#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/19/2011970.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2011970 loop_ _publ_author_name 'Harrison, William T. A.' 'Sobolev, Alexandr N. ' 'Phillips, Mark L. F.' _publ_section_title ; Hexagonal ammonium zinc phosphate, (NH~4~)ZnPO~4~, at 10K ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 508 _journal_page_last 509 _journal_paper_doi 10.1107/S0108270101002992 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety '(N H4), (Zn P O4)' _chemical_formula_sum 'H4 N O4 P Zn' _chemical_formula_weight 178.38 _chemical_melting_point 'decomposes before melting' _chemical_name_systematic ; ? ; _space_group_IT_number 173 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P 6c' _symmetry_space_group_name_H-M 'P 63' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 8 _cell_length_a 10.702(2) _cell_length_b 10.702(2) _cell_length_c 8.703(2) _cell_measurement_reflns_used 20 _cell_measurement_temperature 10(2) _cell_measurement_theta_max 13.7 _cell_measurement_theta_min 13.3 _cell_volume 863.2(3) _computing_cell_refinement 'local routines' _computing_data_collection 'local routines' _computing_data_reduction 'local routines' _computing_molecular_graphics ; ORTEP-3 (Farrugia, 1997) and ATOMS (Shape Software Inc., 1999) ; _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' _diffrn_ambient_temperature 10(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Huber diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0258 _diffrn_reflns_av_sigmaI/netI .0181 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 9471 _diffrn_reflns_theta_full 37.55 _diffrn_reflns_theta_max 37.55 _diffrn_reflns_theta_min 3.21 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 97 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 5.952 _exptl_absorpt_correction_T_max .952 _exptl_absorpt_correction_T_min .824 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details '(ABSORB; Hall et al., 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.745 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'hexagonal prism' _exptl_crystal_F_000 704 _exptl_crystal_size_max .20 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .20 _refine_diff_density_max .378 _refine_diff_density_min -.575 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack .000(5) _refine_ls_extinction_coef .0329(5) _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 109 _refine_ls_number_reflns 3049 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.146 _refine_ls_R_factor_all .0128 _refine_ls_R_factor_gt .0125 _refine_ls_shift/su_max .003 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0130P)^2^+0.0620P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0312 _reflns_number_gt 3026 _reflns_number_total 3049 _reflns_threshold_expression I>2\s(I) _cod_data_source_file gd1138.cif _cod_data_source_block I _cod_database_code 2011970 _cod_database_fobs_code 2011970 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol N1 .05046(8) .53438(8) .75371(10) .00646(10) Uani d . 1 . . N N2 .0000 .0000 .74956(16) .00664(18) Uani d S 1 . . N Zn1 .822249(9) .674521(9) .951768(11) .00320(2) Uani d . 1 . . Zn Zn2 .6667 .3333 .57517(2) .00317(3) Uani d S 1 . . Zn P1 .81947(2) .67342(2) .57189(3) .00309(4) Uani d . 1 . . P P2 .6667 .3333 .96623(5) .00338(6) Uani d S 1 . . P O1 1.02517(7) .81712(7) .97324(7) .00520(10) Uani d . 1 . . O O2 .77303(7) .68119(7) .73743(7) .00543(9) Uani d . 1 . . O O3 .69860(7) .72409(7) 1.07217(8) .00558(9) Uani d . 1 . . O O4 .77175(7) .48534(7) 1.03021(8) .00556(9) Uani d . 1 . . O O5 .71408(7) .52403(7) .50269(8) .00567(9) Uani d . 1 . . O O6 .6667 .3333 .79295(13) .00863(19) Uani d S 1 . . O H11 .084(3) .574(2) .838(3) .018(5) Uiso d . 1 . . H H12 .110(3) .528(2) .697(3) .019(5) Uiso d . 1 . . H H13 -.0144(18) .4453(18) .769(2) .004(3) Uiso d . 1 . . H H14 .011(2) .578(2) .702(3) .017(5) Uiso d . 1 . . H H21 .0000 .0000 .642(4) .022(9) Uiso d S 1 . . H H22 -.082(2) -.026(2) .789(2) .020(5) Uiso d . 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 .0068(2) .0064(2) .0065(3) .0035(2) -.0003(2) -.0004(2) N2 .0065(3) .0065(3) .0069(4) .00325(13) .000 .000 Zn1 .00284(4) .00291(4) .00376(4) .00136(3) -.00003(3) .00007(3) Zn2 .00291(4) .00291(4) .00367(6) .00146(2) .000 .000 P1 .00267(7) .00279(8) .00370(9) .00129(6) -.00002(6) .00023(6) P2 .00327(8) .00327(8) .00359(15) .00164(4) .000 .000 O1 .0039(2) .0052(2) .0065(2) .00225(18) -.00124(16) .00025(17) O2 .0054(2) .0070(2) .0037(2) .00299(19) .00018(17) -.00011(16) O3 .0064(2) .0043(2) .0073(2) .00359(18) .0020(2) .00118(19) O4 .0051(2) .0030(2) .0079(2) .00144(19) -.00142(18) -.00023(18) O5 .0063(2) .0036(2) .0060(2) .00169(19) -.00147(19) -.00037(18) O6 .0111(3) .0111(3) .0036(4) .00556(14) .000 .000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag H11 N1 H12 . . 114(2) no H11 N1 H13 . . 109(2) no H12 N1 H13 . . 103.1(18) no H11 N1 H14 . . 112.1(19) no H12 N1 H14 . . 109(2) no H13 N1 H14 . . 109.1(18) no H21 N2 H22 . . 113.6(13) no O4 Zn1 O1 . . 113.90(3) no O4 Zn1 O2 . . 115.82(3) no O1 Zn1 O2 . . 106.26(3) no O4 Zn1 O3 . . 102.77(3) no O1 Zn1 O3 . . 112.18(3) no O2 Zn1 O3 . . 105.70(3) no O6 Zn2 O5 . 3_665 108.92(2) no O6 Zn2 O5 . 2_655 108.92(2) no O5 Zn2 O5 3_665 2_655 110.02(2) no O6 Zn2 O5 . . 108.92(2) no O5 Zn2 O5 3_665 . 110.02(2) no O5 Zn2 O5 2_655 . 110.02(2) no O2 P1 O3 . 6_654 109.70(4) no O2 P1 O1 . 5_564 109.75(4) no O3 P1 O1 6_654 5_564 108.40(4) no O2 P1 O5 . . 109.40(4) no O3 P1 O5 6_654 . 110.27(4) no O1 P1 O5 5_564 . 109.30(4) no O6 P2 O4 . 3_665 111.10(3) no O6 P2 O4 . . 111.10(3) no O4 P2 O4 3_665 . 107.79(3) no O6 P2 O4 . 2_655 111.10(3) no O4 P2 O4 3_665 2_655 107.79(3) no O4 P2 O4 . 2_655 107.79(3) no P1 O1 Zn1 6_655 . 131.77(4) yes P1 O2 Zn1 . . 142.46(4) yes P1 O3 Zn1 5_565 . 133.60(4) yes P2 O4 Zn1 . . 130.37(4) yes P1 O5 Zn2 . . 129.17(4) yes P2 O6 Zn2 . . 180.0 yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 H11 . .83(2) no N1 H12 . .84(2) no N1 H13 . .865(17) no N1 H14 . .89(2) no N2 H21 . .93(4) no N2 H22 . .85(2) no Zn1 O4 . 1.9399(7) yes Zn1 O1 . 1.9406(8) yes Zn1 O2 . 1.9494(7) yes Zn1 O3 . 1.9577(7) yes Zn2 O6 . 1.8953(12) yes Zn2 O5 3_665 1.9455(7) yes Zn2 O5 2_655 1.9455(7) yes Zn2 O5 . 1.9455(7) yes P1 O2 . 1.5398(7) yes P1 O3 6_654 1.5423(7) yes P1 O1 5_564 1.5423(7) yes P1 O5 . 1.5451(7) yes P2 O6 . 1.5081(13) yes P2 O4 3_665 1.5465(7) yes P2 O4 . 1.5465(7) yes P2 O4 2_655 1.5465(7) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H11 O5 6_555 .83(3) 1.97(2) 2.7843(13) 165(2) yes N1 H12 O4 4_664 .84(3) 1.98(3) 2.8018(14) 169(3) yes N1 H13 O2 3_565 .864(17) 2.070(17) 2.8553(12) 150.7(19) yes N1 H14 O3 6_554 .89(2) 1.90(2) 2.7702(14) 166(2) yes N2 H22 O1 3_565 .85(2) 2.10(2) 2.8670(15) 150.3(17) yes