#------------------------------------------------------------------------------ #$Date: 2009-11-16 01:43:51 +0000 (Mon, 16 Nov 2009) $ #$Revision: 853 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003539.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003539 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 1047 _journal_page_last 1049 _publ_section_title ; Nickel Ultraphosphate, NiP~4~O~11~ ; _chemical_formula_sum 'Ni O11 P4' _chemical_formula_weight 358.59 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3750(10) _cell_length_b 8.0190(10) _cell_length_c 11.135(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.730(10) _cell_angle_gamma 90.00 _cell_volume 822.5(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 2.896 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 18.41 _exptl_absorpt_coefficient_mu 3.020 _cell_measurement_temperature 299(2) _exptl_crystal_description Needle _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_colour 'light green' _chemical_compound_source ? _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method '\q/2\q' _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2144 _exptl_absorpt_correction_T_max 0.2674 _diffrn_reflns_number 6490 _reflns_number_total 3602 _reflns_number_observed 2571 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_theta_max 34.96 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 2.9 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0265 _refine_ls_wR_factor_obs 0.0614 _refine_ls_wR_factor_all 0.0683 _refine_ls_goodness_of_fit_obs 1.100 _refine_ls_goodness_of_fit_all 1.026 _refine_ls_number_reflns 3602 _refine_ls_number_parameters 145 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme ; calc w = 1/[\s^2^(F~o~^2^) + (0.0330P)^2^ + 0.0299P] where P = (F~o~^2^ + 2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.002 _refine_diff_density_max 0.683 _refine_diff_density_min -0.636 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'Ni' 'Ni' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.2850 1.1 'P' 'P' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0900 0.095 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0080 0.006 _computing_data_collection ; CAD-4 Diffractometer Control Software (Enraf-Nonius, 1993) ; _computing_structure_solution ; Enraf-Nonius Structure Determination Package (Frenz, 1993) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Ni1 1 0.03312(3) 1.01493(3) 0.78053(2) 0.00858(6) P2 1 -0.28727(5) 0.62572(6) 0.54285(4) 0.00806(8) P3 1 0.31224(5) 0.88687(6) 0.67510(4) 0.00734(8) P4 1 -0.05998(5) 0.61181(6) 0.75521(4) 0.00736(8) P5 1 0.25814(5) 1.00091(6) 0.42755(4) 0.00742(8) O6 1 0.15712(15) 0.9198(2) 0.66799(13) 0.0119(3) O7 1 0.34376(15) 0.8961(2) 0.53562(12) 0.0098(2) O8 1 0.1132(2) 1.2420(2) 0.76443(13) 0.0138(3) O9 1 -0.0753(2) 0.7855(2) 0.79050(14) 0.0134(3) O10 1 -0.1187(2) 1.0695(2) 0.62728(13) 0.0135(3) O11 1 0.40104(15) 1.0525(2) 0.73149(13) 0.0108(2) O12 1 -0.1300(2) 0.5691(2) 0.62058(12) 0.0123(3) O13 1 -0.1043(2) 1.1173(2) 0.87894(14) 0.0166(3) O14 1 -0.2550(2) 0.8205(2) 0.51975(13) 0.0127(3) O15 1 -0.1302(2) 0.4859(2) 0.83688(13) 0.0110(2) O16 1 0.1973(2) 0.9592(2) 0.92468(13) 0.0137(3) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Ni1 0.00804(10) 0.00007(8) 0.00089(7) 0.00872(10) -0.00052(8) 0.00872(10) P2 0.0083(2) -0.0003(2) 0.00049(14) 0.0085(2) -0.00003(15) 0.0070(2) P3 0.0071(2) 0.00072(15) 0.00078(14) 0.0074(2) 0.00006(15) 0.0072(2) P4 0.0072(2) 0.0004(2) 0.00063(14) 0.0076(2) 0.0006(2) 0.0070(2) P5 0.0073(2) 0.0002(2) 0.00062(13) 0.0082(2) -0.00003(15) 0.0065(2) O6 0.0071(6) 0.0016(5) 0.0015(5) 0.0159(6) -0.0027(5) 0.0126(6) O7 0.0105(6) 0.0033(5) 0.0008(4) 0.0117(6) 0.0010(4) 0.0068(5) O8 0.0177(7) -0.0059(5) 0.0022(5) 0.0107(6) -0.0027(5) 0.0129(6) O9 0.0152(7) 0.0002(5) 0.0036(5) 0.0075(6) -0.0013(5) 0.0178(7) O10 0.0095(6) -0.0018(5) -0.0020(5) 0.0180(7) 0.0011(5) 0.0114(6) O11 0.0074(6) -0.0018(5) 0.0016(5) 0.0124(6) -0.0043(5) 0.0127(6) O12 0.0113(6) 0.0037(5) -0.0015(5) 0.0160(6) -0.0009(5) 0.0083(5) O13 0.0155(7) 0.0004(6) 0.0079(5) 0.0168(7) -0.0026(6) 0.0191(7) O14 0.0188(7) -0.0002(5) 0.0062(5) 0.0076(6) 0.0001(5) 0.0130(6) O15 0.0119(6) -0.0002(5) 0.0050(4) 0.0109(6) 0.0007(5) 0.0113(6) O16 0.0144(7) 0.0002(5) -0.0024(5) 0.0150(6) 0.0039(5) 0.0099(6)