# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Mimoza Gjikaj' _publ_contact_author_email MIMOZA.GJIKAJ@TU-CLAUSTHAL.DE _publ_section_title ; Structural and spectroscopic elucidation of imidazolium and pyridinium based hexachloridophosphates and niobates ; loop_ _publ_author_name 'Mimoza Gjikaj' 'Wolfgang Brockner' 'Johann-Christian Leye' 'Tao Xie' # Attachment '1-5.cif' data_C6_H11_Cl6_N2_P _database_code_depnum_ccdc_archive 'CCDC 746104' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1-ethyl-3-methylimidazolium hexachloridophosphate' ; _chemical_name_common "'1-ethyl-3-methylimidazolium hexachloridophosphate'" _chemical_melting_point ? _chemical_formula_moiety '[C6N2H11][PCl6]' _chemical_formula_sum 'C6 H11 Cl6 N2 P' _chemical_formula_weight 354.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 7.6983(8) _cell_length_b 12.266(2) _cell_length_c 15.0185(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.447(9) _cell_angle_gamma 90.00 _cell_volume 1389.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 19192 _cell_measurement_theta_min 0.971 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.322 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 IPDS 2' _diffrn_reflns_number 11226 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0179 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2414 _reflns_number_gt 2146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe X-Area' _computing_cell_refinement 'Stoe X-Area' _computing_data_reduction 'Stoe X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburger, 1999)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.7884P] 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 0.0142(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2414 _refine_ls_number_parameters 170 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P P 0.48834(8) 0.72988(5) 0.12319(4) 0.02987(16) Uani 1 1 d . . . Cl1 Cl 0.46476(10) 0.68671(7) -0.01546(4) 0.0556(2) Uani 1 1 d . . . Cl2 Cl 0.47786(10) 0.56210(5) 0.15847(6) 0.0545(2) Uani 1 1 d . . . Cl3 Cl 0.77029(8) 0.72166(6) 0.14255(5) 0.04771(19) Uani 1 1 d . . . Cl4 Cl 0.50899(11) 0.77543(7) 0.26255(4) 0.0587(2) Uani 1 1 d . . . Cl5 Cl 0.49643(10) 0.89888(5) 0.08687(6) 0.0525(2) Uani 1 1 d . . . Cl6 Cl 0.20457(8) 0.73991(5) 0.10578(5) 0.04273(18) Uani 1 1 d . . . N3 N 0.9283(3) 0.58342(17) 0.37823(13) 0.0367(5) Uani 1 1 d . . . N1 N 0.9816(3) 0.48669(17) 0.26730(14) 0.0440(5) Uani 1 1 d . . . C2 C 0.8627(4) 0.5097(2) 0.31623(17) 0.0412(6) Uani 1 1 d . . . C5 C 1.1265(4) 0.5489(3) 0.2982(2) 0.0533(7) Uani 1 1 d . . . C4 C 1.0954(4) 0.6092(3) 0.3678(2) 0.0482(7) Uani 1 1 d . . . C6 C 0.9554(7) 0.4060(3) 0.1926(3) 0.0754(12) Uani 1 1 d . . . C7 C 0.9812(6) 0.4493(3) 0.1072(2) 0.0789(12) Uani 1 1 d . . . H7A H 0.9614(8) 0.3880(15) 0.0585(12) 0.118 Uiso 1 1 calc R . . H7B H 1.110(3) 0.4793(8) 0.1145(3) 0.118 Uiso 1 1 calc R . . H7C H 0.891(2) 0.5121(16) 0.0869(6) 0.118 Uiso 1 1 calc R . . C8 C 0.8339(5) 0.6297(3) 0.4451(2) 0.0560(8) Uani 1 1 d . . . H2 H 0.757(4) 0.482(3) 0.310(2) 0.053(9) Uiso 1 1 d . . . H4 H 1.162(4) 0.657(2) 0.401(2) 0.048(8) Uiso 1 1 d . . . H5 H 1.213(5) 0.543(3) 0.278(2) 0.061(10) Uiso 1 1 d . . . H6A H 1.090(10) 0.382(6) 0.182(5) 0.19(3) Uiso 1 1 d . . . H6B H 0.883(7) 0.354(4) 0.200(4) 0.122(19) Uiso 1 1 d . . . H8A H 0.897(7) 0.617(4) 0.504(4) 0.118(17) Uiso 1 1 d . . . H8B H 0.730(6) 0.600(4) 0.436(3) 0.094(15) Uiso 1 1 d . . . H8C H 0.817(7) 0.703(5) 0.439(4) 0.13(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P 0.0299(3) 0.0336(3) 0.0271(3) -0.0003(2) 0.0081(2) 0.0010(2) Cl1 0.0562(4) 0.0801(5) 0.0326(3) -0.0147(3) 0.0140(3) -0.0028(4) Cl2 0.0501(4) 0.0377(4) 0.0817(5) 0.0146(3) 0.0276(4) 0.0056(3) Cl3 0.0294(3) 0.0574(4) 0.0572(4) 0.0062(3) 0.0105(3) 0.0024(3) Cl4 0.0578(5) 0.0900(6) 0.0279(3) -0.0124(3) 0.0076(3) 0.0042(4) Cl5 0.0517(4) 0.0353(3) 0.0756(5) 0.0097(3) 0.0249(4) 0.0019(3) Cl6 0.0295(3) 0.0506(4) 0.0488(4) 0.0009(3) 0.0096(3) 0.0019(2) N3 0.0374(12) 0.0419(11) 0.0314(10) 0.0011(8) 0.0080(8) -0.0009(9) N1 0.0571(15) 0.0394(11) 0.0370(12) -0.0001(9) 0.0127(10) -0.0003(10) C2 0.0436(16) 0.0442(14) 0.0353(13) 0.0020(11) 0.0068(11) -0.0087(12) C5 0.0434(17) 0.071(2) 0.0487(16) 0.0042(14) 0.0178(14) 0.0092(14) C4 0.0392(16) 0.0620(18) 0.0420(15) -0.0019(13) 0.0046(12) -0.0097(13) C6 0.126(4) 0.0512(19) 0.056(2) -0.0111(15) 0.036(2) -0.012(2) C7 0.112(3) 0.080(2) 0.0494(19) -0.0193(17) 0.027(2) -0.032(2) C8 0.058(2) 0.067(2) 0.0474(18) -0.0112(15) 0.0213(16) 0.0019(17) _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 P Cl1 2.1211(9) . ? P Cl2 2.1306(9) . ? P Cl3 2.1343(9) . ? P Cl4 2.1415(9) . ? P Cl5 2.1475(9) . ? P Cl6 2.1515(9) . ? N3 C2 1.324(3) . ? N3 C4 1.364(4) . ? N3 C8 1.465(3) . ? N1 C2 1.313(3) . ? N1 C5 1.355(4) . ? N1 C6 1.480(4) . ? C2 H2 0.87(3) . ? C5 C4 1.340(4) . ? C5 H5 0.79(3) . ? C4 H4 0.87(3) . ? C6 C7 1.438(5) . ? C6 H6A 1.11(7) . ? C6 H6B 0.87(5) . ? C7 H7A 1.0394 . ? C7 H7B 1.0394 . ? C7 H7C 1.0394 . ? C7 H6A 1.51(8) . ? C8 H8A 0.93(5) . ? C8 H8B 0.87(5) . ? C8 H8C 0.91(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 Cl1 P Cl2 90.17(4) . . ? Cl1 P Cl3 90.49(4) . . ? Cl2 P Cl3 90.47(4) . . ? Cl1 P Cl4 179.09(5) . . ? Cl2 P Cl4 90.46(4) . . ? Cl3 P Cl4 90.17(4) . . ? Cl1 P Cl5 89.59(4) . . ? Cl2 P Cl5 179.46(5) . . ? Cl3 P Cl5 90.01(3) . . ? Cl4 P Cl5 89.78(4) . . ? Cl1 P Cl6 90.46(4) . . ? Cl2 P Cl6 89.87(3) . . ? Cl3 P Cl6 178.99(4) . . ? Cl4 P Cl6 88.88(4) . . ? Cl5 P Cl6 89.65(3) . . ? C2 N3 C4 108.3(2) . . ? C2 N3 C8 125.1(3) . . ? C4 N3 C8 126.6(3) . . ? C2 N1 C5 107.8(2) . . ? C2 N1 C6 124.2(3) . . ? C5 N1 C6 128.0(3) . . ? N1 C2 N3 109.2(2) . . ? N1 C2 H2 127(2) . . ? N3 C2 H2 124(2) . . ? C4 C5 N1 108.4(3) . . ? C4 C5 H5 131(3) . . ? N1 C5 H5 121(3) . . ? C5 C4 N3 106.3(3) . . ? C5 C4 H4 130(2) . . ? N3 C4 H4 124(2) . . ? C7 C6 N1 114.0(3) . . ? C7 C6 H6A 71(4) . . ? N1 C6 H6A 107(4) . . ? C7 C6 H6B 126(4) . . ? N1 C6 H6B 113(3) . . ? H6A C6 H6B 118(5) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C7 H6A 44(3) . . ? H7A C7 H6A 96.6 . . ? H7B C7 H6A 74.9 . . ? H7C C7 H6A 149.4 . . ? N3 C8 H8A 110(3) . . ? N3 C8 H8B 108(3) . . ? H8A C8 H8B 111(4) . . ? N3 C8 H8C 113(3) . . ? H8A C8 H8C 107(4) . . ? H8B C8 H8C 107(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.320 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.062 #============================================================================ data_C6H11Cl6N2Nb _database_code_depnum_ccdc_archive 'CCDC 746105' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1-ethyl-3-methylimidazolium hexachloridoniobate' ; _chemical_name_common "'1-ethyl-3-methylimidazolium hexachloridoniobate'" _chemical_melting_point ? _chemical_formula_moiety '[C6N2H11][NbCl6]' _chemical_formula_sum 'C6 H11 Cl6 N2 Nb' _chemical_formula_weight 416.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nb Nb -2.0727 0.6215 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 20.1861(14) _cell_length_b 7.0842(6) _cell_length_c 20.5488(13) _cell_angle_alpha 90.00 _cell_angle_beta 98.455(5) _cell_angle_gamma 90.00 _cell_volume 2906.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30748 _cell_measurement_theta_min 0.984 _cell_measurement_theta_max 29.90 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 1.903 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 IPDS 2' _diffrn_reflns_number 29506 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 29.90 _reflns_number_total 8256 _reflns_number_gt 7250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe X-Area' _computing_cell_refinement 'Stoe X-Area' _computing_data_reduction 'Stoe X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburger, 1999)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+2.0660P] 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 0.0263(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8256 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.464305(9) 0.71719(3) 0.232092(9) 0.02976(6) Uani 1 1 d . . . Nb2 Nb 0.231914(9) 0.14046(3) -0.038302(10) 0.02936(6) Uani 1 1 d . . . Cl1 Cl 0.40607(3) 0.71333(10) 0.32217(3) 0.04222(14) Uani 1 1 d . . . Cl2 Cl 0.38535(3) 0.51321(12) 0.17441(4) 0.05226(17) Uani 1 1 d . . . Cl3 Cl 0.54692(4) 0.92016(11) 0.28507(3) 0.05040(17) Uani 1 1 d . . . Cl4 Cl 0.52851(3) 0.45991(10) 0.27774(4) 0.04670(15) Uani 1 1 d . . . Cl5 Cl 0.40201(3) 0.98491(10) 0.19219(3) 0.04664(15) Uani 1 1 d . . . Cl6 Cl 0.51997(3) 0.71794(11) 0.13822(3) 0.04691(15) Uani 1 1 d . . . Cl7 Cl 0.32151(3) 0.15536(10) -0.09817(3) 0.04075(13) Uani 1 1 d . . . Cl8 Cl 0.28971(3) -0.06602(11) 0.03879(3) 0.04757(15) Uani 1 1 d . . . Cl9 Cl 0.18863(3) -0.11963(10) -0.10116(4) 0.04760(16) Uani 1 1 d . . . Cl10 Cl 0.16965(4) 0.34820(12) -0.11252(4) 0.05572(18) Uani 1 1 d . . . Cl11 Cl 0.27895(3) 0.40014(10) 0.02439(3) 0.04578(15) Uani 1 1 d . . . Cl12 Cl 0.14061(3) 0.13913(11) 0.02211(4) 0.04893(16) Uani 1 1 d . . . N1 N 0.13836(10) 0.6669(3) 0.11415(11) 0.0365(4) Uani 1 1 d . . . N3 N 0.06641(10) 0.7052(3) 0.02615(11) 0.0371(4) Uani 1 1 d . . . C2 C 0.12972(12) 0.6635(4) 0.04902(13) 0.0377(5) Uani 1 1 d . . . C4 C 0.03367(13) 0.7365(4) 0.07940(15) 0.0422(6) Uani 1 1 d . . . C5 C 0.07833(13) 0.7115(4) 0.13365(14) 0.0431(6) Uani 1 1 d . . . C6 C 0.20151(15) 0.6289(5) 0.15799(16) 0.0481(6) Uani 1 1 d . . . C7 C 0.22398(17) 0.7925(7) 0.2010(2) 0.0613(9) Uani 1 1 d . . . C8 C 0.03780(16) 0.7252(6) -0.04315(16) 0.0520(7) Uani 1 1 d . . . N9 N 0.61438(10) 0.2689(3) 0.14090(10) 0.0340(4) Uani 1 1 d . . . N11 N 0.52402(10) 0.2407(3) 0.07082(10) 0.0362(4) Uani 1 1 d . . . C10 C 0.55058(12) 0.2197(4) 0.13346(12) 0.0363(5) Uani 1 1 d . . . C12 C 0.57326(14) 0.3064(4) 0.03708(13) 0.0405(5) Uani 1 1 d . . . C13 C 0.62931(13) 0.3236(4) 0.08047(13) 0.0411(5) Uani 1 1 d . . . C14 C 0.66213(14) 0.2537(4) 0.20238(14) 0.0436(6) Uani 1 1 d . . . C15 C 0.6968(2) 0.4363(7) 0.22136(18) 0.0621(9) Uani 1 1 d . . . C16 C 0.45389(16) 0.2028(6) 0.04340(18) 0.0514(7) Uani 1 1 d . . . H2 H 0.1605(17) 0.648(5) 0.0240(17) 0.048(9) Uiso 1 1 d . . . H4 H -0.0078(18) 0.760(5) 0.0729(17) 0.051(9) Uiso 1 1 d . . . H5 H 0.0703(16) 0.716(5) 0.1752(17) 0.049(9) Uiso 1 1 d . . . H6A H 0.2296(18) 0.595(5) 0.1332(18) 0.053(10) Uiso 1 1 d . . . H6B H 0.193(2) 0.532(7) 0.185(2) 0.072(12) Uiso 1 1 d . . . H7C H 0.193(2) 0.816(7) 0.230(2) 0.080(13) Uiso 1 1 d . . . H7A H 0.264(2) 0.758(7) 0.229(2) 0.084(14) Uiso 1 1 d . . . H7B H 0.225(2) 0.902(7) 0.174(2) 0.081(14) Uiso 1 1 d . . . H8A H 0.047(2) 0.846(7) -0.054(2) 0.084(14) Uiso 1 1 d . . . H8B H 0.061(2) 0.639(6) -0.068(2) 0.068(12) Uiso 1 1 d . . . H8C H -0.008(3) 0.687(8) -0.049(3) 0.104(17) Uiso 1 1 d . . . H10 H 0.5282(16) 0.176(5) 0.1674(17) 0.047(9) Uiso 1 1 d . . . H12 H 0.5672(16) 0.331(5) -0.0055(18) 0.050(9) Uiso 1 1 d . . . H13 H 0.6707(17) 0.366(5) 0.0755(17) 0.051(9) Uiso 1 1 d . . . H14A H 0.6372(16) 0.214(5) 0.2351(17) 0.044(8) Uiso 1 1 d . . . H14B H 0.6979(17) 0.166(5) 0.1930(17) 0.048(9) Uiso 1 1 d . . . H15A H 0.665(3) 0.524(8) 0.225(3) 0.11(2) Uiso 1 1 d . . . H15B H 0.727(2) 0.432(8) 0.262(2) 0.091(14) Uiso 1 1 d . . . H15C H 0.728(2) 0.477(7) 0.190(2) 0.079(13) Uiso 1 1 d . . . H16A H 0.451(2) 0.200(8) 0.003(3) 0.092(16) Uiso 1 1 d . . . H16B H 0.430(2) 0.300(7) 0.054(2) 0.090(16) Uiso 1 1 d . . . H16C H 0.441(2) 0.088(8) 0.060(2) 0.094(16) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.02930(9) 0.03365(11) 0.02644(10) -0.00060(7) 0.00449(6) -0.00357(7) Nb2 0.02663(9) 0.03264(11) 0.02903(10) -0.00141(7) 0.00477(6) 0.00078(7) Cl1 0.0453(3) 0.0491(3) 0.0353(3) 0.0010(3) 0.0160(2) 0.0005(3) Cl2 0.0445(3) 0.0580(4) 0.0530(4) -0.0183(3) 0.0032(3) -0.0156(3) Cl3 0.0498(3) 0.0556(4) 0.0424(3) 0.0006(3) -0.0048(3) -0.0228(3) Cl4 0.0441(3) 0.0473(4) 0.0506(4) 0.0129(3) 0.0133(3) 0.0106(3) Cl5 0.0486(3) 0.0458(3) 0.0451(3) 0.0092(3) 0.0055(3) 0.0095(3) Cl6 0.0496(3) 0.0589(4) 0.0359(3) 0.0027(3) 0.0184(2) 0.0001(3) Cl7 0.0384(3) 0.0438(3) 0.0435(3) -0.0036(3) 0.0175(2) -0.0027(2) Cl8 0.0486(3) 0.0529(4) 0.0401(3) 0.0116(3) 0.0030(2) 0.0087(3) Cl9 0.0486(3) 0.0475(4) 0.0472(3) -0.0139(3) 0.0087(3) -0.0128(3) Cl10 0.0549(4) 0.0582(4) 0.0508(4) 0.0130(3) -0.0032(3) 0.0167(3) Cl11 0.0417(3) 0.0470(3) 0.0492(4) -0.0188(3) 0.0086(2) -0.0056(3) Cl12 0.0393(3) 0.0573(4) 0.0549(4) -0.0062(3) 0.0226(3) -0.0017(3) N1 0.0380(10) 0.0334(10) 0.0385(11) 0.0004(8) 0.0071(8) 0.0049(8) N3 0.0333(9) 0.0371(10) 0.0404(11) 0.0010(9) 0.0039(8) -0.0032(8) C2 0.0351(11) 0.0378(12) 0.0414(13) -0.0010(10) 0.0090(9) 0.0002(9) C4 0.0329(11) 0.0441(14) 0.0512(15) 0.0003(11) 0.0114(10) 0.0027(10) C5 0.0421(12) 0.0488(15) 0.0411(14) -0.0003(12) 0.0147(10) 0.0062(11) C6 0.0453(14) 0.0533(17) 0.0435(15) 0.0009(13) -0.0010(11) 0.0108(13) C7 0.0423(15) 0.079(3) 0.060(2) -0.0192(19) 0.0010(14) 0.0027(16) C8 0.0473(15) 0.061(2) 0.0445(15) 0.0033(14) -0.0022(12) -0.0097(14) N9 0.0356(9) 0.0335(10) 0.0332(10) -0.0006(8) 0.0057(7) 0.0019(8) N11 0.0385(10) 0.0356(10) 0.0340(10) -0.0015(8) 0.0033(8) -0.0002(8) C10 0.0404(11) 0.0359(12) 0.0329(11) -0.0003(9) 0.0063(9) -0.0020(9) C12 0.0485(13) 0.0416(13) 0.0325(12) 0.0034(10) 0.0097(10) -0.0009(11) C13 0.0400(12) 0.0466(14) 0.0389(13) 0.0028(11) 0.0132(10) 0.0007(11) C14 0.0408(12) 0.0485(15) 0.0394(13) 0.0004(11) -0.0013(10) 0.0006(11) C15 0.0605(19) 0.077(3) 0.0458(17) -0.0010(17) -0.0020(14) -0.0274(19) C16 0.0423(14) 0.062(2) 0.0470(17) -0.0018(15) -0.0040(11) -0.0039(14) _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 Nb1 Cl1 2.3342(6) . ? Nb1 Cl2 2.3404(7) . ? Nb1 Cl3 2.3451(7) . ? Nb1 Cl4 2.3503(7) . ? Nb1 Cl5 2.3552(7) . ? Nb1 Cl6 2.3708(6) . ? Nb2 Cl7 2.3345(6) . ? Nb2 Cl8 2.3381(7) . ? Nb2 Cl9 2.3441(7) . ? Nb2 Cl10 2.3469(7) . ? Nb2 Cl11 2.3634(7) . ? Nb2 Cl12 2.3687(6) . ? N1 C2 1.324(3) . ? N1 C5 1.368(3) . ? N1 C6 1.474(3) . ? N3 C2 1.328(3) . ? N3 C4 1.377(3) . ? N3 C8 1.463(4) . ? C4 C5 1.338(4) . ? C6 C7 1.487(5) . ? N9 C10 1.321(3) . ? N9 C13 1.376(3) . ? N9 C14 1.476(3) . ? N11 C10 1.328(3) . ? N11 C12 1.374(3) . ? N11 C16 1.469(4) . ? C12 C13 1.339(4) . ? C14 C15 1.495(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Nb1 Cl2 90.55(3) . . ? Cl1 Nb1 Cl3 92.62(3) . . ? Cl2 Nb1 Cl3 176.82(3) . . ? Cl1 Nb1 Cl4 89.25(2) . . ? Cl2 Nb1 Cl4 91.02(3) . . ? Cl3 Nb1 Cl4 88.71(3) . . ? Cl1 Nb1 Cl5 88.86(3) . . ? Cl2 Nb1 Cl5 91.83(3) . . ? Cl3 Nb1 Cl5 88.55(3) . . ? Cl4 Nb1 Cl5 176.60(3) . . ? Cl1 Nb1 Cl6 178.00(3) . . ? Cl2 Nb1 Cl6 87.61(3) . . ? Cl3 Nb1 Cl6 89.23(3) . . ? Cl4 Nb1 Cl6 91.54(3) . . ? Cl5 Nb1 Cl6 90.44(3) . . ? Cl7 Nb2 Cl8 92.14(3) . . ? Cl7 Nb2 Cl9 90.00(2) . . ? Cl8 Nb2 Cl9 89.43(3) . . ? Cl7 Nb2 Cl10 90.66(3) . . ? Cl8 Nb2 Cl10 177.19(3) . . ? Cl9 Nb2 Cl10 90.81(3) . . ? Cl7 Nb2 Cl11 88.38(2) . . ? Cl8 Nb2 Cl11 89.84(3) . . ? Cl9 Nb2 Cl11 178.20(2) . . ? Cl10 Nb2 Cl11 90.00(3) . . ? Cl7 Nb2 Cl12 177.62(3) . . ? Cl8 Nb2 Cl12 89.52(3) . . ? Cl9 Nb2 Cl12 91.72(3) . . ? Cl10 Nb2 Cl12 87.67(3) . . ? Cl11 Nb2 Cl12 89.92(3) . . ? C2 N1 C5 108.0(2) . . ? C2 N1 C6 126.0(2) . . ? C5 N1 C6 125.9(2) . . ? C2 N3 C4 107.7(2) . . ? C2 N3 C8 126.0(2) . . ? C4 N3 C8 126.2(2) . . ? N1 C2 N3 109.3(2) . . ? C5 C4 N3 107.3(2) . . ? C4 C5 N1 107.7(2) . . ? N1 C6 C7 112.4(3) . . ? C10 N9 C13 108.0(2) . . ? C10 N9 C14 125.6(2) . . ? C13 N9 C14 126.2(2) . . ? C10 N11 C12 107.9(2) . . ? C10 N11 C16 125.5(2) . . ? C12 N11 C16 126.6(2) . . ? N9 C10 N11 109.3(2) . . ? C13 C12 N11 107.3(2) . . ? C12 C13 N9 107.4(2) . . ? N9 C14 C15 112.4(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.90 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.883 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.089 #============================================================================ data_C10H16Cl6NP _database_code_depnum_ccdc_archive 'CCDC 746106' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1-butyl-4-methylpyridinium hexachloridophosphate' ; _chemical_name_common "'1-butyl-4-methylpyridinium hexachloridophosphate'" _chemical_melting_point ? _chemical_formula_moiety '[C10NH16][PCl6]' _chemical_formula_sum 'C10 H16 Cl6 N P' _chemical_formula_weight 393.91 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 14.6807(16) _cell_length_b 7.2421(7) _cell_length_c 16.1568(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.548(9) _cell_angle_gamma 90.00 _cell_volume 1683.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28243 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 IPDS 2' _diffrn_reflns_number 17331 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2977 _reflns_number_gt 2488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe X-Area' _computing_cell_refinement 'Stoe X-Area' _computing_data_reduction 'Stoe X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburger, 1999)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+2.0945P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2977 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0992 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P P 0.21524(6) 0.80592(12) 0.05884(5) 0.0359(2) Uani 1 1 d . . . Cl1 Cl 0.12505(9) 1.03485(15) 0.03046(7) 0.0634(3) Uani 1 1 d . . . Cl2 Cl 0.19993(7) 0.80900(13) 0.18768(5) 0.0481(3) Uani 1 1 d . . . Cl3 Cl 0.33291(8) 0.98588(18) 0.09051(7) 0.0677(4) Uani 1 1 d . . . Cl4 Cl 0.09897(7) 0.62205(14) 0.02774(6) 0.0500(3) Uani 1 1 d . . . Cl5 Cl 0.23222(7) 0.79694(14) -0.07015(5) 0.0484(3) Uani 1 1 d . . . Cl6 Cl 0.30654(7) 0.57055(15) 0.08654(6) 0.0516(3) Uani 1 1 d . . . N1 N 0.2785(2) 0.2761(4) 0.34491(19) 0.0433(7) Uani 1 1 d . . . C2 C 0.2134(3) 0.2017(6) 0.3829(2) 0.0500(10) Uani 1 1 d . . . C3 C 0.1242(3) 0.1773(6) 0.3399(2) 0.0490(10) Uani 1 1 d . . . C4 C 0.0977(3) 0.2268(5) 0.2555(2) 0.0423(8) Uani 1 1 d . . . C5 C 0.1661(3) 0.3091(6) 0.2196(3) 0.0503(10) Uani 1 1 d . . . C6 C 0.2537(3) 0.3319(5) 0.2642(3) 0.0520(10) Uani 1 1 d . . . C7 C 0.0026(4) 0.1919(8) 0.2050(4) 0.0621(12) Uani 1 1 d . . . C8 C 0.3764(3) 0.2931(6) 0.3912(3) 0.0590(11) Uani 1 1 d . . . H8A H 0.3770(3) 0.3438(19) 0.4439(18) 0.071 Uiso 1 1 calc R . . H8B H 0.4078(12) 0.373(3) 0.3621(10) 0.071 Uiso 1 1 calc R . . C9 C 0.4262(4) 0.1122(8) 0.4021(4) 0.0802(16) Uani 1 1 d . . . H9A H 0.509(3) 0.1465(12) 0.4298(10) 0.096 Uiso 1 1 calc R . . H9B H 0.3979(9) 0.029(3) 0.4581(18) 0.096 Uiso 1 1 calc R . . C10 C 0.4231(4) -0.0111(8) 0.3358(4) 0.095(2) Uani 1 1 d . . . H10A H 0.4468(10) 0.054(3) 0.2927(19) 0.114 Uiso 1 1 calc R . . H10B H 0.358(3) -0.0343(12) 0.3132(11) 0.114 Uiso 1 1 calc R . . C11 C 0.4685(4) -0.1892(7) 0.3447(4) 0.092(2) Uani 1 1 d . . . H11A H 0.4571(5) -0.253(2) 0.289(2) 0.138 Uiso 1 1 calc R . . H11B H 0.4433(9) -0.265(3) 0.3861(15) 0.138 Uiso 1 1 calc R . . H11C H 0.536(2) -0.1720(9) 0.3650(9) 0.138 Uiso 1 1 calc R . . H2 H 0.232(3) 0.169(6) 0.437(3) 0.064(13) Uiso 1 1 d . . . H3 H 0.077(3) 0.134(7) 0.369(3) 0.076(15) Uiso 1 1 d . . . H5 H 0.155(3) 0.342(6) 0.170(3) 0.056(13) Uiso 1 1 d . . . H6 H 0.307(3) 0.389(7) 0.242(3) 0.070(14) Uiso 1 1 d . . . H7A H -0.038(4) 0.180(8) 0.236(4) 0.086(19) Uiso 1 1 d . . . H7C H -0.001(5) 0.073(11) 0.177(5) 0.14(3) Uiso 1 1 d . . . H7B H -0.014(5) 0.283(10) 0.163(5) 0.13(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P 0.0395(5) 0.0378(5) 0.0315(4) 0.0000(4) 0.0101(4) -0.0077(4) Cl1 0.0854(8) 0.0505(6) 0.0571(6) 0.0102(5) 0.0211(6) 0.0186(5) Cl2 0.0659(6) 0.0486(5) 0.0338(4) -0.0025(4) 0.0193(4) -0.0050(4) Cl3 0.0740(7) 0.0793(8) 0.0486(6) -0.0022(5) 0.0095(5) -0.0454(6) Cl4 0.0444(5) 0.0585(6) 0.0462(5) 0.0015(4) 0.0066(4) -0.0188(4) Cl5 0.0588(6) 0.0561(6) 0.0325(4) 0.0022(4) 0.0146(4) -0.0091(4) Cl6 0.0508(5) 0.0623(6) 0.0439(5) 0.0067(4) 0.0147(4) 0.0137(5) N1 0.0555(19) 0.0327(15) 0.0411(16) -0.0047(13) 0.0084(14) 0.0068(14) C2 0.068(3) 0.051(2) 0.0321(19) 0.0004(17) 0.0129(19) 0.015(2) C3 0.061(3) 0.049(2) 0.041(2) 0.0062(17) 0.0204(19) 0.0102(19) C4 0.055(2) 0.0306(17) 0.0421(19) -0.0002(14) 0.0117(17) 0.0097(16) C5 0.069(3) 0.044(2) 0.038(2) 0.0114(18) 0.0104(19) 0.0031(19) C6 0.064(3) 0.040(2) 0.053(2) 0.0074(18) 0.013(2) -0.0018(19) C7 0.058(3) 0.066(3) 0.060(3) 0.000(2) 0.007(2) 0.007(2) C8 0.065(3) 0.050(2) 0.058(3) -0.012(2) 0.003(2) 0.001(2) C9 0.055(3) 0.073(3) 0.105(4) -0.032(3) 0.000(3) 0.011(2) C10 0.069(3) 0.077(4) 0.125(5) -0.045(4) -0.014(3) 0.021(3) C11 0.069(3) 0.064(3) 0.144(6) -0.036(3) 0.024(4) 0.009(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 P Cl1 2.1140(14) . ? P Cl2 2.1382(12) . ? P Cl3 2.1425(13) . ? P Cl4 2.1438(12) . ? P Cl5 2.1488(12) . ? P Cl6 2.1592(14) . ? N1 C6 1.343(5) . ? N1 C2 1.348(5) . ? N1 C8 1.487(5) . ? C2 C3 1.365(6) . ? C3 C4 1.389(5) . ? C4 C5 1.390(6) . ? C4 C7 1.492(6) . ? C5 C6 1.353(6) . ? C8 C9 1.494(7) . ? C9 C10 1.389(7) . ? C10 C11 1.446(7) . ? 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 Cl1 P Cl2 91.13(5) . . ? Cl1 P Cl3 90.85(6) . . ? Cl2 P Cl3 89.88(5) . . ? Cl1 P Cl4 90.09(6) . . ? Cl2 P Cl4 90.04(5) . . ? Cl3 P Cl4 179.06(7) . . ? Cl1 P Cl5 90.15(5) . . ? Cl2 P Cl5 178.70(7) . . ? Cl3 P Cl5 90.32(5) . . ? Cl4 P Cl5 89.74(5) . . ? Cl1 P Cl6 179.35(7) . . ? Cl2 P Cl6 89.33(5) . . ? Cl3 P Cl6 89.62(6) . . ? Cl4 P Cl6 89.44(5) . . ? Cl5 P Cl6 89.40(5) . . ? C6 N1 C2 118.9(4) . . ? C6 N1 C8 120.7(4) . . ? C2 N1 C8 120.4(3) . . ? N1 C2 C3 121.0(4) . . ? C2 C3 C4 121.2(4) . . ? C3 C4 C5 115.9(4) . . ? C3 C4 C7 122.7(4) . . ? C5 C4 C7 121.3(4) . . ? C6 C5 C4 121.2(4) . . ? N1 C6 C5 121.6(4) . . ? N1 C8 C9 112.8(4) . . ? C10 C9 C8 122.2(5) . . ? C9 C10 C11 123.6(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.836 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.073 #============================================================================ data_C10H16Cl6NNb _database_code_depnum_ccdc_archive 'CCDC 746107' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1-butyl-4-methylpyridinium hexachloridoniobate' ; _chemical_name_common "'1-butyl-4-methylpyridinium hexachloridoniobate'" _chemical_melting_point ? _chemical_formula_moiety '[C10NH16][PCl6]' _chemical_formula_sum 'C10 H16 Cl6 N1 Nb1' _chemical_formula_weight 455.85 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' Nb Nb -2.0727 0.6215 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 15.1731(19) _cell_length_b 7.3248(7) _cell_length_c 16.1930(18) _cell_angle_alpha 90.00 _cell_angle_beta 101.850(9) _cell_angle_gamma 90.00 _cell_volume 1761.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13394 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.o2 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.577 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 IPDS 2' _diffrn_reflns_number 11551 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.02 _reflns_number_total 3106 _reflns_number_gt 2567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe X-Area' _computing_cell_refinement 'Stoe X-Area' _computing_data_reduction 'Stoe X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburger, 1999)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0279P)^2^+2.4597P] 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 0.0060(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3106 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0809 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb Nb 0.71599(2) 0.32064(5) 0.557875(19) 0.03393(13) Uani 1 1 d . . . Cl1 Cl 0.62016(9) 0.57027(17) 0.52808(7) 0.0652(3) Uani 1 1 d . . . Cl2 Cl 0.59396(7) 0.11922(16) 0.52687(7) 0.0569(3) Uani 1 1 d . . . Cl3 Cl 0.70300(8) 0.32130(15) 0.69943(6) 0.0529(3) Uani 1 1 d . . . Cl4 Cl 0.84153(9) 0.5141(2) 0.59078(7) 0.0773(4) Uani 1 1 d . . . Cl5 Cl 0.72998(8) 0.30930(15) 0.41625(6) 0.0521(3) Uani 1 1 d . . . Cl6 Cl 0.81355(7) 0.06355(16) 0.58630(7) 0.0557(3) Uani 1 1 d . . . N1 N 0.2216(2) 0.2265(4) 0.1579(2) 0.0467(8) Uani 1 1 d . . . C2 C 0.2828(3) 0.3034(6) 0.1193(3) 0.0493(10) Uani 1 1 d . . . C3 C 0.3696(3) 0.3244(6) 0.1594(3) 0.0498(10) Uani 1 1 d . . . C4 C 0.3982(3) 0.2674(6) 0.2426(3) 0.0475(10) Uani 1 1 d . . . C5 C 0.3334(4) 0.1829(6) 0.2791(3) 0.0553(11) Uani 1 1 d . . . C6 C 0.2475(3) 0.1646(6) 0.2369(3) 0.0548(11) Uani 1 1 d . . . C7 C 0.1254(4) 0.2100(8) 0.1130(4) 0.0670(14) Uani 1 1 d . . . C8 C 0.0759(4) 0.3775(12) 0.1146(7) 0.185(8) Uani 1 1 d . . . H8A H 0.0754(4) 0.414(5) 0.075(5) 0.222 Uiso 1 1 calc R . . H8B H 0.033(6) 0.347(4) 0.1130(7) 0.222 Uiso 1 1 calc R . . C9 C 0.0805(4) 0.5148(10) 0.1600(6) 0.152(6) Uani 1 1 d . . . H9A H 0.133(4) 0.544(3) 0.1649(7) 0.182 Uiso 1 1 calc R . . H9B H 0.0774(5) 0.471(4) 0.205(4) 0.182 Uiso 1 1 calc R . . C10 C 0.0383(4) 0.6845(9) 0.1633(6) 0.115(3) Uani 1 1 d . . . H10A H 0.0643(11) 0.746(3) 0.216(2) 0.172 Uiso 1 1 calc R . . H10B H -0.026(3) 0.6659(12) 0.1598(6) 0.172 Uiso 1 1 calc R . . H10C H 0.0473(5) 0.760(3) 0.116(2) 0.172 Uiso 1 1 calc R . . C11 C 0.4924(4) 0.2960(9) 0.2914(4) 0.0719(15) Uani 1 1 d . . . H2 H 0.263(3) 0.338(6) 0.069(3) 0.046(12) Uiso 1 1 d . . . H3 H 0.409(3) 0.381(6) 0.130(3) 0.058(13) Uiso 1 1 d . . . H5 H 0.348(3) 0.150(6) 0.328(3) 0.053(13) Uiso 1 1 d . . . H6 H 0.202(3) 0.110(6) 0.257(3) 0.058(13) Uiso 1 1 d . . . H7A H 0.106(6) 0.109(14) 0.130(6) 0.17(4) Uiso 1 1 d . . . H7B H 0.131(5) 0.171(11) 0.061(5) 0.14(3) Uiso 1 1 d . . . H11A H 0.528(4) 0.300(8) 0.253(4) 0.09(2) Uiso 1 1 d . . . H11B H 0.493(5) 0.421(12) 0.314(5) 0.14(3) Uiso 1 1 d . . . H11C H 0.510(5) 0.204(10) 0.337(5) 0.13(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb 0.03918(19) 0.0349(2) 0.02812(18) -0.00060(13) 0.00780(12) -0.00877(14) Cl1 0.0900(8) 0.0505(7) 0.0591(7) 0.0128(5) 0.0246(6) 0.0199(6) Cl2 0.0474(5) 0.0603(7) 0.0582(6) 0.0070(5) -0.0005(5) -0.0231(5) Cl3 0.0787(7) 0.0516(6) 0.0326(5) 0.0002(4) 0.0209(5) -0.0015(5) Cl4 0.0832(8) 0.0908(10) 0.0543(7) -0.0012(6) 0.0055(6) -0.0574(8) Cl5 0.0717(7) 0.0566(6) 0.0301(5) -0.0008(4) 0.0155(4) -0.0082(5) Cl6 0.0543(6) 0.0668(7) 0.0482(6) 0.0089(5) 0.0159(5) 0.0171(5) N1 0.059(2) 0.0371(18) 0.0442(19) -0.0079(15) 0.0116(16) 0.0064(16) C2 0.066(3) 0.049(2) 0.034(2) 0.0028(19) 0.013(2) 0.014(2) C3 0.064(3) 0.046(2) 0.045(2) 0.0027(19) 0.023(2) 0.006(2) C4 0.058(2) 0.035(2) 0.049(2) -0.0014(17) 0.0100(19) 0.0111(19) C5 0.087(3) 0.041(2) 0.037(2) 0.0080(19) 0.010(2) 0.010(2) C6 0.072(3) 0.040(2) 0.055(3) 0.004(2) 0.021(2) -0.002(2) C7 0.063(3) 0.058(3) 0.076(4) -0.021(3) 0.005(3) 0.001(3) C8 0.050(3) 0.135(8) 0.340(19) -0.141(11) -0.031(6) 0.023(4) C9 0.075(4) 0.096(6) 0.252(13) -0.099(7) -0.043(5) 0.028(4) C10 0.060(3) 0.077(5) 0.201(9) -0.036(5) 0.013(4) 0.015(3) C11 0.070(3) 0.073(4) 0.067(4) -0.001(3) 0.000(3) 0.011(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 Nb Cl1 2.3243(12) . ? Nb Cl2 2.3400(11) . ? Nb Cl3 2.3407(10) . ? Nb Cl4 2.3459(11) . ? Nb Cl5 2.3476(10) . ? Nb Cl6 2.3810(11) . ? N1 C6 1.337(6) . ? N1 C2 1.344(5) . ? N1 C7 1.496(6) . ? C2 C3 1.353(6) . ? C2 H2 0.84(4) . ? C3 C4 1.392(6) . ? C3 H3 0.93(5) . ? C4 C5 1.392(6) . ? C4 C11 1.500(7) . ? C5 C6 1.348(7) . ? C5 H5 0.81(5) . ? C6 H6 0.91(4) . ? C7 C8 1.442(9) . ? C7 H7A 0.86(10) . ? C7 H7B 0.91(8) . ? C8 C9 1.239(9) . ? C8 H8A 0.6878 . ? C8 H8B 0.6878 . ? C9 C10 1.404(8) . ? C9 H9A 0.8133 . ? C9 H9B 0.8133 . ? C10 H10A 0.9773 . ? C10 H10B 0.9773 . ? C10 H10C 0.9773 . ? C11 H11A 0.90(6) . ? C11 H11B 0.98(9) . ? C11 H11C 1.00(8) . ? 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 Cl1 Nb Cl2 91.02(5) . . ? Cl1 Nb Cl3 91.53(4) . . ? Cl2 Nb Cl3 89.39(4) . . ? Cl1 Nb Cl4 90.92(6) . . ? Cl2 Nb Cl4 178.04(5) . . ? Cl3 Nb Cl4 90.23(4) . . ? Cl1 Nb Cl5 90.18(4) . . ? Cl2 Nb Cl5 89.68(4) . . ? Cl3 Nb Cl5 178.06(4) . . ? Cl4 Nb Cl5 90.64(4) . . ? Cl1 Nb Cl6 179.16(4) . . ? Cl2 Nb Cl6 88.62(4) . . ? Cl3 Nb Cl6 89.22(4) . . ? Cl4 Nb Cl6 89.44(5) . . ? Cl5 Nb Cl6 89.06(4) . . ? C6 N1 C2 119.4(4) . . ? C6 N1 C7 120.2(4) . . ? C2 N1 C7 120.4(4) . . ? N1 C2 C3 121.5(4) . . ? N1 C2 H2 116(3) . . ? C3 C2 H2 123(3) . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3 118(3) . . ? C4 C3 H3 121(3) . . ? C3 C4 C5 116.0(4) . . ? C3 C4 C11 122.8(5) . . ? C5 C4 C11 121.2(5) . . ? C6 C5 C4 121.5(4) . . ? C6 C5 H5 121(3) . . ? C4 C5 H5 118(3) . . ? N1 C6 C5 121.0(4) . . ? N1 C6 H6 114(3) . . ? C5 C6 H6 125(3) . . ? C8 C7 N1 112.5(5) . . ? C8 C7 H7A 121(6) . . ? N1 C7 H7A 106(6) . . ? C8 C7 H7B 115(5) . . ? N1 C7 H7B 102(5) . . ? H7A C7 H7B 97(7) . . ? C9 C8 C7 137.4(8) . . ? C9 C8 H8A 102.8 . . ? C7 C8 H8A 102.8 . . ? C9 C8 H8B 102.8 . . ? C7 C8 H8B 102.8 . . ? H8A C8 H8B 105.0 . . ? C8 C9 C10 140.4(9) . . ? C8 C9 H9A 101.9 . . ? C10 C9 H9A 101.9 . . ? C8 C9 H9B 101.9 . . ? C10 C9 H9B 101.9 . . ? H9A C9 H9B 104.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C4 C11 H11A 106(4) . . ? C4 C11 H11B 105(4) . . ? H11A C11 H11B 106(6) . . ? C4 C11 H11C 112(4) . . ? H11A C11 H11C 115(6) . . ? H11B C11 H11C 112(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.641 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.069 #============================================================================ data_C10H16Cl6NNb_a _database_code_depnum_ccdc_archive 'CCDC 746108' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1-butyl-3-methylpyridinium hexachloridoniobate' ; _chemical_name_common "'1-butyl-3-methylpyridinium hexachloridoniobate'" _chemical_melting_point ? _chemical_formula_moiety '[C10NH16][PCl6]' _chemical_formula_sum 'C10 H16 Cl6 N1 Nb1' _chemical_formula_weight 455.85 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' Nb Nb -2.0727 0.6215 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3957(11) _cell_length_b 23.050(2) _cell_length_c 14.9737(16) _cell_angle_alpha 90.00 _cell_angle_beta 102.278(8) _cell_angle_gamma 90.00 _cell_volume 3505.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26135 _cell_measurement_theta_min 0.996 _cell_measurement_theta_max 25.68 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.584 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 IPDS 2' _diffrn_reflns_number 18668 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6632 _reflns_number_gt 5182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe X-Area' _computing_cell_refinement 'Stoe X-Area' _computing_data_reduction 'Stoe X-Area' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburger, 1999)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+2.3213P] 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 0.00125(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6632 _refine_ls_number_parameters 447 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0953 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb -0.00048(4) 0.642195(17) 0.20025(2) 0.03676(11) Uani 1 1 d . . . Nb2 Nb 0.43235(4) 0.883254(16) 0.18579(2) 0.03410(11) Uani 1 1 d . . . Cl1 Cl -0.11618(13) 0.59873(6) 0.06636(8) 0.0550(3) Uani 1 1 d . . . Cl2 Cl -0.17636(12) 0.70643(6) 0.19422(9) 0.0546(3) Uani 1 1 d . . . Cl3 Cl -0.09435(13) 0.57740(6) 0.28975(8) 0.0567(3) Uani 1 1 d . . . Cl4 Cl 0.11217(14) 0.69052(7) 0.33228(8) 0.0634(3) Uani 1 1 d . . . Cl5 Cl 0.10199(13) 0.70458(5) 0.11209(8) 0.0512(3) Uani 1 1 d . . . Cl6 Cl 0.17490(13) 0.57584(6) 0.20867(10) 0.0608(3) Uani 1 1 d . . . Cl7 Cl 0.31433(13) 0.85369(6) 0.04277(7) 0.0567(3) Uani 1 1 d . . . Cl8 Cl 0.60613(12) 0.82167(6) 0.17099(8) 0.0521(3) Uani 1 1 d . . . Cl9 Cl 0.33599(12) 0.80965(5) 0.25759(8) 0.0497(3) Uani 1 1 d . . . Cl10 Cl 0.25868(11) 0.94493(5) 0.20209(8) 0.0439(2) Uani 1 1 d . . . Cl11 Cl 0.55739(13) 0.91535(6) 0.32753(8) 0.0574(3) Uani 1 1 d . . . Cl12 Cl 0.52369(14) 0.95922(6) 0.11356(10) 0.0616(3) Uani 1 1 d . . . N1 N 0.4935(3) 0.62293(16) 0.2523(2) 0.0389(8) Uani 1 1 d . . . N12 N 0.0765(4) 0.38104(17) 0.2842(2) 0.0437(8) Uani 1 1 d . . . C2 C 0.4495(5) 0.6615(2) 0.1863(3) 0.0417(10) Uani 1 1 d . . . C3 C 0.4695(4) 0.6542(2) 0.0991(3) 0.0426(10) Uani 1 1 d . . . C4 C 0.5366(5) 0.6047(2) 0.0829(3) 0.0498(12) Uani 1 1 d . . . C5 C 0.5799(6) 0.5655(3) 0.1510(4) 0.0586(14) Uani 1 1 d . . . C6 C 0.5586(5) 0.5754(2) 0.2355(4) 0.0504(11) Uani 1 1 d . . . C7 C 0.4766(6) 0.6333(3) 0.3482(3) 0.0531(12) Uani 1 1 d . . . C8 C 0.6048(7) 0.6595(3) 0.4063(4) 0.0733(17) Uani 1 1 d . . . C9 C 0.6312(7) 0.7204(3) 0.3805(4) 0.0715(16) Uani 1 1 d . . . C10 C 0.7531(10) 0.7458(4) 0.4394(4) 0.078(2) Uani 1 1 d . . . C11 C 0.4181(9) 0.6981(3) 0.0263(4) 0.0678(17) Uani 1 1 d . . . C13 C 0.1271(5) 0.4315(2) 0.3210(3) 0.0461(11) Uani 1 1 d . . . C14 C 0.1235(5) 0.4454(3) 0.4099(3) 0.0549(13) Uani 1 1 d . . . C15 C 0.0627(6) 0.4049(3) 0.4575(4) 0.0679(19) Uani 1 1 d . . . C16 C 0.0116(6) 0.3541(3) 0.4189(4) 0.0653(15) Uani 1 1 d . . . C17 C 0.0174(5) 0.3432(3) 0.3310(4) 0.0542(12) Uani 1 1 d . . . C18 C 0.0810(5) 0.3655(3) 0.1883(3) 0.0528(12) Uani 1 1 d . . . C19 C -0.0512(5) 0.3755(2) 0.1234(3) 0.0504(12) Uani 1 1 d . . . C20 C -0.0885(5) 0.4388(2) 0.1044(3) 0.0507(12) Uani 1 1 d . . . C21 C -0.2228(7) 0.4449(3) 0.0416(4) 0.0653(15) Uani 1 1 d . . . C22 C 0.1826(8) 0.5013(4) 0.4496(6) 0.086(3) Uani 1 1 d . . . H2 H 0.410(5) 0.692(2) 0.200(3) 0.034(12) Uiso 1 1 d . . . H4 H 0.553(6) 0.596(3) 0.028(4) 0.070(17) Uiso 1 1 d . . . H5 H 0.617(6) 0.533(3) 0.144(4) 0.070(18) Uiso 1 1 d . . . H6 H 0.587(5) 0.551(2) 0.289(3) 0.049(13) Uiso 1 1 d . . . H7A H 0.400(5) 0.657(2) 0.340(3) 0.037(12) Uiso 1 1 d . . . H7B H 0.464(8) 0.593(3) 0.373(5) 0.10(2) Uiso 1 1 d . . . H8A H 0.534(3) 0.6897(14) 0.3869(19) 0.000(6) Uiso 1 1 d . . . H8B H 0.6356 0.6368 0.4740 0.051 Uiso 1 1 d . . . H9A H 0.5441 0.7503 0.3797 0.8(2) Uiso 1 1 d . . . H9B H 0.633(7) 0.723(3) 0.309(4) 0.082(19) Uiso 1 1 d . . . H10A H 0.750(10) 0.786(4) 0.426(6) 0.13(3) Uiso 1 1 d . . . H10B H 0.818(11) 0.727(5) 0.438(7) 0.14(5) Uiso 1 1 d . . . H10C H 0.738(8) 0.750(3) 0.507(6) 0.11(2) Uiso 1 1 d . . . H11A H 0.416(10) 0.685(4) -0.023(7) 0.13(4) Uiso 1 1 d . . . H11B H 0.364(11) 0.724(5) 0.041(7) 0.14(4) Uiso 1 1 d . . . H11C H 0.490(16) 0.712(6) 0.025(9) 0.20(6) Uiso 1 1 d . . . H13 H 0.166(5) 0.457(2) 0.278(3) 0.040(12) Uiso 1 1 d . . . H15 H 0.063(6) 0.412(3) 0.508(4) 0.07(2) Uiso 1 1 d . . . H16 H -0.030(7) 0.322(3) 0.453(4) 0.08(2) Uiso 1 1 d . . . H17 H -0.015(8) 0.310(3) 0.303(5) 0.10(3) Uiso 1 1 d . . . H18A H 0.124(7) 0.325(3) 0.193(4) 0.08(2) Uiso 1 1 d . . . H18B H 0.148(6) 0.386(3) 0.172(4) 0.066(17) Uiso 1 1 d . . . H19A H -0.115(6) 0.356(3) 0.153(4) 0.072(17) Uiso 1 1 d . . . H19B H -0.035(6) 0.356(3) 0.069(4) 0.075(18) Uiso 1 1 d . . . H20A H -0.086(4) 0.4579(19) 0.162(3) 0.038(11) Uiso 1 1 d . . . H20B H -0.026(5) 0.455(2) 0.078(3) 0.047(13) Uiso 1 1 d . . . H21A H -0.238(6) 0.485(3) 0.023(4) 0.073(18) Uiso 1 1 d . . . H21B H -0.225(6) 0.428(3) -0.022(4) 0.069(17) Uiso 1 1 d . . . H21C H -0.300(9) 0.426(4) 0.070(5) 0.12(3) Uiso 1 1 d . . . H22A H 0.262(8) 0.500(3) 0.475(5) 0.08(2) Uiso 1 1 d . . . H22B H 0.146(10) 0.514(4) 0.495(6) 0.14(3) Uiso 1 1 d . . . H22C H 0.206(10) 0.528(4) 0.412(6) 0.13(4) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nb1 0.0333(2) 0.0395(2) 0.03886(19) -0.00108(15) 0.01089(15) -0.00140(17) Nb2 0.03149(19) 0.0368(2) 0.03426(18) 0.00191(14) 0.00758(14) 0.00470(16) Cl1 0.0564(7) 0.0629(7) 0.0474(6) -0.0135(5) 0.0148(5) -0.0159(6) Cl2 0.0443(6) 0.0581(7) 0.0632(7) -0.0023(6) 0.0154(5) 0.0123(6) Cl3 0.0524(7) 0.0670(8) 0.0534(6) 0.0136(6) 0.0175(5) -0.0100(6) Cl4 0.0577(8) 0.0774(9) 0.0488(6) -0.0123(6) -0.0028(5) -0.0050(7) Cl5 0.0547(7) 0.0478(6) 0.0569(6) 0.0000(5) 0.0244(5) -0.0104(6) Cl6 0.0460(7) 0.0488(7) 0.0918(9) 0.0059(6) 0.0240(6) 0.0081(6) Cl7 0.0521(7) 0.0751(8) 0.0387(5) -0.0096(5) 0.0003(5) 0.0114(6) Cl8 0.0408(6) 0.0569(7) 0.0589(6) -0.0017(5) 0.0109(5) 0.0180(5) Cl9 0.0502(7) 0.0418(6) 0.0594(6) 0.0106(5) 0.0170(5) 0.0016(5) Cl10 0.0361(5) 0.0387(5) 0.0585(6) -0.0022(5) 0.0137(5) 0.0056(5) Cl11 0.0482(7) 0.0730(8) 0.0464(6) -0.0125(5) -0.0004(5) 0.0000(6) Cl12 0.0542(7) 0.0586(8) 0.0794(8) 0.0232(6) 0.0309(6) 0.0015(6) N1 0.0322(18) 0.044(2) 0.0411(18) 0.0005(16) 0.0103(14) -0.0012(16) N12 0.038(2) 0.049(2) 0.0451(19) -0.0041(17) 0.0113(16) 0.0057(18) C2 0.037(2) 0.040(2) 0.046(2) -0.0045(19) 0.0064(19) 0.002(2) C3 0.040(2) 0.045(3) 0.042(2) -0.0026(18) 0.0062(18) -0.010(2) C4 0.043(3) 0.062(3) 0.046(3) -0.012(2) 0.015(2) -0.002(2) C5 0.053(3) 0.051(3) 0.072(3) -0.012(3) 0.015(3) 0.013(3) C6 0.047(3) 0.043(3) 0.060(3) 0.001(2) 0.008(2) 0.005(2) C7 0.052(3) 0.069(4) 0.042(2) 0.001(2) 0.019(2) 0.000(3) C8 0.086(5) 0.089(4) 0.042(3) 0.009(3) 0.007(3) 0.010(4) C9 0.080(4) 0.084(4) 0.051(3) 0.000(3) 0.015(3) -0.008(4) C10 0.092(6) 0.082(5) 0.053(3) 0.002(3) -0.001(3) -0.023(5) C11 0.086(5) 0.069(4) 0.048(3) 0.009(3) 0.011(3) -0.003(4) C13 0.035(2) 0.052(3) 0.049(2) -0.011(2) 0.005(2) 0.002(2) C14 0.037(2) 0.074(3) 0.048(2) -0.016(2) -0.003(2) 0.023(3) C15 0.054(3) 0.112(5) 0.038(3) 0.008(3) 0.011(2) 0.041(4) C16 0.057(3) 0.079(4) 0.063(3) 0.019(3) 0.017(3) 0.016(3) C17 0.041(3) 0.053(3) 0.069(3) 0.012(2) 0.012(2) 0.010(2) C18 0.045(3) 0.064(3) 0.054(3) -0.017(2) 0.020(2) 0.000(3) C19 0.054(3) 0.056(3) 0.042(2) -0.014(2) 0.014(2) -0.009(2) C20 0.048(3) 0.062(3) 0.046(2) -0.015(2) 0.018(2) -0.016(2) C21 0.068(4) 0.068(4) 0.056(3) -0.014(3) 0.005(3) -0.007(3) C22 0.056(4) 0.109(6) 0.083(5) -0.055(5) -0.007(4) 0.017(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 Nb1 Cl1 2.3334(12) . ? Nb1 Cl2 2.3395(13) . ? Nb1 Cl3 2.3527(12) . ? Nb1 Cl4 2.3528(13) . ? Nb1 Cl5 2.3543(12) . ? Nb1 Cl6 2.3625(13) . ? Nb2 Cl7 2.3320(12) . ? Nb2 Cl8 2.3448(12) . ? Nb2 Cl9 2.3443(12) . ? Nb2 Cl10 2.3511(11) . ? Nb2 Cl11 2.3597(12) . ? Nb2 Cl12 2.3609(12) . ? N1 C2 1.336(6) . ? N1 C6 1.339(6) . ? N1 C7 1.503(5) . ? N12 C13 1.345(6) . ? N12 C17 1.346(7) . ? N12 C18 1.490(6) . ? C2 C3 1.376(6) . ? C2 H2 0.86(5) . ? C3 C4 1.385(7) . ? C3 C11 1.500(8) . ? C4 C5 1.366(8) . ? C4 H4 0.90(6) . ? C5 C6 1.349(7) . ? C5 H5 0.86(6) . ? C6 H6 0.97(5) . ? C7 C8 1.551(9) . ? C7 H7A 0.96(5) . ? C7 H7B 1.02(7) . ? C8 C9 1.498(9) . ? C8 H8A 1.01(3) . ? C8 H8B 1.124(6) . ? C9 C10 1.500(10) . ? C9 H9A 1.135(7) . ? C9 H9B 1.07(6) . ? C10 H10A 0.94(10) . ? C10 H10B 0.80(11) . ? C10 H10C 1.07(8) . ? C11 H11A 0.80(10) . ? C11 H11B 0.89(11) . ? C11 H11C 0.81(16) . ? C13 C14 1.377(6) . ? C13 H13 1.02(5) . ? C14 C15 1.405(9) . ? C14 C22 1.494(10) . ? C15 C16 1.361(10) . ? C15 H15 0.77(6) . ? C16 C17 1.354(8) . ? C16 H16 1.04(7) . ? C17 H17 0.91(8) . ? C18 C19 1.523(8) . ? C18 H18A 1.02(7) . ? C18 H18B 0.91(6) . ? C19 C20 1.520(8) . ? C19 H19A 0.98(6) . ? C19 H19B 0.99(6) . ? C20 C21 1.515(8) . ? C20 H20A 0.97(4) . ? C20 H20B 0.91(5) . ? C21 H21A 0.97(6) . ? C21 H21B 1.03(6) . ? C21 H21C 1.07(9) . ? C22 H22A 0.83(8) . ? C22 H22B 0.90(10) . ? C22 H22C 0.90(9) . ? 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 Cl1 Nb1 Cl2 89.01(5) . . ? Cl1 Nb1 Cl3 90.94(5) . . ? Cl2 Nb1 Cl3 90.48(5) . . ? Cl1 Nb1 Cl4 177.15(5) . . ? Cl2 Nb1 Cl4 88.74(5) . . ? Cl3 Nb1 Cl4 90.83(5) . . ? Cl1 Nb1 Cl5 89.57(5) . . ? Cl2 Nb1 Cl5 92.00(5) . . ? Cl3 Nb1 Cl5 177.48(5) . . ? Cl4 Nb1 Cl5 88.76(5) . . ? Cl1 Nb1 Cl6 91.08(5) . . ? Cl2 Nb1 Cl6 178.62(5) . . ? Cl3 Nb1 Cl6 88.14(5) . . ? Cl4 Nb1 Cl6 91.21(5) . . ? Cl5 Nb1 Cl6 89.38(5) . . ? Cl7 Nb2 Cl8 90.10(5) . . ? Cl7 Nb2 Cl9 90.97(5) . . ? Cl8 Nb2 Cl9 91.04(5) . . ? Cl7 Nb2 Cl10 90.37(4) . . ? Cl8 Nb2 Cl10 179.47(4) . . ? Cl9 Nb2 Cl10 88.71(4) . . ? Cl7 Nb2 Cl11 177.69(5) . . ? Cl8 Nb2 Cl11 89.23(5) . . ? Cl9 Nb2 Cl11 91.25(5) . . ? Cl10 Nb2 Cl11 90.31(5) . . ? Cl7 Nb2 Cl12 88.88(5) . . ? Cl8 Nb2 Cl12 90.72(5) . . ? Cl9 Nb2 Cl12 178.23(5) . . ? Cl10 Nb2 Cl12 89.52(5) . . ? Cl11 Nb2 Cl12 88.92(5) . . ? C2 N1 C6 120.9(4) . . ? C2 N1 C7 120.6(4) . . ? C6 N1 C7 118.4(4) . . ? C13 N12 C17 121.9(4) . . ? C13 N12 C18 120.8(4) . . ? C17 N12 C18 117.2(5) . . ? N1 C2 C3 121.5(4) . . ? N1 C2 H2 118(3) . . ? C3 C2 H2 121(3) . . ? C2 C3 C4 116.8(4) . . ? C2 C3 C11 120.3(5) . . ? C4 C3 C11 122.9(5) . . ? C5 C4 C3 120.8(4) . . ? C5 C4 H4 116(4) . . ? C3 C4 H4 123(4) . . ? C6 C5 C4 119.7(5) . . ? C6 C5 H5 116(4) . . ? C4 C5 H5 125(4) . . ? N1 C6 C5 120.3(5) . . ? N1 C6 H6 114(3) . . ? C5 C6 H6 126(3) . . ? N1 C7 C8 109.7(4) . . ? N1 C7 H7A 104(3) . . ? C8 C7 H7A 116(3) . . ? N1 C7 H7B 105(4) . . ? C8 C7 H7B 108(4) . . ? H7A C7 H7B 114(5) . . ? C9 C8 C7 113.8(5) . . ? C9 C8 H8A 55.9(18) . . ? C7 C8 H8A 67.7(18) . . ? C9 C8 H8B 129.5(6) . . ? C7 C8 H8B 111.8(6) . . ? H8A C8 H8B 129.2(17) . . ? C8 C9 C10 113.1(6) . . ? C8 C9 H9A 112.4(6) . . ? C10 C9 H9A 110.0(7) . . ? C8 C9 H9B 110(3) . . ? C10 C9 H9B 112(4) . . ? H9A C9 H9B 98(4) . . ? C9 C10 H10A 106(6) . . ? C9 C10 H10B 113(8) . . ? H10A C10 H10B 121(10) . . ? C9 C10 H10C 108(4) . . ? H10A C10 H10C 97(6) . . ? H10B C10 H10C 112(8) . . ? C3 C11 H11A 111(7) . . ? C3 C11 H11B 115(6) . . ? H11A C11 H11B 127(9) . . ? C3 C11 H11C 95(10) . . ? H11A C11 H11C 88(10) . . ? H11B C11 H11C 112(10) . . ? N12 C13 C14 120.6(5) . . ? N12 C13 H13 115(3) . . ? C14 C13 H13 124(3) . . ? C13 C14 C15 116.3(5) . . ? C13 C14 C22 119.5(6) . . ? C15 C14 C22 124.2(6) . . ? C16 C15 C14 122.2(5) . . ? C16 C15 H15 120(5) . . ? C14 C15 H15 117(5) . . ? C17 C16 C15 118.5(6) . . ? C17 C16 H16 117(4) . . ? C15 C16 H16 124(3) . . ? N12 C17 C16 120.4(6) . . ? N12 C17 H17 119(5) . . ? C16 C17 H17 121(5) . . ? N12 C18 C19 111.7(4) . . ? N12 C18 H18A 104(3) . . ? C19 C18 H18A 120(4) . . ? N12 C18 H18B 108(4) . . ? C19 C18 H18B 113(4) . . ? H18A C18 H18B 98(5) . . ? C18 C19 C20 115.1(4) . . ? C18 C19 H19A 104(4) . . ? C20 C19 H19A 111(4) . . ? C18 C19 H19B 100(4) . . ? C20 C19 H19B 112(3) . . ? H19A C19 H19B 115(5) . . ? C21 C20 C19 111.7(5) . . ? C21 C20 H20A 111(3) . . ? C19 C20 H20A 108(3) . . ? C21 C20 H20B 110(3) . . ? C19 C20 H20B 108(3) . . ? H20A C20 H20B 108(4) . . ? C20 C21 H21A 110(4) . . ? C20 C21 H21B 112(4) . . ? H21A C21 H21B 97(5) . . ? C20 C21 H21C 113(4) . . ? H21A C21 H21C 113(6) . . ? H21B C21 H21C 111(5) . . ? C14 C22 H22A 116(5) . . ? C14 C22 H22B 112(7) . . ? H22A C22 H22B 101(7) . . ? C14 C22 H22C 119(6) . . ? H22A C22 H22C 86(8) . . ? H22B C22 H22C 118(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.748 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.083