data_whiteite-(CaMgMg) _audit_creation_method SHELXL-2013 _chemical_name_mineral 'whiteite-(CaMgMg)' _chemical_compound_source 'Candelaria, Nevada' _chemical_formula_sum 'H18 Al2 Ca1.31 Mg2.69 O26 P4' _chemical_formula_weight 729.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Al' 'Al' 0.0645 0.0514 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_H-M_alt 'P 2/a' _space_group_name_Hall 'P 2/a' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, -y, z' _cell_length_a 14.8237(19) _cell_length_b 7.0302(3) _cell_length_c 9.946(3) _cell_angle_alpha 90 _cell_angle_beta 110.115(12) _cell_angle_gamma 90 _cell_volume 973.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 2.491 _exptl_crystal_F_000 741 _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 1.046 _shelx_estimated_absorpt_T_min 0.894 _shelx_estimated_absorpt_T_max 0.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _exptl_special_details ; ? ; _diffrn_radiation_probe X-ray _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Rigaku R-Axis Rapid II' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 7089 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.246 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measured_fraction_theta_full 0.963 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_Laue_measured_fraction_full 0.963 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_point_group_measured_fraction_full 0.963 _reflns_number_total 1703 _reflns_number_gt 1401 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+3.2430P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1703 _refine_ls_number_parameters 197 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.074 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca 0.2500 0.97701(17) 0.0000 0.0231(3) Uani 1 2 d S T P . . Mg1 Mg 0.2500 0.4798(2) 0.0000 0.0164(7) Uani 0.691(16) 2 d S T P . . Ca1 Ca 0.2500 0.4798(2) 0.0000 0.0164(7) Uani 0.309(16) 2 d S T P . . Mg2 Mg 0.5000 0.0000 0.5000 0.0160(4) Uani 1 2 d S . P . . Mg3 Mg 0.2500 0.4934(2) 0.5000 0.0145(4) Uani 1 2 d S T P . . Al1 Al 0.0000 0.0000 0.0000 0.0053(3) Uani 1 2 d S . P . . Al2 Al 0.0000 0.5000 0.0000 0.0047(3) Uani 1 2 d S . P . . P1 P 0.18174(7) 0.26353(14) 0.18641(11) 0.0147(3) Uani 1 1 d . . . . . P2 P 0.08028(7) 0.74723(13) 0.79971(11) 0.0134(3) Uani 1 1 d . . . . . O1 O 0.2760(2) 0.2424(4) 0.1525(3) 0.0224(7) Uani 1 1 d . . . . . O2 O 0.2026(2) 0.2956(4) 0.3442(3) 0.0228(7) Uani 1 1 d . . . . . O3 O 0.1225(2) 0.0829(4) 0.1353(3) 0.0256(7) Uani 1 1 d . . . . . O4 O 0.13406(19) 0.4375(4) 0.0905(3) 0.0219(7) Uani 1 1 d . . . . . O5 O 0.1883(2) 0.6987(5) 0.8559(3) 0.0268(7) Uani 1 1 d . . . . . O6 O 0.0465(2) 0.7779(4) 0.6400(3) 0.0197(7) Uani 1 1 d . . . . . O7 O 0.07179(19) 0.9308(4) 0.8794(3) 0.0188(6) Uani 1 1 d . . . . . O8 O 0.0234(2) 0.5850(4) 0.8345(3) 0.0278(8) Uani 1 1 d . . . . . OH9 O 0.0228(2) 0.7503(4) 0.0830(3) 0.0146(6) Uani 1 1 d D . . . . H9 H 0.001(3) 0.742(7) 0.143(4) 0.022 Uiso 1 1 d D U . . . OW10 O 0.2235(3) 0.7168(5) 0.3453(4) 0.0314(8) Uani 1 1 d D . . . . H10A H 0.167(2) 0.739(7) 0.296(5) 0.038 Uiso 1 1 d D U . . . H10B H 0.249(3) 0.709(8) 0.282(5) 0.038 Uiso 1 1 d D U . . . OW11 O 0.4525(3) 0.2106(4) 0.3456(4) 0.0334(9) Uani 1 1 d D . . . . H11A H 0.446(4) 0.301(6) 0.392(5) 0.040 Uiso 1 1 d D U . . . H11B H 0.404(3) 0.222(7) 0.271(4) 0.040 Uiso 1 1 d D U . . . OW12 O 0.6320(2) -0.0033(5) 0.4672(4) 0.0324(8) Uani 1 1 d D . . . . H12A H 0.658(4) 0.007(7) 0.551(3) 0.039 Uiso 1 1 d D U . . . H12B H 0.653(4) -0.089(6) 0.433(5) 0.039 Uiso 1 1 d D U . . . OW13 O 0.3905(2) 0.5095(4) 0.5080(4) 0.0250(7) Uani 1 1 d D . . . . H13A H 0.432(3) 0.477(6) 0.575(4) 0.030 Uiso 1 1 d D U . . . H13B H 0.408(3) 0.593(6) 0.468(4) 0.030 Uiso 1 1 d 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 Ca 0.0235(7) 0.0164(6) 0.0234(7) 0.000 0.0003(5) 0.000 Mg1 0.0241(10) 0.0125(9) 0.0152(10) 0.000 0.0100(7) 0.000 Ca1 0.0241(10) 0.0125(9) 0.0152(10) 0.000 0.0100(7) 0.000 Mg2 0.0164(10) 0.0139(9) 0.0154(10) -0.0039(7) 0.0027(8) -0.0001(7) Mg3 0.0152(9) 0.0143(9) 0.0146(10) 0.000 0.0060(8) 0.000 Al1 0.0052(7) 0.0036(7) 0.0060(8) -0.0005(5) 0.0005(6) 0.0004(5) Al2 0.0046(7) 0.0032(7) 0.0065(8) 0.0012(5) 0.0023(6) 0.0007(5) P1 0.0123(5) 0.0147(5) 0.0141(6) -0.0042(4) 0.0006(4) 0.0024(4) P2 0.0154(5) 0.0130(5) 0.0119(6) 0.0017(4) 0.0049(4) 0.0036(4) O1 0.0190(16) 0.0292(16) 0.0192(16) 0.0025(13) 0.0068(13) 0.0105(12) O2 0.0258(16) 0.0224(15) 0.0204(17) -0.0070(13) 0.0082(13) -0.0037(12) O3 0.0276(17) 0.0129(14) 0.0248(17) -0.0005(12) -0.0058(13) -0.0007(12) O4 0.0127(14) 0.0134(13) 0.0336(18) -0.0033(13) 0.0005(12) 0.0012(11) O5 0.0181(16) 0.0357(17) 0.0218(17) -0.0078(14) 0.0005(12) 0.0089(13) O6 0.0258(16) 0.0164(14) 0.0139(15) 0.0032(12) 0.0028(12) 0.0024(11) O7 0.0235(15) 0.0143(14) 0.0232(16) -0.0016(12) 0.0141(13) 0.0002(11) O8 0.050(2) 0.0141(14) 0.0272(18) -0.0032(13) 0.0239(15) -0.0051(14) OH9 0.0195(15) 0.0105(13) 0.0152(15) -0.0006(11) 0.0078(12) -0.0010(10) OW10 0.044(2) 0.0288(17) 0.0227(18) 0.0069(15) 0.0134(16) 0.0165(16) OW11 0.044(2) 0.0183(16) 0.0217(18) -0.0011(14) -0.0097(15) -0.0049(14) OW12 0.0257(19) 0.0303(19) 0.043(2) -0.0119(16) 0.0141(16) -0.0024(14) OW13 0.0183(16) 0.0255(17) 0.032(2) 0.0107(14) 0.0103(14) 0.0002(12) _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 Ca O1 2.351(3) 1_565 ? Ca O1 2.351(3) 2_565 ? Ca O5 2.412(3) 1_554 ? Ca O5 2.412(3) 2_556 ? Ca O7 2.519(3) 1_554 ? Ca O7 2.519(3) 2_556 ? Ca O3 2.772(3) 2_565 ? Ca O3 2.772(3) 1_565 ? Ca P2 3.0757(13) 1_554 ? Ca P2 3.0757(13) 2_556 ? Ca P1 3.1319(13) 1_565 ? Ca P1 3.1319(13) 2_565 ? Mg1 O5 2.087(3) 2_556 ? Mg1 O5 2.087(3) 1_554 ? Mg1 O1 2.198(3) . ? Mg1 O1 2.198(3) 2 ? Mg1 O4 2.217(3) 2 ? Mg1 O4 2.217(3) . ? Mg1 P1 2.8396(14) 2 ? Mg1 P1 2.8396(14) . ? Mg1 Ca 3.5347(19) 1_545 ? Mg2 O6 2.048(3) 4_665 ? Mg2 O6 2.048(3) 2_546 ? Mg2 OW11 2.074(3) 3_656 ? Mg2 OW11 2.074(3) . ? Mg2 OW12 2.091(3) 3_656 ? Mg2 OW12 2.091(3) . ? Mg2 H11A 2.39(5) . ? Mg2 H12A 2.22(5) . ? Mg3 O2 2.020(3) . ? Mg3 O2 2.020(3) 2_556 ? Mg3 OW13 2.059(3) 2_556 ? Mg3 OW13 2.059(3) . ? Mg3 OW10 2.139(3) 2_556 ? Mg3 OW10 2.139(3) . ? Al1 OH9 1.920(3) 3_565 ? Al1 OH9 1.920(3) 1_545 ? Al1 O7 1.920(3) 3_566 ? Al1 O7 1.920(3) 1_544 ? Al1 O3 1.941(3) 3 ? Al1 O3 1.941(3) . ? Al1 Ca 3.7094(5) 3_565 ? Al1 Ca 3.7094(5) 1_545 ? Al2 O8 1.892(3) 3_566 ? Al2 O8 1.892(3) 1_554 ? Al2 OH9 1.924(3) . ? Al2 OH9 1.924(3) 3_565 ? Al2 O4 1.929(3) . ? Al2 O4 1.929(3) 3_565 ? Al2 Ca1 3.7086(5) 3_565 ? P1 O2 1.508(3) . ? P1 O3 1.528(3) . ? P1 O1 1.553(3) . ? P1 O4 1.563(3) . ? P1 Ca 3.1319(13) 1_545 ? P2 O6 1.508(3) . ? P2 O8 1.527(3) . ? P2 O7 1.542(3) . ? P2 O5 1.542(3) . ? P2 Ca 3.0758(13) 1_556 ? P2 Ca1 3.2226(14) 1_556 ? O1 Ca 2.351(3) 1_545 ? O3 Ca 2.772(3) 1_545 ? O5 Ca1 2.087(3) 1_556 ? O5 Mg1 2.087(3) 1_556 ? O5 Ca 2.412(3) 1_556 ? O6 Mg2 2.048(3) 2_566 ? O7 Al1 1.920(3) 1_566 ? O7 Ca 2.519(3) 1_556 ? O8 Al2 1.892(3) 1_556 ? OH9 Al1 1.920(3) 1_565 ? OH9 H9 0.77(3) . ? OW10 H10A 0.82(3) . ? OW10 H10B 0.84(3) . ? OW11 H11A 0.81(3) . ? OW11 H11B 0.84(3) . ? OW12 H12A 0.79(3) . ? OW12 H12B 0.80(3) . ? OW13 H13A 0.77(3) . ? OW13 H13B 0.80(3) . ? 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 O1 Ca O1 74.97(15) 1_565 2_565 ? O1 Ca O5 166.32(10) 1_565 1_554 ? O1 Ca O5 108.41(10) 2_565 1_554 ? O1 Ca O5 108.41(10) 1_565 2_556 ? O1 Ca O5 166.32(10) 2_565 2_556 ? O5 Ca O5 71.56(15) 1_554 2_556 ? O1 Ca O7 108.79(10) 1_565 1_554 ? O1 Ca O7 83.26(9) 2_565 1_554 ? O5 Ca O7 59.41(9) 1_554 1_554 ? O5 Ca O7 107.44(10) 2_556 1_554 ? O1 Ca O7 83.26(9) 1_565 2_556 ? O1 Ca O7 108.79(10) 2_565 2_556 ? O5 Ca O7 107.44(10) 1_554 2_556 ? O5 Ca O7 59.41(9) 2_556 2_556 ? O7 Ca O7 165.18(13) 1_554 2_556 ? O1 Ca O3 96.44(10) 1_565 2_565 ? O1 Ca O3 57.43(9) 2_565 2_565 ? O5 Ca O3 96.43(10) 1_554 2_565 ? O5 Ca O3 108.90(10) 2_556 2_565 ? O7 Ca O3 125.58(9) 1_554 2_565 ? O7 Ca O3 59.17(9) 2_556 2_565 ? O1 Ca O3 57.43(9) 1_565 1_565 ? O1 Ca O3 96.44(10) 2_565 1_565 ? O5 Ca O3 108.90(10) 1_554 1_565 ? O5 Ca O3 96.42(10) 2_556 1_565 ? O7 Ca O3 59.17(8) 1_554 1_565 ? O7 Ca O3 125.58(9) 2_556 1_565 ? O3 Ca O3 148.84(12) 2_565 1_565 ? O1 Ca P2 138.65(7) 1_565 1_554 ? O1 Ca P2 94.75(7) 2_565 1_554 ? O5 Ca P2 29.61(7) 1_554 1_554 ? O5 Ca P2 90.99(8) 2_556 1_554 ? O7 Ca P2 29.94(6) 1_554 1_554 ? O7 Ca P2 136.98(8) 2_556 1_554 ? O3 Ca P2 111.65(6) 2_565 1_554 ? O3 Ca P2 85.02(6) 1_565 1_554 ? O1 Ca P2 94.75(7) 1_565 2_556 ? O1 Ca P2 138.65(7) 2_565 2_556 ? O5 Ca P2 90.99(8) 1_554 2_556 ? O5 Ca P2 29.61(7) 2_556 2_556 ? O7 Ca P2 136.98(8) 1_554 2_556 ? O7 Ca P2 29.94(6) 2_556 2_556 ? O3 Ca P2 85.02(6) 2_565 2_556 ? O3 Ca P2 111.65(6) 1_565 2_556 ? P2 Ca P2 116.63(5) 1_554 2_556 ? O1 Ca P1 28.65(7) 1_565 1_565 ? O1 Ca P1 81.77(8) 2_565 1_565 ? O5 Ca P1 137.72(8) 1_554 1_565 ? O5 Ca P1 107.68(8) 2_556 1_565 ? O7 Ca P1 82.27(7) 1_554 1_565 ? O7 Ca P1 107.48(7) 2_556 1_565 ? O3 Ca P1 121.84(7) 2_565 1_565 ? O3 Ca P1 29.19(6) 1_565 1_565 ? P2 Ca P1 111.25(3) 1_554 1_565 ? P2 Ca P1 108.25(3) 2_556 1_565 ? O1 Ca P1 81.77(8) 1_565 2_565 ? O1 Ca P1 28.65(7) 2_565 2_565 ? O5 Ca P1 107.68(8) 1_554 2_565 ? O5 Ca P1 137.72(8) 2_556 2_565 ? O7 Ca P1 107.48(7) 1_554 2_565 ? O7 Ca P1 82.27(7) 2_556 2_565 ? O3 Ca P1 29.19(6) 2_565 2_565 ? O3 Ca P1 121.84(7) 1_565 2_565 ? P2 Ca P1 108.25(3) 1_554 2_565 ? P2 Ca P1 111.25(3) 2_556 2_565 ? P1 Ca P1 99.95(5) 1_565 2_565 ? O5 Mg1 O5 84.99(17) 2_556 1_554 ? O5 Mg1 O1 98.91(11) 2_556 . ? O5 Mg1 O1 164.78(11) 1_554 . ? O5 Mg1 O1 164.78(11) 2_556 2 ? O5 Mg1 O1 98.91(11) 1_554 2 ? O1 Mg1 O1 81.20(16) . 2 ? O5 Mg1 O4 99.20(12) 2_556 2 ? O5 Mg1 O4 92.18(11) 1_554 2 ? O1 Mg1 O4 101.63(11) . 2 ? O1 Mg1 O4 66.08(11) 2 2 ? O5 Mg1 O4 92.18(11) 2_556 . ? O5 Mg1 O4 99.20(12) 1_554 . ? O1 Mg1 O4 66.08(11) . . ? O1 Mg1 O4 101.63(11) 2 . ? O4 Mg1 O4 164.58(16) 2 . ? O5 Mg1 P1 132.28(9) 2_556 2 ? O5 Mg1 P1 96.71(9) 1_554 2 ? O1 Mg1 P1 91.52(9) . 2 ? O1 Mg1 P1 32.89(8) 2 2 ? O4 Mg1 P1 33.19(7) 2 2 ? O4 Mg1 P1 133.88(9) . 2 ? O5 Mg1 P1 96.71(9) 2_556 . ? O5 Mg1 P1 132.28(9) 1_554 . ? O1 Mg1 P1 32.89(8) . . ? O1 Mg1 P1 91.52(9) 2 . ? O4 Mg1 P1 133.88(9) 2 . ? O4 Mg1 P1 33.19(7) . . ? P1 Mg1 P1 115.25(6) 2 . ? O5 Mg1 Ca 42.49(9) 2_556 . ? O5 Mg1 Ca 42.49(9) 1_554 . ? O1 Mg1 Ca 139.40(8) . . ? O1 Mg1 Ca 139.40(8) 2 . ? O4 Mg1 Ca 97.71(8) 2 . ? O4 Mg1 Ca 97.71(8) . . ? P1 Mg1 Ca 122.37(3) 2 . ? P1 Mg1 Ca 122.37(3) . . ? O5 Mg1 Ca 137.51(9) 2_556 1_545 ? O5 Mg1 Ca 137.51(9) 1_554 1_545 ? O1 Mg1 Ca 40.60(8) . 1_545 ? O1 Mg1 Ca 40.60(8) 2 1_545 ? O4 Mg1 Ca 82.29(8) 2 1_545 ? O4 Mg1 Ca 82.29(8) . 1_545 ? P1 Mg1 Ca 57.63(3) 2 1_545 ? P1 Mg1 Ca 57.63(3) . 1_545 ? Ca Mg1 Ca 180.0 . 1_545 ? O6 Mg2 O6 180.0 4_665 2_546 ? O6 Mg2 OW11 95.26(12) 4_665 3_656 ? O6 Mg2 OW11 84.74(12) 2_546 3_656 ? O6 Mg2 OW11 84.74(12) 4_665 . ? O6 Mg2 OW11 95.26(12) 2_546 . ? OW11 Mg2 OW11 180.0 3_656 . ? O6 Mg2 OW12 89.99(13) 4_665 3_656 ? O6 Mg2 OW12 90.01(13) 2_546 3_656 ? OW11 Mg2 OW12 89.43(15) 3_656 3_656 ? OW11 Mg2 OW12 90.57(15) . 3_656 ? O6 Mg2 OW12 90.01(13) 4_665 . ? O6 Mg2 OW12 89.99(13) 2_546 . ? OW11 Mg2 OW12 90.57(15) 3_656 . ? OW11 Mg2 OW12 89.43(15) . . ? OW12 Mg2 OW12 180.0 3_656 . ? O6 Mg2 H11A 67.1(8) 4_665 . ? O6 Mg2 H11A 112.9(8) 2_546 . ? OW11 Mg2 H11A 160.6(8) 3_656 . ? OW11 Mg2 H11A 19.4(8) . . ? OW12 Mg2 H11A 82.8(13) 3_656 . ? OW12 Mg2 H11A 97.2(13) . . ? O6 Mg2 H12A 75.3(10) 4_665 . ? O6 Mg2 H12A 104.7(10) 2_546 . ? OW11 Mg2 H12A 77.5(12) 3_656 . ? OW11 Mg2 H12A 102.5(12) . . ? OW12 Mg2 H12A 159.1(8) 3_656 . ? OW12 Mg2 H12A 20.9(8) . . ? H11A Mg2 H12A 104.3(18) . . ? O2 Mg3 O2 92.98(19) . 2_556 ? O2 Mg3 OW13 85.89(12) . 2_556 ? O2 Mg3 OW13 98.48(13) 2_556 2_556 ? O2 Mg3 OW13 98.48(13) . . ? O2 Mg3 OW13 85.89(12) 2_556 . ? OW13 Mg3 OW13 173.7(2) 2_556 . ? O2 Mg3 OW10 170.77(13) . 2_556 ? O2 Mg3 OW10 91.39(13) 2_556 2_556 ? OW13 Mg3 OW10 85.43(14) 2_556 2_556 ? OW13 Mg3 OW10 89.93(14) . 2_556 ? O2 Mg3 OW10 91.39(13) . . ? O2 Mg3 OW10 170.77(13) 2_556 . ? OW13 Mg3 OW10 89.93(14) 2_556 . ? OW13 Mg3 OW10 85.43(14) . . ? OW10 Mg3 OW10 85.47(19) 2_556 . ? OH9 Al1 OH9 180.00(18) 3_565 1_545 ? OH9 Al1 O7 89.07(12) 3_565 3_566 ? OH9 Al1 O7 90.93(12) 1_545 3_566 ? OH9 Al1 O7 90.93(12) 3_565 1_544 ? OH9 Al1 O7 89.07(12) 1_545 1_544 ? O7 Al1 O7 180.00(12) 3_566 1_544 ? OH9 Al1 O3 89.54(12) 3_565 3 ? OH9 Al1 O3 90.46(12) 1_545 3 ? O7 Al1 O3 85.50(13) 3_566 3 ? O7 Al1 O3 94.50(13) 1_544 3 ? OH9 Al1 O3 90.46(12) 3_565 . ? OH9 Al1 O3 89.54(12) 1_545 . ? O7 Al1 O3 94.50(13) 3_566 . ? O7 Al1 O3 85.50(13) 1_544 . ? O3 Al1 O3 180.0 3 . ? OH9 Al1 Ca 86.10(9) 3_565 3_565 ? OH9 Al1 Ca 93.90(9) 1_545 3_565 ? O7 Al1 Ca 38.79(8) 3_566 3_565 ? O7 Al1 Ca 141.21(8) 1_544 3_565 ? O3 Al1 Ca 46.87(10) 3 3_565 ? O3 Al1 Ca 133.13(10) . 3_565 ? OH9 Al1 Ca 93.90(9) 3_565 1_545 ? OH9 Al1 Ca 86.10(9) 1_545 1_545 ? O7 Al1 Ca 141.21(8) 3_566 1_545 ? O7 Al1 Ca 38.79(8) 1_544 1_545 ? O3 Al1 Ca 133.13(10) 3 1_545 ? O3 Al1 Ca 46.87(10) . 1_545 ? Ca Al1 Ca 180.0 3_565 1_545 ? O8 Al2 O8 180.00(16) 3_566 1_554 ? O8 Al2 OH9 88.47(12) 3_566 . ? O8 Al2 OH9 91.53(12) 1_554 . ? O8 Al2 OH9 91.53(12) 3_566 3_565 ? O8 Al2 OH9 88.47(12) 1_554 3_565 ? OH9 Al2 OH9 180.00(17) . 3_565 ? O8 Al2 O4 89.43(14) 3_566 . ? O8 Al2 O4 90.57(14) 1_554 . ? OH9 Al2 O4 90.43(12) . . ? OH9 Al2 O4 89.58(12) 3_565 . ? O8 Al2 O4 90.57(14) 3_566 3_565 ? O8 Al2 O4 89.43(14) 1_554 3_565 ? OH9 Al2 O4 89.57(12) . 3_565 ? OH9 Al2 O4 90.42(12) 3_565 3_565 ? O4 Al2 O4 180.0 . 3_565 ? O8 Al2 Ca1 61.96(10) 3_566 3_565 ? O8 Al2 Ca1 118.04(10) 1_554 3_565 ? OH9 Al2 Ca1 89.60(9) . 3_565 ? OH9 Al2 Ca1 90.40(9) 3_565 3_565 ? O4 Al2 Ca1 151.37(9) . 3_565 ? O4 Al2 Ca1 28.63(9) 3_565 3_565 ? O2 P1 O3 111.06(18) . . ? O2 P1 O1 111.23(17) . . ? O3 P1 O1 107.73(17) . . ? O2 P1 O4 113.98(17) . . ? O3 P1 O4 111.09(16) . . ? O1 P1 O4 101.19(16) . . ? O2 P1 Mg1 127.42(12) . . ? O3 P1 Mg1 121.36(14) . . ? O1 P1 Mg1 50.23(11) . . ? O4 P1 Mg1 50.96(11) . . ? O2 P1 Ca 136.00(13) . 1_545 ? O3 P1 Ca 62.21(13) . 1_545 ? O1 P1 Ca 46.52(11) . 1_545 ? O4 P1 Ca 108.19(12) . 1_545 ? Mg1 P1 Ca 72.40(4) . 1_545 ? O6 P2 O8 109.66(17) . . ? O6 P2 O7 111.45(16) . . ? O8 P2 O7 111.08(16) . . ? O6 P2 O5 109.91(18) . . ? O8 P2 O5 109.77(19) . . ? O7 P2 O5 104.89(16) . . ? O6 P2 Ca 120.56(12) . 1_556 ? O8 P2 Ca 129.63(13) . 1_556 ? O7 P2 Ca 54.61(11) . 1_556 ? O5 P2 Ca 50.59(12) . 1_556 ? O6 P2 Ca1 129.81(12) . 1_556 ? O8 P2 Ca1 78.39(13) . 1_556 ? O7 P2 Ca1 110.80(12) . 1_556 ? O5 P2 Ca1 32.24(13) . 1_556 ? Ca P2 Ca1 67.37(4) 1_556 1_556 ? P1 O1 Mg1 96.88(13) . . ? P1 O1 Ca 104.83(15) . 1_545 ? Mg1 O1 Ca 101.92(12) . 1_545 ? P1 O2 Mg3 142.54(19) . . ? P1 O3 Al1 140.68(18) . . ? P1 O3 Ca 88.60(15) . 1_545 ? Al1 O3 Ca 102.39(12) . 1_545 ? P1 O4 Al2 129.80(17) . . ? P1 O4 Mg1 95.85(14) . . ? Al2 O4 Mg1 126.73(15) . . ? P2 O5 Ca1 124.5(2) . 1_556 ? P2 O5 Mg1 124.5(2) . 1_556 ? Ca1 O5 Mg1 0.00(5) 1_556 1_556 ? P2 O5 Ca 99.81(15) . 1_556 ? Ca1 O5 Ca 101.73(12) 1_556 1_556 ? Mg1 O5 Ca 101.73(12) 1_556 1_556 ? P2 O6 Mg2 137.52(17) . 2_566 ? P2 O7 Al1 133.93(17) . 1_566 ? P2 O7 Ca 95.46(13) . 1_556 ? Al1 O7 Ca 112.68(12) 1_566 1_556 ? P2 O8 Al2 135.55(19) . 1_556 ? Al1 OH9 Al2 132.28(16) 1_565 . ? Al1 OH9 H9 110(4) 1_565 . ? Al2 OH9 H9 101(4) . . ? Mg3 OW10 H10A 118(4) . . ? Mg3 OW10 H10B 118(4) . . ? H10A OW10 H10B 101(4) . . ? Mg2 OW11 H11A 103(4) . . ? Mg2 OW11 H11B 134(4) . . ? H11A OW11 H11B 101(4) . . ? Mg2 OW12 H12A 89(4) . . ? Mg2 OW12 H12B 126(4) . . ? H12A OW12 H12B 113(4) . . ? Mg3 OW13 H13A 121(4) . . ? Mg3 OW13 H13B 121(3) . . ? H13A OW13 H13B 110(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A OH9 H9 OW11 0.77(3) 2.39(3) 3.139(5) 166(5) 4_565 OW10 H10A OH9 0.82(3) 2.44(4) 3.221(4) 158(5) . OW10 H10B O5 0.84(3) 1.90(3) 2.744(5) 177(5) 2_556 OW11 H11A OW13 0.81(3) 2.19(3) 2.982(5) 164(5) . OW11 H11B O1 0.84(3) 1.86(3) 2.670(4) 160(6) . OW12 H12A OW10 0.79(3) 2.58(5) 3.062(5) 120(5) 3_666 OW12 H12B O2 0.80(3) 1.97(3) 2.774(5) 178(5) 4_655 OW13 H13A O6 0.77(3) 2.39(4) 3.012(4) 137(5) 4_665 OW13 H13A O8 0.77(3) 2.50(3) 3.236(5) 158(5) 4_665 OW13 H13B O6 0.80(3) 1.95(3) 2.746(4) 174(5) 2_556 _refine_diff_density_max 0.718 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.117 _shelxl_version_number 2013-4 _shelx_res_file ; TITL whiteite-(CaMgMg) REM transformed to space group : P2/a:b3 CELL 0.71075 14.8237 7.0302 9.9460 90.000 110.115 90.000 ZERR 2 0.0019 0.0003 0.0025 0.000 0.012 0.000 LATT 1 SYMM 1/2-X,+Y,-Z SFAC AL CA H MG O P UNIT 4 2.62 36 5.38 52 8 L.S. 8 omit -3 1 5 omit -11 3 3 omit -1 2 10 omit 11 3 0 omit -2 3 1 omit 0 2 1 omit -2 0 4 omit -6 0 4 omit 0 2 2 omit 2 2 0 omit -8 0 2 omit 0 0 4 omit -2 2 1 EQIV $1 x-1/2, -y+1, z EQIV $2 -x+1/2, y, -z+1 EQIV $3 -x+1, -y+1, -z+1 EQIV $4 x+1/2, -y, z EQIV $5 x+1/2, -y+1, z HTAB OH9 OW11_$1 HTAB OW10 OH9 HTAB OW10 O5_$2 HTAB OW11 OW13 HTAB OW11 O1 HTAB OW12 OW10_$3 HTAB OW12 O2_$4 HTAB OW13 O6_$5 HTAB OW13 O8_$5 HTAB OW13 O6_$2 EXYZ MG1 CA1 EADP MG1 CA1 FMAP 2 PLAN 8 HTAB BOND $H ACTA DFIX 0.82 0.03 OH9 H9 OW10 H10a OW10 H10b OW11 H11a OW11 H11b DFIX 0.82 0.03 OW12 H12a OW12 H12b OW13 H13a OW13 H13b DFIX 1.30 0.03 H10a H10b H11a H11b H12a H12b H13a H13b SIZE 0.110 0.060 0.010 WGHT 0.050400 3.243000 FVAR 0.45527 0.69090 CA 2 0.250000 0.977012 0.000000 10.50000 0.02348 0.01636 = 0.02339 0.00000 0.00028 0.00000 MG1 4 0.250000 0.479806 0.000000 20.50000 0.02413 0.01246 = 0.01523 0.00000 0.00998 0.00000 CA1 2 0.250000 0.479806 0.000000 -20.50000 0.02413 0.01246 = 0.01523 0.00000 0.00998 0.00000 MG2 4 0.500000 0.000000 0.500000 10.50000 0.01642 0.01392 = 0.01542 -0.00394 0.00268 -0.00009 MG3 4 0.250000 0.493405 0.500000 10.50000 0.01516 0.01429 = 0.01457 0.00000 0.00596 0.00000 AL1 1 0.000000 0.000000 0.000000 10.50000 0.00520 0.00356 = 0.00603 -0.00048 0.00052 0.00043 AL2 1 0.000000 0.500000 0.000000 10.50000 0.00464 0.00319 = 0.00646 0.00116 0.00226 0.00072 P1 6 0.181738 0.263531 0.186407 11.00000 0.01233 0.01470 = 0.01408 -0.00416 0.00063 0.00241 P2 6 0.080281 0.747230 0.799712 11.00000 0.01536 0.01297 = 0.01195 0.00166 0.00492 0.00359 O1 5 0.275999 0.242368 0.152486 11.00000 0.01903 0.02919 = 0.01917 0.00255 0.00675 0.01046 O2 5 0.202622 0.295556 0.344173 11.00000 0.02578 0.02243 = 0.02036 -0.00695 0.00824 -0.00368 O3 5 0.122545 0.082896 0.135261 11.00000 0.02757 0.01294 = 0.02479 -0.00050 -0.00580 -0.00070 O4 5 0.134061 0.437489 0.090472 11.00000 0.01271 0.01338 = 0.03363 -0.00332 0.00049 0.00120 O5 5 0.188326 0.698729 0.855933 11.00000 0.01805 0.03571 = 0.02182 -0.00783 0.00054 0.00894 O6 5 0.046537 0.777851 0.640014 11.00000 0.02575 0.01637 = 0.01393 0.00323 0.00278 0.00245 O7 5 0.071787 0.930808 0.879360 11.00000 0.02349 0.01430 = 0.02325 -0.00158 0.01411 0.00019 O8 5 0.023410 0.585008 0.834517 11.00000 0.05037 0.01415 = 0.02718 -0.00320 0.02393 -0.00509 OH9 5 0.022801 0.750320 0.083029 11.00000 0.01949 0.01045 = 0.01515 -0.00064 0.00780 -0.00099 H9 3 0.001000 0.741553 0.142686 11.00000 -1.50000 OW10 5 0.223496 0.716830 0.345293 11.00000 0.04405 0.02885 = 0.02275 0.00689 0.01336 0.01654 H10A 3 0.167194 0.738995 0.295983 11.00000 -1.20000 H10B 3 0.248782 0.709272 0.281585 11.00000 -1.20000 OW11 5 0.452495 0.210625 0.345593 11.00000 0.04382 0.01832 = 0.02166 -0.00109 -0.00971 -0.00491 H11A 3 0.446120 0.301493 0.391941 11.00000 -1.20000 H11B 3 0.404023 0.222118 0.270935 11.00000 -1.20000 OW12 5 0.631984 -0.003303 0.467178 11.00000 0.02573 0.03031 = 0.04280 -0.01187 0.01405 -0.00236 H12A 3 0.658095 0.006716 0.550886 11.00000 -1.20000 H12B 3 0.652978 -0.088703 0.433282 11.00000 -1.20000 OW13 5 0.390451 0.509516 0.507953 11.00000 0.01832 0.02551 = 0.03236 0.01070 0.01027 0.00020 H13A 3 0.432489 0.477012 0.575083 11.00000 -1.20000 H13B 3 0.408092 0.593267 0.468433 11.00000 -1.20000 HKLF 4 REM whiteite-(CaMgMg) REM R1 = 0.0436 for 1401 Fo > 4sig(Fo) and 0.0555 for all 1703 data REM 197 parameters refined using 13 restraints END WGHT 0.0504 3.2424 REM Instructions for potential hydrogen bonds HTAB OH9 OW11_$1 HTAB OW10 OH9 HTAB OW10 O5_$2 HTAB OW11 O1 HTAB OW12 O2_$4 HTAB OW13 O6_$5 HTAB OW13 O8_$5 HTAB OW13 O6_$2 HTAB OW13 OW11_$3 REM Highest difference peak 0.718, deepest hole -0.502, 1-sigma level 0.117 Q1 1 0.2116 0.7769 0.8203 11.00000 0.05 0.72 Q2 1 0.0851 0.5846 0.8821 11.00000 0.05 0.59 Q3 1 0.3182 0.4989 0.5021 11.00000 0.05 0.53 Q4 1 0.5714 -0.0063 0.4939 11.00000 0.05 0.50 Q5 1 0.0747 0.7313 0.2833 11.00000 0.05 0.43 Q6 1 0.2495 0.0086 0.2569 11.00000 0.05 0.39 Q7 1 0.0808 0.0673 0.1818 11.00000 0.05 0.38 Q8 1 0.2414 0.5039 0.2432 11.00000 0.05 0.37 ; _shelx_res_checksum 83403 _shelx_hkl_file ; -1 0 -1 -1.51 1.46 1 0 1 -0.13 0.90 1 -1 0 142.03 3.58 1 1 0 146.08 3.18 -1 -1 0 145.36 3.11 -1 1 0 145.67 3.58 1 -1 0 147.06 3.26 1 -1 -1 880.77 18.62 -1 1 1 861.74 16.27 1 1 -1 869.97 15.71 -1 -1 1 863.18 15.52 1 1 -1 872.22 13.67 -1 -1 1 871.38 13.79 0 -1 -1 10.32 1.54 0 -1 1 9.97 1.51 0 1 -1 8.93 1.66 0 1 1 10.12 1.59 0 -1 1 10.25 1.21 1 0 -2 2.25 1.45 2 -1 0 432.14 8.06 2 1 0 433.81 5.80 2 1 0 439.32 7.02 -2 -1 0 437.52 7.14 -2 -1 0 420.85 5.60 -2 1 0 436.34 8.23 2 -1 0 428.62 8.80 -2 1 1 514.96 10.03 2 1 -1 551.12 9.54 -2 -1 1 506.90 8.94 2 -1 -1 509.60 9.89 -3 0 1 0.47 0.50 -1 -1 -1 1788.76 32.83 1 -1 1 1799.94 35.78 1 1 1 1799.94 37.30 -1 1 -1 1837.64 36.52 1 -1 1 1785.41 35.47 -1 1 -1 1778.86 35.37 -1 -1 -1 1722.07 36.09 1 1 1 1817.13 33.24 2 0 1 19.96 1.95 -2 0 -1 20.33 3.11 0 0 -2 1388.18 28.21 0 0 2 1386.78 28.14 3 0 0 1.40 1.01 3 0 0 0.16 0.30 -3 0 2 -0.09 0.96 -1 -1 2 933.86 18.27 1 1 -2 916.03 18.01 -1 1 2 911.29 19.21 1 -1 -2 907.21 19.09 -1 0 -2 0.20 1.44 1 0 2 1.36 1.43 -3 1 1 170.69 4.30 -3 -1 1 171.46 3.42 3 -1 -1 179.65 5.96 -2 -1 -1 224.19 4.60 -2 -1 -1 219.49 4.66 2 1 1 216.09 4.70 2 -1 1 218.45 6.02 2 -1 1 227.76 5.26 -2 1 -1 219.97 5.51 -2 1 -1 219.76 6.15 2 1 1 222.57 5.28 2 -1 -2 86.58 3.77 2 -1 -2 83.62 5.73 -2 1 2 72.68 3.70 2 1 -2 78.95 2.92 0 1 2 30.09 3.92 0 -1 -2 24.58 2.28 0 1 -2 25.56 2.40 0 -1 2 26.49 2.43 0 -1 -2 22.18 2.42 3 1 0 1183.71 19.50 -3 -1 0 1174.07 19.37 3 1 0 1214.62 22.19 -3 1 0 1192.32 22.13 3 -1 0 1208.86 25.28 3 -1 0 1173.17 21.88 -4 0 1 1026.57 16.15 -3 0 -1 1.98 1.31 3 0 1 -1.57 1.31 -3 1 2 2062.72 44.40 3 -1 -2 2074.86 44.84 0 2 0 70.43 3.74 0 -2 0 70.85 3.76 0 -2 0 64.94 1.86 1 1 2 278.83 6.83 1 1 2 283.86 7.16 -1 -1 -2 275.26 6.94 -1 -1 -2 289.92 7.01 1 -1 2 281.28 7.41 -1 1 -2 298.40 10.25 4 0 0 3068.75 55.03 4 0 0 2847.15 69.32 1 2 0 6.93 1.91 1 -2 0 7.37 2.13 -1 2 0 8.22 2.15 1 -2 0 5.15 1.39 -1 -2 0 6.39 0.63 -1 -2 0 6.29 1.90 -4 0 2 2539.17 52.93 2 0 2 53.19 3.49 -2 0 -2 75.58 3.85 1 2 -1 0.20 0.60 -1 -2 1 1.12 1.55 -1 2 1 -3.23 2.64 1 2 -1 -0.88 1.47 1 -2 -1 2.27 1.63 -1 -2 1 0.67 0.99 0 2 -1 100.67 4.57 0 2 -1 102.30 2.90 0 -2 1 99.95 4.69 0 -2 -1 98.07 6.76 0 2 1 98.69 4.64 0 -2 1 106.03 3.00 1 0 -3 0.90 1.78 -4 -1 1 1.17 0.60 4 -1 -1 -4.57 1.55 -4 1 1 -0.58 1.56 -3 -1 -1 1911.88 38.93 3 1 1 1925.20 38.47 -3 1 -1 1959.48 44.12 -3 -1 -1 1835.02 35.64 3 1 1 1928.50 37.20 3 -1 1 1921.02 39.22 3 -1 1 1901.55 42.49 -2 -2 0 283.77 9.14 -2 2 0 299.02 7.95 2 -2 0 294.63 7.17 2 -2 0 299.50 7.99 2 2 0 262.81 6.76 -2 -2 1 444.86 10.15 2 -2 -1 428.76 10.80 2 2 -1 443.76 6.50 2 2 -1 437.78 9.89 -2 2 1 429.04 10.68 4 1 0 53.77 2.36 4 -1 0 50.93 3.89 4 1 0 57.03 1.82 -4 1 0 54.58 2.31 4 -1 0 56.67 3.42 -4 -1 0 59.27 1.35 -1 -2 -1 147.70 5.17 -1 2 -1 155.26 4.64 1 -2 1 143.49 5.51 -1 2 -1 156.58 5.62 1 -2 1 143.48 6.03 1 2 1 153.82 5.37 -1 -2 -1 154.04 2.98 0 0 3 1452.25 36.89 0 0 -3 1469.77 33.52 -4 1 2 102.02 3.78 4 -1 -2 100.89 3.85 -2 -1 -2 128.91 4.34 -2 -1 -2 128.98 4.52 -2 1 -2 142.26 5.41 2 1 2 139.91 4.59 2 1 2 136.69 4.49 2 -1 2 135.71 7.71 2 1 -3 128.92 4.74 -2 1 3 120.95 5.23 2 -1 -3 113.56 5.26 -1 1 3 6.69 2.35 1 -1 -3 6.38 2.35 1 -1 -3 4.24 2.20 1 1 -3 6.63 3.41 -1 -1 3 8.39 3.37 -5 0 1 -0.13 0.51 4 0 110075.85 305.62 -4 0 -1 8897.34 276.28 -1 2 2 72.04 4.50 -1 -2 2 71.49 6.35 1 2 -2 69.68 4.11 1 2 -2 73.23 2.87 1 -2 -2 84.38 6.83 -1 -2 2 74.74 2.92 -5 0 2 0.52 0.84 -3 1 3 1746.35 40.24 3 -1 -3 1846.33 42.16 3 1 -3 1824.87 39.88 -4 0 3 5302.92 139.50 -3 2 1 4.84 3.28 3 2 -1 6.82 1.61 3 -2 -1 8.62 3.35 3 2 -1 5.60 0.45 -3 -2 1 6.92 2.73 0 -1 -3 20.61 2.86 0 1 -3 21.99 4.62 0 -1 3 19.48 4.71 0 -1 -3 23.81 2.80 0 1 3 21.22 2.97 2 2 1 168.15 5.39 -2 2 -1 169.72 5.98 -2 -2 -1 175.28 5.40 -2 2 -1 153.73 5.40 -2 -2 -1 175.22 3.36 2 -2 1 178.02 8.19 2 -2 1 175.41 5.60 -3 0 -2 0.05 1.69 3 0 2 1.28 1.63 1 0 3 -0.45 2.07 -1 0 -3 -2.85 2.07 -2 -2 2 232.49 9.14 -2 -2 2 218.67 6.41 2 2 -2 226.26 4.95 -2 2 2 231.52 7.49 2 -2 -2 224.51 7.35 0 2 -220157.78 764.83 0 2 220063.08 760.45 0 -2 -220164.78 766.68 0 -2 220287.82 775.62 0 2 -220241.01 752.78 0 -2 220396.16 759.78 3 2 0 36.42 1.03 -3 2 0 33.64 3.05 3 -2 0 43.70 2.98 3 -2 0 28.04 3.07 -3 -2 0 40.04 2.49 3 2 0 37.34 2.37 5 0 0 0.37 0.38 5 0 0 2.83 1.56 -5 -1 1 98.98 1.82 5 -1 -1 94.75 4.16 -5 1 1 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131.15 12.25 -5 -4 8 40.29 8.10 5 4 -8 28.73 9.98 5 -4 -8 23.19 7.73 5 -4 -8 30.75 9.58 -5 4 8 49.18 8.95 -3 4 8 191.71 16.20 3 4 -8 203.55 13.57 -3 -4 8 185.27 15.12 3 -4 -8 197.89 15.80 3 -4 -8 200.47 19.91 4 -6 3 220.58 12.46 -4 -6 -3 188.38 6.44 -4 -6 -3 217.98 14.26 4 6 3 247.18 13.76 -4 6 -3 256.76 16.12 4 -6 3 219.83 15.51 -12 4 3 -2.97 3.41 12 -4 -3 8.26 5.50 -12 -4 3 0.45 1.99 12 -4 -3 7.11 5.17 12 4 -3 1.56 2.97 14 2 -4 286.51 13.95 -14 2 4 269.14 9.72 -14 0 6 67.45 5.25 -2 -4 -7 154.15 11.89 2 4 7 164.52 13.32 2 -4 7 178.01 13.39 2 -4 7 174.30 13.72 -2 4 -7 143.69 13.78 10 -5 -1 62.09 12.71 10 -5 -1 81.74 15.15 10 5 -1 52.96 8.56 -10 -5 1 74.24 6.24 -10 5 1 74.99 8.31 -4 -5 -5 0.50 4.12 4 5 5 0.76 6.29 4 -5 5 -3.06 4.10 -4 5 -5 -4.77 6.51 4 -5 5 -1.13 4.45 -4 -5 -5 1.67 4.01 -7 -6 0 15.16 7.68 7 -6 0 13.43 6.09 7 6 0 4.27 7.48 7 -6 0 12.13 5.60 -7 6 0 6.33 6.01 1 0 9 -3.99 8.46 -1 0 -9 -2.64 5.78 3 -6 -5 213.77 16.60 3 6 -5 214.17 9.71 -3 -6 5 221.32 15.27 -3 6 5 230.30 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272.32 10.77 14 3 -1 267.41 17.32 -15 -2 5 46.82 1.92 -15 -2 5 45.28 2.58 -15 2 5 62.24 5.22 10 0 -10 190.78 16.51 -10 0 10 215.05 16.25 -8 6 5 378.01 21.35 -8 -6 5 350.81 25.61 8 -6 -5 346.72 22.33 8 -2 -10 1180.28 47.44 -8 2 10 1181.24 47.86 8 2 -10 1109.21 55.07 13 -3 1 1.18 4.65 13 -3 1 -0.77 6.03 13 3 1 3.30 3.40 -13 -3 7 5.53 5.14 -13 3 7 -0.58 4.24 -14 2 7 125.61 9.97 -14 -2 7 121.43 7.79 -14 -2 7 132.02 8.70 -6 -6 6 1.28 5.19 6 -6 -6 -1.03 5.99 -6 6 6 4.22 5.64 6 6 -6 2.55 4.02 13 -2 2 5.71 4.59 13 -2 2 -1.02 1.91 13 2 2 0.04 5.07 -13 2 8 0.55 5.80 -13 -2 8 -0.65 3.51 9 1 6 48.69 6.80 -9 -1 -6 35.24 9.32 9 -1 6 30.66 6.54 9 1 6 40.85 8.95 9 -1 6 54.14 9.99 -9 1 -6 59.40 16.57 -6 5 -5 238.23 25.40 6 -5 5 251.62 16.68 6 -5 5 241.77 17.00 -6 -5 -5 235.98 16.25 -6 -5 -5 245.94 22.15 6 5 5 257.76 15.15 3 -1 9 113.62 13.52 -3 1 -9 116.70 15.21 3 1 9 107.06 12.60 -3 -1 -9 95.85 13.94 3 1 9 107.02 12.62 13 4 -1 19.38 3.55 13 -4 -1 18.10 5.23 -13 4 1 20.84 5.07 13 -4 -1 21.73 8.68 -13 4 5 35.10 7.39 13 -4 -5 49.49 11.68 -13 -4 5 50.92 5.21 9 -6 -4 9.79 7.47 -9 -6 4 15.30 5.80 -9 6 4 16.95 7.35 3 6 5 10.30 6.40 -3 -6 -5 13.91 5.74 3 -6 5 0.37 8.92 -3 6 -5 9.99 5.82 3 -6 5 14.31 11.36 -3 -6 -5 9.15 6.87 0 -6 -6 221.16 17.65 0 6 6 216.93 17.11 0 -6 6 219.99 26.70 0 -6 -6 228.74 12.69 0 -6 6 228.35 19.09 0 6 -6 193.48 13.42 12 4 1 21.81 4.30 12 4 1 25.39 2.47 12 -4 1 31.12 5.91 12 -4 1 25.14 9.41 2 -2 -10 0.13 7.79 -2 2 10 39.83 8.60 2 2 -10 2.15 12.25 5 4 -9 6.27 6.60 5 -4 -9 20.63 7.34 -5 -4 9 24.26 7.83 -5 4 9 14.62 8.18 5 -7 -3 116.65 21.92 5 7 -3 119.49 11.95 -5 7 3 127.84 14.30 5 -7 -3 109.10 14.53 -5 -7 3 108.34 12.04 4 4 -9 475.49 31.44 -4 -4 9 512.72 26.64 4 -4 -9 476.65 24.87 -4 4 9 516.86 28.34 9 6 0 9.06 7.84 9 -6 0 14.98 6.94 9 -6 0 13.41 7.46 -9 6 0 21.20 6.68 -9 -6 0 18.07 5.44 0 0 -10 679.60 33.31 0 0 10 687.40 32.36 -5 -6 -4 10.79 5.76 5 -6 4 12.33 9.88 5 -6 4 7.53 5.33 -5 -6 -4 4.42 2.28 5 6 4 6.20 5.42 2 7 3 261.41 18.12 2 -7 3 248.91 18.19 -2 -7 -3 268.46 18.73 2 -7 3 290.66 20.53 -2 7 -3 247.67 19.42 10 -2 5 0.42 5.73 10 -2 5 3.41 3.60 10 2 5 4.55 4.53 -10 -2 -5 -3.42 4.85 -10 2 -5 8.27 6.24 10 2 5 -0.06 3.06 10 -4 -8 253.42 17.65 -10 4 8 235.06 17.54 -10 -4 8 247.62 15.08 10 4 -8 256.98 13.33 -10 -3 9 6.30 5.12 -10 3 9 5.45 5.99 10 3 -9 1.13 4.96 -12 -3 8 -0.02 3.45 -12 3 8 -4.05 4.13 12 3 -8 1.95 3.55 6 3 7 100.59 9.94 -6 -3 -7 83.65 10.86 -6 3 -7 84.30 13.46 6 3 7 55.35 9.93 6 -3 7 102.09 12.39 6 -3 7 90.60 10.48 8 -4 5 56.48 14.60 8 -4 5 88.65 11.81 -8 4 -5 76.34 11.95 -8 -4 -5 59.30 12.24 8 4 5 73.41 7.72 8 4 5 89.22 8.11 9 5 -7 4.97 3.47 -9 5 7 1.80 6.38 -9 -5 7 6.39 5.40 9 -5 -7 9.43 6.40 -6 -4 9 85.19 11.74 6 4 -9 94.60 9.90 6 -4 -9 97.30 12.26 -6 4 9 102.05 13.15 -14 0 8 17.05 5.51 4 -5 -8 9.72 5.99 4 -5 -8 -2.67 4.57 -4 5 8 -0.06 5.80 4 5 -8 4.23 4.30 -4 -5 8 -2.74 5.51 -2 7 4 250.35 18.31 -2 -7 4 278.41 18.70 2 -7 -4 237.60 19.17 -2 -7 4 211.76 12.69 10 -1 -10 69.99 11.92 -10 -1 10 74.13 10.92 10 1 -10 71.32 11.34 -10 1 10 72.21 11.34 7 2 7 14.65 9.78 -7 2 -7 21.01 14.14 -7 -2 -7 18.71 7.62 7 -2 7 17.78 6.40 7 -2 7 22.28 13.56 7 2 7 16.87 7.15 5 2 8 108.76 12.76 5 -2 8 136.67 12.36 -5 2 -8 137.31 16.55 -5 -2 -8 147.15 14.39 5 -2 8 154.02 15.30 5 2 8 127.89 13.09 -3 -4 9 13.63 7.95 3 4 -9 9.12 6.67 3 -4 -9 5.31 11.10 -3 4 9 17.54 8.08 -6 -7 1 24.48 7.65 6 -7 -1 25.89 9.21 6 -7 -1 23.63 10.08 6 7 -1 22.84 7.14 -6 7 1 35.22 8.71 5 -5 -8 2.16 4.37 5 -5 -8 4.53 5.55 -5 -5 8 -2.29 5.00 5 5 -8 4.05 5.74 -5 5 8 -4.74 5.30 -3 -7 4 23.32 12.49 3 -7 -4 23.40 9.26 -3 7 4 21.25 9.07 5 -7 1 41.40 10.41 -5 7 -1 35.98 9.09 -5 -7 -1 26.74 8.09 5 -7 1 31.90 9.27 5 7 1 21.67 7.64 -1 -7 4 134.62 8.27 -1 7 4 138.64 15.30 -1 -7 4 143.40 14.84 1 -7 -4 135.91 8.54 1 -7 -4 133.60 15.64 3 -5 -8 9.43 10.05 3 5 -8 2.64 4.65 -3 5 8 -0.39 6.28 -3 -5 8 6.73 5.95 3 -5 -8 -1.86 7.82 6 -7 -2 3.03 9.20 -6 -7 2 -4.06 7.96 -6 7 2 4.51 5.69 6 7 -2 2.61 4.70 6 -7 -2 1.78 4.48 15 0 0 -0.09 4.22 -12 5 3 -0.03 4.65 -12 -5 3 2.81 5.13 12 -5 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7 -6 -6 5.48 5.39 -7 6 6 7.89 5.26 -7 -4 9 -0.91 5.24 7 4 -9 -3.00 6.78 -7 4 9 -0.93 5.74 -4 -7 4 32.03 14.18 -4 7 4 35.69 9.93 4 -7 -4 38.34 11.08 -14 -1 8 102.80 9.48 -14 1 8 136.46 14.72 6 0 8 3.20 5.80 6 0 8 10.97 7.23 -6 0 -8 12.14 11.43 -10 -5 -2 51.11 10.42 10 5 2 54.29 9.58 10 -5 2 74.31 17.47 10 -5 2 86.80 8.94 15 2 -1 6.54 6.52 15 -2 -1 7.90 9.42 15 -2 -1 1.57 1.77 0 -7 4 4.23 6.07 0 -7 4 8.34 7.18 0 -7 -4 12.21 10.54 0 7 4 6.39 6.56 0 -7 -4 4.73 3.21 2 5 -8 8.72 6.26 -2 -5 8 13.28 6.21 2 -5 -8 11.03 8.02 2 -5 -8 14.92 10.06 -2 -5 8 17.70 8.14 -2 5 8 15.99 12.27 6 -7 0 273.05 15.47 6 -7 0 271.86 19.61 -6 -7 0 259.53 17.38 6 7 0 285.50 16.05 -6 7 0 243.98 18.63 -2 -4 9 57.40 11.54 -2 4 9 58.53 11.32 2 -4 -9 40.96 14.70 2 4 -9 38.00 9.74 1 -6 6 79.84 9.50 1 -6 6 77.05 18.65 -1 6 -6 61.91 9.30 -1 -6 -6 73.12 7.90 1 6 6 84.55 11.75 -1 -6 -6 55.89 11.45 14 -2 1 13.29 6.99 14 -2 1 8.79 3.42 14 2 1 0.07 5.11 -12 5 4 -0.03 6.53 12 -5 -4 48.29 8.37 12 5 -4 18.51 1.67 -12 -5 4 25.85 4.86 12 5 -4 10.62 2.45 12 -5 -4 21.32 6.84 -15 2 6 33.73 5.74 -15 -2 6 28.34 5.96 -15 -2 6 43.26 3.82 8 -3 6 -2.33 6.96 8 -3 6 -4.56 6.15 -8 3 -6 0.93 6.54 -8 -3 -6 -3.15 4.68 8 3 6 -2.57 6.25 8 3 6 -0.12 4.50 1 -2 -10 0.01 8.19 1 2 -10 -0.44 5.36 12 0 4 1403.24 38.28 12 0 4 1575.26 57.43 -12 0 -4 1479.77 57.11 12 0 4 1423.56 37.64 12 2 -9 534.84 24.14 -12 -2 9 535.86 24.26 -12 2 9 517.67 24.59 15 -1 0 294.24 20.37 15 1 0 288.33 17.24 13 0 3 -0.46 1.30 13 0 3 -0.33 1.36 13 0 3 3.39 4.74 -13 0 9 -0.08 5.60 12 4 -7 154.92 9.59 12 -4 -7 153.35 13.19 -12 4 7 164.75 13.49 -12 -4 7 142.26 10.67 10 -6 -2 23.53 7.03 -10 6 2 22.14 10.76 10 -6 -2 15.31 7.72 -10 -6 2 10.40 5.45 6 7 -3 205.26 16.06 6 -7 -3 226.01 26.74 6 -7 -3 268.28 20.03 -6 7 3 237.29 18.87 -6 -7 3 196.87 15.64 16 -1 -4 28.67 9.03 16 1 -4 23.14 6.94 -15 1 7 173.50 10.25 -15 -1 7 163.60 9.21 8 0 7 264.54 28.33 -8 0 -7 264.74 20.52 8 0 7 325.39 22.85 3 -7 3 81.20 13.08 3 7 3 101.83 11.59 3 -7 3 80.78 8.69 -3 -7 -3 86.70 12.04 -3 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