#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100153.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_1100153 _audit_contact_author_name 'Kruger, Hannes' _audit_contact_author_address ; Institut fur Mineralogie und Petrographie Leopold-Franzens-Universitat Innsbruck Innrain 52 A-6020 Innsbruck Austria ; _audit_contact_author_email Hannes.Krueger@uibk.ac.at _audit_contact_author_fax '+43 512 507 2926' _audit_contact_author_phone '+43 512 507 5502' _publ_requested_journal Unpublished loop_ _publ_author_name 'Kruger, Hannes' 'Kahlenberg, Volker' _chemical_formula_sum 'Ca4 F2 O7 Si2' _chemical_formula_weight 366.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.5397(16) _cell_length_b 10.5338(19) _cell_length_c 10.907(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.557(17) _cell_angle_gamma 90.00 _cell_volume 816.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 6855 _cell_measurement_theta_max 29.41 _cell_measurement_theta_min 0.00 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 2.994 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type 'STOE' _diffrn_detector_area_resol_mean 6.67 _diffrn_source ; sealed X-ray tube, 12 x 0.4 mm long-fine focus ; _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, multiple pinhole' _diffrn_ambient_temperature 300(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 100 mm ; _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_number 8019 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 29.40 _diffrn_reflns_theta_full 29.40 _diffrn_reflns_av_unetI/netI 0.0629 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _reflns_number_total 2238 _reflns_number_gt 1745 _reflns_threshold_expression 'I>2u(I)' _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^)+(0.0293P)^2^+0.2638P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0154(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2238 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0664 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca1 Ca -0.03011(8) 0.40475(6) 0.69828(5) 0.00849(13) Uani 1 1 d . . . Ca2 Ca 0.66300(7) 0.13301(6) 0.58356(5) 0.00847(13) Uani 1 1 d . . . Ca3 Ca 0.83067(8) 0.63499(6) 0.92406(5) 0.00882(13) Uani 1 1 d . . . Ca4 Ca 0.47033(8) 0.41482(5) 0.68450(5) 0.00761(12) Uani 1 1 d . . . Si5 Si 0.27271(10) 0.30739(8) 0.36755(6) 0.00571(15) Uani 1 1 d . . . Si6 Si -0.15215(10) 0.30935(8) 0.37762(6) 0.00572(15) Uani 1 1 d . . . F7 F 0.5742(2) 0.49984(17) 0.89674(15) 0.0106(3) Uani 1 1 d . . . F8 F 0.9268(2) 0.49630(17) 1.10128(15) 0.0106(3) Uani 1 1 d . . . O9 O 0.7224(3) 0.2789(2) 0.76016(18) 0.0120(4) Uani 1 1 d . . . O10 O 0.0635(3) 0.2753(2) 0.3787(2) 0.0140(4) Uani 1 1 d . . . O11 O -0.1390(3) 0.2670(2) 0.52267(18) 0.0109(4) Uani 1 1 d . . . O12 O 0.7302(3) 0.7805(2) 0.75469(18) 0.0110(4) Uani 1 1 d . . . O13 O 0.4103(3) 0.2652(2) 0.50919(19) 0.0118(4) Uani 1 1 d . . . O14 O 0.1983(3) 0.5438(2) 0.6604(2) 0.0138(4) Uani 1 1 d . . . O15 O -0.2831(3) 0.5462(2) 0.6703(2) 0.0151(4) 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 Ca1 0.0084(2) 0.0079(3) 0.0093(2) -0.00168(19) 0.00315(18) -0.0003(2) Ca2 0.0075(2) 0.0079(3) 0.0100(3) -0.00103(19) 0.00302(18) -0.0002(2) Ca3 0.0092(2) 0.0089(3) 0.0084(2) 0.00200(19) 0.00306(18) 0.0007(2) Ca4 0.0070(2) 0.0069(3) 0.0092(2) -0.00067(19) 0.00293(17) -0.0003(2) Si5 0.0054(3) 0.0057(4) 0.0061(3) 0.0006(3) 0.0020(2) 0.0001(3) Si6 0.0056(3) 0.0065(4) 0.0055(3) 0.0008(2) 0.0024(2) 0.0002(3) F7 0.0095(7) 0.0114(9) 0.0104(7) -0.0010(6) 0.0029(6) 0.0000(6) F8 0.0120(7) 0.0098(9) 0.0096(7) 0.0006(6) 0.0032(6) -0.0008(7) O9 0.0134(9) 0.0121(11) 0.0081(8) 0.0002(7) 0.0005(7) 0.0034(8) O10 0.0084(8) 0.0140(11) 0.0220(10) 0.0050(8) 0.0082(7) 0.0013(9) O11 0.0141(10) 0.0131(11) 0.0064(8) 0.0000(7) 0.0048(7) -0.0030(8) O12 0.0132(9) 0.0110(11) 0.0092(8) -0.0017(7) 0.0043(7) 0.0010(8) O13 0.0111(9) 0.0134(11) 0.0083(8) -0.0003(7) -0.0003(7) 0.0031(8) O14 0.0130(10) 0.0076(11) 0.0225(11) 0.0047(8) 0.0084(8) 0.0025(8) O15 0.0119(9) 0.0105(11) 0.0245(11) 0.0037(8) 0.0083(8) -0.0003(9) _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 Ca1 F8 2.3093(18) 3_667 ? Ca1 O11 2.323(2) . ? Ca1 O15 2.359(2) . ? Ca1 O14 2.399(2) . ? Ca1 O12 2.513(2) 2_646 ? Ca1 O9 2.557(2) 1_455 ? Ca1 O10 2.653(2) 4_566 ? Ca1 Si5 3.2853(11) 4_566 ? Ca1 Si6 3.3113(10) 4_566 ? Ca1 Si6 3.4547(11) . ? Ca1 Si5 3.4895(11) 3_566 ? Ca1 Si6 3.5222(11) 3_566 ? Ca2 O13 2.278(2) . ? Ca2 O11 2.307(2) 1_655 ? Ca2 F7 2.3388(18) 2_646 ? Ca2 F8 2.3647(18) 4_565 ? Ca2 F7 2.3761(18) 4_565 ? Ca2 O9 2.386(2) . ? Ca2 O14 2.796(2) 2_646 ? Ca2 Si6 3.0993(11) 4_666 ? Ca2 Si6 3.5403(10) 1_655 ? Ca2 Si5 3.5976(11) . ? Ca2 Ca1 3.6298(10) 1_655 ? Ca2 Ca4 3.6339(9) . ? Ca3 O12 2.323(2) . ? Ca3 F8 2.3363(18) . ? Ca3 F7 2.3384(19) . ? Ca3 F8 2.3813(19) 3_767 ? Ca3 O10 2.510(2) 2_656 ? Ca3 O13 2.569(2) 2_656 ? Ca3 O11 2.602(2) 2_656 ? Ca3 O15 2.771(2) 1_655 ? Ca3 Si5 3.0713(11) 3_666 ? Ca3 Si5 3.2028(10) 2_656 ? Ca3 Si6 3.2276(11) 2_656 ? Ca3 Ca4 3.6663(10) 2_656 ? Ca4 O9 2.301(2) . ? Ca4 O12 2.324(2) 2_646 ? Ca4 F7 2.3582(18) . ? Ca4 O15 2.364(2) 1_655 ? Ca4 O14 2.400(2) . ? Ca4 O13 2.401(2) . ? Ca4 Si5 3.4646(12) . ? Ca4 Ca3 3.6663(10) 2_646 ? Ca4 Ca1 3.7204(11) 1_655 ? Ca4 Ca2 3.7942(10) 2_656 ? Si5 O15 1.605(2) 3_566 ? Si5 O13 1.609(2) . ? Si5 O12 1.617(2) 3_666 ? Si5 O10 1.657(2) . ? Si5 Ca3 3.0713(11) 3_666 ? Si5 Ca3 3.2028(10) 2_646 ? Si5 Ca1 3.2853(11) 4_565 ? Si5 Ca1 3.4895(11) 3_566 ? Si6 O9 1.609(2) 4_465 ? Si6 O14 1.610(2) 3_566 ? Si6 O11 1.615(2) . ? Si6 O10 1.661(2) . ? Si6 Ca2 3.0993(11) 4_465 ? Si6 Ca3 3.2276(11) 2_646 ? Si6 Ca1 3.3113(10) 4_565 ? Si6 Ca1 3.5222(11) 3_566 ? Si6 Ca2 3.5403(10) 1_455 ? F7 Ca2 2.3388(18) 2_656 ? F7 Ca2 2.3761(18) 4_566 ? F8 Ca1 2.3093(17) 3_667 ? F8 Ca2 2.3647(18) 4_566 ? F8 Ca3 2.3813(19) 3_767 ? O9 Si6 1.609(2) 4_666 ? O9 Ca1 2.557(2) 1_655 ? O10 Ca3 2.510(2) 2_646 ? O10 Ca1 2.653(2) 4_565 ? O11 Ca2 2.307(2) 1_455 ? O11 Ca3 2.602(2) 2_646 ? O12 Si5 1.617(2) 3_666 ? O12 Ca4 2.324(2) 2_656 ? O12 Ca1 2.513(2) 2_656 ? O13 Ca3 2.569(2) 2_646 ? O14 Si6 1.610(2) 3_566 ? O14 Ca2 2.796(2) 2_656 ? O15 Si5 1.605(2) 3_566 ? O15 Ca4 2.364(2) 1_455 ? O15 Ca3 2.771(2) 1_455 ? 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 F8 Ca1 O11 167.61(7) 3_667 . ? F8 Ca1 O15 80.74(7) 3_667 . ? O11 Ca1 O15 103.93(8) . . ? F8 Ca1 O14 81.57(7) 3_667 . ? O11 Ca1 O14 108.38(7) . . ? O15 Ca1 O14 100.86(7) . . ? F8 Ca1 O12 92.67(7) 3_667 2_646 ? O11 Ca1 O12 83.59(7) . 2_646 ? O15 Ca1 O12 171.57(8) . 2_646 ? O14 Ca1 O12 72.80(7) . 2_646 ? F8 Ca1 O9 91.65(7) 3_667 1_455 ? O11 Ca1 O9 78.81(7) . 1_455 ? O15 Ca1 O9 74.42(7) . 1_455 ? O14 Ca1 O9 172.36(8) . 1_455 ? O12 Ca1 O9 111.25(7) 2_646 1_455 ? F8 Ca1 O10 72.46(7) 3_667 4_566 ? O11 Ca1 O10 95.62(7) . 4_566 ? O15 Ca1 O10 123.39(7) . 4_566 ? O14 Ca1 O10 122.40(7) . 4_566 ? O12 Ca1 O10 58.56(6) 2_646 4_566 ? O9 Ca1 O10 57.99(7) 1_455 4_566 ? F8 Ca1 Si5 79.88(5) 3_667 4_566 ? O11 Ca1 Si5 91.48(6) . 4_566 ? O15 Ca1 Si5 151.91(6) . 4_566 ? O14 Ca1 Si5 96.19(6) . 4_566 ? O12 Ca1 Si5 28.63(5) 2_646 4_566 ? O9 Ca1 Si5 86.00(5) 1_455 4_566 ? O10 Ca1 Si5 30.07(5) 4_566 4_566 ? F8 Ca1 Si6 79.66(5) 3_667 4_566 ? O11 Ca1 Si6 88.29(6) . 4_566 ? O15 Ca1 Si6 97.70(6) . 4_566 ? O14 Ca1 Si6 151.01(6) . 4_566 ? O12 Ca1 Si6 86.19(5) 2_646 4_566 ? O9 Ca1 Si6 28.27(5) 1_455 4_566 ? O10 Ca1 Si6 29.82(5) 4_566 4_566 ? Si5 Ca1 Si6 58.87(2) 4_566 4_566 ? F8 Ca1 Si6 168.78(5) 3_667 . ? O11 Ca1 Si6 23.46(5) . . ? O15 Ca1 Si6 97.07(6) . . ? O14 Ca1 Si6 88.09(6) . . ? O12 Ca1 Si6 88.38(5) 2_646 . ? O9 Ca1 Si6 98.38(5) 1_455 . ? O10 Ca1 Si6 117.23(5) 4_566 . ? Si5 Ca1 Si6 105.70(3) 4_566 . ? Si6 Ca1 Si6 111.56(2) 4_566 . ? F8 Ca1 Si5 77.88(5) 3_667 3_566 ? O11 Ca1 Si5 110.91(6) . 3_566 ? O15 Ca1 Si5 22.91(5) . 3_566 ? O14 Ca1 Si5 77.96(6) . 3_566 ? O12 Ca1 Si5 150.30(5) 2_646 3_566 ? O9 Ca1 Si5 97.25(5) 1_455 3_566 ? O10 Ca1 Si5 139.89(5) 4_566 3_566 ? Si5 Ca1 Si5 157.60(2) 4_566 3_566 ? Si6 Ca1 Si5 118.90(3) 4_566 3_566 ? Si6 Ca1 Si5 95.79(2) . 3_566 ? F8 Ca1 Si6 78.59(5) 3_667 3_566 ? O11 Ca1 Si6 113.48(6) . 3_566 ? O15 Ca1 Si6 77.98(6) . 3_566 ? O14 Ca1 Si6 22.89(5) . 3_566 ? O12 Ca1 Si6 95.64(5) 2_646 3_566 ? O9 Ca1 Si6 151.88(5) 1_455 3_566 ? O10 Ca1 Si6 139.27(5) 4_566 3_566 ? Si5 Ca1 Si6 117.47(3) 4_566 3_566 ? Si6 Ca1 Si6 158.23(2) 4_566 3_566 ? Si6 Ca1 Si6 90.20(2) . 3_566 ? Si5 Ca1 Si6 55.08(2) 3_566 3_566 ? O13 Ca2 O11 93.91(8) . 1_655 ? O13 Ca2 F7 79.93(7) . 2_646 ? O11 Ca2 F7 168.97(7) 1_655 2_646 ? O13 Ca2 F8 164.00(7) . 4_565 ? O11 Ca2 F8 76.60(7) 1_655 4_565 ? F7 Ca2 F8 107.17(7) 2_646 4_565 ? O13 Ca2 F7 95.31(7) . 4_565 ? O11 Ca2 F7 97.87(7) 1_655 4_565 ? F7 Ca2 F7 73.80(7) 2_646 4_565 ? F8 Ca2 F7 73.66(6) 4_565 4_565 ? O13 Ca2 O9 78.61(7) . . ? O11 Ca2 O9 82.75(7) 1_655 . ? F7 Ca2 O9 104.76(7) 2_646 . ? F8 Ca2 O9 112.31(7) 4_565 . ? F7 Ca2 O9 173.92(7) 4_565 . ? O13 Ca2 O14 123.34(7) . 2_646 ? O11 Ca2 O14 115.56(7) 1_655 2_646 ? F7 Ca2 O14 75.43(6) 2_646 2_646 ? F8 Ca2 O14 72.64(6) 4_565 2_646 ? F7 Ca2 O14 124.20(7) 4_565 2_646 ? O9 Ca2 O14 60.27(7) . 2_646 ? O13 Ca2 Si6 106.35(6) . 4_666 ? O11 Ca2 Si6 93.90(5) 1_655 4_666 ? F7 Ca2 Si6 96.62(5) 2_646 4_666 ? F8 Ca2 Si6 87.35(5) 4_565 4_666 ? F7 Ca2 Si6 154.54(5) 4_565 4_666 ? O9 Ca2 Si6 30.76(5) . 4_666 ? O14 Ca2 Si6 31.15(5) 2_646 4_666 ? O13 Ca2 Si6 85.03(6) . 1_655 ? O11 Ca2 Si6 21.02(5) 1_655 1_655 ? F7 Ca2 Si6 148.05(5) 2_646 1_655 ? F8 Ca2 Si6 81.66(5) 4_565 1_655 ? F7 Ca2 Si6 79.78(5) 4_565 1_655 ? O9 Ca2 Si6 99.61(6) . 1_655 ? O14 Ca2 Si6 135.64(5) 2_646 1_655 ? Si6 Ca2 Si6 114.69(3) 4_666 1_655 ? O13 Ca2 Si5 18.50(5) . . ? O11 Ca2 Si5 88.02(6) 1_655 . ? F7 Ca2 Si5 83.30(5) 2_646 . ? F8 Ca2 Si5 145.98(4) 4_565 . ? F7 Ca2 Si5 78.77(5) 4_565 . ? O9 Ca2 Si5 95.23(6) . . ? O14 Ca2 Si5 140.90(5) 2_646 . ? Si6 Ca2 Si5 124.30(3) 4_666 . ? Si6 Ca2 Si5 74.10(2) 1_655 . ? O13 Ca2 Ca1 90.08(6) . 1_655 ? O11 Ca2 Ca1 38.54(5) 1_655 1_655 ? F7 Ca2 Ca1 149.34(5) 2_646 1_655 ? F8 Ca2 Ca1 90.25(5) 4_565 1_655 ? F7 Ca2 Ca1 136.40(5) 4_565 1_655 ? O9 Ca2 Ca1 44.62(5) . 1_655 ? O14 Ca2 Ca1 86.49(5) 2_646 1_655 ? Si6 Ca2 Ca1 58.32(2) 4_666 1_655 ? Si6 Ca2 Ca1 57.59(2) 1_655 1_655 ? Si5 Ca2 Ca1 96.34(3) . 1_655 ? O13 Ca2 Ca4 40.30(5) . . ? O11 Ca2 Ca4 87.16(6) 1_655 . ? F7 Ca2 Ca4 93.82(5) 2_646 . ? F8 Ca2 Ca4 148.92(5) 4_565 . ? F7 Ca2 Ca4 135.61(5) 4_565 . ? O9 Ca2 Ca4 38.32(5) . . ? O14 Ca2 Ca4 91.48(5) 2_646 . ? Si6 Ca2 Ca4 67.25(2) 4_666 . ? Si6 Ca2 Ca4 92.63(3) 1_655 . ? Si5 Ca2 Ca4 57.25(2) . . ? Ca1 Ca2 Ca4 61.62(2) 1_655 . ? O12 Ca3 F8 176.97(7) . . ? O12 Ca3 F7 105.35(7) . . ? F8 Ca3 F7 74.87(6) . . ? O12 Ca3 F8 110.45(7) . 3_767 ? F8 Ca3 F8 72.25(7) . 3_767 ? F7 Ca3 F8 105.42(6) . 3_767 ? O12 Ca3 O10 102.62(8) . 2_656 ? F8 Ca3 O10 74.79(7) . 2_656 ? F7 Ca3 O10 118.67(7) . 2_656 ? F8 Ca3 O10 113.91(7) 3_767 2_656 ? O12 Ca3 O13 78.46(7) . 2_656 ? F8 Ca3 O13 98.76(6) . 2_656 ? F7 Ca3 O13 74.21(7) . 2_656 ? F8 Ca3 O13 170.56(6) 3_767 2_656 ? O10 Ca3 O13 59.65(7) 2_656 2_656 ? O12 Ca3 O11 81.62(7) . 2_656 ? F8 Ca3 O11 98.21(6) . 2_656 ? F7 Ca3 O11 173.00(7) . 2_656 ? F8 Ca3 O11 70.91(7) 3_767 2_656 ? O10 Ca3 O11 59.34(6) 2_656 2_656 ? O13 Ca3 O11 108.39(7) 2_656 2_656 ? O12 Ca3 O15 61.25(7) . 1_655 ? F8 Ca3 O15 121.45(7) . 1_655 ? F7 Ca3 O15 72.60(6) . 1_655 ? F8 Ca3 O15 71.41(6) 3_767 1_655 ? O10 Ca3 O15 163.32(7) 2_656 1_655 ? O13 Ca3 O15 116.83(7) 2_656 1_655 ? O11 Ca3 O15 110.99(6) 2_656 1_655 ? O12 Ca3 Si5 31.14(5) . 3_666 ? F8 Ca3 Si5 151.80(5) . 3_666 ? F7 Ca3 Si5 94.36(5) . 3_666 ? F8 Ca3 Si5 86.17(4) 3_767 3_666 ? O10 Ca3 Si5 131.98(6) 2_656 3_666 ? O13 Ca3 Si5 103.28(5) 2_656 3_666 ? O11 Ca3 Si5 91.36(5) 2_656 3_666 ? O15 Ca3 Si5 31.36(5) 1_655 3_666 ? O12 Ca3 Si5 95.64(6) . 2_656 ? F8 Ca3 Si5 81.33(5) . 2_656 ? F7 Ca3 Si5 92.77(5) . 2_656 ? F8 Ca3 Si5 142.22(5) 3_767 2_656 ? O10 Ca3 Si5 30.79(5) 2_656 2_656 ? O13 Ca3 Si5 29.87(5) 2_656 2_656 ? O11 Ca3 Si5 87.14(5) 2_656 2_656 ? O15 Ca3 Si5 146.36(5) 1_655 2_656 ? Si5 Ca3 Si5 125.82(3) 3_666 2_656 ? O12 Ca3 Si6 97.43(6) . 2_656 ? F8 Ca3 Si6 81.14(5) . 2_656 ? F7 Ca3 Si6 146.64(5) . 2_656 ? F8 Ca3 Si6 88.55(5) 3_767 2_656 ? O10 Ca3 Si6 30.52(5) 2_656 2_656 ? O13 Ca3 Si6 87.14(5) 2_656 2_656 ? O11 Ca3 Si6 29.76(4) 2_656 2_656 ? O15 Ca3 Si6 140.66(5) 1_655 2_656 ? Si5 Ca3 Si6 117.06(3) 3_666 2_656 ? Si5 Ca3 Si6 60.55(2) 2_656 2_656 ? O12 Ca3 Ca4 37.92(5) . 2_656 ? F8 Ca3 Ca4 139.20(5) . 2_656 ? F7 Ca3 Ca4 93.00(5) . 2_656 ? F8 Ca3 Ca4 147.76(5) 3_767 2_656 ? O10 Ca3 Ca4 77.77(6) 2_656 2_656 ? O13 Ca3 Ca4 40.73(5) 2_656 2_656 ? O11 Ca3 Ca4 93.02(5) 2_656 2_656 ? O15 Ca3 Ca4 89.86(5) 1_655 2_656 ? Si5 Ca3 Ca4 65.89(2) 3_666 2_656 ? Si5 Ca3 Ca4 60.13(2) 2_656 2_656 ? Si6 Ca3 Ca4 90.22(3) 2_656 2_656 ? O9 Ca4 O12 93.27(8) . 2_646 ? O9 Ca4 F7 85.48(7) . . ? O12 Ca4 F7 89.15(7) 2_646 . ? O9 Ca4 O15 79.31(8) . 1_655 ? O12 Ca4 O15 167.50(8) 2_646 1_655 ? F7 Ca4 O15 80.31(7) . 1_655 ? O9 Ca4 O14 164.70(8) . . ? O12 Ca4 O14 76.23(8) 2_646 . ? F7 Ca4 O14 83.30(7) . . ? O15 Ca4 O14 108.87(8) 1_655 . ? O9 Ca4 O13 77.87(7) . . ? O12 Ca4 O13 81.98(8) 2_646 . ? F7 Ca4 O13 160.59(7) . . ? O15 Ca4 O13 105.95(8) 1_655 . ? O14 Ca4 O13 110.99(8) . . ? O9 Ca4 Si5 100.51(5) . . ? O12 Ca4 Si5 88.99(5) 2_646 . ? F7 Ca4 Si5 173.82(5) . . ? O15 Ca4 Si5 102.17(6) 1_655 . ? O14 Ca4 Si5 90.54(6) . . ? O13 Ca4 Si5 24.16(5) . . ? O9 Ca4 Ca2 40.03(5) . . ? O12 Ca4 Ca2 87.33(6) 2_646 . ? F7 Ca4 Ca2 124.93(5) . . ? O15 Ca4 Ca2 93.19(6) 1_655 . ? O14 Ca4 Ca2 147.44(6) . . ? O13 Ca4 Ca2 37.85(5) . . ? Si5 Ca4 Ca2 60.85(2) . . ? O9 Ca4 Ca3 87.89(6) . 2_646 ? O12 Ca4 Ca3 37.91(5) 2_646 2_646 ? F7 Ca4 Ca3 126.07(5) . 2_646 ? O15 Ca4 Ca3 149.88(6) 1_655 2_646 ? O14 Ca4 Ca3 90.33(6) . 2_646 ? O13 Ca4 Ca3 44.26(5) . 2_646 ? Si5 Ca4 Ca3 53.287(19) . 2_646 ? Ca2 Ca4 Ca3 60.82(2) . 2_646 ? O9 Ca4 Ca1 42.62(6) . 1_655 ? O12 Ca4 Ca1 135.87(6) 2_646 1_655 ? F7 Ca4 Ca1 88.40(5) . 1_655 ? O15 Ca4 Ca1 37.97(6) 1_655 1_655 ? O14 Ca4 Ca1 146.83(6) . 1_655 ? O13 Ca4 Ca1 86.09(5) . 1_655 ? Si5 Ca4 Ca1 97.03(3) . 1_655 ? Ca2 Ca4 Ca1 59.135(17) . 1_655 ? Ca3 Ca4 Ca1 119.93(2) 2_646 1_655 ? O9 Ca4 Ca2 120.61(5) . 2_656 ? O12 Ca4 Ca2 80.54(6) 2_646 2_656 ? F7 Ca4 Ca2 35.95(4) . 2_656 ? O15 Ca4 Ca2 94.51(6) 1_655 2_656 ? O14 Ca4 Ca2 47.36(6) . 2_656 ? O13 Ca4 Ca2 155.13(5) . 2_656 ? Si5 Ca4 Ca2 137.88(2) . 2_656 ? Ca2 Ca4 Ca2 156.762(19) . 2_656 ? Ca3 Ca4 Ca2 115.40(2) 2_646 2_656 ? Ca1 Ca4 Ca2 118.75(2) 1_655 2_656 ? O9 Ca4 Ca1 132.49(6) . . ? O12 Ca4 Ca1 39.44(5) 2_646 . ? F7 Ca4 Ca1 88.85(5) . . ? O15 Ca4 Ca1 145.68(6) 1_655 . ? O14 Ca4 Ca1 37.10(5) . . ? O13 Ca4 Ca1 95.03(6) . . ? Si5 Ca4 Ca1 85.98(3) . . ? Ca2 Ca4 Ca1 119.25(2) . . ? Ca3 Ca4 Ca1 58.577(17) 2_646 . ? Ca1 Ca4 Ca1 174.63(2) 1_655 . ? Ca2 Ca4 Ca1 60.390(18) 2_656 . ? O15 Si5 O13 116.19(12) 3_566 . ? O15 Si5 O12 109.03(12) 3_566 3_666 ? O13 Si5 O12 117.38(11) . 3_666 ? O15 Si5 O10 110.16(11) 3_566 . ? O13 Si5 O10 101.35(11) . . ? O12 Si5 O10 101.15(11) 3_666 . ? O15 Si5 Ca3 63.96(8) 3_566 3_666 ? O13 Si5 Ca3 155.19(8) . 3_666 ? O12 Si5 Ca3 47.98(8) 3_666 3_666 ? O10 Si5 Ca3 101.46(8) . 3_666 ? O15 Si5 Ca3 140.52(8) 3_566 2_646 ? O13 Si5 Ca3 52.68(8) . 2_646 ? O12 Si5 Ca3 108.73(8) 3_666 2_646 ? O10 Si5 Ca3 50.83(8) . 2_646 ? Ca3 Si5 Ca3 144.03(3) 3_666 2_646 ? O15 Si5 Ca1 126.41(9) 3_566 4_565 ? O13 Si5 Ca1 117.08(9) . 4_565 ? O12 Si5 Ca1 48.10(8) 3_666 4_565 ? O10 Si5 Ca1 53.35(8) . 4_565 ? Ca3 Si5 Ca1 70.41(2) 3_666 4_565 ? Ca3 Si5 Ca1 74.02(3) 2_646 4_565 ? O15 Si5 Ca4 84.33(9) 3_566 . ? O13 Si5 Ca4 37.66(8) . . ? O12 Si5 Ca4 153.16(8) 3_666 . ? O10 Si5 Ca4 95.46(8) . . ? Ca3 Si5 Ca4 147.58(3) 3_666 . ? Ca3 Si5 Ca4 66.58(2) 2_646 . ? Ca1 Si5 Ca4 140.24(3) 4_565 . ? O15 Si5 Ca1 34.88(8) 3_566 3_566 ? O13 Si5 Ca1 124.26(8) . 3_566 ? O12 Si5 Ca1 117.79(8) 3_666 3_566 ? O10 Si5 Ca1 75.29(8) . 3_566 ? Ca3 Si5 Ca1 71.42(2) 3_666 3_566 ? Ca3 Si5 Ca1 113.79(3) 2_646 3_566 ? Ca1 Si5 Ca1 104.93(3) 4_565 3_566 ? Ca4 Si5 Ca1 86.69(2) . 3_566 ? O15 Si5 Ca2 124.01(9) 3_566 . ? O13 Si5 Ca2 26.71(8) . . ? O12 Si5 Ca2 91.73(8) 3_666 . ? O10 Si5 Ca2 115.96(8) . . ? Ca3 Si5 Ca2 130.36(3) 3_666 . ? Ca3 Si5 Ca2 65.53(2) 2_646 . ? Ca1 Si5 Ca2 106.44(3) 4_565 . ? Ca4 Si5 Ca2 61.90(2) . . ? Ca1 Si5 Ca2 146.71(3) 3_566 . ? O9 Si6 O14 109.34(12) 4_465 3_566 ? O9 Si6 O11 116.57(12) 4_465 . ? O14 Si6 O11 117.10(12) 3_566 . ? O9 Si6 O10 101.20(12) 4_465 . ? O14 Si6 O10 109.64(11) 3_566 . ? O11 Si6 O10 101.21(11) . . ? O9 Si6 Ca2 49.33(8) 4_465 4_465 ? O14 Si6 Ca2 63.98(8) 3_566 4_465 ? O11 Si6 Ca2 157.97(8) . 4_465 ? O10 Si6 Ca2 98.62(8) . 4_465 ? O9 Si6 Ca3 108.32(9) 4_465 2_646 ? O14 Si6 Ca3 140.26(9) 3_566 2_646 ? O11 Si6 Ca3 53.13(8) . 2_646 ? O10 Si6 Ca3 50.11(8) . 2_646 ? Ca2 Si6 Ca3 141.42(3) 4_465 2_646 ? O9 Si6 Ca1 48.83(8) 4_465 4_565 ? O14 Si6 Ca1 125.54(8) 3_566 4_565 ? O11 Si6 Ca1 116.90(9) . 4_565 ? O10 Si6 Ca1 52.59(8) . 4_565 ? Ca2 Si6 Ca1 68.88(2) 4_465 4_565 ? Ca3 Si6 Ca1 73.35(3) 2_646 4_565 ? O9 Si6 Ca1 149.38(8) 4_465 . ? O14 Si6 Ca1 86.72(8) 3_566 . ? O11 Si6 Ca1 34.94(8) . . ? O10 Si6 Ca1 97.30(8) . . ? Ca2 Si6 Ca1 149.98(3) 4_465 . ? Ca3 Si6 Ca1 66.50(2) 2_646 . ? Ca1 Si6 Ca1 139.79(3) 4_565 . ? O9 Si6 Ca1 118.58(8) 4_465 3_566 ? O14 Si6 Ca1 35.43(7) 3_566 3_566 ? O11 Si6 Ca1 124.47(8) . 3_566 ? O10 Si6 Ca1 74.23(8) . 3_566 ? Ca2 Si6 Ca1 70.42(2) 4_465 3_566 ? Ca3 Si6 Ca1 112.30(3) 2_646 3_566 ? Ca1 Si6 Ca1 103.65(2) 4_565 3_566 ? Ca1 Si6 Ca1 89.80(2) . 3_566 ? O9 Si6 Ca2 87.18(8) 4_465 1_455 ? O14 Si6 Ca2 124.81(8) 3_566 1_455 ? O11 Si6 Ca2 30.83(8) . 1_455 ? O10 Si6 Ca2 118.32(8) . 1_455 ? Ca2 Si6 Ca2 128.55(3) 4_465 1_455 ? Ca3 Si6 Ca2 69.09(2) 2_646 1_455 ? Ca1 Si6 Ca2 105.29(3) 4_565 1_455 ? Ca1 Si6 Ca2 62.50(2) . 1_455 ? Ca1 Si6 Ca2 149.90(3) 3_566 1_455 ? Ca3 F7 Ca2 104.38(7) . 2_656 ? Ca3 F7 Ca4 110.19(7) . . ? Ca2 F7 Ca4 107.76(7) 2_656 . ? Ca3 F7 Ca2 105.41(7) . 4_566 ? Ca2 F7 Ca2 106.20(7) 2_656 4_566 ? Ca4 F7 Ca2 121.59(8) . 4_566 ? Ca1 F8 Ca3 114.45(8) 3_667 . ? Ca1 F8 Ca2 110.20(7) 3_667 4_566 ? Ca3 F8 Ca2 105.85(7) . 4_566 ? Ca1 F8 Ca3 110.08(7) 3_667 3_767 ? Ca3 F8 Ca3 107.75(7) . 3_767 ? Ca2 F8 Ca3 108.27(7) 4_566 3_767 ? Si6 O9 Ca4 147.14(12) 4_666 . ? Si6 O9 Ca2 99.91(11) 4_666 . ? Ca4 O9 Ca2 101.65(8) . . ? Si6 O9 Ca1 102.90(10) 4_666 1_655 ? Ca4 O9 Ca1 99.84(8) . 1_655 ? Ca2 O9 Ca1 94.42(7) . 1_655 ? Si5 O10 Si6 155.37(15) . . ? Si5 O10 Ca3 98.39(10) . 2_646 ? Si6 O10 Ca3 99.38(9) . 2_646 ? Si5 O10 Ca1 96.58(9) . 4_565 ? Si6 O10 Ca1 97.60(10) . 4_565 ? Ca3 O10 Ca1 98.28(8) 2_646 4_565 ? Si6 O11 Ca2 128.15(11) . 1_455 ? Si6 O11 Ca1 121.60(12) . . ? Ca2 O11 Ca1 103.23(7) 1_455 . ? Si6 O11 Ca3 97.11(9) . 2_646 ? Ca2 O11 Ca3 102.99(8) 1_455 2_646 ? Ca1 O11 Ca3 96.14(7) . 2_646 ? Si5 O12 Ca3 100.88(11) 3_666 . ? Si5 O12 Ca4 138.87(12) 3_666 2_656 ? Ca3 O12 Ca4 104.17(8) . 2_656 ? Si5 O12 Ca1 103.27(10) 3_666 2_656 ? Ca3 O12 Ca1 98.61(8) . 2_656 ? Ca4 O12 Ca1 104.57(8) 2_656 2_656 ? Si5 O13 Ca2 134.79(12) . . ? Si5 O13 Ca4 118.18(12) . . ? Ca2 O13 Ca4 101.85(8) . . ? Si5 O13 Ca3 97.45(10) . 2_646 ? Ca2 O13 Ca3 99.17(8) . 2_646 ? Ca4 O13 Ca3 95.01(7) . 2_646 ? Si6 O14 Ca1 121.68(11) 3_566 . ? Si6 O14 Ca4 132.49(11) 3_566 . ? Ca1 O14 Ca4 105.80(9) . . ? Si6 O14 Ca2 84.87(10) 3_566 2_656 ? Ca1 O14 Ca2 94.78(7) . 2_656 ? Ca4 O14 Ca2 93.49(7) . 2_656 ? Si5 O15 Ca1 122.21(11) 3_566 . ? Si5 O15 Ca4 133.36(12) 3_566 1_455 ? Ca1 O15 Ca4 103.97(9) . 1_455 ? Si5 O15 Ca3 84.68(10) 3_566 1_455 ? Ca1 O15 Ca3 96.74(8) . 1_455 ? Ca4 O15 Ca3 96.87(7) 1_455 1_455 ? _refine_diff_density_max 0.482 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.120