# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1368 data_cmpd_1b _audit_creation_method SHELXL _chemical_formula_moiety 'Mo2(C15H15N2O2)(CH3CN)6,(BF4)3,(CH3CN)1.59' _chemical_formula_sum 'C30.18 H37.77 B3 F12 Mo2 N9.59 O2' _chemical_formula_weight 1019.20 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.017(8) _cell_length_b 11.065(8) _cell_length_c 18.77(2) _cell_angle_alpha 87.28(3) _cell_angle_beta 85.49(4) _cell_angle_gamma 82.67(5) _cell_volume 2260(4) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 9.1 _cell_measurement_theta_max 20.8 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method ? _exptl_crystal_F_000 1018 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.94 _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius FAST' _diffrn_measurement_method 'Ellipsoid mask-fitting' _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10309 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5562 _reflns_number_observed 4775 _reflns_observed_criterion >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL (Bruker, 1990)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 141 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^)+(0.0800P)^2^+25.0000P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5421 _refine_ls_number_parameters 526 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_obs 0.1007 _refine_ls_wR_factor_all 0.2554 _refine_ls_wR_factor_obs 0.2432 _refine_ls_goodness_of_fit_all 1.256 _refine_ls_goodness_of_fit_obs 1.315 _refine_ls_restrained_S_all 1.256 _refine_ls_restrained_S_obs 1.297 _refine_ls_shift/esd_max -0.006 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.81083(9) 0.76881(10) 0.18643(5) 0.0456(4) Uani 1 d . . Mo2 Mo 0.81429(9) 0.66783(10) 0.28728(5) 0.0454(4) Uani 1 d . . O1 O 1.1314(10) 0.7192(11) -0.1414(5) 0.087(3) Uani 1 d . . O2 O 1.1492(9) 0.1668(10) 0.4302(6) 0.087(3) Uani 1 d . . N1 N 0.9567(9) 0.6499(9) 0.1418(5) 0.049(2) Uani 1 d . . N2 N 0.9618(9) 0.5452(9) 0.2487(5) 0.047(2) Uani 1 d . . N3 N 0.9337(10) 0.8980(10) 0.2039(6) 0.058(3) Uani 1 d . . N4 N 0.9334(10) 0.7644(11) 0.3429(6) 0.064(3) Uani 1 d . . N5 N 0.6622(10) 0.9112(10) 0.2132(6) 0.054(3) Uani 1 d . . N6 N 0.6663(10) 0.7653(11) 0.3503(6) 0.060(3) Uani 1 d . . N7 N 0.6737(9) 0.6867(10) 0.1393(5) 0.053(3) Uani 1 d . . N8 N 0.6796(10) 0.5486(10) 0.2762(6) 0.058(3) Uani 1 d . . C1 C 1.0067(10) 0.5577(11) 0.1824(6) 0.044(3) Uani 1 d . . H1A H 1.0719(10) 0.5035(11) 0.1642(6) 0.053 Uiso 1 calc R . C11 C 1.0052(11) 0.6636(11) 0.0690(6) 0.049(3) Uani 1 d . . C12 C 1.1288(13) 0.6748(15) 0.0540(7) 0.074(4) Uani 1 d . . H12A H 1.1808(13) 0.6717(15) 0.0909(7) 0.088 Uiso 1 calc R . C13 C 1.1749(14) 0.6910(16) -0.0174(8) 0.082(5) Uani 1 d . . H13A H 1.2571(14) 0.7011(16) -0.0273(8) 0.099 Uiso 1 calc R . C14 C 1.1014(12) 0.6922(15) -0.0718(7) 0.065(4) Uani 1 d . . C15 C 0.9761(13) 0.6844(13) -0.0569(7) 0.066(4) Uani 1 d . . H15A H 0.9232(13) 0.6902(13) -0.0935(7) 0.080 Uiso 1 calc R . C16 C 0.9334(12) 0.6678(13) 0.0133(7) 0.062(4) Uani 1 d . . H16A H 0.8508(12) 0.6591(13) 0.0231(7) 0.074 Uiso 1 calc R . C17 C 1.2532(17) 0.7431(22) -0.1594(9) 0.115(7) Uani 1 d . . H17A H 1.2639(17) 0.7610(22) -0.2099(9) 0.173 Uiso 1 calc R . H17B H 1.3090(17) 0.6728(22) -0.1469(9) 0.173 Uiso 1 calc R . H17C H 1.2694(17) 0.8115(22) -0.1338(9) 0.173 Uiso 1 calc R . C21 C 1.0122(11) 0.4446(11) 0.2913(6) 0.050(3) Uani 1 d . . C22 C 1.1362(13) 0.4253(16) 0.3038(10) 0.090(5) Uani 1 d . . H22A H 1.1883(13) 0.4782(16) 0.2821(10) 0.109 Uiso 1 calc R . C23 C 1.1844(14) 0.3296(15) 0.3478(9) 0.084(5) Uani 1 d . . H23A H 1.2685(14) 0.3174(15) 0.3526(9) 0.101 Uiso 1 calc R . C24 C 1.1159(12) 0.2575(12) 0.3821(7) 0.058(3) Uani 1 d . . C25 C 0.9903(16) 0.2731(17) 0.3724(10) 0.099(6) Uani 1 d . . H25A H 0.9394(16) 0.2218(17) 0.3971(10) 0.119 Uiso 1 calc R . C26 C 0.9419(14) 0.3639(15) 0.3267(9) 0.080(5) Uani 1 d . . H26A H 0.8587(14) 0.3709(15) 0.3195(9) 0.096 Uiso 1 calc R . C27 C 1.2733(17) 0.1475(20) 0.4467(13) 0.125(8) Uani 1 d . . H27A H 1.2846(17) 0.0810(20) 0.4812(13) 0.188 Uiso 1 calc R . H27B H 1.2949(17) 0.2200(20) 0.4660(13) 0.188 Uiso 1 calc R . H27C H 1.3246(17) 0.1283(20) 0.4040(13) 0.188 Uiso 1 calc R . C31 C 0.9947(13) 0.9737(13) 0.2115(9) 0.069(4) Uani 1 d . . C32 C 1.0624(20) 1.0717(16) 0.2185(13) 0.130(9) Uani 1 d . . H32A H 1.0549(140) 1.1260(90) 0.1772(47) 0.195 Uiso 1 calc R . H32B H 1.1472(32) 1.0409(22) 0.2225(99) 0.195 Uiso 1 calc R . H32C H 1.0312(108) 1.1149(99) 0.2606(55) 0.195 Uiso 1 calc R . C41 C 0.9824(13) 0.8241(14) 0.3756(7) 0.065(4) Uani 1 d . . C42 C 1.0464(18) 0.8947(20) 0.4198(10) 0.111(7) Uani 1 d . . H42A H 0.9880(18) 0.9441(103) 0.4502(58) 0.167 Uiso 1 calc R . H42B H 1.0945(109) 0.9462(101) 0.3898(10) 0.167 Uiso 1 calc R . H42C H 1.0994(103) 0.8407(20) 0.4486(58) 0.167 Uiso 1 calc R . C51 C 0.5811(15) 0.9765(15) 0.2252(8) 0.071(4) Uani 1 d . . C52 C 0.4743(17) 1.0701(15) 0.2457(11) 0.105(6) Uani 1 d . . H52A H 0.3993(19) 1.0345(42) 0.2455(76) 0.158 Uiso 1 calc R . H52B H 0.4729(79) 1.1382(61) 0.2119(45) 0.158 Uiso 1 calc R . H52C H 0.4825(70) 1.0973(96) 0.2926(33) 0.158 Uiso 1 calc R . C61 C 0.5823(15) 0.8020(15) 0.3842(8) 0.070(4) Uani 1 d . . C62 C 0.4725(18) 0.8447(20) 0.4273(10) 0.117(7) Uani 1 d . . H62A H 0.4018(18) 0.8336(138) 0.4027(39) 0.176 Uiso 1 calc R . H62B H 0.4717(74) 0.9296(41) 0.4359(73) 0.176 Uiso 1 calc R . H62C H 0.4707(75) 0.7992(103) 0.4722(36) 0.176 Uiso 1 calc R . C71 C 0.5915(13) 0.6553(13) 0.1150(7) 0.063(4) Uani 1 d . . C72 C 0.4885(15) 0.6146(19) 0.0870(10) 0.099(6) Uani 1 d . . H72A H 0.4950(63) 0.5272(20) 0.0918(66) 0.148 Uiso 1 calc R . H72B H 0.4861(73) 0.6394(110) 0.0374(22) 0.148 Uiso 1 calc R . H72C H 0.4147(17) 0.6494(99) 0.1129(50) 0.148 Uiso 1 calc R . C81 C 0.5974(13) 0.4957(12) 0.2816(8) 0.064(4) Uani 1 d . . C82 C 0.4926(15) 0.4374(16) 0.2925(11) 0.095(6) Uani 1 d . . H82A H 0.4750(68) 0.4054(101) 0.2483(18) 0.142 Uiso 1 calc R . H82B H 0.4246(30) 0.4946(33) 0.3092(67) 0.142 Uiso 1 calc R . H82C H 0.5058(45) 0.3719(76) 0.3275(51) 0.142 Uiso 1 calc R . B1 B 0.6217(11) 0.7110(12) -0.1021(7) 0.082(6) Uiso 0.54(2) d PD 1 F11 F 0.5147(16) 0.7706(19) -0.0711(11) 0.164(12) Uiso 0.54(2) d PD 1 F12 F 0.5969(19) 0.6551(17) -0.1624(9) 0.129(9) Uiso 0.54(2) d PD 1 F13 F 0.6721(15) 0.6247(15) -0.0541(8) 0.095(7) Uiso 0.54(2) d PD 1 F14 F 0.7024(16) 0.7942(16) -0.1208(11) 0.127(8) Uiso 0.54(2) d PD 1 B1' B 0.6506(15) 0.6851(16) -0.1070(9) 0.082(6) Uiso 0.46(2) d PD 2 F11' F 0.6483(29) 0.7410(29) -0.0428(12) 0.204(18) Uiso 0.46(2) d PD 2 F12' F 0.5323(16) 0.6831(21) -0.1251(13) 0.114(9) Uiso 0.46(2) d PD 2 F13' F 0.7084(23) 0.5678(20) -0.1004(17) 0.179(15) Uiso 0.46(2) d PD 2 F14' F 0.7142(21) 0.7484(24) -0.1592(14) 0.145(12) Uiso 0.46(2) d PD 2 B2 B 0.6891(18) 1.1418(18) 0.3933(10) 0.075(5) Uiso 0.41(3) d PD 1 F21 F 0.7126(29) 1.2137(32) 0.3356(12) 0.158(15) Uiso 0.41(3) d PD 1 F22 F 0.7534(34) 1.0313(23) 0.3853(24) 0.252(27) Uiso 0.41(3) d PD 1 F23 F 0.5689(21) 1.1312(33) 0.4007(14) 0.126(11) Uiso 0.41(3) d PD 1 F24 F 0.7213(22) 1.1911(28) 0.4518(10) 0.099(9) Uiso 0.41(3) d PD 1 B2' B 0.7053(10) 1.1249(11) 0.3932(6) 0.075(5) Uiso 0.59(3) d PD 2 F21' F 0.6672(19) 1.2424(14) 0.3775(13) 0.184(13) Uiso 0.59(3) d PD 2 F22' F 0.7813(14) 1.0776(19) 0.3394(8) 0.134(9) Uiso 0.59(3) d PD 2 F23' F 0.6083(14) 1.0624(18) 0.4032(8) 0.100(6) Uiso 0.59(3) d PD 2 F24' F 0.7642(14) 1.1164(17) 0.4534(7) 0.086(6) Uiso 0.59(3) d PD 2 B3 B 0.3006(20) 0.7696(20) 0.2580(12) 0.086(6) Uiso 1 d . . F31 F 0.1861(7) 0.7363(7) 0.3052(4) 0.070(2) Uani 1 d . . F32 F 0.1993(7) 0.8349(7) 0.2049(4) 0.073(2) Uani 1 d . . F33 F 0.4233(29) 0.7605(34) 0.2427(21) 0.082(11) Uiso 0.31(3) d P . F34 F 0.2602(14) 0.8725(15) 0.2932(9) 0.082 Uiso 0.54(2) d P . F35 F 0.2370(22) 0.6964(23) 0.2289(13) 0.082 Uiso 0.36(2) d P . F36 F 0.2997(34) 0.6962(34) 0.3249(19) 0.082 Uiso 0.24(2) d P . F37 F 0.3284(30) 0.8310(30) 0.1890(17) 0.082 Uiso 0.27(2) d P . F38 F 0.4137(31) 0.7210(36) 0.2714(23) 0.082 Uiso 0.28(3) d P . N9A N 0.7649(32) 0.9132(33) 0.0687(17) 0.099(11) Uiso 0.53(3) d PD 1 N9B N 0.8076(43) 0.9194(38) 0.0686(19) 0.099 Uiso 0.47(3) d PD 2 C91A C 0.7186(37) 0.9682(31) 0.0216(17) 0.089(11) Uiso 0.53(3) d PD 1 C91B C 0.7987(43) 0.9662(35) 0.0122(19) 0.089 Uiso 0.47(3) d PD 2 C92A C 0.6767(43) 1.0455(37) -0.0429(20) 0.115(14) Uiso 0.53(3) d PD 1 C92B C 0.7754(49) 1.0357(42) -0.0582(22) 0.115 Uiso 0.47(3) d PD 2 N10 N 0.8058(37) 0.5572(37) 0.4257(23) 0.164(18) Uiso 0.59(4) d PD . C101 C 0.7962(42) 0.4958(43) 0.4778(24) 0.155(20) Uiso 0.59(4) d PD . C102 C 0.8075(65) 0.4031(57) 0.5395(31) 0.235(32) Uiso 0.59(4) d PD . 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 Mo1 0.0421(6) 0.0484(7) 0.0478(6) -0.0002(5) -0.0048(5) -0.0109(5) Mo2 0.0425(6) 0.0480(7) 0.0472(6) -0.0005(5) -0.0055(5) -0.0098(5) O1 0.088(8) 0.119(9) 0.052(6) 0.010(6) -0.006(5) -0.004(7) O2 0.074(7) 0.099(8) 0.090(8) 0.039(6) -0.034(6) -0.014(6) N1 0.050(6) 0.050(6) 0.048(6) -0.009(5) -0.002(5) -0.009(5) N2 0.050(6) 0.043(6) 0.048(6) 0.003(5) -0.003(5) -0.010(5) N3 0.058(7) 0.058(7) 0.060(7) 0.008(5) -0.003(5) -0.017(6) N4 0.060(7) 0.073(8) 0.061(7) 0.005(6) -0.012(6) -0.012(6) N5 0.048(6) 0.052(7) 0.061(7) 0.006(5) -0.007(5) 0.001(5) N6 0.050(7) 0.073(8) 0.057(7) -0.007(6) 0.000(6) -0.005(6) N7 0.048(6) 0.060(7) 0.051(6) -0.005(5) -0.003(5) -0.012(5) N8 0.048(6) 0.056(7) 0.071(7) -0.005(6) -0.009(5) -0.008(6) C1 0.037(6) 0.048(7) 0.049(7) 0.006(6) -0.008(5) -0.014(5) C11 0.052(8) 0.049(8) 0.044(7) 0.004(6) -0.001(6) 0.003(6) C12 0.057(9) 0.109(13) 0.056(9) 0.013(8) -0.013(7) -0.013(8) C13 0.055(9) 0.121(15) 0.066(10) -0.013(9) 0.015(8) -0.005(9) C14 0.047(8) 0.110(12) 0.043(8) -0.006(7) -0.001(6) -0.023(7) C15 0.071(9) 0.081(11) 0.047(8) 0.005(7) -0.012(7) -0.004(8) C16 0.053(8) 0.067(9) 0.066(9) 0.001(7) -0.011(7) -0.006(7) C17 0.087(13) 0.203(23) 0.059(10) 0.024(12) 0.002(9) -0.042(14) C21 0.047(7) 0.051(8) 0.048(7) -0.004(6) 0.003(6) 0.006(6) C22 0.051(9) 0.100(13) 0.118(14) 0.040(11) -0.004(9) -0.018(8) C23 0.057(9) 0.087(12) 0.103(12) 0.035(10) -0.019(9) 0.001(8) C24 0.064(9) 0.056(8) 0.053(8) 0.018(7) -0.019(7) -0.004(7) C25 0.086(12) 0.102(14) 0.107(13) 0.055(11) -0.011(10) -0.023(10) C26 0.061(9) 0.087(11) 0.093(11) 0.037(10) -0.013(8) -0.021(8) C27 0.085(13) 0.120(17) 0.164(21) 0.054(15) -0.020(13) 0.002(12) C31 0.063(9) 0.046(9) 0.098(11) 0.010(8) 0.000(8) -0.012(7) C32 0.143(18) 0.071(12) 0.193(23) 0.040(14) -0.083(17) -0.051(12) C41 0.062(9) 0.083(11) 0.054(8) -0.018(8) -0.012(7) -0.015(8) C42 0.113(15) 0.152(19) 0.084(12) -0.041(12) -0.014(11) -0.055(14) C51 0.071(10) 0.063(10) 0.081(11) 0.026(8) -0.010(8) -0.022(9) C52 0.106(14) 0.064(11) 0.137(17) 0.005(11) -0.003(12) 0.015(10) C61 0.073(10) 0.089(12) 0.051(8) -0.006(8) -0.005(8) -0.020(9) C62 0.105(14) 0.135(18) 0.101(14) -0.034(13) 0.052(12) 0.001(12) C71 0.064(9) 0.075(10) 0.052(8) -0.001(7) -0.018(7) -0.010(8) C72 0.077(11) 0.136(17) 0.097(13) -0.020(12) -0.022(9) -0.049(11) C81 0.055(9) 0.047(8) 0.092(11) -0.002(7) -0.011(7) -0.006(7) C82 0.072(11) 0.082(12) 0.135(16) 0.006(11) -0.003(10) -0.034(9) F31 0.068(5) 0.068(5) 0.078(5) 0.015(4) -0.010(4) -0.028(4) F32 0.076(5) 0.084(6) 0.065(5) 0.009(4) -0.013(4) -0.030(4) _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 Mo1 N1 2.091(10) . y Mo1 N7 2.128(11) . y Mo1 N3 2.143(11) . y Mo1 Mo2 2.152(2) . y Mo1 N5 2.169(12) . y Mo2 N2 2.086(10) . y Mo2 N8 2.135(11) . y Mo2 N6 2.142(12) . y Mo2 N4 2.152(12) . y O1 C14 1.35(2) . ? O1 C17 1.41(2) . ? O2 C24 1.352(15) . ? O2 C27 1.41(2) . ? N1 C1 1.332(15) . ? N1 C11 1.435(15) . ? N2 C1 1.309(14) . ? N2 C21 1.420(15) . ? N3 C31 1.16(2) . ? N4 C41 1.13(2) . ? N5 C51 1.09(2) . ? N6 C61 1.12(2) . ? N7 C71 1.14(2) . ? N8 C81 1.14(2) . ? C11 C16 1.35(2) . ? C11 C12 1.39(2) . ? C12 C13 1.41(2) . ? C13 C14 1.35(2) . ? C14 C15 1.40(2) . ? C15 C16 1.38(2) . ? C21 C26 1.37(2) . ? C21 C22 1.39(2) . ? C22 C23 1.39(2) . ? C23 C24 1.28(2) . ? C24 C25 1.40(2) . ? C25 C26 1.37(2) . ? C31 C32 1.41(2) . ? C41 C42 1.44(2) . ? C51 C52 1.50(2) . ? C61 C62 1.44(2) . ? C71 C72 1.42(2) . ? C81 C82 1.39(2) . ? B1 F13 1.376(9) . ? B1 F11 1.376(9) . ? B1 F14 1.376(9) . ? B1 F12 1.376(9) . ? B1' F13' 1.375(9) . ? B1' F14' 1.376(9) . ? B1' F12' 1.376(9) . ? B1' F11' 1.376(9) . ? B2 F21 1.340(8) . ? B2 F24 1.341(8) . ? B2 F23 1.341(8) . ? B2 F22 1.341(8) . ? B2' F21' 1.341(8) . ? B2' F24' 1.341(8) . ? B2' F22' 1.341(8) . ? B2' F23' 1.341(8) . ? B3 F35 1.30(3) . ? B3 F38 1.33(4) . ? B3 F33 1.35(4) . ? B3 F34 1.35(2) . ? B3 F37 1.46(4) . ? B3 F36 1.46(4) . ? B3 F31 1.56(2) . ? B3 F32 1.63(2) . ? N9A C91A 1.16(2) . ? N9B C91B 1.16(2) . ? C91A C92A 1.52(3) . ? C91B C92B 1.52(3) . ? N10 C101 1.17(3) . ? C101 C102 1.51(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 N1 Mo1 N7 94.5(4) . . ? N1 Mo1 N3 90.5(4) . . ? N7 Mo1 N3 159.6(4) . . ? N1 Mo1 Mo2 91.6(3) . . ? N7 Mo1 Mo2 99.6(3) . . ? N3 Mo1 Mo2 100.0(3) . . ? N1 Mo1 N5 169.0(4) . . ? N7 Mo1 N5 84.4(4) . . ? N3 Mo1 N5 87.0(4) . . ? Mo2 Mo1 N5 99.3(3) . . ? N2 Mo2 N8 94.7(4) . . ? N2 Mo2 N6 165.8(4) . . ? N8 Mo2 N6 82.2(4) . . ? N2 Mo2 N4 91.6(4) . . ? N8 Mo2 N4 156.6(4) . . ? N6 Mo2 N4 86.2(4) . . ? N2 Mo2 Mo1 91.6(3) . . ? N8 Mo2 Mo1 101.3(3) . . ? N6 Mo2 Mo1 102.6(3) . . ? N4 Mo2 Mo1 101.1(3) . . ? C14 O1 C17 116.8(11) . . ? C24 O2 C27 117.8(12) . . ? C1 N1 C11 118.7(10) . . ? C1 N1 Mo1 118.7(8) . . ? C11 N1 Mo1 122.6(8) . . ? C1 N2 C21 118.5(10) . . ? C1 N2 Mo2 119.6(8) . . ? C21 N2 Mo2 121.9(8) . . ? C31 N3 Mo1 175.5(11) . . ? C41 N4 Mo2 170.9(12) . . ? C51 N5 Mo1 174.1(12) . . ? C61 N6 Mo2 170.8(13) . . ? C71 N7 Mo1 172.0(11) . . ? C81 N8 Mo2 166.9(12) . . ? N2 C1 N1 118.5(11) . . ? C16 C11 C12 118.0(12) . . ? C16 C11 N1 122.0(11) . . ? C12 C11 N1 120.0(11) . . ? C11 C12 C13 119.6(13) . . ? C14 C13 C12 120.9(14) . . ? O1 C14 C13 126.3(12) . . ? O1 C14 C15 113.2(12) . . ? C13 C14 C15 119.7(12) . . ? C16 C15 C14 118.2(12) . . ? C11 C16 C15 123.4(13) . . ? C26 C21 C22 115.0(13) . . ? C26 C21 N2 122.7(11) . . ? C22 C21 N2 122.1(12) . . ? C23 C22 C21 122.0(14) . . ? C24 C23 C22 121.7(14) . . ? C23 C24 O2 127.8(13) . . ? C23 C24 C25 118.9(13) . . ? O2 C24 C25 113.3(12) . . ? C26 C25 C24 120.2(14) . . ? C21 C26 C25 122.1(14) . . ? N3 C31 C32 175.9(16) . . ? N4 C41 C42 177.0(18) . . ? N5 C51 C52 175.8(18) . . ? N6 C61 C62 177.7(18) . . ? N7 C71 C72 178.1(16) . . ? N8 C81 C82 175.4(17) . . ? F13 B1 F11 109.4(5) . . ? F13 B1 F14 109.8(5) . . ? F11 B1 F14 109.1(5) . . ? F13 B1 F12 109.6(5) . . ? F11 B1 F12 109.5(5) . . ? F14 B1 F12 109.3(5) . . ? F13' B1' F14' 109.1(5) . . ? F13' B1' F12' 109.7(5) . . ? F14' B1' F12' 109.8(5) . . ? F13' B1' F11' 109.3(5) . . ? F14' B1' F11' 109.5(5) . . ? F12' B1' F11' 109.4(5) . . ? F21 B2 F24 109.6(5) . . ? F21 B2 F23 109.4(5) . . ? F24 B2 F23 109.2(5) . . ? F21 B2 F22 109.6(5) . . ? F24 B2 F22 109.4(5) . . ? F23 B2 F22 109.6(5) . . ? F21' B2' F24' 109.4(5) . . ? F21' B2' F22' 109.8(5) . . ? F24' B2' F22' 109.5(5) . . ? F21' B2' F23' 109.7(5) . . ? F24' B2' F23' 108.9(5) . . ? F22' B2' F23' 109.5(5) . . ? F35 B3 F38 114.5(25) . . ? F35 B3 F33 119.6(24) . . ? F38 B3 F33 29.7(18) . . ? F35 B3 F34 128.6(22) . . ? F38 B3 F34 114.2(23) . . ? F33 B3 F34 110.7(22) . . ? F35 B3 F37 91.8(21) . . ? F38 B3 F37 99.0(27) . . ? F33 B3 F37 69.8(24) . . ? F34 B3 F37 95.9(20) . . ? F35 B3 F36 91.3(22) . . ? F38 B3 F36 69.1(26) . . ? F33 B3 F36 98.5(27) . . ? F34 B3 F36 91.4(20) . . ? F37 B3 F36 167.9(26) . . ? F35 B3 F31 65.4(15) . . ? F38 B3 F31 121.6(25) . . ? F33 B3 F31 151.3(25) . . ? F34 B3 F31 76.1(13) . . ? F37 B3 F31 138.6(20) . . ? F36 B3 F31 52.9(16) . . ? F35 B3 F32 64.5(15) . . ? F38 B3 F32 152.5(26) . . ? F33 B3 F32 124.3(24) . . ? F34 B3 F32 79.5(13) . . ? F37 B3 F32 54.6(15) . . ? F36 B3 F32 136.8(21) . . ? F31 B3 F32 84.0(11) . . ? N9A C91A C92A 171.5(39) . . ? N9B C91B C92B 174.0(47) . . ? N10 C101 C102 168.7(53) . . ? _refine_diff_density_max 0.978 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.164 #===END data_cmpd_2b _audit_creation_method SHELXL _chemical_formula_moiety 'Mo2(AniF)2(CH3CN)6(BF4)2' _chemical_formula_sum 'C42 H48 B2 F8 Mo2 N10 O4' _chemical_formula_weight 1122.40 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.323(3) _cell_length_b 13.155(2) _cell_length_c 16.817(4) _cell_angle_alpha 94.04(1) _cell_angle_beta 94.78(1) _cell_angle_gamma 111.90(1) _cell_volume 2505.4(9) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 9.0 _cell_measurement_theta_max 20.8 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method ? _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.580 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 213(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 'Nonius FAST area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_standards_number 'None (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13640 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 23.27 _reflns_number_total 6490 _reflns_number_observed 5807 _reflns_observed_criterion >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 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^)+(0.0604P)^2^+10.0561P] 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 6486 _refine_ls_number_parameters 609 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_obs 0.0513 _refine_ls_wR_factor_all 0.1344 _refine_ls_wR_factor_obs 0.1270 _refine_ls_goodness_of_fit_all 1.071 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.142 _refine_ls_restrained_S_obs 1.155 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.74291(3) 0.05989(2) 0.23091(2) 0.02298(8) Uani 1 d . . Mo2 Mo 0.70650(3) -0.07833(2) 0.29916(2) 0.02306(8) Uani 1 d . . N1 N 0.9239(3) 0.1176(2) 0.2745(2) 0.0264(8) Uani 1 d . . N2 N 0.8837(3) -0.0362(2) 0.3404(2) 0.0257(8) Uani 1 d . . N3 N 0.6997(2) 0.1523(2) 0.3223(2) 0.0250(8) Uani 1 d . . N4 N 0.6740(3) 0.0079(2) 0.3973(2) 0.0255(8) Uani 1 d . . N5 N 0.5710(3) 0.0111(3) 0.1598(2) 0.0313(8) Uani 1 d . . N6 N 0.5174(3) -0.1647(3) 0.2702(2) 0.0322(9) Uani 1 d . . N7 N 0.7882(3) -0.0113(2) 0.1234(2) 0.0300(8) Uani 1 d . . N8 N 0.7156(3) -0.2107(2) 0.2178(2) 0.0304(8) Uani 1 d . . N9 N 0.7932(3) 0.2176(3) 0.1394(2) 0.0429(10) Uani 1 d . . N10 N 0.3542(4) -0.4012(4) 0.3990(4) 0.088(2) Uani 1 d . . O1 O 1.2412(3) 0.4951(3) 0.1683(2) 0.0776(12) Uani 1 d . . O2 O 1.0222(2) -0.3540(2) 0.4714(2) 0.0412(8) Uani 1 d . . O3 O 0.6239(3) 0.5437(2) 0.3066(2) 0.0444(8) Uani 1 d . . O4 O 0.6241(3) -0.1723(3) 0.6888(2) 0.0569(10) Uani 1 d . . C1 C 0.9613(3) 0.0520(3) 0.3160(2) 0.0267(10) Uani 1 d . . H1A H 1.0424(3) 0.0685(3) 0.3278(2) 0.032 Uiso 1 calc R . C2 C 0.6733(3) 0.1075(3) 0.3900(2) 0.0271(10) Uani 1 d . . H2A H 0.6543(3) 0.1459(3) 0.4324(2) 0.032 Uiso 1 calc R . C11 C 1.0100(3) 0.2116(3) 0.2487(2) 0.0259(9) Uani 1 d . . C12 C 1.0861(4) 0.2032(3) 0.1967(3) 0.0396(11) Uani 1 d . . H12A H 1.0840(4) 0.1331(3) 0.1788(3) 0.048 Uiso 1 calc R . C13 C 1.1666(4) 0.2957(4) 0.1694(3) 0.0492(13) Uani 1 d . . H13A H 1.2201(4) 0.2882(4) 0.1350(3) 0.059 Uiso 1 calc R . C14 C 1.1676(4) 0.3978(3) 0.1928(3) 0.0448(13) Uani 1 d . . C15 C 1.0906(4) 0.4083(3) 0.2447(3) 0.0461(13) Uani 1 d . . H15A H 1.0910(4) 0.4783(3) 0.2607(3) 0.055 Uiso 1 calc R . C16 C 1.0132(3) 0.3167(3) 0.2733(3) 0.0372(11) Uani 1 d . . H16A H 0.9622(3) 0.3247(3) 0.3095(3) 0.045 Uiso 1 calc R . C17 C 1.3262(6) 0.4883(6) 0.1170(5) 0.122(3) Uani 1 d . . H17A H 1.3726(6) 0.5614(6) 0.1039(5) 0.183 Uiso 1 calc R . H17B H 1.2858(6) 0.4411(6) 0.0680(5) 0.183 Uiso 1 calc R . H17C H 1.3777(6) 0.4579(6) 0.1444(5) 0.183 Uiso 1 calc R . C21 C 0.9251(3) -0.1139(3) 0.3746(2) 0.0253(9) Uani 1 d . . C22 C 0.9151(3) -0.1340(3) 0.4546(2) 0.0291(10) Uani 1 d . . H22A H 0.8848(3) -0.0932(3) 0.4880(2) 0.035 Uiso 1 calc R . C23 C 0.9493(3) -0.2131(3) 0.4846(2) 0.0313(10) Uani 1 d . . H23A H 0.9437(3) -0.2247(3) 0.5389(2) 0.038 Uiso 1 calc R . C24 C 0.9921(3) -0.2765(3) 0.4366(2) 0.0292(10) Uani 1 d . . C25 C 1.0024(3) -0.2573(3) 0.3563(2) 0.0316(10) Uani 1 d . . H25A H 1.0314(3) -0.2990(3) 0.3228(2) 0.038 Uiso 1 calc R . C26 C 0.9693(3) -0.1758(3) 0.3264(2) 0.0314(10) Uani 1 d . . H26A H 0.9769(3) -0.1624(3) 0.2726(2) 0.038 Uiso 1 calc R . C27 C 1.0616(4) -0.4218(4) 0.4208(3) 0.0497(13) Uani 1 d . . H27A H 1.0804(4) -0.4736(4) 0.4519(3) 0.075 Uiso 1 calc R . H27B H 1.1313(4) -0.3759(4) 0.3985(3) 0.075 Uiso 1 calc R . H27C H 0.9999(4) -0.4619(4) 0.3775(3) 0.075 Uiso 1 calc R . C31 C 0.6900(3) 0.2572(3) 0.3179(2) 0.0254(9) Uani 1 d . . C32 C 0.6291(3) 0.2753(3) 0.2512(2) 0.0308(10) Uani 1 d . . H32A H 0.6000(3) 0.2210(3) 0.2069(2) 0.037 Uiso 1 calc R . C33 C 0.6106(4) 0.3718(3) 0.2488(3) 0.0367(11) Uani 1 d . . H33A H 0.5687(4) 0.3828(3) 0.2030(3) 0.044 Uiso 1 calc R . C34 C 0.6535(3) 0.4535(3) 0.3135(2) 0.0327(10) Uani 1 d . . C35 C 0.7190(3) 0.4385(3) 0.3793(2) 0.0324(10) Uani 1 d . . H35A H 0.7505(3) 0.4938(3) 0.4229(2) 0.039 Uiso 1 calc R . C36 C 0.7373(3) 0.3410(3) 0.3801(2) 0.0334(10) Uani 1 d . . H36A H 0.7833(3) 0.3316(3) 0.4243(2) 0.040 Uiso 1 calc R . C37 C 0.6569(4) 0.6235(3) 0.3735(3) 0.0450(12) Uani 1 d . . H37A H 0.6314(4) 0.6827(3) 0.3614(3) 0.068 Uiso 1 calc R . H37B H 0.7419(4) 0.6530(3) 0.3863(3) 0.068 Uiso 1 calc R . H37C H 0.6203(4) 0.5900(3) 0.4191(3) 0.068 Uiso 1 calc R . C41 C 0.6591(3) -0.0343(3) 0.4734(2) 0.0262(9) Uani 1 d . . C42 C 0.7262(3) 0.0280(3) 0.5426(2) 0.0325(10) Uani 1 d . . H42A H 0.7794(3) 0.1003(3) 0.5397(2) 0.039 Uiso 1 calc R . C43 C 0.7164(4) -0.0144(3) 0.6171(2) 0.0371(11) Uani 1 d . . H43A H 0.7617(4) 0.0288(3) 0.6640(2) 0.045 Uiso 1 calc R . C44 C 0.6388(3) -0.1209(3) 0.6198(2) 0.0355(10) Uani 1 d . . C45 C 0.5705(4) -0.1843(3) 0.5509(3) 0.0377(11) Uani 1 d . . H45A H 0.5174(4) -0.2568(3) 0.5536(3) 0.045 Uiso 1 calc R . C46 C 0.5807(3) -0.1406(3) 0.4781(2) 0.0327(10) Uani 1 d . . H46A H 0.5340(3) -0.1834(3) 0.4316(2) 0.039 Uiso 1 calc R . C47 C 0.6698(5) -0.1051(5) 0.7622(3) 0.060(2) Uani 1 d . . H47A H 0.6540(5) -0.1505(5) 0.8062(3) 0.090 Uiso 1 calc R . H47B H 0.6327(5) -0.0520(5) 0.7677(3) 0.090 Uiso 1 calc R . H47C H 0.7541(5) -0.0664(5) 0.7633(3) 0.090 Uiso 1 calc R . C51 C 0.4872(3) -0.0222(3) 0.1158(2) 0.0332(10) Uani 1 d . . C52 C 0.3824(4) -0.0646(5) 0.0595(3) 0.0566(15) Uani 1 d . . H52A H 0.3781(17) -0.0064(9) 0.0285(15) 0.085 Uiso 1 calc R . H52B H 0.3139(4) -0.0912(28) 0.0882(3) 0.085 Uiso 1 calc R . H52C H 0.3845(16) -0.1247(20) 0.0236(14) 0.085 Uiso 1 calc R . C61 C 0.4181(4) -0.2075(3) 0.2589(3) 0.0442(12) Uani 1 d . . C62 C 0.2903(4) -0.2606(5) 0.2466(5) 0.088(2) Uani 1 d . . H62A H 0.2641(5) -0.3135(31) 0.2852(20) 0.131 Uiso 1 calc R . H62B H 0.2654(5) -0.2983(35) 0.1926(11) 0.131 Uiso 1 calc R . H62C H 0.2563(4) -0.2054(7) 0.2538(30) 0.131 Uiso 1 calc R . C71 C 0.8101(3) -0.0427(3) 0.0653(3) 0.0368(11) Uani 1 d . . C72 C 0.8360(4) -0.0842(5) -0.0105(3) 0.0608(15) Uani 1 d . . H72A H 0.8890(27) -0.1221(27) 0.0001(3) 0.091 Uiso 1 calc R . H72B H 0.8729(30) -0.0231(6) -0.0410(10) 0.091 Uiso 1 calc R . H72C H 0.7634(6) -0.1351(24) -0.0411(10) 0.091 Uiso 1 calc R . C81 C 0.7122(4) -0.2846(3) 0.1777(2) 0.0351(11) Uani 1 d . . C82 C 0.7088(5) -0.3796(4) 0.1269(3) 0.0576(14) Uani 1 d . . H82A H 0.7853(10) -0.3643(12) 0.1085(18) 0.086 Uiso 1 calc R . H82B H 0.6497(23) -0.3952(19) 0.0810(12) 0.086 Uiso 1 calc R . H82C H 0.6893(32) -0.4428(8) 0.1572(7) 0.086 Uiso 1 calc R . C91 C 0.8274(4) 0.2906(4) 0.1044(3) 0.0478(13) Uani 1 d . . C92 C 0.8728(7) 0.3877(5) 0.0604(4) 0.095(2) Uani 1 d . . H92A H 0.9359(32) 0.3831(22) 0.0313(26) 0.142 Uiso 1 calc R . H92B H 0.9028(43) 0.4540(5) 0.0980(5) 0.142 Uiso 1 calc R . H92C H 0.8099(13) 0.3900(25) 0.0228(23) 0.142 Uiso 1 calc R . C101 C 0.3483(5) -0.4888(5) 0.3874(4) 0.064(2) Uani 1 d . . C102 C 0.3407(6) -0.6020(5) 0.3728(4) 0.089(2) Uani 1 d . . H10A H 0.3701(43) -0.6235(15) 0.4214(10) 0.134 Uiso 1 calc R . H10B H 0.3877(37) -0.6071(10) 0.3303(22) 0.134 Uiso 1 calc R . H10C H 0.2593(8) -0.6507(7) 0.3568(31) 0.134 Uiso 1 calc R . B1 B 0.5067(3) -0.2789(2) -0.0207(2) 0.0387(13) Uani 1 d D . B2 B 0.9519(3) 0.2022(3) -0.1128(2) 0.084(2) Uani 1 d D . F1 F 0.3923(5) -0.3468(5) -0.0451(4) 0.1003(10) Uani 0.580(4) d PD 1 F2 F 0.5776(5) -0.3232(5) -0.0554(4) 0.1003(10) Uani 0.580(4) d PD 1 F3 F 0.5257(6) -0.1827(4) -0.0547(4) 0.1003(10) Uani 0.580(4) d PD 1 F4 F 0.5392(6) -0.2498(5) 0.0585(3) 0.1003(10) Uani 0.580(4) d PD 1 F1' F 0.4832(7) -0.2521(7) 0.0548(3) 0.1003(10) Uani 0.420(4) d PD 2 F2' F 0.4355(8) -0.3845(5) -0.0471(5) 0.1003(10) Uani 0.420(4) d PD 2 F3' F 0.5055(9) -0.2040(5) -0.0711(4) 0.1003(10) Uani 0.420(4) d PD 2 F4' F 0.6164(5) -0.2822(7) -0.0022(5) 0.1003(10) Uani 0.420(4) d PD 2 F5 F 0.9732(5) 0.3036(4) -0.1384(4) 0.1148(10) Uani 0.717(3) d PD 1 F6 F 0.9203(5) 0.1818(5) -0.0378(3) 0.1148(10) Uani 0.717(3) d PD 1 F7 F 0.8546(4) 0.1310(5) -0.1652(3) 0.1148(10) Uani 0.717(3) d PD 1 F8 F 1.0427(4) 0.1702(5) -0.1241(4) 0.1148(10) Uani 0.717(3) d PD 1 F5' F 0.8501(6) 0.1987(11) -0.0853(7) 0.1148(10) Uani 0.283(3) d PD 2 F6' F 0.9840(11) 0.2788(7) -0.1692(5) 0.1148(10) Uani 0.283(3) d PD 2 F7' F 1.0373(8) 0.2569(10) -0.0475(5) 0.1148(10) Uani 0.283(3) d PD 2 F8' F 0.9703(9) 0.1091(6) -0.1390(8) 0.1148(10) Uani 0.283(3) d PD 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 Mo1 0.02765(15) 0.02057(14) 0.0227(2) 0.00221(12) 0.00128(13) 0.01184(12) Mo2 0.02692(15) 0.01843(14) 0.0249(2) 0.00201(13) 0.00131(13) 0.01027(12) N1 0.0281(14) 0.0221(14) 0.029(2) 0.0010(13) 0.0015(13) 0.0096(12) N2 0.0296(14) 0.0230(14) 0.026(2) 0.0025(13) 0.0029(13) 0.0117(12) N3 0.0301(14) 0.0222(14) 0.027(2) 0.0039(12) 0.0037(13) 0.0141(12) N4 0.0317(14) 0.0230(14) 0.0238(15) 0.0046(12) 0.0046(13) 0.0121(12) N5 0.0314(15) 0.031(2) 0.033(2) 0.0020(14) 0.0024(14) 0.0142(13) N6 0.029(2) 0.027(2) 0.036(2) -0.0013(14) 0.0010(14) 0.0060(13) N7 0.0363(15) 0.0318(15) 0.028(2) 0.0041(13) 0.0024(14) 0.0198(13) N8 0.038(2) 0.0240(15) 0.029(2) -0.0015(14) -0.0017(14) 0.0143(13) N9 0.046(2) 0.036(2) 0.051(2) 0.007(2) 0.004(2) 0.0219(15) N10 0.071(3) 0.074(3) 0.113(4) -0.010(3) 0.002(3) 0.029(2) O1 0.092(2) 0.043(2) 0.094(2) 0.025(2) 0.057(2) 0.009(2) O2 0.058(2) 0.0386(14) 0.039(2) 0.0121(12) 0.0053(13) 0.0309(12) O3 0.067(2) 0.0285(13) 0.046(2) 0.0018(12) -0.0037(14) 0.0307(12) O4 0.080(2) 0.057(2) 0.036(2) 0.0252(14) 0.017(2) 0.024(2) C1 0.023(2) 0.029(2) 0.028(2) -0.001(2) -0.004(2) 0.0113(15) C2 0.026(2) 0.023(2) 0.032(2) -0.001(2) 0.005(2) 0.0099(14) C11 0.029(2) 0.021(2) 0.027(2) 0.0046(15) 0.000(2) 0.0094(14) C12 0.055(2) 0.029(2) 0.042(2) 0.003(2) 0.016(2) 0.021(2) C13 0.060(2) 0.048(2) 0.045(2) 0.011(2) 0.029(2) 0.021(2) C14 0.053(2) 0.031(2) 0.048(2) 0.011(2) 0.018(2) 0.010(2) C15 0.055(2) 0.023(2) 0.057(3) 0.002(2) 0.018(2) 0.008(2) C16 0.034(2) 0.031(2) 0.047(2) 0.001(2) 0.016(2) 0.011(2) C17 0.144(5) 0.079(4) 0.151(5) 0.050(4) 0.117(4) 0.023(4) C21 0.026(2) 0.021(2) 0.029(2) 0.005(2) -0.004(2) 0.0100(14) C22 0.034(2) 0.031(2) 0.023(2) -0.001(2) -0.001(2) 0.015(2) C23 0.040(2) 0.030(2) 0.025(2) 0.002(2) 0.000(2) 0.015(2) C24 0.031(2) 0.025(2) 0.036(2) 0.006(2) 0.001(2) 0.0145(15) C25 0.035(2) 0.034(2) 0.033(2) 0.002(2) 0.005(2) 0.021(2) C26 0.035(2) 0.035(2) 0.030(2) 0.005(2) 0.004(2) 0.019(2) C27 0.064(2) 0.045(2) 0.059(3) 0.014(2) 0.009(2) 0.041(2) C31 0.029(2) 0.022(2) 0.029(2) 0.0035(15) 0.008(2) 0.0122(14) C32 0.038(2) 0.025(2) 0.028(2) -0.002(2) -0.001(2) 0.013(2) C33 0.047(2) 0.034(2) 0.033(2) 0.003(2) -0.006(2) 0.022(2) C34 0.042(2) 0.023(2) 0.038(2) 0.003(2) 0.004(2) 0.017(2) C35 0.038(2) 0.025(2) 0.030(2) -0.004(2) -0.005(2) 0.011(2) C36 0.038(2) 0.028(2) 0.034(2) 0.002(2) -0.005(2) 0.016(2) C37 0.058(2) 0.023(2) 0.059(3) -0.003(2) 0.004(2) 0.022(2) C41 0.032(2) 0.027(2) 0.026(2) 0.0066(15) 0.009(2) 0.0165(14) C42 0.037(2) 0.026(2) 0.035(2) 0.005(2) 0.006(2) 0.011(2) C43 0.046(2) 0.039(2) 0.025(2) 0.002(2) 0.002(2) 0.016(2) C44 0.044(2) 0.046(2) 0.027(2) 0.016(2) 0.014(2) 0.024(2) C45 0.043(2) 0.027(2) 0.045(2) 0.012(2) 0.012(2) 0.013(2) C46 0.039(2) 0.027(2) 0.033(2) 0.006(2) 0.006(2) 0.014(2) C47 0.070(3) 0.085(3) 0.031(2) 0.014(2) 0.012(2) 0.035(3) C51 0.033(2) 0.037(2) 0.034(2) 0.007(2) 0.010(2) 0.017(2) C52 0.040(2) 0.080(3) 0.045(3) -0.002(3) -0.009(2) 0.022(2) C61 0.048(2) 0.029(2) 0.055(3) 0.008(2) -0.001(2) 0.016(2) C62 0.037(3) 0.050(3) 0.161(6) 0.032(4) -0.016(3) 0.001(2) C71 0.042(2) 0.042(2) 0.032(2) 0.002(2) 0.001(2) 0.025(2) C72 0.062(2) 0.097(3) 0.037(2) -0.006(2) 0.009(2) 0.048(2) C81 0.043(2) 0.031(2) 0.034(2) 0.009(2) 0.005(2) 0.017(2) C82 0.088(3) 0.033(2) 0.060(3) 0.002(2) 0.024(3) 0.031(2) C91 0.055(2) 0.038(2) 0.055(3) 0.013(2) 0.006(2) 0.023(2) C92 0.116(5) 0.066(3) 0.103(5) 0.047(3) 0.029(4) 0.024(3) C101 0.053(3) 0.068(3) 0.072(4) 0.001(3) 0.000(3) 0.025(2) C102 0.106(4) 0.080(4) 0.093(5) 0.007(3) -0.012(4) 0.054(3) B1 0.052(2) 0.024(2) 0.042(3) 0.001(2) -0.015(2) 0.022(2) B2 0.061(3) 0.175(6) 0.050(3) 0.043(4) 0.025(3) 0.072(3) F1 0.131(2) 0.088(2) 0.0743(14) 0.0007(13) -0.017(2) 0.0408(15) F2 0.131(2) 0.088(2) 0.0743(14) 0.0007(13) -0.017(2) 0.0408(15) F3 0.131(2) 0.088(2) 0.0743(14) 0.0007(13) -0.017(2) 0.0408(15) F4 0.131(2) 0.088(2) 0.0743(14) 0.0007(13) -0.017(2) 0.0408(15) F1' 0.131(2) 0.088(2) 0.0743(14) 0.0007(13) -0.017(2) 0.0408(15) F2' 0.131(2) 0.088(2) 0.0743(14) 0.0007(13) -0.017(2) 0.0408(15) F3' 0.131(2) 0.088(2) 0.0743(14) 0.0007(13) -0.017(2) 0.0408(15) F4' 0.131(2) 0.088(2) 0.0743(14) 0.0007(13) -0.017(2) 0.0408(15) F5 0.104(2) 0.149(2) 0.100(2) 0.021(2) 0.021(2) 0.055(2) F6 0.104(2) 0.149(2) 0.100(2) 0.021(2) 0.021(2) 0.055(2) F7 0.104(2) 0.149(2) 0.100(2) 0.021(2) 0.021(2) 0.055(2) F8 0.104(2) 0.149(2) 0.100(2) 0.021(2) 0.021(2) 0.055(2) F5' 0.104(2) 0.149(2) 0.100(2) 0.021(2) 0.021(2) 0.055(2) F6' 0.104(2) 0.149(2) 0.100(2) 0.021(2) 0.021(2) 0.055(2) F7' 0.104(2) 0.149(2) 0.100(2) 0.021(2) 0.021(2) 0.055(2) F8' 0.104(2) 0.149(2) 0.100(2) 0.021(2) 0.021(2) 0.055(2) _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 Mo1 Mo2 2.1439(6) . Y Mo1 N1 2.115(3) . Y Mo1 N3 2.117(3) . Y Mo1 N7 2.185(3) . Y Mo1 N5 2.188(3) . Y Mo1 N9 2.590(4) . Y Mo2 N2 2.085(3) . Y Mo2 N4 2.087(3) . Y Mo2 N6 2.172(3) . Y Mo2 N8 2.180(3) . Y N1 C1 1.332(5) . ? N1 C11 1.421(4) . ? N2 C1 1.316(5) . ? N2 C21 1.434(5) . ? N3 C2 1.327(5) . ? N3 C31 1.435(5) . ? N4 C2 1.328(5) . ? N4 C41 1.429(5) . ? N5 C51 1.138(5) . ? N6 C61 1.133(5) . ? N7 C71 1.127(5) . ? N8 C81 1.129(5) . ? N9 C91 1.125(6) . ? N10 C101 1.129(8) . ? O1 C14 1.378(5) . ? O1 C17 1.435(8) . ? O2 C24 1.359(5) . ? O2 C27 1.429(6) . ? O3 C34 1.376(5) . ? O3 C37 1.405(5) . ? O4 C44 1.376(5) . ? O4 C47 1.408(6) . ? C11 C12 1.362(6) . ? C11 C16 1.400(6) . ? C12 C13 1.389(6) . ? C13 C14 1.368(7) . ? C14 C15 1.378(7) . ? C15 C16 1.376(6) . ? C21 C26 1.388(6) . ? C21 C22 1.397(5) . ? C22 C23 1.372(6) . ? C23 C24 1.388(6) . ? C24 C25 1.400(6) . ? C25 C26 1.391(6) . ? C31 C36 1.381(5) . ? C31 C32 1.382(6) . ? C32 C33 1.374(6) . ? C33 C34 1.391(5) . ? C34 C35 1.383(6) . ? C35 C36 1.384(6) . ? C41 C42 1.382(5) . ? C41 C46 1.384(5) . ? C42 C43 1.404(6) . ? C43 C44 1.377(5) . ? C44 C45 1.388(5) . ? C45 C46 1.383(6) . ? C51 C52 1.435(6) . ? C61 C62 1.454(7) . ? C71 C72 1.457(6) . ? C81 C82 1.448(6) . ? C91 C92 1.470(8) . ? C101 C102 1.458(9) . ? B1 F4 1.343(5) . ? B1 F3' 1.348(6) . ? B1 F2' 1.354(5) . ? B1 F2 1.364(6) . ? B1 F1 1.366(5) . ? B1 F3 1.374(5) . ? B1 F1' 1.375(6) . ? B1 F4' 1.379(6) . ? B2 F8 1.357(5) . ? B2 F5' 1.360(7) . ? B2 F6 1.366(5) . ? B2 F5 1.367(5) . ? B2 F8' 1.377(7) . ? B2 F7' 1.400(7) . ? B2 F7 1.400(5) . ? B2 F6' 1.404(7) . ? 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 N1 Mo1 N3 95.10(11) . . Y N1 Mo1 Mo2 90.67(9) . . Y N3 Mo1 Mo2 91.99(8) . . Y N1 Mo1 N7 86.56(12) . . Y N3 Mo1 N7 169.55(12) . . Y Mo2 Mo1 N7 98.31(9) . . Y N1 Mo1 N5 166.86(12) . . Y N3 Mo1 N5 93.30(12) . . Y Mo2 Mo1 N5 99.13(9) . . Y N7 Mo1 N5 83.40(12) . . Y N1 Mo1 N9 88.42(11) . . Y N3 Mo1 N9 92.98(12) . . Y Mo2 Mo1 N9 175.01(9) . . Y N7 Mo1 N9 76.74(12) . . Y N5 Mo1 N9 81.05(11) . . Y N2 Mo2 N4 94.46(12) . . Y N2 Mo2 Mo1 93.12(8) . . Y N4 Mo2 Mo1 91.93(9) . . Y N2 Mo2 N6 163.94(12) . . Y N4 Mo2 N6 88.35(12) . . Y Mo1 Mo2 N6 102.60(9) . . Y N2 Mo2 N8 88.65(12) . . Y N4 Mo2 N8 162.29(12) . . Y Mo1 Mo2 N8 105.33(9) . . Y N6 Mo2 N8 84.09(12) . . Y C1 N1 C11 117.8(3) . . ? C1 N1 Mo1 118.0(2) . . ? C11 N1 Mo1 123.0(3) . . ? C1 N2 C21 118.3(3) . . ? C1 N2 Mo2 117.9(3) . . ? C21 N2 Mo2 121.6(2) . . ? C2 N3 C31 115.6(3) . . ? C2 N3 Mo1 117.4(2) . . ? C31 N3 Mo1 126.9(2) . . ? C2 N4 C41 119.0(3) . . ? C2 N4 Mo2 118.9(2) . . ? C41 N4 Mo2 122.0(2) . . ? C51 N5 Mo1 170.6(3) . . ? C61 N6 Mo2 176.4(4) . . ? C71 N7 Mo1 175.3(3) . . ? C81 N8 Mo2 174.5(3) . . ? C14 O1 C17 117.0(4) . . ? C24 O2 C27 116.8(3) . . ? C34 O3 C37 117.1(3) . . ? C44 O4 C47 117.2(4) . . ? N2 C1 N1 119.4(3) . . ? N3 C2 N4 119.4(3) . . ? C12 C11 C16 118.2(3) . . ? C12 C11 N1 122.3(3) . . ? C16 C11 N1 119.4(3) . . ? C11 C12 C13 121.6(4) . . ? C14 C13 C12 119.7(4) . . ? C13 C14 C15 119.7(4) . . ? C13 C14 O1 125.1(4) . . ? C15 C14 O1 115.2(4) . . ? C16 C15 C14 120.3(4) . . ? C15 C16 C11 120.4(4) . . ? C26 C21 C22 118.8(4) . . ? C26 C21 N2 119.8(3) . . ? C22 C21 N2 121.3(3) . . ? C23 C22 C21 120.1(4) . . ? C22 C23 C24 121.5(4) . . ? O2 C24 C23 117.2(4) . . ? O2 C24 C25 123.9(4) . . ? C23 C24 C25 118.9(4) . . ? C26 C25 C24 119.4(4) . . ? C21 C26 C25 121.2(4) . . ? C36 C31 C32 118.2(4) . . ? C36 C31 N3 121.7(3) . . ? C32 C31 N3 120.1(3) . . ? C33 C32 C31 120.8(3) . . ? C32 C33 C34 120.4(4) . . ? O3 C34 C35 125.1(3) . . ? O3 C34 C33 115.4(4) . . ? C35 C34 C33 119.4(4) . . ? C34 C35 C36 119.0(3) . . ? C31 C36 C35 121.9(4) . . ? C42 C41 C46 119.0(4) . . ? C42 C41 N4 120.8(3) . . ? C46 C41 N4 120.2(3) . . ? C41 C42 C43 121.3(3) . . ? C44 C43 C42 118.3(3) . . ? O4 C44 C43 123.5(3) . . ? O4 C44 C45 115.4(3) . . ? C43 C44 C45 121.0(4) . . ? C46 C45 C44 119.7(4) . . ? C45 C46 C41 120.6(3) . . ? N5 C51 C52 179.2(5) . . ? N6 C61 C62 178.3(5) . . ? N7 C71 C72 178.9(4) . . ? N8 C81 C82 179.3(4) . . ? N9 C91 C92 178.8(5) . . ? N10 C101 C102 179.8(5) . . ? F3' B1 F2' 115.3(5) . . ? F4 B1 F2 112.3(5) . . ? F4 B1 F1 117.7(5) . . ? F2 B1 F1 108.1(4) . . ? F4 B1 F3 106.2(4) . . ? F2 B1 F3 104.8(5) . . ? F1 B1 F3 106.8(4) . . ? F3' B1 F1' 112.2(6) . . ? F2' B1 F1' 109.4(6) . . ? F3' B1 F4' 113.8(6) . . ? F2' B1 F4' 104.8(6) . . ? F1' B1 F4' 100.2(5) . . ? F8 B2 F6 108.9(5) . . ? F8 B2 F5 110.6(4) . . ? F6 B2 F5 120.6(5) . . ? F5' B2 F8' 123.0(7) . . ? F5' B2 F7' 103.2(6) . . ? F8' B2 F7' 107.3(7) . . ? F8 B2 F7 106.9(4) . . ? F6 B2 F7 104.6(4) . . ? F5 B2 F7 104.1(4) . . ? F5' B2 F6' 110.0(8) . . ? F8' B2 F6' 109.7(7) . . ? F7' B2 F6' 101.3(6) . . ? _refine_diff_density_max 1.217 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.101 #===END ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC95230 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C66 H62 B2 F8 Mo2 N12' _chemical_formula_moiety 'C46 H42 Mo2 N8 2+, 2(B F4 -), 4(C5 H5 N)' _chemical_formula_weight 1388.79 _cell_length_a 27.753(6) _cell_length_b 12.462(2) _cell_length_c 18.715(4) _cell_angle_alpha 90 _cell_angle_beta 106.509(10) _cell_angle_gamma 90 _cell_volume 6206(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 140 _cell_measurement_theta_min 9.73 _cell_measurement_theta_max 14.88 _cell_measurement_temperature 98 _exptl_crystal_colour yellow _exptl_crystal_description prism _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.4799 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2+x,1/2+y,z -x,y,1/2-z 1/2-x,1/2+y,1/2-z x,-y,1/2+z 1/2+x,1/2-y,1/2+z -x,-y,-z 1/2-x,1/2-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 98 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5325 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 4 _diffrn_standards_decay_% -0.1 _diffrn_standards_interval_count 300 _reflns_number_total 4080 _reflns_number_gt 3080 _reflns_threshold_expression F>3.0\s(F) _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogen geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source MO Mo -1.825 0.688 'International Tables Vol. IV (1974) Table 2.2B' F F 0.014 0.01 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' B B 0 0.001 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_special_details ; The structure was solved using a combination of direct methods (MULTAN-78) and Fourier techniques. The unique Mo atom was located in the initial E-map and the remaining non-hydrogen atoms were located in successive iterations of least-squares refinement and difference Fourier calculations. The asymmetric unit was found to contain one half of the Mo-dimer, one BF4-anion, and two molecules of pyridine that had been used as solvent during the crystallization. One of the solvent molecules (atoms C(40) through C(51)) was severely disordered. The atoms eventually included in this solvent molecule , using carbon scattering factors, were located after many iterations and as seen from the plots the results are not impressive. The sum of the occupancies of atoms C(40) through C(51) is 6.12. The remaining parts of the structure are well behaved and hydrogen atoms were located on the main molecule as well as on the ordered solvent. The final R(F) was 0.063 for 401 variables and the full unique data. All non-hydrogen atoms, except for the C(40) through C(51), were refined using anisotropic thermal parameters, the hydrogen atoms were included in fixed calculated positions with isotropic temperature factors equal to 1.0 plus the isotropic equivalent of the parent atom. The largest delta/sigma was 0.004 for atoms in the ordered parts of the molecule while for the disordered solvent the largest delta/sigma was 0.4 for a thermal parameter. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 4080 _refine_ls_number_parameters 401 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef -0.3886E-8 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.05F)^2^ _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.0575 _refine_ls_goodness_of_fit_ref 1.3587 _refine_ls_shift/su_max 0.0076 _refine_diff_density_max 0.7 _refine_diff_density_min -0.64 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly MO1 MO 0.78882(3) 0.26545(4) 0.51250(3) 0.0451(4) Uani 1 0 . N2 N 0.7906(3) 0.2254(5) 0.4015(3) 0.049(3) Uani 1 0 . C3 C 0.7474(4) 0.1929(5) 0.3541(4) 0.050(4) Uani 1 0 . N4 N 0.7936(3) 0.3100(4) 0.6243(3) 0.045(3) Uani 1 0 . C5 C 0.8342(4) 0.2375(6) 0.3756(4) 0.053(3) Uani 1 0 . C6 C 0.8317(4) 0.2507(6) 0.3008(4) 0.058(4) Uani 1 0 . C7 C 0.8759(4) 0.2645(7) 0.2799(5) 0.065(4) Uani 1 0 . C8 C 0.9221(4) 0.2656(7) 0.3320(6) 0.075(4) Uani 1 0 . C9 C 0.9246(4) 0.2550(8) 0.4064(6) 0.084(5) Uani 1 0 . C10 C 0.8817(4) 0.2403(7) 0.4282(4) 0.070(4) Uani 1 0 . C11 C 0.8392(4) 0.3484(6) 0.6765(4) 0.049(3) Uani 1 0 . C12 C 0.8388(3) 0.4289(6) 0.7285(4) 0.051(3) Uani 1 0 . C13 C 0.8837(4) 0.4610(7) 0.7780(4) 0.062(4) Uani 1 0 . C14 C 0.9283(5) 0.4165(9) 0.7760(5) 0.089(5) Uani 1 0 . C15 C 0.9283(4) 0.3403(9) 0.7223(5) 0.087(5) Uani 1 0 . C16 C 0.8840(4) 0.3054(7) 0.6737(4) 0.065(4) Uani 1 0 . N17 N 0.8184(3) 0.1032(5) 0.5515(3) 0.053(3) Uani 1 0 . C18 C 0.8240(4) 0.0699(6) 0.6224(4) 0.065(4) Uani 1 0 . C19 C 0.8407(4) -0.0309(7) 0.6474(5) 0.084(5) Uani 1 0 . C20 C 0.8552(5) -0.1003(7) 0.6000(6) 0.110(6) Uani 1 0 . C21 C 0.8502(5) -0.0673(7) 0.5271(5) 0.099(5) Uani 1 0 . C22 C 0.8319(4) 0.0329(6) 0.5057(4) 0.075(4) Uani 1 0 . N23 N 0.7928(3) 0.4403(4) 0.4863(3) 0.049(3) Uani 1 0 . C24 C 0.7973(4) 0.4753(6) 0.4198(4) 0.061(4) Uani 1 0 . C25 C 0.8002(4) 0.5817(6) 0.4022(4) 0.071(5) Uani 1 0 . C26 C 0.7979(5) 0.6581(6) 0.4531(5) 0.090(5) Uani 1 0 . C27 C 0.7925(5) 0.6238(6) 0.5207(5) 0.089(5) Uani 1 0 . C28 C 0.7910(4) 0.5174(6) 0.5344(4) 0.070(4) Uani 1 0 . B29 B 0.7905(5) -0.0988(7) 0.3095(5) 0.058(5) Uani 1 0 . F30 F 0.7591(2) -0.1120(4) 0.3545(3) 0.081(3) Uani 1 0 . F31 F 0.8271(3) -0.0281(5) 0.3407(3) 0.105(3) Uani 1 0 . F32 F 0.7627(3) -0.0593(7) 0.2431(3) 0.141(4) Uani 1 0 . F33 F 0.8097(3) -0.1935(5) 0.2969(4) 0.127(4) Uani 1 0 . N34 N 0.9357(4) 0.6837(10) 0.6044(6) 0.107(5) Uani 1 0 . C35 C 0.9326(5) 0.5036(10) 0.5609(7) 0.100(6) Uani 1 0 . C36 C 0.9319(5) 0.5772(12) 0.6128(7) 0.108(7) Uani 1 0 . C37 C 0.9396(5) 0.7120(10) 0.5378(8) 0.112(7) Uani 1 0 . C38 C 0.9351(8) 0.5357(16) 0.4947(9) 0.156(10) Uani 1 0 . C39 C 0.9399(8) 0.6430(17) 0.4830(8) 0.171(11) Uani 1 0 . C40 C 0.9705(13) 0.159(2) 0.5966(17) 0.084(10) Uiso 0.460822 0 . C41 C 0.9847(15) 0.109(3) 0.671(2) 0.110(10) Uiso 0.372678 0 . C42 C 1.023(2) 0.027(5) 0.704(3) 0.250(19) Uiso 0.427493 0 . C43 C 1.0550(8) 0.0292(16) 0.6206(12) 0.058(5) Uiso 0.455469 0 . C44 C 1.0203(10) 0.011(2) 0.5625(15) 0.092(8) Uiso 0.442758 0 . C45 C 0.9749(9) 0.0672(18) 0.5477(12) 0.077(6) Uiso 0.464276 0 . C46 C 0.9617(9) 0.1263(17) 0.6049(13) 0.086(8) Uiso 0.653222 0 . C47 C 1.0081(8) 0.1867(15) 0.6192(10) 0.104(5) Uiso 0.720856 0 . C48 C 1.0531(6) 0.1314(13) 0.6382(8) 0.079(4) Uiso 0.68909 0 . C49 C 1.0528(8) 0.0303(17) 0.6605(12) 0.107(6) Uiso 0.653597 0 . C50 C 1.0020(16) -0.021(3) 0.642(2) 0.104(11) Uiso 0.328287 0 . C51 C 0.9613(15) 0.057(3) 0.624(2) 0.149(13) Uiso 0.479521 0 . H1 H 0.7475 0.1713 0.3035 0.062 Uiso 1 0 . H2 H 0.7999 0.2507 0.2625 0.0742 Uiso 1 0 . H3 H 0.8746 0.2734 0.2276 0.0806 Uiso 1 0 . H4 H 0.9536 0.275 0.3172 0.093 Uiso 1 0 . H5 H 0.957 0.2568 0.4437 0.0989 Uiso 1 0 . H6 H 0.8841 0.2318 0.4804 0.0826 Uiso 1 0 . H7 H 0.8068 0.4616 0.7292 0.0698 Uiso 1 0 . H8 H 0.8831 0.5163 0.8143 0.0688 Uiso 1 0 . H9 H 0.9595 0.4369 0.8132 0.1049 Uiso 1 0 . H10 H 0.9605 0.3116 0.718 0.1022 Uiso 1 0 . H11 H 0.884 0.2504 0.637 0.0747 Uiso 1 0 . H12 H 0.8139 0.1191 0.657 0.0835 Uiso 1 0 . H13 H 0.8437 -0.0527 0.6984 0.0904 Uiso 1 0 . H14 H 0.8684 -0.171 0.6169 0.1125 Uiso 1 0 . H15 H 0.8612 -0.113 0.4926 0.1009 Uiso 1 0 . H16 H 0.8278 0.0557 0.4545 0.0878 Uiso 1 0 . H17 H 0.799 0.4224 0.3828 0.0629 Uiso 1 0 . H18 H 0.805 0.6023 0.3543 0.0731 Uiso 1 0 . H19 H 0.7977 0.7339 0.4414 0.0955 Uiso 1 0 . H20 H 0.7903 0.6757 0.5583 0.0937 Uiso 1 0 . H21 H 0.7883 0.4955 0.5828 0.0879 Uiso 1 0 . H22 H 0.9283 0.4264 0.5716 0.1156 Uiso 1 0 . H23 H 0.9315 0.5515 0.6617 0.113 Uiso 1 0 . H24 H 0.9419 0.7904 0.5274 0.1309 Uiso 1 0 . H25 H 0.9333 0.4851 0.4559 0.1688 Uiso 1 0 . H26 H 0.9435 0.6674 0.4356 0.1758 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 MO1 0.0911(10) 0.0169(3) 0.0161(3) 0.0077(4) -0.0029(3) -0.0027(3) N2 0.090(6) 0.025(3) 0.020(3) 0.006(4) -0.005(4) -0.002(3) C3 0.112(9) 0.012(4) 0.017(4) 0.010(4) 0.003(5) -0.000(3) N4 0.087(6) 0.022(3) 0.015(3) 0.006(3) -0.005(4) -0.000(2) C5 0.089(7) 0.021(4) 0.033(4) 0.009(4) -0.006(5) -0.009(3) C6 0.089(7) 0.033(5) 0.042(5) -0.004(5) 0.004(5) -0.016(4) C7 0.098(8) 0.042(5) 0.053(5) -0.001(5) 0.016(6) -0.015(4) C8 0.080(7) 0.061(6) 0.076(7) 0.008(5) 0.009(6) -0.034(5) C9 0.089(9) 0.072(7) 0.076(7) 0.038(7) -0.003(6) -0.025(6) C10 0.095(8) 0.060(6) 0.039(5) 0.032(6) -0.006(5) -0.015(4) C11 0.083(7) 0.030(4) 0.020(4) -0.001(4) -0.006(4) 0.001(3) C12 0.098(7) 0.029(4) 0.020(4) -0.007(4) 0.008(4) -0.001(3) C13 0.106(9) 0.053(5) 0.026(4) -0.024(6) 0.015(5) -0.015(4) C14 0.104(10) 0.097(9) 0.050(6) -0.019(7) -0.004(6) -0.035(6) C15 0.073(8) 0.106(9) 0.062(6) 0.014(6) -0.015(6) -0.039(6) C16 0.086(8) 0.059(6) 0.037(5) 0.008(5) -0.003(5) -0.017(4) N17 0.091(6) 0.027(3) 0.027(4) 0.014(3) -0.007(3) -0.004(3) C18 0.119(9) 0.031(4) 0.033(5) 0.015(5) 0.002(5) 0.001(4) C19 0.153(11) 0.040(5) 0.044(5) 0.025(6) 0.002(6) 0.009(4) C20 0.219(15) 0.040(6) 0.057(6) 0.050(7) 0.017(8) 0.012(5) C21 0.197(13) 0.040(5) 0.038(5) 0.043(7) 0.001(6) -0.001(4) C22 0.130(9) 0.039(5) 0.034(5) 0.025(5) -0.012(5) -0.006(4) N23 0.099(6) 0.020(3) 0.021(3) 0.000(3) 0.003(3) -0.001(3) C24 0.121(9) 0.030(4) 0.029(4) 0.004(5) 0.015(5) -0.005(3) C25 0.147(10) 0.037(5) 0.036(5) 0.007(5) 0.037(5) 0.005(4) C26 0.207(13) 0.026(5) 0.038(5) -0.002(6) 0.038(6) 0.000(4) C27 0.208(13) 0.032(5) 0.032(5) 0.006(6) 0.042(6) -0.009(4) C28 0.165(10) 0.023(4) 0.021(4) 0.006(5) 0.023(5) -0.001(3) B29 0.107(10) 0.038(6) 0.022(5) -0.008(6) 0.007(6) 0.000(4) F30 0.115(5) 0.078(4) 0.049(3) -0.003(3) 0.022(3) 0.019(3) F31 0.137(6) 0.083(4) 0.096(5) -0.029(4) 0.031(4) -0.053(4) F32 0.126(6) 0.241(9) 0.055(4) 0.017(6) 0.023(4) 0.069(5) F33 0.212(8) 0.055(4) 0.133(6) -0.003(4) 0.077(6) -0.036(4) N34 0.124(9) 0.120(9) 0.095(8) -0.013(7) 0.062(7) -0.037(7) C35 0.106(10) 0.111(10) 0.080(8) -0.015(8) 0.022(7) -0.024(8) C36 0.146(13) 0.110(11) 0.094(9) -0.014(9) 0.075(9) -0.021(8) C37 0.133(12) 0.104(10) 0.123(11) -0.031(8) 0.076(10) -0.028(9) C38 0.23(2) 0.147(15) 0.085(11) 0.015(14) 0.028(11) -0.063(11) C39 0.27(2) 0.189(18) 0.072(9) -0.000(17) 0.074(12) -0.035(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MO1 MO1 2.1066(17) . 8_656 no MO1 N2 2.151(6) . . no MO1 N4 2.132(6) . . no MO1 N17 2.226(6) . . no MO1 N23 2.243(5) . . no F30 B29 1.383(12) . . no F31 B29 1.347(11) . . no F32 B29 1.355(10) . . no F33 B29 1.343(11) . . no N2 C3 1.335(10) . . no N2 C5 1.435(11) . . no N4 C3 1.312(10) . 8_656 no N4 C11 1.443(10) . . no N17 C18 1.357(9) . . no N17 C22 1.351(10) . . no N23 C24 1.359(9) . . no N23 C28 1.326(9) . . no N34 C36 1.344(15) . . no N34 C37 1.330(15) . . no C5 C6 1.390(11) . . no C5 C10 1.403(12) . . no C6 C7 1.399(12) . . no C7 C8 1.374(12) . . no C8 C9 1.380(14) . . no C9 C10 1.378(14) . . no C11 C12 1.401(10) . . no C11 C16 1.369(12) . . no C12 C13 1.384(12) . . no C13 C14 1.366(14) . . no C14 C15 1.383(13) . . no C15 C16 1.376(12) . . no C18 C19 1.374(11) . . no C19 C20 1.378(13) . . no C20 C21 1.393(13) . . no C21 C22 1.364(11) . . no C24 C25 1.373(11) . . no C25 C26 1.362(11) . . no C26 C27 1.383(11) . . no C27 C28 1.354(11) . . no C35 C36 1.339(15) . . no C35 C38 1.323(19) . . no C37 C39 1.340(18) . . no C38 C39 1.37(2) . . no C40 C41 1.48(5) . . no C40 C45 1.49(4) . . no C40 C46 0.52(3) . . no C40 C47 1.07(3) . . no C40 C51 1.42(4) . . no C41 C42 1.48(6) . . no C41 C46 1.24(4) . . no C41 C47 1.63(4) . . no C41 C50 1.82(5) . . no C41 C51 1.14(4) . . no C42 C43 2.00(6) . . no C42 C49 1.31(6) . . no C42 C50 1.29(6) . . no C42 C51 1.97(7) . . no C43 C44 1.25(3) . . no C43 C48 1.32(3) . . no C43 C49 0.77(2) . . no C43 C50 1.75(5) . . no C44 C45 1.40(3) . . no C44 C49 1.82(3) . . no C44 C50 1.74(4) . . no C45 C46 1.43(3) . . no C45 C47 2.04(3) . . no C45 C50 2.03(5) . . no C45 C51 1.58(4) . . no C46 C47 1.45(3) . . no C46 C51 0.93(4) . . no C47 C48 1.38(2) . . no C48 C49 1.33(2) . . no C49 C50 1.50(4) . . no C50 C51 1.46(5) . . no C3 H1 0.986(7) . . no C6 H2 0.965(9) . . no C7 H3 0.976(9) . . no C8 H4 0.994(11) . . no C9 H5 0.969(10) . . no C10 H6 0.965(9) . . no C12 H7 0.979(9) . . no C13 H8 0.971(8) . . no C14 H9 0.978(10) . . no C15 H10 0.987(10) . . no C16 H11 0.970(8) . . no C18 H12 0.989(8) . . no C19 H13 0.973(9) . . no C20 H14 0.972(9) . . no C21 H15 0.973(10) . . no C22 H16 0.974(9) . . no C24 H17 0.967(7) . . no C25 H18 0.977(8) . . no C26 H19 0.969(8) . . no C27 H20 0.971(8) . . no C28 H21 0.969(7) . . no C35 H22 0.996(13) . . no C36 H23 0.974(12) . . no C37 H24 1.002(13) . . no C38 H25 0.953(13) . . no C39 H26 0.969(15) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag MO1 MO1 N2 92.6(2) 8_656 . . no MO1 MO1 N4 92.3(2) 8_656 . . no MO1 MO1 N17 99.55(19) 8_656 . . no MO1 MO1 N23 103.84(19) 8_656 . . no N2 MO1 N4 175.0(3) . . . no N2 MO1 N17 89.9(2) . . . no N2 MO1 N23 89.9(2) . . . no N4 MO1 N17 90.0(2) . . . no N4 MO1 N23 88.2(2) . . . no N17 MO1 N23 156.6(3) . . . no MO1 N2 C3 116.7(6) . . . no MO1 N2 C5 123.8(5) . . . no C3 N2 C5 119.5(7) . . . no MO1 N4 C3 118.5(5) . . 8_656 no MO1 N4 C11 123.3(6) . . . no C3 N4 C11 118.1(7) 8_656 . . no MO1 N17 C18 121.8(5) . . . no MO1 N17 C22 121.5(5) . . . no C18 N17 C22 116.6(6) . . . no MO1 N23 C24 122.3(4) . . . no MO1 N23 C28 122.8(5) . . . no C24 N23 C28 114.8(6) . . . no C36 N34 C37 113.6(10) . . . no N2 C3 N4 119.9(7) . . 8_656 no N2 C5 C6 123.1(8) . . . no N2 C5 C10 118.6(8) . . . no C6 C5 C10 118.2(10) . . . no C5 C6 C7 119.9(8) . . . no C6 C7 C8 121.3(9) . . . no C7 C8 C9 118.9(10) . . . no C8 C9 C10 120.9(9) . . . no C5 C10 C9 120.9(9) . . . no N4 C11 C12 122.0(8) . . . no N4 C11 C16 118.4(7) . . . no C12 C11 C16 119.6(8) . . . no C11 C12 C13 119.2(9) . . . no C12 C13 C14 121.1(8) . . . no C13 C14 C15 119.0(9) . . . no C14 C15 C16 121.0(10) . . . no C11 C16 C15 120.0(8) . . . no N17 C18 C19 123.0(8) . . . no C18 C19 C20 119.2(8) . . . no C19 C20 C21 118.6(8) . . . no C20 C21 C22 118.9(9) . . . no N17 C22 C21 123.6(8) . . . no N23 C24 C25 123.8(7) . . . no C24 C25 C26 119.3(7) . . . no C25 C26 C27 117.6(7) . . . no C26 C27 C28 119.5(7) . . . no N23 C28 C27 124.9(7) . . . no C36 C35 C38 119.2(14) . . . no N34 C36 C35 125.1(12) . . . no N34 C37 C39 124.6(14) . . . no C35 C38 C39 118.6(13) . . . no C37 C39 C38 118.9(15) . . . no C41 C40 C45 102(2) . . . no C41 C40 C46 54(5) . . . no C41 C40 C47 78(3) . . . no C41 C40 C51 46.2(19) . . . no C45 C40 C46 73(5) . . . no C45 C40 C47 104(3) . . . no C45 C40 C51 66(2) . . . no C46 C40 C47 129(7) . . . no C46 C40 C51 17(5) . . . no C47 C40 C51 114(3) . . . no C40 C41 C42 131(4) . . . no C40 C41 C46 19.8(18) . . . no C40 C41 C47 39.7(14) . . . no C40 C41 C50 97(3) . . . no C40 C41 C51 64(3) . . . no C42 C41 C46 130(4) . . . no C42 C41 C47 107(4) . . . no C42 C41 C50 45(3) . . . no C42 C41 C51 97(4) . . . no C46 C41 C47 59(2) . . . no C46 C41 C50 88(3) . . . no C46 C41 C51 46(3) . . . no C47 C41 C50 100(2) . . . no C47 C41 C51 96(3) . . . no C50 C41 C51 53(3) . . . no C41 C42 C43 95(4) . . . no C41 C42 C49 103(5) . . . no C41 C42 C50 82(4) . . . no C41 C42 C51 35(2) . . . no C43 C42 C49 11.9(18) . . . no C43 C42 C50 60(3) . . . no C43 C42 C51 83(3) . . . no C49 C42 C50 70(4) . . . no C49 C42 C51 95(4) . . . no C50 C42 C51 48(3) . . . no C42 C43 C44 106(3) . . . no C42 C43 C48 76(2) . . . no C42 C43 C49 21(3) . . . no C42 C43 C50 39.7(19) . . . no C44 C43 C48 108(2) . . . no C44 C43 C49 126(4) . . . no C44 C43 C50 69(2) . . . no C48 C43 C49 74(3) . . . no C48 C43 C50 101(2) . . . no C49 C43 C50 59(3) . . . no C43 C44 C45 121(3) . . . no C43 C44 C49 19.9(14) . . . no C43 C44 C50 69(2) . . . no C45 C44 C49 107.1(19) . . . no C45 C44 C50 80(2) . . . no C49 C44 C50 49.7(16) . . . no C40 C45 C44 119(2) . . . no C40 C45 C46 20.4(13) . . . no C40 C45 C47 30.4(13) . . . no C40 C45 C50 87.6(19) . . . no C40 C45 C51 54.9(18) . . . no C44 C45 C46 121(2) . . . no C44 C45 C47 91.3(17) . . . no C44 C45 C50 57.6(17) . . . no C44 C45 C51 102(2) . . . no C46 C45 C47 45.3(12) . . . no C46 C45 C50 75.0(17) . . . no C46 C45 C51 35.7(15) . . . no C47 C45 C50 80.8(15) . . . no C47 C45 C51 69.2(17) . . . no C50 C45 C51 45.6(18) . . . no C40 C46 C41 106(6) . . . no C40 C46 C45 86(6) . . . no C40 C46 C47 35(5) . . . no C40 C46 C51 153(8) . . . no C41 C46 C45 119(3) . . . no C41 C46 C47 74(2) . . . no C41 C46 C51 61(3) . . . no C45 C46 C47 90.1(17) . . . no C45 C46 C51 81(3) . . . no C47 C46 C51 121(4) . . . no C40 C47 C41 62(2) . . . no C40 C47 C45 45(2) . . . no C40 C47 C46 16(2) . . . no C40 C47 C48 131(3) . . . no C41 C47 C45 77.0(17) . . . no C41 C47 C46 47.0(15) . . . no C41 C47 C48 92.0(19) . . . no C45 C47 C46 44.6(12) . . . no C45 C47 C48 90.6(13) . . . no C46 C47 C48 118.7(17) . . . no C43 C48 C47 121.0(17) . . . no C43 C48 C49 33.7(11) . . . no C47 C48 C49 117.9(17) . . . no C42 C49 C43 147(5) . . . no C42 C49 C44 114(3) . . . no C42 C49 C48 107(4) . . . no C42 C49 C50 54(3) . . . no C43 C49 C44 34(2) . . . no C43 C49 C48 73(3) . . . no C43 C49 C50 95(3) . . . no C44 C49 C48 81.6(15) . . . no C44 C49 C50 62.7(19) . . . no C48 C49 C50 115(2) . . . no C41 C50 C42 54(3) . . . no C41 C50 C43 93(2) . . . no C41 C50 C44 103(3) . . . no C41 C50 C45 73(2) . . . no C41 C50 C49 82(2) . . . no C41 C50 C51 39(2) . . . no C42 C50 C43 81(4) . . . no C42 C50 C44 119(4) . . . no C42 C50 C45 119(4) . . . no C42 C50 C49 55(3) . . . no C42 C50 C51 91(4) . . . no C43 C50 C44 42.1(13) . . . no C43 C50 C45 74.7(18) . . . no C43 C50 C49 26.0(12) . . . no C43 C50 C51 111(3) . . . no C44 C50 C45 42.7(13) . . . no C44 C50 C49 68(2) . . . no C44 C50 C51 93(3) . . . no C45 C50 C49 94(2) . . . no C45 C50 C51 51(2) . . . no C49 C50 C51 112(3) . . . no C40 C51 C41 70(3) . . . no C40 C51 C42 104(3) . . . no C40 C51 C45 59(2) . . . no C40 C51 C46 10(3) . . . no C40 C51 C50 118(3) . . . no C41 C51 C42 48(3) . . . no C41 C51 C45 115(4) . . . no C41 C51 C46 73(4) . . . no C41 C51 C50 88(4) . . . no C42 C51 C45 109(3) . . . no C42 C51 C46 111(4) . . . no C42 C51 C50 41(2) . . . no C45 C51 C46 63(3) . . . no C45 C51 C50 84(3) . . . no C46 C51 C50 128(5) . . . no F30 B29 F31 110.0(7) . . . no F30 B29 F32 108.0(9) . . . no F30 B29 F33 110.7(8) . . . no F31 B29 F32 108.8(8) . . . no F31 B29 F33 111.3(10) . . . no F32 B29 F33 108.0(8) . . . no N2 C3 H1 118.3(10) . . . no N4 C3 H1 121.9(9) 8_656 . . no C5 C6 H2 121.5(10) . . . no C7 C6 H2 118.6(8) . . . no C6 C7 H3 120.6(10) . . . no C8 C7 H3 118.1(11) . . . no C7 C8 H4 121.3(10) . . . no C9 C8 H4 119.8(10) . . . no C8 C9 H5 119.6(13) . . . no C10 C9 H5 119.5(11) . . . no C5 C10 H6 119.3(12) . . . no C9 C10 H6 119.8(10) . . . no C11 C12 H7 119.6(8) . . . no C13 C12 H7 121.2(8) . . . no C12 C13 H8 118.8(11) . . . no C14 C13 H8 120.1(10) . . . no C13 C14 H9 120.2(10) . . . no C15 C14 H9 120.8(13) . . . no C14 C15 H10 119.6(10) . . . no C16 C15 H10 119.4(9) . . . no C11 C16 H11 119.2(9) . . . no C15 C16 H11 120.8(11) . . . no N17 C18 H12 118.4(7) . . . no C19 C18 H12 118.5(8) . . . no C18 C19 H13 120.9(9) . . . no C20 C19 H13 119.9(8) . . . no C19 C20 H14 120.7(10) . . . no C21 C20 H14 120.7(10) . . . no C20 C21 H15 120.8(8) . . . no C22 C21 H15 120.2(9) . . . no N17 C22 H16 117.3(7) . . . no C21 C22 H16 119.1(9) . . . no N23 C24 H17 118.3(7) . . . no C25 C24 H17 117.9(8) . . . no C24 C25 H18 120.4(8) . . . no C26 C25 H18 120.2(8) . . . no C25 C26 H19 121.4(8) . . . no C27 C26 H19 121.0(8) . . . no C26 C27 H20 120.1(8) . . . no C28 C27 H20 120.3(8) . . . no N23 C28 H21 117.2(7) . . . no C27 C28 H21 117.8(7) . . . no C36 C35 H22 119.3(14) . . . no C38 C35 H22 121.3(14) . . . no N34 C36 H23 117.1(13) . . . no C35 C36 H23 117.6(15) . . . no N34 C37 H24 117.8(13) . . . no C39 C37 H24 117.6(16) . . . no C35 C38 H25 121(2) . . . no C39 C38 H25 121(2) . . . no C37 C39 H26 122(2) . . . no C38 C39 H26 119.6(18) . . . no # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ ######################################################################## ###### # IUMSC CIF Archive file # ######################################################################## ###### data_MSC96173 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C27 H32 B3 F12 Mo2 N9' _chemical_formula_moiety ? _chemical_formula_weight 934.906 _cell_length_a 23.831(3) _cell_length_b 12.2175(17) _cell_length_c 26.018(4) _cell_angle_alpha 90 _cell_angle_beta 94.130(7) _cell_angle_gamma 90 _cell_volume 7555.8(18) _cell_formula_units_Z 8 _cell_measurement_reflns_used 42 _cell_measurement_theta_min 9.72 _cell_measurement_theta_max 10.48 _cell_measurement_temperature 104. _exptl_crystal_colour red _exptl_crystal_description irregular _exptl_crystal_size_max .40 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .25 _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 0.7555 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 104. _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10814 _diffrn_reflns_av_R_equivalents 0.04 _diffrn_reflns_theta_min 3.05772 _diffrn_reflns_theta_max 22.5002 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_standards_number 4 _diffrn_standards_decay_% 1 _diffrn_standards_interval_count 400 _reflns_number_total 9840 _reflns_number_gt 5337 _reflns_threshold_expression F^2^>2.33\s(F^2^) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source MO Mo -1.825 0.688 'International Tables Vol. IV (1974) Table 2.2B' F F 0.014 0.01 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' B B 0 0.001 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 5337 _refine_ls_number_parameters 956 _refine_ls_hydrogen_treatment NOREF _refine_ls_extinction_coef 0.0000000179(19) _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.03F)^2^ _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.0473 _refine_ls_goodness_of_fit_ref 1.1228 _refine_ls_shift/su_max 1.2188 _refine_diff_density_max 0.71 _refine_diff_density_min -1.04 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly MO1 MO 0.62384(4) 0.13237(7) 0.11439(4) 0.0157(3) Uani 1 0 . MO2 MO 0.63378(4) 0.30602(7) 0.12454(3) 0.0166(3) Uani 1 0 . C3 C 0.7825(4) -0.0077(8) 0.0851(4) 0.022(4) Uani 1 0 . C4 C 0.8053(4) -0.1046(9) 0.0684(4) 0.024(4) Uani 1 0 . C5 C 0.7739(4) -0.1746(9) 0.0344(4) 0.029(4) Uani 1 0 . C6 C 0.7187(4) -0.1458(8) 0.0186(4) 0.022(3) Uani 1 0 . C7 C 0.6956(4) -0.0494(8) 0.0353(4) 0.017(3) Uani 1 0 . C8 C 0.7268(4) 0.0205(8) 0.0668(4) 0.022(4) Uani 1 0 . N9 N 0.7024(3) 0.1203(6) 0.0844(3) 0.018(3) Uani 1 0 . C10 C 0.7350(4) 0.2072(7) 0.0841(4) 0.014(3) Uani 1 0 . N11 N 0.7147(3) 0.3034(6) 0.0998(3) 0.014(3) Uani 1 0 . C12 C 0.7508(4) 0.3967(8) 0.1018(4) 0.021(4) Uani 1 0 . C13 C 0.7257(4) 0.4988(9) 0.0972(5) 0.030(4) Uani 1 0 . C14 C 0.7570(5) 0.5929(8) 0.0973(5) 0.036(4) Uani 1 0 . C15 C 0.8154(5) 0.5858(9) 0.1013(5) 0.034(4) Uani 1 0 . C16 C 0.8416(4) 0.4845(8) 0.1049(4) 0.026(4) Uani 1 0 . C17 C 0.8087(4) 0.3910(8) 0.1062(4) 0.019(3) Uani 1 0 . N18 N 0.6095(4) -0.0771(8) 0.1151(4) 0.029(3) Uani 1 0 . C19 C 0.6054(4) -0.1663(9) 0.1229(4) 0.021(4) Uani 1 0 . C20 C 0.6009(6) -0.2827(9) 0.1322(5) 0.047(5) Uani 1 0 . N21 N 0.5807(3) 0.1262(6) 0.0390(4) 0.020(3) Uani 1 0 . C22 C 0.5562(4) 0.1132(8) 0.0003(4) 0.019(4) Uani 1 0 . C23 C 0.5250(4) 0.0985(9) -0.0489(4) 0.028(4) Uani 1 0 . N24 N 0.5438(4) 0.1142(7) 0.1495(3) 0.021(3) Uani 1 0 . C25 C 0.5043(5) 0.1040(9) 0.1712(5) 0.026(4) Uani 1 0 . C26 C 0.4542(5) 0.0951(10) 0.1998(5) 0.040(5) Uani 1 0 . N27 N 0.6614(4) 0.0843(7) 0.1875(4) 0.021(3) Uani 1 0 . C28 C 0.6811(4) 0.0441(8) 0.2239(4) 0.022(4) Uani 1 0 . C29 C 0.7032(4) -0.0062(8) 0.2716(4) 0.026(4) Uani 1 0 . N30 N 0.5995(3) 0.3622(7) 0.0510(4) 0.024(3) Uani 1 0 . C31 C 0.5765(5) 0.3893(8) 0.0139(5) 0.026(4) Uani 1 0 . C32 C 0.5451(5) 0.4198(8) -0.0340(4) 0.027(4) Uani 1 0 . N33 N 0.5550(4) 0.3611(7) 0.1525(3) 0.024(3) Uani 1 0 . C34 C 0.5141(5) 0.3878(8) 0.1666(4) 0.024(4) Uani 1 0 . C35 C 0.4591(5) 0.4205(10) 0.1846(5) 0.039(5) Uani 1 0 . N36 N 0.6657(3) 0.3195(7) 0.2020(4) 0.023(3) Uani 1 0 . C37 C 0.6757(4) 0.3336(8) 0.2456(5) 0.022(4) Uani 1 0 . C38 C 0.6903(5) 0.3519(9) 0.2997(4) 0.031(4) Uani 1 0 . MO39 MO 0.62182(4) 0.15331(7) 0.61414(4) 0.0166(3) Uani 1 0 . MO40 MO 0.62821(4) 0.32838(7) 0.62094(4) 0.0169(3) Uani 1 0 . C41 C 0.7845(4) 0.0247(8) 0.5901(4) 0.021(4) Uani 1 0 . C42 C 0.8121(5) -0.0673(9) 0.5725(4) 0.030(4) Uani 1 0 . C43 C 0.7854(5) -0.1362(8) 0.5387(4) 0.030(4) Uani 1 0 . C44 C 0.7296(5) -0.1178(8) 0.5215(4) 0.028(4) Uani 1 0 . C45 C 0.7032(4) -0.0261(8) 0.5372(4) 0.022(3) Uani 1 0 . C46 C 0.7301(4) 0.0449(7) 0.5718(4) 0.018(4) Uani 1 0 . N47 N 0.7018(3) 0.1432(6) 0.5856(3) 0.016(3) Uani 1 0 . C48 C 0.7314(4) 0.2344(9) 0.5850(4) 0.018(4) Uani 1 0 . N49 N 0.7101(3) 0.3284(6) 0.5987(3) 0.020(3) Uani 1 0 . C50 C 0.7447(4) 0.4229(8) 0.5983(4) 0.019(4) Uani 1 0 . C51 C 0.7196(4) 0.5230(9) 0.5878(5) 0.036(4) Uani 1 0 . C52 C 0.7515(5) 0.6187(9) 0.5876(5) 0.040(5) Uani 1 0 . C53 C 0.8094(5) 0.6113(9) 0.5951(5) 0.032(4) Uani 1 0 . C54 C 0.8347(4) 0.5145(8) 0.6051(4) 0.021(4) Uani 1 0 . C55 C 0.8035(5) 0.4192(8) 0.6079(4) 0.026(4) Uani 1 0 . N56 N 0.6104(3) -0.0556(7) 0.6143(3) 0.022(3) Uani 1 0 . C57 C 0.6061(4) -0.1467(10) 0.6200(4) 0.027(4) Uani 1 0 . C58 C 0.6006(5) -0.2645(10) 0.6262(5) 0.042(5) Uani 1 0 . N59 N 0.5794(3) 0.1400(7) 0.5396(3) 0.018(3) Uani 1 0 . C60 C 0.5563(4) 0.1215(8) 0.5010(4) 0.019(4) Uani 1 0 . C61 C 0.5243(4) 0.0965(8) 0.4517(4) 0.027(4) Uani 1 0 . N62 N 0.5421(4) 0.1316(6) 0.6478(4) 0.021(3) Uani 1 0 . C63 C 0.5045(5) 0.1187(8) 0.6717(4) 0.024(4) Uani 1 0 . C64 C 0.4566(5) 0.1046(10) 0.7032(5) 0.038(5) Uani 1 0 . N65 N 0.6610(3) 0.1096(7) 0.6881(4) 0.022(3) Uani 1 0 . C66 C 0.6806(4) 0.0738(8) 0.7254(4) 0.021(4) Uani 1 0 . C67 C 0.7054(5) 0.0306(9) 0.7729(4) 0.035(4) Uani 1 0 . N68 N 0.5951(4) 0.3786(6) 0.5460(4) 0.020(3) Uani 1 0 . C69 C 0.5770(4) 0.4073(8) 0.5064(4) 0.020(4) Uani 1 0 . C70 C 0.5525(5) 0.4453(9) 0.4555(4) 0.033(4) Uani 1 0 . N71 N 0.5484(4) 0.3789(6) 0.6489(3) 0.020(3) Uani 1 0 . C72 C 0.5066(5) 0.4024(8) 0.6655(4) 0.023(4) Uani 1 0 . C73 C 0.4542(5) 0.4327(9) 0.6862(5) 0.034(4) Uani 1 0 . N74 N 0.6587(3) 0.3473(7) 0.6995(4) 0.024(3) Uani 1 0 . C75 C 0.6721(4) 0.3628(8) 0.7414(5) 0.024(4) Uani 1 0 . C76 C 0.6878(5) 0.3809(10) 0.7955(4) 0.037(4) Uani 1 0 . B77 B 0.4241(6) 0.2619(11) 0.0370(6) 0.036(5) Uani 1 0 . F78 F 0.4186(5) 0.3031(9) -0.0106(3) 0.110(5) Uani 1 0 . F79 F 0.4288(3) 0.1514(6) 0.0343(4) 0.082(4) Uani 1 0 . F80 F 0.4714(3) 0.3108(7) 0.0609(3) 0.073(3) Uani 1 0 . F81 F 0.3789(3) 0.2899(6) 0.0627(4) 0.080(4) Uani 1 0 . B82 B 0.5519(5) 0.2367(10) 0.8175(5) 0.024(4) Uani 1 0 . F83 F 0.5728(3) 0.2874(5) 0.8611(2) 0.043(3) Uani 1 0 . F84 F 0.5272(3) 0.3121(6) 0.7829(3) 0.061(3) Uani 1 0 . F85 F 0.5118(3) 0.1593(5) 0.8293(3) 0.044(3) Uani 1 0 . F86 F 0.5948(3) 0.1826(5) 0.7938(3) 0.049(3) Uani 1 0 . B87 B 0.8261(6) 0.1699(11) 0.2363(6) 0.034(5) Uani 1 0 . F88 F 0.8475(3) 0.0757(5) 0.2610(3) 0.050(3) Uani 1 0 . F89 F 0.8670(3) 0.2483(6) 0.2405(4) 0.072(3) Uani 1 0 . F90 F 0.7819(3) 0.2069(6) 0.2639(3) 0.063(3) Uani 1 0 . F91 F 0.8090(5) 0.1459(7) 0.1876(3) 0.103(4) Uani 1 0 . B92 B 0.5512(6) 0.2229(9) 0.3147(5) 0.026(4) Uani 1 0 . F93 F 0.5732(2) 0.2741(5) 0.3606(2) 0.039(2) Uani 1 0 . F94 F 0.5286(3) 0.2989(6) 0.2821(3) 0.062(3) Uani 1 0 . F95 F 0.5932(3) 0.1663(5) 0.2940(3) 0.044(3) Uani 1 0 . F96 F 0.5106(3) 0.1480(5) 0.3283(3) 0.040(2) Uani 1 0 . B97 B 0.5794(6) 0.7404(11) 0.4667(5) 0.030(5) Uani 1 0 . F98 F 0.5386(3) 0.6930(5) 0.4960(3) 0.055(3) Uani 1 0 . F99 F 0.5802(3) 0.8521(5) 0.4777(3) 0.045(3) Uani 1 0 . F100 F 0.5681(4) 0.7207(7) 0.4170(3) 0.080(4) Uani 1 0 . F101 F 0.6309(3) 0.6969(6) 0.4829(3) 0.071(3) Uani 1 0 . B102 B 0.3285(5) 0.2920(11) 0.2386(5) 0.028(5) Uani 1 0 . F103 F 0.3447(3) 0.3879(6) 0.2620(3) 0.064(3) Uani 1 0 . F104 F 0.3638(4) 0.2103(7) 0.2536(4) 0.093(4) Uani 1 0 . F105 F 0.2780(4) 0.2635(7) 0.2495(6) 0.145(7) Uani 1 0 . F106 F 0.3319(6) 0.3036(9) 0.1883(4) 0.160(7) Uani 1 0 . H107 H 0.8035 0.0385 0.1085 0.0352 Uiso 1 0 . H108 H 0.8427 -0.1243 0.0799 0.0374 Uiso 1 0 . H109 H 0.7898 -0.2402 0.0225 0.0413 Uiso 1 0 . H110 H 0.697 -0.1932 -0.004 0.0349 Uiso 1 0 . H111 H 0.6577 -0.0317 0.0247 0.03 Uiso 1 0 . H112 H 0.7722 0.2024 0.0737 0.0254 Uiso 1 0 . H113 H 0.6858 0.5039 0.0941 0.0419 Uiso 1 0 . H114 H 0.7391 0.6627 0.0947 0.0486 Uiso 1 0 . H115 H 0.8376 0.6506 0.1017 0.047 Uiso 1 0 . H116 H 0.8813 0.4789 0.1065 0.0395 Uiso 1 0 . H117 H 0.8264 0.3218 0.1104 0.0318 Uiso 1 0 . H118 H 0.5696 -0.2974 0.1533 0.0589 Uiso 1 0 . H119 H 0.5941 -0.3225 0.1009 0.0589 Uiso 1 0 . H120 H 0.634 -0.3108 0.1504 0.0589 Uiso 1 0 . H121 H 0.4867 0.1152 -0.0453 0.0411 Uiso 1 0 . H122 H 0.5398 0.1454 -0.0734 0.0411 Uiso 1 0 . H123 H 0.5284 0.0244 -0.0593 0.0411 Uiso 1 0 . H124 H 0.4561 0.147 0.2271 0.0522 Uiso 1 0 . H125 H 0.4216 0.1101 0.1773 0.0522 Uiso 1 0 . H126 H 0.4516 0.0236 0.2133 0.0522 Uiso 1 0 . H127 H 0.6733 -0.0208 0.2927 0.0376 Uiso 1 0 . H128 H 0.7214 -0.0734 0.264 0.0376 Uiso 1 0 . H129 H 0.7297 0.0413 0.2889 0.0376 Uiso 1 0 . H130 H 0.55 0.4957 -0.0403 0.0407 Uiso 1 0 . H131 H 0.5586 0.3788 -0.0617 0.0407 Uiso 1 0 . H132 H 0.5063 0.4046 -0.0315 0.0407 Uiso 1 0 . H133 H 0.4612 0.494 0.1964 0.0531 Uiso 1 0 . H134 H 0.4311 0.4148 0.1568 0.0531 Uiso 1 0 . H135 H 0.4499 0.3738 0.2117 0.0531 Uiso 1 0 . H136 H 0.6769 0.2927 0.3193 0.0439 Uiso 1 0 . H137 H 0.73 0.3571 0.3058 0.0439 Uiso 1 0 . H138 H 0.6735 0.4181 0.3103 0.0439 Uiso 1 0 . H139 H 0.8034 0.0727 0.6143 0.0337 Uiso 1 0 . H140 H 0.8499 -0.0814 0.5845 0.0428 Uiso 1 0 . H141 H 0.8049 -0.1977 0.5262 0.0433 Uiso 1 0 . H142 H 0.7098 -0.1688 0.4994 0.0401 Uiso 1 0 . H143 H 0.6657 -0.0108 0.524 0.0344 Uiso 1 0 . H144 H 0.7687 0.2321 0.5743 0.0308 Uiso 1 0 . H145 H 0.6801 0.5268 0.5804 0.0492 Uiso 1 0 . H146 H 0.7336 0.6875 0.5821 0.0529 Uiso 1 0 . H147 H 0.8317 0.6758 0.5934 0.0444 Uiso 1 0 . H148 H 0.8747 0.5111 0.6101 0.0338 Uiso 1 0 . H149 H 0.8218 0.352 0.6165 0.0392 Uiso 1 0 . H150 H 0.5638 -0.2814 0.6357 0.0542 Uiso 1 0 . H151 H 0.6068 -0.3001 0.5945 0.0542 Uiso 1 0 . H152 H 0.6275 -0.2897 0.6522 0.0542 Uiso 1 0 . H153 H 0.4859 0.116 0.4537 0.0404 Uiso 1 0 . H154 H 0.5395 0.1366 0.4246 0.0404 Uiso 1 0 . H155 H 0.5268 0.0202 0.4446 0.0404 Uiso 1 0 . H156 H 0.466 0.1336 0.7366 0.0504 Uiso 1 0 . H157 H 0.425 0.1414 0.6876 0.0504 Uiso 1 0 . H158 H 0.4486 0.0285 0.706 0.0504 Uiso 1 0 . H159 H 0.6846 0.0545 0.8013 0.0472 Uiso 1 0 . H160 H 0.7051 -0.0475 0.7725 0.0472 Uiso 1 0 . H161 H 0.7432 0.0552 0.779 0.0472 Uiso 1 0 . H162 H 0.5252 0.5 0.4603 0.0441 Uiso 1 0 . H163 H 0.5817 0.475 0.4366 0.0441 Uiso 1 0 . H164 H 0.5356 0.3854 0.4372 0.0441 Uiso 1 0 . H165 H 0.4528 0.5097 0.6902 0.0459 Uiso 1 0 . H166 H 0.4238 0.4095 0.6631 0.0459 Uiso 1 0 . H167 H 0.4515 0.3982 0.7186 0.0459 Uiso 1 0 . H168 H 0.663 0.3421 0.8156 0.0492 Uiso 1 0 . H169 H 0.7253 0.3557 0.8031 0.0492 Uiso 1 0 . H170 H 0.686 0.4569 0.8027 0.0492 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 MO1 0.012(2) 0.0200(10) 0.015(3) -0.0016(4) 0.0012(4) -0.0002(4) MO2 0.013(2) 0.0197(9) 0.017(3) -0.0010(4) 0.0022(4) -0.0008(4) C3 0.020(7) 0.028(6) 0.018(7) 0.006(5) 0.003(5) -0.004(5) C4 0.011(6) 0.038(7) 0.025(8) 0.006(5) 0.008(5) 0.009(5) C5 0.032(8) 0.033(7) 0.023(8) 0.004(5) 0.014(5) 0.006(5) C6 0.023(7) 0.021(6) 0.021(7) 0.006(4) 0.004(5) 0.001(4) C7 0.018(6) 0.029(6) 0.006(6) -0.002(5) 0.007(4) -0.000(4) C8 0.019(7) 0.033(7) 0.016(7) 0.012(5) 0.013(5) 0.010(5) N9 0.015(5) 0.025(5) 0.012(6) 0.002(4) -0.001(4) -0.002(4) C10 0.013(6) 0.013(6) 0.015(7) 0.011(4) 0.005(4) 0.010(4) N11 0.013(5) 0.019(5) 0.011(5) -0.006(4) 0.002(4) 0.007(4) C12 0.021(7) 0.023(6) 0.020(8) 0.004(5) 0.000(5) 0.008(5) C13 0.011(6) 0.042(8) 0.035(10) -0.013(5) 0.002(5) 0.003(6) C14 0.045(11) 0.016(6) 0.045(12) -0.005(5) -0.000(6) -0.004(5) C15 0.023(8) 0.039(8) 0.040(11) -0.005(5) 0.001(6) -0.004(6) C16 0.025(7) 0.031(7) 0.023(8) -0.008(5) 0.007(5) -0.004(5) C17 0.019(7) 0.030(6) 0.007(6) -0.003(5) -0.003(4) -0.007(4) N18 0.021(7) 0.031(6) 0.036(9) -0.005(4) 0.009(5) 0.003(5) C19 0.020(7) 0.022(7) 0.020(7) 0.000(5) -0.002(5) 0.002(5) C20 0.058(13) 0.028(8) 0.053(14) 0.007(6) -0.007(7) -0.003(6) N21 0.019(6) 0.007(4) 0.034(9) -0.002(3) -0.001(5) -0.007(4) C22 0.022(7) 0.017(6) 0.016(7) -0.007(5) -0.004(5) -0.004(5) C23 0.024(8) 0.035(7) 0.026(9) -0.004(5) 0.007(5) -0.002(5) N24 0.031(8) 0.025(5) 0.006(5) 0.001(4) 0.000(4) -0.004(4) C25 0.014(7) 0.028(7) 0.034(10) 0.007(5) -0.002(6) -0.012(5) C26 0.026(8) 0.057(9) 0.038(11) -0.005(6) 0.008(6) -0.003(6) N27 0.022(6) 0.018(5) 0.023(7) -0.006(4) 0.003(4) -0.003(4) C28 0.027(8) 0.018(6) 0.023(8) -0.005(5) 0.017(5) 0.001(5) C29 0.025(8) 0.028(6) 0.026(9) 0.004(5) 0.005(5) 0.003(5) N30 0.012(5) 0.028(5) 0.031(9) 0.002(4) 0.004(4) 0.001(4) C31 0.024(8) 0.017(6) 0.037(11) 0.008(5) 0.008(6) -0.000(5) C32 0.032(9) 0.032(7) 0.018(7) 0.016(5) 0.005(5) -0.005(5) N33 0.021(7) 0.018(5) 0.033(9) 0.007(4) 0.004(5) -0.010(4) C34 0.035(9) 0.013(6) 0.024(8) 0.006(5) 0.004(6) 0.000(5) C35 0.019(7) 0.057(9) 0.044(12) 0.011(6) 0.013(6) -0.006(6) N36 0.016(5) 0.025(5) 0.029(8) 0.002(4) 0.008(4) -0.002(4) C37 0.018(7) 0.018(6) 0.031(10) 0.003(4) 0.010(5) -0.005(5) C38 0.033(9) 0.037(7) 0.025(8) -0.000(5) 0.005(5) -0.007(5) MO39 0.015(2) 0.0190(9) 0.016(3) -0.0006(4) 0.0019(4) 0.0002(4) MO40 0.013(2) 0.0200(10) 0.018(3) 0.0007(4) 0.0037(4) -0.0002(4) C41 0.018(7) 0.027(6) 0.019(7) 0.001(5) 0.000(5) 0.006(5) C42 0.029(8) 0.032(7) 0.030(9) 0.013(5) 0.007(5) 0.000(5) C43 0.036(9) 0.025(6) 0.030(9) 0.010(5) 0.012(6) 0.001(5) C44 0.042(10) 0.034(7) 0.008(6) -0.004(5) 0.005(5) -0.008(5) C45 0.026(7) 0.021(6) 0.017(7) 0.006(5) -0.004(5) -0.000(5) C46 0.024(8) 0.011(5) 0.018(7) 0.004(4) 0.005(5) 0.006(4) N47 0.014(5) 0.020(5) 0.013(6) -0.001(4) -0.004(4) 0.005(4) C48 0.007(5) 0.035(7) 0.011(6) 0.007(5) 0.000(4) -0.001(5) N49 0.013(5) 0.022(5) 0.025(7) -0.000(4) 0.005(4) 0.000(4) C50 0.019(7) 0.029(6) 0.009(6) 0.005(5) 0.003(5) 0.004(4) C51 0.009(6) 0.042(8) 0.059(14) -0.002(5) 0.008(5) 0.013(6) C52 0.021(8) 0.026(7) 0.074(17) -0.002(5) 0.007(6) 0.014(6) C53 0.026(8) 0.031(7) 0.040(11) -0.012(5) 0.006(6) 0.007(5) C54 0.017(6) 0.031(7) 0.018(7) -0.004(5) 0.011(5) 0.003(5) C55 0.029(8) 0.028(6) 0.020(8) 0.018(5) -0.007(5) 0.001(5) N56 0.023(7) 0.025(6) 0.018(6) -0.007(4) 0.002(4) -0.010(4) C57 0.017(7) 0.042(8) 0.023(8) -0.011(5) 0.012(5) -0.011(6) C58 0.044(11) 0.034(8) 0.048(13) 0.008(6) 0.005(6) 0.007(6) N59 0.019(6) 0.034(6) 0.002(5) -0.001(4) 0.005(4) 0.003(4) C60 0.010(6) 0.021(6) 0.029(9) 0.007(4) 0.014(5) 0.003(5) C61 0.031(8) 0.024(6) 0.025(9) 0.004(5) -0.016(5) -0.004(5) N62 0.011(5) 0.015(5) 0.039(10) 0.003(4) 0.008(5) 0.000(4) C63 0.036(10) 0.009(6) 0.025(9) 0.004(5) 0.000(6) -0.001(5) C64 0.029(9) 0.043(8) 0.046(12) -0.009(6) 0.028(6) -0.014(6) N65 0.016(6) 0.022(5) 0.029(8) 0.002(4) 0.011(4) -0.000(4) C66 0.015(6) 0.022(6) 0.026(9) -0.006(5) -0.001(5) 0.003(5) C67 0.029(8) 0.045(8) 0.028(9) -0.004(5) -0.009(6) 0.015(6) N68 0.021(6) 0.015(5) 0.026(8) 0.004(4) 0.006(4) 0.002(4) C69 0.012(6) 0.028(6) 0.021(8) 0.009(4) 0.008(5) -0.008(5) C70 0.033(9) 0.037(7) 0.027(9) 0.009(5) 0.002(5) -0.001(5) N71 0.017(6) 0.019(5) 0.024(7) -0.004(4) 0.004(4) -0.010(4) C72 0.013(7) 0.026(6) 0.028(9) -0.008(5) -0.004(5) 0.000(5) C73 0.021(7) 0.044(8) 0.039(11) 0.008(5) 0.013(6) 0.014(6) N74 0.014(5) 0.028(6) 0.029(8) -0.000(4) -0.004(4) -0.007(4) C75 0.019(7) 0.014(6) 0.040(11) -0.006(4) 0.007(6) 0.000(5) C76 0.050(11) 0.047(8) 0.015(7) -0.007(6) 0.003(6) -0.010(5) B77 0.046(12) 0.024(8) 0.038(12) -0.001(7) -0.011(8) -0.020(7) F78 0.14(2) 0.142(11) 0.045(10) -0.052(7) -0.020(6) 0.016(6) F79 0.052(10) 0.038(5) 0.16(3) 0.001(4) 0.036(6) -0.017(5) F80 0.039(8) 0.084(7) 0.093(19) -0.016(4) -0.023(4) -0.000(5) F81 0.048(9) 0.068(6) 0.13(3) -0.006(4) 0.052(5) -0.042(5) B82 0.019(7) 0.036(8) 0.019(8) -0.004(6) 0.013(6) -0.008(6) F83 0.050(9) 0.047(5) 0.032(7) -0.012(3) 0.004(3) -0.014(3) F84 0.063(12) 0.048(5) 0.070(14) 0.006(4) -0.022(4) 0.019(4) F85 0.041(8) 0.044(5) 0.049(11) -0.017(3) 0.011(4) -0.011(3) F86 0.041(8) 0.050(5) 0.058(12) -0.000(3) 0.024(4) -0.014(4) B87 0.034(10) 0.028(8) 0.040(12) 0.005(6) 0.007(7) -0.002(7) F88 0.051(10) 0.036(4) 0.064(13) 0.001(3) 0.001(4) 0.002(4) F89 0.031(7) 0.045(5) 0.14(3) -0.014(4) 0.013(5) 0.019(5) F90 0.049(9) 0.056(5) 0.090(18) 0.008(4) 0.039(4) -0.003(4) F91 0.16(3) 0.093(8) 0.049(11) 0.033(6) -0.041(6) -0.023(5) B92 0.035(10) 0.009(6) 0.029(10) 0.007(6) -0.023(7) -0.002(5) F93 0.031(6) 0.049(5) 0.035(8) -0.003(3) 0.002(3) -0.013(3) F94 0.084(15) 0.047(5) 0.051(11) 0.004(4) -0.015(4) 0.013(4) F95 0.032(7) 0.045(5) 0.057(12) 0.000(3) 0.021(3) -0.019(4) F96 0.034(7) 0.040(4) 0.047(10) -0.019(3) 0.016(3) -0.005(3) B97 0.032(10) 0.032(8) 0.027(10) 0.003(6) 0.013(6) 0.007(6) F98 0.056(10) 0.046(5) 0.069(14) -0.015(4) 0.036(4) -0.007(4) F99 0.037(7) 0.028(4) 0.073(15) -0.005(3) 0.021(4) -0.008(3) F100 0.097(17) 0.107(8) 0.036(8) -0.025(5) 0.005(4) -0.017(4) F101 0.039(8) 0.056(5) 0.12(2) 0.014(4) 0.005(4) 0.004(5) B102 0.020(8) 0.038(9) 0.027(10) 0.003(6) 0.005(6) 0.010(6) F103 0.064(12) 0.034(5) 0.091(19) -0.002(4) -0.002(5) -0.014(4) F104 0.090(16) 0.072(7) 0.11(2) 0.051(5) -0.018(6) -0.041(5) F105 0.054(11) 0.070(7) 0.32(6) -0.014(5) 0.099(9) -0.040(8) F106 0.31(5) 0.129(11) 0.036(9) -0.102(10) -0.042(8) 0.019(6) # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_MSC95223 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C36 H37 B2 F8 Mo2 N9' _chemical_formula_moiety 'C36 H37 Mo2 N9 2+, 2(B F4 -)' _chemical_formula_weight 961.24 _cell_length_a 12.027(3) _cell_length_b 17.335(5) _cell_length_c 10.341(3) _cell_angle_alpha 91.758(14) _cell_angle_beta 109.715(16) _cell_angle_gamma 80.431(13) _cell_volume 2000.5(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 46 _cell_measurement_theta_min 9.66 _cell_measurement_theta_max 10.36 _cell_measurement_temperature 103 _exptl_crystal_colour red _exptl_crystal_description prism _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 0.7028 _exptl_absorpt_correction_type none _exptl_absorpt_process_details none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 103 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8745 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_full 0 _diffrn_measured_fraction_theta_max 1 _diffrn_measured_fraction_theta_full 0 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 2 _diffrn_standards_number 4 _diffrn_standards_decay_% 2.7 _diffrn_standards_interval_count 300 _reflns_number_total 7101 _reflns_number_gt 5960 _reflns_threshold_expression F>3.0\s(F) _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogen geom loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source MO Mo -1.825 0.688 'International Tables Vol. IV (1974) Table 2.2B' F F 0.014 0.01 'International Tables Vol. IV (1974) Table 2.2B' N N 0.004 0.003 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' B B 0 0.001 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_special_details ; The structure was solved by locating the two unique Mo atoms in a Patterson function (SHELXS-86). The remaining non-hydrogen atoms were located in several iterations of least-squares refinement followed by difference Fourier calculations. Hydrogen atoms were located in a later difference map ( at least one on each methyl group) and were then included in fixed idealized positions with isotropic thermal parameters fixed at one plus the isotropic equivalent of the parent atom. In the final cycles of refinement, the non-hydrogen atoms were refined using anisotropic thermal parameters to a final R(F) of 0.036 for the 488 total variables using the full unique data. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 7101 _refine_ls_number_parameters 488 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.4652E-6 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack ? _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.05F)^2^ _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_ref 0.0352 _refine_ls_goodness_of_fit_ref 0.9546 _refine_ls_shift/su_max 0.0146 _refine_diff_density_max 0.72 _refine_diff_density_min -0.50 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution SHELXS-86 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly Mo1 Mo 0.22803(3) 0.26086(2) 0.07935(3) 0.01229(13) Uani 1 0 . Mo2 Mo 0.39015(3) 0.25870(2) 0.03445(3) 0.01235(13) Uani 1 0 . N3 N 0.1541(3) 0.2001(2) -0.0978(3) 0.0153(13) Uani 1 0 . C4 C 0.2112(3) 0.1871(2) -0.1870(4) 0.0163(13) Uani 1 0 . N5 N 0.3203(3) 0.2053(2) -0.1565(3) 0.0150(13) Uani 1 0 . C6 C 0.0355(3) 0.1824(2) -0.1355(4) 0.0161(14) Uani 1 0 . C7 C -0.0562(4) 0.2202(2) -0.2456(4) 0.0274(14) Uani 1 0 . C8 C -0.1718(4) 0.2044(3) -0.2732(5) 0.0325(14) Uani 1 0 . C9 C -0.1950(3) 0.1514(3) -0.1921(4) 0.0270(16) Uani 1 0 . C10 C -0.1021(4) 0.1130(2) -0.0843(4) 0.0247(14) Uani 1 0 . C11 C 0.0128(3) 0.1282(2) -0.0537(4) 0.0194(14) Uani 1 0 . C12 C 0.3817(3) 0.1833(2) -0.2514(3) 0.0144(13) Uani 1 0 . C13 C 0.3853(3) 0.1083(2) -0.3044(4) 0.0199(14) Uani 1 0 . C14 C 0.4473(3) 0.0875(2) -0.3958(4) 0.0196(14) Uani 1 0 . C15 C 0.5043(3) 0.1410(2) -0.4352(4) 0.0221(14) Uani 1 0 . C16 C 0.5005(3) 0.2155(2) -0.3823(4) 0.0225(14) Uani 1 0 . C17 C 0.4405(3) 0.2367(2) -0.2909(4) 0.0196(14) Uani 1 0 . N18 N 0.2946(3) 0.1587(2) 0.2039(3) 0.0146(13) Uani 1 0 . C19 C 0.4041(3) 0.1227(2) 0.2137(4) 0.0163(13) Uani 1 0 . N20 N 0.4629(3) 0.1515(2) 0.1444(3) 0.0140(13) Uani 1 0 . C21 C 0.2318(3) 0.1255(2) 0.2783(4) 0.0174(13) Uani 1 0 . C22 C 0.1537(3) 0.1762(2) 0.3298(4) 0.0186(14) Uani 1 0 . C23 C 0.0944(3) 0.1469(2) 0.4063(4) 0.0200(14) Uani 1 0 . C24 C 0.1125(3) 0.0673(2) 0.4343(4) 0.0216(14) Uani 1 0 . C25 C 0.1856(3) 0.0166(2) 0.3783(4) 0.0222(14) Uani 1 0 . C26 C 0.2446(3) 0.0454(2) 0.3011(4) 0.0177(14) Uani 1 0 . C27 C 0.5827(3) 0.1113(2) 0.1656(4) 0.0181(14) Uani 1 0 . C28 C 0.6064(3) 0.0634(2) 0.0646(4) 0.0201(14) Uani 1 0 . C29 C 0.7218(4) 0.0247(2) 0.0853(4) 0.0230(14) Uani 1 0 . C30 C 0.8144(3) 0.0355(2) 0.2031(4) 0.0271(14) Uani 1 0 . C31 C 0.7913(3) 0.0848(3) 0.3021(4) 0.0259(14) Uani 1 0 . C32 C 0.6759(3) 0.1228(2) 0.2837(4) 0.0200(14) Uani 1 0 . N33 N 0.1129(3) 0.3645(2) -0.0357(3) 0.0174(13) Uani 1 0 . C34 C 0.0516(3) 0.4141(2) -0.1074(4) 0.0208(14) Uani 1 0 . C35 C -0.0257(4) 0.4775(3) -0.2011(4) 0.0320(16) Uani 1 0 . N36 N 0.2539(3) 0.3307(2) 0.2633(3) 0.0174(13) Uani 1 0 . C37 C 0.2617(3) 0.3631(2) 0.3632(4) 0.0179(14) Uani 1 0 . C38 C 0.2708(3) 0.4022(2) 0.4920(4) 0.0206(14) Uani 1 0 . N39 N 0.3510(3) 0.3726(2) -0.0694(3) 0.0167(13) Uani 1 0 . C40 C 0.3325(3) 0.4349(2) -0.1103(4) 0.0199(14) Uani 1 0 . C41 C 0.3053(4) 0.5156(2) -0.1615(5) 0.0334(16) Uani 1 0 . N42 N 0.4875(3) 0.3174(2) 0.2175(3) 0.0182(13) Uani 1 0 . C43 C 0.5406(3) 0.3505(2) 0.3079(4) 0.0176(14) Uani 1 0 . C44 C 0.6076(4) 0.3928(2) 0.4231(4) 0.0257(14) Uani 1 0 . N45 N 0.6000(3) 0.2588(2) 0.0158(3) 0.0230(13) Uani 1 0 . C46 C 0.6978(4) 0.2653(2) 0.0464(4) 0.0201(14) Uani 1 0 . C47 C 0.8233(4) 0.2739(3) 0.0896(5) 0.0316(18) Uani 1 0 . B48 B -0.0412(4) 0.3625(3) 0.4581(5) 0.024(2) Uani 1 0 . F49 F 0.0042(2) 0.3647(2) 0.3508(2) 0.0337(11) Uani 1 0 . F50 F -0.1077(2) 0.43477(10) 0.4664(3) 0.0358(13) Uani 1 0 . F51 F -0.1166(2) 0.3064(2) 0.4312(3) 0.0375(13) Uani 1 0 . F52 F 0.0519(2) 0.3442(2) 0.5812(3) 0.0381(11) Uani 1 0 . B53 B 0.3533(5) 0.5556(3) 0.2156(5) 0.029(2) Uani 1 0 . F54 F 0.2443(3) 0.5761(3) 0.1134(3) 0.0806(18) Uani 1 0 . F55 F 0.4310(3) 0.5136(2) 0.1555(3) 0.0485(14) Uani 1 0 . F56 F 0.3418(2) 0.50948(10) 0.3157(2) 0.0376(11) Uani 1 0 . F57 F 0.3996(5) 0.6199(2) 0.2726(4) 0.099(3) Uani 1 0 . H1 H 0.1747 0.1648 -0.2727 0.0287 Uiso 1 0 . H2 H -0.0409 0.2566 -0.3019 0.0386 Uiso 1 0 . H3 H -0.2355 0.2302 -0.3488 0.044 Uiso 1 0 . H4 H -0.2743 0.1416 -0.2107 0.0398 Uiso 1 0 . H5 H -0.1174 0.0754 -0.0302 0.0366 Uiso 1 0 . H6 H 0.076 0.1022 0.0222 0.032 Uiso 1 0 . H7 H 0.3458 0.0716 -0.2783 0.0321 Uiso 1 0 . H8 H 0.4505 0.0363 -0.4314 0.0332 Uiso 1 0 . H9 H 0.5459 0.1268 -0.4981 0.0353 Uiso 1 0 . H10 H 0.5395 0.2523 -0.4092 0.0342 Uiso 1 0 . H11 H 0.439 0.2877 -0.2546 0.0322 Uiso 1 0 . H12 H 0.4395 0.0767 0.2699 0.0284 Uiso 1 0 . H13 H 0.1415 0.2309 0.312 0.0307 Uiso 1 0 . H14 H 0.041 0.1816 0.4397 0.0328 Uiso 1 0 . H15 H 0.0754 0.0476 0.4912 0.0327 Uiso 1 0 . H16 H 0.1952 -0.0383 0.3932 0.0336 Uiso 1 0 . H17 H 0.2943 0.0102 0.2634 0.0302 Uiso 1 0 . H18 H 0.5437 0.0572 -0.0185 0.0318 Uiso 1 0 . H19 H 0.7373 -0.0096 0.0177 0.0358 Uiso 1 0 . H20 H 0.8935 0.0093 0.2163 0.0385 Uiso 1 0 . H21 H 0.855 0.0927 0.3832 0.0374 Uiso 1 0 . H22 H 0.6606 0.1568 0.3518 0.0322 Uiso 1 0 . H23 H 0.0047 0.525 -0.175 0.0446 Uiso 1 0 . H24 H -0.0278 0.4659 -0.2921 0.0446 Uiso 1 0 . H25 H -0.1043 0.483 -0.1969 0.0446 Uiso 1 0 . H26 H 0.3514 0.4089 0.5379 0.0337 Uiso 1 0 . H27 H 0.2206 0.4519 0.4737 0.0337 Uiso 1 0 . H28 H 0.2464 0.3713 0.5484 0.0337 Uiso 1 0 . H29 H 0.374 0.5297 -0.1743 0.0449 Uiso 1 0 . H30 H 0.2411 0.5207 -0.2467 0.0449 Uiso 1 0 . H31 H 0.2829 0.5492 -0.0969 0.0449 Uiso 1 0 . H32 H 0.6018 0.3741 0.5056 0.0374 Uiso 1 0 . H33 H 0.6893 0.3849 0.429 0.0374 Uiso 1 0 . H34 H 0.5758 0.447 0.4101 0.0374 Uiso 1 0 . H35 H 0.872 0.2237 0.1092 0.0449 Uiso 1 0 . H36 H 0.8378 0.2993 0.0181 0.0449 Uiso 1 0 . H37 H 0.8421 0.3044 0.1697 0.0449 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo1 0.0117(2) 0.0132(2) 0.0119(2) -0.00058(10) 0.00495(10) 0.00000(10) Mo2 0.0116(2) 0.0133(2) 0.0119(2) -0.00174(10) 0.00479(10) 0.00008(10) N3 0.012(2) 0.019(2) 0.015(2) -0.0034(10) 0.0056(10) -0.0003(10) C4 0.018(2) 0.016(2) 0.013(2) -0.003(2) 0.0028(10) -0.0013(10) N5 0.016(2) 0.018(2) 0.012(2) -0.0025(10) 0.0067(10) -0.0004(10) C6 0.014(2) 0.018(2) 0.019(2) -0.001(2) 0.008(2) -0.004(2) C7 0.021(2) 0.027(2) 0.027(2) -0.004(2) 0.004(2) 0.006(2) C8 0.021(2) 0.032(2) 0.032(2) -0.004(2) -0.004(2) 0.003(2) C9 0.015(2) 0.037(3) 0.031(2) -0.009(2) 0.007(2) -0.009(2) C10 0.028(2) 0.028(2) 0.021(2) -0.009(2) 0.013(2) -0.003(2) C11 0.021(2) 0.017(2) 0.016(2) -0.001(2) 0.003(2) -0.001(2) C12 0.011(2) 0.022(2) 0.008(2) -0.0009(10) 0.0022(10) 0.0000(10) C13 0.019(2) 0.021(2) 0.017(2) -0.003(2) 0.005(2) 0.000(2) C14 0.018(2) 0.024(2) 0.015(2) 0.003(2) 0.003(2) -0.004(2) C15 0.016(2) 0.037(2) 0.015(2) 0.001(2) 0.008(2) -0.003(2) C16 0.016(2) 0.028(2) 0.021(2) -0.003(2) 0.007(2) 0.004(2) C17 0.017(2) 0.020(2) 0.020(2) 0.000(2) 0.005(2) 0.001(2) N18 0.015(2) 0.016(2) 0.012(2) -0.0034(10) 0.0040(10) -0.0012(10) C19 0.016(2) 0.015(2) 0.014(2) -0.0021(10) 0.0016(10) 0.0019(10) N20 0.012(2) 0.015(2) 0.015(2) -0.0001(10) 0.0064(10) 0.0013(10) C21 0.014(2) 0.022(2) 0.012(2) -0.006(2) 0.0020(10) 0.0019(10) C22 0.018(2) 0.017(2) 0.020(2) -0.002(2) 0.007(2) 0.002(2) C23 0.015(2) 0.022(2) 0.024(2) 0.001(2) 0.008(2) -0.001(2) C24 0.016(2) 0.030(2) 0.016(2) -0.005(2) 0.006(2) 0.005(2) C25 0.021(2) 0.017(2) 0.026(2) -0.005(2) 0.008(2) 0.004(2) C26 0.016(2) 0.018(2) 0.018(2) 0.000(2) 0.006(2) 0.001(2) C27 0.014(2) 0.019(2) 0.021(2) -0.002(2) 0.009(2) 0.005(2) C28 0.020(2) 0.021(2) 0.020(2) -0.006(2) 0.009(2) 0.001(2) C29 0.024(2) 0.022(2) 0.027(2) -0.001(2) 0.015(2) -0.002(2) C30 0.016(2) 0.031(2) 0.031(2) 0.003(2) 0.011(2) 0.011(2) C31 0.016(2) 0.036(2) 0.020(2) -0.000(2) 0.005(2) 0.007(2) C32 0.021(2) 0.022(2) 0.018(2) -0.001(2) 0.010(2) 0.001(2) N33 0.018(2) 0.018(2) 0.015(2) -0.0015(10) 0.0061(10) 0.0008(10) C34 0.019(2) 0.024(2) 0.022(2) -0.001(2) 0.009(2) -0.004(2) C35 0.033(3) 0.028(2) 0.029(2) 0.012(2) 0.010(2) 0.011(2) N36 0.015(2) 0.018(2) 0.018(2) -0.0004(10) 0.0083(10) 0.0030(10) C37 0.014(2) 0.019(2) 0.019(2) -0.002(2) 0.006(2) 0.004(2) C38 0.023(2) 0.023(2) 0.016(2) -0.001(2) 0.008(2) -0.004(2) N39 0.015(2) 0.019(2) 0.015(2) -0.0022(10) 0.0052(10) 0.0010(10) C40 0.019(2) 0.027(2) 0.015(2) -0.002(2) 0.009(2) -0.002(2) C41 0.047(3) 0.021(2) 0.031(2) -0.001(2) 0.017(2) 0.005(2) N42 0.018(2) 0.019(2) 0.018(2) -0.0025(10) 0.0084(10) -0.0016(10) C43 0.017(2) 0.019(2) 0.019(2) -0.003(2) 0.010(2) 0.000(2) C44 0.027(2) 0.028(2) 0.020(2) -0.010(2) 0.006(2) -0.003(2) N45 0.018(2) 0.030(2) 0.024(2) -0.0023(10) 0.0108(10) -0.002(2) C46 0.028(2) 0.018(2) 0.017(2) 0.001(2) 0.012(2) -0.001(2) C47 0.024(2) 0.035(3) 0.036(3) -0.007(2) 0.008(2) -0.010(2) B48 0.022(3) 0.031(3) 0.019(3) 0.004(2) 0.011(2) 0.005(2) F49 0.035(2) 0.041(2) 0.0280(10) -0.0082(10) 0.0170(10) -0.0012(10) F50 0.038(2) 0.030(2) 0.039(2) 0.0081(10) 0.0115(10) -0.0055(10) F51 0.036(2) 0.037(2) 0.045(2) -0.0118(10) 0.0215(10) -0.0034(10) F52 0.0268(10) 0.047(2) 0.031(2) -0.0004(10) 0.0085(10) 0.0131(10) B53 0.038(3) 0.025(3) 0.023(3) -0.004(2) 0.013(2) -0.001(2) F54 0.049(2) 0.130(4) 0.047(2) 0.026(2) 0.023(2) 0.038(2) F55 0.053(2) 0.059(2) 0.037(2) 0.006(2) 0.023(2) 0.001(2) F56 0.051(2) 0.033(2) 0.0264(10) -0.0177(10) 0.0150(10) 0.0020(10) F57 0.209(6) 0.059(2) 0.057(2) -0.080(3) 0.084(3) -0.027(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag MO1 MO2 2.1457(7) . . no MO1 N3 2.086(3) . . no MO1 N18 2.100(3) . . no MO1 N33 2.181(3) . . no MO1 N36 2.183(3) . . no MO2 N5 2.118(3) . . no MO2 N20 2.105(3) . . no MO2 N39 2.180(3) . . no MO2 N42 2.185(3) . . no MO2 N45 2.595(3) . . no F49 B48 1.396(5) . . no F50 B48 1.388(5) . . no F51 B48 1.397(5) . . no F52 B48 1.386(5) . . no F54 B53 1.377(6) . . no F55 B53 1.389(6) . . no F56 B53 1.385(5) . . no F57 B53 1.357(6) . . no N3 C4 1.317(5) . . no N3 C6 1.429(4) . . no N5 C4 1.332(5) . . no N5 C12 1.424(4) . . no N18 C19 1.332(5) . . no N18 C21 1.434(4) . . no N20 C19 1.321(5) . . no N20 C27 1.440(4) . . no N33 C34 1.137(5) . . no N36 C37 1.144(5) . . no N39 C40 1.132(5) . . no N42 C43 1.139(5) . . no N45 C46 1.134(5) . . no C6 C7 1.379(5) . . no C6 C11 1.402(5) . . no C7 C8 1.394(6) . . no C8 C9 1.384(6) . . no C9 C10 1.375(6) . . no C10 C11 1.378(5) . . no C12 C13 1.394(5) . . no C12 C17 1.400(5) . . no C13 C14 1.395(5) . . no C14 C15 1.385(6) . . no C15 C16 1.387(6) . . no C16 C17 1.378(5) . . no C21 C22 1.404(5) . . no C21 C26 1.390(5) . . no C22 C23 1.385(5) . . no C23 C24 1.384(5) . . no C24 C25 1.392(5) . . no C25 C26 1.384(5) . . no C27 C28 1.389(5) . . no C27 C32 1.387(5) . . no C28 C29 1.386(5) . . no C29 C30 1.378(6) . . no C30 C31 1.383(6) . . no C31 C32 1.387(5) . . no C34 C35 1.459(5) . . no C37 C38 1.454(5) . . no C40 C41 1.456(6) . . no C43 C44 1.449(5) . . no C46 C47 1.456(6) . . no C4 H1 0.950(3) . . no C7 H2 0.950(4) . . no C8 H3 0.950(4) . . no C9 H4 0.950(4) . . no C10 H5 0.950(4) . . no C11 H6 0.950(4) . . no C13 H7 0.950(4) . . no C14 H8 0.950(4) . . no C15 H9 0.950(4) . . no C16 H10 0.950(4) . . no C17 H11 0.950(4) . . no C19 H12 0.950(3) . . no C22 H13 0.950(4) . . no C23 H14 0.950(4) . . no C24 H15 0.950(4) . . no C25 H16 0.950(4) . . no C26 H17 0.950(4) . . no C28 H18 0.950(4) . . no C29 H19 0.950(4) . . no C30 H20 0.950(4) . . no C31 H21 0.950(4) . . no C32 H22 0.950(4) . . no C35 H23 0.950(5) . . no C35 H24 0.950(4) . . no C35 H25 0.950(4) . . no C38 H26 0.950(4) . . no C38 H27 0.950(4) . . no C38 H28 0.950(4) . . no C41 H29 0.950(5) . . no C41 H30 0.950(5) . . no C41 H31 0.950(4) . . no C44 H32 0.950(4) . . no C44 H33 0.950(4) . . no C44 H34 0.950(4) . . no C47 H35 0.950(5) . . no C47 H36 0.950(5) . . no C47 H37 0.950(4) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag MO2 MO1 N3 91.68(8) . . . no MO2 MO1 N18 93.76(8) . . . no MO2 MO1 N33 102.75(8) . . . no MO2 MO1 N36 103.77(8) . . . no N3 MO1 N18 93.40(12) . . . no N3 MO1 N33 85.66(12) . . . no N3 MO1 N36 164.03(11) . . . no N18 MO1 N33 163.49(11) . . . no N18 MO1 N36 89.63(11) . . . no N33 MO1 N36 87.00(12) . . . no MO1 MO2 N5 92.14(8) . . . no MO1 MO2 N20 90.04(8) . . . no MO1 MO2 N39 99.95(8) . . . no MO1 MO2 N42 97.90(8) . . . no MO1 MO2 N45 172.16(8) . . . no N5 MO2 N20 94.00(12) . . . no N5 MO2 N39 90.55(12) . . . no N5 MO2 N42 169.71(11) . . . no N5 MO2 N45 95.32(11) . . . no N20 MO2 N39 168.87(11) . . . no N20 MO2 N42 88.28(12) . . . no N20 MO2 N45 87.04(11) . . . no N39 MO2 N42 85.51(12) . . . no N39 MO2 N45 82.42(11) . . . no N42 MO2 N45 74.76(11) . . . no MO1 N3 C4 119.0(2) . . . no MO1 N3 C6 121.8(2) . . . no C4 N3 C6 118.5(3) . . . no MO2 N5 C4 116.8(2) . . . no MO2 N5 C12 126.0(2) . . . no C4 N5 C12 117.1(3) . . . no MO1 N18 C19 116.5(2) . . . no MO1 N18 C21 125.2(2) . . . no C19 N18 C21 118.3(3) . . . no MO2 N20 C19 120.0(2) . . . no MO2 N20 C27 123.6(2) . . . no C19 N20 C27 115.8(3) . . . no MO1 N33 C34 173.0(3) . . . no MO1 N36 C37 173.9(3) . . . no MO2 N39 C40 173.0(3) . . . no MO2 N42 C43 175.8(3) . . . no MO2 N45 C46 159.8(3) . . . no N3 C4 N5 119.8(3) . . . no N3 C6 C7 121.2(3) . . . no N3 C6 C11 118.4(3) . . . no C7 C6 C11 120.3(3) . . . no C6 C7 C8 119.0(4) . . . no C7 C8 C9 120.9(4) . . . no C8 C9 C10 119.3(4) . . . no C9 C10 C11 121.0(4) . . . no C6 C11 C10 119.4(3) . . . no N5 C12 C13 120.6(3) . . . no N5 C12 C17 120.0(3) . . . no C13 C12 C17 119.4(3) . . . no C12 C13 C14 119.7(3) . . . no C13 C14 C15 120.4(4) . . . no C14 C15 C16 119.7(3) . . . no C15 C16 C17 120.5(4) . . . no C12 C17 C16 120.2(4) . . . no N18 C19 N20 119.3(3) . . . no N18 C21 C22 118.5(3) . . . no N18 C21 C26 122.8(3) . . . no C22 C21 C26 118.7(3) . . . no C21 C22 C23 120.5(3) . . . no C22 C23 C24 120.4(3) . . . no C23 C24 C25 119.3(3) . . . no C24 C25 C26 120.5(3) . . . no C21 C26 C25 120.5(3) . . . no N20 C27 C28 120.0(3) . . . no N20 C27 C32 120.3(3) . . . no C28 C27 C32 119.6(3) . . . no C27 C28 C29 119.8(4) . . . no C28 C29 C30 120.6(4) . . . no C29 C30 C31 119.5(4) . . . no C30 C31 C32 120.4(4) . . . no C27 C32 C31 119.9(4) . . . no N33 C34 C35 178.9(4) . . . no N36 C37 C38 178.2(4) . . . no N39 C40 C41 178.0(4) . . . no N42 C43 C44 179.8(4) . . . no N45 C46 C47 178.4(4) . . . no F49 B48 F50 109.5(4) . . . no F49 B48 F51 109.2(4) . . . no F49 B48 F52 110.0(3) . . . no F50 B48 F51 108.4(3) . . . no F50 B48 F52 109.6(4) . . . no F51 B48 F52 110.1(4) . . . no F54 B53 F55 107.4(4) . . . no F54 B53 F56 110.2(4) . . . no F54 B53 F57 111.3(5) . . . no F55 B53 F56 109.6(4) . . . no F55 B53 F57 108.2(4) . . . no F56 B53 F57 110.1(4) . . . no N3 C4 H1 120.1(4) . . . no N5 C4 H1 120.1(4) . . . no C6 C7 H2 120.5(4) . . . no C8 C7 H2 120.5(4) . . . no C7 C8 H3 119.5(4) . . . no C9 C8 H3 119.5(4) . . . no C8 C9 H4 120.3(4) . . . no C10 C9 H4 120.4(4) . . . no C9 C10 H5 119.5(4) . . . no C11 C10 H5 119.5(4) . . . no C6 C11 H6 120.3(4) . . . no C10 C11 H6 120.3(4) . . . no C12 C13 H7 120.1(4) . . . no C14 C13 H7 120.1(4) . . . no C13 C14 H8 119.8(4) . . . no C15 C14 H8 119.8(4) . . . no C14 C15 H9 120.1(4) . . . no C16 C15 H9 120.1(4) . . . no C15 C16 H10 119.7(4) . . . no C17 C16 H10 119.7(4) . . . no C12 C17 H11 119.9(4) . . . no C16 C17 H11 119.9(4) . . . no N18 C19 H12 120.3(3) . . . no N20 C19 H12 120.3(3) . . . no C21 C22 H13 119.8(4) . . . no C23 C22 H13 119.8(4) . . . no C22 C23 H14 119.8(4) . . . no C24 C23 H14 119.8(4) . . . no C23 C24 H15 120.4(4) . . . no C25 C24 H15 120.4(4) . . . no C24 C25 H16 119.7(4) . . . no C26 C25 H16 119.7(4) . . . no C21 C26 H17 119.7(4) . . . no C25 C26 H17 119.7(4) . . . no C27 C28 H18 120.1(4) . . . no C29 C28 H18 120.1(4) . . . no C28 C29 H19 119.7(4) . . . no C30 C29 H19 119.7(4) . . . no C29 C30 H20 120.3(4) . . . no C31 C30 H20 120.2(4) . . . no C30 C31 H21 119.8(4) . . . no C32 C31 H21 119.8(4) . . . no C27 C32 H22 120.0(4) . . . no C31 C32 H22 120.0(4) . . . no C34 C35 H23 109.4(4) . . . no C34 C35 H24 109.5(4) . . . no C34 C35 H25 109.5(4) . . . no H23 C35 H24 109.5(4) . . . no H23 C35 H25 109.5(4) . . . no H24 C35 H25 109.5(5) . . . no C37 C38 H26 109.5(3) . . . no C37 C38 H27 109.5(3) . . . no C37 C38 H28 109.5(3) . . . no H26 C38 H27 109.5(4) . . . no H26 C38 H28 109.5(4) . . . no H27 C38 H28 109.5(4) . . . no C40 C41 H29 109.5(4) . . . no C40 C41 H30 109.5(4) . . . no C40 C41 H31 109.5(4) . . . no H29 C41 H30 109.5(4) . . . no H29 C41 H31 109.5(5) . . . no H30 C41 H31 109.5(4) . . . no C43 C44 H32 109.5(4) . . . no C43 C44 H33 109.4(4) . . . no C43 C44 H34 109.5(4) . . . no H32 C44 H33 109.5(4) . . . no H32 C44 H34 109.5(4) . . . no H33 C44 H34 109.5(4) . . . no C46 C47 H35 109.5(4) . . . no C46 C47 H36 109.5(4) . . . no C46 C47 H37 109.5(4) . . . no H35 C47 H36 109.5(4) . . . no H35 C47 H37 109.5(4) . . . no H36 C47 H37 109.5(4) . . . no # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./