data_NYSM23521_0m_c _publ_section_references ; Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _diffrn_source_voltage '50 kV' _diffrn_source_current '30 mA' _exptl_crystal_recrystallization_method '?' _publ_contact_author_id_orcid '?' _audit_contact_author_phone '?' _audit_contact_author_name 'Hughes, John M.' _audit_contact_author_email 'jmhughes@uvm.edu' _audit_contact_author_address '?' _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0 H1.74 Ca1.98 Cl0.84 Fe2.58 K0.67 Mg2.45 Na0.25 O23.16 Si7.80' _chemical_formula_weight 935.65 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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_H-M_alt 'C 2/m' _space_group_name_Hall '-C 2y' _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, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 9.9124(3) _cell_length_b 18.2035(5) _cell_length_c 5.36220(10) _cell_angle_alpha 90 _cell_angle_beta 104.89 _cell_angle_gamma 90 _cell_volume 935.05(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8460 _cell_measurement_theta_min 2.4025 _cell_measurement_theta_max 33.376 _exptl_crystal_description equant _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.323 _exptl_crystal_F_000 924 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.247 _exptl_crystal_size_mid 0.186 _exptl_crystal_size_min 0.135 _exptl_absorpt_coefficient_mu 3.513 _shelx_estimated_absorpt_T_min 0.477 _shelx_estimated_absorpt_T_max 0.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6589 _exptl_absorpt_correction_T_max 0.7466 _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine focus sealed tube' _diffrn_measurement_device_type 'ApexII CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10493 _diffrn_reflns_av_unetI/netI 0.0082 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.403 _diffrn_reflns_theta_max 33.376 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.967 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.967 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_point_group_measured_fraction_full 0.991 _reflns_number_total 1809 _reflns_number_gt 1780 _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 'Bruker BIS 2016.5.0.1/14-Jun-2016 && APEX3_2016.5-0' _computing_cell_refinement 'SAINT V8.40A' _computing_data_reduction 'SAINT V8.40A' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics ? _computing_publication_material 'FinalCif by Daniel Kratzert, Freiburg 2019' _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^)+(0.0144P)^2^+0.6375P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_extinction_coef 0.0040(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1809 _refine_ls_number_parameters 123 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0137 _refine_ls_R_factor_gt 0.0134 _refine_ls_wR_factor_ref 0.0343 _refine_ls_wR_factor_gt 0.0342 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.001 _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 MgM1 Mg 0.000000 0.0907(5) 0.500000 0.00884(13) Uani 0.417(3) 2 d S T P . . FeM1 Fe 0.000000 0.09571(13) 0.500000 0.00884(13) Uani 0.583(3) 2 d S T P . . MgM2 Mg 0.000000 0.17816(2) 0.000000 0.00596(8) Uani 0.657(2) 2 d S T P . . FeM2 Fe 0.000000 0.17816(2) 0.000000 0.00596(8) Uani 0.343(2) 2 d S T P . . MgM3 Mg 0.000000 0.000000 0.000000 0.00807(9) Uani 0.298(3) 4 d S T P . . FeM3 Fe 0.000000 0.000000 0.000000 0.00807(9) Uani 0.702(3) 4 d S T P . . M4 Ca 0.000000 0.28063(4) 0.500000 0.01018(9) Uani 0.988(3) 2 d S T P . . M4' Fe 0.000000 0.257(2) 0.500000 0.018(6) Uiso 0.012(3) 2 d S . P . . Si1 Si 0.27832(2) 0.08606(2) 0.30145(4) 0.00693(7) Uani 0.966(2) 1 d . . P . . Si2 Si 0.29137(2) 0.17367(2) 0.81221(4) 0.00588(7) Uani 0.9825(19) 1 d . . P . . O1 O 0.10358(6) 0.09093(3) 0.21449(11) 0.01043(11) Uani 1 1 d . . . . . O2 O 0.12089(6) 0.17693(3) 0.73577(11) 0.01031(11) Uani 1 1 d . . . . . O3 O 0.1087(2) 0.000000 0.7070(3) 0.00967(18) Uani 0.5794(19) 2 d DS T P . . H3 H 0.017(7) 0.000000 0.64(7) 0.8(3) Uiso 0.58 2 d DS . P . . Cl3 Cl 0.16378(9) 0.000000 0.73508(12) 0.00967(18) Uani 0.4206(19) 2 d S T P . . O4 O 0.36897(6) 0.25027(3) 0.79457(11) 0.01137(11) Uani 1 1 d . . . . . O5 O 0.34873(6) 0.13742(3) 0.10199(10) 0.01171(11) Uani 1 1 d . . . . . O6 O 0.34337(6) 0.12192(3) 0.59956(11) 0.01268(12) Uani 1 1 d . . . . . O7 O 0.33549(9) 0.000000 0.29685(18) 0.01624(17) Uani 1 2 d S T P . . A2M K 0.500000 0.000000 0.000000 0.0497(11) Uani 0.671(14) 4 d S T P . . A2 Na 0.500000 -0.0350(17) 0.000000 0.027(6) Uiso 0.046(6) 2 d S . P . . AM Na 0.543(3) 0.000000 0.103(7) 0.081(13) Uiso 0.077(11) 2 d S . P . . 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 MgM1 0.00859(11) 0.0119(4) 0.00661(10) 0.000 0.00291(7) 0.000 FeM1 0.00859(11) 0.0119(4) 0.00661(10) 0.000 0.00291(7) 0.000 MgM2 0.00589(12) 0.00591(12) 0.00631(12) 0.000 0.00197(8) 0.000 FeM2 0.00589(12) 0.00591(12) 0.00631(12) 0.000 0.00197(8) 0.000 MgM3 0.00843(13) 0.00612(13) 0.00874(13) 0.000 0.00055(8) 0.000 FeM3 0.00843(13) 0.00612(13) 0.00874(13) 0.000 0.00055(8) 0.000 M4 0.01143(11) 0.0090(2) 0.01220(11) 0.000 0.00678(7) 0.000 Si1 0.00673(10) 0.00687(10) 0.00710(10) -0.00015(6) 0.00163(7) -0.00050(6) Si2 0.00579(10) 0.00623(10) 0.00587(9) 0.00059(6) 0.00197(6) 0.00004(6) O1 0.0099(2) 0.0125(2) 0.0093(2) -0.00122(17) 0.00320(18) -0.00195(18) O2 0.0071(2) 0.0129(2) 0.0106(2) 0.00126(18) 0.00175(17) 0.00101(18) O3 0.0101(4) 0.0097(2) 0.0097(2) 0.000 0.0034(2) 0.000 Cl3 0.0101(4) 0.0097(2) 0.0097(2) 0.000 0.0034(2) 0.000 O4 0.0135(2) 0.0094(2) 0.0125(2) 0.00039(18) 0.00569(18) -0.00158(19) O5 0.0101(2) 0.0134(3) 0.0110(2) 0.00465(18) 0.00169(18) 0.00023(18) O6 0.0102(2) 0.0148(3) 0.0134(2) -0.00441(19) 0.00370(19) 0.00036(19) O7 0.0126(4) 0.0145(4) 0.0214(4) 0.000 0.0039(3) 0.000 A2M 0.0581(16) 0.0352(12) 0.080(2) 0.000 0.0617(16) 0.000 _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 MgM1 O1 2.0509(6) . ? MgM1 O1 2.0509(6) 2_556 ? MgM1 O3 2.122(7) . ? MgM1 O3 2.122(7) 5_556 ? MgM1 O2 2.173(7) . ? MgM1 O2 2.173(7) 2_556 ? MgM1 Cl3 2.428(6) 5_556 ? MgM1 Cl3 2.428(6) . ? FeM1 O1 2.0527(6) . ? FeM1 O1 2.0528(6) 2_556 ? FeM1 O2 2.1075(18) . ? FeM1 O2 2.1075(18) 2_556 ? FeM1 O3 2.194(2) . ? FeM1 O3 2.194(2) 5_556 ? FeM1 Cl3 2.4916(18) 5_556 ? FeM1 Cl3 2.4916(18) . ? MgM2 O4 1.9653(6) 7_556 ? MgM2 O4 1.9653(6) 8_454 ? MgM2 O1 2.0715(6) 2 ? MgM2 O1 2.0715(6) . ? MgM2 O2 2.0777(5) 2_556 ? MgM2 O2 2.0777(5) 1_554 ? MgM3 O3 2.1209(18) 5_556 ? MgM3 O3 2.1209(18) 1_554 ? MgM3 O1 2.1237(6) . ? MgM3 O1 2.1237(6) 5 ? MgM3 O1 2.1237(6) 6 ? MgM3 O1 2.1237(6) 2 ? MgM3 Cl3 2.4165(7) 5_556 ? MgM3 Cl3 2.4165(7) 1_554 ? FeM3 O3 2.1209(18) 5_556 ? FeM3 O3 2.1209(18) 1_554 ? FeM3 O1 2.1237(6) . ? FeM3 O1 2.1237(6) 5 ? FeM3 O1 2.1237(6) 6 ? FeM3 O1 2.1237(6) 2 ? FeM3 Cl3 2.4165(7) 5_556 ? FeM3 Cl3 2.4165(7) 1_554 ? M4 O4 2.3565(6) 7_556 ? M4 O4 2.3565(6) 8_455 ? M4 O2 2.4121(8) 2_556 ? M4 O2 2.4121(8) . ? M4 O6 2.5038(8) 7_556 ? M4 O6 2.5038(8) 8_455 ? M4 O5 2.7173(7) 7_556 ? M4 O5 2.7173(7) 8_455 ? M4' O2 2.09(3) 2_556 ? M4' O2 2.09(3) . ? M4' O4 2.292(3) 8_455 ? M4' O4 2.292(3) 7_556 ? Si1 O7 1.6683(4) . ? Si1 O1 1.6764(6) . ? Si1 O6 1.6933(6) . ? Si1 O5 1.6996(6) . ? Si2 O4 1.6070(6) . ? Si2 O2 1.6343(6) . ? Si2 O5 1.6489(6) 1_556 ? Si2 O6 1.6599(6) . ? O3 Cl3 0.5282(17) . ? Cl3 AM 2.81(3) 5_656 ? Cl3 A2M 3.2697(9) 1_556 ? Cl3 A2 3.331(6) 5_656 ? Cl3 A2 3.331(6) 1_556 ? O5 A2 2.54(2) 5_655 ? O5 A2M 3.0375(6) . ? O6 A2 2.794(18) 5_656 ? O6 AM 2.80(2) 5_656 ? O6 A2M 3.1989(6) 1_556 ? O7 AM 2.53(3) . ? O7 A2M 2.5549(9) . ? O7 A2 2.633(8) 5_655 ? O7 A2 2.633(8) . ? O7 AM 2.71(3) 5_655 ? A2M AM 0.60(4) 5_655 ? A2M AM 0.60(4) . ? A2M A2 0.64(3) 5_655 ? A2M A2 0.64(3) . ? A2 AM 0.88(4) 5_655 ? A2 AM 0.88(4) . ? A2 A2 1.28(6) 5_655 ? AM AM 1.21(8) 5_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 O1 MgM1 O1 179.7(5) . 2_556 ? O1 MgM1 O3 96.2(2) . . ? O1 MgM1 O3 84.00(18) 2_556 . ? O1 MgM1 O3 84.00(18) . 5_556 ? O1 MgM1 O3 96.2(2) 2_556 5_556 ? O3 MgM1 O3 77.9(3) . 5_556 ? O1 MgM1 O2 97.2(2) . . ? O1 MgM1 O2 82.59(16) 2_556 . ? O3 MgM1 O2 97.35(5) . . ? O3 MgM1 O2 175.2(3) 5_556 . ? O1 MgM1 O2 82.59(16) . 2_556 ? O1 MgM1 O2 97.2(2) 2_556 2_556 ? O3 MgM1 O2 175.2(3) . 2_556 ? O3 MgM1 O2 97.35(5) 5_556 2_556 ? O2 MgM1 O2 87.5(3) . 2_556 ? O1 MgM1 Cl3 90.59(17) . 5_556 ? O1 MgM1 Cl3 89.59(17) 2_556 5_556 ? O3 MgM1 Cl3 85.7(3) . 5_556 ? O3 MgM1 Cl3 10.87(5) 5_556 5_556 ? O2 MgM1 Cl3 171.25(13) . 5_556 ? O2 MgM1 Cl3 89.66(2) 2_556 5_556 ? O1 MgM1 Cl3 89.59(17) . . ? O1 MgM1 Cl3 90.59(17) 2_556 . ? O3 MgM1 Cl3 10.87(5) . . ? O3 MgM1 Cl3 85.7(3) 5_556 . ? O2 MgM1 Cl3 89.66(2) . . ? O2 MgM1 Cl3 171.25(13) 2_556 . ? Cl3 MgM1 Cl3 94.4(3) 5_556 . ? O1 FeM1 O1 175.14(14) . 2_556 ? O1 FeM1 O2 99.26(6) . . ? O1 FeM1 O2 84.18(5) 2_556 . ? O1 FeM1 O2 84.18(5) . 2_556 ? O1 FeM1 O2 99.26(6) 2_556 2_556 ? O2 FeM1 O2 90.89(10) . 2_556 ? O1 FeM1 O3 93.96(8) . . ? O1 FeM1 O3 82.16(7) 2_556 . ? O2 FeM1 O3 97.13(5) . . ? O2 FeM1 O3 171.96(10) 2_556 . ? O1 FeM1 O3 82.16(7) . 5_556 ? O1 FeM1 O3 93.96(8) 2_556 5_556 ? O2 FeM1 O3 171.96(10) . 5_556 ? O2 FeM1 O3 97.13(5) 2_556 5_556 ? O3 FeM1 O3 74.85(11) . 5_556 ? O1 FeM1 Cl3 88.79(5) . 5_556 ? O1 FeM1 Cl3 87.82(5) 2_556 5_556 ? O2 FeM1 Cl3 171.95(2) . 5_556 ? O2 FeM1 Cl3 89.49(2) 2_556 5_556 ? O3 FeM1 Cl3 82.64(9) . 5_556 ? O3 FeM1 Cl3 10.71(4) 5_556 5_556 ? O1 FeM1 Cl3 87.82(5) . . ? O1 FeM1 Cl3 88.79(5) 2_556 . ? O2 FeM1 Cl3 89.49(2) . . ? O2 FeM1 Cl3 171.94(2) 2_556 . ? O3 FeM1 Cl3 10.71(4) . . ? O3 FeM1 Cl3 82.64(9) 5_556 . ? Cl3 FeM1 Cl3 91.26(8) 5_556 . ? O4 MgM2 O4 96.95(4) 7_556 8_454 ? O4 MgM2 O1 168.87(2) 7_556 2 ? O4 MgM2 O1 92.01(2) 8_454 2 ? O4 MgM2 O1 92.01(2) 7_556 . ? O4 MgM2 O1 168.87(2) 8_454 . ? O1 MgM2 O1 79.92(3) 2 . ? O4 MgM2 O2 92.23(2) 7_556 2_556 ? O4 MgM2 O2 88.59(2) 8_454 2_556 ? O1 MgM2 O2 94.58(2) 2 2_556 ? O1 MgM2 O2 84.47(2) . 2_556 ? O4 MgM2 O2 88.59(2) 7_556 1_554 ? O4 MgM2 O2 92.23(2) 8_454 1_554 ? O1 MgM2 O2 84.47(2) 2 1_554 ? O1 MgM2 O2 94.59(2) . 1_554 ? O2 MgM2 O2 178.77(3) 2_556 1_554 ? O3 MgM3 O3 180.00(9) 5_556 1_554 ? O3 MgM3 O1 82.28(4) 5_556 . ? O3 MgM3 O1 97.72(4) 1_554 . ? O3 MgM3 O1 97.72(4) 5_556 5 ? O3 MgM3 O1 82.28(4) 1_554 5 ? O1 MgM3 O1 180.0 . 5 ? O3 MgM3 O1 82.28(4) 5_556 6 ? O3 MgM3 O1 97.72(4) 1_554 6 ? O1 MgM3 O1 102.42(3) . 6 ? O1 MgM3 O1 77.58(3) 5 6 ? O3 MgM3 O1 97.72(4) 5_556 2 ? O3 MgM3 O1 82.28(4) 1_554 2 ? O1 MgM3 O1 77.58(3) . 2 ? O1 MgM3 O1 102.42(3) 5 2 ? O1 MgM3 O1 180.00(3) 6 2 ? O3 MgM3 Cl3 11.09(5) 5_556 5_556 ? O3 MgM3 Cl3 168.91(5) 1_554 5_556 ? O1 MgM3 Cl3 89.196(19) . 5_556 ? O1 MgM3 Cl3 90.803(19) 5 5_556 ? O1 MgM3 Cl3 89.197(19) 6 5_556 ? O1 MgM3 Cl3 90.803(19) 2 5_556 ? O3 MgM3 Cl3 168.91(5) 5_556 1_554 ? O3 MgM3 Cl3 11.09(5) 1_554 1_554 ? O1 MgM3 Cl3 90.804(19) . 1_554 ? O1 MgM3 Cl3 89.197(19) 5 1_554 ? O1 MgM3 Cl3 90.803(19) 6 1_554 ? O1 MgM3 Cl3 89.197(19) 2 1_554 ? Cl3 MgM3 Cl3 180.0 5_556 1_554 ? O3 FeM3 O3 180.00(9) 5_556 1_554 ? O3 FeM3 O1 82.28(4) 5_556 . ? O3 FeM3 O1 97.72(4) 1_554 . ? O3 FeM3 O1 97.72(4) 5_556 5 ? O3 FeM3 O1 82.28(4) 1_554 5 ? O1 FeM3 O1 180.0 . 5 ? O3 FeM3 O1 82.28(4) 5_556 6 ? O3 FeM3 O1 97.72(4) 1_554 6 ? O1 FeM3 O1 102.42(3) . 6 ? O1 FeM3 O1 77.58(3) 5 6 ? O3 FeM3 O1 97.72(4) 5_556 2 ? O3 FeM3 O1 82.28(4) 1_554 2 ? O1 FeM3 O1 77.58(3) . 2 ? O1 FeM3 O1 102.42(3) 5 2 ? O1 FeM3 O1 180.00(3) 6 2 ? O3 FeM3 Cl3 11.09(5) 5_556 5_556 ? O3 FeM3 Cl3 168.91(5) 1_554 5_556 ? O1 FeM3 Cl3 89.196(19) . 5_556 ? O1 FeM3 Cl3 90.803(19) 5 5_556 ? O1 FeM3 Cl3 89.197(19) 6 5_556 ? O1 FeM3 Cl3 90.803(19) 2 5_556 ? O3 FeM3 Cl3 168.91(5) 5_556 1_554 ? O3 FeM3 Cl3 11.09(5) 1_554 1_554 ? O1 FeM3 Cl3 90.804(19) . 1_554 ? O1 FeM3 Cl3 89.197(19) 5 1_554 ? O1 FeM3 Cl3 90.803(19) 6 1_554 ? O1 FeM3 Cl3 89.197(19) 2 1_554 ? Cl3 FeM3 Cl3 180.0 5_556 1_554 ? O4 M4 O4 152.39(4) 7_556 8_455 ? O4 M4 O2 75.35(2) 7_556 2_556 ? O4 M4 O2 83.07(2) 8_455 2_556 ? O4 M4 O2 83.07(2) 7_556 . ? O4 M4 O2 75.35(2) 8_455 . ? O2 M4 O2 77.01(3) 2_556 . ? O4 M4 O6 63.085(19) 7_556 7_556 ? O4 M4 O6 142.27(3) 8_455 7_556 ? O2 M4 O6 133.982(18) 2_556 7_556 ? O2 M4 O6 114.486(19) . 7_556 ? O4 M4 O6 142.27(3) 7_556 8_455 ? O4 M4 O6 63.085(19) 8_455 8_455 ? O2 M4 O6 114.487(19) 2_556 8_455 ? O2 M4 O6 133.983(18) . 8_455 ? O6 M4 O6 89.77(3) 7_556 8_455 ? O4 M4 O5 111.69(2) 7_556 7_556 ? O4 M4 O5 83.829(19) 8_455 7_556 ? O2 M4 O5 160.18(3) 2_556 7_556 ? O2 M4 O5 85.324(18) . 7_556 ? O6 M4 O5 62.05(2) 7_556 7_556 ? O6 M4 O5 71.99(2) 8_455 7_556 ? O4 M4 O5 83.829(19) 7_556 8_455 ? O4 M4 O5 111.69(2) 8_455 8_455 ? O2 M4 O5 85.324(18) 2_556 8_455 ? O2 M4 O5 160.18(3) . 8_455 ? O6 M4 O5 71.99(2) 7_556 8_455 ? O6 M4 O5 62.05(2) 8_455 8_455 ? O5 M4 O5 113.40(3) 7_556 8_455 ? O2 M4' O2 91.8(17) 2_556 . ? O2 M4' O4 92.2(9) 2_556 8_455 ? O2 M4' O4 83.2(7) . 8_455 ? O2 M4' O4 83.2(7) 2_556 7_556 ? O2 M4' O4 92.2(9) . 7_556 ? O4 M4' O4 174(2) 8_455 7_556 ? O2 M4' FeM1 45.9(9) 2_556 . ? O2 M4' FeM1 45.9(9) . . ? O4 M4' FeM1 86.8(11) 8_455 . ? O4 M4' FeM1 86.8(11) 7_556 . ? O2 M4' MgM1 45.9(9) 2_556 . ? O2 M4' MgM1 45.9(9) . . ? O4 M4' MgM1 86.8(11) 8_455 . ? O4 M4' MgM1 86.8(11) 7_556 . ? FeM1 M4' MgM1 0.0 . . ? O2 M4' MgM2 43.0(4) 2_556 . ? O2 M4' MgM2 94.3(12) . . ? O4 M4' MgM2 135.2(12) 8_455 . ? O4 M4' MgM2 40.3(3) 7_556 . ? FeM1 M4' MgM2 61.9(7) . . ? MgM1 M4' MgM2 61.9(7) . . ? O2 M4' MgM2 94.3(12) 2_556 1_556 ? O2 M4' MgM2 43.0(4) . 1_556 ? O4 M4' MgM2 40.3(3) 8_455 1_556 ? O4 M4' MgM2 135.2(12) 7_556 1_556 ? FeM1 M4' MgM2 61.9(7) . 1_556 ? MgM1 M4' MgM2 61.9(7) . 1_556 ? MgM2 M4' MgM2 123.8(14) . 1_556 ? O7 Si1 O1 112.09(4) . . ? O7 Si1 O6 109.12(4) . . ? O1 Si1 O6 110.96(3) . . ? O7 Si1 O5 108.13(4) . . ? O1 Si1 O5 110.97(3) . . ? O6 Si1 O5 105.29(3) . . ? O4 Si2 O2 115.68(3) . . ? O4 Si2 O5 110.39(3) . 1_556 ? O2 Si2 O5 109.56(3) . 1_556 ? O4 Si2 O6 102.37(3) . . ? O2 Si2 O6 109.39(3) . . ? O5 Si2 O6 109.12(3) 1_556 . ? Si1 O1 MgM1 118.16(3) . . ? Si1 O1 FeM1 118.29(3) . . ? MgM1 O1 FeM1 2.6(3) . . ? Si1 O1 MgM2 121.61(3) . . ? MgM1 O1 MgM2 98.3(2) . . ? FeM1 O1 MgM2 96.32(6) . . ? Si1 O1 MgM3 115.50(3) . . ? MgM1 O1 MgM3 97.9(2) . . ? FeM1 O1 MgM3 99.91(6) . . ? MgM2 O1 MgM3 101.25(2) . . ? Si1 O1 FeM3 115.50(3) . . ? MgM1 O1 FeM3 97.9(2) . . ? FeM1 O1 FeM3 99.91(6) . . ? MgM2 O1 FeM3 101.25(2) . . ? MgM3 O1 FeM3 0.0 . . ? Si2 O2 MgM2 124.73(3) . 1_556 ? Si2 O2 M4' 124.9(5) . . ? MgM2 O2 M4' 93.64(7) 1_556 . ? Si2 O2 FeM1 121.11(4) . . ? MgM2 O2 FeM1 94.47(2) 1_556 . ? M4' O2 FeM1 88.6(9) . . ? Si2 O2 MgM1 119.98(11) . . ? MgM2 O2 MgM1 94.36(3) 1_556 . ? M4' O2 MgM1 90.4(9) . . ? FeM1 O2 MgM1 1.7(2) . . ? Si2 O2 M4 120.15(3) . . ? MgM2 O2 M4 93.04(2) 1_556 . ? M4' O2 M4 7.4(8) . . ? FeM1 O2 M4 96.05(5) . . ? MgM1 O2 M4 97.77(17) . . ? Cl3 O3 MgM3 118.3(2) . 1_556 ? Cl3 O3 MgM1 119.87(16) . 5_556 ? MgM3 O3 MgM1 95.82(7) 1_556 5_556 ? Cl3 O3 MgM1 119.86(16) . . ? MgM3 O3 MgM1 95.82(7) 1_556 . ? MgM1 O3 MgM1 102.1(3) 5_556 . ? Cl3 O3 FeM1 118.79(11) . . ? MgM3 O3 FeM1 95.63(7) 1_556 . ? MgM1 O3 FeM1 103.65(14) 5_556 . ? MgM1 O3 FeM1 1.50(19) . . ? O3 Cl3 MgM3 50.6(2) . 1_556 ? O3 Cl3 MgM1 49.26(15) . 5_556 ? MgM3 Cl3 MgM1 81.06(3) 1_556 5_556 ? O3 Cl3 MgM1 49.26(15) . . ? MgM3 Cl3 MgM1 81.06(3) 1_556 . ? MgM1 Cl3 MgM1 85.6(3) 5_556 . ? O3 Cl3 FeM1 50.50(9) . . ? MgM3 Cl3 FeM1 81.29(2) 1_556 . ? MgM1 Cl3 FeM1 87.19(12) 5_556 . ? MgM1 Cl3 FeM1 1.55(19) . . ? O3 Cl3 AM 178.6(7) . 5_656 ? MgM3 Cl3 AM 128.0(7) 1_556 5_656 ? MgM1 Cl3 AM 131.4(3) 5_556 5_656 ? MgM1 Cl3 AM 131.4(3) . 5_656 ? FeM1 Cl3 AM 130.1(3) . 5_656 ? O3 Cl3 A2M 171.2(2) . 1_556 ? MgM3 Cl3 A2M 120.56(2) 1_556 1_556 ? MgM1 Cl3 A2M 134.13(14) 5_556 1_556 ? MgM1 Cl3 A2M 134.13(14) . 1_556 ? FeM1 Cl3 A2M 132.74(4) . 1_556 ? AM Cl3 A2M 7.4(7) 5_656 1_556 ? O3 Cl3 A2 165.9(4) . 5_656 ? MgM3 Cl3 A2 119.93(6) 1_556 5_656 ? MgM1 Cl3 A2 144.4(5) 5_556 5_656 ? MgM1 Cl3 A2 123.6(5) . 5_656 ? FeM1 Cl3 A2 122.2(5) . 5_656 ? AM Cl3 A2 13.3(6) 5_656 5_656 ? A2M Cl3 A2 11.0(5) 1_556 5_656 ? O3 Cl3 A2 165.9(4) . 1_556 ? MgM3 Cl3 A2 119.93(6) 1_556 1_556 ? MgM1 Cl3 A2 123.6(5) 5_556 1_556 ? MgM1 Cl3 A2 144.4(5) . 1_556 ? FeM1 Cl3 A2 143.1(5) . 1_556 ? AM Cl3 A2 13.3(6) 5_656 1_556 ? A2M Cl3 A2 11.0(5) 1_556 1_556 ? A2 Cl3 A2 22.1(11) 5_656 1_556 ? Si2 O4 MgM2 143.09(4) . 7_556 ? Si2 O4 M4' 110.9(10) . 7_556 ? MgM2 O4 M4' 90.8(7) 7_556 7_556 ? Si2 O4 M4 100.78(3) . 7_556 ? MgM2 O4 M4 97.77(3) 7_556 7_556 ? M4' O4 M4 10.6(11) 7_556 7_556 ? Si2 O5 Si1 135.66(4) 1_554 . ? Si2 O5 A2 99.8(2) 1_554 5_655 ? Si1 O5 A2 95.3(4) . 5_655 ? Si2 O5 M4 120.49(3) 1_554 7_556 ? Si1 O5 M4 92.33(2) . 7_556 ? A2 O5 M4 109.6(2) 5_655 7_556 ? Si2 O5 A2M 103.09(3) 1_554 . ? Si1 O5 A2M 87.82(2) . . ? A2 O5 A2M 8.2(5) 5_655 . ? M4 O5 A2M 113.29(2) 7_556 . ? Si2 O6 Si1 139.21(4) . . ? Si2 O6 M4 93.64(3) . 7_556 ? Si1 O6 M4 100.27(3) . 7_556 ? Si2 O6 A2 90.1(4) . 5_656 ? Si1 O6 A2 120.6(5) . 5_656 ? M4 O6 A2 108.2(4) 7_556 5_656 ? Si2 O6 AM 102.0(6) . 5_656 ? Si1 O6 AM 103.5(6) . 5_656 ? M4 O6 AM 120.2(6) 7_556 5_656 ? A2 O6 AM 18.1(8) 5_656 5_656 ? Si2 O6 A2M 96.63(2) . 1_556 ? Si1 O6 A2M 111.57(3) . 1_556 ? M4 O6 A2M 114.46(2) 7_556 1_556 ? A2 O6 A2M 9.5(5) 5_656 1_556 ? AM O6 A2M 8.6(6) 5_656 1_556 ? Si1 O7 Si1 139.79(6) 6 . ? Si1 O7 AM 108.72(12) 6 . ? Si1 O7 AM 108.71(12) . . ? Si1 O7 A2M 106.43(3) 6 . ? Si1 O7 A2M 106.43(3) . . ? AM O7 A2M 13.6(9) . . ? Si1 O7 A2 120.1(6) 6 5_655 ? Si1 O7 A2 92.7(7) . 5_655 ? AM O7 A2 19.4(8) . 5_655 ? A2M O7 A2 14.0(7) . 5_655 ? Si1 O7 A2 92.7(7) 6 . ? Si1 O7 A2 120.1(6) . . ? AM O7 A2 19.4(8) . . ? A2M O7 A2 14.0(7) . . ? A2 O7 A2 28.0(13) 5_655 . ? Si1 O7 AM 103.5(2) 6 5_655 ? Si1 O7 AM 103.5(2) . 5_655 ? AM O7 AM 26.3(16) . 5_655 ? A2M O7 AM 12.7(8) . 5_655 ? A2 O7 AM 18.8(7) 5_655 5_655 ? A2 O7 AM 18.8(7) . 5_655 ? AM A2M AM 179.998(16) 5_655 . ? AM A2M A2 90.0 5_655 5_655 ? AM A2M A2 90.0 . 5_655 ? AM A2M A2 90.0 5_655 . ? AM A2M A2 90.0 . . ? A2 A2M A2 180.0 5_655 . ? AM A2M O7 81(2) 5_655 5_655 ? AM A2M O7 99(2) . 5_655 ? A2 A2M O7 90.0 5_655 5_655 ? A2 A2M O7 90.0 . 5_655 ? AM A2M O7 99(2) 5_655 . ? AM A2M O7 81(2) . . ? A2 A2M O7 90.0 5_655 . ? A2 A2M O7 90.0 . . ? O7 A2M O7 180.0 5_655 . ? AM A2M O5 84.1(14) 5_655 . ? AM A2M O5 95.9(14) . . ? A2 A2M O5 34.560(11) 5_655 . ? A2 A2M O5 145.440(11) . . ? O7 A2M O5 122.401(11) 5_655 . ? O7 A2M O5 57.599(11) . . ? AM A2M O5 84.1(14) 5_655 6 ? AM A2M O5 95.9(14) . 6 ? A2 A2M O5 145.441(11) 5_655 6 ? A2 A2M O5 34.559(11) . 6 ? O7 A2M O5 122.401(11) 5_655 6 ? O7 A2M O5 57.599(11) . 6 ? O5 A2M O5 110.88(2) . 6 ? AM A2M O5 95.9(14) 5_655 2_655 ? AM A2M O5 84.1(14) . 2_655 ? A2 A2M O5 34.559(11) 5_655 2_655 ? A2 A2M O5 145.441(11) . 2_655 ? O7 A2M O5 57.599(11) 5_655 2_655 ? O7 A2M O5 122.401(11) . 2_655 ? O5 A2M O5 69.12(2) . 2_655 ? O5 A2M O5 180.000(13) 6 2_655 ? AM A2M O5 95.9(14) 5_655 5_655 ? AM A2M O5 84.1(14) . 5_655 ? A2 A2M O5 145.441(11) 5_655 5_655 ? A2 A2M O5 34.559(11) . 5_655 ? O7 A2M O5 57.599(11) 5_655 5_655 ? O7 A2M O5 122.401(11) . 5_655 ? O5 A2M O5 180.0 . 5_655 ? O5 A2M O5 69.12(2) 6 5_655 ? O5 A2M O5 110.88(2) 2_655 5_655 ? AM A2M O6 43.99(11) 5_655 6_554 ? AM A2M O6 136.01(11) . 6_554 ? A2 A2M O6 133.931(10) 5_655 6_554 ? A2 A2M O6 46.069(10) . 6_554 ? O7 A2M O6 81.905(18) 5_655 6_554 ? O7 A2M O6 98.095(18) . 6_554 ? O5 A2M O6 121.020(15) . 6_554 ? O5 A2M O6 51.142(14) 6 6_554 ? O5 A2M O6 128.858(14) 2_655 6_554 ? O5 A2M O6 58.980(15) 5_655 6_554 ? AM A2M O6 136.01(11) 5_655 2_656 ? AM A2M O6 43.99(11) . 2_656 ? A2 A2M O6 46.069(10) 5_655 2_656 ? A2 A2M O6 133.931(10) . 2_656 ? O7 A2M O6 98.095(18) 5_655 2_656 ? O7 A2M O6 81.905(18) . 2_656 ? O5 A2M O6 58.980(15) . 2_656 ? O5 A2M O6 128.858(14) 6 2_656 ? O5 A2M O6 51.142(14) 2_655 2_656 ? O5 A2M O6 121.020(15) 5_655 2_656 ? O6 A2M O6 180.000(16) 6_554 2_656 ? A2M A2 AM 43(2) . 5_655 ? A2M A2 AM 43(2) . . ? AM A2 AM 87(4) 5_655 . ? A2M A2 A2 0.0 . 5_655 ? AM A2 A2 43(2) 5_655 5_655 ? AM A2 A2 43(2) . 5_655 ? A2M A2 O5 137.2(5) . 6 ? AM A2 O5 116.7(18) 5_655 6 ? AM A2 O5 128.2(18) . 6 ? A2 A2 O5 137.2(5) 5_655 6 ? A2M A2 O5 137.2(5) . 5_655 ? AM A2 O5 128.2(18) 5_655 5_655 ? AM A2 O5 116.7(18) . 5_655 ? A2 A2 O5 137.2(5) 5_655 5_655 ? O5 A2 O5 85.5(10) 6 5_655 ? A2M A2 O7 76.0(7) . 5_655 ? AM A2 O7 73.9(18) 5_655 5_655 ? AM A2 O7 85.7(19) . 5_655 ? A2 A2 O7 76.0(7) 5_655 5_655 ? O5 A2 O7 143.1(10) 6 5_655 ? O5 A2 O7 63.62(19) 5_655 5_655 ? A2M A2 O7 76.0(7) . . ? AM A2 O7 85.7(19) 5_655 . ? AM A2 O7 73.9(18) . . ? A2 A2 O7 76.0(7) 5_655 . ? O5 A2 O7 63.62(19) 6 . ? O5 A2 O7 143.1(10) 5_655 . ? O7 A2 O7 152.0(13) 5_655 . ? A2M A2 O6 124.5(5) . 6_554 ? AM A2 O6 81(2) 5_655 6_554 ? AM A2 O6 168(3) . 6_554 ? A2 A2 O6 124.5(5) 5_655 6_554 ? O5 A2 O6 60.5(5) 6 6_554 ? O5 A2 O6 70.2(6) 5_655 6_554 ? O7 A2 O6 88.9(2) 5_655 6_554 ? O7 A2 O6 107.1(3) . 6_554 ? A2M A2 O6 124.5(5) . 5_656 ? AM A2 O6 168(3) 5_655 5_656 ? AM A2 O6 81(2) . 5_656 ? A2 A2 O6 124.5(5) 5_655 5_656 ? O5 A2 O6 70.2(6) 6 5_656 ? O5 A2 O6 60.5(5) 5_655 5_656 ? O7 A2 O6 107.1(3) 5_655 5_656 ? O7 A2 O6 88.9(2) . 5_656 ? O6 A2 O6 111.1(11) 6_554 5_656 ? A2M A2 Si1 107.0(5) . 6 ? AM A2 Si1 104.0(16) 5_655 6 ? AM A2 Si1 100.5(17) . 6 ? A2 A2 Si1 107.0(5) 5_655 6 ? O5 A2 Si1 32.12(8) 6 6 ? O5 A2 Si1 114.7(10) 5_655 6 ? O7 A2 Si1 173.4(6) 5_655 6 ? O7 A2 Si1 31.57(12) . 6 ? O6 A2 Si1 84.6(5) 6_554 6 ? O6 A2 Si1 76.4(4) 5_656 6 ? A2M A2 Si1 107.0(5) . 5_655 ? AM A2 Si1 100.5(17) 5_655 5_655 ? AM A2 Si1 104.0(16) . 5_655 ? A2 A2 Si1 107.0(5) 5_655 5_655 ? O5 A2 Si1 114.7(10) 6 5_655 ? O5 A2 Si1 32.12(8) 5_655 5_655 ? O7 A2 Si1 31.57(12) 5_655 5_655 ? O7 A2 Si1 173.4(6) . 5_655 ? O6 A2 Si1 76.4(4) 6_554 5_655 ? O6 A2 Si1 84.6(5) 5_656 5_655 ? Si1 A2 Si1 146.1(11) 6 5_655 ? A2M AM A2 47(2) . . ? A2M AM A2 47(2) . 5_655 ? A2 AM A2 93(4) . 5_655 ? A2M AM AM 0.001(7) . 5_655 ? A2 AM AM 47(2) . 5_655 ? A2 AM AM 47(2) 5_655 5_655 ? A2M AM O7 85(2) . . ? A2 AM O7 86.7(17) . . ? A2 AM O7 86.7(17) 5_655 . ? AM AM O7 85(2) 5_655 . ? A2M AM O7 69(2) . 5_655 ? A2 AM O7 75.5(19) . 5_655 ? A2 AM O7 75.5(19) 5_655 5_655 ? AM AM O7 69(2) 5_655 5_655 ? O7 AM O7 153.7(16) . 5_655 ? A2M AM O6 127.4(6) . 2_656 ? A2 AM O6 174(3) . 2_656 ? A2 AM O6 80.8(18) 5_655 2_656 ? AM AM O6 127.4(6) 5_655 2_656 ? O7 AM O6 90.9(7) . 2_656 ? O7 AM O6 104.8(6) 5_655 2_656 ? A2M AM O6 127.4(6) . 5_656 ? A2 AM O6 80.8(18) . 5_656 ? A2 AM O6 174(3) 5_655 5_656 ? AM AM O6 127.4(6) 5_655 5_656 ? O7 AM O6 90.9(7) . 5_656 ? O7 AM O6 104.8(6) 5_655 5_656 ? O6 AM O6 105.1(12) 2_656 5_656 ? A2M AM Cl3 136(3) . 5_656 ? A2 AM Cl3 119.4(19) . 5_656 ? A2 AM Cl3 119.4(19) 5_655 5_656 ? AM AM Cl3 136(3) 5_655 5_656 ? O7 AM Cl3 139.2(15) . 5_656 ? O7 AM Cl3 67.1(6) 5_655 5_656 ? O6 AM Cl3 65.8(7) 2_656 5_656 ? O6 AM Cl3 65.8(7) 5_656 5_656 ? A2M AM Si1 82(2) . . ? A2 AM Si1 104(2) . . ? A2 AM Si1 65.0(15) 5_655 . ? AM AM Si1 82(2) 5_655 . ? O7 AM Si1 27.2(2) . . ? O7 AM Si1 140.4(10) 5_655 . ? O6 AM Si1 71.9(4) 2_656 . ? O6 AM Si1 114.2(9) 5_656 . ? Cl3 AM Si1 135.4(10) 5_656 . ? A2M AM Si1 82(2) . 6 ? A2 AM Si1 65.0(15) . 6 ? A2 AM Si1 104(2) 5_655 6 ? AM AM Si1 82(2) 5_655 6 ? O7 AM Si1 27.2(2) . 6 ? O7 AM Si1 140.4(10) 5_655 6 ? O6 AM Si1 114.2(9) 2_656 6 ? O6 AM Si1 71.9(4) 5_656 6 ? Cl3 AM Si1 135.4(10) 5_656 6 ? Si1 AM Si1 54.0(4) . 6 ? A2M AM Si1 78(2) . 5_655 ? A2 AM Si1 61.9(15) . 5_655 ? A2 AM Si1 100(2) 5_655 5_655 ? AM AM Si1 78(2) 5_655 5_655 ? O7 AM Si1 148.0(8) . 5_655 ? O7 AM Si1 27.6(2) 5_655 5_655 ? O6 AM Si1 121.0(8) 2_656 5_655 ? O6 AM Si1 78.8(4) 5_656 5_655 ? Cl3 AM Si1 62.9(5) 5_656 5_655 ? Si1 AM Si1 160.0(12) . 5_655 ? Si1 AM Si1 122.3(4) 6 5_655 ? _refine_diff_density_max 0.371 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.058 _shelx_res_file ; TITL NYSM23521_0m_c.res in C2/m NYSM23521_0m_c.res created by SHELXL-2018/3 at 15:10:01 on 20-Mar-2020 REM Old TITL NYSM23521_0m in C2/m CELL 0.71073 9.9124 18.2035 5.3622 90.000 104.895 90.000 ZERR 2.000 0.0003 0.0005 0.0001 0.000 0.000 0.000 LATT 7 SYMM -X, Y, -Z SFAC O H NA MG SI CA FE CL AL K UNIT 46.3176 3.48 0.49188 4.8919 15.592 3.95028 5.15782 1.68236 0 1.34202 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 293 SIZE 0.135 0.186 0.247 EADP MGM1 FEM1 HTAB EXYZ MGM2 FEM2 EADP MGM2 FEM2 EADP MGM3 FEM3 OMIT -2 6 1 OMIT 0 0 2 OMIT 4 0 0 OMIT 0 8 0 OMIT 1 1 2 OMIT 5 1 0 OMIT 1 3 2 REM EXYZ SI1 AL1 REM EADP SI1 AL1 REM EXYZ SI2 AL2 REM EADP SI2 AL2 DFIX 0.9 0.03 O3 H3 CONN FEM1 8 CONN MGM1 8 CONN FEM2 6 CONN MGM2 6 CONN MGM3 8 CONN FEM3 8 CONN SI1 4 CONN SI2 4 CONN M4 8 L.S. 12 BOND FMAP 2 PLAN 20 HTAB EADP O3 CL3 ACTA WGHT 0.014400 0.637500 EXTI 0.004024 FVAR 0.31250 0.41690 0.65650 0.29825 0.98756 0.96644 0.98247 FVAR 0.57941 0.67107 0.04577 0.07662 MOLE 1 REM MGM1 4 0.000000 0.090678 0.500000 20.50000 0.00859 0.01185 = 0.00661 0.00000 0.00291 0.00000 FEM1 7 0.000000 0.095711 0.500000 -20.50000 0.00859 0.01185 = 0.00661 0.00000 0.00291 0.00000 MGM2 4 0.000000 0.178162 0.000000 30.50000 0.00589 0.00591 = 0.00631 0.00000 0.00197 0.00000 FEM2 7 0.000000 0.178162 0.000000 -30.50000 0.00589 0.00591 = 0.00631 0.00000 0.00197 0.00000 MGM3 4 0.000000 0.000000 0.000000 40.25000 0.00843 0.00612 = 0.00874 0.00000 0.00055 0.00000 FEM3 7 0.000000 0.000000 0.000000 -40.25000 0.00843 0.00612 = 0.00874 0.00000 0.00055 0.00000 REM REM M4 6 0.000000 0.280628 0.500000 50.50000 0.01143 0.00899 = 0.01220 0.00000 0.00678 0.00000 M4' 7 0.000000 0.256857 0.500000 -50.50000 0.01752 REM REM SI1 5 0.278324 0.086063 0.301450 61.00000 0.00673 0.00687 = 0.00710 -0.00015 0.00163 -0.00050 REM AL1 9 0.278349 0.086007 0.301281 -61.00000 0.00506 0.00522 = REM 0.00552 -0.00009 0.00123 -0.00048 SI2 5 0.291369 0.173666 0.812214 71.00000 0.00579 0.00623 = 0.00587 0.00059 0.00197 0.00004 REM AL2 9 0.291316 0.173588 0.811951 -71.00000 0.00538 0.00574 = REM 0.00539 0.00062 0.00178 -0.00001 REM REM O1 1 0.103581 0.090933 0.214488 11.00000 0.00988 0.01249 = 0.00933 -0.00122 0.00320 -0.00195 O2 1 0.120890 0.176933 0.735769 11.00000 0.00713 0.01294 = 0.01059 0.00126 0.00175 0.00101 REM O3 1 0.108658 0.000000 0.707005 80.50000 0.01010 0.00965 = 0.00974 0.00000 0.00340 0.00000 H3 2 0.016613 0.000000 0.635404 10.29000 0.81349 CL3 8 0.163782 0.000000 0.735079 -80.50000 0.01010 0.00965 = 0.00974 0.00000 0.00340 0.00000 REM O4 1 0.368966 0.250270 0.794570 11.00000 0.01349 0.00938 = 0.01252 0.00039 0.00569 -0.00158 O5 1 0.348734 0.137417 0.101990 11.00000 0.01011 0.01340 = 0.01105 0.00465 0.00169 0.00023 O6 1 0.343366 0.121919 0.599560 11.00000 0.01020 0.01478 = 0.01342 -0.00441 0.00370 0.00036 O7 1 0.335488 0.000000 0.296847 10.50000 0.01259 0.01447 = 0.02142 0.00000 0.00391 0.00000 A2M 10 0.500000 0.000000 0.000000 90.25000 0.05809 0.03519 = 0.07995 0.00000 0.06167 0.00000 A2 3 0.500000 -0.035042 0.000000 100.50000 0.02665 AM 3 0.543074 0.000000 0.102512 110.50000 0.08113 REM MOLE 2 HKLF 4 REM NYSM23521_0m_c.res in C2/m REM wR2 = 0.034323, GooF = S = 1.13700, Restrained GooF = 1.13668 for all data REM R1 = 0.013399 for 1780 Fo > 4sig(Fo) and 0.013698 for all 1809 data REM 123 parameters refined using 1 restraints END WGHT 0.0145 0.6394 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.371, deepest hole -0.212, 1-sigma level 0.058 Q1 1 0.5293 -0.0352 0.0839 11.00000 0.05 0.37 Q2 1 0.0680 0.0000 0.0248 10.50000 0.05 0.32 Q3 1 0.2044 0.1719 0.7781 11.00000 0.05 0.29 Q4 1 0.3073 0.1497 0.6887 11.00000 0.05 0.28 Q5 1 0.0737 0.0908 0.5337 11.00000 0.05 0.27 Q6 1 0.3452 0.2121 0.8120 11.00000 0.05 0.26 Q7 1 0.3126 0.1617 -0.0261 11.00000 0.05 0.24 Q8 1 0.3115 0.0407 0.3179 11.00000 0.05 0.24 Q9 1 0.3147 0.1015 0.4807 11.00000 0.05 0.22 Q10 1 0.1895 0.0855 0.2798 11.00000 0.05 0.22 Q11 1 0.2728 0.0000 0.2723 10.50000 0.05 0.22 Q12 1 0.0919 0.0210 0.7438 11.00000 0.05 0.21 Q13 1 0.0987 0.0000 0.8044 10.50000 0.05 0.20 Q14 1 0.2197 0.0000 0.7545 10.50000 0.05 0.20 Q15 1 0.3209 0.1222 0.1948 11.00000 0.05 0.20 Q16 1 0.0000 0.1405 0.5000 10.50000 0.05 0.19 Q17 1 0.3266 0.1024 0.1297 11.00000 0.05 0.19 Q18 1 0.0923 0.1758 0.8536 11.00000 0.05 0.19 Q19 1 0.1080 0.0000 0.6204 10.50000 0.05 0.18 Q20 1 0.0334 0.0891 0.0323 11.00000 0.05 0.18 ; 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585.54 6.60 2 10 0 583.34 6.80 -4 -10 0 1235.68 15.10 -4 -10 0 1228.48 16.40 4 -10 0 1219.98 16.00 4 -10 0 1238.28 13.80 4 10 0 1219.88 15.70 4 10 0 1225.88 14.90 -4 10 0 1200.78 15.30 -6 -10 0 296.67 4.00 6 -10 0 306.07 4.80 -6 -10 0 300.37 4.70 -6 -10 0 292.47 4.50 -6 10 0 300.07 4.40 -6 10 0 297.67 4.20 6 10 0 297.67 3.90 6 10 0 300.77 4.60 6 10 0 296.27 4.60 8 -10 0 305.17 5.10 -8 -10 0 295.87 4.90 -8 -10 0 301.37 4.90 -8 10 0 308.87 4.60 8 10 0 301.77 5.00 -8 10 0 297.77 4.70 -10 -10 0 420.76 6.70 10 -10 0 428.26 6.70 -10 -10 0 422.36 6.60 -10 10 0 426.76 6.20 -10 10 0 420.76 6.20 10 10 0 416.76 6.70 12 -10 0 242.88 4.90 -12 -10 0 242.08 4.90 12 10 0 243.08 5.00 -1 -11 0 3449.75 39.90 -1 -11 0 3411.06 54.29 -1 -11 0 3270.67 73.39 1 -11 0 3360.06 41.00 1 -11 0 3428.76 38.10 1 -11 0 3412.16 39.40 1 11 0 3362.26 38.90 -1 11 0 3268.37 40.90 -1 11 0 3451.05 37.80 1 11 0 3220.78 40.40 3 -11 0 1432.66 17.80 -3 -11 0 1428.16 18.00 3 -11 0 1352.16 18.90 -3 -11 0 1462.05 18.30 3 -11 0 1411.36 17.60 -3 11 0 1420.06 18.40 3 11 0 1414.96 17.90 3 11 0 1393.86 17.20 -5 -11 0 6.60 0.50 -5 -11 0 5.20 0.60 5 -11 0 4.60 0.60 -5 11 0 4.70 0.40 5 11 0 5.70 0.40 5 11 0 5.00 0.60 -5 11 0 6.30 0.60 -7 -11 0 3864.71 50.29 -7 -11 0 3967.30 49.10 7 -11 0 3919.61 87.89 -7 11 0 3921.61 48.50 7 11 0 3851.31 48.70 -7 11 0 3980.00 47.20 9 -11 0 87.49 2.50 -9 -11 0 90.69 2.50 -9 -11 0 90.39 2.50 -9 11 0 93.29 2.30 9 11 0 91.29 2.50 -9 11 0 87.89 2.20 -11 -11 0 905.61 12.10 11 -11 0 929.31 12.30 -11 -11 0 908.31 12.20 11 11 0 914.71 12.30 -13 -11 0 160.98 4.80 13 -11 0 162.28 4.00 13 11 0 160.28 4.50 0 -12 0 5038.60 68.29 0 -12 0 4971.10 58.49 0 -12 0 4905.91 82.29 0 12 0 4908.11 80.59 0 12 0 4914.41 72.39 -2 -12 0 76.69 1.60 2 -12 0 76.29 1.50 2 -12 0 77.39 1.50 2 -12 0 75.29 1.80 -2 -12 0 74.79 1.60 2 12 0 76.79 1.60 -2 12 0 77.79 1.80 2 12 0 74.29 1.50 -2 12 0 78.69 1.20 -4 -12 0 510.25 6.10 -4 -12 0 479.65 6.30 4 -12 0 477.55 6.70 4 -12 0 495.25 6.00 4 12 0 488.85 6.30 4 12 0 482.55 6.10 -4 12 0 484.45 6.50 6 -12 0 5.00 0.70 -6 -12 0 3.40 0.50 -6 12 0 4.10 0.50 6 12 0 5.00 0.70 -6 12 0 4.10 0.60 6 12 0 4.60 0.60 -8 -12 0 217.78 4.00 -8 -12 0 219.08 4.20 8 -12 0 214.78 4.20 -8 12 0 222.88 3.60 -8 12 0 216.18 3.90 8 12 0 209.68 4.00 -10 -12 0 607.34 8.80 -10 -12 0 595.84 8.70 10 -12 0 591.54 8.80 10 12 0 593.94 8.80 -10 12 0 597.84 8.20 -12 -12 0 79.59 2.70 12 -12 0 83.49 2.80 12 12 0 80.49 2.80 1 -13 0 4.30 0.40 -1 -13 0 4.40 0.50 1 -13 0 4.90 0.60 1 -13 0 5.00 0.40 -1 -13 0 5.20 0.30 -1 -13 0 4.70 0.40 -1 13 0 4.50 0.30 -1 13 0 4.50 0.50 1 13 0 4.30 0.40 1 13 0 3.90 0.50 3 -13 0 23.50 0.80 -3 -13 0 22.40 0.90 -3 -13 0 22.90 0.90 3 -13 0 22.90 0.80 3 -13 0 27.90 1.10 3 13 0 22.50 0.90 3 13 0 24.70 0.90 -3 13 0 22.60 1.00 -5 -13 0 169.18 2.80 -5 -13 0 166.48 3.10 5 -13 0 166.28 3.30 5 13 0 173.08 2.80 5 13 0 168.88 3.10 -5 13 0 186.78 3.30 -5 13 0 172.78 2.80 7 -13 0 55.09 1.90 -7 -13 0 54.89 1.80 -7 13 0 56.69 1.50 7 13 0 54.39 1.80 -7 13 0 56.79 1.70 -9 -13 0 136.09 3.20 9 -13 0 137.89 3.40 -9 13 0 137.39 3.00 9 13 0 139.79 3.30 -11 -13 0 33.10 1.70 11 -13 0 29.10 1.70 11 13 0 32.00 1.70 0 -14 0 72.09 1.30 0 -14 0 72.29 1.80 0 -14 0 74.89 1.60 0 14 0 70.79 1.70 0 14 0 71.89 1.40 2 -14 0 65.69 1.40 -2 -14 0 63.59 1.50 2 -14 0 65.29 1.80 -2 -14 0 66.99 1.30 -2 -14 0 67.19 1.60 2 -14 0 66.19 1.40 -2 14 0 67.09 1.20 2 14 0 66.59 1.60 2 14 0 64.09 1.50 -2 14 0 64.99 1.70 4 -14 0 6.40 0.50 4 -14 0 6.60 0.70 -4 -14 0 6.40 0.60 -4 -14 0 5.70 0.50 -4 14 0 5.40 0.60 4 14 0 5.10 0.60 6 -14 0 59.49 2.00 -6 -14 0 56.79 1.80 -6 14 0 57.29 1.80 -6 14 0 58.69 1.50 6 14 0 58.19 1.80 8 -14 0 0.40 0.40 -8 -14 0 0.70 0.40 8 14 0 0.60 0.40 -8 14 0 0.60 0.30 10 -14 0 95.69 2.90 -10 -14 0 98.79 2.80 -10 14 0 97.79 2.60 10 14 0 94.29 2.80 -12 -14 0 225.68 4.90 12 -14 0 225.48 5.00 12 14 0 224.58 4.90 1 -15 0 133.59 2.10 -1 -15 0 137.39 2.60 1 -15 0 136.39 2.30 -1 -15 0 137.89 2.40 1 -15 0 133.49 2.70 1 15 0 138.59 2.20 -1 15 0 139.99 2.70 -1 15 0 134.79 2.00 1 15 0 134.69 2.60 -3 -15 0 62.59 1.60 3 -15 0 61.89 1.50 3 -15 0 59.69 1.80 -3 -15 0 61.49 1.60 3 -15 0 62.99 1.50 3 15 0 62.99 1.50 -3 15 0 64.99 1.80 3 15 0 59.79 1.60 -5 -15 0 134.69 2.80 5 -15 0 136.39 3.10 -5 -15 0 134.39 2.50 5 15 0 135.19 2.50 -5 15 0 135.09 2.90 -5 15 0 137.39 2.50 5 15 0 134.59 2.70 -7 -15 0 474.25 6.90 7 -15 0 465.55 7.20 -7 15 0 474.55 6.90 7 15 0 473.55 6.90 -9 -15 0 21.40 1.30 9 -15 0 23.50 1.50 -9 15 0 24.60 1.30 9 15 0 23.20 1.40 -11 -15 0 28.50 1.60 11 -15 0 27.60 1.70 -11 15 0 25.60 1.40 11 15 0 25.90 1.60 0 -16 0 12.30 0.80 0 -16 0 12.90 0.70 0 16 0 12.50 0.60 0 16 0 12.20 0.80 -2 -16 0 26.40 1.10 -2 -16 0 26.10 1.00 2 -16 0 25.60 1.20 2 -16 0 26.60 0.90 2 16 0 27.40 0.90 2 16 0 28.20 1.10 -2 16 0 25.80 1.20 -4 -16 0 576.14 7.40 4 -16 0 591.84 7.20 -4 -16 0 575.44 7.60 4 -16 0 574.44 8.10 4 16 0 587.14 7.50 -4 16 0 575.14 7.90 4 16 0 567.24 7.50 -6 -16 0 126.49 2.80 6 -16 0 125.59 3.10 6 16 0 125.39 2.80 -6 16 0 122.29 2.90 -8 -16 0 19.40 1.20 8 -16 0 17.90 1.30 -8 16 0 18.60 1.20 8 16 0 18.20 1.20 -10 -16 0 163.88 3.90 10 -16 0 169.68 4.10 10 16 0 164.38 3.90 -10 16 0 166.38 3.70 1 -17 0 38.50 1.40 -1 -17 0 38.40 1.20 -1 -17 0 36.90 1.30 1 -17 0 37.10 1.20 1 17 0 35.50 1.00 1 17 0 36.80 1.30 -1 17 0 36.40 1.40 3 -17 0 58.79 1.90 3 -17 0 57.19 1.50 -3 -17 0 55.39 1.60 -3 -17 0 55.99 1.60 3 17 0 54.69 1.60 3 17 0 55.19 1.50 -3 17 0 55.69 1.80 -5 -17 0 7.40 0.70 5 -17 0 6.10 0.80 -5 17 0 8.40 0.80 5 17 0 7.10 0.70 5 17 0 8.00 0.70 -7 -17 0 75.49 2.30 7 -17 0 74.19 2.50 -7 17 0 72.39 2.30 7 17 0 75.09 2.20 9 -17 0 67.89 2.50 -9 -17 0 70.09 2.40 9 17 0 72.09 2.40 -9 17 0 71.59 2.30 -11 -17 0 10.40 1.20 11 -17 0 10.50 1.30 -11 17 0 11.60 1.10 11 17 0 9.90 1.20 0 -18 0 103.19 2.10 0 -18 0 99.49 2.40 0 18 0 99.49 2.40 -2 -18 0 269.77 4.20 2 -18 0 268.97 4.70 2 -18 0 276.87 4.00 -2 -18 0 266.97 4.30 2 18 0 270.97 4.00 -2 18 0 272.37 4.60 2 18 0 268.67 4.40 -4 -18 0 154.18 3.40 -4 -18 0 153.58 3.10 4 -18 0 154.18 3.50 -4 18 0 155.08 3.40 4 18 0 155.98 3.00 4 18 0 155.18 3.00 -6 -18 0 368.86 5.90 6 -18 0 377.56 6.30 -6 18 0 375.16 6.10 6 18 0 369.76 5.80 8 -18 0 1.10 0.60 -8 -18 0 2.90 0.60 8 18 0 2.20 0.60 -8 18 0 2.20 0.60 -10 -18 0 149.09 3.80 10 -18 0 152.88 4.00 10 18 0 156.28 3.80 -10 18 0 149.09 3.70 -1 -19 0 2.30 0.50 1 -19 0 0.90 0.40 -1 19 0 5.00 0.70 1 19 0 0.80 0.40 -3 -19 0 197.68 3.60 -3 -19 0 199.08 3.60 3 -19 0 197.98 4.00 3 19 0 198.28 3.70 3 19 0 203.38 3.40 -3 19 0 193.28 3.90 -5 -19 0 60.59 1.90 5 -19 0 69.29 2.30 5 19 0 63.09 1.90 -5 19 0 65.29 2.10 7 -19 0 87.59 2.80 -7 -19 0 89.09 2.60 -7 19 0 87.39 2.60 7 19 0 87.69 2.50 -9 -19 0 1.50 0.60 9 -19 0 1.30 0.60 9 19 0 2.50 0.70 -9 19 0 1.90 0.60 0 -20 0 109.79 2.30 0 -20 0 104.09 2.70 0 20 0 108.09 2.70 2 -20 0 116.69 2.90 -2 -20 0 121.09 2.70 -2 -20 0 116.79 2.50 2 20 0 119.79 2.80 -2 20 0 117.29 2.90 4 -20 0 119.09 3.10 -4 -20 0 117.79 2.70 4 20 0 119.29 2.70 -4 20 0 118.59 3.00 4 20 0 119.29 2.60 6 -20 0 1.50 0.60 -6 -20 0 1.20 0.50 6 20 0 1.00 0.40 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4.40 3 23 0 200.28 4.10 -3 23 0 205.28 4.40 5 -23 0 285.17 5.70 -5 -23 0 287.37 5.10 -5 23 0 288.57 5.50 -7 -23 0 322.17 5.90 7 -23 0 334.47 6.50 7 23 0 330.97 5.70 -7 23 0 328.27 6.10 0 -24 0 710.53 10.10 0 24 0 710.13 10.10 2 -24 0 136.69 3.50 -2 24 0 134.89 3.50 2 24 0 132.19 3.30 4 -24 0 6.60 1.00 -4 24 0 7.70 1.00 6 -24 0 8.80 1.20 -6 -24 0 6.00 0.90 -6 24 0 7.40 1.10 1 -25 0 0.30 0.40 1 25 0 0.40 0.40 -1 25 0 -0.10 0.40 3 -25 0 0.30 0.50 -3 25 0 0.40 0.50 5 -25 0 8.10 1.20 -5 25 0 7.70 1.10 0 -26 0 291.87 5.60 0 26 0 290.67 5.60 2 -26 0 0.60 0.50 -2 26 0 0.30 0.50 2 26 0 1.40 0.60 4 -26 0 17.40 1.50 -4 26 0 18.90 1.80 1 -27 0 11.40 1.20 -1 27 0 12.10 1.20 1 27 0 14.20 1.30 3 -27 0 90.89 3.40 -14 0 1 107.99 3.00 14 0 -1 111.29 3.10 12 0 -1 2.80 0.60 -12 0 1 3.20 0.60 -10 0 1 5.70 0.60 -10 0 1 5.50 0.70 10 0 -1 4.90 0.70 -8 0 1 82.79 1.90 8 0 -1 86.79 2.00 -8 0 1 86.29 1.70 8 0 -1 85.39 1.80 8 0 -1 83.09 1.70 -8 0 1 84.39 1.80 -6 0 1 12.70 0.60 6 0 -1 12.30 0.60 -6 0 1 13.10 0.50 6 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1.90 -9 5 -4 51.89 2.30 14 -6 -4 11.70 1.30 -14 6 4 13.60 1.20 -12 -6 4 8.20 0.90 -12 -6 4 7.50 0.90 12 -6 -4 7.50 1.00 12 6 -4 8.70 1.10 -12 6 4 6.90 0.90 12 6 -4 7.80 1.10 -10 -6 4 71.39 2.20 10 -6 -4 74.69 2.20 -10 -6 4 70.79 2.10 10 -6 -4 71.29 2.20 10 6 -4 68.59 2.30 10 6 -4 71.59 2.30 -10 6 4 69.89 2.30 8 -6 -4 14.40 1.00 8 -6 -4 13.80 0.80 8 -6 -4 14.50 1.00 -8 -6 4 15.20 0.90 -8 -6 4 14.30 1.00 -8 6 4 14.40 1.00 8 6 -4 13.60 1.00 8 6 -4 14.60 1.10 6 -6 -4 4.60 0.60 6 -6 -4 4.20 0.60 -6 -6 4 3.30 0.50 6 -6 -4 4.20 0.50 -6 -6 4 4.30 0.50 6 6 -4 3.90 0.60 -6 6 4 4.40 0.60 6 6 -4 4.40 0.50 6 6 -4 4.50 0.60 -4 -6 4 37.90 1.30 4 -6 -4 37.30 1.20 4 -6 -4 43.80 1.30 -4 -6 4 38.80 1.30 -4 6 4 38.50 1.30 -4 6 4 39.20 1.30 4 6 -4 37.80 1.20 4 6 -4 40.80 1.50 4 6 -4 38.80 1.00 2 -6 -4 12.50 0.70 -2 -6 4 12.90 0.70 2 -6 -4 13.00 0.70 -2 -6 4 12.90 0.80 2 -6 -4 13.00 0.70 -2 -6 4 12.40 0.60 2 6 -4 12.80 0.50 2 6 -4 12.50 0.60 -2 6 4 11.50 0.70 -2 6 4 12.00 0.70 2 6 -4 12.20 0.80 0 -6 -4 0.60 0.30 0 -6 4 0.60 0.30 0 -6 -4 0.10 0.20 0 -6 -4 1.30 0.30 0 -6 4 0.10 0.20 0 6 4 0.30 0.20 0 6 4 0.00 0.20 0 6 -4 0.10 0.20 0 6 -4 0.80 0.30 2 -6 4 15.80 0.90 -2 -6 -4 15.60 0.80 2 -6 4 16.00 0.90 -2 -6 -4 15.00 1.00 -2 -6 -4 14.90 0.90 2 6 4 17.20 0.90 -2 6 -4 16.10 0.80 -4 -6 -4 82.49 2.50 -4 -6 -4 83.99 2.10 4 -6 4 84.89 2.40 4 6 4 85.99 2.30 4 6 4 83.99 2.10 -4 6 -4 82.39 2.20 -6 -6 -4 86.19 2.70 -6 -6 -4 81.89 2.30 6 -6 4 80.69 2.50 6 6 4 86.59 2.30 6 6 4 81.19 2.40 -6 6 -4 85.29 2.40 8 -6 4 13.40 1.20 -8 -6 -4 13.70 1.10 -8 -6 -4 13.10 1.30 8 6 4 14.90 1.20 8 6 4 13.50 1.10 -8 6 -4 13.40 1.10 -10 -6 -4 35.00 1.90 10 -6 4 40.00 2.40 -10 -6 -4 37.10 2.10 10 6 4 37.00 1.90 -10 6 -4 36.40 2.00 10 6 4 37.60 1.80 -10 6 -4 35.20 2.20 -13 -7 4 191.88 4.20 13 -7 -4 200.48 4.40 -13 -7 4 199.78 4.30 13 7 -4 199.78 4.60 -13 7 4 197.98 4.40 13 7 -4 194.68 4.50 11 -7 -4 5.80 0.80 -11 -7 4 5.40 0.80 -11 -7 4 5.20 0.80 -11 7 4 5.40 0.80 11 7 -4 5.90 0.90 11 7 -4 6.20 0.90 -9 -7 4 4.90 0.70 9 -7 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7 -4 105.59 2.10 -3 7 -4 105.19 2.50 -5 -7 -4 410.56 6.70 5 -7 4 403.86 6.50 -5 -7 -4 400.76 6.00 -5 7 -4 403.06 6.20 5 7 4 396.86 6.30 5 7 4 401.66 6.10 7 -7 4 27.40 1.60 -7 -7 -4 29.30 1.50 -7 -7 -4 30.60 1.70 -7 7 -4 29.40 1.50 7 7 4 31.60 1.50 7 7 4 30.70 1.60 -9 -7 -4 5.60 1.10 -9 -7 -4 4.40 0.80 9 -7 4 4.80 0.90 -9 7 -4 5.50 0.90 9 7 4 5.80 0.90 9 7 4 4.50 0.80 -14 -8 4 32.50 1.80 14 -8 -4 31.90 1.80 14 8 -4 32.50 1.90 -12 -8 4 11.50 1.00 12 -8 -4 12.80 1.20 -12 -8 4 12.00 1.00 12 8 -4 13.90 1.30 -12 8 4 13.40 1.20 12 8 -4 13.10 1.20 10 -8 -4 117.69 3.00 10 -8 -4 117.89 2.90 -10 -8 4 114.19 2.90 -10 -8 4 118.79 2.90 10 8 -4 114.89 3.20 -10 8 4 114.59 3.00 10 8 -4 114.89 3.00 -8 -8 4 565.04 7.80 -8 -8 4 553.34 7.60 8 -8 -4 552.14 7.60 8 -8 -4 542.05 7.30 8 -8 -4 532.95 7.60 -8 8 4 545.95 7.90 8 8 -4 538.25 8.10 8 8 -4 553.44 7.80 -6 -8 4 483.15 6.60 6 -8 -4 473.25 6.60 -6 -8 4 469.85 6.70 6 -8 -4 481.95 6.60 6 -8 -4 476.15 6.50 6 8 -4 479.75 7.10 6 8 -4 482.85 6.70 -6 8 4 476.05 6.80 -4 -8 4 3.20 0.50 -4 -8 4 3.10 0.50 4 -8 -4 4.30 0.50 4 -8 -4 3.50 0.50 4 8 -4 4.40 0.50 -4 8 4 3.70 0.50 -4 8 4 3.70 0.50 4 8 -4 3.40 0.60 2 -8 -4 10.00 0.70 -2 -8 4 9.40 0.70 -2 -8 4 9.80 0.60 2 -8 -4 9.40 0.70 2 -8 -4 10.50 0.70 -2 8 4 11.00 0.70 2 8 -4 10.80 0.70 -2 8 4 10.20 0.70 2 8 -4 9.50 0.60 2 8 -4 9.50 0.70 0 -8 4 54.49 1.50 0 -8 4 53.49 1.60 0 -8 -4 54.59 1.60 0 -8 -4 53.59 1.60 0 8 4 55.99 1.40 0 8 -4 56.89 1.50 0 8 -4 56.49 1.50 0 8 4 53.39 1.60 -2 -8 -4 23.90 1.20 2 -8 4 24.50 1.10 -2 -8 -4 24.90 0.90 -2 -8 -4 25.40 1.20 2 -8 4 25.70 1.20 2 8 4 25.20 1.10 -2 8 -4 23.70 1.00 -4 -8 -4 68.59 2.30 -4 -8 -4 70.89 1.90 -4 -8 -4 69.29 2.10 4 -8 4 72.69 2.20 -4 8 -4 73.69 2.10 4 8 4 71.09 2.00 -6 -8 -4 295.07 5.00 -6 -8 -4 301.07 5.70 6 -8 4 289.57 5.40 6 8 4 286.37 5.00 -6 8 -4 300.37 5.30 -8 -8 -4 127.39 3.70 8 -8 4 130.29 3.60 -8 -8 -4 130.69 3.30 8 8 4 130.69 3.30 -8 8 -4 130.49 3.40 -10 -8 -4 31.70 1.90 10 8 4 33.20 1.70 -13 -9 4 23.30 1.50 13 -9 -4 23.90 1.50 13 9 -4 22.80 1.60 -13 9 4 22.80 1.50 13 9 -4 23.20 1.60 11 -9 -4 216.98 4.50 -11 -9 4 218.88 4.40 11 -9 -4 215.88 4.30 -11 -9 4 212.08 4.40 11 9 -4 218.98 4.70 -11 9 4 217.48 4.60 11 9 -4 217.08 4.60 -9 -9 4 7.30 0.80 -9 -9 4 5.90 0.80 9 -9 -4 7.10 0.80 9 -9 -4 8.20 0.80 9 -9 -4 7.70 0.90 9 9 -4 6.80 0.90 -9 9 4 6.30 0.80 9 9 -4 5.30 0.80 -7 -9 4 28.60 1.30 7 -9 -4 27.30 1.20 -7 -9 4 29.00 1.30 7 -9 -4 26.50 1.20 7 -9 -4 28.00 1.20 7 9 -4 28.20 1.30 -7 9 4 25.50 1.30 7 9 -4 25.60 1.40 -5 -9 4 111.69 2.60 -5 -9 4 112.89 2.50 5 -9 -4 110.89 2.40 5 -9 -4 108.79 2.40 5 9 -4 114.49 2.70 5 9 -4 113.99 2.40 -5 9 4 112.99 2.60 -5 9 4 113.09 2.50 -3 -9 4 13.10 0.80 3 -9 -4 12.60 0.80 3 -9 -4 12.40 0.80 3 -9 -4 12.50 0.70 3 9 -4 12.60 0.80 -3 9 4 13.50 0.80 3 9 -4 12.50 0.70 3 9 -4 12.20 0.80 -3 9 4 12.70 0.80 -1 -9 4 174.18 2.90 -1 -9 4 171.88 3.20 1 -9 -4 172.28 3.10 1 -9 -4 172.98 3.20 1 9 -4 171.98 3.10 -1 9 4 170.28 3.10 1 9 -4 170.78 3.10 -1 9 4 172.18 2.90 1 -9 4 31.90 1.30 1 -9 4 33.30 1.30 -1 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10 -4 729.83 9.70 6 -10 -4 216.98 3.80 6 -10 -4 210.48 3.80 -6 -10 4 214.78 3.90 -6 -10 4 215.68 4.00 6 10 -4 217.88 4.20 6 10 -4 213.68 3.80 -6 10 4 213.58 4.00 4 -10 -4 468.05 6.50 4 -10 -4 467.35 6.50 -4 -10 4 475.95 6.60 4 10 -4 478.05 6.30 4 10 -4 469.15 6.70 -4 10 4 479.35 6.70 -4 10 4 470.95 6.50 4 10 -4 464.65 6.80 2 -10 -4 190.58 3.40 -2 -10 4 190.88 3.50 2 -10 -4 192.48 3.30 2 -10 -4 195.68 3.30 2 10 -4 192.18 3.50 -2 10 4 193.18 3.30 2 10 -4 191.18 3.50 -2 10 4 195.18 3.40 0 -10 4 958.60 11.60 0 -10 4 948.71 11.30 0 -10 -4 944.31 11.70 0 -10 -4 959.20 11.70 0 10 -4 942.91 11.20 0 10 4 942.31 11.50 0 10 -4 940.31 11.40 0 10 4 950.50 11.10 -2 -10 -4 373.96 5.80 -2 -10 -4 371.36 5.90 2 -10 4 368.06 5.70 2 -10 4 364.86 5.70 2 10 4 372.06 5.60 -2 10 -4 370.56 5.30 4 -10 4 103.09 2.80 -4 -10 -4 112.19 2.40 -4 -10 -4 105.79 2.70 -4 -10 -4 108.79 3.00 -4 10 -4 111.29 2.30 -4 10 -4 104.29 2.70 4 10 4 109.19 2.70 -6 -10 -4 416.36 7.20 -6 -10 -4 422.06 6.40 -6 -10 -4 426.76 6.80 6 -10 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140.99 3.10 -3 13 4 136.99 2.90 -3 13 4 139.99 2.90 1 -13 -4 8.50 0.70 1 -13 -4 11.40 0.90 1 -13 -4 10.50 0.90 -1 -13 4 9.20 0.80 -1 13 4 9.00 0.80 1 13 -4 8.90 0.80 -1 13 4 13.10 0.80 1 13 -4 9.00 0.80 -1 -13 -4 64.89 2.00 1 -13 4 59.29 1.90 -1 -13 -4 63.59 2.10 1 -13 4 62.69 1.90 1 13 4 61.09 1.90 -1 13 -4 61.29 1.90 3 -13 4 54.99 1.90 3 -13 4 55.99 2.00 -3 -13 -4 56.79 2.10 -3 -13 -4 55.39 2.00 3 13 4 55.69 1.90 -3 13 -4 56.69 1.80 -5 -13 -4 79.89 2.70 5 -13 4 85.49 2.70 -5 -13 -4 79.19 2.50 -5 13 -4 83.79 2.50 5 13 4 83.59 2.50 -7 -13 -4 1.10 0.50 7 -13 4 0.60 0.50 -7 -13 -4 2.00 0.70 7 13 4 0.50 0.50 -7 13 -4 1.30 0.50 -9 -13 -4 6.90 1.20 -12 -14 4 72.79 3.40 12 14 -4 74.89 3.40 12 14 -4 76.89 2.70 10 -14 -4 82.49 2.60 10 -14 -4 84.49 2.70 -10 -14 4 84.29 2.70 10 -14 -4 82.79 2.50 -10 14 4 82.39 2.70 10 14 -4 83.59 2.90 10 14 -4 81.49 2.50 10 14 -4 79.89 2.60 8 -14 -4 132.69 3.20 8 -14 -4 137.09 3.10 -8 -14 4 131.39 3.30 8 -14 -4 136.29 3.30 -8 14 4 139.29 3.40 8 14 -4 142.99 3.30 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334.07 5.70 -3 15 -4 334.17 5.40 3 15 4 329.37 5.60 5 -15 4 60.19 2.30 -5 -15 -4 61.09 2.20 -5 -15 -4 60.59 2.40 5 15 4 58.89 2.20 -5 15 -4 61.49 2.30 -5 15 -4 60.89 2.20 -7 -15 -4 0.70 0.60 7 -15 4 0.10 0.50 -7 -15 -4 0.40 0.50 7 15 4 0.70 0.50 -7 15 -4 -0.10 0.40 -10 -16 4 2.90 0.70 10 -16 -4 2.40 0.70 10 -16 -4 3.40 0.80 10 16 -4 2.50 0.60 -10 16 4 2.60 0.70 10 16 -4 2.70 0.70 10 16 -4 2.50 0.80 8 -16 -4 248.38 4.80 -8 -16 4 240.48 4.80 8 -16 -4 240.98 4.80 8 -16 -4 242.28 4.40 -8 16 4 232.38 4.80 8 16 -4 239.68 5.10 8 16 -4 247.78 4.80 6 -16 -4 31.60 1.60 6 -16 -4 32.30 1.50 -6 -16 4 31.90 1.50 -6 16 4 34.10 1.40 6 16 -4 32.50 1.60 6 16 -4 33.30 1.70 -6 16 4 33.80 1.60 4 -16 -4 33.90 1.60 -4 -16 4 34.00 1.50 4 -16 -4 32.30 1.40 4 16 -4 34.90 1.50 -4 16 4 37.10 1.50 4 16 -4 33.60 1.60 -4 16 4 33.00 1.50 -2 -16 4 99.79 2.60 2 -16 -4 96.29 2.60 2 -16 -4 95.79 2.40 2 16 -4 101.49 2.60 -2 16 4 98.59 2.50 2 16 -4 95.59 2.60 -2 16 4 98.39 2.50 0 -16 -4 39.20 1.50 0 -16 4 39.00 1.60 0 -16 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1.00 0.50 10 10 -5 1.20 0.60 10 10 -5 2.20 0.70 -8 -10 5 85.59 2.60 8 -10 -5 88.09 2.50 8 -10 -5 86.19 2.30 8 -10 -5 84.29 2.50 -8 -10 5 84.19 2.40 8 10 -5 84.19 2.80 -8 10 5 82.89 2.60 8 10 -5 85.09 2.50 6 -10 -5 0.10 0.30 -6 -10 5 0.00 0.30 6 -10 -5 1.60 0.50 -6 -10 5 1.40 0.50 -6 10 5 0.60 0.40 6 10 -5 0.40 0.30 -6 10 5 0.40 0.40 6 10 -5 0.30 0.40 4 -10 -5 26.00 1.20 -4 -10 5 26.70 1.30 4 -10 -5 27.50 1.20 4 10 -5 27.70 1.30 4 10 -5 27.80 1.40 -4 10 5 27.40 1.30 -4 10 5 26.90 1.30 2 -10 -5 6.20 0.70 2 -10 -5 6.30 0.70 2 -10 -5 6.40 0.70 -2 -10 5 5.70 0.70 -2 10 5 5.30 0.60 2 10 -5 5.70 0.70 2 10 -5 5.30 0.70 0 -10 5 184.58 3.50 0 -10 5 187.18 3.70 0 -10 -5 186.78 3.70 0 -10 -5 186.78 3.70 0 10 5 187.28 3.70 0 10 -5 182.68 3.50 -2 -10 -5 58.99 2.10 -2 -10 -5 61.09 2.20 2 -10 5 58.79 2.00 2 -10 5 58.69 2.00 -2 10 -5 58.29 1.80 2 10 5 59.79 2.00 -4 -10 -5 103.99 3.10 4 -10 5 109.09 3.00 -4 -10 -5 107.39 3.00 4 10 5 101.39 2.80 -4 10 -5 107.79 2.90 6 -10 5 7.70 1.10 -6 -10 -5 9.50 1.10 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5 11.10 1.00 -3 -11 -5 12.30 1.10 -3 -11 -5 12.90 1.10 3 11 5 10.80 1.00 -5 -11 -5 40.90 2.10 -5 -11 -5 41.70 1.90 5 -11 5 42.70 2.00 -5 11 -5 40.80 1.90 5 11 5 41.20 1.80 7 -11 5 30.40 1.90 -7 -11 -5 29.80 2.00 -7 -11 -5 27.80 1.70 7 11 5 29.00 1.60 -7 11 -5 27.70 1.70 -12 -12 5 0.70 0.50 12 -12 -5 0.20 0.50 12 12 -5 0.90 0.90 12 12 -5 0.60 0.50 10 -12 -5 216.48 4.60 -10 -12 5 210.78 4.50 10 -12 -5 217.38 4.50 10 12 -5 212.78 5.00 10 12 -5 221.98 4.60 -10 12 5 216.38 4.80 -8 -12 5 60.79 2.10 8 -12 -5 65.19 2.10 8 -12 -5 57.89 2.10 8 -12 -5 59.99 2.10 8 12 -5 58.39 2.10 8 12 -5 58.19 2.40 8 12 -5 59.39 2.10 -8 12 5 62.49 2.30 6 -12 -5 62.69 2.00 -6 -12 5 62.09 2.10 6 -12 -5 59.89 2.00 -6 12 5 58.19 2.10 -6 12 5 62.79 2.00 6 12 -5 63.69 2.30 6 12 -5 60.79 2.10 4 -12 -5 95.99 2.50 -4 -12 5 96.59 2.60 4 -12 -5 93.19 2.40 4 12 -5 95.99 2.60 -4 12 5 94.29 2.50 -4 12 5 93.19 2.50 4 12 -5 93.19 2.60 2 -12 -5 75.59 2.10 -2 -12 5 76.99 2.30 2 -12 -5 78.89 2.30 2 12 -5 79.79 2.30 -2 12 5 80.79 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6.30 1.00 -5 -15 5 150.98 3.50 5 -15 -5 153.68 3.50 5 -15 -5 148.29 3.40 -5 15 5 149.29 3.40 5 15 -5 153.68 3.70 -5 15 5 149.39 3.50 5 15 -5 151.68 3.60 3 -15 -5 2.90 0.70 3 -15 -5 3.10 0.60 -3 -15 5 2.30 0.60 -3 15 5 5.10 0.70 3 15 -5 4.20 0.70 3 15 -5 3.00 0.60 -1 -15 5 1.00 0.50 1 -15 -5 1.10 0.50 1 -15 -5 3.50 0.70 -1 15 5 0.50 0.40 1 15 -5 1.00 0.50 -1 -15 -5 101.99 2.90 -1 -15 -5 102.29 2.90 1 -15 5 98.69 2.80 -1 15 -5 101.89 2.70 1 15 5 102.99 2.80 3 -15 5 4.00 0.70 -3 -15 -5 3.30 0.80 -3 -15 -5 4.00 0.80 3 -15 5 3.60 0.70 -3 15 -5 4.00 0.70 3 15 5 3.20 0.70 5 -15 5 88.69 3.00 -5 -15 -5 91.19 3.20 -5 -15 -5 88.69 2.90 5 15 5 84.29 2.80 -5 15 -5 88.89 2.90 10 16 -5 240.58 5.20 8 -16 -5 452.05 7.30 8 -16 -5 434.86 7.20 -8 -16 5 450.95 7.40 8 -16 -5 445.26 7.00 -8 16 5 450.15 7.60 8 16 -5 448.76 7.80 8 16 -5 441.56 7.40 6 -16 -5 456.65 7.20 -6 -16 5 444.16 7.20 6 -16 -5 447.06 7.10 6 16 -5 448.96 7.60 -6 16 5 441.66 7.20 -6 16 5 447.16 6.90 6 16 -5 450.85 7.30 4 -16 -5 887.51 11.50 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8 21.40 2.00 6 4 -8 19.40 1.90 4 -4 -8 151.38 4.00 4 -4 -8 154.88 3.60 2 -4 -8 83.29 2.70 -2 4 8 83.89 2.70 5 -5 -8 50.29 2.10 5 5 -8 47.70 2.20 3 -5 -8 17.90 1.40 -3 5 8 18.70 2.30 1 -5 -8 3.20 0.90 4 6 -8 16.10 1.30 5 7 -8 31.60 2.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 60874