# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1262 data_global _publ_contact_author ; Dr Duncan H. Gregory School of Chemistry University of Nottingham University Park Nottingham NG7 2RD. ; _publ_contact_author_phone '0115 951 4594' _publ_contact_author_fax '0115 951 3563' _publ_contact_author_email Duncan.Gregory@nottingham.ac.uk _publ_requested_journal 'Chemical Communications' _publ_section_title ; Novel Layered Lithium Nitridonickelates; Effect of Li Vacancy Concentration on N Co-ordination Geometry and Ni Oxidation State ; loop_ _publ_author_name _publ_author_address 'Siddons, Daniel J.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; 'Gregory, Duncan H.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; 'Barker, Marten G.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; 'Blake, Alexander J.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; 'Smith, Susan E.' #<--'Last name, first name' ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; 'Edwards, Peter P.' #<--'Last name, first name' ; School of Chemistry University of Birmingham Birmingmam B15 2TT ; 'Hamor, Thomas A.' #<--'Last name, first name' ; School of Chemistry University of Birmingham Birmingmam B15 2TT ; ############################################################ data_ni3lin _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Li N Ni' _chemical_formula_weight 79.66 _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 'Li' 'Li' -0.0003 0.0001 '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 hexagonal _symmetry_space_group_name_H-M 'P -6 m 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' _cell_length_a 3.7580(10) _cell_length_b 3.7580(10) _cell_length_c 3.5400(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 43.30(2) _cell_formula_units_Z 1 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 11 _cell_measurement_theta_min 5.5 _cell_measurement_theta_max 18.5 _exptl_crystal_description 'Irregular block' _exptl_crystal_colour Black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.055 _exptl_crystal_density_method ? _exptl_crystal_F_000 38 _exptl_absorpt_coefficient_mu 10.606 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.005 _exptl_absorpt_correction_T_max 0.036 _exptl_special_details ; A full sphere of data was collected. ; _diffrn_ambient_temperature 297(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 'Stoe Stadi-4 four-circle diffractometer' _diffrn_measurement_method \w-\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% +/-2 _diffrn_reflns_number 1440 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0126 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 5.76 _diffrn_reflns_theta_max 44.72 _reflns_number_total 171 _reflns_number_observed 164 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STADI4 (Stoe & Cie, 1995a)' _computing_cell_refinement 'STADI4 (Stoe & Cie, 1995a)' _computing_data_reduction 'X-RED (Stoe & Cie, 1995b)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC version 5.03 (Sheldrick, 1995)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0584P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary inference _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(4) _refine_ls_number_reflns 164 _refine_ls_number_parameters 7 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0623 _refine_ls_R_factor_obs 0.0374 _refine_ls_wR_factor_all 0.1095 _refine_ls_wR_factor_obs 0.0803 _refine_ls_goodness_of_fit_all 1.283 _refine_ls_goodness_of_fit_obs 1.283 _refine_ls_restrained_S_all 1.771 _refine_ls_restrained_S_obs 1.283 _refine_ls_shift/esd_max 0.001 _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 Ni Ni 0.6667 0.3333 0.0000 0.0242(2) Uani 1 d S . N N 0.6667 0.3333 -0.5000 0.0202(4) Uani 1 d S . Li Li 1.0000 0.0000 -0.5000 0.033(3) Uani 1 d S . 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 0.0291(2) 0.0291(2) 0.0145(2) 0.000 0.000 0.01455(9) N 0.0244(5) 0.0244(5) 0.0118(7) 0.000 0.000 0.0122(3) Li 0.024(3) 0.024(3) 0.052(10) 0.000 0.000 0.0121(13) _geom_special_details ; The e.s.d.'s are dependent only on the contribution from the unitcell parameter e.s.d.'s as all atoms lie on fixed positions. ; 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 N 1.7700(5) 1_556 y Ni N 1.7700(5) . ? Ni Li 2.8001(5) 1_556 ? Ni Li 2.8001(6) . y Ni Li 2.8001(5) 1_566 ? Ni Li 2.8001(6) 1_455 ? Ni Li 2.8001(5) 1_565 ? Ni Li 2.8001(5) 1_456 ? N Ni 1.7700(5) 1_554 ? N Li 2.1697(6) . y N Li 2.1697(6) 1_565 ? N Li 2.1697(6) 1_455 ? Li N 2.1697(6) 1_655 ? Li N 2.1697(6) 1_545 ? Li Ni 2.8001(5) 1_554 ? Li Ni 2.8001(6) 1_544 ? Li Ni 2.8001(6) 1_655 ? Li Ni 2.8001(5) 1_654 ? Li Ni 2.8001(6) 1_545 ? 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 N Ni N 180.0 1_556 . ? N Ni Li 50.793(11) 1_556 1_556 ? N Ni Li 129.207(11) . 1_556 ? N Ni Li 129.207(11) 1_556 . ? N Ni Li 50.793(11) . . ? Li Ni Li 78.41(2) 1_556 . ? N Ni Li 50.793(11) 1_556 1_566 ? N Ni Li 129.207(11) . 1_566 ? Li Ni Li 84.30(2) 1_556 1_566 ? Li Ni Li 134.410(7) . 1_566 ? N Ni Li 129.207(11) 1_556 1_455 ? N Ni Li 50.793(11) . 1_455 ? Li Ni Li 134.410(7) 1_556 1_455 ? Li Ni Li 84.30(2) . 1_455 ? Li Ni Li 134.410(7) 1_566 1_455 ? N Ni Li 129.207(11) 1_556 1_565 ? N Ni Li 50.793(11) . 1_565 ? Li Ni Li 134.410(7) 1_556 1_565 ? Li Ni Li 84.30(2) . 1_565 ? Li Ni Li 78.41(2) 1_566 1_565 ? Li Ni Li 84.30(2) 1_455 1_565 ? N Ni Li 50.793(11) 1_556 1_456 ? N Ni Li 129.207(11) . 1_456 ? Li Ni Li 84.30(2) 1_556 1_456 ? Li Ni Li 134.410(7) . 1_456 ? Li Ni Li 84.30(2) 1_566 1_456 ? Li Ni Li 78.41(2) 1_455 1_456 ? Li Ni Li 134.410(8) 1_565 1_456 ? Ni N Ni 180.0 1_554 . ? Ni N Li 90.0 1_554 . ? Ni N Li 90.0 . . ? Ni N Li 90.0 1_554 1_565 ? Ni N Li 90.0 . 1_565 ? Li N Li 120.0 . 1_565 ? Ni N Li 90.0 1_554 1_455 ? Ni N Li 90.0 . 1_455 ? Li N Li 120.0 . 1_455 ? Li N Li 120.0 1_565 1_455 ? N Li N 120.0 . 1_655 ? N Li N 120.0 . 1_545 ? N Li N 120.0 1_655 1_545 ? N Li Ni 39.207(11) . . ? N Li Ni 112.795(4) 1_655 . ? N Li Ni 112.795(4) 1_545 . ? N Li Ni 39.207(11) . 1_554 ? N Li Ni 112.795(4) 1_655 1_554 ? N Li Ni 112.795(4) 1_545 1_554 ? Ni Li Ni 78.41(2) . 1_554 ? N Li Ni 112.795(4) . 1_544 ? N Li Ni 112.795(4) 1_655 1_544 ? N Li Ni 39.207(11) 1_545 1_544 ? Ni Li Ni 134.410(7) . 1_544 ? Ni Li Ni 84.30(2) 1_554 1_544 ? N Li Ni 112.795(4) . 1_655 ? N Li Ni 39.207(11) 1_655 1_655 ? N Li Ni 112.795(4) 1_545 1_655 ? Ni Li Ni 84.30(2) . 1_655 ? Ni Li Ni 134.410(7) 1_554 1_655 ? Ni Li Ni 134.410(7) 1_544 1_655 ? N Li Ni 112.795(4) . 1_654 ? N Li Ni 39.207(11) 1_655 1_654 ? N Li Ni 112.795(4) 1_545 1_654 ? Ni Li Ni 134.410(7) . 1_654 ? Ni Li Ni 84.30(2) 1_554 1_654 ? Ni Li Ni 84.30(2) 1_544 1_654 ? Ni Li Ni 78.41(2) 1_655 1_654 ? N Li Ni 112.795(4) . 1_545 ? N Li Ni 112.795(4) 1_655 1_545 ? N Li Ni 39.207(11) 1_545 1_545 ? Ni Li Ni 84.30(2) . 1_545 ? Ni Li Ni 134.410(7) 1_554 1_545 ? Ni Li Ni 78.41(2) 1_544 1_545 ? Ni Li Ni 84.30(2) 1_655 1_545 ? Ni Li Ni 134.410(7) 1_654 1_545 ? _refine_diff_density_max 2.50 _refine_diff_density_min -0.86 _refine_diff_density_rms 0.28 #===END data_linin4321fin77 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'Li5 N3 Ni3' _chemical_formula_weight 252.86 _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 'Ni' 'Ni' 0.3393 1.1124 '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' 'Li' 'Li+' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P-62m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x, y, -z' '-y, x-y, -z' '-x+y, -x, -z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 6.475(3) _cell_length_b 6.475(3) _cell_length_c 3.555(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 129.08(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 868 _cell_measurement_theta_min 3.63 _cell_measurement_theta_max 26.76 _exptl_crystal_description 'Irregular block' _exptl_crystal_colour Gold _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.253 _exptl_crystal_density_method ? _exptl_crystal_F_000 120 _exptl_absorpt_coefficient_mu 10.668 _exptl_absorpt_correction_type 'averaging of equivalent reflections' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoKa _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku R-Axis II area detector' _diffrn_measurement_method 'image plate scanning' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 868 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 26.76 _reflns_number_total '109 [>sigma(I)]' _reflns_number_observed 109 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'R-Axis II software' _computing_cell_refinement 'R-axis II software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ORTEP _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for reflections with I>sigma(I) Weighted R-factors wR and all goodnesses of fit S are based on F^2^. Conventional R-factors R are based on F. 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^)+( 0.0400P)^2^+0.5900P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(35) _refine_ls_number_reflns 109 _refine_ls_number_parameters 15 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_obs 0.0351 _refine_ls_wR_factor_all 0.0884 _refine_ls_wR_factor_obs 0.0884 _refine_ls_goodness_of_fit_all 1.229 _refine_ls_goodness_of_fit_obs 1.229 _refine_ls_restrained_S_all 1.229 _refine_ls_restrained_S_obs 1.229 _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 0.6443(2) 0.0000 0.0000 0.0185(7) Uani 1 d S . N1 N 0.6463(9) 0.0000 0.5000 0.019(2) Uani 1.32 d SP . Li1 Li+ 0.2719(59) 0.0000 0.5000 0.041(6) Uani 1 d S . Li2 Li+ 0.3333 0.6667 0.5000 0.012(6) Uani 1.00 d SP . 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 0.0243(8) 0.0137(8) 0.0140(10) 0.000 0.000 0.0069(4) N1 0.023(2) 0.010(3) 0.019(4) 0.000 0.000 0.0051(14) Li1 0.044(12) 0.010(10) 0.058(19) 0.000 0.000 0.005(5) Li2 0.005(7) 0.005(7) 0.027(14) 0.000 0.000 0.002(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 N1 1.7775(10) . ? Ni1 N1 1.7775(10) 1_554 ? Ni1 Li1 2.740(9) 2_655 ? Ni1 Li1 2.740(9) 3_654 ? Ni1 Li1 2.740(9) 2_654 ? Ni1 Li1 2.740(9) 3_655 ? Ni1 Li2 2.7433(11) 7_556 ? Ni1 Li2 2.7433(11) 7 ? Ni1 Li2 2.7433(11) 1_544 ? Ni1 Li2 2.7433(11) 1_545 ? Ni1 Li1 3.00(3) 1_554 ? Ni1 Li1 3.00(3) . ? N1 Ni1 1.7775(10) 1_556 ? N1 Li1 2.077(12) 2_655 ? N1 Li1 2.077(12) 3_655 ? N1 Li2 2.095(3) 7_556 ? N1 Li2 2.095(3) 1_545 ? N1 Li1 2.42(4) . ? Li1 N1 2.077(12) 2_545 ? Li1 N1 2.077(12) 3_665 ? Li1 Li2 2.38(2) 1_545 ? Li1 Li2 2.38(2) 7_556 ? Li1 Ni1 2.740(9) 2_545 ? Li1 Ni1 2.740(9) 3_666 ? Li1 Ni1 2.740(9) 2_546 ? Li1 Ni1 2.740(9) 3_665 ? Li1 Ni1 3.00(3) 1_556 ? Li1 Li1 3.05(7) 3 ? Li2 N1 2.095(3) 2 ? Li2 N1 2.096(3) 1_565 ? Li2 N1 2.096(3) 3_665 ? Li2 Li1 2.38(2) 1_565 ? Li2 Li1 2.38(2) 2 ? Li2 Li1 2.38(2) 3_665 ? Li2 Ni1 2.7433(11) 2 ? Li2 Ni1 2.7433(11) 2_556 ? Li2 Ni1 2.7433(11) 1_566 ? Li2 Ni1 2.7433(11) 1_565 ? Li2 Ni1 2.7433(11) 3_665 ? Li2 Ni1 2.7433(11) 3_666 ? 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 179.1(4) . 1_554 ? N1 Ni1 Li1 49.3(2) . 2_655 ? N1 Ni1 Li1 130.1(2) 1_554 2_655 ? N1 Ni1 Li1 130.1(2) . 3_654 ? N1 Ni1 Li1 49.3(2) 1_554 3_654 ? Li1 Ni1 Li1 117.4(12) 2_655 3_654 ? N1 Ni1 Li1 130.1(2) . 2_654 ? N1 Ni1 Li1 49.3(2) 1_554 2_654 ? Li1 Ni1 Li1 80.9(3) 2_655 2_654 ? Li1 Ni1 Li1 67.6(14) 3_654 2_654 ? N1 Ni1 Li1 49.3(2) . 3_655 ? N1 Ni1 Li1 130.1(2) 1_554 3_655 ? Li1 Ni1 Li1 67.6(14) 2_655 3_655 ? Li1 Ni1 Li1 80.9(3) 3_654 3_655 ? Li1 Ni1 Li1 117.4(12) 2_654 3_655 ? N1 Ni1 Li2 49.81(8) . 7_556 ? N1 Ni1 Li2 130.58(8) 1_554 7_556 ? Li1 Ni1 Li2 51.5(6) 2_655 7_556 ? Li1 Ni1 Li2 167.5(8) 3_654 7_556 ? Li1 Ni1 Li2 102.6(7) 2_654 7_556 ? Li1 Ni1 Li2 97.8(3) 3_655 7_556 ? N1 Ni1 Li2 130.58(8) . 7 ? N1 Ni1 Li2 49.81(8) 1_554 7 ? Li1 Ni1 Li2 102.6(7) 2_655 7 ? Li1 Ni1 Li2 97.8(3) 3_654 7 ? Li1 Ni1 Li2 51.5(6) 2_654 7 ? Li1 Ni1 Li2 167.5(8) 3_655 7 ? Li2 Ni1 Li2 80.77(4) 7_556 7 ? N1 Ni1 Li2 130.58(8) . 1_544 ? N1 Ni1 Li2 49.81(8) 1_554 1_544 ? Li1 Ni1 Li2 167.5(8) 2_655 1_544 ? Li1 Ni1 Li2 51.5(6) 3_654 1_544 ? Li1 Ni1 Li2 97.8(3) 2_654 1_544 ? Li1 Ni1 Li2 102.6(7) 3_655 1_544 ? Li2 Ni1 Li2 140.19(5) 7_556 1_544 ? Li2 Ni1 Li2 85.90(4) 7 1_544 ? N1 Ni1 Li2 49.81(8) . 1_545 ? N1 Ni1 Li2 130.58(8) 1_554 1_545 ? Li1 Ni1 Li2 97.8(3) 2_655 1_545 ? Li1 Ni1 Li2 102.6(7) 3_654 1_545 ? Li1 Ni1 Li2 167.5(8) 2_654 1_545 ? Li1 Ni1 Li2 51.5(6) 3_655 1_545 ? Li2 Ni1 Li2 85.90(4) 7_556 1_545 ? Li2 Ni1 Li2 140.19(5) 7 1_545 ? Li2 Ni1 Li2 80.77(4) 1_544 1_545 ? N1 Ni1 Li1 126.8(5) . 1_554 ? N1 Ni1 Li1 54.0(5) 1_554 1_554 ? Li1 Ni1 Li1 143.4(6) 2_655 1_554 ? Li1 Ni1 Li1 91.9(7) 3_654 1_554 ? Li1 Ni1 Li1 91.9(7) 2_654 1_554 ? Li1 Ni1 Li1 143.4(6) 3_655 1_554 ? Li2 Ni1 Li1 96.3(3) 7_556 1_554 ? Li2 Ni1 Li1 48.8(2) 7 1_554 ? Li2 Ni1 Li1 48.8(2) 1_544 1_554 ? Li2 Ni1 Li1 96.3(3) 1_545 1_554 ? N1 Ni1 Li1 54.0(5) . . ? N1 Ni1 Li1 126.8(5) 1_554 . ? Li1 Ni1 Li1 91.9(7) 2_655 . ? Li1 Ni1 Li1 143.4(6) 3_654 . ? Li1 Ni1 Li1 143.4(6) 2_654 . ? Li1 Ni1 Li1 91.9(7) 3_655 . ? Li2 Ni1 Li1 48.8(2) 7_556 . ? Li2 Ni1 Li1 96.3(3) 7 . ? Li2 Ni1 Li1 96.3(3) 1_544 . ? Li2 Ni1 Li1 48.8(2) 1_545 . ? Li1 Ni1 Li1 72.8(9) 1_554 . ? Ni1 N1 Ni1 179.1(4) 1_556 . ? Ni1 N1 Li1 90.29(12) 1_556 2_655 ? Ni1 N1 Li1 90.29(12) . 2_655 ? Ni1 N1 Li1 90.29(12) 1_556 3_655 ? Ni1 N1 Li1 90.29(12) . 3_655 ? Li1 N1 Li1 94.5(21) 2_655 3_655 ? Ni1 N1 Li2 89.81(8) 1_556 7_556 ? Ni1 N1 Li2 89.81(8) . 7_556 ? Li1 N1 Li2 69.6(10) 2_655 7_556 ? Li1 N1 Li2 164.1(11) 3_655 7_556 ? Ni1 N1 Li2 89.81(8) 1_556 1_545 ? Ni1 N1 Li2 89.81(8) . 1_545 ? Li1 N1 Li2 164.1(11) 2_655 1_545 ? Li1 N1 Li2 69.6(10) 3_655 1_545 ? Li2 N1 Li2 126.2(3) 7_556 1_545 ? Ni1 N1 Li1 89.6(2) 1_556 . ? Ni1 N1 Li1 89.6(2) . . ? Li1 N1 Li1 132.8(10) 2_655 . ? Li1 N1 Li1 132.8(10) 3_655 . ? Li2 N1 Li1 63.13(14) 7_556 . ? Li2 N1 Li1 63.12(14) 1_545 . ? N1 Li1 N1 145.5(21) 2_545 3_665 ? N1 Li1 Li2 55.6(3) 2_545 1_545 ? N1 Li1 Li2 158.9(18) 3_665 1_545 ? N1 Li1 Li2 158.9(18) 2_545 7_556 ? N1 Li1 Li2 55.6(3) 3_665 7_556 ? Li2 Li1 Li2 103.4(15) 1_545 7_556 ? N1 Li1 N1 107.2(10) 2_545 . ? N1 Li1 N1 107.2(10) 3_665 . ? Li2 Li1 N1 51.7(7) 1_545 . ? Li2 Li1 N1 51.7(7) 7_556 . ? N1 Li1 Ni1 40.4(2) 2_545 2_545 ? N1 Li1 Ni1 129.0(10) 3_665 2_545 ? Li2 Li1 Ni1 64.31(14) 1_545 2_545 ? Li2 Li1 Ni1 135.1(8) 7_556 2_545 ? N1 Li1 Ni1 102.8(8) . 2_545 ? N1 Li1 Ni1 129.0(10) 2_545 3_666 ? N1 Li1 Ni1 40.4(2) 3_665 3_666 ? Li2 Li1 Ni1 135.1(8) 1_545 3_666 ? Li2 Li1 Ni1 64.32(14) 7_556 3_666 ? N1 Li1 Ni1 102.8(8) . 3_666 ? Ni1 Li1 Ni1 154.3(16) 2_545 3_666 ? N1 Li1 Ni1 40.4(2) 2_545 2_546 ? N1 Li1 Ni1 129.0(10) 3_665 2_546 ? Li2 Li1 Ni1 64.31(14) 1_545 2_546 ? Li2 Li1 Ni1 135.1(8) 7_556 2_546 ? N1 Li1 Ni1 102.8(8) . 2_546 ? Ni1 Li1 Ni1 80.9(3) 2_545 2_546 ? Ni1 Li1 Ni1 93.4(4) 3_666 2_546 ? N1 Li1 Ni1 129.0(10) 2_545 3_665 ? N1 Li1 Ni1 40.4(2) 3_665 3_665 ? Li2 Li1 Ni1 135.1(8) 1_545 3_665 ? Li2 Li1 Ni1 64.32(14) 7_556 3_665 ? N1 Li1 Ni1 102.8(8) . 3_665 ? Ni1 Li1 Ni1 93.4(4) 2_545 3_665 ? Ni1 Li1 Ni1 80.9(3) 3_666 3_665 ? Ni1 Li1 Ni1 154.3(16) 2_546 3_665 ? N1 Li1 Ni1 103.8(7) 2_545 1_556 ? N1 Li1 Ni1 103.8(7) 3_665 1_556 ? Li2 Li1 Ni1 60.1(7) 1_545 1_556 ? Li2 Li1 Ni1 60.1(7) 7_556 1_556 ? N1 Li1 Ni1 36.4(4) . 1_556 ? Ni1 Li1 Ni1 124.3(9) 2_545 1_556 ? Ni1 Li1 Ni1 78.1(4) 3_666 1_556 ? Ni1 Li1 Ni1 78.1(4) 2_546 1_556 ? Ni1 Li1 Ni1 124.3(9) 3_665 1_556 ? N1 Li1 Ni1 103.8(7) 2_545 . ? N1 Li1 Ni1 103.8(7) 3_665 . ? Li2 Li1 Ni1 60.1(7) 1_545 . ? Li2 Li1 Ni1 60.1(7) 7_556 . ? N1 Li1 Ni1 36.4(4) . . ? Ni1 Li1 Ni1 78.1(4) 2_545 . ? Ni1 Li1 Ni1 124.3(9) 3_666 . ? Ni1 Li1 Ni1 124.3(9) 2_546 . ? Ni1 Li1 Ni1 78.1(4) 3_665 . ? Ni1 Li1 Ni1 72.8(9) 1_556 . ? N1 Li1 Li1 42.8(10) 2_545 3 ? N1 Li1 Li1 102.8(10) 3_665 3 ? Li2 Li1 Li1 98.3(7) 1_545 3 ? Li2 Li1 Li1 158.3(7) 7_556 3 ? N1 Li1 Li1 150.000(4) . 3 ? Ni1 Li1 Li1 56.2(7) 2_545 3 ? Ni1 Li1 Li1 99.9(7) 3_666 3 ? Ni1 Li1 Li1 56.2(7) 2_546 3 ? Ni1 Li1 Li1 99.9(7) 3_665 3 ? Ni1 Li1 Li1 134.2(3) 1_556 3 ? Ni1 Li1 Li1 134.2(3) . 3 ? N1 Li2 N1 120.001(1) 2 1_565 ? N1 Li2 N1 120.000(2) 2 3_665 ? N1 Li2 N1 119.999(2) 1_565 3_665 ? N1 Li2 Li1 54.8(7) 2 1_565 ? N1 Li2 Li1 65.2(7) 1_565 1_565 ? N1 Li2 Li1 174.8(7) 3_665 1_565 ? N1 Li2 Li1 65.2(7) 2 2 ? N1 Li2 Li1 174.8(7) 1_565 2 ? N1 Li2 Li1 54.8(7) 3_665 2 ? Li1 Li2 Li1 120.001(9) 1_565 2 ? N1 Li2 Li1 174.8(7) 2 3_665 ? N1 Li2 Li1 54.8(7) 1_565 3_665 ? N1 Li2 Li1 65.2(7) 3_665 3_665 ? Li1 Li2 Li1 120.000(9) 1_565 3_665 ? Li1 Li2 Li1 119.999(1) 2 3_665 ? N1 Li2 Ni1 40.39(2) 2 2 ? N1 Li2 Ni1 112.62(10) 1_565 2 ? N1 Li2 Ni1 112.15(10) 3_665 2 ? Li1 Li2 Ni1 64.2(5) 1_565 2 ? Li1 Li2 Ni1 71.1(5) 2 2 ? Li1 Li2 Ni1 139.37(8) 3_665 2 ? N1 Li2 Ni1 40.39(2) 2 2_556 ? N1 Li2 Ni1 112.62(10) 1_565 2_556 ? N1 Li2 Ni1 112.15(10) 3_665 2_556 ? Li1 Li2 Ni1 64.2(5) 1_565 2_556 ? Li1 Li2 Ni1 71.1(5) 2 2_556 ? Li1 Li2 Ni1 139.37(8) 3_665 2_556 ? Ni1 Li2 Ni1 80.77(4) 2 2_556 ? N1 Li2 Ni1 112.15(10) 2 1_566 ? N1 Li2 Ni1 40.39(2) 1_565 1_566 ? N1 Li2 Ni1 112.62(10) 3_665 1_566 ? Li1 Li2 Ni1 71.1(5) 1_565 1_566 ? Li1 Li2 Ni1 139.37(7) 2 1_566 ? Li1 Li2 Ni1 64.2(5) 3_665 1_566 ? Ni1 Li2 Ni1 135.23(2) 2 1_566 ? Ni1 Li2 Ni1 82.55(3) 2_556 1_566 ? N1 Li2 Ni1 112.15(10) 2 1_565 ? N1 Li2 Ni1 40.39(2) 1_565 1_565 ? N1 Li2 Ni1 112.62(10) 3_665 1_565 ? Li1 Li2 Ni1 71.1(5) 1_565 1_565 ? Li1 Li2 Ni1 139.37(7) 2 1_565 ? Li1 Li2 Ni1 64.2(5) 3_665 1_565 ? Ni1 Li2 Ni1 82.55(3) 2 1_565 ? Ni1 Li2 Ni1 135.23(2) 2_556 1_565 ? Ni1 Li2 Ni1 80.77(4) 1_566 1_565 ? N1 Li2 Ni1 112.62(10) 2 3_665 ? N1 Li2 Ni1 112.15(10) 1_565 3_665 ? N1 Li2 Ni1 40.39(2) 3_665 3_665 ? Li1 Li2 Ni1 139.37(8) 1_565 3_665 ? Li1 Li2 Ni1 64.2(5) 2 3_665 ? Li1 Li2 Ni1 71.1(5) 3_665 3_665 ? Ni1 Li2 Ni1 82.55(3) 2 3_665 ? Ni1 Li2 Ni1 135.23(2) 2_556 3_665 ? Ni1 Li2 Ni1 135.23(2) 1_566 3_665 ? Ni1 Li2 Ni1 82.54(3) 1_565 3_665 ? N1 Li2 Ni1 112.62(10) 2 3_666 ? N1 Li2 Ni1 112.15(10) 1_565 3_666 ? N1 Li2 Ni1 40.39(2) 3_665 3_666 ? Li1 Li2 Ni1 139.37(8) 1_565 3_666 ? Li1 Li2 Ni1 64.2(5) 2 3_666 ? Li1 Li2 Ni1 71.1(5) 3_665 3_666 ? Ni1 Li2 Ni1 135.23(2) 2 3_666 ? Ni1 Li2 Ni1 82.55(3) 2_556 3_666 ? Ni1 Li2 Ni1 82.54(3) 1_566 3_666 ? Ni1 Li2 Ni1 135.23(2) 1_565 3_666 ? Ni1 Li2 Ni1 80.77(4) 3_665 3_666 ? _refine_diff_density_max 0.473 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.147