# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'P. Wright' _publ_contact_author_address ; School of Chemistry St Andrews University The Purdie Building St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email PAW2@ST-AND.AC.UK _publ_section_title ; The first route to large pore metal phosphonates ; loop_ _publ_author_name 'P. Wright' 'John A. Groves' 'Philip Lightfoot' 'Caroline Mellot-Draznieks' 'Stuart R. Miller' ; S.J.Warrender ; data_stan346_0m _database_code_depnum_ccdc_archive 'CCDC 603413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C6 H12 Fe N2 O6 P2), O3' _chemical_formula_sum 'C12 H24 Fe2 N4 O15 P4' _chemical_formula_weight 699.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 _symmetry_space_group_name_Hall -p1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3081(7) _cell_length_b 9.1647(7) _cell_length_c 9.1839(7) _cell_angle_alpha 62.781(1) _cell_angle_beta 79.029(1) _cell_angle_gamma 87.088(1) _cell_volume 609.95(8) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 26.79 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 1.536 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0 _exptl_absorpt_correction_T_max 0 _exptl_absorpt_process_details - _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.69999 _diffrn_radiation_type 'synchrotron radiation' _diffrn_radiation_source 'SRS Daresbury Laboratories' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4497 _diffrn_reflns_av_R_equivalents 0.0258 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 26.79 _reflns_number_total 2473 _reflns_number_gt 2128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0596P)^2^+2.1652P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2473 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0583 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1230 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.75944(7) 0.42363(7) 0.57038(7) 0.00941(19) Uani 1 1 d . . . P1 P 0.42074(13) 0.46684(13) 0.75806(13) 0.0098(3) Uani 1 1 d . . . P2 P 0.94306(12) 0.74802(13) 0.53460(13) 0.0077(2) Uani 1 1 d . . . O1 O 0.5580(4) 0.3523(4) 0.7486(4) 0.0181(7) Uani 1 1 d . . . O2 O 0.2973(4) 0.4769(5) 0.6521(4) 0.0307(9) Uani 1 1 d . . . O3 O 0.8726(4) 0.5717(4) 0.6214(4) 0.0134(6) Uani 1 1 d . . . O4 O 1.1009(3) 0.7673(4) 0.4085(4) 0.0123(6) Uani 1 1 d . . . O5 O 0.4814(4) 0.6320(4) 0.7291(4) 0.0204(7) Uani 1 1 d . . . O6 O 0.9580(3) 0.8059(3) 0.6610(4) 0.0114(6) Uani 1 1 d . . . O7 O 0.8058(11) 0.0393(9) 0.9390(9) 0.0281(17) Uiso 0.50 1 d P . . O8 O 0.8903(10) 0.0380(9) 0.9368(9) 0.0252(16) Uiso 0.50 1 d P . . O9 O 0.5513(8) 0.0247(8) 0.9837(9) 0.0232(15) Uiso 0.50 1 d P . . N1 N 0.1484(4) 0.4086(4) 1.0255(4) 0.0088(7) Uani 1 1 d . . . N2 N 0.6373(4) 0.8963(4) 0.4845(4) 0.0097(7) Uani 1 1 d . . . C1 C 0.3158(5) 0.3551(5) 0.9757(5) 0.0100(8) Uani 1 1 d . . . H1A H 0.3052 0.2403 1.0022 0.012 Uiso 1 1 calc R . . H1B H 0.3866 0.3618 1.0453 0.012 Uiso 1 1 calc R . . C2 C 0.8041(5) 0.8766(5) 0.3986(5) 0.0096(8) Uani 1 1 d . . . H2A H 0.8567 0.9848 0.3290 0.012 Uiso 1 1 calc R . . H2B H 0.7893 0.8305 0.3254 0.012 Uiso 1 1 calc R . . C3 C 0.0194(5) 0.3696(5) 0.9523(5) 0.0098(8) Uani 1 1 d . . . H3A H 0.0187 0.2536 0.9820 0.012 Uiso 1 1 calc R . . H3B H 0.0449 0.4311 0.8317 0.012 Uiso 1 1 calc R . . C4 C 0.1481(5) 0.5866(5) 0.9836(5) 0.0096(8) Uani 1 1 d . . . H4A H 0.1764 0.6527 0.8637 0.012 Uiso 1 1 calc R . . H4B H 0.2298 0.6103 1.0333 0.012 Uiso 1 1 calc R . . C5 C 0.5223(5) 0.9623(5) 0.3620(5) 0.0104(8) Uani 1 1 d . . . H5A H 0.5128 0.8863 0.3171 0.013 Uiso 1 1 calc R . . H5B H 0.5670 1.0664 0.2701 0.013 Uiso 1 1 calc R . . C6 C 0.6467(5) 1.0137(5) 0.5556(5) 0.0094(8) Uani 1 1 d . . . H6A H 0.6936 1.1187 0.4672 0.011 Uiso 1 1 calc R . . H6B H 0.7180 0.9714 0.6371 0.011 Uiso 1 1 calc R . . 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 Fe1 0.0063(3) 0.0134(3) 0.0105(3) -0.0084(3) 0.0018(2) -0.0007(2) P1 0.0060(5) 0.0129(5) 0.0076(5) -0.0036(4) 0.0029(4) -0.0013(4) P2 0.0061(5) 0.0086(5) 0.0083(5) -0.0046(4) 0.0007(4) 0.0000(4) O1 0.0139(16) 0.0127(15) 0.0207(17) -0.0066(13) 0.0105(13) -0.0032(12) O2 0.0156(18) 0.060(3) 0.0116(17) -0.0126(17) -0.0001(13) -0.0050(17) O3 0.0168(16) 0.0113(15) 0.0127(15) -0.0059(12) -0.0019(12) -0.0033(12) O4 0.0085(14) 0.0150(15) 0.0119(15) -0.0062(12) 0.0015(11) 0.0018(12) O5 0.0229(18) 0.0086(15) 0.0204(17) -0.0038(13) 0.0106(14) -0.0031(13) O6 0.0120(15) 0.0123(15) 0.0113(15) -0.0073(12) 0.0006(12) -0.0021(12) N1 0.0035(16) 0.0107(17) 0.0120(17) -0.0061(14) 0.0014(13) -0.0007(13) N2 0.0048(16) 0.0139(18) 0.0121(17) -0.0082(15) -0.0001(13) 0.0015(13) C1 0.0061(19) 0.012(2) 0.0088(19) -0.0036(16) 0.0030(15) 0.0010(15) C2 0.0065(19) 0.012(2) 0.0091(19) -0.0052(16) 0.0031(15) 0.0015(15) C3 0.009(2) 0.012(2) 0.0093(19) -0.0059(16) -0.0010(15) -0.0008(15) C4 0.0039(18) 0.0086(19) 0.015(2) -0.0058(17) 0.0044(15) -0.0033(15) C5 0.010(2) 0.013(2) 0.010(2) -0.0062(17) -0.0030(16) 0.0024(16) C6 0.0067(19) 0.0101(19) 0.014(2) -0.0078(17) -0.0019(15) -0.0013(15) _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 Fe1 O3 1.956(3) . ? Fe1 O2 1.962(3) 2_666 ? Fe1 O1 2.000(3) . ? Fe1 O4 2.004(3) 2_766 ? P1 O5 1.508(3) . ? P1 O2 1.515(3) . ? P1 O1 1.527(3) . ? P1 C1 1.833(4) . ? P2 O6 1.507(3) . ? P2 O3 1.526(3) . ? P2 O4 1.533(3) . ? P2 C2 1.830(4) . ? O2 Fe1 1.962(3) 2_666 ? O4 Fe1 2.004(3) 2_766 ? O7 O8 0.698(9) . ? O9 O9 0.916(12) 2_657 ? N1 C4 1.495(5) . ? N1 C3 1.504(5) . ? N1 C1 1.510(5) . ? N2 C6 1.503(5) . ? N2 C2 1.505(5) . ? N2 C5 1.508(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.514(5) 2_567 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C3 1.514(5) 2_567 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.519(5) 2_676 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C5 1.519(5) 2_676 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? 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 O3 Fe1 O2 115.20(15) . 2_666 ? O3 Fe1 O1 102.10(13) . . ? O2 Fe1 O1 111.18(14) 2_666 . ? O3 Fe1 O4 109.57(13) . 2_766 ? O2 Fe1 O4 107.69(15) 2_666 2_766 ? O1 Fe1 O4 111.06(12) . 2_766 ? O5 P1 O2 113.8(2) . . ? O5 P1 O1 113.78(18) . . ? O2 P1 O1 111.6(2) . . ? O5 P1 C1 108.34(19) . . ? O2 P1 C1 106.40(19) . . ? O1 P1 C1 101.87(18) . . ? O6 P2 O3 110.50(17) . . ? O6 P2 O4 114.99(17) . . ? O3 P2 O4 111.07(17) . . ? O6 P2 C2 110.26(18) . . ? O3 P2 C2 107.68(18) . . ? O4 P2 C2 101.80(17) . . ? P1 O1 Fe1 123.60(18) . . ? P1 O2 Fe1 147.3(2) . 2_666 ? P2 O3 Fe1 138.86(19) . . ? P2 O4 Fe1 121.77(17) . 2_766 ? C4 N1 C3 110.0(3) . . ? C4 N1 C1 112.6(3) . . ? C3 N1 C1 112.4(3) . . ? C6 N2 C2 110.9(3) . . ? C6 N2 C5 108.5(3) . . ? C2 N2 C5 109.9(3) . . ? N1 C1 P1 118.1(3) . . ? N1 C1 H1A 107.8 . . ? P1 C1 H1A 107.8 . . ? N1 C1 H1B 107.8 . . ? P1 C1 H1B 107.8 . . ? H1A C1 H1B 107.1 . . ? N2 C2 P2 116.1(3) . . ? N2 C2 H2A 108.3 . . ? P2 C2 H2A 108.3 . . ? N2 C2 H2B 108.3 . . ? P2 C2 H2B 108.3 . . ? H2A C2 H2B 107.4 . . ? N1 C3 C4 110.4(3) . 2_567 ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 2_567 . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 2_567 . ? H3A C3 H3B 108.1 . . ? N1 C4 C3 110.3(3) . 2_567 ? N1 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 2_567 . ? N1 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 2_567 . ? H4A C4 H4B 108.1 . . ? N2 C5 C6 111.2(3) . 2_676 ? N2 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 2_676 . ? N2 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 2_676 . ? H5A C5 H5B 108.0 . . ? N2 C6 C5 111.1(3) . 2_676 ? N2 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 2_676 . ? N2 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 2_676 . ? H6A C6 H6B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.79 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.880 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.129 # Attachment 'ATT165744.txt' data_stan324_0m _database_code_depnum_ccdc_archive 'CCDC 603414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 Co8 N7 O30 P6' _chemical_formula_sum 'C27 H48 Co8 N7 O30 P6' _chemical_formula_weight 1608.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' 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' 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' _symmetry_cell_setting TRIGONAL _symmetry_space_group_name_H-M P-3c1 _symmetry_space_group_name_Hall -P32c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' _cell_length_a 19.1430(16) _cell_length_b 19.1430(16) _cell_length_c 9.2700(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2941.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3612 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 1.807 _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1549 _exptl_absorpt_coefficient_mu 2.444 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0 _exptl_absorpt_correction_T_max 0 _exptl_absorpt_process_details - _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.67130 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'SRS Daresbury Laboratories' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31789 _diffrn_reflns_av_R_equivalents 0.1097 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.03 _reflns_number_total 2831 _reflns_number_gt 2138 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0784P)^2^+12.7950P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2831 _refine_ls_number_parameters 122 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0531 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.6667 0.3333 0.23408(9) 0.0117(2) Uani 1 3 d S . . Co2 Co 0.69663(4) 0.18915(4) -0.31162(6) 0.01532(17) Uani 1 1 d . . . P1 P 0.63284(6) 0.19487(6) -0.00524(11) 0.0122(2) Uani 1 1 d . . . O1 O 0.54406(19) 0.15673(19) 0.0341(3) 0.0180(6) Uani 1 1 d . . . O2 O 0.68832(19) 0.25384(18) 0.1089(3) 0.0147(6) Uani 1 1 d . . . O3 O 0.65141(19) 0.23227(18) -0.1570(3) 0.0140(6) Uani 1 1 d . . . O4 O 0.8114(4) 0.2525(5) -0.1895(8) 0.0238(14) Uiso 0.50 1 d P . . O5 O 0.7535(7) 0.1507(6) -0.4598(11) 0.041(2) Uiso 0.50 1 d P . . O6 O 0.8063(6) 0.2195(6) -0.2282(10) 0.041(2) Uiso 0.50 1 d P . . O7 O 0.7752(7) 0.1498(6) -0.4227(12) 0.045(2) Uiso 0.50 1 d P . . N1 N 0.6397(2) 0.0776(2) -0.1684(4) 0.0145(7) Uani 1 1 d . . . N2 N 0.894(7) -0.004(7) -0.045(12) 0.08(3) Uiso 0.08 1 d P . . C1 C 0.6575(3) 0.1148(3) -0.0224(4) 0.0154(8) Uani 1 1 d . . . H1A H 0.7155 0.1371 -0.0012 0.019 Uiso 1 1 calc R . . H1B H 0.6263 0.0725 0.0501 0.019 Uiso 1 1 calc R . . C2 C 0.6738(3) 0.0229(3) -0.1782(5) 0.0198(9) Uani 1 1 d . . . H2 H 0.6469 -0.0186 -0.1010 0.024 Uiso 1 1 calc R . . C3 C 0.5511(3) 0.0251(3) -0.1812(4) 0.0155(8) Uani 1 1 d . . . H3A H 0.5256 0.0591 -0.1793 0.019 Uiso 1 1 calc R . . H3B H 0.5309 -0.0115 -0.0969 0.019 Uiso 1 1 calc R . . C4 C 0.7641(9) 0.0593(10) -0.156(2) 0.060(5) Uani 0.50 1 d P . . H4A H 0.7798 0.0887 -0.0640 0.090 Uiso 0.50 1 calc PR . . H4B H 0.7932 0.0965 -0.2350 0.090 Uiso 0.50 1 calc PR . . H4C H 0.7775 0.0162 -0.1536 0.090 Uiso 0.50 1 calc PR . . C5 C 0.8245(12) 0.1815(12) -0.3124(19) 0.065(4) Uiso 0.50 1 d P . . C6 C 0.8992(15) 0.1731(15) -0.307(3) 0.092(7) Uiso 0.50 1 d P . . H6A H 0.8984 0.1401 -0.3885 0.138 Uiso 0.50 1 calc PR . . H6B H 0.8999 0.1472 -0.2164 0.138 Uiso 0.50 1 calc PR . . H6C H 0.9474 0.2267 -0.3131 0.138 Uiso 0.50 1 calc PR . . 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 Co1 0.0142(3) 0.0142(3) 0.0067(4) 0.000 0.000 0.00709(15) Co2 0.0184(3) 0.0169(3) 0.0113(3) 0.0002(2) -0.0003(2) 0.0093(2) P1 0.0150(5) 0.0121(5) 0.0078(4) -0.0005(3) 0.0000(3) 0.0055(4) O1 0.0172(15) 0.0167(15) 0.0159(14) -0.0025(11) 0.0029(11) 0.0054(12) O2 0.0184(15) 0.0148(14) 0.0100(13) -0.0011(10) -0.0007(11) 0.0076(12) O3 0.0197(15) 0.0159(14) 0.0074(12) 0.0012(10) 0.0023(10) 0.0095(12) N1 0.0159(16) 0.0165(17) 0.0102(15) -0.0033(12) -0.0022(12) 0.0074(14) C1 0.020(2) 0.0156(19) 0.0096(17) -0.0006(14) -0.0018(14) 0.0079(17) C2 0.018(2) 0.021(2) 0.020(2) -0.0074(17) -0.0053(16) 0.0097(18) C3 0.0157(19) 0.017(2) 0.0119(18) -0.0012(15) 0.0013(14) 0.0067(16) C4 0.051(9) 0.055(9) 0.090(12) -0.043(9) -0.020(8) 0.038(8) _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 Co1 O3 2.069(3) 12_666 ? Co1 O3 2.069(3) 10_656 ? Co1 O3 2.069(3) 11_556 ? Co1 O2 2.113(3) . ? Co1 O2 2.113(3) 2_655 ? Co1 O2 2.113(3) 3_665 ? Co2 O1 2.004(3) 10_655 ? Co2 O6 2.030(10) . ? Co2 O3 2.049(3) . ? Co2 O5 2.101(10) . ? Co2 O2 2.172(3) 12_665 ? Co2 O4 2.217(7) . ? Co2 O7 2.241(11) . ? Co2 N1 2.276(4) . ? P1 O1 1.521(3) . ? P1 O2 1.524(3) . ? P1 O3 1.537(3) . ? P1 C1 1.823(4) . ? O4 O6 0.690(10) . ? O4 C5 1.88(2) . ? O5 O7 0.546(13) . ? O5 C5 1.81(2) . ? O6 C5 1.23(2) . ? O7 C5 1.32(2) . ? N1 C3 1.482(5) . ? N1 C1 1.487(5) . ? N1 C2 1.489(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C4 1.521(15) . ? C2 C2 1.531(8) 4_554 ? C2 H2 1.0000 . ? C3 C3 1.523(8) 4_554 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.52(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? 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 O3 Co1 O3 98.22(10) 12_666 10_656 ? O3 Co1 O3 98.22(10) 12_666 11_556 ? O3 Co1 O3 98.22(10) 10_656 11_556 ? O3 Co1 O2 82.15(11) 12_666 . ? O3 Co1 O2 86.82(11) 10_656 . ? O3 Co1 O2 174.82(12) 11_556 . ? O3 Co1 O2 86.82(11) 12_666 2_655 ? O3 Co1 O2 174.82(12) 10_656 2_655 ? O3 Co1 O2 82.15(11) 11_556 2_655 ? O2 Co1 O2 92.72(11) . 2_655 ? O3 Co1 O2 174.82(12) 12_666 3_665 ? O3 Co1 O2 82.15(11) 10_656 3_665 ? O3 Co1 O2 86.82(11) 11_556 3_665 ? O2 Co1 O2 92.72(11) . 3_665 ? O2 Co1 O2 92.72(11) 2_655 3_665 ? O1 Co2 O6 156.2(3) 10_655 . ? O1 Co2 O3 100.89(13) 10_655 . ? O6 Co2 O3 101.7(3) . . ? O1 Co2 O5 84.3(3) 10_655 . ? O6 Co2 O5 72.9(4) . . ? O3 Co2 O5 174.6(3) . . ? O1 Co2 O2 86.66(12) 10_655 12_665 ? O6 Co2 O2 89.4(3) . 12_665 ? O3 Co2 O2 81.18(11) . 12_665 ? O5 Co2 O2 97.7(3) . 12_665 ? O1 Co2 O4 162.9(2) 10_655 . ? O6 Co2 O4 18.0(3) . . ? O3 Co2 O4 85.7(2) . . ? O5 Co2 O4 88.9(4) . . ? O2 Co2 O4 78.7(2) 12_665 . ? O1 Co2 O7 97.9(3) 10_655 . ? O6 Co2 O7 60.0(4) . . ? O3 Co2 O7 161.2(3) . . ? O5 Co2 O7 14.0(3) . . ? O2 Co2 O7 101.7(3) 12_665 . ? O4 Co2 O7 76.8(4) . . ? O1 Co2 N1 101.07(13) 10_655 . ? O6 Co2 N1 89.3(3) . . ? O3 Co2 N1 82.49(12) . . ? O5 Co2 N1 98.2(3) . . ? O2 Co2 N1 163.00(12) 12_665 . ? O4 Co2 N1 95.4(2) . . ? O7 Co2 N1 92.3(3) . . ? O1 P1 O2 112.74(18) . . ? O1 P1 O3 112.70(18) . . ? O2 P1 O3 112.15(17) . . ? O1 P1 C1 108.31(19) . . ? O2 P1 C1 107.81(18) . . ? O3 P1 C1 102.42(17) . . ? P1 O1 Co2 128.87(19) . 10_656 ? P1 O2 Co1 126.84(19) . . ? P1 O2 Co2 139.41(19) . 12_666 ? Co1 O2 Co2 93.27(11) . 12_666 ? P1 O3 Co2 119.89(17) . . ? P1 O3 Co1 140.67(18) . 10_655 ? Co2 O3 Co1 98.32(12) . 10_655 ? O6 O4 Co2 65.5(11) . . ? C5 O4 Co2 75.5(6) . . ? O7 O5 Co2 97.8(19) . . ? C5 O5 Co2 80.1(7) . . ? O4 O6 C5 156.9(17) . . ? O4 O6 Co2 96.5(12) . . ? C5 O6 Co2 98.5(11) . . ? O5 O7 C5 149(2) . . ? O5 O7 Co2 68.3(18) . . ? C5 O7 Co2 86.3(10) . . ? C3 N1 C1 107.9(3) . . ? C3 N1 C2 105.9(3) . . ? C1 N1 C2 108.4(3) . . ? C3 N1 Co2 116.0(3) . . ? C1 N1 Co2 101.2(2) . . ? C2 N1 Co2 116.9(3) . . ? N1 C1 P1 112.8(3) . . ? N1 C1 H1A 109.0 . . ? P1 C1 H1A 109.0 . . ? N1 C1 H1B 109.0 . . ? P1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? N1 C2 C4 117.8(6) . . ? N1 C2 C2 110.8(3) . 4_554 ? C4 C2 C2 108.4(6) . 4_554 ? N1 C2 H2 106.4 . . ? C4 C2 H2 106.4 . . ? C2 C2 H2 106.4 4_554 . ? N1 C3 C3 112.8(3) . 4_554 ? N1 C3 H3A 109.0 . . ? C3 C3 H3A 109.0 4_554 . ? N1 C3 H3B 109.0 . . ? C3 C3 H3B 109.0 4_554 . ? H3A C3 H3B 107.8 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O6 C5 O7 114.5(16) . . ? O6 C5 C6 127.1(18) . . ? O7 C5 C6 118.2(17) . . ? O6 C5 O5 106.4(13) . . ? C6 C5 O5 125.9(16) . . ? O7 C5 O4 118.6(13) . . ? C6 C5 O4 122.0(15) . . ? O5 C5 O4 110.0(10) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 29.84 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.777 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.166 # Attachment 'ATT165745.txt' data_TEST_publ _database_code_depnum_ccdc_archive 'CCDC 603415' _pd_block_id 2006-06-08T14:27|TEST|SJW|stoe _audit_creation_method 'from EXP file using GSAS2CIF' _audit_creation_date 2006-06-08T14:27 _audit_author_name SJW _audit_update_record ; 2006-06-08T14:27 Initial CIF as created by GSAS2CIF ; #============================================================================= # this information describes the project, paper etc. for the CIF # # Acta Cryst. Section C papers and editorial correspondence is generated # # from the information in this section # # # # (from) CIF submission form for Rietveld refinements (Acta Cryst. C) # # Version 14 December 1998 # #============================================================================= #============================================================================= # 5. OVERALL REFINEMENT & COMPUTING DETAILS _refine_special_details ; ? ; _pd_proc_ls_special_details ; ? ; # The following items are used to identify the programs used. _computing_molecular_graphics ? _computing_publication_material ? _refine_ls_weighting_scheme ? _refine_ls_weighting_details ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method ? _refine_ls_extinction_coef ? _refine_ls_number_constraints ? _refine_ls_restrained_S_all ? _refine_ls_restrained_S_obs ? #============================================================================== # 6. SAMPLE PREPARATION DATA # (In the unusual case where multiple samples are used in a single # Rietveld study, this information should be moved into the phase # blocks) # The following three fields describe the preparation of the material. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? _pd_char_colour ? # use ICDD colour descriptions _refine_ls_shift/su_max 0.02 _refine_ls_shift/su_mean 0.01 _computing_structure_refinement GSAS _refine_ls_number_parameters 42 _refine_ls_goodness_of_fit_all 2.60 _refine_ls_number_restraints 29 _refine_ls_matrix_type full #============================================================================== # 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA _pd_char_particle_morphology ? _chemical_name_systematic ; ? ; _chemical_name_common JAGNipip _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products _symmetry_space_group_name_Hall ? _exptl_crystal_F_000 ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _cell_measurement_temperature ? _cell_special_details ; ? ; _geom_special_details ? # The following item identifies the program(s) used (if appropriate). _computing_structure_solution ? #============================================================================== # 8. Phase information from GSAS _pd_phase_name JAGNipip _cell_length_a 27.9486(4) _cell_length_b 27.9486 _cell_length_c 6.23018(14) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 120.0 _cell_volume 4214.6(1) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +x,+y,+z 2 -y,x-y,+z 3 y-x,-x,+z -1 -x,-y,-z -2 +y,y-x,-z -3 x-y,+x,-z 101 +x+1/3,+y+2/3,+z+2/3 102 -y+1/3,x-y+2/3,+z+2/3 103 y-x+1/3,-x+2/3,+z+2/3 -101 -x+2/3,-y+1/3,-z+1/3 -102 +y+2/3,y-x+1/3,-z+1/3 -103 x-y+2/3,+x+1/3,-z+1/3 201 +x+2/3,+y+1/3,+z+1/3 202 -y+2/3,x-y+1/3,+z+1/3 203 y-x+2/3,-x+1/3,+z+1/3 -201 -x+1/3,-y+2/3,-z+2/3 -202 +y+1/3,y-x+2/3,-z+2/3 -203 x-y+1/3,+x+2/3,-z+2/3 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity NI Ni1 0.63786(19) 0.02840(21) 0.0517(7) 1.0 Uiso 0.0053(4) 18 P P1 0.61355(32) 0.03959(32) -0.4271(13) 1.0 Uiso 0.0053(4) 18 O O1 0.6141(6) 0.0947(5) -0.4815(23) 1.0 Uiso 0.0053(4) 18 O O2 0.6306(7) 0.0104(6) -0.6308(26) 1.0 Uiso 0.0053(4) 18 O O3 0.6611(6) 0.0472(7) -0.2712(25) 1.0 Uiso 0.0053(4) 18 O O4 0.6566(5) 0.1098(6) 0.1253(24) 1.0 Uiso 0.0053(4) 18 N N1 0.5567(9) 0.0062(8) -0.0294(31) 1.0 Uiso 0.0053(4) 18 C C3 0.5437(9) 0.0568(9) -0.014(4) 1.0 Uiso 0.0053(4) 18 C C2 0.5180(10) -0.0387(9) 0.084(4) 1.0 Uiso 0.0053(4) 18 O O5 0.1950(6) 0.0835(6) 0.1743(27) 0.9 Uiso 0.0053(4) 18 O O6 0.0375(6) 0.0745(6) 0.1830(26) 0.9 Uiso 0.0053(4) 18 O O7 0.1422(7) 0.1488(6) 0.4453(25) 0.9 Uiso 0.0053(4) 18 C C1 0.5468(11) -0.0115(8) -0.2700(32) 1.0 Uiso 0.0053(4) 18 # If you change Z, be sure to change all 3 of the following _chemical_formula_sum 'C3 N Ni O6.70 P' _chemical_formula_weight 246.90 _cell_formula_units_Z 18 # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 2.026(17) . 1_556 N Ni1 O2 2.008(15) . 103_655 N Ni1 O3 2.098(17) . 1_555 N Ni1 O3 2.061(15) . 202_545 N Ni1 O4 2.114(16) . 1_555 N Ni1 N1 2.093(20) . 1_555 N P1 O1 1.568(13) . 1_555 N P1 O2 1.701(16) . 1_555 N P1 O3 1.573(14) . 1_555 N P1 C1 1.952(25) . 1_555 N N1 C3 1.628(22) . 1_555 N N1 C2 1.373(25) . 1_555 N N1 C1 1.559(22) . 1_555 N C2 C3 1.596(26) . -1_655 N 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ni1 O2 92.5(7) 1_556 . 103_655 N O2 Ni1 O3 168.0(7) 1_556 . 1_555 N O2 Ni1 O3 75.9(7) 1_556 . 202_545 N O2 Ni1 O4 89.7(6) 1_556 . 1_555 N O2 Ni1 N1 101.7(7) 1_556 . 1_555 N O2 Ni1 O3 75.5(6) 103_655 . 1_555 N O2 Ni1 O3 77.9(6) 103_655 . 202_545 N O2 Ni1 O4 102.3(7) 103_655 . 1_555 N O2 Ni1 N1 160.5(8) 103_655 . 1_555 N O3 Ni1 O3 100.5(7) 1_555 . 202_545 N O3 Ni1 O4 93.4(6) 1_555 . 1_555 N O3 Ni1 N1 89.8(6) 1_555 . 1_555 N O3 Ni1 O4 165.6(7) 202_545 . 1_555 N O3 Ni1 N1 92.5(7) 202_545 . 1_555 N O4 Ni1 N1 91.2(6) 1_555 . 1_555 N O1 P1 O2 116.2(9) 1_555 . 1_555 N O1 P1 O3 114.0(10) 1_555 . 1_555 N O1 P1 C1 111.3(10) 1_555 . 1_555 N O2 P1 O3 96.0(8) 1_555 . 1_555 N O2 P1 C1 114.7(10) 1_555 . 1_555 N O3 P1 C1 102.9(11) 1_555 . 1_555 N Ni1 O2 Ni1 103.7(8) 1_554 . 202_544 N Ni1 O2 P1 128.8(9) 1_554 . 1_555 N Ni1 O2 P1 127.0(10) 202_544 . 1_555 N Ni1 O3 Ni1 99.4(8) 1_555 . 103_654 N Ni1 O3 P1 115.0(9) 1_555 . 1_555 N Ni1 O3 P1 135.6(9) 103_654 . 1_555 N Ni1 N1 C3 114.1(15) 1_555 . 1_555 N Ni1 N1 C2 112.8(17) 1_555 . 1_555 N Ni1 N1 C1 108.6(16) 1_555 . 1_555 N C3 N1 C2 110.4(19) 1_555 . 1_555 N C3 N1 C1 104.5(18) 1_555 . 1_555 N C2 N1 C1 105.7(21) 1_555 . 1_555 N N1 C3 C2 112.6(16) 1_555 . -1_655 N N1 C2 C3 112.4(22) 1_555 . -1_655 N P1 C1 N1 107.4(16) 1_555 . 1_555 N # Powder diffraction data for histogram 3 #============================================================================== # 9. INSTRUMENT CHARACTERIZATION _exptl_special_details ; ? ; # if regions of the data are excluded, the reason(s) are supplied here: _pd_proc_info_excluded_regions ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; ? ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 293 _diffrn_source ? _diffrn_source_target ? _diffrn_source_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method ? # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following two items identify the program(s) used (if appropriate). _computing_data_collection ? _computing_data_reduction ? # Describe any processing performed on the data, prior to refinement. # For example: a manual Lp correction or a precomputed absorption correction _pd_proc_info_data_reduction ? # The following item is used for angular dispersive measurements only. _diffrn_radiation_monochromator ? # The following items are used to define the size of the instrument. # Not all distances are appropriate for all instrument types. _pd_instr_dist_src/mono ? _pd_instr_dist_mono/spec ? _pd_instr_dist_src/spec ? _pd_instr_dist_spec/anal ? _pd_instr_dist_anal/detc ? _pd_instr_dist_spec/detc ? # 10. Specimen size and mounting information # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode ? # options are 'reflection' # or 'transmission' _pd_spec_shape ? # options are 'cylinder' # 'flat_sheet' or 'irregular' loop_ _atom_type_symbol _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source NI 18.0 -2.956 0.509 12.8376 3.87850 7.29200 0.25650 4.44380 12.1763 2.38000 66.3421 1.03410 International_Tables_Vol_C P 18.0 0.283 0.434 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080 68.1645 1.11490 International_Tables_Vol_C O 120.6 0.047 0.032 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700 32.9089 0.25080 International_Tables_Vol_C N 18.0 0.029 0.018 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630 0.58260 -11.529 International_Tables_Vol_C C 54.0 0.017 0.009 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500 51.6512 0.21560 International_Tables_Vol_C _diffrn_radiation_probe x-ray _diffrn_radiation_polarisn_ratio 0.55 _diffrn_radiation_wavelength 1.54056 _diffrn_radiation_type 'Cu K alpha' _pd_proc_ls_prof_R_factor 0.0462 _pd_proc_ls_prof_wR_factor 0.0611 _pd_proc_ls_prof_wR_expected 0.0236 _refine_ls_R_Fsqd_factor 0.11501 _pd_proc_ls_background_function ; GSAS Background function number 2 with 28 terms. Cosine Fourier series 1: 743370. 2: -1.170840E+06 3: 424121. 4: 290869. 5: -567785. 6: 412985. 7: -201653. 8: 205690. 9: -260927. 10: 43584.3 11: 409876. 12: -693958. 13: 546492. 14: -170170. 15: -53434.2 16: 12816.0 17: 102760. 18: -117772. 19: 56594.6 20: -22906.4 21: 38371.9 22: -50420.2 23: 30363.6 24: -812.482 25: -11969.1 26: 8464.28 27: -2418.32 28: 55.4500 ; _exptl_absorpt_process_details ; GSAS Absorption/surface roughness correction: function number 0 Debye-Scherrer absorption correction Term (= MU.r/wave) = 0.73000 Correction is not refined. ; _exptl_absorpt_correction_T_min 0.16219 _exptl_absorpt_correction_T_max 0.20608 # Extinction correction _gsas_exptl_extinct_corr_T_min 1.00000 _gsas_exptl_extinct_corr_T_max 1.00000 _pd_proc_ls_profile_function ; CW Profile function number 3 with 19 terms Pseudovoigt profile coefficients as parameterized in P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83. Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994). J. Appl. Cryst.,27,892-900. #1(GU) = 104.716 #2(GV) = -27.591 #3(GW) = 15.804 #4(GP) = 5.489 #5(LX) = 3.855 #6(LY) = 15.598 #7(S/L) = 0.0253 #8(H/L) = 0.0194 #9(trns) = 4.04 #10(shft)= -1.6170 #11(stec)= -12.91 #12(ptec)= 2.94 #13(sfec)= 0.00 #14(L11) = -0.005 #15(L22) = -0.069 #16(L33) = -0.197 #17(L12) = -0.010 #18(L13) = -0.008 #19(L23) = 0.005 Peak tails are ignored where the intensity is below 0.0100 times the peak Aniso. broadening axis 0.0 0.0 1.0 ; _pd_proc_ls_peak_cutoff 0.01000 _pd_proc_info_datetime 2006-06-08T14:27:35 _pd_calc_method 'Rietveld Refinement'