Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Panayotis Kyritsis' 'Alexios Grigoropoulos' 'Dimitrios Maganas' 'S. Parsons' 'Georgios Pneumatikakis' 'Neil Robertson' 'Sarah S. Staniland' 'Fraser White' _publ_contact_author_name 'Panayotis Kyritsis' _publ_contact_author_address ; Department of Chemistry University of Athens Inorganic Chemistry Laboratory Panepistimiopolis Athens GR-15771 GREECE ; _publ_contact_author_email KYRITSIS@CHEM.UOA.GR _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Structural, spectroscopic and magnetic properties of M[R2P(E)NP(E)R'2]2 complexes, M = Co, Mn, E= S, Se and R, R' = Ph or iPr. Covalency of M-S bonds from experimental data and theoretical calculations. ; # Attachment 'Co[(SPIPr2)(SPPh2)N]2.txt' data_sspk01 #(Complex 3) _database_code_depnum_ccdc_archive 'CCDC 293307' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 Co N2 P4 S4' _chemical_formula_sum 'C36 H48 Co N2 P4 S4' _chemical_formula_weight 819.81 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' P P 0.1023 0.0942 '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' Co Co 0.3494 0.9721 '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' _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 12.6570(3) _cell_length_b 15.6482(4) _cell_length_c 21.4667(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.356(2) _cell_angle_gamma 90.00 _cell_volume 4136.69(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5771 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30.5 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1716 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details 'SADABS version 2004/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30143 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.54 _reflns_number_total 6000 _reflns_number_gt 4997 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'PLATON, ENCIFER, XCIF' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. >>> The Following ALERTS were generated <<< #------------------------------------------ Format: alert-number_ALERT_alert-type_alert-level text 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.43 601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 76.00 A**3 Difference map does not reveal any missing peaks, R factor is 3.3% 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 No action taken 029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 342 Noted see completeness stats below #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 2172 2172 0 23.01 0.550 1.000 2877 2877 0 25.24 0.600 1.000 3737 3737 0 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 4758 4758 0 29.84 0.700 0.974 5933 5778 155 30.54 0.715 0.946 6342 6000 342 ; _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^)+(0.0501P)^2^+1.6942P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6000 _refine_ls_number_parameters 215 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0862 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Co1 Co 0.0000 0.012179(17) 0.7500 0.01916(7) Uani 1 2 d S . . S1 S -0.11258(3) -0.08785(2) 0.686191(17) 0.02458(9) Uani 1 1 d . . . P1 P -0.22299(3) -0.00645(2) 0.634877(17) 0.01982(9) Uani 1 1 d . . . N1 N -0.24254(10) 0.08192(8) 0.66627(6) 0.0238(3) Uani 1 1 d . . . C11 C -0.18417(11) 0.01835(10) 0.56083(7) 0.0239(3) Uani 1 1 d . . . C21 C -0.16556(13) -0.04831(11) 0.52149(8) 0.0316(3) Uani 1 1 d . . . H21 H -0.1728 -0.1059 0.5339 0.038 Uiso 1 1 calc R . . C31 C -0.13650(14) -0.03096(13) 0.46434(8) 0.0373(4) Uani 1 1 d . . . H31 H -0.1245 -0.0766 0.4376 0.045 Uiso 1 1 calc R . . C41 C -0.12493(14) 0.05268(14) 0.44624(8) 0.0391(4) Uani 1 1 d . . . H41 H -0.1045 0.0646 0.4072 0.047 Uiso 1 1 calc R . . C51 C -0.14311(16) 0.11886(13) 0.48493(9) 0.0407(4) Uani 1 1 d . . . H51 H -0.1353 0.1763 0.4724 0.049 Uiso 1 1 calc R . . C61 C -0.17293(14) 0.10183(11) 0.54231(8) 0.0329(4) Uani 1 1 d . . . H61 H -0.1855 0.1477 0.5687 0.039 Uiso 1 1 calc R . . C12 C -0.35055(11) -0.06386(10) 0.60894(7) 0.0237(3) Uani 1 1 d . . . C22 C -0.35516(14) -0.15259(11) 0.60580(9) 0.0369(4) Uani 1 1 d . . . H22 H -0.2905 -0.1852 0.6190 0.044 Uiso 1 1 calc R . . C32 C -0.45364(16) -0.19374(13) 0.58349(10) 0.0488(5) Uani 1 1 d . . . H32 H -0.4563 -0.2544 0.5813 0.059 Uiso 1 1 calc R . . C42 C -0.54797(14) -0.14652(13) 0.56444(9) 0.0434(4) Uani 1 1 d . . . H42 H -0.6154 -0.1748 0.5492 0.052 Uiso 1 1 calc R . . C52 C -0.54454(13) -0.05842(13) 0.56748(8) 0.0369(4) Uani 1 1 d . . . H52 H -0.6095 -0.0262 0.5543 0.044 Uiso 1 1 calc R . . C62 C -0.44593(13) -0.01706(11) 0.58983(8) 0.0304(3) Uani 1 1 d . . . H62 H -0.4437 0.0436 0.5921 0.037 Uiso 1 1 calc R . . S2 S 0.09827(3) 0.09597(3) 0.695332(17) 0.02475(9) Uani 1 1 d . . . P2 P 0.23400(3) 0.12190(2) 0.764575(17) 0.02024(9) Uani 1 1 d . . . C13 C 0.24354(13) 0.23685(9) 0.77740(8) 0.0282(3) Uani 1 1 d . . . H13 H 0.2338 0.2652 0.7347 0.034 Uiso 1 1 calc R . . C23 C 0.15207(18) 0.26648(12) 0.80755(11) 0.0465(5) Uani 1 1 d . . . H23A H 0.0822 0.2477 0.7810 0.070 Uiso 1 1 calc R . . H23B H 0.1530 0.3290 0.8106 0.070 Uiso 1 1 calc R . . H23C H 0.1621 0.2418 0.8505 0.070 Uiso 1 1 calc R . . C33 C 0.35437(16) 0.26276(11) 0.81812(9) 0.0417(4) Uani 1 1 d . . . H33A H 0.4111 0.2461 0.7963 0.063 Uiso 1 1 calc R . . H33B H 0.3668 0.2340 0.8598 0.063 Uiso 1 1 calc R . . H33C H 0.3563 0.3248 0.8245 0.063 Uiso 1 1 calc R . . C14 C 0.34982(12) 0.09097(10) 0.73199(7) 0.0250(3) Uani 1 1 d . . . H14 H 0.4175 0.1031 0.7654 0.030 Uiso 1 1 calc R . . C24 C 0.35479(13) 0.14314(11) 0.67240(8) 0.0323(3) Uani 1 1 d . . . H24A H 0.3565 0.2042 0.6828 0.048 Uiso 1 1 calc R . . H24B H 0.2906 0.1308 0.6382 0.048 Uiso 1 1 calc R . . H24C H 0.4204 0.1278 0.6581 0.048 Uiso 1 1 calc R . . C34 C 0.34708(14) -0.00468(10) 0.71786(8) 0.0307(3) Uani 1 1 d . . . H34A H 0.3441 -0.0365 0.7567 0.046 Uiso 1 1 calc R . . H34B H 0.4126 -0.0209 0.7038 0.046 Uiso 1 1 calc R . . H34C H 0.2828 -0.0180 0.6840 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01638(13) 0.02204(14) 0.01894(13) 0.000 0.00382(10) 0.000 S1 0.02339(18) 0.02121(18) 0.02522(18) -0.00049(13) -0.00242(14) 0.00109(13) P1 0.01919(17) 0.02182(17) 0.01768(17) 0.00014(13) 0.00267(13) 0.00034(13) N1 0.0281(6) 0.0223(6) 0.0206(6) 0.0008(4) 0.0048(5) 0.0035(5) C11 0.0194(6) 0.0326(8) 0.0186(6) 0.0006(5) 0.0021(5) -0.0006(6) C21 0.0336(8) 0.0360(9) 0.0259(7) -0.0028(6) 0.0085(6) -0.0004(7) C31 0.0351(9) 0.0528(11) 0.0253(8) -0.0078(7) 0.0094(7) 0.0017(8) C41 0.0337(9) 0.0635(13) 0.0208(8) 0.0042(8) 0.0079(7) -0.0016(8) C51 0.0469(10) 0.0463(10) 0.0302(9) 0.0099(7) 0.0113(8) -0.0062(8) C61 0.0396(9) 0.0335(8) 0.0263(8) 0.0013(6) 0.0090(7) -0.0023(7) C12 0.0215(6) 0.0294(7) 0.0197(6) 0.0018(5) 0.0037(5) -0.0016(6) C22 0.0289(8) 0.0311(8) 0.0451(10) 0.0066(7) -0.0032(7) -0.0036(7) C32 0.0401(10) 0.0352(10) 0.0622(13) 0.0081(9) -0.0062(9) -0.0135(8) C42 0.0279(8) 0.0554(12) 0.0425(10) 0.0084(9) -0.0009(7) -0.0158(8) C52 0.0215(7) 0.0553(11) 0.0329(9) 0.0020(8) 0.0044(6) 0.0015(7) C62 0.0245(7) 0.0363(9) 0.0297(8) -0.0015(6) 0.0043(6) 0.0022(6) S2 0.01988(17) 0.0341(2) 0.02063(17) 0.00424(14) 0.00540(13) -0.00174(14) P2 0.02031(17) 0.02088(18) 0.02058(17) -0.00021(13) 0.00686(13) -0.00101(13) C13 0.0366(8) 0.0202(7) 0.0300(8) 0.0009(6) 0.0124(7) -0.0016(6) C23 0.0597(12) 0.0280(9) 0.0612(13) -0.0024(8) 0.0332(10) 0.0061(8) C33 0.0519(11) 0.0295(9) 0.0426(10) -0.0081(7) 0.0086(9) -0.0128(8) C14 0.0186(6) 0.0301(8) 0.0270(7) -0.0018(6) 0.0069(6) -0.0008(6) C24 0.0285(8) 0.0387(9) 0.0336(8) 0.0012(7) 0.0150(7) -0.0033(7) C34 0.0296(8) 0.0307(8) 0.0337(8) -0.0054(6) 0.0114(7) 0.0039(6) _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. >>> The Following ALERTS were generated <<< #------------------------------------------ Format: alert-number_ALERT_alert-type_alert-level text 029_ALERT_3_B _diffrn_measured_fraction_theta_full Low ....... 0.95 912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 342 Noted but completeness is 100% to 0.76A INTENSITY STATISTICS FOR DATASET # 1 sspk01.hkl Resolution #Data #Theory %Complete Redundancy Mean I Mean I/s R(int) Rsigma Inf - 1.97 313 315 99.4 10.17 696.5 59.17 0.0203 0.0151 1.97 - 1.56 318 318 100.0 10.47 420.6 54.01 0.0228 0.0148 1.56 - 1.36 312 312 100.0 8.29 271.2 45.30 0.0290 0.0168 1.36 - 1.23 327 327 100.0 7.08 196.4 36.43 0.0351 0.0197 1.23 - 1.13 346 346 100.0 6.49 148.5 31.52 0.0377 0.0221 1.13 - 1.06 354 354 100.0 5.65 128.7 28.35 0.0394 0.0248 1.06 - 1.00 368 368 100.0 4.85 120.8 24.41 0.0457 0.0281 1.00 - 0.96 313 313 100.0 4.59 105.0 22.08 0.0505 0.0321 0.96 - 0.92 338 338 100.0 4.32 83.0 19.14 0.0553 0.0374 0.92 - 0.89 334 334 100.0 4.01 73.1 16.21 0.0574 0.0426 0.89 - 0.86 339 339 100.0 4.02 62.4 15.49 0.0631 0.0464 0.86 - 0.83 426 426 100.0 3.81 55.9 13.08 0.0672 0.0543 0.83 - 0.80 474 474 100.0 3.61 46.2 11.59 0.0760 0.0652 0.80 - 0.78 358 358 100.0 3.65 39.8 10.45 0.0895 0.0753 0.78 - 0.76 404 404 100.0 3.28 43.4 9.73 0.0881 0.0822 0.76 - 0.74 398 447 89.0 2.13 36.6 7.16 0.0893 0.1171 0.74 - 0.72 322 480 67.1 1.12 28.2 4.68 0.0952 0.1777 0.72 - 0.70 154 300 51.3 0.82 32.3 5.44 0.1013 0.1572 #----------------------------------------------------------------------------- 0.80 - 0.70 1800 2153 83.6 2.29 37.5 8.18 0.0886 0.1053 Inf - 0.70 6198 6553 94.6 4.69 137.9 22.53 0.0311 0.0292 Merged [A], lowest resolution = 10.44 Angstroms, 1006 outliers downweighted 094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.43 601_ALERT_2_C Structure Contains Solvent Accessible VOIDS of . 76.00 A**3 There are no significant Q peaks in the space around the molecule and the R factor is 3.2% 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 No action taken ; 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 Co1 S2 2.3061(4) . ? Co1 S2 2.3061(4) 2_556 ? Co1 S1 2.3356(4) . ? Co1 S1 2.3356(4) 2_556 ? S1 P1 2.0194(5) . ? P1 N1 1.5826(12) . ? P1 C11 1.8109(15) . ? P1 C12 1.8189(15) . ? N1 P2 1.5915(12) 2_556 ? C11 C61 1.382(2) . ? C11 C21 1.396(2) . ? C21 C31 1.387(2) . ? C21 H21 0.9500 . ? C31 C41 1.383(3) . ? C31 H31 0.9500 . ? C41 C51 1.380(3) . ? C41 H41 0.9500 . ? C51 C61 1.395(2) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C12 C62 1.390(2) . ? C12 C22 1.391(2) . ? C22 C32 1.386(2) . ? C22 H22 0.9500 . ? C32 C42 1.383(3) . ? C32 H32 0.9500 . ? C42 C52 1.380(3) . ? C42 H42 0.9500 . ? C52 C62 1.389(2) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? S2 P2 2.0361(5) . ? P2 N1 1.5915(12) 2_556 ? P2 C13 1.8196(15) . ? P2 C14 1.8293(15) . ? C13 C23 1.523(2) . ? C13 C33 1.526(2) . ? C13 H13 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C14 C34 1.526(2) . ? C14 C24 1.531(2) . ? C14 H14 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? 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 S2 Co1 S2 110.69(2) . 2_556 ? S2 Co1 S1 114.225(13) . . ? S2 Co1 S1 110.599(13) 2_556 . ? S2 Co1 S1 110.599(13) . 2_556 ? S2 Co1 S1 114.225(13) 2_556 2_556 ? S1 Co1 S1 95.84(2) . 2_556 ? P1 S1 Co1 98.553(18) . . ? N1 P1 C11 106.70(7) . . ? N1 P1 C12 110.30(7) . . ? C11 P1 C12 103.81(6) . . ? N1 P1 S1 118.39(5) . . ? C11 P1 S1 108.67(5) . . ? C12 P1 S1 107.99(5) . . ? P1 N1 P2 139.21(8) . 2_556 ? C61 C11 C21 119.29(14) . . ? C61 C11 P1 121.45(12) . . ? C21 C11 P1 119.26(12) . . ? C31 C21 C11 120.35(16) . . ? C31 C21 H21 119.8 . . ? C11 C21 H21 119.8 . . ? C41 C31 C21 120.06(16) . . ? C41 C31 H31 120.0 . . ? C21 C31 H31 120.0 . . ? C51 C41 C31 119.88(16) . . ? C51 C41 H41 120.1 . . ? C31 C41 H41 120.1 . . ? C41 C51 C61 120.33(17) . . ? C41 C51 H51 119.8 . . ? C61 C51 H51 119.8 . . ? C11 C61 C51 120.09(16) . . ? C11 C61 H61 120.0 . . ? C51 C61 H61 120.0 . . ? C62 C12 C22 119.19(14) . . ? C62 C12 P1 118.62(12) . . ? C22 C12 P1 122.16(12) . . ? C32 C22 C12 120.32(16) . . ? C32 C22 H22 119.8 . . ? C12 C22 H22 119.8 . . ? C42 C32 C22 119.98(18) . . ? C42 C32 H32 120.0 . . ? C22 C32 H32 120.0 . . ? C52 C42 C32 120.27(16) . . ? C52 C42 H42 119.9 . . ? C32 C42 H42 119.9 . . ? C42 C52 C62 119.83(16) . . ? C42 C52 H52 120.1 . . ? C62 C52 H52 120.1 . . ? C52 C62 C12 120.40(16) . . ? C52 C62 H62 119.8 . . ? C12 C62 H62 119.8 . . ? P2 S2 Co1 101.835(18) . . ? N1 P2 C13 105.05(7) 2_556 . ? N1 P2 C14 111.41(7) 2_556 . ? C13 P2 C14 106.76(7) . . ? N1 P2 S2 117.82(5) 2_556 . ? C13 P2 S2 108.83(6) . . ? C14 P2 S2 106.48(5) . . ? C23 C13 C33 111.34(15) . . ? C23 C13 P2 109.56(11) . . ? C33 C13 P2 111.67(12) . . ? C23 C13 H13 108.0 . . ? C33 C13 H13 108.0 . . ? P2 C13 H13 108.0 . . ? C13 C23 H23A 109.5 . . ? C13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C13 C33 H33A 109.5 . . ? C13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34 C14 C24 111.13(13) . . ? C34 C14 P2 110.61(10) . . ? C24 C14 P2 111.70(11) . . ? C34 C14 H14 107.7 . . ? C24 C14 H14 107.7 . . ? P2 C14 H14 107.7 . . ? C14 C24 H24A 109.5 . . ? C14 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C14 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14 C34 H34A 109.5 . . ? C14 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C14 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.575 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.069 # Attachment 'Mn[(SPiPr2)(SPPh2)N]2.txt' data_sspk5a #(Complex 6) _database_code_depnum_ccdc_archive 'CCDC 293308' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 Mn N2 P4 S4, C H2 Cl2' _chemical_formula_sum 'C37 H50 Cl2 Mn N2 P4 S4' _chemical_formula_weight 900.75 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' P P 0.1023 0.0942 '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 triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' _chemical_absolute_configuration unk loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.9405(3) _cell_length_b 10.2453(3) _cell_length_c 11.2043(3) _cell_angle_alpha 96.560(2) _cell_angle_beta 101.4900(10) _cell_angle_gamma 100.4150(10) _cell_volume 1086.35(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6648 _cell_measurement_theta_min 5.02 _cell_measurement_theta_max 57.24 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.301 _exptl_crystal_size_mid 0.207 _exptl_crystal_size_min 0.201 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 469 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS 2004/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11470 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11470 _reflns_number_gt 10848 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'PLATON, ENCIFER, XCIF' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. >>> The Following ALERTS were generated <<< #------------------------------------------ Format: alert-number_ALERT_alert-type_alert-level text 021_ALERT_1_B Ratio Unique / Expected Reflections too High ... 2.58 Crystal was twinned, refinement carried out with an HKLF 5 format file 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 No action taken 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.01 Ratio This appears to be the C in the DCM moiety which is solvent 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 14 911_ALERT_3_B # Missing FCF Refl. Between TH(Min) & STH/L=0.6 17 See completeness stats below #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.998 2270 2266 4 23.01 0.550 0.997 3025 3017 8 25.24 0.600 0.996 3928 3911 17 #----------------------------------------------------------- ACTA Min. Res. ---- 26.37 0.625 0.993 4442 4411 31 ; _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^)+(0.0482P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.033(16) _refine_ls_number_reflns 11470 _refine_ls_number_parameters 452 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.1035 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.27967(5) 0.16878(5) 0.41608(5) 0.02004(12) Uani 1 1 d . . . S1 S 0.04682(9) 0.15383(9) 0.28334(9) 0.0260(2) Uani 1 1 d . . . P1 P 0.02997(9) -0.03244(9) 0.19376(8) 0.01944(19) Uani 1 1 d . . . N1 N 0.1170(3) -0.1294(3) 0.2598(3) 0.0247(7) Uani 1 1 d . . . P2 P 0.16484(9) -0.17030(9) 0.39198(9) 0.0205(2) Uani 1 1 d . . . S2 S 0.27582(9) -0.02077(9) 0.52969(8) 0.0256(2) Uani 1 1 d . . . C11 C -0.1550(4) -0.1136(4) 0.1450(3) 0.0222(8) Uani 1 1 d . . . C21 C -0.2621(4) -0.0438(4) 0.1464(3) 0.0265(8) Uani 1 1 d . . . H21 H -0.2402 0.0500 0.1761 0.032 Uiso 1 1 calc R . . C31 C -0.4010(4) -0.1104(4) 0.1047(4) 0.0348(10) Uani 1 1 d . . . H31 H -0.4745 -0.0631 0.1069 0.042 Uiso 1 1 calc R . . C41 C -0.4318(4) -0.2474(4) 0.0596(4) 0.0346(10) Uani 1 1 d . . . H41 H -0.5269 -0.2930 0.0299 0.041 Uiso 1 1 calc R . . C51 C -0.3270(4) -0.3172(4) 0.0574(4) 0.0358(10) Uani 1 1 d . . . H51 H -0.3495 -0.4109 0.0276 0.043 Uiso 1 1 calc R . . C61 C -0.1869(4) -0.2501(4) 0.0993(4) 0.0289(9) Uani 1 1 d . . . H61 H -0.1136 -0.2977 0.0965 0.035 Uiso 1 1 calc R . . C12 C 0.0836(4) -0.0173(4) 0.0494(3) 0.0244(8) Uani 1 1 d . . . C22 C 0.0201(4) 0.0588(4) -0.0307(4) 0.0326(9) Uani 1 1 d . . . H22 H -0.0479 0.1055 -0.0087 0.039 Uiso 1 1 calc R . . C32 C 0.0570(5) 0.0661(4) -0.1438(4) 0.0407(11) Uani 1 1 d . . . H32 H 0.0129 0.1170 -0.1996 0.049 Uiso 1 1 calc R . . C42 C 0.1564(5) 0.0004(5) -0.1755(4) 0.0462(12) Uani 1 1 d . . . H42 H 0.1831 0.0076 -0.2517 0.055 Uiso 1 1 calc R . . C52 C 0.2175(5) -0.0764(5) -0.0949(4) 0.0445(11) Uani 1 1 d . . . H52 H 0.2845 -0.1238 -0.1179 0.053 Uiso 1 1 calc R . . C62 C 0.1839(4) -0.0858(4) 0.0166(4) 0.0341(9) Uani 1 1 d . . . H62 H 0.2279 -0.1379 0.0711 0.041 Uiso 1 1 calc R . . C15 C 0.2749(4) -0.2915(4) 0.3681(4) 0.0273(8) Uani 1 1 d . . . H15 H 0.3104 -0.3198 0.4490 0.033 Uiso 1 1 calc R . . C35 C 0.4001(5) -0.2234(5) 0.3226(5) 0.0497(13) Uani 1 1 d . . . H35A H 0.4522 -0.1445 0.3827 0.075 Uiso 1 1 calc R . . H35B H 0.3670 -0.1952 0.2431 0.075 Uiso 1 1 calc R . . H35C H 0.4618 -0.2865 0.3126 0.075 Uiso 1 1 calc R . . C25 C 0.1898(5) -0.4158(5) 0.2781(4) 0.0452(12) Uani 1 1 d . . . H25A H 0.1109 -0.4574 0.3108 0.068 Uiso 1 1 calc R . . H25B H 0.2499 -0.4803 0.2674 0.068 Uiso 1 1 calc R . . H25C H 0.1539 -0.3897 0.1983 0.068 Uiso 1 1 calc R . . C16 C 0.0165(4) -0.2575(4) 0.4460(3) 0.0243(8) Uani 1 1 d . . . H16 H -0.0390 -0.3314 0.3786 0.029 Uiso 1 1 calc R . . C36 C 0.0661(4) -0.3212(4) 0.5608(4) 0.0317(9) Uani 1 1 d . . . H36A H 0.1276 -0.3817 0.5422 0.048 Uiso 1 1 calc R . . H36B H -0.0156 -0.3722 0.5840 0.048 Uiso 1 1 calc R . . H36C H 0.1177 -0.2503 0.6293 0.048 Uiso 1 1 calc R . . C26 C -0.0806(4) -0.1624(4) 0.4735(4) 0.0331(10) Uani 1 1 d . . . H26A H -0.1122 -0.1232 0.3998 0.050 Uiso 1 1 calc R . . H26B H -0.0293 -0.0904 0.5412 0.050 Uiso 1 1 calc R . . H26C H -0.1621 -0.2128 0.4972 0.050 Uiso 1 1 calc R . . S3 S 0.29808(9) 0.38989(9) 0.53524(9) 0.0264(2) Uani 1 1 d . . . P3 P 0.49373(9) 0.40671(9) 0.63700(8) 0.01897(19) Uani 1 1 d . . . N2 N 0.5988(3) 0.3340(3) 0.5798(3) 0.0241(7) Uani 1 1 d . . . P4 P 0.63477(9) 0.28965(9) 0.45078(8) 0.01966(19) Uani 1 1 d . . . S4 S 0.47615(10) 0.17666(9) 0.31560(9) 0.0278(2) Uani 1 1 d . . . C13 C 0.4783(4) 0.3401(4) 0.7779(3) 0.0268(8) Uani 1 1 d . . . C23 C 0.5317(5) 0.2270(5) 0.8039(4) 0.0411(11) Uani 1 1 d . . . H23 H 0.5770 0.1847 0.7481 0.049 Uiso 1 1 calc R . . C33 C 0.5184(6) 0.1770(6) 0.9110(5) 0.0574(14) Uani 1 1 d . . . H33 H 0.5525 0.0984 0.9271 0.069 Uiso 1 1 calc R . . C43 C 0.4578(6) 0.2375(6) 0.9936(4) 0.0591(16) Uani 1 1 d . . . H43 H 0.4523 0.2032 1.0682 0.071 Uiso 1 1 calc R . . C53 C 0.4044(5) 0.3485(6) 0.9692(4) 0.0547(15) Uani 1 1 d . . . H53 H 0.3603 0.3905 1.0263 0.066 Uiso 1 1 calc R . . C63 C 0.4148(5) 0.3997(5) 0.8606(4) 0.0404(11) Uani 1 1 d . . . H63 H 0.3775 0.4765 0.8439 0.048 Uiso 1 1 calc R . . C14 C 0.5713(3) 0.5839(3) 0.6884(3) 0.0197(7) Uani 1 1 d . . . C24 C 0.4882(4) 0.6795(4) 0.6911(3) 0.0266(8) Uani 1 1 d . . . H24 H 0.3890 0.6526 0.6646 0.032 Uiso 1 1 calc R . . C34 C 0.5501(4) 0.8148(4) 0.7326(4) 0.0350(9) Uani 1 1 d . . . H34 H 0.4937 0.8804 0.7321 0.042 Uiso 1 1 calc R . . C44 C 0.6942(4) 0.8526(4) 0.7744(4) 0.0351(10) Uani 1 1 d . . . H44 H 0.7366 0.9444 0.8042 0.042 Uiso 1 1 calc R . . C54 C 0.7771(4) 0.7579(4) 0.7733(4) 0.0334(9) Uani 1 1 d . . . H54 H 0.8760 0.7847 0.8020 0.040 Uiso 1 1 calc R . . C64 C 0.7153(4) 0.6229(4) 0.7298(4) 0.0284(9) Uani 1 1 d . . . H64 H 0.7722 0.5578 0.7287 0.034 Uiso 1 1 calc R . . C17 C 0.7132(4) 0.4327(4) 0.3867(4) 0.0237(8) Uani 1 1 d . . . H17 H 0.7935 0.4873 0.4522 0.028 Uiso 1 1 calc R . . C37 C 0.6073(4) 0.5228(4) 0.3534(4) 0.0351(10) Uani 1 1 d . . . H37A H 0.5705 0.5484 0.4256 0.053 Uiso 1 1 calc R . . H37B H 0.5297 0.4736 0.2859 0.053 Uiso 1 1 calc R . . H37C H 0.6542 0.6038 0.3274 0.053 Uiso 1 1 calc R . . C27 C 0.7720(4) 0.3897(4) 0.2750(4) 0.0309(9) Uani 1 1 d . . . H27A H 0.8393 0.3329 0.2984 0.046 Uiso 1 1 calc R . . H27B H 0.8192 0.4696 0.2477 0.046 Uiso 1 1 calc R . . H27C H 0.6949 0.3390 0.2078 0.046 Uiso 1 1 calc R . . C18 C 0.7699(4) 0.1903(4) 0.4858(4) 0.0288(9) Uani 1 1 d . . . H18 H 0.7875 0.1498 0.4063 0.035 Uiso 1 1 calc R . . C38 C 0.9076(4) 0.2774(5) 0.5631(4) 0.0430(11) Uani 1 1 d . . . H38A H 0.9412 0.3490 0.5185 0.065 Uiso 1 1 calc R . . H38B H 0.9779 0.2218 0.5788 0.065 Uiso 1 1 calc R . . H38C H 0.8923 0.3173 0.6417 0.065 Uiso 1 1 calc R . . C28 C 0.7161(5) 0.0772(5) 0.5520(5) 0.0504(13) Uani 1 1 d . . . H28A H 0.6277 0.0226 0.5010 0.076 Uiso 1 1 calc R . . H28B H 0.7001 0.1153 0.6310 0.076 Uiso 1 1 calc R . . H28C H 0.7857 0.0209 0.5667 0.076 Uiso 1 1 calc R . . C1S C 0.0502(7) 0.4137(6) -0.0568(7) 0.087(2) Uani 1 1 d . . . H1S1 H 0.0788 0.3493 -0.1146 0.104 Uiso 1 1 calc R . . H1S2 H 0.0993 0.4081 0.0279 0.104 Uiso 1 1 calc R . . Cl1S Cl 0.1014(2) 0.57500(17) -0.08806(19) 0.0921(6) Uani 1 1 d . . . Cl2S Cl -0.12914(19) 0.36840(19) -0.06996(18) 0.0885(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0195(3) 0.0189(3) 0.0210(3) 0.0026(2) 0.0049(2) 0.00202(19) S1 0.0236(4) 0.0225(5) 0.0283(5) -0.0039(4) -0.0016(4) 0.0090(4) P1 0.0218(4) 0.0179(4) 0.0185(5) 0.0021(4) 0.0039(4) 0.0049(3) N1 0.0275(16) 0.0267(17) 0.0234(17) 0.0066(13) 0.0075(13) 0.0111(13) P2 0.0200(4) 0.0198(5) 0.0237(5) 0.0062(4) 0.0075(4) 0.0048(4) S2 0.0270(5) 0.0254(5) 0.0212(5) 0.0063(4) 0.0034(4) -0.0022(4) C11 0.0266(18) 0.0229(18) 0.0163(18) 0.0059(15) 0.0067(15) -0.0012(15) C21 0.029(2) 0.027(2) 0.024(2) 0.0063(16) 0.0060(16) 0.0066(16) C31 0.027(2) 0.046(3) 0.034(2) 0.007(2) 0.0107(18) 0.0097(18) C41 0.030(2) 0.038(2) 0.027(2) 0.0042(18) 0.0037(17) -0.0128(18) C51 0.040(2) 0.028(2) 0.036(2) 0.0050(19) 0.0100(19) -0.0025(18) C61 0.0257(19) 0.027(2) 0.032(2) 0.0031(17) 0.0066(17) 0.0013(16) C12 0.0259(19) 0.0218(18) 0.020(2) 0.0003(15) 0.0020(15) -0.0028(15) C22 0.038(2) 0.027(2) 0.030(2) 0.0058(17) 0.0096(18) 0.0002(17) C32 0.052(3) 0.037(2) 0.026(2) 0.0119(19) 0.006(2) -0.008(2) C42 0.052(3) 0.054(3) 0.023(2) 0.002(2) 0.014(2) -0.015(2) C52 0.050(3) 0.051(3) 0.036(3) 0.003(2) 0.020(2) 0.010(2) C62 0.038(2) 0.041(2) 0.024(2) -0.0007(18) 0.0101(18) 0.0080(19) C15 0.032(2) 0.026(2) 0.030(2) 0.0086(17) 0.0106(17) 0.0153(16) C35 0.040(2) 0.052(3) 0.080(4) 0.029(3) 0.039(3) 0.030(2) C25 0.057(3) 0.041(3) 0.042(3) -0.001(2) 0.006(2) 0.029(2) C16 0.0203(17) 0.0259(19) 0.025(2) 0.0040(16) 0.0066(15) -0.0002(14) C36 0.030(2) 0.029(2) 0.036(2) 0.0097(18) 0.0128(17) -0.0005(16) C26 0.027(2) 0.038(2) 0.037(2) 0.0068(19) 0.0139(18) 0.0076(18) S3 0.0208(4) 0.0257(5) 0.0288(5) -0.0038(4) -0.0008(4) 0.0070(4) P3 0.0179(4) 0.0204(5) 0.0176(5) 0.0014(4) 0.0036(4) 0.0026(3) N2 0.0229(15) 0.0251(16) 0.0272(18) 0.0085(14) 0.0066(13) 0.0085(13) P4 0.0201(4) 0.0188(4) 0.0221(5) 0.0059(4) 0.0075(4) 0.0045(4) S4 0.0265(5) 0.0311(5) 0.0230(5) 0.0003(4) 0.0102(4) -0.0039(4) C13 0.0224(18) 0.031(2) 0.022(2) 0.0056(16) 0.0029(15) -0.0064(15) C23 0.055(3) 0.040(2) 0.035(3) 0.018(2) 0.017(2) 0.013(2) C33 0.071(4) 0.058(3) 0.049(3) 0.030(3) 0.017(3) 0.011(3) C43 0.073(4) 0.065(3) 0.023(2) 0.017(2) 0.005(2) -0.028(3) C53 0.061(3) 0.066(4) 0.027(3) -0.005(2) 0.022(2) -0.021(3) C63 0.047(3) 0.040(2) 0.033(2) 0.005(2) 0.021(2) -0.005(2) C14 0.0218(17) 0.0188(17) 0.0182(18) 0.0026(14) 0.0078(14) 0.0000(14) C24 0.0274(19) 0.026(2) 0.024(2) 0.0001(16) 0.0008(16) 0.0061(16) C34 0.044(2) 0.026(2) 0.033(2) 0.0015(17) 0.0011(19) 0.0099(18) C44 0.045(2) 0.022(2) 0.031(2) 0.0046(17) 0.0034(19) -0.0066(18) C54 0.028(2) 0.031(2) 0.036(2) 0.0034(18) 0.0056(17) -0.0036(17) C64 0.031(2) 0.024(2) 0.032(2) 0.0069(17) 0.0106(17) 0.0064(16) C17 0.0183(17) 0.0216(18) 0.032(2) 0.0117(16) 0.0079(15) 0.0002(14) C37 0.039(2) 0.036(2) 0.043(3) 0.022(2) 0.021(2) 0.0173(19) C27 0.031(2) 0.030(2) 0.039(2) 0.0157(18) 0.0190(18) 0.0067(16) C18 0.032(2) 0.031(2) 0.032(2) 0.0097(18) 0.0149(17) 0.0145(17) C38 0.031(2) 0.051(3) 0.050(3) 0.008(2) 0.000(2) 0.025(2) C28 0.054(3) 0.038(3) 0.078(4) 0.032(3) 0.031(3) 0.026(2) C1S 0.083(5) 0.055(4) 0.100(5) -0.010(4) -0.020(4) 0.020(3) Cl1S 0.1035(14) 0.0646(10) 0.1047(14) 0.0107(10) 0.0111(11) 0.0239(10) Cl2S 0.0832(11) 0.0856(11) 0.1077(14) 0.0297(10) 0.0165(10) 0.0419(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 S4 2.4348(10) . ? Mn1 S2 2.4394(10) . ? Mn1 S3 2.4515(10) . ? Mn1 S1 2.4578(10) . ? S1 P1 2.0142(12) . ? P1 N1 1.583(3) . ? P1 C12 1.815(4) . ? P1 C11 1.820(3) . ? N1 P2 1.590(3) . ? P2 C16 1.828(4) . ? P2 C15 1.829(4) . ? P2 S2 2.0286(13) . ? C11 C21 1.388(5) . ? C11 C61 1.389(5) . ? C21 C31 1.385(5) . ? C21 H21 0.9500 . ? C31 C41 1.393(6) . ? C31 H31 0.9500 . ? C41 C51 1.368(6) . ? C41 H41 0.9500 . ? C51 C61 1.398(5) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C12 C22 1.387(5) . ? C12 C62 1.401(5) . ? C22 C32 1.395(6) . ? C22 H22 0.9500 . ? C32 C42 1.371(7) . ? C32 H32 0.9500 . ? C42 C52 1.385(7) . ? C42 H42 0.9500 . ? C52 C62 1.365(6) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C15 C35 1.522(6) . ? C15 C25 1.527(6) . ? C15 H15 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C16 C26 1.538(5) . ? C16 C36 1.543(5) . ? C16 H16 1.0000 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? S3 P3 2.0156(12) . ? P3 N2 1.580(3) . ? P3 C13 1.812(4) . ? P3 C14 1.817(3) . ? N2 P4 1.593(3) . ? P4 C17 1.822(3) . ? P4 C18 1.836(4) . ? P4 S4 2.0269(13) . ? C13 C63 1.370(6) . ? C13 C23 1.396(6) . ? C23 C33 1.377(6) . ? C23 H23 0.9500 . ? C33 C43 1.353(8) . ? C33 H33 0.9500 . ? C43 C53 1.373(8) . ? C43 H43 0.9500 . ? C53 C63 1.394(6) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? C14 C64 1.382(5) . ? C14 C24 1.393(5) . ? C24 C34 1.395(5) . ? C24 H24 0.9500 . ? C34 C44 1.383(6) . ? C34 H34 0.9500 . ? C44 C54 1.382(6) . ? C44 H44 0.9500 . ? C54 C64 1.395(5) . ? C54 H54 0.9500 . ? C64 H64 0.9500 . ? C17 C27 1.536(5) . ? C17 C37 1.541(5) . ? C17 H17 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C18 C28 1.520(5) . ? C18 C38 1.526(6) . ? C18 H18 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C1S Cl2S 1.731(7) . ? C1S Cl1S 1.735(7) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? 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 S4 Mn1 S2 107.07(4) . . ? S4 Mn1 S3 109.22(4) . . ? S2 Mn1 S3 116.80(4) . . ? S4 Mn1 S1 117.01(4) . . ? S2 Mn1 S1 110.02(4) . . ? S3 Mn1 S1 96.91(3) . . ? P1 S1 Mn1 95.98(4) . . ? N1 P1 C12 106.46(17) . . ? N1 P1 C11 110.21(16) . . ? C12 P1 C11 103.52(16) . . ? N1 P1 S1 118.50(12) . . ? C12 P1 S1 108.23(13) . . ? C11 P1 S1 108.84(13) . . ? P1 N1 P2 140.8(2) . . ? N1 P2 C16 112.08(16) . . ? N1 P2 C15 104.60(17) . . ? C16 P2 C15 106.92(17) . . ? N1 P2 S2 116.96(12) . . ? C16 P2 S2 107.31(13) . . ? C15 P2 S2 108.48(13) . . ? P2 S2 Mn1 99.35(5) . . ? C21 C11 C61 120.0(3) . . ? C21 C11 P1 122.8(3) . . ? C61 C11 P1 117.2(3) . . ? C31 C21 C11 120.2(4) . . ? C31 C21 H21 119.9 . . ? C11 C21 H21 119.9 . . ? C21 C31 C41 119.4(4) . . ? C21 C31 H31 120.3 . . ? C41 C31 H31 120.3 . . ? C51 C41 C31 120.9(4) . . ? C51 C41 H41 119.5 . . ? C31 C41 H41 119.5 . . ? C41 C51 C61 119.7(4) . . ? C41 C51 H51 120.1 . . ? C61 C51 H51 120.1 . . ? C11 C61 C51 119.8(4) . . ? C11 C61 H61 120.1 . . ? C51 C61 H61 120.1 . . ? C22 C12 C62 120.1(4) . . ? C22 C12 P1 119.3(3) . . ? C62 C12 P1 120.6(3) . . ? C12 C22 C32 119.3(4) . . ? C12 C22 H22 120.3 . . ? C32 C22 H22 120.3 . . ? C42 C32 C22 120.7(4) . . ? C42 C32 H32 119.7 . . ? C22 C32 H32 119.7 . . ? C32 C42 C52 119.2(4) . . ? C32 C42 H42 120.4 . . ? C52 C42 H42 120.4 . . ? C62 C52 C42 121.7(5) . . ? C62 C52 H52 119.1 . . ? C42 C52 H52 119.1 . . ? C52 C62 C12 119.0(4) . . ? C52 C62 H62 120.5 . . ? C12 C62 H62 120.5 . . ? C35 C15 C25 111.9(4) . . ? C35 C15 P2 108.8(3) . . ? C25 C15 P2 110.6(3) . . ? C35 C15 H15 108.5 . . ? C25 C15 H15 108.5 . . ? P2 C15 H15 108.5 . . ? C15 C35 H35A 109.5 . . ? C15 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C15 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C15 C25 H25A 109.5 . . ? C15 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C15 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 C16 C36 110.2(3) . . ? C26 C16 P2 111.1(3) . . ? C36 C16 P2 111.5(2) . . ? C26 C16 H16 107.9 . . ? C36 C16 H16 107.9 . . ? P2 C16 H16 107.9 . . ? C16 C36 H36A 109.5 . . ? C16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C16 C26 H26A 109.5 . . ? C16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? P3 S3 Mn1 96.81(4) . . ? N2 P3 C13 106.62(17) . . ? N2 P3 C14 110.28(16) . . ? C13 P3 C14 104.23(17) . . ? N2 P3 S3 118.55(12) . . ? C13 P3 S3 107.69(12) . . ? C14 P3 S3 108.49(12) . . ? P3 N2 P4 141.2(2) . . ? N2 P4 C17 112.27(17) . . ? N2 P4 C18 105.12(17) . . ? C17 P4 C18 106.61(17) . . ? N2 P4 S4 117.29(12) . . ? C17 P4 S4 107.15(13) . . ? C18 P4 S4 107.83(14) . . ? P4 S4 Mn1 100.93(5) . . ? C63 C13 C23 118.8(4) . . ? C63 C13 P3 120.8(3) . . ? C23 C13 P3 120.3(3) . . ? C33 C23 C13 119.7(5) . . ? C33 C23 H23 120.1 . . ? C13 C23 H23 120.1 . . ? C43 C33 C23 121.3(5) . . ? C43 C33 H33 119.3 . . ? C23 C33 H33 119.3 . . ? C33 C43 C53 119.7(4) . . ? C33 C43 H43 120.2 . . ? C53 C43 H43 120.2 . . ? C43 C53 C63 119.9(5) . . ? C43 C53 H53 120.0 . . ? C63 C53 H53 120.0 . . ? C13 C63 C53 120.5(5) . . ? C13 C63 H63 119.8 . . ? C53 C63 H63 119.8 . . ? C64 C14 C24 119.8(3) . . ? C64 C14 P3 118.9(3) . . ? C24 C14 P3 121.2(3) . . ? C14 C24 C34 120.2(4) . . ? C14 C24 H24 119.9 . . ? C34 C24 H24 119.9 . . ? C44 C34 C24 119.5(4) . . ? C44 C34 H34 120.3 . . ? C24 C34 H34 120.3 . . ? C54 C44 C34 120.5(4) . . ? C54 C44 H44 119.7 . . ? C34 C44 H44 119.7 . . ? C44 C54 C64 120.0(4) . . ? C44 C54 H54 120.0 . . ? C64 C54 H54 120.0 . . ? C14 C64 C54 120.0(4) . . ? C14 C64 H64 120.0 . . ? C54 C64 H64 120.0 . . ? C27 C17 C37 110.8(3) . . ? C27 C17 P4 112.4(3) . . ? C37 C17 P4 110.8(2) . . ? C27 C17 H17 107.5 . . ? C37 C17 H17 107.5 . . ? P4 C17 H17 107.5 . . ? C17 C37 H37A 109.5 . . ? C17 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C17 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C17 C27 H27A 109.5 . . ? C17 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C17 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C28 C18 C38 110.7(4) . . ? C28 C18 P4 109.1(3) . . ? C38 C18 P4 111.5(3) . . ? C28 C18 H18 108.4 . . ? C38 C18 H18 108.4 . . ? P4 C18 H18 108.4 . . ? C18 C38 H38A 109.5 . . ? C18 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C18 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Cl2S C1S Cl1S 112.5(4) . . ? Cl2S C1S H1S1 109.1 . . ? Cl1S C1S H1S1 109.1 . . ? Cl2S C1S H1S2 109.1 . . ? Cl1S C1S H1S2 109.1 . . ? H1S1 C1S H1S2 107.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.485 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.074 # Attachment 'Mn[SPiPr2)2N]2.txt' data_ssmnl2 #(Complex 5) _database_code_depnum_ccdc_archive 'CCDC 293309' #Compound 5 in paper. #Checkcif output under refine special details. _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H56 Mn N2 P4 S4' _chemical_formula_sum 'C24 H56 Mn N2 P4 S4' _chemical_formula_weight 679.77 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' P P 0.1023 0.0942 '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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2500(3) _cell_length_b 12.7940(4) _cell_length_c 16.3400(5) _cell_angle_alpha 79.2030(10) _cell_angle_beta 78.1480(10) _cell_angle_gamma 69.0760(10) _cell_volume 1753.93(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7172 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 29 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 726 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.78 _exptl_absorpt_process_details 'SADABS 2004/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17062 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 28.88 _reflns_number_total 8180 _reflns_number_gt 7228 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'PLATON, ENCIFER, XCIF' _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. 063_ALERT_3_C Crystal Probably too Large for Beam Size ....... 0.71 mm Gorbitz has shown that use of a large crystal does not appear to matter. See C. H. Gorbitz Acta Cryst. (1999). B55, 1090-1098 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N1 Noted, no action taken 912_ALERT_3_A # Missing FCF Reflections Above STH/L=0.6 ...... 1006 911_ALERT_3_B # Missing FCF Refl. Between TH(Min) & STH/L=0.6 51 The data collection strategy used aimed to achieve a complete data set to 2\q = 50 deg. Some higher angle data were collected in the process and these have been included in the refinement. See completeness statistics below #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.999 3673 3671 2 23.01 0.550 0.997 4871 4854 17 25.24 0.600 0.992 6359 6308 51 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.975 8065 7867 198 28.88 0.679 0.886 9237 8180 1057 ; _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^)+(0.0470P)^2^+1.0297P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8180 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0443 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.87728(3) 0.16607(2) 0.248691(19) 0.01647(8) Uani 1 1 d . . . N2 N 1.21287(19) -0.10960(14) 0.24372(11) 0.0179(3) Uani 1 1 d . . . N1 N 0.54261(19) 0.44640(14) 0.25332(11) 0.0178(3) Uani 1 1 d . . . P1 P 0.70141(6) 0.46465(4) 0.20536(3) 0.01409(11) Uani 1 1 d . . . P3 P 1.20554(6) -0.05281(4) 0.32387(3) 0.01550(11) Uani 1 1 d . . . P2 P 0.48387(6) 0.34472(4) 0.30065(3) 0.01434(11) Uani 1 1 d . . . P4 P 1.12099(6) -0.08808(4) 0.16659(3) 0.01502(11) Uani 1 1 d . . . C11 C 0.6468(2) 0.58191(17) 0.12204(13) 0.0198(4) Uani 1 1 d . . . H11 H 0.5644 0.6463 0.1488 0.024 Uiso 1 1 calc R . . C21 C 0.7827(3) 0.6227(2) 0.07776(16) 0.0326(5) Uani 1 1 d . . . H21A H 0.8270 0.6432 0.1195 0.049 Uiso 1 1 calc R . . H21B H 0.7449 0.6887 0.0366 0.049 Uiso 1 1 calc R . . H21C H 0.8636 0.5623 0.0487 0.049 Uiso 1 1 calc R . . C31 C 0.5746(3) 0.5497(2) 0.05876(14) 0.0288(5) Uani 1 1 d . . . H31A H 0.4873 0.5244 0.0885 0.043 Uiso 1 1 calc R . . H31B H 0.6539 0.4887 0.0297 0.043 Uiso 1 1 calc R . . H31C H 0.5362 0.6154 0.0175 0.043 Uiso 1 1 calc R . . C12 C 0.7908(2) 0.51404(17) 0.27385(13) 0.0178(4) Uani 1 1 d . . . H12 H 0.8853 0.5291 0.2391 0.021 Uiso 1 1 calc R . . C22 C 0.8466(3) 0.42409(18) 0.34672(14) 0.0229(4) Uani 1 1 d . . . H22A H 0.9171 0.3544 0.3245 0.034 Uiso 1 1 calc R . . H22B H 0.7562 0.4095 0.3837 0.034 Uiso 1 1 calc R . . H22C H 0.9025 0.4505 0.3789 0.034 Uiso 1 1 calc R . . C32 C 0.6808(3) 0.62526(18) 0.30510(14) 0.0242(4) Uani 1 1 d . . . H32A H 0.6479 0.6812 0.2567 0.036 Uiso 1 1 calc R . . H32B H 0.7357 0.6529 0.3370 0.036 Uiso 1 1 calc R . . H32C H 0.5885 0.6129 0.3415 0.036 Uiso 1 1 calc R . . C13 C 0.3312(2) 0.40138(17) 0.38711(13) 0.0197(4) Uani 1 1 d . . . H13 H 0.2498 0.4680 0.3620 0.024 Uiso 1 1 calc R . . C23 C 0.2500(3) 0.3172(2) 0.43451(15) 0.0287(5) Uani 1 1 d . . . H23A H 0.2077 0.2917 0.3946 0.043 Uiso 1 1 calc R . . H23B H 0.1645 0.3539 0.4771 0.043 Uiso 1 1 calc R . . H23C H 0.3259 0.2523 0.4622 0.043 Uiso 1 1 calc R . . C33 C 0.3981(3) 0.4433(2) 0.44754(14) 0.0276(5) Uani 1 1 d . . . H33A H 0.4492 0.4970 0.4159 0.041 Uiso 1 1 calc R . . H33B H 0.4749 0.3792 0.4753 0.041 Uiso 1 1 calc R . . H33C H 0.3132 0.4806 0.4901 0.041 Uiso 1 1 calc R . . C14 C 0.3866(2) 0.30170(17) 0.23236(13) 0.0187(4) Uani 1 1 d . . . H14 H 0.3453 0.2421 0.2665 0.022 Uiso 1 1 calc R . . C24 C 0.5020(3) 0.24966(19) 0.15734(13) 0.0233(4) Uani 1 1 d . . . H24A H 0.5900 0.1873 0.1779 0.035 Uiso 1 1 calc R . . H24B H 0.5410 0.3071 0.1211 0.035 Uiso 1 1 calc R . . H24C H 0.4488 0.2212 0.1250 0.035 Uiso 1 1 calc R . . C34 C 0.2472(3) 0.3992(2) 0.20256(16) 0.0277(5) Uani 1 1 d . . . H34A H 0.1749 0.4310 0.2515 0.042 Uiso 1 1 calc R . . H34B H 0.1927 0.3714 0.1705 0.042 Uiso 1 1 calc R . . H34C H 0.2844 0.4577 0.1666 0.042 Uiso 1 1 calc R . . C15 C 1.1096(2) -0.11757(18) 0.41890(13) 0.0217(4) Uani 1 1 d . . . H15 H 1.1132 -0.0819 0.4676 0.026 Uiso 1 1 calc R . . C25 C 0.9373(3) -0.0944(2) 0.41431(15) 0.0274(5) Uani 1 1 d . . . H25A H 0.8843 -0.0129 0.4034 0.041 Uiso 1 1 calc R . . H25B H 0.8875 -0.1243 0.4679 0.041 Uiso 1 1 calc R . . H25C H 0.9298 -0.1313 0.3686 0.041 Uiso 1 1 calc R . . C35 C 1.1971(3) -0.24442(19) 0.43625(16) 0.0307(5) Uani 1 1 d . . . H35A H 1.3069 -0.2567 0.4392 0.046 Uiso 1 1 calc R . . H35B H 1.1919 -0.2825 0.3907 0.046 Uiso 1 1 calc R . . H35C H 1.1486 -0.2751 0.4899 0.046 Uiso 1 1 calc R . . C16 C 1.4080(2) -0.08738(17) 0.33997(14) 0.0205(4) Uani 1 1 d . . . H16 H 1.4539 -0.1715 0.3488 0.025 Uiso 1 1 calc R . . C26 C 1.4216(3) -0.0442(2) 0.41831(15) 0.0302(5) Uani 1 1 d . . . H26A H 1.3593 -0.0722 0.4677 0.045 Uiso 1 1 calc R . . H26B H 1.3828 0.0384 0.4107 0.045 Uiso 1 1 calc R . . H26C H 1.5316 -0.0712 0.4267 0.045 Uiso 1 1 calc R . . C36 C 1.5045(3) -0.0461(2) 0.26127(15) 0.0281(5) Uani 1 1 d . . . H36A H 1.4941 -0.0753 0.2122 0.042 Uiso 1 1 calc R . . H36B H 1.6148 -0.0731 0.2689 0.042 Uiso 1 1 calc R . . H36C H 1.4663 0.0365 0.2523 0.042 Uiso 1 1 calc R . . C17 C 1.1303(2) -0.22713(17) 0.14820(14) 0.0210(4) Uani 1 1 d . . . H17 H 1.2426 -0.2764 0.1440 0.025 Uiso 1 1 calc R . . C27 C 1.0742(3) -0.2247(2) 0.06582(16) 0.0333(5) Uani 1 1 d . . . H27A H 1.1345 -0.1909 0.0188 0.050 Uiso 1 1 calc R . . H27B H 0.9629 -0.1799 0.0690 0.050 Uiso 1 1 calc R . . H27C H 1.0895 -0.3019 0.0570 0.050 Uiso 1 1 calc R . . C37 C 1.0396(3) -0.27988(19) 0.22268(16) 0.0296(5) Uani 1 1 d . . . H37A H 1.0777 -0.2810 0.2746 0.044 Uiso 1 1 calc R . . H37B H 1.0546 -0.3572 0.2143 0.044 Uiso 1 1 calc R . . H37C H 0.9279 -0.2354 0.2270 0.044 Uiso 1 1 calc R . . C18 C 1.2215(2) -0.03113(18) 0.06980(13) 0.0201(4) Uani 1 1 d . . . H18 H 1.1600 -0.0215 0.0236 0.024 Uiso 1 1 calc R . . C28 C 1.2249(3) 0.08550(18) 0.07780(14) 0.0242(4) Uani 1 1 d . . . H28A H 1.1179 0.1355 0.0937 0.036 Uiso 1 1 calc R . . H28B H 1.2707 0.1172 0.0237 0.036 Uiso 1 1 calc R . . H28C H 1.2882 0.0783 0.1211 0.036 Uiso 1 1 calc R . . C38 C 1.3870(3) -0.1115(2) 0.04446(15) 0.0288(5) Uani 1 1 d . . . H38A H 1.3819 -0.1852 0.0395 0.043 Uiso 1 1 calc R . . H38B H 1.4516 -0.1202 0.0875 0.043 Uiso 1 1 calc R . . H38C H 1.4334 -0.0806 -0.0098 0.043 Uiso 1 1 calc R . . S1 S 0.87021(6) 0.33625(4) 0.14967(3) 0.01883(11) Uani 1 1 d . . . S2 S 0.64017(6) 0.20445(4) 0.35250(3) 0.01944(11) Uani 1 1 d . . . S3 S 1.10466(6) 0.11715(4) 0.31977(3) 0.02054(11) Uani 1 1 d . . . S4 S 0.89245(6) 0.01050(4) 0.17682(3) 0.01968(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01509(14) 0.01353(15) 0.01908(16) -0.00276(12) -0.00202(12) -0.00263(11) N2 0.0189(8) 0.0158(8) 0.0191(8) -0.0036(7) -0.0023(7) -0.0053(7) N1 0.0167(8) 0.0150(8) 0.0211(9) -0.0022(7) -0.0023(7) -0.0050(6) P1 0.0157(2) 0.0122(2) 0.0149(2) -0.00167(18) -0.00295(19) -0.00484(18) P3 0.0153(2) 0.0132(2) 0.0172(2) -0.00204(19) -0.00288(19) -0.00360(18) P2 0.0132(2) 0.0138(2) 0.0156(2) -0.00249(19) -0.00153(18) -0.00393(18) P4 0.0144(2) 0.0136(2) 0.0169(2) -0.00393(19) 0.00002(19) -0.00477(18) C11 0.0243(10) 0.0149(9) 0.0196(10) 0.0007(8) -0.0062(8) -0.0057(8) C21 0.0389(13) 0.0278(12) 0.0325(13) 0.0099(10) -0.0074(11) -0.0184(11) C31 0.0410(13) 0.0250(11) 0.0238(11) 0.0043(9) -0.0158(10) -0.0128(10) C12 0.0173(9) 0.0177(9) 0.0201(10) -0.0044(8) -0.0026(8) -0.0072(8) C22 0.0240(10) 0.0237(11) 0.0228(10) -0.0060(9) -0.0082(9) -0.0062(9) C32 0.0284(11) 0.0184(10) 0.0273(11) -0.0079(9) -0.0042(9) -0.0071(9) C13 0.0165(9) 0.0195(10) 0.0200(10) -0.0050(8) 0.0004(8) -0.0029(8) C23 0.0234(11) 0.0343(13) 0.0273(12) -0.0049(10) 0.0048(9) -0.0124(10) C33 0.0286(11) 0.0324(12) 0.0230(11) -0.0134(10) 0.0024(9) -0.0102(10) C14 0.0183(9) 0.0190(10) 0.0209(10) -0.0031(8) -0.0029(8) -0.0085(8) C24 0.0270(11) 0.0251(11) 0.0208(10) -0.0065(9) -0.0042(9) -0.0101(9) C34 0.0199(10) 0.0317(12) 0.0334(12) -0.0057(10) -0.0095(9) -0.0070(9) C15 0.0256(10) 0.0223(10) 0.0157(10) 0.0002(8) -0.0024(8) -0.0077(9) C25 0.0238(11) 0.0306(12) 0.0252(11) -0.0008(9) 0.0038(9) -0.0113(9) C35 0.0344(12) 0.0244(12) 0.0296(12) 0.0099(10) -0.0073(10) -0.0107(10) C16 0.0160(9) 0.0174(10) 0.0273(11) -0.0016(8) -0.0066(8) -0.0032(8) C26 0.0272(11) 0.0355(13) 0.0308(12) -0.0061(10) -0.0126(10) -0.0082(10) C36 0.0195(10) 0.0337(12) 0.0309(12) -0.0031(10) -0.0015(9) -0.0101(9) C17 0.0210(10) 0.0163(10) 0.0270(11) -0.0075(8) -0.0011(8) -0.0067(8) C27 0.0445(14) 0.0322(13) 0.0323(13) -0.0118(10) -0.0049(11) -0.0201(11) C37 0.0380(13) 0.0201(11) 0.0349(13) -0.0030(10) -0.0029(11) -0.0162(10) C18 0.0203(10) 0.0222(10) 0.0167(10) -0.0038(8) 0.0015(8) -0.0075(8) C28 0.0249(10) 0.0204(10) 0.0256(11) -0.0001(9) 0.0018(9) -0.0101(9) C38 0.0241(11) 0.0286(12) 0.0305(12) -0.0084(10) 0.0076(9) -0.0089(9) S1 0.0210(2) 0.0149(2) 0.0179(2) -0.00342(19) 0.00141(19) -0.00450(19) S2 0.0172(2) 0.0176(2) 0.0183(2) 0.00140(19) -0.00118(19) -0.00205(19) S3 0.0204(2) 0.0135(2) 0.0286(3) -0.0050(2) -0.0088(2) -0.00266(19) S4 0.0144(2) 0.0191(2) 0.0260(3) -0.0073(2) -0.00194(19) -0.00453(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 S2 2.4379(6) . ? Mn1 S3 2.4404(6) . ? Mn1 S4 2.4432(6) . ? Mn1 S1 2.4464(6) . ? N2 P4 1.5905(17) . ? N2 P3 1.5914(17) . ? N1 P1 1.5906(17) . ? N1 P2 1.5940(17) . ? P1 C11 1.826(2) . ? P1 C12 1.831(2) . ? P1 S1 2.0270(7) . ? P3 C16 1.827(2) . ? P3 C15 1.834(2) . ? P3 S3 2.0311(7) . ? P2 C13 1.830(2) . ? P2 C14 1.831(2) . ? P2 S2 2.0271(7) . ? P4 C17 1.828(2) . ? P4 C18 1.829(2) . ? P4 S4 2.0291(7) . ? C11 C31 1.525(3) . ? C11 C21 1.526(3) . ? C11 H11 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C12 C22 1.524(3) . ? C12 C32 1.531(3) . ? C12 H12 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C13 C33 1.527(3) . ? C13 C23 1.533(3) . ? C13 H13 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C14 C34 1.529(3) . ? C14 C24 1.532(3) . ? C14 H14 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C15 C25 1.528(3) . ? C15 C35 1.534(3) . ? C15 H15 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C16 C36 1.530(3) . ? C16 C26 1.530(3) . ? C16 H16 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C17 C37 1.523(3) . ? C17 C27 1.530(3) . ? C17 H17 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C18 C38 1.532(3) . ? C18 C28 1.534(3) . ? C18 H18 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? 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 S2 Mn1 S3 109.37(2) . . ? S2 Mn1 S4 108.16(2) . . ? S3 Mn1 S4 110.82(2) . . ? S2 Mn1 S1 109.59(2) . . ? S3 Mn1 S1 107.35(2) . . ? S4 Mn1 S1 111.53(2) . . ? P4 N2 P3 139.87(12) . . ? P1 N1 P2 138.20(11) . . ? N1 P1 C11 106.21(9) . . ? N1 P1 C12 111.04(9) . . ? C11 P1 C12 104.87(9) . . ? N1 P1 S1 119.08(7) . . ? C11 P1 S1 106.65(7) . . ? C12 P1 S1 107.99(7) . . ? N2 P3 C16 106.38(9) . . ? N2 P3 C15 110.65(10) . . ? C16 P3 C15 105.95(10) . . ? N2 P3 S3 118.36(7) . . ? C16 P3 S3 107.06(7) . . ? C15 P3 S3 107.71(7) . . ? N1 P2 C13 106.14(9) . . ? N1 P2 C14 110.88(9) . . ? C13 P2 C14 105.49(9) . . ? N1 P2 S2 118.65(7) . . ? C13 P2 S2 106.48(7) . . ? C14 P2 S2 108.31(7) . . ? N2 P4 C17 105.95(9) . . ? N2 P4 C18 111.29(9) . . ? C17 P4 C18 105.77(10) . . ? N2 P4 S4 119.14(7) . . ? C17 P4 S4 107.05(7) . . ? C18 P4 S4 106.82(7) . . ? C31 C11 C21 110.86(19) . . ? C31 C11 P1 109.99(14) . . ? C21 C11 P1 113.21(15) . . ? C31 C11 H11 107.5 . . ? C21 C11 H11 107.5 . . ? P1 C11 H11 107.5 . . ? C11 C21 H21A 109.5 . . ? C11 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C11 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C11 C31 H31A 109.5 . . ? C11 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C11 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C22 C12 C32 111.66(17) . . ? C22 C12 P1 111.66(14) . . ? C32 C12 P1 111.61(14) . . ? C22 C12 H12 107.2 . . ? C32 C12 H12 107.2 . . ? P1 C12 H12 107.2 . . ? C12 C22 H22A 109.5 . . ? C12 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C12 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C12 C32 H32A 109.5 . . ? C12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 C13 C23 110.89(18) . . ? C33 C13 P2 110.28(14) . . ? C23 C13 P2 113.10(15) . . ? C33 C13 H13 107.4 . . ? C23 C13 H13 107.4 . . ? P2 C13 H13 107.4 . . ? C13 C23 H23A 109.5 . . ? C13 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C13 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C13 C33 H33A 109.5 . . ? C13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C34 C14 C24 110.91(18) . . ? C34 C14 P2 111.91(15) . . ? C24 C14 P2 111.45(14) . . ? C34 C14 H14 107.4 . . ? C24 C14 H14 107.4 . . ? P2 C14 H14 107.4 . . ? C14 C24 H24A 109.5 . . ? C14 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C14 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14 C34 H34A 109.5 . . ? C14 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C14 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C25 C15 C35 111.24(19) . . ? C25 C15 P3 111.63(15) . . ? C35 C15 P3 111.51(15) . . ? C25 C15 H15 107.4 . . ? C35 C15 H15 107.4 . . ? P3 C15 H15 107.4 . . ? C15 C25 H25A 109.5 . . ? C15 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C15 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C15 C35 H35A 109.5 . . ? C15 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C15 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C36 C16 C26 111.20(18) . . ? C36 C16 P3 110.92(15) . . ? C26 C16 P3 113.15(15) . . ? C36 C16 H16 107.1 . . ? C26 C16 H16 107.1 . . ? P3 C16 H16 107.1 . . ? C16 C26 H26A 109.5 . . ? C16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C16 C36 H36A 109.5 . . ? C16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C37 C17 C27 110.82(18) . . ? C37 C17 P4 110.63(15) . . ? C27 C17 P4 112.95(15) . . ? C37 C17 H17 107.4 . . ? C27 C17 H17 107.4 . . ? P4 C17 H17 107.4 . . ? C17 C27 H27A 109.5 . . ? C17 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C17 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C17 C37 H37A 109.5 . . ? C17 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C17 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C38 C18 C28 110.92(17) . . ? C38 C18 P4 112.16(15) . . ? C28 C18 P4 110.97(14) . . ? C38 C18 H18 107.5 . . ? C28 C18 H18 107.5 . . ? P4 C18 H18 107.5 . . ? C18 C28 H28A 109.5 . . ? C18 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C18 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C18 C38 H38A 109.5 . . ? C18 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C18 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P1 S1 Mn1 105.60(3) . . ? P2 S2 Mn1 105.57(3) . . ? P3 S3 Mn1 105.56(3) . . ? P4 S4 Mn1 104.75(3) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.595 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.075 _chemical_compound_source 'Sarah Staniland' # Attachment 'Mn[SePPh2)2N]2.txt' data_sspk07 #(Complex 7) _database_code_depnum_ccdc_archive 'CCDC 293310' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H40 Mn N2 P4 Se4' _chemical_formula_sum 'C48 H40 Mn N2 P4 Se4' _chemical_formula_weight 1139.48 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7120(4) _cell_length_b 13.8534(4) _cell_length_c 14.1994(4) _cell_angle_alpha 65.773(2) _cell_angle_beta 82.480(2) _cell_angle_gamma 70.427(2) _cell_volume 2317.53(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6696 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 30.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1126 _exptl_absorpt_coefficient_mu 3.600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.58 _exptl_absorpt_process_details 'SADABS version 2004/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41532 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 30.53 _reflns_number_total 12970 _reflns_number_gt 10646 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'PLATON, XCIF, ENCIFER' _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. 165_ALERT_3_C Nr. of Status R Flagged Non-Hydrogen Atoms ..... 48 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.76 Ratio 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C12 No action taken 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.91 912_ALERT_3_A # Missing FCF Reflections Above STH/L=0.6 ...... 1178 911_ALERT_3_B # Missing FCF Refl. Between TH(Min) & STH/L=0.6 41 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 2 Noted see completeness stats below #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 0.993 4858 4824 34 23.01 0.550 0.994 6453 6416 37 25.24 0.600 0.995 8386 8343 43 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 0.994 10652 10593 59 29.84 0.700 0.946 13324 12611 713 30.53 0.715 0.914 14191 12970 1221 ; _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^)+(0.0369P)^2^+20.3487P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12970 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1760 _refine_ls_wR_factor_gt 0.1695 _refine_ls_goodness_of_fit_ref 1.203 _refine_ls_restrained_S_all 1.203 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.21710(7) 0.10504(7) 0.25416(7) 0.02169(19) Uani 1 1 d . . . N1 N 0.2421(4) -0.1762(4) 0.2481(4) 0.0214(10) Uani 1 1 d . . . N2 N 0.2302(4) 0.3729(4) 0.2665(4) 0.0203(10) Uani 1 1 d . . . P1 P 0.31580(11) -0.11601(12) 0.16552(12) 0.0179(3) Uani 1 1 d . . . P2 P 0.15674(11) -0.13724(12) 0.32334(11) 0.0173(3) Uani 1 1 d . . . P3 P 0.30745(11) 0.26068(12) 0.34187(11) 0.0175(3) Uani 1 1 d . . . P4 P 0.15404(11) 0.40785(12) 0.17471(11) 0.0173(3) Uani 1 1 d . . . Se1 Se 0.38403(5) -0.01368(5) 0.20046(5) 0.02581(15) Uani 1 1 d . . . Se2 Se 0.06171(5) 0.03641(5) 0.26629(5) 0.02398(14) Uani 1 1 d . . . Se3 Se 0.25445(5) 0.11536(5) 0.42122(5) 0.02270(14) Uani 1 1 d . . . Se4 Se 0.16869(5) 0.29215(5) 0.10292(5) 0.02307(14) Uani 1 1 d . . . C11 C 0.4226(3) -0.2287(3) 0.1490(3) 0.0221(12) Uani 1 1 d G . . C21 C 0.5032(3) -0.2051(3) 0.0828(3) 0.0329(15) Uani 1 1 d G . . H21 H 0.5023 -0.1300 0.0455 0.039 Uiso 1 1 calc R . . C31 C 0.5853(3) -0.2913(4) 0.0712(4) 0.043(2) Uani 1 1 d G . . H31 H 0.6405 -0.2751 0.0259 0.052 Uiso 1 1 calc R . . C41 C 0.5867(3) -0.4011(4) 0.1258(4) 0.043(2) Uani 1 1 d G . . H41 H 0.6428 -0.4600 0.1179 0.052 Uiso 1 1 calc R . . C51 C 0.5061(4) -0.4247(3) 0.1920(4) 0.0403(18) Uani 1 1 d G . . H51 H 0.5071 -0.4997 0.2293 0.048 Uiso 1 1 calc R . . C61 C 0.4240(3) -0.3385(3) 0.2036(3) 0.0282(13) Uani 1 1 d G . . H61 H 0.3689 -0.3546 0.2489 0.034 Uiso 1 1 calc R . . C12 C 0.2501(3) -0.0339(3) 0.0409(2) 0.0204(11) Uani 1 1 d G . . C22 C 0.2866(3) 0.0475(4) -0.0357(3) 0.0329(15) Uani 1 1 d G . . H22 H 0.3449 0.0626 -0.0224 0.039 Uiso 1 1 calc R . . C32 C 0.2377(4) 0.1067(4) -0.1316(3) 0.045(2) Uani 1 1 d G . . H32 H 0.2626 0.1623 -0.1840 0.054 Uiso 1 1 calc R . . C42 C 0.1524(4) 0.0846(4) -0.1510(3) 0.050(2) Uani 1 1 d G . . H42 H 0.1191 0.1250 -0.2166 0.060 Uiso 1 1 calc R . . C52 C 0.1160(3) 0.0032(4) -0.0745(4) 0.0420(19) Uani 1 1 d G . . H52 H 0.0577 -0.0119 -0.0877 0.050 Uiso 1 1 calc R . . C62 C 0.1648(3) -0.0560(4) 0.0215(3) 0.0302(14) Uani 1 1 d G . . H62 H 0.1399 -0.1116 0.0738 0.036 Uiso 1 1 calc R . . C13 C 0.2167(3) -0.1722(3) 0.4452(2) 0.0188(11) Uani 1 1 d G . . C23 C 0.3147(3) -0.2501(4) 0.4692(3) 0.0306(14) Uani 1 1 d G . . H23 H 0.3498 -0.2819 0.4215 0.037 Uiso 1 1 calc R . . C33 C 0.3612(3) -0.2814(4) 0.5630(3) 0.0370(16) Uani 1 1 d G . . H33 H 0.4282 -0.3347 0.5794 0.044 Uiso 1 1 calc R . . C43 C 0.3098(3) -0.2348(4) 0.6328(3) 0.0375(17) Uani 1 1 d G . . H43 H 0.3417 -0.2562 0.6969 0.045 Uiso 1 1 calc R . . C53 C 0.2119(3) -0.1569(4) 0.6087(3) 0.0319(15) Uani 1 1 d G . . H53 H 0.1767 -0.1251 0.6564 0.038 Uiso 1 1 calc R . . C63 C 0.1653(3) -0.1256(3) 0.5150(3) 0.0267(13) Uani 1 1 d G . . H63 H 0.0983 -0.0723 0.4985 0.032 Uiso 1 1 calc R . . C14 C 0.0739(3) -0.2243(3) 0.3538(3) 0.0190(11) Uani 1 1 d G . . C24 C 0.1059(3) -0.3151(4) 0.3256(4) 0.0306(14) Uani 1 1 d G . . H24 H 0.1691 -0.3294 0.2897 0.037 Uiso 1 1 calc R . . C34 C 0.0455(4) -0.3850(3) 0.3501(4) 0.0374(17) Uani 1 1 d G . . H34 H 0.0674 -0.4471 0.3308 0.045 Uiso 1 1 calc R . . C44 C -0.0469(3) -0.3641(3) 0.4026(4) 0.0329(15) Uani 1 1 d G . . H44 H -0.0882 -0.4119 0.4193 0.040 Uiso 1 1 calc R . . C54 C -0.0790(3) -0.2733(4) 0.4308(3) 0.0307(14) Uani 1 1 d G . . H54 H -0.1421 -0.2590 0.4668 0.037 Uiso 1 1 calc R . . C64 C -0.0185(3) -0.2034(3) 0.4064(3) 0.0259(13) Uani 1 1 d G . . H64 H -0.0404 -0.1413 0.4256 0.031 Uiso 1 1 calc R . . C15 C 0.4277(3) 0.2190(3) 0.2762(3) 0.0197(11) Uani 1 1 d G . . C25 C 0.4502(3) 0.2960(3) 0.1833(3) 0.0281(14) Uani 1 1 d G . . H25 H 0.4044 0.3701 0.1561 0.034 Uiso 1 1 calc R . . C35 C 0.5396(3) 0.2646(3) 0.1301(3) 0.0334(15) Uani 1 1 d G . . H35 H 0.5549 0.3172 0.0666 0.040 Uiso 1 1 calc R . . C45 C 0.6064(3) 0.1562(4) 0.1698(3) 0.0294(14) Uani 1 1 d G . . H45 H 0.6675 0.1347 0.1335 0.035 Uiso 1 1 calc R . . C55 C 0.5839(3) 0.0792(3) 0.2627(3) 0.0355(16) Uani 1 1 d G . . H55 H 0.6296 0.0051 0.2898 0.043 Uiso 1 1 calc R . . C65 C 0.4945(3) 0.1106(3) 0.3159(3) 0.0297(14) Uani 1 1 d G . . H65 H 0.4792 0.0580 0.3794 0.036 Uiso 1 1 calc R . . C16 C 0.3410(3) 0.2974(3) 0.4397(3) 0.0198(11) Uani 1 1 d G . . C26 C 0.3917(4) 0.2153(3) 0.5302(3) 0.0340(16) Uani 1 1 d G . . H26 H 0.4073 0.1389 0.5424 0.041 Uiso 1 1 calc R . . C36 C 0.4197(4) 0.2449(4) 0.6027(3) 0.0404(18) Uani 1 1 d G . . H36 H 0.4544 0.1888 0.6645 0.048 Uiso 1 1 calc R . . C46 C 0.3969(4) 0.3567(4) 0.5848(4) 0.0417(19) Uani 1 1 d G . . H46 H 0.4160 0.3769 0.6343 0.050 Uiso 1 1 calc R . . C56 C 0.3462(4) 0.4388(3) 0.4943(4) 0.047(2) Uani 1 1 d G . . H56 H 0.3306 0.5151 0.4821 0.057 Uiso 1 1 calc R . . C66 C 0.3182(4) 0.4091(3) 0.4218(3) 0.0356(16) Uani 1 1 d G . . H66 H 0.2835 0.4653 0.3600 0.043 Uiso 1 1 calc R . . C17 C 0.1709(3) 0.5324(3) 0.0724(3) 0.0200(11) Uani 1 1 d G . . C27 C 0.2254(3) 0.5913(3) 0.0911(2) 0.0240(12) Uani 1 1 d G . . H27 H 0.2562 0.5644 0.1568 0.029 Uiso 1 1 calc R . . C37 C 0.2348(4) 0.6895(3) 0.0134(3) 0.0320(15) Uani 1 1 d G . . H37 H 0.2721 0.7298 0.0261 0.038 Uiso 1 1 calc R . . C47 C 0.1897(4) 0.7288(3) -0.0828(3) 0.0349(16) Uani 1 1 d G . . H47 H 0.1961 0.7959 -0.1359 0.042 Uiso 1 1 calc R . . C57 C 0.1352(4) 0.6699(4) -0.1015(2) 0.0314(15) Uani 1 1 d G . . H57 H 0.1043 0.6967 -0.1672 0.038 Uiso 1 1 calc R . . C67 C 0.1257(3) 0.5717(3) -0.0238(3) 0.0268(13) Uani 1 1 d G . . H67 H 0.0885 0.5314 -0.0365 0.032 Uiso 1 1 calc R . . C18 C 0.0220(2) 0.4473(3) 0.2196(3) 0.0182(11) Uani 1 1 d G . . C28 C -0.0497(3) 0.5502(3) 0.1674(3) 0.0253(12) Uani 1 1 d G . . H28 H -0.0294 0.6037 0.1079 0.030 Uiso 1 1 calc R . . C38 C -0.1510(3) 0.5748(3) 0.2022(3) 0.0330(15) Uani 1 1 d G . . H38 H -0.2000 0.6451 0.1665 0.040 Uiso 1 1 calc R . . C48 C -0.1807(2) 0.4965(4) 0.2892(4) 0.0374(17) Uani 1 1 d G . . H48 H -0.2499 0.5133 0.3129 0.045 Uiso 1 1 calc R . . C58 C -0.1090(3) 0.3936(3) 0.3414(3) 0.0371(17) Uani 1 1 d G . . H58 H -0.1293 0.3401 0.4008 0.045 Uiso 1 1 calc R . . C68 C -0.0077(3) 0.3690(3) 0.3066(3) 0.0306(14) Uani 1 1 d G . . H68 H 0.0413 0.2987 0.3423 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0244(5) 0.0173(4) 0.0242(5) -0.0090(4) -0.0018(4) -0.0057(3) N1 0.020(2) 0.024(2) 0.020(2) -0.009(2) 0.0037(19) -0.007(2) N2 0.018(2) 0.018(2) 0.023(2) -0.0058(19) -0.0060(19) -0.0022(18) P1 0.0168(7) 0.0194(7) 0.0188(7) -0.0089(6) -0.0001(5) -0.0054(5) P2 0.0171(7) 0.0162(6) 0.0178(7) -0.0068(5) 0.0001(5) -0.0042(5) P3 0.0178(7) 0.0152(6) 0.0174(7) -0.0050(5) -0.0031(5) -0.0029(5) P4 0.0169(7) 0.0154(6) 0.0179(7) -0.0045(5) -0.0031(5) -0.0043(5) Se1 0.0213(3) 0.0260(3) 0.0358(4) -0.0175(3) -0.0017(3) -0.0067(2) Se2 0.0195(3) 0.0171(3) 0.0311(3) -0.0068(2) -0.0035(2) -0.0026(2) Se3 0.0276(3) 0.0189(3) 0.0212(3) -0.0063(2) 0.0013(2) -0.0091(2) Se4 0.0281(3) 0.0196(3) 0.0211(3) -0.0083(2) -0.0017(2) -0.0059(2) C11 0.019(3) 0.024(3) 0.024(3) -0.013(2) -0.004(2) -0.002(2) C21 0.024(3) 0.038(4) 0.036(4) -0.017(3) 0.002(3) -0.007(3) C31 0.020(3) 0.068(6) 0.053(5) -0.041(5) 0.007(3) -0.008(3) C41 0.021(3) 0.053(5) 0.054(5) -0.037(4) -0.010(3) 0.014(3) C51 0.040(4) 0.029(4) 0.045(4) -0.018(3) -0.015(3) 0.008(3) C61 0.032(3) 0.023(3) 0.027(3) -0.011(3) -0.001(3) -0.003(3) C12 0.017(3) 0.022(3) 0.019(3) -0.008(2) 0.000(2) -0.002(2) C22 0.042(4) 0.029(3) 0.023(3) -0.005(3) -0.004(3) -0.012(3) C32 0.059(5) 0.029(4) 0.029(4) 0.000(3) -0.005(4) -0.004(4) C42 0.052(5) 0.050(5) 0.022(3) -0.006(3) -0.015(3) 0.013(4) C52 0.027(4) 0.060(5) 0.038(4) -0.024(4) -0.013(3) -0.001(3) C62 0.021(3) 0.041(4) 0.027(3) -0.017(3) -0.001(2) -0.004(3) C13 0.020(3) 0.022(3) 0.017(3) -0.007(2) -0.001(2) -0.009(2) C23 0.023(3) 0.037(4) 0.031(3) -0.016(3) -0.001(3) -0.005(3) C33 0.027(3) 0.044(4) 0.036(4) -0.016(3) -0.007(3) -0.003(3) C43 0.041(4) 0.047(4) 0.029(4) -0.014(3) -0.009(3) -0.017(3) C53 0.041(4) 0.035(4) 0.025(3) -0.017(3) 0.004(3) -0.013(3) C63 0.027(3) 0.025(3) 0.029(3) -0.015(3) 0.000(3) -0.004(2) C14 0.019(3) 0.018(2) 0.020(3) -0.008(2) -0.001(2) -0.005(2) C24 0.031(3) 0.032(3) 0.037(4) -0.021(3) 0.007(3) -0.013(3) C34 0.041(4) 0.031(4) 0.058(5) -0.032(4) 0.005(4) -0.016(3) C44 0.040(4) 0.035(4) 0.032(4) -0.012(3) -0.004(3) -0.021(3) C54 0.029(3) 0.040(4) 0.031(3) -0.016(3) 0.008(3) -0.021(3) C64 0.027(3) 0.031(3) 0.025(3) -0.016(3) 0.004(2) -0.012(3) C15 0.020(3) 0.021(3) 0.019(3) -0.007(2) -0.001(2) -0.008(2) C25 0.023(3) 0.028(3) 0.022(3) 0.000(2) -0.002(2) -0.005(2) C35 0.031(4) 0.042(4) 0.022(3) -0.007(3) 0.004(3) -0.013(3) C45 0.024(3) 0.038(4) 0.033(3) -0.020(3) 0.005(3) -0.013(3) C55 0.032(4) 0.025(3) 0.047(4) -0.016(3) 0.006(3) -0.005(3) C65 0.029(3) 0.019(3) 0.031(3) -0.006(3) 0.003(3) -0.001(2) C16 0.014(3) 0.021(3) 0.022(3) -0.009(2) -0.002(2) -0.002(2) C26 0.035(4) 0.033(4) 0.027(3) -0.010(3) -0.011(3) 0.001(3) C36 0.039(4) 0.049(5) 0.029(4) -0.015(3) -0.015(3) -0.003(3) C46 0.031(4) 0.063(5) 0.041(4) -0.038(4) -0.009(3) -0.002(4) C56 0.063(6) 0.036(4) 0.053(5) -0.030(4) -0.011(4) -0.009(4) C66 0.048(4) 0.022(3) 0.036(4) -0.013(3) -0.014(3) -0.003(3) C17 0.016(3) 0.017(2) 0.024(3) -0.006(2) 0.001(2) -0.005(2) C27 0.029(3) 0.023(3) 0.021(3) -0.008(2) -0.007(2) -0.008(2) C37 0.035(4) 0.029(3) 0.031(3) -0.004(3) -0.006(3) -0.017(3) C47 0.044(4) 0.031(3) 0.029(3) -0.001(3) -0.002(3) -0.023(3) C57 0.039(4) 0.032(3) 0.020(3) -0.001(3) -0.007(3) -0.016(3) C67 0.029(3) 0.029(3) 0.023(3) -0.006(3) -0.007(2) -0.013(3) C18 0.017(3) 0.021(3) 0.018(3) -0.008(2) -0.003(2) -0.005(2) C28 0.024(3) 0.025(3) 0.023(3) -0.008(2) -0.005(2) -0.003(2) C38 0.026(3) 0.034(4) 0.030(3) -0.013(3) -0.008(3) 0.005(3) C48 0.021(3) 0.051(5) 0.039(4) -0.022(4) 0.008(3) -0.007(3) C58 0.027(3) 0.043(4) 0.033(4) -0.008(3) 0.007(3) -0.012(3) C68 0.029(3) 0.026(3) 0.029(3) -0.006(3) 0.000(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 Se4 2.5344(11) . ? Mn1 Se3 2.5603(11) . ? Mn1 Se1 2.5643(11) . ? Mn1 Se2 2.5691(11) . ? N1 P2 1.589(5) . ? N1 P1 1.595(5) . ? N2 P3 1.585(5) . ? N2 P4 1.589(5) . ? P1 C12 1.821(3) . ? P1 C11 1.821(3) . ? P1 Se1 2.1721(16) . ? P2 C14 1.814(3) . ? P2 C13 1.823(3) . ? P2 Se2 2.1721(15) . ? P3 C16 1.818(3) . ? P3 C15 1.823(3) . ? P3 Se3 2.1804(16) . ? P4 C17 1.806(3) . ? P4 C18 1.818(3) . ? P4 Se4 2.1727(16) . ? C11 C21 1.3900 . ? C11 C61 1.3900 . ? C21 C31 1.3900 . ? C21 H21 0.9500 . ? C31 C41 1.3900 . ? C31 H31 0.9500 . ? C41 C51 1.3900 . ? C41 H41 0.9500 . ? C51 C61 1.3900 . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C12 C22 1.3900 . ? C12 C62 1.3900 . ? C22 C32 1.3900 . ? C22 H22 0.9500 . ? C32 C42 1.3900 . ? C32 H32 0.9500 . ? C42 C52 1.3900 . ? C42 H42 0.9500 . ? C52 C62 1.3900 . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C13 C23 1.3900 . ? C13 C63 1.3900 . ? C23 C33 1.3900 . ? C23 H23 0.9500 . ? C33 C43 1.3900 . ? C33 H33 0.9500 . ? C43 C53 1.3900 . ? C43 H43 0.9500 . ? C53 C63 1.3900 . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? C14 C24 1.3900 . ? C14 C64 1.3900 . ? C24 C34 1.3900 . ? C24 H24 0.9500 . ? C34 C44 1.3900 . ? C34 H34 0.9500 . ? C44 C54 1.3900 . ? C44 H44 0.9500 . ? C54 C64 1.3900 . ? C54 H54 0.9500 . ? C64 H64 0.9500 . ? C15 C25 1.3900 . ? C15 C65 1.3900 . ? C25 C35 1.3900 . ? C25 H25 0.9500 . ? C35 C45 1.3900 . ? C35 H35 0.9500 . ? C45 C55 1.3900 . ? C45 H45 0.9500 . ? C55 C65 1.3900 . ? C55 H55 0.9500 . ? C65 H65 0.9500 . ? C16 C26 1.3900 . ? C16 C66 1.3900 . ? C26 C36 1.3900 . ? C26 H26 0.9500 . ? C36 C46 1.3900 . ? C36 H36 0.9500 . ? C46 C56 1.3900 . ? C46 H46 0.9500 . ? C56 C66 1.3900 . ? C56 H56 0.9500 . ? C66 H66 0.9500 . ? C17 C27 1.3900 . ? C17 C67 1.3900 . ? C27 C37 1.3900 . ? C27 H27 0.9500 . ? C37 C47 1.3900 . ? C37 H37 0.9500 . ? C47 C57 1.3900 . ? C47 H47 0.9500 . ? C57 C67 1.3900 . ? C57 H57 0.9500 . ? C67 H67 0.9500 . ? C18 C28 1.3900 . ? C18 C68 1.3900 . ? C28 C38 1.3900 . ? C28 H28 0.9500 . ? C38 C48 1.3900 . ? C38 H38 0.9500 . ? C48 C58 1.3900 . ? C48 H48 0.9500 . ? C58 C68 1.3900 . ? C58 H58 0.9500 . ? C68 H68 0.9500 . ? 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 Se4 Mn1 Se3 113.65(4) . . ? Se4 Mn1 Se1 105.44(4) . . ? Se3 Mn1 Se1 108.01(4) . . ? Se4 Mn1 Se2 102.90(4) . . ? Se3 Mn1 Se2 113.75(4) . . ? Se1 Mn1 Se2 112.81(4) . . ? P2 N1 P1 132.2(3) . . ? P3 N2 P4 136.3(3) . . ? N1 P1 C12 110.1(2) . . ? N1 P1 C11 104.9(2) . . ? C12 P1 C11 106.4(2) . . ? N1 P1 Se1 119.3(2) . . ? C12 P1 Se1 108.44(15) . . ? C11 P1 Se1 106.77(15) . . ? N1 P2 C14 105.1(2) . . ? N1 P2 C13 109.9(2) . . ? C14 P2 C13 105.8(2) . . ? N1 P2 Se2 117.6(2) . . ? C14 P2 Se2 109.04(15) . . ? C13 P2 Se2 108.80(14) . . ? N2 P3 C16 104.4(2) . . ? N2 P3 C15 110.8(2) . . ? C16 P3 C15 106.1(2) . . ? N2 P3 Se3 119.1(2) . . ? C16 P3 Se3 107.67(15) . . ? C15 P3 Se3 107.91(14) . . ? N2 P4 C17 107.6(2) . . ? N2 P4 C18 108.1(2) . . ? C17 P4 C18 106.21(19) . . ? N2 P4 Se4 119.42(19) . . ? C17 P4 Se4 106.01(15) . . ? C18 P4 Se4 108.76(15) . . ? P1 Se1 Mn1 97.43(5) . . ? P2 Se2 Mn1 92.77(5) . . ? P3 Se3 Mn1 94.22(5) . . ? P4 Se4 Mn1 102.67(5) . . ? C21 C11 C61 120.0 . . ? C21 C11 P1 120.1(2) . . ? C61 C11 P1 119.9(2) . . ? C31 C21 C11 120.0 . . ? C31 C21 H21 120.0 . . ? C11 C21 H21 120.0 . . ? C21 C31 C41 120.0 . . ? C21 C31 H31 120.0 . . ? C41 C31 H31 120.0 . . ? C31 C41 C51 120.0 . . ? C31 C41 H41 120.0 . . ? C51 C41 H41 120.0 . . ? C61 C51 C41 120.0 . . ? C61 C51 H51 120.0 . . ? C41 C51 H51 120.0 . . ? C51 C61 C11 120.0 . . ? C51 C61 H61 120.0 . . ? C11 C61 H61 120.0 . . ? C22 C12 C62 120.0 . . ? C22 C12 P1 120.7(2) . . ? C62 C12 P1 119.2(2) . . ? C32 C22 C12 120.0 . . ? C32 C22 H22 120.0 . . ? C12 C22 H22 120.0 . . ? C22 C32 C42 120.0 . . ? C22 C32 H32 120.0 . . ? C42 C32 H32 120.0 . . ? C52 C42 C32 120.0 . . ? C52 C42 H42 120.0 . . ? C32 C42 H42 120.0 . . ? C42 C52 C62 120.0 . . ? C42 C52 H52 120.0 . . ? C62 C52 H52 120.0 . . ? C52 C62 C12 120.0 . . ? C52 C62 H62 120.0 . . ? C12 C62 H62 120.0 . . ? C23 C13 C63 120.0 . . ? C23 C13 P2 118.5(2) . . ? C63 C13 P2 121.5(2) . . ? C13 C23 C33 120.0 . . ? C13 C23 H23 120.0 . . ? C33 C23 H23 120.0 . . ? C43 C33 C23 120.0 . . ? C43 C33 H33 120.0 . . ? C23 C33 H33 120.0 . . ? C33 C43 C53 120.0 . . ? C33 C43 H43 120.0 . . ? C53 C43 H43 120.0 . . ? C43 C53 C63 120.0 . . ? C43 C53 H53 120.0 . . ? C63 C53 H53 120.0 . . ? C53 C63 C13 120.0 . . ? C53 C63 H63 120.0 . . ? C13 C63 H63 120.0 . . ? C24 C14 C64 120.0 . . ? C24 C14 P2 118.6(2) . . ? C64 C14 P2 121.4(2) . . ? C14 C24 C34 120.0 . . ? C14 C24 H24 120.0 . . ? C34 C24 H24 120.0 . . ? C44 C34 C24 120.0 . . ? C44 C34 H34 120.0 . . ? C24 C34 H34 120.0 . . ? C54 C44 C34 120.0 . . ? C54 C44 H44 120.0 . . ? C34 C44 H44 120.0 . . ? C44 C54 C64 120.0 . . ? C44 C54 H54 120.0 . . ? C64 C54 H54 120.0 . . ? C54 C64 C14 120.0 . . ? C54 C64 H64 120.0 . . ? C14 C64 H64 120.0 . . ? C25 C15 C65 120.0 . . ? C25 C15 P3 119.2(2) . . ? C65 C15 P3 120.8(2) . . ? C35 C25 C15 120.0 . . ? C35 C25 H25 120.0 . . ? C15 C25 H25 120.0 . . ? C25 C35 C45 120.0 . . ? C25 C35 H35 120.0 . . ? C45 C35 H35 120.0 . . ? C55 C45 C35 120.0 . . ? C55 C45 H45 120.0 . . ? C35 C45 H45 120.0 . . ? C45 C55 C65 120.0 . . ? C45 C55 H55 120.0 . . ? C65 C55 H55 120.0 . . ? C55 C65 C15 120.0 . . ? C55 C65 H65 120.0 . . ? C15 C65 H65 120.0 . . ? C26 C16 C66 120.0 . . ? C26 C16 P3 120.8(2) . . ? C66 C16 P3 119.2(2) . . ? C36 C26 C16 120.0 . . ? C36 C26 H26 120.0 . . ? C16 C26 H26 120.0 . . ? C26 C36 C46 120.0 . . ? C26 C36 H36 120.0 . . ? C46 C36 H36 120.0 . . ? C56 C46 C36 120.0 . . ? C56 C46 H46 120.0 . . ? C36 C46 H46 120.0 . . ? C46 C56 C66 120.0 . . ? C46 C56 H56 120.0 . . ? C66 C56 H56 120.0 . . ? C56 C66 C16 120.0 . . ? C56 C66 H66 120.0 . . ? C16 C66 H66 120.0 . . ? C27 C17 C67 120.0 . . ? C27 C17 P4 120.1(2) . . ? C67 C17 P4 119.9(2) . . ? C37 C27 C17 120.0 . . ? C37 C27 H27 120.0 . . ? C17 C27 H27 120.0 . . ? C27 C37 C47 120.0 . . ? C27 C37 H37 120.0 . . ? C47 C37 H37 120.0 . . ? C37 C47 C57 120.0 . . ? C37 C47 H47 120.0 . . ? C57 C47 H47 120.0 . . ? C67 C57 C47 120.0 . . ? C67 C57 H57 120.0 . . ? C47 C57 H57 120.0 . . ? C57 C67 C17 120.0 . . ? C57 C67 H67 120.0 . . ? C17 C67 H67 120.0 . . ? C28 C18 C68 120.0 . . ? C28 C18 P4 122.1(2) . . ? C68 C18 P4 117.9(2) . . ? C38 C28 C18 120.0 . . ? C38 C28 H28 120.0 . . ? C18 C28 H28 120.0 . . ? C48 C38 C28 120.0 . . ? C48 C38 H38 120.0 . . ? C28 C38 H38 120.0 . . ? C38 C48 C58 120.0 . . ? C38 C48 H48 120.0 . . ? C58 C48 H48 120.0 . . ? C48 C58 C68 120.0 . . ? C48 C58 H58 120.0 . . ? C68 C58 H58 120.0 . . ? C58 C68 C18 120.0 . . ? C58 C68 H68 120.0 . . ? C18 C68 H68 120.0 . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.914 _refine_diff_density_max 1.334 _refine_diff_density_min -0.750 _refine_diff_density_rms 0.178