#------------------------------------------------------------------------------ #$Date: 2011-09-17 22:27:16 +0200 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003097.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_2003097 _journal_name_full 'Acta Crystallographica, Section B' _journal_volume 55 _journal_year 1999 _journal_page_first 165 _journal_page_last 169 _chemical_formula_sum 'Ca15 I O37 P9' _chemical_formula_iupac '[Ca15 (PO4)9 I O]' _chemical_formula_weight 1598.8 _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'P 63/m' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x-y,x,1/2+z 3 -y,x-y,z 4 -x,-y,1/2+z 5 -x+y,-x,z 6 y,-x+y,1/2+z 7 -x,-y,-z 8 -x+y,-x,1/2-z 9 y,-x+y,-z 10 x,y,1/2-z 11 x-y,x,-z 12 -y,x-y,1/2-z _cell_length_a 9.5670(10) _cell_length_b 9.5670(10) _cell_length_c 20.754(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 1645.07 _cell_formula_units_Z 2 _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 23.9 _cell_measurement_temperature 293 _exptl_crystal_description 'hexagonal rod' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.025 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 3.227 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 3.887 _exptl_absorpt_correction_type 'numerical from crystal shape' _exptl_absorpt_correction_T_min 0.8591 _exptl_absorpt_correction_T_max 0.9169 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'STOE IPDS' _diffrn_measurement_device 'area detector' _diffrn_measurement_method 'phi rotation' _diffrn_reflns_number 878 _diffrn_reflns_av_R_equivalents 0.0836 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.90 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _reflns_number_total 878 _reflns_number_observed 419 _reflns_observed_criterion 'I>2\s(I)' _refine_ls_structure_factor_coef F _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_obs 0.0452 _refine_ls_wR_factor_all 0.0545 _refine_ls_wR_factor_obs 0.0459 _refine_ls_goodness_of_fit_all 1.01 _refine_ls_goodness_of_fit_obs 1.29 _refine_ls_number_reflns 878 _refine_ls_number_parameters 72 _refine_ls_weighting_scheme 'w=1/(\s^2^(F)+0.0004F^2^)' _refine_ls_weighting_details ? _refine_ls_shift/esd_max 0.0001 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_max 2.50 _refine_diff_density_min -2.48 _refine_ls_extinction_method none _refine_ls_extinction_coef - loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ca 0.226 0.306 International_Tables_Vol_C P 0.102 0.094 International_Tables_Vol_C O 0.011 0.006 International_Tables_Vol_C I -0.474 1.812 International_Tables_Vol_C loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy O(11) 0.4730(10) 0.5900(10) 0.25 0.028(3) 1 O(12) 0.4599(9) 0.5848(8) 0.5930(5) 0.028(3) 1 O(21) 0.4810(10) 0.3280(10) 0.25 0.010(2) 1 O(22) 0.4886(8) 0.3353(8) 0.5830(4) 0.010(2) 1 O(31) 0.2680(10) 0.3600(10) 0.1901(5) 0.034(2) 1 O(32) 0.2831(9) 0.3750(10) 0.5186(4) 0.034(2) 1 O(33) 0.2450(10) 0.3180(10) 0.8634(5) 0.034(2) 1 P(11) 0.3731(5) 0.4048(5) 0.25 0.0063(7) 1 P(12) 0.3690(3) 0.3999(3) 0.5826(2) 0.0063(7) 1 Ca(11) 0.333333 0.666667 0.1665(2) 0.0103(5) 1 Ca(12) 0.333333 0.666667 0.5008(3) 0.0103(5) 1 Ca(13) 0.333333 0.666667 0.8297(2) 0.0103(5) 1 Ca(21) 0.2435(5) 0.0041(4) 0.25 0.028(2) 1 Ca(22) 0.2765(3) 0.0144(3) 0.58590(10) 0.0180(10) 1 I(11) 0 0 0 0.0211(9) 0.70(10) I(12) 0 0 0.1716(6) 0.0211(9) 0.174(3) O(41) 0 0 0.237(3) 0.0211(9) 0.35(2) O(42) 0 0 0.384(6) 0.0211(9) 0.14(2) 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 O(11) 0.017(3) 0.010(3) 0.060(6) 0.008(2) 0 0 O(12) 0.017(3) 0.010(3) 0.060(6) 0.008(2) 0 0 O(21) 0.012(2) 0.015(2) 0.011(3) 0.011(2) 0 0 O(22) 0.012(2) 0.015(2) 0.011(3) 0.011(2) 0 0 O(31) 0.029(2) 0.055(3) 0.034(3) 0.033(3) -0.021(2) -0.029(3) O(32) 0.029(2) 0.055(3) 0.034(3) 0.033(3) -0.021(2) -0.029(3) O(33) 0.029(2) 0.055(3) 0.034(3) 0.033(3) -0.021(2) -0.029(3) P(11) 0.0063(9) 0.0078(9) 0.0080(10) 0.0056(7) 0 0 P(12) 0.0063(9) 0.0078(9) 0.0080(10) 0.0056(7) 0 0 Ca(11) 0.0114(6) 0.0114(6) 0.0080(10) 0.0057(3) 0 0 Ca(12) 0.0114(6) 0.0114(6) 0.0080(10) 0.0057(3) 0 0 Ca(13) 0.0114(6) 0.0114(6) 0.0080(10) 0.0057(3) 0 0 Ca(21) 0.052(3) 0.010(2) 0.017(2) 0.012(2) 0 0 Ca(22) 0.0250(10) 0.0150(10) 0.0120(10) 0.0080(10) 0.0010(10) 0.0020(10) I(11) 0.0033(8) 0.0033(8) 0.057(2) 0.0016(4) 0 0 I(12) 0.0033(8) 0.0033(8) 0.057(2) 0.0016(4) 0 0 O(41) 0.0033(8) 0.0033(8) 0.057(2) 0.0016(4) 0 0 O(42) 0.0033(8) 0.0033(8) 0.057(2) 0.0016(4) 0 0 _cod_database_code 2003097