data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Stefan Roggan' _publ_contact_author_email stefan.roggan@googlemail.com loop_ _publ_author_name S.Roggan C.Limberg C.Knispel T.D.Tilley # Attachment '- complex 6_rev.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 765494' #TrackingRef '- complex 6_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H54 N20 Ru, 4 (F6 P)' _chemical_formula_sum 'C52 H54 F24 N20 P4 Ru' _chemical_formula_weight 1640.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Ru Ru -1.2594 0.8363 '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 22.7921(8) _cell_length_b 14.6642(4) _cell_length_c 21.0070(8) _cell_angle_alpha 90.00 _cell_angle_beta 114.483(3) _cell_angle_gamma 90.00 _cell_volume 6389.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24061 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.30 _exptl_crystal_description cube _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3304 _exptl_absorpt_coefficient_mu 0.472 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.9115 _exptl_absorpt_correction_T_max 0.9632 _exptl_absorpt_process_details ; The correction was carried out by ABSCOR (Stoe, 1997), a modification of DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166. In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones. ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine-focus sealed x-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device_type 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,226 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35726 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 28.02 _reflns_number_total 7643 _reflns_number_gt 5735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2007)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2007)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (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. In total 4 geometrical restrains (DFIX) were used to stabilise and fix the geometry of one disordered PF6 counter anion. ; _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^)+(0.0363P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7643 _refine_ls_number_parameters 482 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.0792 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 C1 C 0.60536(11) 0.41370(16) 0.25816(12) 0.0128(5) Uani 1 1 d . . . C2 C 0.62715(12) 0.41087(17) 0.20328(13) 0.0145(5) Uani 1 1 d . . . C3 C 0.66685(13) 0.47696(18) 0.19301(14) 0.0191(5) Uani 1 1 d . . . H3 H 0.6793 0.5293 0.2223 0.023 Uiso 1 1 calc R . . C4 C 0.68786(14) 0.46628(19) 0.14063(15) 0.0234(6) Uani 1 1 d . . . H4 H 0.7152 0.5108 0.1342 0.028 Uiso 1 1 calc R . . C5 C 0.66888(14) 0.38988(19) 0.09695(15) 0.0238(6) Uani 1 1 d . . . H5 H 0.6833 0.3832 0.0607 0.029 Uiso 1 1 calc R . . C6 C 0.62994(12) 0.3246(2) 0.10548(13) 0.0198(5) Uani 1 1 d . . . H6 H 0.6173 0.2733 0.0752 0.024 Uiso 1 1 calc R . . C7 C 0.60850(11) 0.33347(16) 0.15956(12) 0.0136(5) Uani 1 1 d . . . C8 C 0.57114(11) 0.26616(17) 0.17490(12) 0.0129(5) Uani 1 1 d . . . C9 C 0.54900(11) 0.17823(18) 0.13270(12) 0.0143(4) Uani 1 1 d . . . H9 H 0.5643 0.1764 0.0944 0.017 Uiso 1 1 calc R . . C10 C 0.47666(11) 0.17590(18) 0.10262(12) 0.0146(4) Uani 1 1 d . . . C11 C 0.38067(11) 0.1773(2) 0.10044(13) 0.0193(5) Uani 1 1 d . . . H11 H 0.3465 0.1780 0.1152 0.023 Uiso 1 1 calc R . . C12 C 0.37377(12) 0.1761(2) 0.03326(13) 0.0221(5) Uani 1 1 d . . . H12 H 0.3343 0.1756 -0.0074 0.027 Uiso 1 1 calc R . . C13 C 0.45089(13) 0.1756(3) -0.02586(14) 0.0300(6) Uani 1 1 d . . . H13A H 0.4805 0.2260 -0.0217 0.045 Uiso 1 1 calc R . . H13B H 0.4114 0.1831 -0.0687 0.045 Uiso 1 1 calc R . . H13C H 0.4715 0.1177 -0.0277 0.045 Uiso 1 1 calc R . . C14 C 0.57566(12) 0.09909(17) 0.18117(13) 0.0146(5) Uani 1 1 d . . . C15 C 0.59232(12) 0.00997(18) 0.26963(14) 0.0187(5) Uani 1 1 d . . . H15 H 0.5895 -0.0162 0.3097 0.022 Uiso 1 1 calc R . . C16 C 0.63092(13) -0.01945(18) 0.23900(15) 0.0211(6) Uani 1 1 d . . . H16 H 0.6599 -0.0696 0.2535 0.025 Uiso 1 1 calc R . . C17 C 0.65404(14) 0.03263(19) 0.13740(16) 0.0240(6) Uani 1 1 d . . . H17A H 0.6245 0.0107 0.0911 0.036 Uiso 1 1 calc R . . H17B H 0.6906 -0.0093 0.1574 0.036 Uiso 1 1 calc R . . H17C H 0.6697 0.0935 0.1331 0.036 Uiso 1 1 calc R . . C18 C 0.62539(11) 0.49098(16) 0.31198(13) 0.0142(5) Uani 1 1 d . . . H18 H 0.6736 0.4922 0.3345 0.017 Uiso 1 1 calc R . . C19 C 0.60329(12) 0.58296(17) 0.27927(13) 0.0150(5) Uani 1 1 d . . . C20 C 0.54710(12) 0.69397(18) 0.21110(14) 0.0195(5) Uani 1 1 d . . . H20 H 0.5143 0.7257 0.1738 0.023 Uiso 1 1 calc R . . C21 C 0.59815(13) 0.73159(18) 0.26364(15) 0.0207(5) Uani 1 1 d . . . H21 H 0.6081 0.7948 0.2704 0.025 Uiso 1 1 calc R . . C22 C 0.69375(13) 0.6717(2) 0.36844(15) 0.0260(6) Uani 1 1 d . . . H22A H 0.6874 0.6514 0.4096 0.039 Uiso 1 1 calc R . . H22B H 0.7069 0.7358 0.3741 0.039 Uiso 1 1 calc R . . H22C H 0.7273 0.6345 0.3634 0.039 Uiso 1 1 calc R . . C23 C 0.60298(12) 0.47382(17) 0.36924(13) 0.0145(5) Uani 1 1 d . . . C24 C 0.54451(13) 0.46324(19) 0.42721(14) 0.0205(5) Uani 1 1 d . . . H24 H 0.5094 0.4693 0.4402 0.025 Uiso 1 1 calc R . . C25 C 0.60089(13) 0.42019(19) 0.46587(14) 0.0203(5) Uani 1 1 d . . . H25 H 0.6124 0.3906 0.5096 0.024 Uiso 1 1 calc R . . C26 C 0.70336(13) 0.3926(2) 0.44968(15) 0.0231(6) Uani 1 1 d . . . H26A H 0.7043 0.3507 0.4138 0.035 Uiso 1 1 calc R . . H26B H 0.7162 0.3600 0.4942 0.035 Uiso 1 1 calc R . . H26C H 0.7333 0.4432 0.4554 0.035 Uiso 1 1 calc R . . N1 N 0.55387(10) 0.27471(14) 0.22795(11) 0.0134(4) Uani 1 1 d . . . N2 N 0.57139(9) 0.35015(14) 0.27014(11) 0.0134(4) Uani 1 1 d . . . N3 N 0.44557(9) 0.17721(15) 0.14399(10) 0.0152(4) Uani 1 1 d . . . N4 N 0.43476(10) 0.17579(17) 0.03492(11) 0.0188(4) Uani 1 1 d . . . N5 N 0.55788(10) 0.08422(15) 0.23281(11) 0.0153(4) Uani 1 1 d . . . N6 N 0.62019(10) 0.03703(15) 0.18293(11) 0.0168(4) Uani 1 1 d . . . N7 N 0.55117(10) 0.60082(15) 0.22144(12) 0.0163(4) Uani 1 1 d . . . H7 H 0.5208(19) 0.563(3) 0.193(2) 0.049(11) Uiso 1 1 d . . . N8 N 0.63326(10) 0.66155(14) 0.30581(11) 0.0169(4) Uani 1 1 d . . . N9 N 0.54564(10) 0.49683(15) 0.36636(11) 0.0166(4) Uani 1 1 d . . . N10 N 0.63809(10) 0.42842(15) 0.42827(11) 0.0167(4) Uani 1 1 d . . . F1 F 0.67819(11) 0.05625(16) 0.00635(13) 0.0409(7) Uani 0.882(4) 1 d P A 1 F1S F 0.6335(13) 0.0235(4) -0.0394(14) 0.070(7) Uiso 0.118(4) 1 d PD A 2 F2 F 0.68222(10) 0.20687(16) -0.00415(11) 0.0337(6) Uani 0.882(4) 1 d P A 1 F2S F 0.6933(10) 0.149(3) 0.0228(10) 0.108(11) Uiso 0.118(4) 1 d PD A 2 F3 F 0.58662(12) 0.20589(19) -0.09841(14) 0.0452(7) Uani 0.882(4) 1 d P A 1 F3S F 0.6145(16) 0.2361(7) -0.0651(18) 0.095(10) Uiso 0.118(4) 1 d PD A 2 F4 F 0.58241(12) 0.05195(18) -0.08631(13) 0.0455(8) Uani 0.882(4) 1 d P A 1 F4S F 0.5633(6) 0.1201(19) -0.1131(8) 0.068(7) Uiso 0.118(4) 1 d PD A 2 F5 F 0.59426(9) 0.14394(13) 0.00266(9) 0.0322(4) Uani 1 1 d . A . F6 F 0.66745(9) 0.11868(14) -0.09744(10) 0.0395(5) Uani 1 1 d . A . F7 F 0.79506(9) 0.32491(14) 0.36537(9) 0.0380(4) Uani 1 1 d . . . F8 F 0.84142(8) 0.20124(14) 0.33970(10) 0.0374(5) Uani 1 1 d . . . F9 F 0.74276(9) 0.14397(13) 0.27498(10) 0.0373(4) Uani 1 1 d . . . F10 F 0.69737(8) 0.26418(13) 0.30319(9) 0.0325(4) Uani 1 1 d . . . F11 F 0.77235(8) 0.18320(13) 0.38934(8) 0.0309(4) Uani 1 1 d . . . F12 F 0.76702(9) 0.28597(13) 0.25257(9) 0.0335(4) Uani 1 1 d . . . P1 P 0.63126(4) 0.13087(5) -0.04741(4) 0.02481(16) Uani 1 1 d D . . P2 P 0.76924(3) 0.23412(5) 0.32022(3) 0.01727(14) Uani 1 1 d . . . Ru1 Ru 0.5000 0.17950(2) 0.2500 0.01090(7) Uani 1 2 d S . . 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 C1 0.0106(11) 0.0123(11) 0.0140(12) -0.0001(9) 0.0036(10) 0.0006(9) C2 0.0145(11) 0.0130(12) 0.0156(12) 0.0012(9) 0.0057(10) 0.0020(9) C3 0.0211(13) 0.0150(12) 0.0213(13) -0.0009(10) 0.0088(11) -0.0021(10) C4 0.0293(15) 0.0198(14) 0.0255(15) 0.0016(11) 0.0159(13) -0.0072(11) C5 0.0324(16) 0.0213(14) 0.0235(14) 0.0007(11) 0.0175(13) -0.0028(12) C6 0.0249(13) 0.0169(12) 0.0191(12) -0.0018(11) 0.0106(11) -0.0016(12) C7 0.0146(11) 0.0117(12) 0.0129(11) 0.0025(9) 0.0042(9) 0.0007(9) C8 0.0108(11) 0.0126(12) 0.0138(12) 0.0021(9) 0.0036(10) 0.0019(9) C9 0.0148(11) 0.0135(11) 0.0155(11) 0.0007(10) 0.0070(9) 0.0001(10) C10 0.0151(11) 0.0137(11) 0.0140(11) -0.0008(10) 0.0049(9) 0.0004(10) C11 0.0144(11) 0.0202(12) 0.0218(13) -0.0004(12) 0.0060(10) -0.0009(11) C12 0.0134(11) 0.0293(14) 0.0188(12) -0.0014(12) 0.0019(10) 0.0000(12) C13 0.0213(13) 0.0538(19) 0.0146(12) -0.0021(14) 0.0072(11) 0.0004(15) C14 0.0136(12) 0.0127(12) 0.0166(12) -0.0028(9) 0.0055(10) -0.0006(9) C15 0.0183(13) 0.0154(13) 0.0227(14) 0.0040(10) 0.0087(11) 0.0017(10) C16 0.0206(13) 0.0142(13) 0.0287(15) 0.0062(11) 0.0104(12) 0.0057(10) C17 0.0263(14) 0.0205(14) 0.0336(16) 0.0040(12) 0.0209(13) 0.0057(11) C18 0.0129(12) 0.0120(11) 0.0167(12) 0.0000(9) 0.0052(10) -0.0011(9) C19 0.0159(12) 0.0121(12) 0.0187(12) -0.0022(10) 0.0090(10) -0.0008(9) C20 0.0195(12) 0.0175(14) 0.0247(13) 0.0060(10) 0.0124(11) 0.0048(10) C21 0.0238(13) 0.0124(12) 0.0301(15) 0.0020(11) 0.0153(12) 0.0002(10) C22 0.0208(13) 0.0214(14) 0.0290(14) -0.0066(12) 0.0036(11) -0.0044(12) C23 0.0159(12) 0.0121(12) 0.0126(12) -0.0015(9) 0.0030(10) -0.0008(9) C24 0.0189(13) 0.0253(14) 0.0188(13) -0.0020(11) 0.0092(11) -0.0006(11) C25 0.0220(13) 0.0236(14) 0.0157(13) 0.0007(10) 0.0082(11) -0.0008(11) C26 0.0158(13) 0.0284(15) 0.0215(14) 0.0055(11) 0.0042(11) 0.0054(11) N1 0.0127(10) 0.0119(10) 0.0146(10) -0.0005(8) 0.0047(9) 0.0006(8) N2 0.0090(9) 0.0141(10) 0.0155(10) -0.0007(8) 0.0035(8) 0.0004(7) N3 0.0145(9) 0.0142(9) 0.0168(10) -0.0018(9) 0.0062(8) 0.0004(9) N4 0.0171(10) 0.0236(11) 0.0137(10) -0.0012(10) 0.0045(8) 0.0001(10) N5 0.0150(10) 0.0132(11) 0.0179(11) -0.0001(8) 0.0070(9) 0.0000(8) N6 0.0175(11) 0.0144(10) 0.0219(12) -0.0016(9) 0.0115(9) 0.0018(8) N7 0.0143(10) 0.0171(11) 0.0184(11) 0.0008(9) 0.0078(9) -0.0011(9) N8 0.0180(10) 0.0143(11) 0.0191(11) -0.0028(8) 0.0086(9) -0.0025(8) N9 0.0136(10) 0.0187(11) 0.0155(11) -0.0012(8) 0.0041(9) -0.0001(8) N10 0.0151(10) 0.0188(11) 0.0141(10) 0.0008(8) 0.0040(9) 0.0018(8) F1 0.0463(14) 0.0374(13) 0.0504(15) 0.0164(11) 0.0314(12) 0.0223(11) F2 0.0291(11) 0.0392(13) 0.0289(11) -0.0113(9) 0.0080(9) -0.0078(9) F3 0.0340(13) 0.0608(17) 0.0350(13) 0.0252(12) 0.0085(11) 0.0179(12) F4 0.0549(16) 0.0493(16) 0.0452(15) -0.0273(12) 0.0337(13) -0.0286(13) F5 0.0344(10) 0.0370(10) 0.0317(10) -0.0045(8) 0.0202(8) 0.0046(8) F6 0.0479(12) 0.0463(12) 0.0374(10) -0.0115(9) 0.0308(10) -0.0136(9) F7 0.0455(11) 0.0277(9) 0.0336(10) -0.0076(8) 0.0094(8) -0.0065(9) F8 0.0199(8) 0.0530(13) 0.0398(10) 0.0042(9) 0.0127(8) 0.0107(8) F9 0.0402(11) 0.0273(9) 0.0351(10) -0.0094(8) 0.0064(9) -0.0001(8) F10 0.0185(8) 0.0455(11) 0.0327(10) 0.0100(8) 0.0098(8) 0.0115(8) F11 0.0317(9) 0.0371(10) 0.0242(8) 0.0120(8) 0.0120(7) 0.0093(8) F12 0.0375(10) 0.0413(11) 0.0269(9) 0.0095(8) 0.0185(8) 0.0024(8) P1 0.0289(4) 0.0267(4) 0.0213(4) -0.0041(3) 0.0129(3) -0.0020(3) P2 0.0143(3) 0.0206(3) 0.0160(3) 0.0012(3) 0.0054(3) 0.0021(3) Ru1 0.01077(13) 0.00994(13) 0.01205(14) 0.000 0.00480(11) 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 C1 N2 1.301(3) . ? C1 C2 1.433(3) . ? C1 C18 1.531(3) . ? C2 C3 1.402(3) . ? C2 C7 1.410(3) . ? C3 C4 1.379(4) . ? C3 H3 0.9500 . ? C4 C5 1.398(4) . ? C4 H4 0.9500 . ? C5 C6 1.367(4) . ? C5 H5 0.9500 . ? C6 C7 1.417(3) . ? C6 H6 0.9500 . ? C7 C8 1.425(3) . ? C8 N1 1.333(3) . ? C8 C9 1.527(3) . ? C9 C14 1.497(3) . ? C9 C10 1.502(3) . ? C9 H9 1.0000 . ? C10 N3 1.330(3) . ? C10 N4 1.345(3) . ? C11 C12 1.354(3) . ? C11 N3 1.380(3) . ? C11 H11 0.9500 . ? C12 N4 1.376(3) . ? C12 H12 0.9500 . ? C13 N4 1.468(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N5 1.324(3) . ? C14 N6 1.352(3) . ? C15 C16 1.358(4) . ? C15 N5 1.377(3) . ? C15 H15 0.9500 . ? C16 N6 1.376(3) . ? C16 H16 0.9500 . ? C17 N6 1.458(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.503(3) . ? C18 C23 1.510(3) . ? C18 H18 1.0000 . ? C19 N7 1.326(3) . ? C19 N8 1.338(3) . ? C20 C21 1.346(4) . ? C20 N7 1.380(3) . ? C20 H20 0.9500 . ? C21 N8 1.376(3) . ? C21 H21 0.9500 . ? C22 N8 1.466(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N9 1.327(3) . ? C23 N10 1.341(3) . ? C24 C25 1.358(4) . ? C24 N9 1.380(3) . ? C24 H24 0.9500 . ? C25 N10 1.383(3) . ? C25 H25 0.9500 . ? C26 N10 1.462(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N1 N2 1.369(3) . ? N1 Ru1 2.035(2) . ? N3 Ru1 2.052(2) . ? N5 Ru1 2.054(2) . ? N7 H7 0.89(4) . ? F1 P1 1.617(2) . ? F1S P1 1.582(5) . ? F2 P1 1.594(2) . ? F2S P1 1.586(5) . ? F3 P1 1.578(2) . ? F3S P1 1.596(5) . ? F4 P1 1.579(2) . ? F4S P1 1.599(5) . ? F5 P1 1.6091(17) . ? F6 P1 1.5922(17) . ? F7 P2 1.599(2) . ? F8 P2 1.5965(17) . ? F9 P2 1.5936(19) . ? F10 P2 1.5873(16) . ? F11 P2 1.6080(17) . ? F12 P2 1.5940(17) . ? Ru1 N1 2.035(2) 2_655 ? Ru1 N3 2.052(2) 2_655 ? Ru1 N5 2.054(2) 2_655 ? 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 N2 C1 C2 124.6(2) . . ? N2 C1 C18 114.0(2) . . ? C2 C1 C18 121.3(2) . . ? C3 C2 C7 119.7(2) . . ? C3 C2 C1 124.4(2) . . ? C7 C2 C1 115.9(2) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.0(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 121.1(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 120.0(2) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 119.0(2) . . ? C2 C7 C8 117.2(2) . . ? C6 C7 C8 123.7(2) . . ? N1 C8 C7 122.4(2) . . ? N1 C8 C9 115.1(2) . . ? C7 C8 C9 122.6(2) . . ? C14 C9 C10 109.5(2) . . ? C14 C9 C8 108.46(19) . . ? C10 C9 C8 107.73(19) . . ? C14 C9 H9 110.4 . . ? C10 C9 H9 110.4 . . ? C8 C9 H9 110.4 . . ? N3 C10 N4 110.7(2) . . ? N3 C10 C9 120.9(2) . . ? N4 C10 C9 128.3(2) . . ? C12 C11 N3 108.7(2) . . ? C12 C11 H11 125.7 . . ? N3 C11 H11 125.7 . . ? C11 C12 N4 107.1(2) . . ? C11 C12 H12 126.5 . . ? N4 C12 H12 126.5 . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 N6 110.4(2) . . ? N5 C14 C9 120.6(2) . . ? N6 C14 C9 129.0(2) . . ? C16 C15 N5 108.4(2) . . ? C16 C15 H15 125.8 . . ? N5 C15 H15 125.8 . . ? C15 C16 N6 107.1(2) . . ? C15 C16 H16 126.4 . . ? N6 C16 H16 126.4 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 110.73(19) . . ? C19 C18 C1 112.7(2) . . ? C23 C18 C1 111.67(19) . . ? C19 C18 H18 107.1 . . ? C23 C18 H18 107.1 . . ? C1 C18 H18 107.1 . . ? N7 C19 N8 108.7(2) . . ? N7 C19 C18 126.8(2) . . ? N8 C19 C18 124.5(2) . . ? C21 C20 N7 107.3(2) . . ? C21 C20 H20 126.3 . . ? N7 C20 H20 126.3 . . ? C20 C21 N8 107.2(2) . . ? C20 C21 H21 126.4 . . ? N8 C21 H21 126.4 . . ? N8 C22 H22A 109.5 . . ? N8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 N10 111.6(2) . . ? N9 C23 C18 125.0(2) . . ? N10 C23 C18 123.4(2) . . ? C25 C24 N9 110.1(2) . . ? C25 C24 H24 125.0 . . ? N9 C24 H24 125.0 . . ? C24 C25 N10 105.7(2) . . ? C24 C25 H25 127.2 . . ? N10 C25 H25 127.2 . . ? N10 C26 H26A 109.5 . . ? N10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 N1 N2 120.6(2) . . ? C8 N1 Ru1 122.74(17) . . ? N2 N1 Ru1 116.64(14) . . ? C1 N2 N1 119.38(19) . . ? C10 N3 C11 106.4(2) . . ? C10 N3 Ru1 117.60(16) . . ? C11 N3 Ru1 136.02(16) . . ? C10 N4 C12 107.11(19) . . ? C10 N4 C13 126.6(2) . . ? C12 N4 C13 126.3(2) . . ? C14 N5 C15 107.1(2) . . ? C14 N5 Ru1 117.98(17) . . ? C15 N5 Ru1 134.20(17) . . ? C14 N6 C16 107.1(2) . . ? C14 N6 C17 127.4(2) . . ? C16 N6 C17 125.5(2) . . ? C19 N7 C20 108.4(2) . . ? C19 N7 H7 130(3) . . ? C20 N7 H7 121(3) . . ? C19 N8 C21 108.3(2) . . ? C19 N8 C22 126.1(2) . . ? C21 N8 C22 125.6(2) . . ? C23 N9 C24 105.3(2) . . ? C23 N10 C25 107.4(2) . . ? C23 N10 C26 127.2(2) . . ? C25 N10 C26 125.4(2) . . ? F3 P1 F4 92.38(16) . . ? F3 P1 F1S 138.6(10) . . ? F4 P1 F1S 46.4(10) . . ? F3 P1 F2S 126.2(14) . . ? F4 P1 F2S 140.3(14) . . ? F1S P1 F2S 95.2(17) . . ? F3 P1 F6 89.70(12) . . ? F4 P1 F6 91.32(10) . . ? F1S P1 F6 87.5(8) . . ? F2S P1 F6 97.3(12) . . ? F3 P1 F2 90.70(15) . . ? F4 P1 F2 176.64(15) . . ? F1S P1 F2 130.6(10) . . ? F6 P1 F2 90.03(11) . . ? F4 P1 F3S 122.6(13) . . ? F1S P1 F3S 168.8(16) . . ? F2S P1 F3S 95.2(19) . . ? F6 P1 F3S 95.5(11) . . ? F2 P1 F3S 60.3(13) . . ? F3 P1 F4S 50.3(10) . . ? F1S P1 F4S 88.3(14) . . ? F2S P1 F4S 172.0(15) . . ? F6 P1 F4S 90.1(8) . . ? F2 P1 F4S 141.0(10) . . ? F3S P1 F4S 80.9(16) . . ? F3 P1 F5 89.75(11) . . ? F4 P1 F5 88.70(10) . . ? F1S P1 F5 92.9(8) . . ? F2S P1 F5 83.1(12) . . ? F6 P1 F5 179.45(13) . . ? F2 P1 F5 89.97(10) . . ? F3S P1 F5 84.1(11) . . ? F4S P1 F5 89.6(8) . . ? F3 P1 F1 178.38(17) . . ? F4 P1 F1 89.19(15) . . ? F2S P1 F1 52.2(14) . . ? F6 P1 F1 90.65(11) . . ? F2 P1 F1 87.72(13) . . ? F3S P1 F1 147.3(14) . . ? F4S P1 F1 131.3(10) . . ? F5 P1 F1 89.90(10) . . ? F10 P2 F9 89.74(10) . . ? F10 P2 F12 91.03(9) . . ? F9 P2 F12 89.99(11) . . ? F10 P2 F8 177.72(11) . . ? F9 P2 F8 89.87(10) . . ? F12 P2 F8 91.21(10) . . ? F10 P2 F7 89.66(10) . . ? F9 P2 F7 179.41(10) . . ? F12 P2 F7 89.97(10) . . ? F8 P2 F7 90.72(11) . . ? F10 P2 F11 89.29(9) . . ? F9 P2 F11 91.00(11) . . ? F12 P2 F11 178.96(12) . . ? F8 P2 F11 88.47(9) . . ? F7 P2 F11 89.04(10) . . ? N1 Ru1 N1 93.38(11) 2_655 . ? N1 Ru1 N3 85.11(8) 2_655 2_655 ? N1 Ru1 N3 96.18(8) . 2_655 ? N1 Ru1 N3 96.19(8) 2_655 . ? N1 Ru1 N3 85.11(8) . . ? N3 Ru1 N3 178.12(13) 2_655 . ? N1 Ru1 N5 86.25(7) 2_655 2_655 ? N1 Ru1 N5 177.10(9) . 2_655 ? N3 Ru1 N5 86.65(8) 2_655 2_655 ? N3 Ru1 N5 92.08(8) . 2_655 ? N1 Ru1 N5 177.10(9) 2_655 . ? N1 Ru1 N5 86.25(7) . . ? N3 Ru1 N5 92.07(8) 2_655 . ? N3 Ru1 N5 86.65(8) . . ? N5 Ru1 N5 94.26(12) 2_655 . ? 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 N2 C1 C2 C3 -176.2(2) . . . . ? C18 C1 C2 C3 -1.0(4) . . . . ? N2 C1 C2 C7 1.2(4) . . . . ? C18 C1 C2 C7 176.4(2) . . . . ? C7 C2 C3 C4 -0.3(4) . . . . ? C1 C2 C3 C4 177.0(3) . . . . ? C2 C3 C4 C5 0.8(4) . . . . ? C3 C4 C5 C6 -0.5(4) . . . . ? C4 C5 C6 C7 -0.4(4) . . . . ? C3 C2 C7 C6 -0.6(4) . . . . ? C1 C2 C7 C6 -178.1(2) . . . . ? C3 C2 C7 C8 176.6(2) . . . . ? C1 C2 C7 C8 -0.9(3) . . . . ? C5 C6 C7 C2 0.9(4) . . . . ? C5 C6 C7 C8 -176.0(3) . . . . ? C2 C7 C8 N1 0.2(4) . . . . ? C6 C7 C8 N1 177.2(2) . . . . ? C2 C7 C8 C9 -178.7(2) . . . . ? C6 C7 C8 C9 -1.7(4) . . . . ? N1 C8 C9 C14 -58.2(3) . . . . ? C7 C8 C9 C14 120.7(2) . . . . ? N1 C8 C9 C10 60.2(3) . . . . ? C7 C8 C9 C10 -120.8(2) . . . . ? C14 C9 C10 N3 58.0(3) . . . . ? C8 C9 C10 N3 -59.8(3) . . . . ? C14 C9 C10 N4 -124.7(3) . . . . ? C8 C9 C10 N4 117.5(3) . . . . ? N3 C11 C12 N4 -0.3(3) . . . . ? C10 C9 C14 N5 -53.3(3) . . . . ? C8 C9 C14 N5 64.0(3) . . . . ? C10 C9 C14 N6 129.6(3) . . . . ? C8 C9 C14 N6 -113.1(3) . . . . ? N5 C15 C16 N6 0.0(3) . . . . ? N2 C1 C18 C19 -123.2(2) . . . . ? C2 C1 C18 C19 61.2(3) . . . . ? N2 C1 C18 C23 2.2(3) . . . . ? C2 C1 C18 C23 -173.4(2) . . . . ? C23 C18 C19 N7 -96.1(3) . . . . ? C1 C18 C19 N7 29.7(3) . . . . ? C23 C18 C19 N8 82.1(3) . . . . ? C1 C18 C19 N8 -152.0(2) . . . . ? N7 C20 C21 N8 0.1(3) . . . . ? C19 C18 C23 N9 39.8(3) . . . . ? C1 C18 C23 N9 -86.7(3) . . . . ? C19 C18 C23 N10 -144.0(2) . . . . ? C1 C18 C23 N10 89.5(3) . . . . ? N9 C24 C25 N10 0.7(3) . . . . ? C7 C8 N1 N2 0.4(4) . . . . ? C9 C8 N1 N2 179.4(2) . . . . ? C7 C8 N1 Ru1 179.56(17) . . . . ? C9 C8 N1 Ru1 -1.5(3) . . . . ? C2 C1 N2 N1 -0.6(4) . . . . ? C18 C1 N2 N1 -176.1(2) . . . . ? C8 N1 N2 C1 -0.2(3) . . . . ? Ru1 N1 N2 C1 -179.39(17) . . . . ? N4 C10 N3 C11 0.4(3) . . . . ? C9 C10 N3 C11 178.2(2) . . . . ? N4 C10 N3 Ru1 -179.14(17) . . . . ? C9 C10 N3 Ru1 -1.4(3) . . . . ? C12 C11 N3 C10 -0.1(3) . . . . ? C12 C11 N3 Ru1 179.4(2) . . . . ? N3 C10 N4 C12 -0.6(3) . . . . ? C9 C10 N4 C12 -178.2(3) . . . . ? N3 C10 N4 C13 179.2(3) . . . . ? C9 C10 N4 C13 1.7(5) . . . . ? C11 C12 N4 C10 0.6(3) . . . . ? C11 C12 N4 C13 -179.3(3) . . . . ? N6 C14 N5 C15 0.2(3) . . . . ? C9 C14 N5 C15 -177.4(2) . . . . ? N6 C14 N5 Ru1 171.73(16) . . . . ? C9 C14 N5 Ru1 -5.9(3) . . . . ? C16 C15 N5 C14 -0.1(3) . . . . ? C16 C15 N5 Ru1 -169.6(2) . . . . ? N5 C14 N6 C16 -0.2(3) . . . . ? C9 C14 N6 C16 177.1(2) . . . . ? N5 C14 N6 C17 -176.8(2) . . . . ? C9 C14 N6 C17 0.5(4) . . . . ? C15 C16 N6 C14 0.1(3) . . . . ? C15 C16 N6 C17 176.8(3) . . . . ? N8 C19 N7 C20 -0.8(3) . . . . ? C18 C19 N7 C20 177.6(2) . . . . ? C21 C20 N7 C19 0.5(3) . . . . ? N7 C19 N8 C21 0.9(3) . . . . ? C18 C19 N8 C21 -177.6(2) . . . . ? N7 C19 N8 C22 -178.2(2) . . . . ? C18 C19 N8 C22 3.3(4) . . . . ? C20 C21 N8 C19 -0.6(3) . . . . ? C20 C21 N8 C22 178.5(2) . . . . ? N10 C23 N9 C24 -0.4(3) . . . . ? C18 C23 N9 C24 176.2(2) . . . . ? C25 C24 N9 C23 -0.2(3) . . . . ? N9 C23 N10 C25 0.9(3) . . . . ? C18 C23 N10 C25 -175.8(2) . . . . ? N9 C23 N10 C26 -179.8(2) . . . . ? C18 C23 N10 C26 3.5(4) . . . . ? C24 C25 N10 C23 -1.0(3) . . . . ? C24 C25 N10 C26 179.7(2) . . . . ? C8 N1 Ru1 N1 -139.4(2) . . . 2_655 ? N2 N1 Ru1 N1 39.73(13) . . . 2_655 ? C8 N1 Ru1 N3 135.12(19) . . . 2_655 ? N2 N1 Ru1 N3 -45.71(17) . . . 2_655 ? C8 N1 Ru1 N3 -43.52(19) . . . . ? N2 N1 Ru1 N3 135.65(17) . . . . ? C8 N1 Ru1 N5 43.43(19) . . . . ? N2 N1 Ru1 N5 -137.40(17) . . . . ? C10 N3 Ru1 N1 136.9(2) . . . 2_655 ? C11 N3 Ru1 N1 -42.5(3) . . . 2_655 ? C10 N3 Ru1 N1 44.1(2) . . . . ? C11 N3 Ru1 N1 -135.3(3) . . . . ? C10 N3 Ru1 N5 -136.6(2) . . . 2_655 ? C11 N3 Ru1 N5 44.0(3) . . . 2_655 ? C10 N3 Ru1 N5 -42.4(2) . . . . ? C11 N3 Ru1 N5 138.1(3) . . . . ? C14 N5 Ru1 N1 -38.77(18) . . . . ? C15 N5 Ru1 N1 129.9(3) . . . . ? C14 N5 Ru1 N3 -134.84(19) . . . 2_655 ? C15 N5 Ru1 N3 33.8(2) . . . 2_655 ? C14 N5 Ru1 N3 46.54(19) . . . . ? C15 N5 Ru1 N3 -144.8(2) . . . . ? C14 N5 Ru1 N5 138.4(2) . . . 2_655 ? C15 N5 Ru1 N5 -53.0(2) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.539 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.074 # END Validation Reply Form # Attachment '- complex 3_rev.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 765495' #TrackingRef '- complex 3_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 Cl2 Co2 N10 O2, 2(F6 P), unknown solvate' _chemical_formula_sum 'C28 H34 Cl2 Co2 F12 N10 O2 P2' _chemical_formula_weight 1021.35 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_Int_Tables_number 15 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 32.2485(7) _cell_length_b 11.1423(2) _cell_length_c 27.0595(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.431(2) _cell_angle_gamma 90.00 _cell_volume 9530.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 56342 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 26.09 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method none _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.8314 _exptl_absorpt_correction_T_max 0.9273 _exptl_absorpt_process_details ; The correction was carried out by ABSCOR (Stoe, 1997), a modification of DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166. In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device_type 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,281 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4 _diffrn_reflns_number 8967 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 25.63 _reflns_number_total 8967 _reflns_number_gt 6118 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (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. In total 175 geometrical restrains (SADI, SIMU) were used to stabilise and fix the geometry of the two disordered PF6 counter anions. ; _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^)+(0.0782P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8967 _refine_ls_number_parameters 566 _refine_ls_number_restraints 175 _refine_ls_R_factor_all 0.0611 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.946 _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 C1 C 0.73024(13) 0.3695(3) 0.34936(16) 0.0486(10) Uani 1 1 d . . . H1 H 0.7309 0.2850 0.3542 0.058 Uiso 1 1 calc R . . C2 C 0.76384(13) 0.4414(4) 0.35927(15) 0.0457(10) Uani 1 1 d . . . H2 H 0.7923 0.4179 0.3716 0.055 Uiso 1 1 calc R . . C3 C 0.70750(12) 0.5485(3) 0.33049(12) 0.0320(8) Uani 1 1 d . . . C4 C 0.77540(12) 0.6641(4) 0.35341(16) 0.0451(9) Uani 1 1 d . . . H4A H 0.7700 0.7086 0.3215 0.054 Uiso 1 1 calc R . . H4B H 0.8053 0.6415 0.3620 0.054 Uiso 1 1 calc R . . H4C H 0.7684 0.7148 0.3802 0.054 Uiso 1 1 calc R . . C5 C 0.59762(13) 0.5416(4) 0.21379(14) 0.0457(9) Uani 1 1 d . . . H5 H 0.5770 0.4855 0.1980 0.055 Uiso 1 1 calc R . . C6 C 0.60687(14) 0.6485(4) 0.19365(14) 0.0494(10) Uani 1 1 d . . . H6 H 0.5942 0.6799 0.1616 0.059 Uiso 1 1 calc R . . C7 C 0.64711(11) 0.6269(3) 0.26861(12) 0.0316(7) Uani 1 1 d . . . C8 C 0.65912(15) 0.8162(4) 0.22255(15) 0.0496(10) Uani 1 1 d . . . H8A H 0.6439 0.8567 0.1922 0.060 Uiso 1 1 calc R . . H8B H 0.6884 0.8010 0.2192 0.060 Uiso 1 1 calc R . . H8C H 0.6590 0.8674 0.2520 0.060 Uiso 1 1 calc R . . C9 C 0.67717(10) 0.6505(3) 0.31719(11) 0.0272(7) Uani 1 1 d . . . H9 H 0.6932 0.7263 0.3144 0.033 Uiso 1 1 calc R . . C10 C 0.65202(10) 0.6626(3) 0.35961(11) 0.0265(7) Uani 1 1 d . . . C11 C 0.65207(10) 0.7662(3) 0.39035(12) 0.0281(7) Uani 1 1 d . . . C12 C 0.67326(11) 0.8730(3) 0.38289(13) 0.0330(8) Uani 1 1 d . . . H12 H 0.6885 0.8787 0.3563 0.040 Uiso 1 1 calc R . . C13 C 0.67185(12) 0.9689(3) 0.41422(14) 0.0393(9) Uani 1 1 d . . . H13 H 0.6855 1.0418 0.4088 0.047 Uiso 1 1 calc R . . C14 C 0.65040(13) 0.9601(3) 0.45410(15) 0.0424(9) Uani 1 1 d . . . H14 H 0.6503 1.0268 0.4760 0.051 Uiso 1 1 calc R . . C15 C 0.62964(12) 0.8575(3) 0.46223(13) 0.0365(8) Uani 1 1 d . . . H15 H 0.6150 0.8533 0.4894 0.044 Uiso 1 1 calc R . . C16 C 0.62989(11) 0.7580(3) 0.43029(12) 0.0291(7) Uani 1 1 d . . . C17 C 0.60881(11) 0.6475(3) 0.43493(12) 0.0287(7) Uani 1 1 d . . . C18 C 0.62466(12) 0.3300(3) 0.52176(13) 0.0368(8) Uani 1 1 d . . . H18 H 0.6289 0.2463 0.5180 0.044 Uiso 1 1 calc R . . C19 C 0.64015(12) 0.3945(3) 0.56372(13) 0.0364(8) Uani 1 1 d . . . H19 H 0.6570 0.3658 0.5942 0.044 Uiso 1 1 calc R . . C20 C 0.60368(11) 0.5118(3) 0.50551(12) 0.0309(7) Uani 1 1 d . . . C21 C 0.63488(14) 0.6134(4) 0.58760(15) 0.0483(10) Uani 1 1 d . . . H21A H 0.6510 0.6744 0.5733 0.058 Uiso 1 1 calc R . . H21B H 0.6514 0.5858 0.6200 0.058 Uiso 1 1 calc R . . H21C H 0.6081 0.6479 0.5927 0.058 Uiso 1 1 calc R . . C22 C 0.58418(11) 0.6202(3) 0.47685(12) 0.0309(7) Uani 1 1 d . . . H22 H 0.5858 0.6905 0.5001 0.037 Uiso 1 1 calc R . . C23 C 0.53889(11) 0.5940(3) 0.45375(12) 0.0335(8) Uani 1 1 d . . . C24 C 0.48369(12) 0.5073(4) 0.41047(14) 0.0426(9) Uani 1 1 d . . . H25 H 0.4662 0.4516 0.3893 0.051 Uiso 1 1 calc R . . C25 C 0.46986(13) 0.6048(4) 0.43183(14) 0.0457(10) Uani 1 1 d . . . H24 H 0.4413 0.6303 0.4285 0.055 Uiso 1 1 calc R . . C26 C 0.50578(14) 0.7712(4) 0.48888(16) 0.0510(10) Uani 1 1 d . . . H26A H 0.5237 0.8309 0.4767 0.061 Uiso 1 1 calc R . . H26B H 0.5170 0.7543 0.5246 0.061 Uiso 1 1 calc R . . H26C H 0.4769 0.8025 0.4850 0.061 Uiso 1 1 calc R . . C27 C 0.65265(15) 0.2423(4) 0.23516(15) 0.0514(11) Uani 1 1 d . . . H27A H 0.6781 0.2926 0.2417 0.062 Uiso 1 1 calc R . . H27B H 0.6338 0.2695 0.2042 0.062 Uiso 1 1 calc R . . H27C H 0.6607 0.1586 0.2312 0.062 Uiso 1 1 calc R . . C28 C 0.55031(17) 0.1173(4) 0.4077(2) 0.0671(13) Uani 1 1 d . . . H28A H 0.5729 0.1004 0.4368 0.080 Uiso 1 1 calc R . . H28B H 0.5608 0.1042 0.3765 0.080 Uiso 1 1 calc R . . H28C H 0.5263 0.0637 0.4084 0.080 Uiso 1 1 calc R . . Cl1 Cl 0.63743(3) 0.27579(8) 0.39477(4) 0.0427(2) Uani 1 1 d . . . Cl2 Cl 0.55351(3) 0.39482(10) 0.31682(4) 0.0509(3) Uani 1 1 d . . . Co1 Co 0.629743(17) 0.40452(4) 0.319219(18) 0.03614(14) Uani 1 1 d . . . Co2 Co 0.575358(16) 0.38816(4) 0.408310(17) 0.03335(13) Uani 1 1 d . . . F1 F 0.78426(9) 0.1452(2) 0.34252(11) 0.0438(8) Uani 0.800(5) 1 d PDU A 1 F1S F 0.7684(4) 0.0964(11) 0.3609(4) 0.049(3) Uiso 0.200(5) 1 d PDU A 2 F2 F 0.71548(8) 0.0768(2) 0.32212(10) 0.0623(7) Uani 1 1 d D A 1 F3 F 0.76821(9) -0.0382(2) 0.36779(10) 0.0483(9) Uani 0.800(5) 1 d PDU A 1 F3S F 0.7513(4) -0.0964(10) 0.3307(5) 0.056(4) Uiso 0.200(5) 1 d PDU A 2 F4 F 0.73811(12) -0.0870(3) 0.28973(14) 0.0686(11) Uani 0.800(5) 1 d PDU A 1 F4S F 0.7422(5) -0.0199(16) 0.2545(5) 0.083(5) Uiso 0.200(5) 1 d PDU A 2 F5 F 0.80556(8) -0.0147(3) 0.30621(9) 0.0639(7) Uani 1 1 d D A 1 F6 F 0.75488(10) 0.0992(3) 0.26245(10) 0.0520(9) Uani 0.800(5) 1 d PDU A 1 F6S F 0.7560(4) 0.1592(12) 0.2806(5) 0.056(4) Uiso 0.200(5) 1 d PDU A 2 F7 F 0.5894(2) 0.1416(3) 0.60135(12) 0.082(2) Uani 0.777(9) 1 d PDU B 1 F7S F 0.6214(4) 0.1180(10) 0.6038(4) 0.042(3) Uiso 0.223(9) 1 d PDU B 2 F8 F 0.54456(16) -0.0085(6) 0.5906(3) 0.119(2) Uani 0.777(9) 1 d PDU B 1 F8S F 0.5540(3) 0.0536(12) 0.6004(4) 0.048(4) Uiso 0.223(9) 1 d PDU B 2 F9 F 0.60926(14) -0.0349(3) 0.64293(9) 0.1046(13) Uani 1 1 d D B . F10 F 0.5938(2) -0.1331(3) 0.57249(14) 0.0646(14) Uani 0.777(9) 1 d PDU B 1 F10S F 0.5714(5) -0.1221(12) 0.5677(6) 0.063(5) Uiso 0.223(9) 1 d PDU B 2 F11 F 0.63866(14) 0.0196(7) 0.5775(2) 0.122(3) Uani 0.777(9) 1 d PDU B 1 F11S F 0.6363(3) -0.0570(11) 0.5723(4) 0.044(3) Uiso 0.223(9) 1 d PDU B 2 F12 F 0.57955(10) 0.0424(2) 0.52907(8) 0.0667(8) Uani 1 1 d D B . N1 N 0.69436(10) 0.4353(2) 0.33107(11) 0.0377(7) Uani 1 1 d . . . N2 N 0.74931(9) 0.5563(3) 0.34821(11) 0.0346(7) Uani 1 1 d . . . N3 N 0.62329(10) 0.5285(3) 0.26088(11) 0.0375(7) Uani 1 1 d . . . N4 N 0.63826(10) 0.7022(3) 0.22893(11) 0.0384(7) Uani 1 1 d . . . N5 N 0.63077(9) 0.5651(2) 0.36610(10) 0.0280(6) Uani 1 1 d . . . N6 N 0.60879(9) 0.5578(2) 0.40375(10) 0.0297(6) Uani 1 1 d . . . N7 N 0.60206(9) 0.4030(2) 0.48552(10) 0.0326(6) Uani 1 1 d . . . N8 N 0.62621(9) 0.5120(2) 0.55297(10) 0.0335(6) Uani 1 1 d . . . N9 N 0.52700(10) 0.5006(3) 0.42387(11) 0.0365(7) Uani 1 1 d . . . N10 N 0.50533(10) 0.6604(3) 0.45953(11) 0.0393(7) Uani 1 1 d . . . O1 O 0.63139(14) 0.2515(3) 0.27632(13) 0.0891(14) Uani 1 1 d . . . H1Y H 0.6191 0.1612 0.2751 0.107 Uiso 1 1 d R . . O2 O 0.53730(10) 0.2360(2) 0.40970(11) 0.0480(7) Uani 1 1 d D . . H2Y H 0.5106(8) 0.250(4) 0.3962(16) 0.058 Uiso 1 1 d D . . P1 P 0.76047(3) 0.03132(8) 0.31333(4) 0.0393(2) Uani 1 1 d D . . P2 P 0.59308(3) 0.00359(8) 0.58676(3) 0.0377(2) Uani 1 1 d 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 C1 0.063(3) 0.0294(19) 0.064(3) 0.0109(18) 0.037(2) 0.0192(19) C2 0.049(2) 0.046(2) 0.048(2) 0.0089(18) 0.0240(19) 0.0163(19) C3 0.048(2) 0.0276(17) 0.0263(16) -0.0003(13) 0.0226(15) 0.0051(15) C4 0.041(2) 0.046(2) 0.049(2) -0.0124(18) 0.0111(18) 0.0005(18) C5 0.051(2) 0.057(2) 0.0303(19) -0.0039(18) 0.0108(17) -0.005(2) C6 0.057(3) 0.063(3) 0.0272(18) 0.0041(18) 0.0048(17) 0.003(2) C7 0.0401(19) 0.0344(18) 0.0243(16) 0.0030(14) 0.0158(14) 0.0030(15) C8 0.075(3) 0.040(2) 0.036(2) 0.0138(17) 0.016(2) 0.003(2) C9 0.0360(18) 0.0238(15) 0.0255(15) -0.0001(13) 0.0156(14) 0.0005(14) C10 0.0371(18) 0.0214(15) 0.0245(15) 0.0034(12) 0.0147(14) 0.0048(14) C11 0.0369(18) 0.0234(15) 0.0270(16) 0.0038(13) 0.0135(14) 0.0051(14) C12 0.047(2) 0.0242(16) 0.0336(17) 0.0017(14) 0.0229(16) 0.0042(15) C13 0.052(2) 0.0257(17) 0.048(2) -0.0024(15) 0.0290(18) -0.0018(16) C14 0.063(3) 0.0266(18) 0.046(2) -0.0063(16) 0.0312(19) 0.0011(17) C15 0.053(2) 0.0254(16) 0.0379(19) -0.0023(14) 0.0261(17) 0.0026(15) C16 0.0400(19) 0.0248(16) 0.0270(16) 0.0027(13) 0.0171(14) 0.0064(14) C17 0.0423(19) 0.0232(15) 0.0250(16) 0.0050(13) 0.0173(14) 0.0072(14) C18 0.049(2) 0.0261(17) 0.041(2) 0.0080(15) 0.0218(17) 0.0066(16) C19 0.045(2) 0.0314(18) 0.0352(18) 0.0073(15) 0.0148(16) 0.0052(16) C20 0.0415(19) 0.0271(16) 0.0288(17) 0.0060(14) 0.0181(15) 0.0050(15) C21 0.066(3) 0.038(2) 0.041(2) -0.0067(17) 0.0109(19) -0.0011(19) C22 0.047(2) 0.0232(16) 0.0279(16) 0.0032(13) 0.0218(15) 0.0034(14) C23 0.045(2) 0.0311(18) 0.0290(17) 0.0090(14) 0.0191(15) 0.0068(16) C24 0.042(2) 0.053(2) 0.036(2) 0.0127(18) 0.0173(17) -0.0001(18) C25 0.045(2) 0.057(2) 0.041(2) 0.0182(19) 0.0204(18) 0.011(2) C26 0.068(3) 0.044(2) 0.049(2) 0.0038(19) 0.032(2) 0.020(2) C27 0.077(3) 0.045(2) 0.039(2) -0.0079(18) 0.027(2) 0.005(2) C28 0.078(3) 0.036(2) 0.091(4) -0.005(2) 0.026(3) -0.013(2) Cl1 0.0651(6) 0.0255(4) 0.0466(5) 0.0036(4) 0.0332(5) 0.0039(4) Cl2 0.0661(6) 0.0522(6) 0.0400(5) -0.0046(4) 0.0243(5) -0.0140(5) Co1 0.0545(3) 0.0264(2) 0.0343(3) -0.00422(19) 0.0255(2) -0.0048(2) Co2 0.0476(3) 0.0269(2) 0.0308(2) 0.00136(19) 0.0207(2) -0.0017(2) F1 0.0532(17) 0.0272(14) 0.0501(16) -0.0030(12) 0.0083(13) -0.0027(12) F2 0.0685(16) 0.0524(15) 0.0769(17) 0.0259(13) 0.0410(14) 0.0119(12) F3 0.0671(19) 0.0410(16) 0.0419(16) 0.0179(13) 0.0233(14) 0.0039(14) F4 0.092(3) 0.0360(17) 0.070(3) -0.0157(16) -0.0030(19) -0.0113(16) F5 0.0744(17) 0.0742(18) 0.0542(15) 0.0051(13) 0.0395(13) 0.0176(14) F6 0.076(2) 0.056(2) 0.0285(14) 0.0134(14) 0.0210(14) 0.0152(16) F7 0.174(6) 0.0272(17) 0.0424(19) -0.0081(13) 0.015(2) 0.001(2) F8 0.088(3) 0.097(4) 0.202(6) -0.015(4) 0.100(4) -0.008(3) F9 0.209(4) 0.0626(19) 0.0313(14) 0.0112(13) -0.0019(19) 0.000(2) F10 0.119(4) 0.0241(16) 0.057(2) -0.0045(13) 0.032(2) 0.0129(19) F11 0.065(3) 0.141(6) 0.163(5) 0.053(5) 0.029(3) -0.026(3) F12 0.105(2) 0.0590(16) 0.0349(12) -0.0015(11) 0.0116(13) 0.0323(15) N1 0.0576(19) 0.0225(14) 0.0417(17) 0.0007(12) 0.0306(15) 0.0048(13) N2 0.0407(17) 0.0337(15) 0.0326(15) -0.0002(12) 0.0151(13) 0.0084(13) N3 0.0478(18) 0.0409(17) 0.0278(15) -0.0019(13) 0.0171(13) -0.0063(14) N4 0.0537(19) 0.0356(16) 0.0282(15) 0.0075(13) 0.0136(14) 0.0035(14) N5 0.0387(16) 0.0248(14) 0.0249(13) 0.0013(11) 0.0166(12) 0.0024(12) N6 0.0420(16) 0.0242(14) 0.0285(14) 0.0045(11) 0.0203(12) 0.0033(12) N7 0.0471(17) 0.0261(14) 0.0296(14) 0.0032(12) 0.0196(13) 0.0037(13) N8 0.0452(17) 0.0277(14) 0.0312(15) 0.0020(12) 0.0165(13) 0.0005(13) N9 0.0456(18) 0.0373(16) 0.0319(15) 0.0074(13) 0.0201(13) 0.0015(14) N10 0.0508(19) 0.0408(17) 0.0340(16) 0.0115(14) 0.0270(15) 0.0137(15) O1 0.165(4) 0.0478(18) 0.083(2) -0.0360(17) 0.092(3) -0.049(2) O2 0.0615(18) 0.0368(15) 0.0514(17) 0.0034(12) 0.0253(14) -0.0077(14) P1 0.0603(6) 0.0250(4) 0.0396(5) -0.0018(4) 0.0265(5) -0.0024(4) P2 0.0543(6) 0.0292(5) 0.0308(5) -0.0022(4) 0.0112(4) -0.0014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.332(6) . ? C1 N1 1.377(5) . ? C1 H1 0.9500 . ? C2 N2 1.376(5) . ? C2 H2 0.9500 . ? C3 N1 1.331(4) . ? C3 N2 1.341(5) . ? C3 C9 1.497(5) . ? C4 N2 1.458(5) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.368(6) . ? C5 N3 1.383(5) . ? C5 H5 0.9500 . ? C6 N4 1.382(5) . ? C6 H6 0.9500 . ? C7 N3 1.332(5) . ? C7 N4 1.348(4) . ? C7 C9 1.494(5) . ? C8 N4 1.464(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.537(4) . ? C9 H9 1.0000 . ? C10 N5 1.314(4) . ? C10 C11 1.422(4) . ? C11 C12 1.407(5) . ? C11 C16 1.412(4) . ? C12 C13 1.370(5) . ? C12 H12 0.9500 . ? C13 C14 1.396(5) . ? C13 H13 0.9500 . ? C14 C15 1.365(5) . ? C14 H14 0.9500 . ? C15 C16 1.407(5) . ? C15 H15 0.9500 . ? C16 C17 1.424(5) . ? C17 N6 1.308(4) . ? C17 C22 1.539(4) . ? C18 C19 1.353(5) . ? C18 N7 1.368(4) . ? C18 H18 0.9500 . ? C19 N8 1.396(4) . ? C19 H19 0.9500 . ? C20 N7 1.324(4) . ? C20 N8 1.344(4) . ? C20 C22 1.504(4) . ? C21 N8 1.458(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.499(5) . ? C22 H22 1.0000 . ? C23 N9 1.328(5) . ? C23 N10 1.345(4) . ? C24 C25 1.347(6) . ? C24 N9 1.374(5) . ? C24 H25 0.9500 . ? C25 N10 1.384(5) . ? C25 H24 0.9500 . ? C26 N10 1.467(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O1 1.422(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O2 1.391(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? Cl1 Co2 2.4494(10) . ? Cl1 Co1 2.4693(10) . ? Cl2 Co2 2.4372(11) . ? Cl2 Co1 2.4488(12) . ? Co1 O1 2.069(3) . ? Co1 N1 2.073(3) . ? Co1 N3 2.077(3) . ? Co1 N5 2.190(3) . ? Co2 O2 2.098(3) . ? Co2 N7 2.103(3) . ? Co2 N9 2.107(3) . ? Co2 N6 2.192(3) . ? F1 P1 1.607(3) . ? F1S P1 1.455(10) . ? F2 P1 1.598(3) . ? F3 P1 1.639(3) . ? F3S P1 1.546(10) . ? F4 P1 1.576(3) . ? F4S P1 1.683(12) . ? F5 P1 1.589(3) . ? F6 P1 1.550(3) . ? F6S P1 1.670(11) . ? F7 P2 1.598(3) . ? F7S P2 1.582(9) . ? F8 P2 1.595(4) . ? F8S P2 1.489(10) . ? F9 P2 1.566(3) . ? F10 P2 1.572(3) . ? F10S P2 1.603(12) . ? F11 P2 1.550(4) . ? F11S P2 1.662(9) . ? F12 P2 1.595(2) . ? N5 N6 1.354(4) . ? O1 H1Y 1.0800 . ? O2 H2Y 0.88(2) . ? 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 C2 C1 N1 110.1(3) . . ? C2 C1 H1 124.9 . . ? N1 C1 H1 124.9 . . ? C1 C2 N2 106.7(3) . . ? C1 C2 H2 126.6 . . ? N2 C2 H2 126.6 . . ? N1 C3 N2 110.9(3) . . ? N1 C3 C9 121.9(3) . . ? N2 C3 C9 126.8(3) . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N3 108.7(4) . . ? C6 C5 H5 125.6 . . ? N3 C5 H5 125.6 . . ? C5 C6 N4 106.8(3) . . ? C5 C6 H6 126.6 . . ? N4 C6 H6 126.6 . . ? N3 C7 N4 111.3(3) . . ? N3 C7 C9 122.4(3) . . ? N4 C7 C9 126.1(3) . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 C3 110.9(3) . . ? C7 C9 C10 109.0(3) . . ? C3 C9 C10 107.7(2) . . ? C7 C9 H9 109.7 . . ? C3 C9 H9 109.7 . . ? C10 C9 H9 109.7 . . ? N5 C10 C11 122.2(3) . . ? N5 C10 C9 113.2(3) . . ? C11 C10 C9 124.6(3) . . ? C12 C11 C16 119.9(3) . . ? C12 C11 C10 123.2(3) . . ? C16 C11 C10 116.9(3) . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 121.1(3) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 119.9(3) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C11 119.0(3) . . ? C15 C16 C17 124.5(3) . . ? C11 C16 C17 116.5(3) . . ? N6 C17 C16 122.9(3) . . ? N6 C17 C22 112.9(3) . . ? C16 C17 C22 124.2(3) . . ? C19 C18 N7 109.9(3) . . ? C19 C18 H18 125.0 . . ? N7 C18 H18 125.0 . . ? C18 C19 N8 105.9(3) . . ? C18 C19 H19 127.1 . . ? N8 C19 H19 127.1 . . ? N7 C20 N8 111.2(3) . . ? N7 C20 C22 123.1(3) . . ? N8 C20 C22 125.6(3) . . ? N8 C21 H21A 109.5 . . ? N8 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N8 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C20 109.4(3) . . ? C23 C22 C17 109.5(3) . . ? C20 C22 C17 108.4(3) . . ? C23 C22 H22 109.9 . . ? C20 C22 H22 109.9 . . ? C17 C22 H22 109.9 . . ? N9 C23 N10 111.1(3) . . ? N9 C23 C22 123.1(3) . . ? N10 C23 C22 125.8(3) . . ? C25 C24 N9 109.7(4) . . ? C25 C24 H25 125.2 . . ? N9 C24 H25 125.2 . . ? C24 C25 N10 106.6(3) . . ? C24 C25 H24 126.7 . . ? N10 C25 H24 126.7 . . ? N10 C26 H26A 109.5 . . ? N10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 H27A 109.5 . . ? O1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O2 C28 H28A 109.5 . . ? O2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Co2 Cl1 Co1 82.88(3) . . ? Co2 Cl2 Co1 83.56(4) . . ? O1 Co1 N1 94.95(14) . . ? O1 Co1 N3 97.55(13) . . ? N1 Co1 N3 87.36(12) . . ? O1 Co1 N5 177.61(16) . . ? N1 Co1 N5 82.88(11) . . ? N3 Co1 N5 83.37(11) . . ? O1 Co1 Cl2 94.94(12) . . ? N1 Co1 Cl2 169.89(8) . . ? N3 Co1 Cl2 93.46(9) . . ? N5 Co1 Cl2 87.21(8) . . ? O1 Co1 Cl1 88.65(11) . . ? N1 Co1 Cl1 92.01(9) . . ? N3 Co1 Cl1 173.80(9) . . ? N5 Co1 Cl1 90.43(7) . . ? Cl2 Co1 Cl1 86.09(4) . . ? O2 Co2 N7 99.88(11) . . ? O2 Co2 N9 91.04(12) . . ? N7 Co2 N9 85.88(11) . . ? O2 Co2 N6 173.82(12) . . ? N7 Co2 N6 83.05(11) . . ? N9 Co2 N6 83.71(11) . . ? O2 Co2 Cl2 89.45(8) . . ? N7 Co2 Cl2 170.41(8) . . ? N9 Co2 Cl2 96.23(9) . . ? N6 Co2 Cl2 87.88(8) . . ? O2 Co2 Cl1 95.03(9) . . ? N7 Co2 Cl1 90.17(8) . . ? N9 Co2 Cl1 173.25(9) . . ? N6 Co2 Cl1 90.39(7) . . ? Cl2 Co2 Cl1 86.78(4) . . ? C3 N1 C1 105.2(3) . . ? C3 N1 Co1 117.9(2) . . ? C1 N1 Co1 135.7(3) . . ? C3 N2 C2 107.0(3) . . ? C3 N2 C4 127.4(3) . . ? C2 N2 C4 125.5(3) . . ? C7 N3 C5 106.2(3) . . ? C7 N3 Co1 117.4(2) . . ? C5 N3 Co1 136.2(3) . . ? C7 N4 C6 106.9(3) . . ? C7 N4 C8 127.2(3) . . ? C6 N4 C8 125.8(3) . . ? C10 N5 N6 121.0(3) . . ? C10 N5 Co1 123.1(2) . . ? N6 N5 Co1 115.88(19) . . ? C17 N6 N5 120.4(3) . . ? C17 N6 Co2 124.1(2) . . ? N5 N6 Co2 115.54(19) . . ? C20 N7 C18 106.2(3) . . ? C20 N7 Co2 117.0(2) . . ? C18 N7 Co2 136.1(2) . . ? C20 N8 C19 106.7(3) . . ? C20 N8 C21 127.9(3) . . ? C19 N8 C21 125.4(3) . . ? C23 N9 C24 105.9(3) . . ? C23 N9 Co2 116.9(2) . . ? C24 N9 Co2 137.2(3) . . ? C23 N10 C25 106.8(3) . . ? C23 N10 C26 127.1(3) . . ? C25 N10 C26 126.1(3) . . ? C27 O1 Co1 124.7(3) . . ? C27 O1 H1Y 98.1 . . ? Co1 O1 H1Y 137.3 . . ? C28 O2 Co2 125.8(3) . . ? C28 O2 H2Y 116(3) . . ? Co2 O2 H2Y 112(3) . . ? F1S P1 F3S 101.6(8) . . ? F1S P1 F6 120.8(5) . . ? F3S P1 F6 136.4(6) . . ? F1S P1 F4 139.6(6) . . ? F6 P1 F4 94.9(2) . . ? F1S P1 F5 105.3(5) . . ? F3S P1 F5 88.6(5) . . ? F6 P1 F5 89.87(15) . . ? F4 P1 F5 92.11(18) . . ? F1S P1 F2 73.5(5) . . ? F3S P1 F2 90.7(5) . . ? F6 P1 F2 91.62(15) . . ? F4 P1 F2 88.27(18) . . ? F5 P1 F2 178.42(15) . . ? F3S P1 F1 132.8(5) . . ? F6 P1 F1 90.67(18) . . ? F4 P1 F1 174.45(19) . . ? F5 P1 F1 87.45(16) . . ? F2 P1 F1 92.03(15) . . ? F1S P1 F3 58.1(5) . . ? F3S P1 F3 45.2(5) . . ? F6 P1 F3 177.78(19) . . ? F4 P1 F3 86.85(17) . . ? F5 P1 F3 88.65(14) . . ? F2 P1 F3 89.84(14) . . ? F1 P1 F3 87.62(16) . . ? F1S P1 F6S 91.5(7) . . ? F3S P1 F6S 161.0(7) . . ? F4 P1 F6S 120.9(5) . . ? F5 P1 F6S 101.3(5) . . ? F2 P1 F6S 79.8(5) . . ? F1 P1 F6S 64.5(5) . . ? F3 P1 F6S 149.6(6) . . ? F1S P1 F4S 166.5(7) . . ? F3S P1 F4S 85.6(8) . . ? F6 P1 F4S 50.8(6) . . ? F5 P1 F4S 86.2(6) . . ? F2 P1 F4S 95.2(6) . . ? F1 P1 F4S 140.9(6) . . ? F3 P1 F4S 130.7(6) . . ? F6S P1 F4S 79.1(8) . . ? F8S P2 F11 150.8(6) . . ? F8S P2 F9 89.8(5) . . ? F11 P2 F9 92.6(3) . . ? F8S P2 F10 118.5(5) . . ? F11 P2 F10 90.7(3) . . ? F9 P2 F10 87.4(2) . . ? F8S P2 F7S 95.4(6) . . ? F11 P2 F7S 56.2(5) . . ? F9 P2 F7S 82.9(4) . . ? F10 P2 F7S 144.7(5) . . ? F11 P2 F8 174.2(3) . . ? F9 P2 F8 93.2(3) . . ? F10 P2 F8 89.8(3) . . ? F7S P2 F8 124.5(5) . . ? F8S P2 F12 93.5(5) . . ? F11 P2 F12 83.9(2) . . ? F9 P2 F12 176.5(2) . . ? F10 P2 F12 92.11(18) . . ? F7S P2 F12 95.5(4) . . ? F8 P2 F12 90.3(3) . . ? F8S P2 F7 58.1(5) . . ? F11 P2 F7 92.8(3) . . ? F9 P2 F7 92.91(18) . . ? F10 P2 F7 176.5(3) . . ? F8 P2 F7 86.8(3) . . ? F12 P2 F7 87.78(16) . . ? F8S P2 F10S 94.0(7) . . ? F11 P2 F10S 114.5(6) . . ? F9 P2 F10S 96.5(6) . . ? F7S P2 F10S 170.6(7) . . ? F8 P2 F10S 65.0(6) . . ? F12 P2 F10S 84.6(6) . . ? F7 P2 F10S 150.6(6) . . ? F8S P2 F11S 177.9(6) . . ? F9 P2 F11S 89.0(4) . . ? F10 P2 F11S 59.7(4) . . ? F7S P2 F11S 86.2(6) . . ? F8 P2 F11S 149.3(5) . . ? F12 P2 F11S 87.7(4) . . ? F7 P2 F11S 123.8(5) . . ? F10S P2 F11S 84.4(7) . . ? 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 N1 C1 C2 N2 1.3(4) . . . . ? N3 C5 C6 N4 -0.6(4) . . . . ? N3 C7 C9 C3 55.1(4) . . . . ? N4 C7 C9 C3 -129.4(3) . . . . ? N3 C7 C9 C10 -63.3(4) . . . . ? N4 C7 C9 C10 112.2(4) . . . . ? N1 C3 C9 C7 -51.2(4) . . . . ? N2 C3 C9 C7 136.6(3) . . . . ? N1 C3 C9 C10 68.1(4) . . . . ? N2 C3 C9 C10 -104.2(4) . . . . ? C7 C9 C10 N5 61.0(4) . . . . ? C3 C9 C10 N5 -59.4(4) . . . . ? C7 C9 C10 C11 -120.7(3) . . . . ? C3 C9 C10 C11 118.9(3) . . . . ? N5 C10 C11 C12 -177.5(3) . . . . ? C9 C10 C11 C12 4.4(5) . . . . ? N5 C10 C11 C16 3.2(5) . . . . ? C9 C10 C11 C16 -174.9(3) . . . . ? C16 C11 C12 C13 -0.6(5) . . . . ? C10 C11 C12 C13 -179.9(3) . . . . ? C11 C12 C13 C14 1.5(6) . . . . ? C12 C13 C14 C15 -1.5(6) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C14 C15 C16 C11 0.4(5) . . . . ? C14 C15 C16 C17 -179.0(4) . . . . ? C12 C11 C16 C15 -0.3(5) . . . . ? C10 C11 C16 C15 179.0(3) . . . . ? C12 C11 C16 C17 179.2(3) . . . . ? C10 C11 C16 C17 -1.5(5) . . . . ? C15 C16 C17 N6 178.2(3) . . . . ? C11 C16 C17 N6 -1.3(5) . . . . ? C15 C16 C17 C22 -2.4(5) . . . . ? C11 C16 C17 C22 178.1(3) . . . . ? N7 C18 C19 N8 0.5(4) . . . . ? N7 C20 C22 C23 52.1(4) . . . . ? N8 C20 C22 C23 -131.0(3) . . . . ? N7 C20 C22 C17 -67.2(4) . . . . ? N8 C20 C22 C17 109.7(4) . . . . ? N6 C17 C22 C23 -60.8(4) . . . . ? C16 C17 C22 C23 119.7(3) . . . . ? N6 C17 C22 C20 58.4(4) . . . . ? C16 C17 C22 C20 -121.0(3) . . . . ? C20 C22 C23 N9 -54.7(4) . . . . ? C17 C22 C23 N9 63.9(4) . . . . ? C20 C22 C23 N10 126.1(3) . . . . ? C17 C22 C23 N10 -115.3(3) . . . . ? N9 C24 C25 N10 -0.3(4) . . . . ? Co2 Cl2 Co1 O1 121.69(11) . . . . ? Co2 Cl2 Co1 N1 -46.1(5) . . . . ? Co2 Cl2 Co1 N3 -140.41(9) . . . . ? Co2 Cl2 Co1 N5 -57.23(7) . . . . ? Co2 Cl2 Co1 Cl1 33.39(3) . . . . ? Co2 Cl1 Co1 O1 -128.30(13) . . . . ? Co2 Cl1 Co1 N1 136.80(8) . . . . ? Co2 Cl1 Co1 N5 53.91(8) . . . . ? Co2 Cl1 Co1 Cl2 -33.26(3) . . . . ? Co1 Cl2 Co2 O2 -128.74(9) . . . . ? Co1 Cl2 Co2 N9 140.27(9) . . . . ? Co1 Cl2 Co2 N6 56.84(8) . . . . ? Co1 Cl2 Co2 Cl1 -33.67(3) . . . . ? Co1 Cl1 Co2 O2 122.57(8) . . . . ? Co1 Cl1 Co2 N7 -137.49(8) . . . . ? Co1 Cl1 Co2 N6 -54.44(8) . . . . ? Co1 Cl1 Co2 Cl2 33.41(3) . . . . ? N2 C3 N1 C1 -1.1(4) . . . . ? C9 C3 N1 C1 -174.5(3) . . . . ? N2 C3 N1 Co1 167.9(2) . . . . ? C9 C3 N1 Co1 -5.5(4) . . . . ? C2 C1 N1 C3 -0.2(4) . . . . ? C2 C1 N1 Co1 -166.2(3) . . . . ? O1 Co1 N1 C3 141.5(3) . . . . ? N3 Co1 N1 C3 44.2(3) . . . . ? N5 Co1 N1 C3 -39.5(2) . . . . ? Cl2 Co1 N1 C3 -50.7(6) . . . . ? Cl1 Co1 N1 C3 -129.6(2) . . . . ? O1 Co1 N1 C1 -53.7(4) . . . . ? N3 Co1 N1 C1 -151.1(4) . . . . ? N5 Co1 N1 C1 125.3(4) . . . . ? Cl2 Co1 N1 C1 114.1(5) . . . . ? Cl1 Co1 N1 C1 35.1(4) . . . . ? N1 C3 N2 C2 1.9(4) . . . . ? C9 C3 N2 C2 174.9(3) . . . . ? N1 C3 N2 C4 179.8(3) . . . . ? C9 C3 N2 C4 -7.2(5) . . . . ? C1 C2 N2 C3 -1.9(4) . . . . ? C1 C2 N2 C4 -179.9(3) . . . . ? N4 C7 N3 C5 -0.3(4) . . . . ? C9 C7 N3 C5 175.8(3) . . . . ? N4 C7 N3 Co1 -176.9(2) . . . . ? C9 C7 N3 Co1 -0.8(4) . . . . ? C6 C5 N3 C7 0.5(4) . . . . ? C6 C5 N3 Co1 176.1(3) . . . . ? O1 Co1 N3 C7 -135.6(3) . . . . ? N1 Co1 N3 C7 -40.9(3) . . . . ? N5 Co1 N3 C7 42.2(3) . . . . ? Cl2 Co1 N3 C7 129.0(2) . . . . ? O1 Co1 N3 C5 49.2(4) . . . . ? N1 Co1 N3 C5 143.9(4) . . . . ? N5 Co1 N3 C5 -133.0(4) . . . . ? Cl2 Co1 N3 C5 -46.2(4) . . . . ? N3 C7 N4 C6 0.0(4) . . . . ? C9 C7 N4 C6 -175.9(3) . . . . ? N3 C7 N4 C8 -177.0(3) . . . . ? C9 C7 N4 C8 7.1(6) . . . . ? C5 C6 N4 C7 0.4(4) . . . . ? C5 C6 N4 C8 177.4(4) . . . . ? C11 C10 N5 N6 -2.0(5) . . . . ? C9 C10 N5 N6 176.3(3) . . . . ? C11 C10 N5 Co1 179.7(2) . . . . ? C9 C10 N5 Co1 -2.0(4) . . . . ? N1 Co1 N5 C10 45.5(3) . . . . ? N3 Co1 N5 C10 -42.7(3) . . . . ? Cl2 Co1 N5 C10 -136.5(3) . . . . ? Cl1 Co1 N5 C10 137.4(3) . . . . ? N1 Co1 N5 N6 -132.9(2) . . . . ? N3 Co1 N5 N6 138.9(2) . . . . ? Cl2 Co1 N5 N6 45.1(2) . . . . ? Cl1 Co1 N5 N6 -40.9(2) . . . . ? C16 C17 N6 N5 2.7(5) . . . . ? C22 C17 N6 N5 -176.8(3) . . . . ? C16 C17 N6 Co2 -178.3(2) . . . . ? C22 C17 N6 Co2 2.2(4) . . . . ? C10 N5 N6 C17 -1.0(5) . . . . ? Co1 N5 N6 C17 177.5(2) . . . . ? C10 N5 N6 Co2 179.9(2) . . . . ? Co1 N5 N6 Co2 -1.7(3) . . . . ? N7 Co2 N6 C17 -45.0(3) . . . . ? N9 Co2 N6 C17 41.6(3) . . . . ? Cl2 Co2 N6 C17 138.1(3) . . . . ? Cl1 Co2 N6 C17 -135.2(3) . . . . ? N7 Co2 N6 N5 134.0(2) . . . . ? N9 Co2 N6 N5 -139.4(2) . . . . ? Cl2 Co2 N6 N5 -42.8(2) . . . . ? Cl1 Co2 N6 N5 43.9(2) . . . . ? N8 C20 N7 C18 -0.1(4) . . . . ? C22 C20 N7 C18 177.2(3) . . . . ? N8 C20 N7 Co2 -171.9(2) . . . . ? C22 C20 N7 Co2 5.4(4) . . . . ? C19 C18 N7 C20 -0.2(4) . . . . ? C19 C18 N7 Co2 169.2(3) . . . . ? O2 Co2 N7 C20 -135.9(2) . . . . ? N9 Co2 N7 C20 -45.6(3) . . . . ? N6 Co2 N7 C20 38.6(2) . . . . ? Cl1 Co2 N7 C20 129.0(2) . . . . ? O2 Co2 N7 C18 55.5(3) . . . . ? N9 Co2 N7 C18 145.9(3) . . . . ? N6 Co2 N7 C18 -130.0(3) . . . . ? Cl1 Co2 N7 C18 -39.6(3) . . . . ? N7 C20 N8 C19 0.4(4) . . . . ? C22 C20 N8 C19 -176.8(3) . . . . ? N7 C20 N8 C21 -179.3(3) . . . . ? C22 C20 N8 C21 3.4(5) . . . . ? C18 C19 N8 C20 -0.5(4) . . . . ? C18 C19 N8 C21 179.2(3) . . . . ? N10 C23 N9 C24 -0.7(4) . . . . ? C22 C23 N9 C24 -180.0(3) . . . . ? N10 C23 N9 Co2 178.2(2) . . . . ? C22 C23 N9 Co2 -1.1(4) . . . . ? C25 C24 N9 C23 0.6(4) . . . . ? C25 C24 N9 Co2 -177.9(3) . . . . ? O2 Co2 N9 C23 143.2(2) . . . . ? N7 Co2 N9 C23 43.4(2) . . . . ? N6 Co2 N9 C23 -40.0(2) . . . . ? Cl2 Co2 N9 C23 -127.2(2) . . . . ? O2 Co2 N9 C24 -38.4(3) . . . . ? N7 Co2 N9 C24 -138.2(3) . . . . ? N6 Co2 N9 C24 138.3(3) . . . . ? Cl2 Co2 N9 C24 51.2(3) . . . . ? N9 C23 N10 C25 0.5(4) . . . . ? C22 C23 N10 C25 179.8(3) . . . . ? N9 C23 N10 C26 -178.8(3) . . . . ? C22 C23 N10 C26 0.4(5) . . . . ? C24 C25 N10 C23 -0.1(4) . . . . ? C24 C25 N10 C26 179.2(3) . . . . ? N1 Co1 O1 C27 -48.6(4) . . . . ? N3 Co1 O1 C27 39.3(4) . . . . ? Cl2 Co1 O1 C27 133.5(4) . . . . ? Cl1 Co1 O1 C27 -140.5(4) . . . . ? N7 Co2 O2 C28 -86.1(4) . . . . ? N9 Co2 O2 C28 -172.1(4) . . . . ? Cl2 Co2 O2 C28 91.7(4) . . . . ? Cl1 Co2 O2 C28 5.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.781 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.082 # SQUEEZE RESULTS 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 1 0.250 0.918 0.000 233.5 72.8 2 0.750 0.418 0.000 233.5 72.8 3 0.500 0.936 0.250 370.9 97.2 4 1.000 0.436 0.250 370.9 97.2 5 0.250 -0.010 0.500 233.5 73.0 6 0.750 0.472 0.500 233.5 73.0 7 0.500 0.064 0.750 371.0 95.1 8 1.000 0.564 0.750 371.0 95.1 _platon_squeeze_details ; ? ; # Start Validation Reply Form _vrf_PLAT606_3 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! RESPONSE: In the crystal structure there is a region of disordered solvent molecules, which could not be modeled satisfactory (Trial modeling attempts indicated a mixture of methanol/diethyl ether). The program SQUEEZE (Platon) was used to remove the contribution of these diffusely scattering species from the structure factor calculation. The program calculated a solvent accessible region of 2404 Ang^3 (676 electrons) per unit cell (25% of the total unit cell volume). The reported formula weigth, F(000) and density reflect the known unit cell contents only. ; # END Validation Reply Form # Attachment '- complex 4_rev.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 765496' #TrackingRef '- complex 4_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H52 Cl2 F12 N12 O3 P2 Ru2 S2' _chemical_formula_weight 1352.02 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' F F 0.0171 0.0103 '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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 33.4681(12) _cell_length_b 13.7678(5) _cell_length_c 11.1687(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5146.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 48995 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 27.19 _exptl_crystal_description lath _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details ; The correction was carried out by ABSCOR (Stoe, 1997), a modification of DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166. In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones. ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'long fine focus sealed X-ray tube' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_ambient_temperature 100(2) _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,202 exposures' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40436 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_full 26.80 _reflns_number_total 9913 _reflns_number_gt 8884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material 'SHELXL97 (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. In total 11 geometrical restrains (DFIX) were used to stabilise and fix the geometry of two disordered solvent molecules (acetonitrile), of one neutral ligand (dmso) and of one N-methylimidazole ring of the bimptz ligand. According to the structure refinement the investigated crystal is a twin. In the final refinement this was taken into account by the use of the instruction TWIN -1 0 0 0 -1 0 0 -1 2 and BASF of the program SHELXL97. The amounts of the two twin components are 0.426 and 0.574. ; _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^)+(0.0671P)^2^+38.9492P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 4669 Friedel pairs' _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_number_reflns 9913 _refine_ls_number_parameters 630 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0754 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1682 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.878 _refine_diff_density_min -1.401 _refine_diff_density_rms 0.135 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 C1 C 0.8674(3) 0.5573(6) 0.7956(11) 0.030(2) Uani 1 1 d . . . C2 C 0.8886(3) 0.5797(6) 0.8990(10) 0.030(2) Uani 1 1 d . . . C3 C 0.8892(4) 0.5238(7) 1.0050(12) 0.046(3) Uani 1 1 d . . . H3 H 0.8758 0.4630 1.0053 0.055 Uiso 1 1 calc R . . C4 C 0.9075(4) 0.5524(10) 1.1044(13) 0.062(4) Uani 1 1 d . . . H4 H 0.9055 0.5139 1.1747 0.075 Uiso 1 1 calc R . . C5 C 0.9297(4) 0.6382(9) 1.1073(12) 0.049(3) Uani 1 1 d . . . H5 H 0.9433 0.6568 1.1784 0.059 Uiso 1 1 calc R . . C6 C 0.9319(3) 0.6946(7) 1.0083(10) 0.032(2) Uani 1 1 d . . . H6 H 0.9473 0.7525 1.0100 0.038 Uiso 1 1 calc R . . C7 C 0.9112(3) 0.6682(6) 0.9015(10) 0.0273(19) Uani 1 1 d . . . C8 C 0.9107(3) 0.7246(6) 0.7940(10) 0.0253(19) Uani 1 1 d . . . C9 C 0.8434(3) 0.4626(6) 0.7789(13) 0.041(3) Uani 1 1 d . . . H9 H 0.8450 0.4212 0.8523 0.049 Uiso 1 1 calc R . . C10 C 0.8009(3) 0.4921(7) 0.7543(12) 0.040(3) Uani 1 1 d . . . C11 C 0.7499(3) 0.5568(10) 0.6678(13) 0.055(3) Uani 1 1 d . . . H11 H 0.7340 0.5916 0.6120 0.066 Uiso 1 1 calc R . . C12 C 0.7365(4) 0.5156(10) 0.7631(13) 0.056(3) Uani 1 1 d . . . H12 H 0.7094 0.5144 0.7886 0.068 Uiso 1 1 calc R . . C13 C 0.7664(4) 0.4164(10) 0.9312(13) 0.059(3) Uani 1 1 d . . . H13A H 0.7756 0.3501 0.9151 0.088 Uiso 1 1 calc R . . H13B H 0.7387 0.4146 0.9600 0.088 Uiso 1 1 calc R . . H13C H 0.7835 0.4462 0.9923 0.088 Uiso 1 1 calc R . . C14 C 0.8602(4) 0.4092(7) 0.6707(13) 0.045(3) Uani 1 1 d . . . C15 C 0.8792(4) 0.3793(10) 0.4936(13) 0.055(3) Uani 1 1 d . . . H15 H 0.8842 0.3842 0.4101 0.066 Uiso 1 1 calc R . . C16 C 0.8907(4) 0.3070(9) 0.5639(19) 0.070(4) Uani 1 1 d . . . H16 H 0.9050 0.2512 0.5382 0.084 Uiso 1 1 calc R . . C17 C 0.8887(5) 0.2684(10) 0.7830(11) 0.034(3) Uiso 0.70 1 d PD . . H17A H 0.8719 0.2101 0.7858 0.051 Uiso 0.70 1 calc PR . . H17B H 0.8835 0.3085 0.8538 0.051 Uiso 0.70 1 calc PR . . H17C H 0.9169 0.2494 0.7818 0.051 Uiso 0.70 1 calc PR . . C172 C 0.866(2) 0.265(5) 0.776(5) 0.13(3) Uiso 0.30 1 d PD . . H17D H 0.8383 0.2828 0.7966 0.202 Uiso 0.30 1 calc PR . . H17E H 0.8832 0.2765 0.8450 0.202 Uiso 0.30 1 calc PR . . H17F H 0.8668 0.1961 0.7540 0.202 Uiso 0.30 1 calc PR . . S11 S 0.79744(12) 0.5399(4) 0.3886(6) 0.0840(15) Uani 1 1 d D . . O11 O 0.7746(4) 0.4424(9) 0.4095(14) 0.101(4) Uani 1 1 d . . . C18 C 0.7608(5) 0.6197(12) 0.3488(16) 0.076(5) Uani 1 1 d . . . H18A H 0.7467 0.5950 0.2782 0.114 Uiso 1 1 calc R . . H18B H 0.7727 0.6829 0.3301 0.114 Uiso 1 1 calc R . . H18C H 0.7419 0.6270 0.4152 0.114 Uiso 1 1 calc R . . C19 C 0.8246(5) 0.506(2) 0.2658(14) 0.051(8) Uiso 0.63(6) 1 d PD . . H19A H 0.8407 0.4488 0.2851 0.076 Uiso 0.63(6) 1 calc PR . . H19B H 0.8423 0.5597 0.2423 0.076 Uiso 0.63(6) 1 calc PR . . H19C H 0.8064 0.4910 0.1996 0.076 Uiso 0.63(6) 1 calc PR . . C192 C 0.8193(13) 0.564(5) 0.253(2) 0.071(16) Uiso 0.37(6) 1 d PD . . H19D H 0.8477 0.5461 0.2569 0.107 Uiso 0.37(6) 1 calc PR . . H19E H 0.8167 0.6328 0.2349 0.107 Uiso 0.37(6) 1 calc PR . . H19F H 0.8061 0.5252 0.1909 0.107 Uiso 0.37(6) 1 calc PR . . C20 C 0.9334(3) 0.8210(6) 0.7815(9) 0.0236(18) Uani 1 1 d . . . H20 H 0.9502 0.8325 0.8542 0.028 Uiso 1 1 calc R . . C21 C 0.9027(3) 0.8973(6) 0.7712(10) 0.0259(18) Uani 1 1 d . . . C22 C 0.8495(3) 0.9732(7) 0.7003(11) 0.034(2) Uani 1 1 d . . . H22 H 0.8276 0.9908 0.6507 0.041 Uiso 1 1 calc R . . C23 C 0.8593(3) 1.0140(7) 0.8059(11) 0.037(2) Uani 1 1 d . . . H23 H 0.8460 1.0668 0.8434 0.045 Uiso 1 1 calc R . . C24 C 0.9141(3) 0.9888(7) 0.9607(11) 0.037(2) Uani 1 1 d . . . H24A H 0.9133 0.9327 1.0146 0.056 Uiso 1 1 calc R . . H24B H 0.9017 1.0448 1.0002 0.056 Uiso 1 1 calc R . . H24C H 0.9419 1.0042 0.9411 0.056 Uiso 1 1 calc R . . C25 C 0.9589(3) 0.8180(6) 0.6738(10) 0.0233(18) Uani 1 1 d . . . C26 C 0.9740(3) 0.7982(6) 0.4835(11) 0.030(2) Uani 1 1 d . . . H26 H 0.9717 0.7911 0.3992 0.036 Uiso 1 1 calc R . . C27 C 1.0088(2) 0.8022(6) 0.5479(13) 0.0317(17) Uani 1 1 d . . . H27 H 1.0351 0.7983 0.5162 0.038 Uiso 1 1 calc R . . C28 C 1.0270(3) 0.8203(8) 0.7679(11) 0.038(2) Uani 1 1 d . . . H28A H 1.0246 0.8845 0.8050 0.057 Uiso 1 1 calc R . . H28B H 1.0543 0.8111 0.7386 0.057 Uiso 1 1 calc R . . H28C H 1.0208 0.7701 0.8273 0.057 Uiso 1 1 calc R . . C29 C 0.9127(3) 0.9819(7) 0.3832(12) 0.039(2) Uani 1 1 d . . . H29A H 0.9043 1.0339 0.3289 0.059 Uiso 1 1 calc R . . H29B H 0.9351 0.9463 0.3475 0.059 Uiso 1 1 calc R . . H29C H 0.9211 1.0100 0.4598 0.059 Uiso 1 1 calc R . . C30 C 0.8673(4) 0.8502(11) 0.2634(12) 0.057(3) Uani 1 1 d . . . H30A H 0.8458 0.8021 0.2631 0.086 Uiso 1 1 calc R . . H30B H 0.8925 0.8188 0.2410 0.086 Uiso 1 1 calc R . . H30C H 0.8612 0.9018 0.2059 0.086 Uiso 1 1 calc R . . N100 N 0.7934(7) 0.2502(14) 0.6927(10) 0.071(6) Uiso 0.60 1 d PD . . C101 C 0.7975(5) 0.2264(11) 0.5966(9) 0.034(4) Uiso 0.60 1 d PD . . C102 C 0.8040(7) 0.1904(17) 0.4762(11) 0.064(6) Uiso 0.60 1 d PD . . H10A H 0.8324 0.1747 0.4657 0.096 Uiso 0.60 1 calc PR . . H10B H 0.7963 0.2402 0.4181 0.096 Uiso 0.60 1 calc PR . . H10C H 0.7880 0.1318 0.4634 0.096 Uiso 0.60 1 calc PR . . N200 N 0.8055(10) 0.657(2) 1.030(3) 0.135(13) Uiso 0.50 1 d PD . . C201 C 0.8013(8) 0.7150(18) 0.959(2) 0.065(7) Uiso 0.50 1 d PD . . C202 C 0.7979(9) 0.7912(18) 0.870(2) 0.062(7) Uiso 0.50 1 d PD . . H20A H 0.8005 0.8547 0.9089 0.093 Uiso 0.50 1 calc PR . . H20B H 0.7718 0.7868 0.8305 0.093 Uiso 0.50 1 calc PR . . H20C H 0.8191 0.7837 0.8102 0.093 Uiso 0.50 1 calc PR . . O300 O 0.9863(4) 0.6078(8) 0.7617(11) 0.066(3) Uani 0.877(19) 1 d P . . C301 C 1.0044(6) 0.5395(13) 0.8381(19) 0.077(6) Uani 0.877(19) 1 d P . . H30D H 1.0026 0.5618 0.9222 0.092 Uiso 0.877(19) 1 calc PR . . H30E H 1.0329 0.5318 0.8170 0.092 Uiso 0.877(19) 1 calc PR . . C302 C 0.9831(6) 0.4453(11) 0.8241(17) 0.077(6) Uani 0.877(19) 1 d P . . H30F H 0.9604 0.4388 0.8802 0.092 Uiso 0.877(19) 1 calc PR . . H30G H 1.0013 0.3889 0.8326 0.092 Uiso 0.877(19) 1 calc PR . . C303 C 0.9689(6) 0.4606(11) 0.690(2) 0.086(7) Uani 0.877(19) 1 d P . . H30H H 0.9797 0.4091 0.6371 0.103 Uiso 0.877(19) 1 calc PR . . H30I H 0.9394 0.4606 0.6844 0.103 Uiso 0.877(19) 1 calc PR . . C304 C 0.9848(5) 0.5534(9) 0.6585(16) 0.057(4) Uani 0.877(19) 1 d P . . H30J H 1.0119 0.5461 0.6242 0.069 Uiso 0.877(19) 1 calc PR . . H30K H 0.9676 0.5854 0.5984 0.069 Uiso 0.877(19) 1 calc PR . . Cl1 Cl 0.89011(8) 0.64886(19) 0.4265(6) 0.0372(5) Uani 1 1 d . . . Cl2 Cl 0.81212(6) 0.75167(17) 0.5472(6) 0.0397(5) Uani 1 1 d . . . F1 F 0.8130(3) 0.2438(6) 0.1999(9) 0.068(2) Uani 1 1 d . . . F2 F 0.8630(5) 0.1336(12) 0.1937(16) 0.153(5) Uiso 1 1 d . . . F3 F 0.8300(2) 0.1664(6) 0.0281(10) 0.072(2) Uani 1 1 d . . . F4 F 0.8436(3) 0.3204(5) 0.0525(15) 0.092(3) Uani 1 1 d . . . F51 F 0.8786(4) 0.3126(10) 0.1963(14) 0.069(4) Uiso 0.60 1 d P . . F52 F 0.8749(6) 0.2538(14) 0.2497(19) 0.058(5) Uiso 0.40 1 d P . . F6 F 0.89322(18) 0.2132(6) 0.0511(13) 0.084(3) Uani 1 1 d . . . F7 F 0.9878(2) 1.0374(5) 0.7606(9) 0.065(2) Uani 1 1 d . . . F8 F 1.0317(2) 1.1416(5) 0.6785(8) 0.0562(18) Uani 1 1 d . . . F9 F 0.9741(3) 1.1960(6) 0.7534(9) 0.071(2) Uani 1 1 d . . . F10 F 0.93947(19) 1.0917(4) 0.6388(8) 0.0446(15) Uani 1 1 d . . . F11 F 0.9967(2) 1.0364(7) 0.5633(11) 0.084(3) Uani 1 1 d . . . F12 F 0.9830(2) 1.1949(6) 0.5572(10) 0.084(3) Uani 1 1 d . . . N1 N 0.8680(3) 0.6161(5) 0.6989(9) 0.0315(18) Uani 1 1 d . . . N2 N 0.7905(3) 0.5436(7) 0.6578(10) 0.040(2) Uiso 1 1 d . . . N3 N 0.7684(3) 0.4734(7) 0.8214(11) 0.048(2) Uani 1 1 d . . . N4 N 0.8582(3) 0.4482(6) 0.5640(12) 0.048(3) Uani 1 1 d . . . N5 N 0.8794(3) 0.3242(6) 0.6743(10) 0.065(4) Uani 1 1 d D . . N6 N 0.8893(2) 0.7001(5) 0.7001(9) 0.0247(16) Uani 1 1 d . . . N7 N 0.8774(3) 0.9002(7) 0.6772(11) 0.036(2) Uani 1 1 d . . . N8 N 0.8919(2) 0.9659(5) 0.8493(9) 0.0317(18) Uani 1 1 d . . . N9 N 0.9431(2) 0.8063(5) 0.5638(10) 0.0273(16) Uani 1 1 d . . . N10 N 0.9988(2) 0.8129(5) 0.6670(9) 0.0255(16) Uani 1 1 d . . . O2 O 0.8372(2) 0.9616(6) 0.4247(9) 0.0430(19) Uani 1 1 d . . . P1 P 0.85305(9) 0.2285(2) 0.1262(6) 0.0445(7) Uani 1 1 d . . . P2 P 0.98507(9) 1.11653(18) 0.6579(6) 0.0346(6) Uani 1 1 d . . . S2 S 0.87190(9) 0.9006(2) 0.4078(6) 0.0347(6) Uani 1 1 d . . . Ru2 Ru 0.882550(19) 0.79187(5) 0.5522(5) 0.02866(16) Uani 1 1 d . . . Ru1 Ru 0.83459(2) 0.58478(6) 0.5439(5) 0.0391(2) 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 C1 0.019(5) 0.014(4) 0.056(6) -0.004(4) 0.013(4) -0.005(3) C2 0.031(5) 0.021(4) 0.037(5) 0.001(4) 0.008(4) -0.004(4) C3 0.049(7) 0.024(5) 0.065(7) 0.016(5) 0.001(5) 0.003(4) C4 0.069(9) 0.067(8) 0.051(7) 0.040(6) -0.021(7) -0.034(7) C5 0.057(8) 0.045(6) 0.045(6) 0.027(5) -0.011(5) 0.002(5) C6 0.034(5) 0.028(5) 0.033(5) -0.001(4) 0.000(4) -0.003(4) C7 0.033(5) 0.016(4) 0.033(5) 0.003(4) 0.002(4) 0.009(3) C8 0.023(5) 0.012(4) 0.040(5) 0.000(3) 0.003(4) -0.001(3) C9 0.036(6) 0.014(4) 0.072(8) -0.002(5) 0.020(5) -0.007(4) C10 0.018(5) 0.034(5) 0.067(7) -0.030(5) 0.013(5) -0.011(4) C11 0.024(6) 0.084(9) 0.057(8) -0.018(7) 0.002(5) -0.014(5) C12 0.034(7) 0.083(9) 0.052(7) -0.021(7) 0.013(6) -0.017(6) C13 0.044(7) 0.073(9) 0.060(8) 0.004(7) 0.021(6) -0.017(6) C14 0.045(7) 0.020(5) 0.072(8) -0.005(5) 0.026(6) -0.006(4) C15 0.049(8) 0.058(8) 0.059(7) -0.030(6) 0.016(6) -0.016(6) C16 0.085(10) 0.037(6) 0.088(11) 0.003(8) 0.023(10) -0.008(6) S11 0.047(2) 0.128(4) 0.077(3) -0.068(3) -0.0023(18) -0.010(2) O11 0.095(9) 0.078(7) 0.131(11) -0.034(8) -0.014(8) -0.036(7) C18 0.068(10) 0.086(11) 0.073(10) -0.003(8) -0.036(8) 0.002(8) C20 0.023(5) 0.023(4) 0.025(4) 0.007(3) -0.004(3) 0.001(3) C21 0.023(5) 0.016(4) 0.038(5) 0.003(4) 0.000(4) -0.006(3) C22 0.031(6) 0.027(5) 0.046(6) -0.011(4) -0.004(4) -0.001(4) C23 0.036(6) 0.023(5) 0.052(6) 0.006(4) 0.005(5) 0.012(4) C24 0.054(7) 0.020(4) 0.038(5) -0.007(4) 0.005(5) -0.004(4) C25 0.026(5) 0.013(4) 0.031(5) -0.006(3) 0.003(4) -0.002(3) C26 0.024(5) 0.010(4) 0.057(6) 0.014(4) 0.005(4) 0.001(3) C27 0.028(4) 0.031(4) 0.037(4) 0.000(5) 0.012(6) 0.003(3) C28 0.027(5) 0.048(6) 0.040(6) 0.006(5) -0.014(4) -0.001(4) C29 0.029(6) 0.033(5) 0.056(7) 0.016(5) -0.006(5) 0.000(4) C30 0.065(9) 0.078(9) 0.029(6) 0.011(6) -0.011(5) -0.005(7) O300 0.075(8) 0.062(7) 0.060(7) 0.014(5) 0.014(6) 0.010(6) C301 0.084(14) 0.068(11) 0.079(13) 0.021(9) -0.004(10) 0.029(10) C302 0.122(17) 0.047(9) 0.062(10) 0.028(8) 0.030(11) 0.030(10) C303 0.081(13) 0.032(8) 0.14(2) -0.040(10) 0.009(12) 0.000(8) C304 0.071(11) 0.038(7) 0.062(9) -0.010(7) 0.031(8) 0.005(7) Cl1 0.0348(13) 0.0386(13) 0.0383(13) -0.0108(11) 0.0049(10) -0.0093(11) Cl2 0.0263(10) 0.0474(12) 0.0456(12) -0.0098(15) -0.0013(14) -0.0043(8) F1 0.074(6) 0.066(5) 0.065(5) -0.015(4) 0.021(4) 0.004(4) F3 0.059(4) 0.083(5) 0.075(6) -0.015(5) 0.005(4) -0.029(4) F4 0.096(6) 0.037(3) 0.145(8) 0.018(6) 0.049(8) 0.012(3) F6 0.036(4) 0.091(5) 0.124(7) -0.058(6) 0.009(6) 0.006(3) F7 0.058(5) 0.052(4) 0.084(5) 0.037(4) 0.011(4) 0.011(3) F8 0.052(4) 0.066(4) 0.050(4) 0.017(4) -0.006(3) -0.019(3) F9 0.082(6) 0.067(5) 0.064(5) -0.031(4) -0.029(4) 0.029(4) F10 0.047(4) 0.033(3) 0.054(4) -0.004(3) 0.006(3) -0.002(3) F11 0.053(4) 0.117(7) 0.081(6) -0.065(6) 0.011(5) 0.008(4) F12 0.091(6) 0.099(6) 0.062(5) 0.055(5) -0.038(5) -0.046(5) N1 0.043(5) 0.013(3) 0.039(5) 0.003(3) 0.009(4) 0.001(3) N3 0.043(6) 0.044(5) 0.055(6) -0.013(4) 0.015(5) -0.017(4) N4 0.052(5) 0.027(4) 0.066(7) -0.027(5) 0.017(6) -0.022(4) N5 0.077(8) 0.024(4) 0.094(9) -0.017(5) 0.061(7) -0.010(5) N6 0.021(4) 0.011(3) 0.042(5) -0.010(3) -0.002(3) -0.004(3) N7 0.023(5) 0.038(5) 0.046(5) 0.012(4) 0.007(4) 0.010(4) N8 0.039(5) 0.011(3) 0.046(5) -0.005(3) 0.001(4) 0.004(3) N9 0.029(4) 0.018(3) 0.035(5) 0.006(3) 0.000(4) -0.001(2) N10 0.020(4) 0.018(3) 0.039(4) -0.001(3) -0.004(3) -0.002(3) O2 0.035(4) 0.058(5) 0.036(4) 0.018(4) 0.004(3) 0.011(3) P1 0.0428(17) 0.0346(14) 0.0561(18) -0.0102(13) -0.0042(13) 0.0132(11) P2 0.0445(16) 0.0260(12) 0.0333(13) -0.0018(10) 0.0012(11) -0.0050(11) S2 0.0278(13) 0.0415(15) 0.0347(13) 0.0058(11) -0.0029(11) -0.0023(11) Ru2 0.0242(3) 0.0294(3) 0.0324(3) 0.0001(4) -0.0001(4) -0.0026(3) Ru1 0.0305(4) 0.0423(4) 0.0446(4) -0.0182(5) 0.0076(5) -0.0111(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 C1 N1 1.350(13) . ? C1 C2 1.392(15) . ? C1 C9 1.543(12) . ? C2 C3 1.412(14) . ? C2 C7 1.435(12) . ? C3 C4 1.328(17) . ? C3 H3 0.9500 . ? C4 C5 1.395(18) . ? C4 H4 0.9500 . ? C5 C6 1.354(13) . ? C5 H5 0.9500 . ? C6 C7 1.425(13) . ? C6 H6 0.9500 . ? C7 C8 1.430(13) . ? C8 N6 1.314(12) . ? C8 C20 1.535(11) . ? C9 C10 1.504(15) . ? C9 C14 1.523(16) . ? C9 H9 1.0000 . ? C10 N2 1.336(16) . ? C10 N3 1.345(13) . ? C11 C12 1.287(19) . ? C11 N2 1.376(15) . ? C11 H11 0.9500 . ? C12 N3 1.380(17) . ? C12 H12 0.9500 . ? C13 N3 1.457(16) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N4 1.308(17) . ? C14 N5 1.335(14) . ? C15 C16 1.32(2) . ? C15 N4 1.418(14) . ? C15 H15 0.9500 . ? C16 N5 1.31(2) . ? C16 H16 0.9500 . ? C17 N5 1.4701(10) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C172 N5 1.4700(11) . ? C172 H17D 0.9800 . ? C172 H17E 0.9800 . ? C172 H17F 0.9800 . ? S11 O11 1.563(12) . ? S11 C18 1.706(15) . ? S11 C19 1.7099(10) . ? S11 C192 1.7100(10) . ? S11 Ru1 2.221(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C192 H19D 0.9800 . ? C192 H19E 0.9800 . ? C192 H19F 0.9800 . ? C20 C21 1.475(12) . ? C20 C25 1.475(12) . ? C20 H20 1.0000 . ? C21 N8 1.335(12) . ? C21 N7 1.348(14) . ? C22 C23 1.347(15) . ? C22 N7 1.397(14) . ? C22 H22 0.9500 . ? C23 N8 1.365(12) . ? C23 H23 0.9500 . ? C24 N8 1.483(13) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 N10 1.340(12) . ? C25 N9 1.347(13) . ? C26 C27 1.370(14) . ? C26 N9 1.375(12) . ? C26 H26 0.9500 . ? C27 N10 1.380(15) . ? C27 H27 0.9500 . ? C28 N10 1.473(12) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 S2 1.787(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 S2 1.761(12) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? N100 C101 1.1305(9) . ? C101 C102 1.4504(9) . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? N200 C201 1.1302(10) . ? C201 C202 1.4502(9) . ? C202 H20A 0.9800 . ? C202 H20B 0.9800 . ? C202 H20C 0.9800 . ? O300 C304 1.375(18) . ? O300 C301 1.406(19) . ? C301 C302 1.49(3) . ? C301 H30D 0.9900 . ? C301 H30E 0.9900 . ? C302 C303 1.59(3) . ? C302 H30F 0.9900 . ? C302 H30G 0.9900 . ? C303 C304 1.43(2) . ? C303 H30H 0.9900 . ? C303 H30I 0.9900 . ? C304 H30J 0.9900 . ? C304 H30K 0.9900 . ? Cl1 Ru2 2.431(3) . ? Cl1 Ru1 2.439(3) . ? Cl2 Ru1 2.418(2) . ? Cl2 Ru2 2.422(2) . ? F1 P1 1.586(8) . ? F2 P1 1.545(17) . ? F3 P1 1.590(9) . ? F4 P1 1.542(10) . ? F51 P1 1.638(15) . ? F52 P1 1.60(2) . ? F6 P1 1.599(9) . ? F7 P2 1.585(7) . ? F8 P2 1.616(7) . ? F9 P2 1.571(7) . ? F10 P2 1.578(7) . ? F11 P2 1.576(8) . ? F12 P2 1.560(7) . ? N1 N6 1.359(10) . ? N1 Ru1 2.105(9) . ? N2 Ru1 2.028(10) . ? N4 Ru1 2.053(9) . ? N6 Ru2 2.093(8) . ? N7 Ru2 2.050(10) . ? N9 Ru2 2.039(7) . ? O2 S2 1.446(8) . ? S2 Ru2 2.229(7) . ? 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 N1 C1 C2 121.6(8) . . ? N1 C1 C9 114.7(9) . . ? C2 C1 C9 123.6(9) . . ? C1 C2 C3 125.6(9) . . ? C1 C2 C7 118.3(8) . . ? C3 C2 C7 116.1(9) . . ? C4 C3 C2 123.0(10) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 121.1(10) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 119.7(11) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 120.8(9) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C7 C8 124.8(8) . . ? C6 C7 C2 119.2(8) . . ? C8 C7 C2 116.0(8) . . ? N6 C8 C7 122.5(8) . . ? N6 C8 C20 114.8(8) . . ? C7 C8 C20 122.6(8) . . ? C10 C9 C14 109.6(10) . . ? C10 C9 C1 106.6(8) . . ? C14 C9 C1 108.1(8) . . ? C10 C9 H9 110.8 . . ? C14 C9 H9 110.8 . . ? C1 C9 H9 110.8 . . ? N2 C10 N3 110.0(10) . . ? N2 C10 C9 122.4(10) . . ? N3 C10 C9 127.6(12) . . ? C12 C11 N2 110.8(13) . . ? C12 C11 H11 124.6 . . ? N2 C11 H11 124.6 . . ? C11 C12 N3 107.8(11) . . ? C11 C12 H12 126.1 . . ? N3 C12 H12 126.1 . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N3 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 N5 114.3(10) . . ? N4 C14 C9 120.4(9) . . ? N5 C14 C9 125.2(12) . . ? C16 C15 N4 108.6(13) . . ? C16 C15 H15 125.7 . . ? N4 C15 H15 125.7 . . ? N5 C16 C15 109.7(12) . . ? N5 C16 H16 125.2 . . ? C15 C16 H16 125.2 . . ? N5 C17 H17A 109.5 . . ? N5 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N5 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C172 H17D 109.5 . . ? N5 C172 H17E 109.5 . . ? H17D C172 H17E 109.5 . . ? N5 C172 H17F 109.5 . . ? H17D C172 H17F 109.5 . . ? H17E C172 H17F 109.5 . . ? O11 S11 C18 103.9(8) . . ? O11 S11 C19 98.5(10) . . ? C18 S11 C19 110.3(11) . . ? O11 S11 C192 120(2) . . ? C18 S11 C192 87(2) . . ? O11 S11 Ru1 113.4(6) . . ? C18 S11 Ru1 115.3(6) . . ? C19 S11 Ru1 113.8(7) . . ? C192 S11 Ru1 113.4(16) . . ? S11 C18 H18A 109.5 . . ? S11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? S11 C19 H19A 109.5 . . ? S11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? S11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? S11 C192 H19D 109.5 . . ? S11 C192 H19E 109.5 . . ? H19D C192 H19E 109.5 . . ? S11 C192 H19F 109.5 . . ? H19D C192 H19F 109.5 . . ? H19E C192 H19F 109.5 . . ? C21 C20 C25 111.1(7) . . ? C21 C20 C8 106.1(7) . . ? C25 C20 C8 109.6(7) . . ? C21 C20 H20 110.0 . . ? C25 C20 H20 110.0 . . ? C8 C20 H20 110.0 . . ? N8 C21 N7 108.6(8) . . ? N8 C21 C20 129.9(9) . . ? N7 C21 C20 121.2(8) . . ? C23 C22 N7 107.3(10) . . ? C23 C22 H22 126.3 . . ? N7 C22 H22 126.3 . . ? C22 C23 N8 107.7(9) . . ? C22 C23 H23 126.2 . . ? N8 C23 H23 126.2 . . ? N8 C24 H24A 109.5 . . ? N8 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N8 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N10 C25 N9 109.5(8) . . ? N10 C25 C20 128.6(8) . . ? N9 C25 C20 121.3(8) . . ? C27 C26 N9 107.2(10) . . ? C27 C26 H26 126.4 . . ? N9 C26 H26 126.4 . . ? C26 C27 N10 107.7(8) . . ? C26 C27 H27 126.2 . . ? N10 C27 H27 126.2 . . ? N10 C28 H28A 109.5 . . ? N10 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N10 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? S2 C29 H29A 109.5 . . ? S2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? S2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? S2 C30 H30A 109.5 . . ? S2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? S2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N100 C101 C102 176.2(16) . . ? C101 C102 H10A 109.5 . . ? C101 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? C101 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? N200 C201 C202 177(3) . . ? C201 C202 H20A 109.5 . . ? C201 C202 H20B 109.5 . . ? H20A C202 H20B 109.5 . . ? C201 C202 H20C 109.5 . . ? H20A C202 H20C 109.5 . . ? H20B C202 H20C 109.5 . . ? C304 O300 C301 99.2(13) . . ? O300 C301 C302 108.3(16) . . ? O300 C301 H30D 110.0 . . ? C302 C301 H30D 110.0 . . ? O300 C301 H30E 110.0 . . ? C302 C301 H30E 110.0 . . ? H30D C301 H30E 108.4 . . ? C301 C302 C303 97.3(13) . . ? C301 C302 H30F 112.3 . . ? C303 C302 H30F 112.3 . . ? C301 C302 H30G 112.3 . . ? C303 C302 H30G 112.3 . . ? H30F C302 H30G 109.9 . . ? C304 C303 C302 103.8(15) . . ? C304 C303 H30H 111.0 . . ? C302 C303 H30H 111.0 . . ? C304 C303 H30I 111.0 . . ? C302 C303 H30I 111.0 . . ? H30H C303 H30I 109.0 . . ? O300 C304 C303 107.2(14) . . ? O300 C304 H30J 110.3 . . ? C303 C304 H30J 110.3 . . ? O300 C304 H30K 110.3 . . ? C303 C304 H30K 110.3 . . ? H30J C304 H30K 108.5 . . ? Ru2 Cl1 Ru1 84.45(19) . . ? Ru1 Cl2 Ru2 85.11(7) . . ? C1 N1 N6 120.7(8) . . ? C1 N1 Ru1 121.8(6) . . ? N6 N1 Ru1 117.5(6) . . ? C10 N2 C11 105.1(10) . . ? C10 N2 Ru1 117.8(7) . . ? C11 N2 Ru1 137.0(9) . . ? C10 N3 C12 106.4(10) . . ? C10 N3 C13 127.5(11) . . ? C12 N3 C13 126.0(10) . . ? C14 N4 C15 101.8(10) . . ? C14 N4 Ru1 119.6(7) . . ? C15 N4 Ru1 138.0(10) . . ? C16 N5 C14 105.6(11) . . ? C16 N5 C172 136(4) . . ? C14 N5 C172 111(4) . . ? C16 N5 C17 128.3(11) . . ? C14 N5 C17 125.9(11) . . ? C8 N6 N1 120.9(8) . . ? C8 N6 Ru2 122.3(6) . . ? N1 N6 Ru2 116.7(6) . . ? C21 N7 C22 107.3(9) . . ? C21 N7 Ru2 117.2(7) . . ? C22 N7 Ru2 134.8(8) . . ? C21 N8 C23 109.1(8) . . ? C21 N8 C24 124.3(8) . . ? C23 N8 C24 126.4(8) . . ? C25 N9 C26 108.0(8) . . ? C25 N9 Ru2 117.4(6) . . ? C26 N9 Ru2 134.3(7) . . ? C25 N10 C27 107.6(7) . . ? C25 N10 C28 126.3(8) . . ? C27 N10 C28 126.1(8) . . ? F4 P1 F2 177.0(8) . . ? F4 P1 F1 89.7(5) . . ? F2 P1 F1 92.4(7) . . ? F4 P1 F3 88.5(6) . . ? F2 P1 F3 89.2(7) . . ? F1 P1 F3 91.1(5) . . ? F4 P1 F6 90.1(6) . . ? F2 P1 F6 87.8(8) . . ? F1 P1 F6 179.6(6) . . ? F3 P1 F6 88.6(5) . . ? F4 P1 F52 112.0(9) . . ? F2 P1 F52 70.4(9) . . ? F1 P1 F52 84.8(8) . . ? F3 P1 F52 159.0(8) . . ? F6 P1 F52 95.5(8) . . ? F4 P1 F51 77.4(7) . . ? F2 P1 F51 104.5(8) . . ? F1 P1 F51 95.7(6) . . ? F3 P1 F51 164.3(6) . . ? F6 P1 F51 84.6(6) . . ? F12 P2 F9 89.8(5) . . ? F12 P2 F11 90.7(6) . . ? F9 P2 F11 179.0(5) . . ? F12 P2 F10 90.5(4) . . ? F9 P2 F10 91.0(4) . . ? F11 P2 F10 89.8(4) . . ? F12 P2 F7 179.1(4) . . ? F9 P2 F7 90.1(5) . . ? F11 P2 F7 89.4(5) . . ? F10 P2 F7 90.3(4) . . ? F12 P2 F8 89.9(4) . . ? F9 P2 F8 88.8(4) . . ? F11 P2 F8 90.4(4) . . ? F10 P2 F8 179.5(4) . . ? F7 P2 F8 89.3(4) . . ? O2 S2 C30 106.2(6) . . ? O2 S2 C29 105.6(5) . . ? C30 S2 C29 99.9(6) . . ? O2 S2 Ru2 115.1(3) . . ? C30 S2 Ru2 114.3(5) . . ? C29 S2 Ru2 114.2(4) . . ? N9 Ru2 N7 88.2(3) . . ? N9 Ru2 N6 84.3(3) . . ? N7 Ru2 N6 84.8(3) . . ? N9 Ru2 S2 98.0(2) . . ? N7 Ru2 S2 89.5(2) . . ? N6 Ru2 S2 173.8(2) . . ? N9 Ru2 Cl2 172.1(2) . . ? N7 Ru2 Cl2 95.8(3) . . ? N6 Ru2 Cl2 89.2(2) . . ? S2 Ru2 Cl2 88.92(11) . . ? N9 Ru2 Cl1 90.7(2) . . ? N7 Ru2 Cl1 172.3(3) . . ? N6 Ru2 Cl1 87.5(2) . . ? S2 Ru2 Cl1 98.20(30) . . ? Cl2 Ru2 Cl1 84.44(9) . . ? N2 Ru1 N4 87.5(4) . . ? N2 Ru1 N1 85.8(4) . . ? N4 Ru1 N1 83.9(4) . . ? N2 Ru1 S11 90.3(3) . . ? N4 Ru1 S11 92.6(3) . . ? N1 Ru1 S11 174.9(3) . . ? N2 Ru1 Cl2 91.7(3) . . ? N4 Ru1 Cl2 171.4(3) . . ? N1 Ru1 Cl2 87.6(2) . . ? S11 Ru1 Cl2 95.87(16) . . ? N2 Ru1 Cl1 172.7(3) . . ? N4 Ru1 Cl1 95.5(3) . . ? N1 Ru1 Cl1 87.9(2) . . ? S11 Ru1 Cl1 96.17(30) . . ? Cl2 Ru1 Cl1 84.35(9) . . ? 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 N1 C1 C2 C3 178.7(9) . . . . ? C9 C1 C2 C3 -4.7(15) . . . . ? N1 C1 C2 C7 0.6(14) . . . . ? C9 C1 C2 C7 177.3(8) . . . . ? C1 C2 C3 C4 -174.6(13) . . . . ? C7 C2 C3 C4 3.5(17) . . . . ? C2 C3 C4 C5 -4(2) . . . . ? C3 C4 C5 C6 2(2) . . . . ? C4 C5 C6 C7 0.9(18) . . . . ? C5 C6 C7 C8 178.0(10) . . . . ? C5 C6 C7 C2 -1.2(15) . . . . ? C1 C2 C7 C6 177.4(9) . . . . ? C3 C2 C7 C6 -0.9(13) . . . . ? C1 C2 C7 C8 -1.9(13) . . . . ? C3 C2 C7 C8 179.9(9) . . . . ? C6 C7 C8 N6 -175.9(9) . . . . ? C2 C7 C8 N6 3.4(13) . . . . ? C6 C7 C8 C20 1.0(14) . . . . ? C2 C7 C8 C20 -179.8(8) . . . . ? N1 C1 C9 C10 -61.6(11) . . . . ? C2 C1 C9 C10 121.5(11) . . . . ? N1 C1 C9 C14 56.2(12) . . . . ? C2 C1 C9 C14 -120.7(11) . . . . ? C14 C9 C10 N2 -54.0(12) . . . . ? C1 C9 C10 N2 62.8(12) . . . . ? C14 C9 C10 N3 126.6(11) . . . . ? C1 C9 C10 N3 -116.7(11) . . . . ? N2 C11 C12 N3 0.5(15) . . . . ? C10 C9 C14 N4 52.4(13) . . . . ? C1 C9 C14 N4 -63.5(14) . . . . ? C10 C9 C14 N5 -130.7(12) . . . . ? C1 C9 C14 N5 113.4(12) . . . . ? N4 C15 C16 N5 -0.9(16) . . . . ? N6 C8 C20 C21 64.5(10) . . . . ? C7 C8 C20 C21 -112.6(9) . . . . ? N6 C8 C20 C25 -55.5(10) . . . . ? C7 C8 C20 C25 127.4(9) . . . . ? C25 C20 C21 N8 -131.9(10) . . . . ? C8 C20 C21 N8 109.0(10) . . . . ? C25 C20 C21 N7 54.9(11) . . . . ? C8 C20 C21 N7 -64.1(11) . . . . ? N7 C22 C23 N8 -1.7(12) . . . . ? C21 C20 C25 N10 133.7(9) . . . . ? C8 C20 C25 N10 -109.4(9) . . . . ? C21 C20 C25 N9 -55.9(10) . . . . ? C8 C20 C25 N9 61.1(10) . . . . ? N9 C26 C27 N10 -0.1(9) . . . . ? C304 O300 C301 C302 -47.7(18) . . . . ? O300 C301 C302 C303 28.1(19) . . . . ? C301 C302 C303 C304 1.0(17) . . . . ? C301 O300 C304 C303 47.8(18) . . . . ? C302 C303 C304 O300 -30.4(18) . . . . ? C2 C1 N1 N6 -0.5(13) . . . . ? C9 C1 N1 N6 -177.5(8) . . . . ? C2 C1 N1 Ru1 -178.2(7) . . . . ? C9 C1 N1 Ru1 4.8(11) . . . . ? N3 C10 N2 C11 0.2(11) . . . . ? C9 C10 N2 C11 -179.3(9) . . . . ? N3 C10 N2 Ru1 178.3(7) . . . . ? C9 C10 N2 Ru1 -1.3(12) . . . . ? C12 C11 N2 C10 -0.4(14) . . . . ? C12 C11 N2 Ru1 -177.9(9) . . . . ? N2 C10 N3 C12 0.1(12) . . . . ? C9 C10 N3 C12 179.5(10) . . . . ? N2 C10 N3 C13 177.5(11) . . . . ? C9 C10 N3 C13 -3.0(17) . . . . ? C11 C12 N3 C10 -0.3(13) . . . . ? C11 C12 N3 C13 -177.8(12) . . . . ? N5 C14 N4 C15 -1.0(13) . . . . ? C9 C14 N4 C15 176.3(10) . . . . ? N5 C14 N4 Ru1 -174.3(8) . . . . ? C9 C14 N4 Ru1 3.0(14) . . . . ? C16 C15 N4 C14 1.1(13) . . . . ? C16 C15 N4 Ru1 172.4(9) . . . . ? C15 C16 N5 C14 0.3(16) . . . . ? C15 C16 N5 C172 146(5) . . . . ? C15 C16 N5 C17 -174.0(13) . . . . ? N4 C14 N5 C16 0.5(15) . . . . ? C9 C14 N5 C16 -176.6(11) . . . . ? N4 C14 N5 C172 -154(4) . . . . ? C9 C14 N5 C172 29(4) . . . . ? N4 C14 N5 C17 175.0(12) . . . . ? C9 C14 N5 C17 -2.1(19) . . . . ? C7 C8 N6 N1 -3.4(13) . . . . ? C20 C8 N6 N1 179.5(7) . . . . ? C7 C8 N6 Ru2 171.6(6) . . . . ? C20 C8 N6 Ru2 -5.5(10) . . . . ? C1 N1 N6 C8 1.9(12) . . . . ? Ru1 N1 N6 C8 179.7(6) . . . . ? C1 N1 N6 Ru2 -173.3(6) . . . . ? Ru1 N1 N6 Ru2 4.5(8) . . . . ? N8 C21 N7 C22 -1.0(11) . . . . ? C20 C21 N7 C22 173.5(8) . . . . ? N8 C21 N7 Ru2 -172.7(6) . . . . ? C20 C21 N7 Ru2 1.7(12) . . . . ? C23 C22 N7 C21 1.6(12) . . . . ? C23 C22 N7 Ru2 171.3(8) . . . . ? N7 C21 N8 C23 -0.1(11) . . . . ? C20 C21 N8 C23 -173.9(9) . . . . ? N7 C21 N8 C24 -176.2(8) . . . . ? C20 C21 N8 C24 10.0(15) . . . . ? C22 C23 N8 C21 1.1(12) . . . . ? C22 C23 N8 C24 177.2(9) . . . . ? N10 C25 N9 C26 -2.9(9) . . . . ? C20 C25 N9 C26 -175.0(7) . . . . ? N10 C25 N9 Ru2 171.6(5) . . . . ? C20 C25 N9 Ru2 -0.5(10) . . . . ? C27 C26 N9 C25 1.8(9) . . . . ? C27 C26 N9 Ru2 -171.4(6) . . . . ? N9 C25 N10 C27 2.9(9) . . . . ? C20 C25 N10 C27 174.2(8) . . . . ? N9 C25 N10 C28 -178.8(8) . . . . ? C20 C25 N10 C28 -7.4(14) . . . . ? C26 C27 N10 C25 -1.7(9) . . . . ? C26 C27 N10 C28 179.9(8) . . . . ? C25 N9 Ru2 N7 41.9(6) . . . . ? C26 N9 Ru2 N7 -145.4(8) . . . . ? C25 N9 Ru2 N6 -43.1(6) . . . . ? C26 N9 Ru2 N6 129.6(7) . . . . ? C25 N9 Ru2 S2 131.1(5) . . . . ? C26 N9 Ru2 S2 -56.2(7) . . . . ? C25 N9 Ru2 Cl1 -130.5(5) . . . . ? C26 N9 Ru2 Cl1 42.2(7) . . . . ? C21 N7 Ru2 N9 -42.6(7) . . . . ? C22 N7 Ru2 N9 148.6(11) . . . . ? C21 N7 Ru2 N6 41.9(7) . . . . ? C22 N7 Ru2 N6 -126.9(11) . . . . ? C21 N7 Ru2 S2 -140.6(7) . . . . ? C22 N7 Ru2 S2 50.6(10) . . . . ? C21 N7 Ru2 Cl2 130.5(7) . . . . ? C22 N7 Ru2 Cl2 -38.3(10) . . . . ? C8 N6 Ru2 N9 47.9(7) . . . . ? N1 N6 Ru2 N9 -137.0(6) . . . . ? C8 N6 Ru2 N7 -40.8(7) . . . . ? N1 N6 Ru2 N7 134.3(7) . . . . ? C8 N6 Ru2 Cl2 -136.7(7) . . . . ? N1 N6 Ru2 Cl2 38.5(6) . . . . ? C8 N6 Ru2 Cl1 138.8(7) . . . . ? N1 N6 Ru2 Cl1 -46.0(6) . . . . ? O2 S2 Ru2 N9 -138.7(5) . . . . ? C30 S2 Ru2 N9 98.0(6) . . . . ? C29 S2 Ru2 N9 -16.2(5) . . . . ? O2 S2 Ru2 N7 -50.6(5) . . . . ? C30 S2 Ru2 N7 -173.9(6) . . . . ? C29 S2 Ru2 N7 71.9(5) . . . . ? O2 S2 Ru2 Cl2 45.2(4) . . . . ? C30 S2 Ru2 Cl2 -78.1(5) . . . . ? C29 S2 Ru2 Cl2 167.7(5) . . . . ? O2 S2 Ru2 Cl1 129.4(4) . . . . ? C30 S2 Ru2 Cl1 6.1(5) . . . . ? C29 S2 Ru2 Cl1 -108.1(4) . . . . ? Ru1 Cl2 Ru2 N7 -137.9(3) . . . . ? Ru1 Cl2 Ru2 N6 -53.2(2) . . . . ? Ru1 Cl2 Ru2 S2 132.66(12) . . . . ? Ru1 Cl2 Ru2 Cl1 34.32(10) . . . . ? Ru1 Cl1 Ru2 N9 139.7(2) . . . . ? Ru1 Cl1 Ru2 N6 55.4(2) . . . . ? Ru1 Cl1 Ru2 S2 -122.12(10) . . . . ? Ru1 Cl1 Ru2 Cl2 -34.01(10) . . . . ? C10 N2 Ru1 N4 42.3(8) . . . . ? C11 N2 Ru1 N4 -140.5(12) . . . . ? C10 N2 Ru1 N1 -41.8(7) . . . . ? C11 N2 Ru1 N1 135.5(12) . . . . ? C10 N2 Ru1 S11 134.9(7) . . . . ? C11 N2 Ru1 S11 -47.9(12) . . . . ? C10 N2 Ru1 Cl2 -129.2(7) . . . . ? C11 N2 Ru1 Cl2 48.0(12) . . . . ? C14 N4 Ru1 N2 -43.8(8) . . . . ? C15 N4 Ru1 N2 146.0(11) . . . . ? C14 N4 Ru1 N1 42.2(8) . . . . ? C15 N4 Ru1 N1 -127.9(11) . . . . ? C14 N4 Ru1 S11 -134.0(8) . . . . ? C15 N4 Ru1 S11 55.8(11) . . . . ? C14 N4 Ru1 Cl1 129.5(8) . . . . ? C15 N4 Ru1 Cl1 -40.6(11) . . . . ? C1 N1 Ru1 N2 40.8(7) . . . . ? N6 N1 Ru1 N2 -137.0(7) . . . . ? C1 N1 Ru1 N4 -47.1(7) . . . . ? N6 N1 Ru1 N4 135.1(7) . . . . ? C1 N1 Ru1 Cl2 132.7(7) . . . . ? N6 N1 Ru1 Cl2 -45.1(6) . . . . ? C1 N1 Ru1 Cl1 -142.9(7) . . . . ? N6 N1 Ru1 Cl1 39.3(6) . . . . ? O11 S11 Ru1 N2 -41.1(6) . . . . ? C18 S11 Ru1 N2 78.4(8) . . . . ? C19 S11 Ru1 N2 -152.6(11) . . . . ? C192 S11 Ru1 N2 177(2) . . . . ? O11 S11 Ru1 N4 46.3(7) . . . . ? C18 S11 Ru1 N4 165.9(8) . . . . ? C19 S11 Ru1 N4 -65.1(11) . . . . ? C192 S11 Ru1 N4 -95(2) . . . . ? O11 S11 Ru1 Cl2 -132.9(6) . . . . ? C18 S11 Ru1 Cl2 -13.3(8) . . . . ? C19 S11 Ru1 Cl2 115.6(11) . . . . ? C192 S11 Ru1 Cl2 85(2) . . . . ? O11 S11 Ru1 Cl1 142.2(6) . . . . ? C18 S11 Ru1 Cl1 -98.2(7) . . . . ? C19 S11 Ru1 Cl1 30.7(11) . . . . ? C192 S11 Ru1 Cl1 0(2) . . . . ? Ru2 Cl2 Ru1 N2 139.7(3) . . . . ? Ru2 Cl2 Ru1 N1 54.0(2) . . . . ? Ru2 Cl2 Ru1 S11 -129.84(14) . . . . ? Ru2 Cl2 Ru1 Cl1 -34.19(10) . . . . ? Ru2 Cl1 Ru1 N4 -137.3(3) . . . . ? Ru2 Cl1 Ru1 N1 -53.7(2) . . . . ? Ru2 Cl1 Ru1 S11 129.40(15) . . . . ? Ru2 Cl1 Ru1 Cl2 34.08(10) . . . . ? data_1 _database_code_depnum_ccdc_archive 'CCDC 765497' #TrackingRef '- complex 1_rev.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H26 Cl4 Mn2 N10, 2(C H4 O)' _chemical_formula_sum 'C28 H34 Cl4 Mn2 N10 O2' _chemical_formula_weight 794.33 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _Symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1972(6) _cell_length_b 16.7605(7) _cell_length_c 15.8055(8) _cell_angle_alpha 90.00 _cell_angle_beta 104.000(4) _cell_angle_gamma 90.00 _cell_volume 3392.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18308 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 29.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.103 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6922 _exptl_absorpt_correction_T_max 0.8095 _exptl_absorpt_process_details ; The crystal faces were indexed by microscope on the diffractometer. After that a numerical absorption correction basing on a Gaussian algorithsm was applied, which is implemented in the X-RED program (Stoe, 2002). ; _exptl_special_details ; During data collection the crystal was in cold N~2~ gas of the Cryostream Cooler (Oxford Cryosystems) mounted on a 2-circle goniometer supplied with an area detector. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device_type 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,217 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6116 _diffrn_reflns_av_R_equivalents 0.1548 _diffrn_reflns_av_sigmaI/netI 0.1606 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.25 _reflns_number_total 6116 _reflns_number_gt 3497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL97 (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. In total 15 geometrical restrains (DFIX, SIMU) were used to stabilise and fix the geometry of one N-methyl-imidazol of the ligand bimptz ans one disordered solvent molecules (MeoH). ; _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^)+(0.0270P)^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 6116 _refine_ls_number_parameters 396 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1409 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3729(5) 0.3861(4) 0.2172(4) 0.0149(14) Uani 1 1 d . . . C2 C 0.3818(5) 0.4676(4) 0.2480(4) 0.0133(14) Uani 1 1 d . . . C3 C 0.3031(5) 0.5102(4) 0.2740(4) 0.0216(16) Uani 1 1 d . . . H3 H 0.2368 0.4861 0.2692 0.026 Uiso 1 1 calc R . . C4 C 0.3204(5) 0.5851(4) 0.3058(5) 0.0274(18) Uani 1 1 d . . . H4 H 0.2665 0.6127 0.3241 0.033 Uiso 1 1 calc R . . C5 C 0.4176(5) 0.6227(4) 0.3122(4) 0.0253(17) Uani 1 1 d . . . H5 H 0.4283 0.6760 0.3331 0.030 Uiso 1 1 calc R . . C6 C 0.4966(5) 0.5825(4) 0.2881(4) 0.0187(16) Uani 1 1 d . . . H6 H 0.5623 0.6076 0.2930 0.022 Uiso 1 1 calc R . . C7 C 0.4806(5) 0.5035(4) 0.2560(4) 0.0160(14) Uani 1 1 d . . . C8 C 0.5588(5) 0.4569(4) 0.2321(3) 0.0132(14) Uani 1 1 d . . . C9 C 0.2723(5) 0.3378(4) 0.2079(4) 0.0172(15) Uani 1 1 d . . . H9 H 0.2160 0.3734 0.2187 0.021 Uiso 1 1 calc R . . C10 C 0.2381(5) 0.3026(4) 0.1170(4) 0.0139(13) Uani 1 1 d . . . C11 C 0.2372(5) 0.2310(4) 0.0036(4) 0.0225(16) Uani 1 1 d . . . H11 H 0.2573 0.1930 -0.0339 0.027 Uiso 1 1 calc R . . C12 C 0.1521(6) 0.2770(5) -0.0166(4) 0.035(2) Uani 1 1 d . . . H12 H 0.1014 0.2777 -0.0707 0.042 Uiso 1 1 calc R . . C13 C 0.0682(6) 0.3773(6) 0.0634(5) 0.056(3) Uani 1 1 d . . . H13A H 0.0228 0.3510 0.0956 0.083 Uiso 1 1 calc R . . H13B H 0.0272 0.3919 0.0051 0.083 Uiso 1 1 calc R . . H13C H 0.0984 0.4255 0.0947 0.083 Uiso 1 1 calc R . . C14 C 0.2948(5) 0.2740(4) 0.2758(4) 0.0171(15) Uani 1 1 d . . . C15 C 0.3654(6) 0.1729(5) 0.3520(4) 0.031(2) Uani 1 1 d . . . H15 H 0.4071 0.1270 0.3707 0.037 Uiso 1 1 calc R . . C16 C 0.3016(7) 0.2069(5) 0.3952(4) 0.041(2) Uani 1 1 d . . . H16 H 0.2897 0.1895 0.4492 0.050 Uiso 1 1 calc R . . C17 C 0.1800(8) 0.3264(5) 0.3709(5) 0.053(3) Uani 1 1 d . . . H17A H 0.2103 0.3800 0.3812 0.080 Uiso 1 1 calc R . . H17B H 0.1623 0.3071 0.4241 0.080 Uiso 1 1 calc R . . H17C H 0.1168 0.3285 0.3233 0.080 Uiso 1 1 calc R . . C18 C 0.6665(5) 0.4888(4) 0.2296(4) 0.0112(13) Uani 1 1 d . . . H18 H 0.6724 0.5454 0.2502 0.013 Uiso 1 1 calc R . . C19 C 0.7531(5) 0.4411(4) 0.2862(4) 0.0124(13) Uani 1 1 d . . . C20 C 0.8612(5) 0.3471(4) 0.3331(3) 0.0106(13) Uiso 1 1 d U . . H20 H 0.8965 0.2973 0.3372 0.013 Uiso 1 1 calc R . . C21 C 0.8876(5) 0.4073(4) 0.3901(4) 0.0176(15) Uani 1 1 d U . . H21 H 0.9431 0.4076 0.4412 0.021 Uiso 1 1 calc R . . C22 C 0.8187(5) 0.5452(4) 0.4022(4) 0.0185(15) Uani 1 1 d . . . H22A H 0.8571 0.5839 0.3753 0.028 Uiso 1 1 calc R . . H22B H 0.8526 0.5401 0.4643 0.028 Uiso 1 1 calc R . . H22C H 0.7467 0.5636 0.3953 0.028 Uiso 1 1 calc R . . C23 C 0.6687(5) 0.4871(4) 0.1347(4) 0.0134(14) Uani 1 1 d . . . C24 C 0.6626(5) 0.4485(4) 0.0051(4) 0.0231(17) Uani 1 1 d . . . H24 H 0.6644 0.4149 -0.0430 0.028 Uiso 1 1 calc R . . C25 C 0.6450(6) 0.5281(4) -0.0007(4) 0.0269(18) Uani 1 1 d . . . H25 H 0.6328 0.5601 -0.0518 0.032 Uiso 1 1 calc R . . C26 C 0.6289(5) 0.6340(4) 0.1092(4) 0.0247(17) Uani 1 1 d . . . H26A H 0.5614 0.6357 0.1248 0.037 Uiso 1 1 calc R . . H26B H 0.6275 0.6708 0.0607 0.037 Uiso 1 1 calc R . . H26C H 0.6844 0.6499 0.1596 0.037 Uiso 1 1 calc R . . C27 C -0.0732(5) 0.4903(5) 0.1641(5) 0.040(2) Uani 1 1 d D . . H27A H -0.0900 0.4374 0.1834 0.059 Uiso 1 1 d R A . H27B H -0.0951 0.4934 0.1004 0.059 Uiso 1 1 d R . . H27C H -0.1099 0.5312 0.1896 0.059 Uiso 1 1 d R . . Cl1 Cl 0.41296(13) 0.06591(10) 0.12286(11) 0.0235(4) Uani 1 1 d . . . Cl2 Cl 0.53569(12) 0.24559(10) 0.04200(9) 0.0150(3) Uani 1 1 d . . . Cl3 Cl 0.62494(11) 0.19957(10) 0.25857(9) 0.0171(3) Uani 1 1 d . . . Cl4 Cl 0.83173(13) 0.23858(10) 0.12178(10) 0.0219(4) Uani 1 1 d . . . Mn1 Mn 0.44483(7) 0.20581(6) 0.16424(6) 0.0138(2) Uani 1 1 d . . . Mn2 Mn 0.68150(7) 0.30282(6) 0.15656(5) 0.0114(2) Uani 1 1 d . . . N1 N 0.4492(4) 0.3475(3) 0.1984(3) 0.0106(11) Uani 1 1 d . . . N2 N 0.5442(4) 0.3823(3) 0.2051(3) 0.0117(11) Uani 1 1 d . . . N3 N 0.2914(4) 0.2481(3) 0.0884(3) 0.0140(11) Uani 1 1 d . . . N4 N 0.1511(4) 0.3235(4) 0.0557(3) 0.0284(16) Uani 1 1 d . . . N5 N 0.3617(4) 0.2148(3) 0.2752(3) 0.0210(13) Uani 1 1 d . . . N6 N 0.2560(5) 0.2722(4) 0.3473(3) 0.0312(16) Uani 1 1 d . . . N7 N 0.7752(4) 0.3680(3) 0.2675(3) 0.0105(11) Uani 1 1 d U . . N8 N 0.8185(4) 0.4687(3) 0.3601(3) 0.0127(12) Uani 1 1 d . . . N9 N 0.6774(4) 0.4229(3) 0.0896(3) 0.0135(11) Uani 1 1 d . . . N10 N 0.6485(4) 0.5530(3) 0.0829(3) 0.0171(13) Uani 1 1 d . . . O1 O 0.0415(7) 0.4856(9) 0.2051(8) 0.021(4) Uiso 0.47(3) 1 d PDU A 1 H1 H 0.0513 0.5198 0.2431 0.025 Uiso 1 1 d R . . O1S O 0.0279(8) 0.5195(8) 0.1764(8) 0.027(4) Uiso 0.53(3) 1 d PDU A 2 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 C1 0.014(4) 0.023(4) 0.007(3) 0.001(3) 0.001(3) 0.000(3) C2 0.010(3) 0.016(4) 0.011(3) -0.002(2) -0.003(2) 0.000(3) C3 0.012(4) 0.020(4) 0.031(4) -0.002(3) 0.002(3) 0.000(3) C4 0.018(4) 0.030(5) 0.038(4) -0.001(3) 0.014(3) 0.015(3) C5 0.025(4) 0.020(4) 0.033(4) -0.010(3) 0.010(3) 0.007(3) C6 0.017(4) 0.021(4) 0.016(3) 0.004(3) 0.000(3) -0.002(3) C7 0.011(3) 0.018(4) 0.017(3) 0.000(3) 0.000(3) 0.002(3) C8 0.015(4) 0.015(4) 0.008(3) 0.001(2) 0.000(2) -0.005(3) C9 0.012(4) 0.023(4) 0.016(3) -0.005(3) 0.004(3) -0.002(3) C10 0.013(3) 0.015(3) 0.014(3) 0.000(3) 0.003(2) 0.002(3) C11 0.024(4) 0.028(4) 0.014(3) -0.007(3) 0.001(3) -0.005(3) C12 0.028(4) 0.060(6) 0.012(3) -0.006(3) -0.006(3) 0.018(4) C13 0.034(5) 0.085(8) 0.037(5) -0.024(5) -0.013(4) 0.038(5) C14 0.012(3) 0.032(4) 0.007(3) -0.004(3) 0.003(2) -0.010(3) C15 0.026(4) 0.043(5) 0.020(4) 0.016(3) -0.004(3) -0.019(4) C16 0.060(6) 0.056(5) 0.013(4) -0.001(4) 0.018(4) -0.023(5) C17 0.081(7) 0.056(6) 0.042(5) -0.006(4) 0.053(5) -0.007(5) C18 0.013(3) 0.010(3) 0.010(3) -0.006(2) 0.002(3) 0.002(3) C19 0.008(3) 0.012(4) 0.017(3) 0.003(3) 0.002(3) 0.002(3) C21 0.012(3) 0.016(4) 0.025(4) 0.008(3) 0.003(3) 0.001(3) C22 0.017(4) 0.012(3) 0.020(3) -0.008(3) -0.007(3) 0.004(3) C23 0.008(3) 0.018(4) 0.013(3) 0.007(3) 0.000(3) -0.003(3) C24 0.018(4) 0.036(5) 0.015(3) 0.005(3) 0.005(3) -0.006(3) C25 0.031(5) 0.025(5) 0.023(4) 0.013(3) 0.004(3) -0.001(3) C26 0.022(4) 0.015(4) 0.030(4) 0.011(3) -0.008(3) 0.005(3) C27 0.031(5) 0.045(5) 0.049(5) -0.021(4) 0.021(4) -0.015(4) Cl1 0.0192(9) 0.0172(9) 0.0334(10) 0.0000(7) 0.0049(7) -0.0032(8) Cl2 0.0157(8) 0.0181(9) 0.0100(7) 0.0012(6) 0.0009(6) 0.0005(7) Cl3 0.0152(8) 0.0218(9) 0.0126(7) 0.0036(7) 0.0000(6) -0.0037(8) Cl4 0.0211(9) 0.0245(10) 0.0212(8) -0.0009(7) 0.0076(7) 0.0074(8) Mn1 0.0118(5) 0.0160(6) 0.0121(5) 0.0022(4) 0.0004(4) -0.0023(5) Mn2 0.0124(5) 0.0116(5) 0.0103(4) 0.0003(4) 0.0027(4) -0.0001(5) N1 0.011(3) 0.017(3) 0.005(2) 0.001(2) 0.003(2) -0.006(2) N2 0.007(3) 0.017(3) 0.011(2) 0.002(2) 0.003(2) -0.001(2) N3 0.016(3) 0.017(3) 0.009(2) -0.001(2) 0.002(2) -0.005(2) N4 0.019(3) 0.040(4) 0.023(3) -0.006(3) -0.001(3) 0.010(3) N5 0.020(3) 0.031(4) 0.008(2) 0.005(2) -0.004(2) -0.010(3) N6 0.040(4) 0.037(4) 0.021(3) -0.002(3) 0.017(3) -0.018(3) N7 0.011(3) 0.011(3) 0.009(2) 0.003(2) 0.001(2) 0.000(2) N8 0.011(3) 0.012(3) 0.011(3) -0.002(2) -0.004(2) -0.004(2) N9 0.014(3) 0.016(3) 0.014(2) 0.000(2) 0.011(2) -0.003(3) N10 0.012(3) 0.013(3) 0.021(3) 0.009(2) -0.005(2) -0.001(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 C1 N1 1.291(8) . ? C1 C2 1.445(8) . ? C1 C9 1.531(9) . ? C2 C3 1.401(9) . ? C2 C7 1.414(9) . ? C3 C4 1.351(9) . ? C3 H3 0.9500 . ? C4 C5 1.412(10) . ? C4 H4 0.9500 . ? C5 C6 1.371(9) . ? C5 H5 0.9500 . ? C6 C7 1.415(9) . ? C6 H6 0.9500 . ? C7 C8 1.416(9) . ? C8 N2 1.321(7) . ? C8 C18 1.527(8) . ? C9 C14 1.493(9) . ? C9 C10 1.517(8) . ? C9 H9 1.0000 . ? C10 N3 1.299(8) . ? C10 N4 1.358(7) . ? C11 C12 1.335(9) . ? C11 N3 1.389(7) . ? C11 H11 0.9500 . ? C12 N4 1.385(8) . ? C12 H12 0.9500 . ? C13 N4 1.446(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N5 1.331(8) . ? C14 N6 1.348(7) . ? C15 C16 1.334(11) . ? C15 N5 1.393(8) . ? C15 H15 0.9500 . ? C16 N6 1.383(10) . ? C16 H16 0.9500 . ? C17 N6 1.467(10) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.501(8) . ? C18 C23 1.508(8) . ? C18 H18 1.0000 . ? C19 N7 1.311(8) . ? C19 N8 1.354(7) . ? C20 C21 1.340(8) . ? C20 N7 1.384(7) . ? C20 H20 0.9500 . ? C21 N8 1.381(8) . ? C21 H21 0.9500 . ? C22 N8 1.445(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N9 1.310(8) . ? C23 N10 1.363(7) . ? C24 C25 1.353(9) . ? C24 N9 1.373(7) . ? C24 H24 0.9500 . ? C25 N10 1.376(8) . ? C25 H25 0.9500 . ? C26 N10 1.461(8) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 O1S 1.390(10) . ? C27 O1 1.498(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Cl1 Mn1 2.4432(19) . ? Cl2 Mn2 2.4932(17) . ? Cl2 Mn1 2.5954(17) . ? Cl3 Mn1 2.4837(16) . ? Cl3 Mn2 2.5949(17) . ? Cl4 Mn2 2.4330(18) . ? Mn1 N3 2.205(5) . ? Mn1 N5 2.287(5) . ? Mn1 N1 2.432(5) . ? Mn2 N7 2.179(5) . ? Mn2 N9 2.268(5) . ? Mn2 N2 2.514(5) . ? N1 N2 1.364(7) . ? O1 H1 0.8168 . ? O1S H1 1.0241 . ? 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 N1 C1 C2 123.2(6) . . ? N1 C1 C9 114.8(6) . . ? C2 C1 C9 122.0(6) . . ? C3 C2 C7 119.3(6) . . ? C3 C2 C1 125.1(6) . . ? C7 C2 C1 115.5(6) . . ? C4 C3 C2 120.8(7) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.7(7) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C6 C5 C4 120.0(6) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 120.2(6) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C2 C7 C6 119.0(6) . . ? C2 C7 C8 117.2(6) . . ? C6 C7 C8 123.8(6) . . ? N2 C8 C7 123.3(6) . . ? N2 C8 C18 112.8(5) . . ? C7 C8 C18 123.8(5) . . ? C14 C9 C10 111.4(6) . . ? C14 C9 C1 107.0(5) . . ? C10 C9 C1 110.4(5) . . ? C14 C9 H9 109.3 . . ? C10 C9 H9 109.3 . . ? C1 C9 H9 109.3 . . ? N3 C10 N4 111.6(5) . . ? N3 C10 C9 122.8(5) . . ? N4 C10 C9 125.6(6) . . ? C12 C11 N3 108.6(6) . . ? C12 C11 H11 125.7 . . ? N3 C11 H11 125.7 . . ? C11 C12 N4 107.7(6) . . ? C11 C12 H12 126.2 . . ? N4 C12 H12 126.2 . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 N6 112.1(6) . . ? N5 C14 C9 123.0(5) . . ? N6 C14 C9 124.7(6) . . ? C16 C15 N5 109.7(7) . . ? C16 C15 H15 125.2 . . ? N5 C15 H15 125.2 . . ? C15 C16 N6 107.6(6) . . ? C15 C16 H16 126.2 . . ? N6 C16 H16 126.2 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 112.8(5) . . ? C19 C18 C8 112.2(5) . . ? C23 C18 C8 105.1(4) . . ? C19 C18 H18 108.9 . . ? C23 C18 H18 108.9 . . ? C8 C18 H18 108.9 . . ? N7 C19 N8 112.5(5) . . ? N7 C19 C18 122.9(5) . . ? N8 C19 C18 124.6(5) . . ? C21 C20 N7 110.3(6) . . ? C21 C20 H20 124.9 . . ? N7 C20 H20 124.9 . . ? C20 C21 N8 106.7(6) . . ? C20 C21 H21 126.7 . . ? N8 C21 H21 126.7 . . ? N8 C22 H22A 109.5 . . ? N8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N9 C23 N10 111.7(5) . . ? N9 C23 C18 125.6(5) . . ? N10 C23 C18 122.3(6) . . ? C25 C24 N9 110.8(6) . . ? C25 C24 H24 124.6 . . ? N9 C24 H24 124.6 . . ? C24 C25 N10 105.6(6) . . ? C24 C25 H25 127.2 . . ? N10 C25 H25 127.2 . . ? N10 C26 H26A 109.5 . . ? N10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1S C27 H27A 123.8 . . ? O1 C27 H27A 95.7 . . ? O1S C27 H27B 99.2 . . ? O1 C27 H27B 117.6 . . ? H27A C27 H27B 109.5 . . ? O1S C27 H27C 104.5 . . ? O1 C27 H27C 114.1 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Mn2 Cl2 Mn1 88.43(5) . . ? Mn1 Cl3 Mn2 88.65(5) . . ? N3 Mn1 N5 81.24(18) . . ? N3 Mn1 N1 77.07(18) . . ? N5 Mn1 N1 75.84(18) . . ? N3 Mn1 Cl1 94.99(15) . . ? N5 Mn1 Cl1 100.67(15) . . ? N1 Mn1 Cl1 171.67(13) . . ? N3 Mn1 Cl3 163.57(15) . . ? N5 Mn1 Cl3 96.29(13) . . ? N1 Mn1 Cl3 86.56(12) . . ? Cl1 Mn1 Cl3 101.42(7) . . ? N3 Mn1 Cl2 92.39(13) . . ? N5 Mn1 Cl2 161.33(16) . . ? N1 Mn1 Cl2 85.65(12) . . ? Cl1 Mn1 Cl2 97.35(6) . . ? Cl3 Mn1 Cl2 84.85(5) . . ? N7 Mn2 N9 82.86(18) . . ? N7 Mn2 Cl4 93.94(14) . . ? N9 Mn2 Cl4 102.49(14) . . ? N7 Mn2 Cl2 164.88(14) . . ? N9 Mn2 Cl2 94.32(14) . . ? Cl4 Mn2 Cl2 101.16(6) . . ? N7 Mn2 N2 78.44(17) . . ? N9 Mn2 N2 74.58(18) . . ? Cl4 Mn2 N2 172.07(13) . . ? Cl2 Mn2 N2 86.49(12) . . ? N7 Mn2 Cl3 91.53(13) . . ? N9 Mn2 Cl3 154.61(14) . . ? Cl4 Mn2 Cl3 102.59(6) . . ? Cl2 Mn2 Cl3 84.67(5) . . ? N2 Mn2 Cl3 80.05(12) . . ? C1 N1 N2 121.4(5) . . ? C1 N1 Mn1 124.3(4) . . ? N2 N1 Mn1 114.0(4) . . ? C8 N2 N1 119.4(5) . . ? C8 N2 Mn2 122.7(4) . . ? N1 N2 Mn2 117.8(4) . . ? C10 N3 C11 106.5(5) . . ? C10 N3 Mn1 122.7(4) . . ? C11 N3 Mn1 130.5(4) . . ? C10 N4 C12 105.6(6) . . ? C10 N4 C13 128.8(6) . . ? C12 N4 C13 125.4(6) . . ? C14 N5 C15 104.7(6) . . ? C14 N5 Mn1 119.9(4) . . ? C15 N5 Mn1 135.4(5) . . ? C14 N6 C16 105.9(6) . . ? C14 N6 C17 128.4(6) . . ? C16 N6 C17 125.7(6) . . ? C19 N7 C20 104.7(5) . . ? C19 N7 Mn2 122.4(4) . . ? C20 N7 Mn2 132.8(4) . . ? C19 N8 C21 105.8(5) . . ? C19 N8 C22 129.0(5) . . ? C21 N8 C22 125.2(5) . . ? C23 N9 C24 105.2(5) . . ? C23 N9 Mn2 118.1(4) . . ? C24 N9 Mn2 135.6(4) . . ? C23 N10 C25 106.6(5) . . ? C23 N10 C26 127.3(5) . . ? C25 N10 C26 126.0(5) . . ? C27 O1 H1 104.2 . . ? C27 O1S H1 100.7 . . ? 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 N1 C1 C2 C3 -176.0(6) . . . . ? C9 C1 C2 C3 1.4(9) . . . . ? N1 C1 C2 C7 0.5(8) . . . . ? C9 C1 C2 C7 177.9(5) . . . . ? C7 C2 C3 C4 0.5(10) . . . . ? C1 C2 C3 C4 176.9(6) . . . . ? C2 C3 C4 C5 1.2(10) . . . . ? C3 C4 C5 C6 -1.8(10) . . . . ? C4 C5 C6 C7 0.7(10) . . . . ? C3 C2 C7 C6 -1.5(9) . . . . ? C1 C2 C7 C6 -178.3(5) . . . . ? C3 C2 C7 C8 177.6(6) . . . . ? C1 C2 C7 C8 0.9(8) . . . . ? C5 C6 C7 C2 0.9(9) . . . . ? C5 C6 C7 C8 -178.2(6) . . . . ? C2 C7 C8 N2 -1.6(8) . . . . ? C6 C7 C8 N2 177.6(5) . . . . ? C2 C7 C8 C18 174.8(5) . . . . ? C6 C7 C8 C18 -6.1(9) . . . . ? N1 C1 C9 C14 66.5(6) . . . . ? C2 C1 C9 C14 -111.1(6) . . . . ? N1 C1 C9 C10 -54.9(7) . . . . ? C2 C1 C9 C10 127.5(6) . . . . ? C14 C9 C10 N3 -52.1(8) . . . . ? C1 C9 C10 N3 66.6(8) . . . . ? C14 C9 C10 N4 128.6(7) . . . . ? C1 C9 C10 N4 -112.7(7) . . . . ? N3 C11 C12 N4 -0.4(8) . . . . ? C10 C9 C14 N5 54.8(8) . . . . ? C1 C9 C14 N5 -66.0(7) . . . . ? C10 C9 C14 N6 -129.8(6) . . . . ? C1 C9 C14 N6 109.4(7) . . . . ? N5 C15 C16 N6 -0.5(8) . . . . ? N2 C8 C18 C19 -60.0(6) . . . . ? C7 C8 C18 C19 123.3(6) . . . . ? N2 C8 C18 C23 63.0(6) . . . . ? C7 C8 C18 C23 -113.7(6) . . . . ? C23 C18 C19 N7 -48.6(8) . . . . ? C8 C18 C19 N7 69.9(7) . . . . ? C23 C18 C19 N8 129.6(6) . . . . ? C8 C18 C19 N8 -111.9(6) . . . . ? N7 C20 C21 N8 -1.0(7) . . . . ? C19 C18 C23 N9 48.9(8) . . . . ? C8 C18 C23 N9 -73.7(7) . . . . ? C19 C18 C23 N10 -139.5(6) . . . . ? C8 C18 C23 N10 97.9(6) . . . . ? N9 C24 C25 N10 -0.2(8) . . . . ? Mn2 Cl3 Mn1 N3 -54.3(5) . . . . ? Mn2 Cl3 Mn1 N5 -134.64(15) . . . . ? Mn2 Cl3 Mn1 N1 -59.31(12) . . . . ? Mn2 Cl3 Mn1 Cl1 123.10(6) . . . . ? Mn2 Cl3 Mn1 Cl2 26.62(6) . . . . ? Mn2 Cl2 Mn1 N3 135.96(14) . . . . ? Mn2 Cl2 Mn1 N5 66.6(4) . . . . ? Mn2 Cl2 Mn1 N1 59.12(12) . . . . ? Mn2 Cl2 Mn1 Cl1 -128.69(6) . . . . ? Mn2 Cl2 Mn1 Cl3 -27.81(6) . . . . ? Mn1 Cl2 Mn2 N7 -49.4(5) . . . . ? Mn1 Cl2 Mn2 N9 -128.01(14) . . . . ? Mn1 Cl2 Mn2 Cl4 128.33(6) . . . . ? Mn1 Cl2 Mn2 N2 -53.79(12) . . . . ? Mn1 Cl2 Mn2 Cl3 26.53(6) . . . . ? Mn1 Cl3 Mn2 N7 137.52(14) . . . . ? Mn1 Cl3 Mn2 N9 61.0(3) . . . . ? Mn1 Cl3 Mn2 Cl4 -128.09(6) . . . . ? Mn1 Cl3 Mn2 Cl2 -27.82(6) . . . . ? Mn1 Cl3 Mn2 N2 59.54(12) . . . . ? C2 C1 N1 N2 -1.3(8) . . . . ? C9 C1 N1 N2 -178.9(5) . . . . ? C2 C1 N1 Mn1 171.8(4) . . . . ? C9 C1 N1 Mn1 -5.8(7) . . . . ? N3 Mn1 N1 C1 44.4(4) . . . . ? N5 Mn1 N1 C1 -39.6(4) . . . . ? Cl3 Mn1 N1 C1 -137.0(4) . . . . ? Cl2 Mn1 N1 C1 137.9(4) . . . . ? N3 Mn1 N1 N2 -142.0(4) . . . . ? N5 Mn1 N1 N2 134.0(4) . . . . ? Cl3 Mn1 N1 N2 36.6(3) . . . . ? Cl2 Mn1 N1 N2 -48.5(3) . . . . ? C7 C8 N2 N1 0.8(8) . . . . ? C18 C8 N2 N1 -175.9(4) . . . . ? C7 C8 N2 Mn2 177.2(4) . . . . ? C18 C8 N2 Mn2 0.5(6) . . . . ? C1 N1 N2 C8 0.7(7) . . . . ? Mn1 N1 N2 C8 -173.1(4) . . . . ? C1 N1 N2 Mn2 -175.9(4) . . . . ? Mn1 N1 N2 Mn2 10.3(4) . . . . ? N7 Mn2 N2 C8 39.4(4) . . . . ? N9 Mn2 N2 C8 -46.3(4) . . . . ? Cl2 Mn2 N2 C8 -141.7(4) . . . . ? Cl3 Mn2 N2 C8 133.1(4) . . . . ? N7 Mn2 N2 N1 -144.1(4) . . . . ? N9 Mn2 N2 N1 130.2(4) . . . . ? Cl2 Mn2 N2 N1 34.7(3) . . . . ? Cl3 Mn2 N2 N1 -50.5(3) . . . . ? N4 C10 N3 C11 -0.3(7) . . . . ? C9 C10 N3 C11 -179.7(6) . . . . ? N4 C10 N3 Mn1 174.5(4) . . . . ? C9 C10 N3 Mn1 -4.9(8) . . . . ? C12 C11 N3 C10 0.4(8) . . . . ? C12 C11 N3 Mn1 -173.8(5) . . . . ? N5 Mn1 N3 C10 40.6(5) . . . . ? N1 Mn1 N3 C10 -36.7(5) . . . . ? Cl1 Mn1 N3 C10 140.7(5) . . . . ? Cl3 Mn1 N3 C10 -41.8(8) . . . . ? Cl2 Mn1 N3 C10 -121.7(5) . . . . ? N5 Mn1 N3 C11 -145.9(6) . . . . ? N1 Mn1 N3 C11 136.8(6) . . . . ? Cl1 Mn1 N3 C11 -45.8(5) . . . . ? Cl3 Mn1 N3 C11 131.6(5) . . . . ? Cl2 Mn1 N3 C11 51.8(5) . . . . ? N3 C10 N4 C12 0.1(8) . . . . ? C9 C10 N4 C12 179.4(6) . . . . ? N3 C10 N4 C13 175.3(8) . . . . ? C9 C10 N4 C13 -5.4(12) . . . . ? C11 C12 N4 C10 0.2(8) . . . . ? C11 C12 N4 C13 -175.2(8) . . . . ? N6 C14 N5 C15 -0.2(7) . . . . ? C9 C14 N5 C15 175.7(5) . . . . ? N6 C14 N5 Mn1 -177.6(4) . . . . ? C9 C14 N5 Mn1 -1.7(8) . . . . ? C16 C15 N5 C14 0.4(8) . . . . ? C16 C15 N5 Mn1 177.2(5) . . . . ? N3 Mn1 N5 C14 -37.1(5) . . . . ? N1 Mn1 N5 C14 41.7(4) . . . . ? Cl1 Mn1 N5 C14 -130.6(4) . . . . ? Cl3 Mn1 N5 C14 126.5(4) . . . . ? Cl2 Mn1 N5 C14 34.0(7) . . . . ? N3 Mn1 N5 C15 146.5(6) . . . . ? N1 Mn1 N5 C15 -134.8(6) . . . . ? Cl1 Mn1 N5 C15 53.0(6) . . . . ? Cl3 Mn1 N5 C15 -49.9(6) . . . . ? Cl2 Mn1 N5 C15 -142.5(5) . . . . ? N5 C14 N6 C16 -0.1(8) . . . . ? C9 C14 N6 C16 -175.9(6) . . . . ? N5 C14 N6 C17 -179.4(7) . . . . ? C9 C14 N6 C17 4.8(11) . . . . ? C15 C16 N6 C14 0.3(8) . . . . ? C15 C16 N6 C17 179.7(7) . . . . ? N8 C19 N7 C20 -0.7(7) . . . . ? C18 C19 N7 C20 177.7(5) . . . . ? N8 C19 N7 Mn2 177.0(4) . . . . ? C18 C19 N7 Mn2 -4.6(8) . . . . ? C21 C20 N7 C19 1.0(7) . . . . ? C21 C20 N7 Mn2 -176.3(4) . . . . ? N9 Mn2 N7 C19 40.2(5) . . . . ? Cl4 Mn2 N7 C19 142.3(4) . . . . ? Cl2 Mn2 N7 C19 -39.9(8) . . . . ? N2 Mn2 N7 C19 -35.5(5) . . . . ? Cl3 Mn2 N7 C19 -115.0(5) . . . . ? N9 Mn2 N7 C20 -142.9(5) . . . . ? Cl4 Mn2 N7 C20 -40.8(5) . . . . ? Cl2 Mn2 N7 C20 137.0(5) . . . . ? N2 Mn2 N7 C20 141.5(5) . . . . ? Cl3 Mn2 N7 C20 62.0(5) . . . . ? N7 C19 N8 C21 0.1(7) . . . . ? C18 C19 N8 C21 -178.2(6) . . . . ? N7 C19 N8 C22 -179.3(6) . . . . ? C18 C19 N8 C22 2.4(10) . . . . ? C20 C21 N8 C19 0.5(7) . . . . ? C20 C21 N8 C22 180.0(6) . . . . ? N10 C23 N9 C24 0.2(7) . . . . ? C18 C23 N9 C24 172.6(6) . . . . ? N10 C23 N9 Mn2 -169.1(4) . . . . ? C18 C23 N9 Mn2 3.3(8) . . . . ? C25 C24 N9 C23 0.0(8) . . . . ? C25 C24 N9 Mn2 166.5(5) . . . . ? N7 Mn2 N9 C23 -38.7(5) . . . . ? Cl4 Mn2 N9 C23 -131.2(4) . . . . ? Cl2 Mn2 N9 C23 126.3(5) . . . . ? N2 Mn2 N9 C23 41.2(4) . . . . ? Cl3 Mn2 N9 C23 39.7(7) . . . . ? N7 Mn2 N9 C24 156.1(6) . . . . ? Cl4 Mn2 N9 C24 63.6(6) . . . . ? Cl2 Mn2 N9 C24 -38.9(6) . . . . ? N2 Mn2 N9 C24 -124.0(6) . . . . ? Cl3 Mn2 N9 C24 -125.5(5) . . . . ? N9 C23 N10 C25 -0.3(7) . . . . ? C18 C23 N10 C25 -173.0(6) . . . . ? N9 C23 N10 C26 176.7(6) . . . . ? C18 C23 N10 C26 4.0(9) . . . . ? C24 C25 N10 C23 0.3(7) . . . . ? C24 C25 N10 C26 -176.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.477 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.102 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.000 0.000 0.000 142.0 6.5 2 0.500 0.500 0.500 141.9 6.3 _platon_squeeze_details ; Before SQUEEZE two methanol molecules had been identified. One of these molecules was gossly disordered and was excluded using the program SQUEEZE (Platon). ; # Start Validation Reply Form _vrf_PLAT605_1 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 147.00 A**3 RESPONSE: One disordered solvent molecule (MeOH) could not be modeled successfully and were removed from the reflection data using the program SQUEEZE (Platon). The reported formula weigth, F(000), density, etc. reflect the unit cell content including the removed solvent molecule. ;