#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/81/2008122.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_2008122 loop_ _publ_author_name 'Yakubovich, Olga V.' 'Karimova, Oksana V.' 'Dimitrova, Olga V.' 'Massa, Werner' _publ_section_title ; Layer structure of (NH~4~)CoPO~4~ ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 151 _journal_page_last 153 _journal_paper_doi 10.1107/S0108270198011639 _journal_volume 55 _journal_year 1999 _chemical_formula_analytical 'NH4 Co PO4 H2O' _chemical_formula_moiety '(N H4 ) Co P O4 .H2 O' _chemical_formula_structural NH4[CoPO4(H2O)] _chemical_formula_sum 'Co H6 N O5 P' _chemical_formula_weight 189.96 _chemical_name_systematic ; cobalt ammonium hydrate phosphate ; _space_group_IT_number 31 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac -2' _symmetry_space_group_name_H-M 'P m n 21' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 5.6210(10) _cell_length_b 8.7660(10) _cell_length_c 4.7970(10) _cell_measurement_reflns_used 2085 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.0 _cell_measurement_theta_min 2.4 _cell_volume 236.37(7) _computing_cell_refinement 'IPDS CELL (Stoe 1997)' _computing_data_collection 'IPDS EXPOSE (Stoe 1997)' _computing_data_reduction 'IPDS INTEGRATE (Stoe 1997)' _computing_molecular_graphics 'DIAMOND (Bergerhoff 1996)' _computing_publication_material SHELXL-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device 'STOE IPDS diffractometer' _diffrn_measurement_method '\f = 0-200\%, (\D\f = 2\%, d = 60 mm, t = 5 min)' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_number 1702 _diffrn_reflns_theta_full 28.04 _diffrn_reflns_theta_max 28.04 _diffrn_reflns_theta_min 4.31 _exptl_absorpt_coefficient_mu 3.897 _exptl_absorpt_correction_T_max 0.865 _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_type numerical _exptl_crystal_colour 'dark pink' _exptl_crystal_density_diffrn 2.669 _exptl_crystal_density_meas ? _exptl_crystal_description plate _exptl_crystal_F_000 190 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.308 _refine_diff_density_min -0.311 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 0.000(15) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 594 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.142 _refine_ls_R_factor_all 0.0152 _refine_ls_R_factor_gt 0.0145 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0236P)^2^+0.0176P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0368 _reflns_number_observed 580 _reflns_number_total 594 _reflns_observed_criterion >2sigma(I) _cod_data_source_file av1025.cif _cod_data_source_block coph2 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_cell_volume 236.37(8) _cod_original_formula_sum 'H6 Co N O5 P' _cod_database_code 2008122 _cod_database_fobs_code 2008122 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' 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 Co 1.0000 1.02055(4) 0.5000 0.00870(11) Uani d S 1 . . Co P 1.0000 0.80662(7) 0.93261(15) 0.00699(15) Uani d S 1 . . P N 1.0000 0.4725(3) 0.3703(6) 0.0170(5) Uani d SD 1 . . N H1 1.0000 0.535(5) 0.506(7) 0.041(6) Uiso d SD 1 . . H H2 1.120(3) 0.413(3) 0.378(6) 0.041(6) Uiso d D 1 . . H H3 1.0000 0.536(4) 0.237(7) 0.041(6) Uiso d SD 1 . . H O2 0.7820(2) 0.88417(16) 0.7906(3) 0.0120(3) Uani d . 1 . . O O1 1.0000 0.8316(2) 1.2461(4) 0.0117(4) Uani d S 1 . . O O3 1.0000 0.6351(2) 0.8716(4) 0.0135(4) Uani d S 1 . . O O4 1.0000 1.2093(3) 0.7978(6) 0.0160(4) Uani d S 1 . . O H4 1.103(5) 1.195(4) 0.892(8) 0.043(10) 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 Co 0.00788(15) 0.01065(16) 0.00756(18) 0.000 0.000 0.00076(19) P 0.0072(3) 0.0077(3) 0.0061(4) 0.000 0.000 0.0001(2) N 0.0204(13) 0.0169(13) 0.0137(13) 0.000 0.000 0.0035(9) O2 0.0106(6) 0.0161(7) 0.0094(7) 0.0042(5) 0.0012(5) 0.0009(4) O1 0.0154(10) 0.0132(9) 0.0066(11) 0.000 0.000 -0.0017(7) O3 0.0210(10) 0.0075(9) 0.0120(10) 0.000 0.000 -0.0005(7) O4 0.0113(10) 0.0198(11) 0.0169(12) 0.000 0.000 0.0001(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source N N 0.0061 0.0033 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 O2 Co O2 2_674 3_574 101.01(8) yes O2 Co O1 2_674 1_554 92.16(6) yes O2 Co O1 3_574 1_554 92.16(6) yes O2 Co O4 2_674 . 90.68(6) yes O2 Co O4 3_574 . 90.68(6) yes O1 Co O4 1_554 . 175.53(10) yes O2 Co O2 2_674 . 95.78(4) yes O2 Co O2 3_574 . 163.19(6) yes O1 Co O2 1_554 . 86.44(6) yes O4 Co O2 . . 89.84(8) yes O2 Co O2 2_674 4_755 163.20(6) yes O2 Co O2 3_574 4_755 95.78(4) yes O1 Co O2 1_554 4_755 86.44(6) yes O4 Co O2 . 4_755 89.84(7) yes O2 Co O2 . 4_755 67.43(7) yes O2 Co P 2_674 . 129.45(4) no O2 Co P 3_574 . 129.45(4) no O1 Co P 1_554 . 84.23(6) no O4 Co P . . 91.29(8) no O2 Co P . . 33.74(3) no O2 Co P 4_755 . 33.74(3) no O1 P O3 . . 109.31(11) yes O1 P O2 . . 111.70(7) yes O3 P O2 . . 110.17(7) yes O1 P O2 . 4_755 111.70(7) yes O3 P O2 . 4_755 110.17(7) yes O2 P O2 . 4_755 103.70(11) yes O1 P Co . . 129.59(9) no O3 P Co . . 121.10(8) no O2 P Co . . 51.91(6) no O2 P Co 4_755 . 51.91(6) no H1 N H2 . . 111(3) yes H1 N H3 . . 99(5) yes H2 N H3 . . 116(3) yes P O2 Co . 2_675 124.78(8) yes P O2 Co . . 94.35(7) yes Co O2 Co 2_675 . 121.12(7) yes P O1 Co . 1_556 134.64(13) yes Co O4 H4 . . 106(3) 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 Co O2 2_674 2.0542(14) yes Co O2 3_574 2.0542(14) yes Co O1 1_554 2.056(2) yes Co O4 . 2.186(2) yes Co O2 . 2.2077(14) yes Co O2 4_755 2.2077(14) yes Co P . 2.7971(9) no P O1 . 1.520(2) yes P O3 . 1.532(2) yes P O2 . 1.5581(14) yes P O2 4_75 1.5581(14) yes N H1 . 0.8500(11) no N H2 . 0.8500(11) no N H3 . 0.8500(11) no O2 Co 2_675 2.0542(14) no O1 Co 1_556 2.056(2) no O4 H4 . 0.74(3) no 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 O4 H4 O1 3_574 0.75(3) 2.35(3) 2.8440(10) 125(3) O4 H4 O2 3_575 0.75(3) 2.27(4) 2.962(3) 155(3) N H1 O3 . 0.850(10) 1.96(4) 2.795(3) 166(4) N H2 O3 3_564 0.850(10) 2.18(2) 2.9650(10) 153(2) N H3 O3 1_554 0.850(10) 1.96(3) 2.785(3) 165(3)