# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Francisco M. Romero' _publ_contact_author_address ; Instituto de Ciencia Molecular Universitat de Valencia Valencia 46035 SPAIN ; _publ_contact_author_email FMRM@UV.ES _publ_section_title ; Layered ferromagnets hosting tetraalkylammonium-substituted nitronyl nitroxide free radicals ; loop_ _publ_author_name 'Francisco M. Romero' 'Eugenio Coronado' 'Carlos Gimenez-Saiz' 'Carlos Gomez-Garcia' 'Ana Tarazon' data_RadMnCr _database_code_depnum_ccdc_archive 'CCDC 655470' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C6 O12 Cr Mn 1-), (C20 H41 N3 O2 1+)' _chemical_formula_sum 'C26 H41 Cr Mn N3 O14' _chemical_formula_weight 726.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 63' _symmetry_space_group_name_Hall 'P 6c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x-y, z' '-x+y, -x, z' 'x-y, x, z+1/2' 'y, -x+y, z+1/2' _cell_length_a 9.410(2) _cell_length_b 9.410(2) _cell_length_c 17.809(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1365.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8053 _exptl_absorpt_correction_T_max 0.9034 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'horizonally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11318 _diffrn_reflns_av_R_equivalents 0.1060 _diffrn_reflns_av_sigmaI/netI 0.0997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 30.51 _reflns_number_total 2660 _reflns_number_gt 1231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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. The atomic positions of the anionic 2D [CrMn(C2O4)]3- network were easily located and refined anisotropically. However, the ammonium cation (n-Bu3NC8H14N2O2)+ was severely disordered due to the numerous energetically similar conformations that the n-butyl chains can adopt and also to the site symmetry on which the cation lies (a three-fold axis). This kind of disorder has also been found in most of the previously reported crystal structures containing a 2D, hexagonal, bimetallic oxalate network and (nBu4N)+ cations (see text of the manuscript). In spite of this, the quaternary nitrogen and the carbon atoms of the butyl chains could be located and refined isotropically using distance restraints. The nitrogen atom was located on the three-fold axis and one of the butyl chains (the axial one) inserts into the hexagonal void of the anionic network. For the equatorial butyl chain, two different conformations could be assigned. However, the atomic positions of the nitronyl nitroxide radical fragment could not be found due to the severe disorder and the fact that it is present in less proportion than the butyl chains, although its presence in the crystal has been unambiguously demonstrated by means of its physical properties (see text). Therefore, the atoms of the nitronyl nitroxide radical were included in the formula of the compound for the calculations of F(000), absorption coefficient, molecular weight and density. The positions of the hydrogen atoms bonded to carbon atoms were included in calculated positions by using the PART instructions in SHELXL-97 and treated as riding atoms. #============================================================================== # PLATON/CHECK-(270606) versus check.def version of 270606 for entry: str530fc # Data From: str530fco7.cif - Data Type: CIF Bond Precision C-C = 0.0130 A # Refl Data: str530fco7.fcf - Data Type: SHELXL # # UCL 9.410(2) 9.410(2) 17.809(4) 90 90 120 # WaveLength 0.71073 Volume Reported 1365.7(5) Calculated 1365.7(5) # SpaceGroup from Symmetry P 63 Hall: P 6c # Reported P 63 P 6c # MoietyFormula C11.88 H26.73 N, C6 Cr Mn O12 # Reported (C6 O12 CR MN 1-), (C20 H41 N3 O2 1+) # SumFormula C17.88 H26.73 Cr Mn N O12 # Reported C26 H41 CR MN N3 O14 # Mr = 554.63[Calc], 726.56[Rep] # Dx,gcm-3 = 1.349[Calc], 1.767[Rep] # Z = 2[Calc], 2[Rep] # Mu (mm-1) = 0.913[Calc], 0.943[Rep] # F000 = 572.0[Calc], 758.0[Rep] or F000' = 573.64[Calc] # Reported T limits: Tmin=0.805 Tmax=0.903 'MULTI-SCAN' # Calculated T limits: Tmin=0.825 Tmin'=0.797 Tmax=0.901 # Reported Hmax= 13, Kmax= 13, Lmax= 25, Nref= 2660 , Th(max)= 30.510 # Obs in FCF Hmax= 11, Kmax= 13, Lmax= 25, Nref= 2660 , Th(max)= 30.506 # Calculated Hmax= 13, Kmax= 13, Lmax= 25, Nref= 1445( 2807), Ratio= 1.84(0.95) # rho(min) = -1.00, rho(max) = 0.59 e/Ang^3 # R= 0.0967( 1231), wR2= 0.2790( 2660), S = 1.051, Npar= 79, Flack= 0.42(10) #============================================================================== >>> The Following ALERTS were generated <<< #------------------------------------------ Format: alert-number_ALERT_alert-type_alert-level text 043_ALERT_1_A Check Reported Molecular Weight ................ 726.56 Author response: The atomic positions of the nitronyl nitroxide radical fragment could not be located due to the severe disorder. The atoms of the nitronyl nitroxide radical were included in the formula of the compound for the calculations of F(000), absorption coefficient, molecular weight and density. 044_ALERT_1_A Calculated and Reported Dx Differ .............. ? Author response: The same as before. 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C1B 241_ALERT_2_A Check High Ueq as Compared to Neighbors for C1X 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for N1 Author response: The nitrogen N1 is placed on a special position and it is the surrounding carbon atoms which are severely disordered. The nitrogen Ueq will be smaller than those of the carbon atoms as a consequence of this. #============================================================================== 112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... 2 112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... 2 112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... 2 112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... 2 112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... 2 112_ALERT_2_B ADDSYM Detects Additional (Pseudo) Symm. Elem... 2 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 1 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C2A 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C2X 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C3X #============================================================================== 020_ALERT_3_C The value of Rint is greater than 0.10 ......... 0.11 026_ALERT_3_C Ratio Observed / Unique Reflections too Low .... 46 Perc. 033_ALERT_2_C Flack Parameter Value Deviates from Zero ....... 0.42 041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? 051_ALERT_1_C Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 3.22 Perc. 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? 084_ALERT_2_C High R2 Value .................................. 0.28 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C1A 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C4B 241_ALERT_2_C Check High Ueq as Compared to Neighbors for O3 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C4A 301_ALERT_3_C Main Residue Disorder ......................... 16.00 Perc. 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 13 369_ALERT_2_C Long C(sp2)-C(sp2) Bond C1 - C2 ... 1.55 Ang. 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 27 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 4 915_ALERT_3_C Low Friedel Pair Coverage ...................... 89.50 Perc #============================================================================== 199_ALERT_1_G Check the Reported _cell_measurement_temperature 293 K 200_ALERT_1_G Check the Reported _diffrn_ambient_temperature . 293 K #============================================================================== ALERT_Level and ALERT_Type Summary #================================= 5 ALERT_Level_A = In General: Serious Problem. 10 ALERT_Level_B = Potentially Serious Problem. 18 ALERT_Level_C = Check & Explain. 2 ALERT_Level_G = Issues to Check, Not Necessarily Errors. 8 ALERT_Type_1 CIF Construction/Syntax Error, Inconsistent or Missing Data. 20 ALERT_Type_2 Indicator that the Structure Model may be Wrong or Deficient. 6 ALERT_Type_3 Indicator that the Structure Quality may be Low. 1 ALERT_Type_4 Improvement, Methodology, Query or Suggestion. #============================================================================== ; _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^)+(0.1447P)^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 noref _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 0.42(10) _refine_ls_number_reflns 2660 _refine_ls_number_parameters 79 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.2000 _refine_ls_R_factor_gt 0.0967 _refine_ls_wR_factor_ref 0.2790 _refine_ls_wR_factor_gt 0.2294 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.083 _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 Mn1 Mn 0.3333 0.6667 0.9106(2) 0.0559(5) Uani 1 3 d S . . Cr1 Cr 0.0000 0.0000 0.91178(16) 0.0501(5) Uani 1 3 d S . . O1 O 0.3124(7) 0.4639(7) 0.9753(3) 0.0600(15) Uani 1 1 d . . . O2 O 0.0177(6) 0.1889(7) 0.8504(3) 0.0603(16) Uani 1 1 d . . . O3 O 0.1605(7) 0.4658(7) 0.8481(4) 0.0666(17) Uani 1 1 d . . . O4 O 0.1780(6) 0.1931(7) 0.9743(3) 0.0606(16) Uani 1 1 d . . . C1 C 0.2120(9) 0.3264(10) 0.9488(5) 0.050(2) Uani 1 1 d . . . C2 C 0.1251(9) 0.3299(8) 0.8754(5) 0.045(2) Uani 1 1 d . . . N1 N 0.6667 0.3333 0.7184(13) 0.179(11) Uiso 1 3 d SD . . C1X C 0.678(2) 0.3373(14) 0.8033(13) 0.27(3) Uiso 0.33 1 d PDU A -1 H1X1 H 0.6772 0.2357 0.8140 0.329 Uiso 0.33 1 calc PR A -1 H1X2 H 0.7911 0.4227 0.8115 0.329 Uiso 0.33 1 calc PR A -1 C2X C 0.600(2) 0.3540(14) 0.8668(13) 0.155(16) Uiso 0.33 1 d PRDU A -1 H2X1 H 0.5012 0.2495 0.8752 0.186 Uiso 0.33 1 calc PR A -1 H2X2 H 0.5659 0.4330 0.8548 0.186 Uiso 0.33 1 calc PR A -1 C3X C 0.695(2) 0.4069(14) 0.9411(13) 0.125(15) Uiso 0.33 1 d PRDU A -1 H3X1 H 0.7913 0.5094 0.9271 0.150 Uiso 0.33 1 calc PR A -1 H3X2 H 0.6286 0.4393 0.9703 0.150 Uiso 0.33 1 calc PR A -1 C4X C 0.762(2) 0.3437(14) 1.0013(13) 0.19(2) Uiso 0.33 1 d PRDU A -1 H4X1 H 0.8153 0.4263 1.0392 0.290 Uiso 0.33 1 calc PR A -1 H4X2 H 0.8399 0.3182 0.9794 0.290 Uiso 0.33 1 calc PR A -1 H4X3 H 0.6738 0.2467 1.0235 0.290 Uiso 0.33 1 calc PR A -1 C1A C 0.617(2) 0.1633(14) 0.6892(13) 0.28(2) Uiso 0.33 1 d PRDU A -2 H1A1 H 0.6503 0.1751 0.6369 0.341 Uiso 0.33 1 calc PR A -2 H1A2 H 0.4984 0.0994 0.6901 0.341 Uiso 0.33 1 calc PR A -2 C2A C 0.681(2) 0.0612(14) 0.7273(13) 0.25(2) Uiso 0.33 1 d PRDU A -2 H2A1 H 0.7991 0.1117 0.7233 0.305 Uiso 0.33 1 calc PR A -2 H2A2 H 0.6486 0.0405 0.7797 0.305 Uiso 0.33 1 calc PR A -2 C3A C 0.593(2) -0.0921(14) 0.6805(13) 0.27(3) Uiso 0.33 1 d PRDU A -2 H3A1 H 0.5045 -0.1778 0.7095 0.320 Uiso 0.33 1 calc PR A -2 H3A2 H 0.5457 -0.0703 0.6367 0.320 Uiso 0.33 1 calc PR A -2 C4A C 0.708(2) -0.1492(14) 0.6560(13) 0.26(3) Uiso 0.33 1 d PRDU A -2 H4A1 H 0.6500 -0.2469 0.6263 0.384 Uiso 0.33 1 calc PR A -2 H4A2 H 0.7540 -0.1724 0.6994 0.384 Uiso 0.33 1 calc PR A -2 H4A3 H 0.7953 -0.0650 0.6266 0.384 Uiso 0.33 1 calc PR A -2 C1B C 0.703(2) 0.2077(14) 0.6862(13) 0.31(2) Uiso 0.33 1 d PRDU A -3 H1B1 H 0.8216 0.2557 0.6859 0.367 Uiso 0.33 1 calc PR A -3 H1B2 H 0.6680 0.1911 0.6342 0.367 Uiso 0.33 1 calc PR A -3 C2B C 0.628(2) 0.0326(14) 0.7238(13) 0.28(2) Uiso 0.33 1 d PRDU A -3 H2B1 H 0.6616 0.0389 0.7758 0.333 Uiso 0.33 1 calc PR A -3 H2B2 H 0.5095 -0.0293 0.7202 0.333 Uiso 0.33 1 calc PR A -3 C3B C 0.709(2) -0.0363(14) 0.6730(13) 0.28(2) Uiso 0.33 1 d PRDU A -3 H3B1 H 0.7878 0.0503 0.6405 0.334 Uiso 0.33 1 calc PR A -3 H3B2 H 0.7692 -0.0742 0.7036 0.334 Uiso 0.33 1 calc PR A -3 C4B C 0.587(2) -0.1747(14) 0.6260(13) 0.29(3) Uiso 0.33 1 d PRDU A -3 H4B1 H 0.6431 -0.2146 0.5949 0.431 Uiso 0.33 1 calc PR A -3 H4B2 H 0.5295 -0.1371 0.5949 0.431 Uiso 0.33 1 calc PR A -3 H4B3 H 0.5109 -0.2615 0.6580 0.431 Uiso 0.33 1 calc PR A -3 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 Mn1 0.0418(6) 0.0418(6) 0.0840(12) 0.000 0.000 0.0209(3) Cr1 0.0361(6) 0.0361(6) 0.0781(12) 0.000 0.000 0.0180(3) O1 0.051(3) 0.053(3) 0.074(4) -0.001(3) -0.015(3) 0.024(3) O2 0.059(3) 0.056(3) 0.076(4) -0.009(3) -0.020(3) 0.037(3) O3 0.051(3) 0.060(4) 0.090(5) 0.003(3) -0.015(3) 0.028(3) O4 0.058(3) 0.062(4) 0.069(4) 0.010(3) -0.012(3) 0.035(3) C1 0.033(3) 0.051(5) 0.072(7) -0.002(4) -0.006(4) 0.026(3) C2 0.043(4) 0.041(4) 0.057(6) 0.000(3) -0.004(3) 0.026(3) _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 Mn1 O3 2.094(6) 4_565 ? Mn1 O3 2.094(6) . ? Mn1 O3 2.094(6) 3_665 ? Mn1 O1 2.152(6) 4_565 ? Mn1 O1 2.152(6) 3_665 ? Mn1 O1 2.152(6) . ? Cr1 O2 2.022(6) 3 ? Cr1 O2 2.022(6) 4 ? Cr1 O2 2.022(6) . ? Cr1 O4 2.075(6) . ? Cr1 O4 2.075(6) 4 ? Cr1 O4 2.075(6) 3 ? O1 C1 1.252(9) . ? O2 C2 1.280(9) . ? O3 C2 1.248(8) . ? O4 C1 1.217(9) . ? C1 C2 1.551(9) . ? N1 C1B 1.501(8) . ? N1 C1B 1.501(8) 3_655 ? N1 C1B 1.501(8) 4_665 ? N1 C1X 1.515(10) . ? N1 C1X 1.515(10) 4_665 ? N1 C1X 1.515(10) 3_655 ? N1 C1A 1.518(8) . ? N1 C1A 1.518(8) 3_655 ? N1 C1A 1.518(8) 4_665 ? C1X C2X 1.3995 . ? C1X H1X1 0.9700 . ? C1X H1X2 0.9700 . ? C2X C3X 1.5324 . ? C2X H2X1 0.9700 . ? C2X H2X2 0.9700 . ? C3X C4X 1.5096 . ? C3X H3X1 0.9700 . ? C3X H3X2 0.9700 . ? C4X H4X1 0.9600 . ? C4X H4X2 0.9600 . ? C4X H4X3 0.9600 . ? C1A C2A 1.5216 . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A C3A 1.5052 . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C4A 1.4974 . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C4A H4A3 0.9600 . ? C1B C2B 1.5812 . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B C3B 1.5224 . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B C4B 1.4899 . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C4B H4B3 0.9600 . ? 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 O3 Mn1 O3 94.3(3) 4_565 . ? O3 Mn1 O3 94.3(3) 4_565 3_665 ? O3 Mn1 O3 94.3(3) . 3_665 ? O3 Mn1 O1 78.4(2) 4_565 4_565 ? O3 Mn1 O1 94.20(19) . 4_565 ? O3 Mn1 O1 169.18(19) 3_665 4_565 ? O3 Mn1 O1 94.20(19) 4_565 3_665 ? O3 Mn1 O1 169.18(19) . 3_665 ? O3 Mn1 O1 78.4(2) 3_665 3_665 ? O1 Mn1 O1 94.0(2) 4_565 3_665 ? O3 Mn1 O1 169.18(19) 4_565 . ? O3 Mn1 O1 78.4(2) . . ? O3 Mn1 O1 94.20(19) 3_665 . ? O1 Mn1 O1 94.0(2) 4_565 . ? O1 Mn1 O1 94.0(2) 3_665 . ? O2 Cr1 O2 93.5(3) 3 4 ? O2 Cr1 O2 93.5(3) 3 . ? O2 Cr1 O2 93.5(3) 4 . ? O2 Cr1 O4 172.5(2) 3 . ? O2 Cr1 O4 92.0(2) 4 . ? O2 Cr1 O4 81.1(2) . . ? O2 Cr1 O4 92.0(2) 3 4 ? O2 Cr1 O4 81.1(2) 4 4 ? O2 Cr1 O4 172.5(2) . 4 ? O4 Cr1 O4 93.9(2) . 4 ? O2 Cr1 O4 81.1(2) 3 3 ? O2 Cr1 O4 172.5(2) 4 3 ? O2 Cr1 O4 92.0(2) . 3 ? O4 Cr1 O4 93.9(2) . 3 ? O4 Cr1 O4 93.9(2) 4 3 ? C1 O1 Mn1 113.7(5) . . ? C2 O2 Cr1 113.5(5) . . ? C2 O3 Mn1 114.0(5) . . ? C1 O4 Cr1 112.5(5) . . ? O4 C1 O1 126.7(8) . . ? O4 C1 C2 117.8(6) . . ? O1 C1 C2 115.4(7) . . ? O3 C2 O2 126.5(8) . . ? O3 C2 C1 118.5(6) . . ? O2 C2 C1 115.0(6) . . ? C1B N1 C1B 106.3(5) . 3_655 ? C1B N1 C1B 106.3(5) . 4_665 ? C1B N1 C1B 106.3(5) 3_655 4_665 ? C1B N1 C1X 111.1(7) . . ? C1B N1 C1X 110.3(6) 3_655 . ? C1B N1 C1X 116.1(8) 4_665 . ? C1B N1 C1X 110.3(6) . 4_665 ? C1B N1 C1X 116.1(8) 3_655 4_665 ? C1B N1 C1X 111.1(7) 4_665 4_665 ? C1B N1 C1X 116.1(8) . 3_655 ? C1B N1 C1X 111.1(7) 3_655 3_655 ? C1B N1 C1X 110.3(6) 4_665 3_655 ? C1X N1 C1A 110.4(7) . . ? C1X N1 C1A 106.7(7) 4_665 . ? C1X N1 C1A 113.0(7) 3_655 . ? C1X N1 C1A 106.7(7) . 3_655 ? C1X N1 C1A 113.0(7) 4_665 3_655 ? C1X N1 C1A 110.4(7) 3_655 3_655 ? C1A N1 C1A 108.9(4) . 3_655 ? C1X N1 C1A 113.0(7) . 4_665 ? C1X N1 C1A 110.4(7) 4_665 4_665 ? C1X N1 C1A 106.7(7) 3_655 4_665 ? C1A N1 C1A 108.9(4) . 4_665 ? C1A N1 C1A 108.9(4) 3_655 4_665 ? C2X C1X N1 140.7(6) . . ? C2X C1X H1X1 101.9 . . ? N1 C1X H1X1 101.9 . . ? C2X C1X H1X2 101.9 . . ? N1 C1X H1X2 101.9 . . ? H1X1 C1X H1X2 104.7 . . ? C1X C2X C3X 118.7 . . ? C1X C2X H2X1 107.6 . . ? C3X C2X H2X1 107.6 . . ? C1X C2X H2X2 107.6 . . ? C3X C2X H2X2 107.6 . . ? H2X1 C2X H2X2 107.1 . . ? C4X C3X C2X 140.8 . . ? C4X C3X H3X1 101.8 . . ? C2X C3X H3X1 101.8 . . ? C4X C3X H3X2 101.8 . . ? C2X C3X H3X2 101.8 . . ? H3X1 C3X H3X2 104.7 . . ? C3X C4X H4X1 109.5 . . ? C3X C4X H4X2 109.5 . . ? H4X1 C4X H4X2 109.5 . . ? C3X C4X H4X3 109.5 . . ? H4X1 C4X H4X3 109.5 . . ? H4X2 C4X H4X3 109.5 . . ? N1 C1A C2A 120.2(5) . . ? N1 C1A H1A1 107.3 . . ? C2A C1A H1A1 107.3 . . ? N1 C1A H1A2 107.3 . . ? C2A C1A H1A2 107.3 . . ? H1A1 C1A H1A2 106.9 . . ? C3A C2A C1A 99.0 . . ? C3A C2A H2A1 112.0 . . ? C1A C2A H2A1 112.0 . . ? C3A C2A H2A2 112.0 . . ? C1A C2A H2A2 112.0 . . ? H2A1 C2A H2A2 109.6 . . ? C4A C3A C2A 110.9 . . ? C4A C3A H3A1 109.5 . . ? C2A C3A H3A1 109.5 . . ? C4A C3A H3A2 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 108.0 . . ? C3A C4A H4A1 109.5 . . ? C3A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C3A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? N1 C1B C2B 120.0(5) . . ? N1 C1B H1B1 107.3 . . ? C2B C1B H1B1 107.3 . . ? N1 C1B H1B2 107.3 . . ? C2B C1B H1B2 107.3 . . ? H1B1 C1B H1B2 106.9 . . ? C3B C2B C1B 97.7 . . ? C3B C2B H2B1 112.2 . . ? C1B C2B H2B1 112.2 . . ? C3B C2B H2B2 112.2 . . ? C1B C2B H2B2 112.2 . . ? H2B1 C2B H2B2 109.8 . . ? C4B C3B C2B 112.0 . . ? C4B C3B H3B1 109.2 . . ? C2B C3B H3B1 109.2 . . ? C4B C3B H3B2 109.2 . . ? C2B C3B H3B2 109.2 . . ? H3B1 C3B H3B2 107.9 . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.591 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.121