# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2001 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Font-Bardia, Merce' 'Monfort, Montserrat' 'Resino, Inmaculada' 'Ribas, Joan' 'Solans, Xavier' _publ_contact_author_name 'Dr Montserrat Monfort' _publ_contact_author_address ; Department de Quimica Inorganica Universitat de Barcelona Mart i Franques 1,11 Barcelona 08028 SPAIN ; _publ_contact_author_email 'MONTSERRAT.MONFORT@QI.UB.ES' _publ_section_title ; Synthesis of New Complexes With NiII, N,N,N'-Me3en As a Blocking Ligand and Different Bridging Ligands. Structure of a Neutral AF-F Alternating 1D Complex Synthesised With N3-. ; data_?Ni(?1,1-N3)(?1,3-N3)(N,N,N'-Me3en)?n #(compound 3 ) _database_code_CSD 162464 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H14 N8 Ni' _chemical_formula_weight 244.95 _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' '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 7.132(4) _cell_length_b 10.122(2) _cell_length_c 14.614(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.22(2) _cell_angle_gamma 90.00 _cell_volume 1031.1(7) _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 1.578 _exptl_crystal_density_method ? _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 1.859 _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 3137 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 29.94 _reflns_number_total 2997 _reflns_number_observed 1688 _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^)+(0.0568P)^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 0.0036(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2947 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1373 _refine_ls_R_factor_obs 0.0504 _refine_ls_wR_factor_all 0.1395 _refine_ls_wR_factor_obs 0.1008 _refine_ls_goodness_of_fit_all 1.005 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.106 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max 1.890 _refine_ls_shift/esd_mean 0.060 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 0.65226(6) 0.08264(5) 0.95213(3) 0.0354(2) Uani 1 d . . N1 N 0.4320(5) 0.1159(3) 1.0277(2) 0.0416(8) Uani 1 d . . N2 N 0.4089(6) 0.2009(4) 1.0803(3) 0.0549(9) Uani 1 d . . N3 N 0.3841(9) 0.2832(4) 1.1302(4) 0.104(2) Uani 1 d . . N4 N 0.8448(5) 0.0103(4) 0.8744(2) 0.0545(10) Uani 1 d . . N5 N 0.9966(5) -0.0357(3) 0.8997(2) 0.0351(7) Uani 1 d . . N6 N 1.1474(5) -0.0836(4) 0.9193(3) 0.0610(10) Uani 1 d . . N7 N 0.4371(5) 0.1075(4) 0.8313(2) 0.0469(9) Uani 1 d . . N8 N 0.7255(5) 0.2824(4) 0.9234(3) 0.0551(9) Uani 1 d . . C1 C 0.4192(8) 0.2479(6) 0.8121(4) 0.0710(15) Uani 1 d . . C2 C 0.6109(9) 0.3088(6) 0.8268(4) 0.078(2) Uani 1 d . . C3 C 0.4427(10) 0.0265(7) 0.7497(4) 0.074(2) Uani 1 d . . C4 C 0.9283(9) 0.3005(7) 0.9202(6) 0.094(2) Uani 1 d . . C5 C 0.6817(13) 0.3744(6) 0.9912(6) 0.094(2) Uani 1 d . . H5 H 0.5451(94) 0.3810(61) 0.9841(47) 0.109 Uiso 1 calc . . H5A H 0.7333(93) 0.4596(64) 0.9816(43) 0.109 Uiso 1 calc . . H5B H 0.7375(97) 0.3438(64) 1.0532(46) 0.109 Uiso 1 calc . . H7N H 0.3567(95) 0.0864(63) 0.8474(50) 0.109(7) Uiso 1 d . . H1 H 0.3438(85) 0.2633(55) 0.7433(47) 0.109(7) Uiso 1 d . . H1A H 0.3986(86) 0.3112(53) 0.8745(46) 0.109(7) Uiso 1 d . . H2 H 0.6656(88) 0.2401(53) 0.7714(43) 0.109(7) Uiso 1 d . . H2A H 0.6073(93) 0.4007(58) 0.8160(44) 0.109(7) Uiso 1 d . . H3 H 0.3147(96) 0.0446(56) 0.6939(45) 0.109(7) Uiso 1 d . . H3B H 0.4653(94) -0.0629(59) 0.7658(45) 0.109(7) Uiso 1 d . . H3A H 0.4913(113) 0.0728(66) 0.7297(54) 0.109(7) Uiso 1 d . . H4 H 0.9666(90) 0.3968(59) 0.9058(42) 0.109(7) Uiso 1 d . . H4A H 1.0046(99) 0.2468(60) 0.8822(46) 0.109(7) Uiso 1 d . . H4B H 0.9833(90) 0.2959(56) 1.0156(47) 0.109(7) 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 0.0312(3) 0.0417(3) 0.0351(3) 0.0035(2) 0.0109(2) 0.0059(2) N1 0.045(2) 0.039(2) 0.046(2) 0.0028(15) 0.0229(15) 0.0092(14) N2 0.068(3) 0.044(2) 0.062(2) -0.001(2) 0.034(2) 0.002(2) N3 0.178(6) 0.055(3) 0.107(4) -0.022(3) 0.091(4) -0.006(3) N4 0.038(2) 0.084(3) 0.045(2) 0.004(2) 0.015(2) 0.015(2) N5 0.036(2) 0.042(2) 0.0295(15) -0.0023(13) 0.0120(13) -0.0034(14) N6 0.047(2) 0.087(3) 0.047(2) -0.011(2) 0.004(2) 0.019(2) N7 0.044(2) 0.059(2) 0.038(2) 0.006(2) 0.0086(15) 0.007(2) N8 0.056(2) 0.052(2) 0.060(2) 0.006(2) 0.019(2) -0.007(2) C1 0.072(4) 0.061(3) 0.071(3) 0.021(3) -0.005(3) 0.010(3) C2 0.086(4) 0.067(3) 0.084(4) 0.032(3) 0.023(3) 0.003(3) C3 0.084(4) 0.079(4) 0.051(3) 0.001(3) -0.004(3) 0.004(3) C4 0.070(4) 0.088(4) 0.134(6) 0.023(4) 0.040(4) -0.019(3) C5 0.136(6) 0.057(3) 0.100(5) -0.014(4) 0.048(5) -0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 2.091(3) . ? Ni1 N7 2.095(4) . ? Ni1 N6 2.107(4) 3_757 ? Ni1 N1 2.130(3) . ? Ni1 N1 2.136(3) 3_657 ? Ni1 N8 2.152(4) . ? N1 N2 1.188(5) . ? N1 Ni1 2.136(3) 3_657 ? N2 N3 1.145(5) . ? N4 N5 1.164(4) . ? N5 N6 1.159(4) . ? N6 Ni1 2.107(4) 3_757 ? N7 C1 1.449(7) . ? N7 C3 1.456(8) . ? N7 H7N 0.70(7) . ? N8 C5 1.442(8) . ? N8 C4 1.468(7) . ? N8 C2 1.497(7) . ? C1 C2 1.474(8) . ? C1 H1 1.05(6) . ? C1 H1A 1.15(6) . ? C2 H2 1.19(6) . ? C2 H2A 0.94(6) . ? C3 H3 1.10(7) . ? C3 H3B 0.94(6) . ? C3 H3A 0.68(7) . ? C4 H4 1.05(6) . ? C4 H4A 1.01(7) . ? C4 H4B 1.37(7) . ? C5 H5 1.03(6) . ? C5 H5A 0.97(6) . ? C5 H5B 1.02(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 Ni1 N7 91.87(14) . . ? N4 Ni1 N6 94.97(15) . 3_757 ? N7 Ni1 N6 171.48(14) . 3_757 ? N4 Ni1 N1 168.07(14) . . ? N7 Ni1 N1 85.91(14) . . ? N6 Ni1 N1 88.40(14) 3_757 . ? N4 Ni1 N1 88.94(14) . 3_657 ? N7 Ni1 N1 92.98(14) . 3_657 ? N6 Ni1 N1 92.22(15) 3_757 3_657 ? N1 Ni1 N1 79.48(13) . 3_657 ? N4 Ni1 N8 90.49(15) . . ? N7 Ni1 N8 83.54(15) . . ? N6 Ni1 N8 91.3(2) 3_757 . ? N1 Ni1 N8 100.89(14) . . ? N1 Ni1 N8 176.45(13) 3_657 . ? N2 N1 Ni1 132.0(3) . . ? N2 N1 Ni1 120.7(3) . 3_657 ? Ni1 N1 Ni1 100.52(13) . 3_657 ? N3 N2 N1 179.0(6) . . ? N5 N4 Ni1 129.9(3) . . ? N6 N5 N4 175.9(4) . . ? N5 N6 Ni1 129.6(3) . 3_757 ? C1 N7 C3 114.2(4) . . ? C1 N7 Ni1 107.5(3) . . ? C3 N7 Ni1 118.7(3) . . ? C1 N7 H7N 108.7(54) . . ? C3 N7 H7N 105.7(58) . . ? Ni1 N7 H7N 100.8(58) . . ? C5 N8 C4 107.4(6) . . ? C5 N8 C2 112.2(5) . . ? C4 N8 C2 107.1(5) . . ? C5 N8 Ni1 112.1(3) . . ? C4 N8 Ni1 113.9(4) . . ? C2 N8 Ni1 104.2(3) . . ? N7 C1 C2 110.0(4) . . ? N7 C1 H1 109.8(32) . . ? C2 C1 H1 110.5(34) . . ? N7 C1 H1A 114.5(28) . . ? C2 C1 H1A 85.5(31) . . ? H1 C1 H1A 123.6(44) . . ? C1 C2 N8 111.5(4) . . ? C1 C2 H2 94.8(30) . . ? N8 C2 H2 110.1(29) . . ? C1 C2 H2A 113.4(41) . . ? N8 C2 H2A 108.9(39) . . ? H2 C2 H2A 117.5(48) . . ? N7 C3 H3 110.5(32) . . ? N7 C3 H3B 111.7(40) . . ? H3 C3 H3B 114.6(48) . . ? N7 C3 H3A 93.9(68) . . ? H3 C3 H3A 89.1(67) . . ? H3B C3 H3A 133.7(78) . . ? N8 C4 H4 115.1(35) . . ? N8 C4 H4A 126.6(39) . . ? H4 C4 H4A 101.3(50) . . ? N8 C4 H4B 92.1(27) . . ? H4 C4 H4B 101.9(42) . . ? H4A C4 H4B 118.0(46) . . ? N8 C5 H5 103.7(39) . . ? N8 C5 H5A 106.3(39) . . ? H5 C5 H5A 108.4(53) . . ? N8 C5 H5B 108.0(37) . . ? H5 C5 H5B 119.0(55) . . ? H5A C5 H5B 110.6(56) . . ? _refine_diff_density_max 0.586 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.095 #=== END data_?Ni(NO2)(N,N,N'-Me3en)2?PF6 #(Compound 6) _database_code_CSD 162465 _audit_creation_method SHELXL _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H28 F6 N5 Ni O2 P' _chemical_formula_weight 454.05 _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' 'O' 'O' 0.0106 0.0060 '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+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 12.698(2) _cell_length_b 10.1097(14) _cell_length_c 15.698(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2015.2(8) _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 1.497 _exptl_crystal_density_method ? _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.108 _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 5326 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 29.96 _reflns_number_total 2811 _reflns_number_observed 2562 _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^)+(0.0717P)^2^+0.0256P] 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 0.0101(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 2761 _refine_ls_number_parameters 240 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_obs 0.0372 _refine_ls_wR_factor_all 0.1184 _refine_ls_wR_factor_obs 0.0945 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.302 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.31733(2) 0.33659(3) 0.11734(6) 0.03877(12) Uani 1 d . . P P 0.26098(12) 0.87544(11) 0.33726(10) 0.0674(3) Uani 1 d . . O1 O 0.2109(3) 0.3528(3) 0.0104(2) 0.0662(8) Uani 1 d . . O2 O 0.1665(2) 0.4415(3) 0.1251(3) 0.0628(7) Uani 1 d . . N1 N 0.4342(2) 0.2187(3) 0.0542(2) 0.0575(7) Uani 1 d . . N2 N 0.2471(3) 0.1524(3) 0.1451(3) 0.0574(8) Uani 1 d . . N3 N 0.3925(2) 0.5197(3) 0.0936(2) 0.0538(7) Uani 1 d . . N4 N 0.3676(3) 0.3730(3) 0.2471(2) 0.0522(6) Uani 1 d . . N5 N 0.1430(3) 0.4191(4) 0.0487(3) 0.0674(9) Uani 1 d . . C1 C 0.4055(4) 0.0781(4) 0.0786(4) 0.0763(12) Uani 1 d . . H1 H 0.4346(4) 0.0178(4) 0.0367(4) 0.100(5) Uiso 1 calc R . H1A H 0.4371(4) 0.0574(4) 0.1332(4) 0.100(5) Uiso 1 calc R . C2 C 0.2892(5) 0.0570(5) 0.0841(4) 0.0787(13) Uani 1 d . . H2 H 0.2570(5) 0.0701(5) 0.0287(4) 0.100(5) Uiso 1 calc R . H2A H 0.2742(5) -0.0324(5) 0.1029(4) 0.100(5) Uiso 1 calc R . C3 C 0.3954(4) 0.5870(4) 0.1763(4) 0.0726(12) Uani 1 d . . H3 H 0.3255(4) 0.6178(4) 0.1912(4) 0.100(5) Uiso 1 calc R . H3A H 0.4419(4) 0.6630(4) 0.1733(4) 0.100(5) Uiso 1 calc R . C4 C 0.4340(4) 0.4932(4) 0.2418(3) 0.0687(11) Uani 1 d . . H4 H 0.5057(4) 0.4678(4) 0.2284(3) 0.100(5) Uiso 1 calc R . H4A H 0.4346(4) 0.5370(4) 0.2968(3) 0.100(5) Uiso 1 calc R . C11 C 0.5472(3) 0.2398(4) 0.0764(4) 0.0684(10) Uani 1 d . . H11 H 0.5565(3) 0.2298(4) 0.1367(4) 0.112(26) Uiso 1 calc R . H11A H 0.5681(3) 0.3273(4) 0.0596(4) 0.060(13) Uiso 1 calc R . H11B H 0.5898(3) 0.1759(4) 0.0470(4) 0.100(5) Uiso 1 calc R . C12 C 0.4210(6) 0.2344(7) -0.0392(3) 0.088(2) Uani 1 d . . H12 H 0.3485(6) 0.2210(7) -0.0541(3) 0.100(5) Uiso 1 calc R . H12A H 0.4639(6) 0.1705(7) -0.0683(3) 0.100(5) Uiso 1 calc R . H12B H 0.4422(6) 0.3219(7) -0.0557(3) 0.100(5) Uiso 1 calc R . C21 C 0.1295(4) 0.1410(5) 0.1528(5) 0.087(2) Uani 1 d . . H21 H 0.1042(4) 0.2048(5) 0.1932(5) 0.100(5) Uiso 1 calc R . H21A H 0.1113(4) 0.0537(5) 0.1717(5) 0.106(23) Uiso 1 calc R . H21B H 0.0977(4) 0.1574(5) 0.0983(5) 0.100(5) Uiso 1 calc R . C31 C 0.3531(5) 0.6074(5) 0.0237(5) 0.089(2) Uani 1 d . . H31 H 0.3526(5) 0.5592(5) -0.0290(5) 0.100(5) Uiso 1 calc R . H31A H 0.3985(5) 0.6829(5) 0.0184(5) 0.100(5) Uiso 1 calc R . H31B H 0.2830(5) 0.6364(5) 0.0368(5) 0.100(5) Uiso 1 calc R . C41 C 0.2691(4) 0.4051(6) 0.2961(3) 0.0767(13) Uani 1 d . . H41 H 0.2300(4) 0.4720(6) 0.2664(3) 0.100(5) Uiso 1 calc R . H41A H 0.2877(4) 0.4369(6) 0.3518(3) 0.100(5) Uiso 1 calc R . H41B H 0.2268(4) 0.3269(6) 0.3016(3) 0.100(5) Uiso 1 calc R . C42 C 0.4247(5) 0.2712(6) 0.2943(3) 0.0803(14) Uani 1 d . . H42 H 0.3822(5) 0.1929(6) 0.2980(3) 0.100(5) Uiso 1 calc R . H42A H 0.4401(5) 0.3028(6) 0.3506(3) 0.100(5) Uiso 1 calc R . H42B H 0.4893(5) 0.2510(6) 0.2653(3) 0.100(5) Uiso 1 calc R . F1 F 0.2207(4) 1.0231(4) 0.3215(3) 0.1183(15) Uani 1 d . . F2 F 0.1696(7) 0.8579(5) 0.4040(5) 0.163(3) Uani 1 d . . F3 F 0.3141(5) 0.7404(5) 0.3581(4) 0.155(2) Uani 1 d . . F4 F 0.1989(5) 0.8153(8) 0.2631(6) 0.172(3) Uani 1 d . . F5 F 0.3381(5) 0.9409(6) 0.4092(4) 0.149(2) Uani 1 d . . F6 F 0.3534(4) 0.9038(6) 0.2705(4) 0.137(2) Uani 1 d . . H2N H 0.2675(33) 0.1456(35) 0.2048(30) 0.037(9) Uiso 1 d . . H3N H 0.4643(56) 0.5023(65) 0.0808(40) 0.094(19) 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 0.0377(2) 0.0429(2) 0.0357(2) 0.0041(2) -0.0005(2) 0.00367(12) P 0.0967(8) 0.0562(5) 0.0494(5) 0.0048(4) 0.0019(5) 0.0064(6) O1 0.067(2) 0.082(2) 0.0495(15) 0.0093(13) -0.0121(14) 0.0124(14) O2 0.0486(11) 0.0694(14) 0.070(2) 0.006(2) 0.0163(14) 0.0096(10) N1 0.0533(15) 0.066(2) 0.053(2) -0.0095(14) -0.0041(13) 0.0170(14) N2 0.058(2) 0.0501(15) 0.064(2) 0.0097(13) -0.0153(13) -0.0061(12) N3 0.0451(13) 0.0534(14) 0.063(2) 0.0163(12) 0.0123(11) 0.0041(11) N4 0.053(2) 0.066(2) 0.0378(13) -0.0022(12) -0.0007(12) -0.0068(13) N5 0.047(2) 0.075(2) 0.081(3) 0.017(2) -0.011(2) 0.011(2) C1 0.087(3) 0.058(2) 0.083(3) -0.019(2) -0.018(2) 0.020(2) C2 0.096(3) 0.060(2) 0.081(3) -0.004(2) -0.018(3) -0.007(2) C3 0.080(3) 0.049(2) 0.089(3) -0.008(2) 0.017(2) -0.011(2) C4 0.067(2) 0.078(3) 0.060(2) -0.016(2) -0.001(2) -0.022(2) C11 0.044(2) 0.073(2) 0.088(3) -0.005(2) 0.005(2) 0.012(2) C12 0.100(4) 0.113(4) 0.052(2) -0.002(3) 0.007(2) 0.032(3) C21 0.063(2) 0.076(3) 0.122(5) 0.028(3) -0.024(3) -0.024(2) C31 0.077(3) 0.078(3) 0.110(4) 0.051(3) 0.005(3) -0.002(3) C41 0.073(3) 0.118(4) 0.040(2) -0.001(2) 0.020(2) -0.006(3) C42 0.093(4) 0.091(3) 0.057(2) 0.013(2) -0.023(2) 0.002(3) F1 0.145(4) 0.081(2) 0.129(4) 0.035(2) 0.023(3) 0.028(2) F2 0.225(7) 0.114(3) 0.150(6) 0.028(3) 0.111(6) 0.000(3) F3 0.239(7) 0.076(2) 0.150(5) -0.008(3) -0.031(4) 0.061(3) F4 0.130(4) 0.229(7) 0.156(6) -0.081(5) -0.041(4) -0.018(4) F5 0.186(5) 0.146(4) 0.115(4) -0.046(3) -0.054(4) 0.033(4) F6 0.127(4) 0.161(4) 0.123(4) -0.020(3) 0.053(3) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.110(3) . ? Ni1 N3 2.116(3) . ? Ni1 N1 2.146(3) . ? Ni1 O1 2.162(4) . ? Ni1 N4 2.166(4) . ? Ni1 O2 2.192(2) . ? P F4 1.532(6) . ? P F3 1.557(4) . ? P F2 1.574(6) . ? P F1 1.597(4) . ? P F6 1.599(5) . ? P F5 1.634(5) . ? O1 N5 1.246(5) . ? O2 N5 1.256(6) . ? N1 C12 1.485(6) . ? N1 C11 1.492(5) . ? N1 C1 1.516(6) . ? N2 C2 1.461(7) . ? N2 C21 1.503(7) . ? N2 H2N 0.97(5) . ? N3 C3 1.465(6) . ? N3 C31 1.497(6) . ? N3 H3N 0.95(7) . ? N4 C42 1.460(6) . ? N4 C4 1.482(5) . ? N4 C41 1.505(5) . ? C1 C2 1.495(8) . ? C1 H1 0.97 . ? C1 H1A 0.97 . ? C2 H2 0.97 . ? C2 H2A 0.97 . ? C3 C4 1.482(8) . ? C3 H3 0.97 . ? C3 H3A 0.97 . ? C4 H4 0.97 . ? C4 H4A 0.97 . ? C11 H11 0.96 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C12 H12 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C21 H21 0.96 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C31 H31 0.96 . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C41 H41 0.96 . ? C41 H41A 0.96 . ? C41 H41B 0.96 . ? C42 H42 0.96 . ? C42 H42A 0.96 . ? C42 H42B 0.96 . ? 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 N3 177.5(2) . . ? N2 Ni1 N1 84.1(2) . . ? N3 Ni1 N1 95.31(13) . . ? N2 Ni1 O1 87.90(14) . . ? N3 Ni1 O1 94.54(14) . . ? N1 Ni1 O1 96.66(14) . . ? N2 Ni1 N4 94.6(2) . . ? N3 Ni1 N4 83.32(13) . . ? N1 Ni1 N4 108.95(13) . . ? O1 Ni1 N4 154.39(13) . . ? N2 Ni1 O2 92.66(13) . . ? N3 Ni1 O2 88.89(11) . . ? N1 Ni1 O2 154.0(2) . . ? O1 Ni1 O2 57.3(2) . . ? N4 Ni1 O2 97.1(2) . . ? F4 P F3 92.0(4) . . ? F4 P F2 94.7(5) . . ? F3 P F2 94.6(4) . . ? F4 P F1 95.1(4) . . ? F3 P F1 172.1(4) . . ? F2 P F1 88.4(3) . . ? F4 P F6 87.2(4) . . ? F3 P F6 88.7(4) . . ? F2 P F6 176.1(3) . . ? F1 P F6 88.0(3) . . ? F4 P F5 173.7(4) . . ? F3 P F5 87.2(3) . . ? F2 P F5 91.6(5) . . ? F1 P F5 85.4(3) . . ? F6 P F5 86.6(4) . . ? N5 O1 Ni1 95.6(3) . . ? N5 O2 Ni1 93.8(2) . . ? C12 N1 C11 108.9(4) . . ? C12 N1 C1 108.8(4) . . ? C11 N1 C1 107.8(3) . . ? C12 N1 Ni1 108.6(3) . . ? C11 N1 Ni1 118.6(3) . . ? C1 N1 Ni1 103.8(3) . . ? C2 N2 C21 111.4(4) . . ? C2 N2 Ni1 107.0(3) . . ? C21 N2 Ni1 120.3(3) . . ? C2 N2 H2N 119.2(23) . . ? C21 N2 H2N 100.5(25) . . ? Ni1 N2 H2N 98.5(23) . . ? C3 N3 C31 112.5(4) . . ? C3 N3 Ni1 105.2(2) . . ? C31 N3 Ni1 119.7(3) . . ? C3 N3 H3N 104.4(39) . . ? C31 N3 H3N 106.0(38) . . ? Ni1 N3 H3N 107.9(40) . . ? C42 N4 C4 108.9(4) . . ? C42 N4 C41 107.8(4) . . ? C4 N4 C41 108.9(4) . . ? C42 N4 Ni1 120.2(3) . . ? C4 N4 Ni1 104.8(3) . . ? C41 N4 Ni1 105.8(3) . . ? O1 N5 O2 113.2(3) . . ? C2 C1 N1 112.7(4) . . ? C2 C1 H1 109.0(3) . . ? N1 C1 H1 109.0(2) . . ? C2 C1 H1A 109.0(3) . . ? N1 C1 H1A 109.0(2) . . ? H1 C1 H1A 107.8 . . ? N2 C2 C1 107.8(4) . . ? N2 C2 H2 110.1(3) . . ? C1 C2 H2 110.1(3) . . ? N2 C2 H2A 110.1(3) . . ? C1 C2 H2A 110.1(3) . . ? H2 C2 H2A 108.5 . . ? N3 C3 C4 109.0(4) . . ? N3 C3 H3 109.9(2) . . ? C4 C3 H3 109.9(3) . . ? N3 C3 H3A 109.9(2) . . ? C4 C3 H3A 109.9(2) . . ? H3 C3 H3A 108.3 . . ? N4 C4 C3 112.1(4) . . ? N4 C4 H4 109.2(2) . . ? C3 C4 H4 109.2(3) . . ? N4 C4 H4A 109.2(2) . . ? C3 C4 H4A 109.2(3) . . ? H4 C4 H4A 107.9 . . ? N1 C11 H11 109.5(3) . . ? N1 C11 H11A 109.5(2) . . ? H11 C11 H11A 109.5 . . ? N1 C11 H11B 109.5(2) . . ? H11 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C12 H12 109.5(3) . . ? N1 C12 H12A 109.5(3) . . ? H12 C12 H12A 109.5 . . ? N1 C12 H12B 109.5(3) . . ? H12 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C21 H21 109.5(3) . . ? N2 C21 H21A 109.5(2) . . ? H21 C21 H21A 109.5 . . ? N2 C21 H21B 109.5(3) . . ? H21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C31 H31 109.5(3) . . ? N3 C31 H31A 109.5(3) . . ? H31 C31 H31A 109.5 . . ? N3 C31 H31B 109.5(3) . . ? H31 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N4 C41 H41 109.5(3) . . ? N4 C41 H41A 109.5(2) . . ? H41 C41 H41A 109.5 . . ? N4 C41 H41B 109.5(3) . . ? H41 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C42 H42 109.5(3) . . ? N4 C42 H42A 109.5(3) . . ? H42 C42 H42A 109.5 . . ? N4 C42 H42B 109.5(3) . . ? H42 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? _refine_diff_density_max 0.446 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.058 #===End