# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 182/1858 data_global _publ_contact_author ; Dr Eric J.L. McInnes Deparment of Chemistry, University of Manchester, Manchester M13 9PL, U.K. ; _publ_contact_author_email mbdssejm@mail1.mcc.ac.uk _publ_contact_author_phone (+44)161-275-4469 _publ_requested_journal 'JCS Chem. Commun.' _publ_section_title ; Solvothermal synthesis of [Cr10(m2-O2CMe)10(m2-OR)20] "chromic wheels" with antiferromagnetic (R = Et) and ferromagnetic (R = Me) Cr(III)···Cr(III) interactions. ; loop_ _publ_author_name _publ_author_address 'Eric J.L. McInnes' ; Deparment of Chemistry, University of Manchester, Manchester M13 9PL, U.K. ; 'Christopher E. Anson' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ U.K. ; 'Annie K. Powell' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ U.K. ; 'Andrew J. Thompson' ; School of Chemical Sciences University of East Anglia Norwich NR4 7TJ U.K. ; 'Sandrine Poussereau' ; Universita degli Studi di Firenze, Dipartimento di Chimica, Via Maragliano 75/77, 50144 Firenze, Italy ; 'Roberta Sessoli' ; Universita degli Studi di Firenze, Dipartimento di Chimica, Via Maragliano 75/77, 50144 Firenze, Italy ; data_eric _audit_creation_method SHELXL-97 _chemical_name_systematic ; cyclo-decakis-[\m-ethanoato-bis-(\m-methoxy)chromium(III)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H90 Cr10 O40' _chemical_formula_weight 1731.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2(1)/n 1' 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 17.663(5) _cell_length_b 15.968(4) _cell_length_c 26.142(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.89(3) _cell_angle_gamma 90.00 _cell_volume 7285(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 11.42 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 1.516 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.395 _exptl_absorpt_correction_T_max 0.484 _exptl_absorpt_process_details 'XSCANS 2.2 (Siemens Corp., 1994)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 11.6 _diffrn_reflns_number 12837 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.1739 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10960 _reflns_number_gt 5064 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS 2.2 (Siemens Corp., 1994)' _computing_cell_refinement 'XSCANS 2.2 (Siemens Corp., 1994)' _computing_data_reduction 'XSCANS 2.2 (Siemens Corp., 1994)' _computing_structure_solution 'XS in SHELXTL/PC 4.11 (Siemens, 1995)' _computing_structure_refinement 'XL in SHELXTL/PC 4.11 (Siemens, 1995)' _computing_molecular_graphics 'XP in SHELXTL/PC 4.11 (Siemens, 1995)' _computing_publication_material 'XCIF in SHELXTL/PC 4.11 (Siemens, 1995)' _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^)+(0.0675P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10960 _refine_ls_number_parameters 855 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1875 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.1918 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 1.00632(11) 0.21027(12) 0.44892(7) 0.0416(5) Uani 1 1 d . . . Cr2 Cr 0.90510(11) 0.30081(12) 0.36449(6) 0.0411(5) Uani 1 1 d . A . Cr3 Cr 0.83721(11) 0.46796(12) 0.33254(7) 0.0425(5) Uani 1 1 d . A . Cr4 Cr 0.83468(12) 0.64684(12) 0.36537(7) 0.0449(6) Uani 1 1 d . A . Cr5 Cr 0.89557(11) 0.76945(11) 0.44797(6) 0.0421(5) Uani 1 1 d . A . O1 O 0.9227(4) 0.2933(4) 0.4398(3) 0.0347(18) Uani 1 1 d . . . C1A C 0.8655(13) 0.2882(15) 0.4684(8) 0.074(7) Uani 0.66 1 d P A 1 H11 H 0.8868 0.2848 0.5045 0.111 Uiso 0.66 1 calc PR A 1 H12 H 0.8353 0.2392 0.4586 0.111 Uiso 0.66 1 calc PR A 1 H13 H 0.8337 0.3371 0.4626 0.111 Uiso 0.66 1 calc PR A 1 C1B C 0.905(3) 0.355(3) 0.4771(13) 0.077(15) Uani 0.34 1 d P A 2 H14 H 0.9191 0.3337 0.5115 0.116 Uiso 0.34 1 calc PR A 2 H15 H 0.8505 0.3662 0.4711 0.116 Uiso 0.34 1 calc PR A 2 H16 H 0.9320 0.4059 0.4732 0.116 Uiso 0.34 1 calc PR A 2 O2 O 1.0077(4) 0.2509(4) 0.3790(2) 0.039(2) Uani 1 1 d . . . C2 C 1.0435(7) 0.2120(8) 0.3410(4) 0.063(4) Uani 1 1 d . A . H21 H 1.0355 0.2450 0.3100 0.094 Uiso 1 1 calc R . . H22 H 1.0220 0.1572 0.3339 0.094 Uiso 1 1 calc R . . H23 H 1.0974 0.2072 0.3532 0.094 Uiso 1 1 calc R . . O3 O 0.9319(5) 0.1208(5) 0.4237(3) 0.053(2) Uani 1 1 d . . . C3 C 0.8749(8) 0.1250(8) 0.3885(5) 0.055(4) Uani 1 1 d . A . C4 C 0.8230(8) 0.0507(9) 0.3811(5) 0.089(5) Uani 1 1 d . . . H41 H 0.7821 0.0613 0.3531 0.134 Uiso 1 1 calc R A . H42 H 0.8020 0.0406 0.4123 0.134 Uiso 1 1 calc R . . H43 H 0.8515 0.0025 0.3731 0.134 Uiso 1 1 calc R . . O4 O 0.8553(5) 0.1878(5) 0.3601(3) 0.054(2) Uani 1 1 d . . . O5 O 0.9377(4) 0.4183(4) 0.3608(3) 0.040(2) Uani 1 1 d . . . C5A C 1.0066(10) 0.4420(10) 0.3439(7) 0.056(5) Uani 0.71 1 d P A 1 H51 H 1.0114 0.5019 0.3451 0.085 Uiso 0.71 1 calc PR A 1 H52 H 1.0062 0.4229 0.3090 0.085 Uiso 0.71 1 calc PR A 1 H53 H 1.0492 0.4173 0.3660 0.085 Uiso 0.71 1 calc PR A 1 C5B C 0.994(2) 0.463(3) 0.3958(16) 0.063(13) Uiso 0.29 1 d P A 2 H54 H 0.9982 0.5191 0.3838 0.095 Uiso 0.29 1 calc PR A 2 H55 H 1.0430 0.4352 0.3973 0.095 Uiso 0.29 1 calc PR A 2 H56 H 0.9798 0.4634 0.4297 0.095 Uiso 0.29 1 calc PR A 2 O6 O 0.8053(4) 0.3603(4) 0.3577(3) 0.042(2) Uani 1 1 d . . . C6 C 0.7359(7) 0.3185(8) 0.3406(5) 0.066(4) Uani 1 1 d . A . H61 H 0.7346 0.2668 0.3593 0.099 Uiso 1 1 calc R . . H62 H 0.7319 0.3068 0.3042 0.099 Uiso 1 1 calc R . . H63 H 0.6938 0.3532 0.3466 0.099 Uiso 1 1 calc R . . O7 O 0.8981(4) 0.2935(5) 0.2884(3) 0.048(2) Uani 1 1 d . . . C7 C 0.8742(8) 0.3478(8) 0.2547(5) 0.052(4) Uani 1 1 d . A . C8 C 0.8774(9) 0.3260(8) 0.1989(4) 0.072(5) Uani 1 1 d . . . H81 H 0.8579 0.3721 0.1771 0.108 Uiso 1 1 calc R A . H82 H 0.8467 0.2772 0.1894 0.108 Uiso 1 1 calc R . . H83 H 0.9295 0.3150 0.1946 0.108 Uiso 1 1 calc R . . O8 O 0.8456(4) 0.4187(5) 0.2644(3) 0.044(2) Uani 1 1 d . . . O9 O 0.8256(4) 0.5347(5) 0.3937(3) 0.045(2) Uani 1 1 d . . . C9 C 0.7727(10) 0.5155(10) 0.4266(6) 0.109(6) Uani 1 1 d . A . H91 H 0.7774 0.4575 0.4361 0.164 Uiso 1 1 calc R . . H92 H 0.7218 0.5262 0.4090 0.164 Uiso 1 1 calc R . . H93 H 0.7827 0.5496 0.4571 0.164 Uiso 1 1 calc R . . O10 O 0.8790(4) 0.5772(4) 0.3149(3) 0.042(2) Uani 1 1 d . . . C10 C 0.8880(9) 0.6029(8) 0.2639(4) 0.082(5) Uani 1 1 d . A . H101 H 0.9094 0.6582 0.2651 0.123 Uiso 1 1 calc R . . H102 H 0.8389 0.6029 0.2421 0.123 Uiso 1 1 calc R . . H103 H 0.9217 0.5647 0.2501 0.123 Uiso 1 1 calc R . . O11 O 0.7321(4) 0.5020(5) 0.3003(3) 0.049(2) Uani 1 1 d . . . C11 C 0.7003(7) 0.5722(9) 0.3022(4) 0.048(4) Uani 1 1 d . A . C12 C 0.6210(7) 0.5838(9) 0.2725(5) 0.090(5) Uani 1 1 d . . . H121 H 0.6035 0.5321 0.2561 0.135 Uiso 1 1 calc R A . H122 H 0.6220 0.6263 0.2466 0.135 Uiso 1 1 calc R . . H123 H 0.5868 0.6006 0.2958 0.135 Uiso 1 1 calc R . . O12 O 0.7309(5) 0.6354(5) 0.3258(3) 0.055(2) Uani 1 1 d . . . O13 O 0.9318(4) 0.6773(5) 0.4090(3) 0.037(2) Uani 1 1 d . . . C13A C 0.9996(15) 0.6815(14) 0.3889(9) 0.076(8) Uani 0.60 1 d PU A 1 H131 H 1.0070 0.6302 0.3712 0.114 Uiso 0.60 1 calc PR A 1 H132 H 1.0415 0.6898 0.4165 0.114 Uiso 0.60 1 calc PR A 1 H133 H 0.9973 0.7274 0.3650 0.114 Uiso 0.60 1 calc PR A 1 C13B C 0.9947(18) 0.622(2) 0.4275(13) 0.063(10) Uani 0.40 1 d PU A 2 H134 H 1.0011 0.5820 0.4010 0.095 Uiso 0.40 1 calc PR A 2 H135 H 0.9841 0.5927 0.4578 0.095 Uiso 0.40 1 calc PR A 2 H136 H 1.0409 0.6540 0.4362 0.095 Uiso 0.40 1 calc PR A 2 O14 O 0.8008(4) 0.7100(5) 0.4208(3) 0.041(2) Uani 1 1 d . . . C14 C 0.7273(8) 0.7421(9) 0.4230(5) 0.074(5) Uani 1 1 d . A . H141 H 0.7274 0.7708 0.4553 0.111 Uiso 1 1 calc R . . H142 H 0.6910 0.6969 0.4204 0.111 Uiso 1 1 calc R . . H143 H 0.7131 0.7804 0.3949 0.111 Uiso 1 1 calc R . . O15 O 0.8450(6) 0.7501(5) 0.3234(3) 0.065(3) Uani 1 1 d . . . C15 C 0.8712(7) 0.8194(7) 0.3382(5) 0.044(3) Uani 1 1 d . A . C16 C 0.8801(9) 0.8823(9) 0.2971(5) 0.086(5) Uani 1 1 d . . . H161 H 0.9010 0.9332 0.3129 0.130 Uiso 1 1 calc R A . H162 H 0.8310 0.8935 0.2769 0.130 Uiso 1 1 calc R . . H163 H 0.9141 0.8604 0.2750 0.130 Uiso 1 1 calc R . . O16 O 0.8900(5) 0.8406(5) 0.3848(3) 0.060(3) Uani 1 1 d . . . O17 O 0.9143(4) 0.7142(4) 0.5159(2) 0.0352(18) Uani 1 1 d . . . C17A C 0.8589(12) 0.6796(15) 0.5400(8) 0.065(7) Uani 0.62 1 d P A 1 H171 H 0.8819 0.6562 0.5726 0.098 Uiso 0.62 1 calc PR A 1 H172 H 0.8332 0.6361 0.5186 0.098 Uiso 0.62 1 calc PR A 1 H173 H 0.8226 0.7219 0.5458 0.098 Uiso 0.62 1 calc PR A 1 C17B C 0.900(2) 0.628(2) 0.5273(14) 0.069(12) Uiso 0.38 1 d P A 2 H174 H 0.9157 0.6178 0.5637 0.103 Uiso 0.38 1 calc PR A 2 H175 H 0.9296 0.5924 0.5079 0.103 Uiso 0.38 1 calc PR A 2 H176 H 0.8469 0.6156 0.5179 0.103 Uiso 0.38 1 calc PR A 2 O18 O 0.9959(4) 0.8158(5) 0.4777(3) 0.042(2) Uani 1 1 d . . . C18 C 1.0307(7) 0.8880(9) 0.4588(5) 0.073(5) Uani 1 1 d . A . H181 H 1.0241 0.8861 0.4216 0.110 Uiso 1 1 calc R . . H182 H 1.0843 0.8887 0.4724 0.110 Uiso 1 1 calc R . . H183 H 1.0069 0.9377 0.4695 0.110 Uiso 1 1 calc R . . O19 O 0.8422(5) 0.8627(5) 0.4773(3) 0.048(2) Uani 1 1 d . . . C19 C 0.8556(8) 0.8958(7) 0.5221(5) 0.049(3) Uani 1 1 d . A . C20 C 0.8029(7) 0.9628(7) 0.5361(4) 0.061(4) Uani 1 1 d . . . H201 H 0.8203 0.9816 0.5707 0.092 Uiso 1 1 calc R A . H202 H 0.7520 0.9406 0.5338 0.092 Uiso 1 1 calc R . . H203 H 0.8027 1.0089 0.5125 0.092 Uiso 1 1 calc R . . O20 O 0.9140(5) 0.8760(4) 0.5559(3) 0.049(2) Uani 1 1 d . . . Cr6 Cr 0.61539(11) 0.64250(12) 0.65311(7) 0.0422(5) Uani 1 1 d . . . Cr7 Cr 0.52952(11) 0.76899(12) 0.58199(6) 0.0430(5) Uani 1 1 d . B . Cr8 Cr 0.42942(11) 0.79599(12) 0.48020(6) 0.0430(5) Uani 1 1 d . B . Cr9 Cr 0.35459(11) 0.70560(12) 0.38559(7) 0.0428(5) Uani 1 1 d . B . Cr10 Cr 0.33919(11) 0.53758(12) 0.33447(7) 0.0423(5) Uani 1 1 d . B . O21 O 0.6004(4) 0.6749(5) 0.5794(3) 0.039(2) Uani 1 1 d . . . C21A C 0.6616(14) 0.6745(13) 0.5498(7) 0.078(7) Uani 0.67 1 d P B 1 H211 H 0.6882 0.6220 0.5544 0.117 Uiso 0.67 1 calc PR B 1 H212 H 0.6965 0.7193 0.5612 0.117 Uiso 0.67 1 calc PR B 1 H213 H 0.6414 0.6821 0.5138 0.117 Uiso 0.67 1 calc PR B 1 C21B C 0.609(3) 0.630(3) 0.5395(18) 0.094(18) Uiso 0.33 1 d P B 2 H214 H 0.6466 0.5873 0.5495 0.141 Uiso 0.33 1 calc PR B 2 H215 H 0.6249 0.6647 0.5133 0.141 Uiso 0.33 1 calc PR B 2 H216 H 0.5608 0.6036 0.5260 0.141 Uiso 0.33 1 calc PR B 2 O22 O 0.5196(4) 0.7084(5) 0.6461(2) 0.042(2) Uani 1 1 d . . . C22 C 0.4834(7) 0.7376(9) 0.6853(4) 0.065(4) Uani 1 1 d . B . H221 H 0.4865 0.6962 0.7122 0.097 Uiso 1 1 calc R . . H222 H 0.4306 0.7487 0.6721 0.097 Uiso 1 1 calc R . . H223 H 0.5078 0.7882 0.6991 0.097 Uiso 1 1 calc R . . O23 O 0.6800(5) 0.7440(6) 0.6706(3) 0.059(3) Uani 1 1 d . . . C23 C 0.6731(7) 0.8142(9) 0.6493(5) 0.051(4) Uani 1 1 d . B . C24 C 0.7348(6) 0.8788(7) 0.6673(5) 0.059(4) Uani 1 1 d . . . H241 H 0.7236 0.9298 0.6482 0.088 Uiso 1 1 calc R B . H242 H 0.7838 0.8577 0.6616 0.088 Uiso 1 1 calc R . . H243 H 0.7361 0.8895 0.7036 0.088 Uiso 1 1 calc R . . O24 O 0.6179(4) 0.8381(5) 0.6155(3) 0.049(2) Uani 1 1 d . . . O25 O 0.4393(4) 0.7196(5) 0.5392(2) 0.040(2) Uani 1 1 d . . . C25A C 0.3768(10) 0.6828(14) 0.5587(8) 0.058(6) Uani 0.63 1 d P B 1 H251 H 0.3955 0.6476 0.5877 0.087 Uiso 0.63 1 calc PR B 1 H252 H 0.3473 0.6497 0.5321 0.087 Uiso 0.63 1 calc PR B 1 H253 H 0.3449 0.7260 0.5695 0.087 Uiso 0.63 1 calc PR B 1 C25B C 0.413(2) 0.638(2) 0.5410(14) 0.065(11) Uiso 0.37 1 d P B 2 H254 H 0.4270 0.6163 0.5754 0.097 Uiso 0.37 1 calc PR B 2 H255 H 0.4357 0.6041 0.5171 0.097 Uiso 0.37 1 calc PR B 2 H256 H 0.3583 0.6373 0.5318 0.097 Uiso 0.37 1 calc PR B 2 O26 O 0.5347(4) 0.8173(5) 0.5136(3) 0.042(2) Uani 1 1 d . . . C26 C 0.5791(7) 0.8901(8) 0.5047(4) 0.072(5) Uani 1 1 d . B . H261 H 0.6288 0.8865 0.5255 0.107 Uiso 1 1 calc R . . H262 H 0.5534 0.9396 0.5141 0.107 Uiso 1 1 calc R . . H263 H 0.5845 0.8929 0.4688 0.107 Uiso 1 1 calc R . . O27 O 0.4654(5) 0.8636(5) 0.5989(3) 0.053(2) Uani 1 1 d . . . C27 C 0.4114(7) 0.8996(8) 0.5703(5) 0.046(3) Uani 1 1 d . B . C28 C 0.3726(8) 0.9679(8) 0.5943(4) 0.071(4) Uani 1 1 d . . . H281 H 0.3327 0.9910 0.5692 0.106 Uiso 1 1 calc R B . H282 H 0.4091 1.0109 0.6062 0.106 Uiso 1 1 calc R . . H283 H 0.3509 0.9462 0.6231 0.106 Uiso 1 1 calc R . . O28 O 0.3885(5) 0.8841(5) 0.5228(3) 0.053(2) Uani 1 1 d . . . O29 O 0.4539(4) 0.7130(4) 0.4310(3) 0.0368(19) Uani 1 1 d . . . C29A C 0.5238(9) 0.7154(12) 0.4122(7) 0.059(5) Uani 0.70 1 d P B 1 H291 H 0.5260 0.6699 0.3884 0.089 Uiso 0.70 1 calc PR B 1 H292 H 0.5651 0.7102 0.4405 0.089 Uiso 0.70 1 calc PR B 1 H293 H 0.5283 0.7676 0.3947 0.089 Uiso 0.70 1 calc PR B 1 C29B C 0.507(2) 0.641(3) 0.4415(15) 0.057(12) Uiso 0.31 1 d P B 2 H294 H 0.5086 0.6101 0.4100 0.085 Uiso 0.31 1 calc PR B 2 H295 H 0.4902 0.6045 0.4667 0.085 Uiso 0.31 1 calc PR B 2 H296 H 0.5580 0.6608 0.4545 0.085 Uiso 0.31 1 calc PR B 2 O30 O 0.3273(5) 0.7589(5) 0.4479(3) 0.047(2) Uani 1 1 d . . . C30 C 0.2605(7) 0.8075(9) 0.4475(5) 0.070(4) Uani 1 1 d . B . H301 H 0.2171 0.7776 0.4297 0.106 Uiso 1 1 calc R . . H302 H 0.2660 0.8595 0.4300 0.106 Uiso 1 1 calc R . . H303 H 0.2528 0.8185 0.4824 0.106 Uiso 1 1 calc R . . O31 O 0.4329(5) 0.8848(5) 0.4264(3) 0.050(2) Uani 1 1 d . . . C31 C 0.4075(7) 0.8789(8) 0.3783(5) 0.050(3) Uani 1 1 d . B . C32 C 0.4211(8) 0.9533(7) 0.3445(4) 0.068(4) Uani 1 1 d . . . H321 H 0.4470 0.9967 0.3658 0.102 Uiso 1 1 calc R B . H322 H 0.3728 0.9739 0.3273 0.102 Uiso 1 1 calc R . . H323 H 0.4520 0.9361 0.3193 0.102 Uiso 1 1 calc R . . O32 O 0.3738(5) 0.8164(5) 0.3558(3) 0.053(2) Uani 1 1 d . . . O33 O 0.3347(4) 0.5888(5) 0.4022(3) 0.041(2) Uani 1 1 d . . . C33 C 0.2776(10) 0.5662(8) 0.4318(5) 0.093(6) Uani 1 1 d . B . H331 H 0.2769 0.5064 0.4356 0.139 Uiso 1 1 calc R . . H332 H 0.2286 0.5849 0.4146 0.139 Uiso 1 1 calc R . . H333 H 0.2885 0.5918 0.4654 0.139 Uiso 1 1 calc R . . O34 O 0.3916(4) 0.6442(5) 0.3298(3) 0.046(2) Uani 1 1 d . . . C34 C 0.4051(8) 0.6820(8) 0.2820(4) 0.065(4) Uani 1 1 d . B . H341 H 0.4317 0.7341 0.2892 0.097 Uiso 1 1 calc R . . H342 H 0.3570 0.6921 0.2602 0.097 Uiso 1 1 calc R . . H343 H 0.4357 0.6450 0.2646 0.097 Uiso 1 1 calc R . . O35 O 0.2494(4) 0.7141(5) 0.3463(3) 0.052(2) Uani 1 1 d . . . C35 C 0.2122(7) 0.6597(8) 0.3185(5) 0.045(3) Uani 1 1 d . B . C36 C 0.1320(7) 0.6796(8) 0.2944(4) 0.065(4) Uani 1 1 d . . . H361 H 0.1106 0.6328 0.2741 0.098 Uiso 1 1 calc R B . H362 H 0.1321 0.7279 0.2725 0.098 Uiso 1 1 calc R . . H363 H 0.1016 0.6910 0.3210 0.098 Uiso 1 1 calc R . . O36 O 0.2385(4) 0.5897(5) 0.3064(3) 0.045(2) Uani 1 1 d . . . O37 O 0.4312(4) 0.4687(5) 0.3571(3) 0.039(2) Uani 1 1 d . . . C37A C 0.5050(15) 0.4864(15) 0.3405(10) 0.069(9) Uani 0.50 1 d P B 1 H371 H 0.5191 0.5436 0.3484 0.103 Uiso 0.50 1 calc PR B 1 H372 H 0.5010 0.4775 0.3039 0.103 Uiso 0.50 1 calc PR B 1 H373 H 0.5435 0.4499 0.3584 0.103 Uiso 0.50 1 calc PR B 1 C37B C 0.4899(16) 0.4912(16) 0.3990(10) 0.076(10) Uani 0.50 1 d PU B 2 H374 H 0.5036 0.5489 0.3957 0.115 Uiso 0.50 1 calc PR B 2 H375 H 0.5341 0.4565 0.3982 0.115 Uiso 0.50 1 calc PR B 2 H376 H 0.4713 0.4832 0.4313 0.115 Uiso 0.50 1 calc PR B 2 O38 O 0.2930(4) 0.4294(5) 0.3475(3) 0.039(2) Uani 1 1 d . . . C38 C 0.2177(7) 0.4060(9) 0.3255(6) 0.086(5) Uani 1 1 d . B . H381 H 0.2070 0.3508 0.3370 0.129 Uiso 1 1 calc R . . H382 H 0.2132 0.4065 0.2885 0.129 Uiso 1 1 calc R . . H383 H 0.1818 0.4450 0.3362 0.129 Uiso 1 1 calc R . . O39 O 0.3452(5) 0.5054(5) 0.2613(3) 0.051(2) Uani 1 1 d . . . C39 C 0.3640(8) 0.4353(9) 0.2444(5) 0.057(4) Uani 1 1 d . B . C40 C 0.3630(4) 0.4284(4) 0.1865(2) 0.106(7) Uani 1 1 d U . . H401 H 0.3493 0.4815 0.1705 0.159 Uiso 1 1 calc R B . H402 H 0.3262 0.3869 0.1725 0.159 Uiso 1 1 calc R . . H403 H 0.4130 0.4123 0.1798 0.159 Uiso 1 1 calc R . . O40 O 0.3809(4) 0.3715(4) 0.2707(2) 0.054(2) Uani 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0553(13) 0.0340(12) 0.0317(10) -0.0012(9) -0.0056(9) 0.0000(10) Cr2 0.0549(13) 0.0344(12) 0.0295(10) -0.0008(9) -0.0072(9) -0.0006(10) Cr3 0.0531(13) 0.0389(12) 0.0311(10) -0.0033(9) -0.0074(10) 0.0044(11) Cr4 0.0629(14) 0.0368(12) 0.0305(10) -0.0022(9) -0.0069(10) 0.0038(11) Cr5 0.0597(13) 0.0338(11) 0.0282(10) -0.0005(9) -0.0077(9) 0.0021(10) O1 0.040(5) 0.029(4) 0.036(4) -0.003(4) 0.008(4) -0.001(4) C1A 0.10(2) 0.064(17) 0.055(14) 0.019(14) -0.002(14) 0.001(16) C1B 0.14(4) 0.06(3) 0.03(2) -0.01(2) -0.01(3) 0.05(3) O2 0.048(5) 0.038(5) 0.028(4) -0.002(4) -0.004(4) 0.014(4) C2 0.076(10) 0.066(10) 0.042(7) -0.009(7) -0.007(7) 0.027(8) O3 0.060(6) 0.033(5) 0.059(5) 0.008(4) -0.012(5) -0.009(4) C3 0.061(10) 0.048(9) 0.050(8) -0.013(7) -0.014(7) -0.007(8) C4 0.075(11) 0.077(12) 0.098(12) 0.005(10) -0.038(10) -0.033(9) O4 0.059(6) 0.038(5) 0.056(5) 0.000(5) -0.013(5) -0.009(5) O5 0.047(5) 0.038(5) 0.032(4) -0.003(4) -0.006(4) -0.004(4) C5A 0.060(13) 0.041(11) 0.072(14) 0.007(10) 0.023(11) -0.001(10) O6 0.045(5) 0.032(5) 0.043(5) 0.001(4) -0.008(4) -0.004(4) C6 0.047(9) 0.054(9) 0.095(11) -0.008(8) 0.003(8) -0.019(7) O7 0.062(6) 0.037(5) 0.040(5) -0.010(4) -0.011(4) 0.007(5) C7 0.071(10) 0.034(8) 0.046(8) -0.019(7) -0.010(7) 0.010(7) C8 0.131(14) 0.054(9) 0.033(7) -0.002(7) 0.016(8) 0.009(9) O8 0.062(6) 0.042(5) 0.026(4) -0.009(4) -0.002(4) 0.008(4) O9 0.057(6) 0.041(5) 0.033(4) 0.006(4) -0.005(4) -0.002(4) C9 0.176(19) 0.069(12) 0.082(12) -0.003(10) 0.021(13) -0.007(13) O10 0.062(6) 0.032(5) 0.032(4) -0.003(4) 0.009(4) 0.009(4) C10 0.157(16) 0.052(9) 0.040(8) 0.005(7) 0.028(9) 0.001(10) O11 0.052(6) 0.054(6) 0.032(5) -0.007(4) -0.021(4) 0.013(5) C11 0.049(8) 0.065(10) 0.024(6) -0.002(6) -0.012(6) 0.027(8) C12 0.056(10) 0.080(11) 0.116(13) -0.026(10) -0.041(9) 0.030(9) O12 0.064(6) 0.048(6) 0.040(5) -0.020(4) -0.027(4) 0.005(5) O13 0.034(5) 0.037(5) 0.038(4) 0.001(4) -0.002(4) 0.005(4) C13A 0.11(2) 0.047(16) 0.065(16) -0.045(13) -0.010(16) -0.016(15) C13B 0.06(2) 0.05(2) 0.09(3) -0.03(2) 0.02(2) 0.022(19) O14 0.039(5) 0.038(5) 0.041(5) -0.008(4) -0.007(4) 0.009(4) C14 0.081(11) 0.090(12) 0.050(8) -0.027(8) 0.008(8) 0.012(9) O15 0.121(8) 0.026(5) 0.041(5) 0.008(4) -0.013(5) 0.006(5) C15 0.065(9) 0.018(7) 0.048(8) 0.010(6) 0.001(7) 0.011(6) C16 0.129(14) 0.084(12) 0.044(8) 0.020(8) 0.005(9) -0.007(11) O16 0.107(7) 0.036(5) 0.031(4) 0.003(4) -0.010(5) -0.012(5) O17 0.047(5) 0.026(4) 0.031(4) -0.001(4) -0.002(4) -0.004(4) C17A 0.049(14) 0.076(18) 0.060(14) -0.002(13) -0.026(12) -0.029(14) O18 0.051(5) 0.041(5) 0.031(4) 0.000(4) 0.000(4) -0.005(4) C18 0.067(10) 0.088(12) 0.063(9) 0.013(9) 0.001(8) -0.046(9) O19 0.068(6) 0.040(5) 0.028(4) -0.003(4) -0.013(4) 0.016(4) C19 0.066(9) 0.026(7) 0.056(9) 0.021(7) 0.012(8) 0.010(7) C20 0.059(9) 0.051(9) 0.066(9) -0.017(7) -0.012(7) 0.019(7) O20 0.072(6) 0.034(5) 0.038(5) -0.002(4) -0.001(4) 0.022(4) Cr6 0.0531(13) 0.0376(12) 0.0309(10) 0.0023(9) -0.0091(10) -0.0003(10) Cr7 0.0561(13) 0.0360(12) 0.0314(10) 0.0009(9) -0.0101(10) -0.0007(10) Cr8 0.0525(13) 0.0395(12) 0.0322(10) 0.0033(9) -0.0087(9) 0.0008(10) Cr9 0.0539(13) 0.0362(12) 0.0333(10) 0.0032(9) -0.0091(9) -0.0012(10) Cr10 0.0538(13) 0.0379(12) 0.0310(10) 0.0035(9) -0.0070(10) -0.0005(11) O21 0.054(5) 0.038(5) 0.025(4) -0.004(4) 0.002(4) -0.001(4) C21A 0.12(2) 0.063(16) 0.055(14) 0.039(12) 0.017(15) 0.004(15) O22 0.053(5) 0.047(5) 0.024(4) 0.001(4) -0.004(4) 0.008(4) C22 0.059(9) 0.103(12) 0.028(6) 0.005(8) -0.006(6) 0.013(8) O23 0.061(6) 0.053(6) 0.052(5) 0.009(5) -0.023(5) 0.001(5) C23 0.037(8) 0.069(11) 0.046(8) -0.003(8) 0.000(7) -0.003(8) C24 0.043(8) 0.054(9) 0.071(9) 0.003(7) -0.019(7) -0.013(7) O24 0.052(5) 0.035(5) 0.053(5) 0.001(4) -0.016(4) -0.017(4) O25 0.041(5) 0.045(5) 0.033(4) 0.002(4) -0.005(4) -0.006(4) C25A 0.019(11) 0.083(17) 0.072(15) 0.004(13) 0.004(10) 0.000(12) O26 0.049(5) 0.039(5) 0.036(4) 0.001(4) -0.006(4) -0.007(4) C26 0.066(10) 0.085(11) 0.054(8) 0.041(8) -0.022(7) -0.028(9) O27 0.074(6) 0.046(5) 0.035(5) -0.004(4) -0.008(5) 0.015(5) C27 0.042(8) 0.048(8) 0.054(8) -0.001(7) 0.021(7) 0.005(7) C28 0.087(11) 0.076(11) 0.052(8) -0.011(8) 0.018(8) 0.009(9) O28 0.070(6) 0.054(6) 0.030(4) 0.000(4) -0.010(4) 0.018(5) O29 0.033(5) 0.035(5) 0.039(4) 0.002(4) -0.005(4) 0.007(4) C29A 0.037(12) 0.070(15) 0.067(13) -0.019(12) -0.003(10) -0.001(11) O30 0.055(5) 0.044(5) 0.038(5) -0.008(4) -0.004(4) -0.005(4) C30 0.055(9) 0.086(12) 0.066(9) -0.001(9) -0.005(8) 0.010(9) O31 0.075(6) 0.043(5) 0.027(4) 0.009(4) -0.011(4) -0.002(5) C31 0.060(9) 0.052(9) 0.040(8) 0.016(7) 0.013(7) 0.005(7) C32 0.114(12) 0.038(8) 0.045(8) 0.012(7) -0.011(8) -0.005(8) O32 0.070(6) 0.042(6) 0.041(5) 0.005(4) -0.014(4) 0.000(5) O33 0.043(5) 0.048(5) 0.032(4) 0.004(4) 0.001(4) -0.008(4) C33 0.148(16) 0.048(10) 0.074(11) -0.017(8) -0.008(12) -0.004(11) O34 0.059(5) 0.044(5) 0.030(4) 0.006(4) -0.003(4) -0.010(4) C34 0.102(12) 0.052(9) 0.042(8) 0.005(7) 0.015(8) -0.016(8) O35 0.052(5) 0.046(6) 0.051(5) 0.006(4) -0.015(4) 0.003(5) C35 0.052(9) 0.044(9) 0.039(7) 0.005(7) 0.006(7) -0.003(7) C36 0.056(9) 0.068(10) 0.060(8) 0.005(7) -0.031(7) -0.002(8) O36 0.041(5) 0.049(5) 0.037(5) -0.002(4) -0.018(4) 0.004(4) O37 0.044(5) 0.044(5) 0.025(4) 0.004(4) -0.004(4) 0.005(4) C37A 0.09(2) 0.044(18) 0.07(2) 0.016(15) 0.005(18) -0.019(16) C37B 0.09(2) 0.06(2) 0.07(2) 0.029(17) -0.023(18) -0.032(17) O38 0.034(5) 0.043(5) 0.039(5) -0.001(4) -0.001(4) 0.005(4) C38 0.057(10) 0.068(11) 0.128(14) 0.017(10) -0.002(10) 0.001(9) O39 0.075(6) 0.040(5) 0.034(5) 0.006(4) -0.007(4) 0.007(5) C39 0.078(11) 0.054(9) 0.035(8) 0.011(7) -0.004(7) -0.005(8) C40 0.20(2) 0.083(12) 0.037(8) 0.014(8) 0.021(11) 0.050(13) O40 0.081(6) 0.046(6) 0.030(4) 0.002(4) -0.007(4) 0.007(5) _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 O17 1.966(7) 3_766 ? Cr1 O18 1.968(7) 3_766 ? Cr1 O20 1.988(8) 3_766 ? Cr1 O1 1.971(7) . yes O1 Cr2 1.948(7) . yes Cr1 O2 1.942(7) . yes O2 Cr2 1.963(7) . yes Cr1 O3 1.984(8) . yes O4 Cr2 2.003(8) . yes Cr2 O5 1.969(7) . yes O5 Cr3 1.980(7) . yes Cr2 O6 1.985(8) . yes O6 Cr3 1.954(7) . yes Cr2 O7 1.977(7) . yes O8 Cr3 1.973(7) . yes Cr3 O9 1.960(8) . yes O9 Cr4 1.954(8) . yes Cr3 O10 1.977(8) . yes O10 Cr4 1.978(7) . yes Cr3 O11 1.992(8) . yes O12 Cr4 1.969(8) . yes Cr4 O13 1.969(7) . yes O13 Cr5 1.953(8) . yes Cr4 O14 1.935(7) . yes O14 Cr5 1.959(7) . yes Cr4 O15 2.005(8) . yes O16 Cr5 1.994(8) . yes Cr5 O17 1.965(7) . yes O17 Cr1 1.966(7) 3_766 yes Cr5 O18 1.966(7) . yes O18 Cr1 1.968(7) 3_766 yes Cr5 O19 1.979(8) . yes O20 Cr1 1.988(8) 3_766 yes O1 C1A 1.35(2) . ? O1 C1B 1.46(3) . ? O2 C2 1.402(12) . ? O3 C3 1.258(12) . ? C3 O4 1.263(13) . ? C3 C4 1.493(16) . ? O5 C5A 1.411(17) . ? O5 C5B 1.43(4) . ? O6 C6 1.408(12) . ? O7 C7 1.263(13) . ? C7 O8 1.281(12) . ? C7 C8 1.510(14) . ? O9 C9 1.397(16) . ? O10 C10 1.426(12) . ? O11 C11 1.258(13) . ? C11 O12 1.260(13) . ? C11 C12 1.506(15) . ? O13 C13A 1.38(3) . ? O13 C13B 1.44(3) . ? O14 C14 1.406(13) . ? O15 C15 1.239(13) . ? C15 O16 1.258(12) . ? C15 C16 1.498(15) . ? O17 C17A 1.36(2) . ? O17 C17B 1.44(4) . ? O18 C18 1.431(13) . ? O19 C19 1.274(13) . ? C19 O20 1.289(13) . ? C19 C20 1.499(15) . ? Cr6 O37 1.958(8) 3_666 ? Cr6 O38 1.987(7) 3_666 ? Cr6 O40 1.994(7) 3_666 ? Cr6 O21 1.972(7) . yes O21 Cr7 1.963(8) . yes Cr6 O22 1.977(7) . yes O22 Cr7 1.965(7) . yes Cr6 O23 1.995(9) . yes O24 Cr7 2.000(7) . yes Cr7 O25 1.965(7) . yes O25 Cr8 1.953(7) . yes Cr7 O26 1.963(7) . yes O26 Cr8 1.958(7) . yes Cr7 O27 1.979(8) . yes O28 Cr8 1.998(8) . yes Cr8 O29 1.941(7) . yes O29 Cr9 1.964(7) . yes Cr8 O30 1.961(8) . yes O30 Cr9 1.962(8) . yes Cr8 O31 2.005(7) . yes O32 Cr9 1.984(8) . yes Cr9 O33 1.960(8) . yes O33 Cr10 1.963(7) . yes Cr9 O34 1.952(8) . yes O34 Cr10 1.951(8) . yes Cr9 O35 1.984(8) . yes O36 Cr10 1.998(7) . yes Cr10 O37 1.976(7) . yes O37 Cr6 1.958(8) 3_666 yes? Cr10 O38 1.963(8) . yes O38 Cr6 1.987(7) 3_666 yes Cr10 O39 2.000(8) . yes O40 Cr6 1.994(7) 3_666 yes O21 C21B 1.30(5) . ? O21 C21A 1.43(2) . ? O22 C22 1.371(12) . ? O23 C23 1.249(14) . ? C23 O24 1.270(13) . ? C23 C24 1.521(15) . ? O25 C25B 1.39(4) . ? O25 C25A 1.414(19) . ? O26 C26 1.440(13) . ? O27 C27 1.257(13) . ? C27 O28 1.268(13) . ? C27 C28 1.479(15) . ? O29 C29A 1.398(17) . ? O29 C29B 1.49(4) . ? O30 C30 1.412(13) . ? O31 C31 1.272(12) . ? C31 O32 1.260(13) . ? C31 C32 1.520(15) . ? O33 C33 1.409(16) . ? O34 C34 1.440(12) . ? O35 C35 1.253(13) . ? C35 O36 1.270(13) . ? C35 C36 1.493(15) . ? O37 C37B 1.43(2) . ? O37 C37A 1.46(3) . ? O38 C38 1.415(13) . ? O39 C39 1.266(14) . ? C39 O40 1.239(13) . ? C39 C40 1.517(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cr1 O17 97.1(3) . 3_766 ? O2 Cr1 O18 172.7(3) . 3_766 ? O17 Cr1 O18 78.1(3) 3_766 3_766 ? O2 Cr1 O1 77.3(3) . . ? O17 Cr1 O1 96.4(3) 3_766 . ? O18 Cr1 O1 97.7(3) 3_766 . ? O2 Cr1 O3 91.8(3) . . ? O17 Cr1 O3 170.0(3) 3_766 . ? O18 Cr1 O3 93.4(3) 3_766 . ? O1 Cr1 O3 89.9(3) . . ? O2 Cr1 O20 93.4(3) . 3_766 ? O17 Cr1 O20 89.7(3) 3_766 3_766 ? O18 Cr1 O20 92.0(3) 3_766 3_766 ? O1 Cr1 O20 169.4(3) . 3_766 ? O3 Cr1 O20 85.4(3) . 3_766 ? O1 Cr2 O2 77.3(3) . . ? O1 Cr2 O5 96.0(3) . . ? O2 Cr2 O5 97.4(3) . . ? O1 Cr2 O7 171.1(3) . . ? O2 Cr2 O7 94.8(3) . . ? O5 Cr2 O7 88.9(3) . . ? O1 Cr2 O6 96.9(3) . . ? O2 Cr2 O6 172.7(3) . . ? O5 Cr2 O6 78.6(3) . . ? O7 Cr2 O6 91.3(3) . . ? O1 Cr2 O4 90.1(3) . . ? O2 Cr2 O4 91.7(3) . . ? O5 Cr2 O4 169.9(3) . . ? O7 Cr2 O4 86.0(3) . . ? O6 Cr2 O4 92.8(3) . . ? O6 Cr3 O9 97.6(3) . . ? O6 Cr3 O8 91.1(3) . . ? O9 Cr3 O8 170.3(3) . . ? O6 Cr3 O10 173.0(3) . . ? O9 Cr3 O10 78.5(3) . . ? O8 Cr3 O10 93.3(3) . . ? O6 Cr3 O5 79.0(3) . . ? O9 Cr3 O5 96.5(3) . . ? O8 Cr3 O5 89.4(3) . . ? O10 Cr3 O5 95.5(3) . . ? O6 Cr3 O11 94.8(3) . . ? O9 Cr3 O11 89.3(3) . . ? O8 Cr3 O11 85.5(3) . . ? O10 Cr3 O11 91.0(3) . . ? O5 Cr3 O11 172.0(3) . . ? O14 Cr4 O9 98.1(3) . . ? O14 Cr4 O12 94.1(3) . . ? O9 Cr4 O12 89.4(3) . . ? O14 Cr4 O13 77.3(3) . . ? O9 Cr4 O13 97.0(3) . . ? O12 Cr4 O13 169.9(3) . . ? O14 Cr4 O10 173.3(3) . . ? O9 Cr4 O10 78.6(3) . . ? O12 Cr4 O10 91.7(3) . . ? O13 Cr4 O10 97.3(3) . . ? O14 Cr4 O15 92.6(3) . . ? O9 Cr4 O15 168.9(3) . . ? O12 Cr4 O15 86.8(4) . . ? O13 Cr4 O15 88.3(3) . . ? O10 Cr4 O15 91.1(3) . . ? O13 Cr5 O14 77.1(3) . . ? O13 Cr5 O17 96.3(3) . . ? O14 Cr5 O17 97.2(3) . . ? O13 Cr5 O18 98.2(3) . . ? O14 Cr5 O18 173.1(3) . . ? O17 Cr5 O18 78.2(3) . . ? O13 Cr5 O19 169.4(3) . . ? O14 Cr5 O19 94.2(3) . . ? O17 Cr5 O19 90.6(3) . . ? O18 Cr5 O19 91.0(3) . . ? O13 Cr5 O16 88.6(3) . . ? O14 Cr5 O16 92.6(3) . . ? O17 Cr5 O16 169.8(3) . . ? O18 Cr5 O16 92.3(3) . . ? O19 Cr5 O16 85.8(3) . . ? C1A O1 C1B 54(2) . . ? C1A O1 Cr2 123.2(10) . . ? C1B O1 Cr2 128.1(15) . . ? C1A O1 Cr1 120.2(10) . . ? C1B O1 Cr1 127.8(15) . . ? Cr2 O1 Cr1 99.4(3) . . yes C2 O2 Cr1 126.3(6) . . ? C2 O2 Cr2 123.1(6) . . ? Cr1 O2 Cr2 99.9(3) . . yes C3 O3 Cr1 128.2(8) . . ? O3 C3 O4 126.1(12) . . ? O3 C3 C4 117.2(12) . . ? O4 C3 C4 116.6(11) . . ? C3 O4 Cr2 127.1(8) . . ? C5A O5 C5B 61.1(18) . . ? C5A O5 Cr2 122.9(8) . . ? C5B O5 Cr2 128.4(18) . . ? C5A O5 Cr3 122.9(8) . . ? C5B O5 Cr3 122.5(18) . . ? Cr2 O5 Cr3 98.5(3) . . yes C6 O6 Cr3 126.4(7) . . ? C6 O6 Cr2 121.3(7) . . ? Cr3 O6 Cr2 98.8(3) . . yes C7 O7 Cr2 128.6(7) . . ? O7 C7 O8 124.7(11) . . ? O7 C7 C8 117.2(11) . . ? O8 C7 C8 118.0(11) . . ? C7 O8 Cr3 128.2(8) . . ? C9 O9 Cr4 122.5(8) . . ? C9 O9 Cr3 123.1(8) . . ? Cr4 O9 Cr3 99.4(3) . . yes C10 O10 Cr3 124.9(7) . . ? C10 O10 Cr4 125.1(7) . . ? Cr3 O10 Cr4 98.0(3) . . yes C11 O11 Cr3 128.2(8) . . ? O11 C11 O12 124.9(11) . . ? O11 C11 C12 118.4(12) . . ? O12 C11 C12 116.7(11) . . ? C11 O12 Cr4 128.7(8) . . ? C13A O13 C13B 59.4(15) . . ? C13A O13 Cr5 122.3(10) . . ? C13B O13 Cr5 125.7(13) . . ? C13A O13 Cr4 121.3(10) . . ? C13B O13 Cr4 126.8(13) . . ? Cr5 O13 Cr4 99.3(3) . . yes C14 O14 Cr4 128.0(6) . . ? C14 O14 Cr5 123.5(7) . . ? Cr4 O14 Cr5 100.3(4) . . yes C15 O15 Cr4 128.7(8) . . ? O15 C15 O16 125.0(11) . . ? O15 C15 C16 116.7(11) . . ? O16 C15 C16 118.3(11) . . ? C15 O16 Cr5 128.3(8) . . ? C17A O17 C17B 50.0(16) . . ? C17A O17 Cr5 124.7(9) . . ? C17B O17 Cr5 127.3(15) . . ? C17A O17 Cr1 123.0(9) . 3_766 ? C17B O17 Cr1 128.5(15) . 3_766 ? Cr5 O17 Cr1 98.9(3) . 3_766 yes C18 O18 Cr5 125.1(7) . . ? C18 O18 Cr1 125.6(7) . 3_766 ? Cr5 O18 Cr1 98.8(3) . 3_766 yes C19 O19 Cr5 129.5(7) . . ? O19 C19 O20 122.9(11) . . ? O19 C19 C20 119.0(11) . . ? O20 C19 C20 118.0(11) . . ? C19 O20 Cr1 128.7(8) . 3_766 ? O37 Cr6 O21 96.6(3) 3_666 . ? O37 Cr6 O22 97.7(3) 3_666 . ? O21 Cr6 O22 77.6(3) . . ? O37 Cr6 O38 78.5(3) 3_666 3_666 ? O21 Cr6 O38 97.5(3) . 3_666 ? O22 Cr6 O38 173.5(3) . 3_666 ? O37 Cr6 O40 89.0(3) 3_666 3_666 ? O21 Cr6 O40 169.4(3) . 3_666 ? O22 Cr6 O40 92.8(3) . 3_666 ? O38 Cr6 O40 92.4(3) 3_666 3_666 ? O37 Cr6 O23 169.1(3) 3_666 . ? O21 Cr6 O23 89.8(3) . . ? O22 Cr6 O23 92.3(3) . . ? O38 Cr6 O23 91.9(3) 3_666 . ? O40 Cr6 O23 86.1(3) 3_666 . ? O21 Cr7 O26 98.6(3) . . ? O21 Cr7 O25 98.0(3) . . ? O26 Cr7 O25 77.7(3) . . ? O21 Cr7 O22 78.1(3) . . ? O26 Cr7 O22 173.2(3) . . ? O25 Cr7 O22 96.7(3) . . ? O21 Cr7 O27 169.0(3) . . ? O26 Cr7 O27 90.7(3) . . ? O25 Cr7 O27 89.5(3) . . ? O22 Cr7 O27 93.2(3) . . ? O21 Cr7 O24 88.8(3) . . ? O26 Cr7 O24 92.2(3) . . ? O25 Cr7 O24 168.6(3) . . ? O22 Cr7 O24 93.7(3) . . ? O27 Cr7 O24 85.1(3) . . ? O29 Cr8 O25 95.5(3) . . ? O29 Cr8 O26 96.9(3) . . ? O25 Cr8 O26 78.1(3) . . ? O29 Cr8 O30 78.0(3) . . ? O25 Cr8 O30 96.6(3) . . ? O26 Cr8 O30 172.4(3) . . ? O29 Cr8 O28 170.7(3) . . ? O25 Cr8 O28 89.7(3) . . ? O26 Cr8 O28 91.7(3) . . ? O30 Cr8 O28 93.8(3) . . ? O29 Cr8 O31 89.1(3) . . ? O25 Cr8 O31 170.8(3) . . ? O26 Cr8 O31 93.4(3) . . ? O30 Cr8 O31 92.2(3) . . ? O28 Cr8 O31 87.0(3) . . ? O34 Cr9 O33 77.3(3) . . ? O34 Cr9 O30 172.5(3) . . ? O33 Cr9 O30 98.8(3) . . ? O34 Cr9 O29 96.4(3) . . ? O33 Cr9 O29 95.6(3) . . ? O30 Cr9 O29 77.5(3) . . ? O34 Cr9 O32 93.3(3) . . ? O33 Cr9 O32 169.7(3) . . ? O30 Cr9 O32 91.1(3) . . ? O29 Cr9 O32 89.5(3) . . ? O34 Cr9 O35 92.5(3) . . ? O33 Cr9 O35 89.7(3) . . ? O30 Cr9 O35 94.0(3) . . ? O29 Cr9 O35 170.5(3) . . ? O32 Cr9 O35 86.5(3) . . ? O34 Cr10 O33 77.2(3) . . ? O34 Cr10 O38 173.3(3) . . ? O33 Cr10 O38 97.7(3) . . ? O34 Cr10 O37 97.4(3) . . ? O33 Cr10 O37 96.2(3) . . ? O38 Cr10 O37 78.6(3) . . ? O34 Cr10 O36 91.0(3) . . ? O33 Cr10 O36 90.0(3) . . ? O38 Cr10 O36 93.4(3) . . ? O37 Cr10 O36 170.5(3) . . ? O34 Cr10 O39 93.9(3) . . ? O33 Cr10 O39 170.3(3) . . ? O38 Cr10 O39 91.4(3) . . ? O37 Cr10 O39 88.9(3) . . ? O36 Cr10 O39 86.1(3) . . ? C21B O21 C21A 51(2) . . ? C21B O21 Cr7 127(2) . . ? C21A O21 Cr7 124.3(9) . . ? C21B O21 Cr6 129(2) . . ? C21A O21 Cr6 122.1(9) . . ? Cr7 O21 Cr6 99.1(3) . . yes C22 O22 Cr7 125.7(7) . . ? C22 O22 Cr6 127.0(6) . . ? Cr7 O22 Cr6 98.8(3) . . yes C23 O23 Cr6 127.9(8) . . ? O23 C23 O24 126.3(12) . . ? O23 C23 C24 117.0(11) . . ? O24 C23 C24 116.6(12) . . ? C23 O24 Cr7 127.0(8) . . ? C25B O25 C25A 46.6(16) . . ? C25B O25 Cr8 128.6(15) . . ? C25A O25 Cr8 124.4(9) . . ? C25B O25 Cr7 127.2(16) . . ? C25A O25 Cr7 124.9(9) . . ? Cr8 O25 Cr7 99.5(3) . . yes C26 O26 Cr8 124.9(6) . . ? C26 O26 Cr7 124.5(6) . . ? Cr8 O26 Cr7 99.4(3) . . yes C27 O27 Cr7 128.6(8) . . ? O27 C27 O28 126.2(11) . . ? O27 C27 C28 116.3(11) . . ? O28 C27 C28 117.4(11) . . ? C27 O28 Cr8 126.6(8) . . ? C29A O29 C29B 61.1(17) . . ? C29A O29 Cr8 121.0(9) . . ? C29B O29 Cr8 127.4(15) . . ? C29A O29 Cr9 122.9(8) . . ? C29B O29 Cr9 123.1(16) . . ? Cr8 O29 Cr9 99.9(3) . . yes C30 O30 Cr9 123.0(7) . . ? C30 O30 Cr8 123.3(7) . . ? Cr9 O30 Cr8 99.3(4) . . yes C31 O31 Cr8 126.7(8) . . ? O32 C31 O31 126.1(11) . . ? O32 C31 C32 116.9(10) . . ? O31 C31 C32 116.9(12) . . ? C31 O32 Cr9 128.3(7) . . ? C33 O33 Cr9 122.2(8) . . ? C33 O33 Cr10 121.4(7) . . ? Cr9 O33 Cr10 99.3(3) . . yes C34 O34 Cr10 124.3(7) . . ? C34 O34 Cr9 123.9(7) . . ? Cr10 O34 Cr9 100.1(4) . . yes C35 O35 Cr9 128.2(8) . . ? O35 C35 O36 125.2(12) . . ? O35 C35 C36 118.4(12) . . ? O36 C35 C36 116.3(11) . . ? C35 O36 Cr10 127.9(8) . . ? C37B O37 C37A 66.8(14) . . ? C37B O37 Cr6 124.8(11) . 3_666 ? C37A O37 Cr6 120.7(11) . 3_666 ? C37B O37 Cr10 123.6(13) . . ? C37A O37 Cr10 122.2(11) . . ? Cr6 O37 Cr10 98.9(3) . 3_666 yes C38 O38 Cr10 123.5(7) . . ? C38 O38 Cr6 124.1(8) . 3_666 ? Cr10 O38 Cr6 98.4(3) 3_666 . yes C39 O39 Cr10 128.0(8) . . ? O40 C39 O39 125.9(11) . . ? O40 C39 C40 117.4(11) . . ? O39 C39 C40 116.7(10) . . ? C39 O40 Cr6 127.9(8) . 3_666 ? _diffrn_measured_fraction_theta_max 0.855 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.855 _refine_diff_density_max 0.515 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.105 data_eric4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cyclo-decakis-[\m-ethanoato-bis-(-\m-ethoxy)chromium(III)] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H130 Cr10 O40' _chemical_formula_weight 2011.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2(1)/n 1' 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 9.446(2) _cell_length_b 16.052(3) _cell_length_c 28.659(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.037(14) _cell_angle_gamma 90.00 _cell_volume 4344.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 55 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 14.37 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2100 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.761 _exptl_absorpt_process_details SHELXTL _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.2 _diffrn_reflns_number 9844 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_sigmaI/netI 0.1251 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7645 _reflns_number_gt 3533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Siemens, 1995)' _computing_cell_refinement 'XSCANS (Siemens, 1995)' _computing_data_reduction 'XSCANS (Siemens, 1995)' _computing_structure_solution 'XS in SHELXTL/PC 5.03 (Siemens, 1995)' _computing_structure_refinement 'XL in SHELXTL/PC 5.03 (Siemens, 1995)' _computing_molecular_graphics 'XP in SHELXTL/PC 5.03 (Siemens, 1995)' _computing_publication_material 'XCIF in SHELXTL/PC 5.03 (Siemens, 1995)' _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^)+(0.1337P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment geom _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7645 _refine_ls_number_parameters 514 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1840 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2634 _refine_ls_wR_factor_gt 0.1963 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.39545(18) 0.79497(9) 0.47765(5) 0.0558(5) Uani 1 1 d . . . Cr2 Cr 0.35715(18) 0.70732(9) 0.38595(5) 0.0554(5) Uani 1 1 d . . . Cr3 Cr 0.37671(18) 0.54284(9) 0.33741(5) 0.0563(5) Uani 1 1 d . . . Cr4 Cr 0.44022(19) 0.36154(9) 0.35120(5) 0.0567(5) Uani 1 1 d . . . Cr5 Cr 0.52493(18) 0.23259(9) 0.42182(5) 0.0539(5) Uani 1 1 d . . . O1 O 0.4926(7) 0.7124(4) 0.4390(2) 0.0554(16) Uani 1 1 d D . . C1A C 0.649(4) 0.708(3) 0.4341(14) 0.182(14) Uiso 0.60 1 d P . . C1B C 0.560(7) 0.647(4) 0.459(2) 0.22(3) Uiso 0.40 1 d PD . . C2A C 0.724(9) 0.636(6) 0.426(3) 0.271 Uiso 0.40 1 d P . . C2B C 0.717(15) 0.586(11) 0.485(5) 0.30(7) Uiso 0.25 1 d P . . C2C C 0.735(9) 0.668(6) 0.478(3) 0.23(3) Uiso 0.35 1 d P . . O2 O 0.2434(7) 0.7577(4) 0.4351(2) 0.0599(17) Uani 1 1 d . . . C3A C 0.113(3) 0.791(3) 0.4266(9) 0.133(16) Uani 0.65 1 d P . . C3B C 0.085(6) 0.786(3) 0.4401(15) 0.061(12) Uiso 0.35 1 d P . . C4A C 0.051(4) 0.855(3) 0.4147(13) 0.093(12) Uiso 0.40 1 d P . . C4B C 0.111(4) 0.871(2) 0.4028(11) 0.073(9) Uiso 0.40 1 d P . . C4C C -0.009(7) 0.760(4) 0.416(2) 0.079(16) Uiso 0.20 1 d P . . O3 O 0.4535(8) 0.8848(4) 0.4338(2) 0.069(2) Uani 1 1 d . . . C5 C 0.4506(13) 0.8808(6) 0.3901(3) 0.072(3) Uani 1 1 d . . . C6 C 0.5046(16) 0.9583(7) 0.3638(4) 0.096(4) Uani 1 1 d . . . O4 O 0.4220(8) 0.8191(4) 0.3652(2) 0.072(2) Uani 1 1 d . . . O5 O 0.3033(7) 0.5899(4) 0.39520(19) 0.0528(16) Uani 1 1 d . . . C7A C 0.296(4) 0.549(2) 0.4374(12) 0.153(11) Uiso 0.60 1 d P . . C7B C 0.163(5) 0.560(3) 0.4118(18) 0.146(16) Uiso 0.40 1 d P . . C8A C 0.122(9) 0.497(7) 0.440(3) 0.28(4) Uiso 0.40 1 d P . . C8B C 0.142(5) 0.555(3) 0.4578(18) 0.126(14) Uiso 0.40 1 d P . . C8C C 0.430(13) 0.469(8) 0.447(4) 0.20(5) Uiso 0.20 1 d P . . O6 O 0.4794(7) 0.6502(4) 0.3412(2) 0.0619(18) Uani 1 1 d . . . C9A C 0.526(3) 0.6952(13) 0.3008(8) 0.111(9) Uani 0.80 1 d P . . C9B C 0.649(10) 0.680(6) 0.317(3) 0.10(2) Uiso 0.20 1 d P . . C10A C 0.669(12) 0.643(7) 0.293(4) 0.11(3) Uiso 0.15 1 d P . . C10B C 0.653(5) 0.733(3) 0.2998(16) 0.111(13) Uiso 0.40 1 d P . . C10C C 0.686(6) 0.736(4) 0.325(2) 0.087(16) Uiso 0.25 1 d P . . C10D C 0.546(9) 0.690(5) 0.280(3) 0.08(3) Uiso 0.20 1 d P . . O7 O 0.2014(8) 0.7174(4) 0.3387(2) 0.071(2) Uani 1 1 d . . . C11 C 0.1629(13) 0.6654(7) 0.3084(3) 0.067(3) Uani 1 1 d . . . C12 C 0.0295(14) 0.6888(8) 0.2788(4) 0.093(4) Uani 1 1 d . . . O8 O 0.2181(8) 0.5956(4) 0.3017(2) 0.069(2) Uani 1 1 d . . . O9 O 0.5189(7) 0.4713(4) 0.3681(2) 0.0539(16) Uani 1 1 d . . . C13A C 0.671(4) 0.491(2) 0.3712(12) 0.109(9) Uiso 0.50 1 d P . . C13B C 0.595(5) 0.489(3) 0.4043(15) 0.157(14) Uiso 0.50 1 d P . . C14A C 0.751(7) 0.513(4) 0.343(2) 0.15(2) Uiso 0.30 1 d P . . C14B C 0.766(9) 0.471(6) 0.407(3) 0.19(3) Uiso 0.30 1 d P . . C14C C 0.721(6) 0.542(4) 0.404(2) 0.164(19) Uiso 0.40 1 d P . . O10 O 0.2789(7) 0.4359(4) 0.3404(2) 0.0579(17) Uani 1 1 d D . . C15A C 0.1433(19) 0.4135(11) 0.3227(7) 0.081(5) Uani 0.80 1 d P . . C15B C 0.117(4) 0.443(6) 0.338(3) 0.10(3) Uiso 0.20 1 d PD . . C16A C 0.108(5) 0.404(2) 0.2741(15) 0.066(10) Uiso 0.40 1 d P . . C16B C 0.170(4) 0.3992(19) 0.2644(10) 0.062(9) Uiso 0.40 1 d P . . C16C C 0.111(12) 0.413(6) 0.293(4) 0.11(4) Uiso 0.20 1 d P . . O11 O 0.4595(9) 0.5143(4) 0.2758(2) 0.079(2) Uani 1 1 d . . . C17 C 0.5067(14) 0.4450(7) 0.2622(3) 0.080(4) Uani 1 1 d . . . C18 C 0.570(2) 0.4423(7) 0.2148(4) 0.156(8) Uani 1 1 d U . . H18A H 0.5632 0.4964 0.2006 0.234 Uiso 1 1 calc R . . H18B H 0.5198 0.4025 0.1958 0.234 Uiso 1 1 calc R . . H18C H 0.6678 0.4264 0.2175 0.234 Uiso 1 1 calc R . . O12 O 0.5053(9) 0.3783(4) 0.2861(2) 0.080(2) Uani 1 1 d . . . O13 O 0.3955(7) 0.3267(4) 0.4152(2) 0.0538(16) Uani 1 1 d . . . C19 C 0.349(5) 0.379(3) 0.4446(15) 0.325(19) Uiso 1 1 d . . . C20 C 0.208(4) 0.354(3) 0.4558(13) 0.318(18) Uiso 1 1 d . . . O14 O 0.6044(7) 0.2919(4) 0.3687(2) 0.0612(18) Uani 1 1 d . . . C21 C 0.6936(18) 0.2523(12) 0.3346(6) 0.132(7) Uani 1 1 d . . . H21A H 0.6718 0.1933 0.3327 0.158 Uiso 1 1 calc R . . H21B H 0.6766 0.2768 0.3041 0.158 Uiso 1 1 calc R . . C22 C 0.826(3) 0.2626(16) 0.3472(9) 0.249(14) Uani 1 1 d U . . H22A H 0.8859 0.2362 0.3249 0.299 Uiso 1 1 calc R . . H22B H 0.8420 0.2381 0.3774 0.299 Uiso 1 1 calc R . . H22C H 0.8471 0.3210 0.3486 0.299 Uiso 1 1 calc R . . O15 O 0.3339(8) 0.2638(4) 0.3270(2) 0.070(2) Uani 1 1 d . . . C23 C 0.3237(13) 0.1931(7) 0.3443(4) 0.070(3) Uani 1 1 d . . . C24 C 0.2173(14) 0.1301(7) 0.3235(4) 0.090(4) Uani 1 1 d . . . O16 O 0.3986(7) 0.1670(4) 0.3793(2) 0.0613(18) Uani 1 1 d . . . O17 O 0.6441(7) 0.2836(4) 0.47142(19) 0.0538(16) Uani 1 1 d . . . C25A C 0.668(4) 0.370(3) 0.4765(13) 0.179(14) Uiso 0.60 1 d P . . C25B C 0.788(8) 0.321(4) 0.463(2) 0.18(2) Uiso 0.40 1 d P . . C26A C 0.822(7) 0.404(4) 0.505(3) 0.32(3) Uiso 0.60 1 d P . . C26B C 0.849(7) 0.372(5) 0.460(3) 0.21(3) Uiso 0.40 1 d P . . O18 O 0.4463(7) 0.1817(4) 0.47863(19) 0.0574(17) Uani 1 1 d . . . C27 C 0.3736(14) 0.1025(8) 0.4782(4) 0.086(4) Uani 1 1 d . . . H27A H 0.3929 0.0737 0.5073 0.103 Uiso 1 1 calc R . . H27B H 0.4094 0.0685 0.4530 0.103 Uiso 1 1 calc R . . C28 C 0.2215(18) 0.1128(12) 0.4719(6) 0.161(8) Uani 1 1 d . . . H28A H 0.1768 0.0591 0.4716 0.194 Uiso 1 1 calc R . . H28B H 0.2020 0.1408 0.4429 0.194 Uiso 1 1 calc R . . H28C H 0.1854 0.1453 0.4972 0.194 Uiso 1 1 calc R . . O19 O 0.6640(8) 0.1404(4) 0.4168(2) 0.0626(18) Uani 1 1 d . . . C29 C 0.7400(13) 0.1062(6) 0.4489(4) 0.069(3) Uani 1 1 d . . . C30 C 0.8489(14) 0.0435(8) 0.4341(4) 0.096(4) Uani 1 1 d . . . O20 O 0.7275(8) 0.1210(4) 0.4914(2) 0.070(2) 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 Cr1 0.0789(12) 0.0424(8) 0.0459(8) -0.0038(7) -0.0015(8) 0.0060(9) Cr2 0.0794(12) 0.0411(8) 0.0455(8) -0.0031(7) -0.0045(8) 0.0032(9) Cr3 0.0851(13) 0.0397(8) 0.0439(8) -0.0015(6) -0.0013(8) 0.0003(9) Cr4 0.0862(13) 0.0400(8) 0.0436(8) -0.0022(6) -0.0038(8) -0.0006(9) Cr5 0.0767(11) 0.0394(8) 0.0456(8) -0.0024(6) -0.0028(8) 0.0001(8) O1 0.065(4) 0.048(4) 0.053(3) -0.005(3) -0.008(3) 0.000(4) O2 0.064(4) 0.058(4) 0.058(4) -0.008(3) -0.001(3) 0.013(4) C3A 0.09(2) 0.25(4) 0.063(16) -0.07(2) -0.015(15) 0.07(2) O3 0.117(6) 0.037(3) 0.053(4) 0.001(3) -0.007(4) -0.006(4) C5 0.123(10) 0.039(5) 0.053(6) -0.004(5) -0.005(6) -0.003(6) C6 0.180(14) 0.045(6) 0.062(7) 0.003(5) -0.006(8) -0.011(8) O4 0.123(6) 0.040(4) 0.053(4) 0.001(3) 0.003(4) -0.008(4) O5 0.074(5) 0.042(3) 0.042(3) 0.005(3) 0.003(3) -0.007(3) O6 0.081(5) 0.043(4) 0.062(4) -0.004(3) 0.017(4) -0.007(4) C9A 0.14(2) 0.091(13) 0.102(14) -0.032(12) 0.079(15) -0.052(14) O7 0.096(6) 0.059(4) 0.057(4) -0.001(3) -0.016(4) 0.014(4) C11 0.096(9) 0.056(6) 0.048(5) 0.006(5) -0.010(6) -0.006(7) C12 0.103(10) 0.099(10) 0.077(7) 0.016(7) -0.038(7) 0.018(8) O8 0.107(6) 0.047(4) 0.052(4) -0.005(3) -0.018(4) 0.006(4) O9 0.070(5) 0.042(3) 0.050(3) 0.001(3) -0.006(3) -0.004(3) O10 0.073(5) 0.041(4) 0.059(4) 0.000(3) -0.012(4) -0.005(3) C15A 0.104(14) 0.069(11) 0.068(11) -0.015(9) -0.039(9) 0.004(10) O11 0.135(7) 0.051(4) 0.051(4) -0.003(3) 0.014(4) 0.004(5) C17 0.137(11) 0.050(6) 0.052(6) -0.002(5) 0.032(7) 0.004(7) C18 0.33(2) 0.068(8) 0.071(8) 0.014(6) 0.074(12) 0.065(12) O12 0.137(7) 0.054(4) 0.048(4) -0.002(3) 0.010(4) 0.008(5) O13 0.075(5) 0.037(3) 0.049(3) -0.004(3) -0.004(3) 0.005(3) O14 0.077(5) 0.049(4) 0.058(4) 0.002(3) 0.004(4) 0.013(4) C21 0.104(12) 0.164(17) 0.128(13) 0.075(13) 0.016(11) 0.024(14) C22 0.21(3) 0.23(3) 0.31(3) 0.06(3) 0.10(3) 0.02(3) O15 0.106(6) 0.040(4) 0.063(4) 0.001(3) -0.023(4) -0.010(4) C23 0.090(9) 0.061(7) 0.057(6) -0.008(5) -0.006(6) -0.013(7) C24 0.123(11) 0.058(7) 0.087(8) -0.012(6) -0.035(7) -0.030(7) O16 0.092(5) 0.043(4) 0.048(4) -0.002(3) -0.008(4) 0.001(4) O17 0.072(5) 0.039(3) 0.050(3) -0.002(3) -0.002(3) -0.004(3) O18 0.073(5) 0.048(4) 0.051(4) 0.003(3) -0.002(3) -0.001(4) C27 0.103(11) 0.093(9) 0.061(7) 0.011(6) -0.003(7) -0.027(9) C28 0.126(15) 0.18(2) 0.175(18) 0.040(15) -0.001(13) -0.059(15) O19 0.087(5) 0.049(4) 0.053(4) -0.007(3) 0.001(4) 0.013(4) C29 0.086(8) 0.046(6) 0.076(7) -0.001(5) -0.005(7) -0.002(6) C30 0.108(10) 0.096(10) 0.084(8) -0.017(7) -0.008(7) 0.055(9) O20 0.098(6) 0.056(4) 0.056(4) -0.008(3) -0.012(4) 0.020(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 Cr1 O1 1.966(6) . yes Cr1 O2 1.961(7) . yes Cr1 O3 1.996(6) . yes Cr1 O17 1.969(6) 3_666 yes Cr1 O18 1.969(6) 3_666 yes Cr1 O20 1.998(7) 3_666 yes Cr2 O1 1.970(6) . yes Cr2 O2 1.961(6) . yes Cr2 O4 1.991(7) . yes Cr2 O5 1.971(6) . yes Cr2 O6 1.968(6) . yes Cr2 O7 1.989(7) . yes Cr3 O5 1.959(6) . yes Cr3 O6 1.980(6) . yes Cr3 O8 1.988(7) . yes Cr3 O9 1.962(6) . yes Cr3 O10 1.951(6) . yes Cr3 O11 1.998(7) . yes Cr4 O9 1.970(6) . yes Cr4 O10 1.956(7) . yes Cr4 O12 1.993(6) . yes Cr4 O13 1.972(6) . yes Cr4 O14 1.969(7) . yes Cr4 O15 1.981(7) . yes Cr5 O13 1.951(6) . yes Cr5 O14 1.957(7) . yes Cr5 O16 1.992(6) . yes Cr5 O17 1.975(6) . yes Cr5 O18 1.978(6) . yes Cr5 O19 1.985(7) . yes O1 C1B 1.35(4) . ? O1 C1A 1.48(4) . ? C1A C2A 1.38(9) . ? C1A C1B 1.48(7) . ? C1A C2C 1.61(9) . ? C1B C2B 1.92(15) . ? C1B C2C 1.76(10) . ? C1B C2A 1.83(10) . ? C2A C2C 1.56(10) . ? C2A C14C 1.64(9) . ? C2A C2B 1.86(16) . ? C2B C2C 1.35(16) . ? O2 C3A 1.36(3) . ? O2 C3B 1.57(5) . ? C3A C4A 1.22(5) . ? C3A C4C 1.28(7) . ? C3A C4B 1.46(5) . ? C3B C4C 1.18(8) . ? C3B C4A 1.36(7) . ? C3B C4B 1.76(5) . ? C4A C4B 0.72(4) . ? C4A C4C 1.61(7) . ? O3 C5 1.255(11) . ? C5 O4 1.247(11) . ? C5 C6 1.545(14) . ? O5 C7A 1.38(3) . ? O5 C7B 1.50(5) . ? C7A C7B 1.45(5) . ? C7A C8B 1.58(5) . ? C7A C8A 1.84(10) . ? C7A C8C 1.82(12) . ? C7B C8A 1.35(10) . ? C7B C8B 1.34(6) . ? C8A C8B 1.08(9) . ? C8B C26A 1.30(7) 3_666 ? C8C C19 1.64(12) . ? C8C C13B 2.02(12) . ? O6 C9A 1.44(2) . ? O6 C9B 1.82(10) . ? C9A C10D 0.62(7) . ? C9A C9B 1.27(8) . ? C9A C10B 1.35(5) . ? C9A C10A 1.61(12) . ? C9A C10C 1.77(6) . ? C9B C10A 0.94(11) . ? C9B C10B 0.98(9) . ? C9B C10D 1.42(13) . ? C9B C10C 0.98(10) . ? C10A C10D 1.42(12) . ? C10A C10B 1.47(12) . ? C10A C10C 1.76(13) . ? C10B C10C 0.77(6) . ? C10B C10D 1.35(9) . ? C10C C10D 1.96(10) . ? O7 C11 1.253(11) . ? C11 O8 1.253(12) . ? C11 C12 1.552(15) . ? O9 C13B 1.29(4) . ? O9 C13A 1.47(4) . ? C13A C14A 1.17(6) . ? C13A C13B 1.20(4) . ? C13A C14B 1.40(8) . ? C13A C14C 1.32(6) . ? C13B C14C 1.46(6) . ? C13B C14B 1.64(9) . ? C14A C14B 1.97(10) . ? C14A C14C 1.84(8) . ? C14B C14C 1.22(9) . ? O10 C15A 1.415(16) . ? O10 C15B 1.53(4) . ? C15A C15B 0.71(8) . ? C15A C16C 0.90(11) . ? C15A C16A 1.43(4) . ? C15A C16B 1.71(3) . ? C15B C16C 1.39(12) . ? C15B C16A 1.95(10) . ? C16A C16B 0.66(4) . ? C16B C16C 1.02(10) . ? O11 C17 1.263(12) . ? C17 O12 1.273(11) . ? C17 C18 1.494(15) . ? O13 C19 1.27(4) . ? C19 C20 1.44(5) . ? O14 C21 1.450(18) . ? C21 C22 1.30(2) . ? O15 C23 1.243(12) . ? C23 O16 1.285(12) . ? C23 C24 1.538(14) . ? O17 C25A 1.41(4) . ? O17 C25B 1.51(8) . ? O17 Cr1 1.969(6) 3_666 ? C25A C25B 1.45(6) . ? C25A C26B 1.78(8) . ? C25A C26A 1.74(7) . ? C25B C26B 1.01(8) . ? C25B C26A 1.83(9) . ? C26A C8B 1.30(7) 3_666 ? C26A C26B 1.41(9) . ? O18 C27 1.445(13) . ? O18 Cr1 1.969(6) 3_666 ? C27 C28 1.453(18) . ? O19 C29 1.279(12) . ? C29 O20 1.250(12) . ? C29 C30 1.505(15) . ? O20 Cr1 1.998(7) 3_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 O1 Cr1 O2 77.7(3) . . ? O1 Cr1 O18 97.5(3) . 3_666 ? O2 Cr1 O18 173.2(3) . 3_666 ? O1 Cr1 O17 94.8(3) . 3_666 ? O2 Cr1 O17 96.8(3) . 3_666 ? O18 Cr1 O17 78.6(3) 3_666 3_666 ? O1 Cr1 O3 89.8(3) . . ? O2 Cr1 O3 92.0(3) . . ? O18 Cr1 O3 92.8(3) 3_666 . ? O17 Cr1 O3 170.7(3) 3_666 . ? O1 Cr1 O20 170.6(3) . 3_666 ? O2 Cr1 O20 93.2(3) . 3_666 ? O18 Cr1 O20 91.7(3) 3_666 3_666 ? O17 Cr1 O20 89.1(3) 3_666 3_666 ? O3 Cr1 O20 87.7(3) . 3_666 ? O2 Cr2 O6 174.7(3) . . ? O2 Cr2 O5 98.7(3) . . ? O6 Cr2 O5 78.4(3) . . ? O2 Cr2 O1 77.6(3) . . ? O6 Cr2 O1 98.1(3) . . ? O5 Cr2 O1 95.8(3) . . ? O2 Cr2 O7 92.7(3) . . ? O6 Cr2 O7 91.7(3) . . ? O5 Cr2 O7 88.8(3) . . ? O1 Cr2 O7 169.8(3) . . ? O2 Cr2 O4 91.1(3) . . ? O6 Cr2 O4 92.2(3) . . ? O5 Cr2 O4 169.6(3) . . ? O1 Cr2 O4 89.7(3) . . ? O7 Cr2 O4 87.2(3) . . ? O10 Cr3 O5 97.3(3) . . ? O10 Cr3 O9 77.7(3) . . ? O5 Cr3 O9 95.5(3) . . ? O10 Cr3 O6 174.3(3) . . ? O5 Cr3 O6 78.4(3) . . ? O9 Cr3 O6 98.9(3) . . ? O10 Cr3 O8 92.5(3) . . ? O5 Cr3 O8 89.8(3) . . ? O9 Cr3 O8 169.4(3) . . ? O6 Cr3 O8 91.2(3) . . ? O10 Cr3 O11 91.7(3) . . ? O5 Cr3 O11 170.5(3) . . ? O9 Cr3 O11 89.2(3) . . ? O6 Cr3 O11 92.8(3) . . ? O8 Cr3 O11 86.9(3) . . ? O10 Cr4 O14 173.9(3) . . ? O10 Cr4 O9 77.4(3) . . ? O14 Cr4 O9 98.8(3) . . ? O10 Cr4 O13 98.1(3) . . ? O14 Cr4 O13 77.5(3) . . ? O9 Cr4 O13 96.4(2) . . ? O10 Cr4 O15 92.3(3) . . ? O14 Cr4 O15 91.8(3) . . ? O9 Cr4 O15 168.9(3) . . ? O13 Cr4 O15 89.1(3) . . ? O10 Cr4 O12 91.3(3) . . ? O14 Cr4 O12 93.4(3) . . ? O9 Cr4 O12 89.3(3) . . ? O13 Cr4 O12 169.9(3) . . ? O15 Cr4 O12 86.7(3) . . ? O13 Cr5 O14 78.2(3) . . ? O13 Cr5 O17 95.5(3) . . ? O14 Cr5 O17 97.9(3) . . ? O13 Cr5 O18 98.9(3) . . ? O14 Cr5 O18 175.0(3) . . ? O17 Cr5 O18 78.2(3) . . ? O13 Cr5 O19 169.9(3) . . ? O14 Cr5 O19 92.5(3) . . ? O17 Cr5 O19 89.5(3) . . ? O18 Cr5 O19 90.6(3) . . ? O13 Cr5 O16 89.0(3) . . ? O14 Cr5 O16 90.9(3) . . ? O17 Cr5 O16 170.8(3) . . ? O18 Cr5 O16 93.2(3) . . ? O19 Cr5 O16 87.2(3) . . ? C1B O1 C1A 63(3) . . ? C1B O1 Cr1 120(3) . . ? C1A O1 Cr1 124.1(17) . . ? C1B O1 Cr2 126(3) . . ? C1A O1 Cr2 123.8(16) . . ? Cr1 O1 Cr2 99.2(3) . . yes C2A C1A C1B 80(5) . . ? C2A C1A O1 125(5) . . ? C1B C1A O1 54(2) . . ? C2A C1A C2C 62(5) . . ? C1B C1A C2C 69(4) . . ? O1 C1A C2C 116(4) . . ? O1 C1B C1A 63(3) . . ? O1 C1B C2B 157(7) . . ? C1A C1B C2B 95(6) . . ? O1 C1B C2C 114(6) . . ? C1A C1B C2C 59(4) . . ? C2B C1B C2C 43(5) . . ? O1 C1B C2A 105(5) . . ? C1A C1B C2A 48(4) . . ? C2B C1B C2A 59(5) . . ? C2C C1B C2A 52(4) . . ? C1A C2A C2C 66(6) . . ? C1A C2A C14C 146(7) . . ? C2C C2A C14C 133(8) . . ? C1A C2A C2B 101(8) . . ? C2C C2A C2B 45(5) . . ? C14C C2A C2B 88(7) . . ? C1A C2A C1B 53(4) . . ? C2C C2A C1B 62(5) . . ? C14C C2A C1B 107(6) . . ? C2B C2A C1B 63(5) . . ? C2C C2B C1B 63(8) . . ? C2C C2B C2A 56(7) . . ? C1B C2B C2A 58(5) . . ? C2B C2C C2A 79(9) . . ? C2B C2C C1A 116(10) . . ? C2A C2C C1A 51(5) . . ? C2B C2C C1B 75(8) . . ? C2A C2C C1B 66(5) . . ? C1A C2C C1B 52(3) . . ? C3A O2 C3B 17(2) . . ? C3A O2 Cr2 122.8(11) . . ? C3B O2 Cr2 136.0(16) . . ? C3A O2 Cr1 129.9(13) . . ? C3B O2 Cr1 122.9(16) . . ? Cr2 O2 Cr1 99.6(3) . . yes C4A C3A C4C 80(4) . . ? C4A C3A O2 144(4) . . ? C4C C3A O2 134(5) . . ? C4A C3A C4B 29(2) . . ? C4C C3A C4B 103(4) . . ? O2 C3A C4B 116(3) . . ? C4C C3B C4A 79(5) . . ? C4C C3B O2 123(4) . . ? C4A C3B O2 114(3) . . ? C4C C3B C4B 91(4) . . ? C4A C3B C4B 22(2) . . ? O2 C3B C4B 92(3) . . ? C4B C4A C3A 94(6) . . ? C4B C4A C3B 112(6) . . ? C3A C4A C3B 20(3) . . ? C4B C4A C4C 130(6) . . ? C3A C4A C4C 51(3) . . ? C3B C4A C4C 46(3) . . ? C4A C4B C3A 57(4) . . ? C4A C4B C3B 46(5) . . ? C3A C4B C3B 13(2) . . ? C3B C4C C3A 22(3) . . ? C3B C4C C4A 55(4) . . ? C3A C4C C4A 48(3) . . ? C5 O3 Cr1 126.1(6) . . ? O4 C5 O3 127.8(9) . . ? O4 C5 C6 115.5(9) . . ? O3 C5 C6 116.3(9) . . ? C5 O4 Cr2 127.5(6) . . ? C7A O5 C7B 61(2) . . ? C7A O5 Cr3 125.7(15) . . ? C7B O5 Cr3 118(2) . . ? C7A O5 Cr2 126.1(14) . . ? C7B O5 Cr2 126(2) . . ? Cr3 O5 Cr2 99.1(3) . . yes O5 C7A C7B 64(3) . . ? O5 C7A C8B 111(3) . . ? C7B C7A C8B 52(3) . . ? O5 C7A C8A 108(4) . . ? C7B C7A C8A 47(3) . . ? C8B C7A C8A 36(3) . . ? O5 C7A C8C 115(4) . . ? C7B C7A C8C 139(5) . . ? C8B C7A C8C 129(5) . . ? C8A C7A C8C 107(5) . . ? C8A C7B C8B 47(4) . . ? C8A C7B C7A 82(5) . . ? C8B C7B C7A 69(3) . . ? C8A C7B O5 134(6) . . ? C8B C7B O5 119(4) . . ? C7A C7B O5 56(2) . . ? C8B C8A C7B 66(7) . . ? C8B C8A C7A 59(6) . . ? C7B C8A C7A 51(4) . . ? C8A C8B C26A 150(8) . 3_666 ? C8A C8B C7B 67(6) . . ? C26A C8B C7B 138(6) 3_666 . ? C8A C8B C7A 85(6) . . ? C26A C8B C7A 96(5) 3_666 . ? C7B C8B C7A 59(3) . . ? C19 C8C C7A 107(7) . . ? C19 C8C C13B 119(7) . . ? C7A C8C C13B 110(7) . . ? C9A O6 C9B 44(3) . . ? C9A O6 Cr2 118.8(9) . . ? C9B O6 Cr2 131(3) . . ? C9A O6 Cr3 123.3(9) . . ? C9B O6 Cr3 130(3) . . ? Cr2 O6 Cr3 98.5(3) . . yes C10D C9A C9B 91(10) . . ? C10D C9A O6 141(9) . . ? C9B C9A O6 85(5) . . ? C10D C9A C10B 76(9) . . ? C9B C9A C10B 44(4) . . ? O6 C9A C10B 122(3) . . ? C10D C9A C10A 61(9) . . ? C9B C9A C10A 36(5) . . ? O6 C9A C10A 97(4) . . ? C10B C9A C10A 59(4) . . ? C10D C9A C10C 98(9) . . ? C9B C9A C10C 32(4) . . ? O6 C9A C10C 98(3) . . ? C10B C9A C10C 24(2) . . ? C10A C9A C10C 62(5) . . ? C10A C9B C10B 100(10) . . ? C10A C9B C10D 70(9) . . ? C10B C9B C10D 65(7) . . ? C10A C9B C9A 92(10) . . ? C10B C9B C9A 73(6) . . ? C10D C9B C9A 26(4) . . ? C10A C9B C10C 132(10) . . ? C10B C9B C10C 46(6) . . ? C10D C9B C10C 108(9) . . ? C9A C9B C10C 104(9) . . ? C10A C9B O6 107(10) . . ? C10B C9B O6 118(8) . . ? C10D C9B O6 73(6) . . ? C9A C9B O6 52(4) . . ? C10C C9B O6 118(9) . . ? C9B C10A C10D 71(10) . . ? C9B C10A C10B 41(7) . . ? C10D C10A C10B 55(6) . . ? C9B C10A C10C 24(8) . . ? C10D C10A C10C 75(7) . . ? C10B C10A C10C 26(3) . . ? C9B C10A C9A 52(8) . . ? C10D C10A C9A 23(3) . . ? C10B C10A C9A 52(4) . . ? C10C C10A C9A 63(5) . . ? C10C C10B C10D 134(9) . . ? C10C C10B C9B 67(7) . . ? C10D C10B C9B 74(8) . . ? C10C C10B C10A 98(8) . . ? C10D C10B C10A 60(6) . . ? C9B C10B C10A 39(6) . . ? C10C C10B C9A 110(7) . . ? C10D C10B C9A 27(3) . . ? C9B C10B C9A 63(6) . . ? C10A C10B C9A 69(5) . . ? C10B C10C C9B 67(7) . . ? C10B C10C C10A 56(7) . . ? C9B C10C C10A 23(7) . . ? C10B C10C C10D 30(6) . . ? C9B C10C C10D 44(7) . . ? C10A C10C C10D 44(4) . . ? C10B C10C C9A 46(6) . . ? C9B C10C C9A 44(6) . . ? C10A C10C C9A 54(4) . . ? C10D C10C C9A 18(2) . . ? C9A C10D C10B 77(9) . . ? C9A C10D C9B 63(9) . . ? C10B C10D C9B 41(5) . . ? C9A C10D C10A 96(10) . . ? C10B C10D C10A 64(6) . . ? C9B C10D C10A 39(5) . . ? C9A C10D C10C 63(8) . . ? C10B C10D C10C 16(3) . . ? C9B C10D C10C 28(4) . . ? C10A C10D C10C 60(6) . . ? C11 O7 Cr2 128.3(7) . . ? O7 C11 O8 125.8(10) . . ? O7 C11 C12 116.1(10) . . ? O8 C11 C12 118.0(10) . . ? C11 O8 Cr3 128.0(6) . . ? C13B O9 C13A 51(2) . . ? C13B O9 Cr3 127(2) . . ? C13A O9 Cr3 123.8(14) . . ? C13B O9 Cr4 127(2) . . ? C13A O9 Cr4 125.0(14) . . ? Cr3 O9 Cr4 99.3(3) . . yes C14A C13A C13B 163(5) . . ? C14A C13A C14B 99(5) . . ? C13B C13A C14B 78(4) . . ? C14A C13A C14C 94(5) . . ? C13B C13A C14C 71(3) . . ? C14B C13A C14C 53(4) . . ? C14A C13A O9 132(4) . . ? C13B C13A O9 57(3) . . ? C14B C13A O9 127(4) . . ? C14C C13A O9 121(4) . . ? C13A C13B O9 72(3) . . ? C13A C13B C14C 59(3) . . ? O9 C13B C14C 124(4) . . ? C13A C13B C14B 57(3) . . ? O9 C13B C14B 123(4) . . ? C14C C13B C14B 46(3) . . ? C13A C13B C8C 163(5) . . ? O9 C13B C8C 91(4) . . ? C14C C13B C8C 138(5) . . ? C14B C13B C8C 135(5) . . ? C13A C14A C14B 45(4) . . ? C13A C14A C14C 46(3) . . ? C14B C14A C14C 37(3) . . ? C14C C14B C13A 60(5) . . ? C14C C14B C13B 59(5) . . ? C13A C14B C13B 46(3) . . ? C14C C14B C14A 65(5) . . ? C13A C14B C14A 36(3) . . ? C13B C14B C14A 81(4) . . ? C14B C14C C13A 67(5) . . ? C14B C14C C13B 75(5) . . ? C13A C14C C13B 51(3) . . ? C14B C14C C2A 145(8) . . ? C13A C14C C2A 148(6) . . ? C13B C14C C2A 122(6) . . ? C14B C14C C14A 77(6) . . ? C13A C14C C14A 40(3) . . ? C13B C14C C14A 90(4) . . ? C2A C14C C14A 128(6) . . ? C15A O10 C15B 27(3) . . ? C15A O10 Cr3 129.3(8) . . ? C15B O10 Cr3 114(3) . . ? C15A O10 Cr4 126.8(8) . . ? C15B O10 Cr4 146(3) . . ? Cr3 O10 Cr4 100.1(3) . . yes C15B C15A C16C 119(10) . . ? C15B C15A O10 86(4) . . ? C16C C15A O10 129(8) . . ? C15B C15A C16A 128(7) . . ? C16C C15A C16A 9(8) . . ? O10 C15A C16A 124(2) . . ? C15B C15A C16B 141(8) . . ? C16C C15A C16B 29(7) . . ? O10 C15A C16B 103.5(16) . . ? C16A C15A C16B 22.1(17) . . ? C15A C15B C16C 34(7) . . ? C15A C15B O10 67(3) . . ? C16C C15B O10 92(6) . . ? C15A C15B C16A 36(6) . . ? C16C C15B C16A 1(5) . . ? O10 C15B C16A 92(4) . . ? C16B C16A C15A 103(5) . . ? C16B C16A C15B 114(6) . . ? C15A C16A C15B 17(2) . . ? C16A C16B C16C 30(8) . . ? C16A C16B C15A 55(5) . . ? C16C C16B C15A 26(7) . . ? C16B C16C C15A 125(10) . . ? C16B C16C C15B 144(10) . . ? C15A C16C C15B 26(5) . . ? C17 O11 Cr3 128.4(6) . . ? O11 C17 O12 124.6(9) . . ? O11 C17 C18 117.1(9) . . ? O12 C17 C18 118.3(10) . . ? C17 O12 Cr4 128.7(7) . . ? C19 O13 Cr5 132.0(19) . . ? C19 O13 Cr4 121(2) . . ? Cr4 O13 Cr5 99.5(3) . . yes O13 C19 C20 108(4) . . ? O13 C19 C8C 116(5) . . ? C20 C19 C8C 132(6) . . ? C21 O14 Cr5 123.1(8) . . ? C21 O14 Cr4 122.8(7) . . ? Cr4 O14 Cr5 99.4(3) . . yes C22 C21 O14 109(2) . . ? C23 O15 Cr4 128.8(7) . . ? O15 C23 O16 124.2(10) . . ? O15 C23 C24 120.0(10) . . ? O16 C23 C24 115.8(9) . . ? C23 O16 Cr5 128.3(6) . . ? C25A O17 C25B 59(3) . . ? C25A O17 Cr1 125.7(16) . 3_666 ? C25B O17 Cr1 124(2) . 3_666 ? C25A O17 Cr5 124.7(17) . . ? C25B O17 Cr5 123(2) . . ? Cr1 O17 Cr5 98.9(3) 3_666 . yes O17 C25A C25B 64(4) . . ? O17 C25A C26B 98(4) . . ? C25B C25A C26B 34(3) . . ? O17 C25A C26A 119(4) . . ? C25B C25A C26A 69(4) . . ? C26B C25A C26A 47(3) . . ? C26B C25B C25A 91(7) . . ? C26B C25B O17 148(8) . . ? C25A C25B O17 57(3) . . ? C26B C25B C26A 50(6) . . ? C25A C25B C26A 63(3) . . ? O17 C25B C26A 109(5) . . ? C8B C26A C26B 153(8) 3_666 . ? C8B C26A C25A 138(6) 3_666 . ? C26B C26A C25A 68(5) . . ? C8B C26A C25B 163(6) 3_666 . ? C26B C26A C25B 33(4) . . ? C25A C26A C25B 48(3) . . ? C25B C26B C26A 97(8) . . ? C25B C26B C25A 54(5) . . ? C26A C26B C25A 65(4) . . ? C27 O18 Cr1 121.9(6) . 3_666 ? C27 O18 Cr5 122.8(6) . . ? Cr1 O18 Cr5 98.8(3) 3_666 . yes O18 C27 C28 111.7(13) . . ? C29 O19 Cr5 129.2(6) . . ? O20 C29 O19 123.8(10) . . ? O20 C29 C30 118.6(10) . . ? O19 C29 C30 117.6(10) . . ? C29 O20 Cr1 128.8(7) . 3_666 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.606 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.108