#------------------------------------------------------------------------------ #$Date: 2011-01-03 14:48:23 +0200 (Mon, 03 Jan 2011) $ #$Revision: 5312 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7012467.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7012467 loop_ _publ_author_name 'Baker, Charles F.' 'Barker, Marten G.' 'Blake, Alexander J.' 'Wilson, Claire' 'Gregory, Duncan H.' _publ_section_title ; Synthesis and structure of new mixed alkaline-earth nitridomolybdates and nitridotungstates, (Ba,Ca)3[MN4] (M = Mo, W)Dedicated to Dr Marten G. Barker in memoriam. ; _journal_issue 6 _journal_name_full 'Dalton Transactions' _journal_page_first 1065 _journal_year 2003 _chemical_compound_source 'synthesis as described' _chemical_formula_moiety 'Ba6 Ca6 N16 W4' _chemical_formula_sum 'Ba1.44 Ca1.56 N4 W' _chemical_formula_weight 499.94 _chemical_name_systematic ; ? ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_creation_date 2002-10-25T09:52:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.3049(10) _cell_length_b 9.5822(9) _cell_length_c 11.7405(11) _cell_measurement_reflns_used 1401 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.56 _cell_measurement_theta_min 3.38 _cell_volume 1159.30(19) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_molecular_graphics 'ATOMS 4.1 (Dowty, 1998)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.906 _diffrn_measured_fraction_theta_max 0.906 _diffrn_measurement_device_type 'Bruker Smart CCD' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_unetI/netI 0.044 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4876 _diffrn_reflns_theta_full 28.69 _diffrn_reflns_theta_max 28.69 _diffrn_reflns_theta_min 3.38 _diffrn_standards_decay_% none _exptl_absorpt_coefficient_mu 30.754 _exptl_absorpt_correction_T_max 0.296 _exptl_absorpt_correction_T_min 0.149 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SAINT V6.01/SADABS' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 5.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 1710 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _refine_diff_density_max 3.19 _refine_diff_density_min -3.204 _refine_diff_density_rms 0.47 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.94 _refine_ls_matrix_type full _refine_ls_number_parameters 74 _refine_ls_number_reflns 1352 _refine_ls_number_restraints 24 _refine_ls_restrained_S_all 0.935 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0357 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _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_wR_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.0822 _reflns_number_gt 1058 _reflns_number_total 1564 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b211138a.txt _[local]_cod_data_source_block cabawn _[local]_cod_cif_authors_sg_H-M Pbca _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multiscan' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 7012467 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' 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) 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_ _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 ? 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 ?