# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Simon Clarke' 'Oltan Gal' 'Nicholas Watney' 'D. Webster' 'Simon J. Clarke' _publ_contact_author_name 'Dr Simon Clarke' _publ_contact_author_address ; Inorganic Chemistry Laboratory University of Oxford South Parks Road Oxford OX1 3QR ; _publ_contact_author_email SIMON.CLARKE@CHEM.OX.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; The first ternary tin (II) nitride: NaSnN ; data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 269578' _audit_creation_date 05-04-11 _audit_creation_method CRYSTALS_ver_12.39 _oxford_structure_analysis_title 'mw019-2-p63unm in P 63 m c' _chemical_name_systematic 'Sodium tin(II) nitride' _chemical_melting_point ? _cell_length_a 3.33060(10) _cell_length_b 3.33060(10) _cell_length_c 10.8919(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 104.636(7) _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63 m c ' _symmetry_space_group_name_Hall 'P 6c -2c' loop_ _symmetry_equiv_pos_as_xyz x,y,z x-y,x,z+1/2 -y,x-y,z -x,-y,z+1/2 -x+y,-x,z y,-x+y,z+1/2 -x+y,y,z y,x,z+1/2 x,x-y,z x-y,-y,z+1/2 -y,-x,z -x,-x+y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Na 0.0362 0.0249 4.7626 3.2850 3.1736 8.8422 1.2674 0.3136 1.1128 129.4240 0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572 4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = N1 Na1 Sn1 # Dc = 4.94 Fooo = 136.00 Mu = 119.38 M = 25.95 # Found Formula = N1 Na1 Sn1 # Dc = 4.94 FOOO = 136.00 Mu = 119.38 M = 25.95 _chemical_formula_sum 'N Na Sn' _chemical_formula_moiety 'N Sn, Na' _chemical_compound_source ? _chemical_formula_weight 155.69 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 4053 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 42.106 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.02 -1 -2 -14 0.031 0 0 -1 0.028 1 6 15 0.034 -7 2 -15 0.032 6 -14 3 0.037 3 1 -11 0.041 -1 2 12 0.029 10 -9 5 0.043 0 2 -13 0.034 -4 3 -5 0.037 2 -6 -15 0.032 _exptl_crystal_density_diffrn 4.941 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 136 _exptl_absorpt_coefficient_mu 11.938 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.4378 _exptl_absorpt_correction_T_max 0.62 _exptl_absorpt_correction_T_ave 0.5467 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 220(2) _diffrn_reflns_number 4545 _reflns_number_total 340 _diffrn_reflns_av_R_equivalents 0.034 # Number of reflections with Friedels Law is 247 # Number of reflections without Friedels Law is 340 # Theoretical number of reflections is about 122 _diffrn_reflns_theta_min 7.077 _diffrn_reflns_theta_max 42.024 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 42.024 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -3 _reflns_limit_h_max 0 _reflns_limit_k_min 0 _reflns_limit_k_max 6 _reflns_limit_l_min -20 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.84 _refine_diff_density_max 1.05 _refine_ls_number_reflns 247 _refine_ls_number_restraints 1 _refine_ls_number_parameters 12 #_refine_ls_R_factor_ref 0.0176 _refine_ls_wR_factor_ref 0.0133 _refine_ls_goodness_of_fit_ref 1.1071 #_reflns_number_all 340 _refine_ls_R_factor_all 0.0262 _refine_ls_wR_factor_all 0.0137 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 247 _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_gt 0.0133 _refine_ls_shift/su_max 0.000051 _refine_ls_abs_structure_Flack 0.0(2) _refine_ls_abs_structure_details 'Flack, 93 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.868 -0.776 0.540 -0.667 0.268 ; _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Sn1 Sn 0.0000 0.0000 0.00004(18) 0.0069 1.0000 Uani S T . . . . Na1 Na 0.3333 0.6667 0.2466(7) 0.0128 1.0000 Uani S T . . . . N1 N 0.6667 0.3333 0.0980(4) 0.0081 1.0000 Uani S T . . . . 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 Sn1 0.00627(9) 0.00627(9) 0.00823(12) 0.0000 0.0000 0.00313(5) Na1 0.0128(5) 0.0128(5) 0.0127(9) 0.0000 0.0000 0.0064(3) N1 0.0067(10) 0.0067(10) 0.0108(16) 0.0000 0.0000 0.0033(5) _refine_ls_extinction_coef 2.95(16) _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _oxford_refine_ls_scale 1.176(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Sn1 . N1 1_445 2.199(3) yes Sn1 . N1 5_565 2.199(3) yes Sn1 . N1 . 2.199(3) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 1_445 Sn1 . N1 5_565 98.43(17) yes N1 1_445 Sn1 . N1 . 98.43(17) yes N1 5_565 Sn1 . N1 . 98.43(17) yes Sn1 11_665 N1 . Sn1 . 98.43(17) yes Sn1 11_665 N1 . Sn1 1_655 98.43(17) yes Sn1 . N1 . Sn1 1_655 98.43(17) yes