# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Montserrat Monfort' 'Inmaculada Resino' 'Joan Ribas' 'Xavier Solans' 'Mercé Font-Bardia' 'Helen Stoeckli-Evans' _publ_contact_author_name 'Dr Montserrat Monfort' _publ_contact_author_address ; Quimica Inorganica Universitat de Barcelona Marti i Franques 1-11 Barcelona 08028 SPAIN ; _publ_contact_author_email 'MONTSERRAT.MONFORT@QI.UB.ES' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; New Four NiII Antiferromagnetic Complexes with Azido Bridges ; data_for_Compound1 _database_code_CSD 186790 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'trans-[Ni(N-Pren)2(mu1,3-N3)]n(ClO4)n' _chemical_formula_sum 'C10 H28 Cl N7 Ni O4' _chemical_formula_weight 404.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1320 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.2850 1.1130 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(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 8.3715(7) _cell_length_b 18.4000(12) _cell_length_c 12.2042(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.958(10) _cell_angle_gamma 90.00 _cell_volume 1869.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.97 _exptl_crystal_description plate _exptl_crystal_colour 'pale purple-blus' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6277 _exptl_absorpt_correction_T_max 0.8944 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'STOE Image Plate Diffraction system' _diffrn_measurement_method 'Phi rotation' _diffrn_detector_area_resol_mean 0.81 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14522 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.97 _reflns_number_total 3628 _reflns_number_gt 1986 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie GmbH, Darmstadt, 1996)' _computing_cell_refinement 'CELL (Stoe & Cie GmbH, Darmstadt, 1996)' _computing_data_reduction 'INTEGRATE (Stoe & Cie GmbH, Darmstadt, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Xtal_GX (Hall & du Boulay, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3628 _refine_ls_number_parameters 231 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 0.801 _refine_ls_restrained_S_all 0.813 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.14304(5) 0.27188(3) 0.86736(3) 0.05287(16) Uani 1 d . . . N1 N 0.2478(4) 0.3756(2) 0.9014(3) 0.0807(10) Uani 1 d . . . H1N1 H 0.3180 0.3691 0.9627 0.121 Uiso 1 calc R . . N2 N -0.0728(3) 0.3276(2) 0.8761(3) 0.0738(10) Uani 1 d . . . H2AN H -0.1440 0.3158 0.8185 0.111 Uiso 1 calc R . . H2BN H -0.1152 0.3161 0.9386 0.111 Uiso 1 calc R . . N3 N 0.0371(4) 0.16827(18) 0.8368(2) 0.0665(8) Uani 1 d . . . H3N3 H -0.0365 0.1734 0.7770 0.100 Uiso 1 calc R . . N4 N 0.3574(3) 0.2152(2) 0.8585(2) 0.0690(9) Uani 1 d . . . H4AN H 0.3954 0.2233 0.7933 0.103 Uiso 1 calc R . . H4BN H 0.4318 0.2297 0.9126 0.103 Uiso 1 calc R . . N5 N 0.1094(5) 0.2945(2) 0.6968(2) 0.0915(12) Uani 1 d . . . N6 N 0.1436(3) 0.26769(17) 0.61816(19) 0.0528(7) Uani 1 d . . . N7 N 0.1776(5) 0.2591(2) 1.0409(2) 0.1091(16) Uani 1 d . . . C1 C 0.1133(7) 0.4204(3) 0.9391(5) 0.123(2) Uani 1 d . . . H1A H 0.1024 0.4098 1.0158 0.148 Uiso 1 calc R . . H1B H 0.1385 0.4716 0.9332 0.148 Uiso 1 calc R . . C2 C -0.0352(6) 0.4050(3) 0.8739(5) 0.1136(18) Uani 1 d . . . H2A H -0.0278 0.4202 0.7985 0.136 Uiso 1 calc R . . H2B H -0.1211 0.4325 0.9021 0.136 Uiso 1 calc R . . C3 C 0.3410(8) 0.4092(5) 0.8219(5) 0.152(3) Uani 1 d D . . H3A H 0.2670 0.4360 0.7704 0.183 Uiso 0.50 calc PR A 1 H3B H 0.3857 0.3705 0.7806 0.183 Uiso 0.50 calc PR A 1 H3C H 0.2794 0.4021 0.7509 0.183 Uiso 0.50 d PR A 2 H3D H 0.3382 0.4610 0.8365 0.183 Uiso 0.50 d PR A 2 C4A C 0.4719(17) 0.4581(10) 0.8591(16) 0.183(9) Uani 0.564(18) d PD B 1 H4A H 0.5413 0.4370 0.9194 0.220 Uiso 0.564(18) calc PR B 1 H4B H 0.4317 0.5045 0.8824 0.220 Uiso 0.564(18) calc PR B 1 C5A C 0.557(4) 0.466(2) 0.760(3) 0.34(3) Uani 0.564(18) d PD B 1 H5A H 0.5694 0.4194 0.7270 0.505 Uiso 0.564(18) calc PR B 1 H5B H 0.6607 0.4874 0.7796 0.505 Uiso 0.564(18) calc PR B 1 H5C H 0.4957 0.4972 0.7077 0.505 Uiso 0.564(18) calc PR B 1 C4B C 0.4812(14) 0.3933(11) 0.8053(12) 0.106(7) Uani 0.436(18) d PD B 2 H4C H 0.4785 0.3480 0.7645 0.128 Uiso 0.436(18) calc PR B 2 H4D H 0.5423 0.3847 0.8760 0.128 Uiso 0.436(18) calc PR B 2 C5B C 0.571(3) 0.450(2) 0.743(2) 0.23(2) Uani 0.436(18) d PD B 2 H5D H 0.5103 0.4604 0.6737 0.339 Uiso 0.436(18) calc PR B 2 H5E H 0.6743 0.4306 0.7298 0.339 Uiso 0.436(18) calc PR B 2 H5F H 0.5854 0.4933 0.7859 0.339 Uiso 0.436(18) calc PR B 2 C6 C 0.1668(5) 0.1213(2) 0.8017(3) 0.0827(12) Uani 1 d . . . H6A H 0.1791 0.1299 0.7246 0.099 Uiso 1 calc R . . H6B H 0.1393 0.0706 0.8105 0.099 Uiso 1 calc R . . C7 C 0.3213(5) 0.1383(3) 0.8708(4) 0.0875(14) Uani 1 d . . . H7A H 0.3111 0.1273 0.9474 0.105 Uiso 1 calc R . . H7B H 0.4076 0.1089 0.8470 0.105 Uiso 1 calc R . . C8 C -0.0501(5) 0.1374(3) 0.9258(3) 0.0878(14) Uani 1 d . . . H8A H 0.0289 0.1198 0.9835 0.105 Uiso 1 calc R . . H8B H -0.1083 0.1766 0.9571 0.105 Uiso 1 calc R . . C9 C -0.1631(7) 0.0788(3) 0.8964(5) 0.129(2) Uani 1 d . . . H9A H -0.1056 0.0372 0.8712 0.154 Uiso 1 calc R . . H9B H -0.2403 0.0945 0.8362 0.154 Uiso 1 calc R . . C10 C -0.2520(6) 0.0562(4) 0.9940(5) 0.148(3) Uani 1 d . . . H10A H -0.3172 0.0143 0.9743 0.222 Uiso 1 calc R . . H10B H -0.3191 0.0955 1.0134 0.222 Uiso 1 calc R . . H10C H -0.1755 0.0446 1.0556 0.222 Uiso 1 calc R . . Cl1 Cl 0.65329(10) 0.30700(7) 1.12008(7) 0.0743(3) Uani 1 d . . . O1 O 0.7900(4) 0.3527(2) 1.1176(3) 0.1155(12) Uani 1 d . . . O2 O 0.5132(4) 0.3483(2) 1.1259(3) 0.1259(13) Uani 1 d . . . O3 O 0.6359(4) 0.2679(3) 1.0208(3) 0.1439(17) Uani 1 d . . . O4 O 0.6742(5) 0.2644(2) 1.2156(3) 0.1313(14) Uani 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 0.0532(2) 0.0769(3) 0.02889(18) -0.0019(2) 0.00586(14) -0.0037(2) N1 0.076(2) 0.092(3) 0.075(2) -0.0042(19) 0.0078(17) -0.021(2) N2 0.0611(19) 0.092(3) 0.070(2) -0.0189(18) 0.0166(15) -0.0010(17) N3 0.0692(19) 0.077(2) 0.0502(15) 0.0052(15) -0.0102(13) -0.0033(16) N4 0.0602(17) 0.084(3) 0.0636(18) 0.0115(17) 0.0082(13) 0.0019(16) N5 0.132(3) 0.109(3) 0.0330(16) 0.0025(17) 0.0063(17) 0.035(2) N6 0.0574(15) 0.073(2) 0.0280(13) 0.0056(15) 0.0021(10) 0.0019(15) N7 0.124(3) 0.174(5) 0.0289(15) 0.0090(19) 0.0027(16) -0.072(3) C1 0.124(5) 0.091(4) 0.152(5) -0.047(4) 0.001(4) -0.001(3) C2 0.096(4) 0.096(5) 0.148(5) -0.032(4) 0.011(3) 0.008(3) C3 0.150(6) 0.190(7) 0.114(4) 0.052(5) -0.004(4) -0.091(6) C4A 0.158(13) 0.119(15) 0.29(2) 0.064(14) 0.092(13) -0.006(10) C5A 0.19(3) 0.29(4) 0.55(7) 0.22(4) 0.10(4) 0.03(3) C4B 0.079(8) 0.129(16) 0.118(10) 0.044(9) 0.043(7) 0.028(8) C5B 0.092(14) 0.35(5) 0.24(3) 0.24(3) 0.051(16) 0.01(2) C6 0.105(3) 0.064(3) 0.077(3) 0.002(2) 0.000(2) 0.005(2) C7 0.078(3) 0.089(4) 0.093(3) 0.020(3) -0.004(2) 0.015(3) C8 0.081(3) 0.103(4) 0.074(3) 0.021(3) -0.014(2) -0.027(3) C9 0.120(4) 0.130(5) 0.125(4) 0.045(4) -0.043(3) -0.052(4) C10 0.108(4) 0.158(6) 0.171(6) 0.093(5) -0.014(4) -0.049(4) Cl1 0.0532(5) 0.1146(10) 0.0540(5) -0.0052(5) 0.0007(4) 0.0001(5) O1 0.086(2) 0.171(4) 0.090(2) -0.006(2) 0.0093(16) -0.041(2) O2 0.083(2) 0.170(4) 0.125(3) 0.008(3) 0.0139(19) 0.037(2) O3 0.114(3) 0.217(5) 0.103(3) -0.083(3) 0.023(2) -0.040(3) O4 0.123(3) 0.159(4) 0.112(3) 0.056(3) 0.012(2) 0.016(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 Ni1 N4 2.088(3) . ? Ni1 N2 2.090(3) . ? Ni1 N5 2.113(3) . ? Ni1 N3 2.119(3) . ? Ni1 N7 2.121(3) . ? Ni1 N1 2.124(4) . ? N1 C3 1.446(6) . ? N1 C1 1.505(6) . ? N2 C2 1.460(6) . ? N3 C8 1.484(5) . ? N3 C6 1.485(5) . ? N4 C7 1.457(5) . ? N5 N6 1.141(4) . ? N6 N7 1.126(4) 4_565 ? N7 N6 1.126(4) 4_566 ? C1 C2 1.433(7) . ? C3 C4B 1.246(10) . ? C3 C4A 1.454(14) . ? C4A C5A 1.477(18) . ? C4B C5B 1.531(17) . ? C6 C7 1.501(6) . ? C8 C9 1.456(6) . ? C9 C10 1.526(7) . ? Cl1 O4 1.401(3) . ? Cl1 O3 1.404(3) . ? Cl1 O2 1.405(3) . ? Cl1 O1 1.423(3) . ? 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 N4 Ni1 N2 179.39(14) . . ? N4 Ni1 N5 94.28(13) . . ? N2 Ni1 N5 85.77(13) . . ? N4 Ni1 N3 83.55(13) . . ? N2 Ni1 N3 95.84(13) . . ? N5 Ni1 N3 89.60(14) . . ? N4 Ni1 N7 88.13(15) . . ? N2 Ni1 N7 91.87(16) . . ? N5 Ni1 N7 175.03(17) . . ? N3 Ni1 N7 95.00(13) . . ? N4 Ni1 N1 96.87(14) . . ? N2 Ni1 N1 83.73(14) . . ? N5 Ni1 N1 91.48(15) . . ? N3 Ni1 N1 178.81(12) . . ? N7 Ni1 N1 83.91(14) . . ? C3 N1 C1 116.4(5) . . ? C3 N1 Ni1 119.6(4) . . ? C1 N1 Ni1 104.2(3) . . ? C2 N2 Ni1 106.8(3) . . ? C8 N3 C6 114.7(3) . . ? C8 N3 Ni1 116.4(3) . . ? C6 N3 Ni1 105.6(2) . . ? C7 N4 Ni1 106.9(2) . . ? N6 N5 Ni1 136.4(3) . . ? N7 N6 N5 179.6(4) 4_565 . ? N6 N7 Ni1 149.8(3) 4_566 . ? C2 C1 N1 110.8(4) . . ? C1 C2 N2 111.0(5) . . ? C4B C3 N1 126.3(8) . . ? C4B C3 C4A 60.3(8) . . ? N1 C3 C4A 119.8(8) . . ? C3 C4A C5A 102.6(19) . . ? C3 C4B C5B 116.2(16) . . ? N3 C6 C7 109.3(4) . . ? N4 C7 C6 108.7(3) . . ? C9 C8 N3 117.3(4) . . ? C8 C9 C10 111.4(5) . . ? O4 Cl1 O3 115.1(3) . . ? O4 Cl1 O2 107.0(2) . . ? O3 Cl1 O2 108.0(2) . . ? O4 Cl1 O1 108.5(2) . . ? O3 Cl1 O1 107.2(2) . . ? O2 Cl1 O1 111.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Ni1 N1 C3 61.9(4) . . . . ? N2 Ni1 N1 C3 -118.2(4) . . . . ? N5 Ni1 N1 C3 -32.6(4) . . . . ? N3 Ni1 N1 C3 173(6) . . . . ? N7 Ni1 N1 C3 149.3(4) . . . . ? N4 Ni1 N1 C1 -166.0(3) . . . . ? N2 Ni1 N1 C1 13.9(3) . . . . ? N5 Ni1 N1 C1 99.5(3) . . . . ? N3 Ni1 N1 C1 -55(6) . . . . ? N7 Ni1 N1 C1 -78.6(3) . . . . ? N4 Ni1 N2 C2 -174(100) . . . . ? N5 Ni1 N2 C2 -79.0(3) . . . . ? N3 Ni1 N2 C2 -168.2(3) . . . . ? N7 Ni1 N2 C2 96.6(3) . . . . ? N1 Ni1 N2 C2 12.9(3) . . . . ? N4 Ni1 N3 C8 115.8(3) . . . . ? N2 Ni1 N3 C8 -64.2(3) . . . . ? N5 Ni1 N3 C8 -149.9(3) . . . . ? N7 Ni1 N3 C8 28.2(3) . . . . ? N1 Ni1 N3 C8 5(6) . . . . ? N4 Ni1 N3 C6 -12.8(2) . . . . ? N2 Ni1 N3 C6 167.3(2) . . . . ? N5 Ni1 N3 C6 81.6(2) . . . . ? N7 Ni1 N3 C6 -100.3(3) . . . . ? N1 Ni1 N3 C6 -124(6) . . . . ? N2 Ni1 N4 C7 -11(11) . . . . ? N5 Ni1 N4 C7 -106.0(3) . . . . ? N3 Ni1 N4 C7 -16.9(2) . . . . ? N7 Ni1 N4 C7 78.4(3) . . . . ? N1 Ni1 N4 C7 162.0(3) . . . . ? N4 Ni1 N5 N6 28.4(5) . . . . ? N2 Ni1 N5 N6 -151.0(5) . . . . ? N3 Ni1 N5 N6 -55.1(5) . . . . ? N7 Ni1 N5 N6 147.3(16) . . . . ? N1 Ni1 N5 N6 125.4(5) . . . . ? Ni1 N5 N6 N7 8(70) . . . 4_565 ? N4 Ni1 N7 N6 -106.9(8) . . . 4_566 ? N2 Ni1 N7 N6 72.5(8) . . . 4_566 ? N5 Ni1 N7 N6 133.9(15) . . . 4_566 ? N3 Ni1 N7 N6 -23.6(8) . . . 4_566 ? N1 Ni1 N7 N6 156.0(8) . . . 4_566 ? C3 N1 C1 C2 93.5(6) . . . . ? Ni1 N1 C1 C2 -40.4(6) . . . . ? N1 C1 C2 N2 56.1(7) . . . . ? Ni1 N2 C2 C1 -40.1(5) . . . . ? C1 N1 C3 C4B 156.5(14) . . . . ? Ni1 N1 C3 C4B -76.9(14) . . . . ? C1 N1 C3 C4A 83.2(12) . . . . ? Ni1 N1 C3 C4A -150.2(10) . . . . ? C4B C3 C4A C5A 50(2) . . . . ? N1 C3 C4A C5A 167.4(18) . . . . ? N1 C3 C4B C5B -162.6(18) . . . . ? C4A C3 C4B C5B -56(2) . . . . ? C8 N3 C6 C7 -89.4(4) . . . . ? Ni1 N3 C6 C7 40.1(4) . . . . ? Ni1 N4 C7 C6 43.7(4) . . . . ? N3 C6 C7 N4 -57.9(5) . . . . ? C6 N3 C8 C9 -74.3(5) . . . . ? Ni1 N3 C8 C9 161.8(4) . . . . ? N3 C8 C9 C10 -176.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.430 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.052 data_for_compound2 _database_code_CSD 186791 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'trans-[Ni (N,N-Me2en)2(mu1,3-N3)]n(PF6)n' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C8 H24 F6 N7 Ni P' _chemical_formula_weight 422.02 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.385(21) _cell_length_b 8.841(36) _cell_length_c 9.102(7) _cell_angle_alpha 116.77(22) _cell_angle_beta 91.86(19) _cell_angle_gamma 109.07(27) _cell_volume 423.6(22) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method ? _exptl_crystal_F_000 218 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1770 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 29.96 _reflns_number_total 1770 _reflns_number_observed 1566 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 50 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0695P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(142) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1720 _refine_ls_number_parameters 111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_obs 0.0542 _refine_ls_wR_factor_all 0.1599 _refine_ls_wR_factor_obs 0.1262 _refine_ls_goodness_of_fit_all 0.984 _refine_ls_goodness_of_fit_obs 1.028 _refine_ls_restrained_S_all 1.269 _refine_ls_restrained_S_obs 1.028 _refine_ls_shift/esd_max -8.520 _refine_ls_shift/esd_mean 0.079 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.0000 0.0000 0.0000 0.0197(3) Uani 1 d S . N1 N 0.1802(6) 0.2952(5) 0.1669(5) 0.0396(8) Uani 1 d . . N2 N 0.0410(7) 0.0703(6) -0.1905(5) 0.0528(10) Uani 1 d . . H1N H 0.1198(7) 0.0120(6) -0.2594(5) 0.649(67) Uiso 1 calc R . H1NA H -0.0952(7) 0.0373(6) -0.2519(5) 0.649(67) Uiso 1 calc R . N3 N 0.3034(6) -0.0506(6) -0.0197(5) 0.0482(9) Uani 1 d . . N4 N 0.5000 0.0000 0.0000 0.0337(10) Uani 1 d S . C1 C 0.1338(9) 0.3758(7) 0.0670(7) 0.0572(13) Uani 1 d . . H1 H 0.2325(9) 0.5045(7) 0.1210(7) 0.649(67) Uiso 1 calc R . H1A H -0.0219(9) 0.3674(7) 0.0612(7) 0.649(67) Uiso 1 calc R . C2 C 0.1706(10) 0.2799(8) -0.1065(7) 0.0651(15) Uani 1 d . . H2 H 0.3314(10) 0.3070(8) -0.1019(7) 0.649(67) Uiso 1 calc R . H3A H 0.1203(10) 0.3254(8) -0.1743(7) 0.649(67) Uiso 1 calc R . C3 C 0.0941(9) 0.3672(8) 0.3251(7) 0.0619(14) Uani 1 d . . H3 H 0.1242(9) 0.3150(8) 0.3918(7) 0.649(67) Uiso 1 calc R . H3A' H -0.0664(9) 0.3346(8) 0.2972(7) 0.649(67) Uiso 1 calc R . H3B H 0.1691(9) 0.4983(8) 0.3879(7) 0.649(67) Uiso 1 calc R . C4 C 0.4293(9) 0.3602(8) 0.2307(7) 0.0647(15) Uani 1 d . . H4 H 0.4539(9) 0.3049(8) 0.2959(7) 0.649(67) Uiso 1 calc R . H4A H 0.4913(9) 0.4911(8) 0.3000(7) 0.649(67) Uiso 1 calc R . H4B H 0.5025(9) 0.3262(8) 0.1371(7) 0.649(67) Uiso 1 calc R . P1 P 0.5000 0.0000 0.5000 0.0466(4) Uani 1 d S . F1 F 0.2665(9) -0.1288(8) 0.4997(8) 0.146(2) Uani 1 d . . F2 F 0.3755(9) 0.1406(7) 0.5140(6) 0.121(2) Uani 1 d . . F3 F 0.4268(8) -0.1156(7) 0.3014(5) 0.114(2) Uani 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 0.0147(3) 0.0202(4) 0.0223(4) 0.0098(3) 0.0039(2) 0.0054(2) N1 0.032(2) 0.040(2) 0.043(2) 0.018(2) 0.0115(15) 0.012(2) N2 0.046(2) 0.052(2) 0.051(2) 0.025(2) 0.009(2) 0.008(2) N3 0.035(2) 0.051(2) 0.058(2) 0.027(2) 0.009(2) 0.015(2) N4 0.030(2) 0.033(2) 0.039(3) 0.018(2) 0.010(2) 0.013(2) C1 0.059(3) 0.053(3) 0.056(3) 0.023(3) 0.017(2) 0.022(3) C2 0.067(4) 0.056(3) 0.064(3) 0.026(3) 0.021(3) 0.019(3) C3 0.059(3) 0.055(3) 0.060(3) 0.021(3) 0.015(3) 0.017(3) C4 0.050(3) 0.058(3) 0.072(4) 0.026(3) 0.005(3) 0.011(3) P1 0.0411(9) 0.0477(10) 0.0472(10) 0.0227(9) 0.0087(8) 0.0132(8) F1 0.108(4) 0.133(5) 0.185(6) 0.081(4) 0.048(4) 0.029(4) F2 0.126(4) 0.112(4) 0.114(4) 0.044(3) 0.015(3) 0.052(3) F3 0.113(4) 0.127(4) 0.092(3) 0.049(3) 0.013(3) 0.040(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 N2 2.087(5) . ? Ni1 N2 2.087(5) 2 ? Ni1 N3 2.122(8) . ? Ni1 N3 2.122(8) 2 ? Ni1 N1 2.190(12) 2 ? Ni1 N1 2.190(12) . ? N1 C1 1.459(7) . ? N1 C4 1.496(9) . ? N1 C3 1.495(7) . ? N2 C2 1.544(11) . ? N2 H1N 0.90 . ? N2 H1NA 0.90 . ? N3 N4 1.164(6) . ? N4 N3 1.164(6) 2_655 ? C1 C2 1.489(8) . ? C1 H1 0.97 . ? C1 H1A 0.97 . ? C2 H2 0.97 . ? C2 H3A 0.97 . ? C3 H3 0.96 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C4 H4 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? P1 F1 1.551(8) 2_656 ? P1 F1 1.551(8) . ? P1 F3 1.581(6) . ? P1 F3 1.581(6) 2_656 ? P1 F2 1.644(8) . ? P1 F2 1.644(8) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N2 180.0 . 2 ? N2 Ni1 N3 90.0(2) . . ? N2 Ni1 N3 90.0(2) 2 . ? N2 Ni1 N3 90.0(2) . 2 ? N2 Ni1 N3 90.0(2) 2 2 ? N3 Ni1 N3 180.0 . 2 ? N2 Ni1 N1 96.2(3) . 2 ? N2 Ni1 N1 83.8(3) 2 2 ? N3 Ni1 N1 86.7(4) . 2 ? N3 Ni1 N1 93.3(4) 2 2 ? N2 Ni1 N1 83.8(3) . . ? N2 Ni1 N1 96.2(3) 2 . ? N3 Ni1 N1 93.3(4) . . ? N3 Ni1 N1 86.7(4) 2 . ? N1 Ni1 N1 180.0 2 . ? C1 N1 C4 111.6(4) . . ? C1 N1 C3 108.9(4) . . ? C4 N1 C3 103.0(5) . . ? C1 N1 Ni1 103.6(4) . . ? C4 N1 Ni1 116.5(5) . . ? C3 N1 Ni1 113.2(4) . . ? C2 N2 Ni1 107.9(4) . . ? C2 N2 H1N 110.1(4) . . ? Ni1 N2 H1N 110.1(2) . . ? C2 N2 H1NA 110.1(4) . . ? Ni1 N2 H1NA 110.1(2) . . ? H1N N2 H1NA 108.4 . . ? N4 N3 Ni1 151.4(4) . . ? N3 N4 N3 180.0 2_655 . ? N1 C1 C2 111.0(5) . . ? N1 C1 H1 109.4(4) . . ? C2 C1 H1 109.4(4) . . ? N1 C1 H1A 109.4(3) . . ? C2 C1 H1A 109.4(4) . . ? H1 C1 H1A 108.0 . . ? C1 C2 N2 111.7(5) . . ? C1 C2 H2 109.3(4) . . ? N2 C2 H2 109.3(4) . . ? C1 C2 H3A 109.3(4) . . ? N2 C2 H3A 109.3(4) . . ? H2 C2 H3A 107.9 . . ? N1 C3 H3 109.5(3) . . ? N1 C3 H3A 109.5(4) . . ? H3 C3 H3A 109.5 . . ? N1 C3 H3B 109.5(4) . . ? H3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C4 H4 109.5(3) . . ? N1 C4 H4A 109.5(4) . . ? H4 C4 H4A 109.5 . . ? N1 C4 H4B 109.5(4) . . ? H4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? F1 P1 F1 180.0 2_656 . ? F1 P1 F3 94.1(5) 2_656 . ? F1 P1 F3 85.9(5) . . ? F1 P1 F3 85.9(5) 2_656 2_656 ? F1 P1 F3 94.1(5) . 2_656 ? F3 P1 F3 180.000(1) . 2_656 ? F1 P1 F2 93.4(4) 2_656 . ? F1 P1 F2 86.6(4) . . ? F3 P1 F2 93.9(3) . . ? F3 P1 F2 86.1(4) 2_656 . ? F1 P1 F2 86.6(4) 2_656 2_656 ? F1 P1 F2 93.4(4) . 2_656 ? F3 P1 F2 86.1(4) . 2_656 ? F3 P1 F2 93.9(3) 2_656 2_656 ? F2 P1 F2 180.000(1) . 2_656 ? _refine_diff_density_max 1.360 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.120 data_for_compound_3 _database_code_CSD 186792 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; trans-[Ni (N,N'-Pren)2(mu1,3-N3)]n(PF6)n ; _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H32 F6 N7 Ni P' _chemical_formula_weight 526.17 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 11.258(3) _cell_length_b 12.380(10) _cell_length_c 18.941(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.43(2) _cell_angle_gamma 90.00 _cell_volume 2567.7(23) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method ? _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.877 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7161 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.1384 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 29.98 _reflns_number_total 6879 _reflns_number_observed 2297 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2060 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4826P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4819 _refine_ls_number_parameters 372 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2190 _refine_ls_R_factor_obs 0.0611 _refine_ls_wR_factor_all 0.2485 _refine_ls_wR_factor_obs 0.1466 _refine_ls_goodness_of_fit_all 1.006 _refine_ls_goodness_of_fit_obs 1.137 _refine_ls_restrained_S_all 1.100 _refine_ls_restrained_S_obs 1.150 _refine_ls_shift/esd_max 0.356 _refine_ls_shift/esd_mean 0.024 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.0000 0.5000 0.0000 0.0443(3) Uani 1 d S . Ni2 Ni 0.0000 1.0000 0.0000 0.0454(3) Uani 1 d S . N1 N 0.0468(5) 0.6622(4) 0.0307(3) 0.066(2) Uani 1 d . . N2 N 0.0152(4) 0.7474(4) 0.0086(2) 0.0487(12) Uani 1 d . . N3 N -0.0185(5) 0.8323(4) -0.0150(3) 0.071(2) Uani 1 d . . N4 N -0.0381(5) 0.4809(4) 0.1031(3) 0.0549(14) Uani 1 d . . N5 N 0.1806(4) 0.4540(4) 0.0568(3) 0.0517(13) Uani 1 d . . N6 N 0.1861(5) 0.9943(4) -0.0106(3) 0.0581(14) Uani 1 d . . N7 N 0.0869(5) 0.9909(4) 0.1143(3) 0.0566(14) Uani 1 d . . C1 C 0.0807(7) 0.4739(6) 0.1565(4) 0.065(2) Uani 1 d . . C2 C 0.1670(6) 0.4067(5) 0.1250(3) 0.063(2) Uani 1 d . . H2 H 0.2459(6) 0.4035(5) 0.1590(3) 0.117(5) Uiso 1 calc R . H2A H 0.1357(6) 0.3337(5) 0.1166(3) 0.117(5) Uiso 1 calc R . C3 C -0.1233(6) 0.3965(6) 0.1138(4) 0.073(2) Uani 1 d . . H3 H -0.0808(6) 0.3277(6) 0.1195(4) 0.117(5) Uiso 1 calc R . H3A H -0.1890(6) 0.3920(6) 0.0705(4) 0.117(5) Uiso 1 calc R . C4 C -0.1781(9) 0.4141(10) 0.1787(5) 0.123(4) Uani 1 d D . C5 C -0.2759(15) 0.4875(13) 0.1700(8) 0.115(8) Uani 0.61(2) d PD . C6 C 0.2532(6) 0.3860(5) 0.0184(4) 0.069(2) Uani 1 d . . H6 H 0.2488(6) 0.4176(5) -0.0290(4) 0.117(5) Uiso 1 calc R . H6A H 0.2150(6) 0.3154(5) 0.0106(4) 0.117(5) Uiso 1 calc R . C7 C 0.3834(7) 0.3706(7) 0.0543(5) 0.108(3) Uani 1 d . . H7 H 0.4215(7) 0.4408(7) 0.0655(5) 0.117(5) Uiso 1 calc R . H7A H 0.3891(7) 0.3327(7) 0.0998(5) 0.117(5) Uiso 1 calc R . C8 C 0.4510(9) 0.3095(10) 0.0096(6) 0.153(4) Uani 1 d . . H8 H 0.5346(9) 0.3019(10) 0.0355(6) 0.117(5) Uiso 1 calc R . H8A H 0.4473(9) 0.3474(10) -0.0351(6) 0.117(5) Uiso 1 calc R . H8B H 0.4150(9) 0.2392(10) -0.0007(6) 0.117(5) Uiso 1 calc R . C9 C 0.2644(6) 0.9732(7) 0.0625(4) 0.081(2) Uani 1 d . . H9 H 0.3465(6) 0.9992(7) 0.0648(4) 0.117(5) Uiso 1 calc R . H9A H 0.2687(6) 0.8960(7) 0.0718(4) 0.117(5) Uiso 1 calc R . C10 C 0.2126(6) 1.0293(6) 0.1190(4) 0.079(2) Uani 1 d . . H10 H 0.2629(6) 1.0143(6) 0.1669(4) 0.117(5) Uiso 1 calc R . H10A H 0.2121(6) 1.1068(6) 0.1112(4) 0.117(5) Uiso 1 calc R . C11 C 0.2207(6) 0.9289(5) -0.0670(4) 0.074(2) Uani 1 d . . H11 H 0.1557(6) 0.9309(5) -0.1107(4) 0.117(5) Uiso 1 calc R . H11A H 0.2317(6) 0.8544(5) -0.0509(4) 0.117(5) Uiso 1 calc R . C12 C 0.3407(10) 0.9712(14) -0.0841(7) 0.177(7) Uani 1 d . . H12 H 0.3315(10) 1.0467(14) -0.0980(7) 0.117(5) Uiso 1 calc R . H12A H 0.4071(10) 0.9652(14) -0.0413(7) 0.117(5) Uiso 1 calc R . C13 C 0.3661(12) 0.9136(12) -0.1377(11) 0.255(10) Uani 1 d . . H13 H 0.4401(12) 0.9400(12) -0.1486(11) 0.117(5) Uiso 1 calc R . H13A H 0.3003(12) 0.9200(12) -0.1800(11) 0.117(5) Uiso 1 calc R . H13B H 0.3764(12) 0.8392(12) -0.1234(11) 0.117(5) Uiso 1 calc R . C14 C 0.0882(7) 0.8914(5) 0.1565(3) 0.072(2) Uani 1 d . . H14 H 0.1225(7) 0.8339(5) 0.1327(3) 0.117(5) Uiso 1 calc R . H14A H 0.1421(7) 0.9021(5) 0.2040(3) 0.117(5) Uiso 1 calc R . C15 C -0.0296(8) 0.8566(5) 0.1663(4) 0.088(2) Uani 1 d . . H15 H -0.0803(8) 0.8361(5) 0.1195(4) 0.117(5) Uiso 1 calc R . H15A H -0.0690(8) 0.9168(5) 0.1844(4) 0.117(5) Uiso 1 calc R . C16 C -0.0219(10) 0.7618(6) 0.2185(5) 0.115(3) Uani 1 d . . H16 H -0.1026(10) 0.7426(6) 0.2228(5) 0.117(5) Uiso 1 calc R . H16A H 0.0267(10) 0.7819(6) 0.2653(5) 0.117(5) Uiso 1 calc R . H16B H 0.0149(10) 0.7011(6) 0.2002(5) 0.117(5) Uiso 1 calc R . P1 P 0.4208(2) 0.67868(15) 0.20130(11) 0.0726(6) Uani 1 d . . F1 F 0.4475(39) 0.8022(27) 0.1852(18) 0.262(20) Uani 0.50 d P . F2 F 0.5073(32) 0.6802(28) 0.2758(15) 0.162(15) Uani 0.50 d P . F3 F 0.3519(24) 0.6630(21) 0.1182(11) 0.117(9) Uani 0.50 d P . F6 F 0.3200(33) 0.7307(37) 0.2332(18) 0.275(19) Uani 0.50 d P . F5 F 0.3997(30) 0.5564(16) 0.2116(12) 0.161(14) Uani 0.50 d P . F4 F 0.5484(21) 0.6920(33) 0.1781(12) 0.141(10) Uani 0.50 d P . H4N H -0.0577(39) 0.5389(39) 0.1083(24) 0.020(13) Uiso 1 d . . H5N H 0.2244(43) 0.5180(39) 0.0685(27) 0.036(14) Uiso 1 d . . H6N H 0.1747(82) 1.0464(67) -0.0192(50) 0.117(5) Uiso 1 d . . H7N H 0.0505(41) 1.0346(41) 0.1368(26) 0.028(15) Uiso 1 d . . H1 H 0.0880(41) 0.4501(39) 0.2104(29) 0.043(14) Uiso 1 d . . H1A H 0.1197(59) 0.5391(63) 0.1614(36) 0.085(24) Uiso 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 0.0610(6) 0.0238(5) 0.0405(6) 0.0020(4) -0.0035(5) 0.0031(5) Ni2 0.0652(7) 0.0229(5) 0.0402(6) 0.0019(4) -0.0039(5) 0.0019(5) N1 0.088(4) 0.026(3) 0.067(4) -0.002(2) -0.018(3) -0.001(2) N2 0.070(3) 0.029(3) 0.043(3) -0.008(3) 0.006(2) -0.008(3) N3 0.126(5) 0.020(3) 0.060(4) 0.002(2) 0.004(3) -0.003(3) N4 0.075(4) 0.034(3) 0.049(3) -0.001(2) 0.003(3) 0.011(2) N5 0.060(3) 0.036(3) 0.052(3) 0.003(2) -0.002(3) 0.001(3) N6 0.067(3) 0.047(3) 0.054(3) 0.000(3) 0.002(2) 0.007(3) N7 0.081(4) 0.043(3) 0.041(3) 0.001(2) 0.004(3) 0.013(3) C1 0.079(5) 0.064(5) 0.043(4) -0.004(3) -0.006(3) 0.004(4) C2 0.075(4) 0.061(4) 0.040(3) 0.010(3) -0.012(3) 0.009(3) C3 0.071(4) 0.075(5) 0.074(5) 0.014(4) 0.018(4) 0.005(4) C4 0.098(6) 0.194(11) 0.088(6) 0.027(7) 0.041(5) 0.039(8) C5 0.128(14) 0.139(18) 0.085(11) 0.003(9) 0.039(10) 0.033(11) C6 0.072(4) 0.067(4) 0.065(4) 0.005(4) 0.007(4) 0.018(3) C7 0.090(6) 0.124(7) 0.106(7) -0.006(6) 0.013(5) 0.031(5) C8 0.115(7) 0.185(11) 0.161(10) 0.018(8) 0.036(7) 0.075(8) C9 0.067(4) 0.108(6) 0.056(4) 0.002(4) -0.009(3) 0.009(4) C10 0.072(5) 0.087(5) 0.063(5) -0.004(4) -0.018(4) -0.006(4) C11 0.081(5) 0.072(5) 0.064(5) -0.008(4) 0.009(4) 0.017(4) C12 0.097(8) 0.302(19) 0.126(9) -0.118(11) 0.014(6) 0.059(9) C13 0.119(10) 0.216(18) 0.391(29) 0.131(19) -0.024(14) 0.005(11) C14 0.113(6) 0.053(4) 0.047(4) 0.009(3) 0.012(4) 0.014(4) C15 0.132(7) 0.046(4) 0.089(6) 0.012(4) 0.032(5) 0.004(4) C16 0.198(10) 0.067(6) 0.085(6) 0.006(4) 0.044(6) -0.016(5) P1 0.0887(14) 0.0565(12) 0.0626(12) -0.0033(10) -0.0029(11) -0.0064(10) F1 0.325(37) 0.202(24) 0.225(29) 0.077(19) -0.005(22) -0.160(24) F2 0.148(18) 0.173(20) 0.116(21) 0.043(15) -0.069(18) -0.043(13) F3 0.157(16) 0.137(18) 0.048(7) -0.029(9) 0.004(8) -0.065(14) F6 0.268(36) 0.372(52) 0.193(22) -0.057(32) 0.075(26) 0.164(33) F5 0.291(30) 0.080(14) 0.081(8) 0.007(8) -0.017(13) -0.108(19) F4 0.100(10) 0.214(25) 0.104(11) -0.016(13) 0.011(10) -0.029(13) _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 N4 2.108(5) 3_565 ? Ni1 N4 2.108(5) . ? Ni1 N1 2.123(5) . ? Ni1 N1 2.123(5) 3_565 ? Ni1 N5 2.144(5) 3_565 ? Ni1 N5 2.144(5) . ? Ni2 N3 2.099(5) 3_575 ? Ni2 N3 2.099(5) . ? Ni2 N6 2.152(6) 3_575 ? Ni2 N6 2.152(6) . ? Ni2 N7 2.161(5) 3_575 ? Ni2 N7 2.161(5) . ? N1 N2 1.159(6) . ? N2 N3 1.171(6) . ? N4 C3 1.463(8) . ? N4 C1 1.480(8) . ? N4 H4N 0.76(5) . ? N5 C2 1.459(7) . ? N5 C6 1.477(7) . ? N5 H5N 0.93(5) . ? N6 C11 1.464(8) . ? N6 C9 1.482(8) . ? N6 H6N 0.67(8) . ? N7 C14 1.467(8) . ? N7 C10 1.475(8) . ? N7 H7N 0.85(5) . ? C1 C2 1.502(9) . ? C1 H1 1.05(5) . ? C1 H1A 0.91(7) . ? C2 H2 0.97 . ? C2 H2A 0.97 . ? C3 C4 1.514(10) . ? C3 H3 0.97 . ? C3 H3A 0.97 . ? C4 C5 1.407(13) . ? C6 C7 1.478(10) . ? C6 H6 0.97 . ? C6 H6A 0.97 . ? C7 C8 1.472(11) . ? C7 H7 0.97 . ? C7 H7A 0.97 . ? C8 H8 0.96 . ? C8 H8A 0.96 . ? C8 H8B 0.96 . ? C9 C10 1.502(10) . ? C9 H9 0.97 . ? C9 H9A 0.97 . ? C10 H10 0.97 . ? C10 H10A 0.97 . ? C11 C12 1.552(15) . ? C11 H11 0.97 . ? C11 H11A 0.97 . ? C12 C13 1.32(2) . ? C12 H12 0.97 . ? C12 H12A 0.97 . ? C13 H13 0.96 . ? C13 H13A 0.96 . ? C13 H13B 0.96 . ? C14 C15 1.446(9) . ? C14 H14 0.97 . ? C14 H14A 0.97 . ? C15 C16 1.525(9) . ? C15 H15 0.97 . ? C15 H15A 0.97 . ? C16 H16 0.96 . ? C16 H16A 0.96 . ? C16 H16B 0.96 . ? P1 F2 1.52(2) . ? P1 F6 1.54(3) . ? P1 F5 1.55(2) . ? P1 F3 1.60(2) . ? P1 F4 1.61(3) . ? P1 F1 1.60(3) . ? 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 N4 Ni1 N4 180.0 3_565 . ? N4 Ni1 N1 93.2(2) 3_565 . ? N4 Ni1 N1 86.8(2) . . ? N4 Ni1 N1 86.8(2) 3_565 3_565 ? N4 Ni1 N1 93.2(2) . 3_565 ? N1 Ni1 N1 180.0 . 3_565 ? N4 Ni1 N5 83.0(2) 3_565 3_565 ? N4 Ni1 N5 97.0(2) . 3_565 ? N1 Ni1 N5 91.8(2) . 3_565 ? N1 Ni1 N5 88.2(2) 3_565 3_565 ? N4 Ni1 N5 97.0(2) 3_565 . ? N4 Ni1 N5 83.0(2) . . ? N1 Ni1 N5 88.2(2) . . ? N1 Ni1 N5 91.8(2) 3_565 . ? N5 Ni1 N5 180.0 3_565 . ? N3 Ni2 N3 180.0 3_575 . ? N3 Ni2 N6 91.3(2) 3_575 3_575 ? N3 Ni2 N6 88.7(2) . 3_575 ? N3 Ni2 N6 88.7(2) 3_575 . ? N3 Ni2 N6 91.3(2) . . ? N6 Ni2 N6 180.0 3_575 . ? N3 Ni2 N7 95.3(2) 3_575 3_575 ? N3 Ni2 N7 84.7(2) . 3_575 ? N6 Ni2 N7 82.4(2) 3_575 3_575 ? N6 Ni2 N7 97.6(2) . 3_575 ? N3 Ni2 N7 84.7(2) 3_575 . ? N3 Ni2 N7 95.3(2) . . ? N6 Ni2 N7 97.6(2) 3_575 . ? N6 Ni2 N7 82.4(2) . . ? N7 Ni2 N7 180.0 3_575 . ? N2 N1 Ni1 136.5(4) . . ? N1 N2 N3 178.5(5) . . ? N2 N3 Ni2 145.4(4) . . ? C3 N4 C1 112.4(5) . . ? C3 N4 Ni1 119.3(4) . . ? C1 N4 Ni1 107.0(4) . . ? C3 N4 H4N 115.8(35) . . ? C1 N4 H4N 102.0(33) . . ? Ni1 N4 H4N 98.1(34) . . ? C2 N5 C6 113.1(5) . . ? C2 N5 Ni1 105.6(4) . . ? C6 N5 Ni1 118.3(4) . . ? C2 N5 H5N 106.7(31) . . ? C6 N5 H5N 106.2(29) . . ? Ni1 N5 H5N 106.3(29) . . ? C11 N6 C9 112.5(5) . . ? C11 N6 Ni2 121.0(4) . . ? C9 N6 Ni2 107.4(4) . . ? C11 N6 H6N 115.0(82) . . ? C9 N6 H6N 116.0(81) . . ? Ni2 N6 H6N 81.6(80) . . ? C14 N7 C10 110.5(5) . . ? C14 N7 Ni2 122.4(4) . . ? C10 N7 Ni2 104.4(4) . . ? C14 N7 H7N 101.8(34) . . ? C10 N7 H7N 109.3(33) . . ? Ni2 N7 H7N 108.0(32) . . ? N4 C1 C2 109.1(5) . . ? N4 C1 H1 122.4(26) . . ? C2 C1 H1 108.6(27) . . ? N4 C1 H1A 110.8(43) . . ? C2 C1 H1A 101.0(43) . . ? H1 C1 H1A 102.8(50) . . ? N5 C2 C1 109.9(5) . . ? N5 C2 H2 109.7(3) . . ? C1 C2 H2 109.7(3) . . ? N5 C2 H2A 109.7(3) . . ? C1 C2 H2A 109.7(4) . . ? H2 C2 H2A 108.2 . . ? N4 C3 C4 114.4(7) . . ? N4 C3 H3 108.6(3) . . ? C4 C3 H3 108.7(5) . . ? N4 C3 H3A 108.7(3) . . ? C4 C3 H3A 108.7(4) . . ? H3 C3 H3A 107.6 . . ? C5' C4 C5 73.0(13) . . ? C5' C4 C3 122.4(14) . . ? C5 C4 C3 117.0(9) . . ? C4 C5 C5' 52.9(8) . . ? C4 C5' C5 54.0(9) . . ? N5 C6 C7 116.7(6) . . ? N5 C6 H6 108.1(3) . . ? C7 C6 H6 108.1(5) . . ? N5 C6 H6A 108.1(3) . . ? C7 C6 H6A 108.1(5) . . ? H6 C6 H6A 107.3 . . ? C8 C7 C6 113.0(8) . . ? C8 C7 H7 109.0(6) . . ? C6 C7 H7 109.0(4) . . ? C8 C7 H7A 109.0(6) . . ? C6 C7 H7A 109.0(5) . . ? H7 C7 H7A 107.8 . . ? C7 C8 H8 109.5(5) . . ? C7 C8 H8A 109.5(6) . . ? H8 C8 H8A 109.5 . . ? C7 C8 H8B 109.5(6) . . ? H8 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N6 C9 C10 109.7(5) . . ? N6 C9 H9 109.7(4) . . ? C10 C9 H9 109.7(4) . . ? N6 C9 H9A 109.7(4) . . ? C10 C9 H9A 109.7(5) . . ? H9 C9 H9A 108.2 . . ? N7 C10 C9 109.5(6) . . ? N7 C10 H10 109.8(3) . . ? C9 C10 H10 109.8(4) . . ? N7 C10 H10A 109.8(4) . . ? C9 C10 H10A 109.8(5) . . ? H10 C10 H10A 108.2 . . ? N6 C11 C12 111.0(6) . . ? N6 C11 H11 109.4(3) . . ? C12 C11 H11 109.4(6) . . ? N6 C11 H11A 109.4(3) . . ? C12 C11 H11A 109.5(6) . . ? H11 C11 H11A 108.0 . . ? C13 C12 C11 109.4(13) . . ? C13 C12 H12 109.8(11) . . ? C11 C12 H12 109.8(6) . . ? C13 C12 H12A 109.8(9) . . ? C11 C12 H12A 109.8(6) . . ? H12 C12 H12A 108.2 . . ? C12 C13 H13 109.5(10) . . ? C12 C13 H13A 109.5(9) . . ? H13 C13 H13A 109.5 . . ? C12 C13 H13B 109.5(11) . . ? H13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C15 C14 N7 115.2(6) . . ? C15 C14 H14 108.5(4) . . ? N7 C14 H14 108.5(4) . . ? C15 C14 H14A 108.5(4) . . ? N7 C14 H14A 108.4(3) . . ? H14 C14 H14A 107.5 . . ? C14 C15 C16 113.3(7) . . ? C14 C15 H15 108.9(4) . . ? C16 C15 H15 108.9(5) . . ? C14 C15 H15A 108.9(4) . . ? C16 C15 H15A 108.9(5) . . ? H15 C15 H15A 107.7 . . ? C15 C16 H16 109.5(5) . . ? C15 C16 H16A 109.5(5) . . ? H16 C16 H16A 109.5 . . ? C15 C16 H16B 109.5(4) . . ? H16 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? F4' P1 F3' 92.4(21) . . ? F4' P1 F2 88.7(23) . . ? F3' P1 F2 176.0(17) . . ? F4' P1 F5' 71.0(22) . . ? F3' P1 F5' 93.3(15) . . ? F2 P1 F5' 90.7(17) . . ? F4' P1 F1' 102.7(20) . . ? F3' P1 F1' 84.2(13) . . ? F2 P1 F1' 91.8(14) . . ? F5' P1 F1' 173.1(16) . . ? F4' P1 F6 163.8(25) . . ? F3' P1 F6 87.8(18) . . ? F2 P1 F6 90.1(19) . . ? F5' P1 F6 125.2(22) . . ? F1' P1 F6 61.3(18) . . ? F4' P1 F6' 162.5(20) . . ? F3' P1 F6' 80.8(16) . . ? F2 P1 F6' 99.2(17) . . ? F5' P1 F6' 93.2(15) . . ? F1' P1 F6' 92.8(11) . . ? F6 P1 F6' 33.0(17) . . ? F4' P1 F5 94.0(22) . . ? F3' P1 F5 94.9(14) . . ? F2 P1 F5 88.8(15) . . ? F5' P1 F5 23.2(21) . . ? F1' P1 F5 163.3(15) . . ? F6 P1 F5 102.1(21) . . ? F6' P1 F5 70.7(14) . . ? F4' P1 F2' 102.6(20) . . ? F3' P1 F2' 164.7(19) . . ? F2 P1 F2' 14.0(26) . . ? F5' P1 F2' 94.4(15) . . ? F1' P1 F2' 89.5(11) . . ? F6 P1 F2' 77.0(17) . . ? F6' P1 F2' 85.6(15) . . ? F5 P1 F2' 87.0(11) . . ? F4' P1 F3 80.4(19) . . ? F3' P1 F3 14.8(21) . . ? F2 P1 F3 168.0(18) . . ? F5' P1 F3 81.3(15) . . ? F1' P1 F3 95.2(11) . . ? F6 P1 F3 101.7(16) . . ? F6' P1 F3 90.1(12) . . ? F5 P1 F3 87.2(11) . . ? F2' P1 F3 173.7(12) . . ? F4' P1 F4 16.6(26) . . ? F3' P1 F4 99.8(16) . . ? F2 P1 F4 80.3(17) . . ? F5' P1 F4 85.5(19) . . ? F1' P1 F4 88.6(17) . . ? F6 P1 F4 148.2(22) . . ? F6' P1 F4 178.6(16) . . ? F5 P1 F4 107.9(19) . . ? F2' P1 F4 94.0(15) . . ? F3 P1 F4 90.2(11) . . ? F4' P1 F1 81.8(24) . . ? F3' P1 F1 83.1(16) . . ? F2 P1 F1 93.3(17) . . ? F5' P1 F1 152.4(21) . . ? F1' P1 F1 20.9(19) . . ? F6 P1 F1 82.2(20) . . ? F6' P1 F1 113.1(18) . . ? F5 P1 F1 175.3(19) . . ? F2' P1 F1 96.0(14) . . ? F3 P1 F1 89.9(14) . . ? F4 P1 F1 68.3(19) . . ? F1' F1 P1 72.3(32) . . ? F6' F6 P1 73.1(23) . . ? F6' F6 F1' 128.7(34) . . ? P1 F6 F1' 58.9(14) . . ? F5' F5 P1 76.5(31) . . ? F1 F1' P1 86.8(39) . . ? F1 F1' F6 146.5(42) . . ? P1 F1' F6 59.9(11) . . ? P1 F4' F5' 57.4(16) . . ? F5 F5' P1 80.3(34) . . ? F5 F5' F4' 131.6(40) . . ? P1 F5' F4' 51.6(13) . . ? F6 F6' P1 73.9(26) . . ? _refine_diff_density_max 0.643 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.078 data_compound_4 _database_code_CSD 186793 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Ni(N-Metn)2(mu1,3-N3)]2(ClO4)2' _chemical_formula_sum 'C8 H24 Cl N7 Ni O4' _chemical_formula_weight 376.50 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' 'Cl' 'Cl' 0.1484 0.1585 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 10.401(2) _cell_length_b 9.286(3) _cell_length_c 17.429(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.406(12) _cell_angle_gamma 90.00 _cell_volume 1614.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 1.393 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4836 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 29.98 _reflns_number_total 4640 _reflns_number_gt 2780 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4640 _refine_ls_number_parameters 287 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.060 _refine_ls_shift/su_mean 0.009 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.43124(4) 0.66244(4) 0.10703(2) 0.03137(14) Uani 1 d . . . Cl Cl 0.43954(11) 1.16629(11) 0.26436(7) 0.0554(3) Uani 1 d . . . N1 N 0.4321(3) 0.7053(3) -0.01297(17) 0.0393(6) Uani 1 d . . . N2 N 0.4398(2) 0.6160(3) -0.05889(16) 0.0325(6) Uani 1 d . . . N3 N 0.4449(3) 0.5297(3) -0.10656(17) 0.0420(7) Uani 1 d . . . N4 N 0.3253(4) 0.8493(4) 0.1161(2) 0.0462(7) Uani 1 d . . . N5 N 0.2395(3) 0.5572(3) 0.06090(18) 0.0413(7) Uani 1 d . . . N6 N 0.4344(4) 0.5916(4) 0.22148(18) 0.0459(8) Uani 1 d . . . N7 N 0.6216(3) 0.7670(3) 0.14765(17) 0.0386(7) Uani 1 d . . . C1 C 0.2188(5) 0.8940(5) 0.0445(3) 0.0564(11) Uani 1 d . . . C2 C 0.1084(4) 0.7840(6) 0.0223(3) 0.0577(11) Uani 1 d . . . C3 C 0.1452(4) 0.6384(5) -0.0043(2) 0.0518(10) Uani 1 d . . . C4 C 0.2489(5) 0.4075(5) 0.0359(4) 0.0570(11) Uani 1 d . . . C5 C 0.5196(5) 0.6603(6) 0.2940(2) 0.0549(10) Uani 1 d . . . C6 C 0.6570(4) 0.6902(5) 0.2888(2) 0.0517(10) Uani 1 d . . . C7 C 0.6683(4) 0.8101(4) 0.2324(2) 0.0458(9) Uani 1 d . . . C8 C 0.6492(5) 0.8835(5) 0.0977(3) 0.0533(10) Uani 1 d . . . O1 O 0.4654(4) 1.1430(4) 0.1900(2) 0.0842(11) Uani 1 d . . . O2 O 0.3875(4) 1.0423(4) 0.2901(3) 0.0978(13) Uani 1 d . . . O3 O 0.3453(6) 1.2751(5) 0.2597(4) 0.071(2) Uani 1 d . . . O4 O 0.5547(6) 1.2086(10) 0.3185(4) 0.106(4) Uani 1 d . . . H4N H 0.292(4) 0.841(4) 0.157(3) 0.044(11) Uiso 1 d . . . H4AN H 0.381(4) 0.913(5) 0.132(2) 0.046(12) Uiso 1 d . . . H5N H 0.204(4) 0.557(4) 0.096(2) 0.041(11) Uiso 1 d . . . H6N H 0.348(4) 0.583(4) 0.224(2) 0.048(11) Uiso 1 d . . . H6AN H 0.449(4) 0.504(5) 0.220(3) 0.053(13) Uiso 1 d . . . H7N H 0.670(4) 0.703(4) 0.146(2) 0.042(12) Uiso 1 d . . . H1 H 0.175(4) 0.980(5) 0.057(3) 0.067(13) Uiso 1 d . . . H1A H 0.261(4) 0.893(5) 0.010(3) 0.060(13) Uiso 1 d . . . H2 H 0.067(4) 0.774(4) 0.065(3) 0.051(11) Uiso 1 d . . . H2A H 0.038(4) 0.826(4) -0.020(3) 0.051(11) Uiso 1 d . . . H3 H 0.191(4) 0.655(4) -0.042(3) 0.048(11) Uiso 1 d . . . H3A H 0.060(4) 0.587(5) -0.025(2) 0.059(12) Uiso 1 d . . . H4 H 0.297(5) 0.357(5) 0.078(3) 0.067(15) Uiso 1 d . . . H4A H 0.165(5) 0.367(5) 0.013(3) 0.059(12) Uiso 1 d . . . H4B H 0.287(5) 0.410(6) -0.007(3) 0.092(18) Uiso 1 d . . . H5 H 0.488(4) 0.736(5) 0.305(2) 0.047(12) Uiso 1 d . . . H5A H 0.517(4) 0.608(5) 0.342(3) 0.060(12) Uiso 1 d . . . H6 H 0.697(5) 0.607(6) 0.264(3) 0.094(17) Uiso 1 d . . . H6A H 0.716(5) 0.722(5) 0.341(3) 0.079(14) Uiso 1 d . . . H7 H 0.618(5) 0.892(5) 0.240(3) 0.072(14) Uiso 1 d . . . H7A H 0.762(5) 0.833(4) 0.248(3) 0.052(11) Uiso 1 d . . . H8 H 0.601(4) 0.969(5) 0.106(2) 0.050(11) Uiso 1 d . . . H8A H 0.738(5) 0.916(5) 0.108(3) 0.078(15) Uiso 1 d . . . H8B H 0.616(6) 0.854(5) 0.052(4) 0.083(18) Uiso 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 Ni 0.0326(2) 0.0354(2) 0.0260(2) -0.00070(18) 0.00805(14) -0.00159(19) Cl 0.0639(6) 0.0465(5) 0.0685(6) -0.0077(5) 0.0396(5) -0.0070(5) N1 0.0450(16) 0.0404(15) 0.0327(14) -0.0014(13) 0.0114(12) 0.0000(13) N2 0.0271(13) 0.0388(14) 0.0289(13) 0.0051(12) 0.0038(10) -0.0022(11) N3 0.0434(16) 0.0417(16) 0.0370(15) -0.0058(13) 0.0051(12) -0.0011(13) N4 0.0458(17) 0.0480(19) 0.0458(18) -0.0028(16) 0.0146(15) 0.0031(17) N5 0.0339(15) 0.0541(19) 0.0369(15) 0.0017(14) 0.0116(12) -0.0049(13) N6 0.057(2) 0.048(2) 0.0339(16) 0.0004(14) 0.0140(14) -0.0040(17) N7 0.0383(15) 0.0362(16) 0.0375(16) -0.0046(13) 0.0047(12) -0.0037(14) C1 0.059(3) 0.056(3) 0.056(3) 0.014(2) 0.020(2) 0.019(2) C2 0.042(2) 0.082(3) 0.049(2) 0.020(2) 0.0114(18) 0.016(2) C3 0.0339(18) 0.077(3) 0.042(2) 0.008(2) 0.0066(15) -0.0041(19) C4 0.040(2) 0.055(3) 0.074(3) -0.011(2) 0.013(2) -0.012(2) C5 0.078(3) 0.057(3) 0.0303(17) -0.004(2) 0.0170(18) 0.000(2) C6 0.056(2) 0.053(2) 0.0355(18) -0.0041(17) -0.0051(17) 0.0032(19) C7 0.047(2) 0.044(2) 0.0403(19) -0.0118(16) 0.0017(16) -0.0029(17) C8 0.054(3) 0.057(3) 0.049(2) 0.001(2) 0.014(2) -0.019(2) O1 0.128(3) 0.068(2) 0.080(2) -0.0049(17) 0.068(2) -0.002(2) O2 0.142(4) 0.060(2) 0.124(3) 0.013(2) 0.091(3) 0.001(2) O3 0.115(6) 0.073(3) 0.080(5) 0.039(3) 0.044(5) 0.062(3) O4 0.115(4) 0.084(11) 0.129(5) -0.050(6) 0.052(4) -0.041(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 Ni N4 2.085(3) . ? Ni N6 2.092(3) . ? Ni N1 2.131(3) . ? Ni N7 2.139(3) . ? Ni N5 2.162(3) . ? Ni N3 2.202(3) 3_665 ? Cl O4 1.357(5) . ? Cl O3 1.394(4) . ? Cl O2 1.399(3) . ? Cl O1 1.412(3) . ? N1 N2 1.171(4) . ? N2 N3 1.166(4) . ? N3 Ni 2.202(3) 3_665 ? N4 C1 1.476(5) . ? N4 H4N 0.88(5) . ? N4 H4AN 0.82(4) . ? N5 C4 1.467(6) . ? N5 C3 1.481(5) . ? N5 H5N 0.80(4) . ? N6 C5 1.468(5) . ? N6 H6N 0.91(4) . ? N6 H6AN 0.83(5) . ? N7 C8 1.467(5) . ? N7 C7 1.473(4) . ? N7 H7N 0.79(4) . ? C1 C2 1.503(7) . ? C1 H1 0.98(5) . ? C1 H1A 0.84(5) . ? C2 C3 1.513(7) . ? C2 H2 0.96(4) . ? C2 H2A 0.96(4) . ? C3 H3 0.92(4) . ? C3 H3A 0.98(4) . ? C4 H4 0.90(5) . ? C4 H4A 0.93(5) . ? C4 H4B 0.94(6) . ? C5 C6 1.484(6) . ? C5 H5 0.83(4) . ? C5 H5A 0.98(5) . ? C6 C7 1.512(6) . ? C6 H6 1.03(6) . ? C6 H6A 0.99(5) . ? C7 H7 0.95(5) . ? C7 H7A 0.96(5) . ? C8 H8 0.97(4) . ? C8 H8A 0.94(5) . ? C8 H8B 0.82(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 N4 Ni N6 93.17(15) . . ? N4 Ni N1 93.92(13) . . ? N6 Ni N1 172.34(13) . . ? N4 Ni N7 93.25(14) . . ? N6 Ni N7 93.63(13) . . ? N1 Ni N7 88.85(11) . . ? N4 Ni N5 87.29(14) . . ? N6 Ni N5 88.68(13) . . ? N1 Ni N5 88.78(12) . . ? N7 Ni N5 177.60(12) . . ? N4 Ni N3 175.34(12) . 3_665 ? N6 Ni N3 84.08(14) . 3_665 ? N1 Ni N3 89.03(11) . 3_665 ? N7 Ni N3 83.19(12) . 3_665 ? N5 Ni N3 96.39(12) . 3_665 ? O4 Cl O3 107.4(5) . . ? O4 Cl O2 111.1(4) . . ? O3 Cl O2 106.6(3) . . ? O4 Cl O1 108.9(3) . . ? O3 Cl O1 111.7(3) . . ? O2 Cl O1 111.1(2) . . ? N2 N1 Ni 124.0(2) . . ? N3 N2 N1 177.9(3) . . ? N2 N3 Ni 134.7(2) . 3_665 ? C1 N4 Ni 117.1(3) . . ? C1 N4 H4N 110(3) . . ? Ni N4 H4N 109(2) . . ? C1 N4 H4AN 112(3) . . ? Ni N4 H4AN 106(3) . . ? H4N N4 H4AN 101(4) . . ? C4 N5 C3 109.8(4) . . ? C4 N5 Ni 114.0(3) . . ? C3 N5 Ni 113.3(2) . . ? C4 N5 H5N 108(3) . . ? C3 N5 H5N 104(3) . . ? Ni N5 H5N 107(3) . . ? C5 N6 Ni 121.8(3) . . ? C5 N6 H6N 111(2) . . ? Ni N6 H6N 109(2) . . ? C5 N6 H6AN 113(3) . . ? Ni N6 H6AN 103(3) . . ? H6N N6 H6AN 96(4) . . ? C8 N7 C7 109.3(3) . . ? C8 N7 Ni 117.1(3) . . ? C7 N7 Ni 117.8(2) . . ? C8 N7 H7N 107(3) . . ? C7 N7 H7N 103(3) . . ? Ni N7 H7N 100(3) . . ? N4 C1 C2 111.2(4) . . ? N4 C1 H1 109(3) . . ? C2 C1 H1 104(3) . . ? N4 C1 H1A 100(3) . . ? C2 C1 H1A 109(3) . . ? H1 C1 H1A 123(4) . . ? C1 C2 C3 116.5(4) . . ? C1 C2 H2 110(3) . . ? C3 C2 H2 111(3) . . ? C1 C2 H2A 106(2) . . ? C3 C2 H2A 109(2) . . ? H2 C2 H2A 103(3) . . ? N5 C3 C2 112.9(3) . . ? N5 C3 H3 105(2) . . ? C2 C3 H3 107(2) . . ? N5 C3 H3A 112(2) . . ? C2 C3 H3A 105(3) . . ? H3 C3 H3A 114(3) . . ? N5 C4 H4 109(3) . . ? N5 C4 H4A 112(3) . . ? H4 C4 H4A 112(4) . . ? N5 C4 H4B 107(4) . . ? H4 C4 H4B 114(5) . . ? H4A C4 H4B 103(4) . . ? N6 C5 C6 112.7(3) . . ? N6 C5 H5 113(3) . . ? C6 C5 H5 108(3) . . ? N6 C5 H5A 112(3) . . ? C6 C5 H5A 114(2) . . ? H5 C5 H5A 96(4) . . ? C5 C6 C7 115.5(4) . . ? C5 C6 H6 114(3) . . ? C7 C6 H6 100(3) . . ? C5 C6 H6A 110(3) . . ? C7 C6 H6A 104(3) . . ? H6 C6 H6A 113(4) . . ? N7 C7 C6 112.8(3) . . ? N7 C7 H7 108(3) . . ? C6 C7 H7 110(3) . . ? N7 C7 H7A 111(3) . . ? C6 C7 H7A 104(3) . . ? H7 C7 H7A 110(4) . . ? N7 C8 H8 109(2) . . ? N7 C8 H8A 118(3) . . ? H8 C8 H8A 103(4) . . ? N7 C8 H8B 103(4) . . ? H8 C8 H8B 109(4) . . ? H8A C8 H8B 114(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 29.98 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.572 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.091