data_ammoniozippeite _audit_creation_method 'SHELXL-2016/6' _shelx_SHELXL_version_number '2016/6' _chemical_name_mineral 'ammoniozippeite' _chemical_compound_source 'Burro mine, Colorado' _chemical_formula_sum 'H2 N2 O11 S U2' _chemical_formula_weight 714.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 64 _space_group_name_H-M_alt 'C m c a' _space_group_name_Hall '-C 2bc 2' _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, -y+1/2, z+1/2' 'x, y+1/2, -z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, -z' 'x+1/2, -y+1, z+1/2' 'x+1/2, y+1, -z+1/2' '-x, -y, -z' '-x, y, z' '-x, y-1/2, -z-1/2' '-x, -y-1/2, z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, z' '-x+1/2, y, -z-1/2' '-x+1/2, -y, z-1/2' _cell_length_a 14.3296(7) _cell_length_b 8.7944(4) _cell_length_c 17.1718(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2164.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 4.384 _exptl_crystal_F_000 2432 _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.015 _exptl_absorpt_coefficient_mu 30.141 _shelx_estimated_absorpt_T_min 0.111 _shelx_estimated_absorpt_T_max 0.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details Higashi2001 _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 10176 _diffrn_reflns_av_unetI/netI 0.0287 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.608 _diffrn_reflns_theta_max 27.461 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_point_group_measured_fraction_full 0.988 _reflns_number_total 1249 _reflns_number_gt 923 _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-2016/6 (Sheldrick, 2016)' _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^)+(0.0371P)^2^+159.1080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 1249 _refine_ls_number_parameters 69 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 U1 U 0.23208(3) 0.12645(5) 0.41343(2) 0.01678(18) Uani 1 1 d . . . . . S1 S 0.250000 0.3749(5) 0.250000 0.0181(8) Uani 1 2 d S T P . . O1 O 0.2435(9) 0.3740(9) 0.4559(5) 0.039(3) Uani 1 1 d . . . . . O2 O 0.3098(7) 0.4683(10) 0.3005(5) 0.025(2) Uani 1 1 d . . . . . O3 O 0.1880(7) 0.2799(9) 0.2991(5) 0.024(2) Uani 1 1 d . . . . . O4 O 0.1098(8) 0.1239(10) 0.4310(6) 0.033(2) Uani 1 1 d . . . . . O5 O 0.3521(7) 0.1313(12) 0.3856(6) 0.034(2) Uani 1 1 d . . . . . N1 N 0.000000 0.139(3) 0.2516(17) 0.086(9) Uiso 1 2 d S . P . . N2 N 0.000000 -0.149(3) 0.4034(17) 0.080(8) Uiso 1 2 d S . P . . N3 N 0.000000 0.413(5) 0.440(2) 0.124(14) Uiso 1 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 U1 0.0251(3) 0.0162(3) 0.0090(2) 0.00009(18) 0.00016(16) 0.00196(19) S1 0.034(2) 0.0092(18) 0.0108(18) 0.000 0.0004(15) 0.000 O1 0.100(9) 0.003(4) 0.012(4) 0.004(3) 0.000(5) -0.008(5) O2 0.035(6) 0.017(5) 0.024(5) -0.007(3) 0.004(4) -0.002(4) O3 0.040(6) 0.019(5) 0.014(4) 0.004(3) 0.001(4) -0.005(4) O4 0.045(6) 0.016(5) 0.037(5) 0.009(4) 0.016(4) 0.007(4) O5 0.024(5) 0.046(6) 0.031(5) 0.001(5) -0.004(4) 0.001(5) _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 U1 O4 1.778(11) . ? U1 O5 1.786(10) . ? U1 O1 2.271(9) 13_556 ? U1 O1 2.302(8) . ? U1 O1 2.363(8) 14_545 ? U1 O2 2.460(8) 14_545 ? U1 O3 2.465(8) . ? U1 U1 3.7130(8) 2_556 ? U1 U1 3.7183(8) 13_556 ? U1 N2 4.120(17) . ? U1 N3 4.20(3) . ? U1 N3 4.298(19) 5_545 ? S1 O2 1.470(9) . ? S1 O2 1.470(9) 15_556 ? S1 O3 1.482(9) . ? S1 O3 1.482(9) 15_556 ? S1 N1 4.138(16) . ? S1 N1 4.138(16) 15_556 ? S1 N1 4.271(17) 5 ? S1 N1 4.271(17) 11_566 ? S1 N2 4.452(17) 11_566 ? S1 N2 4.452(17) 5 ? O1 N3 3.517(14) . ? O1 N2 3.790(14) 5 ? O2 N1 3.225(19) 5 ? O2 N2 3.41(2) 5 ? O2 N1 4.07(2) 15_556 ? O3 N1 3.074(17) . ? O3 N3 3.81(3) . ? O4 N2 2.91(3) . ? O4 N3 3.00(4) . ? O4 N2 3.26(3) 9_556 ? O4 N1 3.46(3) . ? O5 N2 2.88(2) 5 ? O5 N3 3.01(3) 5_545 ? O5 N1 3.17(2) 15_556 ? O5 N3 3.69(4) 13_556 ? N1 N2 3.25(4) 11_566 ? N3 N3 2.56(9) 9_566 ? 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 O4 U1 O5 174.2(4) . . ? O4 U1 O1 89.1(5) . 13_556 ? O5 U1 O1 96.7(4) . 13_556 ? O4 U1 O1 91.6(4) . . ? O5 U1 O1 89.6(5) . . ? O1 U1 O1 71.2(3) 13_556 . ? O4 U1 O1 94.7(4) . 14_545 ? O5 U1 O1 87.8(4) . 14_545 ? O1 U1 O1 70.8(3) 13_556 14_545 ? O1 U1 O1 141.3(4) . 14_545 ? O4 U1 O2 83.5(4) . 14_545 ? O5 U1 O2 92.1(4) . 14_545 ? O1 U1 O2 144.6(3) 13_556 14_545 ? O1 U1 O2 143.3(3) . 14_545 ? O1 U1 O2 75.4(3) 14_545 14_545 ? O4 U1 O3 83.7(4) . . ? O5 U1 O3 91.2(4) . . ? O1 U1 O3 145.8(3) 13_556 . ? O1 U1 O3 75.7(3) . . ? O1 U1 O3 143.0(3) 14_545 . ? O2 U1 O3 67.6(3) 14_545 . ? O4 U1 U1 81.7(3) . 2_556 ? O5 U1 U1 103.2(3) . 2_556 ? O1 U1 U1 37.6(2) 13_556 2_556 ? O1 U1 U1 108.2(2) . 2_556 ? O1 U1 U1 35.9(2) 14_545 2_556 ? O2 U1 U1 107.0(2) 14_545 2_556 ? O3 U1 U1 165.0(2) . 2_556 ? O4 U1 U1 90.4(3) . 13_556 ? O5 U1 U1 93.9(3) . 13_556 ? O1 U1 U1 35.88(19) 13_556 13_556 ? O1 U1 U1 35.3(2) . 13_556 ? O1 U1 U1 106.4(2) 14_545 13_556 ? O2 U1 U1 173.8(2) 14_545 13_556 ? O3 U1 U1 110.6(2) . 13_556 ? U1 U1 U1 73.130(14) 2_556 13_556 ? O4 U1 N2 37.3(4) . . ? O5 U1 N2 141.3(5) . . ? O1 U1 N2 99.5(5) 13_556 . ? O1 U1 N2 128.9(5) . . ? O1 U1 N2 65.1(5) 14_545 . ? O2 U1 N2 55.8(5) 14_545 . ? O3 U1 N2 94.7(4) . . ? U1 U1 N2 71.4(4) 2_556 . ? U1 U1 N2 119.3(4) 13_556 . ? O4 U1 N3 37.7(5) . . ? O5 U1 N3 141.1(6) . . ? O1 U1 N3 90.8(6) 13_556 . ? O1 U1 N3 56.9(6) . . ? O1 U1 N3 130.4(6) 14_545 . ? O2 U1 N3 103.5(6) 14_545 . ? O3 U1 N3 63.6(6) . . ? U1 U1 N3 105.8(5) 2_556 . ? U1 U1 N3 70.8(5) 13_556 . ? N2 U1 N3 73.7(6) . . ? O4 U1 N3 148.9(6) . 5_545 ? O5 U1 N3 34.8(6) . 5_545 ? O1 U1 N3 75.9(6) 13_556 5_545 ? O1 U1 N3 108.4(6) . 5_545 ? O1 U1 N3 54.9(6) 14_545 5_545 ? O2 U1 N3 93.2(6) 14_545 5_545 ? O3 U1 N3 123.6(6) . 5_545 ? U1 U1 N3 69.7(5) 2_556 5_545 ? U1 U1 N3 92.6(6) 13_556 5_545 ? N2 U1 N3 117.9(6) . 5_545 ? N3 U1 N3 163.3(11) . 5_545 ? O2 S1 O2 112.0(8) . 15_556 ? O2 S1 O3 109.2(5) . . ? O2 S1 O3 107.6(5) 15_556 . ? O2 S1 O3 107.6(5) . 15_556 ? O2 S1 O3 109.2(5) 15_556 15_556 ? O3 S1 O3 111.4(7) . 15_556 ? O2 S1 N1 141.3(5) . . ? O2 S1 N1 77.2(5) 15_556 . ? O3 S1 N1 36.4(5) . . ? O3 S1 N1 103.9(6) 15_556 . ? O2 S1 N1 77.2(5) . 15_556 ? O2 S1 N1 141.3(5) 15_556 15_556 ? O3 S1 N1 103.9(6) . 15_556 ? O3 S1 N1 36.4(5) 15_556 15_556 ? N1 S1 N1 119.9(8) . 15_556 ? O2 S1 N1 37.2(5) . 5 ? O2 S1 N1 100.8(6) 15_556 5 ? O3 S1 N1 143.7(5) . 5 ? O3 S1 N1 78.9(5) 15_556 5 ? N1 S1 N1 176.9(7) . 5 ? N1 S1 N1 63.03(2) 15_556 5 ? O2 S1 N1 100.8(5) . 11_566 ? O2 S1 N1 37.2(5) 15_556 11_566 ? O3 S1 N1 78.9(5) . 11_566 ? O3 S1 N1 143.7(5) 15_556 11_566 ? N1 S1 N1 63.03(2) . 11_566 ? N1 S1 N1 176.9(7) 15_556 11_566 ? N1 S1 N1 114.0(7) 5 11_566 ? O2 S1 N2 147.7(6) . 11_566 ? O2 S1 N2 37.7(5) 15_556 11_566 ? O3 S1 N2 80.1(5) . 11_566 ? O3 S1 N2 96.8(5) 15_556 11_566 ? N1 S1 N2 44.2(5) . 11_566 ? N1 S1 N2 132.0(5) 15_556 11_566 ? N1 S1 N2 134.8(5) 5 11_566 ? N1 S1 N2 49.3(5) 11_566 11_566 ? O2 S1 N2 37.7(5) . 5 ? O2 S1 N2 147.7(6) 15_556 5 ? O3 S1 N2 96.8(5) . 5 ? O3 S1 N2 80.1(5) 15_556 5 ? N1 S1 N2 132.0(5) . 5 ? N1 S1 N2 44.2(5) 15_556 5 ? N1 S1 N2 49.3(5) 5 5 ? N1 S1 N2 134.8(5) 11_566 5 ? N2 S1 N2 174.5(8) 11_566 5 ? U1 O1 U1 108.8(3) 13_556 . ? U1 O1 U1 106.5(3) 13_556 14 ? U1 O1 U1 143.3(4) . 14 ? U1 O1 N3 103.2(8) 13_556 . ? U1 O1 N3 89.9(8) . . ? U1 O1 N3 91.8(7) 14 . ? U1 O1 N2 94.9(6) 13_556 5 ? U1 O1 N2 86.7(6) . 5 ? U1 O1 N2 80.5(5) 14 5 ? N3 O1 N2 161.7(8) . 5 ? S1 O2 U1 129.7(6) . 14 ? S1 O2 N1 126.8(7) . 5 ? U1 O2 N1 98.5(6) 14 5 ? S1 O2 N2 127.0(7) . 5 ? U1 O2 N2 87.6(5) 14 5 ? N1 O2 N2 66.5(6) 5 5 ? S1 O2 N1 82.2(5) . 15_556 ? U1 O2 N1 137.5(5) 14 15_556 ? N1 O2 N1 73.0(3) 5 15_556 ? N2 O2 N1 50.4(6) 5 15_556 ? S1 O3 U1 127.5(6) . . ? S1 O3 N1 126.9(7) . . ? U1 O3 N1 102.5(6) . . ? S1 O3 N3 127.7(7) . . ? U1 O3 N3 81.0(6) . . ? N1 O3 N3 70.9(7) . . ? U1 O4 N2 121.0(5) . . ? U1 O4 N3 121.0(6) . . ? N2 O4 N3 115.2(7) . . ? U1 O4 N2 128.6(6) . 9_556 ? N2 O4 N2 86.5(8) . 9_556 ? N3 O4 N2 69.0(9) . 9_556 ? U1 O4 N1 107.2(5) . . ? N2 O4 N1 69.0(7) . . ? N3 O4 N1 77.0(9) . . ? N2 O4 N1 123.7(5) 9_556 . ? U1 O5 N2 134.1(7) . 5 ? U1 O5 N3 125.4(7) . 5_545 ? N2 O5 N3 82.8(8) 5 5_545 ? U1 O5 N1 147.5(6) . 15_556 ? N2 O5 N1 64.7(8) 5 15_556 ? N3 O5 N1 77.0(8) 5_545 15_556 ? U1 O5 N3 109.5(6) . 13_556 ? N2 O5 N3 64.0(8) 5 13_556 ? N3 O5 N3 43.5(14) 5_545 13_556 ? N1 O5 N3 102.8(6) 15_556 13_556 ? O3 N1 O3 122.4(10) . 10 ? O3 N1 O5 142.4(10) . 8_445 ? O3 N1 O5 67.7(3) 10 8_445 ? O3 N1 O5 67.7(3) . 15_556 ? O3 N1 O5 142.4(10) 10 15_556 ? O5 N1 O5 83.9(8) 8_445 15_556 ? O3 N1 O2 149.2(10) . 5_445 ? O3 N1 O2 51.5(3) 10 5_445 ? O5 N1 O2 67.5(3) 8_445 5_445 ? O5 N1 O2 138.4(10) 15_556 5_445 ? O3 N1 O2 51.5(3) . 14_545 ? O3 N1 O2 149.2(10) 10 14_545 ? O5 N1 O2 138.4(10) 8_445 14_545 ? O5 N1 O2 67.5(3) 15_556 14_545 ? O2 N1 O2 115.4(10) 5_445 14_545 ? O3 N1 N2 89.3(7) . 11_566 ? O3 N1 N2 89.3(7) 10 11_566 ? O5 N1 N2 53.4(5) 8_445 11_566 ? O5 N1 N2 53.4(5) 15_556 11_566 ? O2 N1 N2 118.7(5) 5_445 11_566 ? O2 N1 N2 118.7(5) 14_545 11_566 ? O3 N1 O4 100.3(8) . 10 ? O3 N1 O4 51.8(4) 10 10 ? O5 N1 O4 110.9(3) 8_445 10 ? O5 N1 O4 164.7(6) 15_556 10 ? O2 N1 O4 50.6(4) 5_445 10 ? O2 N1 O4 97.7(8) 14_545 10 ? N2 N1 O4 138.8(8) 11_566 10 ? O5 N2 O5 94.7(9) 5_445 14_545 ? O5 N2 O4 99.9(3) 5_445 10 ? O5 N2 O4 165.3(8) 14_545 10 ? O5 N2 O4 165.3(8) 5_445 . ? O5 N2 O4 99.9(3) 14_545 . ? O4 N2 O4 65.4(7) 10 . ? O5 N2 N1 62.0(7) 5_445 11_556 ? O5 N2 N1 62.0(7) 14_545 11_556 ? O4 N2 N1 127.3(8) 10 11_556 ? O4 N2 N1 127.3(8) . 11_556 ? O5 N2 O4 119.6(9) 5_445 2_556 ? O5 N2 O4 77.5(5) 14_545 2_556 ? O4 N2 O4 93.5(8) 10 2_556 ? O4 N2 O4 62.6(6) . 2_556 ? N1 N2 O4 139.1(8) 11_556 2_556 ? O5 N2 O4 77.5(5) 5_445 9_556 ? O5 N2 O4 119.6(9) 14_545 9_556 ? O4 N2 O4 62.6(6) 10 9_556 ? O4 N2 O4 93.5(8) . 9_556 ? N1 N2 O4 139.1(8) 11_556 9_556 ? O4 N2 O4 57.8(6) 2_556 9_556 ? O5 N2 O2 63.9(3) 5_445 5_445 ? O5 N2 O2 137.4(10) 14_545 5_445 ? O4 N2 O2 53.2(4) 10 5_445 ? O4 N2 O2 105.4(8) . 5_445 ? N1 N2 O2 75.4(6) 11_556 5_445 ? O4 N2 O2 144.8(9) 2_556 5_445 ? O4 N2 O2 92.6(4) 9_556 5_445 ? N3 N3 O4 123.3(19) 9_566 . ? N3 N3 O4 123.3(19) 9_566 10 ? O4 N3 O4 63.4(9) . 10 ? N3 N3 O5 82.5(15) 9_566 14 ? O4 N3 O5 98.9(5) . 14 ? O4 N3 O5 153.5(15) 10 14 ? N3 N3 O5 82.5(15) 9_566 5_455 ? O4 N3 O5 153.5(15) . 5_455 ? O4 N3 O5 98.9(5) 10 5_455 ? O5 N3 O5 89.6(12) 14 5_455 ? N3 N3 O1 89.8(7) 9_566 10 ? O4 N3 O1 116.2(11) . 10 ? O4 N3 O1 53.1(4) 10 10 ? O5 N3 O1 141.7(12) 14 10 ? O5 N3 O1 52.2(3) 5_455 10 ? N3 N3 O1 89.8(7) 9_566 . ? O4 N3 O1 53.1(4) . . ? O4 N3 O1 116.2(11) 10 . ? O5 N3 O1 52.2(3) 14 . ? O5 N3 O1 141.7(12) 5_455 . ? O1 N3 O1 165.7(14) 10 . ? N3 N3 N2 77.5(19) 9_566 9_556 ? O4 N3 N2 59.0(8) . 9_556 ? O4 N3 N2 59.0(8) 10 9_556 ? O5 N3 N2 130.8(8) 14 9_556 ? O5 N3 N2 130.8(8) 5_455 9_556 ? O1 N3 N2 83.0(7) 10 9_556 ? O1 N3 N2 83.0(7) . 9_556 ? _refine_diff_density_max 3.938 _refine_diff_density_min -1.791 _refine_diff_density_rms 0.388 _shelx_res_file ; TITL ammoniozippeite (JM-13687) 13687.res created by SHELXL-2016/6 at 18:39:07 on 06-Jul-2017 CELL 0.71075 14.32960 8.79436 17.17180 90.00000 90.00000 90.00000 ZERR 8 0.00070 0.00035 0.00121 0.00000 0.00000 0.00000 LATT 7 SYMM +X, -Y, -Z SYMM +X, .50-Y, .50+Z SYMM +X, .50+Y, .50-Z SFAC H N O S U UNIT 16 16 88 8 16 L.S. 20 omit 0 8 1 CONN 8 3.0 N1 CONN 8 3.0 N2 CONN 8 3.0 N3 FMAP 2 PLAN 8 ACTA SIZE 0.130 0.050 0.015 WGHT 0.037100 159.108002 FVAR 0.07181 U1 5 0.232076 0.126448 0.413428 11.00000 0.02507 0.01625 = 0.00901 0.00009 0.00016 0.00196 S1 4 0.250000 0.374930 0.250000 10.50000 0.03442 0.00923 = 0.01075 0.00000 0.00044 0.00000 O1 3 0.243533 0.374024 0.455902 11.00000 0.09996 0.00331 = 0.01245 0.00399 0.00007 -0.00799 O2 3 0.309756 0.468327 0.300504 11.00000 0.03531 0.01733 = 0.02366 -0.00682 0.00354 -0.00229 O3 3 0.188027 0.279905 0.299093 11.00000 0.03997 0.01884 = 0.01359 0.00436 0.00080 -0.00483 O4 3 0.109804 0.123865 0.431048 11.00000 0.04538 0.01555 = 0.03731 0.00907 0.01573 0.00657 O5 3 0.352135 0.131259 0.385565 11.00000 0.02434 0.04625 = 0.03126 0.00059 -0.00370 0.00125 N1 2 0.000000 0.139420 0.251593 10.50000 0.08577 N2 2 0.000000 -0.149486 0.403446 10.50000 0.07983 N3 2 0.000000 0.413180 0.440199 10.50000 0.12432 HKLF 4 REM ammoniozippeite (JM-13687) REM R1 = 0.0396 for 923 Fo > 4sig(Fo) and 0.0559 for all 1249 data REM 69 parameters refined using 0 restraints END WGHT 0.0371 159.1149 REM Highest difference peak 3.938, deepest hole -1.791, 1-sigma level 0.388 Q1 1 0.2969 0.1094 0.4139 11.00000 0.05 3.94 Q2 1 0.2432 0.1270 0.3606 11.00000 0.05 2.35 Q3 1 0.0000 0.0000 0.5000 10.25000 0.05 2.31 Q4 1 0.0000 -0.1304 0.3603 10.50000 0.05 2.31 Q5 1 0.1734 0.1188 0.4096 11.00000 0.05 2.27 Q6 1 0.2384 0.1235 0.4590 11.00000 0.05 2.01 Q7 1 0.0000 0.3935 0.3645 10.50000 0.05 1.89 Q8 1 0.0000 0.2247 0.2389 10.50000 0.05 1.71 ; _shelx_res_checksum 17401 _shelx_hkl_file ; -2 0 1 0.49 0.37 2 0 -1 1.04 0.40 -2 0 1 0.61 0.62 -2 0 -1 1.03 0.99 2 0 1 0.94 0.66 2 0 -1 1.76 0.64 0 0 3 21.29 2.98 0 0 3 10.93 2.14 0 0 -3 19.16 3.07 0 0 -3 15.98 2.17 1 -1 -2 43.34 1.60 1 1 -2 40.75 1.54 -1 -1 -2 39.94 1.80 -1 1 2 40.87 1.62 -1 -1 -2 37.70 1.52 1 -1 2 42.43 1.59 1 1 2 41.91 1.66 -1 1 2 38.52 1.50 -1 1 -2 43.20 1.52 1 -1 -2 39.35 2.18 -1 -1 2 36.74 2.34 1 1 2 36.25 1.51 2 0 2 877.89 18.49 2 0 -2 893.96 18.84 -2 0 2 940.71 18.26 2 0 -2 964.88 18.97 -2 0 -2 917.48 19.19 -2 0 2 916.77 19.13 1 -1 3 0.20 1.01 1 -1 -3 -0.60 0.95 -1 1 -3 0.53 1.03 1 -1 -3 -1.78 0.94 -1 -1 -3 -0.31 1.31 -1 1 3 0.04 0.98 -1 -1 -3 1.38 1.09 1 1 -3 -0.28 0.95 -1 -1 3 -1.67 1.56 1 1 3 2.53 1.16 -1 1 3 0.32 0.94 1 1 3 2.13 0.97 2 0 -3 6.29 1.27 -2 0 -3 1.22 2.07 -2 0 3 4.44 1.26 2 0 -3 3.12 1.28 -2 0 3 6.86 1.22 2 0 3 2.64 1.27 0 -2 0 6.88 0.85 0 0 -4 1688.88 56.77 0 0 -4 1624.69 49.19 0 0 4 1586.49 47.41 0 0 4 1649.64 55.14 0 2 1 1197.87 26.35 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