Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_rh2 _database_code_CSD 179026 _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Maxim N. Sokolov' 'Rita Hernandez-Molina' 'William Clegg' 'Vladimir P. Fedin' 'Alfredo Mederos' _publ_contact_author_name 'Dr Maxim Sokolov' _publ_contact_author_address ; Institute of Inorganic Chemistry pr. Lavrentyeva 3 Novosibirsk 630090 RUSSIAN FEDERATION ; _publ_contact_author_email CLUSTER@CHE.NSK.SU _publ_section_title ; Stabilization of the previously unknown tautomer HP(OH)2 of hypophosphorous acid as ligand; preparation of [W3(Ni(HP(OH)2))Q4(H2O)9]4+ (Q = S, Se) as well as corresponding As(OH)3 complexes ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H77 Cl4 N24 Ni O34 P Se4 W3' _chemical_formula_weight 2489.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.5728(5) _cell_length_b 18.5868(6) _cell_length_c 48.7091(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.391(2) _cell_angle_gamma 90.00 _cell_volume 14803.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 42315 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.57 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9616 _exptl_absorpt_coefficient_mu 7.132 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.209 _exptl_absorpt_correction_T_max 0.764 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 62151 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -64 _diffrn_reflns_limit_l_max 65 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.58 _reflns_number_total 17547 _reflns_number_gt 14922 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+928.1026P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000038(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 17547 _refine_ls_number_parameters 965 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1496 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.633 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.16480(2) 0.63046(2) 0.656335(8) 0.01557(10) Uani 1 1 d . . . O11 O 0.1572(4) 0.6463(4) 0.70092(16) 0.0214(16) Uani 1 1 d . . . O12 O 0.0727(4) 0.7237(4) 0.65578(16) 0.0232(17) Uani 1 1 d . . . O13 O 0.2480(5) 0.7197(4) 0.66933(17) 0.0261(17) Uani 1 1 d . . . W2 W 0.25739(2) 0.56577(2) 0.621466(8) 0.01683(10) Uani 1 1 d . . . O21 O 0.3566(4) 0.6416(4) 0.62612(16) 0.0220(16) Uani 1 1 d . . . O22 O 0.2855(5) 0.5744(6) 0.57906(17) 0.036(2) Uani 1 1 d . . . O23 O 0.3601(5) 0.4937(5) 0.62325(18) 0.0271(18) Uani 1 1 d . . . W3 W 0.17052(2) 0.48165(2) 0.652674(8) 0.01333(9) Uani 1 1 d . . . O31 O 0.2565(4) 0.3929(4) 0.66259(15) 0.0179(15) Uani 1 1 d . . . O32 O 0.0895(4) 0.3865(4) 0.64875(15) 0.0190(15) Uani 1 1 d . . . O33 O 0.1614(4) 0.4538(4) 0.69618(15) 0.0192(15) Uani 1 1 d . . . Ni Ni 0.09162(8) 0.56031(8) 0.61012(3) 0.0187(3) Uani 1 1 d . . . Se1 Se 0.16162(6) 0.66665(6) 0.60725(2) 0.0217(2) Uani 1 1 d . . . Se2 Se 0.17119(6) 0.46280(6) 0.60241(2) 0.0185(2) Uani 1 1 d . . . Se3 Se 0.04298(6) 0.55180(6) 0.65175(2) 0.0167(2) Uani 1 1 d . . . Se4 Se 0.28843(6) 0.55743(6) 0.67303(2) 0.0160(2) Uani 1 1 d . . . P P -0.01263(19) 0.5596(2) 0.57818(7) 0.0322(7) Uani 1 1 d . . . O41 O 0.0034(8) 0.5764(6) 0.5476(2) 0.055(3) Uani 1 1 d . . . O42 O -0.0675(6) 0.4871(7) 0.5753(3) 0.059(3) Uani 1 1 d . . . Cl1 Cl -0.09699(17) 0.53605(19) 0.70731(6) 0.0341(7) Uani 1 1 d . . . Cl2 Cl -0.0001(2) 0.3390(2) 0.59285(7) 0.0441(9) Uani 1 1 d . . . Cl3 Cl 0.27776(16) 0.86682(14) 0.64872(6) 0.0223(5) Uani 1 1 d . . . Cl4 Cl 0.2778(3) 0.2404(2) 0.63683(10) 0.0595(11) Uani 1 1 d . . . C401 C 0.4164(6) 0.2949(5) 0.7228(2) 0.0148(19) Uani 1 1 d . . . C402 C 0.4826(6) 0.3779(5) 0.6932(2) 0.0140(18) Uani 1 1 d . . . C403 C 0.5750(6) 0.4278(5) 0.6631(2) 0.0142(19) Uani 1 1 d . . . C404 C 0.5575(6) 0.5612(6) 0.6629(2) 0.0147(18) Uani 1 1 d . . . C405 C 0.5758(6) 0.6939(5) 0.66257(19) 0.0149(19) Uani 1 1 d . . . C406 C 0.4821(6) 0.7391(5) 0.6939(2) 0.0135(18) Uani 1 1 d . . . C407 C 0.4156(6) 0.8209(6) 0.7231(2) 0.0158(19) Uani 1 1 d . . . C408 C 0.6710(6) 0.3703(6) 0.7525(2) 0.017(2) Uani 1 1 d . . . C409 C 0.7411(6) 0.4328(5) 0.7187(2) 0.0164(19) Uani 1 1 d . . . C410 C 0.7303(6) 0.5633(6) 0.7243(2) 0.0168(19) Uani 1 1 d . . . C411 C 0.7451(6) 0.6934(5) 0.7156(2) 0.0151(19) Uani 1 1 d . . . C412 C 0.6734(6) 0.7501(5) 0.7510(2) 0.0152(19) Uani 1 1 d . . . C413 C 0.5707(6) 0.3028(5) 0.7238(2) 0.0133(18) Uani 1 1 d . . . C414 C 0.6219(6) 0.3466(5) 0.7052(2) 0.0155(19) Uani 1 1 d . . . C415 C 0.6899(6) 0.5184(5) 0.67906(19) 0.0128(18) Uani 1 1 d . . . C416 C 0.6904(6) 0.6030(5) 0.6783(2) 0.0143(19) Uani 1 1 d . . . C417 C 0.6198(6) 0.7759(5) 0.7046(2) 0.0131(18) Uani 1 1 d . . . C418 C 0.5678(6) 0.8143(5) 0.7240(2) 0.0149(19) Uani 1 1 d . . . N401 N 0.4883(5) 0.3311(5) 0.71561(18) 0.0152(16) Uani 1 1 d . . . N402 N 0.5609(5) 0.3919(4) 0.68847(17) 0.0141(16) Uani 1 1 d . . . N403 N 0.6052(5) 0.5011(4) 0.66718(17) 0.0120(16) Uani 1 1 d . . . N404 N 0.6054(5) 0.6200(5) 0.66796(19) 0.0170(17) Uani 1 1 d . . . N405 N 0.5599(5) 0.7310(5) 0.68737(18) 0.0174(17) Uani 1 1 d . . . N406 N 0.4864(5) 0.7836(4) 0.71658(17) 0.0126(16) Uani 1 1 d . . . N407 N 0.6083(5) 0.3224(5) 0.75194(17) 0.0156(17) Uani 1 1 d . . . N408 N 0.6790(5) 0.3862(4) 0.72572(17) 0.0148(16) Uani 1 1 d . . . N409 N 0.7101(5) 0.5025(4) 0.70876(17) 0.0137(16) Uani 1 1 d . . . N410 N 0.7182(5) 0.6222(4) 0.70701(18) 0.0160(17) Uani 1 1 d . . . N411 N 0.6795(5) 0.7367(5) 0.72384(18) 0.0167(17) Uani 1 1 d . . . N412 N 0.6098(5) 0.7971(4) 0.75152(18) 0.0158(17) Uani 1 1 d . . . O402 O 0.4203(4) 0.4034(4) 0.68027(16) 0.0206(16) Uani 1 1 d . . . O404 O 0.4832(4) 0.5621(4) 0.65402(16) 0.0194(15) Uani 1 1 d . . . O406 O 0.4199(4) 0.7136(4) 0.68052(15) 0.0186(15) Uani 1 1 d . . . O408 O 0.7127(5) 0.3925(5) 0.77384(16) 0.0259(17) Uani 1 1 d . . . O410 O 0.7560(5) 0.5660(4) 0.74925(15) 0.0200(15) Uani 1 1 d . . . O412 O 0.7192(5) 0.7273(4) 0.77160(15) 0.0220(16) Uani 1 1 d . . . C501 C 0.4569(7) 0.2316(6) 0.5142(2) 0.021(2) Uani 1 1 d . . . C502 C 0.5331(7) 0.3057(6) 0.5515(2) 0.021(2) Uani 1 1 d . . . C503 C 0.6351(7) 0.3557(6) 0.5894(2) 0.022(2) Uani 1 1 d . . . C504 C 0.5983(7) 0.4842(6) 0.5918(2) 0.023(2) Uani 1 1 d . . . C505 C 0.5982(7) 0.6171(7) 0.5968(2) 0.026(2) Uani 1 1 d . . . C506 C 0.4839(7) 0.6651(6) 0.5619(2) 0.022(2) Uani 1 1 d . . . C507 C 0.3960(7) 0.7444(6) 0.5303(2) 0.022(2) Uani 1 1 d . . . C508 C 0.6975(7) 0.3301(6) 0.5038(2) 0.022(2) Uani 1 1 d . . . C509 C 0.7802(7) 0.3862(6) 0.5455(2) 0.023(2) Uani 1 1 d . . . C510 C 0.7598(7) 0.5178(7) 0.5435(2) 0.026(2) Uani 1 1 d . . . C511 C 0.7473(7) 0.6460(6) 0.5544(3) 0.028(3) Uani 1 1 d . . . C512 C 0.6490(7) 0.6942(6) 0.5152(2) 0.021(2) Uani 1 1 d . . . C513 C 0.6131(7) 0.2483(6) 0.5229(2) 0.022(2) Uani 1 1 d . . . C514 C 0.6703(6) 0.2879(6) 0.5467(2) 0.021(2) Uani 1 1 d . . . C515 C 0.7319(7) 0.4602(6) 0.5836(2) 0.021(2) Uani 1 1 d . . . C516 C 0.7220(7) 0.5424(6) 0.5867(2) 0.020(2) Uani 1 1 d . . . C517 C 0.6152(7) 0.7110(6) 0.5597(2) 0.020(2) Uani 1 1 d . . . C518 C 0.5513(6) 0.7494(6) 0.5380(2) 0.021(2) Uani 1 1 d . . . N501 N 0.5315(5) 0.2666(5) 0.52766(19) 0.0224(19) Uani 1 1 d . . . N502 N 0.6117(6) 0.3229(5) 0.56199(19) 0.024(2) Uani 1 1 d . . . N503 N 0.6540(6) 0.4311(5) 0.5881(2) 0.0211(19) Uani 1 1 d . . . N504 N 0.6365(6) 0.5505(5) 0.5897(2) 0.024(2) Uani 1 1 d . . . N505 N 0.5660(6) 0.6593(5) 0.5725(2) 0.024(2) Uani 1 1 d . . . N506 N 0.4746(6) 0.7128(5) 0.54053(19) 0.0218(19) Uani 1 1 d . . . N507 N 0.6367(6) 0.2791(5) 0.4979(2) 0.024(2) Uani 1 1 d . . . N508 N 0.7160(6) 0.3372(5) 0.5321(2) 0.024(2) Uani 1 1 d . . . N509 N 0.7480(6) 0.4514(5) 0.55535(19) 0.0225(19) Uani 1 1 d . . . N510 N 0.7439(6) 0.5701(5) 0.5610(2) 0.026(2) Uani 1 1 d . . . N511 N 0.6685(6) 0.6759(5) 0.5425(2) 0.025(2) Uani 1 1 d . . . N512 N 0.5795(6) 0.7357(5) 0.51192(19) 0.0208(19) Uani 1 1 d . . . O502 O 0.4725(5) 0.3217(5) 0.56234(17) 0.0258(17) Uani 1 1 d . . . O504 O 0.5305(5) 0.4743(5) 0.59743(17) 0.0278(18) Uani 1 1 d . . . O506 O 0.4296(5) 0.6321(5) 0.57076(18) 0.033(2) Uani 1 1 d . . . O508 O 0.7306(5) 0.3609(5) 0.48649(18) 0.0316(19) Uani 1 1 d . . . O510 O 0.7836(5) 0.5253(5) 0.52108(19) 0.034(2) Uani 1 1 d . . . O512 O 0.6880(5) 0.6780(5) 0.49671(19) 0.035(2) Uani 1 1 d . . . O601 O 0.362(3) 0.4938(11) 0.5239(5) 0.29(2) Uani 1 1 d . . . O602 O -0.0401(8) 0.7622(10) 0.6146(3) 0.103(7) Uani 1 1 d . . . O603 O -0.0421(7) 0.4215(6) 0.5162(2) 0.048(3) Uani 1 1 d . . . O604 O 0.3652(6) 0.4248(6) 0.5775(2) 0.053(3) Uani 1 1 d . . . O605 O 0.2475(8) 0.3256(6) 0.5513(2) 0.058(3) Uani 1 1 d . . . O606 O 0.1365(7) 0.4144(6) 0.5198(2) 0.049(3) Uani 1 1 d . . . O607 O -0.0612(7) 0.6874(6) 0.6790(2) 0.049(3) Uani 1 1 d . . . O608 O 0.3426(5) 0.7693(5) 0.60473(19) 0.0314(19) Uani 1 1 d . . . O609 O 0.1586(7) 0.5533(6) 0.5380(2) 0.048(3) Uani 1 1 d . . . O610 O -0.0410(5) 0.4021(5) 0.67290(17) 0.0283(18) Uani 1 1 d . . . O611 O 0.0839(5) 0.5428(5) 0.72615(17) 0.0294(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01337(18) 0.0182(2) 0.01354(19) 0.00224(15) -0.00257(14) -0.00265(15) O11 0.019(4) 0.025(4) 0.020(4) -0.002(3) 0.000(3) 0.001(3) O12 0.018(4) 0.033(4) 0.018(4) -0.018(3) 0.002(3) -0.008(3) O13 0.024(4) 0.025(4) 0.027(4) 0.003(3) -0.004(3) -0.011(3) W2 0.01152(18) 0.0254(2) 0.01317(19) 0.00477(16) 0.00094(14) -0.00545(15) O21 0.014(3) 0.032(4) 0.020(4) 0.010(3) 0.002(3) -0.007(3) O22 0.027(4) 0.064(6) 0.019(4) 0.014(4) 0.007(3) -0.011(4) O23 0.020(4) 0.031(4) 0.031(5) -0.002(4) 0.007(3) -0.005(3) W3 0.00997(17) 0.01839(19) 0.01124(18) 0.00334(14) 0.00059(13) -0.00252(14) O31 0.012(3) 0.028(4) 0.013(3) -0.001(3) 0.002(3) -0.001(3) O32 0.013(3) 0.024(4) 0.018(4) 0.007(3) -0.003(3) -0.006(3) O33 0.017(3) 0.027(4) 0.013(3) 0.006(3) 0.003(3) -0.001(3) Ni 0.0143(6) 0.0260(7) 0.0145(6) 0.0045(5) -0.0017(5) -0.0038(5) Se1 0.0197(5) 0.0256(5) 0.0177(5) 0.0098(4) -0.0032(4) -0.0057(4) Se2 0.0155(5) 0.0264(5) 0.0134(5) 0.0001(4) 0.0020(4) -0.0047(4) Se3 0.0115(4) 0.0231(5) 0.0151(5) 0.0023(4) 0.0007(3) -0.0015(4) Se4 0.0111(4) 0.0220(5) 0.0138(4) 0.0040(4) -0.0016(3) -0.0034(4) P 0.0256(15) 0.0382(18) 0.0281(16) -0.0007(14) -0.0096(12) 0.0020(14) O41 0.075(8) 0.061(7) 0.023(5) 0.008(5) -0.006(5) 0.015(6) O42 0.035(6) 0.061(7) 0.073(8) -0.012(6) -0.015(5) -0.012(5) Cl1 0.0185(12) 0.059(2) 0.0265(14) -0.0056(14) 0.0079(11) -0.0065(13) Cl2 0.051(2) 0.053(2) 0.0306(17) -0.0170(15) 0.0156(15) -0.0263(17) Cl3 0.0211(12) 0.0211(12) 0.0243(13) -0.0011(10) 0.0025(10) 0.0002(10) Cl4 0.067(3) 0.048(2) 0.065(3) -0.004(2) 0.015(2) -0.009(2) C401 0.014(4) 0.016(5) 0.015(5) -0.002(4) 0.004(4) -0.008(4) C402 0.014(4) 0.014(5) 0.013(4) -0.003(4) 0.001(4) 0.000(4) C403 0.019(5) 0.015(5) 0.009(4) -0.002(4) 0.004(4) -0.004(4) C404 0.013(4) 0.021(5) 0.011(4) 0.002(4) 0.003(3) -0.002(4) C405 0.016(5) 0.021(5) 0.007(4) 0.003(4) -0.002(3) 0.006(4) C406 0.011(4) 0.012(4) 0.016(5) 0.004(4) -0.002(4) 0.000(3) C407 0.010(4) 0.022(5) 0.015(5) -0.002(4) 0.001(4) 0.004(4) C408 0.016(5) 0.017(5) 0.017(5) -0.004(4) 0.000(4) 0.003(4) C409 0.014(4) 0.016(5) 0.020(5) 0.001(4) 0.004(4) 0.002(4) C410 0.009(4) 0.019(5) 0.023(5) -0.004(4) 0.004(4) 0.001(4) C411 0.010(4) 0.016(5) 0.018(5) -0.005(4) -0.001(4) -0.001(4) C412 0.014(4) 0.013(4) 0.019(5) -0.003(4) 0.001(4) -0.005(4) C413 0.016(5) 0.013(4) 0.010(4) 0.001(3) 0.000(4) 0.002(4) C414 0.013(4) 0.018(5) 0.017(5) -0.001(4) 0.006(4) 0.002(4) C415 0.012(4) 0.013(4) 0.012(4) -0.002(4) -0.003(3) -0.003(3) C416 0.010(4) 0.011(4) 0.022(5) 0.002(4) 0.003(4) -0.003(3) C417 0.012(4) 0.013(4) 0.013(4) -0.003(4) -0.002(3) -0.002(3) C418 0.011(4) 0.015(5) 0.018(5) 0.001(4) 0.002(4) -0.003(4) N401 0.011(4) 0.017(4) 0.018(4) -0.001(3) 0.002(3) -0.005(3) N402 0.013(4) 0.017(4) 0.012(4) -0.004(3) -0.001(3) -0.003(3) N403 0.011(4) 0.008(4) 0.016(4) 0.000(3) -0.002(3) -0.003(3) N404 0.010(4) 0.017(4) 0.024(5) 0.000(3) 0.002(3) -0.005(3) N405 0.016(4) 0.022(4) 0.015(4) -0.001(3) 0.005(3) -0.005(3) N406 0.008(4) 0.015(4) 0.015(4) -0.001(3) 0.002(3) 0.000(3) N407 0.016(4) 0.022(4) 0.008(4) -0.001(3) -0.001(3) -0.005(3) N408 0.017(4) 0.015(4) 0.011(4) 0.000(3) -0.001(3) -0.004(3) N409 0.013(4) 0.011(4) 0.016(4) 0.003(3) 0.000(3) 0.003(3) N410 0.016(4) 0.014(4) 0.016(4) -0.001(3) -0.004(3) 0.002(3) N411 0.012(4) 0.017(4) 0.020(4) 0.001(3) 0.001(3) 0.004(3) N412 0.011(4) 0.014(4) 0.022(5) 0.000(3) 0.003(3) 0.003(3) O402 0.014(3) 0.022(4) 0.023(4) 0.010(3) -0.002(3) 0.004(3) O404 0.012(3) 0.020(4) 0.025(4) -0.004(3) -0.003(3) 0.002(3) O406 0.015(3) 0.023(4) 0.017(4) -0.002(3) 0.002(3) 0.003(3) O408 0.022(4) 0.038(5) 0.015(4) -0.003(3) -0.005(3) -0.010(3) O410 0.025(4) 0.022(4) 0.011(3) -0.001(3) -0.002(3) 0.003(3) O412 0.020(4) 0.027(4) 0.017(4) 0.001(3) -0.002(3) 0.004(3) C501 0.022(5) 0.022(5) 0.018(5) 0.003(4) 0.000(4) -0.009(4) C502 0.029(6) 0.013(5) 0.021(5) 0.011(4) 0.006(4) 0.006(4) C503 0.029(6) 0.023(6) 0.014(5) 0.002(4) 0.005(4) -0.008(4) C504 0.027(6) 0.029(6) 0.013(5) 0.007(4) 0.000(4) -0.003(5) C505 0.033(6) 0.031(6) 0.018(5) 0.007(5) 0.014(5) -0.001(5) C506 0.021(5) 0.029(6) 0.018(5) -0.002(4) 0.003(4) -0.002(4) C507 0.020(5) 0.034(6) 0.015(5) -0.001(4) 0.004(4) 0.001(4) C508 0.020(5) 0.022(5) 0.025(6) 0.006(4) 0.007(4) 0.004(4) C509 0.021(5) 0.018(5) 0.030(6) 0.008(4) 0.006(4) 0.000(4) C510 0.017(5) 0.032(6) 0.029(6) 0.016(5) 0.006(4) 0.007(5) C511 0.022(5) 0.018(5) 0.045(7) 0.014(5) 0.011(5) -0.001(4) C512 0.024(5) 0.022(5) 0.019(5) 0.003(4) 0.003(4) -0.004(4) C513 0.026(6) 0.023(5) 0.016(5) 0.005(4) 0.005(4) 0.001(4) C514 0.016(5) 0.026(6) 0.019(5) 0.007(4) 0.001(4) 0.000(4) C515 0.021(5) 0.017(5) 0.023(5) 0.005(4) 0.004(4) 0.000(4) C516 0.023(5) 0.019(5) 0.021(5) 0.005(4) 0.009(4) -0.002(4) C517 0.023(5) 0.020(5) 0.017(5) 0.001(4) 0.005(4) -0.001(4) C518 0.014(5) 0.030(6) 0.018(5) -0.001(4) 0.004(4) -0.002(4) N501 0.016(4) 0.032(5) 0.021(5) 0.001(4) 0.008(4) -0.001(4) N502 0.020(4) 0.034(5) 0.017(5) 0.006(4) 0.005(4) 0.003(4) N503 0.023(4) 0.017(4) 0.025(5) 0.004(4) 0.010(4) 0.000(4) N504 0.023(5) 0.024(5) 0.027(5) 0.005(4) 0.009(4) 0.000(4) N505 0.021(5) 0.027(5) 0.026(5) 0.005(4) 0.008(4) -0.006(4) N506 0.021(4) 0.026(5) 0.020(5) 0.005(4) 0.008(4) -0.003(4) N507 0.018(4) 0.033(5) 0.021(5) 0.003(4) 0.005(4) -0.002(4) N508 0.024(5) 0.028(5) 0.021(5) 0.006(4) 0.005(4) -0.005(4) N509 0.022(4) 0.025(5) 0.020(5) -0.003(4) 0.003(4) 0.000(4) N510 0.025(5) 0.025(5) 0.030(5) 0.009(4) 0.013(4) -0.001(4) N511 0.021(5) 0.030(5) 0.025(5) 0.007(4) 0.007(4) -0.001(4) N512 0.023(5) 0.023(5) 0.018(4) 0.003(4) 0.006(4) 0.002(4) O502 0.022(4) 0.032(4) 0.026(4) -0.002(3) 0.008(3) -0.001(3) O504 0.025(4) 0.034(5) 0.026(4) 0.002(4) 0.011(3) -0.004(4) O506 0.028(4) 0.042(5) 0.032(5) 0.004(4) 0.016(4) -0.013(4) O508 0.030(4) 0.039(5) 0.027(4) 0.009(4) 0.008(4) -0.008(4) O510 0.035(5) 0.034(5) 0.035(5) 0.016(4) 0.017(4) 0.003(4) O512 0.030(5) 0.049(6) 0.031(5) -0.002(4) 0.016(4) 0.006(4) O601 0.61(6) 0.071(14) 0.105(17) 0.000(12) -0.17(3) -0.01(2) O602 0.057(8) 0.172(17) 0.085(11) 0.092(11) 0.024(8) 0.032(10) O603 0.059(7) 0.040(6) 0.047(6) -0.006(5) 0.014(5) -0.005(5) O604 0.037(6) 0.064(7) 0.060(7) -0.024(6) 0.012(5) 0.010(5) O605 0.072(8) 0.053(7) 0.057(7) -0.013(6) 0.034(6) -0.018(6) O606 0.063(7) 0.049(6) 0.040(6) -0.010(5) 0.022(5) -0.023(5) O607 0.061(7) 0.040(6) 0.049(6) -0.008(5) 0.020(5) 0.011(5) O608 0.026(4) 0.032(5) 0.036(5) 0.003(4) 0.005(4) 0.002(4) O609 0.070(7) 0.049(6) 0.025(5) 0.007(4) 0.008(5) -0.011(5) O610 0.022(4) 0.042(5) 0.022(4) 0.004(4) 0.008(3) -0.006(4) O611 0.020(4) 0.045(5) 0.024(4) 0.001(4) 0.005(3) -0.001(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 W1 O11 2.216(8) . ? W1 O12 2.307(8) . ? W1 O13 2.184(8) . ? W1 W2 2.7451(6) . ? W1 W3 2.7742(6) . ? W1 Ni 2.7107(14) . ? W1 Se1 2.4760(11) . ? W1 Se3 2.4731(11) . ? W1 Se4 2.4815(11) . ? W2 O21 2.150(7) . ? W2 O22 2.196(8) . ? W2 O23 2.156(8) . ? W2 W3 2.7463(5) . ? W2 Ni 2.7145(13) . ? W2 Se1 2.4812(12) . ? W2 Se2 2.4763(11) . ? W2 Se4 2.4853(10) . ? W3 O31 2.183(7) . ? W3 O32 2.210(7) . ? W3 O33 2.211(7) . ? W3 Ni 2.6943(14) . ? W3 Se2 2.4749(11) . ? W3 Se3 2.4777(11) . ? W3 Se4 2.4805(10) . ? Ni Se1 2.3077(17) . ? Ni Se2 2.3077(18) . ? Ni Se3 2.3065(16) . ? Ni P 2.128(3) . ? P O41 1.588(11) . ? P O42 1.618(12) . ? C401 N401 1.460(12) . ? C401 N407 1.453(12) 2_656 ? C402 N401 1.387(13) . ? C402 N402 1.378(12) . ? C402 O402 1.214(12) . ? C403 N402 1.458(12) . ? C403 N403 1.453(12) . ? C404 N403 1.364(13) . ? C404 N404 1.350(13) . ? C404 O404 1.237(11) . ? C405 N404 1.467(13) . ? C405 N405 1.452(13) . ? C406 N405 1.385(12) . ? C406 N406 1.374(13) . ? C406 O406 1.221(12) . ? C407 N406 1.444(12) . ? C407 N412 1.439(13) 2_656 ? C408 N407 1.365(13) . ? C408 N408 1.366(13) . ? C408 O408 1.221(12) . ? C409 N408 1.430(12) . ? C409 N409 1.448(12) . ? C410 N409 1.372(13) . ? C410 N410 1.377(13) . ? C410 O410 1.219(12) . ? C411 N410 1.437(12) . ? C411 N411 1.459(12) . ? C412 N411 1.368(13) . ? C412 N412 1.372(12) . ? C412 O412 1.229(12) . ? C413 C414 1.565(13) . ? C413 N401 1.457(12) . ? C413 N407 1.456(12) . ? C414 N402 1.459(13) . ? C414 N408 1.458(13) . ? C415 C416 1.573(13) . ? C415 N403 1.464(11) . ? C415 N409 1.461(12) . ? C416 N404 1.452(12) . ? C416 N410 1.444(13) . ? C417 C418 1.551(13) . ? C417 N405 1.454(12) . ? C417 N411 1.444(12) . ? C418 N406 1.455(12) . ? C418 N412 1.443(13) . ? N407 C401 1.453(12) 2_656 ? N412 C407 1.439(13) 2_656 ? C501 N501 1.455(13) . ? C501 N512 1.450(14) 5_666 ? C502 N501 1.368(14) . ? C502 N502 1.358(15) . ? C502 O502 1.244(13) . ? C503 N502 1.462(14) . ? C503 N503 1.441(14) . ? C504 N503 1.382(15) . ? C504 N504 1.398(14) . ? C504 O504 1.213(13) . ? C505 N504 1.456(15) . ? C505 N505 1.449(15) . ? C506 N505 1.378(14) . ? C506 N506 1.358(14) . ? C506 O506 1.224(13) . ? C507 N506 1.441(14) . ? C507 N507 1.457(14) 5_666 ? C508 N507 1.379(15) . ? C508 N508 1.369(15) . ? C508 O508 1.223(13) . ? C509 N508 1.469(15) . ? C509 N509 1.438(14) . ? C510 N509 1.390(15) . ? C510 N510 1.346(16) . ? C510 O510 1.229(14) . ? C511 N510 1.450(14) . ? C511 N511 1.451(15) . ? C512 N511 1.358(14) . ? C512 N512 1.374(14) . ? C512 O512 1.228(13) . ? C513 C514 1.559(16) . ? C513 N501 1.450(14) . ? C513 N507 1.455(13) . ? C514 N502 1.468(14) . ? C514 N508 1.446(13) . ? C515 C516 1.547(15) . ? C515 N503 1.449(13) . ? C515 N509 1.455(14) . ? C516 N504 1.457(14) . ? C516 N510 1.452(13) . ? C517 C518 1.541(15) . ? C517 N505 1.464(13) . ? C517 N511 1.467(14) . ? C518 N506 1.465(13) . ? C518 N512 1.447(13) . ? N507 C507 1.457(14) 5_666 ? N512 C501 1.450(14) 5_666 ? 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 O11 W1 O12 76.6(3) . . ? O11 W1 O13 75.5(3) . . ? O11 W1 W2 142.33(19) . . ? O11 W1 W3 101.7(2) . . ? O11 W1 Ni 142.1(2) . . ? O11 W1 Se1 156.2(2) . . ? O11 W1 Se3 89.5(2) . . ? O11 W1 Se4 85.83(19) . . ? O12 W1 O13 79.5(3) . . ? O12 W1 W2 139.2(2) . . ? O12 W1 W3 141.06(19) . . ? O12 W1 Ni 98.40(18) . . ? O12 W1 Se1 82.8(2) . . ? O12 W1 Se3 85.08(19) . . ? O12 W1 Se4 157.55(18) . . ? O13 W1 W2 97.0(2) . . ? O13 W1 W3 138.5(2) . . ? O13 W1 Ni 141.4(2) . . ? O13 W1 Se1 89.2(2) . . ? O13 W1 Se3 160.5(2) . . ? O13 W1 Se4 82.6(2) . . ? W2 W1 W3 59.677(15) . . ? W2 W1 Ni 59.67(3) . . ? W2 W1 Se1 56.46(3) . . ? W2 W1 Se3 102.46(3) . . ? W2 W1 Se4 56.51(3) . . ? W3 W1 Ni 58.83(3) . . ? W3 W1 Se1 101.79(3) . . ? W3 W1 Se3 56.00(3) . . ? W3 W1 Se4 55.99(3) . . ? Ni W1 Se1 52.60(4) . . ? Ni W1 Se3 52.60(4) . . ? Ni W1 Se4 104.05(4) . . ? Se1 W1 Se3 100.66(4) . . ? Se1 W1 Se4 110.58(4) . . ? Se3 W1 Se4 108.93(4) . . ? W1 W2 O21 98.2(2) . . ? W1 W2 O22 140.9(3) . . ? W1 W2 O23 139.8(2) . . ? W1 W2 W3 60.688(15) . . ? W1 W2 Ni 59.53(3) . . ? W1 W2 Se1 56.28(3) . . ? W1 W2 Se2 102.93(3) . . ? W1 W2 Se4 56.38(3) . . ? O21 W2 O22 77.0(3) . . ? O21 W2 O23 79.5(3) . . ? O21 W2 W3 140.9(2) . . ? O21 W2 Ni 141.0(2) . . ? O21 W2 Se1 88.7(2) . . ? O21 W2 Se2 158.6(2) . . ? O21 W2 Se4 84.6(2) . . ? O22 W2 O23 78.2(3) . . ? O22 W2 W3 140.6(3) . . ? O22 W2 Ni 100.0(2) . . ? O22 W2 Se1 84.6(3) . . ? O22 W2 Se2 84.4(3) . . ? O22 W2 Se4 156.1(2) . . ? O23 W2 W3 96.1(2) . . ? O23 W2 Ni 138.7(2) . . ? O23 W2 Se1 161.0(2) . . ? O23 W2 Se2 86.5(2) . . ? O23 W2 Se4 83.6(2) . . ? W3 W2 Ni 59.12(3) . . ? W3 W2 Se1 102.44(3) . . ? W3 W2 Se2 56.29(3) . . ? W3 W2 Se4 56.34(3) . . ? Ni W2 Se1 52.50(4) . . ? Ni W2 Se2 52.55(4) . . ? Ni W2 Se4 103.83(4) . . ? Se1 W2 Se2 100.12(4) . . ? Se1 W2 Se4 110.28(4) . . ? Se2 W2 Se4 110.01(4) . . ? W1 W3 W2 59.635(15) . . ? W1 W3 O31 140.12(19) . . ? W1 W3 O32 140.98(19) . . ? W1 W3 O33 99.4(2) . . ? W1 W3 Ni 59.41(3) . . ? W1 W3 Se2 102.15(3) . . ? W1 W3 Se3 55.84(3) . . ? W1 W3 Se4 56.02(3) . . ? W2 W3 O31 99.81(19) . . ? W2 W3 O32 140.69(19) . . ? W2 W3 O33 142.00(19) . . ? W2 W3 Ni 59.85(3) . . ? W2 W3 Se2 56.34(3) . . ? W2 W3 Se3 102.30(3) . . ? W2 W3 Se4 56.51(3) . . ? O31 W3 O32 77.3(3) . . ? O31 W3 O33 75.8(3) . . ? O31 W3 Ni 142.94(19) . . ? O31 W3 Se2 90.22(18) . . ? O31 W3 Se3 157.88(19) . . ? O31 W3 Se4 84.10(19) . . ? O32 W3 O33 76.1(3) . . ? O32 W3 Ni 98.97(18) . . ? O32 W3 Se2 84.36(19) . . ? O32 W3 Se3 85.14(19) . . ? O32 W3 Se4 156.47(18) . . ? O33 W3 Ni 139.82(19) . . ? O33 W3 Se2 158.0(2) . . ? O33 W3 Se3 87.07(19) . . ? O33 W3 Se4 85.55(19) . . ? Ni W3 Se2 52.82(4) . . ? Ni W3 Se3 52.77(4) . . ? Ni W3 Se4 104.55(4) . . ? Se2 W3 Se3 101.42(4) . . ? Se2 W3 Se4 110.21(4) . . ? Se3 W3 Se4 108.81(4) . . ? W1 Ni W2 60.80(3) . . ? W1 Ni W3 61.76(3) . . ? W1 Ni Se1 58.47(4) . . ? W1 Ni Se2 108.83(5) . . ? W1 Ni Se3 58.40(4) . . ? W1 Ni P 144.10(12) . . ? W2 Ni W3 61.03(3) . . ? W2 Ni Se1 58.55(4) . . ? W2 Ni Se2 58.42(4) . . ? W2 Ni Se3 108.11(5) . . ? W2 Ni P 145.40(12) . . ? W3 Ni Se1 109.01(5) . . ? W3 Ni Se2 58.70(4) . . ? W3 Ni Se3 58.79(4) . . ? W3 Ni P 142.50(12) . . ? Se1 Ni Se2 110.89(7) . . ? Se1 Ni Se3 111.30(7) . . ? Se1 Ni P 108.50(12) . . ? Se2 Ni Se3 112.34(7) . . ? Se2 Ni P 107.07(12) . . ? Se3 Ni P 106.49(11) . . ? W1 Se1 W2 67.25(3) . . ? W1 Se1 Ni 68.93(4) . . ? W2 Se1 Ni 68.95(5) . . ? W2 Se2 W3 67.38(3) . . ? W2 Se2 Ni 69.03(4) . . ? W3 Se2 Ni 68.47(4) . . ? W1 Se3 W3 68.16(3) . . ? W1 Se3 Ni 69.00(4) . . ? W3 Se3 Ni 68.44(4) . . ? W1 Se4 W2 67.10(3) . . ? W1 Se4 W3 67.99(3) . . ? W2 Se4 W3 67.15(3) . . ? Ni P O41 116.4(5) . . ? Ni P O42 116.5(5) . . ? O41 P O42 105.1(7) . . ? N401 C401 N407 113.2(8) . 2_656 ? N401 C402 N402 107.8(8) . . ? N401 C402 O402 126.6(9) . . ? N402 C402 O402 125.7(9) . . ? N402 C403 N403 114.3(8) . . ? N403 C404 N404 109.1(8) . . ? N403 C404 O404 125.7(9) . . ? N404 C404 O404 125.0(10) . . ? N404 C405 N405 113.3(8) . . ? N405 C406 N406 108.7(8) . . ? N405 C406 O406 125.0(9) . . ? N406 C406 O406 126.2(9) . . ? N406 C407 N412 113.8(8) . 2_656 ? N407 C408 N408 108.2(8) . . ? N407 C408 O408 124.2(10) . . ? N408 C408 O408 127.5(10) . . ? N408 C409 N409 113.1(8) . . ? N409 C410 N410 108.5(9) . . ? N409 C410 O410 126.7(10) . . ? N410 C410 O410 124.7(10) . . ? N410 C411 N411 112.2(8) . . ? N411 C412 N412 108.1(9) . . ? N411 C412 O412 126.4(9) . . ? N412 C412 O412 125.4(10) . . ? C414 C413 N401 103.1(7) . . ? C414 C413 N407 103.0(8) . . ? N401 C413 N407 114.0(8) . . ? C413 C414 N402 103.4(7) . . ? C413 C414 N408 102.7(8) . . ? N402 C414 N408 113.9(8) . . ? C416 C415 N403 102.6(7) . . ? C416 C415 N409 102.9(8) . . ? N403 C415 N409 113.4(8) . . ? C415 C416 N404 102.6(7) . . ? C415 C416 N410 103.1(8) . . ? N404 C416 N410 114.8(8) . . ? C418 C417 N405 102.8(7) . . ? C418 C417 N411 103.2(8) . . ? N405 C417 N411 114.6(8) . . ? C417 C418 N406 104.6(8) . . ? C417 C418 N412 103.4(8) . . ? N406 C418 N412 115.5(8) . . ? C401 N401 C402 121.6(8) . . ? C401 N401 C413 122.3(8) . . ? C402 N401 C413 112.4(8) . . ? C402 N402 C403 120.9(8) . . ? C402 N402 C414 112.5(8) . . ? C403 N402 C414 123.2(8) . . ? C403 N403 C404 124.6(8) . . ? C403 N403 C415 123.1(8) . . ? C404 N403 C415 112.0(8) . . ? C404 N404 C405 123.9(8) . . ? C404 N404 C416 113.2(8) . . ? C405 N404 C416 122.9(8) . . ? C405 N405 C406 122.9(8) . . ? C405 N405 C417 123.6(8) . . ? C406 N405 C417 112.3(8) . . ? C406 N406 C407 122.0(8) . . ? C406 N406 C418 111.1(8) . . ? C407 N406 C418 120.7(8) . . ? C401 N407 C408 122.0(8) 2_656 . ? C401 N407 C413 125.0(8) 2_656 . ? C408 N407 C413 113.0(8) . . ? C408 N408 C409 123.1(8) . . ? C408 N408 C414 113.1(8) . . ? C409 N408 C414 123.7(8) . . ? C409 N409 C410 120.7(8) . . ? C409 N409 C415 121.5(8) . . ? C410 N409 C415 112.2(8) . . ? C410 N410 C411 123.1(8) . . ? C410 N410 C416 112.8(8) . . ? C411 N410 C416 123.1(8) . . ? C411 N411 C412 122.8(8) . . ? C411 N411 C417 124.2(8) . . ? C412 N411 C417 112.6(8) . . ? C407 N412 C412 123.0(9) 2_656 . ? C407 N412 C418 124.4(8) 2_656 . ? C412 N412 C418 112.4(8) . . ? N501 C501 N512 114.1(9) . 5_666 ? N501 C502 N502 109.2(9) . . ? N501 C502 O502 125.6(11) . . ? N502 C502 O502 125.2(11) . . ? N502 C503 N503 113.1(9) . . ? N503 C504 N504 107.5(9) . . ? N503 C504 O504 125.7(11) . . ? N504 C504 O504 126.6(11) . . ? N504 C505 N505 112.6(9) . . ? N505 C506 N506 108.5(9) . . ? N505 C506 O506 124.6(11) . . ? N506 C506 O506 126.8(11) . . ? N506 C507 N507 112.4(9) . 5_666 ? N507 C508 N508 108.3(9) . . ? N507 C508 O508 124.9(11) . . ? N508 C508 O508 126.7(11) . . ? N508 C509 N509 112.9(9) . . ? N509 C510 N510 108.9(10) . . ? N509 C510 O510 123.9(12) . . ? N510 C510 O510 127.2(11) . . ? N510 C511 N511 113.4(9) . . ? N511 C512 N512 108.4(9) . . ? N511 C512 O512 125.8(11) . . ? N512 C512 O512 125.8(10) . . ? C514 C513 N501 103.8(9) . . ? C514 C513 N507 102.8(9) . . ? N501 C513 N507 115.3(9) . . ? C513 C514 N502 102.5(8) . . ? C513 C514 N508 103.8(9) . . ? N502 C514 N508 114.3(9) . . ? C516 C515 N503 104.1(8) . . ? C516 C515 N509 103.9(8) . . ? N503 C515 N509 114.0(9) . . ? C515 C516 N504 103.4(8) . . ? C515 C516 N510 102.9(9) . . ? N504 C516 N510 115.9(9) . . ? C518 C517 N505 103.2(9) . . ? C518 C517 N511 103.0(8) . . ? N505 C517 N511 112.5(9) . . ? C517 C518 N506 103.6(9) . . ? C517 C518 N512 103.7(8) . . ? N506 C518 N512 113.6(9) . . ? C501 N501 C502 121.2(9) . . ? C501 N501 C513 124.6(9) . . ? C502 N501 C513 111.9(9) . . ? C502 N502 C503 122.4(9) . . ? C502 N502 C514 112.2(9) . . ? C503 N502 C514 123.4(9) . . ? C503 N503 C504 122.3(9) . . ? C503 N503 C515 125.1(9) . . ? C504 N503 C515 112.6(9) . . ? C504 N504 C505 120.8(9) . . ? C504 N504 C516 112.1(9) . . ? C505 N504 C516 125.5(9) . . ? C505 N505 C506 123.8(9) . . ? C505 N505 C517 123.2(9) . . ? C506 N505 C517 112.0(9) . . ? C506 N506 C507 121.0(9) . . ? C506 N506 C518 112.1(9) . . ? C507 N506 C518 122.0(9) . . ? C507 N507 C508 123.4(9) 5_666 . ? C507 N507 C513 124.1(9) 5_666 . ? C508 N507 C513 112.4(9) . . ? C508 N508 C509 122.3(9) . . ? C508 N508 C514 112.5(9) . . ? C509 N508 C514 125.1(9) . . ? C509 N509 C510 121.7(9) . . ? C509 N509 C515 123.1(9) . . ? C510 N509 C515 110.7(9) . . ? C510 N510 C511 122.9(10) . . ? C510 N510 C516 113.0(9) . . ? C511 N510 C516 124.1(10) . . ? C511 N511 C512 122.9(10) . . ? C511 N511 C517 121.9(10) . . ? C512 N511 C517 112.2(9) . . ? C501 N512 C512 123.9(9) 5_666 . ? C501 N512 C518 123.4(9) 5_666 . ? C512 N512 C518 112.4(9) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.614 _refine_diff_density_min -5.188 _refine_diff_density_rms 0.283