Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Dr Duncan Gregory' _publ_contact_author_address ; Dept of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_phone '0115 951 4594' _publ_contact_author_fax '0115 951 3563' _publ_contact_author_email Duncan.Gregory@nottingham.ac.uk _publ_section_title ; Synthesis and structure of new mixed alkaline-earth nitridomolybdates and nitridotungstates, (Ba,Ca)3[MN4] (M=Mo, W) ; loop_ _publ_author_name _publ_author_address C.F.Baker ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; D.H.Gregory ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; M.G.Barker ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; C.Wilson ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; A.J.Blake ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD England ; ##################################################################### data_cabwn4 _database_code_CSD 197516 _chemical_name_common 'Tri(barium,calcium) tetranitridomolybdate (VI)' _audit_creation_date 2002-10-25T09:11:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Tri(barium,calcium) tetranitridomolybdate (VI) ; _chemical_formula_moiety 'Ba8.92 Ca3.08 N16 Mo4' _chemical_formula_sum 'Ba2.23 Ca0.77 Mo N4' _chemical_formula_weight 488.87 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.441(2) _cell_length_b 9.967(2) _cell_length_c 11.938(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1242.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 881 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 28.44 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description tablet _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 5.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1682 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 16.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_absorpt_correction_T_min 0.203 _exptl_absorpt_correction_T_max 0.335 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD' _diffrn_measurement_method omega _diffrn_standards_decay_% none _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_av_unetI/netI 0.0537 _diffrn_reflns_number 7236 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.3 _diffrn_reflns_theta_max 28.84 _diffrn_reflns_theta_full 28.84 _diffrn_measured_fraction_theta_full 0.915 _diffrn_measured_fraction_theta_max 0.915 _reflns_number_total 1730 _reflns_number_gt 1130 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS 4.1 (Dowty, 1998)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_number_reflns 1492 _refine_ls_number_parameters 74 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.085 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.956 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.93 _refine_diff_density_min -2.334 _refine_diff_density_rms 0.467 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ba1 Ba 0.73414(6) -0.30888(7) 0.11601(4) 0.01367(17) Uani 1 1 d . . . Ba2 Ba 0.46749(6) -0.62280(6) 0.14527(4) 0.01251(17) Uani 1 1 d . . . Ba3 Ba 0.37700(13) 0.03328(13) 0.10520(10) 0.0129(5) Uani 0.227(4) 1 d P . . Ca3 Ca 0.37700(13) 0.03328(13) 0.10520(10) 0.0129(5) Uani 0.773(4) 1 d P . . Mo1 Mo 0.40505(8) -0.28913(9) 0.11922(6) 0.0123(2) Uani 1 1 d . . . N1 N 0.5065(8) -0.1756(9) 0.0322(7) 0.0177(19) Uani 1 1 d U . . N2 N 0.2848(8) -0.1801(10) 0.1901(7) 0.024(2) Uani 1 1 d U . . N3 N 0.5078(7) -0.3739(9) 0.2255(7) 0.0148(18) Uani 1 1 d U . . N4 N 0.3334(8) -0.4207(9) 0.0254(7) 0.0188(19) Uani 1 1 d U . . 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 Ba1 0.0132(3) 0.0225(4) 0.0053(3) -0.0008(2) 0.0009(2) -0.0008(2) Ba2 0.0177(3) 0.0149(3) 0.0050(3) 0.0004(2) -0.0014(2) -0.0009(2) Ba3 0.0173(8) 0.0148(8) 0.0067(7) 0.0003(5) -0.0020(5) -0.0001(5) Ca3 0.0173(8) 0.0148(8) 0.0067(7) 0.0003(5) -0.0020(5) -0.0001(5) Mo1 0.0125(4) 0.0190(5) 0.0055(4) 0.0029(3) -0.0002(3) 0.0001(3) N1 0.018(2) 0.018(3) 0.016(2) -0.0002(18) 0.0004(17) -0.0009(18) N2 0.023(3) 0.025(3) 0.023(3) 0.0023(18) 0.0026(18) 0.0020(18) N3 0.016(2) 0.015(2) 0.013(2) -0.0003(18) 0.0004(17) -0.0001(18) N4 0.020(2) 0.020(3) 0.016(2) 0.0011(18) -0.0018(17) -0.0021(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ba1 N2 2.699(9) 6_656 ? Ba1 N3 2.778(8) . ? Ba1 N1 2.901(8) . ? Ba1 N4 3.027(9) 3_545 ? Ba1 N4 3.257(9) 5_645 ? Ba1 N1 3.353(8) 3_545 ? Ba1 Mo1 3.4419(12) . ? Ba1 Mo1 3.4676(11) 3_545 ? Ba1 N3 3.487(8) 6_656 ? Ba1 Mo1 3.6351(12) 6_656 ? Ba1 Ba2 3.6423(10) 7_765 ? Ba1 N2 3.695(9) 3_545 ? Ba2 N3 2.693(9) . ? Ba2 N2 2.749(9) 7_655 ? Ba2 N4 2.840(9) . ? Ba2 N1 2.933(9) 5_645 ? Ba2 N4 2.943(8) 5_645 ? Ba2 N3 2.951(9) 4_645 ? Ba2 N2 3.298(9) 4_645 ? Ba2 Mo1 3.4032(13) . ? Ba2 Mo1 3.5248(11) 4_645 ? Ba2 Mo1 3.5371(12) 5_645 ? Ba2 Ca3 3.5877(16) 1_545 ? Ba2 Ba3 3.5877(16) 1_545 ? Ba3 N4 2.438(8) 7_665 ? Ba3 N1 2.486(9) 5_655 ? Ba3 N3 2.527(8) 4_655 ? Ba3 N2 2.545(9) . ? Ba3 N1 2.631(9) . ? Ba3 Mo1 3.2312(17) . ? Ba3 Mo1 3.4400(16) 7_665 ? Ba3 N2 3.470(10) 7_665 ? Ba3 Ba2 3.5877(16) 1_565 ? Ba3 Ca3 3.653(3) 5_655 ? Ba3 Ba3 3.653(3) 5_655 ? Ba3 Ba2 3.7323(15) 4_655 ? Mo1 N2 1.863(9) . ? Mo1 N3 1.864(8) . ? Mo1 N1 1.866(9) . ? Mo1 N4 1.880(9) . ? Mo1 Ca3 3.4400(16) 7_655 ? Mo1 Ba3 3.4400(16) 7_655 ? Mo1 Ba1 3.4676(11) 3_445 ? Mo1 Ba2 3.5248(11) 4_655 ? N1 Ca3 2.486(9) 5_655 ? N1 Ba3 2.486(9) 5_655 ? N1 Ba2 2.933(9) 5_645 ? N1 N2 2.986(12) . ? N1 N3 3.039(13) . ? N1 N4 3.041(13) . ? N1 Ba1 3.353(8) 3_445 ? N1 N1 3.586(18) 5_655 ? N2 Ba1 2.699(9) 6_556 ? N2 Ba2 2.749(9) 7_665 ? N2 N3 3.054(12) . ? N2 N4 3.143(13) . ? N2 Ba2 3.298(9) 4_655 ? N2 Ca3 3.470(10) 7_655 ? N2 Ba3 3.470(10) 7_655 ? N2 N4 3.475(13) 7_665 ? N3 Ca3 2.527(8) 4_645 ? N3 Ba3 2.527(8) 4_645 ? N3 Ba2 2.951(9) 4_655 ? N3 N4 3.040(11) . ? N3 Ba1 3.487(8) 6_556 ? N3 N2 3.621(12) 6_656 ? N3 N1 3.694(12) 8_556 ? N4 Ca3 2.438(8) 7_655 ? N4 Ba3 2.438(8) 7_655 ? N4 Ba2 2.943(8) 5_645 ? N4 Ba1 3.027(9) 3_445 ? N4 Ba1 3.257(9) 5_645 ? N4 N2 3.475(13) 7_655 ? N4 N1 3.611(12) 3_445 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ba1 N3 82.8(3) 6_656 . ? N2 Ba1 N1 103.8(3) 6_656 . ? N3 Ba1 N1 64.7(3) . . ? N2 Ba1 N4 93.0(3) 6_656 3_545 ? N3 Ba1 N4 136.9(2) . 3_545 ? N1 Ba1 N4 75.0(2) . 3_545 ? N2 Ba1 N4 151.7(2) 6_656 5_645 ? N3 Ba1 N4 82.3(2) . 5_645 ? N1 Ba1 N4 91.3(2) . 5_645 ? N4 Ba1 N4 114.3(3) 3_545 5_645 ? N2 Ba1 N1 107.9(2) 6_656 3_545 ? N3 Ba1 N1 163.6(3) . 3_545 ? N1 Ba1 N1 122.28(6) . 3_545 ? N4 Ba1 N1 56.7(2) 3_545 3_545 ? N4 Ba1 N1 82.6(2) 5_645 3_545 ? N2 Ba1 Mo1 99.15(19) 6_656 . ? N3 Ba1 Mo1 32.72(17) . . ? N1 Ba1 Mo1 32.83(17) . . ? N4 Ba1 Mo1 107.74(16) 3_545 . ? N4 Ba1 Mo1 80.62(15) 5_645 . ? N1 Ba1 Mo1 148.79(14) 3_545 . ? N2 Ba1 Mo1 117.4(2) 6_656 3_545 ? N3 Ba1 Mo1 152.23(17) . 3_545 ? N1 Ba1 Mo1 90.76(17) . 3_545 ? N4 Ba1 Mo1 32.78(16) 3_545 3_545 ? N4 Ba1 Mo1 85.69(15) 5_645 3_545 ? N1 Ba1 Mo1 31.70(15) 3_545 3_545 ? Mo1 Ba1 Mo1 120.44(2) . 3_545 ? N2 Ba1 N3 57.5(2) 6_656 6_656 ? N3 Ba1 N3 113.48(11) . 6_656 ? N1 Ba1 N3 160.6(2) . 6_656 ? N4 Ba1 N3 99.4(2) 3_545 6_656 ? N4 Ba1 N3 107.7(2) 5_645 6_656 ? N1 Ba1 N3 65.3(2) 3_545 6_656 ? Mo1 Ba1 N3 145.33(13) . 6_656 ? Mo1 Ba1 N3 94.02(13) 3_545 6_656 ? N2 Ba1 Mo1 29.8(2) 6_656 6_656 ? N3 Ba1 Mo1 91.20(17) . 6_656 ? N1 Ba1 Mo1 132.63(17) . 6_656 ? N4 Ba1 Mo1 106.02(16) 3_545 6_656 ? N4 Ba1 Mo1 126.99(15) 5_645 6_656 ? N1 Ba1 Mo1 92.58(14) 3_545 6_656 ? Mo1 Ba1 Mo1 118.51(2) . 6_656 ? Mo1 Ba1 Mo1 115.87(3) 3_545 6_656 ? N3 Ba1 Mo1 30.25(14) 6_656 6_656 ? N2 Ba1 Ba2 60.52(19) 6_656 7_765 ? N3 Ba1 Ba2 143.26(17) . 7_765 ? N1 Ba1 Ba2 120.04(18) . 7_765 ? N4 Ba1 Ba2 51.37(16) 3_545 7_765 ? N4 Ba1 Ba2 131.00(15) 5_645 7_765 ? N1 Ba1 Ba2 49.36(15) 3_545 7_765 ? Mo1 Ba1 Ba2 145.45(3) . 7_765 ? Mo1 Ba1 Ba2 59.61(2) 3_545 7_765 ? N3 Ba1 Ba2 48.84(14) 6_656 7_765 ? Mo1 Ba1 Ba2 57.939(19) 6_656 7_765 ? N2 Ba1 N2 146.5(2) 6_656 3_545 ? N3 Ba1 N2 125.5(2) . 3_545 ? N1 Ba1 N2 77.9(2) . 3_545 ? N4 Ba1 N2 54.7(2) 3_545 3_545 ? N4 Ba1 N2 59.6(2) 5_645 3_545 ? N1 Ba1 N2 49.8(2) 3_545 3_545 ? Mo1 Ba1 N2 98.96(14) . 3_545 ? Mo1 Ba1 N2 29.95(14) 3_545 3_545 ? N3 Ba1 N2 114.44(19) 6_656 3_545 ? Mo1 Ba1 N2 142.32(14) 6_656 3_545 ? Ba2 Ba1 N2 89.28(14) 7_765 3_545 ? N3 Ba2 N2 105.8(3) . 7_655 ? N3 Ba2 N4 66.6(2) . . ? N2 Ba2 N4 76.9(3) 7_655 . ? N3 Ba2 N1 150.9(2) . 5_645 ? N2 Ba2 N1 95.0(3) 7_655 5_645 ? N4 Ba2 N1 99.6(2) . 5_645 ? N3 Ba2 N4 90.0(2) . 5_645 ? N2 Ba2 N4 147.4(2) 7_655 5_645 ? N4 Ba2 N4 84.0(3) . 5_645 ? N1 Ba2 N4 62.3(2) 5_645 5_645 ? N3 Ba2 N3 125.57(4) . 4_645 ? N2 Ba2 N3 78.8(2) 7_655 4_645 ? N4 Ba2 N3 155.2(2) . 4_645 ? N1 Ba2 N3 77.8(2) 5_645 4_645 ? N4 Ba2 N3 115.1(2) 5_645 4_645 ? N3 Ba2 N2 79.9(2) . 4_645 ? N2 Ba2 N2 126.84(16) 7_655 4_645 ? N4 Ba2 N2 144.1(2) . 4_645 ? N1 Ba2 N2 103.8(2) 5_645 4_645 ? N4 Ba2 N2 83.3(2) 5_645 4_645 ? N3 Ba2 N2 58.2(2) 4_645 4_645 ? N3 Ba2 Mo1 33.08(18) . . ? N2 Ba2 Mo1 92.1(2) 7_655 . ? N4 Ba2 Mo1 33.54(17) . . ? N1 Ba2 Mo1 128.41(17) 5_645 . ? N4 Ba2 Mo1 85.87(18) 5_645 . ? N3 Ba2 Mo1 153.28(16) 4_645 . ? N2 Ba2 Mo1 111.96(17) 4_645 . ? N3 Ba2 Mo1 95.19(18) . 4_645 ? N2 Ba2 Mo1 96.24(19) 7_655 4_645 ? N4 Ba2 Mo1 157.17(17) . 4_645 ? N1 Ba2 Mo1 102.65(17) 5_645 4_645 ? N4 Ba2 Mo1 110.78(17) 5_645 4_645 ? N3 Ba2 Mo1 31.92(16) 4_645 4_645 ? N2 Ba2 Mo1 31.48(16) 4_645 4_645 ? Mo1 Ba2 Mo1 127.22(2) . 4_645 ? N3 Ba2 Mo1 119.18(17) . 5_645 ? N2 Ba2 Mo1 118.88(19) 7_655 5_645 ? N4 Ba2 Mo1 84.93(17) . 5_645 ? N1 Ba2 Mo1 31.81(17) 5_645 5_645 ? N4 Ba2 Mo1 32.10(17) 5_645 5_645 ? N3 Ba2 Mo1 102.89(16) 4_645 5_645 ? N2 Ba2 Mo1 101.18(15) 4_645 5_645 ? Mo1 Ba2 Mo1 103.48(2) . 5_645 ? Mo1 Ba2 Mo1 116.95(3) 4_645 5_645 ? N3 Ba2 Ca3 165.67(18) . 1_545 ? N2 Ba2 Ca3 64.8(2) 7_655 1_545 ? N4 Ba2 Ca3 118.72(18) . 1_545 ? N1 Ba2 Ca3 43.40(17) 5_645 1_545 ? N4 Ba2 Ca3 103.57(18) 5_645 1_545 ? N3 Ba2 Ca3 44.15(16) 4_645 1_545 ? N2 Ba2 Ca3 96.92(17) 4_645 1_545 ? Mo1 Ba2 Ca3 150.58(3) . 1_545 ? Mo1 Ba2 Ca3 75.90(3) 4_645 1_545 ? Mo1 Ba2 Ca3 75.11(3) 5_645 1_545 ? N3 Ba2 Ba3 165.67(18) . 1_545 ? N2 Ba2 Ba3 64.8(2) 7_655 1_545 ? N4 Ba2 Ba3 118.72(18) . 1_545 ? N1 Ba2 Ba3 43.40(17) 5_645 1_545 ? N4 Ba2 Ba3 103.57(18) 5_645 1_545 ? N3 Ba2 Ba3 44.15(16) 4_645 1_545 ? N2 Ba2 Ba3 96.92(17) 4_645 1_545 ? Mo1 Ba2 Ba3 150.58(3) . 1_545 ? Mo1 Ba2 Ba3 75.90(3) 4_645 1_545 ? Mo1 Ba2 Ba3 75.11(3) 5_645 1_545 ? Ca3 Ba2 Ba3 0.00(4) 1_545 1_545 ? N4 Ba3 N1 94.3(3) 7_665 5_655 ? N4 Ba3 N3 132.3(3) 7_665 4_655 ? N1 Ba3 N3 94.9(3) 5_655 4_655 ? N4 Ba3 N2 88.4(3) 7_665 . ? N1 Ba3 N2 157.6(3) 5_655 . ? N3 Ba3 N2 99.6(3) 4_655 . ? N4 Ba3 N1 118.8(3) 7_665 . ? N1 Ba3 N1 88.9(3) 5_655 . ? N3 Ba3 N1 108.0(3) 4_655 . ? N2 Ba3 N1 70.4(3) . . ? N4 Ba3 Mo1 106.8(2) 7_665 . ? N1 Ba3 Mo1 123.9(2) 5_655 . ? N3 Ba3 Mo1 106.2(2) 4_655 . ? N2 Ba3 Mo1 35.2(2) . . ? N1 Ba3 Mo1 35.28(19) . . ? N4 Ba3 Mo1 31.9(2) 7_665 7_665 ? N1 Ba3 Mo1 99.0(2) 5_655 7_665 ? N3 Ba3 Mo1 100.39(19) 4_655 7_665 ? N2 Ba3 Mo1 95.0(2) . 7_665 ? N1 Ba3 Mo1 149.69(19) . 7_665 ? Mo1 Ba3 Mo1 125.93(4) . 7_665 ? N4 Ba3 N2 61.4(3) 7_665 7_665 ? N1 Ba3 N2 87.8(3) 5_655 7_665 ? N3 Ba3 N2 72.4(2) 4_655 7_665 ? N2 Ba3 N2 112.79(19) . 7_665 ? N1 Ba3 N2 176.7(2) . 7_665 ? Mo1 Ba3 N2 147.95(16) . 7_665 ? Mo1 Ba3 N2 31.28(15) 7_665 7_665 ? N4 Ba3 Ba2 96.3(2) 7_665 1_565 ? N1 Ba3 Ba2 54.1(2) 5_655 1_565 ? N3 Ba3 Ba2 54.4(2) 4_655 1_565 ? N2 Ba3 Ba2 147.7(2) . 1_565 ? N1 Ba3 Ba2 131.67(19) . 1_565 ? Mo1 Ba3 Ba2 156.85(5) . 1_565 ? Mo1 Ba3 Ba2 74.18(3) 7_665 1_565 ? N2 Ba3 Ba2 45.80(15) 7_665 1_565 ? N4 Ba3 Ca3 113.5(2) 7_665 5_655 ? N1 Ba3 Ca3 46.1(2) 5_655 5_655 ? N3 Ba3 Ca3 106.35(19) 4_655 5_655 ? N2 Ba3 Ca3 112.8(2) . 5_655 ? N1 Ba3 Ca3 42.88(19) . 5_655 ? Mo1 Ba3 Ca3 77.95(5) . 5_655 ? Mo1 Ba3 Ca3 136.78(6) 7_665 5_655 ? N2 Ba3 Ca3 133.85(16) 7_665 5_655 ? Ba2 Ba3 Ca3 94.59(5) 1_565 5_655 ? N4 Ba3 Ba3 113.5(2) 7_665 5_655 ? N1 Ba3 Ba3 46.1(2) 5_655 5_655 ? N3 Ba3 Ba3 106.35(19) 4_655 5_655 ? N2 Ba3 Ba3 112.8(2) . 5_655 ? N1 Ba3 Ba3 42.88(19) . 5_655 ? Mo1 Ba3 Ba3 77.95(5) . 5_655 ? Mo1 Ba3 Ba3 136.78(6) 7_665 5_655 ? N2 Ba3 Ba3 133.85(16) 7_665 5_655 ? Ba2 Ba3 Ba3 94.59(5) 1_565 5_655 ? Ca3 Ba3 Ba3 0.00(4) 5_655 5_655 ? N4 Ba3 Ba2 141.5(2) 7_665 4_655 ? N1 Ba3 Ba2 123.5(2) 5_655 4_655 ? N3 Ba3 Ba2 46.2(2) 4_655 4_655 ? N2 Ba3 Ba2 59.9(2) . 4_655 ? N1 Ba3 Ba2 73.20(19) . 4_655 ? Mo1 Ba3 Ba2 60.31(3) . 4_655 ? Mo1 Ba3 Ba2 123.23(4) 7_665 4_655 ? N2 Ba3 Ba2 108.77(15) 7_665 4_655 ? Ba2 Ba3 Ba2 100.21(3) 1_565 4_655 ? Ca3 Ba3 Ba2 99.63(5) 5_655 4_655 ? Ba3 Ba3 Ba2 99.63(5) 5_655 4_655 ? N2 Mo1 N3 110.0(4) . . ? N2 Mo1 N1 106.4(4) . . ? N3 Mo1 N1 109.1(4) . . ? N2 Mo1 N4 114.2(4) . . ? N3 Mo1 N4 108.6(4) . . ? N1 Mo1 N4 108.5(4) . . ? N2 Mo1 Ba3 51.9(3) . . ? N3 Mo1 Ba3 122.6(3) . . ? N1 Mo1 Ba3 54.5(3) . . ? N4 Mo1 Ba3 128.8(3) . . ? N2 Mo1 Ba2 131.1(3) . . ? N3 Mo1 Ba2 52.0(3) . . ? N1 Mo1 Ba2 122.3(3) . . ? N4 Mo1 Ba2 56.6(3) . . ? Ba3 Mo1 Ba2 173.71(4) . . ? N2 Mo1 Ca3 75.3(3) . 7_655 ? N3 Mo1 Ca3 107.0(3) . 7_655 ? N1 Mo1 Ca3 140.4(3) . 7_655 ? N4 Mo1 Ca3 43.2(3) . 7_655 ? Ba3 Mo1 Ca3 115.57(3) . 7_655 ? Ba2 Mo1 Ca3 70.47(3) . 7_655 ? N2 Mo1 Ba3 75.3(3) . 7_655 ? N3 Mo1 Ba3 107.0(3) . 7_655 ? N1 Mo1 Ba3 140.4(3) . 7_655 ? N4 Mo1 Ba3 43.2(3) . 7_655 ? Ba3 Mo1 Ba3 115.57(3) . 7_655 ? Ba2 Mo1 Ba3 70.47(3) . 7_655 ? Ca3 Mo1 Ba3 0.00(5) 7_655 7_655 ? N2 Mo1 Ba1 135.3(3) . . ? N3 Mo1 Ba1 53.7(2) . . ? N1 Mo1 Ba1 57.4(3) . . ? N4 Mo1 Ba1 110.5(3) . . ? Ba3 Mo1 Ba1 98.44(3) . . ? Ba2 Mo1 Ba1 75.75(2) . . ? Ca3 Mo1 Ba1 145.55(4) 7_655 . ? Ba3 Mo1 Ba1 145.55(4) 7_655 . ? N2 Mo1 Ba1 81.8(3) . 3_445 ? N3 Mo1 Ba1 167.2(3) . 3_445 ? N1 Mo1 Ba1 70.8(3) . 3_445 ? N4 Mo1 Ba1 60.6(3) . 3_445 ? Ba3 Mo1 Ba1 68.36(3) . 3_445 ? Ba2 Mo1 Ba1 116.61(3) . 3_445 ? Ca3 Mo1 Ba1 70.43(3) 7_655 3_445 ? Ba3 Mo1 Ba1 70.43(3) 7_655 3_445 ? Ba1 Mo1 Ba1 121.39(2) . 3_445 ? N2 Mo1 Ba2 67.5(3) . 4_655 ? N3 Mo1 Ba2 56.8(3) . 4_655 ? N1 Mo1 Ba2 86.8(3) . 4_655 ? N4 Mo1 Ba2 162.5(3) . 4_655 ? Ba3 Mo1 Ba2 66.91(3) . 4_655 ? Ba2 Mo1 Ba2 108.33(2) . 4_655 ? Ca3 Mo1 Ba2 127.16(3) 7_655 4_655 ? Ba3 Mo1 Ba2 127.16(3) 7_655 4_655 ? Ba1 Mo1 Ba2 70.05(2) . 4_655 ? Ba1 Mo1 Ba2 135.05(3) 3_445 4_655 ? Mo1 N1 Ca3 172.3(4) . 5_655 ? Mo1 N1 Ba3 172.3(4) . 5_655 ? Ca3 N1 Ba3 0.00(8) 5_655 5_655 ? Mo1 N1 Ba3 90.2(3) . . ? Ca3 N1 Ba3 91.1(3) 5_655 . ? Ba3 N1 Ba3 91.1(3) 5_655 . ? Mo1 N1 Ba1 89.7(3) . . ? Ca3 N1 Ba1 95.1(3) 5_655 . ? Ba3 N1 Ba1 95.1(3) 5_655 . ? Ba3 N1 Ba1 132.0(3) . . ? Mo1 N1 Ba2 92.2(3) . 5_645 ? Ca3 N1 Ba2 82.5(2) 5_655 5_645 ? Ba3 N1 Ba2 82.5(2) 5_655 5_645 ? Ba3 N1 Ba2 146.0(3) . 5_645 ? Ba1 N1 Ba2 81.9(2) . 5_645 ? Mo1 N1 N2 36.8(2) . . ? Ca3 N1 N2 143.6(4) 5_655 . ? Ba3 N1 N2 143.6(4) 5_655 . ? Ba3 N1 N2 53.4(2) . . ? Ba1 N1 N2 114.2(3) . . ? Ba2 N1 N2 121.2(3) 5_645 . ? Mo1 N1 N3 35.4(2) . . ? Ca3 N1 N3 150.5(4) 5_655 . ? Ba3 N1 N3 150.5(4) 5_655 . ? Ba3 N1 N3 105.4(3) . . ? Ba1 N1 N3 55.7(2) . . ? Ba2 N1 N3 95.9(3) 5_645 . ? N2 N1 N3 60.9(3) . . ? Mo1 N1 N4 35.9(2) . . ? Ca3 N1 N4 137.0(4) 5_655 . ? Ba3 N1 N4 137.0(4) 5_655 . ? Ba3 N1 N4 109.8(3) . . ? Ba1 N1 N4 97.4(3) . . ? Ba2 N1 N4 59.0(2) 5_645 . ? N2 N1 N4 62.9(3) . . ? N3 N1 N4 60.0(3) . . ? Mo1 N1 Ba1 77.5(3) . 3_445 ? Ca3 N1 Ba1 95.3(3) 5_655 3_445 ? Ba3 N1 Ba1 95.3(3) 5_655 3_445 ? Ba3 N1 Ba1 77.0(2) . 3_445 ? Ba1 N1 Ba1 148.8(3) . 3_445 ? Ba2 N1 Ba1 70.47(18) 5_645 3_445 ? N2 N1 Ba1 71.0(2) . 3_445 ? N3 N1 Ba1 112.0(3) . 3_445 ? N4 N1 Ba1 56.3(2) . 3_445 ? Mo1 N1 N1 133.6(5) . 5_655 ? Ca3 N1 N1 47.2(2) 5_655 5_655 ? Ba3 N1 N1 47.2(2) 5_655 5_655 ? Ba3 N1 N1 43.9(2) . 5_655 ? Ba1 N1 N1 123.5(4) . 5_655 ? Ba2 N1 N1 121.2(4) 5_645 5_655 ? N2 N1 N1 96.9(4) . 5_655 ? N3 N1 N1 142.9(4) . 5_655 ? N4 N1 N1 139.1(4) . 5_655 ? Ba1 N1 N1 84.2(3) 3_445 5_655 ? Mo1 N2 Ba3 93.0(3) . . ? Mo1 N2 Ba1 104.2(4) . 6_556 ? Ba3 N2 Ba1 144.4(4) . 6_556 ? Mo1 N2 Ba2 132.7(4) . 7_665 ? Ba3 N2 Ba2 96.4(3) . 7_665 ? Ba1 N2 Ba2 94.5(3) 6_556 7_665 ? Mo1 N2 N1 36.8(2) . . ? Ba3 N2 N1 56.1(3) . . ? Ba1 N2 N1 134.5(4) 6_556 . ? Ba2 N2 N1 128.1(4) 7_665 . ? Mo1 N2 N3 35.0(2) . . ? Ba3 N2 N3 107.2(3) . . ? Ba1 N2 N3 74.3(3) 6_556 . ? Ba2 N2 N3 152.7(4) 7_665 . ? N1 N2 N3 60.4(3) . . ? Mo1 N2 N4 33.1(2) . . ? Ba3 N2 N4 109.1(3) . . ? Ba1 N2 N4 101.9(3) 6_556 . ? Ba2 N2 N4 101.0(3) 7_665 . ? N1 N2 N4 59.4(3) . . ? N3 N2 N4 58.7(3) . . ? Mo1 N2 Ba2 81.0(3) . 4_655 ? Ba3 N2 Ba2 78.2(2) . 4_655 ? Ba1 N2 Ba2 74.1(2) 6_556 4_655 ? Ba2 N2 Ba2 146.3(3) 7_665 4_655 ? N1 N2 Ba2 76.5(3) . 4_655 ? N3 N2 Ba2 55.2(2) . 4_655 ? N4 N2 Ba2 112.3(3) . 4_655 ? Mo1 N2 Ca3 73.5(3) . 7_655 ? Ba3 N2 Ca3 139.1(3) . 7_655 ? Ba1 N2 Ca3 76.3(2) 6_556 7_655 ? Ba2 N2 Ca3 69.4(2) 7_665 7_655 ? N1 N2 Ca3 101.9(3) . 7_655 ? N3 N2 Ca3 83.7(3) . 7_655 ? N4 N2 Ca3 42.9(2) . 7_655 ? Ba2 N2 Ca3 134.3(3) 4_655 7_655 ? Mo1 N2 Ba3 73.5(3) . 7_655 ? Ba3 N2 Ba3 139.1(3) . 7_655 ? Ba1 N2 Ba3 76.3(2) 6_556 7_655 ? Ba2 N2 Ba3 69.4(2) 7_665 7_655 ? N1 N2 Ba3 101.9(3) . 7_655 ? N3 N2 Ba3 83.7(3) . 7_655 ? N4 N2 Ba3 42.9(2) . 7_655 ? Ba2 N2 Ba3 134.3(3) 4_655 7_655 ? Ca3 N2 Ba3 0.00(4) 7_655 7_655 ? Mo1 N2 N4 114.6(4) . 7_665 ? Ba3 N2 N4 44.5(2) . 7_665 ? Ba1 N2 N4 140.3(3) 6_556 7_665 ? Ba2 N2 N4 52.7(2) 7_665 7_665 ? N1 N2 N4 84.6(3) . 7_665 ? N3 N2 N4 145.0(4) . 7_665 ? N4 N2 N4 105.7(3) . 7_665 ? Ba2 N2 N4 119.1(3) 4_655 7_665 ? Ca3 N2 N4 105.9(3) 7_655 7_665 ? Ba3 N2 N4 105.9(3) 7_655 7_665 ? Mo1 N3 Ca3 169.8(4) . 4_645 ? Mo1 N3 Ba3 169.8(4) . 4_645 ? Ca3 N3 Ba3 0.00(8) 4_645 4_645 ? Mo1 N3 Ba2 94.9(3) . . ? Ca3 N3 Ba2 91.2(3) 4_645 . ? Ba3 N3 Ba2 91.2(3) 4_645 . ? Mo1 N3 Ba1 93.6(3) . . ? Ca3 N3 Ba1 93.3(3) 4_645 . ? Ba3 N3 Ba1 93.3(3) 4_645 . ? Ba2 N3 Ba1 100.4(3) . . ? Mo1 N3 Ba2 91.3(3) . 4_655 ? Ca3 N3 Ba2 81.4(2) 4_645 4_655 ? Ba3 N3 Ba2 81.4(2) 4_645 4_655 ? Ba2 N3 Ba2 168.8(3) . 4_655 ? Ba1 N3 Ba2 88.5(2) . 4_655 ? Mo1 N3 N1 35.5(2) . . ? Ca3 N3 N1 147.9(4) 4_645 . ? Ba3 N3 N1 147.9(4) 4_645 . ? Ba2 N3 N1 109.2(3) . . ? Ba1 N3 N1 59.6(2) . . ? Ba2 N3 N1 81.1(3) 4_655 . ? Mo1 N3 N4 35.9(2) . . ? Ca3 N3 N4 149.0(4) 4_645 . ? Ba3 N3 N4 149.0(4) 4_645 . ? Ba2 N3 N4 59.0(2) . . ? Ba1 N3 N4 100.1(3) . . ? Ba2 N3 N4 126.4(3) 4_655 . ? N1 N3 N4 60.0(3) . . ? Mo1 N3 N2 35.0(2) . . ? Ca3 N3 N2 134.8(4) 4_645 . ? Ba3 N3 N2 134.8(4) 4_645 . ? Ba2 N3 N2 114.5(3) . . ? Ba1 N3 N2 115.8(3) . . ? Ba2 N3 N2 66.6(3) 4_655 . ? N1 N3 N2 58.7(3) . . ? N4 N3 N2 62.1(3) . . ? Mo1 N3 Ba1 79.3(3) . 6_556 ? Ca3 N3 Ba1 91.4(2) 4_645 6_556 ? Ba3 N3 Ba1 91.4(2) 4_645 6_556 ? Ba2 N3 Ba1 103.7(2) . 6_556 ? Ba1 N3 Ba1 155.4(3) . 6_556 ? Ba2 N3 Ba1 68.32(17) 4_655 6_556 ? N1 N3 Ba1 106.7(3) . 6_556 ? N4 N3 Ba1 87.9(3) . 6_556 ? N2 N3 Ba1 48.2(2) . 6_556 ? Mo1 N3 N2 114.0(4) . 6_656 ? Ca3 N3 N2 66.0(2) 4_645 6_656 ? Ba3 N3 N2 66.0(2) 4_645 6_656 ? Ba2 N3 N2 135.7(3) . 6_656 ? Ba1 N3 N2 47.68(19) . 6_656 ? Ba2 N3 N2 48.12(19) 4_655 6_656 ? N1 N3 N2 82.4(3) . 6_656 ? N4 N3 N2 141.2(4) . 6_656 ? N2 N3 N2 108.1(4) . 6_656 ? Ba1 N3 N2 113.9(3) 6_556 6_656 ? Mo1 N3 N1 127.7(4) . 8_556 ? Ca3 N3 N1 42.11(19) 4_645 8_556 ? Ba3 N3 N1 42.11(19) 4_645 8_556 ? Ba2 N3 N1 118.4(3) . 8_556 ? Ba1 N3 N1 116.0(3) . 8_556 ? Ba2 N3 N1 50.89(18) 4_655 8_556 ? N1 N3 N1 131.8(3) . 8_556 ? N4 N3 N1 142.9(3) . 8_556 ? N2 N3 N1 92.9(3) . 8_556 ? Ba1 N3 N1 55.58(18) 6_556 8_556 ? N2 N3 N1 69.9(2) 6_656 8_556 ? Mo1 N4 Ca3 104.9(4) . 7_655 ? Mo1 N4 Ba3 104.9(4) . 7_655 ? Ca3 N4 Ba3 0.00(8) 7_655 7_655 ? Mo1 N4 Ba2 89.9(3) . . ? Ca3 N4 Ba2 96.5(3) 7_655 . ? Ba3 N4 Ba2 96.5(3) 7_655 . ? Mo1 N4 Ba2 91.6(3) . 5_645 ? Ca3 N4 Ba2 159.2(3) 7_655 5_645 ? Ba3 N4 Ba2 159.2(3) 7_655 5_645 ? Ba2 N4 Ba2 96.0(3) . 5_645 ? Mo1 N4 Ba1 86.6(3) . 3_445 ? Ca3 N4 Ba1 93.0(3) 7_655 3_445 ? Ba3 N4 Ba1 93.0(3) 7_655 3_445 ? Ba2 N4 Ba1 170.4(3) . 3_445 ? Ba2 N4 Ba1 75.2(2) 5_645 3_445 ? Mo1 N4 N3 35.5(2) . . ? Ca3 N4 N3 105.1(3) 7_655 . ? Ba3 N4 N3 105.1(3) 7_655 . ? Ba2 N4 N3 54.4(2) . . ? Ba2 N4 N3 95.6(3) 5_645 . ? Ba1 N4 N3 121.8(3) 3_445 . ? Mo1 N4 N1 35.6(2) . . ? Ca3 N4 N1 132.6(4) 7_655 . ? Ba3 N4 N1 132.6(4) 7_655 . ? Ba2 N4 N1 105.3(3) . . ? Ba2 N4 N1 58.7(2) 5_645 . ? Ba1 N4 N1 67.1(2) 3_445 . ? N3 N4 N1 60.0(3) . . ? Mo1 N4 N2 32.7(2) . . ? Ca3 N4 N2 75.7(3) 7_655 . ? Ba3 N4 N2 75.7(3) 7_655 . ? Ba2 N4 N2 107.8(3) . . ? Ba2 N4 N2 115.8(3) 5_645 . ? Ba1 N4 N2 73.5(3) 3_445 . ? N3 N4 N2 59.2(3) . . ? N1 N4 N2 57.7(3) . . ? Mo1 N4 Ba1 166.4(4) . 5_645 ? Ca3 N4 Ba1 81.5(2) 7_655 5_645 ? Ba3 N4 Ba1 81.5(2) 7_655 5_645 ? Ba2 N4 Ba1 77.4(2) . 5_645 ? Ba2 N4 Ba1 85.2(2) 5_645 5_645 ? Ba1 N4 Ba1 105.2(2) 3_445 5_645 ? N3 N4 Ba1 131.6(3) . 5_645 ? N1 N4 Ba1 143.8(3) . 5_645 ? N2 N4 Ba1 157.1(3) . 5_645 ? Mo1 N4 N2 108.9(4) . 7_655 ? Ca3 N4 N2 47.1(2) 7_655 7_655 ? Ba3 N4 N2 47.1(2) 7_655 7_655 ? Ba2 N4 N2 50.4(2) . 7_655 ? Ba2 N4 N2 138.8(3) 5_645 7_655 ? Ba1 N4 N2 139.2(3) 3_445 7_655 ? N3 N4 N2 83.2(3) . 7_655 ? N1 N4 N2 142.5(3) . 7_655 ? N2 N4 N2 99.0(3) . 7_655 ? Ba1 N4 N2 66.5(2) 5_645 7_655 ? Mo1 N4 N1 107.7(4) . 3_445 ? Ca3 N4 N1 43.4(2) 7_655 3_445 ? Ba3 N4 N1 43.4(2) 7_655 3_445 ? Ba2 N4 N1 138.6(3) . 3_445 ? Ba2 N4 N1 119.8(3) 5_645 3_445 ? Ba1 N4 N1 50.90(19) 3_445 3_445 ? N3 N4 N1 132.4(3) . 3_445 ? N1 N4 N1 110.7(3) . 3_445 ? N2 N4 N1 76.3(3) . 3_445 ? Ba1 N4 N1 85.2(2) 5_645 3_445 ? N2 N4 N1 88.3(3) 7_655 3_445 ? #===END data_cabamo _database_code_CSD 197517 _chemical_name_common 'Tri (barium, calcium) tetranitridomolybdate (VI)' _audit_creation_date 2002-10-15T18:12:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; Tri (barium, calcium) tetranitridomolybdate (VI) ; _chemical_formula_moiety 'Ba6 Ca6 N16 Mo4' _chemical_formula_sum 'Ba1.52 Ca1.48 Mo N4' _chemical_formula_weight 420.06 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.271(5) _cell_length_b 9.595(5) _cell_length_c 11.721(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 1155.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4448 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 28.41 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 4.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1478 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.03 1 0 -1 0.05 -1 0 -1 0.06 0 -1 0 0.03 -1 0 1 0.05 1 0 1 0.06 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 13.613 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.208 _exptl_absorpt_correction_T_max 0.464 _exptl_absorpt_process_details 'SAINT V6.01/XPREP' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart1000 CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_unetI/netI 0.0218 _diffrn_reflns_number 8166 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.39 _diffrn_reflns_theta_max 28.73 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.939 _diffrn_measured_fraction_theta_max 0.939 _reflns_number_total 1638 _reflns_number_gt 1282 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Sir97 (Giacovazzo, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS 4.1 (Dowty, 1998)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0515P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_number_reflns 1404 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0658 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.743 _refine_diff_density_min -1.22 _refine_diff_density_rms 0.281 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ba1 Ba 0.73697(3) -0.31781(3) 0.11801(2) 0.01328(12) Uani 1 1 d . . . Ba2 Ba 0.46801(4) -0.62591(4) 0.14622(3) 0.01288(16) Uani 0.523(2) 1 d P . . Ca2 Ca 0.46801(4) -0.62591(4) 0.14622(3) 0.01288(16) Uani 0.477(2) 1 d P . . Ca3 Ca 0.37900(9) 0.03295(10) 0.10288(7) 0.01098(19) Uani 1 1 d . . . Mo1 Mo 0.40359(4) -0.29452(5) 0.11614(3) 0.01202(13) Uani 1 1 d . . . N1 N 0.5093(4) -0.1775(4) 0.0308(3) 0.0135(8) Uani 1 1 d . . . N2 N 0.2728(5) -0.1884(5) 0.1781(4) 0.0279(11) Uani 1 1 d . . . N3 N 0.5010(4) -0.3800(5) 0.2307(3) 0.0214(9) Uani 1 1 d . . . N4 N 0.3379(4) -0.4288(4) 0.0167(3) 0.0163(8) Uani 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 Ba1 0.00750(17) 0.02128(19) 0.01106(18) 0.00147(9) 0.00035(8) -0.00224(10) Ba2 0.0092(2) 0.0133(2) 0.0161(2) -0.00117(15) 0.00214(15) 0.00005(14) Ca2 0.0092(2) 0.0133(2) 0.0161(2) -0.00117(15) 0.00214(15) 0.00005(14) Ca3 0.0072(4) 0.0164(5) 0.0094(4) 0.0005(3) -0.0001(3) -0.0021(3) Mo1 0.0065(2) 0.0186(2) 0.0110(2) 0.00411(13) -0.00041(13) -0.00179(15) N1 0.0097(18) 0.020(2) 0.0108(18) 0.0020(13) 0.0008(14) -0.0040(14) N2 0.028(3) 0.027(3) 0.029(2) 0.0138(19) 0.018(2) 0.0057(18) N3 0.015(2) 0.035(3) 0.0138(18) 0.0100(17) -0.0030(16) -0.0016(18) N4 0.0134(17) 0.0162(19) 0.0192(19) 0.0047(15) -0.0010(15) -0.0026(15) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ba1 N2 2.718(5) 6_656 ? Ba1 N3 2.823(4) . ? Ba1 N1 2.885(4) . ? Ba1 N4 2.999(4) 5_645 ? Ba1 N4 3.028(4) 3_545 ? Ba1 N3 3.295(4) 6_656 ? Ba1 N1 3.297(4) 3_545 ? Ba1 Mo1 3.4091(11) 3_545 ? Ba1 Mo1 3.4316(17) . ? Ba1 N2 3.491(5) 3_545 ? Ba1 Ca2 3.5611(14) 7_765 ? Ba1 Ba2 3.5611(14) 7_765 ? Ba2 N2 2.573(5) 7_655 ? Ba2 N3 2.581(5) . ? Ba2 N4 2.769(4) . ? Ba2 N4 2.810(4) 5_645 ? Ba2 N1 2.814(4) 5_645 ? Ba2 N3 2.851(5) 4_645 ? Ba2 Mo1 3.2669(17) . ? Ba2 N2 3.418(6) 4_645 ? Ba2 Mo1 3.4320(13) 5_645 ? Ba2 Ca3 3.4362(19) 1_545 ? Ba2 Mo1 3.4807(12) 4_645 ? Ba2 Ba1 3.5611(14) 7_755 ? Ca3 N1 2.386(4) 5_655 ? Ca3 N3 2.454(4) 4_655 ? Ca3 N4 2.473(4) 7_665 ? Ca3 N2 2.545(4) . ? Ca3 N1 2.566(4) . ? Ca3 Mo1 3.1560(19) . ? Ca3 N2 3.218(5) 7_665 ? Ca3 Mo1 3.3450(16) 7_665 ? Ca3 Ca2 3.4362(19) 1_565 ? Ca3 Ba2 3.4362(19) 1_565 ? Ca3 Ca3 3.520(2) 5_655 ? Ca3 Ba1 3.6183(14) 3_445 ? Mo1 N2 1.835(5) . ? Mo1 N1 1.855(4) . ? Mo1 N4 1.864(4) . ? Mo1 N3 1.865(4) . ? Mo1 Ca3 3.3450(16) 7_655 ? Mo1 Ba1 3.4091(12) 3_445 ? Mo1 Ca2 3.4320(13) 5_645 ? Mo1 Ba2 3.4320(13) 5_645 ? N1 Ca3 2.386(4) 5_655 ? N1 Ca2 2.814(4) 5_645 ? N1 Ba2 2.814(4) 5_645 ? N1 N2 2.982(6) . ? N1 N4 2.991(6) . ? N1 N3 3.045(5) . ? N1 Ba1 3.297(4) 3_445 ? N1 N1 3.486(8) 5_655 ? N1 N3 3.561(6) 8 ? N2 Ca2 2.573(5) 7_665 ? N2 Ba2 2.573(5) 7_665 ? N2 Ba1 2.718(5) 6_556 ? N2 N3 3.042(7) . ? N2 N4 3.057(6) . ? N2 Ca3 3.218(5) 7_655 ? N2 N4 3.328(6) 7_665 ? N2 Ca2 3.418(6) 4_655 ? N2 Ba2 3.418(6) 4_655 ? N3 Ca3 2.454(4) 4_645 ? N3 Ca2 2.851(5) 4_655 ? N3 Ba2 2.851(5) 4_655 ? N3 N4 3.053(6) . ? N3 Ba1 3.295(4) 6_556 ? N3 N2 3.509(7) 6_656 ? N4 Ca3 2.473(4) 7_655 ? N4 Ca2 2.810(4) 5_645 ? N4 Ba2 2.810(4) 5_645 ? N4 Ba1 2.999(4) 5_645 ? N4 Ba1 3.028(4) 3_445 ? N4 N2 3.328(6) 7_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ba1 N3 78.56(14) 6_656 . ? N2 Ba1 N1 102.02(12) 6_656 . ? N3 Ba1 N1 64.46(11) . . ? N2 Ba1 N4 150.21(13) 6_656 5_645 ? N3 Ba1 N4 81.65(12) . 5_645 ? N1 Ba1 N4 89.09(11) . 5_645 ? N2 Ba1 N4 93.15(13) 6_656 3_545 ? N3 Ba1 N4 134.66(12) . 3_545 ? N1 Ba1 N4 74.21(11) . 3_545 ? N4 Ba1 N4 116.55(13) 5_645 3_545 ? N2 Ba1 N3 59.86(12) 6_656 6_656 ? N3 Ba1 N3 114.61(6) . 6_656 ? N1 Ba1 N3 160.43(10) . 6_656 ? N4 Ba1 N3 110.34(11) 5_645 6_656 ? N4 Ba1 N3 98.07(11) 3_545 6_656 ? N2 Ba1 N1 110.87(13) 6_656 3_545 ? N3 Ba1 N1 166.59(12) . 3_545 ? N1 Ba1 N1 120.44(4) . 3_545 ? N4 Ba1 N1 85.87(10) 5_645 3_545 ? N4 Ba1 N1 56.25(10) 3_545 3_545 ? N3 Ba1 N1 65.40(10) 6_656 3_545 ? N2 Ba1 Mo1 119.69(12) 6_656 3_545 ? N3 Ba1 Mo1 150.94(8) . 3_545 ? N1 Ba1 Mo1 88.50(8) . 3_545 ? N4 Ba1 Mo1 87.78(8) 5_645 3_545 ? N4 Ba1 Mo1 32.99(7) 3_545 3_545 ? N3 Ba1 Mo1 94.44(8) 6_656 3_545 ? N1 Ba1 Mo1 32.07(6) 3_545 3_545 ? N2 Ba1 Mo1 96.38(11) 6_656 . ? N3 Ba1 Mo1 32.89(8) . . ? N1 Ba1 Mo1 32.73(8) . . ? N4 Ba1 Mo1 78.09(8) 5_645 . ? N4 Ba1 Mo1 106.70(8) 3_545 . ? N3 Ba1 Mo1 146.78(7) 6_656 . ? N1 Ba1 Mo1 147.59(7) 3_545 . ? Mo1 Ba1 Mo1 118.371(19) 3_545 . ? N2 Ba1 N2 148.43(10) 6_656 3_545 ? N3 Ba1 N2 124.00(11) . 3_545 ? N1 Ba1 N2 74.05(11) . 3_545 ? N4 Ba1 N2 61.15(10) 5_645 3_545 ? N4 Ba1 N2 55.39(10) 3_545 3_545 ? N3 Ba1 N2 116.83(11) 6_656 3_545 ? N1 Ba1 N2 52.03(10) 3_545 3_545 ? Mo1 Ba1 N2 30.82(8) 3_545 3_545 ? Mo1 Ba1 N2 95.62(8) . 3_545 ? N2 Ba1 Ca2 64.33(11) 6_656 7_765 ? N3 Ba1 Ca2 142.76(9) . 7_765 ? N1 Ba1 Ca2 118.76(8) . 7_765 ? N4 Ba1 Ca2 133.33(8) 5_645 7_765 ? N4 Ba1 Ca2 49.68(8) 3_545 7_765 ? N3 Ba1 Ca2 48.95(8) 6_656 7_765 ? N1 Ba1 Ca2 48.26(7) 3_545 7_765 ? Mo1 Ba1 Ca2 58.95(2) 3_545 7_765 ? Mo1 Ba1 Ca2 144.69(2) . 7_765 ? N2 Ba1 Ca2 89.64(8) 3_545 7_765 ? N2 Ba1 Ba2 64.33(11) 6_656 7_765 ? N3 Ba1 Ba2 142.76(9) . 7_765 ? N1 Ba1 Ba2 118.76(8) . 7_765 ? N4 Ba1 Ba2 133.33(8) 5_645 7_765 ? N4 Ba1 Ba2 49.68(8) 3_545 7_765 ? N3 Ba1 Ba2 48.95(8) 6_656 7_765 ? N1 Ba1 Ba2 48.26(7) 3_545 7_765 ? Mo1 Ba1 Ba2 58.95(2) 3_545 7_765 ? Mo1 Ba1 Ba2 144.69(2) . 7_765 ? N2 Ba1 Ba2 89.64(8) 3_545 7_765 ? Ca2 Ba1 Ba2 0.000(14) 7_765 7_765 ? N2 Ba2 N3 106.48(15) 7_655 . ? N2 Ba2 N4 76.98(12) 7_655 . ? N3 Ba2 N4 69.47(12) . . ? N2 Ba2 N4 145.53(13) 7_655 5_645 ? N3 Ba2 N4 89.80(12) . 5_645 ? N4 Ba2 N4 80.92(13) . 5_645 ? N2 Ba2 N1 91.74(14) 7_655 5_645 ? N3 Ba2 N1 152.23(11) . 5_645 ? N4 Ba2 N1 95.37(12) . 5_645 ? N4 Ba2 N1 64.26(11) 5_645 5_645 ? N2 Ba2 N3 80.47(13) 7_655 4_645 ? N3 Ba2 N3 124.96(4) . 4_645 ? N4 Ba2 N3 156.26(12) . 4_645 ? N4 Ba2 N3 115.13(12) 5_645 4_645 ? N1 Ba2 N3 77.91(11) 5_645 4_645 ? N2 Ba2 Mo1 92.74(10) 7_655 . ? N3 Ba2 Mo1 34.74(9) . . ? N4 Ba2 Mo1 34.75(8) . . ? N4 Ba2 Mo1 83.60(8) 5_645 . ? N1 Ba2 Mo1 126.15(8) 5_645 . ? N3 Ba2 Mo1 155.44(8) 4_645 . ? N2 Ba2 N2 128.34(9) 7_655 4_645 ? N3 Ba2 N2 80.04(12) . 4_645 ? N4 Ba2 N2 145.68(11) . 4_645 ? N4 Ba2 N2 83.66(11) 5_645 4_645 ? N1 Ba2 N2 105.19(11) 5_645 4_645 ? N3 Ba2 N2 57.20(11) 4_645 4_645 ? Mo1 Ba2 N2 113.17(7) . 4_645 ? N2 Ba2 Mo1 116.60(11) 7_655 5_645 ? N3 Ba2 Mo1 119.76(9) . 5_645 ? N4 Ba2 Mo1 81.15(9) . 5_645 ? N4 Ba2 Mo1 32.87(8) 5_645 5_645 ? N1 Ba2 Mo1 32.70(8) 5_645 5_645 ? N3 Ba2 Mo1 102.74(8) 4_645 5_645 ? Mo1 Ba2 Mo1 101.40(2) . 5_645 ? N2 Ba2 Mo1 101.63(8) 4_645 5_645 ? N2 Ba2 Ca3 62.85(11) 7_655 1_545 ? N3 Ba2 Ca3 164.25(9) . 1_545 ? N4 Ba2 Ca3 116.18(9) . 1_545 ? N4 Ba2 Ca3 105.44(8) 5_645 1_545 ? N1 Ba2 Ca3 43.47(8) 5_645 1_545 ? N3 Ba2 Ca3 44.76(8) 4_645 1_545 ? Mo1 Ba2 Ca3 149.02(3) . 1_545 ? N2 Ba2 Ca3 97.42(8) 4_645 1_545 ? Mo1 Ba2 Ca3 75.99(2) 5_645 1_545 ? N2 Ba2 Mo1 98.03(10) 7_655 4_645 ? N3 Ba2 Mo1 93.91(9) . 4_645 ? N4 Ba2 Mo1 159.90(8) . 4_645 ? N4 Ba2 Mo1 111.21(9) 5_645 4_645 ? N1 Ba2 Mo1 104.30(8) 5_645 4_645 ? N3 Ba2 Mo1 32.35(8) 4_645 4_645 ? Mo1 Ba2 Mo1 127.986(18) . 4_645 ? N2 Ba2 Mo1 30.83(8) 4_645 4_645 ? Mo1 Ba2 Mo1 117.91(3) 5_645 4_645 ? Ca3 Ba2 Mo1 77.08(3) 1_545 4_645 ? N2 Ba2 Ba1 135.33(11) 7_655 7_755 ? N3 Ba2 Ba1 113.35(10) . 7_755 ? N4 Ba2 Ba1 135.47(8) . 7_755 ? N4 Ba2 Ba1 55.24(8) 5_645 7_755 ? N1 Ba2 Ba1 60.95(8) 5_645 7_755 ? N3 Ba2 Ba1 60.66(9) 4_645 7_755 ? Mo1 Ba2 Ba1 131.727(18) . 7_755 ? N2 Ba2 Ba1 45.79(7) 4_645 7_755 ? Mo1 Ba2 Ba1 58.318(15) 5_645 7_755 ? Ca3 Ba2 Ba1 73.75(3) 1_545 7_755 ? Mo1 Ba2 Ba1 60.76(2) 4_645 7_755 ? N1 Ca3 N3 94.75(15) 5_655 4_655 ? N1 Ca3 N4 94.51(14) 5_655 7_665 ? N3 Ca3 N4 136.58(14) 4_655 7_665 ? N1 Ca3 N2 156.70(15) 5_655 . ? N3 Ca3 N2 102.93(17) 4_655 . ? N4 Ca3 N2 83.08(15) 7_665 . ? N1 Ca3 N1 89.44(13) 5_655 . ? N3 Ca3 N1 105.54(14) 4_655 . ? N4 Ca3 N1 116.88(13) 7_665 . ? N2 Ca3 N1 71.40(14) . . ? N1 Ca3 Mo1 124.93(10) 5_655 . ? N3 Ca3 Mo1 105.04(11) 4_655 . ? N4 Ca3 Mo1 103.88(9) 7_665 . ? N2 Ca3 Mo1 35.55(10) . . ? N1 Ca3 Mo1 36.01(9) . . ? N1 Ca3 N2 85.99(13) 5_655 7_665 ? N3 Ca3 N2 75.09(14) 4_655 7_665 ? N4 Ca3 N2 63.40(12) 7_665 7_665 ? N2 Ca3 N2 113.00(10) . 7_665 ? N1 Ca3 N2 175.42(12) . 7_665 ? Mo1 Ca3 N2 148.47(9) . 7_665 ? N1 Ca3 Mo1 99.21(10) 5_655 7_665 ? N3 Ca3 Mo1 103.31(11) 4_655 7_665 ? N4 Ca3 Mo1 33.29(9) 7_665 7_665 ? N2 Ca3 Mo1 91.44(11) . 7_665 ? N1 Ca3 Mo1 149.03(9) . 7_665 ? Mo1 Ca3 Mo1 124.04(3) . 7_665 ? N2 Ca3 Mo1 32.40(8) 7_665 7_665 ? N1 Ca3 Ca2 54.24(9) 5_655 1_565 ? N3 Ca3 Ca2 54.88(11) 4_655 1_565 ? N4 Ca3 Ca2 99.13(9) 7_665 1_565 ? N2 Ca3 Ca2 149.06(12) . 1_565 ? N1 Ca3 Ca2 131.26(10) . 1_565 ? Mo1 Ca3 Ca2 156.89(3) . 1_565 ? N2 Ca3 Ca2 45.34(9) 7_665 1_565 ? Mo1 Ca3 Ca2 75.67(4) 7_665 1_565 ? N1 Ca3 Ba2 54.24(9) 5_655 1_565 ? N3 Ca3 Ba2 54.88(11) 4_655 1_565 ? N4 Ca3 Ba2 99.13(9) 7_665 1_565 ? N2 Ca3 Ba2 149.06(12) . 1_565 ? N1 Ca3 Ba2 131.26(10) . 1_565 ? Mo1 Ca3 Ba2 156.89(3) . 1_565 ? N2 Ca3 Ba2 45.34(9) 7_665 1_565 ? Mo1 Ca3 Ba2 75.67(4) 7_665 1_565 ? Ca2 Ca3 Ba2 0.000(14) 1_565 1_565 ? N1 Ca3 Ca3 46.78(10) 5_655 5_655 ? N3 Ca3 Ca3 104.56(11) 4_655 5_655 ? N4 Ca3 Ca3 112.50(10) 7_665 5_655 ? N2 Ca3 Ca3 112.95(11) . 5_655 ? N1 Ca3 Ca3 42.66(9) . 5_655 ? Mo1 Ca3 Ca3 78.37(3) . 5_655 ? N2 Ca3 Ca3 132.77(10) 7_665 5_655 ? Mo1 Ca3 Ca3 137.17(4) 7_665 5_655 ? Ca2 Ca3 Ca3 94.85(4) 1_565 5_655 ? Ba2 Ca3 Ca3 94.85(4) 1_565 5_655 ? N1 Ca3 Ba1 93.19(10) 5_655 3_445 ? N3 Ca3 Ba1 164.90(11) 4_655 3_445 ? N4 Ca3 Ba1 55.20(9) 7_665 3_445 ? N2 Ca3 Ba1 66.36(13) . 3_445 ? N1 Ca3 Ba1 61.68(9) . 3_445 ? Mo1 Ca3 Ba1 59.97(3) . 3_445 ? N2 Ca3 Ba1 118.33(9) 7_665 3_445 ? Mo1 Ca3 Ba1 88.04(3) 7_665 3_445 ? Ca2 Ca3 Ba1 139.15(3) 1_565 3_445 ? Ba2 Ca3 Ba1 139.15(3) 1_565 3_445 ? Ca3 Ca3 Ba1 72.06(4) 5_655 3_445 ? N2 Mo1 N1 107.82(18) . . ? N2 Mo1 N4 111.5(2) . . ? N1 Mo1 N4 107.04(17) . . ? N2 Mo1 N3 110.6(2) . . ? N1 Mo1 N3 109.89(18) . . ? N4 Mo1 N3 109.91(18) . . ? N2 Mo1 Ca3 53.74(14) . . ? N1 Mo1 Ca3 54.38(12) . . ? N4 Mo1 Ca3 128.94(12) . . ? N3 Mo1 Ca3 121.08(14) . . ? N2 Mo1 Ba2 130.21(13) . . ? N1 Mo1 Ba2 121.93(13) . . ? N4 Mo1 Ba2 57.86(12) . . ? N3 Mo1 Ba2 52.08(14) . . ? Ca3 Mo1 Ba2 172.11(2) . . ? N2 Mo1 Ca3 70.00(16) . 7_655 ? N1 Mo1 Ca3 141.48(12) . 7_655 ? N4 Mo1 Ca3 46.74(12) . 7_655 ? N3 Mo1 Ca3 106.36(14) . 7_655 ? Ca3 Mo1 Ca3 114.90(3) . 7_655 ? Ba2 Mo1 Ca3 72.49(3) . 7_655 ? N2 Mo1 Ba1 77.05(16) . 3_445 ? N1 Mo1 Ba1 70.63(12) . 3_445 ? N4 Mo1 Ba1 62.18(12) . 3_445 ? N3 Mo1 Ba1 171.16(14) . 3_445 ? Ca3 Mo1 Ba1 66.76(2) . 3_445 ? Ba2 Mo1 Ba1 119.752(17) . 3_445 ? Ca3 Mo1 Ba1 71.55(3) 7_655 3_445 ? N2 Mo1 Ba1 139.80(17) . . ? N1 Mo1 Ba1 57.23(12) . . ? N4 Mo1 Ba1 108.67(12) . . ? N3 Mo1 Ba1 55.32(13) . . ? Ca3 Mo1 Ba1 98.34(2) . . ? Ba2 Mo1 Ba1 74.562(14) . . ? Ca3 Mo1 Ba1 146.50(3) 7_655 . ? Ba1 Mo1 Ba1 121.777(19) 3_445 . ? N2 Mo1 Ca2 139.40(16) . 5_645 ? N1 Mo1 Ca2 55.00(12) . 5_645 ? N4 Mo1 Ca2 54.90(12) . 5_645 ? N3 Mo1 Ca2 109.93(14) . 5_645 ? Ca3 Mo1 Ca2 102.01(2) . 5_645 ? Ba2 Mo1 Ca2 78.60(2) . 5_645 ? Ca3 Mo1 Ca2 100.47(3) 7_655 5_645 ? Ba1 Mo1 Ca2 62.74(3) 3_445 5_645 ? Ba1 Mo1 Ca2 66.906(18) . 5_645 ? N2 Mo1 Ba2 139.40(16) . 5_645 ? N1 Mo1 Ba2 55.00(12) . 5_645 ? N4 Mo1 Ba2 54.90(12) . 5_645 ? N3 Mo1 Ba2 109.93(14) . 5_645 ? Ca3 Mo1 Ba2 102.01(2) . 5_645 ? Ba2 Mo1 Ba2 78.60(2) . 5_645 ? Ca3 Mo1 Ba2 100.47(3) 7_655 5_645 ? Ba1 Mo1 Ba2 62.74(3) 3_445 5_645 ? Ba1 Mo1 Ba2 66.906(18) . 5_645 ? Ca2 Mo1 Ba2 0.000(12) 5_645 5_645 ? Mo1 N1 Ca3 170.9(2) . 5_655 ? Mo1 N1 Ca3 89.61(15) . . ? Ca3 N1 Ca3 90.56(13) 5_655 . ? Mo1 N1 Ca2 92.30(15) . 5_645 ? Ca3 N1 Ca2 82.29(12) 5_655 5_645 ? Ca3 N1 Ca2 144.46(16) . 5_645 ? Mo1 N1 Ba2 92.30(15) . 5_645 ? Ca3 N1 Ba2 82.29(12) 5_655 5_645 ? Ca3 N1 Ba2 144.46(16) . 5_645 ? Ca2 N1 Ba2 0.000(19) 5_645 5_645 ? Mo1 N1 Ba1 90.04(14) . . ? Ca3 N1 Ba1 96.57(14) 5_655 . ? Ca3 N1 Ba1 132.32(15) . . ? Ca2 N1 Ba1 83.18(11) 5_645 . ? Ba2 N1 Ba1 83.18(11) 5_645 . ? Mo1 N1 N2 35.86(11) . . ? Ca3 N1 N2 142.40(18) 5_655 . ? Ca3 N1 N2 53.98(12) . . ? Ca2 N1 N2 118.08(16) 5_645 . ? Ba2 N1 N2 118.08(16) 5_645 . ? Ba1 N1 N2 116.00(16) . . ? Mo1 N1 N4 36.58(10) . . ? Ca3 N1 N4 135.69(17) 5_655 . ? Ca3 N1 N4 110.21(16) . . ? Ca2 N1 N4 57.81(11) 5_645 . ? Ba2 N1 N4 57.81(11) 5_645 . ? Ba1 N1 N4 96.91(14) . . ? N2 N1 N4 61.58(14) . . ? Mo1 N1 N3 35.15(11) . . ? Ca3 N1 N3 152.81(18) 5_655 . ? Ca3 N1 N3 103.54(15) . . ? Ca2 N1 N3 98.14(15) 5_645 . ? Ba2 N1 N3 98.14(15) 5_645 . ? Ba1 N1 N3 56.78(11) . . ? N2 N1 N3 60.61(14) . . ? N4 N1 N3 60.75(13) . . ? Mo1 N1 Ba1 77.30(13) . 3_445 ? Ca3 N1 Ba1 93.94(12) 5_655 3_445 ? Ca3 N1 Ba1 75.07(10) . 3_445 ? Ca2 N1 Ba1 70.79(8) 5_645 3_445 ? Ba2 N1 Ba1 70.79(8) 5_645 3_445 ? Ba1 N1 Ba1 150.30(14) . 3_445 ? N2 N1 Ba1 67.34(14) . 3_445 ? N4 N1 Ba1 57.32(10) . 3_445 ? N3 N1 Ba1 111.99(14) . 3_445 ? Mo1 N1 N1 132.1(2) . 5_655 ? Ca3 N1 N1 47.38(9) 5_655 5_655 ? Ca3 N1 N1 43.18(9) . 5_655 ? Ca2 N1 N1 120.47(17) 5_645 5_655 ? Ba2 N1 N1 120.47(17) 5_645 5_655 ? Ba1 N1 N1 125.01(18) . 5_655 ? N2 N1 N1 96.28(18) . 5_655 ? N4 N1 N1 138.1(2) . 5_655 ? N3 N1 N1 141.3(2) . 5_655 ? Ba1 N1 N1 81.80(14) 3_445 5_655 ? Mo1 N1 N3 127.76(17) . 8 ? Ca3 N1 N3 43.37(10) 5_655 8 ? Ca3 N1 N3 101.02(14) . 8 ? Ca2 N1 N3 51.51(9) 5_645 8 ? Ba2 N1 N3 51.51(9) 5_645 8 ? Ba1 N1 N3 116.21(13) . 8 ? N2 N1 N3 123.91(17) . 8 ? N4 N1 N3 93.22(14) . 8 ? N3 N1 N3 149.10(14) . 8 ? Ba1 N1 N3 57.28(9) 3_445 8 ? N1 N1 N3 69.10(14) 5_655 8 ? Mo1 N2 Ca3 90.71(17) . . ? Mo1 N2 Ca2 140.8(3) . 7_665 ? Ca3 N2 Ca2 99.62(16) . 7_665 ? Mo1 N2 Ba2 140.8(3) . 7_665 ? Ca3 N2 Ba2 99.62(16) . 7_665 ? Ca2 N2 Ba2 0.000(18) 7_665 7_665 ? Mo1 N2 Ba1 101.17(19) . 6_556 ? Ca3 N2 Ba1 138.1(2) . 6_556 ? Ca2 N2 Ba1 95.96(14) 7_665 6_556 ? Ba2 N2 Ba1 95.96(14) 7_665 6_556 ? Mo1 N2 N1 36.32(11) . . ? Ca3 N2 N1 54.62(12) . . ? Ca2 N2 N1 133.7(2) 7_665 . ? Ba2 N2 N1 133.7(2) 7_665 . ? Ba1 N2 N1 129.47(19) 6_556 . ? Mo1 N2 N3 35.01(12) . . ? Ca3 N2 N3 104.14(19) . . ? Ca2 N2 N3 155.7(2) 7_665 . ? Ba2 N2 N3 155.7(2) 7_665 . ? Ba1 N2 N3 69.53(13) 6_556 . ? N1 N2 N3 60.72(14) . . ? Mo1 N2 N4 34.57(13) . . ? Ca3 N2 N4 108.76(17) . . ? Ca2 N2 N4 107.2(2) 7_665 . ? Ba2 N2 N4 107.2(2) 7_665 . ? Ba1 N2 N4 103.24(15) 6_556 . ? N1 N2 N4 59.35(14) . . ? N3 N2 N4 60.07(14) . . ? Mo1 N2 Ca3 77.60(16) . 7_655 ? Ca3 N2 Ca3 143.7(2) . 7_655 ? Ca2 N2 Ca3 71.81(13) 7_665 7_655 ? Ba2 N2 Ca3 71.81(13) 7_665 7_655 ? Ba1 N2 Ca3 78.21(11) 6_556 7_655 ? N1 N2 Ca3 105.39(16) . 7_655 ? N3 N2 Ca3 85.81(15) . 7_655 ? N4 N2 Ca3 46.34(10) . 7_655 ? Mo1 N2 N4 116.1(2) . 7_665 ? Ca3 N2 N4 47.54(10) . 7_665 ? Ca2 N2 N4 54.16(11) 7_665 7_665 ? Ba2 N2 N4 54.16(11) 7_665 7_665 ? Ba1 N2 N4 142.69(17) 6_556 7_665 ? N1 N2 N4 85.57(15) . 7_665 ? N3 N2 N4 146.17(18) . 7_665 ? N4 N2 N4 106.71(18) . 7_665 ? Ca3 N2 N4 107.48(17) 7_655 7_665 ? Mo1 N2 Ca2 76.46(17) . 4_655 ? Ca3 N2 Ca2 74.26(13) . 4_655 ? Ca2 N2 Ca2 142.69(18) 7_665 4_655 ? Ba2 N2 Ca2 142.69(18) 7_665 4_655 ? Ba1 N2 Ca2 69.88(12) 6_556 4_655 ? N1 N2 Ca2 73.05(14) . 4_655 ? N3 N2 Ca2 51.97(12) . 4_655 ? N4 N2 Ca2 109.57(16) . 4_655 ? Ca3 N2 Ca2 133.48(14) 7_655 4_655 ? N4 N2 Ca2 118.51(15) 7_665 4_655 ? Mo1 N2 Ba2 76.46(17) . 4_655 ? Ca3 N2 Ba2 74.26(13) . 4_655 ? Ca2 N2 Ba2 142.69(18) 7_665 4_655 ? Ba2 N2 Ba2 142.69(18) 7_665 4_655 ? Ba1 N2 Ba2 69.88(12) 6_556 4_655 ? N1 N2 Ba2 73.05(14) . 4_655 ? N3 N2 Ba2 51.97(12) . 4_655 ? N4 N2 Ba2 109.57(16) . 4_655 ? Ca3 N2 Ba2 133.48(14) 7_655 4_655 ? N4 N2 Ba2 118.51(15) 7_665 4_655 ? Ca2 N2 Ba2 0.000(14) 4_655 4_655 ? Mo1 N3 Ca3 172.6(2) . 4_645 ? Mo1 N3 Ba2 93.18(17) . . ? Ca3 N3 Ba2 93.42(15) 4_645 . ? Mo1 N3 Ba1 91.78(15) . . ? Ca3 N3 Ba1 90.74(14) 4_645 . ? Ba2 N3 Ba1 97.28(14) . . ? Mo1 N3 Ca2 92.76(18) . 4_655 ? Ca3 N3 Ca2 80.37(12) 4_645 4_655 ? Ba2 N3 Ca2 172.11(16) . 4_655 ? Ba1 N3 Ca2 87.73(12) . 4_655 ? Mo1 N3 Ba2 92.76(18) . 4_655 ? Ca3 N3 Ba2 80.37(12) 4_645 4_655 ? Ba2 N3 Ba2 172.11(16) . 4_655 ? Ba1 N3 Ba2 87.73(12) . 4_655 ? Ca2 N3 Ba2 0.000(14) 4_655 4_655 ? Mo1 N3 N2 34.38(12) . . ? Ca3 N3 N2 138.9(2) 4_645 . ? Ba2 N3 N2 111.93(18) . . ? Ba1 N3 N2 116.04(16) . . ? Ca2 N3 N2 70.83(15) 4_655 . ? Ba2 N3 N2 70.83(15) 4_655 . ? Mo1 N3 N1 34.96(11) . . ? Ca3 N3 N1 144.58(19) 4_645 . ? Ba2 N3 N1 106.98(15) . . ? Ba1 N3 N1 58.76(11) . . ? Ca2 N3 N1 80.83(14) 4_655 . ? Ba2 N3 N1 80.83(14) 4_655 . ? N2 N3 N1 58.67(13) . . ? Mo1 N3 N4 35.04(11) . . ? Ca3 N3 N4 151.2(2) 4_645 . ? Ba2 N3 N4 58.16(11) . . ? Ba1 N3 N4 96.85(14) . . ? Ca2 N3 N4 127.47(17) 4_655 . ? Ba2 N3 N4 127.47(17) 4_655 . ? N2 N3 N4 60.22(15) . . ? N1 N3 N4 58.74(12) . . ? Mo1 N3 Ba1 82.30(15) . 6_556 ? Ca3 N3 Ba1 92.69(12) 4_645 6_556 ? Ba2 N3 Ba1 105.29(14) . 6_556 ? Ba1 N3 Ba1 156.92(17) . 6_556 ? Ca2 N3 Ba1 70.39(10) 4_655 6_556 ? Ba2 N3 Ba1 70.39(10) 4_655 6_556 ? N2 N3 Ba1 50.61(11) . 6_556 ? N1 N3 Ba1 108.76(15) . 6_556 ? N4 N3 Ba1 91.04(14) . 6_556 ? Mo1 N3 N2 114.6(2) . 6_656 ? Ca3 N3 N2 62.40(12) 4_645 6_656 ? Ba2 N3 N2 134.45(18) . 6_656 ? Ba1 N3 N2 49.39(11) . 6_656 ? Ca2 N3 N2 46.30(10) 4_655 6_656 ? Ba2 N3 N2 46.30(10) 4_655 6_656 ? N2 N3 N2 111.0(2) . 6_656 ? N1 N3 N2 82.99(15) . 6_656 ? N4 N3 N2 140.12(18) . 6_656 ? Ba1 N3 N2 113.32(15) 6_556 6_656 ? Mo1 N4 Ca3 99.97(17) . 7_655 ? Mo1 N4 Ba2 87.39(14) . . ? Ca3 N4 Ba2 96.28(13) 7_655 . ? Mo1 N4 Ca2 92.23(15) . 5_645 ? Ca3 N4 Ca2 160.78(16) 7_655 5_645 ? Ba2 N4 Ca2 99.08(13) . 5_645 ? Mo1 N4 Ba2 92.23(15) . 5_645 ? Ca3 N4 Ba2 160.78(16) 7_655 5_645 ? Ba2 N4 Ba2 99.08(13) . 5_645 ? Ca2 N4 Ba2 0.00(2) 5_645 5_645 ? Mo1 N4 N1 36.38(10) . . ? Ca3 N4 N1 128.86(17) 7_655 . ? Ba2 N4 N1 103.67(15) . . ? Ca2 N4 N1 57.93(10) 5_645 . ? Ba2 N4 N1 57.93(10) 5_645 . ? Mo1 N4 Ba1 169.23(19) . 5_645 ? Ca3 N4 Ba1 82.17(11) 7_655 5_645 ? Ba2 N4 Ba1 81.88(10) . 5_645 ? Ca2 N4 Ba1 88.61(11) 5_645 5_645 ? Ba2 N4 Ba1 88.61(11) 5_645 5_645 ? N1 N4 Ba1 146.48(16) . 5_645 ? Mo1 N4 Ba1 84.82(13) . 3_445 ? Ca3 N4 Ba1 91.18(12) 7_655 3_445 ? Ba2 N4 Ba1 170.04(15) . 3_445 ? Ca2 N4 Ba1 75.08(9) 5_645 3_445 ? Ba2 N4 Ba1 75.08(9) 5_645 3_445 ? N1 N4 Ba1 66.43(11) . 3_445 ? Ba1 N4 Ba1 105.74(12) 5_645 3_445 ? Mo1 N4 N3 35.05(11) . . ? Ca3 N4 N3 100.46(15) 7_655 . ? Ba2 N4 N3 52.36(11) . . ? Ca2 N4 N3 98.06(15) 5_645 . ? Ba2 N4 N3 98.06(15) 5_645 . ? N1 N4 N3 60.51(13) . . ? Ba1 N4 N3 134.24(16) 5_645 . ? Ba1 N4 N3 119.76(16) 3_445 . ? Mo1 N4 N2 33.95(12) . . ? Ca3 N4 N2 70.27(13) 7_655 . ? Ba2 N4 N2 106.35(15) . . ? Ca2 N4 N2 115.76(15) 5_645 . ? Ba2 N4 N2 115.76(15) 5_645 . ? N1 N4 N2 59.08(13) . . ? Ba1 N4 N2 151.81(17) 5_645 . ? Ba1 N4 N2 70.01(12) 3_445 . ? N3 N4 N2 59.72(15) . . ? Mo1 N4 N2 106.59(17) . 7_655 ? Ca3 N4 N2 49.38(11) 7_655 7_655 ? Ba2 N4 N2 48.86(10) . 7_655 ? Ca2 N4 N2 140.22(16) 5_645 7_655 ? Ba2 N4 N2 140.22(16) 5_645 7_655 ? N1 N4 N2 140.65(16) . 7_655 ? Ba1 N4 N2 66.73(12) 5_645 7_655 ? Ba1 N4 N2 139.85(16) 3_445 7_655 ? N3 N4 N2 80.53(14) . 7_655 ? N2 N4 N2 97.94(16) . 7_655 ? #===END data_cabawn _database_code_CSD 197518 _audit_creation_date 2002-10-25T09:52:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'Ba6 Ca6 N16 W4' _chemical_formula_sum 'Ba1.44 Ca1.56 N4 W' _chemical_formula_weight 499.94 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3049(10) _cell_length_b 9.5822(9) _cell_length_c 11.7405(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1159.30(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1401 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 28.56 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description irregular _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 5.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1710 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 30.754 _exptl_absorpt_correction_type Multiscan _exptl_absorpt_process_details 'SAINT V6.01/SADABS' _exptl_absorpt_correction_T_min 0.149 _exptl_absorpt_correction_T_max 0.296 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_unetI/netI 0.044 _diffrn_reflns_number 4876 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 28.69 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.906 _diffrn_measured_fraction_theta_max 0.906 _reflns_number_total 1564 _reflns_number_gt 1058 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ATOMS 4.1 (Dowty, 1998)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_number_reflns 1352 _refine_ls_number_parameters 74 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0788 _refine_ls_goodness_of_fit_ref 0.94 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.19 _refine_diff_density_min -3.204 _refine_diff_density_rms 0.47 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.849 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ba1 Ba 0.73701(6) -0.31931(6) 0.11841(5) 0.01155(18) Uani 1 1 d . . . Ba2 Ba 0.46756(10) -0.62687(11) 0.14617(10) 0.0122(4) Uani 0.436(5) 1 d P . . Ca2 Ca 0.46756(10) -0.62687(11) 0.14617(10) 0.0122(4) Uani 0.564(5) 1 d P . . Ca3 Ca 0.37894(19) 0.0332(2) 0.10269(18) 0.0097(4) Uani 1 1 d . . . W1 W 0.40337(4) -0.29611(4) 0.11535(4) 0.00986(15) Uani 1 1 d . . . N1 N 0.5095(8) -0.1776(8) 0.0293(7) 0.0089(18) Uani 1 1 d U . . N2 N 0.2702(10) -0.1899(9) 0.1766(9) 0.022(2) Uani 1 1 d U . . N3 N 0.4996(9) -0.3820(10) 0.2305(9) 0.020(2) Uani 1 1 d U . . N4 N 0.3379(8) -0.4318(9) 0.0153(8) 0.0138(19) Uani 1 1 d U . . 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 Ba1 0.0077(3) 0.0195(3) 0.0075(4) 0.0012(3) 0.0001(2) -0.0020(2) Ba2 0.0106(6) 0.0111(6) 0.0151(7) -0.0011(4) 0.0030(4) -0.0001(4) Ca2 0.0106(6) 0.0111(6) 0.0151(7) -0.0011(4) 0.0030(4) -0.0001(4) Ca3 0.0076(9) 0.0145(10) 0.0069(12) -0.0004(8) -0.0001(7) -0.0028(8) W1 0.0063(2) 0.0157(2) 0.0076(3) 0.00371(17) -0.00038(15) -0.00185(15) N1 0.009(2) 0.010(2) 0.008(2) -0.0001(18) 0.0016(18) -0.0010(17) N2 0.022(3) 0.022(3) 0.022(3) 0.0027(19) 0.0027(19) 0.0011(18) N3 0.018(3) 0.021(3) 0.020(3) 0.0025(19) 0.0005(18) -0.0004(18) N4 0.014(2) 0.014(2) 0.014(3) -0.0006(18) -0.0017(18) -0.0005(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ba1 N2 2.729(10) 6_656 ? Ba1 N3 2.842(10) . ? Ba1 N1 2.904(9) . ? Ba1 N4 2.957(9) 5_645 ? Ba1 N4 3.055(9) 3_545 ? Ba1 N3 3.291(10) 6_656 ? Ba1 N1 3.301(9) 3_545 ? Ba1 W1 3.4196(8) 3_545 ? Ba1 W1 3.4456(8) . ? Ba1 N2 3.482(10) 3_545 ? Ba1 W1 3.5719(8) 6_656 ? Ba1 Ca2 3.5741(12) 7_765 ? Ba2 N2 2.549(10) 7_655 ? Ba2 N3 2.568(10) . ? Ba2 N4 2.764(9) . ? Ba2 N1 2.795(8) 5_645 ? Ba2 N4 2.815(9) 5_645 ? Ba2 N3 2.861(10) 4_645 ? Ba2 W1 3.2579(11) . ? Ba2 Ca3 3.421(2) 1_545 ? Ba2 W1 3.4266(12) 5_645 ? Ba2 N2 3.463(10) 4_645 ? Ba2 W1 3.4983(12) 4_645 ? Ba2 Ba1 3.5741(13) 7_755 ? Ca3 N1 2.374(9) 5_655 ? Ca3 N3 2.462(10) 4_655 ? Ca3 N4 2.482(9) 7_665 ? Ca3 N2 2.565(10) . ? Ca3 N1 2.576(9) . ? Ca3 W1 3.169(2) . ? Ca3 N2 3.186(10) 7_665 ? Ca3 W1 3.341(2) 7_665 ? Ca3 Ca2 3.421(2) 1_565 ? Ca3 Ba2 3.421(2) 1_565 ? Ca3 Ca3 3.528(4) 5_655 ? Ca3 Ba1 3.617(2) 3_445 ? W1 N2 1.853(10) . ? W1 N3 1.867(10) . ? W1 N1 1.873(8) . ? W1 N4 1.878(9) . ? W1 Ca3 3.341(2) 7_655 ? W1 Ba1 3.4196(8) 3_445 ? W1 Ca2 3.4266(12) 5_645 ? W1 Ba2 3.4266(12) 5_645 ? N1 Ca3 2.374(9) 5_655 ? N1 Ca2 2.795(8) 5_645 ? N1 Ba2 2.795(8) 5_645 ? N1 N2 3.014(13) . ? N1 N4 3.015(12) . ? N1 N3 3.070(14) . ? N1 Ba1 3.301(9) 3_445 ? N1 N1 3.477(16) 5_655 ? N1 N3 3.556(14) 8 ? N2 Ca2 2.549(10) 7_665 ? N2 Ba2 2.549(10) 7_665 ? N2 Ba1 2.729(10) 6_556 ? N2 N3 3.061(14) . ? N2 N4 3.074(13) . ? N2 Ca3 3.186(10) 7_655 ? N2 N4 3.309(13) 7_665 ? N2 Ca2 3.463(10) 4_655 ? N2 Ba2 3.463(10) 4_655 ? N3 Ca3 2.462(10) 4_645 ? N3 Ca2 2.861(10) 4_655 ? N3 Ba2 2.861(10) 4_655 ? N3 N4 3.064(13) . ? N3 Ba1 3.291(10) 6_556 ? N3 N2 3.515(14) 6_656 ? N4 Ca3 2.482(9) 7_655 ? N4 Ca2 2.815(9) 5_645 ? N4 Ba2 2.815(9) 5_645 ? N4 Ba1 2.957(9) 5_645 ? N4 Ba1 3.055(9) 3_445 ? N4 N2 3.309(13) 7_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ba1 N3 78.2(3) 6_656 . ? N2 Ba1 N1 101.9(3) 6_656 . ? N3 Ba1 N1 64.6(3) . . ? N2 Ba1 N4 150.1(3) 6_656 5_645 ? N3 Ba1 N4 81.4(3) . 5_645 ? N1 Ba1 N4 88.6(2) . 5_645 ? N2 Ba1 N4 93.0(3) 6_656 3_545 ? N3 Ba1 N4 134.2(2) . 3_545 ? N1 Ba1 N4 73.8(2) . 3_545 ? N4 Ba1 N4 116.8(3) 5_645 3_545 ? N2 Ba1 N3 60.3(3) 6_656 6_656 ? N3 Ba1 N3 114.81(12) . 6_656 ? N1 Ba1 N3 160.6(2) . 6_656 ? N4 Ba1 N3 110.7(2) 5_645 6_656 ? N4 Ba1 N3 98.1(2) 3_545 6_656 ? N2 Ba1 N1 111.1(3) 6_656 3_545 ? N3 Ba1 N1 166.8(2) . 3_545 ? N1 Ba1 N1 120.11(5) . 3_545 ? N4 Ba1 N1 86.3(2) 5_645 3_545 ? N4 Ba1 N1 56.5(2) 3_545 3_545 ? N3 Ba1 N1 65.3(2) 6_656 3_545 ? N2 Ba1 W1 119.9(2) 6_656 3_545 ? N3 Ba1 W1 150.6(2) . 3_545 ? N1 Ba1 W1 87.95(17) . 3_545 ? N4 Ba1 W1 88.04(17) 5_645 3_545 ? N4 Ba1 W1 33.11(16) 3_545 3_545 ? N3 Ba1 W1 94.56(17) 6_656 3_545 ? N1 Ba1 W1 32.31(15) 3_545 3_545 ? N2 Ba1 W1 96.0(2) 6_656 . ? N3 Ba1 W1 32.8(2) . . ? N1 Ba1 W1 32.93(17) . . ? N4 Ba1 W1 77.64(16) 5_645 . ? N4 Ba1 W1 106.47(16) 3_545 . ? N3 Ba1 W1 146.91(18) 6_656 . ? N1 Ba1 W1 147.58(15) 3_545 . ? W1 Ba1 W1 118.100(19) 3_545 . ? N2 Ba1 N2 148.60(18) 6_656 3_545 ? N3 Ba1 N2 123.4(3) . 3_545 ? N1 Ba1 N2 73.1(2) . 3_545 ? N4 Ba1 N2 61.2(2) 5_645 3_545 ? N4 Ba1 N2 55.6(2) 3_545 3_545 ? N3 Ba1 N2 117.4(2) 6_656 3_545 ? N1 Ba1 N2 52.7(2) 3_545 3_545 ? W1 Ba1 N2 31.14(16) 3_545 3_545 ? W1 Ba1 N2 94.94(17) . 3_545 ? N2 Ba1 W1 30.7(2) 6_656 6_656 ? N3 Ba1 W1 91.2(2) . 6_656 ? N1 Ba1 W1 132.34(17) . 6_656 ? N4 Ba1 W1 129.78(17) 5_645 6_656 ? N4 Ba1 W1 103.72(17) 3_545 6_656 ? N3 Ba1 W1 31.23(17) 6_656 6_656 ? N1 Ba1 W1 92.98(15) 3_545 6_656 ? W1 Ba1 W1 116.21(2) 3_545 6_656 ? W1 Ba1 W1 118.946(19) . 6_656 ? N2 Ba1 W1 145.27(17) 3_545 6_656 ? N2 Ba1 Ca2 65.1(2) 6_656 7_765 ? N3 Ba1 Ca2 143.1(2) . 7_765 ? N1 Ba1 Ca2 118.62(16) . 7_765 ? N4 Ba1 Ca2 133.38(17) 5_645 7_765 ? N4 Ba1 Ca2 49.51(16) 3_545 7_765 ? N3 Ba1 Ca2 49.05(17) 6_656 7_765 ? N1 Ba1 Ca2 47.77(15) 3_545 7_765 ? W1 Ba1 Ca2 58.62(2) 3_545 7_765 ? W1 Ba1 Ca2 144.85(3) . 7_765 ? N2 Ba1 Ca2 89.65(16) 3_545 7_765 ? W1 Ba1 Ca2 58.62(2) 6_656 7_765 ? N2 Ba2 N3 106.6(3) 7_655 . ? N2 Ba2 N4 76.9(3) 7_655 . ? N3 Ba2 N4 70.0(3) . . ? N2 Ba2 N1 91.5(3) 7_655 5_645 ? N3 Ba2 N1 152.4(3) . 5_645 ? N4 Ba2 N1 94.8(3) . 5_645 ? N2 Ba2 N4 145.7(3) 7_655 5_645 ? N3 Ba2 N4 89.2(3) . 5_645 ? N4 Ba2 N4 80.5(3) . 5_645 ? N1 Ba2 N4 65.0(3) 5_645 5_645 ? N2 Ba2 N3 80.8(3) 7_655 4_645 ? N3 Ba2 N3 124.78(6) . 4_645 ? N4 Ba2 N3 156.4(3) . 4_645 ? N1 Ba2 N3 77.9(3) 5_645 4_645 ? N4 Ba2 N3 115.3(3) 5_645 4_645 ? N2 Ba2 W1 92.9(2) 7_655 . ? N3 Ba2 W1 34.9(2) . . ? N4 Ba2 W1 35.14(18) . . ? N1 Ba2 W1 125.99(18) 5_645 . ? N4 Ba2 W1 82.85(18) 5_645 . ? N3 Ba2 W1 155.7(2) 4_645 . ? N2 Ba2 Ca3 62.5(2) 7_655 1_545 ? N3 Ba2 Ca3 164.1(2) . 1_545 ? N4 Ba2 Ca3 115.58(18) . 1_545 ? N1 Ba2 Ca3 43.46(18) 5_645 1_545 ? N4 Ba2 Ca3 106.25(18) 5_645 1_545 ? N3 Ba2 Ca3 45.1(2) 4_645 1_545 ? W1 Ba2 Ca3 148.81(5) . 1_545 ? N2 Ba2 W1 116.6(2) 7_655 5_645 ? N3 Ba2 W1 119.5(2) . 5_645 ? N4 Ba2 W1 80.50(19) . 5_645 ? N1 Ba2 W1 33.11(17) 5_645 5_645 ? N4 Ba2 W1 33.22(18) 5_645 5_645 ? N3 Ba2 W1 102.9(2) 4_645 5_645 ? W1 Ba2 W1 100.88(3) . 5_645 ? Ca3 Ba2 W1 76.40(4) 1_545 5_645 ? N2 Ba2 N2 128.64(18) 7_655 4_645 ? N3 Ba2 N2 80.1(3) . 4_645 ? N4 Ba2 N2 146.0(2) . 4_645 ? N1 Ba2 N2 105.1(2) 5_645 4_645 ? N4 Ba2 N2 83.3(2) 5_645 4_645 ? N3 Ba2 N2 56.9(3) 4_645 4_645 ? W1 Ba2 N2 113.26(15) . 4_645 ? Ca3 Ba2 N2 97.57(16) 1_545 4_645 ? W1 Ba2 N2 101.42(17) 5_645 4_645 ? N2 Ba2 W1 98.2(2) 7_655 4_645 ? N3 Ba2 W1 93.8(2) . 4_645 ? N4 Ba2 W1 160.43(19) . 4_645 ? N1 Ba2 W1 104.30(18) 5_645 4_645 ? N4 Ba2 W1 111.15(18) 5_645 4_645 ? N3 Ba2 W1 32.2(2) 4_645 4_645 ? W1 Ba2 W1 128.10(3) . 4_645 ? Ca3 Ba2 W1 77.27(4) 1_545 4_645 ? W1 Ba2 W1 118.02(3) 5_645 4_645 ? N2 Ba2 W1 30.87(16) 4_645 4_645 ? N2 Ba2 Ba1 135.2(2) 7_655 7_755 ? N3 Ba2 Ba1 113.4(2) . 7_755 ? N4 Ba2 Ba1 135.22(19) . 7_755 ? N1 Ba2 Ba1 60.98(18) 5_645 7_755 ? N4 Ba2 Ba1 55.61(18) 5_645 7_755 ? N3 Ba2 Ba1 60.30(19) 4_645 7_755 ? W1 Ba2 Ba1 131.66(3) . 7_755 ? Ca3 Ba2 Ba1 73.89(4) 1_545 7_755 ? W1 Ba2 Ba1 58.43(2) 5_645 7_755 ? N2 Ba2 Ba1 45.60(16) 4_645 7_755 ? W1 Ba2 Ba1 60.66(2) 4_645 7_755 ? N1 Ca3 N3 94.6(3) 5_655 4_655 ? N1 Ca3 N4 95.0(3) 5_655 7_665 ? N3 Ca3 N4 137.9(3) 4_655 7_665 ? N1 Ca3 N2 156.6(3) 5_655 . ? N3 Ca3 N2 103.2(3) 4_655 . ? N4 Ca3 N2 81.9(3) 7_665 . ? N1 Ca3 N1 89.2(3) 5_655 . ? N3 Ca3 N1 105.0(3) 4_655 . ? N4 Ca3 N1 116.0(3) 7_665 . ? N2 Ca3 N1 71.8(3) . . ? N1 Ca3 W1 124.9(2) 5_655 . ? N3 Ca3 W1 104.5(2) 4_655 . ? N4 Ca3 W1 103.0(2) 7_665 . ? N2 Ca3 W1 35.8(2) . . ? N1 Ca3 W1 36.23(19) . . ? N1 Ca3 N2 85.8(3) 5_655 7_665 ? N3 Ca3 N2 75.8(3) 4_655 7_665 ? N4 Ca3 N2 64.3(3) 7_665 7_665 ? N2 Ca3 N2 113.0(2) . 7_665 ? N1 Ca3 N2 174.9(3) . 7_665 ? W1 Ca3 N2 148.71(19) . 7_665 ? N1 Ca3 W1 99.5(2) 5_655 7_665 ? N3 Ca3 W1 104.2(2) 4_655 7_665 ? N4 Ca3 W1 33.7(2) 7_665 7_665 ? N2 Ca3 W1 90.7(2) . 7_665 ? N1 Ca3 W1 148.6(2) . 7_665 ? W1 Ca3 W1 123.68(6) . 7_665 ? N2 Ca3 W1 32.88(18) 7_665 7_665 ? N1 Ca3 Ca2 54.1(2) 5_655 1_565 ? N3 Ca3 Ca2 55.3(2) 4_655 1_565 ? N4 Ca3 Ca2 100.0(2) 7_665 1_565 ? N2 Ca3 Ca2 149.3(2) . 1_565 ? N1 Ca3 Ca2 131.1(2) . 1_565 ? W1 Ca3 Ca2 156.90(7) . 1_565 ? N2 Ca3 Ca2 45.21(18) 7_665 1_565 ? W1 Ca3 Ca2 76.10(5) 7_665 1_565 ? N1 Ca3 Ba2 54.1(2) 5_655 1_565 ? N3 Ca3 Ba2 55.3(2) 4_655 1_565 ? N4 Ca3 Ba2 100.0(2) 7_665 1_565 ? N2 Ca3 Ba2 149.3(2) . 1_565 ? N1 Ca3 Ba2 131.1(2) . 1_565 ? W1 Ca3 Ba2 156.90(7) . 1_565 ? N2 Ca3 Ba2 45.21(18) 7_665 1_565 ? W1 Ca3 Ba2 76.10(5) 7_665 1_565 ? Ca2 Ca3 Ba2 0.00(4) 1_565 1_565 ? N1 Ca3 Ca3 46.9(2) 5_655 5_655 ? N3 Ca3 Ca3 104.1(2) 4_655 5_655 ? N4 Ca3 Ca3 112.2(2) 7_665 5_655 ? N2 Ca3 Ca3 112.9(2) . 5_655 ? N1 Ca3 Ca3 42.28(19) . 5_655 ? W1 Ca3 Ca3 78.24(7) . 5_655 ? N2 Ca3 Ca3 132.7(2) 7_665 5_655 ? W1 Ca3 Ca3 137.28(10) 7_665 5_655 ? Ca2 Ca3 Ca3 94.88(8) 1_565 5_655 ? Ba2 Ca3 Ca3 94.88(8) 1_565 5_655 ? N1 Ca3 Ba1 93.3(2) 5_655 3_445 ? N3 Ca3 Ba1 164.5(2) 4_655 3_445 ? N4 Ca3 Ba1 54.2(2) 7_665 3_445 ? N2 Ca3 Ba1 66.0(2) . 3_445 ? N1 Ca3 Ba1 61.7(2) . 3_445 ? W1 Ca3 Ba1 60.09(4) . 3_445 ? N2 Ca3 Ba1 118.18(19) 7_665 3_445 ? W1 Ca3 Ba1 87.55(5) 7_665 3_445 ? Ca2 Ca3 Ba1 139.00(7) 1_565 3_445 ? Ba2 Ca3 Ba1 139.00(7) 1_565 3_445 ? Ca3 Ca3 Ba1 72.13(7) 5_655 3_445 ? N2 W1 N3 110.7(4) . . ? N2 W1 N1 108.0(4) . . ? N3 W1 N1 110.3(4) . . ? N2 W1 N4 110.9(4) . . ? N3 W1 N4 109.8(4) . . ? N1 W1 N4 107.0(4) . . ? N2 W1 Ca3 54.0(3) . . ? N3 W1 Ca3 121.0(3) . . ? N1 W1 Ca3 54.4(3) . . ? N4 W1 Ca3 129.2(3) . . ? N2 W1 Ba2 129.9(3) . . ? N3 W1 Ba2 51.9(3) . . ? N1 W1 Ba2 122.1(3) . . ? N4 W1 Ba2 57.9(3) . . ? Ca3 W1 Ba2 171.90(4) . . ? N2 W1 Ca3 69.0(3) . 7_655 ? N3 W1 Ca3 106.2(3) . 7_655 ? N1 W1 Ca3 141.4(3) . 7_655 ? N4 W1 Ca3 47.2(3) . 7_655 ? Ca3 W1 Ca3 114.59(4) . 7_655 ? Ba2 W1 Ca3 72.88(4) . 7_655 ? N2 W1 Ba1 76.3(3) . 3_445 ? N3 W1 Ba1 171.7(3) . 3_445 ? N1 W1 Ba1 70.3(3) . 3_445 ? N4 W1 Ba1 62.7(3) . 3_445 ? Ca3 W1 Ba1 66.45(4) . 3_445 ? Ba2 W1 Ba1 120.37(3) . 3_445 ? Ca3 W1 Ba1 71.70(4) 7_655 3_445 ? N2 W1 Ca2 138.9(3) . 5_645 ? N3 W1 Ca2 110.3(3) . 5_645 ? N1 W1 Ca2 54.6(3) . 5_645 ? N4 W1 Ca2 55.2(3) . 5_645 ? Ca3 W1 Ca2 101.73(4) . 5_645 ? Ba2 W1 Ca2 79.12(3) . 5_645 ? Ca3 W1 Ca2 101.11(4) 7_655 5_645 ? Ba1 W1 Ca2 62.94(2) 3_445 5_645 ? N2 W1 Ba2 138.9(3) . 5_645 ? N3 W1 Ba2 110.3(3) . 5_645 ? N1 W1 Ba2 54.6(3) . 5_645 ? N4 W1 Ba2 55.2(3) . 5_645 ? Ca3 W1 Ba2 101.73(4) . 5_645 ? Ba2 W1 Ba2 79.12(3) . 5_645 ? Ca3 W1 Ba2 101.11(4) 7_655 5_645 ? Ba1 W1 Ba2 62.94(2) 3_445 5_645 ? Ca2 W1 Ba2 0.00(3) 5_645 5_645 ? N2 W1 Ba1 140.4(3) . . ? N3 W1 Ba1 55.5(3) . . ? N1 W1 Ba1 57.4(3) . . ? N4 W1 Ba1 108.7(3) . . ? Ca3 W1 Ba1 98.28(4) . . ? Ba2 W1 Ba1 74.54(2) . . ? Ca3 W1 Ba1 146.92(4) 7_655 . ? Ba1 W1 Ba1 121.968(16) 3_445 . ? Ca2 W1 Ba1 66.93(2) 5_645 . ? Ba2 W1 Ba1 66.93(2) 5_645 . ? W1 N1 Ca3 171.2(5) . 5_655 ? W1 N1 Ca3 89.4(3) . . ? Ca3 N1 Ca3 90.8(3) 5_655 . ? W1 N1 Ca2 92.3(3) . 5_645 ? Ca3 N1 Ca2 82.5(3) 5_655 5_645 ? Ca3 N1 Ca2 144.7(4) . 5_645 ? W1 N1 Ba2 92.3(3) . 5_645 ? Ca3 N1 Ba2 82.5(3) 5_655 5_645 ? Ca3 N1 Ba2 144.7(4) . 5_645 ? Ca2 N1 Ba2 0.00(5) 5_645 5_645 ? W1 N1 Ba1 89.6(3) . . ? Ca3 N1 Ba1 96.7(3) 5_655 . ? Ca3 N1 Ba1 131.9(3) . . ? Ca2 N1 Ba1 83.3(2) 5_645 . ? Ba2 N1 Ba1 83.3(2) 5_645 . ? W1 N1 N2 35.8(2) . . ? Ca3 N1 N2 142.5(4) 5_655 . ? Ca3 N1 N2 53.9(2) . . ? Ca2 N1 N2 117.8(3) 5_645 . ? Ba2 N1 N2 117.8(3) 5_645 . ? Ba1 N1 N2 115.8(3) . . ? W1 N1 N4 36.6(2) . . ? Ca3 N1 N4 136.0(4) 5_655 . ? Ca3 N1 N4 110.2(3) . . ? Ca2 N1 N4 57.8(2) 5_645 . ? Ba2 N1 N4 57.8(2) 5_645 . ? Ba1 N1 N4 96.6(3) . . ? N2 N1 N4 61.3(3) . . ? W1 N1 N3 34.8(2) . . ? Ca3 N1 N3 152.9(4) 5_655 . ? Ca3 N1 N3 103.0(3) . . ? Ca2 N1 N3 98.2(3) 5_645 . ? Ba2 N1 N3 98.2(3) 5_645 . ? Ba1 N1 N3 56.7(2) . . ? N2 N1 N3 60.4(3) . . ? N4 N1 N3 60.5(3) . . ? W1 N1 Ba1 77.3(3) . 3_445 ? Ca3 N1 Ba1 94.3(3) 5_655 3_445 ? Ca3 N1 Ba1 74.8(2) . 3_445 ? Ca2 N1 Ba1 71.25(19) 5_645 3_445 ? Ba2 N1 Ba1 71.25(19) 5_645 3_445 ? Ba1 N1 Ba1 150.7(3) . 3_445 ? N2 N1 Ba1 66.7(3) . 3_445 ? N4 N1 Ba1 57.7(2) . 3_445 ? N3 N1 Ba1 111.7(3) . 3_445 ? W1 N1 N1 131.8(5) . 5_655 ? Ca3 N1 N1 47.8(2) 5_655 5_655 ? Ca3 N1 N1 43.05(19) . 5_655 ? Ca2 N1 N1 121.0(4) 5_645 5_655 ? Ba2 N1 N1 121.0(4) 5_645 5_655 ? Ba1 N1 N1 125.1(4) . 5_655 ? N2 N1 N1 96.1(4) . 5_655 ? N4 N1 N1 138.3(4) . 5_655 ? N3 N1 N1 140.8(5) . 5_655 ? Ba1 N1 N1 81.8(3) 3_445 5_655 ? W1 N1 N3 127.8(4) . 8 ? Ca3 N1 N3 43.7(2) 5_655 8 ? Ca3 N1 N3 100.9(3) . 8 ? Ca2 N1 N3 51.9(2) 5_645 8 ? Ba2 N1 N3 51.9(2) 5_645 8 ? Ba1 N1 N3 117.0(3) . 8 ? N2 N1 N3 123.3(3) . 8 ? N4 N1 N3 93.4(3) . 8 ? N3 N1 N3 149.4(3) . 8 ? Ba1 N1 N3 57.2(2) 3_445 8 ? N1 N1 N3 69.3(3) 5_655 8 ? W1 N2 Ca2 141.9(5) . 7_665 ? W1 N2 Ba2 141.9(5) . 7_665 ? Ca2 N2 Ba2 0.00(5) 7_665 7_665 ? W1 N2 Ca3 90.2(4) . . ? Ca2 N2 Ca3 100.1(3) 7_665 . ? Ba2 N2 Ca3 100.1(3) 7_665 . ? W1 N2 Ba1 100.7(4) . 6_556 ? Ca2 N2 Ba1 96.4(3) 7_665 6_556 ? Ba2 N2 Ba1 96.4(3) 7_665 6_556 ? Ca3 N2 Ba1 137.0(4) . 6_556 ? W1 N2 N1 36.2(2) . . ? Ca2 N2 N1 134.2(4) 7_665 . ? Ba2 N2 N1 134.2(4) 7_665 . ? Ca3 N2 N1 54.3(2) . . ? Ba1 N2 N1 128.8(4) 6_556 . ? W1 N2 N3 34.8(3) . . ? Ca2 N2 N3 156.0(4) 7_665 . ? Ba2 N2 N3 156.0(4) 7_665 . ? Ca3 N2 N3 103.5(4) . . ? Ba1 N2 N3 69.0(3) 6_556 . ? N1 N2 N3 60.7(3) . . ? W1 N2 N4 34.8(2) . . ? Ca2 N2 N4 108.1(4) 7_665 . ? Ba2 N2 N4 108.1(4) 7_665 . ? Ca3 N2 N4 108.7(4) . . ? Ba1 N2 N4 103.3(3) 6_556 . ? N1 N2 N4 59.4(3) . . ? N3 N2 N4 59.9(3) . . ? W1 N2 Ca3 78.1(3) . 7_655 ? Ca2 N2 Ca3 72.3(2) 7_665 7_655 ? Ba2 N2 Ca3 72.3(2) 7_665 7_655 ? Ca3 N2 Ca3 144.3(4) . 7_655 ? Ba1 N2 Ca3 78.5(2) 6_556 7_655 ? N1 N2 Ca3 105.7(3) . 7_655 ? N3 N2 Ca3 85.9(3) . 7_655 ? N4 N2 Ca3 46.7(2) . 7_655 ? W1 N2 N4 116.0(4) . 7_665 ? Ca2 N2 N4 54.5(2) 7_665 7_665 ? Ba2 N2 N4 54.5(2) 7_665 7_665 ? Ca3 N2 N4 48.0(2) . 7_665 ? Ba1 N2 N4 143.3(4) 6_556 7_665 ? N1 N2 N4 85.3(3) . 7_665 ? N3 N2 N4 145.9(4) . 7_665 ? N4 N2 N4 106.7(4) . 7_665 ? Ca3 N2 N4 107.7(3) 7_655 7_665 ? W1 N2 Ca2 75.6(3) . 4_655 ? Ca2 N2 Ca2 142.5(4) 7_665 4_655 ? Ba2 N2 Ca2 142.5(4) 7_665 4_655 ? Ca3 N2 Ca2 73.6(2) . 4_655 ? Ba1 N2 Ca2 69.3(2) 6_556 4_655 ? N1 N2 Ca2 72.5(3) . 4_655 ? N3 N2 Ca2 51.6(2) . 4_655 ? N4 N2 Ca2 109.0(3) . 4_655 ? Ca3 N2 Ca2 133.3(3) 7_655 4_655 ? N4 N2 Ca2 118.4(3) 7_665 4_655 ? W1 N2 Ba2 75.6(3) . 4_655 ? Ca2 N2 Ba2 142.5(4) 7_665 4_655 ? Ba2 N2 Ba2 142.5(4) 7_665 4_655 ? Ca3 N2 Ba2 73.6(2) . 4_655 ? Ba1 N2 Ba2 69.3(2) 6_556 4_655 ? N1 N2 Ba2 72.5(3) . 4_655 ? N3 N2 Ba2 51.6(2) . 4_655 ? N4 N2 Ba2 109.0(3) . 4_655 ? Ca3 N2 Ba2 133.3(3) 7_655 4_655 ? N4 N2 Ba2 118.4(3) 7_665 4_655 ? Ca2 N2 Ba2 0.00(4) 4_655 4_655 ? W1 N3 Ca3 172.3(5) . 4_645 ? W1 N3 Ba2 93.2(4) . . ? Ca3 N3 Ba2 94.0(3) 4_645 . ? W1 N3 Ba1 91.7(4) . . ? Ca3 N3 Ba1 90.0(3) 4_645 . ? Ba2 N3 Ba1 97.2(3) . . ? W1 N3 Ca2 93.0(4) . 4_655 ? Ca3 N3 Ca2 79.6(3) 4_645 4_655 ? Ba2 N3 Ca2 172.3(4) . 4_655 ? Ba1 N3 Ca2 87.2(3) . 4_655 ? W1 N3 Ba2 93.0(4) . 4_655 ? Ca3 N3 Ba2 79.6(3) 4_645 4_655 ? Ba2 N3 Ba2 172.3(4) . 4_655 ? Ba1 N3 Ba2 87.2(3) . 4_655 ? Ca2 N3 Ba2 0.00(4) 4_655 4_655 ? W1 N3 N2 34.5(3) . . ? Ca3 N3 N2 139.0(4) 4_645 . ? Ba2 N3 N2 111.7(4) . . ? Ba1 N3 N2 116.2(4) . . ? Ca2 N3 N2 71.5(3) 4_655 . ? Ba2 N3 N2 71.5(3) 4_655 . ? W1 N3 N4 35.2(2) . . ? Ca3 N3 N4 151.7(4) 4_645 . ? Ba2 N3 N4 58.0(3) . . ? Ba1 N3 N4 96.8(3) . . ? Ca2 N3 N4 127.9(4) 4_655 . ? Ba2 N3 N4 127.9(4) 4_655 . ? N2 N3 N4 60.2(3) . . ? W1 N3 N1 34.9(2) . . ? Ca3 N3 N1 143.7(4) 4_645 . ? Ba2 N3 N1 106.9(4) . . ? Ba1 N3 N1 58.7(2) . . ? Ca2 N3 N1 80.8(3) 4_655 . ? Ba2 N3 N1 80.8(3) 4_655 . ? N2 N3 N1 58.9(3) . . ? N4 N3 N1 58.9(3) . . ? W1 N3 Ba1 82.7(3) . 6_556 ? Ca3 N3 Ba1 92.8(3) 4_645 6_556 ? Ba2 N3 Ba1 105.6(3) . 6_556 ? Ba1 N3 Ba1 156.8(4) . 6_556 ? Ca2 N3 Ba1 70.6(2) 4_655 6_556 ? Ba2 N3 Ba1 70.6(2) 4_655 6_556 ? N2 N3 Ba1 50.7(2) . 6_556 ? N4 N3 Ba1 91.5(3) . 6_556 ? N1 N3 Ba1 109.0(3) . 6_556 ? W1 N3 N2 114.5(4) . 6_656 ? Ca3 N3 N2 61.5(3) 4_645 6_656 ? Ba2 N3 N2 134.4(4) . 6_656 ? Ba1 N3 N2 49.5(2) . 6_656 ? Ca2 N3 N2 45.7(2) 4_655 6_656 ? Ba2 N3 N2 45.7(2) 4_655 6_656 ? N2 N3 N2 111.2(4) . 6_656 ? N4 N3 N2 140.3(4) . 6_656 ? N1 N3 N2 83.0(3) . 6_656 ? Ba1 N3 N2 112.9(3) 6_556 6_656 ? W1 N4 Ca3 99.1(4) . 7_655 ? W1 N4 Ba2 86.9(3) . . ? Ca3 N4 Ba2 96.5(3) 7_655 . ? W1 N4 Ca2 91.6(3) . 5_645 ? Ca3 N4 Ca2 161.2(4) 7_655 5_645 ? Ba2 N4 Ca2 99.5(3) . 5_645 ? W1 N4 Ba2 91.6(3) . 5_645 ? Ca3 N4 Ba2 161.2(4) 7_655 5_645 ? Ba2 N4 Ba2 99.5(3) . 5_645 ? Ca2 N4 Ba2 0.00(5) 5_645 5_645 ? W1 N4 Ba1 169.8(4) . 5_645 ? Ca3 N4 Ba1 82.8(2) 7_655 5_645 ? Ba2 N4 Ba1 82.9(2) . 5_645 ? Ca2 N4 Ba1 89.4(3) 5_645 5_645 ? Ba2 N4 Ba1 89.4(3) 5_645 5_645 ? W1 N4 N1 36.5(2) . . ? Ca3 N4 N1 127.9(4) 7_655 . ? Ba2 N4 N1 103.5(3) . . ? Ca2 N4 N1 57.2(2) 5_645 . ? Ba2 N4 N1 57.2(2) 5_645 . ? Ba1 N4 N1 146.5(4) 5_645 . ? W1 N4 Ba1 84.2(3) . 3_445 ? Ca3 N4 Ba1 90.7(3) 7_655 3_445 ? Ba2 N4 Ba1 169.3(3) . 3_445 ? Ca2 N4 Ba1 74.9(2) 5_645 3_445 ? Ba2 N4 Ba1 74.9(2) 5_645 3_445 ? Ba1 N4 Ba1 105.9(3) 5_645 3_445 ? N1 N4 Ba1 65.9(2) . 3_445 ? W1 N4 N3 35.0(2) . . ? Ca3 N4 N3 99.8(4) 7_655 . ? Ba2 N4 N3 52.0(2) . . ? Ca2 N4 N3 97.9(3) 5_645 . ? Ba2 N4 N3 97.9(3) 5_645 . ? Ba1 N4 N3 134.9(4) 5_645 . ? N1 N4 N3 60.7(3) . . ? Ba1 N4 N3 119.1(3) 3_445 . ? W1 N4 N2 34.3(2) . . ? Ca3 N4 N2 69.1(3) 7_655 . ? Ba2 N4 N2 106.1(3) . . ? Ca2 N4 N2 115.2(3) 5_645 . ? Ba2 N4 N2 115.2(3) 5_645 . ? Ba1 N4 N2 151.1(4) 5_645 . ? N1 N4 N2 59.3(3) . . ? Ba1 N4 N2 69.2(3) 3_445 . ? N3 N4 N2 59.8(3) . . ? W1 N4 N2 106.3(4) . 7_655 ? Ca3 N4 N2 50.1(2) 7_655 7_655 ? Ba2 N4 N2 48.6(2) . 7_655 ? Ca2 N4 N2 140.8(3) 5_645 7_655 ? Ba2 N4 N2 140.8(3) 5_645 7_655 ? Ba1 N4 N2 67.2(2) 5_645 7_655 ? N1 N4 N2 140.4(4) . 7_655 ? Ba1 N4 N2 140.2(3) 3_445 7_655 ? N3 N4 N2 80.1(3) . 7_655 ? N2 N4 N2 97.7(3) . 7_655 ? #===END