# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Cheng Wang' _publ_contact_author_address ; Changchun Institute of Applied Chemistry Changchun Jilin 130022 CHINA ; _publ_contact_author_email CWANG@CIAC.JL.CN _publ_section_title ;Preparation of one dimensional Group 14 metal sulfides: Different roles of metal-amino complexes ; loop_ _publ_author_name 'Cheng Wang.' 'Yanfeng Bi.' 'Zhenqing Wang.' 'Gong-Feng Xu.' # Attachment 'crystal.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 746742' #TrackingRef 'crystal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H34 Ge3 Mn3 N8 O S9' _chemical_formula_sum 'C8 H34 Ge3 Mn3 N8 O S9' _chemical_formula_weight 929.56 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' N N 0.0061 0.0033 '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' Ge Ge 0.1547 1.8001 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/m ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.4001(4) _cell_length_b 19.4843(9) _cell_length_c 10.4745(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.2160(10) _cell_angle_gamma 90.00 _cell_volume 1506.19(13) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4497 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 26.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 2.050 _exptl_crystal_density_diffrn 2.050 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 922 _exptl_absorpt_coefficient_mu 4.819 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8117 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2736 _reflns_number_gt 2324 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.6891P] 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 2736 _refine_ls_number_parameters 152 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.50283(9) 0.7500 0.04860(7) 0.02449(18) Uani 1 2 d S . . Mn2 Mn 0.4997(2) 0.52178(6) -0.01294(15) 0.0431(4) Uani 0.50 1 d P . . Mn3 Mn 0.22388(12) 0.7500 -0.50384(9) 0.0400(2) Uani 1 2 d S . . Ge1 Ge 0.99480(6) 0.7500 0.07752(5) 0.02162(14) Uani 1 2 d S . . Ge2 Ge 0.75284(5) 0.654197(18) -0.18687(3) 0.02414(12) Uani 1 1 d . . . S1 S 0.74855(17) 0.7500 -0.30642(11) 0.0266(3) Uani 1 2 d S . . S2 S 1.00277(11) 0.65703(4) -0.04857(8) 0.0271(2) Uani 1 1 d . . . S3 S 0.76953(16) 0.7500 0.20131(11) 0.0280(3) Uani 1 2 d S . . S4 S 0.50493(12) 0.64619(5) -0.08387(9) 0.0308(2) Uani 1 1 d . . . S5 S 1.25616(16) 0.7500 0.19174(11) 0.0322(3) Uani 1 2 d S . . S6 S 0.78976(15) 0.57356(5) -0.31987(9) 0.0417(3) Uani 1 1 d . . . O1 O 0.2347(6) 0.7500 -0.2948(4) 0.0644(13) Uani 1 2 d S . . N1 N 0.4757(5) 0.54358(19) 0.1905(3) 0.0536(10) Uani 1 1 d . . . H1A H 0.4173 0.5082 0.2242 0.064 Uiso 1 1 d R . . H1B H 0.4107 0.5819 0.2016 0.064 Uiso 1 1 d R . . N2 N 0.2159(2) 0.49643(9) -0.06113(17) 0.0497(9) Uani 1 1 d . . . H2A H 0.1380 0.5276 -0.0333 0.060 Uiso 1 1 d R . . H2B H 0.1894 0.4544 -0.0319 0.060 Uiso 1 1 d R . . N3 N 0.4154(2) 0.66150(9) -0.52811(17) 0.0452(9) Uani 1 1 d R . . H3C H 0.4532 0.6609 -0.6078 0.054 Uiso 1 1 calc R . . H3D H 0.5127 0.6645 -0.4716 0.054 Uiso 1 1 calc R . . N4 N 0.0291(2) 0.66555(9) -0.54630(17) 0.0383(8) Uani 1 1 d R . . H4C H -0.0345 0.6576 -0.4778 0.046 Uiso 1 1 calc R . . H4D H -0.0492 0.6773 -0.6125 0.046 Uiso 1 1 calc R . . C1 C 0.6574(2) 0.54976(9) 0.25517(17) 0.0859(19) Uani 1 1 d R . . H1C H 0.6474 0.5441 0.3454 0.103 Uiso 1 1 d R . . H1D H 0.7035 0.5950 0.2410 0.103 Uiso 1 1 d R . . C2 C 0.2246(2) 0.49809(9) -0.21329(17) 0.0598(19) Uani 0.570(7) 1 d PRU . . H2C H 0.2614 0.5430 -0.2389 0.072 Uiso 0.570(7) 1 d PR . . H2D H 0.1060 0.4894 -0.2534 0.072 Uiso 0.570(7) 1 d PR . . C2' C 0.1889(16) 0.4572(6) -0.1743(11) 0.0598(19) Uani 0.430(7) 1 d P . . H2'A H 0.0839 0.4725 -0.2258 0.072 Uiso 0.430(7) 1 d PR . . H2'B H 0.1656 0.4115 -0.1460 0.072 Uiso 0.430(7) 1 d PR . . C3 C 0.3087(7) 0.6000(2) -0.5043(4) 0.0572(13) Uani 1 1 d . . . H3A H 0.2913 0.5966 -0.4136 0.069 Uiso 1 1 calc R . . H3B H 0.3740 0.5595 -0.5290 0.069 Uiso 1 1 calc R . . C4 C 0.1287(6) 0.6028(2) -0.5785(4) 0.0512(11) Uani 1 1 d . . . H4A H 0.1459 0.6024 -0.6694 0.061 Uiso 1 1 calc R . . H4B H 0.0582 0.5627 -0.5591 0.061 Uiso 1 1 calc R . . H1E H 0.2662 0.7106 -0.2650 0.061 Uiso 0.50 1 d PR . . H1F H 0.1204 0.7501 -0.2809 0.061 Uiso 1 2 d SR . . 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 0.0196(4) 0.0292(4) 0.0249(4) 0.000 0.0032(3) 0.000 Mn2 0.0319(6) 0.0597(11) 0.0386(8) -0.0095(9) 0.0087(5) -0.0022(10) Mn3 0.0391(5) 0.0276(5) 0.0518(5) 0.000 -0.0051(4) 0.000 Ge1 0.0175(3) 0.0251(3) 0.0220(3) 0.000 -0.0002(2) 0.000 Ge2 0.0260(2) 0.0196(2) 0.0268(2) -0.00177(14) 0.00190(15) -0.00160(15) S1 0.0325(7) 0.0232(7) 0.0238(6) 0.000 -0.0001(5) 0.000 S2 0.0242(5) 0.0229(5) 0.0339(5) -0.0018(4) -0.0002(4) 0.0039(4) S3 0.0204(6) 0.0399(8) 0.0239(6) 0.000 0.0017(5) 0.000 S4 0.0239(5) 0.0299(5) 0.0391(5) -0.0036(4) 0.0061(4) -0.0045(4) S5 0.0180(6) 0.0560(9) 0.0223(6) 0.000 -0.0008(5) 0.000 S6 0.0579(7) 0.0261(5) 0.0430(6) -0.0122(4) 0.0166(5) -0.0074(5) O1 0.051(3) 0.074(3) 0.068(3) 0.000 0.003(2) 0.000 N1 0.061(3) 0.055(2) 0.048(2) -0.0049(18) 0.0194(19) -0.0157(19) N2 0.036(2) 0.0330(19) 0.080(3) 0.0085(18) 0.0055(18) 0.0048(15) N3 0.045(2) 0.049(2) 0.0391(19) -0.0051(16) -0.0099(16) 0.0074(17) N4 0.043(2) 0.0382(19) 0.0337(17) 0.0005(14) 0.0008(15) -0.0040(15) C1 0.083(4) 0.113(5) 0.060(3) -0.014(3) -0.007(3) -0.023(4) C2 0.063(4) 0.049(5) 0.064(4) 0.014(4) -0.020(3) -0.001(4) C2' 0.063(4) 0.049(5) 0.064(4) 0.014(4) -0.020(3) -0.001(4) C3 0.084(4) 0.041(3) 0.048(3) 0.006(2) 0.007(3) 0.018(2) C4 0.068(3) 0.034(2) 0.052(3) -0.007(2) 0.007(2) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 S5 2.4458(14) 1_455 ? Mn1 S3 2.4474(14) . ? Mn1 S4 2.4535(10) 4_575 ? Mn1 S4 2.4535(10) . ? Mn2 Mn2 0.891(2) 3_665 ? Mn2 N2 2.180(2) . ? Mn2 N1 2.192(4) . ? Mn2 N2 2.218(2) 3_665 ? Mn2 N1 2.272(4) 3_665 ? Mn2 S4 2.5365(15) . ? Mn3 O1 2.185(5) . ? Mn3 N4 2.2112(19) 4_575 ? Mn3 N4 2.2112(19) . ? Mn3 N3 2.2582(19) 4_575 ? Mn3 N3 2.2582(19) . ? Ge1 S3 2.1859(13) . ? Ge1 S5 2.1981(13) . ? Ge1 S2 2.2451(9) 4_575 ? Ge1 S2 2.2451(9) . ? Ge2 S6 2.1306(10) . ? Ge2 S4 2.2011(9) . ? Ge2 S1 2.2467(7) . ? Ge2 S2 2.2647(9) . ? S1 Ge2 2.2467(7) 4_575 ? S5 Mn1 2.4458(14) 1_655 ? N1 C1 1.465(4) . ? N1 Mn2 2.272(4) 3_665 ? N2 C2' 1.412(12) . ? N2 C2 1.6002 . ? N2 Mn2 2.218(2) 3_665 ? N3 C3 1.467(5) . ? N4 C4 1.479(5) . ? C1 C2 1.371(4) 3_665 ? C1 C2' 1.473(12) 3_665 ? C2 C2' 0.941(12) . ? C2 C1 1.371(4) 3_665 ? C2' C1 1.473(12) 3_665 ? C3 C4 1.493(6) . ? 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 S5 Mn1 S3 101.64(5) 1_455 . ? S5 Mn1 S4 112.50(3) 1_455 4_575 ? S3 Mn1 S4 109.35(3) . 4_575 ? S5 Mn1 S4 112.50(3) 1_455 . ? S3 Mn1 S4 109.35(3) . . ? S4 Mn1 S4 111.05(5) 4_575 . ? Mn2 Mn2 N2 80.7(2) 3_665 . ? Mn2 Mn2 N1 83.6(2) 3_665 . ? N2 Mn2 N1 97.10(12) . . ? Mn2 Mn2 N2 76.0(2) 3_665 3_665 ? N2 Mn2 N2 156.65(6) . 3_665 ? N1 Mn2 N2 80.41(12) . 3_665 ? Mn2 Mn2 N1 73.5(2) 3_665 3_665 ? N2 Mn2 N1 79.47(12) . 3_665 ? N1 Mn2 N1 157.07(7) . 3_665 ? N2 Mn2 N1 93.76(12) 3_665 3_665 ? Mn2 Mn2 S4 178.7(3) 3_665 . ? N2 Mn2 S4 100.60(8) . . ? N1 Mn2 S4 95.95(11) . . ? N2 Mn2 S4 102.75(7) 3_665 . ? N1 Mn2 S4 106.98(11) 3_665 . ? O1 Mn3 N4 100.19(9) . 4_575 ? O1 Mn3 N4 100.19(9) . . ? N4 Mn3 N4 96.18(10) 4_575 . ? O1 Mn3 N3 97.80(9) . 4_575 ? N4 Mn3 N3 79.30(6) 4_575 4_575 ? N4 Mn3 N3 161.96(10) . 4_575 ? O1 Mn3 N3 97.80(9) . . ? N4 Mn3 N3 161.96(10) 4_575 . ? N4 Mn3 N3 79.30(6) . . ? N3 Mn3 N3 99.57(10) 4_575 . ? S3 Ge1 S5 110.86(5) . . ? S3 Ge1 S2 113.77(3) . 4_575 ? S5 Ge1 S2 105.07(3) . 4_575 ? S3 Ge1 S2 113.77(3) . . ? S5 Ge1 S2 105.07(3) . . ? S2 Ge1 S2 107.58(5) 4_575 . ? S6 Ge2 S4 114.82(4) . . ? S6 Ge2 S1 104.21(4) . . ? S4 Ge2 S1 110.73(4) . . ? S6 Ge2 S2 107.35(4) . . ? S4 Ge2 S2 111.04(4) . . ? S1 Ge2 S2 108.28(4) . . ? Ge2 S1 Ge2 112.37(5) 4_575 . ? Ge1 S2 Ge2 109.90(4) . . ? Ge1 S3 Mn1 103.05(5) . . ? Ge2 S4 Mn1 105.01(4) . . ? Ge2 S4 Mn2 104.04(5) . . ? Mn1 S4 Mn2 128.41(5) . . ? Ge1 S5 Mn1 109.44(5) . 1_655 ? C1 N1 Mn2 109.2(2) . . ? C1 N1 Mn2 107.4(2) . 3_665 ? Mn2 N1 Mn2 22.93(7) . 3_665 ? C2' N2 C2 35.7(5) . . ? C2' N2 Mn2 113.0(5) . . ? C2 N2 Mn2 96.72(6) . . ? C2' N2 Mn2 106.2(5) . 3_665 ? C2 N2 Mn2 104.16(6) . 3_665 ? Mn2 N2 Mn2 23.35(6) . 3_665 ? C3 N3 Mn3 104.8(2) . . ? C4 N4 Mn3 109.4(2) . . ? C2 C1 N1 112.3(2) 3_665 . ? C2 C1 C2' 38.4(5) 3_665 3_665 ? N1 C1 C2' 116.6(5) . 3_665 ? C2' C2 C1 76.7(8) . 3_665 ? C2' C2 N2 61.2(7) . . ? C1 C2 N2 112.23(15) 3_665 . ? C2 C2' N2 83.1(8) . . ? C2 C2' C1 64.9(7) . 3_665 ? N2 C2' C1 117.8(8) . 3_665 ? N3 C3 C4 110.6(3) . . ? N4 C4 C3 110.7(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.567 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.084 ### end data_2 _database_code_depnum_ccdc_archive 'CCDC 746743' #TrackingRef 'crystal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H16 Mn N4 S3 Sn' _chemical_formula_sum 'C4 H16 Mn N4 S3 Sn' _chemical_formula_weight 390.02 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' N N 0.0061 0.0033 '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' Sn Sn -0.6537 1.4246 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.122(3) _cell_length_b 13.308(5) _cell_length_c 9.630(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.310(5) _cell_angle_gamma 90.00 _cell_volume 1262.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5160 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 26.14 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 2.052 _exptl_crystal_density_diffrn 2.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 3.442 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6633 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.11 _reflns_number_total 2461 _reflns_number_gt 2298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0865P)^2^+32.3142P] 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 SHELXL _refine_ls_extinction_coef 0.0042(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2461 _refine_ls_number_parameters 119 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1992 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.160 _refine_ls_restrained_S_all 1.160 _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 Sn1 Sn 0.61370(7) 0.99146(5) 0.15641(7) 0.0143(3) Uani 1 1 d . . . Mn1 Mn 0.31765(17) 1.01073(11) 0.39974(17) 0.0182(4) Uani 1 1 d . . . S1 S 0.8446(3) 1.0234(2) 0.1987(3) 0.0231(6) Uani 1 1 d . . . S2 S 0.5373(2) 0.93269(19) 0.3551(2) 0.0173(5) Uani 1 1 d . . . S3 S 0.4762(3) 1.13011(19) 0.0334(3) 0.0194(6) Uani 1 1 d . . . N1 N 0.3201(9) 1.1673(6) 0.3108(9) 0.0195(17) Uani 1 1 d . . . H1A H 0.3875 1.2034 0.3657 0.023 Uiso 1 1 calc R . . H1B H 0.3342 1.1647 0.2219 0.023 Uiso 1 1 calc R . . N2 N 0.1338(9) 1.0836(7) 0.4614(9) 0.0228(19) Uani 1 1 d . . . H2A H 0.0561 1.0630 0.4024 0.027 Uiso 1 1 calc R . . H2B H 0.1313 1.0670 0.5514 0.027 Uiso 1 1 calc R . . N3 N 0.1869(11) 0.9475(9) 0.1931(10) 0.033(2) Uani 1 1 d . . . H3A H 0.1015 0.9712 0.1782 0.040 Uiso 1 1 calc R . . H3B H 0.2215 0.9642 0.1182 0.040 Uiso 1 1 calc R . . N4 N 0.2588(10) 0.8579(7) 0.4708(11) 0.030(2) Uani 1 1 d . . . H4A H 0.3322 0.8178 0.4922 0.036 Uiso 1 1 calc R . . H4B H 0.2256 0.8646 0.5494 0.036 Uiso 1 1 calc R . . C1 C 0.1880(12) 1.2147(8) 0.3083(12) 0.026(2) Uani 1 1 d . . . H1C H 0.1191 1.1880 0.2298 0.031 Uiso 1 1 calc R . . H1D H 0.1938 1.2867 0.2952 0.031 Uiso 1 1 calc R . . C2 C 0.1506(11) 1.1927(9) 0.4489(11) 0.025(2) Uani 1 1 d . . . H2C H 0.2215 1.2167 0.5275 0.030 Uiso 1 1 calc R . . H2D H 0.0668 1.2268 0.4524 0.030 Uiso 1 1 calc R . . C3 C 0.1890(13) 0.8375(10) 0.2130(15) 0.037(3) Uani 1 1 d . . . H3C H 0.2782 0.8115 0.2119 0.045 Uiso 1 1 calc R . . H3D H 0.1234 0.8063 0.1356 0.045 Uiso 1 1 calc R . . C4 C 0.1546(13) 0.8130(10) 0.3541(16) 0.038(3) Uani 1 1 d . . . H4C H 0.0658 0.8398 0.3557 0.045 Uiso 1 1 calc R . . H4D H 0.1524 0.7408 0.3664 0.045 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 Sn1 0.0133(4) 0.0188(4) 0.0115(4) 0.0002(2) 0.0045(3) 0.0013(2) Mn1 0.0200(9) 0.0204(8) 0.0152(8) -0.0001(5) 0.0058(7) -0.0007(6) S1 0.0146(12) 0.0326(14) 0.0239(13) 0.0030(11) 0.0078(10) -0.0019(10) S2 0.0159(11) 0.0247(12) 0.0126(11) 0.0006(9) 0.0056(9) 0.0001(9) S3 0.0244(13) 0.0197(12) 0.0135(11) -0.0012(9) 0.0032(9) 0.0045(10) N1 0.022(4) 0.019(4) 0.020(4) 0.002(3) 0.011(3) 0.002(3) N2 0.019(4) 0.034(5) 0.016(4) 0.003(4) 0.005(3) 0.000(4) N3 0.029(5) 0.052(7) 0.020(5) -0.008(4) 0.008(4) -0.005(5) N4 0.028(5) 0.024(5) 0.038(5) 0.002(4) 0.012(4) 0.002(4) C1 0.030(6) 0.023(5) 0.025(5) 0.008(4) 0.009(5) 0.009(5) C2 0.024(5) 0.031(6) 0.021(5) 0.003(4) 0.008(4) 0.010(4) C3 0.028(6) 0.042(7) 0.046(7) -0.026(6) 0.014(6) -0.003(5) C4 0.028(6) 0.027(6) 0.062(9) -0.011(6) 0.018(6) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 S1 2.317(3) . ? Sn1 S2 2.356(2) . ? Sn1 S3 2.446(3) . ? Sn1 S3 2.454(3) 3_675 ? Mn1 N1 2.256(9) . ? Mn1 N4 2.269(10) . ? Mn1 N3 2.282(10) . ? Mn1 N2 2.295(9) . ? Mn1 S2 2.578(3) . ? Mn1 S2 2.589(3) 3_676 ? S2 Mn1 2.589(3) 3_676 ? S3 Sn1 2.454(3) 3_675 ? N1 C1 1.474(13) . ? N2 C2 1.470(15) . ? N3 C3 1.475(18) . ? N4 C4 1.479(16) . ? C1 C2 1.516(15) . ? C3 C4 1.514(19) . ? 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 S1 Sn1 S2 115.12(10) . . ? S1 Sn1 S3 112.65(10) . . ? S2 Sn1 S3 112.77(9) . . ? S1 Sn1 S3 115.97(10) . 3_675 ? S2 Sn1 S3 104.54(9) . 3_675 ? S3 Sn1 S3 93.70(8) . 3_675 ? N1 Mn1 N4 165.8(3) . . ? N1 Mn1 N3 93.7(4) . . ? N4 Mn1 N3 78.0(4) . . ? N1 Mn1 N2 77.8(3) . . ? N4 Mn1 N2 90.9(3) . . ? N3 Mn1 N2 92.3(4) . . ? N1 Mn1 S2 102.9(2) . . ? N4 Mn1 S2 89.2(3) . . ? N3 Mn1 S2 93.2(3) . . ? N2 Mn1 S2 174.5(2) . . ? N1 Mn1 S2 91.4(2) . 3_676 ? N4 Mn1 S2 96.8(3) . 3_676 ? N3 Mn1 S2 174.8(3) . 3_676 ? N2 Mn1 S2 88.0(2) . 3_676 ? S2 Mn1 S2 86.53(9) . 3_676 ? Sn1 S2 Mn1 117.30(10) . . ? Sn1 S2 Mn1 114.87(11) . 3_676 ? Mn1 S2 Mn1 93.47(9) . 3_676 ? Sn1 S3 Sn1 86.30(8) . 3_675 ? C1 N1 Mn1 108.2(6) . . ? C2 N2 Mn1 106.2(6) . . ? C3 N3 Mn1 105.4(8) . . ? C4 N4 Mn1 108.9(8) . . ? N1 C1 C2 108.4(8) . . ? N2 C2 C1 108.8(9) . . ? N3 C3 C4 109.3(10) . . ? N4 C4 C3 108.9(10) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 4.873 _refine_diff_density_min -1.591 _refine_diff_density_rms 0.304 ### end