Electronic Supplementary Material for CrystEngComm This Journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Dr Maria Carla Aragoni' _publ_contact_author_address ; Dipartimento di Chimica Inorganica ed Analitica Universita degli Studi di Cagliari SS 554 bivio per Sestu Monserrato I-09042 ITALY ; _publ_contact_author_email ARAGONI@UNICA.IT _publ_section_title ; Synthesis and structural characterisation of coordination polymers designed using discrete phosphonodithioato NiII complexes and bi-pyridyl donor ligands ; loop_ _publ_author_name 'Maria Carla Aragoni' 'Massimiliano Arca' 'Neil Champness' 'M.De Pasquale' 'F. A. Devillanova' ; F.Isaia ; 'Vito Lippolis' 'Neil S. Oxtoby' 'Claire Wilson' data_nimppp _database_code_depnum_ccdc_archive 'CCDC 249546' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 N2 Ni O4 P2 S4' _chemical_formula_weight 781.51 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9890(12) _cell_length_b 9.8015(13) _cell_length_c 11.403(2) _cell_angle_alpha 112.076(2) _cell_angle_beta 94.424(2) _cell_angle_gamma 108.021(2) _cell_volume 863.8(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2555 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.4 _exptl_crystal_description lath _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 404 _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7912 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3878 _reflns_number_gt 3032 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' ?' _computing_publication_material 'PLATON (Spek, 2003)' _refine_special_details ; Disorder of PPPh ligand, necessary in P-1 but apparent in P1 as well. Refinement in P-1 gives much more reasonable displacement ellipsoids. Ph and triple bonded C modelled over 2 half occupied sites with restraints applied to Ph geometry. ; _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^)+(0.0341P)^2^+0.5314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3878 _refine_ls_number_parameters 238 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.004 _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 Ni1 Ni 0.0000 0.0000 0.0000 0.01565(12) Uani 1 2 d S . . S1 S 0.07003(7) -0.23643(8) -0.05848(6) 0.01996(15) Uani 1 1 d . . . S2 S -0.04851(8) -0.04982(8) 0.19503(6) 0.02168(15) Uani 1 1 d . . . P1 P 0.01976(8) -0.23313(8) 0.10978(7) 0.01996(16) Uani 1 1 d . . . O1 O -0.1122(2) -0.3947(2) 0.0942(2) 0.0277(4) Uani 1 1 d . . . O2 O 0.5697(2) -0.2215(3) 0.4443(2) 0.0400(6) Uani 1 1 d . . . C1 C 0.1858(3) -0.2312(3) 0.2103(3) 0.0220(6) Uani 1 1 d . . . C2 C 0.1649(3) -0.3294(3) 0.2748(3) 0.0260(6) Uani 1 1 d . . . H2A H 0.0609 -0.4009 0.2659 0.031 Uiso 1 1 calc R . . C3 C 0.2963(3) -0.3222(4) 0.3517(3) 0.0299(6) Uani 1 1 d . . . H3A H 0.2817 -0.3888 0.3959 0.036 Uiso 1 1 calc R . . C4 C 0.4493(3) -0.2190(4) 0.3652(3) 0.0310(7) Uani 1 1 d . . . C5 C 0.4716(4) -0.1212(4) 0.3012(3) 0.0357(7) Uani 1 1 d . . . H5A H 0.5758 -0.0500 0.3101 0.043 Uiso 1 1 calc R . . C6 C 0.3395(3) -0.1287(4) 0.2239(3) 0.0320(7) Uani 1 1 d . . . H6A H 0.3545 -0.0624 0.1794 0.038 Uiso 1 1 calc R . . C7 C 0.7290(4) -0.1078(5) 0.4684(3) 0.0503(10) Uani 1 1 d . . . H7A H 0.8038 -0.1218 0.5261 0.075 Uiso 1 1 calc R . . H7B H 0.7283 -0.0005 0.5094 0.075 Uiso 1 1 calc R . . H7C H 0.7628 -0.1242 0.3861 0.075 Uiso 1 1 calc R . . C8 C -0.2752(3) -0.4443(4) 0.0269(3) 0.0329(7) Uani 1 1 d . . . H8A H -0.3393 -0.5455 0.0266 0.049 Uiso 1 1 calc R . . H8B H -0.2771 -0.4567 -0.0626 0.049 Uiso 1 1 calc R . . H8C H -0.3202 -0.3644 0.0709 0.049 Uiso 1 1 calc R . . N1' N 0.2391(2) 0.1483(2) 0.0983(2) 0.0190(4) Uani 1 1 d . . . C2' C 0.2705(3) 0.2517(3) 0.2227(3) 0.0244(6) Uani 1 1 d . . . H2'A H 0.1833 0.2702 0.2592 0.029 Uiso 1 1 calc R . . C3' C 0.4228(3) 0.3325(3) 0.3001(3) 0.0275(6) Uani 1 1 d . . . H3'A H 0.4389 0.4041 0.3879 0.033 Uiso 1 1 calc R . . C4' C 0.5533(3) 0.3085(3) 0.2485(3) 0.0230(6) Uani 1 1 d . A . C5' C 0.5198(3) 0.2077(3) 0.1168(3) 0.0219(5) Uani 1 1 d . . . H5'A H 0.6048 0.1919 0.0757 0.026 Uiso 1 1 calc R . . C6' C 0.3662(3) 0.1325(3) 0.0479(3) 0.0206(5) Uani 1 1 d . . . H6'A H 0.3472 0.0646 -0.0414 0.025 Uiso 1 1 calc R . . C7' C 0.7143(3) 0.3796(3) 0.3325(3) 0.0265(6) Uani 1 1 d D . . C8' C 0.7791(6) 0.5362(6) 0.4227(5) 0.0256(12) Uani 0.50 1 d PD A -1 H8'A H 0.7204 0.6025 0.4253 0.031 Uiso 0.50 1 calc PR A -1 C9' C 0.9251(6) 0.6007(6) 0.5092(5) 0.0269(12) Uani 0.50 1 d PD A -1 H9'A H 0.9687 0.7084 0.5704 0.032 Uiso 0.50 1 calc PR A -1 C10' C 1.0000 0.5000 0.5000 0.0319(10) Uani 1 2 d SD . . C11' C 0.9495(6) 0.3421(6) 0.4207(5) 0.0258(12) Uani 0.50 1 d PD A -1 H11A H 1.0092 0.2784 0.4239 0.031 Uiso 0.50 1 calc PR A -1 C12' C 0.8023(6) 0.2830(6) 0.3346(5) 0.0228(11) Uani 0.50 1 d PD A -1 H12A H 0.7598 0.1744 0.2756 0.027 Uiso 0.50 1 calc PR A -1 C13' C 0.8364(6) 0.4353(7) 0.3999(5) 0.0295(13) Uani 0.50 1 d P A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0120(2) 0.0180(2) 0.0156(2) 0.00631(19) 0.00037(17) 0.00530(18) S1 0.0174(3) 0.0201(3) 0.0210(3) 0.0076(3) 0.0024(3) 0.0069(3) S2 0.0211(3) 0.0262(4) 0.0195(3) 0.0105(3) 0.0050(3) 0.0098(3) P1 0.0160(3) 0.0207(3) 0.0237(4) 0.0117(3) 0.0019(3) 0.0051(3) O1 0.0194(10) 0.0266(10) 0.0398(12) 0.0211(9) 0.0020(8) 0.0040(8) O2 0.0298(12) 0.0637(16) 0.0384(13) 0.0314(12) 0.0020(10) 0.0213(11) C1 0.0200(13) 0.0241(14) 0.0255(14) 0.0141(12) 0.0030(11) 0.0088(11) C2 0.0266(15) 0.0266(15) 0.0273(15) 0.0145(13) 0.0054(12) 0.0090(12) C3 0.0340(16) 0.0371(17) 0.0298(15) 0.0230(14) 0.0071(13) 0.0164(13) C4 0.0282(15) 0.0452(18) 0.0245(15) 0.0162(14) 0.0024(12) 0.0187(14) C5 0.0216(15) 0.0480(19) 0.0401(18) 0.0275(16) 0.0007(13) 0.0064(13) C6 0.0234(15) 0.0390(17) 0.0385(17) 0.0272(15) -0.0003(13) 0.0059(13) C7 0.0299(18) 0.086(3) 0.044(2) 0.035(2) 0.0019(15) 0.0237(19) C8 0.0158(14) 0.0310(16) 0.0431(18) 0.0160(14) -0.0025(13) -0.0011(12) N1' 0.0150(10) 0.0206(11) 0.0192(11) 0.0078(9) 0.0001(9) 0.0052(9) C2' 0.0196(13) 0.0281(15) 0.0223(14) 0.0070(12) 0.0039(11) 0.0096(11) C3' 0.0213(14) 0.0302(15) 0.0218(14) 0.0046(12) -0.0021(11) 0.0072(12) C4' 0.0181(13) 0.0230(14) 0.0237(14) 0.0091(12) -0.0019(11) 0.0045(11) C5' 0.0196(13) 0.0221(13) 0.0228(13) 0.0095(11) 0.0058(11) 0.0057(11) C6' 0.0232(13) 0.0225(14) 0.0190(13) 0.0095(11) 0.0069(11) 0.0105(11) C7' 0.0194(14) 0.0311(16) 0.0245(14) 0.0095(13) 0.0040(12) 0.0064(12) C8' 0.023(3) 0.025(3) 0.029(3) 0.010(2) 0.000(2) 0.012(2) C9' 0.019(3) 0.026(3) 0.023(3) 0.004(2) 0.000(2) 0.002(2) C10' 0.022(2) 0.040(3) 0.029(2) 0.013(2) 0.0101(18) 0.0062(18) C11' 0.019(3) 0.035(3) 0.026(3) 0.014(3) 0.004(2) 0.011(2) C12' 0.027(3) 0.022(3) 0.019(3) 0.007(2) 0.006(2) 0.009(2) C13' 0.017(3) 0.043(4) 0.023(3) 0.013(3) 0.002(2) 0.005(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 Ni1 N1' 2.112(2) 2 ? Ni1 N1' 2.112(2) . ? Ni1 S1 2.4530(7) . ? Ni1 S1 2.4530(7) 2 ? Ni1 S2 2.4917(8) . ? Ni1 S2 2.4917(8) 2 ? S1 P1 1.9956(10) . ? S2 P1 2.0027(9) . ? P1 O1 1.5934(19) . ? P1 C1 1.801(3) . ? O1 C8 1.442(3) . ? O2 C4 1.367(3) . ? O2 C7 1.445(4) . ? C1 C6 1.391(4) . ? C1 C2 1.394(4) . ? C2 C3 1.382(4) . ? C3 C4 1.388(4) . ? C4 C5 1.386(4) . ? C5 C6 1.389(4) . ? N1' C2' 1.341(3) . ? N1' C6' 1.343(3) . ? C2' C3' 1.378(4) . ? C3' C4' 1.396(4) . ? C4' C5' 1.397(4) . ? C4' C7' 1.469(4) . ? C5' C6' 1.355(4) . ? C7' C13' 1.130(6) . ? C7' C8' 1.386(5) . ? C7' C12' 1.414(5) . ? C8' C9' 1.383(5) . ? C9' C10' 1.335(5) . ? C10' C9' 1.335(5) 2_766 ? C10' C11' 1.367(5) . ? C10' C11' 1.367(5) 2_766 ? C10' C13' 1.577(5) 2_766 ? C10' C13' 1.577(5) . ? C11' C12' 1.396(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1' Ni1 N1' 180.00(16) 2 . ? N1' Ni1 S1 88.81(6) 2 . ? N1' Ni1 S1 91.19(6) . . ? N1' Ni1 S1 91.19(6) 2 2 ? N1' Ni1 S1 88.81(6) . 2 ? S1 Ni1 S1 180.00(4) . 2 ? N1' Ni1 S2 90.30(6) 2 . ? N1' Ni1 S2 89.70(6) . . ? S1 Ni1 S2 82.09(2) . . ? S1 Ni1 S2 97.91(2) 2 . ? N1' Ni1 S2 89.70(6) 2 2 ? N1' Ni1 S2 90.30(6) . 2 ? S1 Ni1 S2 97.91(2) . 2 ? S1 Ni1 S2 82.09(2) 2 2 ? S2 Ni1 S2 180.00(3) . 2 ? P1 S1 Ni1 85.24(3) . . ? P1 S2 Ni1 84.06(3) . . ? O1 P1 C1 99.17(11) . . ? O1 P1 S1 113.09(8) . . ? C1 P1 S1 111.29(9) . . ? O1 P1 S2 111.16(8) . . ? C1 P1 S2 113.39(9) . . ? S1 P1 S2 108.61(4) . . ? C8 O1 P1 120.60(17) . . ? C4 O2 C7 117.4(2) . . ? C6 C1 C2 119.0(2) . . ? C6 C1 P1 119.0(2) . . ? C2 C1 P1 122.0(2) . . ? C3 C2 C1 119.7(3) . . ? C2 C3 C4 120.9(3) . . ? O2 C4 C5 124.3(3) . . ? O2 C4 C3 115.7(3) . . ? C5 C4 C3 119.9(3) . . ? C4 C5 C6 119.1(3) . . ? C5 C6 C1 121.4(3) . . ? C2' N1' C6' 116.6(2) . . ? C2' N1' Ni1 119.78(17) . . ? C6' N1' Ni1 123.13(17) . . ? N1' C2' C3' 123.3(2) . . ? C2' C3' C4' 119.5(3) . . ? C3' C4' C5' 116.5(2) . . ? C3' C4' C7' 120.5(2) . . ? C5' C4' C7' 122.9(2) . . ? C6' C5' C4' 120.0(2) . . ? N1' C6' C5' 123.8(2) . . ? C13' C7' C8' 56.1(4) . . ? C13' C7' C12' 60.9(4) . . ? C8' C7' C12' 116.8(4) . . ? C13' C7' C4' 178.2(4) . . ? C8' C7' C4' 122.9(3) . . ? C12' C7' C4' 119.9(3) . . ? C9' C8' C7' 123.2(4) . . ? C10' C9' C8' 114.8(4) . . ? C9' C10' C9' 180.000(3) 2_766 . ? C9' C10' C11' 51.1(3) 2_766 . ? C9' C10' C11' 128.9(3) . . ? C9' C10' C11' 128.9(3) 2_766 2_766 ? C9' C10' C11' 51.1(3) . 2_766 ? C11' C10' C11' 180.0(3) . 2_766 ? C9' C10' C13' 62.8(3) 2_766 2_766 ? C9' C10' C13' 117.2(3) . 2_766 ? C11' C10' C13' 113.7(3) . 2_766 ? C11' C10' C13' 66.3(3) 2_766 2_766 ? C9' C10' C13' 117.2(3) 2_766 . ? C9' C10' C13' 62.8(3) . . ? C11' C10' C13' 66.3(3) . . ? C11' C10' C13' 113.7(3) 2_766 . ? C13' C10' C13' 180.000(1) 2_766 . ? C10' C11' C12' 114.0(4) . . ? C11' C12' C7' 122.1(4) . . ? C7' C13' C10' 174.0(5) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.601 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.077 data_dztzni _database_code_depnum_ccdc_archive 'CCDC 265935' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 N6 Ni O4 P2 S4' _chemical_formula_weight 761.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ni Ni 0.3393 1.1124 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4357(10) _cell_length_b 9.7115(13) _cell_length_c 12.026(2) _cell_angle_alpha 70.913(2) _cell_angle_beta 81.101(2) _cell_angle_gamma 80.143(2) _cell_volume 804.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3547 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.45 _exptl_crystal_description lath _exptl_crystal_colour orange _exptl_crystal_size_max 0.83 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392 _exptl_absorpt_coefficient_mu 1.008 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.879 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7284 _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3621 _reflns_number_gt 3276 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _refine_special_details ; OMe group on P1 disordered over 2 half occupied sites, refined with isotropic adps and distance restraints applied. ; _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^)+(0.0342P)^2^+0.6570P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3621 _refine_ls_number_parameters 208 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.990 _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 Ni1 Ni 1.5000 0.0000 0.5000 0.01535(9) Uani 1 2 d S . . P1 P 1.59296(6) -0.30331(5) 0.66101(4) 0.01969(11) Uani 1 1 d D . . O1A O 1.5496(5) -0.4636(3) 0.6782(3) 0.0237(8) Uani 0.50 1 d PD A 1 C8A C 1.7089(6) -0.5730(5) 0.6804(4) 0.0344(9) Uiso 0.50 1 d PD A 1 H8A1 H 1.6692 -0.6682 0.6914 0.052 Uiso 0.50 1 calc PR A 1 H8A2 H 1.7779 -0.5809 0.7458 0.052 Uiso 0.50 1 calc PR A 1 H8A3 H 1.7873 -0.5441 0.6054 0.052 Uiso 0.50 1 calc PR A 1 O1B O 1.6055(5) -0.4789(4) 0.6769(4) 0.0204(10) Uiso 0.50 1 d PD A 2 C8B C 1.5552(7) -0.5244(5) 0.5833(4) 0.0403(10) Uiso 0.50 1 d PD A 2 H8B1 H 1.5472 -0.6302 0.6121 0.060 Uiso 0.50 1 calc PR A 2 H8B2 H 1.6485 -0.5029 0.5151 0.060 Uiso 0.50 1 calc PR A 2 H8B3 H 1.4360 -0.4708 0.5597 0.060 Uiso 0.50 1 calc PR A 2 S1 S 1.74875(6) -0.21372(5) 0.51252(4) 0.02015(11) Uani 1 1 d . A . S2 S 1.34147(6) -0.19284(5) 0.66061(4) 0.02293(11) Uani 1 1 d . A . C1 C 1.6949(2) -0.31625(19) 0.79158(15) 0.0191(3) Uani 1 1 d . A . C2 C 1.5865(3) -0.3364(2) 0.89967(16) 0.0246(4) Uani 1 1 d . . . H2A H 1.4599 -0.3442 0.9037 0.030 Uiso 1 1 calc R A . C3 C 1.6598(3) -0.3454(2) 1.00185(16) 0.0244(4) Uani 1 1 d . A . H3A H 1.5844 -0.3604 1.0751 0.029 Uiso 1 1 calc R . . C4 C 1.8450(3) -0.3322(2) 0.99553(16) 0.0216(4) Uani 1 1 d . . . C5 C 1.9551(2) -0.3133(2) 0.88823(16) 0.0221(4) Uani 1 1 d . A . H5A H 2.0818 -0.3059 0.8843 0.027 Uiso 1 1 calc R . . C6 C 1.8809(2) -0.30533(19) 0.78724(16) 0.0202(4) Uani 1 1 d . . . H6A H 1.9571 -0.2923 0.7144 0.024 Uiso 1 1 calc R A . O2 O 1.93027(19) -0.33319(15) 1.08840(12) 0.0273(3) Uani 1 1 d . A . C7 C 1.8260(3) -0.3649(3) 1.20251(17) 0.0339(5) Uani 1 1 d . . . H7A H 1.9018 -0.3624 1.2614 0.051 Uiso 1 1 calc R A . H7B H 1.7875 -0.4628 1.2241 0.051 Uiso 1 1 calc R . . H7C H 1.7173 -0.2913 1.2000 0.051 Uiso 1 1 calc R . . N1' N 1.38055(19) -0.05379(16) 0.37561(12) 0.0164(3) Uani 1 1 d . . . C2' C 1.4699(2) -0.04861(19) 0.26882(15) 0.0188(3) Uani 1 1 d . . . H2'A H 1.5987 -0.0461 0.2576 0.023 Uiso 1 1 calc R . . C3' C 1.3838(2) -0.0467(2) 0.17435(15) 0.0192(3) Uani 1 1 d . . . H3'A H 1.4525 -0.0443 0.1004 0.023 Uiso 1 1 calc R . . C4' C 1.1943(2) -0.04834(19) 0.18953(15) 0.0170(3) Uani 1 1 d . . . C5' C 1.1028(2) -0.06324(19) 0.30197(15) 0.0186(3) Uani 1 1 d . . . H5'A H 0.9752 -0.0713 0.3167 0.022 Uiso 1 1 calc R . . C6' C 1.2000(2) -0.06619(19) 0.39178(15) 0.0174(3) Uani 1 1 d . . . H6'A H 1.1366 -0.0775 0.4685 0.021 Uiso 1 1 calc R . . C7' C 1.0910(2) -0.02556(19) 0.08835(15) 0.0179(3) Uani 1 1 d . . . N8' N 0.9072(2) -0.01387(18) 0.10905(13) 0.0214(3) Uani 1 1 d . . . N9' N 0.8132(2) 0.01307(19) 0.01791(13) 0.0225(3) 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 Ni1 0.01423(15) 0.02079(17) 0.01147(15) -0.00343(12) -0.00293(11) -0.00510(11) P1 0.0222(2) 0.0203(2) 0.0164(2) -0.00183(17) -0.00423(17) -0.00805(17) O1A 0.0147(18) 0.0217(16) 0.0349(18) -0.0076(12) -0.0046(15) -0.0037(13) S1 0.0191(2) 0.0238(2) 0.0164(2) -0.00463(17) -0.00152(16) -0.00322(16) S2 0.0171(2) 0.0315(3) 0.0171(2) 0.00018(18) -0.00375(16) -0.00859(17) C1 0.0212(8) 0.0174(8) 0.0176(8) -0.0016(7) -0.0052(7) -0.0041(6) C2 0.0203(9) 0.0308(10) 0.0209(9) -0.0029(8) -0.0039(7) -0.0069(7) C3 0.0251(9) 0.0281(10) 0.0170(8) -0.0023(7) -0.0013(7) -0.0054(7) C4 0.0273(9) 0.0177(8) 0.0192(8) -0.0025(7) -0.0085(7) -0.0025(7) C5 0.0194(9) 0.0233(9) 0.0222(9) -0.0032(7) -0.0054(7) -0.0037(7) C6 0.0200(8) 0.0194(9) 0.0190(8) -0.0026(7) -0.0027(7) -0.0032(6) O2 0.0308(7) 0.0327(8) 0.0196(6) -0.0061(6) -0.0081(6) -0.0066(6) C7 0.0417(12) 0.0407(12) 0.0200(9) -0.0081(9) -0.0063(9) -0.0071(9) N1' 0.0147(7) 0.0196(7) 0.0149(7) -0.0045(6) -0.0026(5) -0.0035(5) C2' 0.0146(8) 0.0242(9) 0.0175(8) -0.0060(7) -0.0015(6) -0.0034(6) C3' 0.0176(8) 0.0259(9) 0.0145(8) -0.0068(7) -0.0011(6) -0.0035(6) C4' 0.0187(8) 0.0194(8) 0.0149(8) -0.0058(7) -0.0041(6) -0.0046(6) C5' 0.0149(8) 0.0243(9) 0.0169(8) -0.0054(7) -0.0017(6) -0.0055(6) C6' 0.0174(8) 0.0204(8) 0.0144(8) -0.0043(7) -0.0018(6) -0.0044(6) C7' 0.0182(8) 0.0220(9) 0.0157(8) -0.0068(7) -0.0026(6) -0.0057(6) N8' 0.0182(7) 0.0331(9) 0.0158(7) -0.0094(6) -0.0035(6) -0.0062(6) N9' 0.0184(7) 0.0365(9) 0.0154(7) -0.0096(6) -0.0029(6) -0.0064(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. ; 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 Ni1 N1' 2.0929(14) . ? Ni1 N1' 2.0929(14) 2_856 ? Ni1 S2 2.5126(5) . ? Ni1 S2 2.5126(5) 2_856 ? Ni1 S1 2.5138(5) . ? Ni1 S1 2.5138(5) 2_856 ? P1 O1A 1.585(3) . ? P1 O1B 1.641(4) . ? P1 C1 1.8061(18) . ? P1 S2 1.9900(7) . ? P1 S1 1.9941(7) . ? O1A C8A 1.446(5) . ? O1B C8B 1.454(5) . ? C1 C2 1.393(3) . ? C1 C6 1.397(2) . ? C2 C3 1.391(3) . ? C3 C4 1.393(3) . ? C4 O2 1.364(2) . ? C4 C5 1.393(3) . ? C5 C6 1.384(2) . ? O2 C7 1.434(2) . ? N1' C2' 1.341(2) . ? N1' C6' 1.347(2) . ? C2' C3' 1.381(2) . ? C3' C4' 1.395(2) . ? C4' C5' 1.390(2) . ? C4' C7' 1.474(2) . ? C5' C6' 1.380(2) . ? C7' N9' 1.342(2) 2_755 ? C7' N8' 1.343(2) . ? N8' N9' 1.321(2) . ? N9' C7' 1.342(2) 2_755 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1' Ni1 N1' 180.0 . 2_856 ? N1' Ni1 S2 88.70(4) . . ? N1' Ni1 S2 91.30(4) 2_856 . ? N1' Ni1 S2 91.30(4) . 2_856 ? N1' Ni1 S2 88.70(4) 2_856 2_856 ? S2 Ni1 S2 180.0 . 2_856 ? N1' Ni1 S1 91.01(4) . . ? N1' Ni1 S1 88.99(4) 2_856 . ? S2 Ni1 S1 81.390(17) . . ? S2 Ni1 S1 98.610(17) 2_856 . ? N1' Ni1 S1 88.99(4) . 2_856 ? N1' Ni1 S1 91.01(4) 2_856 2_856 ? S2 Ni1 S1 98.610(17) . 2_856 ? S2 Ni1 S1 81.390(17) 2_856 2_856 ? S1 Ni1 S1 180.0 . 2_856 ? O1A P1 C1 105.82(15) . . ? O1B P1 C1 99.24(15) . . ? O1A P1 S2 101.23(14) . . ? O1B P1 S2 115.92(13) . . ? C1 P1 S2 110.92(6) . . ? O1A P1 S1 115.50(14) . . ? O1B P1 S1 107.49(14) . . ? C1 P1 S1 112.11(6) . . ? S2 P1 S1 110.69(3) . . ? C8A O1A P1 115.1(3) . . ? C8B O1B P1 119.6(3) . . ? P1 S1 Ni1 81.94(2) . . ? P1 S2 Ni1 82.05(2) . . ? C2 C1 C6 118.57(16) . . ? C2 C1 P1 119.79(14) . . ? C6 C1 P1 121.63(14) . . ? C3 C2 C1 121.42(17) . . ? C2 C3 C4 119.22(17) . . ? O2 C4 C5 115.56(16) . . ? O2 C4 C3 124.52(17) . . ? C5 C4 C3 119.91(17) . . ? C6 C5 C4 120.34(17) . . ? C5 C6 C1 120.52(17) . . ? C4 O2 C7 117.26(15) . . ? C2' N1' C6' 117.43(14) . . ? C2' N1' Ni1 121.24(11) . . ? C6' N1' Ni1 120.07(11) . . ? N1' C2' C3' 123.26(16) . . ? C2' C3' C4' 118.79(16) . . ? C5' C4' C3' 118.14(15) . . ? C5' C4' C7' 120.45(15) . . ? C3' C4' C7' 121.30(15) . . ? C6' C5' C4' 119.09(15) . . ? N1' C6' C5' 122.98(15) . . ? N9' C7' N8' 124.96(16) 2_755 . ? N9' C7' C4' 117.78(15) 2_755 . ? N8' C7' C4' 117.22(15) . . ? N9' N8' C7' 117.63(15) . . ? N8' N9' C7' 117.41(15) . 2_755 ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.540 _refine_diff_density_min -0.303 _refine_diff_density_rms 0.067 data_dptzni _database_code_depnum_ccdc_archive 'CCDC 265936' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 N6 Ni O4 P2 S4' _chemical_formula_weight 789.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ni Ni 0.3393 1.1124 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9179(9) _cell_length_b 10.7325(14) _cell_length_c 12.898(2) _cell_angle_alpha 66.496(2) _cell_angle_beta 86.813(2) _cell_angle_gamma 89.574(2) _cell_volume 876.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2791 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 27.35 _exptl_crystal_description lath _exptl_crystal_colour pink _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 7722 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3900 _reflns_number_gt 3042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' ?' _computing_publication_material 'enCIFer (CCDC, 2003); PLATON (Spek, 2003)' _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^)+(0.0559P)^2^+0.2155P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3900 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Ni1 Ni 0.5000 0.0000 0.0000 0.01461(12) Uani 1 2 d S . . S1 S 0.29237(9) 0.16214(7) 0.04672(5) 0.02045(15) Uani 1 1 d . . . S2 S 0.69756(8) 0.01687(6) 0.14874(5) 0.01917(15) Uani 1 1 d . . . P1 P 0.45893(9) 0.10603(7) 0.17842(5) 0.01739(15) Uani 1 1 d . . . O1 O 0.5140(3) 0.22985(18) 0.21133(15) 0.0247(4) Uani 1 1 d . . . C8 C 0.6415(5) 0.3377(3) 0.1344(3) 0.0384(7) Uani 1 1 d . . . H8A H 0.6028 0.3650 0.0557 0.046 Uiso 1 1 calc R . . H8B H 0.7765 0.3056 0.1384 0.046 Uiso 1 1 calc R . . C9 C 0.6276(6) 0.4557(3) 0.1677(3) 0.0505(9) Uani 1 1 d . . . H9A H 0.7135 0.5294 0.1167 0.076 Uiso 1 1 calc R . . H9B H 0.6663 0.4278 0.2457 0.076 Uiso 1 1 calc R . . H9C H 0.4939 0.4874 0.1627 0.076 Uiso 1 1 calc R . . C1 C 0.3319(4) -0.0042(3) 0.3082(2) 0.0186(5) Uani 1 1 d . . . C2 C 0.1331(4) -0.0252(3) 0.3155(2) 0.0237(6) Uani 1 1 d . . . H2A H 0.0606 0.0201 0.2508 0.028 Uiso 1 1 calc R . . C3 C 0.0391(4) -0.1117(3) 0.4162(2) 0.0261(6) Uani 1 1 d . . . H3A H -0.0968 -0.1265 0.4199 0.031 Uiso 1 1 calc R . . C4 C 0.1427(4) -0.1762(3) 0.5109(2) 0.0258(6) Uani 1 1 d . . . C5 C 0.3439(4) -0.1554(3) 0.5043(2) 0.0307(6) Uani 1 1 d . . . H5A H 0.4162 -0.1995 0.5693 0.037 Uiso 1 1 calc R . . C6 C 0.4356(4) -0.0714(3) 0.4043(2) 0.0263(6) Uani 1 1 d . . . H6A H 0.5720 -0.0586 0.4001 0.032 Uiso 1 1 calc R . . O2 O 0.0658(3) -0.2620(2) 0.61422(16) 0.0361(5) Uani 1 1 d . . . C7 C -0.1399(4) -0.2777(3) 0.6271(3) 0.0381(8) Uani 1 1 d . . . H7A H -0.1776 -0.3416 0.7044 0.057 Uiso 1 1 calc R . . H7B H -0.1846 -0.3129 0.5730 0.057 Uiso 1 1 calc R . . H7C H -0.1988 -0.1894 0.6127 0.057 Uiso 1 1 calc R . . N1' N 0.3330(3) -0.1659(2) 0.12349(16) 0.0164(4) Uani 1 1 d . . . C2' C 0.4137(3) -0.2501(2) 0.21635(19) 0.0165(5) Uani 1 1 d . . . H2'A H 0.5497 -0.2433 0.2203 0.020 Uiso 1 1 calc R . . C3' C 0.3101(3) -0.3479(2) 0.30835(19) 0.0157(5) Uani 1 1 d . . . C4' C 0.1106(3) -0.3604(3) 0.3016(2) 0.0204(5) Uani 1 1 d . . . H4'A H 0.0343 -0.4246 0.3628 0.024 Uiso 1 1 calc R . . C5' C 0.0280(4) -0.2770(3) 0.2035(2) 0.0216(5) Uani 1 1 d . . . H5'A H -0.1061 -0.2858 0.1951 0.026 Uiso 1 1 calc R . . C6' C 0.1405(3) -0.1804(3) 0.1176(2) 0.0193(5) Uani 1 1 d . . . H6'A H 0.0801 -0.1219 0.0516 0.023 Uiso 1 1 calc R . . C7' C 0.4109(3) -0.4298(2) 0.4105(2) 0.0170(5) Uani 1 1 d . . . N8' N 0.6067(3) -0.4243(2) 0.40347(17) 0.0221(5) Uani 1 1 d . . . N9' N 0.6969(3) -0.4962(2) 0.49581(17) 0.0219(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 Ni1 0.0113(2) 0.0180(2) 0.0126(2) -0.00362(18) -0.00378(16) -0.00059(16) S1 0.0172(3) 0.0242(3) 0.0188(3) -0.0066(3) -0.0068(2) 0.0040(2) S2 0.0131(3) 0.0261(3) 0.0173(3) -0.0071(3) -0.0046(2) 0.0003(2) P1 0.0147(3) 0.0209(3) 0.0166(3) -0.0071(3) -0.0043(2) 0.0001(2) O1 0.0274(10) 0.0248(10) 0.0220(9) -0.0093(8) -0.0022(8) -0.0054(8) C8 0.0457(19) 0.0313(16) 0.0358(17) -0.0109(14) 0.0012(14) -0.0160(14) C9 0.077(3) 0.0283(17) 0.042(2) -0.0092(15) -0.0082(18) -0.0129(17) C1 0.0162(12) 0.0238(13) 0.0175(12) -0.0098(10) -0.0024(9) 0.0015(10) C2 0.0158(13) 0.0297(14) 0.0271(14) -0.0125(12) -0.0051(10) 0.0017(10) C3 0.0147(13) 0.0330(15) 0.0322(15) -0.0150(12) 0.0001(11) -0.0012(11) C4 0.0245(14) 0.0294(14) 0.0245(14) -0.0126(12) 0.0047(11) -0.0033(11) C5 0.0222(14) 0.0442(17) 0.0215(14) -0.0084(13) -0.0055(11) 0.0030(12) C6 0.0151(13) 0.0368(15) 0.0242(14) -0.0091(12) -0.0035(10) 0.0001(11) O2 0.0291(11) 0.0435(13) 0.0266(11) -0.0056(9) 0.0081(9) -0.0063(9) C7 0.0299(16) 0.0401(18) 0.0426(18) -0.0171(15) 0.0187(14) -0.0144(13) N1' 0.0132(10) 0.0190(10) 0.0160(10) -0.0057(8) -0.0031(8) -0.0002(8) C2' 0.0125(11) 0.0189(12) 0.0172(12) -0.0059(10) -0.0033(9) -0.0001(9) C3' 0.0145(11) 0.0181(12) 0.0141(11) -0.0059(10) -0.0021(9) 0.0013(9) C4' 0.0144(12) 0.0240(13) 0.0183(12) -0.0039(10) 0.0003(10) -0.0032(10) C5' 0.0109(12) 0.0269(14) 0.0236(13) -0.0060(11) -0.0040(10) 0.0003(10) C6' 0.0144(12) 0.0233(13) 0.0182(12) -0.0056(10) -0.0059(10) 0.0021(10) C7' 0.0133(12) 0.0179(12) 0.0197(12) -0.0070(10) -0.0041(9) -0.0001(9) N8' 0.0135(10) 0.0277(12) 0.0176(10) -0.0008(9) -0.0031(8) -0.0011(9) N9' 0.0147(10) 0.0267(11) 0.0169(10) -0.0005(9) -0.0044(8) 0.0002(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 Ni1 N1' 2.1459(19) . ? Ni1 N1' 2.1459(19) 2_655 ? Ni1 S2 2.4806(6) 2_655 ? Ni1 S2 2.4806(6) . ? Ni1 S1 2.4815(7) 2_655 ? Ni1 S1 2.4815(7) . ? S1 P1 1.9918(9) . ? S2 P1 1.9965(9) . ? P1 O1 1.6021(19) . ? P1 C1 1.801(3) . ? O1 C8 1.450(3) . ? C8 C9 1.492(5) . ? C1 C2 1.387(3) . ? C1 C6 1.396(3) . ? C2 C3 1.388(4) . ? C3 C4 1.378(4) . ? C4 O2 1.362(3) . ? C4 C5 1.405(4) . ? C5 C6 1.367(4) . ? O2 C7 1.427(3) . ? N1' C2' 1.329(3) . ? N1' C6' 1.352(3) . ? C2' C3' 1.395(3) . ? C3' C4' 1.398(3) . ? C3' C7' 1.471(3) . ? C4' C5' 1.377(3) . ? C5' C6' 1.381(3) . ? C7' N9' 1.338(3) 2_646 ? C7' N8' 1.353(3) . ? N8' N9' 1.321(3) . ? N9' C7' 1.338(3) 2_646 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1' Ni1 N1' 180.00(17) . 2_655 ? N1' Ni1 S2 88.77(5) . 2_655 ? N1' Ni1 S2 91.23(5) 2_655 2_655 ? N1' Ni1 S2 91.23(5) . . ? N1' Ni1 S2 88.77(5) 2_655 . ? S2 Ni1 S2 180.00(3) 2_655 . ? N1' Ni1 S1 90.39(6) . 2_655 ? N1' Ni1 S1 89.61(6) 2_655 2_655 ? S2 Ni1 S1 82.61(2) 2_655 2_655 ? S2 Ni1 S1 97.39(2) . 2_655 ? N1' Ni1 S1 89.61(6) . . ? N1' Ni1 S1 90.39(6) 2_655 . ? S2 Ni1 S1 97.39(2) 2_655 . ? S2 Ni1 S1 82.61(2) . . ? S1 Ni1 S1 180.00(4) 2_655 . ? P1 S1 Ni1 81.61(3) . . ? P1 S2 Ni1 81.54(3) . . ? O1 P1 C1 100.10(10) . . ? O1 P1 S1 112.68(8) . . ? C1 P1 S1 112.24(8) . . ? O1 P1 S2 110.61(8) . . ? C1 P1 S2 110.40(9) . . ? S1 P1 S2 110.42(4) . . ? C8 O1 P1 119.20(17) . . ? O1 C8 C9 108.4(3) . . ? C2 C1 C6 118.7(2) . . ? C2 C1 P1 121.84(19) . . ? C6 C1 P1 119.44(19) . . ? C1 C2 C3 120.7(2) . . ? C4 C3 C2 120.1(2) . . ? O2 C4 C3 125.2(2) . . ? O2 C4 C5 115.2(2) . . ? C3 C4 C5 119.6(2) . . ? C6 C5 C4 119.9(3) . . ? C5 C6 C1 121.0(2) . . ? C4 O2 C7 117.0(2) . . ? C2' N1' C6' 117.3(2) . . ? C2' N1' Ni1 119.88(16) . . ? C6' N1' Ni1 122.43(16) . . ? N1' C2' C3' 123.8(2) . . ? C2' C3' C4' 118.2(2) . . ? C2' C3' C7' 119.5(2) . . ? C4' C3' C7' 122.2(2) . . ? C5' C4' C3' 118.1(2) . . ? C4' C5' C6' 119.9(2) . . ? N1' C6' C5' 122.7(2) . . ? N9' C7' N8' 124.4(2) 2_646 . ? N9' C7' C3' 118.0(2) 2_646 . ? N8' C7' C3' 117.6(2) . . ? N9' N8' C7' 117.5(2) . . ? N8' N9' C7' 118.0(2) . 2_646 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.714 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.088