####################################################################### # # 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_a1 _database_code_depnum_ccdc_archive 'CCDC 886125' #TrackingRef '- 1(CCDC_886125).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H116 Cl2 Mn6 N6 O25 P8' _chemical_formula_weight 2066.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 'z, x, y' '-z+1/2, -x, y+1/2' 'z+1/2, -x+1/2, -y' '-z, x+1/2, -y+1/2' 'y, z, x' 'y+1/2, -z+1/2, -x' '-y, z+1/2, -x+1/2' '-y+1/2, -z, x+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' '-z, -x, -y' 'z-1/2, x, -y-1/2' '-z-1/2, x-1/2, y' 'z, -x-1/2, y-1/2' '-y, -z, -x' '-y-1/2, z-1/2, x' 'y, -z-1/2, x-1/2' 'y-1/2, z, -x-1/2' _cell_length_a 21.244(2) _cell_length_b 21.244(2) _cell_length_c 21.244(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9587.6(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4223 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 27.64 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4279 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.874 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details '(SADABS; Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _diffrn_measurement_method w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53895 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2822 _reflns_number_gt 2664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; L.S. 5 FMAP 2 PLAN 20 ACTA BOND $H omit -2 50 omit 9 3 11 omit 4 4 7 omit 5 4 10 omit 4 1 12 omit 5 3 8 omit 4 3 11 omit 6 6 6 simu 0.01 mn1 p1 o1 delu 0.01 mn1 p1 o1 WGHT 0.000000 200.286499 FVAR 0.12489 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^)+(0.0000P)^2^+200.2865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2822 _refine_ls_number_parameters 176 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0934 _refine_ls_wR_factor_ref 0.2019 _refine_ls_wR_factor_gt 0.2004 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.102 _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 0.52752(5) 0.46481(5) 0.36066(5) 0.0190(3) Uani 1 1 d U . . P1 P 0.44795(9) 0.59115(9) 0.36036(9) 0.0198(4) Uani 1 1 d U . . P2 P 0.39852(9) 0.39852(9) 0.39852(9) 0.0188(7) Uani 1 3 d S . . Cl1 Cl 0.0000 0.0000 0.5000 0.0252(10) Uani 1 6 d S . . Cl2 Cl 0.0000 0.0000 0.0000 0.0614(18) Uani 1 6 d S . . O1 O 0.4838(4) 0.5361(4) 0.3354(3) 0.067(2) Uani 1 1 d U . . O1W O 0.0832(13) 0.0832(13) 0.0832(13) 0.18(2) Uani 0.50 3 d SP . . O2 O 0.4882(4) 0.6330(3) 0.3983(4) 0.073(3) Uani 1 1 d . . . O3 O 0.3899(3) 0.5717(4) 0.3945(3) 0.058(2) Uani 1 1 d . . . O4 O 0.4526(3) 0.4190(4) 0.3586(3) 0.064(3) Uani 1 1 d . . . C1 C 0.5766(6) 0.3866(5) 0.1438(5) 0.048(3) Uani 1 1 d . . . C3 C 0.5201(5) 0.4168(6) 0.1563(5) 0.061(3) Uani 1 1 d . . . H3A H 0.4901 0.4219 0.1249 0.073 Uiso 1 1 calc R . . C6 C 0.4231(4) 0.6378(4) 0.2925(4) 0.0236(17) Uani 1 1 d . . . C14 C 0.6194(6) 0.3847(6) 0.1917(5) 0.059(3) Uani 1 1 d . . . H14A H 0.6586 0.3665 0.1850 0.071 Uiso 1 1 calc R . . C16 C 0.5897(7) 0.3594(6) 0.0790(6) 0.075(4) Uani 1 1 d . . . H16A H 0.6306 0.3402 0.0787 0.113 Uiso 1 1 calc R . . H16B H 0.5884 0.3924 0.0482 0.113 Uiso 1 1 calc R . . H16C H 0.5584 0.3283 0.0691 0.113 Uiso 1 1 calc R . . C29 C 0.3856(8) 0.6930(6) 0.3142(6) 0.096(6) Uani 1 1 d . . . H29A H 0.3725 0.7174 0.2785 0.143 Uiso 1 1 calc R . . H29B H 0.4109 0.7186 0.3415 0.143 Uiso 1 1 calc R . . H29C H 0.3491 0.6785 0.3367 0.143 Uiso 1 1 calc R . . C30 C 0.3841(10) 0.5976(6) 0.2498(7) 0.132(9) Uani 1 1 d . . . H30A H 0.3710 0.6220 0.2141 0.198 Uiso 1 1 calc R . . H30B H 0.3477 0.5828 0.2722 0.198 Uiso 1 1 calc R . . H30C H 0.4086 0.5624 0.2358 0.198 Uiso 1 1 calc R . . C33 C 0.6050(5) 0.4091(6) 0.2493(5) 0.053(3) Uani 1 1 d . . . H33A H 0.6348 0.4063 0.2812 0.063 Uiso 1 1 calc R . . C41 C 0.3234(5) 0.3884(5) 0.2948(5) 0.052(3) Uani 1 1 d . . . H41A H 0.2972 0.3625 0.2686 0.078 Uiso 1 1 calc R . . H41B H 0.3577 0.4047 0.2704 0.078 Uiso 1 1 calc R . . H41C H 0.2989 0.4227 0.3113 0.078 Uiso 1 1 calc R . . C44 C 0.5094(5) 0.4392(5) 0.2167(4) 0.047(3) Uani 1 1 d . . . H44A H 0.4704 0.4571 0.2252 0.057 Uiso 1 1 calc R . . C83 C 0.4793(6) 0.6598(8) 0.2579(7) 0.115(8) Uani 1 1 d . . . H83A H 0.4664 0.6842 0.2222 0.172 Uiso 1 1 calc R . . H83B H 0.5032 0.6241 0.2439 0.172 Uiso 1 1 calc R . . H83C H 0.5048 0.6852 0.2852 0.172 Uiso 1 1 calc R . . C93 C 0.3491(3) 0.3491(3) 0.3491(3) 0.026(3) Uani 1 3 d S . . N1 N 0.5498(3) 0.4371(3) 0.2620(3) 0.0266(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0190(6) 0.0184(6) 0.0198(6) 0.0007(5) 0.0014(4) 0.0008(4) P1 0.0205(10) 0.0207(10) 0.0183(9) 0.0029(8) -0.0001(8) 0.0029(8) P2 0.0188(7) 0.0188(7) 0.0188(7) -0.0013(8) -0.0013(8) -0.0013(8) Cl1 0.0252(10) 0.0252(10) 0.0252(10) 0.0015(11) -0.0015(11) -0.0015(11) Cl2 0.0614(18) 0.0614(18) 0.0614(18) 0.005(2) 0.005(2) 0.005(2) O1 0.115(6) 0.062(4) 0.026(3) 0.011(3) 0.016(4) 0.061(4) O1W 0.18(2) 0.18(2) 0.18(2) -0.05(2) -0.05(2) -0.05(2) O2 0.108(7) 0.045(4) 0.068(5) 0.036(4) -0.064(5) -0.047(5) O3 0.019(3) 0.091(6) 0.063(5) 0.061(5) -0.001(3) -0.001(3) O4 0.043(4) 0.123(7) 0.027(3) -0.029(4) 0.010(3) -0.051(5) C1 0.067(7) 0.031(5) 0.045(6) -0.009(4) 0.015(5) -0.001(5) C3 0.047(6) 0.095(10) 0.042(6) -0.019(6) -0.002(5) -0.008(6) C6 0.025(4) 0.027(4) 0.019(4) 0.005(3) -0.005(3) 0.001(3) C14 0.062(7) 0.073(8) 0.042(6) 0.012(6) 0.021(5) 0.038(6) C16 0.094(10) 0.073(9) 0.058(8) -0.039(7) 0.020(7) -0.010(8) C29 0.156(15) 0.085(10) 0.046(7) 0.025(7) 0.018(8) 0.099(11) C30 0.25(2) 0.065(9) 0.080(10) 0.028(8) -0.122(14) -0.061(12) C33 0.046(6) 0.078(8) 0.035(5) 0.008(5) 0.001(5) 0.028(6) C41 0.054(6) 0.054(7) 0.047(6) 0.004(5) -0.031(5) -0.015(5) C44 0.036(5) 0.072(7) 0.035(5) -0.023(5) -0.002(4) 0.006(5) C83 0.051(8) 0.192(18) 0.100(11) 0.124(12) 0.035(7) 0.044(9) C93 0.026(3) 0.026(3) 0.026(3) -0.007(3) -0.007(3) -0.007(3) N1 0.031(4) 0.024(3) 0.025(4) 0.000(3) 0.003(3) 0.002(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 1.856(7) . ? Mn1 O4 1.867(6) . ? Mn1 O2 1.870(7) 17_666 ? Mn1 O3 1.871(6) 9 ? Mn1 N1 2.228(7) . ? P1 O2 1.474(7) . ? P1 O3 1.488(6) . ? P1 O1 1.493(7) . ? P1 C6 1.827(8) . ? P2 O4 1.492(6) 9 ? P2 O4 1.492(6) 5 ? P2 O4 1.492(6) . ? P2 C93 1.818(13) . ? O2 Mn1 1.870(7) 21_666 ? O3 Mn1 1.871(6) 5 ? C1 C14 1.364(16) . ? C1 C3 1.387(15) . ? C1 C16 1.518(14) . ? C3 C44 1.389(14) . ? C3 H3A 0.9300 . ? C6 C83 1.478(13) . ? C6 C29 1.490(13) . ? C6 C30 1.495(14) . ? C14 C33 1.365(15) . ? C14 H14A 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 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 . ? C33 N1 1.342(12) . ? C33 H33A 0.9300 . ? C41 C93 1.525(10) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C44 N1 1.289(11) . ? C44 H44A 0.9300 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C93 C41 1.525(10) 9 ? C93 C41 1.525(10) 5 ? 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 O4 89.5(4) . . ? O1 Mn1 O2 90.4(5) . 17_666 ? O4 Mn1 O2 177.1(3) . 17_666 ? O1 Mn1 O3 177.3(3) . 9 ? O4 Mn1 O3 91.1(4) . 9 ? O2 Mn1 O3 88.9(4) 17_666 9 ? O1 Mn1 N1 92.9(3) . . ? O4 Mn1 N1 91.2(3) . . ? O2 Mn1 N1 91.7(3) 17_666 . ? O3 Mn1 N1 89.7(3) 9 . ? O2 P1 O3 112.4(5) . . ? O2 P1 O1 111.8(6) . . ? O3 P1 O1 112.2(5) . . ? O2 P1 C6 105.8(4) . . ? O3 P1 C6 107.2(4) . . ? O1 P1 C6 107.0(4) . . ? O4 P2 O4 112.2(2) 9 5 ? O4 P2 O4 112.2(2) 9 . ? O4 P2 O4 112.2(2) 5 . ? O4 P2 C93 106.5(3) 9 . ? O4 P2 C93 106.5(3) 5 . ? O4 P2 C93 106.5(3) . . ? P1 O1 Mn1 142.3(4) . . ? P1 O2 Mn1 144.5(4) . 21_666 ? P1 O3 Mn1 143.5(4) . 5 ? P2 O4 Mn1 142.7(4) . . ? C14 C1 C3 116.6(9) . . ? C14 C1 C16 122.8(11) . . ? C3 C1 C16 120.6(11) . . ? C1 C3 C44 118.5(11) . . ? C1 C3 H3A 120.7 . . ? C44 C3 H3A 120.7 . . ? C83 C6 C29 109.7(11) . . ? C83 C6 C30 109.0(12) . . ? C29 C6 C30 109.9(12) . . ? C83 C6 P1 109.2(6) . . ? C29 C6 P1 109.7(6) . . ? C30 C6 P1 109.2(7) . . ? C1 C14 C33 120.6(10) . . ? C1 C14 H14A 119.7 . . ? C33 C14 H14A 119.7 . . ? C1 C16 H16A 109.5 . . ? C1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C6 C29 H29A 109.5 . . ? C6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C6 C30 H30A 109.5 . . ? C6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C33 C14 123.0(10) . . ? N1 C33 H33A 118.5 . . ? C14 C33 H33A 118.5 . . ? C93 C41 H41A 109.5 . . ? C93 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C93 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N1 C44 C3 124.7(10) . . ? N1 C44 H44A 117.7 . . ? C3 C44 H44A 117.7 . . ? C6 C83 H83A 109.5 . . ? C6 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C6 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C41 C93 C41 109.8(6) . 9 ? C41 C93 C41 109.8(6) . 5 ? C41 C93 C41 109.8(6) 9 5 ? C41 C93 P2 109.1(6) . . ? C41 C93 P2 109.1(6) 9 . ? C41 C93 P2 109.1(6) 5 . ? C44 N1 C33 116.6(8) . . ? C44 N1 Mn1 123.5(6) . . ? C33 N1 Mn1 119.4(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.115 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.148 data_a2 _database_code_depnum_ccdc_archive 'CCDC 886126' #TrackingRef '- 2(CCDC_886126).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H112 Cl5 Mn7 N6 O29 P8' _chemical_formula_weight 2215.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 '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/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.577(5) _cell_length_b 35.726(7) _cell_length_c 14.376(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.59(3) _cell_angle_gamma 90.00 _cell_volume 12269(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 27145 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 26.65 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4551 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_process_details '(SADABS; Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _diffrn_measurement_method w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 131252 _diffrn_reflns_av_R_equivalents 0.1023 _diffrn_reflns_av_sigmaI/netI 0.0770 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21598 _reflns_number_gt 14485 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; omit -2 50 omit 2 2 2 omit 0 3 1 omit -9 8 3 omit 0 2 0 omit 2 1 0 FMAP 2 PLAN 20 ACTA isor 0.01 cl8a isor 0.0001 cl7 isor 0.01 c39 BOND $H WGHT 0.300000 FVAR 1.00939 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^)+(0.3000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21598 _refine_ls_number_parameters 1103 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1451 _refine_ls_R_factor_gt 0.1093 _refine_ls_wR_factor_ref 0.3693 _refine_ls_wR_factor_gt 0.3338 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.983 _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 0.20996(5) 0.03600(3) 0.77401(8) 0.0198(3) Uani 1 1 d . . . Mn2 Mn 0.19720(5) 0.14859(3) 0.64404(8) 0.0185(3) Uani 1 1 d . . . Mn3 Mn 0.35970(5) 0.10506(3) 0.80240(8) 0.0219(3) Uani 1 1 d . . . Mn4 Mn 0.33741(5) 0.00470(3) 0.62055(8) 0.0247(3) Uani 1 1 d . . . Mn5 Mn 0.17396(6) 0.04857(3) 0.46049(9) 0.0278(3) Uani 1 1 d . . . Mn6 Mn 0.32553(5) 0.11667(3) 0.49163(8) 0.0250(3) Uani 1 1 d . . . P8 P 0.34037(9) 0.01889(6) 0.84093(14) 0.0227(5) Uani 1 1 d . . . P9 P 0.32329(8) 0.17385(6) 0.66029(14) 0.0218(5) Uani 1 1 d . . . P10 P 0.11558(8) 0.07836(6) 0.62071(15) 0.0240(5) Uani 1 1 d . . . P11 P 0.21160(9) -0.02028(6) 0.60272(14) 0.0246(5) Uani 1 1 d . . . P12 P 0.24227(8) 0.11793(5) 0.85540(13) 0.0202(4) Uani 1 1 d . . . P13 P 0.19559(9) 0.13483(6) 0.42495(14) 0.0253(5) Uani 1 1 d . . . P14 P 0.42019(9) 0.07441(6) 0.64476(16) 0.0280(5) Uani 1 1 d . . . P15 P 0.29077(11) 0.03506(6) 0.40820(15) 0.0320(6) Uani 1 1 d . . . O3 O 0.1218(2) 0.07073(15) 0.5206(4) 0.0274(13) Uani 1 1 d . . . O4 O 0.3397(2) -0.00393(15) 0.7508(4) 0.0252(12) Uani 1 1 d . . . O5 O 0.1720(2) 0.14737(15) 0.5094(4) 0.0217(12) Uani 1 1 d . . . O6 O 0.3431(2) 0.15427(15) 0.7560(4) 0.0263(12) Uani 1 1 d . . . O7 O 0.2073(2) 0.08213(14) 0.8359(4) 0.0209(11) Uani 1 1 d . . . O8 O 0.2233(2) 0.14742(14) 0.7779(3) 0.0215(12) Uani 1 1 d . . . O9 O 0.2140(2) -0.00863(15) 0.7062(4) 0.0251(12) Uani 1 1 d . . . O10 O 0.1370(2) 0.11729(14) 0.6555(4) 0.0204(11) Uani 1 1 d . . . O11 O 0.3911(2) 0.09051(16) 0.5468(4) 0.0294(13) Uani 1 1 d . . . O12 O 0.3019(2) 0.07758(15) 0.4039(4) 0.0293(13) Uani 1 1 d . . . O13 O 0.1798(3) 0.09396(16) 0.3965(4) 0.0327(14) Uani 1 1 d . . . O14 O 0.2819(2) 0.02633(15) 0.8546(4) 0.0250(12) Uani 1 1 d . . . O15 O 0.1409(2) 0.04735(14) 0.6895(4) 0.0241(12) Uani 1 1 d . . . O16 O 0.3311(3) 0.01629(17) 0.4912(4) 0.0341(15) Uani 1 1 d . . . O17 O 0.3045(2) 0.10965(14) 0.8738(4) 0.0223(12) Uani 1 1 d . . . O18 O 0.2599(2) 0.17748(14) 0.6321(4) 0.0215(11) Uani 1 1 d . . . O19 O 0.2701(2) -0.02259(15) 0.5839(4) 0.0268(13) Uani 1 1 d . . . O20 O 0.2300(3) 0.02742(16) 0.4074(4) 0.0331(14) Uani 1 1 d . . . O22 O 0.2580(2) 0.14192(15) 0.4421(4) 0.0264(12) Uani 1 1 d . . . O23 O 0.3741(2) 0.05505(15) 0.8452(4) 0.0260(12) Uani 1 1 d . . . O24 O 0.3473(2) 0.15600(15) 0.5825(4) 0.0256(12) Uani 1 1 d . . . O26 O 0.4032(2) 0.03418(16) 0.6564(4) 0.0301(13) Uani 1 1 d . . . O35 O 0.1721(2) 0.00399(15) 0.5305(4) 0.0293(13) Uani 1 1 d . . . O37 O 0.4128(2) 0.09966(16) 0.7278(4) 0.0284(13) Uani 1 1 d . . . N25 N 0.1440(3) 0.20005(18) 0.6452(5) 0.0268(16) Uani 1 1 d . . . N27 N 0.1719(3) 0.00435(19) 0.8779(5) 0.0270(15) Uani 1 1 d . . . N36 N 0.3869(4) -0.0479(2) 0.6139(6) 0.040(2) Uani 1 1 d . . . N39 N 0.4259(3) 0.1281(2) 0.9239(5) 0.0346(18) Uani 1 1 d . . . N40 N 0.3673(3) 0.1442(2) 0.3876(5) 0.0350(18) Uani 1 1 d . . . N45 N 0.1052(4) 0.0300(2) 0.3400(5) 0.043(2) Uani 1 1 d . . . C13 C 0.4215(4) 0.1629(3) 0.9566(7) 0.039(2) Uani 1 1 d . . . H13A H 0.3896 0.1767 0.9300 0.047 Uiso 1 1 calc R . . C14 C 0.4397(5) 0.1829(3) 0.3576(8) 0.052(3) Uani 1 1 d . . . H14A H 0.4682 0.2001 0.3793 0.062 Uiso 1 1 calc R . . C15 C 0.1088(5) -0.0015(3) 0.2902(7) 0.046(3) Uani 1 1 d . . . H15A H 0.1415 -0.0156 0.3066 0.055 Uiso 1 1 calc R . . C16 C 0.1263(4) -0.0669(4) 0.6152(9) 0.059(3) Uani 1 1 d . . . H16A H 0.1135 -0.0920 0.6198 0.089 Uiso 1 1 calc R . . H16B H 0.0996 -0.0536 0.5670 0.089 Uiso 1 1 calc R . . H16C H 0.1303 -0.0545 0.6757 0.089 Uiso 1 1 calc R . . C17 C 0.4256(5) 0.1720(3) 0.2600(8) 0.049(3) Uani 1 1 d . . . H17A H 0.4461 0.1809 0.2180 0.059 Uiso 1 1 calc R . . C18 C 0.0659(6) -0.0137(4) 0.2158(7) 0.057(3) Uani 1 1 d . . . H18A H 0.0693 -0.0356 0.1826 0.068 Uiso 1 1 calc R . . C21 C 0.4616(5) 0.1790(3) 1.0270(8) 0.055(3) Uani 1 1 d . . . H21A H 0.4580 0.2037 1.0450 0.066 Uiso 1 1 calc R . . C22 C 0.5115(5) 0.1226(4) 1.0396(9) 0.072(4) Uani 1 1 d . . . H22A H 0.5424 0.1077 1.0655 0.086 Uiso 1 1 calc R . . C23 C 0.5087(5) 0.1576(4) 1.0724(9) 0.066(3) Uani 1 1 d . . . H23A H 0.5364 0.1672 1.1223 0.079 Uiso 1 1 calc R . . C24 C 0.0578(5) 0.0497(3) 0.3140(7) 0.055(3) Uani 1 1 d . . . H24A H 0.0539 0.0713 0.3478 0.066 Uiso 1 1 calc R . . C25 C 0.1670(4) 0.1443(3) 0.9497(7) 0.042(2) Uani 1 1 d . . . H25A H 0.1601 0.1549 1.0072 0.063 Uiso 1 1 calc R . . H25B H 0.1471 0.1211 0.9360 0.063 Uiso 1 1 calc R . . H25C H 0.1544 0.1614 0.8975 0.063 Uiso 1 1 calc R . . C26 C 0.3828(5) 0.1489(3) 0.2292(7) 0.052(3) Uani 1 1 d . . . H26A H 0.3724 0.1423 0.1648 0.063 Uiso 1 1 calc R . . C27 C 0.1581(6) -0.0528(3) 0.9519(10) 0.076(4) Uani 1 1 d . . . H27A H 0.1632 -0.0786 0.9555 0.091 Uiso 1 1 calc R . . C28 C 0.0183(6) 0.0076(4) 0.1927(8) 0.069(4) Uani 1 1 d . . . H28A H -0.0116 -0.0001 0.1439 0.083 Uiso 1 1 calc R . . C29 C 0.1754(6) -0.0807(3) 0.4838(8) 0.066(4) Uani 1 1 d . . . H29A H 0.1665 -0.1069 0.4788 0.099 Uiso 1 1 calc R . . H29B H 0.2098 -0.0764 0.4649 0.099 Uiso 1 1 calc R . . H29C H 0.1458 -0.0668 0.4426 0.099 Uiso 1 1 calc R . . C30 C 0.3522(3) 0.2212(3) 0.6765(6) 0.032(2) Uani 1 1 d . . . C31 C 0.4378(5) -0.0518(3) 0.6690(8) 0.059(3) Uani 1 1 d . . . H31A H 0.4549 -0.0319 0.7066 0.071 Uiso 1 1 calc R . . C32 C 0.3626(5) -0.0766(3) 0.5567(10) 0.062(4) Uani 1 1 d . . . H32A H 0.3271 -0.0738 0.5168 0.075 Uiso 1 1 calc R . . C33 C 0.3841(5) 0.0143(4) 1.0330(7) 0.062(3) Uani 1 1 d . . . H33A H 0.4068 0.0008 1.0860 0.092 Uiso 1 1 calc R . . H33B H 0.3481 0.0192 1.0454 0.092 Uiso 1 1 calc R . . H33C H 0.4020 0.0375 1.0245 0.092 Uiso 1 1 calc R . . C34 C 0.3635(5) 0.0251(4) 0.2946(8) 0.067(4) Uani 1 1 d . . . H34A H 0.3708 0.0160 0.2359 0.100 Uiso 1 1 calc R . . H34B H 0.3894 0.0140 0.3479 0.100 Uiso 1 1 calc R . . H34C H 0.3677 0.0518 0.2975 0.100 Uiso 1 1 calc R . . C35 C 0.2623(6) 0.0320(3) 0.2137(7) 0.067(4) Uani 1 1 d . . . H35A H 0.2624 0.0178 0.1570 0.100 Uiso 1 1 calc R . . H35B H 0.2730 0.0574 0.2050 0.100 Uiso 1 1 calc R . . H35C H 0.2255 0.0317 0.2255 0.100 Uiso 1 1 calc R . . C36 C 0.1859(7) 0.1526(3) 0.2373(7) 0.077(5) Uani 1 1 d . . . H36A H 0.1672 0.1666 0.1820 0.116 Uiso 1 1 calc R . . H36B H 0.1799 0.1264 0.2250 0.116 Uiso 1 1 calc R . . H36C H 0.2253 0.1578 0.2509 0.116 Uiso 1 1 calc R . . C37 C 0.3921(8) -0.1107(3) 0.5589(17) 0.118(8) Uani 1 1 d . . . H37A H 0.3758 -0.1302 0.5192 0.141 Uiso 1 1 calc R . . C38 C 0.1626(4) 0.1639(2) 0.3236(6) 0.034(2) Uani 1 1 d . . . C39 C 0.4424(7) -0.1154(5) 0.6161(12) 0.084(4) Uani 1 1 d U . . H39A H 0.4610 -0.1382 0.6188 0.101 Uiso 1 1 calc R . . C40 C 0.4658(6) -0.0862(5) 0.6702(12) 0.088(5) Uani 1 1 d . . . H40A H 0.5015 -0.0889 0.7096 0.106 Uiso 1 1 calc R . . C41 C 0.1817(4) -0.0676(2) 0.5888(6) 0.038(2) Uani 1 1 d . . . C42 C 0.3037(5) 0.0148(3) 0.2986(7) 0.049(3) Uani 1 1 d . . . C43 C 0.3767(4) -0.0094(3) 0.9416(6) 0.038(2) Uani 1 1 d . . . C44 C 0.2285(4) 0.1374(2) 0.9628(6) 0.0251(18) Uani 1 1 d . . . C45 C 0.0997(6) 0.1612(5) 0.3119(11) 0.118(7) Uani 1 1 d . . . H45A H 0.0812 0.1772 0.2604 0.177 Uiso 1 1 calc R . . H45B H 0.0902 0.1690 0.3701 0.177 Uiso 1 1 calc R . . H45C H 0.0879 0.1358 0.2978 0.177 Uiso 1 1 calc R . . C46 C 0.0146(5) 0.0393(4) 0.2397(9) 0.067(4) Uani 1 1 d . . . H46A H -0.0171 0.0542 0.2222 0.081 Uiso 1 1 calc R . . C47 C 0.0405(3) 0.0775(3) 0.6187(7) 0.037(2) Uani 1 1 d . . . C48 C 0.4686(4) 0.1086(3) 0.9674(7) 0.048(3) Uani 1 1 d . . . H48A H 0.4706 0.0837 0.9494 0.057 Uiso 1 1 calc R . . C50 C 0.3535(4) 0.1344(3) 0.2935(6) 0.038(2) Uani 1 1 d . . . H50A H 0.3240 0.1179 0.2716 0.045 Uiso 1 1 calc R . . C52 C 0.4949(4) 0.0734(3) 0.6494(8) 0.042(2) Uani 1 1 d . . . C53 C 0.3246(4) 0.2414(3) 0.7479(7) 0.039(2) Uani 1 1 d . . . H53A H 0.3384 0.2666 0.7567 0.059 Uiso 1 1 calc R . . H53B H 0.3335 0.2285 0.8081 0.059 Uiso 1 1 calc R . . H53C H 0.2848 0.2417 0.7233 0.059 Uiso 1 1 calc R . . C54 C 0.1418(4) 0.0219(3) 0.9335(6) 0.036(2) Uani 1 1 d . . . H54A H 0.1351 0.0475 0.9260 0.044 Uiso 1 1 calc R . . C58 C 0.1211(5) 0.0025(3) 1.0013(8) 0.057(3) Uani 1 1 d . . . H58A H 0.1013 0.0150 1.0394 0.068 Uiso 1 1 calc R . . C59 C 0.1763(6) 0.2054(3) 0.3460(7) 0.060(3) Uani 1 1 d . . . H59A H 0.1599 0.2203 0.2910 0.089 Uiso 1 1 calc R . . H59B H 0.2161 0.2088 0.3621 0.089 Uiso 1 1 calc R . . H59C H 0.1613 0.2130 0.3990 0.089 Uiso 1 1 calc R . . C60 C 0.0998(4) 0.1993(3) 0.6828(8) 0.046(3) Uani 1 1 d . . . H60A H 0.0944 0.1788 0.7194 0.055 Uiso 1 1 calc R . . C61 C 0.1124(5) 0.2582(3) 0.5734(8) 0.056(3) Uani 1 1 d . . . H61A H 0.1185 0.2782 0.5358 0.067 Uiso 1 1 calc R . . C63 C 0.2498(4) 0.1084(3) 1.0453(6) 0.038(2) Uani 1 1 d . . . H63A H 0.2446 0.1185 1.1045 0.057 Uiso 1 1 calc R . . H63B H 0.2888 0.1034 1.0508 0.057 Uiso 1 1 calc R . . H63C H 0.2289 0.0856 1.0309 0.057 Uiso 1 1 calc R . . C65 C 0.4143(4) 0.2193(3) 0.7111(7) 0.039(2) Uani 1 1 d . . . H65A H 0.4293 0.2442 0.7185 0.059 Uiso 1 1 calc R . . H65B H 0.4298 0.2059 0.6655 0.059 Uiso 1 1 calc R . . H65C H 0.4237 0.2066 0.7716 0.059 Uiso 1 1 calc R . . C66 C 0.5041(5) 0.0488(3) 0.5696(9) 0.057(3) Uani 1 1 d . . . H66A H 0.5435 0.0466 0.5736 0.085 Uiso 1 1 calc R . . H66B H 0.4860 0.0596 0.5092 0.085 Uiso 1 1 calc R . . H66C H 0.4887 0.0244 0.5752 0.085 Uiso 1 1 calc R . . C68 C 0.5268(4) 0.0584(3) 0.7475(8) 0.054(3) Uani 1 1 d . . . H68A H 0.5656 0.0552 0.7475 0.080 Uiso 1 1 calc R . . H68B H 0.5113 0.0347 0.7596 0.080 Uiso 1 1 calc R . . H68C H 0.5235 0.0759 0.7965 0.080 Uiso 1 1 calc R . . C69 C 0.3409(6) -0.0448(4) 0.9474(10) 0.083(5) Uani 1 1 d . . . H69A H 0.3561 -0.0578 1.0061 0.124 Uiso 1 1 calc R . . H69B H 0.3413 -0.0609 0.8941 0.124 Uiso 1 1 calc R . . H69C H 0.3031 -0.0374 0.9455 0.124 Uiso 1 1 calc R . . C70 C 0.0119(4) 0.1081(3) 0.5512(8) 0.045(3) Uani 1 1 d . . . H70A H -0.0275 0.1078 0.5480 0.067 Uiso 1 1 calc R . . H70B H 0.0181 0.1038 0.4885 0.067 Uiso 1 1 calc R . . H70C H 0.0272 0.1320 0.5744 0.067 Uiso 1 1 calc R . . C75 C 0.0174(4) 0.0391(3) 0.5807(9) 0.052(3) Uani 1 1 d . . . H75A H -0.0205 0.0366 0.5869 0.078 Uiso 1 1 calc R . . H75B H 0.0399 0.0197 0.6168 0.078 Uiso 1 1 calc R . . H75C H 0.0182 0.0369 0.5145 0.078 Uiso 1 1 calc R . . C77 C 0.1501(4) 0.2289(2) 0.5925(6) 0.032(2) Uani 1 1 d . . . H77A H 0.1813 0.2298 0.5666 0.039 Uiso 1 1 calc R . . C80 C 0.0660(5) 0.2573(3) 0.6107(9) 0.059(3) Uani 1 1 d . . . H80A H 0.0387 0.2758 0.5969 0.071 Uiso 1 1 calc R . . C81 C 0.5129(4) 0.1139(3) 0.6348(10) 0.064(4) Uani 1 1 d . . . H81A H 0.5527 0.1162 0.6584 0.096 Uiso 1 1 calc R . . H81B H 0.4943 0.1308 0.6690 0.096 Uiso 1 1 calc R . . H81C H 0.5030 0.1199 0.5678 0.096 Uiso 1 1 calc R . . C83 C 0.3352(4) 0.2420(3) 0.5799(7) 0.041(2) Uani 1 1 d . . . H83A H 0.3517 0.2665 0.5864 0.061 Uiso 1 1 calc R . . H83B H 0.2952 0.2442 0.5612 0.061 Uiso 1 1 calc R . . H83C H 0.3482 0.2283 0.5320 0.061 Uiso 1 1 calc R . . C84 C 0.4108(4) 0.1676(3) 0.4208(7) 0.039(2) Uani 1 1 d . . . H84A H 0.4213 0.1734 0.4856 0.047 Uiso 1 1 calc R . . C85 C 0.0350(4) 0.0841(3) 0.7221(8) 0.051(3) Uani 1 1 d . . . H85A H -0.0035 0.0816 0.7248 0.076 Uiso 1 1 calc R . . H85B H 0.0479 0.1089 0.7421 0.076 Uiso 1 1 calc R . . H85C H 0.0572 0.0661 0.7639 0.076 Uiso 1 1 calc R . . C87 C 0.2965(7) -0.0283(3) 0.3014(8) 0.074(4) Uani 1 1 d . . . H87A H 0.3009 -0.0389 0.2422 0.111 Uiso 1 1 calc R . . H87B H 0.2599 -0.0341 0.3101 0.111 Uiso 1 1 calc R . . H87C H 0.3243 -0.0385 0.3535 0.111 Uiso 1 1 calc R . . C88 C 0.2235(5) -0.0939(3) 0.6590(8) 0.049(3) Uani 1 1 d . . . H88A H 0.2105 -0.1193 0.6504 0.074 Uiso 1 1 calc R . . H88B H 0.2257 -0.0863 0.7238 0.074 Uiso 1 1 calc R . . H88C H 0.2599 -0.0922 0.6456 0.074 Uiso 1 1 calc R . . C89 C 0.1786(5) -0.0324(3) 0.8870(7) 0.048(3) Uani 1 1 d . . . H89A H 0.1980 -0.0448 0.8478 0.057 Uiso 1 1 calc R . . C90 C 0.4326(4) -0.0207(3) 0.9269(7) 0.042(2) Uani 1 1 d . . . H90A H 0.4534 -0.0334 0.9830 0.062 Uiso 1 1 calc R . . H90B H 0.4527 0.0012 0.9154 0.062 Uiso 1 1 calc R . . H90C H 0.4276 -0.0372 0.8728 0.062 Uiso 1 1 calc R . . C91 C 0.2616(4) 0.1738(3) 0.9878(7) 0.041(2) Uani 1 1 d . . . H91A H 0.2576 0.1827 1.0488 0.061 Uiso 1 1 calc R . . H91B H 0.2475 0.1922 0.9397 0.061 Uiso 1 1 calc R . . H91C H 0.3005 0.1692 0.9905 0.061 Uiso 1 1 calc R . . C92 C 0.0620(4) 0.2278(3) 0.6691(8) 0.051(3) Uani 1 1 d . . . H92A H 0.0328 0.2272 0.7001 0.061 Uiso 1 1 calc R . . C95 C 0.1300(6) -0.0353(3) 1.0117(10) 0.074(4) Uani 1 1 d . . . H95A H 0.1173 -0.0487 1.0580 0.089 Uiso 1 1 calc R . . Mn7 Mn 0.58715(14) 0.25324(10) 0.1774(3) 0.0560(9) Uani 0.50 1 d P . . Cl2 Cl 0.5540(3) 0.21189(19) 0.2758(5) 0.0694(18) Uani 0.50 1 d P . . Cl5 Cl 0.5245(4) 0.2820(3) 0.0564(5) 0.103(3) Uani 0.50 1 d P . . Cl1 Cl 0.26803(8) 0.07673(6) 0.63293(13) 0.0280(5) Uani 1 1 d . . . Cl3 Cl 0.6946(2) 0.20787(17) 0.1203(4) 0.0568(14) Uani 0.50 1 d P . . Cl4 Cl 0.6925(3) 0.19784(18) 0.8052(5) 0.0654(16) Uani 0.50 1 d P . . O1W O 0.7897(3) 0.25569(19) 0.2532(5) 0.0429(16) Uani 1 1 d . . . O2W O 0.0181(6) 0.0782(8) 0.9841(13) 0.121(11) Uani 0.50 1 d P . . Mn8 Mn -0.10861(11) 0.29693(8) 0.5561(3) 0.0558(10) Uani 0.50 1 d P . . Cl9A Cl -0.0974(3) 0.29734(18) 0.3484(5) 0.0164(14) Uani 0.25 1 d P . . Cl6A Cl -0.0703(3) 0.2551(4) 0.6830(6) 0.054(3) Uani 0.25 1 d P . . Cl8A Cl -0.2335(3) 0.2598(2) 0.4597(5) 0.0174(14) Uani 0.25 1 d PU . . Cl6B Cl -0.0887(3) 0.27724(18) 0.7667(5) 0.0140(13) Uiso 0.25 1 d P . . Cl9B Cl -0.0592(4) 0.2699(3) 0.4280(7) 0.045(2) Uiso 0.25 1 d P . . Cl8B Cl -0.2273(3) 0.25167(18) 0.5305(5) 0.0134(13) Uiso 0.25 1 d P . . Cl7 Cl -0.1031(5) 0.3595(3) 0.6434(8) 0.122(3) Uiso 0.50 1 d P . . 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 0.0248(6) 0.0179(6) 0.0172(6) 0.0003(5) 0.0063(5) 0.0017(5) Mn2 0.0213(6) 0.0189(6) 0.0151(6) 0.0016(4) 0.0036(5) 0.0001(5) Mn3 0.0228(6) 0.0255(7) 0.0172(6) 0.0051(5) 0.0040(5) 0.0005(5) Mn4 0.0358(7) 0.0222(7) 0.0200(6) 0.0055(5) 0.0142(5) 0.0091(5) Mn5 0.0403(8) 0.0222(7) 0.0181(6) -0.0023(5) 0.0014(5) 0.0050(6) Mn6 0.0325(7) 0.0252(7) 0.0203(6) 0.0076(5) 0.0126(5) 0.0075(5) P8 0.0269(11) 0.0258(11) 0.0159(10) 0.0084(8) 0.0059(8) 0.0058(9) P9 0.0235(11) 0.0216(10) 0.0204(10) 0.0041(8) 0.0050(8) -0.0022(8) P10 0.0207(10) 0.0217(11) 0.0269(11) -0.0011(9) 0.0002(9) 0.0003(8) P11 0.0378(12) 0.0177(10) 0.0174(10) -0.0010(8) 0.0049(9) 0.0042(9) P12 0.0277(11) 0.0199(10) 0.0136(10) -0.0013(8) 0.0061(8) -0.0006(8) P13 0.0351(12) 0.0240(11) 0.0148(10) 0.0049(8) 0.0018(9) 0.0055(9) P14 0.0242(11) 0.0300(12) 0.0337(12) 0.0145(10) 0.0150(9) 0.0093(9) P15 0.0560(15) 0.0273(12) 0.0166(11) 0.0032(9) 0.0163(10) 0.0144(11) O3 0.029(3) 0.023(3) 0.027(3) -0.004(2) 0.000(2) 0.003(2) O4 0.032(3) 0.025(3) 0.019(3) 0.012(2) 0.006(2) 0.007(2) O5 0.019(3) 0.027(3) 0.020(3) 0.001(2) 0.004(2) 0.005(2) O6 0.031(3) 0.024(3) 0.023(3) 0.002(2) 0.004(2) 0.001(2) O7 0.024(3) 0.023(3) 0.017(3) 0.000(2) 0.007(2) 0.000(2) O8 0.030(3) 0.020(3) 0.014(3) -0.001(2) 0.003(2) -0.003(2) O9 0.033(3) 0.020(3) 0.023(3) 0.006(2) 0.008(2) 0.005(2) O10 0.024(3) 0.016(3) 0.025(3) -0.003(2) 0.011(2) 0.000(2) O11 0.036(3) 0.028(3) 0.029(3) 0.008(2) 0.017(3) 0.006(3) O12 0.047(4) 0.025(3) 0.022(3) 0.005(2) 0.020(3) 0.013(3) O13 0.052(4) 0.028(3) 0.017(3) 0.004(2) 0.006(3) 0.004(3) O14 0.032(3) 0.028(3) 0.014(3) 0.001(2) 0.005(2) 0.002(2) O15 0.026(3) 0.014(3) 0.029(3) 0.004(2) 0.001(2) -0.001(2) O16 0.053(4) 0.035(3) 0.020(3) 0.008(2) 0.020(3) 0.019(3) O17 0.033(3) 0.019(3) 0.016(3) 0.002(2) 0.008(2) 0.002(2) O18 0.026(3) 0.017(3) 0.021(3) 0.000(2) 0.007(2) -0.002(2) O19 0.042(3) 0.021(3) 0.018(3) -0.004(2) 0.007(2) 0.006(2) O20 0.055(4) 0.027(3) 0.018(3) 0.005(2) 0.010(3) 0.010(3) O22 0.037(3) 0.022(3) 0.020(3) 0.004(2) 0.006(2) 0.004(2) O23 0.026(3) 0.031(3) 0.020(3) 0.008(2) 0.003(2) 0.007(2) O24 0.030(3) 0.023(3) 0.028(3) 0.004(2) 0.014(2) 0.003(2) O26 0.025(3) 0.034(3) 0.034(3) 0.011(3) 0.013(3) 0.011(3) O35 0.039(3) 0.022(3) 0.025(3) 0.000(2) 0.004(3) 0.004(3) O37 0.020(3) 0.033(3) 0.033(3) 0.014(3) 0.009(2) -0.001(2) N25 0.030(4) 0.020(4) 0.028(4) -0.002(3) 0.003(3) 0.010(3) N27 0.028(4) 0.029(4) 0.025(4) 0.003(3) 0.009(3) -0.001(3) N36 0.065(6) 0.025(4) 0.042(5) 0.016(4) 0.037(4) 0.017(4) N39 0.026(4) 0.050(5) 0.026(4) 0.000(3) 0.003(3) -0.005(3) N40 0.049(5) 0.033(4) 0.030(4) 0.015(3) 0.025(4) 0.010(4) N45 0.059(5) 0.029(4) 0.031(4) -0.001(3) -0.006(4) 0.003(4) C13 0.047(6) 0.033(5) 0.036(5) 0.003(4) 0.007(4) 0.012(4) C14 0.067(7) 0.042(6) 0.058(7) 0.014(5) 0.040(6) 0.008(5) C15 0.076(8) 0.029(5) 0.035(5) -0.005(4) 0.020(5) -0.015(5) C16 0.043(6) 0.065(8) 0.071(8) -0.015(6) 0.013(6) -0.020(6) C17 0.055(7) 0.053(7) 0.051(7) 0.031(5) 0.035(5) 0.019(6) C18 0.078(9) 0.072(8) 0.024(5) -0.018(5) 0.017(5) -0.048(7) C21 0.052(7) 0.053(7) 0.054(7) -0.011(5) 0.000(5) -0.007(5) C22 0.060(8) 0.058(8) 0.071(8) -0.022(6) -0.037(6) 0.019(6) C23 0.053(7) 0.072(9) 0.055(7) -0.007(6) -0.023(6) 0.004(6) C24 0.070(8) 0.044(6) 0.036(6) 0.007(5) -0.020(5) -0.002(6) C25 0.060(7) 0.041(6) 0.033(5) 0.004(4) 0.025(5) 0.009(5) C26 0.066(7) 0.064(7) 0.033(6) 0.021(5) 0.025(5) 0.007(6) C27 0.114(11) 0.038(6) 0.099(11) 0.027(7) 0.071(9) 0.004(7) C28 0.070(9) 0.096(11) 0.039(6) -0.007(7) 0.005(6) -0.066(8) C29 0.122(11) 0.024(5) 0.054(7) -0.013(5) 0.027(7) -0.012(6) C30 0.025(4) 0.037(5) 0.038(5) 0.008(4) 0.014(4) 0.003(4) C31 0.067(8) 0.063(8) 0.056(7) 0.032(6) 0.030(6) 0.040(6) C32 0.075(8) 0.032(6) 0.098(10) 0.006(6) 0.057(8) 0.020(6) C33 0.073(8) 0.093(9) 0.016(5) 0.007(5) 0.004(5) 0.024(7) C34 0.098(10) 0.077(8) 0.043(6) 0.019(6) 0.052(7) 0.044(7) C35 0.135(12) 0.041(6) 0.028(5) -0.003(5) 0.025(6) 0.028(7) C36 0.165(14) 0.054(7) 0.015(5) 0.004(5) 0.025(7) 0.038(8) C37 0.135(16) 0.020(6) 0.24(2) -0.007(9) 0.133(17) -0.002(8) C38 0.052(6) 0.029(5) 0.013(4) 0.007(3) -0.010(4) 0.002(4) C39 0.086(8) 0.063(7) 0.109(9) 0.015(7) 0.034(7) 0.030(6) C40 0.069(9) 0.094(12) 0.117(13) 0.047(10) 0.050(9) 0.055(9) C41 0.055(6) 0.015(4) 0.035(5) -0.010(4) -0.005(4) 0.001(4) C42 0.090(8) 0.039(6) 0.025(5) 0.000(4) 0.026(5) 0.010(5) C43 0.035(5) 0.048(6) 0.028(5) 0.015(4) 0.003(4) 0.007(4) C44 0.040(5) 0.019(4) 0.021(4) -0.003(3) 0.017(4) -0.006(3) C45 0.077(10) 0.161(17) 0.081(10) 0.080(11) -0.051(8) -0.027(10) C46 0.067(8) 0.066(8) 0.054(7) 0.015(6) -0.016(6) -0.023(7) C47 0.020(4) 0.035(5) 0.055(6) 0.010(4) 0.007(4) -0.010(4) C48 0.046(6) 0.040(6) 0.046(6) -0.007(5) -0.015(5) 0.014(5) C50 0.050(6) 0.040(5) 0.027(5) 0.006(4) 0.017(4) 0.010(4) C52 0.024(5) 0.039(5) 0.071(7) 0.021(5) 0.027(5) 0.009(4) C53 0.036(5) 0.033(5) 0.047(6) -0.002(4) 0.007(4) -0.005(4) C54 0.043(5) 0.037(5) 0.033(5) 0.003(4) 0.017(4) 0.011(4) C58 0.062(7) 0.064(8) 0.062(7) 0.011(6) 0.048(6) 0.013(6) C59 0.108(10) 0.037(6) 0.029(5) 0.007(4) 0.007(6) 0.026(6) C60 0.038(6) 0.042(6) 0.061(7) -0.009(5) 0.020(5) -0.008(5) C61 0.071(8) 0.033(6) 0.050(7) 0.007(5) -0.012(6) 0.012(5) C63 0.062(6) 0.043(6) 0.014(4) 0.003(4) 0.016(4) 0.006(5) C65 0.038(5) 0.034(5) 0.044(6) 0.003(4) 0.006(4) -0.009(4) C66 0.047(6) 0.064(7) 0.071(8) 0.004(6) 0.039(6) 0.021(6) C68 0.029(5) 0.079(8) 0.056(7) 0.028(6) 0.017(5) 0.017(5) C69 0.088(10) 0.073(9) 0.079(10) 0.051(8) 0.002(8) -0.017(8) C70 0.025(5) 0.032(5) 0.073(7) 0.004(5) 0.004(5) 0.006(4) C75 0.031(5) 0.042(6) 0.079(8) 0.018(6) 0.003(5) -0.004(4) C77 0.052(6) 0.018(4) 0.028(5) 0.003(4) 0.010(4) 0.003(4) C80 0.047(7) 0.041(6) 0.081(9) -0.012(6) -0.001(6) 0.018(5) C81 0.037(6) 0.060(8) 0.097(10) 0.036(7) 0.023(6) 0.004(5) C83 0.045(6) 0.031(5) 0.048(6) 0.010(4) 0.011(5) 0.003(4) C84 0.050(6) 0.034(5) 0.041(5) 0.012(4) 0.024(5) 0.021(5) C85 0.036(6) 0.057(7) 0.066(7) 0.013(6) 0.027(5) 0.005(5) C87 0.155(13) 0.044(7) 0.032(6) 0.003(5) 0.041(7) 0.024(8) C88 0.065(7) 0.018(5) 0.067(7) 0.015(5) 0.018(6) 0.004(5) C89 0.078(8) 0.031(5) 0.039(6) 0.010(4) 0.023(5) -0.001(5) C90 0.037(5) 0.040(6) 0.043(6) 0.002(4) 0.000(4) 0.006(4) C91 0.058(6) 0.035(5) 0.029(5) -0.015(4) 0.011(4) -0.008(5) C92 0.035(6) 0.044(6) 0.072(8) -0.009(6) 0.007(5) 0.012(5) C95 0.092(10) 0.058(8) 0.093(10) 0.031(7) 0.062(8) -0.013(7) Mn7 0.050(2) 0.060(2) 0.057(2) -0.0048(17) 0.0104(17) 0.0008(17) Cl2 0.072(4) 0.079(4) 0.070(4) -0.013(3) 0.042(3) -0.033(3) Cl5 0.096(6) 0.142(8) 0.061(4) 0.011(4) 0.001(4) 0.067(5) Cl1 0.0324(11) 0.0298(11) 0.0225(10) 0.0007(8) 0.0079(8) 0.0032(9) Cl3 0.054(3) 0.060(3) 0.058(3) 0.001(3) 0.015(3) 0.005(3) Cl4 0.060(4) 0.062(4) 0.069(4) 0.019(3) 0.005(3) -0.005(3) O1W 0.037(4) 0.046(4) 0.045(4) 0.006(3) 0.008(3) -0.001(3) O2W 0.027(8) 0.27(3) 0.078(13) 0.101(17) 0.031(8) 0.047(13) Mn8 0.0178(14) 0.0189(14) 0.111(3) 0.0172(16) -0.0248(16) -0.0071(11) Cl9A 0.009(3) 0.015(3) 0.024(4) -0.002(3) 0.002(3) -0.010(3) Cl6A 0.005(3) 0.141(11) 0.013(4) -0.010(5) -0.001(3) 0.029(5) Cl8A 0.009(3) 0.026(4) 0.015(3) -0.004(3) 0.000(2) -0.001(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 O7 1.882(5) . ? Mn1 O9 1.884(5) . ? Mn1 O15 1.885(5) . ? Mn1 O14 1.904(5) . ? Mn1 N27 2.245(7) . ? Mn2 O8 1.880(5) . ? Mn2 O5 1.889(5) . ? Mn2 O10 1.892(5) . ? Mn2 O18 1.895(5) . ? Mn2 N25 2.258(6) . ? Mn3 O37 1.883(6) . ? Mn3 O6 1.891(5) . ? Mn3 O17 1.892(5) . ? Mn3 O23 1.896(5) . ? Mn3 N39 2.244(7) . ? Mn4 O16 1.876(5) . ? Mn4 O19 1.885(6) . ? Mn4 O4 1.886(5) . ? Mn4 O26 1.898(6) . ? Mn4 N36 2.252(7) . ? Mn5 O3 1.882(6) . ? Mn5 O20 1.882(6) . ? Mn5 O13 1.887(6) . ? Mn5 O35 1.890(6) . ? Mn5 N45 2.218(8) . ? Mn6 O11 1.870(6) . ? Mn6 O22 1.877(6) . ? Mn6 O12 1.880(6) . ? Mn6 O24 1.908(6) . ? Mn6 N40 2.231(7) . ? P8 O14 1.519(6) . ? P8 O4 1.527(6) . ? P8 O23 1.528(6) . ? P8 C43 1.820(9) . ? P9 O6 1.518(6) . ? P9 O18 1.521(5) . ? P9 O24 1.522(6) . ? P9 C30 1.828(9) . ? P10 O3 1.507(6) . ? P10 O15 1.517(5) . ? P10 O10 1.529(5) . ? P10 C47 1.839(8) . ? P11 O35 1.516(6) . ? P11 O19 1.527(6) . ? P11 O9 1.532(6) . ? P11 C41 1.836(9) . ? P12 O17 1.518(6) . ? P12 O8 1.525(5) . ? P12 O7 1.529(5) . ? P12 C44 1.797(8) . ? P13 O22 1.516(6) . ? P13 O5 1.529(5) . ? P13 O13 1.541(6) . ? P13 C38 1.818(8) . ? P14 O26 1.517(6) . ? P14 O11 1.533(6) . ? P14 O37 1.541(6) . ? P14 C52 1.823(9) . ? P15 O16 1.516(6) . ? P15 O20 1.516(7) . ? P15 O12 1.547(6) . ? P15 C42 1.828(9) . ? N25 C77 1.309(11) . ? N25 C60 1.322(11) . ? N27 C89 1.325(11) . ? N27 C54 1.363(11) . ? N36 C31 1.320(14) . ? N36 C32 1.362(15) . ? N39 C48 1.292(12) . ? N39 C13 1.343(12) . ? N40 C84 1.352(13) . ? N40 C50 1.360(12) . ? N45 C24 1.335(14) . ? N45 C15 1.350(12) . ? C13 C21 1.363(14) . ? C13 H13A 0.9300 . ? C14 C84 1.391(13) . ? C14 C17 1.418(15) . ? C14 H14A 0.9300 . ? C15 C18 1.384(15) . ? C15 H15A 0.9300 . ? C16 C41 1.498(14) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C26 1.328(16) . ? C17 H17A 0.9300 . ? C18 C28 1.370(19) . ? C18 H18A 0.9300 . ? C21 C23 1.414(16) . ? C21 H21A 0.9300 . ? C22 C23 1.342(16) . ? C22 C48 1.389(14) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C46 1.367(15) . ? C24 H24A 0.9300 . ? C25 C44 1.500(13) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C50 1.398(13) . ? C26 H26A 0.9300 . ? C27 C89 1.371(14) . ? C27 C95 1.375(17) . ? C27 H27A 0.9300 . ? C28 C46 1.331(19) . ? C28 H28A 0.9300 . ? C29 C41 1.552(14) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C65 1.490(12) . ? C30 C53 1.537(13) . ? C30 C83 1.545(12) . ? C31 C40 1.410(17) . ? C31 H31A 0.9300 . ? C32 C37 1.413(16) . ? C32 H32A 0.9300 . ? C33 C43 1.537(14) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C42 1.528(17) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C42 1.523(15) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C38 1.539(14) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C39 1.33(2) . ? C37 H37A 0.9300 . ? C38 C45 1.518(17) . ? C38 C59 1.536(14) . ? C39 C40 1.34(2) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 C88 1.570(13) . ? C42 C87 1.553(15) . ? C43 C90 1.492(13) . ? C43 C69 1.552(15) . ? C44 C91 1.530(12) . ? C44 C63 1.568(11) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9300 . ? C47 C70 1.520(13) . ? C47 C75 1.536(14) . ? C47 C85 1.542(14) . ? C48 H48A 0.9300 . ? C50 H50A 0.9300 . ? C52 C66 1.503(15) . ? C52 C68 1.539(14) . ? C52 C81 1.543(14) . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 C58 1.387(13) . ? C54 H54A 0.9300 . ? C58 C95 1.370(16) . ? C58 H58A 0.9300 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C92 1.361(14) . ? C60 H60A 0.9300 . ? C61 C80 1.369(16) . ? C61 C77 1.379(13) . ? C61 H61A 0.9300 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C77 H77A 0.9300 . ? C80 C92 1.365(16) . ? C80 H80A 0.9300 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 H84A 0.9300 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 H89A 0.9300 . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C92 H92A 0.9300 . ? C95 H95A 0.9300 . ? Mn7 Cl5 2.280(8) . ? Mn7 Cl2 2.322(7) . ? Mn8 Cl6A 2.374(11) . ? Mn8 Cl7 2.552(12) . ? Mn8 Cl9B 2.617(11) . ? Cl9A Cl9B 1.626(12) . ? Cl6A Cl6B 1.591(10) . ? Cl8A Cl8B 1.035(9) . ? 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 O7 Mn1 O9 176.6(2) . . ? O7 Mn1 O15 89.5(2) . . ? O9 Mn1 O15 89.8(2) . . ? O7 Mn1 O14 90.1(2) . . ? O9 Mn1 O14 90.4(2) . . ? O15 Mn1 O14 176.5(2) . . ? O7 Mn1 N27 93.4(2) . . ? O9 Mn1 N27 89.9(2) . . ? O15 Mn1 N27 94.9(2) . . ? O14 Mn1 N27 88.6(2) . . ? O8 Mn2 O5 177.3(2) . . ? O8 Mn2 O10 89.1(2) . . ? O5 Mn2 O10 90.1(2) . . ? O8 Mn2 O18 90.9(2) . . ? O5 Mn2 O18 89.8(2) . . ? O10 Mn2 O18 176.8(2) . . ? O8 Mn2 N25 94.0(2) . . ? O5 Mn2 N25 88.6(2) . . ? O10 Mn2 N25 90.8(2) . . ? O18 Mn2 N25 92.4(2) . . ? O37 Mn3 O6 90.9(2) . . ? O37 Mn3 O17 178.0(3) . . ? O6 Mn3 O17 89.3(2) . . ? O37 Mn3 O23 89.3(2) . . ? O6 Mn3 O23 177.9(2) . . ? O17 Mn3 O23 90.5(2) . . ? O37 Mn3 N39 90.5(3) . . ? O6 Mn3 N39 89.5(3) . . ? O17 Mn3 N39 91.6(2) . . ? O23 Mn3 N39 92.7(3) . . ? O16 Mn4 O19 88.5(3) . . ? O16 Mn4 O4 175.5(2) . . ? O19 Mn4 O4 90.7(2) . . ? O16 Mn4 O26 90.8(3) . . ? O19 Mn4 O26 177.4(2) . . ? O4 Mn4 O26 89.8(2) . . ? O16 Mn4 N36 93.5(3) . . ? O19 Mn4 N36 90.2(3) . . ? O4 Mn4 N36 90.9(3) . . ? O26 Mn4 N36 92.3(3) . . ? O3 Mn5 O20 176.2(3) . . ? O3 Mn5 O13 90.0(2) . . ? O20 Mn5 O13 90.0(3) . . ? O3 Mn5 O35 90.3(2) . . ? O20 Mn5 O35 89.4(2) . . ? O13 Mn5 O35 176.4(3) . . ? O3 Mn5 N45 90.4(3) . . ? O20 Mn5 N45 93.4(3) . . ? O13 Mn5 N45 90.4(3) . . ? O35 Mn5 N45 93.1(3) . . ? O11 Mn6 O22 176.7(2) . . ? O11 Mn6 O12 90.7(3) . . ? O22 Mn6 O12 89.8(2) . . ? O11 Mn6 O24 90.1(2) . . ? O22 Mn6 O24 89.3(2) . . ? O12 Mn6 O24 178.0(2) . . ? O11 Mn6 N40 91.1(3) . . ? O22 Mn6 N40 92.2(3) . . ? O12 Mn6 N40 89.7(3) . . ? O24 Mn6 N40 92.0(3) . . ? O14 P8 O4 112.4(3) . . ? O14 P8 O23 111.6(3) . . ? O4 P8 O23 112.5(3) . . ? O14 P8 C43 107.3(4) . . ? O4 P8 C43 106.5(4) . . ? O23 P8 C43 106.1(4) . . ? O6 P9 O18 111.8(3) . . ? O6 P9 O24 112.0(3) . . ? O18 P9 O24 113.0(3) . . ? O6 P9 C30 106.1(4) . . ? O18 P9 C30 107.4(3) . . ? O24 P9 C30 106.0(3) . . ? O3 P10 O15 111.8(3) . . ? O3 P10 O10 111.9(3) . . ? O15 P10 O10 113.2(3) . . ? O3 P10 C47 108.0(4) . . ? O15 P10 C47 104.7(4) . . ? O10 P10 C47 106.7(4) . . ? O35 P11 O19 112.8(3) . . ? O35 P11 O9 112.5(3) . . ? O19 P11 O9 111.4(3) . . ? O35 P11 C41 106.1(4) . . ? O19 P11 C41 107.4(4) . . ? O9 P11 C41 106.2(4) . . ? O17 P12 O8 112.6(3) . . ? O17 P12 O7 111.6(3) . . ? O8 P12 O7 112.5(3) . . ? O17 P12 C44 108.1(3) . . ? O8 P12 C44 105.9(3) . . ? O7 P12 C44 105.7(3) . . ? O22 P13 O5 112.3(3) . . ? O22 P13 O13 112.5(3) . . ? O5 P13 O13 111.7(3) . . ? O22 P13 C38 106.2(4) . . ? O5 P13 C38 106.7(4) . . ? O13 P13 C38 107.0(4) . . ? O26 P14 O11 112.1(3) . . ? O26 P14 O37 112.6(3) . . ? O11 P14 O37 112.2(3) . . ? O26 P14 C52 106.1(4) . . ? O11 P14 C52 106.9(4) . . ? O37 P14 C52 106.6(4) . . ? O16 P15 O20 112.7(3) . . ? O16 P15 O12 112.2(4) . . ? O20 P15 O12 111.1(3) . . ? O16 P15 C42 106.8(4) . . ? O20 P15 C42 107.0(5) . . ? O12 P15 C42 106.6(4) . . ? P10 O3 Mn5 138.4(4) . . ? P8 O4 Mn4 138.3(3) . . ? P13 O5 Mn2 136.6(3) . . ? P9 O6 Mn3 138.1(4) . . ? P12 O7 Mn1 137.6(3) . . ? P12 O8 Mn2 137.3(3) . . ? P11 O9 Mn1 137.5(3) . . ? P10 O10 Mn2 136.5(3) . . ? P14 O11 Mn6 138.3(3) . . ? P15 O12 Mn6 137.0(3) . . ? P13 O13 Mn5 136.7(3) . . ? P8 O14 Mn1 136.5(3) . . ? P10 O15 Mn1 138.3(3) . . ? P15 O16 Mn4 139.9(4) . . ? P12 O17 Mn3 138.0(3) . . ? P9 O18 Mn2 137.2(3) . . ? P11 O19 Mn4 136.3(3) . . ? P15 O20 Mn5 137.6(4) . . ? P13 O22 Mn6 138.8(3) . . ? P8 O23 Mn3 136.5(3) . . ? P9 O24 Mn6 135.8(3) . . ? P14 O26 Mn4 137.3(3) . . ? P11 O35 Mn5 139.0(4) . . ? P14 O37 Mn3 136.5(4) . . ? C77 N25 C60 117.9(8) . . ? C77 N25 Mn2 119.5(6) . . ? C60 N25 Mn2 121.3(6) . . ? C89 N27 C54 118.1(8) . . ? C89 N27 Mn1 120.2(6) . . ? C54 N27 Mn1 121.7(6) . . ? C31 N36 C32 120.1(9) . . ? C31 N36 Mn4 120.5(8) . . ? C32 N36 Mn4 119.3(7) . . ? C48 N39 C13 116.9(8) . . ? C48 N39 Mn3 122.4(7) . . ? C13 N39 Mn3 120.6(6) . . ? C84 N40 C50 120.1(8) . . ? C84 N40 Mn6 119.0(6) . . ? C50 N40 Mn6 120.5(7) . . ? C24 N45 C15 116.9(9) . . ? C24 N45 Mn5 121.1(7) . . ? C15 N45 Mn5 122.0(7) . . ? N39 C13 C21 123.3(9) . . ? N39 C13 H13A 118.4 . . ? C21 C13 H13A 118.4 . . ? C84 C14 C17 119.6(11) . . ? C84 C14 H14A 120.2 . . ? C17 C14 H14A 120.2 . . ? N45 C15 C18 122.6(11) . . ? N45 C15 H15A 118.7 . . ? C18 C15 H15A 118.7 . . ? C41 C16 H16A 109.5 . . ? C41 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C41 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C26 C17 C14 119.5(9) . . ? C26 C17 H17A 120.3 . . ? C14 C17 H17A 120.3 . . ? C28 C18 C15 117.7(11) . . ? C28 C18 H18A 121.2 . . ? C15 C18 H18A 121.2 . . ? C13 C21 C23 118.9(11) . . ? C13 C21 H21A 120.5 . . ? C23 C21 H21A 120.5 . . ? C23 C22 C48 120.4(10) . . ? C23 C22 H22A 119.8 . . ? C48 C22 H22A 119.8 . . ? C22 C23 C21 116.5(10) . . ? C22 C23 H23A 121.7 . . ? C21 C23 H23A 121.7 . . ? N45 C24 C46 122.8(12) . . ? N45 C24 H24A 118.6 . . ? C46 C24 H24A 118.6 . . ? C44 C25 H25A 109.5 . . ? C44 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C44 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C17 C26 C50 119.9(10) . . ? C17 C26 H26A 120.0 . . ? C50 C26 H26A 120.0 . . ? C89 C27 C95 120.2(11) . . ? C89 C27 H27A 119.9 . . ? C95 C27 H27A 119.9 . . ? C46 C28 C18 120.3(11) . . ? C46 C28 H28A 119.8 . . ? C18 C28 H28A 119.8 . . ? C41 C29 H29A 109.5 . . ? C41 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C41 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C65 C30 C53 112.1(8) . . ? C65 C30 C83 111.2(7) . . ? C53 C30 C83 107.8(7) . . ? C65 C30 P9 109.8(6) . . ? C53 C30 P9 107.5(6) . . ? C83 C30 P9 108.4(6) . . ? N36 C31 C40 119.4(14) . . ? N36 C31 H31A 120.3 . . ? C40 C31 H31A 120.3 . . ? N36 C32 C37 119.1(14) . . ? N36 C32 H32A 120.5 . . ? C37 C32 H32A 120.5 . . ? C43 C33 H33A 109.5 . . ? C43 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C43 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C42 C34 H34A 109.5 . . ? C42 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C42 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C42 C35 H35A 109.5 . . ? C42 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C42 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 H36A 109.5 . . ? C38 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C38 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C32 121.4(17) . . ? C39 C37 H37A 119.3 . . ? C32 C37 H37A 119.3 . . ? C45 C38 C59 104.5(11) . . ? C45 C38 C36 117.2(11) . . ? C59 C38 C36 108.5(9) . . ? C45 C38 P13 107.7(7) . . ? C59 C38 P13 110.4(6) . . ? C36 C38 P13 108.4(7) . . ? C37 C39 C40 118.1(14) . . ? C37 C39 H39A 121.0 . . ? C40 C39 H39A 121.0 . . ? C39 C40 C31 121.8(15) . . ? C39 C40 H40A 119.1 . . ? C31 C40 H40A 119.1 . . ? C16 C41 C29 111.2(9) . . ? C16 C41 C88 110.2(9) . . ? C29 C41 C88 110.3(8) . . ? C16 C41 P11 108.7(7) . . ? C29 C41 P11 109.2(7) . . ? C88 C41 P11 107.2(6) . . ? C35 C42 C34 109.9(9) . . ? C35 C42 C87 111.3(10) . . ? C34 C42 C87 110.8(10) . . ? C35 C42 P15 108.2(7) . . ? C34 C42 P15 107.5(8) . . ? C87 C42 P15 109.0(7) . . ? C90 C43 C33 110.0(8) . . ? C90 C43 C69 109.9(9) . . ? C33 C43 C69 110.9(10) . . ? C90 C43 P8 109.5(6) . . ? C33 C43 P8 108.1(7) . . ? C69 C43 P8 108.4(7) . . ? C25 C44 C91 110.7(8) . . ? C25 C44 C63 110.5(7) . . ? C91 C44 C63 108.7(7) . . ? C25 C44 P12 110.1(6) . . ? C91 C44 P12 109.5(6) . . ? C63 C44 P12 107.3(5) . . ? C38 C45 H45A 109.5 . . ? C38 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C38 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C28 C46 C24 119.6(13) . . ? C28 C46 H46A 120.2 . . ? C24 C46 H46A 120.2 . . ? C70 C47 C75 109.8(8) . . ? C70 C47 C85 111.9(8) . . ? C75 C47 C85 111.8(8) . . ? C70 C47 P10 108.0(6) . . ? C75 C47 P10 107.8(7) . . ? C85 C47 P10 107.3(6) . . ? N39 C48 C22 123.7(10) . . ? N39 C48 H48A 118.1 . . ? C22 C48 H48A 118.1 . . ? N40 C50 C26 121.1(10) . . ? N40 C50 H50A 119.5 . . ? C26 C50 H50A 119.5 . . ? C66 C52 C68 111.1(8) . . ? C66 C52 C81 110.2(9) . . ? C68 C52 C81 110.5(10) . . ? C66 C52 P14 108.3(8) . . ? C68 C52 P14 109.4(6) . . ? C81 C52 P14 107.1(6) . . ? C30 C53 H53A 109.5 . . ? C30 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C30 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N27 C54 C58 121.3(9) . . ? N27 C54 H54A 119.4 . . ? C58 C54 H54A 119.4 . . ? C95 C58 C54 119.8(10) . . ? C95 C58 H58A 120.1 . . ? C54 C58 H58A 120.1 . . ? C38 C59 H59A 109.5 . . ? C38 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C38 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N25 C60 C92 121.6(10) . . ? N25 C60 H60A 119.2 . . ? C92 C60 H60A 119.2 . . ? C80 C61 C77 119.1(10) . . ? C80 C61 H61A 120.5 . . ? C77 C61 H61A 120.5 . . ? C44 C63 H63A 109.5 . . ? C44 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C44 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C30 C65 H65A 109.5 . . ? C30 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C30 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C52 C66 H66A 109.5 . . ? C52 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C52 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C52 C68 H68A 109.5 . . ? C52 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C52 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C43 C69 H69A 109.5 . . ? C43 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C43 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C47 C70 H70A 109.5 . . ? C47 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C47 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C47 C75 H75A 109.5 . . ? C47 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C47 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? N25 C77 C61 123.4(10) . . ? N25 C77 H77A 118.3 . . ? C61 C77 H77A 118.3 . . ? C92 C80 C61 116.5(10) . . ? C92 C80 H80A 121.8 . . ? C61 C80 H80A 121.8 . . ? C52 C81 H81A 109.5 . . ? C52 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C52 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C30 C83 H83A 109.5 . . ? C30 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C30 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N40 C84 C14 119.7(10) . . ? N40 C84 H84A 120.1 . . ? C14 C84 H84A 120.1 . . ? C47 C85 H85A 109.5 . . ? C47 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C47 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C42 C87 H87A 109.5 . . ? C42 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C42 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C41 C88 H88A 109.5 . . ? C41 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C41 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? N27 C89 C27 122.5(10) . . ? N27 C89 H89A 118.7 . . ? C27 C89 H89A 118.7 . . ? C43 C90 H90A 109.5 . . ? C43 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C43 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C44 C91 H91A 109.5 . . ? C44 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C44 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C60 C92 C80 121.4(11) . . ? C60 C92 H92A 119.3 . . ? C80 C92 H92A 119.3 . . ? C58 C95 C27 118.0(10) . . ? C58 C95 H95A 121.0 . . ? C27 C95 H95A 121.0 . . ? Cl5 Mn7 Cl2 118.7(4) . . ? Cl6A Mn8 Cl7 102.0(4) . . ? Cl6A Mn8 Cl9B 98.2(3) . . ? Cl7 Mn8 Cl9B 133.6(4) . . ? Cl6B Cl6A Mn8 97.9(6) . . ? Cl9A Cl9B Mn8 89.2(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.981 _refine_diff_density_min -1.422 _refine_diff_density_rms 0.198 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 0.808 0.250 0.006 1287 138 ' ' 2 0.192 0.750 -0.117 1287 143 ' ' _platon_squeeze_details ; The PLATON SQUEEZE procedure was used to treat regions of diffuse solvent which could not be sensibly modelled in terms of atomic sites. Their contribution to the diffraction pattern was removed and modified F(obs)**2 written to a new HKL file. The number of electrons thus located, 138 per unit cell, is included in the formula, formula weight, calculated density, and F(000). This residual electron density was assigned to three and one half molecules of the water solvent, [138/4 = 34.5e per molecule; three and one half molecules of the water would give 35e]. ; data_a5 _database_code_depnum_ccdc_archive 'CCDC 886127' #TrackingRef '- 5 (CCDC_886127).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H100 Cl2 Mn6 N6 O24 P8' _chemical_formula_weight 1961.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 23.109(5) _cell_length_b 17.421(3) _cell_length_c 14.250(3) _cell_angle_alpha 90.00 _cell_angle_beta 128.07(3) _cell_angle_gamma 90.00 _cell_volume 4516.3(24) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6022 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.89 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2020 _exptl_absorpt_coefficient_mu 1.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.925 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details '(SADABS; Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _diffrn_measurement_method w-scan? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13201 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4094 _reflns_number_gt 3161 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; L.S. 5 omit -2 50 omit 1 1 1 FMAP 2 PLAN 20 ACTA isor 0.01 c3 isor 0.01 c13 isor 0.01 c33 BOND $H WGHT 0.128400 37.196899 FVAR 0.06929 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^)+(0.1284P)^2^+37.1969P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4094 _refine_ls_number_parameters 263 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1116 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2361 _refine_ls_wR_factor_gt 0.2223 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.068 _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 -0.13520(7) 0.5000 -0.50646(12) 0.0220(4) Uani 1 2 d S . . Mn2 Mn 0.10109(8) 0.5000 -0.22559(12) 0.0231(4) Uani 1 2 d S . . Mn3 Mn 0.0000 0.32653(8) -0.5000 0.0242(4) Uani 1 2 d S . . P1 P -0.02321(10) 0.37861(9) -0.31429(15) 0.0223(4) Uani 1 1 d . . . P2 P -0.16344(10) 0.37850(11) -0.69288(16) 0.0295(5) Uani 1 1 d . . . O1 O -0.0901(3) 0.4249(4) -0.3903(6) 0.064(2) Uani 1 1 d . . . O2 O 0.0414(4) 0.4267(4) -0.2320(5) 0.063(2) Uani 1 1 d . . . O3 O -0.0130(5) 0.3272(3) -0.3851(6) 0.069(2) Uani 1 1 d . . . O4 O -0.1768(3) 0.4254(4) -0.6218(6) 0.071(2) Uani 1 1 d . . . O5 O -0.0994(3) 0.3274(3) -0.6189(7) 0.072(2) Uani 1 1 d . . . O6 O -0.1572(4) 0.4255(4) -0.7737(5) 0.068(2) Uani 1 1 d . . . N1 N -0.2324(4) 0.5000 -0.5107(7) 0.033(2) Uani 1 2 d S . . N2 N 0.1723(5) 0.5000 -0.0304(7) 0.039(2) Uani 1 2 d S . . N3 N 0.0000 0.1998(5) -0.5000 0.036(2) Uani 1 2 d S . . C1 C -0.0342(5) 0.3177(4) -0.2229(7) 0.0390(19) Uani 1 1 d . . . C2 C -0.2416(5) 0.3155(6) -0.7829(8) 0.056(3) Uani 1 1 d . . . C3 C 0.292(2) 0.5000 0.158(3) 0.187(14) Uani 1 2 d SU . . H3A H 0.3426 0.5000 0.2019 0.225 Uiso 1 2 calc SR . . C12 C -0.0293(6) 0.1607(5) -0.5976(8) 0.059(3) Uani 1 1 d . . . H12A H -0.0516 0.1874 -0.6687 0.071 Uiso 1 1 calc R . . C13 C 0.0000 0.0427(5) -0.5000 0.033(2) Uani 1 2 d SU . . C14 C -0.0936(6) 0.2597(6) -0.3052(10) 0.070(3) Uani 1 1 d . . . H14A H -0.1012 0.2266 -0.2598 0.106 Uiso 1 1 calc R . . H14B H -0.0787 0.2296 -0.3434 0.106 Uiso 1 1 calc R . . H14C H -0.1385 0.2861 -0.3645 0.106 Uiso 1 1 calc R . . C15 C -0.0588(6) 0.3688(6) -0.1668(9) 0.059(3) Uani 1 1 d . . . H15A H -0.0656 0.3382 -0.1183 0.089 Uiso 1 1 calc R . . H15B H -0.1043 0.3933 -0.2284 0.089 Uiso 1 1 calc R . . H15C H -0.0220 0.4071 -0.1183 0.089 Uiso 1 1 calc R . . C16 C -0.0290(7) 0.0836(5) -0.6005(9) 0.064(3) Uani 1 1 d . . . H16A H -0.0488 0.0584 -0.6720 0.077 Uiso 1 1 calc R . . C18 C -0.2650(6) 0.4386(7) -0.5192(11) 0.073(3) Uani 1 1 d . . . H18A H -0.2435 0.3929 -0.5172 0.088 Uiso 1 1 calc R . . C19 C 0.0356(6) 0.2788(6) -0.1313(9) 0.063(3) Uani 1 1 d . . . H19A H 0.0293 0.2467 -0.0835 0.094 Uiso 1 1 calc R . . H19B H 0.0729 0.3164 -0.0815 0.094 Uiso 1 1 calc R . . H19C H 0.0502 0.2479 -0.1693 0.094 Uiso 1 1 calc R . . C23 C -0.2443(7) 0.2630(8) -0.7049(11) 0.101(5) Uani 1 1 d . . . H23A H -0.2860 0.2295 -0.7527 0.152 Uiso 1 1 calc R . . H23B H -0.2487 0.2922 -0.6524 0.152 Uiso 1 1 calc R . . H23C H -0.2001 0.2330 -0.6587 0.152 Uiso 1 1 calc R . . C30 C 0.1458(9) 0.5000 0.0295(11) 0.071(4) Uani 1 2 d S . . H30A H 0.0951 0.5000 -0.0136 0.085 Uiso 1 2 calc SR . . C31 C 0.1883(13) 0.5000 0.1495(16) 0.102(7) Uani 1 2 d S . . H31A H 0.1670 0.5000 0.1876 0.123 Uiso 1 2 calc SR . . C32 C 0.2575(12) 0.5000 0.2096(15) 0.152(13) Uani 1 2 d S . . H32A H 0.2865 0.5000 0.2923 0.183 Uiso 1 2 calc SR . . C33 C 0.2409(14) 0.5000 0.027(2) 0.125(8) Uani 1 2 d SU . . H33A H 0.2599 0.5000 -0.0151 0.149 Uiso 1 2 calc SR . . C34 C -0.3279(7) 0.4323(10) -0.5310(14) 0.110(6) Uani 1 1 d . . . H34A H -0.3467 0.3853 -0.5303 0.132 Uiso 1 1 calc R . . C35 C -0.3610(10) 0.5000 -0.544(2) 0.124(9) Uani 1 2 d S . . H35A H -0.4071 0.5000 -0.5619 0.148 Uiso 1 2 calc SR . . C36 C -0.2335(7) 0.2741(9) -0.8643(12) 0.112(6) Uani 1 1 d . . . H36A H -0.2743 0.2398 -0.9134 0.169 Uiso 1 1 calc R . . H36B H -0.1886 0.2452 -0.8187 0.169 Uiso 1 1 calc R . . H36C H -0.2323 0.3103 -0.9140 0.169 Uiso 1 1 calc R . . C37 C -0.3086(6) 0.3634(9) -0.8498(14) 0.134(7) Uani 1 1 d . . . H37A H -0.3511 0.3311 -0.8983 0.201 Uiso 1 1 calc R . . H37B H -0.3069 0.3986 -0.8999 0.201 Uiso 1 1 calc R . . H37C H -0.3114 0.3916 -0.7949 0.201 Uiso 1 1 calc R . . Cl1 Cl -0.5000 0.0000 -0.5000 0.0233(7) Uani 1 4 d S . . Cl2 Cl -0.0458(14) 0.0000 -0.840(2) 0.243(11) Uiso 0.50 2 d SP . . 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 0.0184(7) 0.0212(8) 0.0242(8) 0.000 0.0120(6) 0.000 Mn2 0.0230(8) 0.0231(8) 0.0153(7) 0.000 0.0078(6) 0.000 Mn3 0.0438(9) 0.0064(7) 0.0335(8) 0.000 0.0294(8) 0.000 P1 0.0344(10) 0.0116(8) 0.0264(9) 0.0022(7) 0.0214(8) -0.0002(7) P2 0.0253(10) 0.0321(11) 0.0270(10) -0.0139(8) 0.0140(8) -0.0185(8) O1 0.051(4) 0.083(5) 0.082(5) 0.059(4) 0.054(4) 0.026(3) O2 0.067(4) 0.080(5) 0.021(3) 0.000(3) 0.017(3) -0.049(4) O3 0.174(8) 0.011(3) 0.101(5) 0.004(3) 0.124(6) 0.004(4) O4 0.051(4) 0.088(5) 0.095(5) -0.076(4) 0.056(4) -0.052(4) O5 0.043(4) 0.018(3) 0.097(5) -0.014(3) 0.014(3) -0.017(3) O6 0.062(4) 0.087(5) 0.024(3) -0.015(3) 0.011(3) -0.058(4) N1 0.022(4) 0.045(6) 0.031(5) 0.000 0.016(4) 0.000 N2 0.028(5) 0.054(6) 0.016(4) 0.000 0.005(4) 0.000 N3 0.069(7) 0.010(4) 0.052(6) 0.000 0.048(5) 0.000 C1 0.059(5) 0.027(4) 0.048(5) 0.010(4) 0.041(4) -0.001(4) C2 0.042(5) 0.068(7) 0.051(5) -0.031(5) 0.025(4) -0.037(5) C3 0.182(16) 0.203(17) 0.175(16) 0.000 0.109(12) 0.000 C12 0.121(9) 0.011(4) 0.056(5) 0.003(4) 0.060(6) 0.003(5) C13 0.049(6) 0.011(5) 0.049(5) 0.000 0.036(5) 0.000 C14 0.102(9) 0.058(6) 0.077(7) -0.013(5) 0.068(7) -0.044(6) C15 0.099(8) 0.047(6) 0.068(6) 0.006(5) 0.070(6) 0.001(5) C16 0.129(9) 0.017(4) 0.060(6) -0.007(4) 0.066(7) -0.001(5) C18 0.064(7) 0.076(8) 0.104(9) -0.043(7) 0.064(7) -0.029(6) C19 0.078(7) 0.060(6) 0.065(6) 0.042(5) 0.051(6) 0.029(5) C23 0.112(10) 0.114(11) 0.077(8) -0.039(8) 0.058(8) -0.093(9) C30 0.071(10) 0.088(12) 0.029(7) 0.000 0.018(7) 0.000 C31 0.129(19) 0.123(18) 0.056(11) 0.000 0.057(13) 0.000 C32 0.070(13) 0.31(4) 0.024(9) 0.000 0.002(9) 0.000 C33 0.125(11) 0.153(12) 0.103(10) 0.000 0.074(9) 0.000 C34 0.090(10) 0.136(14) 0.157(14) -0.076(12) 0.103(11) -0.065(10) C35 0.044(10) 0.21(3) 0.126(18) 0.000 0.057(12) 0.000 C36 0.107(10) 0.147(13) 0.118(10) -0.115(10) 0.087(9) -0.103(10) C37 0.035(6) 0.113(12) 0.142(13) -0.054(10) -0.002(7) -0.035(7) Cl1 0.0228(16) 0.0168(16) 0.0246(16) 0.000 0.0118(14) 0.000 _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 O4 1.835(5) . ? Mn1 O4 1.835(5) 6_565 ? Mn1 O1 1.847(6) 6_565 ? Mn1 O1 1.847(6) . ? Mn1 N1 2.209(8) . ? Mn2 O6 1.840(6) 5_564 ? Mn2 O6 1.840(6) 2_554 ? Mn2 O2 1.840(5) . ? Mn2 O2 1.840(5) 6_565 ? Mn2 N2 2.191(8) . ? Mn3 O5 1.830(6) . ? Mn3 O5 1.830(6) 2_554 ? Mn3 O3 1.838(5) . ? Mn3 O3 1.838(5) 2_554 ? Mn3 N3 2.207(8) . ? P1 O2 1.465(6) . ? P1 O1 1.466(6) . ? P1 O3 1.473(5) . ? P1 C1 1.815(7) . ? P2 O5 1.473(7) . ? P2 O4 1.474(6) . ? P2 O6 1.490(6) . ? P2 C2 1.804(8) . ? O6 Mn2 1.840(6) 5_564 ? N1 C18 1.270(11) . ? N1 C18 1.270(11) 6_565 ? N2 C33 1.26(3) . ? N2 C30 1.321(18) . ? N3 C12 1.302(10) . ? N3 C12 1.302(10) 2_554 ? C1 C19 1.474(12) . ? C1 C14 1.515(12) . ? C1 C15 1.520(12) . ? C2 C23 1.470(15) . ? C2 C36 1.474(14) . ? C2 C37 1.477(17) . ? C3 C32 1.37(4) . ? C3 C33 1.47(4) . ? C3 H3A 0.9300 . ? C12 C16 1.344(12) . ? C12 H12A 0.9300 . ? C13 C16 1.352(10) 2_554 ? C13 C16 1.352(10) . ? C13 C13 1.487(19) 5_554 ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9300 . ? C18 C34 1.361(14) . ? C18 H18A 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C30 C31 1.35(2) . ? C30 H30A 0.9300 . ? C31 C32 1.27(3) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 C35 1.355(17) . ? C34 H34A 0.9300 . ? C35 C34 1.355(17) 6_565 ? C35 H35A 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 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 O4 Mn1 O4 90.2(6) . 6_565 ? O4 Mn1 O1 177.7(3) . 6_565 ? O4 Mn1 O1 89.7(4) 6_565 6_565 ? O4 Mn1 O1 89.7(4) . . ? O4 Mn1 O1 177.7(3) 6_565 . ? O1 Mn1 O1 90.2(5) 6_565 . ? O4 Mn1 N1 90.8(2) . . ? O4 Mn1 N1 90.8(2) 6_565 . ? O1 Mn1 N1 91.5(2) 6_565 . ? O1 Mn1 N1 91.5(2) . . ? O6 Mn2 O6 89.8(5) 5_564 2_554 ? O6 Mn2 O2 177.4(3) 5_564 . ? O6 Mn2 O2 91.2(4) 2_554 . ? O6 Mn2 O2 91.2(4) 5_564 6_565 ? O6 Mn2 O2 177.4(3) 2_554 6_565 ? O2 Mn2 O2 87.8(5) . 6_565 ? O6 Mn2 N2 91.5(3) 5_564 . ? O6 Mn2 N2 91.5(3) 2_554 . ? O2 Mn2 N2 90.9(2) . . ? O2 Mn2 N2 90.9(2) 6_565 . ? O5 Mn3 O5 179.1(4) . 2_554 ? O5 Mn3 O3 91.3(4) . . ? O5 Mn3 O3 88.7(4) 2_554 . ? O5 Mn3 O3 88.7(4) . 2_554 ? O5 Mn3 O3 91.3(4) 2_554 2_554 ? O3 Mn3 O3 179.3(3) . 2_554 ? O5 Mn3 N3 90.45(18) . . ? O5 Mn3 N3 90.45(18) 2_554 . ? O3 Mn3 N3 90.34(16) . . ? O3 Mn3 N3 90.34(16) 2_554 . ? O2 P1 O1 111.5(4) . . ? O2 P1 O3 112.5(5) . . ? O1 P1 O3 111.7(4) . . ? O2 P1 C1 106.5(3) . . ? O1 P1 C1 107.5(3) . . ? O3 P1 C1 106.8(3) . . ? O5 P2 O4 112.7(5) . . ? O5 P2 O6 110.7(5) . . ? O4 P2 O6 112.8(5) . . ? O5 P2 C2 105.3(4) . . ? O4 P2 C2 106.5(4) . . ? O6 P2 C2 108.4(4) . . ? P1 O1 Mn1 143.8(4) . . ? P1 O2 Mn2 143.0(3) . . ? P1 O3 Mn3 142.8(3) . . ? P2 O4 Mn1 142.4(4) . . ? P2 O5 Mn3 143.2(4) . . ? P2 O6 Mn2 142.7(3) . 5_564 ? C18 N1 C18 114.7(12) . 6_565 ? C18 N1 Mn1 122.4(6) . . ? C18 N1 Mn1 122.4(6) 6_565 . ? C33 N2 C30 119.0(15) . . ? C33 N2 Mn2 118.7(13) . . ? C30 N2 Mn2 122.4(8) . . ? C12 N3 C12 116.9(9) . 2_554 ? C12 N3 Mn3 121.5(5) . . ? C12 N3 Mn3 121.5(5) 2_554 . ? C19 C1 C14 110.7(8) . . ? C19 C1 C15 111.4(8) . . ? C14 C1 C15 110.1(8) . . ? C19 C1 P1 110.0(6) . . ? C14 C1 P1 107.2(6) . . ? C15 C1 P1 107.4(5) . . ? C23 C2 C36 112.1(11) . . ? C23 C2 C37 108.9(12) . . ? C36 C2 C37 111.1(11) . . ? C23 C2 P2 109.4(7) . . ? C36 C2 P2 107.4(7) . . ? C37 C2 P2 107.9(8) . . ? C32 C3 C33 114(3) . . ? C32 C3 H3A 122.9 . . ? C33 C3 H3A 122.9 . . ? N3 C12 C16 123.2(9) . . ? N3 C12 H12A 118.4 . . ? C16 C12 H12A 118.4 . . ? C16 C13 C16 116.3(10) 2_554 . ? C16 C13 C13 121.9(5) 2_554 5_554 ? C16 C13 C13 121.9(5) . 5_554 ? C1 C14 H14A 109.5 . . ? C1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1 C15 H15A 109.5 . . ? C1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C13 120.2(9) . . ? C12 C16 H16A 119.9 . . ? C13 C16 H16A 119.9 . . ? N1 C18 C34 127.2(12) . . ? N1 C18 H18A 116.4 . . ? C34 C18 H18A 116.4 . . ? C1 C19 H19A 109.5 . . ? C1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C30 C31 123.7(17) . . ? N2 C30 H30A 118.2 . . ? C31 C30 H30A 118.2 . . ? C32 C31 C30 119(2) . . ? C32 C31 H31A 120.5 . . ? C30 C31 H31A 120.5 . . ? C31 C32 C3 123(2) . . ? C31 C32 H32A 118.6 . . ? C3 C32 H32A 118.6 . . ? N2 C33 C3 121(2) . . ? N2 C33 H33A 119.4 . . ? C3 C33 H33A 119.4 . . ? C35 C34 C18 114.6(15) . . ? C35 C34 H34A 122.7 . . ? C18 C34 H34A 122.7 . . ? C34 C35 C34 121.1(17) 6_565 . ? C34 C35 H35A 119.5 6_565 . ? C34 C35 H35A 119.5 . . ? C2 C36 H36A 109.5 . . ? C2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C2 C37 H37A 109.5 . . ? C2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.903 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.159 data_a3 _database_code_depnum_ccdc_archive 'CCDC 886524' #TrackingRef '- 3 (CCDC_886524).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H96 Cl2 Mn6 N0 O32 P8' _chemical_formula_weight 1689.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4/m' _symmetry_space_group_name_Hall '-I 4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 14.133(2) _cell_length_b 14.133(2) _cell_length_c 21.552(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4304.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3011 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 27.34 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 0.893 _exptl_absorpt_process_details '(SADABS; Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _diffrn_measurement_method w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9924 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1959 _reflns_number_gt 1828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1124P)^2^+35.7480P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1959 _refine_ls_number_parameters 107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1850 _refine_ls_wR_factor_gt 0.1816 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _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 0.0000 0.0000 0.14367(6) 0.0217(4) Uani 1 4 d S . . Mn2 Mn 0.11288(6) 0.18858(6) 0.0000 0.0200(3) Uani 1 2 d S . . P1 P 0.20856(7) 0.05165(8) 0.09950(5) 0.0219(3) Uani 1 1 d . . . O1 O 0.1901(3) 0.1374(3) 0.0607(2) 0.0676(16) Uani 1 1 d . . . O2 O 0.1276(3) 0.0292(4) 0.14189(17) 0.0715(17) Uani 1 1 d . . . O4 O 0.0000 0.0000 0.2451(3) 0.0429(17) Uani 1 4 d S . . O5 O 0.1970(4) 0.3183(3) 0.0000 0.0367(11) Uani 1 2 d S . . O3 O 0.2359(3) -0.0317(3) 0.0606(2) 0.0668(15) Uani 1 1 d . . . C2 C 0.3937(4) 0.1034(5) 0.1082(3) 0.0567(17) Uani 1 1 d . . . H2A H 0.4470 0.1183 0.1341 0.085 Uiso 1 1 calc R . . H2B H 0.3790 0.1569 0.0825 0.085 Uiso 1 1 calc R . . H2C H 0.4089 0.0500 0.0825 0.085 Uiso 1 1 calc R . . C1 C 0.3092(3) 0.0798(3) 0.1485(2) 0.0300(10) Uani 1 1 d . . . C3 C 0.3326(5) -0.0059(5) 0.1890(3) 0.0593(18) Uani 1 1 d . . . H3A H 0.3859 0.0086 0.2149 0.089 Uiso 1 1 calc R . . H3B H 0.3477 -0.0590 0.1630 0.089 Uiso 1 1 calc R . . H3C H 0.2790 -0.0211 0.2144 0.089 Uiso 1 1 calc R . . C4 C 0.2828(5) 0.1641(5) 0.1889(3) 0.064(2) Uani 1 1 d . . . H4B H 0.3352 0.1802 0.2152 0.096 Uiso 1 1 calc R . . H4C H 0.2291 0.1481 0.2141 0.096 Uiso 1 1 calc R . . H4D H 0.2674 0.2172 0.1630 0.096 Uiso 1 1 calc R . . Cl1 Cl 0.0000 0.0000 0.0000 0.0274(6) Uani 1 8 d S . . O1W O 0.0000 0.0000 0.4717(8) 0.129(6) Uani 1 4 d S . . C5 C 0.1514(10) 0.4097(7) 0.0000 0.104(5) Uani 1 2 d S . . H5A H 0.1985 0.4587 0.0000 0.156 Uiso 1 2 d SR . . H5B H 0.1126 0.4156 -0.0364 0.156 Uiso 0.50 1 d PR . . Cl2 Cl 0.1572(16) 0.1256(16) 0.4205(11) 0.098(5) Uiso 0.13 1 d P . . 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 0.0240(5) 0.0240(5) 0.0173(6) 0.000 0.000 0.000 Mn2 0.0206(5) 0.0212(5) 0.0183(5) 0.000 0.000 0.0008(3) P1 0.0219(6) 0.0243(6) 0.0197(6) -0.0008(4) -0.0039(4) -0.0008(4) O1 0.072(3) 0.042(2) 0.089(3) 0.035(2) -0.063(3) -0.030(2) O2 0.0313(19) 0.164(5) 0.0193(18) 0.004(2) -0.0030(15) -0.034(3) O4 0.056(3) 0.056(3) 0.017(3) 0.000 0.000 0.000 O5 0.040(3) 0.023(2) 0.047(3) 0.000 0.000 -0.0041(19) O3 0.038(2) 0.070(3) 0.093(3) -0.059(3) -0.037(2) 0.028(2) C2 0.033(3) 0.080(5) 0.057(4) 0.004(3) -0.009(3) -0.017(3) C1 0.028(2) 0.031(2) 0.031(2) -0.0009(19) -0.0118(19) -0.0018(18) C3 0.059(4) 0.056(4) 0.063(4) 0.020(3) -0.036(3) -0.004(3) C4 0.061(4) 0.066(4) 0.066(4) -0.038(3) -0.029(3) 0.008(3) Cl1 0.0291(9) 0.0291(9) 0.0240(14) 0.000 0.000 0.000 O1W 0.134(8) 0.134(8) 0.121(13) 0.000 0.000 0.000 C5 0.084(8) 0.029(5) 0.200(17) 0.000 0.000 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O2 1.850(4) 3 ? Mn1 O2 1.850(4) 4 ? Mn1 O2 1.850(4) . ? Mn1 O2 1.850(4) 2 ? Mn1 O4 2.185(7) . ? Mn2 O1 1.851(4) . ? Mn2 O1 1.851(4) 11 ? Mn2 O3 1.863(4) 2 ? Mn2 O3 1.863(4) 12 ? Mn2 O5 2.185(5) . ? P1 O1 1.495(4) . ? P1 O3 1.496(4) . ? P1 O2 1.498(4) . ? P1 C1 1.815(4) . ? O5 C5 1.443(11) . ? O3 Mn2 1.863(4) 10 ? C2 C1 1.514(8) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C1 C4 1.524(8) . ? C1 C3 1.529(7) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4 H4D 0.9600 . ? O1W O1W 1.22(3) 9_556 ? C5 H5A 0.9603 . ? C5 H5B 0.9601 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mn1 O2 89.975(5) 3 4 ? O2 Mn1 O2 177.6(2) 3 . ? O2 Mn1 O2 89.975(5) 4 . ? O2 Mn1 O2 89.975(5) 3 2 ? O2 Mn1 O2 177.6(2) 4 2 ? O2 Mn1 O2 89.975(5) . 2 ? O2 Mn1 O4 91.19(12) 3 . ? O2 Mn1 O4 91.19(12) 4 . ? O2 Mn1 O4 91.19(12) . . ? O2 Mn1 O4 91.19(12) 2 . ? O1 Mn2 O1 89.9(4) . 11 ? O1 Mn2 O3 90.5(3) . 2 ? O1 Mn2 O3 177.63(17) 11 2 ? O1 Mn2 O3 177.63(17) . 12 ? O1 Mn2 O3 90.5(3) 11 12 ? O3 Mn2 O3 89.1(4) 2 12 ? O1 Mn2 O5 90.42(15) . . ? O1 Mn2 O5 90.42(15) 11 . ? O3 Mn2 O5 91.92(15) 2 . ? O3 Mn2 O5 91.92(15) 12 . ? O1 P1 O3 111.7(3) . . ? O1 P1 O2 112.3(3) . . ? O3 P1 O2 111.8(3) . . ? O1 P1 C1 106.5(2) . . ? O3 P1 C1 107.2(2) . . ? O2 P1 C1 106.9(2) . . ? P1 O1 Mn2 144.6(2) . . ? P1 O2 Mn1 143.5(2) . . ? C5 O5 Mn2 120.6(6) . . ? P1 O3 Mn2 141.7(2) . 10 ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C1 C4 110.4(5) . . ? C2 C1 C3 109.4(5) . . ? C4 C1 C3 110.2(5) . . ? C2 C1 P1 109.5(4) . . ? C4 C1 P1 108.2(4) . . ? C3 C1 P1 109.2(3) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C1 C4 H4D 109.5 . . ? H4B C4 H4D 109.5 . . ? H4C C4 H4D 109.5 . . ? O5 C5 H5A 109.6 . . ? O5 C5 H5B 109.4 . . ? H5A C5 H5B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 Mn2 64.0(7) . . . . ? O2 P1 O1 Mn2 -62.6(8) . . . . ? C1 P1 O1 Mn2 -179.3(6) . . . . ? O1 Mn2 O1 P1 -87.8(7) 11 . . . ? O3 Mn2 O1 P1 89.9(7) 2 . . . ? O3 Mn2 O1 P1 11(7) 12 . . . ? O5 Mn2 O1 P1 -178.2(7) . . . . ? O1 P1 O2 Mn1 59.0(7) . . . . ? O3 P1 O2 Mn1 -67.5(7) . . . . ? C1 P1 O2 Mn1 175.5(6) . . . . ? O2 Mn1 O2 P1 3.5(7) 3 . . . ? O2 Mn1 O2 P1 92.3(7) 4 . . . ? O2 Mn1 O2 P1 -85.3(7) 2 . . . ? O4 Mn1 O2 P1 -176.5(7) . . . . ? O1 Mn2 O5 C5 -135.06(19) . . . . ? O1 Mn2 O5 C5 135.06(19) 11 . . . ? O3 Mn2 O5 C5 -44.6(2) 2 . . . ? O3 Mn2 O5 C5 44.6(2) 12 . . . ? O1 P1 O3 Mn2 -64.7(7) . . . 10 ? O2 P1 O3 Mn2 62.2(7) . . . 10 ? C1 P1 O3 Mn2 179.0(6) . . . 10 ? O1 P1 C1 C2 -59.6(5) . . . . ? O3 P1 C1 C2 60.1(5) . . . . ? O2 P1 C1 C2 -179.9(4) . . . . ? O1 P1 C1 C4 60.8(5) . . . . ? O3 P1 C1 C4 -179.5(5) . . . . ? O2 P1 C1 C4 -59.5(5) . . . . ? O1 P1 C1 C3 -179.3(5) . . . . ? O3 P1 C1 C3 -59.6(5) . . . . ? O2 P1 C1 C3 60.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.726 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.168 data_a4 _database_code_depnum_ccdc_archive 'CCDC 886525' #TrackingRef '- 4 (CCDC_886525).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H96 Cl2 Mn6 N4 O30 P8' _chemical_formula_weight 1953.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 52.51(2) _cell_length_b 15.806(3) _cell_length_c 23.396(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.45(2) _cell_angle_gamma 90.00 _cell_volume 17385(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21342 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 28.01 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8032 _exptl_absorpt_coefficient_mu 1.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details '(SADABS; Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX CCD' _diffrn_measurement_method w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39570 _diffrn_reflns_av_R_equivalents 0.0773 _diffrn_reflns_av_sigmaI/netI 0.1044 _diffrn_reflns_limit_h_min -62 _diffrn_reflns_limit_h_max 62 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15294 _reflns_number_gt 9323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement 'SMART (Bruker, 1997)' _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; FMAP 2 PLAN 20 ACTA htab dfix 0.85 0.01 o1w h1wa dfix 0.85 0.01 o1w h1wb dfix 1.34 0.02 h1wa h1wb dfix 0.85 0.01 o2w h2wa dfix 0.85 0.01 o2w h2wb dfix 1.34 0.02 h2wa h2wb omit -2 50 omit 4 10 0 omit 9 11 1 omit -14 10 6 BOND $H WGHT 0.0799 123.3392 FVAR 0.01702 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^)+(0.0799P)^2^+123.3392P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15294 _refine_ls_number_parameters 979 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1201 _refine_ls_R_factor_gt 0.0747 _refine_ls_wR_factor_ref 0.1989 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.007 _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 -0.06052(2) -0.25884(6) -0.02793(5) 0.0163(3) Uani 1 1 d . . . Mn2 Mn -0.18857(2) -0.25427(6) -0.22069(5) 0.0165(3) Uani 1 1 d . . . Mn3 Mn -0.14048(2) -0.28523(7) -0.01244(5) 0.0170(3) Uani 1 1 d . . . Mn4 Mn -0.10805(2) -0.22973(7) -0.23548(5) 0.0178(3) Uani 1 1 d . . . Mn5 Mn -0.12591(2) -0.06425(7) -0.10717(5) 0.0218(3) Uani 1 1 d . . . Mn6 Mn -0.12323(2) -0.44844(7) -0.14180(5) 0.0204(3) Uani 1 1 d . . . P1 P -0.15655(4) -0.36965(12) -0.28078(9) 0.0199(4) Uani 1 1 d . . . P2 P -0.06757(4) -0.37340(12) -0.14522(9) 0.0196(4) Uani 1 1 d . . . P3 P -0.17902(4) -0.40869(12) -0.12647(9) 0.0199(4) Uani 1 1 d . . . P4 P -0.06999(4) -0.10502(12) -0.12264(9) 0.0213(4) Uani 1 1 d . . . P5 P -0.18109(4) -0.14030(12) -0.10252(9) 0.0209(4) Uani 1 1 d . . . P6 P -0.09219(4) -0.14433(12) 0.03195(9) 0.0205(4) Uani 1 1 d . . . P7 P -0.15837(4) -0.10189(12) -0.25568(9) 0.0217(4) Uani 1 1 d . . . P8 P -0.09085(4) -0.41270(12) 0.00699(9) 0.0199(4) Uani 1 1 d . . . O1W O -0.12674(16) 0.0693(4) -0.0825(3) 0.064(2) Uani 1 1 d D . . H1WA H -0.1122 0.0988 -0.0768 0.096 Uiso 1 1 d RD . . H1WB H -0.1375 0.0767 -0.1225 0.096 Uiso 1 1 d RD . . O2 O 0.07880(15) -0.2833(5) 0.2407(3) 0.069(2) Uani 1 1 d . . . O2W O -0.12085(14) -0.5820(3) -0.1636(3) 0.0512(17) Uani 1 1 d D . . H2WA H -0.1352 -0.6011 -0.1966 0.077 Uiso 1 1 d RD . . H2WB H -0.1218 -0.6100 -0.1331 0.077 Uiso 1 1 d RD . . O3 O -0.13961(10) -0.2970(3) -0.2900(2) 0.0215(11) Uani 1 1 d . . . O4 O -0.15639(11) -0.0792(3) -0.0861(2) 0.0272(12) Uani 1 1 d . . . O6 O -0.05663(10) -0.1530(3) -0.0597(2) 0.0239(12) Uani 1 1 d . . . O7 O -0.11824(10) -0.1904(3) 0.0291(2) 0.0216(11) Uani 1 1 d . . . O8 O -0.05214(10) -0.3131(3) -0.0899(2) 0.0227(12) Uani 1 1 d . . . O9 O -0.15175(11) -0.0546(3) -0.1933(2) 0.0242(12) Uani 1 1 d . . . O10 O -0.09991(10) -0.0794(3) -0.0201(2) 0.0252(12) Uani 1 1 d . . . O12 O -0.06696(10) -0.3653(3) -0.0001(2) 0.0217(11) Uani 1 1 d . . . O14 O -0.16201(10) -0.3795(3) -0.0577(2) 0.0221(11) Uani 1 1 d . . . O15 O -0.20823(18) -0.2428(5) 0.1951(4) 0.077(3) Uani 1 1 d . . . O16 O -0.13144(11) -0.1340(3) -0.2589(2) 0.0236(12) Uani 1 1 d . . . O17 O -0.06956(10) -0.2060(3) 0.0329(2) 0.0213(11) Uani 1 1 d . . . O18 O -0.17265(11) -0.2161(3) -0.0568(2) 0.0237(12) Uani 1 1 d . . . O19 O -0.19590(10) -0.3372(3) -0.1711(2) 0.0230(12) Uani 1 1 d . . . O20 O -0.09568(11) -0.0533(3) -0.1291(2) 0.0260(12) Uani 1 1 d . . . O21 O -0.08565(10) -0.4362(3) -0.1311(2) 0.0237(12) Uani 1 1 d . . . O22 O -0.07715(10) -0.1622(3) -0.1799(2) 0.0237(12) Uani 1 1 d . . . O24 O -0.13724(11) -0.4323(3) -0.2309(2) 0.0226(12) Uani 1 1 d . . . O25 O -0.18083(10) -0.3387(3) -0.2677(2) 0.0217(11) Uani 1 1 d . . . O28 O -0.10816(11) -0.3555(3) 0.0290(2) 0.0241(12) Uani 1 1 d . . . O30 O -0.10972(10) -0.4620(3) -0.0536(2) 0.0223(11) Uani 1 1 d . . . O32 O -0.18015(10) -0.1720(3) -0.2680(2) 0.0220(11) Uani 1 1 d . . . O33 O -0.16080(10) -0.4546(3) -0.1522(2) 0.0243(12) Uani 1 1 d . . . O35 O -0.19411(11) -0.1689(3) -0.1718(2) 0.0248(12) Uani 1 1 d . . . O54 O -0.32544(15) -0.2868(5) -0.4942(3) 0.067(2) Uani 1 1 d . . . O56 O -0.08445(10) -0.3261(3) -0.2085(2) 0.0197(11) Uani 1 1 d . . . O86 O -0.03984(18) -0.2092(5) -0.4432(4) 0.069(2) Uani 1 1 d . . . N5 N -0.01464(13) -0.2636(4) 0.0447(3) 0.0231(15) Uani 1 1 d . . . N11 N -0.23444(13) -0.2559(4) -0.2933(3) 0.0235(15) Uani 1 1 d . . . N23 N -0.09461(13) -0.2131(4) -0.3137(3) 0.0219(14) Uani 1 1 d . . . N26 N -0.15529(13) -0.2961(4) 0.0646(3) 0.0215(14) Uani 1 1 d . . . C4 C -0.04394(17) -0.0284(5) -0.1220(4) 0.033(2) Uani 1 1 d . . . C5 C -0.20378(17) -0.4873(5) -0.1237(4) 0.0298(19) Uani 1 1 d . . . C6 C -0.1865(2) -0.5586(6) -0.0801(5) 0.049(3) Uani 1 1 d . . . H6A H -0.1990 -0.5972 -0.0733 0.073 Uiso 1 1 calc R . . H6B H -0.1731 -0.5356 -0.0399 0.073 Uiso 1 1 calc R . . H6C H -0.1764 -0.5882 -0.0996 0.073 Uiso 1 1 calc R . . C7 C -0.05871(19) -0.5560(5) 0.0436(4) 0.041(2) Uani 1 1 d . . . H7A H -0.0492 -0.5981 0.0757 0.062 Uiso 1 1 calc R . . H7B H -0.0451 -0.5269 0.0338 0.062 Uiso 1 1 calc R . . H7C H -0.0726 -0.5829 0.0057 0.062 Uiso 1 1 calc R . . C8 C -0.22232(19) -0.5186(6) -0.1910(4) 0.044(2) Uani 1 1 d . . . H8A H -0.2343 -0.5636 -0.1896 0.066 Uiso 1 1 calc R . . H8B H -0.2105 -0.5390 -0.2096 0.066 Uiso 1 1 calc R . . H8C H -0.2339 -0.4729 -0.2163 0.066 Uiso 1 1 calc R . . C9 C 0.0717(2) -0.2753(6) 0.1854(5) 0.053(3) Uani 1 1 d . . . H9A H 0.0858 -0.2726 0.1716 0.063 Uiso 1 1 calc R . . C10 C -0.09627(19) -0.5374(6) 0.0818(5) 0.048(3) Uani 1 1 d . . . H10A H -0.0877 -0.5825 0.1118 0.072 Uiso 1 1 calc R . . H10B H -0.1108 -0.5600 0.0429 0.072 Uiso 1 1 calc R . . H10C H -0.1045 -0.4970 0.0994 0.072 Uiso 1 1 calc R . . C12 C -0.0517(2) -0.4491(6) 0.1293(4) 0.046(2) Uani 1 1 d . . . H12A H -0.0429 -0.4903 0.1626 0.070 Uiso 1 1 calc R . . H12B H -0.0614 -0.4076 0.1425 0.070 Uiso 1 1 calc R . . H12C H -0.0374 -0.4217 0.1210 0.070 Uiso 1 1 calc R . . C13 C -0.3190(2) -0.2881(6) -0.4391(5) 0.053(3) Uani 1 1 d . . . H13A H -0.3331 -0.2978 -0.4264 0.064 Uiso 1 1 calc R . . C14 C -0.01714(18) -0.0774(6) -0.1137(4) 0.040(2) Uani 1 1 d . . . H14A H -0.0030 -0.0383 -0.1130 0.060 Uiso 1 1 calc R . . H14B H -0.0220 -0.1161 -0.1486 0.060 Uiso 1 1 calc R . . H14C H -0.0097 -0.1084 -0.0742 0.060 Uiso 1 1 calc R . . C16 C -0.2224(2) -0.4456(6) -0.0959(5) 0.052(3) Uani 1 1 d . . . H16A H -0.2364 -0.4853 -0.0970 0.078 Uiso 1 1 calc R . . H16B H -0.2316 -0.3967 -0.1208 0.078 Uiso 1 1 calc R . . H16C H -0.2106 -0.4289 -0.0525 0.078 Uiso 1 1 calc R . . C17 C -0.03697(19) 0.0304(5) -0.0656(4) 0.041(2) Uani 1 1 d . . . H17A H -0.0220 0.0682 -0.0617 0.061 Uiso 1 1 calc R . . H17B H -0.0310 -0.0023 -0.0272 0.061 Uiso 1 1 calc R . . H17C H -0.0536 0.0626 -0.0723 0.061 Uiso 1 1 calc R . . C18 C -0.0567(2) 0.0190(6) -0.1852(4) 0.047(3) Uani 1 1 d . . . H18A H -0.0439 0.0629 -0.1843 0.070 Uiso 1 1 calc R . . H18B H -0.0745 0.0436 -0.1919 0.070 Uiso 1 1 calc R . . H18C H -0.0598 -0.0196 -0.2193 0.070 Uiso 1 1 calc R . . C19 C -0.2003(2) 0.0121(7) -0.3162(5) 0.068(3) Uani 1 1 d . . . H19A H -0.2091 0.0527 -0.3498 0.102 Uiso 1 1 calc R . . H19B H -0.1945 0.0393 -0.2756 0.102 Uiso 1 1 calc R . . H19C H -0.2136 -0.0323 -0.3210 0.102 Uiso 1 1 calc R . . C20 C -0.1824(3) -0.0689(7) -0.3824(5) 0.071(4) Uani 1 1 d . . . H20A H -0.1912 -0.0288 -0.4165 0.107 Uiso 1 1 calc R . . H20B H -0.1956 -0.1137 -0.3873 0.107 Uiso 1 1 calc R . . H20C H -0.1657 -0.0920 -0.3835 0.107 Uiso 1 1 calc R . . C27 C -0.06697(17) -0.2055(5) -0.2982(4) 0.0303(19) Uani 1 1 d . . . H27A H -0.0542 -0.2011 -0.2552 0.036 Uiso 1 1 calc R . . C29 C -0.07332(17) -0.4935(5) 0.0679(4) 0.0296(19) Uani 1 1 d . . . C31 C -0.00763(19) -0.2644(5) 0.1072(4) 0.032(2) Uani 1 1 d . . . H31A H -0.0222 -0.2615 0.1195 0.038 Uiso 1 1 calc R . . C34 C -0.17299(17) -0.4281(5) -0.3553(4) 0.0300(19) Uani 1 1 d . . . C36 C -0.20880(17) -0.0815(5) -0.0938(4) 0.032(2) Uani 1 1 d . . . C37 C -0.1742(2) -0.0254(6) -0.3196(4) 0.045(2) Uani 1 1 d . . . C38 C -0.19311(18) -0.2748(5) 0.0936(4) 0.032(2) Uani 1 1 d . . . H38A H -0.2124 -0.2672 0.0810 0.038 Uiso 1 1 calc R . . C39 C -0.05645(18) -0.2039(6) -0.3426(4) 0.036(2) Uani 1 1 d . . . H39A H -0.0370 -0.1988 -0.3299 0.043 Uiso 1 1 calc R . . C40 C -0.04056(17) -0.4354(5) -0.1545(4) 0.0300(19) Uani 1 1 d . . . C41 C -0.05595(19) -0.4967(6) -0.2109(4) 0.046(2) Uani 1 1 d . . . H41A H -0.0422 -0.5328 -0.2154 0.069 Uiso 1 1 calc R . . H41B H -0.0660 -0.4649 -0.2495 0.069 Uiso 1 1 calc R . . H41C H -0.0692 -0.5306 -0.2029 0.069 Uiso 1 1 calc R . . C42 C -0.23461(18) -0.1384(6) -0.1108(5) 0.049(3) Uani 1 1 d . . . H42A H -0.2503 -0.1052 -0.1132 0.073 Uiso 1 1 calc R . . H42B H -0.2302 -0.1813 -0.0787 0.073 Uiso 1 1 calc R . . H42C H -0.2396 -0.1647 -0.1514 0.073 Uiso 1 1 calc R . . C43 C 0.00677(16) -0.2645(5) 0.0281(4) 0.0289(19) Uani 1 1 d . . . H43A H 0.0024 -0.2624 -0.0150 0.035 Uiso 1 1 calc R . . C44 C -0.14542(19) -0.2869(5) 0.1748(4) 0.036(2) Uani 1 1 d . . . H44A H -0.1322 -0.2883 0.2176 0.043 Uiso 1 1 calc R . . C47 C -0.10347(19) -0.2171(5) -0.4233(4) 0.035(2) Uani 1 1 d . . . H47A H -0.1165 -0.2205 -0.4662 0.042 Uiso 1 1 calc R . . C49 C -0.07530(19) -0.2100(5) -0.4060(4) 0.032(2) Uani 1 1 d . . . C50 C -0.14932(18) -0.4656(6) -0.3697(4) 0.041(2) Uani 1 1 d . . . H50A H -0.1577 -0.4927 -0.4107 0.062 Uiso 1 1 calc R . . H50B H -0.1386 -0.5062 -0.3375 0.062 Uiso 1 1 calc R . . H50C H -0.1369 -0.4210 -0.3700 0.062 Uiso 1 1 calc R . . C52 C -0.25568(17) -0.2734(5) -0.2788(4) 0.0305(19) Uani 1 1 d . . . H52A H -0.2518 -0.2792 -0.2362 0.037 Uiso 1 1 calc R . . C54 C -0.28939(17) -0.2750(5) -0.3889(4) 0.0297(19) Uani 1 1 d . . . C55 C -0.17368(19) -0.2748(5) 0.1575(4) 0.033(2) Uani 1 1 d . . . C57 C -0.24038(18) -0.2472(5) -0.3550(4) 0.0269(19) Uani 1 1 d . . . H57A H -0.2257 -0.2338 -0.3653 0.032 Uiso 1 1 calc R . . C58 C -0.1839(3) -0.2599(7) 0.2067(5) 0.062(3) Uani 1 1 d . . . H58A H -0.1707 -0.2640 0.2493 0.075 Uiso 1 1 calc R . . C59 C -0.02372(18) -0.4846(5) -0.0935(4) 0.038(2) Uani 1 1 d . . . H59A H -0.0099 -0.5195 -0.0986 0.057 Uiso 1 1 calc R . . H59B H -0.0364 -0.5196 -0.0844 0.057 Uiso 1 1 calc R . . H59C H -0.0142 -0.4458 -0.0589 0.057 Uiso 1 1 calc R . . C61 C 0.04141(17) -0.2695(5) 0.1364(4) 0.032(2) Uani 1 1 d . . . C62 C -0.26744(19) -0.2572(5) -0.4038(4) 0.033(2) Uani 1 1 d . . . H62A H -0.2708 -0.2519 -0.4461 0.040 Uiso 1 1 calc R . . C63 C -0.13697(18) -0.2971(5) 0.1269(4) 0.0299(19) Uani 1 1 d . . . H63A H -0.1177 -0.3050 0.1384 0.036 Uiso 1 1 calc R . . C64 C -0.0989(2) -0.0236(5) 0.1078(4) 0.045(2) Uani 1 1 d . . . H64A H -0.0910 0.0064 0.1477 0.068 Uiso 1 1 calc R . . H64B H -0.1154 -0.0543 0.1033 0.068 Uiso 1 1 calc R . . H64C H -0.1041 0.0161 0.0733 0.068 Uiso 1 1 calc R . . C66 C -0.07683(17) -0.0853(5) 0.1062(4) 0.0284(19) Uani 1 1 d . . . C67 C -0.28355(17) -0.2834(5) -0.3258(4) 0.031(2) Uani 1 1 d . . . H67A H -0.2980 -0.2956 -0.3146 0.038 Uiso 1 1 calc R . . C68 C -0.1526(2) 0.0442(6) -0.3108(5) 0.049(3) Uani 1 1 d . . . H68A H -0.1611 0.0860 -0.3437 0.074 Uiso 1 1 calc R . . H68B H -0.1364 0.0201 -0.3134 0.074 Uiso 1 1 calc R . . H68C H -0.1467 0.0702 -0.2698 0.074 Uiso 1 1 calc R . . C71 C -0.1914(2) -0.3665(6) -0.4106(4) 0.047(2) Uani 1 1 d . . . H71A H -0.2000 -0.3973 -0.4500 0.070 Uiso 1 1 calc R . . H71B H -0.1796 -0.3225 -0.4139 0.070 Uiso 1 1 calc R . . H71C H -0.2060 -0.3420 -0.4017 0.070 Uiso 1 1 calc R . . C72 C -0.1915(2) -0.4984(6) -0.3477(5) 0.051(3) Uani 1 1 d . . . H72A H -0.1964 -0.5387 -0.3816 0.077 Uiso 1 1 calc R . . H72B H -0.2086 -0.4740 -0.3494 0.077 Uiso 1 1 calc R . . H72C H -0.1811 -0.5262 -0.3074 0.077 Uiso 1 1 calc R . . C73 C -0.18281(16) -0.2863(5) 0.0499(4) 0.0289(19) Uani 1 1 d . . . H73A H -0.1958 -0.2874 0.0070 0.035 Uiso 1 1 calc R . . C74 C 0.01976(18) -0.2692(6) 0.1538(4) 0.038(2) Uani 1 1 d . . . H74A H 0.0236 -0.2723 0.1966 0.045 Uiso 1 1 calc R . . C76 C -0.04993(19) -0.0389(6) 0.1103(4) 0.044(2) Uani 1 1 d . . . H76A H -0.0415 -0.0064 0.1490 0.066 Uiso 1 1 calc R . . H76B H -0.0552 -0.0018 0.0743 0.066 Uiso 1 1 calc R . . H76C H -0.0364 -0.0798 0.1101 0.066 Uiso 1 1 calc R . . C81 C -0.0645(2) -0.2091(6) -0.4548(5) 0.046(2) Uani 1 1 d . . . H81A H -0.0778 -0.2083 -0.4975 0.055 Uiso 1 1 calc R . . C83 C -0.0677(2) -0.1492(5) 0.1626(4) 0.044(2) Uani 1 1 d . . . H83A H -0.0595 -0.1190 0.2024 0.066 Uiso 1 1 calc R . . H83B H -0.0539 -0.1879 0.1611 0.066 Uiso 1 1 calc R . . H83C H -0.0841 -0.1802 0.1592 0.066 Uiso 1 1 calc R . . C90 C -0.11271(17) -0.2190(5) -0.3755(4) 0.0270(18) Uani 1 1 d . . . H90A H -0.1320 -0.2246 -0.3873 0.032 Uiso 1 1 calc R . . C91 C -0.2168(2) -0.0058(6) -0.1388(4) 0.045(2) Uani 1 1 d . . . H91A H -0.2313 0.0264 -0.1347 0.068 Uiso 1 1 calc R . . H91B H -0.2236 -0.0254 -0.1819 0.068 Uiso 1 1 calc R . . H91C H -0.2003 0.0291 -0.1280 0.068 Uiso 1 1 calc R . . C95 C -0.02123(18) -0.3766(6) -0.1703(5) 0.044(2) Uani 1 1 d . . . H95A H -0.0078 -0.4099 -0.1780 0.066 Uiso 1 1 calc R . . H95B H -0.0112 -0.3392 -0.1350 0.066 Uiso 1 1 calc R . . H95C H -0.0326 -0.3441 -0.2077 0.066 Uiso 1 1 calc R . . C98 C -0.1976(2) -0.0506(6) -0.0241(4) 0.044(2) Uani 1 1 d . . . H98A H -0.2123 -0.0201 -0.0194 0.067 Uiso 1 1 calc R . . H98B H -0.1815 -0.0141 -0.0139 0.067 Uiso 1 1 calc R . . H98C H -0.1920 -0.0984 0.0041 0.067 Uiso 1 1 calc R . . C99 C 0.03489(17) -0.2682(5) 0.0723(4) 0.035(2) Uani 1 1 d . . . H99A H 0.0492 -0.2699 0.0593 0.042 Uiso 1 1 calc R . . Cl1 Cl -0.12444(4) -0.25672(11) -0.12418(9) 0.0239(4) Uani 1 1 d . . . Cl2 Cl -0.12636(10) -0.75362(18) -0.12049(19) 0.1045(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0151(6) 0.0214(6) 0.0141(6) 0.0007(4) 0.0080(5) -0.0026(4) Mn2 0.0170(6) 0.0197(6) 0.0148(6) -0.0014(4) 0.0087(5) 0.0007(4) Mn3 0.0149(6) 0.0202(6) 0.0166(6) -0.0007(5) 0.0077(5) -0.0007(5) Mn4 0.0152(6) 0.0241(6) 0.0150(6) -0.0006(5) 0.0075(5) -0.0023(5) Mn5 0.0247(7) 0.0187(6) 0.0202(7) 0.0007(5) 0.0084(6) -0.0010(5) Mn6 0.0200(6) 0.0192(6) 0.0224(7) -0.0005(5) 0.0097(5) -0.0008(5) P1 0.0177(10) 0.0244(10) 0.0173(10) -0.0057(8) 0.0075(9) -0.0026(8) P2 0.0174(10) 0.0233(10) 0.0197(11) -0.0019(8) 0.0095(9) 0.0028(8) P3 0.0184(11) 0.0232(10) 0.0195(11) -0.0017(8) 0.0099(9) -0.0063(8) P4 0.0222(11) 0.0230(10) 0.0181(11) 0.0011(8) 0.0085(9) -0.0089(8) P5 0.0212(11) 0.0230(10) 0.0197(11) -0.0013(8) 0.0102(9) 0.0059(8) P6 0.0217(11) 0.0235(10) 0.0149(10) -0.0050(8) 0.0069(9) -0.0048(8) P7 0.0246(11) 0.0214(10) 0.0181(11) 0.0062(8) 0.0086(9) 0.0021(8) P8 0.0190(11) 0.0217(10) 0.0198(11) 0.0057(8) 0.0092(9) 0.0021(8) O1W 0.098(6) 0.024(3) 0.064(5) -0.008(3) 0.032(5) 0.000(4) O2 0.043(5) 0.102(6) 0.033(4) -0.012(4) -0.009(4) 0.012(4) O2W 0.071(5) 0.028(3) 0.055(4) -0.007(3) 0.028(4) -0.001(3) O3 0.021(3) 0.026(3) 0.018(3) -0.004(2) 0.010(2) -0.003(2) O4 0.028(3) 0.028(3) 0.026(3) 0.001(2) 0.012(3) 0.006(2) O6 0.020(3) 0.030(3) 0.021(3) 0.001(2) 0.009(2) -0.007(2) O7 0.023(3) 0.024(3) 0.020(3) 0.000(2) 0.012(2) 0.000(2) O8 0.019(3) 0.030(3) 0.020(3) 0.008(2) 0.010(2) 0.004(2) O9 0.030(3) 0.021(3) 0.023(3) 0.000(2) 0.013(3) 0.002(2) O10 0.023(3) 0.028(3) 0.020(3) -0.010(2) 0.006(2) -0.011(2) O12 0.016(3) 0.024(3) 0.019(3) 0.003(2) 0.003(2) -0.001(2) O14 0.025(3) 0.019(3) 0.025(3) -0.003(2) 0.013(3) -0.008(2) O15 0.073(6) 0.113(7) 0.077(6) -0.022(5) 0.062(5) -0.016(5) O16 0.028(3) 0.022(3) 0.020(3) 0.003(2) 0.010(3) 0.003(2) O17 0.021(3) 0.027(3) 0.015(3) -0.002(2) 0.007(2) -0.003(2) O18 0.023(3) 0.034(3) 0.014(3) 0.005(2) 0.008(2) 0.005(2) O19 0.017(3) 0.032(3) 0.020(3) 0.002(2) 0.008(2) -0.001(2) O20 0.022(3) 0.030(3) 0.023(3) -0.002(2) 0.007(2) -0.009(2) O21 0.019(3) 0.028(3) 0.023(3) 0.003(2) 0.009(2) 0.003(2) O22 0.020(3) 0.027(3) 0.024(3) 0.003(2) 0.009(2) -0.005(2) O24 0.028(3) 0.024(3) 0.019(3) -0.009(2) 0.013(2) -0.007(2) O25 0.019(3) 0.029(3) 0.018(3) -0.004(2) 0.008(2) -0.002(2) O28 0.025(3) 0.029(3) 0.016(3) 0.006(2) 0.007(2) 0.003(2) O30 0.020(3) 0.018(3) 0.026(3) 0.001(2) 0.008(2) 0.000(2) O32 0.020(3) 0.028(3) 0.016(3) 0.002(2) 0.006(2) 0.004(2) O33 0.021(3) 0.027(3) 0.026(3) -0.004(2) 0.011(3) -0.006(2) O35 0.023(3) 0.029(3) 0.020(3) 0.000(2) 0.008(2) 0.011(2) O54 0.043(5) 0.100(6) 0.032(4) 0.000(4) -0.007(4) -0.011(4) O56 0.019(3) 0.026(3) 0.016(3) -0.004(2) 0.009(2) -0.001(2) O86 0.084(6) 0.082(5) 0.075(6) -0.017(4) 0.066(5) -0.022(5) N5 0.017(4) 0.034(4) 0.016(4) 0.000(3) 0.005(3) -0.005(3) N11 0.013(4) 0.036(4) 0.018(4) -0.002(3) 0.004(3) 0.003(3) N23 0.020(4) 0.023(3) 0.022(4) 0.003(3) 0.010(3) -0.002(3) N26 0.022(4) 0.022(3) 0.021(4) 0.004(3) 0.010(3) -0.001(3) C4 0.029(5) 0.038(5) 0.023(4) 0.016(4) 0.004(4) -0.017(4) C5 0.027(5) 0.039(5) 0.025(5) 0.000(4) 0.013(4) -0.014(4) C6 0.045(6) 0.048(6) 0.047(6) 0.004(5) 0.014(5) -0.023(5) C7 0.035(5) 0.044(5) 0.044(6) 0.009(4) 0.016(5) 0.016(4) C8 0.045(6) 0.044(5) 0.036(6) -0.004(4) 0.012(5) -0.023(5) C9 0.031(6) 0.057(6) 0.052(7) -0.007(5) 0.002(5) 0.003(5) C10 0.034(5) 0.062(6) 0.049(6) 0.027(5) 0.019(5) 0.002(5) C12 0.049(6) 0.051(6) 0.031(5) 0.015(4) 0.011(5) 0.008(5) C13 0.033(6) 0.065(7) 0.043(7) 0.003(5) 0.000(5) -0.001(5) C14 0.036(5) 0.049(6) 0.040(6) -0.009(4) 0.021(5) -0.020(4) C16 0.038(6) 0.062(7) 0.068(7) -0.020(5) 0.035(6) -0.022(5) C17 0.043(6) 0.034(5) 0.036(5) 0.005(4) 0.010(5) -0.022(4) C18 0.049(6) 0.050(6) 0.035(5) 0.015(4) 0.014(5) -0.024(5) C19 0.037(6) 0.081(8) 0.079(9) 0.048(7) 0.019(6) 0.020(6) C20 0.108(10) 0.055(7) 0.033(6) 0.021(5) 0.015(7) 0.013(7) C27 0.026(5) 0.044(5) 0.021(4) 0.001(4) 0.011(4) -0.007(4) C29 0.024(5) 0.030(4) 0.030(5) 0.010(4) 0.008(4) 0.002(4) C31 0.030(5) 0.039(5) 0.029(5) 0.001(4) 0.015(4) -0.002(4) C34 0.030(5) 0.026(4) 0.036(5) -0.010(4) 0.016(4) -0.007(4) C36 0.027(5) 0.039(5) 0.031(5) -0.017(4) 0.014(4) 0.005(4) C37 0.043(6) 0.052(6) 0.035(6) 0.028(5) 0.013(5) 0.003(5) C38 0.028(5) 0.038(5) 0.042(6) -0.001(4) 0.027(5) -0.004(4) C39 0.021(5) 0.058(6) 0.037(5) -0.002(4) 0.020(4) -0.007(4) C40 0.023(5) 0.027(4) 0.035(5) -0.002(4) 0.008(4) 0.007(3) C41 0.039(6) 0.056(6) 0.040(6) -0.020(5) 0.015(5) 0.014(5) C42 0.028(5) 0.057(6) 0.065(7) -0.012(5) 0.025(5) 0.013(5) C43 0.015(4) 0.041(5) 0.028(5) 0.002(4) 0.007(4) -0.004(4) C44 0.036(5) 0.052(6) 0.023(5) -0.002(4) 0.016(4) -0.011(4) C47 0.042(6) 0.045(5) 0.015(4) -0.008(4) 0.010(4) -0.007(4) C49 0.036(5) 0.038(5) 0.027(5) 0.000(4) 0.019(4) 0.002(4) C50 0.037(5) 0.054(6) 0.031(5) -0.023(4) 0.013(4) -0.001(4) C52 0.023(5) 0.044(5) 0.023(5) -0.004(4) 0.009(4) 0.001(4) C54 0.019(5) 0.039(5) 0.026(5) -0.006(4) 0.005(4) 0.004(4) C55 0.038(5) 0.041(5) 0.026(5) -0.006(4) 0.020(4) -0.010(4) C57 0.024(5) 0.029(4) 0.028(5) -0.003(3) 0.012(4) 0.003(3) C58 0.072(9) 0.099(9) 0.037(6) -0.021(6) 0.044(7) -0.023(7) C59 0.032(5) 0.043(5) 0.037(5) 0.009(4) 0.014(4) 0.020(4) C61 0.014(4) 0.035(5) 0.037(5) 0.002(4) 0.002(4) 0.001(3) C62 0.032(5) 0.041(5) 0.022(5) -0.001(4) 0.007(4) 0.001(4) C63 0.025(5) 0.038(5) 0.032(5) -0.001(4) 0.018(4) -0.004(4) C64 0.057(7) 0.040(5) 0.040(6) -0.027(4) 0.022(5) -0.008(5) C66 0.028(5) 0.034(5) 0.020(4) -0.013(3) 0.008(4) -0.006(4) C67 0.019(5) 0.040(5) 0.036(5) -0.001(4) 0.013(4) -0.001(4) C68 0.053(7) 0.040(5) 0.057(7) 0.025(5) 0.028(6) 0.009(5) C71 0.045(6) 0.058(6) 0.023(5) -0.012(4) 0.003(5) -0.007(5) C72 0.051(6) 0.048(6) 0.054(7) -0.027(5) 0.023(5) -0.026(5) C73 0.015(4) 0.045(5) 0.025(5) 0.003(4) 0.006(4) -0.005(4) C74 0.025(5) 0.058(6) 0.015(5) -0.003(4) -0.005(4) 0.010(4) C76 0.039(6) 0.049(6) 0.034(5) -0.021(4) 0.008(5) -0.019(4) C81 0.059(7) 0.051(6) 0.043(6) -0.006(5) 0.035(6) -0.001(5) C83 0.067(7) 0.043(5) 0.021(5) -0.009(4) 0.018(5) -0.010(5) C90 0.026(5) 0.039(5) 0.020(4) 0.002(4) 0.014(4) -0.001(4) C91 0.046(6) 0.048(6) 0.042(6) 0.009(4) 0.020(5) 0.025(5) C95 0.020(5) 0.066(6) 0.051(6) 0.008(5) 0.021(5) 0.010(4) C98 0.046(6) 0.051(6) 0.034(5) -0.015(4) 0.015(5) 0.021(5) C99 0.018(5) 0.049(5) 0.041(6) 0.007(4) 0.016(4) 0.002(4) Cl1 0.0214(9) 0.0278(10) 0.0225(10) 0.0004(8) 0.0097(8) -0.0003(8) Cl2 0.168(4) 0.0460(18) 0.124(3) 0.0305(18) 0.087(3) 0.004(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 O6 1.877(5) . ? Mn1 O17 1.885(5) . ? Mn1 O12 1.888(5) . ? Mn1 O8 1.897(5) . ? Mn1 N5 2.247(6) . ? Mn2 O35 1.874(5) . ? Mn2 O25 1.885(5) . ? Mn2 O32 1.884(5) . ? Mn2 O19 1.900(5) . ? Mn2 N11 2.246(6) . ? Mn3 O14 1.885(5) . ? Mn3 O7 1.883(5) . ? Mn3 O18 1.887(5) . ? Mn3 O28 1.894(5) . ? Mn3 N26 2.264(6) . ? Mn4 O16 1.871(5) . ? Mn4 O56 1.886(5) . ? Mn4 O22 1.894(5) . ? Mn4 O3 1.903(5) . ? Mn4 N23 2.251(6) . ? Mn5 O9 1.868(5) . ? Mn5 O20 1.881(5) . ? Mn5 O4 1.888(5) . ? Mn5 O10 1.896(5) . ? Mn5 O1W 2.194(6) . ? Mn6 O30 1.872(5) . ? Mn6 O33 1.880(5) . ? Mn6 O21 1.885(5) . ? Mn6 O24 1.894(5) . ? Mn6 O2W 2.188(6) . ? P1 O25 1.519(5) . ? P1 O24 1.522(5) . ? P1 O3 1.526(5) . ? P1 C34 1.816(8) . ? P2 O21 1.509(5) . ? P2 O8 1.519(5) . ? P2 O56 1.538(5) . ? P2 C40 1.816(8) . ? P3 O33 1.522(5) . ? P3 O14 1.522(5) . ? P3 O19 1.526(5) . ? P3 C5 1.821(7) . ? P4 O22 1.517(5) . ? P4 O6 1.523(5) . ? P4 O20 1.527(5) . ? P4 C4 1.822(7) . ? P5 O35 1.520(5) . ? P5 O4 1.522(5) . ? P5 O18 1.535(5) . ? P5 C36 1.813(7) . ? P6 O10 1.503(5) . ? P6 O7 1.525(5) . ? P6 O17 1.529(5) . ? P6 C66 1.815(7) . ? P7 O32 1.524(5) . ? P7 O16 1.536(5) . ? P7 O9 1.535(5) . ? P7 C37 1.812(8) . ? P8 O28 1.525(5) . ? P8 O30 1.532(5) . ? P8 O12 1.532(5) . ? P8 C29 1.828(8) . ? O1W H1WA 0.8546 . ? O1W H1WB 0.8590 . ? O2 C9 1.183(12) . ? O2W H2WA 0.8597 . ? O2W H2WB 0.8606 . ? O15 C58 1.211(13) . ? O54 C13 1.177(11) . ? O86 C81 1.199(11) . ? N5 C31 1.339(10) . ? N5 C43 1.343(10) . ? N11 C52 1.332(10) . ? N11 C57 1.341(10) . ? N23 C27 1.335(9) . ? N23 C90 1.334(9) . ? N26 C73 1.338(9) . ? N26 C63 1.342(10) . ? C4 C17 1.519(12) . ? C4 C18 1.522(11) . ? C4 C14 1.541(12) . ? C5 C6 1.519(12) . ? C5 C8 1.519(11) . ? C5 C16 1.542(11) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C29 1.510(11) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C61 1.493(12) . ? C9 H9A 0.9300 . ? C10 C29 1.546(11) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C12 C29 1.547(12) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C54 1.487(12) . ? C13 H13A 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C37 1.525(13) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C37 1.499(13) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C27 C39 1.377(10) . ? C27 H27A 0.9300 . ? C31 C74 1.366(11) . ? C31 H31A 0.9300 . ? C34 C72 1.537(11) . ? C34 C50 1.544(11) . ? C34 C71 1.562(12) . ? C36 C42 1.525(12) . ? C36 C91 1.523(12) . ? C36 C98 1.544(11) . ? C37 C68 1.528(12) . ? C38 C73 1.365(10) . ? C38 C55 1.384(12) . ? C38 H38A 0.9300 . ? C39 C49 1.372(11) . ? C39 H39A 0.9300 . ? C40 C59 1.516(11) . ? C40 C95 1.537(11) . ? C40 C41 1.543(11) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C99 1.376(11) . ? C43 H43A 0.9300 . ? C44 C55 1.367(12) . ? C44 C63 1.387(11) . ? C44 H44A 0.9300 . ? C47 C49 1.353(12) . ? C47 C90 1.404(10) . ? C47 H47A 0.9300 . ? C49 C81 1.485(11) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C52 C67 1.393(11) . ? C52 H52A 0.9300 . ? C54 C67 1.373(11) . ? C54 C62 1.374(12) . ? C55 C58 1.490(12) . ? C57 C62 1.379(11) . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C61 C74 1.369(12) . ? C61 C99 1.381(12) . ? C62 H62A 0.9300 . ? C63 H63A 0.9300 . ? C64 C66 1.527(11) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C66 C76 1.556(11) . ? C66 C83 1.559(11) . ? C67 H67A 0.9300 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C73 H73A 0.9300 . ? C74 H74A 0.9300 . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C81 H81A 0.9300 . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C90 H90A 0.9300 . ? C91 H91A 0.9600 . ? C91 H91B 0.9600 . ? C91 H91C 0.9600 . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C99 H99A 0.9300 . ? 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 O6 Mn1 O17 90.7(2) . . ? O6 Mn1 O12 176.2(2) . . ? O17 Mn1 O12 89.4(2) . . ? O6 Mn1 O8 89.8(2) . . ? O17 Mn1 O8 178.9(2) . . ? O12 Mn1 O8 90.0(2) . . ? O6 Mn1 N5 93.5(2) . . ? O17 Mn1 N5 89.4(2) . . ? O12 Mn1 N5 90.3(2) . . ? O8 Mn1 N5 91.6(2) . . ? O35 Mn2 O25 176.8(2) . . ? O35 Mn2 O32 90.2(2) . . ? O25 Mn2 O32 88.7(2) . . ? O35 Mn2 O19 89.7(2) . . ? O25 Mn2 O19 91.3(2) . . ? O32 Mn2 O19 178.3(2) . . ? O35 Mn2 N11 93.7(2) . . ? O25 Mn2 N11 89.3(2) . . ? O32 Mn2 N11 90.9(2) . . ? O19 Mn2 N11 90.8(2) . . ? O14 Mn3 O7 176.7(2) . . ? O14 Mn3 O18 89.0(2) . . ? O7 Mn3 O18 91.2(2) . . ? O14 Mn3 O28 90.0(2) . . ? O7 Mn3 O28 89.7(2) . . ? O18 Mn3 O28 177.8(2) . . ? O14 Mn3 N26 93.1(2) . . ? O7 Mn3 N26 90.2(2) . . ? O18 Mn3 N26 86.6(2) . . ? O28 Mn3 N26 95.4(2) . . ? O16 Mn4 O56 177.6(2) . . ? O16 Mn4 O22 89.7(2) . . ? O56 Mn4 O22 89.5(2) . . ? O16 Mn4 O3 89.6(2) . . ? O56 Mn4 O3 91.1(2) . . ? O22 Mn4 O3 178.5(2) . . ? O16 Mn4 N23 94.0(2) . . ? O56 Mn4 N23 88.3(2) . . ? O22 Mn4 N23 90.6(2) . . ? O3 Mn4 N23 90.9(2) . . ? O9 Mn5 O20 89.7(2) . . ? O9 Mn5 O4 90.0(2) . . ? O20 Mn5 O4 178.0(2) . . ? O9 Mn5 O10 177.4(2) . . ? O20 Mn5 O10 90.8(2) . . ? O4 Mn5 O10 89.5(2) . . ? O9 Mn5 O1W 96.6(2) . . ? O20 Mn5 O1W 95.8(3) . . ? O4 Mn5 O1W 86.2(3) . . ? O10 Mn5 O1W 85.9(2) . . ? O30 Mn6 O33 89.8(2) . . ? O30 Mn6 O21 90.3(2) . . ? O33 Mn6 O21 177.1(2) . . ? O30 Mn6 O24 178.7(2) . . ? O33 Mn6 O24 89.7(2) . . ? O21 Mn6 O24 90.2(2) . . ? O30 Mn6 O2W 96.5(2) . . ? O33 Mn6 O2W 94.9(2) . . ? O21 Mn6 O2W 88.0(2) . . ? O24 Mn6 O2W 84.7(2) . . ? O25 P1 O24 112.8(3) . . ? O25 P1 O3 112.4(3) . . ? O24 P1 O3 111.5(3) . . ? O25 P1 C34 105.9(3) . . ? O24 P1 C34 105.9(3) . . ? O3 P1 C34 107.7(3) . . ? O21 P2 O8 112.1(3) . . ? O21 P2 O56 112.4(3) . . ? O8 P2 O56 112.0(3) . . ? O21 P2 C40 105.8(3) . . ? O8 P2 C40 107.0(3) . . ? O56 P2 C40 107.0(3) . . ? O33 P3 O14 112.7(3) . . ? O33 P3 O19 111.0(3) . . ? O14 P3 O19 112.8(3) . . ? O33 P3 C5 105.9(3) . . ? O14 P3 C5 105.2(3) . . ? O19 P3 C5 108.9(3) . . ? O22 P4 O6 112.6(3) . . ? O22 P4 O20 111.8(3) . . ? O6 P4 O20 111.6(3) . . ? O22 P4 C4 107.1(3) . . ? O6 P4 C4 107.6(3) . . ? O20 P4 C4 105.8(4) . . ? O35 P5 O4 112.7(3) . . ? O35 P5 O18 111.3(3) . . ? O4 P5 O18 111.7(3) . . ? O35 P5 C36 105.7(3) . . ? O4 P5 C36 106.4(3) . . ? O18 P5 C36 108.6(3) . . ? O10 P6 O7 112.2(3) . . ? O10 P6 O17 112.0(3) . . ? O7 P6 O17 111.9(3) . . ? O10 P6 C66 105.6(3) . . ? O7 P6 C66 107.1(3) . . ? O17 P6 C66 107.6(3) . . ? O32 P7 O16 112.4(3) . . ? O32 P7 O9 111.5(3) . . ? O16 P7 O9 112.6(3) . . ? O32 P7 C37 107.4(4) . . ? O16 P7 C37 105.9(4) . . ? O9 P7 C37 106.7(4) . . ? O28 P8 O30 112.1(3) . . ? O28 P8 O12 112.7(3) . . ? O30 P8 O12 111.9(3) . . ? O28 P8 C29 108.6(3) . . ? O30 P8 C29 105.0(3) . . ? O12 P8 C29 105.9(3) . . ? Mn5 O1W H1WA 116.3 . . ? Mn5 O1W H1WB 85.6 . . ? H1WA O1W H1WB 101.7 . . ? Mn6 O2W H2WA 115.4 . . ? Mn6 O2W H2WB 105.8 . . ? H2WA O2W H2WB 102.2 . . ? P1 O3 Mn4 135.6(3) . . ? P5 O4 Mn5 137.7(3) . . ? P4 O6 Mn1 137.9(3) . . ? P6 O7 Mn3 137.8(3) . . ? P2 O8 Mn1 135.8(3) . . ? P7 O9 Mn5 137.2(3) . . ? P6 O10 Mn5 139.7(3) . . ? P8 O12 Mn1 139.0(3) . . ? P3 O14 Mn3 139.2(3) . . ? P7 O16 Mn4 138.7(3) . . ? P6 O17 Mn1 136.6(3) . . ? P5 O18 Mn3 138.2(3) . . ? P3 O19 Mn2 135.6(3) . . ? P4 O20 Mn5 137.7(3) . . ? P2 O21 Mn6 139.6(3) . . ? P4 O22 Mn4 137.9(3) . . ? P1 O24 Mn6 137.0(3) . . ? P1 O25 Mn2 139.8(3) . . ? P8 O28 Mn3 135.1(3) . . ? P8 O30 Mn6 137.1(3) . . ? P7 O32 Mn2 138.0(3) . . ? P3 O33 Mn6 137.1(3) . . ? P5 O35 Mn2 138.3(3) . . ? P2 O56 Mn4 136.5(3) . . ? C31 N5 C43 117.2(7) . . ? C31 N5 Mn1 120.4(5) . . ? C43 N5 Mn1 122.3(5) . . ? C52 N11 C57 118.4(7) . . ? C52 N11 Mn2 123.2(5) . . ? C57 N11 Mn2 118.1(5) . . ? C27 N23 C90 117.7(7) . . ? C27 N23 Mn4 119.0(5) . . ? C90 N23 Mn4 122.9(5) . . ? C73 N26 C63 116.7(7) . . ? C73 N26 Mn3 120.1(5) . . ? C63 N26 Mn3 122.1(5) . . ? C17 C4 C18 112.0(7) . . ? C17 C4 C14 110.2(7) . . ? C18 C4 C14 110.6(7) . . ? C17 C4 P4 107.7(6) . . ? C18 C4 P4 108.3(6) . . ? C14 C4 P4 107.9(5) . . ? C6 C5 C8 111.7(7) . . ? C6 C5 C16 109.6(7) . . ? C8 C5 C16 110.0(7) . . ? C6 C5 P3 107.9(6) . . ? C8 C5 P3 108.8(5) . . ? C16 C5 P3 108.6(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C29 C7 H7A 109.5 . . ? C29 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C29 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C61 123.8(10) . . ? O2 C9 H9A 118.1 . . ? C61 C9 H9A 118.1 . . ? C29 C10 H10A 109.5 . . ? C29 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C29 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C29 C12 H12A 109.5 . . ? C29 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C29 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O54 C13 C54 123.6(10) . . ? O54 C13 H13A 118.2 . . ? C54 C13 H13A 118.2 . . ? C4 C14 H14A 109.5 . . ? C4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 C16 H16A 109.5 . . ? C5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C4 C17 H17A 109.5 . . ? C4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C37 C19 H19A 109.5 . . ? C37 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C37 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C37 C20 H20A 109.5 . . ? C37 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C37 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N23 C27 C39 123.3(8) . . ? N23 C27 H27A 118.4 . . ? C39 C27 H27A 118.4 . . ? C7 C29 C10 111.1(7) . . ? C7 C29 C12 111.2(7) . . ? C10 C29 C12 109.1(7) . . ? C7 C29 P8 109.1(6) . . ? C10 C29 P8 108.0(6) . . ? C12 C29 P8 108.3(5) . . ? N5 C31 C74 123.5(8) . . ? N5 C31 H31A 118.2 . . ? C74 C31 H31A 118.2 . . ? C72 C34 C50 111.1(7) . . ? C72 C34 C71 110.8(7) . . ? C50 C34 C71 108.7(7) . . ? C72 C34 P1 108.1(6) . . ? C50 C34 P1 108.7(6) . . ? C71 C34 P1 109.4(5) . . ? C42 C36 C91 110.1(8) . . ? C42 C36 C98 109.9(7) . . ? C91 C36 C98 109.8(7) . . ? C42 C36 P5 109.4(5) . . ? C91 C36 P5 108.1(6) . . ? C98 C36 P5 109.5(6) . . ? C20 C37 C19 110.9(9) . . ? C20 C37 C68 109.5(8) . . ? C19 C37 C68 110.1(8) . . ? C20 C37 P7 109.2(7) . . ? C19 C37 P7 107.9(6) . . ? C68 C37 P7 109.2(6) . . ? C73 C38 C55 117.5(8) . . ? C73 C38 H38A 121.3 . . ? C55 C38 H38A 121.3 . . ? C49 C39 C27 118.4(8) . . ? C49 C39 H39A 120.8 . . ? C27 C39 H39A 120.8 . . ? C59 C40 C95 111.4(7) . . ? C59 C40 C41 110.3(7) . . ? C95 C40 C41 109.0(7) . . ? C59 C40 P2 108.8(6) . . ? C95 C40 P2 109.7(5) . . ? C41 C40 P2 107.6(5) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 C43 C99 122.6(8) . . ? N5 C43 H43A 118.7 . . ? C99 C43 H43A 118.7 . . ? C55 C44 C63 118.2(8) . . ? C55 C44 H44A 120.9 . . ? C63 C44 H44A 120.9 . . ? C49 C47 C90 118.9(8) . . ? C49 C47 H47A 120.6 . . ? C90 C47 H47A 120.6 . . ? C47 C49 C39 119.7(7) . . ? C47 C49 C81 120.8(8) . . ? C39 C49 C81 119.5(8) . . ? C34 C50 H50A 109.5 . . ? C34 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C34 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N11 C52 C67 121.8(8) . . ? N11 C52 H52A 119.1 . . ? C67 C52 H52A 119.1 . . ? C67 C54 C62 118.8(8) . . ? C67 C54 C13 119.4(8) . . ? C62 C54 C13 121.8(8) . . ? C44 C55 C38 120.1(8) . . ? C44 C55 C58 120.7(9) . . ? C38 C55 C58 119.2(9) . . ? N11 C57 C62 122.6(8) . . ? N11 C57 H57A 118.7 . . ? C62 C57 H57A 118.7 . . ? O15 C58 C55 124.7(11) . . ? O15 C58 H58A 117.7 . . ? C55 C58 H58A 117.7 . . ? C40 C59 H59A 109.5 . . ? C40 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C40 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C74 C61 C99 119.1(8) . . ? C74 C61 C9 120.9(9) . . ? C99 C61 C9 119.9(8) . . ? C54 C62 C57 119.1(8) . . ? C54 C62 H62A 120.5 . . ? C57 C62 H62A 120.5 . . ? N26 C63 C44 123.0(8) . . ? N26 C63 H63A 118.5 . . ? C44 C63 H63A 118.5 . . ? C66 C64 H64A 109.5 . . ? C66 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C66 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C64 C66 C76 112.0(7) . . ? C64 C66 C83 110.1(7) . . ? C76 C66 C83 109.0(7) . . ? C64 C66 P6 109.5(6) . . ? C76 C66 P6 107.8(5) . . ? C83 C66 P6 108.4(5) . . ? C54 C67 C52 119.4(8) . . ? C54 C67 H67A 120.3 . . ? C52 C67 H67A 120.3 . . ? C37 C68 H68A 109.5 . . ? C37 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C37 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C34 C71 H71A 109.5 . . ? C34 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C34 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C34 C72 H72A 109.5 . . ? C34 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C34 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N26 C73 C38 124.6(8) . . ? N26 C73 H73A 117.7 . . ? C38 C73 H73A 117.7 . . ? C31 C74 C61 118.7(8) . . ? C31 C74 H74A 120.6 . . ? C61 C74 H74A 120.6 . . ? C66 C76 H76A 109.5 . . ? C66 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C66 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? O86 C81 C49 124.9(10) . . ? O86 C81 H81A 117.6 . . ? C49 C81 H81A 117.6 . . ? C66 C83 H83A 109.5 . . ? C66 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C66 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N23 C90 C47 122.0(7) . . ? N23 C90 H90A 119.0 . . ? C47 C90 H90A 119.0 . . ? C36 C91 H91A 109.5 . . ? C36 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C36 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C40 C95 H95A 109.5 . . ? C40 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C40 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C36 C98 H98A 109.5 . . ? C36 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C36 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? C43 C99 C61 118.8(8) . . ? C43 C99 H99A 120.6 . . ? C61 C99 H99A 120.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.296 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.131