# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_HC013 # start Validation Reply Form _vrf_CHEMW03_HC013 ; PROBLEM: The ratio of given/expected molecular weight as RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 2 tolunene molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_THETM01_HC013 ; PROBLEM: The value of sine(theta_max)/wavelength RESPONSE: 2theta was cut-off at 47 degrees. These crystals diffracted very weakly and no significant diffraction was observed above this level. ; _vrf_PLAT022_HC013 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) RESPONSE: Many of the atoms were involved in disorder. The disorder was modeled, however, some atoms still exhibited non-ideal behaviour. Restraints were applied. Please see iucr_refine_instructions_details for a full list of the applied restraints. ; _vrf_PLAT234_HC013 ; PROBLEM: Hirshfeld Test Diff RESPONSE: Due to weak diffraction and large structure size some of the light atoms show some discontinuities in anisotropic displacement. Attempts to model the largest differences using SIMU were made (please see iucr_refine_instructions_details for a full list of the applied restraints.) The atoms identified by the Hirshfeld Rigid Bond Test were carefully examined to ensure that they are not the result of an incorrect atom-type assignment. ; _vrf_PLAT341_HC013 ; PROBLEM: Low Bond Precision on C-C Bonds RESPONSE: The large associated su's on the C-C bonds, and many of the light atom angles, is the expected result of the weakly diffracting data-set. ; _vrf_PLAT413_HC013 ; PROBLEM: Short Inter XH3 .. XHn RESPONSE: H-atoms were introduced in calculated positions and refined on a riding model. H-atoms on disordered methyl groups were refined using HFIX 33 instead of HFIX137 due to the weak quality of the collected data. ; _vrf_RFACG01_HC013 ; PROBLEM: The value of the R factor is > 0.10 RESPONSE: The crystal under consideration diffracted weakly and therefore the high weighted R factor does not indicate an incorrect model. ; _vrf_RFACR01_HC013 ; PROBLEM: The value of the weighted R factor is > 0.25 RESPONSE: The crystal under consideration diffracted weakly and therefore the high weighted R factor does not indicate an incorrect model. ; _vrf_PLAT020_HC013 ; PROBLEM: The value of Rint is greater than 0.12 RESPONSE: The crystal under consideration diffracted weakly. ; _vrf_RINTA01_HC013 ; PROBLEM: The value of Rint is greater than 0.12 RESPONSE: The crystal under consideration diffracted weakly. ; _vrf_PLAT041_HC013 ; PROBLEM: Calc. and Reported SumFormula RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 2 tolunene molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT068_HC013 ; PROBLEM: Reported F000 Differs from Calcd (or Missing) RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 2 tolunene molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT082_HC013 ; PROBLEM: High R1 Value RESPONSE: The crystal under consideration diffracted weakly and therefore the high weighted R factor does not indicate an incorrect model. ; _vrf_PLAT084_HC013 ; PROBLEM: High wR2 Value RESPONSE: The crystal under consideration diffracted weakly and therefore the high weighted R factor does not indicate an incorrect model. ; _vrf_PLAT094_HC013 ; PROBLEM: Ratio of Maximum / Minimum Residual Density RESPONSE: From shelxl.lst Electron density synthesis with coefficients Fo-Fc Highest peak 1.09 at 0.9092 0.5223 0.1449 [ 0.05 A from CR1 ] Deepest hole -0.34 at 0.1118 0.7292 0.1358 [ 1.26 A from LI1 ] ; _vrf_PLAT222_HC013 ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) RESPONSE: H-atoms were introduced in calculated positions and refined on a riding model. Large H-atoms are associated with disordered groups. Attempts to model the disorder are described in _refine_special_details. ; _vrf_PLAT230_HC013 ; PROBLEM: Hirshfeld Test Diff RESPONSE: Due to weak diffraction and large structure size some of the light atoms show some discontinuities in anisotropic displacement. Attempts to model the largest differences using SIMU were made (please see iucr_refine_instructions_details for a full list of the applied restraints.) The atoms identified by the Hirshfeld Rigid Bond Test were carefully examined to ensure that they are not the result of an incorrect atom-type assignment. ; _vrf_PLAT241_HC013 ; PROBLEM: Check High Ueq as Compared to Neighbors for RESPONSE: Due to weak diffraction and large structure size some of the light atoms show some discontinuities in anisotropic displacement. Attempts to model the largest differences using SIMU were made (please see iucr_refine_instructions_details for a full list of the applied restraints.) The atoms identified by the Hirshfeld Rigid Bond Test were carefully examined to ensure that they are not the result of an incorrect atom-type assignment. ; _vrf_PLAT242_HC013 ; PROBLEM: Check Low Ueq as Compared to Neighbors for RESPONSE: Due to weak diffraction and large structure size some of the light atoms show some discontinuities in anisotropic displacement. Attempts to model the largest differences using SIMU were made (please see iucr_refine_instructions_details for a full list of the applied restraints.) The atoms identified by the Hirshfeld Rigid Bond Test were carefully examined to ensure that they are not the result of an incorrect atom-type assignment. ; _vrf_PLAT309_HC013 ; PROBLEM: Single Bonded Oxygen RESPONSE: The atoms in question is part of a disordered THF group. The disorder crosses a symmetry element (a two-fold screw axis) and therefore this group was treated with a PART -1 instruction. The O-atom is in fact bonded within THF, and coordinated to a Li atom. ; _vrf_PLAT334_HC013 ; PROBLEM: Small Average Benzene C-C RESPONSE: Many of the light atoms were involved in various disorders. DFIX restraints were applied to these groups (please see iucr_refine_instructions_details for a full list of the applied restraints.) ; _vrf_PLAT366_HC013 ; PROBLEM: Short? C(sp?)-C(sp?) Bond RESPONSE: Many of the light atoms were involved in various disorders. DFIX restraints were applied to these groups (please see iucr_refine_instructions_details for a full list of the applied restraints.) ; _vrf_PLAT410_HC013 ; PROBLEM: Short Inter XH3 .. XHn RESPONSE: H-atoms were introduced in calculated positions and refined on a riding model. H-atoms on disordered methyl groups were refined using HFIX 33 instead of HFIX137 due to the weak quality of the collected data. ; _vrf_PLAT722_HC013 ; PROBLEM: Angle Calc RESPONSE: Deviations here may be due to applied restraints and that the calculated values by checkCIF are done without access to the variance/covariance matrix. ; _vrf_FORMU01_HC013 ; PROBLEM: There is a discrepancy between the atom counts in the RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 2 tolunene molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_CELLZ01_HC013 ; PROBLEM: Difference between formula and atom_site contents detected RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 2 tolunene molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _vrf_PLAT002_HC013 ; PROBLEM: Number of Distance or Angle Restraints on AtSite RESPONSE: Due to weak diffraction and large structure size some of the light atoms exhibitied non-ideal behaviour. Attempts to model the largest differences using DFIX, SIMU and ISOR were made (please see iucr_refine_instructions_ details for a full list of the applied restraints.) ; _vrf_PLAT003_HC013 ; PROBLEM: Number of Uiso or Uij Restrained Atom Sites RESPONSE: Due to weak diffraction and large structure size some of the light atoms exhibitied non-ideal behaviour. Attempts to model the largest differences using DFIX, SIMU and ISOR were made (please see iucr_refine_instructions_ details for a full list of the applied restraints.) ; _vrf_PLAT042_HC013 ; PROBLEM: Difference between formula and atom_site contents detected RESPONSE: This structure was treated via Platon's Squeeze procedure. Please see platon_squeeze_details for full details. 2 tolunene molecules that were omitted from the model were included in the formula for calculation of the intensive properties. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H110 Cl3 Cr2 Li N2 O5, 2(C7 H8)' _chemical_formula_sum 'C92 H126 Cl3 Cr2 Li N2 O5' _chemical_formula_weight 1557.24 _chemical_absolute_configuration ad 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' Cl Cl 0.1484 0.1585 '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' 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'P 31 2 1' _symmetry_space_group_name_Hall 'P 31 2"' _symmetry_Int_Tables_number 152 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 18.945(9) _cell_length_b 18.945(9) _cell_length_c 25.390(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7892(7) _cell_formula_units_Z 3 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 16882 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 30.0 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.983 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2502 _exptl_absorpt_coefficient_mu 0.324 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_correction_T_min 0.888 _exptl_absorpt_process_details 'T. Higashi, 2000' _exptl_special_details ; Crystals were air-sensitive, and were therefore kept under paratone oil. While they were reasonably sized and regular in appearance, they diffracted weakly. The high refinement statistics are the result of this marginal diffraction strength. ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite - Rigaku SHINE' _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 73179 _diffrn_reflns_av_R_equivalents 0.1281 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 23.49 _reflns_number_total 7780 _reflns_number_gt 6060 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_structure_solution 'SHELXS-97 (Acta Cryst.2008, A64, 112-122)' _computing_structure_refinement 'SHELXL-97 (Acta Cryst.2008, A64, 112-122)' _computing_molecular_graphics 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _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. SIMU, DFIX, DANG and ISOR restraints were applied to the benzene rings and the disordered groups. For further details, see iucr_refine_instructions_details. Selected bond valence sums: #----------------------------------------------------------------------------- Atom no. Valence state Most consistent Bond Valence % Deviation from assumed valence state Sum assumed valence state #----------------------------------------------------------------------------- Cr1 Cr1(2) 2.977 49 Cr1 Cr1(3) * 2.919 3 A.S. Wills, VaList, Program available from www.ccp14.ac.uk Therefore, overall charge balance is achieved by the sum formula: [{(L-2H)2 Cr(III)2 Cl3} Li(THF)] 2(toluene) = (-4) + (+6) + (-3) + (+1) = 0 Note that in the structure the Li(THF) group is both disordered in the asymmetric unit, and overall present at only 0.5-occupancy (therefore, there is one Li(THF) present on average in the symmetry expanded Cr2 cluster.) ; _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.12(5) _refine_ls_number_reflns 7780 _refine_ls_number_parameters 561 _refine_ls_number_restraints 280 _refine_ls_R_factor_all 0.1351 _refine_ls_R_factor_gt 0.1211 _refine_ls_wR_factor_ref 0.3327 _refine_ls_wR_factor_gt 0.3154 _refine_ls_goodness_of_fit_ref 1.187 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.002 2567 356 ' ' _platon_squeeze_details ; The Platon SQUEEZE procedure was applied to recover 356 electrons per unit cell in one void; that is 118.7 electrons per formula unit. Disordered toluene was present prior to the application of SQUEEZE, and were assigned as 2 toluene molecules (50 electrons/C7H8) in the formula for calculation of the intensive properties. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13. ; 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 0.91052(8) 0.52150(8) 0.14358(5) 0.0850(5) Uani 1 1 d . . . Cl1 Cl 0.96479(15) 0.59892(14) 0.22474(9) 0.1004(7) Uani 1 1 d . . . Cl2 Cl 1.0000 0.47189(13) 0.1667 0.0757(7) Uani 1 2 d S . . O1 O 0.8654(5) 0.5894(4) 0.1258(2) 0.1096(19) Uani 1 1 d . . . O2 O 0.8776(3) 0.4600(3) 0.08162(19) 0.0857(14) Uani 1 1 d . . . N1 N 0.8033(4) 0.4359(5) 0.1826(3) 0.0935(19) Uani 1 1 d . . . C1 C 0.7857(7) 0.5627(7) 0.1189(4) 0.117(3) Uani 1 1 d D . . C2 C 0.7627(8) 0.5918(9) 0.0777(6) 0.162(6) Uani 1 1 d D . . C3 C 0.6836(9) 0.5700(9) 0.0763(4) 0.149(5) Uani 1 1 d D . . H3 H 0.6662 0.5902 0.0479 0.179 Uiso 1 1 calc R . . C4 C 0.6266(8) 0.5217(8) 0.1118(4) 0.125(4) Uani 1 1 d D B . C5 C 0.6513(7) 0.4907(8) 0.1536(3) 0.124(4) Uani 1 1 d D . . H5 H 0.6133 0.4562 0.1793 0.148 Uiso 1 1 calc R . . C6 C 0.7345(5) 0.5120(7) 0.1565(3) 0.100(3) Uani 1 1 d D . . C7 C 0.7619(5) 0.4809(6) 0.1999(3) 0.092(2) Uani 1 1 d . . . H7A H 0.7141 0.4442 0.2217 0.111 Uiso 1 1 calc R . . H7B H 0.7998 0.5272 0.2223 0.111 Uiso 1 1 calc R . . C8 C 0.7475(5) 0.3704(6) 0.1474(3) 0.091(2) Uani 1 1 d . . . H8A H 0.7227 0.3923 0.1227 0.109 Uiso 1 1 calc R . . H8B H 0.7031 0.3271 0.1685 0.109 Uiso 1 1 calc R . . C9 C 0.7889(5) 0.3335(5) 0.1160(3) 0.095(2) Uani 1 1 d D . . C10 C 0.7532(5) 0.2487(6) 0.1150(4) 0.099(3) Uani 1 1 d D . . H10 H 0.7103 0.2161 0.1387 0.119 Uiso 1 1 calc R . . C11 C 0.7802(5) 0.2129(6) 0.0800(3) 0.099(3) Uani 1 1 d D C . C12 C 0.8381(5) 0.2628(5) 0.0436(4) 0.113(3) Uani 1 1 d D . . H12 H 0.8532 0.2378 0.0169 0.135 Uiso 1 1 calc R . . C13 C 0.8747(5) 0.3459(6) 0.0437(3) 0.094(2) Uani 1 1 d D . . C14 C 0.8504(5) 0.3821(6) 0.0796(3) 0.095(2) Uani 1 1 d D . . C15 C 0.8271(6) 0.4026(6) 0.2293(3) 0.098(2) Uani 1 1 d . . . H15A H 0.8518 0.3706 0.2161 0.117 Uiso 1 1 calc R . . H15B H 0.8693 0.4489 0.2498 0.117 Uiso 1 1 calc R . . C16 C 0.7574(5) 0.3493(5) 0.2655(3) 0.088(2) Uani 1 1 d DU A . C17 C 0.751(2) 0.2738(15) 0.2630(16) 0.070(9) Uani 0.20(3) 1 d PDU A 1 H17 H 0.7866 0.2594 0.2453 0.084 Uiso 0.20(3) 1 calc PR A 1 C18 C 0.682(2) 0.224(3) 0.2920(17) 0.064(9) Uani 0.20(3) 1 d PDU A 1 H18 H 0.6749 0.1720 0.3022 0.077 Uiso 0.20(3) 1 calc PR A 1 C19 C 0.624(2) 0.242(3) 0.307(2) 0.081(10) Uani 0.20(3) 1 d PDU A 1 H19 H 0.5667 0.2113 0.3017 0.097 Uiso 0.20(3) 1 calc PR A 1 C20 C 0.667(3) 0.317(3) 0.3335(17) 0.097(10) Uani 0.20(3) 1 d PDU A 1 H20 H 0.6541 0.3241 0.3683 0.116 Uiso 0.20(3) 1 calc PR A 1 C17A C 0.7131(9) 0.2679(7) 0.2631(5) 0.104(4) Uani 0.80(3) 1 d PDU A 2 H17A H 0.7278 0.2430 0.2361 0.125 Uiso 0.80(3) 1 calc PR A 2 C18A C 0.6503(10) 0.2163(11) 0.2942(6) 0.119(6) Uani 0.80(3) 1 d PDU A 2 H18A H 0.6219 0.1588 0.2897 0.143 Uiso 0.80(3) 1 calc PR A 2 C19A C 0.6317(10) 0.2546(12) 0.3324(6) 0.130(6) Uani 0.80(3) 1 d PDU A 2 H19A H 0.5881 0.2213 0.3555 0.155 Uiso 0.80(3) 1 calc PR A 2 C20A C 0.6705(10) 0.3374(11) 0.3404(6) 0.134(6) Uani 0.80(3) 1 d PDU A 2 H20A H 0.6558 0.3623 0.3674 0.161 Uiso 0.80(3) 1 calc PR A 2 C21 C 0.7321(6) 0.3802(6) 0.3055(3) 0.105(3) Uani 1 1 d DU . . H21 H 0.7551 0.4365 0.3132 0.126 Uiso 1 1 calc R A 1 C22 C 0.8203(12) 0.6441(13) 0.0318(6) 0.177(7) Uani 1 1 d . . . C23 C 0.887(2) 0.7237(13) 0.0551(9) 0.252(12) Uani 1 1 d . . . H23A H 0.8703 0.7319 0.0900 0.379 Uiso 1 1 calc R . . H23B H 0.8967 0.7691 0.0320 0.379 Uiso 1 1 calc R . . H23C H 0.9375 0.7213 0.0583 0.379 Uiso 1 1 calc R . . C24 C 0.7744(15) 0.659(2) -0.0125(7) 0.280(16) Uani 1 1 d . . . H24A H 0.7362 0.6074 -0.0293 0.420 Uiso 1 1 calc R . . H24B H 0.8135 0.6960 -0.0388 0.420 Uiso 1 1 calc R . . H24C H 0.7443 0.6844 0.0022 0.420 Uiso 1 1 calc R . . C25 C 0.8536(9) 0.5926(10) 0.0090(4) 0.157(6) Uani 1 1 d . . . H25A H 0.8910 0.6221 -0.0200 0.236 Uiso 1 1 calc R . . H25B H 0.8084 0.5412 -0.0042 0.236 Uiso 1 1 calc R . . H25C H 0.8829 0.5812 0.0364 0.236 Uiso 1 1 calc R . . C26 C 0.5376(8) 0.4990(9) 0.1081(4) 0.142(4) Uani 1 1 d DU . . C27 C 0.501(2) 0.489(3) 0.0530(7) 0.171(14) Uani 0.44(2) 1 d PDU B 3 H27A H 0.4600 0.5059 0.0535 0.256 Uiso 0.44(2) 1 calc PR B 3 H27B H 0.4759 0.4319 0.0422 0.256 Uiso 0.44(2) 1 calc PR B 3 H27C H 0.5445 0.5232 0.0281 0.256 Uiso 0.44(2) 1 calc PR B 3 C28 C 0.4853(16) 0.4174(14) 0.1352(10) 0.146(11) Uani 0.44(2) 1 d PDU B 3 H28A H 0.4584 0.3746 0.1086 0.218 Uiso 0.44(2) 1 calc PR B 3 H28B H 0.4440 0.4202 0.1570 0.218 Uiso 0.44(2) 1 calc PR B 3 H28C H 0.5198 0.4050 0.1576 0.218 Uiso 0.44(2) 1 calc PR B 3 C29 C 0.528(2) 0.5607(18) 0.1411(12) 0.169(12) Uani 0.44(2) 1 d PDU B 3 H29A H 0.5395 0.5556 0.1781 0.253 Uiso 0.44(2) 1 calc PR B 3 H29B H 0.4719 0.5502 0.1378 0.253 Uiso 0.44(2) 1 calc PR B 3 H29C H 0.5660 0.6158 0.1286 0.253 Uiso 0.44(2) 1 calc PR B 3 C27A C 0.4938(15) 0.4307(16) 0.0668(11) 0.170(11) Uani 0.56(2) 1 d PDU B 4 H27D H 0.5303 0.4406 0.0369 0.254 Uiso 0.56(2) 1 calc PR B 4 H27E H 0.4445 0.4303 0.0545 0.254 Uiso 0.56(2) 1 calc PR B 4 H27F H 0.4788 0.3779 0.0828 0.254 Uiso 0.56(2) 1 calc PR B 4 C28A C 0.4967(14) 0.471(2) 0.1601(7) 0.183(13) Uani 0.56(2) 1 d PDU B 4 H28D H 0.4446 0.4707 0.1594 0.275 Uiso 0.56(2) 1 calc PR B 4 H28E H 0.5317 0.5089 0.1876 0.275 Uiso 0.56(2) 1 calc PR B 4 H28F H 0.4868 0.4164 0.1675 0.275 Uiso 0.56(2) 1 calc PR B 4 C29A C 0.5361(12) 0.5742(13) 0.0905(10) 0.160(10) Uani 0.56(2) 1 d PDU B 4 H29D H 0.5710 0.6199 0.1137 0.240 Uiso 0.56(2) 1 calc PR B 4 H29E H 0.4801 0.5641 0.0921 0.240 Uiso 0.56(2) 1 calc PR B 4 H29F H 0.5561 0.5875 0.0542 0.240 Uiso 0.56(2) 1 calc PR B 4 C30 C 0.7427(7) 0.1200(8) 0.0796(6) 0.158(5) Uani 1 1 d DU . . C31 C 0.7511(15) 0.0970(9) 0.1366(8) 0.172(10) Uani 0.63(2) 1 d PDU C 5 H31A H 0.7388 0.0403 0.1377 0.258 Uiso 0.63(2) 1 calc PR C 5 H31B H 0.7129 0.1034 0.1594 0.258 Uiso 0.63(2) 1 calc PR C 5 H31C H 0.8070 0.1329 0.1490 0.258 Uiso 0.63(2) 1 calc PR C 5 C32 C 0.6553(9) 0.0843(10) 0.0639(9) 0.173(11) Uani 0.63(2) 1 d PDU C 5 H32A H 0.6303 0.1096 0.0846 0.259 Uiso 0.63(2) 1 calc PR C 5 H32B H 0.6264 0.0254 0.0704 0.259 Uiso 0.63(2) 1 calc PR C 5 H32C H 0.6522 0.0944 0.0264 0.259 Uiso 0.63(2) 1 calc PR C 5 C33 C 0.7831(16) 0.0830(19) 0.0491(13) 0.243(18) Uani 0.63(2) 1 d PDU C 5 H33A H 0.7697 0.0813 0.0117 0.365 Uiso 0.63(2) 1 calc PR C 5 H33B H 0.7641 0.0275 0.0618 0.365 Uiso 0.63(2) 1 calc PR C 5 H33C H 0.8423 0.1159 0.0537 0.365 Uiso 0.63(2) 1 calc PR C 5 C31A C 0.684(2) 0.068(2) 0.1203(13) 0.27(3) Uani 0.37(2) 1 d PDU C 6 H31D H 0.7089 0.0436 0.1423 0.406 Uiso 0.37(2) 1 calc PR C 6 H31E H 0.6351 0.0241 0.1032 0.406 Uiso 0.37(2) 1 calc PR C 6 H31F H 0.6686 0.1005 0.1422 0.406 Uiso 0.37(2) 1 calc PR C 6 C32A C 0.702(2) 0.101(2) 0.0243(11) 0.180(12) Uani 0.37(2) 1 d PDU C 6 H32D H 0.7333 0.1474 0.0009 0.270 Uiso 0.37(2) 1 calc PR C 6 H32E H 0.6462 0.0896 0.0273 0.270 Uiso 0.37(2) 1 calc PR C 6 H32F H 0.7023 0.0527 0.0097 0.270 Uiso 0.37(2) 1 calc PR C 6 C33A C 0.8063(15) 0.0922(14) 0.0748(12) 0.108(9) Uani 0.37(2) 1 d PDU C 6 H33D H 0.8444 0.1139 0.1044 0.161 Uiso 0.37(2) 1 calc PR C 6 H33E H 0.8363 0.1125 0.0416 0.161 Uiso 0.37(2) 1 calc PR C 6 H33F H 0.7785 0.0325 0.0752 0.161 Uiso 0.37(2) 1 calc PR C 6 C34 C 0.9338(6) 0.3935(7) -0.0020(4) 0.116(3) Uani 1 1 d . . . C35 C 0.8966(7) 0.4365(8) -0.0321(4) 0.136(4) Uani 1 1 d . . . H35A H 0.9188 0.4487 -0.0679 0.204 Uiso 1 1 calc R . . H35B H 0.9099 0.4874 -0.0140 0.204 Uiso 1 1 calc R . . H35C H 0.8373 0.4012 -0.0336 0.204 Uiso 1 1 calc R . . C36 C 1.0156(5) 0.4552(6) 0.0229(3) 0.106(3) Uani 1 1 d . . . H36A H 1.0419 0.4262 0.0376 0.159 Uiso 1 1 calc R . . H36B H 1.0062 0.4848 0.0511 0.159 Uiso 1 1 calc R . . H36C H 1.0510 0.4938 -0.0040 0.159 Uiso 1 1 calc R . . C37 C 0.9451(6) 0.3397(7) -0.0391(3) 0.117(3) Uani 1 1 d . . . H37A H 0.8918 0.2944 -0.0496 0.175 Uiso 1 1 calc R . . H37B H 0.9767 0.3181 -0.0220 0.175 Uiso 1 1 calc R . . H37C H 0.9744 0.3709 -0.0704 0.175 Uiso 1 1 calc R . . O3 O 0.9261(16) 0.7506(11) 0.1950(8) 0.176(7) Uani 0.50 1 d PDU D -1 C38 C 0.839(2) 0.710(3) 0.210(2) 0.158(12) Uani 0.25 1 d PDU D -1 H38A H 0.8308 0.6943 0.2474 0.190 Uiso 0.25 1 calc PR D -1 H38B H 0.8059 0.6609 0.1878 0.190 Uiso 0.25 1 calc PR D -1 C39 C 0.820(3) 0.775(2) 0.1983(18) 0.155(11) Uani 0.25 1 d PDU D -1 H39A H 0.7763 0.7699 0.2224 0.186 Uiso 0.25 1 calc PR D -1 H39B H 0.7995 0.7695 0.1617 0.186 Uiso 0.25 1 calc PR D -1 C40 C 0.894(2) 0.857(2) 0.2053(12) 0.185(9) Uani 0.50 1 d PDU D -1 H40A H 0.9062 0.8722 0.2428 0.221 Uiso 0.50 1 calc PR D -1 H40B H 0.8897 0.9003 0.1861 0.221 Uiso 0.50 1 calc PR D -1 C41 C 0.956(2) 0.8383(15) 0.1800(13) 0.213(11) Uani 0.50 1 d PDU D -1 H41A H 0.9566 0.8446 0.1412 0.256 Uiso 0.50 1 calc PR D -1 H41B H 1.0112 0.8747 0.1939 0.256 Uiso 0.50 1 calc PR D -1 C38A C 0.882(4) 0.743(3) 0.2443(19) 0.160(14) Uani 0.25 1 d PDU E 7 C39A C 0.901(3) 0.828(3) 0.2584(13) 0.166(16) Uani 0.25 1 d PDU E 7 Li1 Li 0.943(4) 0.658(4) 0.164(2) 0.088(14) Uani 0.25 1 d PU . 8 Li1A Li 0.941(3) 0.700(4) 0.160(2) 0.075(11) Uani 0.25 1 d PU . 9 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 0.0916(8) 0.0956(9) 0.0744(7) -0.0015(6) -0.0130(6) 0.0516(7) Cl1 0.1210(16) 0.1096(15) 0.0922(13) -0.0233(11) -0.0146(12) 0.0739(13) Cl2 0.0862(16) 0.0795(11) 0.0636(12) -0.0025(6) -0.0050(11) 0.0431(8) O1 0.142(5) 0.119(5) 0.101(4) -0.001(3) -0.017(4) 0.090(4) O2 0.083(3) 0.102(4) 0.062(3) 0.002(2) -0.014(2) 0.038(3) N1 0.100(5) 0.118(5) 0.075(4) -0.001(4) 0.000(3) 0.064(4) C1 0.130(8) 0.163(9) 0.116(7) -0.009(7) -0.027(7) 0.116(8) C2 0.163(11) 0.208(14) 0.203(14) -0.015(12) -0.043(11) 0.159(12) C3 0.229(16) 0.219(15) 0.078(6) -0.009(8) -0.022(9) 0.171(14) C4 0.160(10) 0.183(11) 0.089(6) -0.005(7) -0.019(7) 0.130(9) C5 0.137(8) 0.198(11) 0.071(5) -0.010(6) 0.000(5) 0.110(8) C6 0.102(6) 0.143(8) 0.071(5) -0.011(5) -0.012(4) 0.072(6) C7 0.087(5) 0.124(7) 0.077(5) -0.005(4) -0.005(4) 0.061(5) C8 0.087(5) 0.121(6) 0.072(4) -0.016(4) -0.012(4) 0.058(5) C9 0.085(5) 0.103(6) 0.085(5) -0.003(4) -0.011(4) 0.038(5) C10 0.068(4) 0.117(7) 0.098(6) -0.003(5) -0.003(4) 0.036(5) C11 0.089(5) 0.107(6) 0.084(5) -0.017(5) 0.018(4) 0.036(5) C12 0.087(6) 0.100(7) 0.130(8) -0.047(6) -0.001(5) 0.031(5) C13 0.080(5) 0.129(7) 0.072(5) -0.031(5) -0.009(4) 0.052(5) C14 0.079(5) 0.103(6) 0.081(5) 0.004(5) -0.008(4) 0.029(5) C15 0.106(6) 0.113(6) 0.079(5) 0.018(4) -0.002(4) 0.059(5) C16 0.093(5) 0.118(6) 0.065(4) -0.010(4) -0.004(4) 0.062(5) C17 0.063(15) 0.099(16) 0.069(15) 0.007(13) 0.012(13) 0.057(12) C18 0.070(16) 0.095(17) 0.052(15) 0.026(14) 0.010(14) 0.060(14) C19 0.076(16) 0.091(17) 0.089(19) -0.002(16) 0.015(16) 0.052(13) C20 0.104(12) 0.097(13) 0.089(12) -0.008(9) 0.001(9) 0.050(8) C17A 0.112(8) 0.100(7) 0.090(6) -0.009(5) 0.019(6) 0.045(5) C18A 0.114(11) 0.118(9) 0.112(9) -0.007(8) 0.013(10) 0.048(10) C19A 0.119(9) 0.160(12) 0.088(9) 0.022(9) 0.023(8) 0.054(9) C20A 0.150(8) 0.145(9) 0.122(8) -0.012(7) 0.017(6) 0.085(7) C21 0.140(7) 0.103(5) 0.077(5) 0.001(4) 0.010(5) 0.064(5) C22 0.201(15) 0.220(18) 0.148(12) 0.103(13) 0.021(11) 0.133(14) C23 0.40(4) 0.159(15) 0.22(2) 0.047(16) 0.04(2) 0.16(2) C24 0.28(2) 0.54(5) 0.163(13) 0.16(2) 0.075(15) 0.31(3) C25 0.177(12) 0.264(17) 0.098(7) 0.077(9) 0.044(7) 0.162(13) C26 0.152(9) 0.241(14) 0.092(7) 0.026(8) 0.013(6) 0.142(10) C27 0.18(2) 0.29(4) 0.067(13) 0.00(2) -0.009(14) 0.14(3) C28 0.17(2) 0.20(3) 0.108(18) -0.041(17) -0.076(17) 0.12(2) C29 0.16(2) 0.24(3) 0.12(2) 0.04(2) 0.025(18) 0.11(2) C27A 0.138(18) 0.25(3) 0.15(2) 0.04(2) 0.020(16) 0.118(19) C28A 0.101(14) 0.35(4) 0.105(15) 0.00(2) 0.013(12) 0.12(2) C29A 0.133(15) 0.26(3) 0.16(2) -0.054(18) -0.050(14) 0.152(17) C30 0.105(7) 0.122(8) 0.203(12) -0.058(9) 0.017(8) 0.025(6) C31 0.180(19) 0.054(8) 0.24(2) -0.037(11) -0.068(18) 0.024(10) C32 0.123(14) 0.081(9) 0.25(2) -0.043(13) 0.087(15) 0.003(9) C33 0.15(2) 0.21(2) 0.29(3) -0.16(2) 0.05(2) 0.037(18) C31A 0.20(3) 0.19(3) 0.19(3) -0.08(3) 0.01(3) -0.07(3) C32A 0.134(18) 0.121(16) 0.23(2) -0.041(17) 0.020(18) 0.021(15) C33A 0.152(17) 0.055(10) 0.127(16) -0.034(10) -0.009(13) 0.061(11) C34 0.088(6) 0.127(7) 0.082(5) -0.007(5) 0.007(5) 0.016(5) C35 0.115(8) 0.151(9) 0.082(6) 0.009(6) 0.024(6) 0.021(7) C36 0.083(5) 0.122(7) 0.083(5) 0.005(5) 0.030(4) 0.029(5) C37 0.104(6) 0.142(8) 0.074(5) -0.022(5) 0.009(5) 0.039(6) O3 0.29(2) 0.153(12) 0.140(11) 0.022(10) 0.034(12) 0.150(13) C38 0.26(3) 0.141(19) 0.101(17) 0.062(16) 0.066(18) 0.123(19) C39 0.22(3) 0.156(19) 0.130(18) 0.072(17) 0.078(18) 0.125(18) C40 0.26(2) 0.166(16) 0.168(17) 0.065(15) 0.036(16) 0.132(16) C41 0.29(2) 0.171(16) 0.162(17) 0.077(14) 0.026(17) 0.101(17) C38A 0.20(3) 0.16(3) 0.17(3) 0.06(3) 0.09(3) 0.12(2) C39A 0.19(3) 0.17(3) 0.13(3) 0.08(2) 0.11(2) 0.09(3) Li1 0.093(16) 0.086(16) 0.086(16) 0.003(10) -0.009(10) 0.045(11) Li1A 0.071(14) 0.082(14) 0.082(15) -0.003(9) 0.011(9) 0.046(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 O2 1.870(5) . ? Cr1 O1 1.921(6) . ? Cr1 N1 2.108(7) . ? Cr1 Cl2 2.386(2) . ? Cr1 Li1 2.40(7) . ? Cr1 Cl1 2.425(3) 6_765 ? Cr1 Cl1 2.439(3) . ? Cr1 Li1A 3.15(6) . ? Cl1 Li1 2.06(6) . ? Cl1 Cr1 2.425(3) 6_765 ? Cl1 Li1 2.45(7) 6_765 ? Cl1 Li1A 2.72(6) . ? Cl1 Li1A 2.94(5) 6_765 ? Cl2 Cr1 2.386(2) 6_765 ? O1 C1 1.342(12) . ? O1 Li1 1.70(6) . ? O1 Li1A 2.04(6) . ? O2 C14 1.298(10) . ? N1 C8 1.464(11) . ? N1 C7 1.485(11) . ? N1 C15 1.514(10) . ? C1 C2 1.353(13) . ? C1 C6 1.356(12) . ? C2 C3 1.340(14) . ? C2 C22 1.57(2) . ? C3 C4 1.354(13) . ? C3 H3 0.9500 . ? C4 C5 1.401(12) . ? C4 C26 1.520(16) . ? C5 C6 1.420(12) . ? C5 H5 0.9500 . ? C6 C7 1.462(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.513(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.398(11) . ? C9 C14 1.408(10) . ? C10 C11 1.363(11) . ? C10 H10 0.9500 . ? C11 C12 1.383(11) . ? C11 C30 1.533(16) . ? C12 C13 1.366(11) . ? C12 H12 0.9500 . ? C13 C14 1.353(10) . ? C13 C34 1.550(13) . ? C15 C16 1.508(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17A 1.339(13) . ? C16 C21 1.372(10) . ? C16 C17 1.378(19) . ? C17 C18 1.381(19) . ? C17 H17 0.9500 . ? C18 C19 1.38(2) . ? C18 H18 0.9500 . ? C19 C20 1.39(2) . ? C19 H19 0.9500 . ? C20 C21 1.41(2) . ? C20 H20 0.9500 . ? C17A C18A 1.352(14) . ? C17A H17A 0.9500 . ? C18A C19A 1.360(16) . ? C18A H18A 0.9500 . ? C19A C20A 1.375(16) . ? C19A H19A 0.9500 . ? C20A C21 1.364(14) . ? C20A H20A 0.9500 . ? C21 H21 0.9500 . ? C22 C25 1.52(2) . ? C22 C23 1.52(3) . ? C22 C24 1.53(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C28A 1.488(15) . ? C26 C29A 1.508(16) . ? C26 C28 1.521(18) . ? C26 C29 1.522(17) . ? C26 C27 1.527(16) . ? C26 C27A 1.545(17) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C27A H27D 0.9800 . ? C27A H27E 0.9800 . ? C27A H27F 0.9800 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29D 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C30 C31A 1.479(18) . ? C30 C33 1.488(16) . ? C30 C32 1.495(15) . ? C30 C33A 1.542(17) . ? C30 C31 1.543(16) . ? C30 C32A 1.552(18) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33A H33D 0.9800 . ? C33A H33E 0.9800 . ? C33A H33F 0.9800 . ? C34 C37 1.481(15) . ? C34 C35 1.521(17) . ? C34 C36 1.536(13) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? O3 C38 1.48(2) . ? O3 C41 1.512(18) . ? C38 C39 1.48(2) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.49(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.525(19) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C38A C39A 1.50(2) . ? Li1 Li1 1.86(12) 6_765 ? Li1 Cl1 2.45(7) 6_765 ? Li1A Li1A 1.96(9) 6_765 ? Li1A Cl1 2.94(5) 6_765 ? 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 O1 95.7(3) . . ? O2 Cr1 N1 91.3(3) . . ? O1 Cr1 N1 92.6(3) . . ? O2 Cr1 Cl2 92.40(18) . . ? O1 Cr1 Cl2 164.4(2) . . ? N1 Cr1 Cl2 100.5(2) . . ? O2 Cr1 Li1 133.0(13) . . ? O1 Cr1 Li1 44.8(14) . . ? N1 Cr1 Li1 111.0(15) . . ? Cl2 Cr1 Li1 121.3(14) . . ? O2 Cr1 Cl1 96.59(19) . 6_765 ? O1 Cr1 Cl1 83.6(2) . 6_765 ? N1 Cr1 Cl1 171.5(2) . 6_765 ? Cl2 Cr1 Cl1 82.25(7) . 6_765 ? Li1 Cr1 Cl1 61.1(14) . 6_765 ? O2 Cr1 Cl1 174.19(19) . . ? O1 Cr1 Cl1 89.5(2) . . ? N1 Cr1 Cl1 91.2(2) . . ? Cl2 Cr1 Cl1 81.98(7) . . ? Li1 Cr1 Cl1 50.4(13) . . ? Cl1 Cr1 Cl1 81.26(11) 6_765 . ? O2 Cr1 Li1A 127.2(10) . . ? O1 Cr1 Li1A 38.7(9) . . ? N1 Cr1 Li1A 110.7(8) . . ? Cl2 Cr1 Li1A 127.0(9) . . ? Li1 Cr1 Li1A 6.3(16) . . ? Cl1 Cr1 Li1A 61.9(8) 6_765 . ? Cl1 Cr1 Li1A 56.5(10) . . ? Li1 Cl1 Cr1 97.1(17) . 6_765 ? Li1 Cl1 Cr1 63.8(18) . . ? Cr1 Cl1 Cr1 81.08(8) 6_765 . ? Li1 Cl1 Li1 48(3) . 6_765 ? Cr1 Cl1 Li1 58.9(15) 6_765 6_765 ? Cr1 Cl1 Li1 87.1(13) . 6_765 ? Cr1 Cl1 Li1A 101.9(9) 6_765 . ? Cr1 Cl1 Li1A 75.1(11) . . ? Cr1 Cl1 Li1A 71.3(11) 6_765 6_765 ? Cr1 Cl1 Li1A 95.7(11) . 6_765 ? Cr1 Cl2 Cr1 82.98(10) 6_765 . ? C1 O1 Li1 138(2) . . ? C1 O1 Cr1 124.8(7) . . ? Li1 O1 Cr1 83(2) . . ? C1 O1 Li1A 121.6(15) . . ? Cr1 O1 Li1A 105.3(15) . . ? C14 O2 Cr1 124.2(5) . . ? C8 N1 C7 107.6(6) . . ? C8 N1 C15 111.3(7) . . ? C7 N1 C15 111.2(6) . . ? C8 N1 Cr1 112.0(5) . . ? C7 N1 Cr1 106.3(5) . . ? C15 N1 Cr1 108.4(5) . . ? O1 C1 C2 118.5(11) . . ? O1 C1 C6 116.6(8) . . ? C2 C1 C6 124.7(11) . . ? C3 C2 C1 115.7(13) . . ? C3 C2 C22 119.5(11) . . ? C1 C2 C22 124.7(11) . . ? C2 C3 C4 125.6(11) . . ? C2 C3 H3 117.2 . . ? C4 C3 H3 117.2 . . ? C3 C4 C5 117.8(10) . . ? C3 C4 C26 123.2(9) . . ? C5 C4 C26 119.0(11) . . ? C4 C5 C6 118.4(10) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C1 C6 C5 117.7(9) . . ? C1 C6 C7 122.8(8) . . ? C5 C6 C7 119.4(9) . . ? C6 C7 N1 113.9(7) . . ? C6 C7 H7A 108.8 . . ? N1 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? N1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C9 113.1(7) . . ? N1 C8 H8A 109.0 . . ? C9 C8 H8A 109.0 . . ? N1 C8 H8B 109.0 . . ? C9 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C14 120.4(8) . . ? C10 C9 C8 118.4(7) . . ? C14 C9 C8 119.6(8) . . ? C11 C10 C9 119.8(8) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 117.4(9) . . ? C10 C11 C30 120.2(8) . . ? C12 C11 C30 122.3(8) . . ? C13 C12 C11 124.0(8) . . ? C13 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? C14 C13 C12 118.6(8) . . ? C14 C13 C34 122.6(9) . . ? C12 C13 C34 118.2(8) . . ? O2 C14 C13 124.1(8) . . ? O2 C14 C9 116.4(8) . . ? C13 C14 C9 119.4(9) . . ? C16 C15 N1 114.3(7) . . ? C16 C15 H15A 108.7 . . ? N1 C15 H15A 108.7 . . ? C16 C15 H15B 108.7 . . ? N1 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C17A C16 C21 111.9(10) . . ? C21 C16 C17 127.7(16) . . ? C17A C16 C15 125.4(10) . . ? C21 C16 C15 122.8(8) . . ? C17 C16 C15 104.9(14) . . ? C16 C17 C18 104(3) . . ? C16 C17 H17 127.8 . . ? C18 C17 H17 127.8 . . ? C19 C18 C17 125(4) . . ? C19 C18 H18 117.3 . . ? C17 C18 H18 117.3 . . ? C18 C19 C20 104(5) . . ? C18 C19 H19 127.8 . . ? C20 C19 H19 127.8 . . ? C19 C20 C21 117(4) . . ? C19 C20 H20 121.7 . . ? C21 C20 H20 121.7 . . ? C16 C17A C18A 128.7(14) . . ? C16 C17A H17A 115.7 . . ? C18A C17A H17A 115.7 . . ? C17A C18A C19A 113.6(16) . . ? C17A C18A H18A 123.2 . . ? C19A C18A H18A 123.2 . . ? C18A C19A C20A 125.5(15) . . ? C18A C19A H19A 117.2 . . ? C20A C19A H19A 117.2 . . ? C21 C20A C19A 113.1(14) . . ? C21 C20A H20A 123.5 . . ? C19A C20A H20A 123.5 . . ? C20A C21 C16 127.3(11) . . ? C16 C21 C20 110(2) . . ? C20A C21 H21 108.0 . . ? C16 C21 H21 124.8 . . ? C20 C21 H21 124.8 . . ? C25 C22 C23 112.2(16) . . ? C25 C22 C24 107.3(16) . . ? C23 C22 C24 111.6(17) . . ? C25 C22 C2 105.0(12) . . ? C23 C22 C2 108.0(16) . . ? C24 C22 C2 112.6(14) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28A C26 C29A 110.0(16) . . ? C28A C26 C4 110.7(11) . . ? C29A C26 C4 107.1(12) . . ? C29A C26 C28 141.6(16) . . ? C4 C26 C28 109.0(13) . . ? C28A C26 C29 62.5(16) . . ? C29A C26 C29 51.0(13) . . ? C4 C26 C29 106.9(17) . . ? C28 C26 C29 105.2(15) . . ? C28A C26 C27 130.2(18) . . ? C29A C26 C27 67.9(17) . . ? C4 C26 C27 117.4(16) . . ? C28 C26 C27 105.4(18) . . ? C29 C26 C27 112.2(18) . . ? C28A C26 C27A 109.9(17) . . ? C29A C26 C27A 109.5(14) . . ? C4 C26 C27A 109.6(12) . . ? C28 C26 C27A 69.7(15) . . ? C29 C26 C27A 142.7(18) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C27A H27D 109.5 . . ? C26 C27A H27E 109.5 . . ? H27D C27A H27E 109.5 . . ? C26 C27A H27F 109.5 . . ? H27D C27A H27F 109.5 . . ? H27E C27A H27F 109.5 . . ? C26 C28A H28D 109.5 . . ? C26 C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C26 C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C26 C29A H29D 109.5 . . ? C26 C29A H29E 109.5 . . ? H29D C29A H29E 109.5 . . ? C26 C29A H29F 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C31A C30 C33 116(3) . . ? C31A C30 C32 65.8(19) . . ? C33 C30 C32 111.2(14) . . ? C31A C30 C11 122(2) . . ? C33 C30 C11 119.5(15) . . ? C32 C30 C11 107.1(11) . . ? C31A C30 C33A 106(2) . . ? C32 C30 C33A 134.5(13) . . ? C11 C30 C33A 113.6(11) . . ? C31A C30 C31 46.0(19) . . ? C33 C30 C31 101.9(18) . . ? C32 C30 C31 111.7(14) . . ? C11 C30 C31 105.2(10) . . ? C33A C30 C31 76.7(17) . . ? C31A C30 C32A 110.9(18) . . ? C33 C30 C32A 74.1(19) . . ? C32 C30 C32A 49.4(15) . . ? C11 C30 C32A 99.7(17) . . ? C33A C30 C32A 102.9(17) . . ? C31 C30 C32A 152.9(16) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C31A H31D 109.5 . . ? C30 C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C30 C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C30 C32A H32D 109.5 . . ? C30 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C30 C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? C30 C33A H33D 109.5 . . ? C30 C33A H33E 109.5 . . ? H33D C33A H33E 109.5 . . ? C30 C33A H33F 109.5 . . ? H33D C33A H33F 109.5 . . ? H33E C33A H33F 109.5 . . ? C37 C34 C35 108.4(9) . . ? C37 C34 C36 110.3(9) . . ? C35 C34 C36 111.1(10) . . ? C37 C34 C13 112.7(9) . . ? C35 C34 C13 107.1(8) . . ? C36 C34 C13 107.1(7) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C38 O3 C41 110(2) . . ? O3 C38 C39 101(3) . . ? O3 C38 H38A 111.6 . . ? C39 C38 H38A 111.6 . . ? O3 C38 H38B 111.6 . . ? C39 C38 H38B 111.6 . . ? H38A C38 H38B 109.4 . . ? C38 C39 C40 110(3) . . ? C38 C39 H39A 109.6 . . ? C40 C39 H39A 109.6 . . ? C38 C39 H39B 109.6 . . ? C40 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C39 C40 C41 98(3) . . ? C39 C40 H40A 112.1 . . ? C41 C40 H40A 112.1 . . ? C39 C40 H40B 112.1 . . ? C41 C40 H40B 112.1 . . ? H40A C40 H40B 109.8 . . ? O3 C41 C40 104(2) . . ? O3 C41 H41A 110.9 . . ? C40 C41 H41A 110.9 . . ? O3 C41 H41B 110.9 . . ? C40 C41 H41B 110.9 . . ? H41A C41 H41B 109.0 . . ? O1 Li1 Li1 142(5) . 6_765 ? O1 Li1 Cl1 110(3) . . ? Li1 Li1 Cl1 77(3) 6_765 . ? O1 Li1 Cr1 52.6(18) . . ? Li1 Li1 Cr1 103.8(17) 6_765 . ? Cl1 Li1 Cr1 66(2) . . ? O1 Li1 Cl1 87(3) . 6_765 ? Li1 Li1 Cl1 55(2) 6_765 6_765 ? Cl1 Li1 Cl1 89(2) . 6_765 ? Cr1 Li1 Cl1 60.0(17) . 6_765 ? Li1A Li1A O1 132.3(19) 6_765 . ? Li1A Li1A Cl1 75.9(19) 6_765 . ? O1 Li1A Cl1 79.5(19) . . ? Li1A Li1A Cl1 63.9(18) 6_765 6_765 ? O1 Li1A Cl1 69.2(15) . 6_765 ? Cl1 Li1A Cl1 68.0(13) . 6_765 ? Li1A Li1A Cr1 100.4(9) 6_765 . ? O1 Li1A Cr1 36.0(10) . . ? Cl1 Li1A Cr1 48.4(10) . . ? Cl1 Li1A Cr1 46.8(8) 6_765 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.090 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.091 _iucr_refine_instructions_details ; TITL _HC013 CELL 0.71075 18.94500 18.94500 25.39000 90.000 90.000 120.000 ZERR 3 0.00900 0.00900 0.01300 0.000 0.000 0.000 LATT -1 SYMM -Y, +X-Y, .333+Z SYMM -X+Y, -X, .666+Z SYMM +Y, +X, -Z SYMM +X-Y, -Y, .666-Z SYMM -X, -X+Y, .333-Z SFAC C H CL CR N O LI UNIT 276 378 9 6 6 15 3 SHEL 8.147180 0.891225 L.S. 5 FMAP 2 PLAN -25 TEMP -150.0 ACTA BOND $H SIZE 0.400 0.400 0.320 DFIX 1.5000 0.0200 O3 C38 DFIX 1.5000 0.0200 O3 C38A DFIX 1.5000 0.0200 C38 C39 DFIX 1.5000 0.0200 C38A C39A DFIX 1.5000 0.0200 C39 C40 DFIX 1.5000 0.0200 C39A C40 DFIX 1.5000 0.0200 C40 C41 DFIX 1.5000 0.0200 C41 O3 ISOR 0.01 0.02 C17A C20 C20A C33A Li1 Li1A DFIX 1.5000 0.0200 C26 C29 DFIX 1.5000 0.0200 C26 C29A DFIX 1.5000 0.0200 C26 C27 DFIX 1.5000 0.0200 C26 C27A DFIX 1.5000 0.0200 C26 C28A DFIX 1.5000 0.0200 C26 C28 DFIX 1.5000 0.0200 C30 C31 DFIX 1.5000 0.0200 C30 C31A DFIX 1.5000 0.0200 C30 C32 DFIX 1.5000 0.0200 C30 C32A DFIX 1.5000 0.0200 C30 C33 DFIX 1.5000 0.0200 C30 C33A DFIX 1.395 0.0200 C16 C17 DFIX 1.395 0.0200 C17 C18 DFIX 1.395 0.0200 C18 C19 DFIX 1.395 0.0200 C21 C16 DFIX 1.395 0.0200 C19 C20 DFIX 1.395 0.0200 C20 C21 DFIX 1.395 0.0200 C16 C17A DFIX 1.395 0.0200 C17A C18A DFIX 1.395 0.0200 C18A C19A DFIX 1.395 0.0200 C19A C20A DFIX 1.395 0.0200 C20A C21 DFIX 1.395 0.0200 C1 C2 DFIX 1.395 0.0200 C2 C3 DFIX 1.395 0.0200 C3 C4 DFIX 1.395 0.0200 C4 C5 DFIX 1.395 0.0200 C5 C6 DFIX 1.395 0.0200 C6 C1 DFIX 1.395 0.0200 C9 C10 DFIX 1.395 0.0200 C10 C11 DFIX 1.395 0.0200 C11 C12 DFIX 1.395 0.0200 C12 C13 DFIX 1.395 0.0200 C13 C14 DFIX 1.395 0.0200 C14 C9 SIMU 0.025 0.05 1.7 C26 C29 SIMU 0.025 0.05 1.7 C26 C29A SIMU 0.025 0.05 1.7 C26 C27 SIMU 0.025 0.05 1.7 C26 C27A SIMU 0.025 0.05 1.7 C26 C28A SIMU 0.025 0.05 1.7 C26 C28 SIMU 0.025 0.05 1.7 C30 C31 SIMU 0.025 0.05 1.7 C30 C31A SIMU 0.025 0.05 1.7 C30 C32 SIMU 0.01 0.02 1.7 C30 C32A SIMU 0.025 0.05 1.7 C30 C33 SIMU 0.025 0.05 1.7 C30 C33A SIMU 0.025 0.05 1.7 C16 C17 SIMU 0.025 0.05 1.7 C17 C18 SIMU 0.025 0.05 1.7 C18 C19 SIMU 0.025 0.05 1.7 C21 C16 SIMU 0.025 0.05 1.7 C19 C20 SIMU 0.025 0.05 1.7 C20 C21 SIMU 0.025 0.05 1.7 C16 C17A SIMU 0.025 0.05 1.7 C17A C18A SIMU 0.025 0.05 1.7 C18A C19A SIMU 0.025 0.05 1.7 C19A C20A SIMU 0.025 0.05 1.7 C20A C21 SIMU 0.025 0.05 1.7 O3 C38 SIMU 0.025 0.05 1.7 O3 C38A SIMU 0.025 0.05 1.7 C38 C39 SIMU 0.025 0.05 1.7 C38A C39A SIMU 0.025 0.05 1.7 C39 C40 SIMU 0.025 0.05 1.7 C39A C40 SIMU 0.025 0.05 1.7 C40 C41 SIMU 0.025 0.05 1.7 C41 O3 FLAT 0.0100 C16 C17A C18A C19A C20A C21 DANG 2.4741 0.0400 C33A C31A DANG 2.4647 0.0400 C31A C32A DANG 2.5205 0.0400 C32A C33A DANG 2.4419 0.0400 C33 C31 DANG 2.5116 0.0400 C31 C32 DANG 2.4515 0.0400 C32 C33 DANG 2.5068 0.0400 C27 C28 DANG 2.4936 0.0400 C28 C29 DANG 2.4865 0.0400 C29 C27 DANG 2.4903 0.0400 C27A C28A DANG 2.4592 0.0400 C28A C29A DANG 2.4948 0.0400 C29A C27A WGHT 0.200000 FVAR 1.03072 0.20256 0.44214 0.62660 CR1 4 0.910520 0.521499 0.143584 11.00000 0.09156 0.09562 = 0.07439 -0.00154 -0.01299 0.05163 CL1 3 0.964794 0.598920 0.224744 11.00000 0.12098 0.10957 = 0.09223 -0.02326 -0.01462 0.07393 CL2 3 1.000000 0.471888 0.166667 10.50000 0.08616 0.07950 = 0.06359 -0.00249 -0.00497 0.04308 O1 6 0.865401 0.589426 0.125805 11.00000 0.14168 0.11862 = 0.10124 -0.00061 -0.01676 0.08972 O2 6 0.877631 0.459956 0.081624 11.00000 0.08274 0.10185 = 0.06186 0.00162 -0.01416 0.03808 N1 5 0.803307 0.435906 0.182579 11.00000 0.10030 0.11794 = 0.07496 -0.00146 -0.00007 0.06404 C1 1 0.785706 0.562665 0.118946 11.00000 0.12962 0.16319 = 0.11561 -0.00895 -0.02688 0.11639 C2 1 0.762664 0.591771 0.077711 11.00000 0.16311 0.20777 = 0.20307 -0.01507 -0.04318 0.15910 C3 1 0.683640 0.570002 0.076260 11.00000 0.22905 0.21887 = 0.07839 -0.00912 -0.02188 0.17122 AFIX 43 H3 2 0.666181 0.590215 0.047864 11.00000 -1.20000 AFIX 0 C4 1 0.626564 0.521660 0.111810 11.00000 0.16020 0.18334 = 0.08910 -0.00476 -0.01923 0.13016 C5 1 0.651272 0.490681 0.153559 11.00000 0.13736 0.19755 = 0.07071 -0.00950 0.00038 0.10979 AFIX 43 H5 2 0.613269 0.456225 0.179327 11.00000 -1.20000 AFIX 0 C6 1 0.734488 0.512003 0.156456 11.00000 0.10165 0.14260 = 0.07075 -0.01122 -0.01220 0.07230 C7 1 0.761869 0.480877 0.199872 11.00000 0.08674 0.12395 = 0.07716 -0.00541 -0.00533 0.06109 AFIX 23 H7A 2 0.714136 0.444171 0.221717 11.00000 -1.20000 H7B 2 0.799764 0.527224 0.222293 11.00000 -1.20000 AFIX 0 C8 1 0.747536 0.370431 0.147357 11.00000 0.08670 0.12129 = 0.07198 -0.01578 -0.01175 0.05770 AFIX 23 H8A 2 0.722652 0.392259 0.122700 11.00000 -1.20000 H8B 2 0.703130 0.327091 0.168528 11.00000 -1.20000 AFIX 0 C9 1 0.788947 0.333542 0.115954 11.00000 0.08482 0.10318 = 0.08511 -0.00333 -0.01140 0.03755 C10 1 0.753239 0.248703 0.114996 11.00000 0.06832 0.11713 = 0.09793 -0.00268 -0.00284 0.03625 AFIX 43 H10 2 0.710264 0.216104 0.138661 11.00000 -1.20000 AFIX 0 C11 1 0.780219 0.212875 0.080037 11.00000 0.08921 0.10665 = 0.08429 -0.01678 0.01764 0.03580 C12 1 0.838067 0.262814 0.043628 11.00000 0.08744 0.09997 = 0.13027 -0.04730 -0.00140 0.03121 AFIX 43 H12 2 0.853234 0.237798 0.016940 11.00000 -1.20000 AFIX 0 C13 1 0.874716 0.345872 0.043690 11.00000 0.08019 0.12907 = 0.07192 -0.03121 -0.00880 0.05179 C14 1 0.850395 0.382074 0.079587 11.00000 0.07904 0.10332 = 0.08080 0.00423 -0.00786 0.02858 C15 1 0.827125 0.402562 0.229273 11.00000 0.10576 0.11293 = 0.07915 0.01848 -0.00196 0.05865 AFIX 23 H15A 2 0.851775 0.370594 0.216068 11.00000 -1.20000 H15B 2 0.869295 0.448877 0.249849 11.00000 -1.20000 AFIX 0 C16 1 0.757414 0.349298 0.265463 11.00000 0.09292 0.11778 = 0.06490 -0.00963 -0.00362 0.06239 PART 1 C17 1 0.751335 0.273786 0.262959 21.00000 0.06337 0.09936 = 0.06864 0.00713 0.01173 0.05723 AFIX 43 H17 2 0.786559 0.259448 0.245252 21.00000 -1.20000 AFIX 0 C18 1 0.682485 0.223635 0.291998 21.00000 0.07032 0.09548 = 0.05175 0.02571 0.01028 0.06047 AFIX 43 H18 2 0.674858 0.172014 0.302155 21.00000 -1.20000 AFIX 0 C19 1 0.623831 0.242262 0.307492 21.00000 0.07616 0.09061 = 0.08935 -0.00229 0.01488 0.05218 AFIX 43 H19 2 0.566685 0.211332 0.301727 21.00000 -1.20000 AFIX 0 C20 1 0.667356 0.316595 0.333462 21.00000 0.10405 0.09717 = 0.08915 -0.00815 0.00137 0.04988 AFIX 43 H20 2 0.654054 0.324082 0.368316 21.00000 -1.20000 AFIX 0 PART 2 C17A 1 0.713125 0.267866 0.263127 -21.00000 0.11159 0.10033 = 0.08971 -0.00906 0.01866 0.04504 AFIX 43 H17A 2 0.727784 0.242999 0.236051 -21.00000 -1.20000 AFIX 0 C18A 1 0.650313 0.216297 0.294167 -21.00000 0.11427 0.11807 = 0.11220 -0.00684 0.01325 0.04820 AFIX 43 H18A 2 0.621938 0.158809 0.289706 -21.00000 -1.20000 AFIX 0 C19A 1 0.631658 0.254603 0.332373 -21.00000 0.11931 0.16039 = 0.08809 0.02181 0.02295 0.05438 AFIX 43 H19A 2 0.588121 0.221317 0.355495 -21.00000 -1.20000 AFIX 0 C20A 1 0.670463 0.337415 0.340372 -21.00000 0.15039 0.14463 = 0.12193 -0.01228 0.01733 0.08492 AFIX 43 H20A 2 0.655830 0.362313 0.367442 -21.00000 -1.20000 AFIX 0 PART 0 C21 1 0.732143 0.380182 0.305453 11.00000 0.13986 0.10291 = 0.07712 0.00069 0.00959 0.06432 AFIX 43 H21 2 0.755103 0.436520 0.313169 11.00000 -1.20000 AFIX 0 C22 1 0.820321 0.644146 0.031767 11.00000 0.20079 0.22011 = 0.14786 0.10302 0.02147 0.13281 C23 1 0.887141 0.723688 0.055104 11.00000 0.39812 0.15874 = 0.22487 0.04666 0.03664 0.15749 AFIX 33 H23A 2 0.870295 0.731895 0.089994 11.00000 -1.50000 H23B 2 0.896702 0.769089 0.032018 11.00000 -1.50000 H23C 2 0.937450 0.721292 0.058326 11.00000 -1.50000 AFIX 0 C24 1 0.774442 0.659355 -0.012536 11.00000 0.27652 0.54138 = 0.16303 0.16317 0.07547 0.31045 AFIX 33 H24A 2 0.736179 0.607431 -0.029262 11.00000 -1.50000 H24B 2 0.813521 0.695959 -0.038804 11.00000 -1.50000 H24C 2 0.744323 0.684391 0.002159 11.00000 -1.50000 AFIX 0 C25 1 0.853583 0.592608 0.008961 11.00000 0.17733 0.26405 = 0.09815 0.07683 0.04377 0.16163 AFIX 33 H25A 2 0.890956 0.622144 -0.020039 11.00000 -1.50000 H25B 2 0.808410 0.541166 -0.004234 11.00000 -1.50000 H25C 2 0.882874 0.581218 0.036424 11.00000 -1.50000 AFIX 0 C26 1 0.537604 0.498968 0.108065 11.00000 0.15170 0.24111 = 0.09238 0.02641 0.01333 0.14243 PART 3 C27 1 0.501252 0.489078 0.053044 31.00000 0.17716 0.29268 = 0.06676 0.00032 -0.00943 0.13576 AFIX 33 H27A 2 0.460006 0.505866 0.053495 31.00000 -1.50000 H27B 2 0.475924 0.431863 0.042232 31.00000 -1.50000 H27C 2 0.544497 0.523157 0.028094 31.00000 -1.50000 AFIX 0 C28 1 0.485321 0.417422 0.135228 31.00000 0.17002 0.19805 = 0.10793 -0.04066 -0.07586 0.12134 AFIX 33 H28A 2 0.458425 0.374603 0.108630 31.00000 -1.50000 H28B 2 0.444006 0.420158 0.156962 31.00000 -1.50000 H28C 2 0.519844 0.404962 0.157595 31.00000 -1.50000 AFIX 0 C29 1 0.527879 0.560653 0.141067 31.00000 0.15711 0.24098 = 0.12276 0.03709 0.02498 0.11080 AFIX 33 H29A 2 0.539452 0.555579 0.178056 31.00000 -1.50000 H29B 2 0.471925 0.550250 0.137824 31.00000 -1.50000 H29C 2 0.565999 0.615843 0.128567 31.00000 -1.50000 AFIX 0 PART 4 C27A 1 0.493797 0.430711 0.066772 -31.00000 0.13820 0.24695 = 0.15200 0.03861 0.02023 0.11771 AFIX 33 H27D 2 0.530297 0.440615 0.036860 -31.00000 -1.50000 H27E 2 0.444532 0.430277 0.054512 -31.00000 -1.50000 H27F 2 0.478776 0.377945 0.082750 -31.00000 -1.50000 AFIX 0 C28A 1 0.496686 0.471401 0.160095 -31.00000 0.10142 0.35356 = 0.10539 -0.00235 0.01346 0.12215 AFIX 33 H28D 2 0.444632 0.470728 0.159421 -31.00000 -1.50000 H28E 2 0.531666 0.508888 0.187594 -31.00000 -1.50000 H28F 2 0.486810 0.416431 0.167537 -31.00000 -1.50000 AFIX 0 C29A 1 0.536066 0.574203 0.090477 -31.00000 0.13271 0.25735 = 0.16165 -0.05374 -0.05005 0.15184 AFIX 33 H29D 2 0.570985 0.619882 0.113656 -31.00000 -1.50000 H29E 2 0.480082 0.564108 0.092139 -31.00000 -1.50000 H29F 2 0.556130 0.587519 0.054205 -31.00000 -1.50000 AFIX 0 PART 0 C30 1 0.742708 0.120009 0.079592 11.00000 0.10541 0.12216 = 0.20312 -0.05794 0.01653 0.02547 PART 5 C31 1 0.751119 0.097047 0.136609 41.00000 0.17999 0.05384 = 0.23672 -0.03656 -0.06753 0.02434 AFIX 33 H31A 2 0.738795 0.040289 0.137655 41.00000 -1.50000 H31B 2 0.712939 0.103408 0.159422 41.00000 -1.50000 H31C 2 0.806967 0.132857 0.148970 41.00000 -1.50000 AFIX 0 C32 1 0.655348 0.084306 0.063887 41.00000 0.12322 0.08137 = 0.24887 -0.04270 0.08716 0.00307 AFIX 33 H32A 2 0.630271 0.109635 0.084595 41.00000 -1.50000 H32B 2 0.626359 0.025439 0.070423 41.00000 -1.50000 H32C 2 0.652163 0.094444 0.026351 41.00000 -1.50000 AFIX 0 C33 1 0.783148 0.083026 0.049077 41.00000 0.15046 0.21280 = 0.29433 -0.15515 0.05468 0.03677 AFIX 33 H33A 2 0.769670 0.081310 0.011662 41.00000 -1.50000 H33B 2 0.764074 0.027522 0.061783 41.00000 -1.50000 H33C 2 0.842330 0.115895 0.053692 41.00000 -1.50000 AFIX 0 PART 6 C31A 1 0.683850 0.067617 0.120257 -41.00000 0.19980 0.19122 = 0.19225 -0.08331 0.00693 -0.07349 AFIX 33 H31D 2 0.708853 0.043617 0.142324 -41.00000 -1.50000 H31E 2 0.635069 0.024059 0.103180 -41.00000 -1.50000 H31F 2 0.668632 0.100463 0.142209 -41.00000 -1.50000 AFIX 0 C32A 1 0.702439 0.100622 0.024269 -41.00000 0.13423 0.12118 = 0.22811 -0.04128 0.02046 0.02144 AFIX 33 H32D 2 0.733313 0.147368 0.000902 -41.00000 -1.50000 H32E 2 0.646247 0.089603 0.027258 -41.00000 -1.50000 H32F 2 0.702336 0.052657 0.009721 -41.00000 -1.50000 AFIX 0 C33A 1 0.806296 0.092185 0.074774 -41.00000 0.15194 0.05544 = 0.12742 -0.03425 -0.00928 0.06099 AFIX 33 H33D 2 0.844404 0.113873 0.104431 -41.00000 -1.50000 H33E 2 0.836338 0.112499 0.041648 -41.00000 -1.50000 H33F 2 0.778547 0.032506 0.075183 -41.00000 -1.50000 AFIX 0 PART 0 C34 1 0.933758 0.393484 -0.002035 11.00000 0.08761 0.12706 = 0.08164 -0.00673 0.00714 0.01573 C35 1 0.896631 0.436517 -0.032052 11.00000 0.11480 0.15088 = 0.08162 0.00896 0.02378 0.02092 AFIX 137 H35A 2 0.918774 0.448705 -0.067890 11.00000 -1.50000 H35B 2 0.909889 0.487408 -0.014006 11.00000 -1.50000 H35C 2 0.837311 0.401163 -0.033598 11.00000 -1.50000 AFIX 0 C36 1 1.015614 0.455154 0.022941 11.00000 0.08326 0.12221 = 0.08287 0.00491 0.03016 0.02878 AFIX 137 H36A 2 1.041934 0.426213 0.037559 11.00000 -1.50000 H36B 2 1.006173 0.484785 0.051148 11.00000 -1.50000 H36C 2 1.050952 0.493805 -0.003952 11.00000 -1.50000 AFIX 0 C37 1 0.945106 0.339651 -0.039136 11.00000 0.10370 0.14229 = 0.07442 -0.02221 0.00921 0.03942 AFIX 137 H37A 2 0.891757 0.294397 -0.049584 11.00000 -1.50000 H37B 2 0.976695 0.318069 -0.021952 11.00000 -1.50000 H37C 2 0.974376 0.370863 -0.070427 11.00000 -1.50000 AFIX 0 PART -1 O3 6 0.926085 0.750637 0.195006 10.50000 0.28935 0.15269 = 0.13952 0.02184 0.03377 0.15017 C38 1 0.839030 0.709845 0.209672 10.25000 0.26182 0.14139 = 0.10099 0.06172 0.06580 0.12282 AFIX 23 H38A 2 0.830810 0.694327 0.247350 10.25000 -1.20000 H38B 2 0.805908 0.660892 0.187806 10.25000 -1.20000 AFIX 0 C39 1 0.819775 0.775181 0.198326 10.25000 0.22000 0.15563 = 0.12998 0.07233 0.07832 0.12469 AFIX 23 H39A 2 0.776299 0.769913 0.222411 10.25000 -1.20000 H39B 2 0.799541 0.769519 0.161742 10.25000 -1.20000 AFIX 0 C40 1 0.893989 0.857086 0.205258 10.50000 0.25544 0.16615 = 0.16777 0.06547 0.03644 0.13222 AFIX 23 H40A 2 0.906249 0.872220 0.242841 10.50000 -1.20000 H40B 2 0.889672 0.900296 0.186112 10.50000 -1.20000 AFIX 0 C41 1 0.955787 0.838285 0.179980 10.50000 0.28800 0.17116 = 0.16245 0.07725 0.02556 0.10070 AFIX 23 H41A 2 0.956583 0.844554 0.141239 10.50000 -1.20000 H41B 2 1.011228 0.874693 0.193940 10.50000 -1.20000 AFIX 0 PART 7 C38A 1 0.881660 0.743291 0.244300 10.25000 0.19669 0.15506 = 0.16760 0.05607 0.08598 0.11830 C39A 1 0.900788 0.827764 0.258377 10.25000 0.18978 0.17232 = 0.13463 0.07852 0.11470 0.08954 PART 0 PART 8 LI1 7 0.943370 0.658177 0.164116 10.25000 0.09274 0.08648 = 0.08623 0.00335 -0.00875 0.04547 PART 9 LI1A 7 0.941289 0.699692 0.160003 10.25000 0.07131 0.08201 = 0.08182 -0.00304 0.01105 0.04564 PART 0 HKLF 4 REM _HC013 REM R1 = 0.1211 for 6060 Fo > 4sig(Fo) and 0.1351 for all 7780 data REM 561 parameters refined using 280 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.090, deepest hole -0.340, 1-sigma level 0.091 Q1 1 0.8805 0.7918 0.2550 11.00000 0.05 0.42 Q2 1 0.6923 0.2837 0.2585 11.00000 0.05 0.35 Q3 1 0.9920 0.8592 0.2295 11.00000 0.05 0.30 Q4 1 0.7459 0.1149 -0.0162 11.00000 0.05 0.30 Q5 1 0.7110 0.3769 0.3478 11.00000 0.05 0.30 Q6 1 0.6924 0.0957 0.0008 11.00000 0.05 0.28 Q7 1 0.7235 0.6155 -0.0026 11.00000 0.05 0.27 Q8 1 0.7392 0.5752 0.0536 11.00000 0.05 0.27 Q9 1 0.7809 0.4222 0.3162 11.00000 0.05 0.23 Q10 1 0.7315 0.5996 0.0875 11.00000 0.05 0.23 Q11 1 0.6418 0.4587 0.1594 11.00000 0.05 0.23 Q12 1 0.4987 0.4718 0.0731 11.00000 0.05 0.22 Q13 1 0.9095 0.4235 0.1098 11.00000 0.05 0.22 Q14 1 0.6790 0.0816 0.0999 11.00000 0.05 0.21 Q15 1 0.7983 0.6807 0.0069 11.00000 0.05 0.21 Q16 1 0.4586 0.3646 0.1588 11.00000 0.05 0.21 Q17 1 0.5036 0.5182 0.1516 11.00000 0.05 0.21 Q18 1 0.6296 0.0933 0.0108 11.00000 0.05 0.21 Q19 1 0.9278 0.4535 -0.0011 11.00000 0.05 0.20 Q20 1 0.5175 0.5909 0.0965 11.00000 0.05 0.19 Q21 1 0.8767 0.6986 0.0709 11.00000 0.05 0.19 Q22 1 0.7197 0.8877 0.1594 11.00000 0.05 0.19 Q23 1 0.9494 0.8885 0.2479 11.00000 0.05 0.18 Q24 1 0.6317 0.5413 0.0334 11.00000 0.05 0.18 Q25 1 0.7138 0.7396 0.1617 11.00000 0.05 0.18 ; _database_code_depnum_ccdc_archive 'CCDC 974612'