 H50B H 0.453 0.0998 0.0834 0.083 Uiso 1 1 calc R A 1 C51 C 0.4220(13) 0.1745(8) 0.0222(8) 0.089(6) Uani 0.736(16) 1 d PD B 1 H51A H 0.348 0.1577 0.0053 0.107 Uiso 0.736(16) 1 calc PR B 1 H51B H 0.4495 0.183 -0.0228 0.107 Uiso 0.736(16) 1 calc PR B 1 C52 C 0.4196(13) 0.2295(7) 0.0673(8) 0.111(8) Uani 0.736(16) 1 d PD B 1 H52A H 0.4665 0.26 0.0535 0.133 Uiso 0.736(16) 1 calc PR B 1 H52B H 0.3445 0.2448 0.0586 0.133 Uiso 0.736(16) 1 calc PR B 1 C53 C 0.4620(13) 0.2111(6) 0.1474(8) 0.076(6) Uani 0.736(16) 1 d PD B 1 H53A H 0.4963 0.2441 0.1794 0.091 Uiso 0.736(16) 1 calc PR B 1 H53B H 0.4035 0.1945 0.1681 0.091 Uiso 0.736(16) 1 calc PR B 1 C51A C 0.3786(16) 0.1439(15) 0.059(2) 0.066(12) Uiso 0.264(16) 1 d PD B 2 H51C H 0.3423 0.1141 0.0832 0.079 Uiso 0.264(16) 1 calc PR B 2 H51D H 0.3421 0.1466 0.0045 0.079 Uiso 0.264(16) 1 calc PR B 2 C52A C 0.386(3) 0.2011(15) 0.097(2) 0.056(12) Uiso 0.264(16) 1 d PD B 2 H52C H 0.356 0.1971 0.1421 0.067 Uiso 0.264(16) 1 calc PR B 2 H52D H 0.3401 0.2294 0.0627 0.067 Uiso 0.264(16) 1 calc PR B 2 C53A C 0.498(2) 0.2248(9) 0.122(3) 0.057(15) Uiso 0.264(16) 1 d PD B 2 H53C H 0.5237 0.2432 0.0804 0.069 Uiso 0.264(16) 1 calc PR B 2 H53D H 0.5086 0.2513 0.1657 0.069 Uiso 0.264(16) 1 calc PR B 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 Ca 0.0286(8) 0.0211(8) 0.0277(8) 0.0024(7) 0.0040(7) 0.0023(7) P1 0.0229(10) 0.0207(10) 0.0214(10) 0.0013(8) 0.0025(8) -0.0013(8) P2 0.0219(10) 0.0184(10) 0.0231(10) 0.0012(8) 0.0036(8) 0.0006(8) Si1 0.0433(13) 0.0228(12) 0.0389(13) 0.0052(10) 0.0082(11) 0.0045(10) Si2 0.0349(13) 0.0323(13) 0.0439(14) -0.0068(10) 0.0149(11) 0.0011(10) O 0.082(5) 0.041(4) 0.054(4) 0.004(3) -0.029(4) 0.012(3) N1 0.017(3) 0.026(3) 0.022(3) -0.001(3) -0.002(3) 0.005(3) N2 0.029(3) 0.028(3) 0.014(3) 0.007(3) 0.005(3) 0.001(3) N3 0.032(3) 0.018(3) 0.033(3) 0.006(3) 0.008(3) 0.002(3) C1 0.019(4) 0.024(4) 0.012(4) -0.001(3) 0.001(3) -0.006(3) C2 0.030(4) 0.018(4) 0.019(4) -0.001(3) -0.011(4) 0.003(3) C3 0.032(4) 0.037(5) 0.029(4) -0.003(4) 0.006(4) -0.007(4) C4 0.038(5) 0.045(6) 0.046(5) -0.020(4) 0.007(4) 0.003(4) C5 0.051(6) 0.038(6) 0.064(6) -0.019(5) 0.014(5) 0.008(5) C6 0.052(6) 0.018(5) 0.057(6) -0.004(4) 0.005(5) 0.003(4) C7 0.042(5) 0.027(5) 0.035(5) -0.003(4) 0.000(4) -0.003(4) C8 0.024(4) 0.028(4) 0.021(4) 0.004(3) 0.002(3) -0.003(3) C9 0.026(4) 0.037(5) 0.027(4) 0.002(3) 0.007(4) -0.001(4) C10 0.035(5) 0.050(5) 0.018(4) 0.003(4) 0.004(4) -0.008(4) C11 0.049(5) 0.050(6) 0.032(5) 0.010(4) 0.008(4) -0.017(4) C12 0.038(5) 0.048(6) 0.039(5) 0.000(4) 0.011(4) -0.019(4) C13 0.039(5) 0.032(5) 0.025(4) 0.000(3) 0.002(4) -0.010(4) C14 0.014(4) 0.020(4) 0.020(4) 0.003(3) 0.003(3) 0.005(3) C15 0.027(4) 0.028(5) 0.030(4) 0.002(3) 0.001(4) -0.001(4) C16 0.037(5) 0.024(5) 0.037(5) 0.015(4) 0.006(4) 0.004(4) C17 0.039(5) 0.021(5) 0.050(5) 0.006(4) 0.014(4) 0.011(4) C18 0.033(5) 0.034(5) 0.047(5) 0.003(4) 0.018(4) 0.008(4) C19 0.029(4) 0.022(4) 0.037(5) 0.001(3) 0.010(4) -0.002(3) C20 0.030(4) 0.013(4) 0.025(4) 0.004(3) 0.002(3) -0.004(3) C21 0.031(4) 0.025(4) 0.033(4) 0.002(3) -0.003(4) 0.005(3) C22 0.041(5) 0.039(5) 0.029(5) 0.003(4) -0.017(4) -0.005(4) C23 0.064(6) 0.025(5) 0.036(5) -0.004(4) -0.011(5) -0.009(4) C24 0.054(6) 0.028(5) 0.044(5) -0.007(4) 0.005(5) 0.007(4) C25 0.035(4) 0.021(4) 0.024(4) 0.004(3) 0.003(4) -0.002(3) C26 0.015(4) 0.025(4) 0.027(4) 0.006(3) -0.003(3) -0.006(3) C27 0.027(4) 0.021(4) 0.028(4) 0.004(3) -0.003(4) -0.002(3) C28 0.037(5) 0.034(5) 0.027(4) -0.001(4) -0.006(4) -0.002(4) C29 0.028(4) 0.028(5) 0.035(5) 0.004(4) -0.003(4) -0.004(4) C30 0.029(4) 0.033(5) 0.047(5) 0.008(4) 0.006(4) 0.000(4) C31 0.027(4) 0.024(4) 0.024(4) 0.003(3) 0.006(3) -0.003(3) C32 0.036(5) 0.051(6) 0.031(5) -0.013(4) 0.005(4) -0.002(4) C33 0.032(5) 0.047(6) 0.078(7) -0.008(5) -0.012(5) -0.010(4) C34 0.038(5) 0.039(5) 0.038(5) -0.014(4) 0.009(4) 0.006(4) C35 0.025(4) 0.015(4) 0.026(4) 0.007(3) 0.011(3) 0.004(3) C36 0.030(4) 0.016(4) 0.036(4) 0.011(3) 0.015(4) 0.004(3) C37 0.041(5) 0.026(5) 0.048(5) 0.010(4) 0.014(4) -0.002(4) C38 0.043(5) 0.033(5) 0.057(6) 0.013(4) 0.035(5) 0.016(4) C39 0.056(6) 0.041(5) 0.026(4) 0.003(4) 0.025(4) 0.002(4) C40 0.042(5) 0.026(4) 0.029(4) 0.004(3) 0.008(4) 0.002(4) C41 0.040(5) 0.039(5) 0.044(5) 0.004(4) 0.011(4) -0.012(4) C42 0.087(7) 0.068(7) 0.069(7) 0.006(5) 0.047(6) 0.003(6) C43 0.054(6) 0.063(6) 0.025(4) -0.005(4) 0.009(4) -0.013(5) C44 0.052(6) 0.043(6) 0.061(6) 0.007(4) 0.020(5) 0.000(4) C45 0.079(7) 0.033(5) 0.061(6) 0.006(4) 0.037(5) 0.008(5) C46 0.055(6) 0.030(5) 0.055(6) 0.004(4) 0.002(5) 0.004(4) C47 0.061(6) 0.051(6) 0.060(6) -0.005(5) 0.019(5) 0.004(5) C48 0.050(5) 0.050(6) 0.051(6) -0.006(4) 0.025(5) -0.014(4) C49 0.057(6) 0.048(6) 0.096(8) -0.005(5) 0.025(6) 0.006(5) C50 0.096(8) 0.066(7) 0.034(5) 0.010(5) -0.007(6) -0.015(6) C51 0.055(10) 0.136(16) 0.064(11) 0.004(11) -0.009(8) 0.016(11) C52 0.054(10) 0.097(14) 0.145(17) 0.082(14) -0.044(11) -0.006(10) C53 0.069(11) 0.035(8) 0.099(13) 0.013(9) -0.026(10) 0.015(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ca N3 2.331(6) . ? Ca N1 2.411(6) . ? Ca O 2.433(5) . ? Ca N2 2.467(6) . ? Ca C1 2.713(7) . ? P1 N1 1.609(5) . ? P1 C1 1.733(6) . ? P1 C8 1.807(7) . ? P1 C2 1.830(7) . ? P2 N2 1.601(5) . ? P2 C1 1.702(7) . ? P2 C20 1.818(6) . ? P2 C14 1.821(6) . ? Si1 N3 1.693(6) . ? Si1 C45 1.873(8) . ? Si1 C46 1.879(7) . ? Si1 C44 1.882(8) . ? Si2 N3 1.691(6) . ? Si2 C48 1.868(8) . ? Si2 C49 1.874(8) . ? Si2 C47 1.890(8) . ? O C53A 1.470(17) . ? O C50 1.473(8) . ? O C53 1.480(11) . ? N1 C26 1.444(8) . ? N2 C35 1.415(8) . ? C2 C3 1.380(10) . ? C2 C7 1.399(9) . ? C3 C4 1.384(10) . ? C4 C5 1.360(11) . ? C5 C6 1.380(11) . ? C6 C7 1.389(10) . ? C8 C9 1.386(9) . ? C8 C13 1.403(9) . ? C9 C10 1.379(9) . ? C10 C11 1.377(10) . ? C11 C12 1.370(10) . ? C12 C13 1.395(10) . ? C14 C19 1.375(9) . ? C14 C15 1.413(9) . ? C15 C16 1.390(9) . ? C16 C17 1.351(10) . ? C17 C18 1.374(10) . ? C18 C19 1.394(9) . ? C20 C25 1.402(9) . ? C20 C21 1.404(9) . ? C21 C22 1.371(9) . ? C22 C23 1.347(10) . ? C23 C24 1.369(10) . ? C24 C25 1.391(9) . ? C26 C31 1.408(9) . ? C26 C27 1.414(9) . ? C27 C28 1.414(9) . ? C27 C32 1.491(10) . ? C28 C29 1.381(10) . ? C29 C30 1.384(10) . ? C29 C33 1.506(9) . ? C30 C31 1.379(9) . ? C31 C34 1.486(9) . ? C35 C36 1.418(9) . ? C35 C40 1.424(9) . ? C36 C37 1.393(10) . ? C36 C41 1.506(9) . ? C37 C38 1.394(10) . ? C38 C39 1.392(10) . ? C38 C42 1.505(11) . ? C39 C40 1.371(10) . ? C40 C43 1.505(10) . ? C50 C51A 1.447(16) . ? C50 C51 1.460(12) . ? C51 C52 1.513(13) . ? C52 C53 1.492(13) . ? C51A C52A 1.481(17) . ? C52A C53A 1.484(17) . ? 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 N3 Ca N1 133.1(2) . . ? N3 Ca O 94.80(19) . . ? N1 Ca O 84.86(18) . . ? N3 Ca N2 109.68(19) . . ? N1 Ca N2 103.31(18) . . ? O Ca N2 134.1(2) . . ? N3 Ca C1 105.50(19) . . ? N1 Ca C1 63.13(18) . . ? O Ca C1 147.9(2) . . ? N2 Ca C1 61.30(19) . . ? N1 P1 C1 107.4(3) . . ? N1 P1 C8 114.3(3) . . ? C1 P1 C8 107.5(3) . . ? N1 P1 C2 111.9(3) . . ? C1 P1 C2 111.8(3) . . ? C8 P1 C2 104.0(3) . . ? N1 P1 Ca 48.4(2) . . ? C1 P1 Ca 59.2(2) . . ? C8 P1 Ca 131.3(2) . . ? C2 P1 Ca 124.7(2) . . ? N2 P2 C1 106.6(3) . . ? N2 P2 C20 116.5(3) . . ? C1 P2 C20 103.8(3) . . ? N2 P2 C14 114.7(3) . . ? C1 P2 C14 112.4(3) . . ? C20 P2 C14 102.4(3) . . ? N2 P2 Ca 50.2(2) . . ? C1 P2 Ca 59.1(2) . . ? C20 P2 Ca 111.3(2) . . ? C14 P2 Ca 146.3(2) . . ? N3 Si1 C45 109.5(3) . . ? N3 Si1 C46 112.9(3) . . ? C45 Si1 C46 107.4(4) . . ? N3 Si1 C44 115.8(3) . . ? C45 Si1 C44 104.8(4) . . ? C46 Si1 C44 105.9(4) . . ? N3 Si2 C48 112.7(3) . . ? N3 Si2 C49 112.9(4) . . ? C48 Si2 C49 107.2(4) . . ? N3 Si2 C47 114.0(4) . . ? C48 Si2 C47 103.7(4) . . ? C49 Si2 C47 105.6(4) . . ? C53A O C50 101.2(18) . . ? C53A O C53 31.3(15) . . ? C50 O C53 105.1(8) . . ? C53A O Ca 125.9(15) . . ? C50 O Ca 130.5(5) . . ? C53 O Ca 122.7(6) . . ? C26 N1 P1 126.9(5) . . ? C26 N1 Ca 130.5(4) . . ? P1 N1 Ca 101.6(2) . . ? C35 N2 P2 132.4(5) . . ? C35 N2 Ca 127.7(4) . . ? P2 N2 Ca 99.8(3) . . ? Si2 N3 Si1 123.2(3) . . ? Si2 N3 Ca 127.2(3) . . ? Si1 N3 Ca 109.4(3) . . ? P2 C1 P1 133.2(4) . . ? P2 C1 Ca 88.4(3) . . ? P1 C1 Ca 87.6(2) . . ? C3 C2 C7 117.8(7) . . ? C3 C2 P1 120.1(6) . . ? C7 C2 P1 122.0(6) . . ? C2 C3 C4 121.9(8) . . ? C5 C4 C3 119.3(8) . . ? C4 C5 C6 120.9(8) . . ? C5 C6 C7 119.6(8) . . ? C6 C7 C2 120.4(8) . . ? C9 C8 C13 117.2(6) . . ? C9 C8 P1 122.2(5) . . ? C13 C8 P1 120.5(5) . . ? C10 C9 C8 122.3(7) . . ? C11 C10 C9 119.6(7) . . ? C12 C11 C10 119.9(7) . . ? C11 C12 C13 120.5(7) . . ? C12 C13 C8 120.4(7) . . ? C19 C14 C15 117.9(6) . . ? C19 C14 P2 124.7(5) . . ? C15 C14 P2 117.3(5) . . ? C16 C15 C14 120.6(7) . . ? C17 C16 C15 119.8(7) . . ? C16 C17 C18 121.2(7) . . ? C17 C18 C19 119.7(7) . . ? C14 C19 C18 120.9(7) . . ? C25 C20 C21 116.9(6) . . ? C25 C20 P2 119.3(5) . . ? C21 C20 P2 123.8(5) . . ? C22 C21 C20 120.5(7) . . ? C23 C22 C21 121.7(7) . . ? C22 C23 C24 120.1(7) . . ? C23 C24 C25 119.9(7) . . ? C24 C25 C20 120.9(7) . . ? C31 C26 C27 119.5(6) . . ? C31 C26 N1 117.5(6) . . ? C27 C26 N1 122.6(6) . . ? C28 C27 C26 117.3(7) . . ? C28 C27 C32 119.7(6) . . ? C26 C27 C32 123.0(6) . . ? C29 C28 C27 124.0(7) . . ? C28 C29 C30 116.2(7) . . ? C28 C29 C33 121.2(7) . . ? C30 C29 C33 122.7(7) . . ? C31 C30 C29 123.6(7) . . ? C30 C31 C26 119.4(6) . . ? C30 C31 C34 119.7(7) . . ? C26 C31 C34 120.9(6) . . ? N2 C35 C36 124.9(6) . . ? N2 C35 C40 118.1(6) . . ? C36 C35 C40 116.9(6) . . ? C37 C36 C35 119.6(7) . . ? C37 C36 C41 118.6(7) . . ? C35 C36 C41 121.7(6) . . ? C36 C37 C38 123.3(7) . . ? C39 C38 C37 116.0(7) . . ? C39 C38 C42 121.3(8) . . ? C37 C38 C42 122.8(8) . . ? C40 C39 C38 123.1(7) . . ? C39 C40 C35 120.7(7) . . ? C39 C40 C43 119.4(7) . . ? C35 C40 C43 119.8(7) . . ? C51A C50 C51 48.5(17) . . ? C51A C50 O 104.9(15) . . ? C51 C50 O 106.4(9) . . ? C50 C51 C52 106.7(10) . . ? C53 C52 C51 104.4(11) . . ? O C53 C52 102.4(11) . . ? C50 C51A C52A 97(2) . . ? C51A C52A C53A 114(3) . . ? O C53A C52A 92(2) . . ? #===END data_mar1503 _database_code_CSD 211014 _audit_creation_date 2003-03-24T17:11:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Sr(thf){N(SiMe3)2}(MesNPPh2CHPPh2NMes)]' ; _chemical_formula_moiety 'C53 H69 N3 O1 P2 Si2 Sr1' _chemical_formula_sum 'C53 H69 N3 O1 P2 Si2 Sr1' _chemical_formula_weight 969.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7105(1) _cell_length_b 23.1523(2) _cell_length_c 18.4217(1) _cell_angle_alpha 90 _cell_angle_beta 104.566(3) _cell_angle_gamma 90 _cell_volume 5246.85(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 43541 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7981 _exptl_absorpt_correction_T_max 0.8878 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_unetI/netI 0.0374 _diffrn_reflns_number 66071 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _reflns_number_total 11945 _reflns_number_gt 9793 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The thf group is disordered and its carbon atoms were left isotropic. 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^)+(0.0296P)^2^+5.3258P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 11945 _refine_ls_number_parameters 556 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.947 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Sr Sr 0.191948(16) 0.355122(8) 0.742606(11) 0.02235(6) Uani 1 1 d . A . P1 P 0.19822(4) 0.48804(2) 0.80817(3) 0.01939(11) Uani 1 1 d . A . P2 P 0.41875(4) 0.41825(2) 0.83382(3) 0.01930(11) Uani 1 1 d . A . Si1 Si 0.23716(5) 0.21197(3) 0.77630(4) 0.03039(14) Uani 1 1 d . A . Si2 Si 0.12327(5) 0.26012(3) 0.88729(4) 0.03071(14) Uani 1 1 d . A . O O 0.02461(17) 0.33241(9) 0.63533(11) 0.0570(6) Uani 1 1 d . . . N1 N 0.10968(13) 0.45578(7) 0.74338(9) 0.0220(4) Uani 1 1 d . . . N2 N 0.39284(14) 0.38442(8) 0.75528(9) 0.0228(4) Uani 1 1 d . . . N3 N 0.18494(15) 0.26668(8) 0.81662(10) 0.0268(4) Uani 1 1 d . . . C1 C 0.29697(16) 0.43847(8) 0.85152(11) 0.0197(4) Uani 1 1 d . . . H1 H 0.2808 0.4189 0.8927 0.024 Uiso 1 1 calc R A . C2 C 0.25629(17) 0.55085(9) 0.77229(12) 0.0255(4) Uani 1 1 d . . . C3 C 0.32581(18) 0.54194(11) 0.72528(12) 0.0310(5) Uani 1 1 d . A . H3 H 0.3443 0.5037 0.7146 0.037 Uiso 1 1 calc R . . C4 C 0.3680(2) 0.58831(12) 0.69416(15) 0.0431(6) Uani 1 1 d . . . H4 H 0.4163 0.5817 0.6631 0.052 Uiso 1 1 calc R A . C5 C 0.3401(2) 0.64394(13) 0.70814(18) 0.0525(8) Uani 1 1 d . A . H5 H 0.3687 0.6756 0.6865 0.063 Uiso 1 1 calc R . . C6 C 0.2707(2) 0.65361(11) 0.75349(17) 0.0478(7) Uani 1 1 d . . . H6 H 0.2513 0.692 0.7628 0.057 Uiso 1 1 calc R A . C7 C 0.2286(2) 0.60748(10) 0.78571(13) 0.0331(5) Uani 1 1 d . A . H7 H 0.1809 0.6146 0.817 0.04 Uiso 1 1 calc R . . C8 C 0.14225(17) 0.51801(9) 0.88201(11) 0.0223(4) Uani 1 1 d . . . C9 C 0.19747(17) 0.51446(10) 0.95743(12) 0.0266(5) Uani 1 1 d . A . H9 H 0.2653 0.495 0.9713 0.032 Uiso 1 1 calc R . . C10 C 0.1548(2) 0.53900(11) 1.01255(13) 0.0345(5) Uani 1 1 d . . . H10 H 0.1932 0.536 1.0638 0.041 Uiso 1 1 calc R A . C11 C 0.0566(2) 0.56772(12) 0.99286(13) 0.0382(6) Uani 1 1 d . A . H11 H 0.0277 0.5849 1.0305 0.046 Uiso 1 1 calc R . . C12 C 0.0004(2) 0.57144(12) 0.91839(14) 0.0381(6) Uani 1 1 d . . . H12 H -0.0674 0.5911 0.905 0.046 Uiso 1 1 calc R A . C13 C 0.04217(18) 0.54679(10) 0.86323(13) 0.0310(5) Uani 1 1 d . A . H13 H 0.0027 0.5494 0.8122 0.037 Uiso 1 1 calc R . . C14 C 0.51262(16) 0.47865(9) 0.84015(11) 0.0223(4) Uani 1 1 d . . . C15 C 0.58615(18) 0.48370(10) 0.79565(13) 0.0295(5) Uani 1 1 d . A . H15 H 0.5882 0.455 0.7592 0.035 Uiso 1 1 calc R . . C16 C 0.6565(2) 0.53062(10) 0.80448(15) 0.0358(6) Uani 1 1 d . . . H16 H 0.7061 0.534 0.7738 0.043 Uiso 1 1 calc R A . C17 C 0.6546(2) 0.57225(10) 0.85759(14) 0.0350(5) Uani 1 1 d . A . H17 H 0.7036 0.6039 0.8638 0.042 Uiso 1 1 calc R . . C18 C 0.58153(19) 0.56809(10) 0.90206(13) 0.0319(5) Uani 1 1 d . . . H18 H 0.5799 0.597 0.9384 0.038 Uiso 1 1 calc R A . C19 C 0.51112(18) 0.52167(9) 0.89304(12) 0.0268(5) Uani 1 1 d . A . H19 H 0.4608 0.519 0.9233 0.032 Uiso 1 1 calc R . . C20 C 0.48166(17) 0.37511(9) 0.91666(11) 0.0221(4) Uani 1 1 d . . . C21 C 0.42842(18) 0.32552(9) 0.93146(12) 0.0278(5) Uani 1 1 d . A . H21 H 0.3612 0.3145 0.8985 0.033 Uiso 1 1 calc R . . C22 C 0.4736(2) 0.29218(10) 0.99442(14) 0.0369(6) Uani 1 1 d . . . H22 H 0.4362 0.2589 1.0048 0.044 Uiso 1 1 calc R A . C23 C 0.5725(2) 0.30704(11) 1.04197(14) 0.0414(6) Uani 1 1 d . A . H23 H 0.6027 0.2843 1.0851 0.05 Uiso 1 1 calc R . . C24 C 0.6270(2) 0.35510(11) 1.02639(14) 0.0388(6) Uani 1 1 d . . . H24 H 0.6958 0.365 1.0582 0.047 Uiso 1 1 calc R A . C25 C 0.58182(18) 0.38907(10) 0.96444(12) 0.0303(5) Uani 1 1 d . A . H25 H 0.6197 0.4223 0.9545 0.036 Uiso 1 1 calc R . . C26 C 0.00242(16) 0.47261(9) 0.70528(11) 0.0220(4) Uani 1 1 d . A . C27 C -0.08542(18) 0.44739(9) 0.72808(12) 0.0262(5) Uani 1 1 d . . . C28 C -0.19140(18) 0.45909(10) 0.68856(13) 0.0301(5) Uani 1 1 d . A . H28 H -0.2493 0.4415 0.7044 0.036 Uiso 1 1 calc R . . C29 C -0.21605(19) 0.49547(10) 0.62683(14) 0.0339(5) Uani 1 1 d . . . C30 C -0.12940(19) 0.51922(10) 0.60427(13) 0.0320(5) Uani 1 1 d . A . H30 H -0.1443 0.5439 0.5617 0.038 Uiso 1 1 calc R . . C31 C -0.02101(18) 0.50847(9) 0.64143(12) 0.0266(5) Uani 1 1 d . . . C32 C -0.0652(2) 0.40711(11) 0.79414(14) 0.0374(6) Uani 1 1 d . A . H32C H -0.0273 0.3726 0.7832 0.056 Uiso 1 1 calc R . . H32B H -0.1347 0.3959 0.8039 0.056 Uiso 1 1 calc R . . H32A H -0.0202 0.4266 0.8384 0.056 Uiso 1 1 calc R . . C33 C -0.3330(2) 0.50844(13) 0.58668(18) 0.0508(7) Uani 1 1 d . A . H33F H -0.3703 0.4724 0.5674 0.076 Uiso 0.5 1 calc PR . . H33E H -0.3348 0.5349 0.5449 0.076 Uiso 0.5 1 calc PR . . H33D H -0.3697 0.5264 0.6218 0.076 Uiso 0.5 1 calc PR . . H33C H -0.3463 0.55 0.5886 0.076 Uiso 0.5 1 calc PR . . H33B H -0.3817 0.4876 0.6112 0.076 Uiso 0.5 1 calc PR . . H33A H -0.3468 0.4961 0.5342 0.076 Uiso 0.5 1 calc PR . . C34 C 0.0678(2) 0.53387(12) 0.61046(13) 0.0377(6) Uani 1 1 d . A . H34C H 0.094 0.5698 0.6371 0.057 Uiso 1 1 calc R . . H34B H 0.0392 0.5421 0.5569 0.057 Uiso 1 1 calc R . . H34A H 0.128 0.5063 0.6172 0.057 Uiso 1 1 calc R . . C35 C 0.45271(18) 0.37253(9) 0.70193(12) 0.0246(4) Uani 1 1 d . A . C36 C 0.55611(19) 0.34614(9) 0.71797(13) 0.0293(5) Uani 1 1 d . . . C37 C 0.6076(2) 0.33788(10) 0.66033(15) 0.0361(6) Uani 1 1 d . A . H37 H 0.6778 0.3209 0.6721 0.043 Uiso 1 1 calc R . . C38 C 0.5611(2) 0.35331(11) 0.58671(15) 0.0393(6) Uani 1 1 d . . . C39 C 0.4564(2) 0.37547(11) 0.57076(14) 0.0363(6) Uani 1 1 d . A . H39 H 0.4212 0.3848 0.5203 0.044 Uiso 1 1 calc R . . C40 C 0.40112(19) 0.38456(10) 0.62599(12) 0.0296(5) Uani 1 1 d . . . C41 C 0.6113(2) 0.32636(12) 0.79579(14) 0.0400(6) Uani 1 1 d . A . H41C H 0.6357 0.36 0.8278 0.06 Uiso 1 1 calc R . . H41B H 0.6742 0.3023 0.7942 0.06 Uiso 1 1 calc R . . H41A H 0.5601 0.3038 0.8162 0.06 Uiso 1 1 calc R . . C42 C 0.6213(3) 0.34765(14) 0.52597(18) 0.0569(8) Uani 1 1 d . A . H42F H 0.5812 0.3216 0.4867 0.085 Uiso 0.5 1 calc PR . . H42E H 0.6941 0.3319 0.5476 0.085 Uiso 0.5 1 calc PR . . H42D H 0.6277 0.3857 0.5042 0.085 Uiso 0.5 1 calc PR . . H42C H 0.6874 0.3713 0.539 0.085 Uiso 0.5 1 calc PR . . H42B H 0.5746 0.3609 0.4781 0.085 Uiso 0.5 1 calc PR . . H42A H 0.641 0.3071 0.5214 0.085 Uiso 0.5 1 calc PR . . C43 C 0.2853(2) 0.40540(12) 0.60320(13) 0.0402(6) Uani 1 1 d . A . H43A H 0.2727 0.4258 0.5552 0.06 Uiso 1 1 calc R . . H43B H 0.2719 0.4317 0.6416 0.06 Uiso 1 1 calc R . . H43C H 0.236 0.3723 0.598 0.06 Uiso 1 1 calc R . . C44 C 0.2687(3) 0.23895(11) 0.68689(16) 0.0485(7) Uani 1 1 d . . . H44A H 0.2029 0.2555 0.6539 0.073 Uiso 1 1 calc R A . H44B H 0.2941 0.2067 0.6613 0.073 Uiso 1 1 calc R . . H44C H 0.3255 0.2686 0.6992 0.073 Uiso 1 1 calc R . . C45 C 0.3694(2) 0.18174(12) 0.83332(17) 0.0475(7) Uani 1 1 d . . . H45C H 0.3574 0.1624 0.8779 0.071 Uiso 1 1 calc R A . H45B H 0.4218 0.2132 0.8488 0.071 Uiso 1 1 calc R . . H45A H 0.3978 0.1539 0.803 0.071 Uiso 1 1 calc R . . C46 C 0.1430(2) 0.14852(11) 0.74982(16) 0.0434(6) Uani 1 1 d . . . H46C H 0.174 0.121 0.7205 0.065 Uiso 1 1 calc R A . H46B H 0.0722 0.1619 0.7198 0.065 Uiso 1 1 calc R . . H46A H 0.1337 0.1296 0.7954 0.065 Uiso 1 1 calc R . . C47 C 0.1761(2) 0.19982(12) 0.95475(15) 0.0458(7) Uani 1 1 d . . . H47C H 0.2528 0.2068 0.9795 0.069 Uiso 1 1 calc R A . H47B H 0.1692 0.1631 0.9274 0.069 Uiso 1 1 calc R . . H47A H 0.134 0.198 0.9925 0.069 Uiso 1 1 calc R . . C48 C -0.0280(2) 0.24777(14) 0.85099(18) 0.0546(8) Uani 1 1 d . . . H48C H -0.0407 0.2102 0.8257 0.082 Uiso 1 1 calc R A . H48B H -0.0594 0.2784 0.8154 0.082 Uiso 1 1 calc R . . H48A H -0.0623 0.2483 0.893 0.082 Uiso 1 1 calc R . . C49 C 0.1421(2) 0.32666(11) 0.94794(15) 0.0403(6) Uani 1 1 d . . . H49C H 0.1005 0.3226 0.9858 0.06 Uiso 1 1 calc R A . H49B H 0.1162 0.3606 0.9167 0.06 Uiso 1 1 calc R . . H49A H 0.2194 0.3315 0.9728 0.06 Uiso 1 1 calc R . . C50 C -0.0527(4) 0.2873(2) 0.6374(3) 0.0522(12) Uiso 0.733(8) 1 d P A 1 H50C H -0.1145 0.3014 0.6561 0.063 Uiso 0.733(8) 1 calc PR A 1 H50D H -0.0183 0.2539 0.6679 0.063 Uiso 0.733(8) 1 calc PR A 1 C51 C -0.0883(4) 0.2721(2) 0.5505(3) 0.0608(14) Uiso 0.733(8) 1 d P A 1 H51A H -0.0355 0.2454 0.537 0.073 Uiso 0.733(8) 1 calc PR A 1 H51B H -0.161 0.2538 0.5375 0.073 Uiso 0.733(8) 1 calc PR A 1 C52 C -0.0906(3) 0.32609(17) 0.5120(2) 0.0416(11) Uiso 0.733(8) 1 d P A 1 H52A H -0.1662 0.3396 0.4919 0.05 Uiso 0.733(8) 1 calc PR A 1 H52B H -0.0552 0.3225 0.4701 0.05 Uiso 0.733(8) 1 calc PR A 1 C53 C -0.0282(3) 0.36688(14) 0.57112(18) 0.0567(8) Uiso 0.733(8) 1 d P A 1 H53A H 0.0265 0.3884 0.552 0.068 Uiso 0.733(8) 1 calc PR A 1 H53B H -0.0783 0.395 0.5852 0.068 Uiso 0.733(8) 1 calc PR A 1 C50A C -0.0131(12) 0.2711(6) 0.6207(8) 0.058(4) Uiso 0.267(8) 1 d P A 2 H50A H 0.0366 0.2505 0.596 0.07 Uiso 0.267(8) 1 calc PR A 2 H50B H -0.0093 0.2518 0.6692 0.07 Uiso 0.267(8) 1 calc PR A 2 C51A C -0.1103(14) 0.2673(7) 0.5795(10) 0.076(5) Uiso 0.267(8) 1 d P A 2 H51C H -0.1648 0.2604 0.6086 0.091 Uiso 0.267(8) 1 calc PR A 2 H51D H -0.1179 0.2383 0.539 0.091 Uiso 0.267(8) 1 calc PR A 2 C52A C -0.111(3) 0.3371(16) 0.548(2) 0.205(15) Uiso 0.267(8) 1 d P A 2 H52C H -0.1268 0.3358 0.4921 0.247 Uiso 0.267(8) 1 calc PR A 2 H52D H -0.173 0.3574 0.5602 0.247 Uiso 0.267(8) 1 calc PR A 2 C53A C -0.0282(3) 0.36688(14) 0.57112(18) 0.0567(8) Uiso 0.267(8) 1 d P A 2 H53C H -0.0457 0.4061 0.5858 0.068 Uiso 0.267(8) 1 calc PR A 2 H53D H 0.016 0.3696 0.534 0.068 Uiso 0.267(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sr 0.02313(10) 0.02038(10) 0.02321(10) -0.00136(8) 0.00519(7) -0.00228(8) P1 0.0196(2) 0.0201(3) 0.0184(2) 0.00074(19) 0.0046(2) 0.0016(2) P2 0.0183(2) 0.0194(2) 0.0204(2) -0.0014(2) 0.00513(19) 0.0000(2) Si1 0.0371(4) 0.0216(3) 0.0340(3) -0.0039(3) 0.0117(3) -0.0032(3) Si2 0.0313(3) 0.0291(3) 0.0349(3) 0.0066(3) 0.0143(3) 0.0003(3) O 0.0573(13) 0.0491(12) 0.0479(11) 0.0005(9) -0.0177(10) -0.0105(10) N1 0.0199(8) 0.0255(9) 0.0196(8) -0.0004(7) 0.0032(7) 0.0011(7) N2 0.0225(9) 0.0257(9) 0.0208(8) -0.0026(7) 0.0067(7) 0.0005(7) N3 0.0307(10) 0.0210(9) 0.0298(10) -0.0009(7) 0.0097(8) -0.0030(8) C1 0.0217(10) 0.0194(9) 0.0189(9) 0.0022(7) 0.0066(8) 0.0019(8) C2 0.0251(11) 0.0252(11) 0.0231(10) 0.0040(8) 0.0004(8) -0.0026(9) C3 0.0286(12) 0.0332(12) 0.0300(12) 0.0068(10) 0.0053(9) -0.0017(10) C4 0.0374(14) 0.0481(16) 0.0452(15) 0.0153(12) 0.0132(12) -0.0065(12) C5 0.0502(17) 0.0404(16) 0.0659(19) 0.0220(14) 0.0129(15) -0.0103(13) C6 0.0527(17) 0.0251(13) 0.0612(18) 0.0075(12) 0.0064(14) -0.0038(12) C7 0.0358(13) 0.0252(11) 0.0346(12) 0.0022(9) 0.0019(10) 0.0012(10) C8 0.0237(10) 0.0206(10) 0.0234(10) -0.0016(8) 0.0073(8) 0.0011(8) C9 0.0229(10) 0.0315(12) 0.0243(11) -0.0011(9) 0.0036(9) 0.0034(9) C10 0.0363(13) 0.0447(14) 0.0221(11) -0.0033(10) 0.0067(10) 0.0050(11) C11 0.0413(14) 0.0483(15) 0.0292(12) -0.0054(11) 0.0166(11) 0.0105(12) C12 0.0333(13) 0.0468(15) 0.0343(13) -0.0016(11) 0.0087(10) 0.0169(11) C13 0.0289(12) 0.0363(13) 0.0264(11) -0.0009(9) 0.0045(9) 0.0101(10) C14 0.0220(10) 0.0196(10) 0.0248(10) 0.0000(8) 0.0046(8) 0.0004(8) C15 0.0305(12) 0.0272(11) 0.0339(12) -0.0042(9) 0.0137(10) -0.0038(9) C16 0.0341(13) 0.0315(12) 0.0485(15) -0.0027(11) 0.0231(11) -0.0071(10) C17 0.0328(12) 0.0244(11) 0.0485(14) -0.0020(10) 0.0116(11) -0.0085(10) C18 0.0359(13) 0.0248(11) 0.0349(12) -0.0063(9) 0.0087(10) -0.0023(10) C19 0.0263(11) 0.0263(11) 0.0284(11) -0.0026(9) 0.0078(9) -0.0013(9) C20 0.0241(10) 0.0214(10) 0.0210(10) -0.0017(8) 0.0062(8) 0.0040(8) C21 0.0290(11) 0.0237(11) 0.0292(11) -0.0004(9) 0.0046(9) 0.0011(9) C22 0.0455(15) 0.0253(12) 0.0377(13) 0.0053(10) 0.0063(11) -0.0001(11) C23 0.0529(16) 0.0327(13) 0.0301(13) 0.0064(10) -0.0053(11) 0.0082(12) C24 0.0354(13) 0.0384(14) 0.0335(13) -0.0005(11) -0.0082(10) 0.0033(11) C25 0.0273(11) 0.0302(12) 0.0289(11) -0.0007(9) -0.0014(9) -0.0004(9) C26 0.0220(10) 0.0227(10) 0.0207(10) -0.0032(8) 0.0043(8) 0.0014(8) C27 0.0274(11) 0.0265(11) 0.0248(11) -0.0011(9) 0.0068(9) 0.0021(9) C28 0.0228(11) 0.0314(12) 0.0375(13) -0.0040(10) 0.0101(10) 0.0005(9) C29 0.0258(12) 0.0324(12) 0.0386(13) -0.0028(10) -0.0010(10) 0.0044(10) C30 0.0331(12) 0.0275(12) 0.0296(12) 0.0046(9) -0.0025(10) 0.0021(10) C31 0.0279(11) 0.0262(11) 0.0239(10) 0.0000(9) 0.0029(9) -0.0001(9) C32 0.0341(13) 0.0438(14) 0.0359(13) 0.0094(11) 0.0118(10) -0.0033(11) C33 0.0291(13) 0.0497(17) 0.0658(19) 0.0073(14) -0.0028(13) 0.0086(12) C34 0.0367(13) 0.0457(15) 0.0279(12) 0.0141(11) 0.0030(10) -0.0032(11) C35 0.0274(11) 0.0221(10) 0.0273(11) -0.0062(8) 0.0124(9) -0.0049(9) C36 0.0307(12) 0.0253(11) 0.0342(12) -0.0085(9) 0.0125(10) -0.0026(9) C37 0.0314(12) 0.0321(12) 0.0505(15) -0.0110(11) 0.0207(11) -0.0017(10) C38 0.0470(15) 0.0351(13) 0.0460(15) -0.0120(11) 0.0307(12) -0.0081(12) C39 0.0486(15) 0.0363(13) 0.0289(12) -0.0036(10) 0.0188(11) -0.0062(12) C40 0.0344(12) 0.0306(12) 0.0267(11) -0.0043(9) 0.0130(10) -0.0040(10) C41 0.0314(13) 0.0445(15) 0.0441(14) -0.0050(12) 0.0094(11) 0.0124(11) C42 0.065(2) 0.0604(19) 0.0616(19) -0.0094(15) 0.0460(17) -0.0075(16) C43 0.0404(14) 0.0569(17) 0.0230(12) 0.0000(11) 0.0072(10) 0.0064(13) C44 0.075(2) 0.0308(13) 0.0495(16) -0.0088(12) 0.0343(15) -0.0042(13) C45 0.0452(16) 0.0393(15) 0.0576(17) -0.0078(13) 0.0122(13) 0.0076(13) C46 0.0526(16) 0.0277(13) 0.0513(16) -0.0087(11) 0.0153(13) -0.0080(12) C47 0.0568(17) 0.0398(15) 0.0452(15) 0.0137(12) 0.0207(13) 0.0051(13) C48 0.0390(16) 0.0597(19) 0.068(2) 0.0141(16) 0.0183(14) -0.0090(14) C49 0.0471(15) 0.0392(14) 0.0412(14) 0.0013(11) 0.0231(12) 0.0097(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sr N3 2.4740(18) . ? Sr N1 2.5557(17) . ? Sr O 2.5674(18) . ? Sr N2 2.5951(17) . ? P1 N1 1.6042(17) . ? P1 C1 1.740(2) . ? P1 C8 1.823(2) . ? P1 C2 1.828(2) . ? P2 N2 1.6048(17) . ? P2 C1 1.725(2) . ? P2 C14 1.823(2) . ? P2 C20 1.831(2) . ? Si1 N3 1.6866(19) . ? Si1 C45 1.879(3) . ? Si1 C46 1.880(3) . ? Si1 C44 1.896(3) . ? Si2 N3 1.6868(19) . ? Si2 C47 1.878(3) . ? Si2 C49 1.883(3) . ? Si2 C48 1.892(3) . ? O C50 1.441(5) . ? O C53 1.445(4) . ? O C50A 1.500(13) . ? N1 C26 1.422(3) . ? N2 C35 1.413(3) . ? C2 C7 1.395(3) . ? C2 C3 1.399(3) . ? C3 C4 1.387(3) . ? C4 C5 1.377(4) . ? C5 C6 1.377(4) . ? C6 C7 1.392(4) . ? C8 C9 1.393(3) . ? C8 C13 1.400(3) . ? C9 C10 1.387(3) . ? C10 C11 1.380(3) . ? C11 C12 1.381(3) . ? C12 C13 1.383(3) . ? C14 C15 1.395(3) . ? C14 C19 1.397(3) . ? C15 C16 1.390(3) . ? C16 C17 1.378(3) . ? C17 C18 1.388(3) . ? C18 C19 1.382(3) . ? C20 C25 1.391(3) . ? C20 C21 1.394(3) . ? C21 C22 1.391(3) . ? C22 C23 1.382(4) . ? C23 C24 1.379(4) . ? C24 C25 1.386(3) . ? C26 C31 1.409(3) . ? C26 C27 1.414(3) . ? C27 C28 1.387(3) . ? C27 C32 1.503(3) . ? C28 C29 1.386(3) . ? C29 C30 1.385(3) . ? C29 C33 1.515(3) . ? C30 C31 1.398(3) . ? C31 C34 1.507(3) . ? C35 C36 1.412(3) . ? C35 C40 1.415(3) . ? C36 C37 1.393(3) . ? C36 C41 1.500(3) . ? C37 C38 1.383(4) . ? C38 C39 1.387(4) . ? C38 C42 1.512(3) . ? C39 C40 1.390(3) . ? C40 C43 1.505(3) . ? C50 C51 1.588(7) . ? C51 C52 1.433(6) . ? C52 C53 1.507(5) . ? C50A C51A 1.28(2) . ? C51A C52A 1.72(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 N3 Sr N1 132.85(6) . . ? N3 Sr O 96.72(6) . . ? N1 Sr O 85.99(6) . . ? N3 Sr N2 109.74(6) . . ? N1 Sr N2 98.97(5) . . ? O Sr N2 136.78(7) . . ? N1 P1 C1 108.94(9) . . ? N1 P1 C8 113.57(9) . . ? C1 P1 C8 106.28(9) . . ? N1 P1 C2 111.90(9) . . ? C1 P1 C2 112.36(10) . . ? C8 P1 C2 103.64(10) . . ? N2 P2 C1 108.21(9) . . ? N2 P2 C14 114.50(9) . . ? C1 P2 C14 112.56(10) . . ? N2 P2 C20 115.65(9) . . ? C1 P2 C20 102.42(9) . . ? C14 P2 C20 102.92(9) . . ? N3 Si1 C45 115.43(11) . . ? N3 Si1 C46 113.94(11) . . ? C45 Si1 C46 105.99(13) . . ? N3 Si1 C44 109.13(11) . . ? C45 Si1 C44 104.69(14) . . ? C46 Si1 C44 106.97(13) . . ? N3 Si1 Sr 43.94(6) . . ? C45 Si1 Sr 123.54(9) . . ? C46 Si1 Sr 130.40(9) . . ? C44 Si1 Sr 65.33(8) . . ? N3 Si2 C47 114.80(11) . . ? N3 Si2 C49 111.71(11) . . ? C47 Si2 C49 104.17(13) . . ? N3 Si2 C48 111.65(12) . . ? C47 Si2 C48 106.52(14) . . ? C49 Si2 C48 107.44(14) . . ? C50 O C53 104.0(3) . . ? C50 O C50A 29.5(6) . . ? C53 O C50A 108.3(5) . . ? C50 O Sr 124.5(2) . . ? C53 O Sr 129.90(18) . . ? C50A O Sr 119.8(5) . . ? C26 N1 P1 130.22(14) . . ? C26 N1 Sr 126.16(13) . . ? P1 N1 Sr 102.55(8) . . ? C35 N2 P2 134.25(15) . . ? C35 N2 Sr 125.19(13) . . ? P2 N2 Sr 100.54(8) . . ? Si1 N3 Si2 125.66(11) . . ? Si1 N3 Sr 107.83(9) . . ? Si2 N3 Sr 126.01(10) . . ? P2 C1 P1 132.11(12) . . ? P2 C1 Sr 88.10(8) . . ? P1 C1 Sr 88.14(8) . . ? C7 C2 C3 118.3(2) . . ? C7 C2 P1 122.74(18) . . ? C3 C2 P1 118.79(17) . . ? C4 C3 C2 120.8(2) . . ? C5 C4 C3 120.1(3) . . ? C4 C5 C6 120.0(2) . . ? C5 C6 C7 120.5(3) . . ? C6 C7 C2 120.3(2) . . ? C9 C8 C13 118.25(19) . . ? C9 C8 P1 121.91(16) . . ? C13 C8 P1 119.82(16) . . ? C10 C9 C8 121.0(2) . . ? C11 C10 C9 119.9(2) . . ? C10 C11 C12 119.9(2) . . ? C11 C12 C13 120.4(2) . . ? C12 C13 C8 120.5(2) . . ? C15 C14 C19 118.6(2) . . ? C15 C14 P2 123.46(16) . . ? C19 C14 P2 117.92(16) . . ? C16 C15 C14 120.2(2) . . ? C17 C16 C15 120.3(2) . . ? C16 C17 C18 120.3(2) . . ? C19 C18 C17 119.5(2) . . ? C18 C19 C14 121.1(2) . . ? C25 C20 C21 118.7(2) . . ? C25 C20 P2 122.61(17) . . ? C21 C20 P2 118.72(16) . . ? C22 C21 C20 120.1(2) . . ? C23 C22 C21 120.6(2) . . ? C24 C23 C22 119.6(2) . . ? C23 C24 C25 120.2(2) . . ? C24 C25 C20 120.8(2) . . ? C31 C26 C27 118.32(19) . . ? C31 C26 N1 123.28(19) . . ? C27 C26 N1 118.08(18) . . ? C28 C27 C26 119.9(2) . . ? C28 C27 C32 119.5(2) . . ? C26 C27 C32 120.62(19) . . ? C29 C28 C27 122.6(2) . . ? C30 C29 C28 117.0(2) . . ? C30 C29 C33 122.1(2) . . ? C28 C29 C33 120.8(2) . . ? C29 C30 C31 122.9(2) . . ? C30 C31 C26 119.3(2) . . ? C30 C31 C34 119.0(2) . . ? C26 C31 C34 121.66(19) . . ? C36 C35 N2 125.1(2) . . ? C36 C35 C40 117.88(19) . . ? N2 C35 C40 116.89(19) . . ? C37 C36 C35 119.4(2) . . ? C37 C36 C41 119.3(2) . . ? C35 C36 C41 121.3(2) . . ? C38 C37 C36 123.1(2) . . ? C37 C38 C39 117.0(2) . . ? C37 C38 C42 122.2(3) . . ? C39 C38 C42 120.8(3) . . ? C38 C39 C40 122.4(2) . . ? C39 C40 C35 120.0(2) . . ? C39 C40 C43 118.9(2) . . ? C35 C40 C43 121.1(2) . . ? O C50 C51 99.0(4) . . ? C52 C51 C50 105.8(4) . . ? C51 C52 C53 104.3(3) . . ? O C53 C52 107.3(3) . . ? C51A C50A O 112.9(12) . . ? C50A C51A C52A 93.6(16) . . ? #===END data_apr203 _database_code_CSD 211015 _audit_creation_date 2003-04-02T16:04:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Ba(MesNPPh2CHPPh2NMes)2].1/2(toluene)' ; _chemical_formula_moiety ; '(C86 H86 Ba1 N4 P4) 0.5(C7 H8)' ; _chemical_formula_sum 'C89.5 H90 Ba1 N4 P4' _chemical_formula_weight 1482.88 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0294(2) _cell_length_b 13.3312(2) _cell_length_c 25.5773(4) _cell_angle_alpha 100.566(1) _cell_angle_beta 92.303(1) _cell_angle_gamma 118.149(1) _cell_volume 3809.47(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 131083 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1542 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8719 _exptl_absorpt_correction_T_max 0.988 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0629 _diffrn_reflns_av_unetI/netI 0.0803 _diffrn_reflns_number 45010 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 27.53 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_total 17111 _reflns_number_gt 12563 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The toluene solvate molecule is disodered across an inversion centre. 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^)+(0.0320P)^2^+2.4026P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 17111 _refine_ls_number_parameters 927 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0979 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.463 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.082 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ba Ba 0.249055(16) 0.021772(16) 0.259950(7) 0.02493(6) Uani 1 1 d . . . P1 P 0.17851(7) -0.11025(7) 0.37532(3) 0.02240(16) Uani 1 1 d . . . P2 P 0.44237(6) 0.08177(7) 0.39295(3) 0.02299(16) Uani 1 1 d . . . P3 P 0.29347(7) 0.00385(7) 0.12185(3) 0.02770(18) Uani 1 1 d . . . P4 P 0.08048(7) 0.04800(7) 0.14571(3) 0.02733(17) Uani 1 1 d . . . N1 N 0.1248(2) -0.1540(2) 0.31243(9) 0.0267(5) Uani 1 1 d . . . N2 N 0.4127(2) 0.1428(2) 0.35035(9) 0.0261(5) Uani 1 1 d . . . N3 N 0.3533(2) -0.0156(2) 0.17229(9) 0.0308(6) Uani 1 1 d . . . N4 N 0.1155(2) 0.0961(2) 0.20955(9) 0.0286(6) Uani 1 1 d . . . C1 C 0.3268(2) -0.0515(3) 0.39387(12) 0.0275(7) Uani 1 1 d . . . H1 H 0.3487 -0.102 0.407 0.033 Uiso 1 1 calc R . . C2 C 0.1015(2) -0.2271(2) 0.40998(11) 0.0233(6) Uani 1 1 d . . . C3 C -0.0202(3) -0.2958(3) 0.39714(12) 0.0314(7) Uani 1 1 d . . . H3 H -0.0607 -0.2847 0.3689 0.038 Uiso 1 1 calc R . . C4 C -0.0827(3) -0.3800(3) 0.42500(13) 0.0359(8) Uani 1 1 d . . . H4 H -0.1657 -0.4265 0.4158 0.043 Uiso 1 1 calc R . . C5 C -0.0246(3) -0.3967(3) 0.46624(13) 0.0357(8) Uani 1 1 d . . . H5 H -0.0677 -0.4541 0.4856 0.043 Uiso 1 1 calc R . . C6 C 0.0958(3) -0.3300(3) 0.47910(12) 0.0338(7) Uani 1 1 d . . . H6 H 0.1356 -0.3416 0.5074 0.041 Uiso 1 1 calc R . . C7 C 0.1592(3) -0.2461(3) 0.45101(11) 0.0277(7) Uani 1 1 d . . . H7 H 0.2424 -0.2013 0.4598 0.033 Uiso 1 1 calc R . . C8 C 0.1357(2) -0.0033(2) 0.40555(11) 0.0249(6) Uani 1 1 d . . . C9 C 0.0701(3) 0.0306(3) 0.37615(12) 0.0305(7) Uani 1 1 d . . . H9 H 0.0486 -0.0002 0.3384 0.037 Uiso 1 1 calc R . . C10 C 0.0360(3) 0.1083(3) 0.40140(14) 0.0371(8) Uani 1 1 d . . . H10 H -0.0072 0.1323 0.3809 0.045 Uiso 1 1 calc R . . C11 C 0.0645(3) 0.1517(3) 0.45648(14) 0.0408(8) Uani 1 1 d . . . H11 H 0.0404 0.2049 0.4738 0.049 Uiso 1 1 calc R . . C12 C 0.1281(3) 0.1176(3) 0.48625(13) 0.0408(8) Uani 1 1 d . . . H12 H 0.1472 0.1466 0.5241 0.049 Uiso 1 1 calc R . . C13 C 0.1639(3) 0.0411(3) 0.46095(12) 0.0309(7) Uani 1 1 d . . . H13 H 0.2084 0.0186 0.4816 0.037 Uiso 1 1 calc R . . C14 C 0.5042(3) 0.1822(3) 0.45953(11) 0.0259(6) Uani 1 1 d . . . C15 C 0.4657(3) 0.1392(3) 0.50505(12) 0.0313(7) Uani 1 1 d . . . H15 H 0.4062 0.0603 0.5009 0.038 Uiso 1 1 calc R . . C16 C 0.5134(3) 0.2105(3) 0.55597(12) 0.0390(8) Uani 1 1 d . . . H16 H 0.4863 0.1806 0.5866 0.047 Uiso 1 1 calc R . . C17 C 0.5997(3) 0.3242(3) 0.56226(13) 0.0419(9) Uani 1 1 d . . . H17 H 0.6317 0.373 0.5974 0.05 Uiso 1 1 calc R . . C18 C 0.6407(3) 0.3687(3) 0.51799(13) 0.0402(8) Uani 1 1 d . . . H18 H 0.7007 0.4476 0.5227 0.048 Uiso 1 1 calc R . . C19 C 0.5937(3) 0.2976(3) 0.46677(12) 0.0326(7) Uani 1 1 d . . . H19 H 0.6227 0.3277 0.4364 0.039 Uiso 1 1 calc R . . C20 C 0.5598(3) 0.0446(3) 0.38009(11) 0.0255(6) Uani 1 1 d . . . C21 C 0.6607(3) 0.0871(3) 0.41679(12) 0.0320(7) Uani 1 1 d . . . H21 H 0.6746 0.1438 0.4487 0.038 Uiso 1 1 calc R . . C22 C 0.7413(3) 0.0480(3) 0.40743(13) 0.0384(8) Uani 1 1 d . . . H22 H 0.8095 0.0777 0.433 0.046 Uiso 1 1 calc R . . C23 C 0.7232(3) -0.0332(3) 0.36161(13) 0.0401(8) Uani 1 1 d . . . H23 H 0.7784 -0.0601 0.3555 0.048 Uiso 1 1 calc R . . C24 C 0.6234(3) -0.0762(3) 0.32389(13) 0.0371(8) Uani 1 1 d . . . H24 H 0.6102 -0.1327 0.292 0.045 Uiso 1 1 calc R . . C25 C 0.5436(3) -0.0362(3) 0.33307(11) 0.0296(7) Uani 1 1 d . . . H25 H 0.4766 -0.0643 0.3069 0.035 Uiso 1 1 calc R . . C26 C 0.0593(3) -0.2715(3) 0.28365(11) 0.0290(7) Uani 1 1 d . . . C27 C -0.0534(3) -0.3103(3) 0.25548(12) 0.0344(7) Uani 1 1 d . . . C28 C -0.1183(3) -0.4242(3) 0.22465(13) 0.0425(9) Uani 1 1 d . . . H28 H -0.1933 -0.4481 0.2057 0.051 Uiso 1 1 calc R . . C29 C -0.0775(3) -0.5040(3) 0.22056(13) 0.0444(9) Uani 1 1 d . . . C30 C 0.0330(3) -0.4651(3) 0.24806(12) 0.0393(8) Uani 1 1 d . . . H30 H 0.0629 -0.5182 0.2458 0.047 Uiso 1 1 calc R . . C31 C 0.1019(3) -0.3523(3) 0.27878(12) 0.0330(7) Uani 1 1 d . . . C32 C -0.1024(3) -0.2277(3) 0.25979(14) 0.0445(9) Uani 1 1 d . . . H32A H -0.1804 -0.2671 0.2381 0.067 Uiso 1 1 calc R . . H32B H -0.0498 -0.159 0.2466 0.067 Uiso 1 1 calc R . . H32C H -0.109 -0.203 0.2974 0.067 Uiso 1 1 calc R . . C33 C -0.1492(4) -0.6272(3) 0.18690(17) 0.0666(12) Uani 1 1 d . . . H33A H -0.2241 -0.6382 0.1705 0.1 Uiso 0.5 1 calc PR . . H33B H -0.1643 -0.6828 0.2097 0.1 Uiso 0.5 1 calc PR . . H33C H -0.1056 -0.6405 0.1586 0.1 Uiso 0.5 1 calc PR . . H33D H -0.1052 -0.6695 0.1887 0.1 Uiso 0.5 1 calc PR . . H33E H -0.1651 -0.6249 0.1495 0.1 Uiso 0.5 1 calc PR . . H33F H -0.2238 -0.6671 0.2007 0.1 Uiso 0.5 1 calc PR . . C34 C 0.2238(3) -0.3163(3) 0.30517(13) 0.0400(8) Uani 1 1 d . . . H34A H 0.2236 -0.3122 0.3438 0.06 Uiso 1 1 calc R . . H34B H 0.2797 -0.2395 0.2995 0.06 Uiso 1 1 calc R . . H34C H 0.247 -0.3739 0.2893 0.06 Uiso 1 1 calc R . . C35 C 0.4771(3) 0.2652(3) 0.35216(11) 0.0274(7) Uani 1 1 d . . . C36 C 0.4415(3) 0.3421(3) 0.37966(13) 0.0329(7) Uani 1 1 d . . . C37 C 0.5022(3) 0.4595(3) 0.37866(14) 0.0412(8) Uani 1 1 d . . . H37 H 0.4781 0.5107 0.3981 0.049 Uiso 1 1 calc R . . C38 C 0.5962(3) 0.5056(3) 0.35060(14) 0.0410(8) Uani 1 1 d . . . C39 C 0.6307(3) 0.4295(3) 0.32385(13) 0.0409(8) Uani 1 1 d . . . H39 H 0.695 0.4588 0.3043 0.049 Uiso 1 1 calc R . . C40 C 0.5748(3) 0.3112(3) 0.32445(12) 0.0339(7) Uani 1 1 d . . . C41 C 0.3392(3) 0.3006(3) 0.41067(16) 0.0492(10) Uani 1 1 d . . . H41A H 0.3539 0.2649 0.4383 0.074 Uiso 1 1 calc R . . H41B H 0.2673 0.2426 0.3861 0.074 Uiso 1 1 calc R . . H41C H 0.3296 0.3671 0.4278 0.074 Uiso 1 1 calc R . . C42 C 0.6575(4) 0.6343(3) 0.34952(19) 0.0644(12) Uani 1 1 d . . . H42A H 0.6201 0.6731 0.3709 0.097 Uiso 0.5 1 calc PR . . H42B H 0.6513 0.642 0.3123 0.097 Uiso 0.5 1 calc PR . . H42C H 0.7407 0.6706 0.3646 0.097 Uiso 0.5 1 calc PR . . H42D H 0.7213 0.6507 0.3277 0.097 Uiso 0.5 1 calc PR . . H42E H 0.6901 0.6818 0.3863 0.097 Uiso 0.5 1 calc PR . . H42F H 0.6007 0.6533 0.3339 0.097 Uiso 0.5 1 calc PR . . C43 C 0.6202(3) 0.2344(3) 0.29631(14) 0.0510(10) Uani 1 1 d . . . H43A H 0.673 0.2741 0.2717 0.076 Uiso 1 1 calc R . . H43B H 0.554 0.1606 0.2758 0.076 Uiso 1 1 calc R . . H43C H 0.6634 0.2185 0.323 0.076 Uiso 1 1 calc R . . C44 C 0.1488(3) -0.0281(3) 0.12044(14) 0.0393(8) Uani 1 1 d . . . H44 H 0.0951 -0.1056 0.1013 0.047 Uiso 1 1 calc R . . C45 C 0.3030(3) -0.0771(3) 0.05820(12) 0.0325(7) Uani 1 1 d . . . C46 C 0.4033(3) -0.0857(4) 0.05198(13) 0.0513(10) Uani 1 1 d . . . H46 H 0.465 -0.0524 0.0815 0.062 Uiso 1 1 calc R . . C47 C 0.4159(4) -0.1419(4) 0.00366(15) 0.0704(14) Uani 1 1 d . . . H47 H 0.4861 -0.1463 0.0002 0.085 Uiso 1 1 calc R . . C48 C 0.3277(4) -0.1914(4) -0.03931(16) 0.0716(13) Uani 1 1 d . . . H48 H 0.3358 -0.231 -0.0724 0.086 Uiso 1 1 calc R . . C49 C 0.2281(4) -0.1828(4) -0.03387(16) 0.0762(15) Uani 1 1 d . . . H49 H 0.167 -0.2158 -0.0636 0.091 Uiso 1 1 calc R . . C50 C 0.2152(4) -0.1262(4) 0.01475(14) 0.0561(11) Uani 1 1 d . . . H50 H 0.1453 -0.1213 0.018 0.067 Uiso 1 1 calc R . . C51 C 0.3827(3) 0.1572(3) 0.12108(12) 0.0308(7) Uani 1 1 d . . . C52 C 0.4649(3) 0.2362(3) 0.16456(15) 0.0441(9) Uani 1 1 d . . . H52 H 0.477 0.21 0.1952 0.053 Uiso 1 1 calc R . . C53 C 0.5300(4) 0.3536(3) 0.16399(19) 0.0617(11) Uani 1 1 d . . . H53 H 0.5854 0.4077 0.1943 0.074 Uiso 1 1 calc R . . C54 C 0.5141(4) 0.3912(4) 0.1196(2) 0.0681(13) Uani 1 1 d . . . H54 H 0.5585 0.4715 0.119 0.082 Uiso 1 1 calc R . . C55 C 0.4341(4) 0.3131(4) 0.07582(19) 0.0624(12) Uani 1 1 d . . . H55 H 0.4242 0.3396 0.0449 0.075 Uiso 1 1 calc R . . C56 C 0.3679(3) 0.1969(3) 0.07614(15) 0.0460(9) Uani 1 1 d . . . H56 H 0.3121 0.1437 0.0457 0.055 Uiso 1 1 calc R . . C57 C 0.0986(3) 0.1611(3) 0.11080(12) 0.0344(7) Uani 1 1 d . . . C58 C 0.1045(4) 0.2660(3) 0.13513(14) 0.0502(10) Uani 1 1 d . . . H58 H 0.1035 0.284 0.1727 0.06 Uiso 1 1 calc R . . C59 C 0.1119(4) 0.3446(4) 0.10491(17) 0.0708(13) Uani 1 1 d . . . H59 H 0.1154 0.416 0.1219 0.085 Uiso 1 1 calc R . . C60 C 0.1142(4) 0.3203(4) 0.05043(17) 0.0682(13) Uani 1 1 d . . . H60 H 0.1211 0.3755 0.0301 0.082 Uiso 1 1 calc R . . C61 C 0.1066(4) 0.2161(4) 0.02560(15) 0.0608(11) Uani 1 1 d . . . H61 H 0.1066 0.1984 -0.0121 0.073 Uiso 1 1 calc R . . C62 C 0.0989(3) 0.1373(4) 0.05520(13) 0.0468(9) Uani 1 1 d . . . H62 H 0.0938 0.0655 0.0377 0.056 Uiso 1 1 calc R . . C63 C -0.0745(3) -0.0597(3) 0.12119(12) 0.0338(7) Uani 1 1 d . . . C64 C -0.1190(3) -0.1728(3) 0.12886(14) 0.0463(9) Uani 1 1 d . . . H64 H -0.0679 -0.1939 0.1456 0.056 Uiso 1 1 calc R . . C65 C -0.2361(4) -0.2547(4) 0.11251(17) 0.0674(13) Uani 1 1 d . . . H65 H -0.2645 -0.3311 0.1185 0.081 Uiso 1 1 calc R . . C66 C -0.3116(4) -0.2279(5) 0.08797(17) 0.0804(16) Uani 1 1 d . . . H66 H -0.3918 -0.2853 0.0765 0.096 Uiso 1 1 calc R . . C67 C -0.2706(4) -0.1168(5) 0.07989(15) 0.0690(14) Uani 1 1 d . . . H67 H -0.3229 -0.0975 0.0629 0.083 Uiso 1 1 calc R . . C68 C -0.1530(3) -0.0326(4) 0.09643(13) 0.0492(10) Uani 1 1 d . . . H68 H -0.1258 0.0439 0.0909 0.059 Uiso 1 1 calc R . . C69 C 0.3803(3) -0.1061(3) 0.17451(11) 0.0335(7) Uani 1 1 d . . . C70 C 0.4992(3) -0.0807(3) 0.18106(12) 0.0379(8) Uani 1 1 d . . . C71 C 0.5258(4) -0.1674(4) 0.18739(14) 0.0508(10) Uani 1 1 d . . . H71 H 0.6059 -0.1493 0.1913 0.061 Uiso 1 1 calc R . . C72 C 0.4403(5) -0.2787(4) 0.18822(15) 0.0621(12) Uani 1 1 d . . . C73 C 0.3240(5) -0.3040(3) 0.18036(14) 0.0618(12) Uani 1 1 d . . . H73 H 0.2638 -0.3811 0.1797 0.074 Uiso 1 1 calc R . . C74 C 0.2918(3) -0.2201(3) 0.17333(13) 0.0453(9) Uani 1 1 d . . . C75 C 0.5989(3) 0.0379(3) 0.17955(14) 0.0440(9) Uani 1 1 d . . . H75A H 0.6494 0.074 0.2145 0.066 Uiso 1 1 calc R . . H75B H 0.5669 0.0877 0.1715 0.066 Uiso 1 1 calc R . . H75C H 0.6453 0.0291 0.1516 0.066 Uiso 1 1 calc R . . C76 C 0.4706(6) -0.3713(5) 0.1976(2) 0.107(2) Uani 1 1 d . . . H76A H 0.5563 -0.3385 0.2024 0.161 Uiso 0.5 1 calc PR . . H76B H 0.4349 -0.4381 0.1665 0.161 Uiso 0.5 1 calc PR . . H76C H 0.4403 -0.3972 0.2299 0.161 Uiso 0.5 1 calc PR . . H76D H 0.398 -0.444 0.1968 0.161 Uiso 0.5 1 calc PR . . H76E H 0.5194 -0.3445 0.2327 0.161 Uiso 0.5 1 calc PR . . H76F H 0.514 -0.3853 0.1693 0.161 Uiso 0.5 1 calc PR . . C77 C 0.1634(3) -0.2567(3) 0.16033(14) 0.0531(10) Uani 1 1 d . . . H77A H 0.1452 -0.2026 0.1842 0.08 Uiso 1 1 calc R . . H77B H 0.1151 -0.336 0.1655 0.08 Uiso 1 1 calc R . . H77C H 0.1463 -0.2553 0.1229 0.08 Uiso 1 1 calc R . . C78 C 0.0959(3) 0.1784(3) 0.24546(11) 0.0284(7) Uani 1 1 d . . . C79 C -0.0152(3) 0.1506(3) 0.26159(12) 0.0333(7) Uani 1 1 d . . . C80 C -0.0249(3) 0.2326(3) 0.30046(13) 0.0405(8) Uani 1 1 d . . . H80 H -0.1002 0.214 0.3104 0.049 Uiso 1 1 calc R . . C81 C 0.0703(4) 0.3401(3) 0.32519(13) 0.0465(9) Uani 1 1 d . . . C82 C 0.1783(4) 0.3664(3) 0.30875(13) 0.0455(9) Uani 1 1 d . . . H82 H 0.2447 0.4398 0.325 0.055 Uiso 1 1 calc R . . C83 C 0.1930(3) 0.2886(3) 0.26910(12) 0.0362(8) Uani 1 1 d . . . C84 C -0.1224(3) 0.0360(3) 0.23891(14) 0.0423(8) Uani 1 1 d . . . H84A H -0.1799 0.0209 0.2641 0.063 Uiso 1 1 calc R . . H84B H -0.1011 -0.0261 0.2332 0.063 Uiso 1 1 calc R . . H84C H -0.1566 0.038 0.2045 0.063 Uiso 1 1 calc R . . C85 C 0.0551(5) 0.4232(4) 0.36847(16) 0.0700(13) Uani 1 1 d . . . H85A H -0.0275 0.3884 0.3741 0.105 Uiso 0.5 1 calc PR . . H85B H 0.0782 0.4967 0.3575 0.105 Uiso 0.5 1 calc PR . . H85C H 0.1047 0.4386 0.402 0.105 Uiso 0.5 1 calc PR . . H85D H 0.1311 0.4941 0.3816 0.105 Uiso 0.5 1 calc PR . . H85E H 0.0254 0.3858 0.3983 0.105 Uiso 0.5 1 calc PR . . H85F H -0.0011 0.4439 0.3537 0.105 Uiso 0.5 1 calc PR . . C86 C 0.3112(3) 0.3257(3) 0.25079(14) 0.0453(9) Uani 1 1 d . . . H86A H 0.3639 0.4088 0.267 0.068 Uiso 1 1 calc R . . H86B H 0.3022 0.3131 0.2115 0.068 Uiso 1 1 calc R . . H86C H 0.3446 0.2794 0.2619 0.068 Uiso 1 1 calc R . . C87 C 0.2529(8) 0.5693(7) 0.0072(3) 0.059(2) Uani 0.5 1 d P . . C88 C 0.2134(9) 0.5113(8) -0.0457(4) 0.077(3) Uani 0.5 1 d P . . H88 H 0.267 0.4998 -0.0668 0.092 Uiso 0.5 1 calc PR . . C89 C 0.0999(9) 0.4687(9) -0.0697(3) 0.074(3) Uani 0.5 1 d P . . H89 H 0.0761 0.4278 -0.1064 0.089 Uiso 0.5 1 calc PR . . C90 C 0.0263(10) 0.4846(8) -0.0421(4) 0.070(3) Uani 0.5 1 d P . . H90 H -0.0519 0.4553 -0.0589 0.084 Uiso 0.5 1 calc PR . . C91 C 0.0586(10) 0.5439(9) 0.0117(4) 0.083(3) Uani 0.5 1 d P . . H91 H 0.0035 0.5543 0.032 0.099 Uiso 0.5 1 calc PR . . C92 C 0.1747(9) 0.5877(7) 0.0348(3) 0.063(2) Uani 0.5 1 d P . . H92 H 0.1996 0.6318 0.071 0.076 Uiso 0.5 1 calc PR . . C93 C 0.3738(10) 0.6037(12) 0.0347(5) 0.120(4) Uani 0.5 1 d P . . H93A H 0.384 0.643 0.0724 0.18 Uiso 0.25 1 calc PR . . H93B H 0.4342 0.6567 0.0165 0.18 Uiso 0.25 1 calc PR . . H93C H 0.3814 0.5335 0.033 0.18 Uiso 0.25 1 calc PR . . H93D H 0.4157 0.5791 0.0089 0.18 Uiso 0.25 1 calc PR . . H93E H 0.3656 0.5654 0.0647 0.18 Uiso 0.25 1 calc PR . . H93F H 0.4183 0.6887 0.0483 0.18 Uiso 0.25 1 calc PR . . 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 Ba 0.02558(10) 0.03239(11) 0.01931(9) 0.00802(7) 0.00342(7) 0.01538(8) P1 0.0218(4) 0.0259(4) 0.0217(4) 0.0077(3) 0.0047(3) 0.0124(3) P2 0.0196(4) 0.0282(4) 0.0213(4) 0.0048(3) 0.0026(3) 0.0121(3) P3 0.0240(4) 0.0307(4) 0.0275(4) 0.0008(3) 0.0059(3) 0.0146(4) P4 0.0252(4) 0.0327(5) 0.0281(4) 0.0057(3) 0.0044(3) 0.0177(4) N1 0.0262(14) 0.0317(15) 0.0220(13) 0.0092(11) 0.0023(10) 0.0129(12) N2 0.0254(14) 0.0291(14) 0.0202(12) 0.0031(10) -0.0015(10) 0.0117(12) N3 0.0299(15) 0.0347(15) 0.0268(14) 0.0011(11) 0.0054(11) 0.0169(13) N4 0.0279(14) 0.0347(15) 0.0275(13) 0.0081(11) 0.0021(11) 0.0185(12) C1 0.0227(16) 0.0269(17) 0.0360(17) 0.0078(13) 0.0031(13) 0.0143(14) C2 0.0228(16) 0.0274(16) 0.0201(14) 0.0042(12) 0.0035(12) 0.0130(13) C3 0.0279(17) 0.0371(18) 0.0279(16) 0.0102(14) 0.0035(13) 0.0140(15) C4 0.0264(17) 0.039(2) 0.0381(19) 0.0131(15) 0.0089(14) 0.0110(15) C5 0.043(2) 0.0277(18) 0.0383(19) 0.0123(15) 0.0128(16) 0.0162(16) C6 0.040(2) 0.0339(19) 0.0345(18) 0.0144(15) 0.0056(15) 0.0216(16) C7 0.0264(17) 0.0303(17) 0.0284(16) 0.0075(13) 0.0019(13) 0.0153(14) C8 0.0214(16) 0.0288(16) 0.0262(16) 0.0101(13) 0.0073(12) 0.0120(14) C9 0.0265(17) 0.0365(18) 0.0321(17) 0.0098(14) 0.0075(13) 0.0172(15) C10 0.0290(18) 0.044(2) 0.050(2) 0.0156(17) 0.0105(16) 0.0254(17) C11 0.036(2) 0.040(2) 0.053(2) 0.0049(17) 0.0141(17) 0.0250(17) C12 0.039(2) 0.050(2) 0.0322(18) 0.0005(16) 0.0083(15) 0.0237(18) C13 0.0291(18) 0.0349(18) 0.0319(17) 0.0068(14) 0.0050(14) 0.0184(15) C14 0.0262(16) 0.0348(18) 0.0240(15) 0.0067(13) 0.0018(12) 0.0209(15) C15 0.0311(18) 0.0395(19) 0.0267(16) 0.0095(14) 0.0052(13) 0.0192(15) C16 0.044(2) 0.059(2) 0.0242(17) 0.0096(16) 0.0066(15) 0.032(2) C17 0.050(2) 0.057(2) 0.0268(18) -0.0051(16) -0.0036(16) 0.038(2) C18 0.040(2) 0.0322(19) 0.044(2) -0.0007(16) -0.0079(16) 0.0187(17) C19 0.0345(19) 0.0331(18) 0.0305(17) 0.0059(14) 0.0001(14) 0.0175(16) C20 0.0223(16) 0.0295(17) 0.0254(15) 0.0081(13) 0.0055(12) 0.0125(14) C21 0.0272(17) 0.042(2) 0.0268(16) 0.0040(14) 0.0026(13) 0.0181(16) C22 0.0271(18) 0.057(2) 0.0354(19) 0.0103(17) 0.0025(14) 0.0242(17) C23 0.036(2) 0.057(2) 0.041(2) 0.0123(17) 0.0119(16) 0.0328(19) C24 0.037(2) 0.050(2) 0.0285(17) 0.0054(15) 0.0106(15) 0.0258(17) C25 0.0261(17) 0.0390(19) 0.0240(16) 0.0063(14) 0.0031(13) 0.0167(15) C26 0.0319(18) 0.0341(18) 0.0187(15) 0.0078(13) 0.0050(13) 0.0136(15) C27 0.0330(18) 0.044(2) 0.0221(16) 0.0098(14) 0.0050(14) 0.0142(16) C28 0.0309(19) 0.051(2) 0.0307(18) 0.0083(16) 0.0014(15) 0.0092(18) C29 0.046(2) 0.040(2) 0.0287(18) 0.0020(15) 0.0071(16) 0.0078(18) C30 0.049(2) 0.036(2) 0.0304(18) 0.0064(15) 0.0098(16) 0.0191(18) C31 0.0371(19) 0.0342(19) 0.0229(16) 0.0060(14) 0.0041(14) 0.0138(16) C32 0.036(2) 0.059(2) 0.040(2) 0.0145(18) 0.0006(16) 0.0230(19) C33 0.066(3) 0.048(3) 0.055(3) -0.005(2) 0.006(2) 0.009(2) C34 0.045(2) 0.043(2) 0.0387(19) 0.0044(16) 0.0049(16) 0.0287(18) C35 0.0250(16) 0.0355(18) 0.0242(15) 0.0094(13) 0.0001(13) 0.0162(14) C36 0.0263(17) 0.0349(19) 0.0387(18) 0.0127(15) 0.0052(14) 0.0143(15) C37 0.034(2) 0.035(2) 0.057(2) 0.0121(17) 0.0030(17) 0.0190(17) C38 0.0274(18) 0.036(2) 0.056(2) 0.0209(17) 0.0027(16) 0.0097(16) C39 0.0297(19) 0.052(2) 0.044(2) 0.0261(18) 0.0098(16) 0.0167(17) C40 0.0306(18) 0.047(2) 0.0293(17) 0.0167(15) 0.0067(14) 0.0206(16) C41 0.043(2) 0.046(2) 0.072(3) 0.021(2) 0.028(2) 0.0281(19) C42 0.048(3) 0.050(3) 0.099(3) 0.038(2) 0.017(2) 0.018(2) C43 0.051(2) 0.067(3) 0.045(2) 0.023(2) 0.0284(19) 0.032(2) C44 0.0228(17) 0.0300(18) 0.059(2) -0.0037(16) 0.0063(15) 0.0127(15) C45 0.0338(18) 0.0388(19) 0.0271(16) 0.0024(14) 0.0035(14) 0.0213(16) C46 0.044(2) 0.090(3) 0.0273(18) -0.0019(19) 0.0061(16) 0.044(2) C47 0.066(3) 0.122(4) 0.041(2) -0.004(2) 0.011(2) 0.068(3) C48 0.094(4) 0.100(4) 0.035(2) -0.012(2) 0.006(2) 0.068(3) C49 0.091(4) 0.100(4) 0.040(2) -0.025(2) -0.022(2) 0.065(3) C50 0.054(3) 0.075(3) 0.043(2) -0.016(2) -0.0115(19) 0.047(2) C51 0.0275(17) 0.0311(18) 0.0360(18) 0.0047(14) 0.0116(14) 0.0167(15) C52 0.036(2) 0.038(2) 0.053(2) 0.0047(17) 0.0076(17) 0.0160(18) C53 0.048(3) 0.039(2) 0.077(3) -0.005(2) 0.012(2) 0.011(2) C54 0.069(3) 0.033(2) 0.100(4) 0.018(3) 0.044(3) 0.019(2) C55 0.074(3) 0.053(3) 0.074(3) 0.033(2) 0.032(3) 0.034(3) C56 0.051(2) 0.049(2) 0.044(2) 0.0154(18) 0.0156(18) 0.026(2) C57 0.0369(19) 0.0382(19) 0.0291(17) 0.0075(14) 0.0027(14) 0.0193(16) C58 0.080(3) 0.047(2) 0.0282(18) 0.0080(16) -0.0048(18) 0.036(2) C59 0.109(4) 0.054(3) 0.053(3) 0.016(2) -0.009(2) 0.043(3) C60 0.086(3) 0.072(3) 0.053(3) 0.035(2) 0.002(2) 0.037(3) C61 0.070(3) 0.095(4) 0.032(2) 0.025(2) 0.0104(19) 0.047(3) C62 0.054(2) 0.068(3) 0.0287(18) 0.0122(18) 0.0098(17) 0.037(2) C63 0.0288(18) 0.050(2) 0.0224(16) 0.0042(15) 0.0059(13) 0.0198(16) C64 0.033(2) 0.056(2) 0.038(2) 0.0076(18) 0.0081(16) 0.0139(18) C65 0.035(2) 0.072(3) 0.056(3) 0.008(2) 0.010(2) -0.002(2) C66 0.029(2) 0.114(5) 0.048(3) -0.006(3) 0.003(2) 0.004(3) C67 0.033(2) 0.130(5) 0.039(2) 0.001(3) -0.0005(18) 0.043(3) C68 0.040(2) 0.084(3) 0.0307(19) 0.0061(19) 0.0026(16) 0.038(2) C69 0.046(2) 0.040(2) 0.0188(15) 0.0055(14) 0.0081(14) 0.0238(17) C70 0.051(2) 0.050(2) 0.0223(16) 0.0019(15) 0.0028(15) 0.0351(19) C71 0.073(3) 0.057(3) 0.038(2) 0.0042(18) -0.0001(19) 0.047(2) C72 0.101(4) 0.062(3) 0.042(2) 0.009(2) 0.003(2) 0.057(3) C73 0.104(4) 0.033(2) 0.037(2) 0.0085(17) 0.007(2) 0.024(2) C74 0.063(3) 0.041(2) 0.0235(17) 0.0077(15) 0.0079(16) 0.019(2) C75 0.032(2) 0.053(2) 0.049(2) -0.0019(17) 0.0009(16) 0.0267(18) C76 0.184(7) 0.089(4) 0.091(4) 0.025(3) 0.002(4) 0.100(5) C77 0.055(3) 0.038(2) 0.041(2) 0.0057(17) 0.0085(18) 0.0042(19) C78 0.0329(18) 0.0362(18) 0.0203(15) 0.0107(13) 0.0002(13) 0.0190(15) C79 0.0379(19) 0.044(2) 0.0226(16) 0.0121(14) 0.0034(14) 0.0226(17) C80 0.054(2) 0.049(2) 0.0313(18) 0.0159(16) 0.0140(17) 0.032(2) C81 0.073(3) 0.043(2) 0.0303(19) 0.0065(16) 0.0088(18) 0.034(2) C82 0.058(3) 0.037(2) 0.0313(19) 0.0048(16) -0.0016(17) 0.0160(18) C83 0.041(2) 0.0330(19) 0.0307(18) 0.0080(15) -0.0026(15) 0.0155(16) C84 0.033(2) 0.049(2) 0.043(2) 0.0052(17) 0.0118(16) 0.0198(18) C85 0.103(4) 0.056(3) 0.052(3) 0.004(2) 0.024(2) 0.041(3) C86 0.036(2) 0.040(2) 0.048(2) 0.0071(17) -0.0037(17) 0.0120(17) C87 0.057(6) 0.048(5) 0.052(5) 0.010(4) 0.006(4) 0.012(4) C88 0.078(7) 0.063(6) 0.054(6) 0.007(5) 0.021(5) 0.008(5) C89 0.080(7) 0.080(7) 0.038(5) -0.006(4) -0.009(5) 0.027(6) C90 0.095(8) 0.068(6) 0.053(6) -0.007(5) -0.021(6) 0.054(6) C91 0.097(8) 0.092(8) 0.071(7) -0.017(6) -0.014(6) 0.070(7) C92 0.088(7) 0.064(6) 0.041(5) -0.001(4) -0.012(5) 0.046(5) C93 0.070(8) 0.160(13) 0.105(9) 0.013(9) 0.008(7) 0.043(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ba N2 2.736(2) . ? Ba N4 2.754(2) . ? Ba N3 2.756(2) . ? Ba N1 2.768(2) . ? P1 N1 1.612(2) . ? P1 C1 1.713(3) . ? P1 C2 1.822(3) . ? P1 C8 1.823(3) . ? P2 N2 1.609(2) . ? P2 C1 1.708(3) . ? P2 C14 1.838(3) . ? P2 C20 1.841(3) . ? P3 N3 1.604(3) . ? P3 C44 1.722(3) . ? P3 C51 1.818(3) . ? P3 C45 1.825(3) . ? P4 N4 1.602(2) . ? P4 C44 1.702(3) . ? P4 C57 1.817(3) . ? P4 C63 1.835(3) . ? N1 C26 1.410(4) . ? N2 C35 1.431(4) . ? N3 C69 1.417(4) . ? N4 C78 1.424(4) . ? C2 C3 1.393(4) . ? C2 C7 1.394(4) . ? C3 C4 1.381(4) . ? C4 C5 1.384(4) . ? C5 C6 1.376(4) . ? C6 C7 1.386(4) . ? C8 C9 1.392(4) . ? C8 C13 1.392(4) . ? C9 C10 1.378(4) . ? C10 C11 1.383(5) . ? C11 C12 1.381(5) . ? C12 C13 1.381(4) . ? C14 C19 1.395(4) . ? C14 C15 1.399(4) . ? C15 C16 1.382(4) . ? C16 C17 1.370(5) . ? C17 C18 1.384(5) . ? C18 C19 1.387(4) . ? C20 C21 1.390(4) . ? C20 C25 1.394(4) . ? C21 C22 1.387(4) . ? C22 C23 1.368(5) . ? C23 C24 1.394(5) . ? C24 C25 1.385(4) . ? C26 C27 1.416(4) . ? C26 C31 1.417(4) . ? C27 C28 1.392(5) . ? C27 C32 1.502(5) . ? C28 C29 1.387(5) . ? C29 C30 1.384(5) . ? C29 C33 1.510(5) . ? C30 C31 1.386(4) . ? C31 C34 1.511(4) . ? C35 C36 1.403(4) . ? C35 C40 1.411(4) . ? C36 C37 1.388(4) . ? C36 C41 1.504(4) . ? C37 C38 1.384(5) . ? C38 C39 1.378(5) . ? C38 C42 1.519(5) . ? C39 C40 1.394(5) . ? C40 C43 1.501(5) . ? C45 C50 1.377(5) . ? C45 C46 1.378(4) . ? C46 C47 1.381(5) . ? C47 C48 1.372(6) . ? C48 C49 1.365(6) . ? C49 C50 1.392(5) . ? C51 C52 1.380(5) . ? C51 C56 1.393(4) . ? C52 C53 1.388(5) . ? C53 C54 1.369(6) . ? C54 C55 1.370(6) . ? C55 C56 1.374(5) . ? C57 C58 1.387(4) . ? C57 C62 1.400(4) . ? C58 C59 1.383(5) . ? C59 C60 1.376(6) . ? C60 C61 1.373(6) . ? C61 C62 1.373(5) . ? C63 C64 1.394(5) . ? C63 C68 1.398(4) . ? C64 C65 1.381(5) . ? C65 C66 1.361(7) . ? C66 C67 1.377(7) . ? C67 C68 1.392(6) . ? C69 C74 1.402(5) . ? C69 C70 1.416(5) . ? C70 C71 1.387(5) . ? C70 C75 1.509(5) . ? C71 C72 1.377(6) . ? C72 C73 1.386(6) . ? C72 C76 1.516(5) . ? C73 C74 1.405(5) . ? C74 C77 1.508(5) . ? C78 C83 1.409(4) . ? C78 C79 1.415(4) . ? C79 C80 1.394(4) . ? C79 C84 1.489(5) . ? C80 C81 1.385(5) . ? C81 C82 1.384(5) . ? C81 C85 1.506(5) . ? C82 C83 1.399(5) . ? C83 C86 1.504(5) . ? C87 C92 1.351(12) . ? C87 C88 1.370(11) . ? C87 C93 1.516(13) . ? C88 C89 1.376(13) . ? C89 C90 1.286(13) . ? C90 C91 1.392(13) . ? C91 C92 1.396(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 N2 Ba N4 126.95(7) . . ? N2 Ba N3 110.86(7) . . ? N4 Ba N3 96.10(7) . . ? N2 Ba N1 89.30(7) . . ? N4 Ba N1 114.74(7) . . ? N3 Ba N1 121.45(7) . . ? N1 P1 C1 119.55(13) . . ? N1 P1 C2 110.12(13) . . ? C1 P1 C2 108.46(13) . . ? N1 P1 C8 107.41(13) . . ? C1 P1 C8 108.14(14) . . ? C2 P1 C8 101.66(12) . . ? N2 P2 C1 112.68(13) . . ? N2 P2 C14 111.16(12) . . ? C1 P2 C14 113.95(14) . . ? N2 P2 C20 116.10(13) . . ? C1 P2 C20 101.50(13) . . ? C14 P2 C20 100.67(13) . . ? N3 P3 C44 117.64(15) . . ? N3 P3 C51 105.98(14) . . ? C44 P3 C51 108.57(15) . . ? N3 P3 C45 111.86(13) . . ? C44 P3 C45 106.78(16) . . ? C51 P3 C45 105.32(14) . . ? N4 P4 C44 111.89(15) . . ? N4 P4 C57 112.74(14) . . ? C44 P4 C57 113.10(16) . . ? N4 P4 C63 116.23(13) . . ? C44 P4 C63 101.39(16) . . ? C57 P4 C63 100.59(15) . . ? C26 N1 P1 125.70(19) . . ? C26 N1 Ba 120.68(17) . . ? P1 N1 Ba 109.56(12) . . ? C35 N2 P2 123.94(19) . . ? C35 N2 Ba 111.95(16) . . ? P2 N2 Ba 123.79(12) . . ? C69 N3 P3 128.5(2) . . ? C69 N3 Ba 110.16(17) . . ? P3 N3 Ba 107.71(11) . . ? C78 N4 P4 130.83(19) . . ? C78 N4 Ba 112.67(16) . . ? P4 N4 Ba 116.36(12) . . ? P2 C1 P1 131.40(17) . . ? C3 C2 C7 118.6(3) . . ? C3 C2 P1 118.9(2) . . ? C7 C2 P1 122.4(2) . . ? C4 C3 C2 120.7(3) . . ? C3 C4 C5 120.1(3) . . ? C6 C5 C4 119.9(3) . . ? C5 C6 C7 120.3(3) . . ? C6 C7 C2 120.4(3) . . ? C9 C8 C13 118.6(3) . . ? C9 C8 P1 122.8(2) . . ? C13 C8 P1 118.5(2) . . ? C10 C9 C8 120.5(3) . . ? C9 C10 C11 120.4(3) . . ? C12 C11 C10 119.8(3) . . ? C13 C12 C11 120.0(3) . . ? C12 C13 C8 120.8(3) . . ? C19 C14 C15 118.5(3) . . ? C19 C14 P2 122.6(2) . . ? C15 C14 P2 118.7(2) . . ? C16 C15 C14 120.6(3) . . ? C17 C16 C15 120.0(3) . . ? C16 C17 C18 120.6(3) . . ? C17 C18 C19 119.7(3) . . ? C18 C19 C14 120.5(3) . . ? C21 C20 C25 118.0(3) . . ? C21 C20 P2 123.1(2) . . ? C25 C20 P2 118.7(2) . . ? C22 C21 C20 120.9(3) . . ? C23 C22 C21 120.5(3) . . ? C22 C23 C24 119.7(3) . . ? C25 C24 C23 119.7(3) . . ? C24 C25 C20 121.1(3) . . ? N1 C26 C27 118.6(3) . . ? N1 C26 C31 123.9(3) . . ? C27 C26 C31 117.5(3) . . ? C28 C27 C26 120.2(3) . . ? C28 C27 C32 120.5(3) . . ? C26 C27 C32 119.3(3) . . ? C29 C28 C27 122.4(3) . . ? C30 C29 C28 117.0(3) . . ? C30 C29 C33 121.3(4) . . ? C28 C29 C33 121.6(4) . . ? C29 C30 C31 123.0(3) . . ? C30 C31 C26 120.0(3) . . ? C30 C31 C34 119.1(3) . . ? C26 C31 C34 120.9(3) . . ? C36 C35 C40 118.2(3) . . ? C36 C35 N2 120.6(3) . . ? C40 C35 N2 121.1(3) . . ? C37 C36 C35 119.5(3) . . ? C37 C36 C41 118.8(3) . . ? C35 C36 C41 121.7(3) . . ? C38 C37 C36 123.1(3) . . ? C39 C38 C37 117.0(3) . . ? C39 C38 C42 122.1(3) . . ? C37 C38 C42 121.0(3) . . ? C38 C39 C40 122.5(3) . . ? C39 C40 C35 119.7(3) . . ? C39 C40 C43 119.6(3) . . ? C35 C40 C43 120.7(3) . . ? P4 C44 P3 134.4(2) . . ? C50 C45 C46 118.1(3) . . ? C50 C45 P3 122.4(3) . . ? C46 C45 P3 119.5(2) . . ? C45 C46 C47 121.2(3) . . ? C48 C47 C46 120.4(4) . . ? C49 C48 C47 119.1(4) . . ? C48 C49 C50 120.6(4) . . ? C45 C50 C49 120.6(4) . . ? C52 C51 C56 118.8(3) . . ? C52 C51 P3 121.3(2) . . ? C56 C51 P3 119.9(3) . . ? C51 C52 C53 120.6(4) . . ? C54 C53 C52 119.8(4) . . ? C53 C54 C55 120.0(4) . . ? C54 C55 C56 120.8(4) . . ? C55 C56 C51 120.0(4) . . ? C58 C57 C62 118.1(3) . . ? C58 C57 P4 124.2(2) . . ? C62 C57 P4 117.6(3) . . ? C59 C58 C57 120.3(3) . . ? C60 C59 C58 120.6(4) . . ? C61 C60 C59 119.8(4) . . ? C62 C61 C60 120.1(4) . . ? C61 C62 C57 121.1(4) . . ? C64 C63 C68 117.5(3) . . ? C64 C63 P4 119.6(2) . . ? C68 C63 P4 122.9(3) . . ? C65 C64 C63 121.0(4) . . ? C66 C65 C64 121.1(5) . . ? C65 C66 C67 119.4(4) . . ? C66 C67 C68 120.5(4) . . ? C67 C68 C63 120.5(4) . . ? C74 C69 C70 118.7(3) . . ? C74 C69 N3 121.3(3) . . ? C70 C69 N3 119.9(3) . . ? C71 C70 C69 119.7(3) . . ? C71 C70 C75 118.4(3) . . ? C69 C70 C75 121.8(3) . . ? C72 C71 C70 122.4(4) . . ? C71 C72 C73 117.6(4) . . ? C71 C72 C76 122.0(5) . . ? C73 C72 C76 120.4(5) . . ? C72 C73 C74 122.4(4) . . ? C69 C74 C73 119.0(4) . . ? C69 C74 C77 121.5(3) . . ? C73 C74 C77 119.3(4) . . ? C83 C78 C79 118.7(3) . . ? C83 C78 N4 118.5(3) . . ? C79 C78 N4 122.6(3) . . ? C80 C79 C78 119.1(3) . . ? C80 C79 C84 118.6(3) . . ? C78 C79 C84 122.3(3) . . ? C81 C80 C79 123.0(3) . . ? C82 C81 C80 117.3(3) . . ? C82 C81 C85 122.2(4) . . ? C80 C81 C85 120.5(4) . . ? C81 C82 C83 122.3(3) . . ? C82 C83 C78 119.6(3) . . ? C82 C83 C86 119.5(3) . . ? C78 C83 C86 120.9(3) . . ? C92 C87 C88 116.0(9) . . ? C92 C87 C93 121.3(8) . . ? C88 C87 C93 122.5(9) . . ? C87 C88 C89 123.2(9) . . ? C90 C89 C88 119.5(9) . . ? C89 C90 C91 121.5(10) . . ? C90 C91 C92 117.8(11) . . ? C87 C92 C91 121.9(8) . . ? #===END