data_MLNYSM19349_0m_a _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 H1.13 Ca1.97 Cl0.86 Fe3.45 K0.72 Mg1.59 Na0.11 O23.14 Si7.82' _chemical_formula_weight 962.32 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 9.9285(4) _cell_length_b 18.2576(7) _cell_length_c 5.3666(2) _cell_angle_alpha 90 _cell_angle_beta 104.8100(10) _cell_angle_gamma 90 _cell_volume 940.49(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7068 _cell_measurement_theta_min 2.231 _cell_measurement_theta_max 33.387 _exptl_crystal_description equant _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.398 _exptl_crystal_F_000 947 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.151 _exptl_crystal_size_mid 0.117 _exptl_crystal_size_min 0.104 _exptl_absorpt_coefficient_mu 4.118 _shelx_estimated_absorpt_T_min 0.575 _shelx_estimated_absorpt_T_max 0.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68 _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 10627 _diffrn_reflns_av_unetI/netI 0.0109 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.397 _diffrn_reflns_theta_max 33.387 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.957 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.957 _diffrn_reflns_point_group_measured_fraction_full 0.989 _reflns_number_total 1808 _reflns_number_gt 1728 _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^)+(0.0182P)^2^+0.6628P] 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 0.00151(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1808 _refine_ls_number_parameters 119 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0163 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0391 _refine_ls_wR_factor_gt 0.0386 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _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 0.0873(6) 0.500000 0.00853(11) Uani 0.223(3) 2 d S T P . . FeM1 Fe 0.000000 0.09503(5) 0.500000 0.00853(11) Uani 0.777(3) 2 d S T P . . MgM2 Mg 0.000000 0.17883(2) 0.000000 0.00572(8) Uani 0.500(3) 2 d S T P . . FeM2 Fe 0.000000 0.17883(2) 0.000000 0.00572(8) Uani 0.500(3) 2 d S T P . . MgM3 Mg 0.000000 0.000000 0.000000 0.00799(9) Uani 0.138(4) 4 d S T P . . FeM3 Fe 0.000000 0.000000 0.000000 0.00799(9) Uani 0.862(4) 4 d S T P . . M4 Ca 0.000000 0.28051(4) 0.500000 0.01077(10) Uani 0.984(3) 2 d S T P . . M4' Fe 0.000000 0.256(2) 0.500000 0.016(5) Uiso 0.016(3) 2 d S . P . . Si1 Si 0.27819(3) 0.08597(2) 0.30055(5) 0.00701(8) Uani 0.970(2) 1 d . . P . . Si2 Si 0.29141(2) 0.17336(2) 0.81107(4) 0.00583(8) Uani 0.985(2) 1 d . . P . . O1 O 0.10385(7) 0.09114(4) 0.21415(12) 0.01046(13) Uani 1 1 d . . . . . O2 O 0.12153(7) 0.17752(4) 0.73473(12) 0.01002(12) Uani 1 1 d . . . . . O3 O 0.1099(3) 0.000000 0.7061(4) 0.0095(2) Uani 0.568(3) 2 d DS T P . . H3 H 0.206(3) 0.000000 0.73(2) 0.21(6) Uiso 0.564 2 d DS . P . . Cl3 Cl 0.16383(11) 0.000000 0.73528(14) 0.0095(2) Uani 0.432(3) 2 d S T P . . O4 O 0.36918(7) 0.24964(4) 0.79414(12) 0.01152(13) Uani 1 1 d . . . . . O5 O 0.34801(6) 0.13682(4) 0.09961(12) 0.01145(13) Uani 1 1 d . . . . . O6 O 0.34304(7) 0.12203(4) 0.59757(12) 0.01247(13) Uani 1 1 d . . . . . O7 O 0.33483(10) 0.000000 0.2972(2) 0.01627(19) Uani 1 2 d S T P . . A2M K 0.500000 0.000000 0.000000 0.0569(5) Uani 0.722(10) 4 d S T P . . A2 Na 0.500000 -0.033(2) 0.000000 0.043(7) Uiso 0.056(9) 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 0.00886(11) 0.0107(3) 0.00659(10) 0.000 0.00298(7) 0.000 FeM1 0.00886(11) 0.0107(3) 0.00659(10) 0.000 0.00298(7) 0.000 MgM2 0.00599(12) 0.00516(12) 0.00619(12) 0.000 0.00189(8) 0.000 FeM2 0.00599(12) 0.00516(12) 0.00619(12) 0.000 0.00189(8) 0.000 MgM3 0.00879(14) 0.00583(13) 0.00832(13) 0.000 0.00033(9) 0.000 FeM3 0.00879(14) 0.00583(13) 0.00832(13) 0.000 0.00033(9) 0.000 M4 0.01234(13) 0.0093(2) 0.01290(13) 0.000 0.00738(8) 0.000 Si1 0.00698(12) 0.00686(12) 0.00708(12) -0.00018(7) 0.00158(8) -0.00057(7) Si2 0.00588(11) 0.00601(11) 0.00580(11) 0.00057(7) 0.00187(7) -0.00015(7) O1 0.0098(3) 0.0128(3) 0.0092(3) -0.0012(2) 0.0031(2) -0.0018(2) O2 0.0067(3) 0.0120(3) 0.0109(3) 0.0008(2) 0.0015(2) 0.0011(2) O3 0.0097(5) 0.0097(2) 0.0093(3) 0.000 0.0029(3) 0.000 Cl3 0.0097(5) 0.0097(2) 0.0093(3) 0.000 0.0029(3) 0.000 O4 0.0139(3) 0.0092(3) 0.0125(3) 0.0001(2) 0.0053(2) -0.0021(2) O5 0.0095(3) 0.0135(3) 0.0108(3) 0.0047(2) 0.0016(2) 0.0002(2) O6 0.0103(3) 0.0142(3) 0.0132(3) -0.0044(2) 0.0036(2) 0.0005(2) O7 0.0133(4) 0.0151(4) 0.0205(5) 0.000 0.0046(3) 0.000 A2M 0.0688(8) 0.0348(12) 0.0959(10) 0.000 0.0736(9) 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 2.0567(8) . ? MgM1 O1 2.0567(8) 2_556 ? MgM1 O3 2.083(8) . ? MgM1 O3 2.083(8) 5_556 ? MgM1 O2 2.231(8) 2_556 ? MgM1 O2 2.231(8) . ? MgM1 Cl3 2.394(7) 5_556 ? MgM1 Cl3 2.394(7) . ? FeM1 O1 2.0567(7) . ? FeM1 O1 2.0567(7) 2_556 ? FeM1 O2 2.1293(10) 2_556 ? FeM1 O2 2.1293(10) . ? FeM1 O3 2.1924(17) . ? FeM1 O3 2.1924(17) 5_556 ? FeM1 Cl3 2.4901(10) 5_556 ? FeM1 Cl3 2.4901(10) . ? MgM2 O4 1.9696(7) 7_556 ? MgM2 O4 1.9696(7) 8_454 ? MgM2 O1 2.0835(7) . ? MgM2 O1 2.0835(7) 2 ? MgM2 O2 2.0883(6) 2_556 ? MgM2 O2 2.0883(6) 1_554 ? MgM3 O1 2.1324(6) 5 ? MgM3 O1 2.1324(6) 6 ? MgM3 O1 2.1324(6) 2 ? MgM3 O1 2.1324(6) . ? MgM3 O3 2.135(2) 5_556 ? MgM3 O3 2.135(2) 1_554 ? MgM3 Cl3 2.4177(9) 5_556 ? MgM3 Cl3 2.4177(9) 1_554 ? FeM3 O1 2.1324(6) 5 ? FeM3 O1 2.1324(6) 6 ? FeM3 O1 2.1324(6) 2 ? FeM3 O1 2.1324(6) . ? FeM3 O3 2.135(2) 5_556 ? FeM3 O3 2.135(2) 1_554 ? FeM3 Cl3 2.4177(9) 5_556 ? FeM3 Cl3 2.4177(9) 1_554 ? M4 O4 2.3517(7) 7_556 ? M4 O4 2.3517(7) 8_455 ? M4 O2 2.4086(9) . ? M4 O2 2.4086(9) 2_556 ? M4 O6 2.5073(9) 7_556 ? M4 O6 2.5073(9) 8_455 ? M4 O5 2.7413(8) 7_556 ? M4 O5 2.7413(8) 8_455 ? M4' O2 2.08(3) . ? M4' O2 2.08(3) 2_556 ? M4' O4 2.2885(18) 7_556 ? M4' O4 2.2885(18) 8_455 ? Si1 O7 1.6689(4) . ? Si1 O1 1.6762(7) . ? Si1 O6 1.6924(7) . ? Si1 O5 1.6993(7) . ? Si2 O4 1.6063(7) . ? Si2 O2 1.6326(7) . ? Si2 O5 1.6473(6) 1_556 ? Si2 O6 1.6595(7) . ? O3 Cl3 0.518(2) . ? Cl3 A2M 3.2763(10) 1_556 ? Cl3 A2 3.330(8) 5_656 ? Cl3 A2 3.330(8) 1_556 ? O5 A2 2.57(3) 5_655 ? O5 A2M 3.0357(7) . ? O6 A2 2.84(2) 5_656 ? O6 A2M 3.2149(7) 1_556 ? O7 A2M 2.5633(10) . ? O7 A2 2.631(9) . ? O7 A2 2.631(9) 5_655 ? A2M A2 0.59(4) . ? A2M A2 0.59(4) 5_655 ? A2 A2 1.19(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 176.1(6) . 2_556 ? O1 MgM1 O3 97.3(3) . . ? O1 MgM1 O3 85.7(2) 2_556 . ? O1 MgM1 O3 85.7(2) . 5_556 ? O1 MgM1 O3 97.3(3) 2_556 5_556 ? O3 MgM1 O3 80.1(4) . 5_556 ? O1 MgM1 O2 81.7(2) . 2_556 ? O1 MgM1 O2 95.4(2) 2_556 2_556 ? O3 MgM1 O2 177.5(4) . 2_556 ? O3 MgM1 O2 97.52(5) 5_556 2_556 ? O1 MgM1 O2 95.4(2) . . ? O1 MgM1 O2 81.7(2) 2_556 . ? O3 MgM1 O2 97.52(5) . . ? O3 MgM1 O2 177.5(4) 5_556 . ? O2 MgM1 O2 84.9(4) 2_556 . ? O1 MgM1 Cl3 91.82(19) . 5_556 ? O1 MgM1 Cl3 90.77(19) 2_556 5_556 ? O3 MgM1 Cl3 87.9(4) . 5_556 ? O3 MgM1 Cl3 10.64(6) 5_556 5_556 ? O2 MgM1 Cl3 89.84(2) 2_556 5_556 ? O2 MgM1 Cl3 170.3(2) . 5_556 ? O1 MgM1 Cl3 90.77(19) . . ? O1 MgM1 Cl3 91.82(19) 2_556 . ? O3 MgM1 Cl3 10.65(6) . . ? O3 MgM1 Cl3 87.9(4) 5_556 . ? O2 MgM1 Cl3 170.3(2) 2_556 . ? O2 MgM1 Cl3 89.84(2) . . ? Cl3 MgM1 Cl3 96.5(4) 5_556 . ? O1 FeM1 O1 176.04(7) . 2_556 ? O1 FeM1 O2 84.23(3) . 2_556 ? O1 FeM1 O2 98.59(3) 2_556 2_556 ? O1 FeM1 O2 98.59(3) . . ? O1 FeM1 O2 84.23(3) 2_556 . ? O2 FeM1 O2 89.97(5) 2_556 . ? O1 FeM1 O3 93.97(6) . . ? O1 FeM1 O3 82.89(6) 2_556 . ? O2 FeM1 O3 172.67(6) 2_556 . ? O2 FeM1 O3 97.34(5) . . ? O1 FeM1 O3 82.89(6) . 5_556 ? O1 FeM1 O3 93.97(7) 2_556 5_556 ? O2 FeM1 O3 97.34(5) 2_556 5_556 ? O2 FeM1 O3 172.67(6) . 5_556 ? O3 FeM1 O3 75.37(11) . 5_556 ? O1 FeM1 Cl3 89.13(3) . 5_556 ? O1 FeM1 Cl3 88.12(3) 2_556 5_556 ? O2 FeM1 Cl3 89.71(2) 2_556 5_556 ? O2 FeM1 Cl3 172.20(3) . 5_556 ? O3 FeM1 Cl3 83.15(7) . 5_556 ? O3 FeM1 Cl3 10.42(5) 5_556 5_556 ? O1 FeM1 Cl3 88.12(3) . . ? O1 FeM1 Cl3 89.13(3) 2_556 . ? O2 FeM1 Cl3 172.20(3) 2_556 . ? O2 FeM1 Cl3 89.71(2) . . ? O3 FeM1 Cl3 10.42(5) . . ? O3 FeM1 Cl3 83.15(7) 5_556 . ? Cl3 FeM1 Cl3 91.66(5) 5_556 . ? O4 MgM2 O4 96.94(4) 7_556 8_454 ? O4 MgM2 O1 92.16(3) 7_556 . ? O4 MgM2 O1 168.89(3) 8_454 . ? O4 MgM2 O1 168.89(3) 7_556 2 ? O4 MgM2 O1 92.16(3) 8_454 2 ? O1 MgM2 O1 79.59(4) . 2 ? O4 MgM2 O2 92.19(3) 7_556 2_556 ? O4 MgM2 O2 88.67(3) 8_454 2_556 ? O1 MgM2 O2 84.60(3) . 2_556 ? O1 MgM2 O2 94.39(3) 2 2_556 ? O4 MgM2 O2 88.67(3) 7_556 1_554 ? O4 MgM2 O2 92.19(3) 8_454 1_554 ? O1 MgM2 O2 94.39(3) . 1_554 ? O1 MgM2 O2 84.60(3) 2 1_554 ? O2 MgM2 O2 178.69(4) 2_556 1_554 ? O1 MgM3 O1 77.41(4) 5 6 ? O1 MgM3 O1 102.59(4) 5 2 ? O1 MgM3 O1 180.00(4) 6 2 ? O1 MgM3 O1 180.0 5 . ? O1 MgM3 O1 102.59(4) 6 . ? O1 MgM3 O1 77.41(4) 2 . ? O1 MgM3 O3 97.48(5) 5 5_556 ? O1 MgM3 O3 82.52(5) 6 5_556 ? O1 MgM3 O3 97.48(5) 2 5_556 ? O1 MgM3 O3 82.52(5) . 5_556 ? O1 MgM3 O3 82.52(5) 5 1_554 ? O1 MgM3 O3 97.48(5) 6 1_554 ? O1 MgM3 O3 82.52(5) 2 1_554 ? O1 MgM3 O3 97.48(5) . 1_554 ? O3 MgM3 O3 180.00(11) 5_556 1_554 ? O1 MgM3 Cl3 90.66(2) 5 5_556 ? O1 MgM3 Cl3 89.34(2) 6 5_556 ? O1 MgM3 Cl3 90.66(2) 2 5_556 ? O1 MgM3 Cl3 89.34(2) . 5_556 ? O3 MgM3 Cl3 10.97(6) 5_556 5_556 ? O3 MgM3 Cl3 169.03(6) 1_554 5_556 ? O1 MgM3 Cl3 89.34(2) 5 1_554 ? O1 MgM3 Cl3 90.66(2) 6 1_554 ? O1 MgM3 Cl3 89.34(2) 2 1_554 ? O1 MgM3 Cl3 90.66(2) . 1_554 ? O3 MgM3 Cl3 169.03(6) 5_556 1_554 ? O3 MgM3 Cl3 10.97(6) 1_554 1_554 ? Cl3 MgM3 Cl3 180.00(3) 5_556 1_554 ? O1 FeM3 O1 77.41(4) 5 6 ? O1 FeM3 O1 102.59(4) 5 2 ? O1 FeM3 O1 180.00(4) 6 2 ? O1 FeM3 O1 180.0 5 . ? O1 FeM3 O1 102.59(4) 6 . ? O1 FeM3 O1 77.41(4) 2 . ? O1 FeM3 O3 97.48(5) 5 5_556 ? O1 FeM3 O3 82.52(5) 6 5_556 ? O1 FeM3 O3 97.48(5) 2 5_556 ? O1 FeM3 O3 82.52(5) . 5_556 ? O1 FeM3 O3 82.52(5) 5 1_554 ? O1 FeM3 O3 97.48(5) 6 1_554 ? O1 FeM3 O3 82.52(5) 2 1_554 ? O1 FeM3 O3 97.48(5) . 1_554 ? O3 FeM3 O3 180.00(11) 5_556 1_554 ? O1 FeM3 Cl3 90.66(2) 5 5_556 ? O1 FeM3 Cl3 89.34(2) 6 5_556 ? O1 FeM3 Cl3 90.66(2) 2 5_556 ? O1 FeM3 Cl3 89.34(2) . 5_556 ? O3 FeM3 Cl3 10.97(6) 5_556 5_556 ? O3 FeM3 Cl3 169.03(6) 1_554 5_556 ? O1 FeM3 Cl3 89.34(2) 5 1_554 ? O1 FeM3 Cl3 90.66(2) 6 1_554 ? O1 FeM3 Cl3 89.34(2) 2 1_554 ? O1 FeM3 Cl3 90.66(2) . 1_554 ? O3 FeM3 Cl3 169.03(6) 5_556 1_554 ? O3 FeM3 Cl3 10.97(6) 1_554 1_554 ? Cl3 FeM3 Cl3 180.00(3) 5_556 1_554 ? O4 M4 O4 152.92(5) 7_556 8_455 ? O4 M4 O2 83.08(3) 7_556 . ? O4 M4 O2 75.81(3) 8_455 . ? O4 M4 O2 75.81(3) 7_556 2_556 ? O4 M4 O2 83.08(3) 8_455 2_556 ? O2 M4 O2 77.35(4) . 2_556 ? O4 M4 O6 63.04(2) 7_556 7_556 ? O4 M4 O6 141.79(3) 8_455 7_556 ? O2 M4 O6 114.10(2) . 7_556 ? O2 M4 O6 134.41(2) 2_556 7_556 ? O4 M4 O6 141.79(3) 7_556 8_455 ? O4 M4 O6 63.04(2) 8_455 8_455 ? O2 M4 O6 134.41(2) . 8_455 ? O2 M4 O6 114.10(2) 2_556 8_455 ? O6 M4 O6 89.58(4) 7_556 8_455 ? O4 M4 O5 111.55(2) 7_556 7_556 ? O4 M4 O5 83.72(2) 8_455 7_556 ? O2 M4 O5 85.30(2) . 7_556 ? O2 M4 O5 160.32(3) 2_556 7_556 ? O6 M4 O5 61.70(2) 7_556 7_556 ? O6 M4 O5 72.09(3) 8_455 7_556 ? O4 M4 O5 83.72(2) 7_556 8_455 ? O4 M4 O5 111.55(2) 8_455 8_455 ? O2 M4 O5 160.32(3) . 8_455 ? O2 M4 O5 85.30(2) 2_556 8_455 ? O6 M4 O5 72.09(3) 7_556 8_455 ? O6 M4 O5 61.70(2) 8_455 8_455 ? O5 M4 O5 113.18(4) 7_556 8_455 ? O2 M4' O2 92.9(15) . 2_556 ? O2 M4' O4 92.5(7) . 7_556 ? O2 M4' O4 84.0(6) 2_556 7_556 ? O2 M4' O4 84.0(6) . 8_455 ? O2 M4' O4 92.5(7) 2_556 8_455 ? O4 M4' O4 174.9(18) 7_556 8_455 ? O2 M4' FeM1 46.4(7) . . ? O2 M4' FeM1 46.4(7) 2_556 . ? O4 M4' FeM1 87.5(9) 7_556 . ? O4 M4' FeM1 87.5(9) 8_455 . ? O2 M4' MgM2 43.5(3) . 1_556 ? O2 M4' MgM2 94.9(10) 2_556 1_556 ? O4 M4' MgM2 136.0(10) 7_556 1_556 ? O4 M4' MgM2 40.5(3) 8_455 1_556 ? FeM1 M4' MgM2 62.3(6) . 1_556 ? O2 M4' MgM2 94.9(10) . . ? O2 M4' MgM2 43.5(3) 2_556 . ? O4 M4' MgM2 40.5(3) 7_556 . ? O4 M4' MgM2 136.0(10) 8_455 . ? FeM1 M4' MgM2 62.3(6) . . ? MgM2 M4' MgM2 124.7(12) 1_556 . ? O2 M4' MgM1 46.4(7) . . ? O2 M4' MgM1 46.4(7) 2_556 . ? O4 M4' MgM1 87.5(9) 7_556 . ? O4 M4' MgM1 87.5(9) 8_455 . ? FeM1 M4' MgM1 0.0 . . ? MgM2 M4' MgM1 62.3(6) 1_556 . ? MgM2 M4' MgM1 62.3(6) . . ? O7 Si1 O1 112.15(4) . . ? O7 Si1 O6 109.14(4) . . ? O1 Si1 O6 110.85(3) . . ? O7 Si1 O5 108.29(4) . . ? O1 Si1 O5 110.71(3) . . ? O6 Si1 O5 105.45(3) . . ? O4 Si2 O2 115.22(4) . . ? O4 Si2 O5 110.54(4) . 1_556 ? O2 Si2 O5 109.70(3) . 1_556 ? O4 Si2 O6 102.29(4) . . ? O2 Si2 O6 109.55(3) . . ? O5 Si2 O6 109.21(3) 1_556 . ? Si1 O1 MgM1 118.09(4) . . ? Si1 O1 FeM1 118.34(4) . . ? MgM1 O1 FeM1 3.9(3) . . ? Si1 O1 MgM2 121.76(4) . . ? MgM1 O1 MgM2 99.5(2) . . ? FeM1 O1 MgM2 96.50(4) . . ? Si1 O1 MgM3 115.34(3) . . ? MgM1 O1 MgM3 96.3(2) . . ? FeM1 O1 MgM3 99.40(3) . . ? MgM2 O1 MgM3 101.50(3) . . ? Si1 O1 FeM3 115.34(3) . . ? MgM1 O1 FeM3 96.3(2) . . ? FeM1 O1 FeM3 99.40(3) . . ? MgM2 O1 FeM3 101.50(3) . . ? MgM3 O1 FeM3 0.0 . . ? Si2 O2 M4' 125.9(5) . . ? Si2 O2 MgM2 124.71(4) . 1_556 ? M4' O2 MgM2 93.34(6) . 1_556 ? Si2 O2 FeM1 120.56(4) . . ? M4' O2 FeM1 88.6(7) . . ? MgM2 O2 FeM1 94.16(3) 1_556 . ? Si2 O2 MgM1 118.83(13) . . ? M4' O2 MgM1 91.1(8) . . ? MgM2 O2 MgM1 94.01(3) 1_556 . ? FeM1 O2 MgM1 2.6(2) . . ? Si2 O2 M4 120.99(4) . . ? M4' O2 M4 7.8(7) . . ? MgM2 O2 M4 92.76(2) 1_556 . ? FeM1 O2 M4 96.34(3) . . ? MgM1 O2 M4 98.90(19) . . ? Cl3 O3 MgM1 121.42(19) . 5_556 ? Cl3 O3 MgM1 121.42(19) . . ? MgM1 O3 MgM1 99.9(4) 5_556 . ? Cl3 O3 MgM3 117.4(3) . 1_556 ? MgM1 O3 MgM3 95.46(9) 5_556 1_556 ? MgM1 O3 MgM3 95.46(9) . 1_556 ? Cl3 O3 FeM1 119.68(13) . . ? MgM1 O3 FeM1 102.3(2) 5_556 . ? MgM1 O3 FeM1 2.4(2) . . ? MgM3 O3 FeM1 95.18(8) 1_556 . ? Cl3 O3 FeM1 119.68(13) . 5_556 ? MgM1 O3 FeM1 2.4(2) 5_556 5_556 ? MgM1 O3 FeM1 102.3(2) . 5_556 ? MgM3 O3 FeM1 95.18(8) 1_556 5_556 ? FeM1 O3 FeM1 104.63(11) . 5_556 ? O3 Cl3 MgM1 47.94(19) . 5_556 ? O3 Cl3 MgM1 47.94(19) . . ? MgM1 Cl3 MgM1 83.5(4) 5_556 . ? O3 Cl3 MgM3 51.6(2) . 1_556 ? MgM1 Cl3 MgM3 80.88(4) 5_556 1_556 ? MgM1 Cl3 MgM3 80.88(4) . 1_556 ? O3 Cl3 FeM1 49.90(10) . . ? MgM1 Cl3 FeM1 85.92(18) 5_556 . ? MgM1 Cl3 FeM1 2.4(2) . . ? MgM3 Cl3 FeM1 81.23(3) 1_556 . ? O3 Cl3 FeM1 49.90(10) . 5_556 ? MgM1 Cl3 FeM1 2.4(2) 5_556 5_556 ? MgM1 Cl3 FeM1 85.92(18) . 5_556 ? MgM3 Cl3 FeM1 81.23(3) 1_556 5_556 ? FeM1 Cl3 FeM1 88.34(5) . 5_556 ? O3 Cl3 A2M 172.2(3) . 1_556 ? MgM1 Cl3 A2M 135.09(17) 5_556 1_556 ? MgM1 Cl3 A2M 135.09(17) . 1_556 ? MgM3 Cl3 A2M 120.60(3) 1_556 1_556 ? FeM1 Cl3 A2M 132.91(2) . 1_556 ? FeM1 Cl3 A2M 132.91(2) 5_556 1_556 ? O3 Cl3 A2 167.1(6) . 5_656 ? MgM1 Cl3 A2 144.6(7) 5_556 5_656 ? MgM1 Cl3 A2 125.3(7) . 5_656 ? MgM3 Cl3 A2 120.06(8) 1_556 5_656 ? FeM1 Cl3 A2 123.1(7) . 5_656 ? FeM1 Cl3 A2 142.6(7) 5_556 5_656 ? A2M Cl3 A2 10.3(7) 1_556 5_656 ? O3 Cl3 A2 167.1(6) . 1_556 ? MgM1 Cl3 A2 125.3(7) 5_556 1_556 ? MgM1 Cl3 A2 144.6(7) . 1_556 ? MgM3 Cl3 A2 120.06(8) 1_556 1_556 ? FeM1 Cl3 A2 142.6(7) . 1_556 ? FeM1 Cl3 A2 123.1(7) 5_556 1_556 ? A2M Cl3 A2 10.3(7) 1_556 1_556 ? A2 Cl3 A2 20.5(14) 5_656 1_556 ? Si2 O4 MgM2 143.21(4) . 7_556 ? Si2 O4 M4' 111.5(9) . 7_556 ? MgM2 O4 M4' 90.4(6) 7_556 7_556 ? Si2 O4 M4 101.01(4) . 7_556 ? MgM2 O4 M4 97.67(3) 7_556 7_556 ? M4' O4 M4 11.0(9) 7_556 7_556 ? Si2 O5 Si1 136.16(4) 1_554 . ? Si2 O5 A2 100.5(3) 1_554 5_655 ? Si1 O5 A2 94.8(6) . 5_655 ? Si2 O5 M4 120.06(4) 1_554 7_556 ? Si1 O5 M4 92.04(3) . 7_556 ? A2 O5 M4 109.6(3) 5_655 7_556 ? Si2 O5 A2M 103.48(3) 1_554 . ? Si1 O5 A2M 87.93(3) . . ? A2 O5 A2M 7.5(6) 5_655 . ? M4 O5 A2M 113.10(2) 7_556 . ? Si2 O6 Si1 139.43(4) . . ? Si2 O6 M4 93.53(3) . 7_556 ? Si1 O6 M4 100.75(3) . 7_556 ? Si2 O6 A2 90.4(5) . 5_656 ? Si1 O6 A2 119.7(7) . 5_656 ? M4 O6 A2 108.5(5) 7_556 5_656 ? Si2 O6 A2M 96.30(3) . 1_556 ? Si1 O6 A2M 111.44(3) . 1_556 ? M4 O6 A2M 114.31(2) 7_556 1_556 ? A2 O6 A2M 8.7(7) 5_656 1_556 ? Si1 O7 Si1 140.26(7) . 6 ? Si1 O7 A2M 106.12(4) . . ? Si1 O7 A2M 106.12(4) 6 . ? Si1 O7 A2 118.9(9) . . ? Si1 O7 A2 93.3(9) 6 . ? A2M O7 A2 13.0(9) . . ? Si1 O7 A2 93.3(9) . 5_655 ? Si1 O7 A2 118.9(9) 6 5_655 ? A2M O7 A2 13.0(9) . 5_655 ? A2 O7 A2 26.1(18) . 5_655 ? A2 A2M A2 180.0 . 5_655 ? A2 A2M O7 90.0 . 5_655 ? A2 A2M O7 90.0 5_655 5_655 ? A2 A2M O7 90.0 . . ? A2 A2M O7 90.0 5_655 . ? O7 A2M O7 180.0 5_655 . ? A2 A2M O5 34.627(12) . 6 ? A2 A2M O5 145.373(12) 5_655 6 ? O7 A2M O5 122.376(13) 5_655 6 ? O7 A2M O5 57.624(13) . 6 ? A2 A2M O5 145.373(12) . 2_655 ? A2 A2M O5 34.627(12) 5_655 2_655 ? O7 A2M O5 57.624(13) 5_655 2_655 ? O7 A2M O5 122.376(13) . 2_655 ? O5 A2M O5 180.000(15) 6 2_655 ? A2 A2M O5 34.627(12) . 5_655 ? A2 A2M O5 145.373(12) 5_655 5_655 ? O7 A2M O5 57.624(13) 5_655 5_655 ? O7 A2M O5 122.376(13) . 5_655 ? O5 A2M O5 69.25(2) 6 5_655 ? O5 A2M O5 110.75(2) 2_655 5_655 ? A2 A2M O5 145.373(12) . . ? A2 A2M O5 34.627(12) 5_655 . ? O7 A2M O5 122.376(13) 5_655 . ? O7 A2M O5 57.624(13) . . ? O5 A2M O5 110.75(2) 6 . ? O5 A2M O5 69.25(2) 2_655 . ? O5 A2M O5 180.0 5_655 . ? A2 A2M O6 46.133(12) . 6_554 ? A2 A2M O6 133.867(12) 5_655 6_554 ? O7 A2M O6 81.91(2) 5_655 6_554 ? O7 A2M O6 98.09(2) . 6_554 ? O5 A2M O6 50.996(15) 6 6_554 ? O5 A2M O6 129.004(15) 2_655 6_554 ? O5 A2M O6 59.262(17) 5_655 6_554 ? O5 A2M O6 120.738(17) . 6_554 ? A2 A2M O6 133.867(12) . 2_656 ? A2 A2M O6 46.133(12) 5_655 2_656 ? O7 A2M O6 98.09(2) 5_655 2_656 ? O7 A2M O6 81.91(2) . 2_656 ? O5 A2M O6 129.004(15) 6 2_656 ? O5 A2M O6 50.996(15) 2_655 2_656 ? O5 A2M O6 120.738(17) 5_655 2_656 ? O5 A2M O6 59.262(17) . 2_656 ? O6 A2M O6 180.00(3) 6_554 2_656 ? A2 A2M O6 46.133(12) . 5_656 ? A2 A2M O6 133.867(12) 5_655 5_656 ? O7 A2M O6 98.09(2) 5_655 5_656 ? O7 A2M O6 81.91(2) . 5_656 ? O5 A2M O6 59.262(17) 6 5_656 ? O5 A2M O6 120.738(17) 2_655 5_656 ? O5 A2M O6 50.996(15) 5_655 5_656 ? O5 A2M O6 129.003(15) . 5_656 ? O6 A2M O6 92.27(2) 6_554 5_656 ? O6 A2M O6 87.73(2) 2_656 5_656 ? A2 A2M O6 133.867(12) . 1_554 ? A2 A2M O6 46.133(12) 5_655 1_554 ? O7 A2M O6 81.91(2) 5_655 1_554 ? O7 A2M O6 98.09(2) . 1_554 ? O5 A2M O6 120.738(17) 6 1_554 ? O5 A2M O6 59.262(17) 2_655 1_554 ? O5 A2M O6 129.004(15) 5_655 1_554 ? O5 A2M O6 50.997(15) . 1_554 ? O6 A2M O6 87.73(2) 6_554 1_554 ? O6 A2M O6 92.27(2) 2_656 1_554 ? O6 A2M O6 180.000(18) 5_656 1_554 ? A2M A2 A2 0.0 . 5_655 ? A2M A2 O5 137.8(6) . 6 ? A2 A2 O5 137.8(6) 5_655 6 ? A2M A2 O5 137.8(6) . 5_655 ? A2 A2 O5 137.8(6) 5_655 5_655 ? O5 A2 O5 84.3(12) 6 5_655 ? A2M A2 O7 77.0(9) . 5_655 ? A2 A2 O7 77.0(9) 5_655 5_655 ? O5 A2 O7 141.6(13) 6 5_655 ? O5 A2 O7 63.3(3) 5_655 5_655 ? A2M A2 O7 77.0(9) . . ? A2 A2 O7 77.0(9) 5_655 . ? O5 A2 O7 63.3(3) 6 . ? O5 A2 O7 141.6(13) 5_655 . ? O7 A2 O7 153.9(18) 5_655 . ? A2M A2 O6 125.2(7) . 6_554 ? A2 A2 O6 125.2(7) 5_655 6_554 ? O5 A2 O6 59.6(7) 6 6_554 ? O5 A2 O6 69.6(8) 5_655 6_554 ? O7 A2 O6 88.5(3) 5_655 6_554 ? O7 A2 O6 106.6(4) . 6_554 ? A2M A2 O6 125.2(7) . 5_656 ? A2 A2 O6 125.2(7) 5_655 5_656 ? O5 A2 O6 69.6(8) 6 5_656 ? O5 A2 O6 59.6(7) 5_655 5_656 ? O7 A2 O6 106.6(4) 5_655 5_656 ? O7 A2 O6 88.5(3) . 5_656 ? O6 A2 O6 109.6(14) 6_554 5_656 ? A2M A2 Si1 107.8(7) . 6 ? A2 A2 Si1 107.8(7) 5_655 6 ? O5 A2 Si1 31.98(11) 6 6 ? O5 A2 Si1 113.3(13) 5_655 6 ? O7 A2 Si1 172.4(10) 5_655 6 ? O7 A2 Si1 31.41(17) . 6 ? O6 A2 Si1 83.9(6) 6_554 6 ? O6 A2 Si1 75.8(5) 5_656 6 ? A2M A2 Si1 107.8(7) . 5_655 ? A2 A2 Si1 107.8(7) 5_655 5_655 ? O5 A2 Si1 113.3(13) 6 5_655 ? O5 A2 Si1 31.98(11) 5_655 5_655 ? O7 A2 Si1 31.41(17) 5_655 5_655 ? O7 A2 Si1 172.4(10) . 5_655 ? O6 A2 Si1 75.8(5) 6_554 5_655 ? O6 A2 Si1 83.9(6) 5_656 5_655 ? Si1 A2 Si1 144.5(14) 6 5_655 ? A2M A2 Si2 141.3(5) . 6_554 ? A2 A2 Si2 141.3(5) 5_655 6_554 ? O5 A2 Si2 29.4(3) 6 6_554 ? O5 A2 Si2 73.4(9) 5_655 6_554 ? O7 A2 Si2 115.4(8) 5_655 6_554 ? O7 A2 Si2 85.6(5) . 6_554 ? O6 A2 Si2 30.2(3) 6_554 6_554 ? O6 A2 Si2 88.0(10) 5_656 6_554 ? Si1 A2 Si2 57.1(4) 6 6_554 ? Si1 A2 Si2 93.8(9) 5_655 6_554 ? A2M A2 Si2 141.3(5) . 5_656 ? A2 A2 Si2 141.3(5) 5_655 5_656 ? O5 A2 Si2 73.4(9) 6 5_656 ? O5 A2 Si2 29.4(3) 5_655 5_656 ? O7 A2 Si2 85.6(5) 5_655 5_656 ? O7 A2 Si2 115.4(8) . 5_656 ? O6 A2 Si2 88.0(10) 6_554 5_656 ? O6 A2 Si2 30.2(3) 5_656 5_656 ? Si1 A2 Si2 93.8(9) 6 5_656 ? Si1 A2 Si2 57.1(4) 5_655 5_656 ? Si2 A2 Si2 77.4(9) 6_554 5_656 ? _refine_diff_density_max 0.400 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.070 _shelx_res_file ; TITL MLNYSM19349_0m_a.res in C2/m MLNYSM19349_0m_a.res created by SHELXL-2018/3 at 14:36:51 on 20-Mar-2020 REM Old TITL MLNYSM19349_0m in C2/m REM SHELXT solution in C2/m REM R1 0.105, Rweak 0.002, Alpha 0.028, Orientation as input REM Flack x = 0.497 ( 0.009 ) from Parsons' quotients REM Formula found by SHELXT: Ca5 Cl2 Mg4 Na6 O17 Si4 CELL 0.71073 9.9285 18.2576 5.3666 90.000 104.810 90.000 ZERR 2.000 0.0004 0.0007 0.0002 0.000 0.001 0.000 LATT 7 SYMM -X, Y, -Z SFAC O H NA MG SI CA FE CL AL K UNIT 46.2727 2.256 0.22552 3.17064 15.6375 3.9354 6.89396 1.72732 0 1.44488 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 293 SIZE 0.104 0.117 0.151 EADP MGM1 FEM1 HTAB EXYZ MGM2 FEM2 EADP MGM2 FEM2 EADP MGM3 FEM3 OMIT 0 0 2 OMIT 1 5 2 OMIT -2 6 1 OMIT 2 0 0 OMIT -8 0 2 OMIT 1 3 2 OMIT 0 8 0 OMIT 4 0 0 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 0.018200 0.662800 EXTI 0.001506 FVAR 0.28161 0.22341 0.50004 0.13840 0.98385 0.96992 0.98477 FVAR 0.56817 0.72244 0.05638 MOLE 1 REM MGM1 4 0.000000 0.087320 0.500000 20.50000 0.00886 0.01068 = 0.00659 0.00000 0.00298 0.00000 FEM1 7 0.000000 0.095030 0.500000 -20.50000 0.00886 0.01068 = 0.00659 0.00000 0.00298 0.00000 MGM2 4 0.000000 0.178825 0.000000 30.50000 0.00599 0.00516 = 0.00619 0.00000 0.00189 0.00000 FEM2 7 0.000000 0.178825 0.000000 -30.50000 0.00599 0.00516 = 0.00619 0.00000 0.00189 0.00000 MGM3 4 0.000000 0.000000 0.000000 40.25000 0.00879 0.00583 = 0.00832 0.00000 0.00033 0.00000 FEM3 7 0.000000 0.000000 0.000000 -40.25000 0.00879 0.00583 = 0.00832 0.00000 0.00033 0.00000 REM REM M4 6 0.000000 0.280511 0.500000 50.50000 0.01234 0.00933 = 0.01290 0.00000 0.00738 0.00000 M4' 7 0.000000 0.255902 0.500000 -50.50000 0.01615 REM REM SI1 5 0.278186 0.085967 0.300549 61.00000 0.00698 0.00686 = 0.00708 -0.00018 0.00158 -0.00057 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 0.291413 0.173357 0.811073 71.00000 0.00588 0.00601 = 0.00580 0.00057 0.00187 -0.00015 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 0.103850 0.091143 0.214150 11.00000 0.00979 0.01275 = 0.00920 -0.00120 0.00310 -0.00179 O2 1 0.121528 0.177522 0.734731 11.00000 0.00669 0.01202 = 0.01092 0.00079 0.00149 0.00106 REM O3 1 0.109877 0.000000 0.706061 80.50000 0.00966 0.00969 = 0.00927 0.00000 0.00289 0.00000 H3 2 0.206266 0.000000 0.728173 10.28200 0.20570 CL3 8 0.163829 0.000000 0.735280 -80.50000 0.00966 0.00969 = 0.00927 0.00000 0.00289 0.00000 REM O4 1 0.369176 0.249645 0.794143 11.00000 0.01392 0.00923 = 0.01248 0.00006 0.00530 -0.00207 O5 1 0.348006 0.136818 0.099613 11.00000 0.00952 0.01347 = 0.01079 0.00473 0.00155 0.00024 O6 1 0.343041 0.122027 0.597569 11.00000 0.01032 0.01424 = 0.01319 -0.00437 0.00362 0.00054 O7 1 0.334835 0.000000 0.297213 10.50000 0.01332 0.01508 = 0.02053 0.00000 0.00457 0.00000 A2M 10 0.500000 0.000000 0.000000 90.25000 0.06880 0.03480 = 0.09593 0.00000 0.07359 0.00000 A2 3 0.500000 -0.032514 0.000000 100.50000 0.04339 REM MOLE 2 HKLF 4 REM MLNYSM19349_0m_a.res in C2/m REM wR2 = 0.039085, GooF = S = 1.09961, Restrained GooF = 1.09967 for all data REM R1 = 0.015224 for 1728 Fo > 4sig(Fo) and 0.016313 for all 1808 data REM 119 parameters refined using 1 restraints END WGHT 0.0182 0.6701 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.400, deepest hole -0.375, 1-sigma level 0.070 Q1 1 0.5242 -0.0369 0.0834 11.00000 0.05 0.40 Q2 1 0.3439 0.2098 0.8055 11.00000 0.05 0.38 Q3 1 0.3172 0.1607 -0.0228 11.00000 0.05 0.38 Q4 1 0.3034 0.1132 0.4456 11.00000 0.05 0.33 Q5 1 0.2972 0.0431 0.3045 11.00000 0.05 0.33 Q6 1 0.0879 0.0000 0.8020 10.50000 0.05 0.32 Q7 1 0.2056 0.1788 0.8095 11.00000 0.05 0.32 Q8 1 0.3023 0.1449 0.6879 11.00000 0.05 0.29 Q9 1 0.5359 0.0000 0.1862 10.50000 0.05 0.28 Q10 1 0.0000 0.1328 0.5000 10.50000 0.05 0.28 Q11 1 0.0687 0.0000 0.0125 10.50000 0.05 0.28 Q12 1 0.3079 0.1074 0.1302 11.00000 0.05 0.27 Q13 1 0.0919 0.0287 0.7160 11.00000 0.05 0.26 Q14 1 0.3070 0.1593 0.5369 11.00000 0.05 0.26 Q15 1 0.0755 0.0918 0.5314 11.00000 0.05 0.26 Q16 1 0.3179 0.0000 0.5933 10.50000 0.05 0.23 Q17 1 0.3957 0.2370 0.6935 11.00000 0.05 0.22 Q18 1 0.2506 0.0184 0.5360 11.00000 0.05 0.22 Q19 1 0.0060 0.0000 0.1346 10.50000 0.05 0.22 Q20 1 0.0000 0.0537 0.5000 10.50000 0.05 0.22 ; _shelx_res_checksum 87894 _shelx_hkl_file ; 2 0 0 403.56 7.00 2 0 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33.40 1.40 2 -4 -4 34.90 1.20 -2 -4 4 35.10 1.40 2 4 -4 34.60 1.50 -2 4 4 34.60 1.60 -2 4 4 34.10 1.30 2 4 -4 33.40 1.40 0 -4 4 178.38 4.50 0 -4 -4 176.98 4.10 0 -4 4 179.58 4.30 0 -4 4 175.88 4.10 0 -4 -4 171.58 4.30 0 4 4 181.28 4.20 0 4 4 181.08 4.60 0 4 -4 177.88 4.10 0 4 4 176.98 3.80 2 -4 4 28.30 1.60 2 -4 4 31.40 1.50 -2 -4 -4 27.50 1.20 -2 -4 -4 29.70 1.60 -2 -4 -4 29.30 1.60 -2 4 -4 27.30 1.20 -2 4 -4 31.00 1.70 2 4 4 26.90 1.70 -2 4 -4 28.50 1.40 2 4 4 29.80 1.40 4 -4 4 2.70 0.70 4 -4 4 2.40 0.80 -4 -4 -4 2.30 0.80 -4 -4 -4 1.90 0.70 4 4 4 1.60 0.70 -4 4 -4 3.60 0.70 -4 4 -4 2.10 0.70 -4 4 -4 1.90 0.70 6 -4 4 6.90 1.20 6 -4 4 7.00 1.10 -6 -4 -4 7.50 1.20 -6 -4 -4 6.20 1.20 -6 4 -4 6.40 1.10 -6 4 -4 8.50 1.40 6 4 4 5.60 1.10 8 -4 4 62.79 3.10 -8 -4 -4 59.69 3.10 -8 -4 -4 60.39 3.30 8 -4 4 63.29 3.00 -8 4 -4 64.59 3.10 8 4 4 60.89 3.10 -8 4 -4 61.29 3.30 -10 -4 -4 82.89 3.90 10 -4 4 88.89 3.90 10 -4 4 91.49 4.10 -10 -4 -4 86.19 4.40 10 4 4 80.99 3.90 -10 4 -4 89.09 4.40 -10 4 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2.20 0 8 -4 55.79 1.80 -2 -8 -4 21.60 1.60 -2 -8 -4 21.00 1.40 2 -8 4 18.50 1.40 2 8 4 21.30 1.30 -2 8 -4 18.50 1.10 -2 8 -4 21.30 1.40 2 8 4 19.20 1.50 -2 8 -4 20.10 1.50 -4 -8 -4 36.90 2.20 -4 -8 -4 42.10 2.20 4 -8 4 40.40 2.20 4 8 4 36.30 2.20 -4 8 -4 40.00 2.20 -4 8 -4 39.50 2.00 -6 -8 -4 255.87 6.80 6 -8 4 243.28 6.70 -6 -8 -4 268.47 7.00 -6 8 -4 253.47 6.80 6 8 4 244.08 6.80 -6 8 -4 241.28 7.00 -8 -8 -4 106.89 4.60 8 -8 4 104.49 4.20 -8 -8 -4 103.79 4.20 8 8 4 103.59 4.30 -8 8 -4 100.39 4.30 -8 8 -4 105.39 4.50 -10 8 -4 38.70 4.10 -13 -9 4 21.40 2.40 13 -9 -4 20.70 2.30 -13 9 4 24.20 2.50 11 -9 -4 175.48 5.70 11 -9 -4 167.78 5.00 -11 -9 4 181.28 5.80 11 9 -4 177.78 5.10 -11 9 4 172.38 5.40 -11 9 4 171.68 4.90 11 9 -4 167.68 5.40 9 -9 -4 5.70 1.00 -9 -9 4 2.70 0.90 9 -9 -4 2.10 0.90 9 9 -4 1.80 0.70 -9 9 4 3.40 0.90 9 9 -4 3.40 0.90 -9 9 4 2.40 0.80 7 -9 -4 21.40 1.50 7 -9 -4 22.50 1.80 -7 -9 4 22.20 1.80 7 9 -4 17.80 1.50 -7 9 4 20.60 1.50 -7 9 4 22.20 1.70 7 9 -4 21.90 1.60 5 -9 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15 -4 1.90 0.80 -1 -15 4 92.49 3.40 -1 -15 4 98.29 3.80 1 -15 -4 104.49 3.70 -1 15 4 100.69 3.60 1 15 -4 101.59 3.60 1 15 -4 102.19 3.40 -1 -15 -4 17.30 1.80 1 -15 4 18.30 1.60 -1 15 -4 16.40 1.40 1 15 4 18.30 1.60 -1 15 -4 16.40 1.80 1 15 4 17.80 1.80 -3 -15 -4 301.67 7.80 3 -15 4 308.47 7.70 3 15 4 295.37 7.60 -3 15 -4 294.37 7.80 3 15 4 297.37 7.20 -3 15 -4 304.37 7.60 -5 -15 -4 48.70 3.00 5 -15 4 49.70 2.90 5 15 4 51.79 2.90 -5 15 -4 50.69 2.80 -5 15 -4 47.90 3.00 -7 -15 -4 0.40 1.00 7 -15 4 0.30 0.80 -7 15 -4 0.20 0.90 -7 15 -4 1.60 1.00 7 15 4 -0.30 0.80 -7 15 -4 0.50 0.90 -10 -16 4 1.80 1.00 10 -16 -4 0.30 1.00 10 16 -4 2.10 1.00 -10 16 4 0.40 0.80 8 -16 -4 202.48 6.10 -8 -16 4 191.78 6.10 8 16 -4 205.18 5.60 8 16 -4 199.08 5.90 -8 16 4 191.38 5.70 6 -16 -4 43.20 2.50 -6 -16 4 40.60 2.50 -6 16 4 45.90 2.50 6 16 -4 36.30 2.30 6 16 -4 36.50 2.20 4 -16 -4 26.10 2.00 4 -16 -4 24.60 1.90 -4 -16 4 26.40 2.00 -4 -16 4 25.60 1.70 -4 16 4 28.90 2.00 4 16 -4 25.50 1.90 4 16 -4 25.40 1.90 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_computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 99676