data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H36 Cl6 Cr Mn N O12' _chemical_formula_weight 970.28 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' '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' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.776(5) _cell_length_b 23.339(5) _cell_length_c 16.833(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 101.476(5) _cell_angle_gamma 90.000(5) _cell_volume 5304(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1580 _cell_measurement_theta_min 3.0058 _cell_measurement_theta_max 32.4535 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.791 loop_ _cell_oxdiff_twin_id _cell_oxdiff_twin_matrix_11 _cell_oxdiff_twin_matrix_12 _cell_oxdiff_twin_matrix_13 _cell_oxdiff_twin_matrix_21 _cell_oxdiff_twin_matrix_22 _cell_oxdiff_twin_matrix_23 _cell_oxdiff_twin_matrix_31 _cell_oxdiff_twin_matrix_32 _cell_oxdiff_twin_matrix_33 1 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.5014 0.5127 -0.0029 1.4597 -0.5013 0.0001 -0.3636 -0.1256 -0.9988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9322 _exptl_absorpt_correction_T_max 0.9767 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0267 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11965 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1985 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.13 _reflns_number_total 11965 _reflns_number_gt 4553 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _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 . _refine_ls_hydrogen_treatment . _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11965 _refine_ls_number_parameters 164 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.2755 _refine_ls_R_factor_gt 0.1584 _refine_ls_wR_factor_ref 0.4721 _refine_ls_wR_factor_gt 0.4282 _refine_ls_goodness_of_fit_ref 1.302 _refine_ls_restrained_S_all 1.309 _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 1.5000 0.43425(12) 0.7500 0.0526(8) Uani 0.50 2 d SP . 1 Cr1 Cr 1.5000 0.43425(12) 0.7500 0.0526(8) Uani 0.50 2 d SP . 1 Mn2 Mn 2.0000 0.27141(11) 0.7500 0.0439(7) Uani 0.50 2 d SP . 2 Cr2 Cr 2.0000 0.27141(11) 0.7500 0.0439(7) Uani 0.50 2 d SP . 2 Cl1 Cl 1.7344(3) 0.2874(2) 0.9135(3) 0.1012(18) Uani 1 1 d . . . C1 C 1.7489(9) 0.3230(5) 0.8243(7) 0.053(3) Uiso 1 1 d . . . C2 C 1.6759(10) 0.3620(6) 0.7921(7) 0.054(3) Uiso 1 1 d . . . O2 O 1.5970(7) 0.3717(4) 0.8166(5) 0.065(3) Uiso 1 1 d . . . O3 O 1.6132(6) 0.4260(4) 0.6822(5) 0.054(2) Uiso 1 1 d . . . C3 C 1.6837(9) 0.3931(6) 0.7117(7) 0.049(3) Uiso 1 1 d . . . Cl4 Cl 1.7814(3) 0.42135(14) 0.59447(17) 0.0567(10) Uani 1 1 d . . . C4 C 1.7666(8) 0.3822(4) 0.6783(6) 0.037(3) Uiso 1 1 d . . . O5 O 1.9131(5) 0.3312(3) 0.6854(4) 0.041(2) Uiso 1 1 d . . . C5 C 1.8384(8) 0.3441(5) 0.7135(6) 0.038(3) Uiso 1 1 d . . . O6 O 1.8961(6) 0.2773(3) 0.8159(5) 0.045(2) Uiso 1 1 d . . . C6 C 1.8247(8) 0.3129(5) 0.7870(6) 0.039(3) Uiso 1 1 d . . . Cl11 Cl 1.6809(2) 0.60443(16) 0.8999(2) 0.0697(11) Uani 1 1 d . . . C11 C 1.5841(9) 0.6049(6) 0.8180(7) 0.052(3) Uiso 1 1 d . . . O12 O 1.5707(7) 0.5061(4) 0.8131(5) 0.062(2) Uiso 1 1 d . . . C12 C 1.5438(8) 0.5533(5) 0.7866(7) 0.043(3) Uiso 1 1 d . . . O13 O 1.5727(6) 0.7048(3) 0.8136(4) 0.049(2) Uiso 1 1 d . . . C13 C 1.5419(8) 0.6548(5) 0.7883(7) 0.041(3) Uiso 1 1 d . . . N20 N 1.5764(11) 0.2328(6) 0.5564(8) 0.053(5) Uiso 0.50 1 d PD . . C21 C 1.5517(15) 0.2358(9) 0.6399(9) 0.045(6) Uiso 0.50 1 d PD . . C22 C 1.6067(16) 0.1941(10) 0.7042(10) 0.070 Uiso 0.50 1 d PD . . C23 C 1.5618(15) 0.1974(10) 0.7803(10) 0.070 Uiso 0.50 1 d PD . . C24 C 1.6269(18) 0.1641(11) 0.8494(10) 0.070 Uiso 0.50 1 d PD . . C31 C 1.5704(15) 0.1703(7) 0.5281(14) 0.053(7) Uiso 0.50 1 d PD . . C32A C 1.536(2) 0.1072(11) 0.5390(18) 0.070 Uiso 0.25 1 d PD A 1 C32B C 1.4629(16) 0.1496(9) 0.508(3) 0.070 Uiso 0.25 1 d PD A 2 C33 C 1.4611(15) 0.0907(8) 0.4640(12) 0.070 Uiso 0.50 1 d PD . . C34 C 1.3726(15) 0.0575(9) 0.4869(15) 0.070 Uiso 0.50 1 d PD A . C41 C 1.5077(16) 0.2761(8) 0.5033(14) 0.053(7) Uiso 0.50 1 d PD . . C42A C 1.445(4) 0.3191(11) 0.4414(14) 0.070 Uiso 0.25 1 d PD A 1 C42B C 1.524(2) 0.3407(9) 0.520(3) 0.070 Uiso 0.25 1 d PD A 2 C43 C 1.4299(17) 0.3737(7) 0.4834(14) 0.070 Uiso 0.50 1 d PD . . C44A C 1.397(4) 0.4245(11) 0.427(2) 0.070 Uiso 0.25 1 d PD A 1 C44B C 1.447(3) 0.4376(8) 0.483(3) 0.070 Uiso 0.25 1 d PD A 2 C51 C 1.6863(12) 0.2447(10) 0.5619(11) 0.053(7) Uiso 0.50 1 d PD . . C52 C 1.7216(13) 0.2473(14) 0.4804(11) 0.070 Uiso 0.50 1 d PD . . C53 C 1.8279(13) 0.2706(11) 0.4951(12) 0.070 Uiso 0.50 1 d PD . . C54 C 1.8705(17) 0.2611(12) 0.4179(15) 0.070 Uiso 0.50 1 d PD . . 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 0.0332(16) 0.0504(19) 0.070(2) 0.000 0.0003(15) 0.000 Cr1 0.0332(16) 0.0504(19) 0.070(2) 0.000 0.0003(15) 0.000 Mn2 0.0454(18) 0.0493(19) 0.0342(14) 0.000 0.0010(15) 0.000 Cr2 0.0454(18) 0.0493(19) 0.0342(14) 0.000 0.0010(15) 0.000 Cl1 0.081(3) 0.134(4) 0.103(3) 0.090(3) 0.052(3) 0.037(3) Cl4 0.085(3) 0.0507(19) 0.0354(17) 0.0120(14) 0.0134(17) -0.0038(17) Cl11 0.060(2) 0.072(2) 0.060(2) 0.004(2) -0.0302(16) -0.007(2) _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 2.115(8) . ? Mn1 O3 2.115(8) 2_856 ? Mn1 O12 2.116(9) . ? Mn1 O12 2.116(9) 2_856 ? Mn1 O2 2.140(9) 2_856 ? Mn1 O2 2.140(9) . ? Mn2 O6 1.982(8) 2_956 ? Mn2 O6 1.982(8) . ? Mn2 O5 2.011(7) 2_956 ? Mn2 O5 2.011(7) . ? Mn2 O13 2.034(8) 4_846 ? Mn2 O13 2.034(8) 3_545 ? Cl1 C1 1.761(13) . ? C1 C6 1.342(15) . ? C1 C2 1.384(17) . ? C2 O2 1.258(14) . ? C2 C3 1.558(16) . ? O3 C3 1.261(14) . ? C3 C4 1.392(15) . ? Cl4 C4 1.728(11) . ? C4 C5 1.374(14) . ? O5 C5 1.252(12) . ? C5 C6 1.481(14) . ? O6 C6 1.305(12) . ? Cl11 C11 1.716(12) . ? C11 C13 1.353(15) . ? C11 C12 1.387(16) . ? O12 C12 1.218(13) . ? C12 C12 1.54(2) 2_856 ? O13 C13 1.285(13) . ? O13 Cr2 2.034(8) 3_455 ? O13 Mn2 2.034(8) 3_455 ? C13 C13 1.55(2) 2_856 ? N20 C54 0.78(3) 7_856 ? N20 C21 1.512(9) . ? N20 C51 1.524(9) . ? N20 C31 1.532(9) . ? N20 C41 1.543(9) . ? N20 C53 1.72(3) 7_856 ? C21 C22 1.539(9) . ? C21 C54 1.59(2) 7_856 ? C22 C23 1.530(10) . ? C23 C24 1.532(9) . ? C23 C23 1.80(4) 2_856 ? C31 C32B 1.531(10) . ? C31 C32A 1.567(10) . ? C31 C54 1.94(3) 7_856 ? C31 C53 2.06(2) 7_856 ? C32A C33 1.515(10) . ? C32B C33 1.557(10) . ? C33 C34 1.555(10) . ? C41 C42B 1.541(10) . ? C41 C42A 1.577(10) . ? C42A C43 1.490(10) . ? C42B C43 1.526(10) . ? C43 C44B 1.513(10) . ? C43 C44A 1.527(10) . ? C51 C54 0.92(2) 7_856 ? C51 C53 1.01(3) 7_856 ? C51 C52 1.544(10) . ? C51 C52 1.58(2) 7_856 ? C52 C52 0.93(3) 7_856 ? C52 C53 0.96(3) 7_856 ? C52 C53 1.535(10) . ? C52 C51 1.58(2) 7_856 ? C53 C52 0.96(3) 7_856 ? C53 C51 1.01(3) 7_856 ? C53 C54 1.544(10) . ? C53 N20 1.72(3) 7_856 ? C53 C31 2.06(2) 7_856 ? C54 N20 0.78(3) 7_856 ? C54 C51 0.92(2) 7_856 ? C54 C21 1.59(2) 7_856 ? C54 C31 1.94(3) 7_856 ? 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 169.6(5) . 2_856 ? O3 Mn1 O12 91.6(3) . . ? O3 Mn1 O12 96.6(3) 2_856 . ? O3 Mn1 O12 96.6(3) . 2_856 ? O3 Mn1 O12 91.6(3) 2_856 2_856 ? O12 Mn1 O12 75.2(5) . 2_856 ? O3 Mn1 O2 96.1(3) . 2_856 ? O3 Mn1 O2 76.7(3) 2_856 2_856 ? O12 Mn1 O2 168.8(3) . 2_856 ? O12 Mn1 O2 95.8(3) 2_856 2_856 ? O3 Mn1 O2 76.7(3) . . ? O3 Mn1 O2 96.1(3) 2_856 . ? O12 Mn1 O2 95.8(3) . . ? O12 Mn1 O2 168.8(4) 2_856 . ? O2 Mn1 O2 93.9(5) 2_856 . ? O6 Mn2 O6 172.1(4) 2_956 . ? O6 Mn2 O5 80.6(3) 2_956 2_956 ? O6 Mn2 O5 93.9(3) . 2_956 ? O6 Mn2 O5 93.9(3) 2_956 . ? O6 Mn2 O5 80.6(3) . . ? O5 Mn2 O5 92.2(4) 2_956 . ? O6 Mn2 O13 95.4(3) 2_956 4_846 ? O6 Mn2 O13 90.7(3) . 4_846 ? O5 Mn2 O13 172.9(3) 2_956 4_846 ? O5 Mn2 O13 93.9(3) . 4_846 ? O6 Mn2 O13 90.7(3) 2_956 3_545 ? O6 Mn2 O13 95.4(3) . 3_545 ? O5 Mn2 O13 93.9(3) 2_956 3_545 ? O5 Mn2 O13 172.9(3) . 3_545 ? O13 Mn2 O13 80.3(5) 4_846 3_545 ? C6 C1 C2 120.3(11) . . ? C6 C1 Cl1 123.1(10) . . ? C2 C1 Cl1 116.6(10) . . ? O2 C2 C1 126.7(12) . . ? O2 C2 C3 114.5(11) . . ? C1 C2 C3 118.5(12) . . ? C2 O2 Mn1 116.2(8) . . ? C3 O3 Mn1 115.9(7) . . ? O3 C3 C4 125.6(11) . . ? O3 C3 C2 116.4(11) . . ? C4 C3 C2 118.0(11) . . ? C3 C4 C5 121.5(10) . . ? C3 C4 Cl4 118.3(8) . . ? C5 C4 Cl4 120.1(8) . . ? C5 O5 Mn2 114.1(7) . . ? O5 C5 C4 124.7(10) . . ? O5 C5 C6 116.7(10) . . ? C4 C5 C6 118.5(10) . . ? C6 O6 Mn2 114.2(7) . . ? O6 C6 C1 122.5(10) . . ? O6 C6 C5 114.4(10) . . ? C1 C6 C5 123.0(11) . . ? C13 C11 C12 119.8(11) . . ? C13 C11 Cl11 120.7(10) . . ? C12 C11 Cl11 119.3(9) . . ? C12 O12 Mn1 117.2(8) . . ? O12 C12 C11 125.2(11) . . ? O12 C12 C12 115.1(7) . 2_856 ? C11 C12 C12 119.6(7) . 2_856 ? C13 O13 Cr2 115.1(7) . 3_455 ? C13 O13 Mn2 115.1(7) . 3_455 ? Cr2 O13 Mn2 0.0 3_455 3_455 ? O13 C13 C11 124.8(11) . . ? O13 C13 C13 114.7(6) . 2_856 ? C11 C13 C13 120.1(7) . 2_856 ? C54 N20 C21 80.6(19) 7_856 . ? C54 N20 C51 29.3(19) 7_856 . ? C21 N20 C51 109.9(13) . . ? C54 N20 C31 109(3) 7_856 . ? C21 N20 C31 108.9(15) . . ? C51 N20 C31 100.5(14) . . ? C54 N20 C41 127(3) 7_856 . ? C21 N20 C41 106.4(14) . . ? C51 N20 C41 113.8(16) . . ? C31 N20 C41 117.1(15) . . ? C54 N20 C53 64.0(17) 7_856 7_856 ? C21 N20 C53 143.9(15) . 7_856 ? C51 N20 C53 35.5(11) . 7_856 ? C31 N20 C53 78.3(13) . 7_856 ? C41 N20 C53 100.5(15) . 7_856 ? N20 C21 C22 117.1(13) . . ? N20 C21 C54 29.2(11) . 7_856 ? C22 C21 C54 99.4(16) . 7_856 ? C23 C22 C21 109.4(9) . . ? C22 C23 C24 109.7(9) . . ? C22 C23 C23 91.2(14) . 2_856 ? C24 C23 C23 140.7(14) . 2_856 ? C32B C31 N20 111.1(14) . . ? C32B C31 C32A 55.3(18) . . ? N20 C31 C32A 149(2) . . ? C32B C31 C54 131.5(14) . 7_856 ? N20 C31 C54 22.5(10) . 7_856 ? C32A C31 C54 145.9(18) . 7_856 ? C32B C31 C53 147(2) . 7_856 ? N20 C31 C53 54.8(11) . 7_856 ? C32A C31 C53 152.0(19) . 7_856 ? C54 C31 C53 45.3(6) 7_856 7_856 ? C33 C32A C31 108.3(9) . . ? C31 C32B C33 107.9(9) . . ? C32A C33 C34 111.2(10) . . ? C32A C33 C32B 55.8(18) . . ? C34 C33 C32B 105.1(9) . . ? C42B C41 N20 119.0(17) . . ? C42B C41 C42A 62.6(16) . . ? N20 C41 C42A 173(2) . . ? C43 C42A C41 109.9(10) . . ? C43 C42B C41 109.9(10) . . ? C42A C43 C44B 143(3) . . ? C42A C43 C42B 65.0(17) . . ? C44B C43 C42B 112.2(10) . . ? C42A C43 C44A 115.0(10) . . ? C44B C43 C44A 42(2) . . ? C42B C43 C44A 140(3) . . ? C54 C51 C53 106(2) 7_856 7_856 ? C54 C51 N20 24.6(18) 7_856 . ? C53 C51 N20 82.8(17) 7_856 . ? C54 C51 C52 141(2) 7_856 . ? C53 C51 C52 37.2(15) 7_856 . ? N20 C51 C52 116.0(13) . . ? C54 C51 C52 175(3) 7_856 7_856 ? C53 C51 C52 68.6(15) 7_856 7_856 ? N20 C51 C52 150.3(18) . 7_856 ? C52 C51 C52 34.4(13) . 7_856 ? C52 C52 C53 109(3) 7_856 7_856 ? C52 C52 C53 36.3(18) 7_856 . ? C53 C52 C53 145(2) 7_856 . ? C52 C52 C51 75.1(19) 7_856 . ? C53 C52 C51 39.3(17) 7_856 . ? C53 C52 C51 109.3(9) . . ? C52 C52 C51 70.5(16) 7_856 7_856 ? C53 C52 C51 161(4) 7_856 7_856 ? C53 C52 C51 37.6(10) . 7_856 ? C51 C52 C51 145.6(13) . 7_856 ? C52 C53 C51 104(3) 7_856 7_856 ? C52 C53 C52 35(2) 7_856 . ? C51 C53 C52 73.9(15) 7_856 . ? C52 C53 C54 136(3) 7_856 . ? C51 C53 C54 35.0(13) 7_856 . ? C52 C53 C54 108.9(9) . . ? C52 C53 N20 151(3) 7_856 7_856 ? C51 C53 N20 61.7(13) 7_856 7_856 ? C52 C53 N20 134.9(13) . 7_856 ? C54 C53 N20 27.2(11) . 7_856 ? C52 C53 C31 160(3) 7_856 7_856 ? C51 C53 C31 93.9(18) 7_856 7_856 ? C52 C53 C31 150(2) . 7_856 ? C54 C53 C31 63.2(12) . 7_856 ? N20 C53 C31 46.8(6) 7_856 7_856 ? N20 C54 C51 126(3) 7_856 7_856 ? N20 C54 C53 89(2) 7_856 . ? C51 C54 C53 38.7(18) 7_856 . ? N20 C54 C21 70.2(16) 7_856 7_856 ? C51 C54 C21 163(3) 7_856 7_856 ? C53 C54 C21 157.8(19) . 7_856 ? N20 C54 C31 48(2) 7_856 7_856 ? C51 C54 C31 105(2) 7_856 7_856 ? C53 C54 C31 71.4(12) . 7_856 ? C21 C54 C31 88.7(14) 7_856 7_856 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.092 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.242