Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Luis M. Baraldo' _publ_contact_author_address ; Departamento de Qu\'imica Inorg\'anica Anal\'itica y Qu\'imica F\'isica Facultad de Ciencias Exactas y Naturales - Universidad de Buenos Aires Pabell\'on II - Ciudad Universitaria Ciudad de Buenos Aires C1428EHA ARGENTINA ; _publ_contact_author_email BARALDO@QI.FCEN.UBA.AR _publ_section_title ; Exchange coupling across the cyanide bridge:Structural and DFT interpretation of the magnetic properties of a binuclear chromium(III) complex ; loop_ _publ_author_name 'Luis M. Baraldo' 'Pablo Albores' 'Eva Rentschler' 'Leonardo D. Slep' 'Thomas Weyhermuller' data_1 _database_code_depnum_ccdc_archive 'CCDC 275124' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[C24 H20 P]+, [C16 H25 Cr2 N10 O]-, 4 H2O' _chemical_formula_sum 'C40 H53 Cr2 N10 O5 P' _chemical_formula_weight 888.89 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' Cr Cr 0.3209 0.6236 '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 10.0283(4) _cell_length_b 12.3379(4) _cell_length_c 18.9578(6) _cell_angle_alpha 103.19(1) _cell_angle_beta 93.48(1) _cell_angle_gamma 104.25(1) _cell_volume 2196.42(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 0.585 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8698 _exptl_absorpt_correction_T_max 0.9728 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50kV, 60mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '654 images at 1.5 deg stepwise rotation in omega and phi, 90 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60244 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 31.08 _reflns_number_total 14044 _reflns_number_gt 10733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0389P)^2^+2.0124P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14044 _refine_ls_number_parameters 497 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1124 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.758 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr -0.22734(4) 0.14035(4) 0.29325(2) 0.01301(10) Uani 1 d . . . Cr2 Cr 0.26644(4) 0.32249(4) 0.42527(2) 0.01327(10) Uani 1 d . . . N1 N 0.0649(2) 0.2995(2) 0.38254(13) 0.0165(5) Uani 1 d . . . C1 C -0.0457(3) 0.2544(2) 0.35292(15) 0.0151(5) Uani 1 d . . . N2 N -0.4985(3) -0.0526(3) 0.20411(17) 0.0347(7) Uani 1 d . . . C2 C -0.4008(3) 0.0171(3) 0.23470(16) 0.0210(6) Uani 1 d . . . C3 C -0.1478(3) 0.1664(3) 0.19912(18) 0.0269(7) Uani 1 d . . . N3 N -0.1037(4) 0.1847(4) 0.1472(2) 0.0548(11) Uani 1 d . . . C4 C -0.3267(3) 0.2688(3) 0.29409(16) 0.0182(5) Uani 1 d . . . N4 N -0.3869(3) 0.3376(2) 0.29607(16) 0.0243(6) Uani 1 d . . . C5 C -0.3084(3) 0.1249(3) 0.39038(16) 0.0199(6) Uani 1 d . . . N5 N -0.3541(3) 0.1206(3) 0.44435(16) 0.0318(7) Uani 1 d . . . C6 C -0.1213(3) 0.0168(3) 0.29959(18) 0.0220(6) Uani 1 d . . . N6 N -0.0529(3) -0.0432(3) 0.30732(19) 0.0320(7) Uani 1 d . . . O7 O 0.4528(2) 0.34704(18) 0.46581(12) 0.0179(4) Uani 1 d D . . H7A H 0.487(4) 0.290(2) 0.456(2) 0.023 Uiso 1 d D . . N11 N 0.1978(3) 0.3199(2) 0.52489(13) 0.0162(5) Uani 1 d . . . H11 H 0.1014 0.2979 0.5171 0.019 Uiso 1 calc R . . N15 N 0.2286(3) 0.1440(2) 0.39138(14) 0.0185(5) Uani 1 d . . . H15 H 0.1342 0.1144 0.3757 0.022 Uiso 1 calc R . . N18 N 0.3248(3) 0.3201(2) 0.32245(13) 0.0185(5) Uani 1 d . . . H18 H 0.4211 0.3390 0.3283 0.022 Uiso 1 calc R . . N22 N 0.2938(2) 0.4982(2) 0.45694(13) 0.0155(5) Uani 1 d . . . H22 H 0.3872 0.5313 0.4744 0.019 Uiso 1 calc R . . C12 C 0.2410(3) 0.2380(3) 0.56193(17) 0.0217(6) Uani 1 d . . . H12A H 0.2032 0.2432 0.6092 0.026 Uiso 1 calc R . . H12B H 0.3434 0.2597 0.5720 0.026 Uiso 1 calc R . . C13 C 0.1901(3) 0.1141(3) 0.51521(19) 0.0246(6) Uani 1 d . . . H13A H 0.2011 0.0615 0.5462 0.030 Uiso 1 calc R . . H13B H 0.0897 0.0979 0.4994 0.030 Uiso 1 calc R . . C14 C 0.2623(3) 0.0852(3) 0.44769(18) 0.0233(6) Uani 1 d . . . H14A H 0.3638 0.1088 0.4621 0.028 Uiso 1 calc R . . H14B H 0.2338 0.0006 0.4266 0.028 Uiso 1 calc R . . C16 C 0.3016(3) 0.1204(3) 0.32588(18) 0.0245(6) Uani 1 d . . . H16A H 0.2654 0.0384 0.2985 0.029 Uiso 1 calc R . . H16B H 0.4021 0.1355 0.3409 0.029 Uiso 1 calc R . . C17 C 0.2777(3) 0.1986(3) 0.27792(17) 0.0246(7) Uani 1 d . . . H17A H 0.3305 0.1883 0.2355 0.029 Uiso 1 calc R . . H17B H 0.1780 0.1791 0.2595 0.029 Uiso 1 calc R . . C19 C 0.2860(3) 0.4035(3) 0.28556(17) 0.0238(6) Uani 1 d . . . H19A H 0.1840 0.3823 0.2737 0.029 Uiso 1 calc R . . H19B H 0.3272 0.3990 0.2392 0.029 Uiso 1 calc R . . C20 C 0.3355(3) 0.5273(3) 0.33303(18) 0.0241(6) Uani 1 d . . . H20A H 0.4355 0.5437 0.3499 0.029 Uiso 1 calc R . . H20B H 0.3257 0.5804 0.3022 0.029 Uiso 1 calc R . . C21 C 0.2603(3) 0.5550(3) 0.39985(17) 0.0204(6) Uani 1 d . . . H21A H 0.2864 0.6397 0.4206 0.024 Uiso 1 calc R . . H21B H 0.1590 0.5295 0.3845 0.024 Uiso 1 calc R . . C23 C 0.2149(3) 0.5187(3) 0.52047(16) 0.0183(6) Uani 1 d . . . H23A H 0.1146 0.4999 0.5035 0.022 Uiso 1 calc R . . H23B H 0.2463 0.6008 0.5480 0.022 Uiso 1 calc R . . C24 C 0.2407(3) 0.4416(3) 0.56891(16) 0.0190(6) Uani 1 d . . . H24A H 0.3402 0.4633 0.5880 0.023 Uiso 1 calc R . . H24B H 0.1866 0.4508 0.6108 0.023 Uiso 1 calc R . . P1 P -0.21140(8) -0.30030(7) 0.03360(4) 0.01945(16) Uani 1 d . . . C31 C -0.1798(6) -0.4094(4) -0.0298(4) 0.0199(8) Uani 0.50 d PG A 1 C32 C -0.2344(5) -0.5232(4) -0.0271(2) 0.0276(10) Uani 0.50 d PG A 1 H32 H -0.2807 -0.5395 0.0130 0.033 Uiso 0.50 calc PR A 1 C33 C -0.2214(6) -0.6132(4) -0.0833(3) 0.0347(12) Uani 0.50 d PG A 1 H33 H -0.2587 -0.6910 -0.0815 0.042 Uiso 0.50 calc PR A 1 C34 C -0.1537(8) -0.5894(6) -0.1421(3) 0.0358(16) Uani 0.50 d PG A 1 H34 H -0.1448 -0.6509 -0.1804 0.043 Uiso 0.50 calc PR A 1 C35 C -0.0991(7) -0.4756(8) -0.1447(4) 0.0320(15) Uani 0.50 d PG A 1 H35 H -0.0528 -0.4593 -0.1849 0.038 Uiso 0.50 calc PR A 1 C36 C -0.1121(6) -0.3855(5) -0.0886(5) 0.0253(15) Uani 0.50 d PG A 1 H36 H -0.0748 -0.3077 -0.0904 0.030 Uiso 0.50 calc PR A 1 C31X C -0.1885(6) -0.4206(4) -0.0420(4) 0.0199(8) Uani 0.50 d PG A 2 C32X C -0.2877(5) -0.5265(4) -0.0637(3) 0.0276(10) Uani 0.50 d PG A 2 H32X H -0.3648 -0.5420 -0.0373 0.033 Uiso 0.50 calc PR A 2 C33X C -0.2743(6) -0.6097(4) -0.1240(3) 0.0347(12) Uani 0.50 d PG A 2 H33X H -0.3421 -0.6821 -0.1389 0.042 Uiso 0.50 calc PR A 2 C34X C -0.1616(7) -0.5871(7) -0.1627(3) 0.0358(16) Uani 0.50 d PG A 2 H34X H -0.1524 -0.6439 -0.2040 0.043 Uiso 0.50 calc PR A 2 C35X C -0.0623(6) -0.4812(8) -0.1411(4) 0.0320(15) Uani 0.50 d PG A 2 H35X H 0.0147 -0.4656 -0.1675 0.038 Uiso 0.50 calc PR A 2 C36X C -0.0757(5) -0.3979(5) -0.0807(5) 0.0253(15) Uani 0.50 d PG A 2 H36X H -0.0079 -0.3256 -0.0659 0.030 Uiso 0.50 calc PR A 2 C41 C -0.3484(7) -0.2469(7) 0.0010(4) 0.0153(7) Uani 0.50 d PG A 1 C42 C -0.4140(4) -0.1791(5) 0.0482(3) 0.0186(10) Uani 0.50 d PG A 1 H42 H -0.3778 -0.1499 0.0983 0.022 Uiso 0.50 calc PR A 1 C43 C -0.5324(4) -0.1540(4) 0.0220(2) 0.0233(9) Uani 0.50 d PG A 1 H43 H -0.5771 -0.1077 0.0542 0.028 Uiso 0.50 calc PR A 1 C44 C -0.5853(5) -0.1968(5) -0.0514(3) 0.0260(11) Uani 0.50 d PG A 1 H44 H -0.6662 -0.1796 -0.0693 0.031 Uiso 0.50 calc PR A 1 C45 C -0.5197(9) -0.2646(7) -0.0985(3) 0.0265(11) Uani 0.50 d PG A 1 H45 H -0.5559 -0.2938 -0.1487 0.032 Uiso 0.50 calc PR A 1 C46 C -0.4013(10) -0.2897(9) -0.0723(4) 0.0231(8) Uani 0.50 d PG A 1 H46 H -0.3566 -0.3360 -0.1046 0.028 Uiso 0.50 calc PR A 1 C41X C -0.3394(7) -0.2447(7) -0.0052(4) 0.0153(7) Uani 0.50 d PG A 2 C42X C -0.3647(4) -0.1484(5) 0.0404(3) 0.0186(10) Uani 0.50 d PG A 2 H42X H -0.3134 -0.1157 0.0875 0.022 Uiso 0.50 calc PR A 2 C43X C -0.4651(5) -0.0998(4) 0.0170(2) 0.0233(9) Uani 0.50 d PG A 2 H43X H -0.4824 -0.0339 0.0482 0.028 Uiso 0.50 calc PR A 2 C44X C -0.5402(5) -0.1476(5) -0.0519(3) 0.0260(11) Uani 0.50 d PG A 2 H44X H -0.6088 -0.1144 -0.0678 0.031 Uiso 0.50 calc PR A 2 C45X C -0.5149(9) -0.2440(7) -0.0975(3) 0.0265(11) Uani 0.50 d PG A 2 H45X H -0.5661 -0.2766 -0.1446 0.032 Uiso 0.50 calc PR A 2 C46X C -0.4145(11) -0.2925(8) -0.0742(4) 0.0231(8) Uani 0.50 d PG A 2 H46X H -0.3972 -0.3584 -0.1053 0.028 Uiso 0.50 calc PR A 2 C51 C -0.2612(4) -0.3373(4) 0.1162(2) 0.0159(11) Uani 0.50 d PG A 1 C52 C -0.1630(3) -0.3293(4) 0.1735(2) 0.0224(9) Uani 0.50 d PG A 1 H52 H -0.0676 -0.2959 0.1717 0.027 Uiso 0.50 calc PR A 1 C53 C -0.2045(4) -0.3701(4) 0.2334(2) 0.0262(9) Uani 0.50 d PG A 1 H53 H -0.1374 -0.3646 0.2726 0.031 Uiso 0.50 calc PR A 1 C54 C -0.3441(4) -0.4190(5) 0.2360(2) 0.0251(11) Uani 0.50 d PG A 1 H54 H -0.3725 -0.4469 0.2770 0.030 Uiso 0.50 calc PR A 1 C55 C -0.4422(3) -0.4270(4) 0.1787(2) 0.0280(10) Uani 0.50 d PG A 1 H55 H -0.5377 -0.4604 0.1805 0.034 Uiso 0.50 calc PR A 1 C56 C -0.4008(4) -0.3862(4) 0.1188(2) 0.0236(9) Uani 0.50 d PG A 1 H56 H -0.4679 -0.3917 0.0796 0.028 Uiso 0.50 calc PR A 1 C51X C -0.2752(5) -0.3690(4) 0.1042(2) 0.0159(11) Uani 0.50 d PG A 2 C52X C -0.2254(4) -0.4578(4) 0.1197(2) 0.0224(9) Uani 0.50 d PG A 2 H52X H -0.1705 -0.4931 0.0875 0.027 Uiso 0.50 calc PR A 2 C53X C -0.2561(5) -0.4950(4) 0.1822(2) 0.0262(9) Uani 0.50 d PG A 2 H53X H -0.2221 -0.5557 0.1927 0.031 Uiso 0.50 calc PR A 2 C54X C -0.3364(5) -0.4434(4) 0.2292(2) 0.0251(11) Uani 0.50 d PG A 2 H54X H -0.3574 -0.4689 0.2719 0.030 Uiso 0.50 calc PR A 2 C55X C -0.3862(5) -0.3546(4) 0.2138(2) 0.0280(10) Uani 0.50 d PG A 2 H55X H -0.4411 -0.3194 0.2460 0.034 Uiso 0.50 calc PR A 2 C56X C -0.3555(5) -0.3174(3) 0.1513(2) 0.0236(9) Uani 0.50 d PG A 2 H56X H -0.3895 -0.2567 0.1408 0.028 Uiso 0.50 calc PR A 2 C61 C -0.0470(3) -0.1812(3) 0.0604(2) 0.0173(7) Uani 0.50 d PG A 1 C62 C -0.0425(3) -0.0646(3) 0.0780(2) 0.0223(9) Uani 0.50 d PG A 1 H62 H -0.1261 -0.0415 0.0759 0.027 Uiso 0.50 calc PR A 1 C63 C 0.0841(4) 0.0184(3) 0.0988(3) 0.0266(10) Uani 0.50 d PG A 1 H63 H 0.0872 0.0981 0.1109 0.032 Uiso 0.50 calc PR A 1 C64 C 0.2064(3) -0.0153(3) 0.1020(3) 0.0298(11) Uani 0.50 d PG A 1 H64 H 0.2930 0.0414 0.1162 0.036 Uiso 0.50 calc PR A 1 C65 C 0.2019(3) -0.1319(4) 0.0844(3) 0.0265(10) Uani 0.50 d PG A 1 H65 H 0.2855 -0.1550 0.0866 0.032 Uiso 0.50 calc PR A 1 C66 C 0.0752(4) -0.2149(3) 0.0636(2) 0.0223(9) Uani 0.50 d PG A 1 H66 H 0.0722 -0.2946 0.0515 0.027 Uiso 0.50 calc PR A 1 C61X C -0.0574(2) -0.20015(19) 0.06382(8) 0.0173(7) Uani 0.50 d PG A 2 C62X C 0.0049(2) -0.1364(2) 0.01720(8) 0.0223(9) Uani 0.50 d PG A 2 H62X H -0.0401 -0.1477 -0.0305 0.027 Uiso 0.50 calc PR A 2 C63X C 0.1331(2) -0.0562(2) 0.04037(9) 0.0266(10) Uani 0.50 d PG A 2 H63X H 0.1757 -0.0127 0.0085 0.032 Uiso 0.50 calc PR A 2 C64X C 0.1989(2) -0.0397(2) 0.11015(10) 0.0298(11) Uani 0.50 d PG A 2 H64X H 0.2866 0.0152 0.1260 0.036 Uiso 0.50 calc PR A 2 C65X C 0.13658(19) -0.10339(18) 0.15677(9) 0.0265(10) Uani 0.50 d PG A 2 H65X H 0.1816 -0.0921 0.2045 0.032 Uiso 0.50 calc PR A 2 C66X C 0.0084(2) -0.18362(17) 0.13360(8) 0.0223(9) Uani 0.50 d PG A 2 H66X H -0.0342 -0.2272 0.1655 0.027 Uiso 0.50 calc PR A 2 O10 O -0.08376(17) 0.25088(15) 0.54315(8) 0.0315(6) Uani 1 d GD . . H10A H -0.1610 0.2097 0.5169 0.041 Uiso 1 d GD . . H10B H -0.0930 0.2304 0.5838 0.041 Uiso 1 d GD . . O20 O 0.07654(19) -0.22260(17) 0.31887(10) 0.0422(7) Uani 1 d GD . . H20C H 0.1367 -0.2067 0.3061 0.055 Uiso 1 d GD . . H20D H 0.0530 -0.1670 0.3150 0.055 Uiso 1 d GD . . O30 O -0.47321(18) 0.12707(18) 0.58012(9) 0.0466(7) Uani 1 d GD . . H30A H -0.4379 0.1087 0.5327 0.061 Uiso 1 d GD . . H30B H -0.5325 0.0483 0.5689 0.061 Uiso 1 d GD . . O40 O -0.66125(14) -0.20009(19) 0.28273(11) 0.0351(10) Uani 0.833(9) d PGD . . H40A H -0.6073 -0.1583 0.2631 0.046 Uiso 1 d GD . . H40B H -0.6176 -0.1947 0.3226 0.046 Uiso 1 d GD . . O40X O -0.59922(14) -0.15319(17) 0.33085(10) 0.041(6) Uani 0.167(9) d PG . . 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 Cr1 0.0092(2) 0.0166(2) 0.0122(2) 0.00335(16) 0.00031(15) 0.00221(16) Cr2 0.00894(19) 0.0154(2) 0.0127(2) -0.00005(16) 0.00031(15) 0.00167(16) N1 0.0136(11) 0.0187(11) 0.0155(11) 0.0024(9) 0.0012(9) 0.0030(9) C1 0.0143(12) 0.0166(12) 0.0147(12) 0.0040(10) 0.0028(10) 0.0039(10) N2 0.0250(15) 0.0421(18) 0.0256(15) 0.0031(13) -0.0052(12) -0.0053(13) C2 0.0171(14) 0.0270(15) 0.0165(13) 0.0044(11) 0.0012(11) 0.0029(12) C3 0.0203(15) 0.0378(19) 0.0190(14) 0.0076(13) 0.0026(12) 0.0008(13) N3 0.044(2) 0.085(3) 0.0282(18) 0.0204(19) 0.0113(16) -0.003(2) C4 0.0130(12) 0.0212(14) 0.0187(13) 0.0049(11) 0.0002(10) 0.0021(11) N4 0.0186(13) 0.0253(13) 0.0293(14) 0.0076(11) 0.0020(11) 0.0060(11) C5 0.0143(13) 0.0245(15) 0.0186(13) 0.0066(11) -0.0004(10) 0.0002(11) N5 0.0228(14) 0.0459(18) 0.0230(14) 0.0109(13) 0.0038(11) -0.0001(13) C6 0.0158(13) 0.0192(14) 0.0273(15) 0.0028(12) -0.0005(11) 0.0012(11) N6 0.0254(15) 0.0237(14) 0.0452(18) 0.0046(13) -0.0027(13) 0.0086(12) O7 0.0111(9) 0.0179(10) 0.0216(10) -0.0004(8) -0.0011(8) 0.0039(8) N11 0.0138(11) 0.0191(12) 0.0145(11) 0.0034(9) 0.0011(9) 0.0031(9) N15 0.0123(11) 0.0184(12) 0.0211(12) -0.0008(9) -0.0003(9) 0.0033(9) N18 0.0135(11) 0.0228(12) 0.0156(11) 0.0000(9) 0.0021(9) 0.0024(9) N22 0.0118(10) 0.0175(11) 0.0160(11) 0.0023(9) 0.0010(8) 0.0035(9) C12 0.0205(14) 0.0257(15) 0.0200(14) 0.0079(12) 0.0010(11) 0.0069(12) C13 0.0243(16) 0.0209(15) 0.0300(17) 0.0105(13) 0.0026(13) 0.0049(12) C14 0.0206(15) 0.0184(14) 0.0301(16) 0.0042(12) -0.0010(12) 0.0064(12) C16 0.0202(15) 0.0228(15) 0.0260(16) -0.0040(12) 0.0039(12) 0.0065(12) C17 0.0223(15) 0.0267(16) 0.0179(14) -0.0046(12) 0.0033(11) 0.0032(13) C19 0.0213(15) 0.0321(17) 0.0169(14) 0.0071(12) 0.0032(11) 0.0038(13) C20 0.0204(15) 0.0290(16) 0.0234(15) 0.0113(13) 0.0025(12) 0.0033(13) C21 0.0180(14) 0.0210(14) 0.0225(14) 0.0064(11) 0.0005(11) 0.0059(11) C23 0.0141(13) 0.0209(14) 0.0183(13) 0.0001(11) 0.0015(10) 0.0063(11) C24 0.0170(13) 0.0224(14) 0.0146(12) -0.0006(11) 0.0012(10) 0.0045(11) P1 0.0163(3) 0.0290(4) 0.0176(3) 0.0115(3) 0.0046(3) 0.0085(3) C31 0.0205(16) 0.0224(17) 0.017(2) 0.0024(15) 0.0004(15) 0.0092(14) C32 0.027(3) 0.026(2) 0.026(3) 0.000(2) 0.0015(18) 0.008(2) C33 0.032(3) 0.028(2) 0.038(3) -0.005(2) -0.003(2) 0.011(2) C34 0.043(3) 0.043(2) 0.021(4) -0.007(3) -0.003(3) 0.027(2) C35 0.034(4) 0.048(3) 0.0221(19) 0.0077(18) 0.007(3) 0.027(3) C36 0.026(4) 0.034(2) 0.021(3) 0.0070(18) 0.007(3) 0.015(2) C31X 0.0205(16) 0.0224(17) 0.017(2) 0.0024(15) 0.0004(15) 0.0092(14) C32X 0.027(3) 0.026(2) 0.026(3) 0.000(2) 0.0015(18) 0.008(2) C33X 0.032(3) 0.028(2) 0.038(3) -0.005(2) -0.003(2) 0.011(2) C34X 0.043(3) 0.043(2) 0.021(4) -0.007(3) -0.003(3) 0.027(2) C35X 0.034(4) 0.048(3) 0.0221(19) 0.0077(18) 0.007(3) 0.027(3) C36X 0.026(4) 0.034(2) 0.021(3) 0.0070(18) 0.007(3) 0.015(2) C41 0.0140(14) 0.0177(13) 0.0150(16) 0.0071(12) 0.0027(12) 0.0026(11) C42 0.018(3) 0.022(3) 0.0168(19) 0.0059(18) 0.004(2) 0.005(2) C43 0.022(2) 0.024(2) 0.028(2) 0.0094(19) 0.0064(19) 0.0096(17) C44 0.020(3) 0.027(3) 0.033(2) 0.015(3) -0.003(2) 0.006(2) C45 0.0265(18) 0.027(3) 0.0235(16) 0.0071(16) -0.0080(13) 0.005(2) C46 0.026(2) 0.0264(16) 0.0172(14) 0.0043(12) -0.0013(13) 0.0086(15) C41X 0.0140(14) 0.0177(13) 0.0150(16) 0.0071(12) 0.0027(12) 0.0026(11) C42X 0.018(3) 0.022(3) 0.0168(19) 0.0059(18) 0.004(2) 0.005(2) C43X 0.022(2) 0.024(2) 0.028(2) 0.0094(19) 0.0064(19) 0.0096(17) C44X 0.020(3) 0.027(3) 0.033(2) 0.015(3) -0.003(2) 0.006(2) C45X 0.0265(18) 0.027(3) 0.0235(16) 0.0071(16) -0.0080(13) 0.005(2) C46X 0.026(2) 0.0264(16) 0.0172(14) 0.0043(12) -0.0013(13) 0.0086(15) C51 0.0188(17) 0.013(3) 0.016(2) 0.005(2) 0.0027(15) 0.0033(19) C52 0.019(2) 0.026(2) 0.023(2) 0.0080(17) 0.0025(16) 0.0051(17) C53 0.027(2) 0.032(2) 0.023(2) 0.0132(19) 0.0026(18) 0.009(2) C54 0.0303(19) 0.026(3) 0.0209(18) 0.0119(19) 0.0059(14) 0.0051(18) C55 0.027(3) 0.035(3) 0.024(2) 0.0128(18) 0.0086(18) 0.004(2) C56 0.023(2) 0.028(2) 0.021(2) 0.0103(16) 0.0025(17) 0.0048(19) C51X 0.0188(17) 0.013(3) 0.016(2) 0.005(2) 0.0027(15) 0.0033(19) C52X 0.019(2) 0.026(2) 0.023(2) 0.0080(17) 0.0025(16) 0.0051(17) C53X 0.027(2) 0.032(2) 0.023(2) 0.0132(19) 0.0026(18) 0.009(2) C54X 0.0303(19) 0.026(3) 0.0209(18) 0.0119(19) 0.0059(14) 0.0051(18) C55X 0.027(3) 0.035(3) 0.024(2) 0.0128(18) 0.0086(18) 0.004(2) C56X 0.023(2) 0.028(2) 0.021(2) 0.0103(16) 0.0025(17) 0.0048(19) C61 0.0152(14) 0.0174(17) 0.0178(14) 0.0039(12) 0.0011(11) 0.0023(13) C62 0.021(2) 0.026(2) 0.021(2) 0.0098(17) 0.0036(16) 0.0062(17) C63 0.023(2) 0.023(2) 0.031(2) 0.0076(19) 0.0076(19) 0.0016(18) C64 0.0179(17) 0.027(3) 0.035(2) -0.0033(19) 0.0024(15) -0.0007(17) C65 0.021(2) 0.027(2) 0.025(2) 0.0016(18) 0.0007(17) 0.0019(18) C66 0.022(2) 0.022(2) 0.021(2) 0.0048(16) 0.0020(16) 0.0037(17) C61X 0.0152(14) 0.0174(17) 0.0178(14) 0.0039(12) 0.0011(11) 0.0023(13) C62X 0.021(2) 0.026(2) 0.021(2) 0.0098(17) 0.0036(16) 0.0062(17) C63X 0.023(2) 0.023(2) 0.031(2) 0.0076(19) 0.0076(19) 0.0016(18) C64X 0.0179(17) 0.027(3) 0.035(2) -0.0033(19) 0.0024(15) -0.0007(17) C65X 0.021(2) 0.027(2) 0.025(2) 0.0016(18) 0.0007(17) 0.0019(18) C66X 0.022(2) 0.022(2) 0.021(2) 0.0048(16) 0.0020(16) 0.0037(17) O10 0.0173(11) 0.0489(16) 0.0275(12) 0.0121(11) 0.0051(9) 0.0044(11) O20 0.0580(19) 0.0474(17) 0.0353(15) 0.0172(13) 0.0107(13) 0.0327(15) O30 0.0449(17) 0.0552(19) 0.0403(17) 0.0155(15) 0.0075(14) 0.0108(15) O40 0.0357(19) 0.0378(19) 0.0316(19) 0.0115(15) 0.0076(14) 0.0057(15) O40X 0.050(12) 0.033(9) 0.036(11) 0.002(7) 0.008(8) 0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C3 2.057(3) . ? Cr1 C2 2.065(3) . ? Cr1 C4 2.067(3) . ? Cr1 C6 2.082(3) . ? Cr1 C1 2.083(3) . ? Cr1 C5 2.086(3) . ? Cr2 O7 1.902(2) . ? Cr2 N11 2.053(2) . ? Cr2 N22 2.056(2) . ? Cr2 N1 2.058(2) . ? Cr2 N18 2.065(3) . ? Cr2 N15 2.078(3) . ? N1 C1 1.155(4) . ? N2 C2 1.151(4) . ? C3 N3 1.150(5) . ? C4 N4 1.153(4) . ? C5 N5 1.153(4) . ? C6 N6 1.153(4) . ? N11 C24 1.484(4) . ? N11 C12 1.485(4) . ? N15 C14 1.487(4) . ? N15 C16 1.488(4) . ? N18 C19 1.480(4) . ? N18 C17 1.486(4) . ? N22 C21 1.481(4) . ? N22 C23 1.489(4) . ? C12 C13 1.525(4) . ? C13 C14 1.524(5) . ? C16 C17 1.518(5) . ? C19 C20 1.528(5) . ? C20 C21 1.528(4) . ? C23 C24 1.518(4) . ? P1 C61X 1.694(2) . ? P1 C31 1.695(5) . ? P1 C41X 1.791(5) . ? P1 C51 1.794(3) . ? P1 C41 1.798(5) . ? P1 C51X 1.810(3) . ? P1 C61 1.871(3) . ? P1 C31X 1.884(5) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C31X C32X 1.3900 . ? C31X C36X 1.3900 . ? C32X C33X 1.3900 . ? C33X C34X 1.3900 . ? C34X C35X 1.3900 . ? C35X C36X 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C41X C42X 1.3900 . ? C41X C46X 1.3900 . ? C42X C43X 1.3900 . ? C43X C44X 1.3900 . ? C44X C45X 1.3900 . ? C45X C46X 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C51X C52X 1.3900 . ? C51X C56X 1.3900 . ? C52X C53X 1.3900 . ? C53X C54X 1.3900 . ? C54X C55X 1.3900 . ? C55X C56X 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? C61X C62X 1.3900 . ? C61X C66X 1.3900 . ? C62X C63X 1.3900 . ? C63X C64X 1.3900 . ? C64X C65X 1.3900 . ? C65X C66X 1.3900 . ? O30 O40X 1.723(4) 2_456 ? O40 O40X 1.0330 . ? O40X O30 1.723(4) 2_456 ? 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 C3 Cr1 C2 91.78(13) . . ? C3 Cr1 C4 90.16(14) . . ? C2 Cr1 C4 90.61(12) . . ? C3 Cr1 C6 92.15(14) . . ? C2 Cr1 C6 92.43(12) . . ? C4 Cr1 C6 176.13(12) . . ? C3 Cr1 C1 88.69(12) . . ? C2 Cr1 C1 175.63(12) . . ? C4 Cr1 C1 93.73(11) . . ? C6 Cr1 C1 83.22(11) . . ? C3 Cr1 C5 176.36(14) . . ? C2 Cr1 C5 89.95(12) . . ? C4 Cr1 C5 86.62(12) . . ? C6 Cr1 C5 90.98(13) . . ? C1 Cr1 C5 89.84(11) . . ? O7 Cr2 N11 91.25(10) . . ? O7 Cr2 N22 88.37(9) . . ? N11 Cr2 N22 85.81(10) . . ? O7 Cr2 N1 178.77(10) . . ? N11 Cr2 N1 88.37(10) . . ? N22 Cr2 N1 90.43(10) . . ? O7 Cr2 N18 91.61(10) . . ? N11 Cr2 N18 176.89(10) . . ? N22 Cr2 N18 95.48(10) . . ? N1 Cr2 N18 88.79(10) . . ? O7 Cr2 N15 94.45(10) . . ? N11 Cr2 N15 93.99(10) . . ? N22 Cr2 N15 177.18(10) . . ? N1 Cr2 N15 86.75(10) . . ? N18 Cr2 N15 84.58(10) . . ? C1 N1 Cr2 160.3(2) . . ? N1 C1 Cr1 166.9(2) . . ? N2 C2 Cr1 177.8(3) . . ? N3 C3 Cr1 177.7(4) . . ? N4 C4 Cr1 176.8(3) . . ? N5 C5 Cr1 177.3(3) . . ? N6 C6 Cr1 173.5(3) . . ? C24 N11 C12 113.7(2) . . ? C24 N11 Cr2 105.89(18) . . ? C12 N11 Cr2 115.51(19) . . ? C14 N15 C16 113.1(2) . . ? C14 N15 Cr2 116.27(19) . . ? C16 N15 Cr2 106.26(19) . . ? C19 N18 C17 113.4(2) . . ? C19 N18 Cr2 116.98(19) . . ? C17 N18 Cr2 107.62(19) . . ? C21 N22 C23 113.0(2) . . ? C21 N22 Cr2 116.93(18) . . ? C23 N22 Cr2 105.85(18) . . ? N11 C12 C13 111.3(2) . . ? C14 C13 C12 116.0(3) . . ? N15 C14 C13 112.0(3) . . ? N15 C16 C17 108.5(3) . . ? N18 C17 C16 108.2(2) . . ? N18 C19 C20 111.9(2) . . ? C21 C20 C19 115.9(3) . . ? N22 C21 C20 112.4(2) . . ? N22 C23 C24 107.9(2) . . ? N11 C24 C23 108.5(2) . . ? C61X P1 C31 106.8(2) . . ? C61X P1 C41X 113.2(3) . . ? C31 P1 C41X 110.0(3) . . ? C61X P1 C51 101.85(15) . . ? C31 P1 C51 114.6(3) . . ? C41X P1 C51 110.2(3) . . ? C61X P1 C41 115.3(3) . . ? C31 P1 C41 112.8(3) . . ? C41X P1 C41 5.0(5) . . ? C51 P1 C41 105.2(3) . . ? C61X P1 C51X 111.45(17) . . ? C31 P1 C51X 103.4(3) . . ? C41X P1 C51X 111.4(3) . . ? C51 P1 C51X 12.4(2) . . ? C41 P1 C51X 106.5(3) . . ? C61X P1 C61 5.94(16) . . ? C31 P1 C61 107.7(2) . . ? C41X P1 C61 107.7(3) . . ? C51 P1 C61 106.4(2) . . ? C41 P1 C61 110.0(3) . . ? C51X P1 C61 116.5(2) . . ? C61X P1 C31X 109.81(18) . . ? C31 P1 C31X 4.7(3) . . ? C41X P1 C31X 105.3(3) . . ? C51 P1 C31X 116.8(3) . . ? C41 P1 C31X 108.1(3) . . ? C51X P1 C31X 105.2(3) . . ? C61 P1 C31X 110.3(2) . . ? C32 C31 C36 120.0 . . ? C32 C31 P1 119.9(4) . . ? C36 C31 P1 119.8(4) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C32X C31X C36X 120.0 . . ? C32X C31X P1 121.4(4) . . ? C36X C31X P1 118.4(4) . . ? C31X C32X C33X 120.0 . . ? C32X C33X C34X 120.0 . . ? C35X C34X C33X 120.0 . . ? C36X C35X C34X 120.0 . . ? C35X C36X C31X 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 P1 122.0(4) . . ? C46 C41 P1 117.3(4) . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C42X C41X C46X 120.0 . . ? C42X C41X P1 114.8(4) . . ? C46X C41X P1 125.2(4) . . ? C43X C42X C41X 120.0 . . ? C42X C43X C44X 120.0 . . ? C43X C44X C45X 120.0 . . ? C46X C45X C44X 120.0 . . ? C45X C46X C41X 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 P1 121.6(2) . . ? C56 C51 P1 118.1(2) . . ? C51 C52 C53 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? C52X C51X C56X 120.0 . . ? C52X C51X P1 121.0(2) . . ? C56X C51X P1 118.0(2) . . ? C51X C52X C53X 120.0 . . ? C52X C53X C54X 120.0 . . ? C55X C54X C53X 120.0 . . ? C56X C55X C54X 120.0 . . ? C55X C56X C51X 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 P1 123.7(2) . . ? C66 C61 P1 116.3(2) . . ? C63 C62 C61 120.0 . . ? C64 C63 C62 120.0 . . ? C65 C64 C63 120.0 . . ? C64 C65 C66 120.0 . . ? C65 C66 C61 120.0 . . ? C62X C61X C66X 120.0 . . ? C62X C61X P1 119.22(7) . . ? C66X C61X P1 120.76(8) . . ? C61X C62X C63X 120.0 . . ? C62X C63X C64X 120.0 . . ? C65X C64X C63X 120.0 . . ? C64X C65X C66X 120.0 . . ? C65X C66X C61X 120.0 . . ? O40 O40X O30 156.45(11) . 2_456 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 31.08 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.836 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.072 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 275125' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '3 [C24 H20 P]+, [C6 Cr N6]3-, 2 H2O' _chemical_formula_sum 'C78 H64 Cr N6 O2 P3' _chemical_formula_weight 1262.26 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.1811(6) _cell_length_b 20.3170(8) _cell_length_c 21.2304(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.78(1) _cell_angle_gamma 90.00 _cell_volume 6432.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2636 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.9330 _exptl_absorpt_correction_T_max 0.9684 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode, 50kV, 80mA' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '959 images at 1.0 deg. stepwise rotation in omega and phi, 20 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 107094 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12597 _reflns_number_gt 11046 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+6.2791P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12597 _refine_ls_number_parameters 823 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.121238(18) 0.150053(13) 0.762621(13) 0.01123(7) Uani 1 d . . . C11 C 0.19409(12) 0.06267(9) 0.76558(8) 0.0162(4) Uani 1 d . . . N12 N 0.23636(11) 0.01605(8) 0.76147(8) 0.0218(4) Uani 1 d . . . C21 C 0.23846(12) 0.20146(9) 0.79748(9) 0.0174(4) Uani 1 d . . . N22 N 0.30133(12) 0.23161(9) 0.81808(9) 0.0303(4) Uani 1 d . . . C31 C 0.13491(12) 0.15616(9) 0.66735(9) 0.0154(4) Uani 1 d . . . N32 N 0.14158(11) 0.15894(8) 0.61438(8) 0.0221(4) Uani 1 d . . . C41 C 0.00018(12) 0.09951(9) 0.73767(8) 0.0148(4) Uani 1 d . . . N42 N -0.06677(11) 0.07127(8) 0.73070(8) 0.0217(4) Uani 1 d . . . C51 C 0.05870(12) 0.24190(9) 0.75130(8) 0.0145(4) Uani 1 d . . . N52 N 0.03157(10) 0.29489(8) 0.74419(7) 0.0190(3) Uani 1 d . . . C61 C 0.09653(12) 0.13839(8) 0.85520(8) 0.0158(4) Uani 1 d . . . N62 N 0.07397(12) 0.12882(8) 0.90338(8) 0.0233(4) Uani 1 d . . . P1 P 0.48200(3) 0.15224(2) 1.01343(2) 0.01189(9) Uani 1 d . . . C101 C 0.58765(12) 0.13482(9) 1.06439(8) 0.0140(3) Uani 1 d . . . C102 C 0.63527(13) 0.07865(9) 1.05268(9) 0.0185(4) Uani 1 d . . . H102 H 0.6121 0.0505 1.0178 0.022 Uiso 1 calc R . . C103 C 0.71628(13) 0.06431(10) 1.09216(9) 0.0216(4) Uani 1 d . . . H103 H 0.7490 0.0262 1.0844 0.026 Uiso 1 calc R . . C104 C 0.74983(12) 0.10565(9) 1.14318(9) 0.0190(4) Uani 1 d . . . H104 H 0.8056 0.0958 1.1701 0.023 Uiso 1 calc R . . C105 C 0.70267(12) 0.16101(9) 1.15497(9) 0.0180(4) Uani 1 d . . . H105 H 0.7258 0.1888 1.1901 0.022 Uiso 1 calc R . . C106 C 0.62138(12) 0.17612(9) 1.11544(8) 0.0159(4) Uani 1 d . . . H106 H 0.5891 0.2144 1.1233 0.019 Uiso 1 calc R . . C111 C 0.39510(12) 0.10174(9) 1.03473(8) 0.0144(3) Uani 1 d . . . C112 C 0.41484(13) 0.05177(9) 1.07988(8) 0.0175(4) Uani 1 d . . . H112 H 0.4751 0.0437 1.1002 0.021 Uiso 1 calc R . . C113 C 0.34571(13) 0.01367(9) 1.09503(9) 0.0208(4) Uani 1 d . . . H113 H 0.3590 -0.0211 1.1252 0.025 Uiso 1 calc R . . C114 C 0.25758(13) 0.02607(10) 1.06640(9) 0.0217(4) Uani 1 d . . . H114 H 0.2107 0.0001 1.0774 0.026 Uiso 1 calc R . . C115 C 0.23745(13) 0.07618(9) 1.02172(9) 0.0200(4) Uani 1 d . . . H115 H 0.1769 0.0847 1.0023 0.024 Uiso 1 calc R . . C116 C 0.30592(12) 0.11385(9) 1.00550(9) 0.0175(4) Uani 1 d . . . H116 H 0.2924 0.1479 0.9745 0.021 Uiso 1 calc R . . C121 C 0.45169(11) 0.23636(8) 1.02286(8) 0.0134(3) Uani 1 d . . . C122 C 0.45521(12) 0.28229(9) 0.97478(9) 0.0167(4) Uani 1 d . . . H122 H 0.4713 0.2690 0.9355 0.020 Uiso 1 calc R . . C123 C 0.43495(13) 0.34773(9) 0.98467(9) 0.0195(4) Uani 1 d . . . H123 H 0.4375 0.3795 0.9522 0.023 Uiso 1 calc R . . C124 C 0.41117(12) 0.36657(9) 1.04168(9) 0.0194(4) Uani 1 d . . . H124 H 0.3975 0.4114 1.0482 0.023 Uiso 1 calc R . . C125 C 0.40702(12) 0.32087(9) 1.08965(9) 0.0180(4) Uani 1 d . . . H125 H 0.3906 0.3344 1.1287 0.022 Uiso 1 calc R . . C126 C 0.42695(12) 0.25553(9) 1.08032(8) 0.0154(4) Uani 1 d . . . H126 H 0.4238 0.2239 1.1128 0.018 Uiso 1 calc R . . C131 C 0.49346(12) 0.13626(8) 0.93196(8) 0.0130(3) Uani 1 d . . . C132 C 0.56820(12) 0.16227(9) 0.91123(9) 0.0164(4) Uani 1 d . . . H132 H 0.6117 0.1865 0.9401 0.020 Uiso 1 calc R . . C133 C 0.57882(12) 0.15262(9) 0.84838(9) 0.0173(4) Uani 1 d . . . H133 H 0.6296 0.1703 0.8341 0.021 Uiso 1 calc R . . C134 C 0.51521(12) 0.11708(9) 0.80645(9) 0.0179(4) Uani 1 d . . . H134 H 0.5223 0.1109 0.7633 0.021 Uiso 1 calc R . . C135 C 0.44173(13) 0.09063(9) 0.82699(9) 0.0203(4) Uani 1 d . . . H135 H 0.3989 0.0658 0.7981 0.024 Uiso 1 calc R . . C136 C 0.43028(12) 0.10021(9) 0.88981(9) 0.0170(4) Uani 1 d . . . H136 H 0.3795 0.0822 0.9039 0.020 Uiso 1 calc R . . P2 P 0.21553(3) 0.09894(2) 0.40506(2) 0.01214(10) Uani 1 d . . . C201 C 0.22861(12) 0.03979(9) 0.46863(8) 0.0162(4) Uani 1 d . . . C202 C 0.29305(13) -0.00995(9) 0.47203(9) 0.0211(4) Uani 1 d . . . H202 H 0.3268 -0.0146 0.4388 0.025 Uiso 1 calc R . . C203 C 0.30748(15) -0.05235(10) 0.52396(10) 0.0280(5) Uani 1 d . . . H203 H 0.3508 -0.0864 0.5262 0.034 Uiso 1 calc R . . C204 C 0.25898(16) -0.04518(10) 0.57252(10) 0.0311(5) Uani 1 d . . . H204 H 0.2699 -0.0738 0.6085 0.037 Uiso 1 calc R . . C205 C 0.19469(16) 0.00352(10) 0.56895(10) 0.0287(5) Uani 1 d . . . H205 H 0.1616 0.0081 0.6025 0.034 Uiso 1 calc R . . C206 C 0.17802(14) 0.04590(9) 0.51673(9) 0.0222(4) Uani 1 d . . . H206 H 0.1327 0.0786 0.5139 0.027 Uiso 1 calc R . . C211 C 0.09972(12) 0.10571(9) 0.36802(8) 0.0159(4) Uani 1 d . . . C212 C 0.06291(13) 0.16678(10) 0.34820(9) 0.0201(4) Uani 1 d . . . H212 H 0.0991 0.2052 0.3544 0.024 Uiso 1 calc R . . C213 C -0.02689(14) 0.17138(12) 0.31930(9) 0.0278(5) Uani 1 d . . . H213 H -0.0526 0.2130 0.3063 0.033 Uiso 1 calc R . . C214 C -0.07858(14) 0.11485(13) 0.30968(9) 0.0316(5) Uani 1 d . . . H214 H -0.1402 0.1180 0.2906 0.038 Uiso 1 calc R . . C215 C -0.04177(13) 0.05394(12) 0.32741(10) 0.0280(5) Uani 1 d . . . H215 H -0.0775 0.0154 0.3190 0.034 Uiso 1 calc R . . C216 C 0.04735(13) 0.04895(10) 0.35757(9) 0.0208(4) Uani 1 d . . . H216 H 0.0724 0.0073 0.3710 0.025 Uiso 1 calc R . . C221 C 0.28174(12) 0.07341(8) 0.34804(8) 0.0146(4) Uani 1 d . . . C222 C 0.24317(13) 0.04003(9) 0.29238(9) 0.0200(4) Uani 1 d . . . H222 H 0.1804 0.0320 0.2830 0.024 Uiso 1 calc R . . C223 C 0.29772(14) 0.01870(10) 0.25083(10) 0.0265(5) Uani 1 d . . . H223 H 0.2721 -0.0041 0.2127 0.032 Uiso 1 calc R . . C224 C 0.38922(14) 0.03036(10) 0.26445(10) 0.0247(4) Uani 1 d . . . H224 H 0.4258 0.0159 0.2354 0.030 Uiso 1 calc R . . C225 C 0.42777(13) 0.06303(9) 0.32011(9) 0.0209(4) Uani 1 d . . . H225 H 0.4906 0.0707 0.3294 0.025 Uiso 1 calc R . . C226 C 0.37431(12) 0.08434(9) 0.36197(9) 0.0178(4) Uani 1 d . . . H226 H 0.4005 0.1065 0.4003 0.021 Uiso 1 calc R . . C231 C 0.25444(11) 0.17854(8) 0.43482(8) 0.0132(3) Uani 1 d . . . C232 C 0.27904(12) 0.22377(9) 0.39140(8) 0.0162(4) Uani 1 d . . . H232 H 0.2804 0.2107 0.3486 0.019 Uiso 1 calc R . . C233 C 0.30139(12) 0.28758(9) 0.41093(9) 0.0189(4) Uani 1 d . . . H233 H 0.3184 0.3184 0.3817 0.023 Uiso 1 calc R . . C234 C 0.29889(12) 0.30644(9) 0.47354(9) 0.0188(4) Uani 1 d . . . H234 H 0.3132 0.3504 0.4868 0.023 Uiso 1 calc R . . C235 C 0.27564(12) 0.26160(9) 0.51660(9) 0.0185(4) Uani 1 d . . . H235 H 0.2751 0.2748 0.5594 0.022 Uiso 1 calc R . . C236 C 0.25302(12) 0.19732(9) 0.49777(8) 0.0157(4) Uani 1 d . . . H236 H 0.2368 0.1666 0.5274 0.019 Uiso 1 calc R . . P3 P 0.07025(3) 0.24728(2) 0.10049(2) 0.01250(10) Uani 1 d . . . C301 C -0.01323(12) 0.30308(9) 0.11835(8) 0.0149(4) Uani 1 d . . . C302 C -0.01246(13) 0.36859(9) 0.09882(9) 0.0197(4) Uani 1 d . . . H302 H 0.0293 0.3828 0.0735 0.024 Uiso 1 calc R . . C303 C -0.07300(13) 0.41285(10) 0.11656(9) 0.0240(4) Uani 1 d . . . H303 H -0.0724 0.4576 0.1036 0.029 Uiso 1 calc R . . C304 C -0.13410(13) 0.39209(11) 0.15306(9) 0.0237(4) Uani 1 d . . . H304 H -0.1756 0.4226 0.1648 0.028 Uiso 1 calc R . . C305 C -0.13519(13) 0.32727(11) 0.17256(9) 0.0229(4) Uani 1 d . . . H305 H -0.1773 0.3133 0.1977 0.028 Uiso 1 calc R . . C306 C -0.07484(12) 0.28268(10) 0.15538(8) 0.0182(4) Uani 1 d . . . H306 H -0.0755 0.2381 0.1689 0.022 Uiso 1 calc R . . C311 C 0.16961(12) 0.25570(9) 0.16056(8) 0.0148(4) Uani 1 d . . . C312 C 0.23195(12) 0.20446(9) 0.17177(9) 0.0179(4) Uani 1 d . . . H312 H 0.2195 0.1634 0.1505 0.021 Uiso 1 calc R . . C313 C 0.31233(12) 0.21401(10) 0.21425(9) 0.0201(4) Uani 1 d . . . H313 H 0.3550 0.1794 0.2221 0.024 Uiso 1 calc R . . C314 C 0.33044(12) 0.27380(10) 0.24514(9) 0.0207(4) Uani 1 d . . . H314 H 0.3860 0.2804 0.2735 0.025 Uiso 1 calc R . . C315 C 0.26796(13) 0.32411(10) 0.23489(9) 0.0220(4) Uani 1 d . . . H315 H 0.2804 0.3647 0.2569 0.026 Uiso 1 calc R . . C316 C 0.18746(12) 0.31556(9) 0.19267(9) 0.0185(4) Uani 1 d . . . H316 H 0.1447 0.3502 0.1856 0.022 Uiso 1 calc R . . C321 C 0.03160(12) 0.16413(9) 0.10058(8) 0.0149(4) Uani 1 d . . . C322 C 0.00135(12) 0.13217(9) 0.04250(9) 0.0167(4) Uani 1 d . . . H322 H 0.0047 0.1533 0.0031 0.020 Uiso 1 calc R . . C323 C -0.03373(13) 0.06924(9) 0.04272(9) 0.0202(4) Uani 1 d . . . H323 H -0.0553 0.0474 0.0033 0.024 Uiso 1 calc R . . C324 C -0.03754(13) 0.03794(9) 0.10001(10) 0.0231(4) Uani 1 d . . . H324 H -0.0625 -0.0050 0.0997 0.028 Uiso 1 calc R . . C325 C -0.00515(13) 0.06892(10) 0.15787(10) 0.0234(4) Uani 1 d . . . H325 H -0.0066 0.0468 0.1971 0.028 Uiso 1 calc R . . C326 C 0.02924(13) 0.13192(9) 0.15861(9) 0.0200(4) Uani 1 d . . . H326 H 0.0512 0.1533 0.1982 0.024 Uiso 1 calc R . . C331 C 0.09543(12) 0.26798(8) 0.02375(8) 0.0131(3) Uani 1 d . . . C332 C 0.18380(12) 0.26608(9) 0.01429(9) 0.0154(4) Uani 1 d . . . H332 H 0.2311 0.2561 0.0490 0.018 Uiso 1 calc R . . C333 C 0.20247(12) 0.27877(9) -0.04601(9) 0.0167(4) Uani 1 d . . . H333 H 0.2627 0.2778 -0.0525 0.020 Uiso 1 calc R . . C334 C 0.13363(12) 0.29279(8) -0.09666(9) 0.0163(4) Uani 1 d . . . H334 H 0.1467 0.3013 -0.1380 0.020 Uiso 1 calc R . . C335 C 0.04554(12) 0.29450(9) -0.08749(9) 0.0165(4) Uani 1 d . . . H335 H -0.0015 0.3040 -0.1226 0.020 Uiso 1 calc R . . C336 C 0.02577(12) 0.28246(9) -0.02754(8) 0.0153(4) Uani 1 d . . . H336 H -0.0345 0.2840 -0.0212 0.018 Uiso 1 calc R . . O400 O -0.11622(10) 0.07687(7) 0.86120(7) 0.0284(3) Uani 1 d D . . H401 H -0.0644(11) 0.0934(12) 0.8781(11) 0.037 Uiso 1 d D . . H402 H -0.1081(17) 0.0679(12) 0.8227(7) 0.037 Uiso 1 d D . . O500 O 0.38747(15) -0.06453(10) 0.73077(12) 0.0603(6) Uani 1 d D . . H501 H 0.420(2) -0.0707(18) 0.7686(10) 0.078 Uiso 1 d D . . H502 H 0.3372(14) -0.0531(17) 0.7417(16) 0.078 Uiso 1 d 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 Cr1 0.01134(14) 0.01112(14) 0.01142(14) 0.00024(10) 0.00259(10) -0.00080(11) C11 0.0137(8) 0.0179(9) 0.0160(9) 0.0006(7) 0.0002(7) -0.0039(7) N12 0.0183(8) 0.0185(8) 0.0280(9) 0.0015(7) 0.0029(7) 0.0003(7) C21 0.0169(9) 0.0169(9) 0.0193(9) -0.0014(7) 0.0060(7) 0.0009(7) N22 0.0214(9) 0.0304(10) 0.0402(11) -0.0113(8) 0.0090(8) -0.0073(8) C31 0.0128(8) 0.0142(9) 0.0191(9) 0.0005(7) 0.0028(7) 0.0016(7) N32 0.0226(9) 0.0258(9) 0.0188(9) -0.0001(7) 0.0066(7) 0.0037(7) C41 0.0167(9) 0.0132(8) 0.0145(8) 0.0001(7) 0.0029(7) 0.0026(7) N42 0.0192(8) 0.0187(8) 0.0272(9) -0.0037(7) 0.0043(7) -0.0003(7) C51 0.0130(8) 0.0187(9) 0.0120(8) -0.0015(7) 0.0027(7) -0.0034(7) N52 0.0193(8) 0.0184(8) 0.0190(8) 0.0006(6) 0.0033(6) 0.0007(6) C61 0.0179(9) 0.0124(8) 0.0158(9) -0.0009(7) -0.0001(7) -0.0024(7) N62 0.0350(10) 0.0177(8) 0.0180(8) -0.0010(7) 0.0072(7) -0.0051(7) P1 0.0123(2) 0.0120(2) 0.0114(2) -0.00005(17) 0.00222(17) 0.00000(17) C101 0.0129(8) 0.0162(9) 0.0130(8) 0.0027(7) 0.0028(7) -0.0004(7) C102 0.0209(9) 0.0183(9) 0.0152(9) -0.0031(7) 0.0009(7) 0.0028(7) C103 0.0210(10) 0.0218(10) 0.0221(10) 0.0002(8) 0.0043(8) 0.0071(8) C104 0.0145(9) 0.0255(10) 0.0162(9) 0.0054(8) 0.0007(7) 0.0004(8) C105 0.0185(9) 0.0219(10) 0.0129(8) -0.0008(7) 0.0012(7) -0.0026(7) C106 0.0166(9) 0.0157(9) 0.0158(9) 0.0003(7) 0.0043(7) -0.0007(7) C111 0.0157(9) 0.0132(8) 0.0154(8) -0.0027(7) 0.0057(7) -0.0012(7) C112 0.0204(9) 0.0175(9) 0.0153(9) 0.0009(7) 0.0051(7) 0.0024(7) C113 0.0290(11) 0.0166(9) 0.0179(9) 0.0017(7) 0.0073(8) -0.0009(8) C114 0.0237(10) 0.0225(10) 0.0212(10) -0.0035(8) 0.0100(8) -0.0076(8) C115 0.0147(9) 0.0241(10) 0.0215(9) -0.0042(8) 0.0044(7) -0.0017(7) C116 0.0190(9) 0.0161(9) 0.0173(9) 0.0012(7) 0.0030(7) 0.0020(7) C121 0.0104(8) 0.0141(8) 0.0154(8) -0.0005(7) 0.0017(7) 0.0005(7) C122 0.0162(9) 0.0184(9) 0.0163(9) 0.0003(7) 0.0055(7) 0.0005(7) C123 0.0208(9) 0.0155(9) 0.0224(10) 0.0050(7) 0.0044(8) 0.0008(7) C124 0.0174(9) 0.0140(9) 0.0259(10) -0.0031(8) 0.0012(8) 0.0007(7) C125 0.0151(9) 0.0216(9) 0.0165(9) -0.0048(7) 0.0012(7) 0.0010(7) C126 0.0132(8) 0.0188(9) 0.0140(8) 0.0013(7) 0.0016(7) -0.0002(7) C131 0.0143(8) 0.0131(8) 0.0117(8) 0.0009(7) 0.0021(7) 0.0028(7) C132 0.0158(9) 0.0158(9) 0.0169(9) -0.0027(7) 0.0012(7) -0.0016(7) C133 0.0156(9) 0.0191(9) 0.0182(9) -0.0007(7) 0.0056(7) 0.0008(7) C134 0.0210(9) 0.0206(9) 0.0118(8) -0.0014(7) 0.0024(7) 0.0053(8) C135 0.0186(9) 0.0228(10) 0.0169(9) -0.0046(8) -0.0038(7) -0.0012(8) C136 0.0141(9) 0.0175(9) 0.0189(9) 0.0004(7) 0.0024(7) -0.0009(7) P2 0.0128(2) 0.0121(2) 0.0122(2) -0.00109(17) 0.00401(17) -0.00087(17) C201 0.0200(9) 0.0130(8) 0.0157(9) 0.0003(7) 0.0033(7) -0.0050(7) C202 0.0217(10) 0.0158(9) 0.0252(10) 0.0017(8) 0.0032(8) -0.0021(8) C203 0.0316(11) 0.0175(10) 0.0320(11) 0.0053(8) -0.0017(9) -0.0033(8) C204 0.0474(14) 0.0192(10) 0.0236(11) 0.0062(8) -0.0014(10) -0.0110(10) C205 0.0459(13) 0.0243(11) 0.0184(10) -0.0020(8) 0.0124(9) -0.0153(10) C206 0.0306(11) 0.0167(9) 0.0211(10) -0.0026(8) 0.0094(8) -0.0068(8) C211 0.0129(8) 0.0233(9) 0.0122(8) -0.0052(7) 0.0047(7) -0.0002(7) C212 0.0209(10) 0.0246(10) 0.0155(9) -0.0038(8) 0.0052(8) 0.0042(8) C213 0.0223(10) 0.0442(13) 0.0159(9) -0.0052(9) 0.0013(8) 0.0131(9) C214 0.0148(10) 0.0642(16) 0.0154(9) -0.0131(10) 0.0018(8) 0.0046(10) C215 0.0182(10) 0.0458(13) 0.0219(10) -0.0167(9) 0.0084(8) -0.0097(9) C216 0.0187(9) 0.0272(10) 0.0183(9) -0.0087(8) 0.0077(8) -0.0047(8) C221 0.0172(9) 0.0125(8) 0.0153(8) 0.0001(7) 0.0066(7) 0.0011(7) C222 0.0175(9) 0.0231(10) 0.0207(9) -0.0051(8) 0.0070(8) -0.0034(8) C223 0.0286(11) 0.0288(11) 0.0246(10) -0.0116(9) 0.0113(9) -0.0080(9) C224 0.0276(11) 0.0228(10) 0.0286(11) -0.0049(8) 0.0177(9) -0.0002(8) C225 0.0167(9) 0.0204(10) 0.0274(10) 0.0015(8) 0.0085(8) 0.0007(7) C226 0.0167(9) 0.0186(9) 0.0181(9) -0.0010(7) 0.0037(7) -0.0014(7) C231 0.0113(8) 0.0127(8) 0.0153(8) -0.0010(7) 0.0018(7) 0.0001(7) C232 0.0162(9) 0.0182(9) 0.0141(8) 0.0002(7) 0.0028(7) -0.0009(7) C233 0.0151(9) 0.0162(9) 0.0247(10) 0.0031(8) 0.0021(8) -0.0011(7) C234 0.0128(9) 0.0147(9) 0.0275(10) -0.0049(8) 0.0000(8) -0.0004(7) C235 0.0152(9) 0.0219(9) 0.0173(9) -0.0064(7) 0.0002(7) 0.0029(7) C236 0.0147(9) 0.0182(9) 0.0140(8) 0.0007(7) 0.0018(7) 0.0015(7) P3 0.0115(2) 0.0145(2) 0.0116(2) -0.00046(17) 0.00239(17) -0.00022(17) C301 0.0118(8) 0.0188(9) 0.0133(8) -0.0038(7) 0.0007(7) 0.0002(7) C302 0.0169(9) 0.0216(10) 0.0209(9) 0.0007(8) 0.0043(8) 0.0019(7) C303 0.0241(10) 0.0220(10) 0.0239(10) -0.0015(8) -0.0002(8) 0.0071(8) C304 0.0177(9) 0.0347(11) 0.0174(9) -0.0068(8) -0.0003(8) 0.0102(8) C305 0.0149(9) 0.0375(12) 0.0172(9) -0.0038(8) 0.0050(7) 0.0032(8) C306 0.0147(9) 0.0242(10) 0.0149(9) -0.0003(7) 0.0008(7) -0.0011(7) C311 0.0117(8) 0.0218(9) 0.0111(8) 0.0012(7) 0.0025(7) -0.0011(7) C312 0.0187(9) 0.0199(9) 0.0152(9) 0.0010(7) 0.0035(7) -0.0001(7) C313 0.0156(9) 0.0283(10) 0.0166(9) 0.0067(8) 0.0038(7) 0.0032(8) C314 0.0139(9) 0.0347(11) 0.0131(8) 0.0027(8) 0.0018(7) -0.0038(8) C315 0.0196(10) 0.0273(10) 0.0191(9) -0.0039(8) 0.0038(8) -0.0064(8) C316 0.0163(9) 0.0214(10) 0.0179(9) -0.0018(7) 0.0039(7) 0.0000(7) C321 0.0134(8) 0.0153(9) 0.0165(9) -0.0005(7) 0.0043(7) 0.0007(7) C322 0.0152(9) 0.0178(9) 0.0173(9) -0.0005(7) 0.0034(7) 0.0030(7) C323 0.0185(9) 0.0174(9) 0.0238(10) -0.0047(8) 0.0014(8) 0.0018(7) C324 0.0197(10) 0.0128(9) 0.0379(12) 0.0015(8) 0.0085(9) 0.0017(7) C325 0.0269(10) 0.0211(10) 0.0247(10) 0.0068(8) 0.0110(8) 0.0038(8) C326 0.0241(10) 0.0209(10) 0.0159(9) 0.0003(7) 0.0060(8) 0.0020(8) C331 0.0155(9) 0.0122(8) 0.0121(8) -0.0007(7) 0.0039(7) -0.0007(7) C332 0.0141(9) 0.0146(9) 0.0172(9) -0.0004(7) 0.0025(7) -0.0003(7) C333 0.0141(9) 0.0152(9) 0.0223(9) -0.0012(7) 0.0072(7) -0.0016(7) C334 0.0227(9) 0.0124(8) 0.0150(9) -0.0012(7) 0.0066(7) -0.0018(7) C335 0.0189(9) 0.0148(9) 0.0147(8) -0.0006(7) 0.0005(7) 0.0018(7) C336 0.0117(8) 0.0169(9) 0.0173(9) -0.0014(7) 0.0028(7) 0.0003(7) O400 0.0249(8) 0.0286(8) 0.0342(8) 0.0030(7) 0.0121(7) 0.0042(6) O500 0.0640(14) 0.0420(11) 0.0916(16) 0.0287(11) 0.0579(13) 0.0242(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 C31 2.0751(18) . ? Cr1 C21 2.0768(19) . ? Cr1 C61 2.0823(18) . ? Cr1 C41 2.0854(18) . ? Cr1 C11 2.0865(19) . ? Cr1 C51 2.0871(18) . ? C11 N12 1.156(2) . ? C21 N22 1.149(3) . ? C31 N32 1.149(2) . ? C41 N42 1.152(2) . ? C51 N52 1.152(2) . ? C61 N62 1.154(2) . ? P1 C121 1.7908(18) . ? P1 C101 1.7941(18) . ? P1 C111 1.7948(18) . ? P1 C131 1.8000(17) . ? C101 C106 1.390(2) . ? C101 C102 1.398(3) . ? C102 C103 1.383(3) . ? C103 C104 1.390(3) . ? C104 C105 1.381(3) . ? C105 C106 1.391(3) . ? C111 C112 1.390(3) . ? C111 C116 1.402(3) . ? C112 C113 1.389(3) . ? C113 C114 1.385(3) . ? C114 C115 1.386(3) . ? C115 C116 1.385(3) . ? C121 C122 1.391(2) . ? C121 C126 1.397(2) . ? C122 C123 1.389(3) . ? C123 C124 1.380(3) . ? C124 C125 1.388(3) . ? C125 C126 1.384(3) . ? C131 C136 1.391(2) . ? C131 C132 1.395(2) . ? C132 C133 1.388(3) . ? C133 C134 1.387(3) . ? C134 C135 1.380(3) . ? C135 C136 1.391(3) . ? P2 C221 1.7888(18) . ? P2 C201 1.7904(18) . ? P2 C211 1.7920(18) . ? P2 C231 1.7957(18) . ? C201 C206 1.393(3) . ? C201 C202 1.399(3) . ? C202 C203 1.384(3) . ? C203 C204 1.382(3) . ? C204 C205 1.382(3) . ? C205 C206 1.389(3) . ? C211 C212 1.393(3) . ? C211 C216 1.395(3) . ? C212 C213 1.390(3) . ? C213 C214 1.384(3) . ? C214 C215 1.381(3) . ? C215 C216 1.388(3) . ? C221 C222 1.393(3) . ? C221 C226 1.399(3) . ? C222 C223 1.388(3) . ? C223 C224 1.385(3) . ? C224 C225 1.386(3) . ? C225 C226 1.380(3) . ? C231 C236 1.394(2) . ? C231 C232 1.401(2) . ? C232 C233 1.384(3) . ? C233 C234 1.391(3) . ? C234 C235 1.382(3) . ? C235 C236 1.390(3) . ? P3 C321 1.7884(18) . ? P3 C331 1.7918(17) . ? P3 C311 1.7920(18) . ? P3 C301 1.7930(18) . ? C301 C306 1.393(3) . ? C301 C302 1.395(3) . ? C302 C303 1.387(3) . ? C303 C304 1.381(3) . ? C304 C305 1.382(3) . ? C305 C306 1.385(3) . ? C311 C316 1.396(3) . ? C311 C312 1.397(3) . ? C312 C313 1.389(3) . ? C313 C314 1.383(3) . ? C314 C315 1.384(3) . ? C315 C316 1.385(3) . ? C321 C322 1.393(2) . ? C321 C326 1.401(3) . ? C322 C323 1.385(3) . ? C323 C324 1.383(3) . ? C324 C325 1.386(3) . ? C325 C326 1.381(3) . ? C331 C332 1.394(2) . ? C331 C336 1.400(2) . ? C332 C333 1.386(3) . ? C333 C334 1.382(3) . ? C334 C335 1.387(3) . ? C335 C336 1.383(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 C31 Cr1 C21 94.70(7) . . ? C31 Cr1 C61 174.46(7) . . ? C21 Cr1 C61 90.83(7) . . ? C31 Cr1 C41 91.49(7) . . ? C21 Cr1 C41 173.69(7) . . ? C61 Cr1 C41 82.99(7) . . ? C31 Cr1 C11 86.05(7) . . ? C21 Cr1 C11 90.18(7) . . ? C61 Cr1 C11 93.60(7) . . ? C41 Cr1 C11 91.47(7) . . ? C31 Cr1 C51 87.74(7) . . ? C21 Cr1 C51 86.12(7) . . ? C61 Cr1 C51 92.98(7) . . ? C41 Cr1 C51 92.91(7) . . ? C11 Cr1 C51 172.49(7) . . ? N12 C11 Cr1 173.28(16) . . ? N22 C21 Cr1 177.18(16) . . ? N32 C31 Cr1 179.09(17) . . ? N42 C41 Cr1 172.79(16) . . ? N52 C51 Cr1 173.73(15) . . ? N62 C61 Cr1 172.43(16) . . ? C121 P1 C101 109.89(8) . . ? C121 P1 C111 107.52(8) . . ? C101 P1 C111 110.59(8) . . ? C121 P1 C131 110.65(8) . . ? C101 P1 C131 107.92(8) . . ? C111 P1 C131 110.28(8) . . ? C106 C101 C102 120.25(16) . . ? C106 C101 P1 120.56(14) . . ? C102 C101 P1 119.18(14) . . ? C103 C102 C101 119.66(17) . . ? C102 C103 C104 119.97(18) . . ? C105 C104 C103 120.43(17) . . ? C104 C105 C106 120.13(17) . . ? C101 C106 C105 119.55(17) . . ? C112 C111 C116 119.96(17) . . ? C112 C111 P1 121.17(14) . . ? C116 C111 P1 118.87(14) . . ? C113 C112 C111 119.46(17) . . ? C114 C113 C112 120.43(17) . . ? C113 C114 C115 120.34(18) . . ? C116 C115 C114 119.77(18) . . ? C115 C116 C111 120.03(17) . . ? C122 C121 C126 120.47(16) . . ? C122 C121 P1 120.80(14) . . ? C126 C121 P1 118.70(13) . . ? C123 C122 C121 119.40(17) . . ? C124 C123 C122 119.97(17) . . ? C123 C124 C125 120.86(17) . . ? C126 C125 C124 119.70(17) . . ? C125 C126 C121 119.60(17) . . ? C136 C131 C132 120.00(16) . . ? C136 C131 P1 122.28(14) . . ? C132 C131 P1 117.71(13) . . ? C133 C132 C131 119.82(17) . . ? C134 C133 C132 119.89(17) . . ? C135 C134 C133 120.44(17) . . ? C134 C135 C136 120.13(17) . . ? C135 C136 C131 119.71(17) . . ? C221 P2 C201 108.56(8) . . ? C221 P2 C211 110.78(8) . . ? C201 P2 C211 110.11(9) . . ? C221 P2 C231 108.05(8) . . ? C201 P2 C231 110.88(8) . . ? C211 P2 C231 108.45(8) . . ? C206 C201 C202 120.17(17) . . ? C206 C201 P2 119.60(15) . . ? C202 C201 P2 120.11(14) . . ? C203 C202 C201 119.72(19) . . ? C204 C203 C202 120.1(2) . . ? C203 C204 C205 120.26(19) . . ? C204 C205 C206 120.6(2) . . ? C205 C206 C201 119.11(19) . . ? C212 C211 C216 120.26(17) . . ? C212 C211 P2 120.40(14) . . ? C216 C211 P2 119.31(15) . . ? C213 C212 C211 119.88(19) . . ? C214 C213 C212 119.4(2) . . ? C215 C214 C213 120.93(19) . . ? C214 C215 C216 120.1(2) . . ? C215 C216 C211 119.36(19) . . ? C222 C221 C226 120.19(17) . . ? C222 C221 P2 120.99(14) . . ? C226 C221 P2 118.72(13) . . ? C223 C222 C221 119.03(18) . . ? C224 C223 C222 120.55(18) . . ? C223 C224 C225 120.47(18) . . ? C226 C225 C224 119.58(18) . . ? C225 C226 C221 120.17(17) . . ? C236 C231 C232 120.35(16) . . ? C236 C231 P2 121.40(14) . . ? C232 C231 P2 118.02(13) . . ? C233 C232 C231 119.86(17) . . ? C232 C233 C234 119.71(17) . . ? C235 C234 C233 120.43(17) . . ? C234 C235 C236 120.59(17) . . ? C235 C236 C231 119.06(17) . . ? C321 P3 C331 110.40(8) . . ? C321 P3 C311 108.79(8) . . ? C331 P3 C311 109.29(8) . . ? C321 P3 C301 110.61(8) . . ? C331 P3 C301 108.86(8) . . ? C311 P3 C301 108.87(8) . . ? C306 C301 C302 119.71(17) . . ? C306 C301 P3 120.47(14) . . ? C302 C301 P3 119.66(14) . . ? C303 C302 C301 119.67(18) . . ? C304 C303 C302 120.19(19) . . ? C303 C304 C305 120.41(18) . . ? C304 C305 C306 119.94(18) . . ? C305 C306 C301 120.08(18) . . ? C316 C311 C312 120.18(16) . . ? C316 C311 P3 119.44(14) . . ? C312 C311 P3 120.22(14) . . ? C313 C312 C311 119.43(18) . . ? C314 C313 C312 120.21(18) . . ? C313 C314 C315 120.30(17) . . ? C314 C315 C316 120.35(18) . . ? C315 C316 C311 119.52(18) . . ? C322 C321 C326 120.13(17) . . ? C322 C321 P3 119.55(14) . . ? C326 C321 P3 120.29(14) . . ? C323 C322 C321 119.37(17) . . ? C324 C323 C322 120.44(18) . . ? C323 C324 C325 120.28(18) . . ? C326 C325 C324 120.11(18) . . ? C325 C326 C321 119.63(18) . . ? C332 C331 C336 120.08(16) . . ? C332 C331 P3 119.96(13) . . ? C336 C331 P3 119.87(13) . . ? C333 C332 C331 119.77(16) . . ? C334 C333 C332 120.11(17) . . ? C333 C334 C335 120.30(17) . . ? C336 C335 C334 120.36(17) . . ? C335 C336 C331 119.39(16) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.458 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.050 #===END