# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_962811 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H118 Mn6 N18 O16, 2(Cl O4), 2(C9 H13 N), 2(C2 H6 O), 4(H2 O)' _chemical_formula_sum 'C114 H140 Cl Mn6 N20 O20' _chemical_formula_weight 2475.55 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' 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 'P 2/n' _symmetry_space_group_name_Hall '- P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 20.8577(5) _cell_length_b 14.8207(3) _cell_length_c 22.7739(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.550(2) _cell_angle_gamma 90.00 _cell_volume 7007.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12058 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.30 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2582 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 1.038 _exptl_absorpt_correction_T_max 1.965 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60339 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_unetI/netI 0.0718 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12824 _reflns_number_gt 8964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2013)' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2d (Crystal Impact, 2000)' _computing_publication_material 'Bruker SHELXTL' _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 contribution to the diffraction pattern from ethanol and water molecules of crystallization (with 22.5 % percentage void volume of the unit cell) was subtracted from the observed data by using the SQUEEZE method, as implemented in PLATON. ; _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^)+(0.1360P)^2^+13.6764P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12824 _refine_ls_number_parameters 726 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2124 _refine_ls_wR_factor_gt 0.1914 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.888 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _platon_squeeze_details ; The final formulation of the compound is in agreement with the residual electron density and volume. ; 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 0.162 -0.258 0.338 1530 194 ' ' 2 0.731 0.118 0.136 10 9 ' ' 3 0.769 0.118 0.364 10 9 ' ' 4 0.231 0.881 0.636 10 9 ' ' 5 0.269 0.881 0.864 10 9 ' ' 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 0.50858(3) 0.10341(4) 0.52722(3) 0.02650(19) Uani 1 1 d . . . Mn2 Mn 0.49109(3) 0.07275(4) 0.66705(3) 0.02819(19) Uani 1 1 d . . . Mn3 Mn 0.37168(3) 0.03109(4) 0.56885(3) 0.02680(19) Uani 1 1 d . . . Cl1 Cl 0.7500 0.29909(12) 0.2500 0.0505(5) Uani 1 2 d S . . O1 O 0.45404(13) 0.08203(18) 0.58751(12) 0.0269(6) Uani 1 1 d . . . O2 O 0.56424(14) 0.12163(18) 0.46697(13) 0.0290(7) Uani 1 1 d . . . O3 O 0.57188(15) 0.1095(2) 0.64574(13) 0.0340(7) Uani 1 1 d . . . O4 O 0.52758(14) 0.0569(2) 0.74587(13) 0.0345(7) Uani 1 1 d . . . O5 O 0.36720(14) -0.01082(19) 0.64647(13) 0.0318(7) Uani 1 1 d . . . O6 O 0.29271(14) -0.02772(19) 0.54731(13) 0.0316(7) Uani 1 1 d . . . O7 O 0.44669(13) 0.04697(18) 0.46993(13) 0.0271(6) Uani 1 1 d . . . O8 O 0.51275(14) -0.07635(19) 0.64650(13) 0.0323(7) Uani 1 1 d . . . O9 O 0.7048(2) 0.2400(3) 0.27636(19) 0.0690(12) Uani 1 1 d . . . O10 O 0.7836(3) 0.3500(4) 0.2946(2) 0.0923(16) Uani 1 1 d . . . N1 N 0.57804(17) 0.1378(2) 0.58806(16) 0.0319(8) Uani 1 1 d . . . N2 N 0.67995(18) 0.1680(3) 0.62844(18) 0.0408(10) Uani 1 1 d . . . H2A H 0.6692 0.1514 0.6623 0.049 Uiso 1 1 calc R . . H2B H 0.7186 0.1862 0.6249 0.049 Uiso 1 1 calc R . . N3 N 0.40795(16) 0.0302(2) 0.69027(15) 0.0273(8) Uani 1 1 d . . . N4 N 0.33185(18) -0.0179(3) 0.74992(17) 0.0362(9) Uani 1 1 d . . . H4A H 0.3080 -0.0360 0.7193 0.043 Uiso 1 1 calc R . . H4B H 0.3191 -0.0245 0.7845 0.043 Uiso 1 1 calc R . . N5 N 0.38298(16) 0.0487(2) 0.48533(16) 0.0270(8) Uani 1 1 d . . . N6 N 0.35457(19) 0.0591(3) 0.38507(17) 0.0363(9) Uani 1 1 d . . . H6A H 0.3943 0.0648 0.3786 0.044 Uiso 1 1 calc R . . H6B H 0.3250 0.0596 0.3560 0.044 Uiso 1 1 calc R . . N7 N 0.46354(19) 0.2417(2) 0.50361(18) 0.0375(9) Uani 1 1 d . . . N8 N 0.47361(18) 0.2266(2) 0.69294(17) 0.0356(9) Uani 1 1 d . . . N9 N 0.30960(18) 0.1544(2) 0.58413(17) 0.0357(9) Uani 1 1 d . . . N10 N 0.4984(2) -0.1768(3) 0.74183(19) 0.0485(11) Uani 1 1 d . . . C1 C 0.6158(2) 0.1787(3) 0.4714(2) 0.0328(10) Uani 1 1 d . . . C2 C 0.6535(2) 0.1967(3) 0.5236(2) 0.0347(11) Uani 1 1 d . . . C3 C 0.7100(3) 0.2473(3) 0.5213(2) 0.0471(13) Uani 1 1 d . . . H3A H 0.7358 0.2594 0.5560 0.056 Uiso 1 1 calc R . . C4 C 0.7280(3) 0.2796(3) 0.4683(3) 0.0510(14) Uani 1 1 d . . . H4C H 0.7669 0.3102 0.4674 0.061 Uiso 1 1 calc R . . C5 C 0.6884(3) 0.2666(3) 0.4169(2) 0.0461(13) Uani 1 1 d . . . H5A H 0.6992 0.2913 0.3816 0.055 Uiso 1 1 calc R . . C6 C 0.6321(2) 0.2160(3) 0.4183(2) 0.0389(11) Uani 1 1 d . . . H6C H 0.6052 0.2070 0.3837 0.047 Uiso 1 1 calc R . . C7 C 0.6372(2) 0.1659(3) 0.5820(2) 0.0320(10) Uani 1 1 d . . . C8 C 0.4962(2) 0.0694(3) 0.7938(2) 0.0355(10) Uani 1 1 d . . . C9 C 0.4293(2) 0.0522(3) 0.7955(2) 0.0325(10) Uani 1 1 d . . . C10 C 0.4023(2) 0.0659(3) 0.8485(2) 0.0375(11) Uani 1 1 d . . . H10C H 0.3584 0.0557 0.8495 0.045 Uiso 1 1 calc R . . C11 C 0.4373(3) 0.0937(4) 0.8988(2) 0.0483(13) Uani 1 1 d . . . H11A H 0.4181 0.1013 0.9336 0.058 Uiso 1 1 calc R . . C12 C 0.5022(3) 0.1102(5) 0.8966(2) 0.0585(15) Uani 1 1 d . . . H12A H 0.5269 0.1302 0.9303 0.070 Uiso 1 1 calc R . . C13 C 0.5306(2) 0.0974(4) 0.8455(2) 0.0531(14) Uani 1 1 d . . . H13A H 0.5745 0.1079 0.8456 0.064 Uiso 1 1 calc R . . C14 C 0.3887(2) 0.0204(3) 0.74386(19) 0.0271(9) Uani 1 1 d . . . C15 C 0.2515(2) -0.0002(3) 0.5028(2) 0.0307(10) Uani 1 1 d . . . C16 C 0.2703(2) 0.0391(3) 0.4503(2) 0.0346(10) Uani 1 1 d . . . C17 C 0.2234(2) 0.0655(4) 0.4068(2) 0.0462(13) Uani 1 1 d . . . H17A H 0.2356 0.0920 0.3725 0.055 Uiso 1 1 calc R . . C18 C 0.1592(3) 0.0537(5) 0.4130(3) 0.0591(16) Uani 1 1 d . . . H18A H 0.1283 0.0715 0.3830 0.071 Uiso 1 1 calc R . . C19 C 0.1405(2) 0.0151(4) 0.4639(2) 0.0514(14) Uani 1 1 d . . . H19A H 0.0970 0.0066 0.4680 0.062 Uiso 1 1 calc R . . C20 C 0.1856(2) -0.0103(4) 0.5080(2) 0.0420(12) Uani 1 1 d . . . H20A H 0.1723 -0.0350 0.5424 0.050 Uiso 1 1 calc R . . C21 C 0.3388(2) 0.0496(3) 0.44012(19) 0.0286(9) Uani 1 1 d . . . C22 C 0.4574(3) 0.3049(3) 0.5448(3) 0.0514(14) Uani 1 1 d . . . H22A H 0.4740 0.2922 0.5832 0.062 Uiso 1 1 calc R . . C23 C 0.4286(3) 0.3858(4) 0.5341(3) 0.0646(18) Uani 1 1 d . . . H23A H 0.4250 0.4259 0.5651 0.078 Uiso 1 1 calc R . . C24 C 0.4052(3) 0.4086(4) 0.4788(3) 0.0632(19) Uani 1 1 d . . . C25 C 0.4106(3) 0.3434(4) 0.4352(3) 0.0605(16) Uani 1 1 d . . . H25A H 0.3947 0.3559 0.3965 0.073 Uiso 1 1 calc R . . C26 C 0.4391(3) 0.2612(3) 0.4484(2) 0.0477(13) Uani 1 1 d . . . H26A H 0.4414 0.2186 0.4186 0.057 Uiso 1 1 calc R . . C27 C 0.3748(3) 0.5014(4) 0.4664(3) 0.079(2) Uani 1 1 d D . . C28 C 0.3029(3) 0.4962(4) 0.4741(4) 0.093(3) Uani 1 1 d D . . H28A H 0.2827 0.4530 0.4468 0.139 Uiso 1 1 calc R . . H28B H 0.2836 0.5544 0.4666 0.139 Uiso 1 1 calc R . . H28C H 0.2972 0.4779 0.5137 0.139 Uiso 1 1 calc R . . C29 C 0.4056(4) 0.5727(4) 0.5115(4) 0.097(3) Uani 1 1 d D . . H29A H 0.4509 0.5779 0.5074 0.145 Uiso 1 1 calc R . . H29B H 0.3996 0.5538 0.5510 0.145 Uiso 1 1 calc R . . H29C H 0.3853 0.6302 0.5039 0.145 Uiso 1 1 calc R . . C30 C 0.3896(7) 0.5391(7) 0.4108(5) 0.173(6) Uani 1 1 d D . . H30A H 0.3728 0.5005 0.3791 0.259 Uiso 1 1 calc R . . H30B H 0.4355 0.5441 0.4105 0.259 Uiso 1 1 calc R . . H30C H 0.3705 0.5978 0.4057 0.259 Uiso 1 1 calc R . . C31 C 0.4164(2) 0.2684(3) 0.6901(3) 0.0499(14) Uani 1 1 d . . . H31A H 0.3794 0.2335 0.6834 0.060 Uiso 1 1 calc R . . C32 C 0.4092(3) 0.3599(4) 0.6965(3) 0.0540(14) Uani 1 1 d . . . H32A H 0.3679 0.3844 0.6931 0.065 Uiso 1 1 calc R . . C33 C 0.4601(3) 0.4152(3) 0.7076(2) 0.0485(14) Uani 1 1 d . . . C34 C 0.5204(3) 0.3722(3) 0.7129(3) 0.0552(15) Uani 1 1 d . . . H34A H 0.5578 0.4058 0.7212 0.066 Uiso 1 1 calc R . . C35 C 0.5241(3) 0.2795(3) 0.7058(2) 0.0473(13) Uani 1 1 d . . . H35A H 0.5647 0.2529 0.7103 0.057 Uiso 1 1 calc R . . C36 C 0.4550(3) 0.5172(4) 0.7165(3) 0.0658(18) Uani 1 1 d D . . C37 C 0.4704(6) 0.5384(5) 0.7803(4) 0.130(4) Uani 1 1 d D . . H37A H 0.5138 0.5205 0.7925 0.195 Uiso 1 1 calc R . . H37B H 0.4413 0.5063 0.8030 0.195 Uiso 1 1 calc R . . H37C H 0.4658 0.6021 0.7863 0.195 Uiso 1 1 calc R . . C38 C 0.4933(6) 0.5666(5) 0.6759(5) 0.148(5) Uani 1 1 d D . . H38A H 0.4725 0.5628 0.6365 0.221 Uiso 1 1 calc R . . H38B H 0.5355 0.5406 0.6772 0.221 Uiso 1 1 calc R . . H38C H 0.4968 0.6288 0.6877 0.221 Uiso 1 1 calc R . . C39 C 0.3851(4) 0.5490(5) 0.7023(6) 0.134(4) Uani 1 1 d D . . H39A H 0.3828 0.6131 0.7078 0.201 Uiso 1 1 calc R . . H39B H 0.3580 0.5193 0.7281 0.201 Uiso 1 1 calc R . . H39C H 0.3707 0.5344 0.6621 0.201 Uiso 1 1 calc R . . C40 C 0.2740(2) 0.1526(4) 0.6304(2) 0.0432(12) Uani 1 1 d . . . H40A H 0.2786 0.1039 0.6562 0.052 Uiso 1 1 calc R . . C41 C 0.2311(2) 0.2193(4) 0.6413(3) 0.0495(14) Uani 1 1 d . . . H41A H 0.2086 0.2157 0.6746 0.059 Uiso 1 1 calc R . . C42 C 0.2210(3) 0.2917(4) 0.6035(3) 0.0627(17) Uani 1 1 d . . . C43 C 0.2571(3) 0.2921(4) 0.5559(3) 0.0691(19) Uani 1 1 d . . . H43A H 0.2524 0.3391 0.5287 0.083 Uiso 1 1 calc R . . C44 C 0.3003(2) 0.2236(3) 0.5481(2) 0.0445(12) Uani 1 1 d . . . H44A H 0.3241 0.2265 0.5156 0.053 Uiso 1 1 calc R . . C45 C 0.1734(4) 0.3671(4) 0.6150(4) 0.091(3) Uani 1 1 d D . . C46 C 0.1130(4) 0.3300(6) 0.6360(6) 0.132(4) Uani 1 1 d D . . H46A H 0.1231 0.2987 0.6726 0.199 Uiso 1 1 calc R . . H46B H 0.0932 0.2889 0.6071 0.199 Uiso 1 1 calc R . . H46C H 0.0838 0.3785 0.6417 0.199 Uiso 1 1 calc R . . C47 C 0.2073(5) 0.4300(8) 0.6563(9) 0.260(12) Uani 1 1 d D . . H47A H 0.2202 0.3995 0.6927 0.390 Uiso 1 1 calc R . . H47B H 0.1793 0.4794 0.6636 0.390 Uiso 1 1 calc R . . H47C H 0.2448 0.4527 0.6398 0.390 Uiso 1 1 calc R . . C48 C 0.1497(6) 0.4147(9) 0.5568(6) 0.180(6) Uani 1 1 d D . . H48A H 0.1199 0.4616 0.5645 0.271 Uiso 1 1 calc R . . H48B H 0.1287 0.3717 0.5299 0.271 Uiso 1 1 calc R . . H48C H 0.1858 0.4405 0.5397 0.271 Uiso 1 1 calc R . . C49 C 0.5446(3) -0.1889(5) 0.7835(3) 0.0698(18) Uani 1 1 d . . . H49A H 0.5865 -0.1791 0.7743 0.084 Uiso 1 1 calc R . . C50 C 0.5361(3) -0.2156(5) 0.8406(3) 0.0657(17) Uani 1 1 d . . . H50A H 0.5716 -0.2249 0.8678 0.079 Uiso 1 1 calc R . . C51 C 0.4746(3) -0.2281(3) 0.8567(2) 0.0429(12) Uani 1 1 d . . . C52 C 0.4253(3) -0.2145(3) 0.8128(2) 0.0440(12) Uani 1 1 d . . . H52A H 0.3826 -0.2213 0.8208 0.053 Uiso 1 1 calc R . . C53 C 0.4395(3) -0.1908(3) 0.7571(2) 0.0457(12) Uani 1 1 d . . . H53A H 0.4053 -0.1840 0.7280 0.055 Uiso 1 1 calc R . . C54 C 0.4591(3) -0.2538(4) 0.9186(2) 0.0545(14) Uani 1 1 d . . . C55 C 0.5188(4) -0.2584(6) 0.9622(3) 0.085(2) Uani 1 1 d . . . H55A H 0.5477 -0.3032 0.9494 0.128 Uiso 1 1 calc R . . H55B H 0.5067 -0.2742 1.0004 0.128 Uiso 1 1 calc R . . H55C H 0.5399 -0.2007 0.9642 0.128 Uiso 1 1 calc R . . C56 C 0.4218(5) -0.3406(5) 0.9165(3) 0.091(3) Uani 1 1 d . . . H56A H 0.4474 -0.3880 0.9020 0.137 Uiso 1 1 calc R . . H56B H 0.3828 -0.3337 0.8909 0.137 Uiso 1 1 calc R . . H56C H 0.4114 -0.3557 0.9555 0.137 Uiso 1 1 calc R . . C57 C 0.4152(4) -0.1795(5) 0.9422(3) 0.079(2) Uani 1 1 d . . . H57A H 0.3768 -0.1731 0.9156 0.118 Uiso 1 1 calc R . . H57B H 0.4380 -0.1232 0.9451 0.118 Uiso 1 1 calc R . . H57C H 0.4037 -0.1966 0.9805 0.118 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0306(4) 0.0212(3) 0.0306(4) -0.0012(2) 0.0177(3) -0.0007(2) Mn2 0.0290(4) 0.0285(3) 0.0296(4) -0.0019(3) 0.0159(3) -0.0007(3) Mn3 0.0292(4) 0.0251(3) 0.0288(4) -0.0013(3) 0.0167(3) -0.0016(3) Cl1 0.0675(12) 0.0462(10) 0.0414(10) 0.000 0.0241(9) 0.000 O1 0.0316(15) 0.0256(14) 0.0267(15) -0.0014(12) 0.0186(13) -0.0011(12) O2 0.0342(16) 0.0242(14) 0.0312(16) -0.0014(12) 0.0176(13) -0.0046(12) O3 0.0382(17) 0.0370(17) 0.0292(16) 0.0012(13) 0.0159(14) -0.0019(13) O4 0.0296(16) 0.0451(18) 0.0304(17) 0.0008(14) 0.0117(13) 0.0024(13) O5 0.0343(16) 0.0338(16) 0.0296(16) -0.0038(13) 0.0143(13) -0.0064(13) O6 0.0317(16) 0.0307(16) 0.0347(17) 0.0009(13) 0.0156(14) -0.0027(12) O7 0.0272(15) 0.0246(14) 0.0319(16) -0.0002(12) 0.0158(12) 0.0008(11) O8 0.0382(17) 0.0283(15) 0.0338(17) -0.0002(13) 0.0203(14) 0.0027(13) O9 0.073(3) 0.071(3) 0.066(3) 0.008(2) 0.024(2) -0.015(2) O10 0.104(4) 0.083(3) 0.094(4) -0.042(3) 0.032(3) -0.022(3) N1 0.038(2) 0.0264(18) 0.035(2) -0.0033(15) 0.0205(17) -0.0011(15) N2 0.031(2) 0.049(2) 0.044(2) 0.0011(19) 0.0175(19) -0.0071(18) N3 0.0311(19) 0.0261(17) 0.0271(19) -0.0039(14) 0.0149(16) -0.0017(14) N4 0.036(2) 0.047(2) 0.029(2) -0.0006(17) 0.0194(17) -0.0066(17) N5 0.0257(18) 0.0244(17) 0.034(2) -0.0014(15) 0.0175(16) 0.0000(14) N6 0.034(2) 0.046(2) 0.031(2) 0.0051(17) 0.0134(17) 0.0084(17) N7 0.047(2) 0.0246(18) 0.045(2) 0.0014(17) 0.0253(19) 0.0019(16) N8 0.039(2) 0.0320(19) 0.037(2) -0.0056(16) 0.0120(17) -0.0070(17) N9 0.036(2) 0.032(2) 0.042(2) -0.0112(17) 0.0170(18) -0.0010(16) N10 0.068(3) 0.038(2) 0.041(2) 0.0035(19) 0.010(2) -0.006(2) C1 0.042(3) 0.019(2) 0.042(3) -0.0001(18) 0.028(2) 0.0056(18) C2 0.042(3) 0.024(2) 0.042(3) -0.0056(19) 0.022(2) -0.0053(19) C3 0.050(3) 0.041(3) 0.054(3) -0.005(2) 0.025(3) -0.011(2) C4 0.059(3) 0.039(3) 0.060(4) -0.002(2) 0.032(3) -0.015(2) C5 0.062(3) 0.036(3) 0.046(3) -0.002(2) 0.037(3) -0.010(2) C6 0.052(3) 0.027(2) 0.042(3) -0.002(2) 0.030(2) -0.001(2) C7 0.032(2) 0.026(2) 0.040(3) -0.0052(19) 0.016(2) -0.0011(18) C8 0.042(3) 0.038(2) 0.028(2) -0.0005(19) 0.013(2) -0.002(2) C9 0.035(2) 0.030(2) 0.034(2) -0.0025(19) 0.011(2) 0.0055(18) C10 0.037(3) 0.043(3) 0.035(3) -0.002(2) 0.015(2) 0.000(2) C11 0.048(3) 0.068(4) 0.031(3) -0.009(2) 0.017(2) -0.001(3) C12 0.051(3) 0.089(4) 0.035(3) -0.018(3) 0.007(3) -0.006(3) C13 0.029(3) 0.088(4) 0.042(3) -0.002(3) 0.005(2) -0.007(3) C14 0.032(2) 0.022(2) 0.030(2) 0.0015(17) 0.0122(18) 0.0032(17) C15 0.029(2) 0.030(2) 0.034(2) -0.0062(19) 0.0084(19) 0.0019(18) C16 0.036(2) 0.033(2) 0.038(3) -0.0011(19) 0.019(2) 0.0051(19) C17 0.036(3) 0.062(3) 0.043(3) 0.005(2) 0.017(2) 0.010(2) C18 0.039(3) 0.097(5) 0.042(3) 0.008(3) 0.004(2) 0.011(3) C19 0.028(3) 0.079(4) 0.049(3) -0.004(3) 0.014(2) 0.003(2) C20 0.032(2) 0.055(3) 0.040(3) -0.003(2) 0.014(2) -0.003(2) C21 0.032(2) 0.025(2) 0.031(2) 0.0027(17) 0.015(2) 0.0069(17) C22 0.067(4) 0.029(3) 0.061(3) -0.012(2) 0.021(3) 0.002(2) C23 0.093(5) 0.033(3) 0.074(4) -0.001(3) 0.037(4) 0.008(3) C24 0.069(4) 0.037(3) 0.093(5) 0.010(3) 0.055(4) 0.011(3) C25 0.068(4) 0.064(4) 0.055(3) 0.029(3) 0.030(3) 0.023(3) C26 0.063(3) 0.037(3) 0.049(3) 0.012(2) 0.035(3) 0.014(2) C27 0.092(5) 0.046(3) 0.105(6) 0.025(4) 0.044(4) 0.024(3) C28 0.067(4) 0.044(4) 0.168(9) 0.012(4) 0.014(5) 0.017(3) C29 0.095(6) 0.043(4) 0.154(9) 0.007(4) 0.026(6) 0.003(4) C30 0.283(16) 0.088(7) 0.162(11) 0.077(7) 0.102(11) 0.104(9) C31 0.042(3) 0.042(3) 0.069(4) -0.019(3) 0.022(3) -0.002(2) C32 0.056(3) 0.042(3) 0.067(4) -0.011(3) 0.023(3) 0.006(3) C33 0.072(4) 0.034(3) 0.045(3) -0.003(2) 0.032(3) 0.006(3) C34 0.067(4) 0.037(3) 0.064(4) -0.010(3) 0.021(3) -0.019(3) C35 0.052(3) 0.035(3) 0.057(3) -0.007(2) 0.015(3) 0.000(2) C36 0.092(5) 0.032(3) 0.081(5) -0.009(3) 0.045(4) 0.003(3) C37 0.257(14) 0.044(4) 0.093(6) -0.027(4) 0.035(8) -0.013(6) C38 0.262(14) 0.033(4) 0.173(10) -0.010(5) 0.149(10) -0.007(5) C39 0.113(7) 0.055(5) 0.243(14) -0.016(6) 0.068(8) 0.013(5) C40 0.035(3) 0.049(3) 0.049(3) -0.006(2) 0.019(2) 0.001(2) C41 0.045(3) 0.048(3) 0.060(3) -0.019(3) 0.029(3) -0.001(2) C42 0.060(4) 0.041(3) 0.093(5) -0.020(3) 0.034(3) 0.011(3) C43 0.090(5) 0.038(3) 0.085(5) 0.008(3) 0.037(4) 0.022(3) C44 0.052(3) 0.033(3) 0.053(3) 0.000(2) 0.026(3) 0.009(2) C45 0.094(5) 0.044(4) 0.143(8) -0.017(4) 0.054(5) 0.027(4) C46 0.077(5) 0.096(6) 0.235(13) -0.023(7) 0.069(7) 0.041(5) C47 0.078(6) 0.157(10) 0.54(3) -0.260(16) -0.002(11) 0.034(6) C48 0.155(11) 0.150(11) 0.239(17) -0.025(11) 0.032(11) 0.104(9) C49 0.062(4) 0.082(5) 0.068(4) 0.011(4) 0.020(4) -0.025(3) C50 0.058(4) 0.087(5) 0.050(4) 0.015(3) -0.002(3) -0.010(3) C51 0.057(3) 0.031(2) 0.042(3) -0.001(2) 0.009(3) -0.001(2) C52 0.053(3) 0.040(3) 0.042(3) -0.003(2) 0.017(2) 0.003(2) C53 0.060(3) 0.037(3) 0.042(3) -0.002(2) 0.012(3) 0.004(2) C54 0.075(4) 0.053(3) 0.037(3) 0.004(2) 0.011(3) 0.004(3) C55 0.085(5) 0.124(6) 0.047(4) 0.011(4) 0.011(4) 0.016(5) C56 0.146(7) 0.077(5) 0.055(4) 0.007(4) 0.028(5) -0.025(5) C57 0.100(5) 0.091(5) 0.048(4) -0.004(3) 0.016(4) 0.026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 1.893(3) . ? Mn1 O2 1.900(3) . ? Mn1 O7 1.934(3) . ? Mn1 N1 1.972(4) . ? Mn1 N7 2.296(4) . ? Mn1 O7 2.415(3) 3_656 ? Mn2 O3 1.879(3) . ? Mn2 O4 1.895(3) . ? Mn2 O1 1.904(3) . ? Mn2 N3 1.965(3) . ? Mn2 O8 2.312(3) . ? Mn2 N8 2.392(4) . ? Mn3 O5 1.884(3) . ? Mn3 O6 1.886(3) . ? Mn3 O1 1.887(3) . ? Mn3 N5 1.957(3) . ? Mn3 N9 2.285(4) . ? Cl1 O10 1.398(5) . ? Cl1 O10 1.398(5) 2_655 ? Cl1 O9 1.459(4) . ? Cl1 O9 1.459(4) 2_655 ? O2 C1 1.363(5) . ? O3 N1 1.397(5) . ? O4 C8 1.338(5) . ? O5 N3 1.387(5) . ? O6 C15 1.328(5) . ? O7 N5 1.407(4) . ? O7 Mn1 2.415(3) 3_656 ? N1 C7 1.323(5) . ? N2 C7 1.317(6) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C14 1.329(5) . ? N4 C14 1.334(5) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 C21 1.313(6) . ? N6 C21 1.334(5) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? N7 C22 1.340(6) . ? N7 C26 1.343(7) . ? N8 C35 1.323(6) . ? N8 C31 1.341(6) . ? N9 C44 1.316(6) . ? N9 C40 1.348(6) . ? N10 C49 1.297(8) . ? N10 C53 1.326(7) . ? C1 C2 1.386(7) . ? C1 C6 1.402(6) . ? C2 C3 1.401(6) . ? C2 C7 1.477(6) . ? C3 C4 1.383(7) . ? C3 H3A 0.9300 . ? C4 C5 1.380(8) . ? C4 H4C 0.9300 . ? C5 C6 1.398(7) . ? C5 H5A 0.9300 . ? C6 H6C 0.9300 . ? C8 C13 1.383(7) . ? C8 C9 1.423(6) . ? C9 C10 1.394(6) . ? C9 C14 1.460(6) . ? C10 C11 1.362(7) . ? C10 H10C 0.9300 . ? C11 C12 1.380(8) . ? C11 H11A 0.9300 . ? C12 C13 1.370(8) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C15 C20 1.399(6) . ? C15 C16 1.419(6) . ? C16 C17 1.380(7) . ? C16 C21 1.478(6) . ? C17 C18 1.371(7) . ? C17 H17A 0.9300 . ? C18 C19 1.381(8) . ? C18 H18A 0.9300 . ? C19 C20 1.362(8) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C22 C23 1.352(8) . ? C22 H22A 0.9300 . ? C23 C24 1.351(10) . ? C23 H23A 0.9300 . ? C24 C25 1.397(9) . ? C24 C27 1.529(8) . ? C25 C26 1.376(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C30 1.445(10) . ? C27 C28 1.529(9) . ? C27 C29 1.570(10) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.374(7) . ? C31 H31A 0.9300 . ? C32 C33 1.346(8) . ? C32 H32A 0.9300 . ? C33 C34 1.405(8) . ? C33 C36 1.529(7) . ? C34 C35 1.386(7) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 C38 1.472(9) . ? C36 C37 1.490(10) . ? C36 C39 1.537(10) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 C41 1.372(7) . ? C40 H40A 0.9300 . ? C41 C42 1.379(9) . ? C41 H41A 0.9300 . ? C42 C43 1.380(8) . ? C42 C45 1.534(7) . ? C43 C44 1.380(7) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 C47 1.459(11) . ? C45 C46 1.495(10) . ? C45 C48 1.540(13) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.386(9) . ? C49 H49A 0.9300 . ? C50 C51 1.380(8) . ? C50 H50A 0.9300 . ? C51 C52 1.378(7) . ? C51 C54 1.525(7) . ? C52 C53 1.377(7) . ? C52 H52A 0.9300 . ? C53 H53A 0.9300 . ? C54 C56 1.502(9) . ? C54 C55 1.518(9) . ? C54 C57 1.561(8) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 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 O1 Mn1 O2 178.44(12) . . ? O1 Mn1 O7 90.47(12) . . ? O2 Mn1 O7 89.36(12) . . ? O1 Mn1 N1 89.18(13) . . ? O2 Mn1 N1 90.69(13) . . ? O7 Mn1 N1 169.24(13) . . ? O1 Mn1 N7 93.34(12) . . ? O2 Mn1 N7 88.21(12) . . ? O7 Mn1 N7 89.81(13) . . ? N1 Mn1 N7 100.94(15) . . ? O1 Mn1 O7 94.81(10) . 3_656 ? O2 Mn1 O7 83.64(10) . 3_656 ? O7 Mn1 O7 81.37(12) . 3_656 ? N1 Mn1 O7 87.94(12) . 3_656 ? N7 Mn1 O7 168.03(12) . 3_656 ? O3 Mn2 O4 89.58(13) . . ? O3 Mn2 O1 91.42(13) . . ? O4 Mn2 O1 177.01(13) . . ? O3 Mn2 N3 177.99(14) . . ? O4 Mn2 N3 89.39(14) . . ? O1 Mn2 N3 89.52(13) . . ? O3 Mn2 O8 91.56(12) . . ? O4 Mn2 O8 90.27(12) . . ? O1 Mn2 O8 86.89(11) . . ? N3 Mn2 O8 86.71(12) . . ? O3 Mn2 N8 87.08(13) . . ? O4 Mn2 N8 86.66(14) . . ? O1 Mn2 N8 96.20(13) . . ? N3 Mn2 N8 94.58(13) . . ? O8 Mn2 N8 176.65(13) . . ? O5 Mn3 O6 88.31(13) . . ? O5 Mn3 O1 92.71(13) . . ? O6 Mn3 O1 175.30(12) . . ? O5 Mn3 N5 167.82(13) . . ? O6 Mn3 N5 89.60(14) . . ? O1 Mn3 N5 88.44(13) . . ? O5 Mn3 N9 92.32(13) . . ? O6 Mn3 N9 85.17(13) . . ? O1 Mn3 N9 99.37(13) . . ? N5 Mn3 N9 99.46(14) . . ? O10 Cl1 O10 114.7(5) . 2_655 ? O10 Cl1 O9 108.9(3) . . ? O10 Cl1 O9 108.9(3) 2_655 . ? O10 Cl1 O9 108.9(3) . 2_655 ? O10 Cl1 O9 108.9(3) 2_655 2_655 ? O9 Cl1 O9 106.2(4) . 2_655 ? Mn3 O1 Mn1 120.11(15) . . ? Mn3 O1 Mn2 117.52(13) . . ? Mn1 O1 Mn2 119.02(15) . . ? C1 O2 Mn1 124.5(3) . . ? N1 O3 Mn2 119.8(3) . . ? C8 O4 Mn2 124.8(3) . . ? N3 O5 Mn3 116.6(2) . . ? C15 O6 Mn3 122.7(3) . . ? N5 O7 Mn1 114.1(2) . . ? N5 O7 Mn1 112.5(2) . 3_656 ? Mn1 O7 Mn1 98.63(12) . 3_656 ? C7 N1 O3 111.4(4) . . ? C7 N1 Mn1 129.6(3) . . ? O3 N1 Mn1 117.1(2) . . ? C7 N2 H2A 120.0 . . ? C7 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C14 N3 O5 113.2(3) . . ? C14 N3 Mn2 129.4(3) . . ? O5 N3 Mn2 116.3(2) . . ? C14 N4 H4A 120.0 . . ? C14 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C21 N5 O7 114.4(3) . . ? C21 N5 Mn3 128.5(3) . . ? O7 N5 Mn3 116.4(3) . . ? C21 N6 H6A 120.0 . . ? C21 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C22 N7 C26 116.9(4) . . ? C22 N7 Mn1 121.7(4) . . ? C26 N7 Mn1 121.4(3) . . ? C35 N8 C31 115.0(4) . . ? C35 N8 Mn2 118.8(3) . . ? C31 N8 Mn2 125.8(3) . . ? C44 N9 C40 116.3(4) . . ? C44 N9 Mn3 125.4(3) . . ? C40 N9 Mn3 117.8(3) . . ? C49 N10 C53 115.4(5) . . ? O2 C1 C2 124.2(4) . . ? O2 C1 C6 115.8(4) . . ? C2 C1 C6 119.9(4) . . ? C1 C2 C3 118.8(4) . . ? C1 C2 C7 123.4(4) . . ? C3 C2 C7 117.8(5) . . ? C4 C3 C2 121.2(5) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C5 C4 C3 120.1(5) . . ? C5 C4 H4C 120.0 . . ? C3 C4 H4C 120.0 . . ? C4 C5 C6 119.4(4) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? C5 C6 C1 120.4(5) . . ? C5 C6 H6C 119.8 . . ? C1 C6 H6C 119.8 . . ? N2 C7 N1 119.3(4) . . ? N2 C7 C2 121.3(4) . . ? N1 C7 C2 119.4(4) . . ? O4 C8 C13 118.8(4) . . ? O4 C8 C9 123.8(4) . . ? C13 C8 C9 117.3(4) . . ? C10 C9 C8 118.5(4) . . ? C10 C9 C14 119.6(4) . . ? C8 C9 C14 121.9(4) . . ? C11 C10 C9 122.9(4) . . ? C11 C10 H10C 118.5 . . ? C9 C10 H10C 118.5 . . ? C10 C11 C12 118.1(5) . . ? C10 C11 H11A 120.9 . . ? C12 C11 H11A 120.9 . . ? C13 C12 C11 120.8(5) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 C8 122.3(5) . . ? C12 C13 H13A 118.8 . . ? C8 C13 H13A 118.8 . . ? N3 C14 N4 119.5(4) . . ? N3 C14 C9 120.1(4) . . ? N4 C14 C9 120.4(4) . . ? O6 C15 C20 118.1(4) . . ? O6 C15 C16 123.9(4) . . ? C20 C15 C16 118.0(4) . . ? C17 C16 C15 119.1(4) . . ? C17 C16 C21 119.1(4) . . ? C15 C16 C21 121.7(4) . . ? C18 C17 C16 121.4(5) . . ? C18 C17 H17A 119.3 . . ? C16 C17 H17A 119.3 . . ? C17 C18 C19 119.8(5) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C20 C19 C18 120.2(5) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C15 121.4(5) . . ? C19 C20 H20A 119.3 . . ? C15 C20 H20A 119.3 . . ? N5 C21 N6 121.4(4) . . ? N5 C21 C16 119.4(4) . . ? N6 C21 C16 119.2(4) . . ? N7 C22 C23 124.5(6) . . ? N7 C22 H22A 117.8 . . ? C23 C22 H22A 117.8 . . ? C24 C23 C22 120.2(6) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 116.3(5) . . ? C23 C24 C27 120.2(6) . . ? C25 C24 C27 123.5(6) . . ? C26 C25 C24 121.4(6) . . ? C26 C25 H25A 119.3 . . ? C24 C25 H25A 119.3 . . ? N7 C26 C25 120.7(5) . . ? N7 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C30 C27 C28 114.6(9) . . ? C30 C27 C24 112.9(6) . . ? C28 C27 C24 109.1(5) . . ? C30 C27 C29 101.8(8) . . ? C28 C27 C29 107.6(6) . . ? C24 C27 C29 110.4(6) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N8 C31 C32 123.9(5) . . ? N8 C31 H31A 118.1 . . ? C32 C31 H31A 118.1 . . ? C33 C32 C31 121.9(5) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C34 115.0(5) . . ? C32 C33 C36 124.3(5) . . ? C34 C33 C36 120.7(5) . . ? C35 C34 C33 120.0(5) . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? N8 C35 C34 124.1(5) . . ? N8 C35 H35A 118.0 . . ? C34 C35 H35A 118.0 . . ? C38 C36 C37 115.3(8) . . ? C38 C36 C33 111.1(5) . . ? C37 C36 C33 109.0(5) . . ? C38 C36 C39 106.1(8) . . ? C37 C36 C39 104.5(7) . . ? C33 C36 C39 110.6(6) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N9 C40 C41 123.1(5) . . ? N9 C40 H40A 118.5 . . ? C41 C40 H40A 118.5 . . ? C40 C41 C42 120.7(5) . . ? C40 C41 H41A 119.6 . . ? C42 C41 H41A 119.6 . . ? C41 C42 C43 115.6(5) . . ? C41 C42 C45 121.5(6) . . ? C43 C42 C45 122.9(6) . . ? C42 C43 C44 120.7(6) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? N9 C44 C43 123.5(5) . . ? N9 C44 H44A 118.2 . . ? C43 C44 H44A 118.2 . . ? C47 C45 C46 113.6(9) . . ? C47 C45 C42 107.1(7) . . ? C46 C45 C42 111.5(6) . . ? C47 C45 C48 110.9(11) . . ? C46 C45 C48 103.5(9) . . ? C42 C45 C48 110.2(7) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N10 C49 C50 124.9(6) . . ? N10 C49 H49A 117.5 . . ? C50 C49 H49A 117.5 . . ? C51 C50 C49 119.6(6) . . ? C51 C50 H50A 120.2 . . ? C49 C50 H50A 120.2 . . ? C52 C51 C50 115.8(5) . . ? C52 C51 C54 119.7(5) . . ? C50 C51 C54 124.4(5) . . ? C53 C52 C51 119.6(5) . . ? C53 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? N10 C53 C52 124.7(5) . . ? N10 C53 H53A 117.7 . . ? C52 C53 H53A 117.7 . . ? C56 C54 C55 111.8(6) . . ? C56 C54 C51 109.9(5) . . ? C55 C54 C51 112.4(5) . . ? C56 C54 C57 107.2(6) . . ? C55 C54 C57 106.1(5) . . ? C51 C54 C57 109.1(5) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.003 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.098 _database_code_depnum_ccdc_archive 'CCDC 962811' ####################################################################### # # 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_962812 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H70 Mn6 N24 O16, 2(Cl O4), 6(C2 H6 O)' _chemical_formula_sum 'C76 H106 Cl2 Mn6 N24 O30' _chemical_formula_weight 2236.39 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.2304(2) _cell_length_b 12.7593(2) _cell_length_c 25.9852(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.473(2) _cell_angle_gamma 90.00 _cell_volume 4713.74(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8618 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 75.73 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.116 _exptl_crystal_size_min 0.016 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2308 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.470 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37593 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.56 _reflns_number_total 9606 _reflns_number_gt 7054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Agilent Technologies, 2013)' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2d (Crystal Impact, 2000)' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0872P)^2^+11.8016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9606 _refine_ls_number_parameters 622 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1836 _refine_ls_wR_factor_gt 0.1638 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.49602(5) 0.58188(6) 0.04732(3) 0.02386(17) Uani 1 1 d . . . Mn2 Mn 0.71811(5) 0.59308(6) 0.08612(3) 0.02565(18) Uani 1 1 d . . . Mn3 Mn 0.60703(5) 0.37166(6) 0.09010(3) 0.02611(18) Uani 1 1 d . . . Cl1 Cl 0.09094(13) 0.04659(15) 0.15425(7) 0.0618(4) Uani 1 1 d . . . O1 O 0.6040(2) 0.5175(3) 0.07769(12) 0.0243(6) Uani 1 1 d . . . O2 O 0.3942(2) 0.6493(3) 0.00810(12) 0.0260(7) Uani 1 1 d . . . O3 O 0.6630(2) 0.7134(3) 0.05476(12) 0.0257(7) Uani 1 1 d . . . O4 O 0.8368(2) 0.6605(3) 0.08359(12) 0.0264(7) Uani 1 1 d . . . O5 O 0.7405(2) 0.3696(3) 0.09857(13) 0.0281(7) Uani 1 1 d . . . O6 O 0.6067(2) 0.2232(3) 0.09637(13) 0.0295(7) Uani 1 1 d . . . O7 O 0.4395(2) 0.4453(2) 0.03533(12) 0.0232(6) Uani 1 1 d . . . O8 O 0.7558(2) 0.5194(3) 0.00262(12) 0.0252(7) Uani 1 1 d . . . O9 O 0.8145(3) 0.8278(4) 0.00609(18) 0.0529(11) Uani 1 1 d . . . H9A H 0.8173 0.7806 0.0275 0.079 Uiso 1 1 calc R . . O10 O 0.7908(3) 0.1583(3) 0.13872(16) 0.0433(9) Uani 1 1 d . . . H10A H 0.7392 0.1828 0.1301 0.065 Uiso 1 1 calc R . . O11 O 0.0930(3) 0.3015(4) 0.20982(19) 0.0571(12) Uani 1 1 d . . . H11A H 0.0860 0.2438 0.1963 0.086 Uiso 1 1 calc R . . O12 O 0.1405(8) -0.0166(8) 0.1904(3) 0.165(4) Uani 1 1 d . . . O13 O 0.0179(5) 0.1009(7) 0.1801(3) 0.122(3) Uani 1 1 d . . . O14 O 0.0491(5) -0.0192(5) 0.1137(3) 0.0893(19) Uani 1 1 d . . . O15 O 0.1470(4) 0.1232(5) 0.1319(3) 0.0865(19) Uani 1 1 d . . . N1 N 0.5652(3) 0.7165(3) 0.05084(14) 0.0242(8) Uani 1 1 d . . . N2 N 0.5917(3) 0.8909(3) 0.03927(19) 0.0375(10) Uani 1 1 d . . . H2A H 0.6513 0.8804 0.0431 0.045 Uiso 1 1 calc R . . H2B H 0.5706 0.9531 0.0336 0.045 Uiso 1 1 calc R . . N3 N 0.7816(3) 0.4649(3) 0.11269(14) 0.0248(8) Uani 1 1 d . . . N4 N 0.9004(3) 0.3632(3) 0.14757(17) 0.0349(10) Uani 1 1 d . . . H4A H 0.8683 0.3077 0.1403 0.042 Uiso 1 1 calc R . . H4B H 0.9553 0.3580 0.1626 0.042 Uiso 1 1 calc R . . N5 N 0.4716(3) 0.3681(3) 0.07068(14) 0.0243(8) Uani 1 1 d . . . N6 N 0.3212(3) 0.3011(3) 0.06113(16) 0.0292(9) Uani 1 1 d . . . H6A H 0.3028 0.3549 0.0435 0.035 Uiso 1 1 calc R . . H6B H 0.2822 0.2515 0.0672 0.035 Uiso 1 1 calc R . . N7 N 0.4192(3) 0.6096(3) 0.11888(16) 0.0309(9) Uani 1 1 d . . . N8 N 0.3836(4) 0.6773(4) 0.1934(2) 0.0541(14) Uani 1 1 d . . . H8A H 0.3861 0.7164 0.2204 0.065 Uiso 1 1 calc R . . N9 N 0.6936(3) 0.6565(3) 0.16634(16) 0.0320(9) Uani 1 1 d . . . N10 N 0.6712(3) 0.6737(4) 0.24893(17) 0.0413(11) Uani 1 1 d . . . H10B H 0.6681 0.6585 0.2811 0.050 Uiso 1 1 calc R . . N11 N 0.5895(3) 0.3818(3) 0.17442(15) 0.0304(9) Uani 1 1 d . . . N12 N 0.5400(5) 0.4027(7) 0.2515(2) 0.083(2) Uani 1 1 d . . . H12B H 0.5079 0.4263 0.2763 0.100 Uiso 1 1 calc R . . C1 C 0.3656(3) 0.7466(4) 0.02162(17) 0.0249(9) Uani 1 1 d . . . C2 C 0.4292(3) 0.8275(4) 0.03764(18) 0.0274(10) Uani 1 1 d . . . C3 C 0.3933(4) 0.9244(4) 0.0510(2) 0.0352(11) Uani 1 1 d . . . H3A H 0.4346 0.9771 0.0619 0.042 Uiso 1 1 calc R . . C4 C 0.2976(4) 0.9448(4) 0.0486(2) 0.0391(12) Uani 1 1 d . . . H4C H 0.2749 1.0102 0.0578 0.047 Uiso 1 1 calc R . . C5 C 0.2359(4) 0.8658(4) 0.0321(2) 0.0374(12) Uani 1 1 d . . . H5A H 0.1714 0.8782 0.0303 0.045 Uiso 1 1 calc R . . C6 C 0.2703(3) 0.7691(4) 0.0183(2) 0.0332(11) Uani 1 1 d . . . H6C H 0.2284 0.7177 0.0065 0.040 Uiso 1 1 calc R . . C7 C 0.5318(3) 0.8102(4) 0.04215(18) 0.0276(10) Uani 1 1 d . . . C8 C 0.9067(3) 0.6464(4) 0.11896(18) 0.0277(10) Uani 1 1 d . . . C9 C 0.9201(3) 0.5534(4) 0.14705(17) 0.0267(9) Uani 1 1 d . . . C10 C 0.9940(3) 0.5483(4) 0.1854(2) 0.0352(11) Uani 1 1 d . . . H10C H 1.0017 0.4882 0.2054 0.042 Uiso 1 1 calc R . . C11 C 1.0543(4) 0.6313(5) 0.1933(2) 0.0410(13) Uani 1 1 d . . . H11B H 1.1019 0.6276 0.2189 0.049 Uiso 1 1 calc R . . C12 C 1.0447(4) 0.7200(5) 0.1634(2) 0.0389(12) Uani 1 1 d . . . H12C H 1.0877 0.7744 0.1679 0.047 Uiso 1 1 calc R . . C13 C 0.9714(3) 0.7287(4) 0.1269(2) 0.0324(11) Uani 1 1 d . . . H13B H 0.9650 0.7896 0.1073 0.039 Uiso 1 1 calc R . . C14 C 0.8652(3) 0.4574(4) 0.13558(17) 0.0253(9) Uani 1 1 d . . . C15 C 0.5359(3) 0.1724(4) 0.11743(19) 0.0303(10) Uani 1 1 d . . . C16 C 0.4405(3) 0.2033(4) 0.11146(17) 0.0271(9) Uani 1 1 d . . . C17 C 0.3721(3) 0.1461(4) 0.13612(19) 0.0315(10) Uani 1 1 d . . . H17A H 0.3097 0.1673 0.1326 0.038 Uiso 1 1 calc R . . C18 C 0.3945(4) 0.0589(4) 0.1655(2) 0.0366(12) Uani 1 1 d . . . H18A H 0.3478 0.0220 0.1817 0.044 Uiso 1 1 calc R . . C19 C 0.4875(4) 0.0270(4) 0.1706(2) 0.0383(12) Uani 1 1 d . . . H19A H 0.5034 -0.0325 0.1898 0.046 Uiso 1 1 calc R . . C20 C 0.5565(4) 0.0833(4) 0.1473(2) 0.0359(11) Uani 1 1 d . . . H20A H 0.6187 0.0614 0.1515 0.043 Uiso 1 1 calc R . . C21 C 0.4110(3) 0.2943(4) 0.07924(17) 0.0255(9) Uani 1 1 d . . . C22 C 0.8525(3) 0.4884(4) -0.00338(19) 0.0302(10) Uani 1 1 d . . . H22A H 0.8646 0.4239 0.0155 0.036 Uiso 1 1 calc R . . H22B H 0.8938 0.5420 0.0114 0.036 Uiso 1 1 calc R . . C23 C 0.8746(4) 0.4722(5) -0.0583(2) 0.0418(13) Uani 1 1 d . . . H23A H 0.9392 0.4518 -0.0603 0.063 Uiso 1 1 calc R . . H23B H 0.8640 0.5363 -0.0770 0.063 Uiso 1 1 calc R . . H23C H 0.8348 0.4182 -0.0729 0.063 Uiso 1 1 calc R . . C24 C 0.4396(4) 0.6820(5) 0.1541(2) 0.0425(13) Uani 1 1 d . . . H24A H 0.4878 0.7307 0.1515 0.051 Uiso 1 1 calc R . . C25 C 0.3213(5) 0.5984(5) 0.1829(3) 0.0549(17) Uani 1 1 d . . . H25A H 0.2728 0.5770 0.2033 0.066 Uiso 1 1 calc R . . C26 C 0.3430(4) 0.5575(5) 0.1374(2) 0.0394(12) Uani 1 1 d . . . H26A H 0.3115 0.5022 0.1209 0.047 Uiso 1 1 calc R . . C27 C 0.6969(4) 0.6086(5) 0.2114(2) 0.0391(12) Uani 1 1 d . . . H27A H 0.7147 0.5391 0.2165 0.047 Uiso 1 1 calc R . . C28 C 0.6509(4) 0.7677(5) 0.2268(2) 0.0473(15) Uani 1 1 d . . . H28A H 0.6311 0.8280 0.2432 0.057 Uiso 1 1 calc R . . C29 C 0.6652(4) 0.7559(5) 0.1763(2) 0.0432(13) Uani 1 1 d . . . H29A H 0.6570 0.8084 0.1517 0.052 Uiso 1 1 calc R . . C30 C 0.5279(4) 0.4278(6) 0.2019(2) 0.0565(18) Uani 1 1 d . . . H30A H 0.4813 0.4727 0.1887 0.068 Uiso 1 1 calc R . . C31 C 0.6120(5) 0.3331(7) 0.2559(2) 0.061(2) Uani 1 1 d . . . H31A H 0.6350 0.3003 0.2859 0.074 Uiso 1 1 calc R . . C32 C 0.6432(4) 0.3216(5) 0.2085(2) 0.0467(14) Uani 1 1 d . . . H32A H 0.6935 0.2794 0.1999 0.056 Uiso 1 1 calc R . . C33 C 0.9076(5) 0.8626(5) -0.0039(3) 0.0528(16) Uani 1 1 d . . . H33A H 0.9361 0.8921 0.0274 0.063 Uiso 1 1 calc R . . H33B H 0.9037 0.9179 -0.0296 0.063 Uiso 1 1 calc R . . C34 C 0.9682(5) 0.7784(6) -0.0222(3) 0.0599(18) Uani 1 1 d . . . H34A H 1.0293 0.8062 -0.0286 0.090 Uiso 1 1 calc R . . H34B H 0.9409 0.7494 -0.0535 0.090 Uiso 1 1 calc R . . H34C H 0.9741 0.7244 0.0035 0.090 Uiso 1 1 calc R . . C35 C 0.8131(7) 0.0718(8) 0.1040(3) 0.092(3) Uani 1 1 d . . . H35A H 0.8750 0.0828 0.0907 0.111 Uiso 1 1 calc R . . H35B H 0.7677 0.0705 0.0750 0.111 Uiso 1 1 calc R . . C36 C 0.8112(6) -0.0292(7) 0.1314(5) 0.106(4) Uani 1 1 d . . . H36A H 0.8262 -0.0848 0.1082 0.158 Uiso 1 1 calc R . . H36B H 0.7496 -0.0406 0.1440 0.158 Uiso 1 1 calc R . . H36C H 0.8566 -0.0281 0.1598 0.158 Uiso 1 1 calc R . . C37 C 0.1768(4) 0.3456(6) 0.1947(3) 0.0600(19) Uani 1 1 d . . . H37A H 0.1712 0.4213 0.1962 0.072 Uiso 1 1 calc R . . H37B H 0.1856 0.3268 0.1590 0.072 Uiso 1 1 calc R . . C38 C 0.2604(5) 0.3143(7) 0.2253(3) 0.0633(19) Uani 1 1 d . . . H38A H 0.3147 0.3481 0.2123 0.095 Uiso 1 1 calc R . . H38B H 0.2680 0.2396 0.2234 0.095 Uiso 1 1 calc R . . H38C H 0.2535 0.3344 0.2606 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0210(3) 0.0259(4) 0.0244(4) -0.0020(3) -0.0034(2) -0.0001(3) Mn2 0.0213(3) 0.0294(4) 0.0257(4) -0.0009(3) -0.0040(3) -0.0006(3) Mn3 0.0222(3) 0.0278(4) 0.0279(4) 0.0020(3) -0.0036(3) -0.0003(3) Cl1 0.0666(11) 0.0609(11) 0.0577(10) 0.0097(8) 0.0023(8) -0.0058(8) O1 0.0216(15) 0.0279(17) 0.0231(16) -0.0005(12) -0.0047(12) -0.0002(12) O2 0.0219(15) 0.0286(18) 0.0271(17) -0.0033(13) -0.0036(12) 0.0011(12) O3 0.0178(14) 0.0267(17) 0.0319(17) 0.0016(13) -0.0046(12) -0.0002(12) O4 0.0223(15) 0.0300(18) 0.0264(16) 0.0015(13) -0.0051(12) -0.0019(13) O5 0.0214(15) 0.0264(17) 0.0361(18) 0.0012(13) -0.0041(13) -0.0015(13) O6 0.0231(15) 0.0282(18) 0.0370(19) 0.0055(14) -0.0019(13) -0.0007(13) O7 0.0212(14) 0.0229(16) 0.0252(16) 0.0013(12) -0.0036(12) 0.0008(12) O8 0.0190(14) 0.0295(18) 0.0266(16) -0.0005(13) -0.0026(12) 0.0018(12) O9 0.039(2) 0.049(3) 0.070(3) 0.022(2) -0.008(2) -0.0093(19) O10 0.037(2) 0.037(2) 0.055(3) 0.0080(18) -0.0092(17) 0.0052(16) O11 0.051(2) 0.050(3) 0.070(3) 0.015(2) 0.001(2) 0.002(2) O12 0.246(12) 0.141(8) 0.102(6) 0.029(6) -0.062(7) 0.046(8) O13 0.097(5) 0.157(7) 0.115(6) -0.054(5) 0.046(5) -0.024(5) O14 0.095(4) 0.073(4) 0.100(5) -0.016(3) 0.000(4) -0.024(3) O15 0.062(3) 0.100(5) 0.097(5) 0.010(4) -0.002(3) -0.039(3) N1 0.0217(17) 0.025(2) 0.0257(19) -0.0028(15) -0.0036(14) 0.0014(14) N2 0.031(2) 0.024(2) 0.056(3) 0.0073(19) -0.0092(19) -0.0005(17) N3 0.0248(18) 0.026(2) 0.0235(19) 0.0006(15) -0.0037(14) 0.0003(15) N4 0.0237(19) 0.034(2) 0.046(3) 0.0092(19) -0.0115(17) -0.0033(17) N5 0.0256(18) 0.027(2) 0.0198(18) 0.0023(14) -0.0013(14) -0.0010(15) N6 0.0221(18) 0.029(2) 0.036(2) 0.0037(17) -0.0021(16) -0.0026(16) N7 0.0246(19) 0.034(2) 0.033(2) -0.0021(17) -0.0010(16) 0.0000(16) N8 0.060(3) 0.050(3) 0.053(3) -0.024(3) 0.021(3) -0.016(3) N9 0.0252(19) 0.039(2) 0.031(2) -0.0106(18) -0.0050(16) -0.0035(17) N10 0.043(2) 0.054(3) 0.027(2) -0.010(2) -0.0023(19) -0.007(2) N11 0.030(2) 0.038(2) 0.0218(19) 0.0035(16) -0.0059(15) -0.0047(17) N12 0.070(4) 0.155(7) 0.025(3) 0.008(3) 0.009(3) 0.042(4) C1 0.028(2) 0.023(2) 0.023(2) -0.0004(17) -0.0027(17) 0.0034(17) C2 0.026(2) 0.027(2) 0.029(2) 0.0008(18) -0.0045(18) 0.0054(18) C3 0.037(3) 0.026(3) 0.041(3) -0.004(2) -0.009(2) 0.001(2) C4 0.040(3) 0.029(3) 0.047(3) -0.009(2) -0.006(2) 0.008(2) C5 0.031(2) 0.034(3) 0.047(3) -0.005(2) -0.006(2) 0.008(2) C6 0.027(2) 0.028(3) 0.045(3) -0.002(2) -0.007(2) 0.0027(19) C7 0.027(2) 0.027(2) 0.029(2) -0.0041(18) -0.0055(18) -0.0043(18) C8 0.021(2) 0.037(3) 0.025(2) -0.0046(19) 0.0013(17) -0.0002(18) C9 0.021(2) 0.036(3) 0.022(2) -0.0029(18) -0.0032(16) 0.0007(18) C10 0.030(2) 0.042(3) 0.032(3) 0.004(2) -0.009(2) 0.002(2) C11 0.034(3) 0.053(4) 0.035(3) -0.003(2) -0.015(2) -0.002(2) C12 0.028(2) 0.042(3) 0.046(3) -0.008(2) -0.009(2) -0.005(2) C13 0.027(2) 0.036(3) 0.035(3) -0.003(2) -0.0016(19) -0.001(2) C14 0.023(2) 0.033(3) 0.021(2) 0.0014(18) -0.0024(16) -0.0018(18) C15 0.029(2) 0.030(3) 0.032(3) 0.0009(19) -0.0051(19) -0.0017(19) C16 0.029(2) 0.032(3) 0.020(2) -0.0035(18) -0.0028(17) -0.0005(19) C17 0.028(2) 0.033(3) 0.033(3) -0.004(2) -0.0017(19) -0.0037(19) C18 0.048(3) 0.032(3) 0.030(3) 0.002(2) 0.001(2) -0.011(2) C19 0.049(3) 0.032(3) 0.033(3) 0.007(2) -0.008(2) -0.008(2) C20 0.033(3) 0.036(3) 0.038(3) 0.003(2) -0.006(2) -0.001(2) C21 0.022(2) 0.032(3) 0.022(2) -0.0029(18) -0.0018(16) 0.0016(18) C22 0.023(2) 0.034(3) 0.033(3) -0.001(2) 0.0004(18) 0.0012(19) C23 0.032(3) 0.061(4) 0.033(3) -0.006(2) 0.006(2) 0.006(2) C24 0.043(3) 0.045(3) 0.040(3) -0.012(2) 0.012(2) -0.010(2) C25 0.048(3) 0.058(4) 0.061(4) -0.015(3) 0.027(3) -0.012(3) C26 0.032(3) 0.048(3) 0.038(3) -0.004(2) 0.005(2) -0.006(2) C27 0.045(3) 0.045(3) 0.027(3) -0.010(2) -0.006(2) -0.001(2) C28 0.047(3) 0.053(4) 0.041(3) -0.022(3) -0.010(2) 0.008(3) C29 0.046(3) 0.041(3) 0.042(3) -0.011(2) -0.012(2) 0.002(2) C30 0.042(3) 0.091(5) 0.037(3) 0.001(3) 0.000(3) 0.021(3) C31 0.047(3) 0.103(6) 0.034(3) 0.017(3) -0.002(3) 0.009(4) C32 0.047(3) 0.061(4) 0.032(3) 0.005(3) -0.014(2) 0.009(3) C33 0.052(3) 0.049(4) 0.056(4) 0.015(3) -0.009(3) -0.017(3) C34 0.049(4) 0.068(5) 0.063(4) 0.014(4) -0.002(3) -0.009(3) C35 0.117(7) 0.113(8) 0.049(4) 0.023(4) 0.023(5) 0.074(6) C36 0.066(5) 0.056(6) 0.195(13) -0.032(7) 0.010(6) 0.002(4) C37 0.035(3) 0.063(5) 0.083(5) 0.020(4) 0.008(3) 0.011(3) C38 0.047(4) 0.078(5) 0.066(5) 0.007(4) 0.005(3) -0.007(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 O1 1.886(3) . ? Mn1 O2 1.937(3) . ? Mn1 O7 1.938(3) . ? Mn1 N1 1.980(4) . ? Mn1 N7 2.226(4) . ? Mn1 O7 2.397(3) 3_665 ? Mn1 Mn1 3.2327(14) 3_665 ? Mn2 O3 1.892(3) . ? Mn2 O1 1.893(3) . ? Mn2 O4 1.900(3) . ? Mn2 N3 1.978(4) . ? Mn2 N9 2.277(4) . ? Mn2 O8 2.445(3) . ? Mn3 O1 1.888(3) . ? Mn3 O6 1.902(3) . ? Mn3 O5 1.902(3) . ? Mn3 N5 1.972(4) . ? Mn3 N11 2.220(4) . ? Cl1 O15 1.403(6) . ? Cl1 O12 1.405(8) . ? Cl1 O13 1.439(7) . ? Cl1 O14 1.454(6) . ? O2 C1 1.357(6) . ? O3 N1 1.392(5) . ? O4 C8 1.337(6) . ? O5 N3 1.392(5) . ? O6 C15 1.334(6) . ? O7 N5 1.409(5) . ? O7 Mn1 2.397(3) 3_665 ? O8 C22 1.446(5) . ? O9 C33 1.432(7) . ? O9 H9A 0.8200 . ? O10 C35 1.469(9) . ? O10 H10A 0.8200 . ? O11 C37 1.391(7) . ? O11 H11A 0.8200 . ? N1 C7 1.303(6) . ? N2 C7 1.341(6) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C14 1.311(6) . ? N4 C14 1.334(6) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 C21 1.302(6) . ? N6 C21 1.346(6) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? N7 C24 1.323(7) . ? N7 C26 1.377(6) . ? N8 C24 1.325(7) . ? N8 C25 1.362(8) . ? N8 H8A 0.8600 . ? N9 C27 1.319(7) . ? N9 C29 1.360(7) . ? N10 C27 1.344(7) . ? N10 C28 1.356(8) . ? N10 H10B 0.8600 . ? N11 C30 1.296(7) . ? N11 C32 1.379(7) . ? N12 C30 1.331(8) . ? N12 C31 1.357(9) . ? N12 H12B 0.8600 . ? C1 C6 1.385(6) . ? C1 C2 1.423(7) . ? C2 C3 1.388(7) . ? C2 C7 1.476(6) . ? C3 C4 1.385(7) . ? C3 H3A 0.9300 . ? C4 C5 1.392(8) . ? C4 H4C 0.9300 . ? C5 C6 1.381(7) . ? C5 H5A 0.9300 . ? C6 H6C 0.9300 . ? C8 C9 1.401(7) . ? C8 C13 1.406(7) . ? C9 C10 1.419(6) . ? C9 C14 1.476(7) . ? C10 C11 1.373(8) . ? C10 H10C 0.9300 . ? C11 C12 1.375(8) . ? C11 H11B 0.9300 . ? C12 C13 1.385(7) . ? C12 H12C 0.9300 . ? C13 H13B 0.9300 . ? C15 C20 1.401(7) . ? C15 C16 1.416(7) . ? C16 C17 1.394(7) . ? C16 C21 1.482(7) . ? C17 C18 1.379(7) . ? C17 H17A 0.9300 . ? C18 C19 1.385(8) . ? C18 H18A 0.9300 . ? C19 C20 1.377(7) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C22 C23 1.489(7) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9300 . ? C25 C26 1.339(8) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 C29 1.343(8) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C32 1.335(9) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.471(10) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.474(13) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.459(9) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 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 O1 Mn1 O2 172.57(14) . . ? O1 Mn1 O7 90.02(13) . . ? O2 Mn1 O7 91.10(13) . . ? O1 Mn1 N1 87.95(14) . . ? O2 Mn1 N1 89.88(15) . . ? O7 Mn1 N1 171.55(14) . . ? O1 Mn1 N7 98.08(14) . . ? O2 Mn1 N7 89.18(14) . . ? O7 Mn1 N7 93.56(14) . . ? N1 Mn1 N7 94.84(15) . . ? O1 Mn1 O7 88.58(12) . 3_665 ? O2 Mn1 O7 84.23(12) . 3_665 ? O7 Mn1 O7 84.13(12) . 3_665 ? N1 Mn1 O7 87.62(13) . 3_665 ? N7 Mn1 O7 172.96(13) . 3_665 ? O1 Mn1 Mn1 88.96(10) . 3_665 ? O2 Mn1 Mn1 86.38(10) . 3_665 ? O7 Mn1 Mn1 47.52(9) . 3_665 ? N1 Mn1 Mn1 124.21(11) . 3_665 ? N7 Mn1 Mn1 140.62(11) . 3_665 ? O7 Mn1 Mn1 36.61(8) 3_665 3_665 ? O3 Mn2 O1 91.50(13) . . ? O3 Mn2 O4 88.31(14) . . ? O1 Mn2 O4 170.53(14) . . ? O3 Mn2 N3 174.58(15) . . ? O1 Mn2 N3 89.73(15) . . ? O4 Mn2 N3 89.61(15) . . ? O3 Mn2 N9 91.66(15) . . ? O1 Mn2 N9 97.04(14) . . ? O4 Mn2 N9 92.43(14) . . ? N3 Mn2 N9 93.44(16) . . ? O3 Mn2 O8 91.85(13) . . ? O1 Mn2 O8 85.48(12) . . ? O4 Mn2 O8 85.06(12) . . ? N3 Mn2 O8 82.98(13) . . ? N9 Mn2 O8 175.63(13) . . ? O1 Mn3 O6 174.92(15) . . ? O1 Mn3 O5 92.78(14) . . ? O6 Mn3 O5 89.01(14) . . ? O1 Mn3 N5 87.95(15) . . ? O6 Mn3 N5 89.59(15) . . ? O5 Mn3 N5 171.55(15) . . ? O1 Mn3 N11 96.24(15) . . ? O6 Mn3 N11 88.43(16) . . ? O5 Mn3 N11 92.32(15) . . ? N5 Mn3 N11 95.97(15) . . ? O15 Cl1 O12 113.5(6) . . ? O15 Cl1 O13 107.0(5) . . ? O12 Cl1 O13 108.4(6) . . ? O15 Cl1 O14 109.0(4) . . ? O12 Cl1 O14 109.3(5) . . ? O13 Cl1 O14 109.6(4) . . ? Mn1 O1 Mn3 120.86(16) . . ? Mn1 O1 Mn2 120.37(17) . . ? Mn3 O1 Mn2 118.01(16) . . ? C1 O2 Mn1 119.7(3) . . ? N1 O3 Mn2 116.7(2) . . ? C8 O4 Mn2 123.5(3) . . ? N3 O5 Mn3 115.1(2) . . ? C15 O6 Mn3 121.6(3) . . ? N5 O7 Mn1 113.8(2) . . ? N5 O7 Mn1 110.9(2) . 3_665 ? Mn1 O7 Mn1 95.87(12) . 3_665 ? C22 O8 Mn2 116.5(3) . . ? C33 O9 H9A 109.5 . . ? C35 O10 H10A 109.5 . . ? C37 O11 H11A 109.5 . . ? C7 N1 O3 113.3(4) . . ? C7 N1 Mn1 127.7(3) . . ? O3 N1 Mn1 118.2(3) . . ? C7 N2 H2A 120.0 . . ? C7 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C14 N3 O5 114.8(4) . . ? C14 N3 Mn2 127.6(3) . . ? O5 N3 Mn2 116.7(3) . . ? C14 N4 H4A 120.0 . . ? C14 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C21 N5 O7 114.8(4) . . ? C21 N5 Mn3 128.3(3) . . ? O7 N5 Mn3 115.9(3) . . ? C21 N6 H6A 120.0 . . ? C21 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C24 N7 C26 104.3(4) . . ? C24 N7 Mn1 126.0(3) . . ? C26 N7 Mn1 129.6(4) . . ? C24 N8 C25 106.6(5) . . ? C24 N8 H8A 126.7 . . ? C25 N8 H8A 126.7 . . ? C27 N9 C29 105.2(5) . . ? C27 N9 Mn2 130.3(4) . . ? C29 N9 Mn2 124.4(4) . . ? C27 N10 C28 107.3(5) . . ? C27 N10 H10B 126.3 . . ? C28 N10 H10B 126.3 . . ? C30 N11 C32 105.5(5) . . ? C30 N11 Mn3 132.7(4) . . ? C32 N11 Mn3 121.3(4) . . ? C30 N12 C31 107.8(6) . . ? C30 N12 H12B 126.1 . . ? C31 N12 H12B 126.1 . . ? O2 C1 C6 118.5(4) . . ? O2 C1 C2 123.0(4) . . ? C6 C1 C2 118.4(4) . . ? C3 C2 C1 118.9(4) . . ? C3 C2 C7 119.1(4) . . ? C1 C2 C7 122.0(4) . . ? C4 C3 C2 121.9(5) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C3 C4 C5 118.9(5) . . ? C3 C4 H4C 120.5 . . ? C5 C4 H4C 120.5 . . ? C6 C5 C4 120.1(5) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C1 121.8(5) . . ? C5 C6 H6C 119.1 . . ? C1 C6 H6C 119.1 . . ? N1 C7 N2 119.1(4) . . ? N1 C7 C2 120.2(4) . . ? N2 C7 C2 120.7(4) . . ? O4 C8 C9 123.5(4) . . ? O4 C8 C13 117.6(4) . . ? C9 C8 C13 118.9(4) . . ? C8 C9 C10 119.0(5) . . ? C8 C9 C14 122.6(4) . . ? C10 C9 C14 118.2(4) . . ? C11 C10 C9 120.6(5) . . ? C11 C10 H10C 119.7 . . ? C9 C10 H10C 119.7 . . ? C10 C11 C12 120.3(5) . . ? C10 C11 H11B 119.9 . . ? C12 C11 H11B 119.9 . . ? C11 C12 C13 120.5(5) . . ? C11 C12 H12C 119.7 . . ? C13 C12 H12C 119.7 . . ? C12 C13 C8 120.6(5) . . ? C12 C13 H13B 119.7 . . ? C8 C13 H13B 119.7 . . ? N3 C14 N4 119.8(4) . . ? N3 C14 C9 119.5(4) . . ? N4 C14 C9 120.7(4) . . ? O6 C15 C20 118.5(4) . . ? O6 C15 C16 123.9(4) . . ? C20 C15 C16 117.6(4) . . ? C17 C16 C15 119.3(5) . . ? C17 C16 C21 119.0(4) . . ? C15 C16 C21 121.8(4) . . ? C18 C17 C16 121.9(5) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 119.1(5) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C20 C19 C18 120.1(5) . . ? C20 C19 H19A 120.0 . . ? C18 C19 H19A 120.0 . . ? C19 C20 C15 122.0(5) . . ? C19 C20 H20A 119.0 . . ? C15 C20 H20A 119.0 . . ? N5 C21 N6 121.3(4) . . ? N5 C21 C16 119.4(4) . . ? N6 C21 C16 119.3(4) . . ? O8 C22 C23 112.5(4) . . ? O8 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? O8 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? 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 . . ? N7 C24 N8 112.4(5) . . ? N7 C24 H24A 123.8 . . ? N8 C24 H24A 123.8 . . ? C26 C25 N8 107.0(5) . . ? C26 C25 H25A 126.5 . . ? N8 C25 H25A 126.5 . . ? C25 C26 N7 109.6(5) . . ? C25 C26 H26A 125.2 . . ? N7 C26 H26A 125.2 . . ? N9 C27 N10 111.0(5) . . ? N9 C27 H27A 124.5 . . ? N10 C27 H27A 124.5 . . ? C29 C28 N10 106.1(5) . . ? C29 C28 H28A 126.9 . . ? N10 C28 H28A 126.9 . . ? C28 C29 N9 110.4(6) . . ? C28 C29 H29A 124.8 . . ? N9 C29 H29A 124.8 . . ? N11 C30 N12 111.2(6) . . ? N11 C30 H30A 124.4 . . ? N12 C30 H30A 124.4 . . ? C32 C31 N12 105.9(6) . . ? C32 C31 H31A 127.1 . . ? N12 C31 H31A 127.1 . . ? C31 C32 N11 109.5(6) . . ? C31 C32 H32A 125.2 . . ? N11 C32 H32A 125.2 . . ? O9 C33 C34 113.1(5) . . ? O9 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? O9 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O10 C35 C36 110.5(7) . . ? O10 C35 H35A 109.5 . . ? C36 C35 H35A 109.5 . . ? O10 C35 H35B 109.5 . . ? C36 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O11 C37 C38 115.0(6) . . ? O11 C37 H37A 108.5 . . ? C38 C37 H37A 108.5 . . ? O11 C37 H37B 108.5 . . ? C38 C37 H37B 108.5 . . ? H37A C37 H37B 107.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.56 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.894 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.112 _database_code_depnum_ccdc_archive 'CCDC 962812'