# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2009 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Filipe Paz' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Duarte Ananias' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Luis Carlos' . ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW United Kingdom ; 'Luis Cunha-Silva' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Sergio Lima' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Luis Mafra' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; ; M.Pillinger ; . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Joao Rocha' . ; Department of Physics University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Patricia Silva' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Anabela A Valente' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; _publ_contact_author_name 'Filipe Paz' _publ_contact_author_email FILIPE.PAZ@UA.PT _publ_section_title ; Multi-Functional Rare-Earth Hybrid Layered Networks: Photoluminescence and Catalysis Studies ; _publ_contact_author_address ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; _publ_contact_author_fax '+351 234 370084' _publ_contact_author_phone '+351 234 370200' data_01 _database_code_depnum_ccdc_archive 'CCDC 705159' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '01 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 N O9 P2 Y' _chemical_formula_sum 'C4 H10 N O9 P2 Y' _chemical_formula_weight 366.98 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Y 17.77600 1.40290 10.29460 12.80060 5.72629 0.12560 3.26588 104.35400 1.91213 -0.38600 2.02500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.28300 0.43400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.7510(8) _cell_length_b 10.1889(8) _cell_length_c 20.6391(8) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2050.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298 _exptl_crystal_density_diffrn 2.377 _cell_special_details ; ? ; _pd_spec_mounting ; Glass slide ; _pd_spec_mount_mode Reflection _pd_spec_shape 'Flat sheet' #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; Conventional powder diffractometer instrument belonging to the University of Aveiro and located at the Central Analytical Laboratory ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source 'X-ray tube' _diffrn_radiation_type X-ray _diffrn_source_target Cu _diffrn_radiation_monochromator None _diffrn_measurement_method Bragg-Brentano _diffrn_detector_type 'X Celerator detector' _pd_meas_scan_method cont _pd_meas_special_details ; Data were collected in a continuous mode over the angular range 4-110. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 10971 _pd_meas_2theta_range_min 5.00000 _pd_meas_2theta_range_max 114.99619 _pd_meas_2theta_range_inc 0.010027 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function 'Fixed Points' _pd_proc_ls_pref_orient_corr ; Modified March's function along the [002] vector. G1 refined to about 0.468(1) which is consistent with the platy crystal habit of the material (as revealed by SEM pictures). ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 4.7131 _pd_proc_ls_prof_wR_factor 5.9986 _pd_proc_ls_prof_wR_expected 0.9338 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 17.0554 _pd_proc_ls_prof_cwR_factor 13.9626 _pd_proc_ls_prof_cwR_expected 2.1735 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 41.2686 _pd_proc_ls_prof_echi2 41.6809 # Items related to LS refinement _refine_ls_R_I_factor 9.2249 _refine_ls_number_reflns 3010 _refine_ls_number_parameters 64 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.9303 _pd_proc_2theta_range_max 114.9265 _pd_proc_2theta_range_inc 0.010027 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol Y1 0.3646(5) 0.5436(5) 0.33570(8) 0.01267 1.00000 Uiso Y P1 1.0814(7) 0.7269(7) 0.4154(3) 0.01267 1.00000 Uiso P P2 1.0272(7) 0.3928(7) 0.3045(3) 0.01267 1.00000 Uiso P O2 0.52321(12) 0.5933(12) 0.4329(5) 0.01267 1.00000 Uiso O C1 0.63002(9) 0.5459(3) 0.41020(8) 0.01267 1.00000 Uiso C O4 1.1466(16) 0.8630(7) 0.4083(4) 0.01267 1.00000 Uiso O O6 0.9314(10) 0.4511(12) 0.2559(5) 0.01267 1.00000 Uiso O O8 1.1682(9) 0.4504(13) 0.3053(5) 0.01267 1.00000 Uiso O O1 0.6166(5) 0.5126(19) 0.3527(2) 0.01267 1.00000 Uiso O O7 1.0233(13) 0.2463(6) 0.3045(5) 0.01267 1.00000 Uiso O O5 1.1961(13) 0.6275(10) 0.4087(4) 0.01267 1.00000 Uiso O O1W 0.255(2) 0.687(3) 0.2531(4) 0.01267 1.00000 Uiso O O3 1.0276(15) 0.7211(12) 0.4882(4) 0.01267 1.00000 Uiso O H3 1.03656 0.79455 0.50537 0.01267 1.00000 Uiso H C2 0.76823(9) 0.5886(7) 0.43559(19) 0.01267 1.00000 Uiso C H2A 0.77330 0.67916 0.45064 0.01267 1.00000 Uiso H H2B 0.80339 0.53413 0.47126 0.01267 1.00000 Uiso H C3 0.9736(19) 0.4585(17) 0.3832(5) 0.01267 1.00000 Uiso C H3A 0.93612 0.39309 0.40902 0.01267 1.00000 Uiso H H3B 1.05082 0.49801 0.40383 0.01267 1.00000 Uiso H N1 0.8611(10) 0.5648(8) 0.3745(5) 0.01267 1.00000 Uiso N H1 0.80882 0.55359 0.33998 0.01267 1.00000 Uiso H C4 0.9384(14) 0.6963(12) 0.3621(5) 0.01267 1.00000 Uiso C H4A 0.87339 0.77394 0.37554 0.01267 1.00000 Uiso H H4B 0.96392 0.71382 0.32147 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Y1 O6 2.213(5) 8_556 ? Y1 O8 2.228(5) 1_455 ? Y1 O4 2.376(6) 6_755 ? Y1 O5 2.390(5) 1_455 ? Y1 O7 2.426(6) 6_765 ? Y1 O1W 2.486(5) . ? Y1 O1 2.502(6) . ? Y1 O2 2.588(5) . ? Y1 C1 3.013(9) . ? P1 O5 1.516(5) . ? P1 O4 1.532(6) . ? P1 O3 1.594(6) . ? P1 C4 1.799(7) . ? P2 O7 1.491(6) . ? P2 O6 1.491(5) . ? P2 O8 1.494(5) . ? P2 C3 1.832(8) . ? O2 C1 1.243(9) . ? C1 O1 1.239(9) . ? C1 C2 1.509(12) . ? O4 Y1 2.376(6) 6_765 ? O6 Y1 2.213(5) 8_656 ? O8 Y1 2.228(5) 1_655 ? O7 Y1 2.426(6) 6_755 ? O5 Y1 2.390(5) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.563(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.556(12) . ? C3 H3A 0.9300 . ? C3 H3B 0.9700 . ? N1 C4 1.562(11) . ? N1 H1 0.9100 . ? C4 H4A 1.9700 . ? C4 H4B 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 O6 Y1 O8 80.31(19) 8_556 1_455 ? O6 Y1 O4 102.9(2) 8_556 6_755 ? O8 Y1 O4 78.9(2) 1_455 6_755 ? O6 Y1 O5 153.57(16) 8_556 1_455 ? O8 Y1 O5 74.8(2) 1_455 1_455 ? O4 Y1 O5 81.14(19) 6_755 1_455 ? O6 Y1 O7 90.3(2) 8_556 6_765 ? O8 Y1 O7 132.6(2) 1_455 6_765 ? O4 Y1 O7 148.00(19) 6_755 6_765 ? O5 Y1 O7 99.93(16) 1_455 6_765 ? O6 Y1 O1W 78.0(2) 8_556 . ? O8 Y1 O1W 71.9(2) 1_455 . ? O4 Y1 O1W 150.3(2) 6_755 . ? O5 Y1 O1W 85.82(18) 1_455 . ? O7 Y1 O1W 60.6(2) 6_765 . ? O6 Y1 O1 77.18(17) 8_556 . ? O8 Y1 O1 146.2(2) 1_455 . ? O4 Y1 O1 81.9(2) 6_755 . ? O5 Y1 O1 129.11(16) 1_455 . ? O7 Y1 O1 72.62(15) 6_765 . ? O1W Y1 O1 126.25(17) . . ? O6 Y1 O2 124.88(19) 8_556 . ? O8 Y1 O2 144.7(2) 1_455 . ? O4 Y1 O2 71.9(2) 6_755 . ? O5 Y1 O2 81.39(18) 1_455 . ? O7 Y1 O2 76.60(19) 6_765 . ? O1W Y1 O2 132.26(19) . . ? O1 Y1 O2 47.73(16) . . ? O6 Y1 C1 100.76(19) 8_556 . ? O8 Y1 C1 152.5(2) 1_455 . ? O4 Y1 C1 74.0(2) 6_755 . ? O5 Y1 C1 105.41(18) 1_455 . ? O7 Y1 C1 74.9(2) 6_765 . ? O1W Y1 C1 135.5(2) . . ? O1 Y1 C1 23.7(2) . . ? O2 Y1 C1 24.13(18) . . ? O5 P1 O4 106.8(3) . . ? O5 P1 O3 107.4(3) . . ? O4 P1 O3 105.5(4) . . ? O5 P1 C4 113.8(4) . . ? O4 P1 C4 114.8(4) . . ? O3 P1 C4 108.0(3) . . ? O7 P2 O6 112.4(4) . . ? O7 P2 O8 114.7(3) . . ? O6 P2 O8 115.3(4) . . ? O7 P2 C3 110.8(5) . . ? O6 P2 C3 105.7(4) . . ? O8 P2 C3 96.2(4) . . ? C1 O2 Y1 97.5(5) . . ? O2 C1 O1 112.3(7) . . ? O2 C1 C2 120.4(8) . . ? O1 C1 C2 120.4(8) . . ? O2 C1 Y1 58.4(4) . . ? O1 C1 Y1 54.3(4) . . ? C2 C1 Y1 161.1(6) . . ? P1 O4 Y1 137.8(3) . 6_765 ? P2 O6 Y1 158.0(3) . 8_656 ? P2 O8 Y1 164.1(3) . 1_655 ? C1 O1 Y1 102.0(5) . . ? P2 O7 Y1 147.2(3) . 6_755 ? P1 O5 Y1 143.3(3) . 1_655 ? P1 O3 H3 109.1 . . ? C1 C2 N1 101.0(7) . . ? C1 C2 H2A 111.4 . . ? N1 C2 H2A 111.6 . . ? C1 C2 H2B 111.7 . . ? N1 C2 H2B 111.7 . . ? H2A C2 H2B 109.4 . . ? N1 C3 P2 110.9(5) . . ? N1 C3 H3A 109.5 . . ? P2 C3 H3A 109.5 . . ? N1 C3 H3B 109.4 . . ? P2 C3 H3B 109.4 . . ? H3A C3 H3B 108.1 . . ? C3 N1 C4 105.9(7) . . ? C3 N1 C2 115.1(5) . . ? C4 N1 C2 106.0(6) . . ? C3 N1 H1 109.7 . . ? C4 N1 H1 110.0 . . ? C2 N1 H1 109.9 . . ? N1 C4 P1 115.1(5) . . ? N1 C4 H4A 108.4 . . ? P1 C4 H4A 108.6 . . ? N1 C4 H4B 108.4 . . ? P1 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Y1 O2 C1 -2.2(6) 8_556 . . . ? O8 Y1 O2 C1 126.9(5) 1_455 . . . ? O4 Y1 O2 C1 91.2(5) 6_755 . . . ? O5 Y1 O2 C1 174.6(5) 1_455 . . . ? O7 Y1 O2 C1 -83.0(5) 6_765 . . . ? O1W Y1 O2 C1 -109.1(5) . . . . ? O1 Y1 O2 C1 -4.4(5) . . . . ? Y1 O2 C1 O1 7.1(8) . . . . ? Y1 O2 C1 C2 157.9(7) . . . . ? O6 Y1 C1 O2 178.2(5) 8_556 . . . ? O8 Y1 C1 O2 -92.2(7) 1_455 . . . ? O4 Y1 C1 O2 -81.3(5) 6_755 . . . ? O5 Y1 C1 O2 -5.5(5) 1_455 . . . ? O7 Y1 C1 O2 90.8(5) 6_765 . . . ? O1W Y1 C1 O2 94.4(5) . . . . ? O1 Y1 C1 O2 171.9(9) . . . . ? O6 Y1 C1 O1 6.3(6) 8_556 . . . ? O8 Y1 C1 O1 95.9(6) 1_455 . . . ? O4 Y1 C1 O1 106.8(5) 6_755 . . . ? O5 Y1 C1 O1 -177.4(5) 1_455 . . . ? O7 Y1 C1 O1 -81.0(5) 6_765 . . . ? O1W Y1 C1 O1 -77.5(6) . . . . ? O2 Y1 C1 O1 -171.9(9) . . . . ? O6 Y1 C1 C2 86(2) 8_556 . . . ? O8 Y1 C1 C2 175.9(17) 1_455 . . . ? O4 Y1 C1 C2 -173.3(19) 6_755 . . . ? O5 Y1 C1 C2 -97.4(19) 1_455 . . . ? O7 Y1 C1 C2 -1.1(19) 6_765 . . . ? O1W Y1 C1 C2 2(2) . . . . ? O1 Y1 C1 C2 80.0(19) . . . . ? O2 Y1 C1 C2 -92(2) . . . . ? O5 P1 O4 Y1 116.1(5) . . . 6_765 ? O3 P1 O4 Y1 -129.8(5) . . . 6_765 ? C4 P1 O4 Y1 -11.1(7) . . . 6_765 ? O7 P2 O6 Y1 -101.0(12) . . . 8_656 ? O8 P2 O6 Y1 33.1(13) . . . 8_656 ? C3 P2 O6 Y1 138.0(12) . . . 8_656 ? O7 P2 O8 Y1 -100.5(14) . . . 1_655 ? O6 P2 O8 Y1 126.4(13) . . . 1_655 ? C3 P2 O8 Y1 15.8(15) . . . 1_655 ? O2 C1 O1 Y1 -7.5(8) . . . . ? C2 C1 O1 Y1 -158.3(7) . . . . ? O6 Y1 O1 C1 -173.7(6) 8_556 . . . ? O8 Y1 O1 C1 -124.3(5) 1_455 . . . ? O4 Y1 O1 C1 -68.4(5) 6_755 . . . ? O5 Y1 O1 C1 3.2(6) 1_455 . . . ? O7 Y1 O1 C1 92.0(5) 6_765 . . . ? O1W Y1 O1 C1 121.9(5) . . . . ? O2 Y1 O1 C1 4.5(5) . . . . ? O6 P2 O7 Y1 162.6(5) . . . 6_755 ? O8 P2 O7 Y1 28.2(8) . . . 6_755 ? C3 P2 O7 Y1 -79.4(7) . . . 6_755 ? O4 P1 O5 Y1 -63.4(6) . . . 1_655 ? O3 P1 O5 Y1 -176.2(4) . . . 1_655 ? C4 P1 O5 Y1 64.3(6) . . . 1_655 ? O2 C1 C2 N1 -152.7(7) . . . . ? O1 C1 C2 N1 -4.2(10) . . . . ? Y1 C1 C2 N1 -72(2) . . . . ? O7 P2 C3 N1 -129.3(7) . . . . ? O6 P2 C3 N1 -7.2(8) . . . . ? O8 P2 C3 N1 111.3(7) . . . . ? P2 C3 N1 C4 -85.7(8) . . . . ? P2 C3 N1 C2 157.6(6) . . . . ? C1 C2 N1 C3 -115.8(8) . . . . ? C1 C2 N1 C4 127.5(7) . . . . ? C3 N1 C4 P1 -45.2(7) . . . . ? C2 N1 C4 P1 77.6(7) . . . . ? O5 P1 C4 N1 63.2(7) . . . . ? O4 P1 C4 N1 -173.3(5) . . . . ? O3 P1 C4 N1 -55.9(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.73 2.500(9) 155.5 2_566 data_02 _database_code_depnum_ccdc_archive 'CCDC 705160' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '11 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 La N O9 P2' _chemical_formula_sum 'C4 H10 La N O9 P2' _chemical_formula_weight 416.98 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source LA 20.57800 2.94817 19.59900 0.24448 11.37270 18.77260 3.28719 133.12399 2.14678 -0.58800 2.45200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.09000 0.09500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.00800 0.00600 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.00200 0.00200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.00400 0.00300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.8645(16) _cell_length_b 10.3423(16) _cell_length_c 20.454(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2086.7(6) _exptl_crystal_density_diffrn 2.655 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Hilgenberg borosilicate glass capillary (ca. 0.4 mm of diameter) ; #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; MAR 345 Imaging Plate instrument belonging to the Swiss-Norwegian BM01a beam line (bending magnet source) at the European Synchrotron Radiation Facility (ESRF), Grenoble, France. ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source Synchrotron _diffrn_radiation_type X-ray _diffrn_radiation_monochromator 0.71013(1) _diffrn_measurement_method Debye-Scherrer _diffrn_detector 'Imaging Plate' _diffrn_detector_type 'MAR 345' _pd_meas_scan_method cont _pd_meas_special_details ; The powdered sample was slowly spun 180 degrees (in phi scanning mode) during data collection to improve powder averaging. Two-dimensional powder data was collected using a MAR2300 imaging plate detector and then integrated using the software Fit2D. The monochromatic wavelength (0.71013 A) and sample-to-detector distance (d of about 150 mm) were calibrated from an individual run using the standard LaB6. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 1312 _pd_meas_2theta_range_min 2.02483 _pd_meas_2theta_range_max 49.00845 _pd_meas_2theta_range_inc 0.035838 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Gaussian _pd_proc_ls_background_function 'Fixed points' _pd_proc_ls_pref_orient_corr ; None ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 5.3683 _pd_proc_ls_prof_wR_factor 7.2414 _pd_proc_ls_prof_wR_expected 1.5482 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 11.8676 _pd_proc_ls_prof_cwR_factor 13.6476 _pd_proc_ls_prof_cwR_expected 2.9178 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 21.8781 _pd_proc_ls_prof_echi2 21.8781 # Items related to LS refinement _refine_ls_R_I_factor 9.1349 _refine_ls_number_reflns 2195 _refine_ls_number_parameters 62 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0386 _pd_proc_2theta_range_max 49.0222 _pd_proc_2theta_range_inc 0.035838 _pd_proc_wavelength 0.710130 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol LA1 0.3601(4) 0.5419(4) 0.33860(18) 0.01267 1.00000 Uiso LA P1 1.0891(8) 0.7172(7) 0.4177(4) 0.01267 1.00000 Uiso P P2 1.0122(8) 0.3752(7) 0.3121(4) 0.01267 1.00000 Uiso P O2 0.5268(3) 0.586(3) 0.4376(7) 0.01267 1.00000 Uiso O C1 0.63097(11) 0.5627(6) 0.4056(2) 0.01267 1.00000 Uiso C O4 1.1530(19) 0.8496(8) 0.4056(10) 0.01267 1.00000 Uiso O O6 0.9232(14) 0.4476(12) 0.2623(11) 0.01267 1.00000 Uiso O O8 1.1578(9) 0.4216(13) 0.3043(10) 0.01267 1.00000 Uiso O O1 0.6220(3) 0.485(2) 0.3597(9) 0.01267 1.00000 Uiso O O7 1.0038(16) 0.2313(6) 0.2970(12) 0.01267 1.00000 Uiso O O5 1.1992(16) 0.6155(11) 0.4236(10) 0.01267 1.00000 Uiso O O1W 0.238(4) 0.684(3) 0.2471(15) 0.01267 1.00000 Uiso O O3 1.010(2) 0.7221(13) 0.4824(9) 0.01267 1.00000 Uiso O H3 1.02765 0.79137 0.50280 0.01267 1.00000 Uiso H C2 0.76819(13) 0.6016(12) 0.4319(4) 0.01267 1.00000 Uiso C H2A 0.76825 0.68791 0.44284 0.01267 1.00000 Uiso H H2B 0.78064 0.54649 0.46918 0.01267 1.00000 Uiso H C3 0.943(3) 0.4390(15) 0.3885(6) 0.01267 1.00000 Uiso C H3A 0.88056 0.37593 0.40741 0.01267 1.00000 Uiso H H3B 1.01292 0.45398 0.41953 0.01267 1.00000 Uiso H N1 0.8651(12) 0.5663(8) 0.3755(7) 0.01267 1.00000 Uiso N H1 0.81283 0.55149 0.34004 0.01267 1.00000 Uiso H C4 0.9604(17) 0.6778(17) 0.3572(7) 0.01267 1.00000 Uiso C H4A 0.90262 0.75418 0.35188 0.01267 1.00000 Uiso H H4B 1.00073 0.65924 0.31758 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 La1 O6 2.3654(16) 8_556 ? La1 O4 2.4184(18) 6_755 ? La1 O8 2.4531(17) 1_455 ? La1 O5 2.4759(15) 1_455 ? La1 O7 2.522(2) 6_765 ? La1 O2 2.6468(18) . ? La1 O1W 2.6689(19) . ? La1 O1 2.685(2) . ? La1 C1 3.011(3) . ? P1 O5 1.5156(17) . ? P1 O4 1.5266(18) . ? P1 O3 1.5373(18) . ? P1 C4 1.820(3) . ? P2 O7 1.5213(19) . ? P2 O8 1.5243(18) . ? P2 O6 1.5390(17) . ? P2 C3 1.827(3) . ? O2 C1 1.240(3) . ? C1 O1 1.241(3) . ? C1 C2 1.505(3) . ? O4 La1 2.4184(18) 6_765 ? O6 La1 2.3654(16) 8_656 ? O8 La1 2.4531(17) 1_655 ? O7 La1 2.522(2) 6_755 ? O5 La1 2.4759(15) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.548(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.548(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.535(3) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O6 La1 O4 99.73(6) 8_556 6_755 ? O6 La1 O8 75.88(5) 8_556 1_455 ? O4 La1 O8 72.65(6) 6_755 1_455 ? O6 La1 O5 155.33(6) 8_556 1_455 ? O4 La1 O5 79.69(6) 6_755 1_455 ? O8 La1 O5 80.51(6) 1_455 1_455 ? O6 La1 O7 83.47(7) 8_556 6_765 ? O4 La1 O7 149.13(7) 6_755 6_765 ? O8 La1 O7 136.87(6) 1_455 6_765 ? O5 La1 O7 109.80(7) 1_455 6_765 ? O6 La1 O2 125.02(6) 8_556 . ? O4 La1 O2 74.93(5) 6_755 . ? O8 La1 O2 144.11(5) 1_455 . ? O5 La1 O2 78.95(5) 1_455 . ? O7 La1 O2 78.19(6) 6_765 . ? O6 La1 O1W 74.58(6) 8_556 . ? O4 La1 O1W 145.65(6) 6_755 . ? O8 La1 O1W 73.13(6) 1_455 . ? O5 La1 O1W 91.90(6) 1_455 . ? O7 La1 O1W 64.96(6) 6_765 . ? O2 La1 O1W 136.41(6) . . ? O6 La1 O1 78.27(6) 8_556 . ? O4 La1 O1 77.26(6) 6_755 . ? O8 La1 O1 135.84(5) 1_455 . ? O5 La1 O1 124.86(5) 1_455 . ? O7 La1 O1 73.34(5) 6_765 . ? O2 La1 O1 46.89(5) . . ? O1W La1 O1 132.04(5) . . ? O6 La1 C1 101.15(6) 8_556 . ? O4 La1 C1 81.30(7) 6_755 . ? O8 La1 C1 152.68(6) 1_455 . ? O5 La1 C1 103.11(6) 1_455 . ? O7 La1 C1 68.03(6) 6_765 . ? O2 La1 C1 24.23(6) . . ? O1W La1 C1 132.98(6) . . ? O1 La1 C1 24.32(6) . . ? O5 P1 O4 109.86(10) . . ? O5 P1 O3 108.44(9) . . ? O4 P1 O3 108.69(10) . . ? O5 P1 C4 113.47(12) . . ? O4 P1 C4 112.23(13) . . ? O3 P1 C4 103.83(12) . . ? O7 P2 O8 109.74(11) . . ? O7 P2 O6 108.14(11) . . ? O8 P2 O6 108.30(11) . . ? O7 P2 C3 120.35(13) . . ? O8 P2 C3 109.16(11) . . ? O6 P2 C3 100.27(11) . . ? C1 O2 La1 94.59(15) . . ? O1 C1 O2 117.5(2) . . ? O1 C1 C2 120.4(2) . . ? O2 C1 C2 120.3(2) . . ? O1 C1 La1 62.95(15) . . ? O2 C1 La1 61.18(14) . . ? C2 C1 La1 167.51(17) . . ? P1 O4 La1 143.82(12) . 6_765 ? P2 O6 La1 158.20(10) . 8_656 ? P2 O8 La1 153.76(10) . 1_655 ? C1 O1 La1 92.73(16) . . ? P2 O7 La1 131.54(12) . 6_755 ? P1 O5 La1 128.04(9) . 1_655 ? P1 O3 H3 109.4 . . ? C1 C2 N1 103.20(18) . . ? C1 C2 H2A 111.2 . . ? N1 C2 H2A 111.0 . . ? C1 C2 H2B 111.1 . . ? N1 C2 H2B 111.1 . . ? H2A C2 H2B 109.1 . . ? N1 C3 P2 110.16(19) . . ? N1 C3 H3A 109.5 . . ? P2 C3 H3A 109.6 . . ? N1 C3 H3B 109.7 . . ? P2 C3 H3B 109.7 . . ? H3A C3 H3B 108.1 . . ? C4 N1 C2 112.7(2) . . ? C4 N1 C3 112.25(17) . . ? C2 N1 C3 112.4(2) . . ? C4 N1 H1 106.4 . . ? C2 N1 H1 106.2 . . ? C3 N1 H1 106.4 . . ? N1 C4 P1 115.47(18) . . ? N1 C4 H4A 108.4 . . ? P1 C4 H4A 108.4 . . ? N1 C4 H4B 108.4 . . ? P1 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 La1 O2 C1 11.06(15) 8_556 . . . ? O4 La1 O2 C1 102.50(15) 6_755 . . . ? O8 La1 O2 C1 128.46(14) 1_455 . . . ? O5 La1 O2 C1 -175.33(14) 1_455 . . . ? O7 La1 O2 C1 -62.17(13) 6_765 . . . ? O1W La1 O2 C1 -94.32(14) . . . . ? O1 La1 O2 C1 15.98(12) . . . . ? La1 O2 C1 O1 -29.3(2) . . . . ? La1 O2 C1 C2 165.7(2) . . . . ? O6 La1 C1 O1 -19.99(14) 8_556 . . . ? O4 La1 C1 O1 78.29(12) 6_755 . . . ? O8 La1 C1 O1 60.8(2) 1_455 . . . ? O5 La1 C1 O1 155.49(13) 1_455 . . . ? O7 La1 C1 O1 -98.18(14) 6_765 . . . ? O2 La1 C1 O1 150.8(2) . . . . ? O1W La1 C1 O1 -99.23(15) . . . . ? O6 La1 C1 O2 -170.78(13) 8_556 . . . ? O4 La1 C1 O2 -72.50(13) 6_755 . . . ? O8 La1 C1 O2 -90.0(2) 1_455 . . . ? O5 La1 C1 O2 4.70(14) 1_455 . . . ? O7 La1 C1 O2 111.02(15) 6_765 . . . ? O1W La1 C1 O2 109.98(12) . . . . ? O1 La1 C1 O2 -150.8(2) . . . . ? O6 La1 C1 C2 88.8(7) 8_556 . . . ? O4 La1 C1 C2 -172.9(7) 6_755 . . . ? O8 La1 C1 C2 169.6(6) 1_455 . . . ? O5 La1 C1 C2 -95.7(7) 1_455 . . . ? O7 La1 C1 C2 10.6(7) 6_765 . . . ? O2 La1 C1 C2 -100.4(8) . . . . ? O1W La1 C1 C2 9.5(8) . . . . ? O1 La1 C1 C2 108.8(7) . . . . ? O5 P1 O4 La1 133.22(16) . . . 6_765 ? O3 P1 O4 La1 -108.27(19) . . . 6_765 ? C4 P1 O4 La1 6.0(2) . . . 6_765 ? O7 P2 O6 La1 -77.5(3) . . . 8_656 ? O8 P2 O6 La1 41.4(3) . . . 8_656 ? C3 P2 O6 La1 155.7(3) . . . 8_656 ? O7 P2 O8 La1 -134.9(2) . . . 1_655 ? O6 P2 O8 La1 107.2(2) . . . 1_655 ? C3 P2 O8 La1 -1.1(2) . . . 1_655 ? O2 C1 O1 La1 28.8(2) . . . . ? C2 C1 O1 La1 -166.26(19) . . . . ? O6 La1 O1 C1 159.97(14) 8_556 . . . ? O4 La1 O1 C1 -97.10(13) 6_755 . . . ? O8 La1 O1 C1 -144.89(13) 1_455 . . . ? O5 La1 O1 C1 -29.49(16) 1_455 . . . ? O7 La1 O1 C1 73.36(13) 6_765 . . . ? O2 La1 O1 C1 -15.93(11) . . . . ? O1W La1 O1 C1 103.53(14) . . . . ? O8 P2 O7 La1 50.83(17) . . . 6_755 ? O6 P2 O7 La1 168.78(11) . . . 6_755 ? C3 P2 O7 La1 -77.1(2) . . . 6_755 ? O4 P1 O5 La1 -65.08(16) . . . 1_655 ? O3 P1 O5 La1 176.26(13) . . . 1_655 ? C4 P1 O5 La1 61.45(15) . . . 1_655 ? O1 C1 C2 N1 19.9(3) . . . . ? O2 C1 C2 N1 -175.6(2) . . . . ? La1 C1 C2 N1 -82.2(8) . . . . ? O7 P2 C3 N1 -137.47(17) . . . . ? O8 P2 C3 N1 94.37(18) . . . . ? O6 P2 C3 N1 -19.26(18) . . . . ? C1 C2 N1 C4 129.7(2) . . . . ? C1 C2 N1 C3 -102.3(2) . . . . ? P2 C3 N1 C4 -70.0(2) . . . . ? P2 C3 N1 C2 161.75(18) . . . . ? C2 N1 C4 P1 69.4(3) . . . . ? C3 N1 C4 P1 -58.7(3) . . . . ? O5 P1 C4 N1 70.7(2) . . . . ? O4 P1 C4 N1 -164.06(16) . . . . ? O3 P1 C4 N1 -46.86(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.79 2.582(3) 160.9 2_566 data_02s _database_code_depnum_ccdc_archive 'CCDC 705161' # ======================================================================= _audit_creation_method 'SHELXL-97 plus manual editing' _audit_creation_date '11 October 2008' # ======================================================================= _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 La N O9 P2' _chemical_formula_sum 'C4 H10 La N O9 P2' _chemical_formula_weight 416.98 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 9.9654(8) _cell_length_b 10.4467(9) _cell_length_c 20.708(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2155.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 4.299 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min 0.9190 _exptl_absorpt_correction_T_max 0.9190 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71013 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Snchrotron, BM01a at ESRF' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8759 _diffrn_reflns_av_R_equivalents 0.2071 _diffrn_reflns_av_sigmaI/netI 0.1108 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 26.35 _reflns_number_total 2113 _reflns_number_gt 1797 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrysAllisCCD _computing_cell_refinement CrysAllisRED _computing_data_reduction CrysAllisRED _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2006)' _computing_publication_material 'SHELXTL v.6.14 (Sheldrick, 2002)' _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^)+(0.1470P)^2^+954.0359P] 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 2113 _refine_ls_number_parameters 85 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2022 _refine_ls_R_factor_gt 0.1909 _refine_ls_wR_factor_ref 0.4537 _refine_ls_wR_factor_gt 0.4470 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 La1 La 0.35885(18) 0.54169(19) 0.33890(10) 0.0111(7) Uani 1 1 d . . . P1 P 1.0897(9) 0.7188(8) 0.4201(4) 0.0115(18) Uani 1 1 d . . . P2 P 1.0143(9) 0.3810(9) 0.3102(5) 0.0117(18) Uani 1 1 d . . . O2 O 0.528(3) 0.592(3) 0.4371(12) 0.016(5) Uiso 1 1 d . . . C1 C 0.631(3) 0.555(3) 0.4058(15) 0.009(6) Uiso 1 1 d . . . O4 O 1.133(3) 0.843(3) 0.4016(12) 0.017(5) Uiso 1 1 d . . . O6 O 0.920(3) 0.438(2) 0.2589(11) 0.014(5) Uiso 1 1 d . . . O8 O 1.158(3) 0.430(3) 0.3028(12) 0.017(6) Uiso 1 1 d . . . O1 O 0.623(3) 0.491(3) 0.3547(12) 0.018(5) Uiso 1 1 d . . . O7 O 1.005(3) 0.235(2) 0.3117(11) 0.013(5) Uiso 1 1 d . . . O5 O 1.194(2) 0.616(2) 0.4189(11) 0.013(5) Uiso 1 1 d . . . O1W O 0.238(3) 0.688(2) 0.2552(11) 0.013(5) Uiso 1 1 d . . . O3 O 1.013(3) 0.715(2) 0.4856(11) 0.015(5) Uiso 1 1 d . . . H3 H 1.0506 0.7644 0.5120 0.018 Uiso 1 1 calc R . . C2 C 0.769(4) 0.592(4) 0.4291(17) 0.017(7) Uiso 1 1 d . . . H2A H 0.7715 0.6844 0.4398 0.021 Uiso 1 1 calc R . . H2B H 0.7927 0.5429 0.4684 0.021 Uiso 1 1 calc R . . C3 C 0.945(4) 0.437(4) 0.386(2) 0.024(9) Uiso 1 1 d . . . H3A H 0.8843 0.3709 0.4043 0.029 Uiso 1 1 calc R . . H3B H 1.0186 0.4512 0.4176 0.029 Uiso 1 1 calc R . . N1 N 0.866(3) 0.563(3) 0.3761(13) 0.008(5) Uiso 1 1 d . . . H1 H 0.8158 0.5526 0.3387 0.009 Uiso 1 1 calc R . . C4 C 0.960(4) 0.680(4) 0.364(2) 0.027(9) Uiso 1 1 d . . . H4A H 0.9022 0.7565 0.3597 0.033 Uiso 1 1 calc R . . H4B H 1.0036 0.6666 0.3214 0.033 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 La1 0.0027(10) 0.0027(10) 0.0280(12) -0.0006(7) -0.0004(7) -0.0006(7) P1 0.007(4) 0.005(4) 0.022(5) 0.001(3) 0.002(3) 0.000(3) P2 0.002(4) 0.007(4) 0.026(5) -0.002(3) -0.001(3) 0.002(3) _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 La1 O6 2.38(2) 6_556 ? La1 O8 2.43(3) 1_455 ? La1 O4 2.45(3) 7_755 ? La1 O5 2.46(2) 1_455 ? La1 O7 2.50(3) 7_765 ? La1 O1W 2.60(2) . ? La1 O2 2.69(3) . ? La1 O1 2.70(3) . ? P1 O4 1.41(3) . ? P1 O5 1.49(3) . ? P1 O3 1.56(2) . ? P1 C4 1.78(4) . ? P2 O7 1.52(3) . ? P2 O8 1.53(3) . ? P2 O6 1.54(3) . ? P2 C3 1.82(4) . ? O2 C1 1.27(4) . ? C1 O1 1.25(4) . ? C1 C2 1.51(5) . ? O4 La1 2.45(3) 7_765 ? O6 La1 2.38(2) 6_656 ? O8 La1 2.43(3) 1_655 ? O7 La1 2.50(3) 7_755 ? O5 La1 2.46(2) 1_655 ? O3 H3 0.8400 . ? C2 N1 1.49(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N1 1.55(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N1 C4 1.56(5) . ? N1 H1 0.9300 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? 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 O6 La1 O8 74.3(9) 6_556 1_455 ? O6 La1 O4 93.1(8) 6_556 7_755 ? O8 La1 O4 77.5(9) 1_455 7_755 ? O6 La1 O5 152.7(8) 6_556 1_455 ? O8 La1 O5 79.0(8) 1_455 1_455 ? O4 La1 O5 86.2(8) 7_755 1_455 ? O6 La1 O7 92.3(8) 6_556 7_765 ? O8 La1 O7 139.9(8) 1_455 7_765 ? O4 La1 O7 141.9(8) 7_755 7_765 ? O5 La1 O7 105.0(8) 1_455 7_765 ? O6 La1 O1W 79.5(8) 6_556 . ? O8 La1 O1W 72.4(8) 1_455 . ? O4 La1 O1W 149.9(8) 7_755 . ? O5 La1 O1W 87.4(8) 1_455 . ? O7 La1 O1W 68.0(8) 7_765 . ? O6 La1 O2 125.0(8) 6_556 . ? O8 La1 O2 147.1(8) 1_455 . ? O4 La1 O2 75.2(8) 7_755 . ? O5 La1 O2 81.2(8) 1_455 . ? O7 La1 O2 70.9(8) 7_765 . ? O1W La1 O2 132.6(8) . . ? O6 La1 O1 76.4(8) 6_556 . ? O8 La1 O1 138.0(8) 1_455 . ? O4 La1 O1 74.8(8) 7_755 . ? O5 La1 O1 129.1(8) 1_455 . ? O7 La1 O1 70.0(8) 7_765 . ? O1W La1 O1 130.1(8) . . ? O2 La1 O1 48.6(8) . . ? O4 P1 O5 116.2(15) . . ? O4 P1 O3 114.1(15) . . ? O5 P1 O3 109.7(14) . . ? O4 P1 C4 104.5(19) . . ? O5 P1 C4 109.1(18) . . ? O3 P1 C4 102.0(18) . . ? O7 P2 O8 113.0(15) . . ? O7 P2 O6 111.3(14) . . ? O8 P2 O6 112.1(14) . . ? O7 P2 C3 106.3(17) . . ? O8 P2 C3 109.6(17) . . ? O6 P2 C3 104.0(17) . . ? C1 O2 La1 93.4(19) . . ? O1 C1 O2 123(3) . . ? O1 C1 C2 118(3) . . ? O2 C1 C2 120(3) . . ? P1 O4 La1 158.2(17) . 7_765 ? P2 O6 La1 157.1(15) . 6_656 ? P2 O8 La1 154.2(15) . 1_655 ? C1 O1 La1 93(2) . . ? P2 O7 La1 141.4(15) . 7_755 ? P1 O5 La1 134.6(14) . 1_655 ? P1 O3 H3 109.5 . . ? N1 C2 C1 108(3) . . ? N1 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N1 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.5 . . ? N1 C3 P2 110(3) . . ? N1 C3 H3A 109.6 . . ? P2 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? P2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C2 N1 C3 114(3) . . ? C2 N1 C4 111(3) . . ? C3 N1 C4 113(3) . . ? C2 N1 H1 106.5 . . ? C3 N1 H1 106.5 . . ? C4 N1 H1 106.5 . . ? N1 C4 P1 120(3) . . ? N1 C4 H4A 107.2 . . ? P1 C4 H4A 107.2 . . ? N1 C4 H4B 107.2 . . ? P1 C4 H4B 107.2 . . ? H4A C4 H4B 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 La1 O2 C1 6(2) 6_556 . . . ? O8 La1 O2 C1 125(2) 1_455 . . . ? O4 La1 O2 C1 90(2) 7_755 . . . ? O5 La1 O2 C1 178(2) 1_455 . . . ? O7 La1 O2 C1 -73(2) 7_765 . . . ? O1W La1 O2 C1 -104(2) . . . . ? O1 La1 O2 C1 7.2(19) . . . . ? La1 O2 C1 O1 -14(4) . . . . ? La1 O2 C1 C2 163(3) . . . . ? O5 P1 O4 La1 120(4) . . . 7_765 ? O3 P1 O4 La1 -111(4) . . . 7_765 ? C4 P1 O4 La1 0(5) . . . 7_765 ? O7 P2 O6 La1 -110(4) . . . 6_656 ? O8 P2 O6 La1 18(4) . . . 6_656 ? C3 P2 O6 La1 136(4) . . . 6_656 ? O7 P2 O8 La1 -115(3) . . . 1_655 ? O6 P2 O8 La1 118(3) . . . 1_655 ? C3 P2 O8 La1 3(4) . . . 1_655 ? O2 C1 O1 La1 14(4) . . . . ? C2 C1 O1 La1 -163(3) . . . . ? O6 La1 O1 C1 172(2) 6_556 . . . ? O8 La1 O1 C1 -141(2) 1_455 . . . ? O4 La1 O1 C1 -91(2) 7_755 . . . ? O5 La1 O1 C1 -19(2) 1_455 . . . ? O7 La1 O1 C1 74(2) 7_765 . . . ? O1W La1 O1 C1 109(2) . . . . ? O2 La1 O1 C1 -7.3(19) . . . . ? O8 P2 O7 La1 25(3) . . . 7_755 ? O6 P2 O7 La1 152(2) . . . 7_755 ? C3 P2 O7 La1 -95(2) . . . 7_755 ? O4 P1 O5 La1 -50(2) . . . 1_655 ? O3 P1 O5 La1 178.4(17) . . . 1_655 ? C4 P1 O5 La1 67(3) . . . 1_655 ? O1 C1 C2 N1 11(4) . . . . ? O2 C1 C2 N1 -167(3) . . . . ? O7 P2 C3 N1 -144(2) . . . . ? O8 P2 C3 N1 94(3) . . . . ? O6 P2 C3 N1 -26(3) . . . . ? C1 C2 N1 C3 -101(3) . . . . ? C1 C2 N1 C4 132(3) . . . . ? P2 C3 N1 C2 160(2) . . . . ? P2 C3 N1 C4 -73(3) . . . . ? C2 N1 C4 P1 73(4) . . . . ? C3 N1 C4 P1 -55(4) . . . . ? O4 P1 C4 N1 -167(3) . . . . ? O5 P1 C4 N1 68(3) . . . . ? O3 P1 C4 N1 -48(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.93 2.05 2.58(4) 114.2 . N1 H1 O6 0.93 2.29 2.81(4) 114.7 . O3 H3 O2 0.84 1.84 2.58(4) 144.5 3_566 N1 H1 O1W 0.93 2.52 3.27(4) 137.7 6_656 _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.35 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 12.407 _refine_diff_density_min -3.824 _refine_diff_density_rms 0.693 data_03 _database_code_depnum_ccdc_archive 'CCDC 705162' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '04 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 N O9 P2 Pr' _chemical_formula_sum 'C4 H10 N O9 P2 Pr' _chemical_formula_weight 418.98 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source PR 22.04400 2.77393 19.66970 0.22209 12.38560 16.76690 2.82428 143.64400 2.05830 -0.53000 2.84500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.09000 0.09500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.00800 0.00600 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.00200 0.00200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.00400 0.00300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.7951(9) _cell_length_b 10.2777(9) _cell_length_c 20.4047(18) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2054.2(3) _exptl_crystal_density_diffrn 2.710 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Hilgenberg borosilicate glass capillary (ca. 0.4 mm of diameter) ; #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; MAR 345 Imaging Plate instrument belonging to the Swiss-Norwegian BM01a beam line (bending magnet source) at the European Synchrotron Radiation Facility (ESRF), Grenoble, France. ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source Synchrotron _diffrn_radiation_type X-ray _diffrn_radiation_monochromator 0.71013(1) _diffrn_measurement_method Debye-Scherrer _diffrn_detector 'Imaging Plate' _diffrn_detector_type 'MAR 345' _pd_meas_scan_method cont _pd_meas_special_details ; The powdered sample was slowly spun 180 degrees (in phi scanning mode) during data collection to improve powder averaging. Two-dimensional powder data was collected using a MAR2300 imaging plate detector and then integrated using the software Fit2D. The monochromatic wavelength (0.71013 A) and sample-to-detector distance (d of about 150 mm) were calibrated from an individual run using the standard LaB6. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 1312 _pd_meas_2theta_range_min 2.02483 _pd_meas_2theta_range_max 49.00845 _pd_meas_2theta_range_inc 0.035838 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Gaussian _pd_proc_ls_background_function 'Fixed points' _pd_proc_ls_pref_orient_corr ; None ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 3.8551 _pd_proc_ls_prof_wR_factor 5.5171 _pd_proc_ls_prof_wR_expected 2.0174 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 10.3614 _pd_proc_ls_prof_cwR_factor 12.3058 _pd_proc_ls_prof_cwR_expected 4.4997 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 7.4791 _pd_proc_ls_prof_echi2 7.4791 # Items related to LS refinement _refine_ls_R_I_factor 8.8946 _refine_ls_number_reflns 2083 _refine_ls_number_parameters 62 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0514 _pd_proc_2theta_range_max 49.0350 _pd_proc_2theta_range_inc 0.035838 _pd_proc_wavelength 0.710130 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol PR1 0.3602(3) 0.5429(3) 0.33803(15) 0.01267 1.00000 Uiso PR P1 1.0879(7) 0.7218(7) 0.4184(4) 0.01267 1.00000 Uiso P P2 1.0141(7) 0.3778(7) 0.3119(4) 0.01267 1.00000 Uiso P O2 0.52031(18) 0.589(2) 0.4349(7) 0.01267 1.00000 Uiso O C1 0.62601(10) 0.5627(8) 0.4042(3) 0.01267 1.00000 Uiso C O4 1.1506(19) 0.8553(8) 0.4068(9) 0.01267 1.00000 Uiso O O6 0.9269(13) 0.4459(13) 0.2601(10) 0.01267 1.00000 Uiso O O8 1.1616(9) 0.4213(13) 0.3046(10) 0.01267 1.00000 Uiso O O1 0.6173(3) 0.4893(19) 0.3562(7) 0.01267 1.00000 Uiso O O7 1.0023(15) 0.2315(7) 0.3024(11) 0.01267 1.00000 Uiso O O5 1.1999(16) 0.6193(11) 0.4178(9) 0.01267 1.00000 Uiso O O1W 0.234(3) 0.682(3) 0.2525(13) 0.01267 1.00000 Uiso O O3 1.020(2) 0.7194(13) 0.4865(8) 0.01267 1.00000 Uiso O H3 1.02981 0.79210 0.50530 0.01267 1.00000 Uiso H C2 0.76401(11) 0.5989(14) 0.4317(5) 0.01267 1.00000 Uiso C H2A 0.78144 0.54608 0.46823 0.01267 1.00000 Uiso H H2B 0.76702 0.68726 0.44111 0.01267 1.00000 Uiso H C3 0.944(3) 0.4379(15) 0.3894(6) 0.01267 1.00000 Uiso C H3A 0.88359 0.37419 0.40821 0.01267 1.00000 Uiso H H3B 1.01646 0.45398 0.42023 0.01267 1.00000 Uiso H N1 0.8647(11) 0.5653(8) 0.3761(7) 0.01267 1.00000 Uiso N H1 0.81551 0.54907 0.33911 0.01267 1.00000 Uiso H C4 0.9597(17) 0.6784(16) 0.3576(7) 0.01267 1.00000 Uiso C H4A 1.00582 0.65820 0.31732 0.01267 1.00000 Uiso H H4B 0.90390 0.75415 0.34930 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY 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 Pr1 O6 2.3310(6) 8_556 ? Pr1 O4 2.3861(6) 6_755 ? Pr1 O5 2.3924(6) 1_455 ? Pr1 O8 2.4109(6) 1_455 ? Pr1 O7 2.4708(7) 6_765 ? Pr1 O2 2.5667(8) . ? Pr1 O1W 2.5767(6) . ? Pr1 O1 2.6039(7) . ? Pr1 C1 2.9390(10) . ? P1 O4 1.5223(6) . ? P1 O5 1.5218(7) . ? P1 O3 1.5409(8) . ? P1 C4 1.8215(9) . ? P2 O8 1.5196(6) . ? P2 O7 1.5203(7) . ? P2 O6 1.5275(6) . ? P2 C3 1.8315(8) . ? O2 C1 1.2394(12) . ? C1 O1 1.2398(9) . ? C1 C2 1.5103(11) . ? O4 Pr1 2.3861(6) 6_765 ? O6 Pr1 2.3310(6) 8_656 ? O8 Pr1 2.4109(6) 1_655 ? O7 Pr1 2.4708(7) 6_755 ? O5 Pr1 2.3924(6) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.5446(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.5458(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.5384(13) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O6 Pr1 O4 99.89(2) 8_556 6_755 ? O6 Pr1 O5 155.25(2) 8_556 1_455 ? O4 Pr1 O5 80.59(2) 6_755 1_455 ? O6 Pr1 O8 76.18(2) 8_556 1_455 ? O4 Pr1 O8 73.25(2) 6_755 1_455 ? O5 Pr1 O8 80.379(19) 1_455 1_455 ? O6 Pr1 O7 85.97(2) 8_556 6_765 ? O4 Pr1 O7 146.22(2) 6_755 6_765 ? O5 Pr1 O7 107.51(2) 1_455 6_765 ? O8 Pr1 O7 139.785(18) 1_455 6_765 ? O6 Pr1 O2 124.71(2) 8_556 . ? O4 Pr1 O2 73.99(2) 6_755 . ? O5 Pr1 O2 79.46(2) 1_455 . ? O8 Pr1 O2 143.78(2) 1_455 . ? O7 Pr1 O2 75.42(2) 6_765 . ? O6 Pr1 O1W 77.96(2) 8_556 . ? O4 Pr1 O1W 145.72(2) 6_755 . ? O5 Pr1 O1W 87.80(2) 1_455 . ? O8 Pr1 O1W 73.06(2) 1_455 . ? O7 Pr1 O1W 68.06(2) 6_765 . ? O2 Pr1 O1W 135.42(2) . . ? O6 Pr1 O1 76.143(17) 8_556 . ? O4 Pr1 O1 77.77(2) 6_755 . ? O5 Pr1 O1 127.401(17) 1_455 . ? O8 Pr1 O1 135.277(19) 1_455 . ? O7 Pr1 O1 71.38(2) 6_765 . ? O2 Pr1 O1 48.634(19) . . ? O1W Pr1 O1 132.82(2) . . ? O6 Pr1 C1 100.14(2) 8_556 . ? O4 Pr1 C1 79.92(2) 6_755 . ? O5 Pr1 C1 104.26(2) 1_455 . ? O8 Pr1 C1 151.69(2) 1_455 . ? O7 Pr1 C1 66.30(2) 6_765 . ? O2 Pr1 C1 24.86(2) . . ? O1W Pr1 C1 134.33(2) . . ? O1 Pr1 C1 24.919(18) . . ? O4 P1 O5 109.42(4) . . ? O4 P1 O3 109.18(4) . . ? O5 P1 O3 107.95(3) . . ? O4 P1 C4 113.07(4) . . ? O5 P1 C4 108.75(4) . . ? O3 P1 C4 108.34(3) . . ? O8 P2 O7 110.57(3) . . ? O8 P2 O6 109.21(3) . . ? O7 P2 O6 108.77(4) . . ? O8 P2 C3 110.10(4) . . ? O7 P2 C3 114.44(4) . . ? O6 P2 C3 103.43(4) . . ? C1 O2 Pr1 94.63(5) . . ? O2 C1 O1 118.39(10) . . ? O2 C1 C2 120.36(7) . . ? O1 C1 C2 120.35(8) . . ? O2 C1 Pr1 60.51(6) . . ? O1 C1 Pr1 62.24(5) . . ? C2 C1 Pr1 168.62(6) . . ? P1 O4 Pr1 143.34(4) . 6_765 ? P2 O6 Pr1 161.20(4) . 8_656 ? P2 O8 Pr1 153.07(3) . 1_655 ? C1 O1 Pr1 92.84(6) . . ? P2 O7 Pr1 134.14(4) . 6_755 ? P1 O5 Pr1 134.95(3) . 1_655 ? P1 O3 H3 109.5 . . ? C1 C2 N1 104.06(7) . . ? C1 C2 H2A 110.9 . . ? N1 C2 H2A 110.9 . . ? C1 C2 H2B 111.0 . . ? N1 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? N1 C3 P2 108.80(5) . . ? N1 C3 H3A 109.9 . . ? P2 C3 H3A 110.0 . . ? N1 C3 H3B 109.9 . . ? P2 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? C4 N1 C2 113.48(7) . . ? C4 N1 C3 112.38(7) . . ? C2 N1 C3 112.42(6) . . ? C4 N1 H1 105.9 . . ? C2 N1 H1 106.0 . . ? C3 N1 H1 105.9 . . ? N1 C4 P1 115.71(6) . . ? N1 C4 H4A 108.3 . . ? P1 C4 H4A 108.4 . . ? N1 C4 H4B 108.4 . . ? P1 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Pr1 O2 C1 9.69(7) 8_556 . . . ? O4 Pr1 O2 C1 100.75(6) 6_755 . . . ? O5 Pr1 O2 C1 -176.12(6) 1_455 . . . ? O8 Pr1 O2 C1 126.68(6) 1_455 . . . ? O7 Pr1 O2 C1 -64.74(6) 6_765 . . . ? O1W Pr1 O2 C1 -100.27(6) . . . . ? O1 Pr1 O2 C1 13.10(5) . . . . ? Pr1 O2 C1 O1 -23.96(8) . . . . ? Pr1 O2 C1 C2 166.90(7) . . . . ? O6 Pr1 C1 O2 -171.92(6) 8_556 . . . ? O4 Pr1 C1 O2 -73.56(6) 6_755 . . . ? O5 Pr1 C1 O2 3.93(6) 1_455 . . . ? O8 Pr1 C1 O2 -92.28(7) 1_455 . . . ? O7 Pr1 C1 O2 107.08(6) 6_765 . . . ? O1W Pr1 C1 O2 105.06(5) . . . . ? O1 Pr1 C1 O2 -156.19(8) . . . . ? O6 Pr1 C1 O1 -15.74(4) 8_556 . . . ? O4 Pr1 C1 O1 82.63(4) 6_755 . . . ? O5 Pr1 C1 O1 160.12(4) 1_455 . . . ? O8 Pr1 C1 O1 63.91(5) 1_455 . . . ? O7 Pr1 C1 O1 -96.73(4) 6_765 . . . ? O2 Pr1 C1 O1 156.19(8) . . . . ? O1W Pr1 C1 O1 -98.75(5) . . . . ? O6 Pr1 C1 C2 90.4(3) 8_556 . . . ? O4 Pr1 C1 C2 -171.2(3) 6_755 . . . ? O5 Pr1 C1 C2 -93.7(3) 1_455 . . . ? O8 Pr1 C1 C2 170.1(3) 1_455 . . . ? O7 Pr1 C1 C2 9.4(3) 6_765 . . . ? O2 Pr1 C1 C2 -97.6(3) . . . . ? O1W Pr1 C1 C2 7.4(3) . . . . ? O1 Pr1 C1 C2 106.2(3) . . . . ? O5 P1 O4 Pr1 124.60(5) . . . 6_765 ? O3 P1 O4 Pr1 -117.46(6) . . . 6_765 ? C4 P1 O4 Pr1 3.22(8) . . . 6_765 ? O8 P2 O6 Pr1 33.12(14) . . . 8_656 ? O7 P2 O6 Pr1 -87.63(13) . . . 8_656 ? C3 P2 O6 Pr1 150.34(13) . . . 8_656 ? O7 P2 O8 Pr1 -134.62(6) . . . 1_655 ? O6 P2 O8 Pr1 105.73(7) . . . 1_655 ? C3 P2 O8 Pr1 -7.19(9) . . . 1_655 ? O2 C1 O1 Pr1 23.55(8) . . . . ? C2 C1 O1 Pr1 -167.31(7) . . . . ? O6 Pr1 O1 C1 164.04(4) 8_556 . . . ? O4 Pr1 O1 C1 -92.40(4) 6_755 . . . ? O5 Pr1 O1 C1 -24.52(5) 1_455 . . . ? O8 Pr1 O1 C1 -142.75(4) 1_455 . . . ? O7 Pr1 O1 C1 73.65(4) 6_765 . . . ? O2 Pr1 O1 C1 -13.07(4) . . . . ? O1W Pr1 O1 C1 105.47(4) . . . . ? O8 P2 O7 Pr1 41.41(5) . . . 6_755 ? O6 P2 O7 Pr1 161.32(4) . . . 6_755 ? C3 P2 O7 Pr1 -83.60(5) . . . 6_755 ? O4 P1 O5 Pr1 -62.31(6) . . . 1_655 ? O3 P1 O5 Pr1 178.98(4) . . . 1_655 ? C4 P1 O5 Pr1 61.64(6) . . . 1_655 ? O2 C1 C2 N1 -173.31(8) . . . . ? O1 C1 C2 N1 17.76(10) . . . . ? Pr1 C1 C2 N1 -82.2(3) . . . . ? O8 P2 C3 N1 96.46(7) . . . . ? O7 P2 C3 N1 -138.28(6) . . . . ? O6 P2 C3 N1 -20.13(7) . . . . ? C1 C2 N1 C4 127.37(8) . . . . ? C1 C2 N1 C3 -103.71(9) . . . . ? P2 C3 N1 C4 -69.36(7) . . . . ? P2 C3 N1 C2 161.14(6) . . . . ? C2 N1 C4 P1 69.51(9) . . . . ? C3 N1 C4 P1 -59.43(8) . . . . ? O4 P1 C4 N1 -163.55(6) . . . . ? O5 P1 C4 N1 74.70(7) . . . . ? O3 P1 C4 N1 -42.39(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.76 2.5386(10) 158.9 2_566 data_04 _database_code_depnum_ccdc_archive 'CCDC 705163' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '04 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 N Nd O9 P2' _chemical_formula_sum 'C4 H10 N Nd O9 P2' _chemical_formula_weight 422.31 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source ND 22.68450 2.66248 19.68470 0.21063 12.77400 15.88500 2.85137 137.90300 1.98486 -0.53500 3.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.09000 0.09500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.00800 0.00600 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.00200 0.00200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.00400 0.00300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.7736(14) _cell_length_b 10.2529(15) _cell_length_c 20.400(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2044.2(5) _exptl_crystal_density_diffrn 2.744 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Hilgenberg borosilicate glass capillary (ca. 0.4 mm of diameter) ; #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; MAR 345 Imaging Plate instrument belonging to the Swiss-Norwegian BM01a beam line (bending magnet source) at the European Synchrotron Radiation Facility (ESRF), Grenoble, France. ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source Synchrotron _diffrn_radiation_type X-ray _diffrn_radiation_monochromator 0.71013(1) _diffrn_measurement_method Debye-Scherrer _diffrn_detector 'Imaging Plate' _diffrn_detector_type 'MAR 345' _pd_meas_scan_method cont _pd_meas_special_details ; The powdered sample was slowly spun 180 degrees (in phi scanning mode) during data collection to improve powder averaging. Two-dimensional powder data was collected using a MAR2300 imaging plate detector and then integrated using the software Fit2D. The monochromatic wavelength (0.71013 A) and sample-to-detector distance (d of about 150 mm) were calibrated from an individual run using the standard LaB6. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 1312 _pd_meas_2theta_range_min 2.00000 _pd_meas_2theta_range_max 48.98362 _pd_meas_2theta_range_inc 0.035838 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Gaussian _pd_proc_ls_background_function 'Fixed points' _pd_proc_ls_pref_orient_corr ; None ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 4.6961 _pd_proc_ls_prof_wR_factor 6.3289 _pd_proc_ls_prof_wR_expected 1.9777 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 11.8444 _pd_proc_ls_prof_cwR_factor 13.5092 _pd_proc_ls_prof_cwR_expected 4.2215 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 10.2407 _pd_proc_ls_prof_echi2 10.2407 # Items related to LS refinement _refine_ls_R_I_factor 9.8831 _refine_ls_number_reflns 2170 _refine_ls_number_parameters 62 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0475 _pd_proc_2theta_range_max 49.0311 _pd_proc_2theta_range_inc 0.035838 _pd_proc_wavelength 0.710130 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol ND1 0.3610(4) 0.5421(4) 0.33734(19) 0.01267 1.00000 Uiso ND P1 1.0842(8) 0.7203(8) 0.4157(4) 0.01267 1.00000 Uiso P P2 1.0163(8) 0.3784(7) 0.3112(4) 0.01267 1.00000 Uiso P O2 0.5235(3) 0.591(3) 0.4358(7) 0.01267 1.00000 Uiso O C1 0.62789(10) 0.5703(5) 0.40287(18) 0.01267 1.00000 Uiso C O4 1.148(2) 0.8550(8) 0.4057(10) 0.01267 1.00000 Uiso O O6 0.9260(14) 0.4510(13) 0.2618(11) 0.01267 1.00000 Uiso O O8 1.1642(9) 0.4220(13) 0.3025(11) 0.01267 1.00000 Uiso O O1 0.6172(3) 0.490(2) 0.3576(10) 0.01267 1.00000 Uiso O O7 1.0047(16) 0.2326(7) 0.2981(13) 0.01267 1.00000 Uiso O O5 1.1973(17) 0.6182(11) 0.4140(10) 0.01267 1.00000 Uiso O O1W 0.248(4) 0.681(4) 0.2489(16) 0.01267 1.00000 Uiso O O3 1.016(2) 0.7164(13) 0.4833(9) 0.01267 1.00000 Uiso O H3 1.02728 0.78884 0.50347 0.01267 1.00000 Uiso H C2 0.76708(12) 0.6069(10) 0.4292(4) 0.01267 1.00000 Uiso C H2A 0.77417 0.69829 0.43656 0.01267 1.00000 Uiso H H2B 0.78996 0.55824 0.46584 0.01267 1.00000 Uiso H C3 0.944(3) 0.4428(17) 0.3873(6) 0.01267 1.00000 Uiso C H3A 0.88512 0.38102 0.40679 0.01267 1.00000 Uiso H H3B 1.01718 0.46324 0.41761 0.01267 1.00000 Uiso H N1 0.8632(12) 0.5687(8) 0.3721(7) 0.01267 1.00000 Uiso N H1 0.81275 0.55216 0.33491 0.01267 1.00000 Uiso H C4 0.9595(17) 0.6811(17) 0.3522(7) 0.01267 1.00000 Uiso C H4A 0.90817 0.75857 0.34175 0.01267 1.00000 Uiso H H4B 1.01113 0.65921 0.31245 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Nd1 O6 2.316(4) 8_556 ? Nd1 O5 2.372(4) 1_455 ? Nd1 O4 2.372(5) 6_755 ? Nd1 O8 2.393(4) 1_455 ? Nd1 O7 2.486(4) 6_765 ? Nd1 O1W 2.554(5) . ? Nd1 O1 2.593(4) . ? Nd1 O2 2.610(4) . ? Nd1 C1 2.948(7) . ? P1 O5 1.520(5) . ? P1 O4 1.531(5) . ? P1 O3 1.534(4) . ? P1 C4 1.826(6) . ? P2 O7 1.522(4) . ? P2 O8 1.523(5) . ? P2 O6 1.533(5) . ? P2 C3 1.831(7) . ? O2 C1 1.239(7) . ? C1 O1 1.243(7) . ? C1 C2 1.508(11) . ? O4 Nd1 2.372(5) 6_765 ? O6 Nd1 2.316(4) 8_656 ? O8 Nd1 2.393(4) 1_655 ? O7 Nd1 2.486(4) 6_755 ? O5 Nd1 2.372(4) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.548(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.544(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.541(8) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O6 Nd1 O5 153.33(16) 8_556 1_455 ? O6 Nd1 O4 101.38(17) 8_556 6_755 ? O5 Nd1 O4 81.58(16) 1_455 6_755 ? O6 Nd1 O8 75.73(15) 8_556 1_455 ? O5 Nd1 O8 79.73(16) 1_455 1_455 ? O4 Nd1 O8 74.23(15) 6_755 1_455 ? O6 Nd1 O7 83.76(18) 8_556 6_765 ? O5 Nd1 O7 108.09(18) 1_455 6_765 ? O4 Nd1 O7 147.52(14) 6_755 6_765 ? O8 Nd1 O7 137.25(14) 1_455 6_765 ? O6 Nd1 O1W 74.22(17) 8_556 . ? O5 Nd1 O1W 89.32(16) 1_455 . ? O4 Nd1 O1W 148.36(13) 6_755 . ? O8 Nd1 O1W 74.35(16) 1_455 . ? O7 Nd1 O1W 64.04(15) 6_765 . ? O6 Nd1 O1 77.99(16) 8_556 . ? O5 Nd1 O1 127.96(14) 1_455 . ? O4 Nd1 O1 77.05(13) 6_755 . ? O8 Nd1 O1 135.88(14) 1_455 . ? O7 Nd1 O1 72.69(12) 6_765 . ? O1W Nd1 O1 130.27(14) . . ? O6 Nd1 O2 125.65(14) 8_556 . ? O5 Nd1 O2 80.84(11) 1_455 . ? O4 Nd1 O2 74.08(15) 6_755 . ? O8 Nd1 O2 144.79(14) 1_455 . ? O7 Nd1 O2 76.97(16) 6_765 . ? O1W Nd1 O2 134.40(17) . . ? O1 Nd1 O2 47.85(15) . . ? O6 Nd1 C1 101.19(17) 8_556 . ? O5 Nd1 C1 105.45(16) 1_455 . ? O4 Nd1 C1 81.06(18) 6_755 . ? O8 Nd1 C1 153.78(18) 1_455 . ? O7 Nd1 C1 66.52(18) 6_765 . ? O1W Nd1 C1 130.56(19) . . ? O1 Nd1 C1 24.88(14) . . ? O2 Nd1 C1 24.80(14) . . ? O5 P1 O4 108.8(2) . . ? O5 P1 O3 108.8(3) . . ? O4 P1 O3 108.8(3) . . ? O5 P1 C4 108.5(3) . . ? O4 P1 C4 112.0(3) . . ? O3 P1 C4 109.8(3) . . ? O7 P2 O8 109.8(3) . . ? O7 P2 O6 108.5(3) . . ? O8 P2 O6 109.2(3) . . ? O7 P2 C3 118.3(3) . . ? O8 P2 C3 111.0(3) . . ? O6 P2 C3 99.3(3) . . ? C1 O2 Nd1 93.1(4) . . ? O2 C1 O1 116.5(7) . . ? O2 C1 C2 120.6(5) . . ? O1 C1 C2 120.3(7) . . ? O2 C1 Nd1 62.1(3) . . ? O1 C1 Nd1 61.4(4) . . ? C2 C1 Nd1 169.6(5) . . ? P1 O4 Nd1 142.6(2) . 6_765 ? P2 O6 Nd1 158.1(3) . 8_656 ? P2 O8 Nd1 151.6(3) . 1_655 ? C1 O1 Nd1 93.8(4) . . ? P2 O7 Nd1 132.4(3) . 6_755 ? P1 O5 Nd1 137.1(3) . 1_655 ? P1 O3 H3 109.4 . . ? C1 C2 N1 102.6(5) . . ? C1 C2 H2A 111.2 . . ? N1 C2 H2A 111.3 . . ? C1 C2 H2B 111.2 . . ? N1 C2 H2B 111.2 . . ? H2A C2 H2B 109.2 . . ? N1 C3 P2 109.0(4) . . ? N1 C3 H3A 109.9 . . ? P2 C3 H3A 109.8 . . ? N1 C3 H3B 109.9 . . ? P2 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? C4 N1 C3 111.6(5) . . ? C4 N1 C2 112.3(4) . . ? C3 N1 C2 111.6(4) . . ? C4 N1 H1 106.9 . . ? C3 N1 H1 107.1 . . ? C2 N1 H1 107.0 . . ? N1 C4 P1 112.6(4) . . ? N1 C4 H4A 109.2 . . ? P1 C4 H4A 109.1 . . ? N1 C4 H4B 109.0 . . ? P1 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Nd1 O2 C1 10.7(5) 8_556 . . . ? O5 Nd1 O2 C1 -172.8(5) 1_455 . . . ? O4 Nd1 O2 C1 103.4(4) 6_755 . . . ? O8 Nd1 O2 C1 130.0(4) 1_455 . . . ? O7 Nd1 O2 C1 -61.7(5) 6_765 . . . ? O1W Nd1 O2 C1 -92.9(5) . . . . ? O1 Nd1 O2 C1 16.6(4) . . . . ? Nd1 O2 C1 O1 -29.6(6) . . . . ? Nd1 O2 C1 C2 168.5(6) . . . . ? O6 Nd1 C1 O2 -171.2(4) 8_556 . . . ? O5 Nd1 C1 O2 7.4(5) 1_455 . . . ? O4 Nd1 C1 O2 -71.3(4) 6_755 . . . ? O8 Nd1 C1 O2 -90.8(5) 1_455 . . . ? O7 Nd1 C1 O2 110.7(5) 6_765 . . . ? O1W Nd1 C1 O2 110.1(4) . . . . ? O1 Nd1 C1 O2 -149.7(7) . . . . ? O6 Nd1 C1 O1 -21.5(4) 8_556 . . . ? O5 Nd1 C1 O1 157.1(4) 1_455 . . . ? O4 Nd1 C1 O1 78.5(3) 6_755 . . . ? O8 Nd1 C1 O1 58.9(6) 1_455 . . . ? O7 Nd1 C1 O1 -99.5(4) 6_765 . . . ? O1W Nd1 C1 O1 -100.2(4) . . . . ? O2 Nd1 C1 O1 149.7(7) . . . . ? O6 Nd1 C1 C2 81(3) 8_556 . . . ? O5 Nd1 C1 C2 -101(3) 1_455 . . . ? O4 Nd1 C1 C2 -179(100) 6_755 . . . ? O8 Nd1 C1 C2 161(2) 1_455 . . . ? O7 Nd1 C1 C2 3(3) 6_765 . . . ? O1W Nd1 C1 C2 2(3) . . . . ? O1 Nd1 C1 C2 102(3) . . . . ? O2 Nd1 C1 C2 -108(3) . . . . ? O5 P1 O4 Nd1 122.9(4) . . . 6_765 ? O3 P1 O4 Nd1 -118.7(4) . . . 6_765 ? C4 P1 O4 Nd1 2.9(5) . . . 6_765 ? O7 P2 O6 Nd1 -78.2(10) . . . 8_656 ? O8 P2 O6 Nd1 41.5(11) . . . 8_656 ? C3 P2 O6 Nd1 157.7(9) . . . 8_656 ? O7 P2 O8 Nd1 -135.7(5) . . . 1_655 ? O6 P2 O8 Nd1 105.4(6) . . . 1_655 ? C3 P2 O8 Nd1 -3.0(7) . . . 1_655 ? O2 C1 O1 Nd1 29.9(6) . . . . ? C2 C1 O1 Nd1 -168.2(6) . . . . ? O6 Nd1 O1 C1 158.5(4) 8_556 . . . ? O5 Nd1 O1 C1 -28.4(4) 1_455 . . . ? O4 Nd1 O1 C1 -96.7(4) 6_755 . . . ? O8 Nd1 O1 C1 -147.1(4) 1_455 . . . ? O7 Nd1 O1 C1 71.3(4) 6_765 . . . ? O1W Nd1 O1 C1 101.5(4) . . . . ? O2 Nd1 O1 C1 -16.6(4) . . . . ? O8 P2 O7 Nd1 48.2(4) . . . 6_755 ? O6 P2 O7 Nd1 167.5(3) . . . 6_755 ? C3 P2 O7 Nd1 -80.6(4) . . . 6_755 ? O4 P1 O5 Nd1 -62.0(4) . . . 1_655 ? O3 P1 O5 Nd1 179.6(4) . . . 1_655 ? C4 P1 O5 Nd1 60.2(5) . . . 1_655 ? O2 C1 C2 N1 -177.9(6) . . . . ? O1 C1 C2 N1 20.9(8) . . . . ? Nd1 C1 C2 N1 -75(3) . . . . ? O7 P2 C3 N1 -135.2(4) . . . . ? O8 P2 C3 N1 96.5(4) . . . . ? O6 P2 C3 N1 -18.2(5) . . . . ? P2 C3 N1 C4 -69.5(6) . . . . ? P2 C3 N1 C2 164.0(4) . . . . ? C1 C2 N1 C4 128.2(5) . . . . ? C1 C2 N1 C3 -105.7(6) . . . . ? C3 N1 C4 P1 -58.8(6) . . . . ? C2 N1 C4 P1 67.3(6) . . . . ? O5 P1 C4 N1 77.5(5) . . . . ? O4 P1 C4 N1 -162.3(4) . . . . ? O3 P1 C4 N1 -41.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.79 2.574(7) 160.5 2_566 data_05 _database_code_depnum_ccdc_archive 'CCDC 705164' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '07 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 N O9 P2 Sm' _chemical_formula_sum 'C4 H10 N O9 P2 Sm' _chemical_formula_weight 428.42 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source SM 24.00420 2.47274 19.42580 0.19645 13.43960 14.39960 2.89604 128.00700 2.20963 -5.69600 12.32000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.28300 0.43400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.8402(7) _cell_length_b 10.3073(8) _cell_length_c 20.6805(13) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2097.5(3) _exptl_crystal_density_diffrn 2.713 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Glass slide ; _pd_spec_mount_mode Reflection _pd_spec_shape 'Flat sheet' #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; Conventional powder diffractometer instrument belonging to the University of Aveiro and located at the Central Analytical Laboratory ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source 'X-ray tube' _diffrn_radiation_type X-ray _diffrn_source_target Cu _diffrn_radiation_monochromator None _diffrn_measurement_method Bragg-Brentano _diffrn_detector_type 'X Celerator detector' _pd_meas_scan_method cont _pd_meas_special_details ; Data were collected in a continuous mode over the angular range 4-110. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 8977 _pd_meas_2theta_range_min 5.00000 _pd_meas_2theta_range_max 95.00235 _pd_meas_2theta_range_inc 0.010027 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function 'Fixed Points' _pd_proc_ls_pref_orient_corr ; Modified March's function along the [002] vector. G1 refined to about 0.713(2) which is consistent with the platy crystal habit of the material (as revealed by SEM pictures). ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 2.4662 _pd_proc_ls_prof_wR_factor 3.1942 _pd_proc_ls_prof_wR_expected 1.4393 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 20.2285 _pd_proc_ls_prof_cwR_factor 15.1753 _pd_proc_ls_prof_cwR_expected 6.8381 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 4.9250 _pd_proc_ls_prof_echi2 4.9629 # Items related to LS refinement _refine_ls_R_I_factor 8.9106 _refine_ls_number_reflns 2156 _refine_ls_number_parameters 64 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.9414 _pd_proc_2theta_range_max 94.9438 _pd_proc_2theta_range_inc 0.010027 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol SM1 0.3630(3) 0.5418(3) 0.33727(9) 0.01267 1.00000 Uiso SM P1 1.0905(7) 0.7249(7) 0.4159(3) 0.01267 1.00000 Uiso P P2 1.0148(7) 0.3941(7) 0.3063(3) 0.01267 1.00000 Uiso P O2 0.52903(18) 0.6037(18) 0.4323(7) 0.01267 1.00000 Uiso O C1 0.63487(10) 0.5592(6) 0.40846(16) 0.01267 1.00000 Uiso C O4 1.1568(18) 0.8591(7) 0.4135(7) 0.01267 1.00000 Uiso O O6 0.9215(11) 0.4637(12) 0.2601(7) 0.01267 1.00000 Uiso O O8 1.1566(9) 0.4457(12) 0.3044(6) 0.01267 1.00000 Uiso O O1 0.6272(3) 0.5122(19) 0.3534(4) 0.01267 1.00000 Uiso O O7 0.9967(14) 0.2508(7) 0.3041(7) 0.01267 1.00000 Uiso O O5 1.1983(15) 0.6220(10) 0.4069(7) 0.01267 1.00000 Uiso O O1W 0.257(3) 0.701(3) 0.2522(7) 0.01267 1.00000 Uiso O O3 1.0278(17) 0.7086(12) 0.4853(6) 0.01267 1.00000 Uiso O H3 1.03721 0.77939 0.50624 0.01267 1.00000 Uiso H C2 0.77146(10) 0.5928(11) 0.4372(3) 0.01267 1.00000 Uiso C H2A 0.77315 0.69057 0.45196 0.01267 1.00000 Uiso H H2B 0.79565 0.54696 0.47463 0.01267 1.00000 Uiso H C3 0.966(2) 0.4578(16) 0.3856(5) 0.01267 1.00000 Uiso C H3A 0.91701 0.39152 0.40982 0.01267 1.00000 Uiso H H3B 1.04075 0.48488 0.40868 0.01267 1.00000 Uiso H N1 0.8646(11) 0.5729(8) 0.3772(6) 0.01267 1.00000 Uiso N H1 0.80782 0.55903 0.34500 0.01267 1.00000 Uiso H C4 0.9472(14) 0.6970(13) 0.3605(7) 0.01267 1.00000 Uiso C H4A 0.89293 0.77167 0.35776 0.01267 1.00000 Uiso H H4B 0.98682 0.68319 0.31662 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Sm1 O6 2.242(4) 8_556 ? Sm1 O5 2.319(5) 1_455 ? Sm1 O8 2.359(4) 1_455 ? Sm1 O4 2.465(5) 6_755 ? Sm1 O1W 2.623(5) . ? Sm1 O2 2.630(5) . ? Sm1 O1 2.639(5) . ? Sm1 O7 2.645(5) 6_765 ? Sm1 C1 3.055(8) . ? P1 O5 1.513(4) . ? P1 O4 1.529(5) . ? P1 O3 1.564(5) . ? P1 C4 1.843(6) . ? P2 O7 1.490(6) . ? P2 O8 1.493(4) . ? P2 O6 1.507(5) . ? P2 C3 1.828(6) . ? O2 C1 1.240(9) . ? C1 O1 1.244(7) . ? C1 C2 1.515(10) . ? O4 Sm1 2.465(5) 6_765 ? O6 Sm1 2.242(4) 8_656 ? O8 Sm1 2.359(4) 1_655 ? O7 Sm1 2.645(5) 6_755 ? O5 Sm1 2.319(5) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.553(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.557(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.552(8) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O6 Sm1 O5 149.93(17) 8_556 1_455 ? O6 Sm1 O8 79.28(15) 8_556 1_455 ? O5 Sm1 O8 74.18(16) 1_455 1_455 ? O6 Sm1 O4 108.68(17) 8_556 6_755 ? O5 Sm1 O4 79.64(15) 1_455 6_755 ? O8 Sm1 O4 78.23(14) 1_455 6_755 ? O6 Sm1 O1W 74.22(17) 8_556 . ? O5 Sm1 O1W 85.04(16) 1_455 . ? O8 Sm1 O1W 74.19(16) 1_455 . ? O4 Sm1 O1W 151.21(16) 6_755 . ? O6 Sm1 O2 126.75(16) 8_556 . ? O5 Sm1 O2 83.11(15) 1_455 . ? O8 Sm1 O2 148.04(14) 1_455 . ? O4 Sm1 O2 75.76(13) 6_755 . ? O1W Sm1 O2 126.53(14) . . ? O6 Sm1 O1 79.47(14) 8_556 . ? O5 Sm1 O1 130.57(13) 1_455 . ? O8 Sm1 O1 146.70(13) 1_455 . ? O4 Sm1 O1 84.68(13) 6_755 . ? O1W Sm1 O1 123.39(14) . . ? O2 Sm1 O1 47.54(12) . . ? O6 Sm1 O7 85.84(18) 8_556 6_765 ? O5 Sm1 O7 103.45(15) 1_455 6_765 ? O8 Sm1 O7 135.76(16) 1_455 6_765 ? O4 Sm1 O7 145.81(11) 6_755 6_765 ? O1W Sm1 O7 61.68(15) . 6_765 ? O2 Sm1 O7 70.93(14) . 6_765 ? O1 Sm1 O7 67.28(12) . 6_765 ? O6 Sm1 C1 103.25(17) 8_556 . ? O5 Sm1 C1 106.75(15) 1_455 . ? O8 Sm1 C1 156.24(16) 1_455 . ? O4 Sm1 C1 78.63(16) 6_755 . ? O1W Sm1 C1 129.47(16) . . ? O2 Sm1 C1 23.73(16) . . ? O1 Sm1 C1 23.84(13) . . ? O7 Sm1 C1 67.79(15) 6_765 . ? O5 P1 O4 109.4(2) . . ? O5 P1 O3 108.4(3) . . ? O4 P1 O3 106.9(3) . . ? O5 P1 C4 110.7(3) . . ? O4 P1 C4 116.6(3) . . ? O3 P1 C4 104.5(3) . . ? O7 P2 O8 117.6(2) . . ? O7 P2 O6 112.5(3) . . ? O8 P2 O6 112.6(3) . . ? O7 P2 C3 110.3(3) . . ? O8 P2 C3 98.4(3) . . ? O6 P2 C3 103.7(3) . . ? C1 O2 Sm1 97.7(5) . . ? O2 C1 O1 117.5(8) . . ? O2 C1 C2 120.8(6) . . ? O1 C1 C2 119.6(7) . . ? O2 C1 Sm1 58.5(4) . . ? O1 C1 Sm1 59.0(4) . . ? C2 C1 Sm1 168.7(5) . . ? P1 O4 Sm1 132.7(3) . 6_765 ? P2 O6 Sm1 153.9(3) . 8_656 ? P2 O8 Sm1 161.3(3) . 1_655 ? C1 O1 Sm1 97.1(5) . . ? P2 O7 Sm1 137.7(3) . 6_755 ? P1 O5 Sm1 144.7(3) . 1_655 ? P1 O3 H3 109.5 . . ? C1 C2 N1 100.8(6) . . ? C1 C2 H2A 111.4 . . ? N1 C2 H2A 111.7 . . ? C1 C2 H2B 111.6 . . ? N1 C2 H2B 111.7 . . ? H2A C2 H2B 109.5 . . ? N1 C3 P2 110.1(4) . . ? N1 C3 H3A 110.0 . . ? P2 C3 H3A 109.9 . . ? N1 C3 H3B 109.3 . . ? P2 C3 H3B 109.3 . . ? H3A C3 H3B 108.2 . . ? C4 N1 C2 112.0(5) . . ? C4 N1 C3 109.0(5) . . ? C2 N1 C3 112.7(5) . . ? C4 N1 H1 107.7 . . ? C2 N1 H1 107.7 . . ? C3 N1 H1 107.5 . . ? N1 C4 P1 112.9(4) . . ? N1 C4 H4A 109.1 . . ? P1 C4 H4A 109.0 . . ? N1 C4 H4B 109.0 . . ? P1 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Sm1 O2 C1 -8.8(4) 8_556 . . . ? O5 Sm1 O2 C1 175.1(4) 1_455 . . . ? O8 Sm1 O2 C1 130.6(4) 1_455 . . . ? O4 Sm1 O2 C1 94.1(4) 6_755 . . . ? O1W Sm1 O2 C1 -106.3(4) . . . . ? O1 Sm1 O2 C1 -1.8(3) . . . . ? O7 Sm1 O2 C1 -78.0(4) 6_765 . . . ? Sm1 O2 C1 O1 3.1(6) . . . . ? Sm1 O2 C1 C2 166.8(5) . . . . ? O6 Sm1 C1 O2 172.8(4) 8_556 . . . ? O5 Sm1 C1 O2 -5.1(4) 1_455 . . . ? O8 Sm1 C1 O2 -93.7(5) 1_455 . . . ? O4 Sm1 C1 O2 -80.5(4) 6_755 . . . ? O1W Sm1 C1 O2 92.5(4) . . . . ? O1 Sm1 C1 O2 176.8(6) . . . . ? O7 Sm1 C1 O2 93.0(3) 6_765 . . . ? O6 Sm1 C1 O1 -4.0(4) 8_556 . . . ? O5 Sm1 C1 O1 178.2(3) 1_455 . . . ? O8 Sm1 C1 O1 89.5(5) 1_455 . . . ? O4 Sm1 C1 O1 102.8(3) 6_755 . . . ? O1W Sm1 C1 O1 -84.3(3) . . . . ? O2 Sm1 C1 O1 -176.8(6) . . . . ? O7 Sm1 C1 O1 -83.8(3) 6_765 . . . ? O6 Sm1 C1 C2 82(3) 8_556 . . . ? O5 Sm1 C1 C2 -95(3) 1_455 . . . ? O8 Sm1 C1 C2 176(2) 1_455 . . . ? O4 Sm1 C1 C2 -171(3) 6_755 . . . ? O1W Sm1 C1 C2 2(3) . . . . ? O2 Sm1 C1 C2 -90(2) . . . . ? O1 Sm1 C1 C2 86(3) . . . . ? O7 Sm1 C1 C2 3(2) 6_765 . . . ? O5 P1 O4 Sm1 114.4(3) . . . 6_765 ? O3 P1 O4 Sm1 -128.5(3) . . . 6_765 ? C4 P1 O4 Sm1 -12.2(4) . . . 6_765 ? O7 P2 O6 Sm1 -84.1(8) . . . 8_656 ? O8 P2 O6 Sm1 51.5(8) . . . 8_656 ? C3 P2 O6 Sm1 156.8(7) . . . 8_656 ? O7 P2 O8 Sm1 -108.0(8) . . . 1_655 ? O6 P2 O8 Sm1 118.8(8) . . . 1_655 ? C3 P2 O8 Sm1 10.2(8) . . . 1_655 ? O2 C1 O1 Sm1 -3.1(6) . . . . ? C2 C1 O1 Sm1 -167.0(5) . . . . ? O6 Sm1 O1 C1 176.1(4) 8_556 . . . ? O5 Sm1 O1 C1 -2.3(4) 1_455 . . . ? O8 Sm1 O1 C1 -132.8(3) 1_455 . . . ? O4 Sm1 O1 C1 -73.8(3) 6_755 . . . ? O1W Sm1 O1 C1 113.1(3) . . . . ? O2 Sm1 O1 C1 1.8(3) . . . . ? O7 Sm1 O1 C1 86.2(4) 6_765 . . . ? O8 P2 O7 Sm1 26.8(5) . . . 6_755 ? O6 P2 O7 Sm1 160.0(3) . . . 6_755 ? C3 P2 O7 Sm1 -84.8(4) . . . 6_755 ? O4 P1 O5 Sm1 -61.2(5) . . . 1_655 ? O3 P1 O5 Sm1 -177.4(4) . . . 1_655 ? C4 P1 O5 Sm1 68.6(5) . . . 1_655 ? O2 C1 C2 N1 -154.8(6) . . . . ? O1 C1 C2 N1 8.5(8) . . . . ? Sm1 C1 C2 N1 -71(3) . . . . ? O7 P2 C3 N1 -129.7(5) . . . . ? O8 P2 C3 N1 106.7(5) . . . . ? O6 P2 C3 N1 -9.1(6) . . . . ? C1 C2 N1 C4 123.2(5) . . . . ? C1 C2 N1 C3 -113.5(7) . . . . ? P2 C3 N1 C4 -79.8(6) . . . . ? P2 C3 N1 C2 155.2(4) . . . . ? C2 N1 C4 P1 75.6(6) . . . . ? C3 N1 C4 P1 -49.8(5) . . . . ? O5 P1 C4 N1 68.1(5) . . . . ? O4 P1 C4 N1 -166.0(4) . . . . ? O3 P1 C4 N1 -48.3(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.79 2.581(7) 162.2 2_566 data_06 _database_code_depnum_ccdc_archive 'CCDC 705165' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '02 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Eu N O9 P2' _chemical_formula_sum 'C4 H10 Eu N O9 P2' _chemical_formula_weight 430.03 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source EU 24.62740 2.38790 19.08860 0.19420 13.76030 13.75460 2.92270 123.17400 2.57450 -7.71800 11.27600 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.28300 0.43400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.8328(10) _cell_length_b 10.2989(11) _cell_length_c 20.6667(12) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2092.8(3) _exptl_crystal_density_diffrn 2.730 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Glass slide ; _pd_spec_mount_mode Reflection _pd_spec_shape 'Flat sheet' #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; Conventional powder diffractometer instrument belonging to the University of Aveiro and located at the Central Analytical Laboratory ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source 'X-ray tube' _diffrn_radiation_type X-ray _diffrn_source_target Cu _diffrn_radiation_monochromator None _diffrn_measurement_method Bragg-Brentano _diffrn_detector_type 'X Celerator detector' _pd_meas_scan_method cont _pd_meas_special_details ; Data were collected in a continuous mode over the angular range 4-110. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 5287 _pd_meas_2theta_range_min 4.00000 _pd_meas_2theta_range_max 110.00544 _pd_meas_2theta_range_inc 0.020054 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function 'Fixed Points' _pd_proc_ls_pref_orient_corr ; Modified March's function along the [002] vector. G1 refined to about 0.539(1) which is consistent with the platy crystal habit of the material (as revealed by SEM pictures). ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 2.0946 _pd_proc_ls_prof_wR_factor 2.7813 _pd_proc_ls_prof_wR_expected 1.0606 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 17.8216 _pd_proc_ls_prof_cwR_factor 13.0300 _pd_proc_ls_prof_cwR_expected 4.9686 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 6.8775 _pd_proc_ls_prof_echi2 6.9561 # Items related to LS refinement _refine_ls_R_I_factor 9.1133 _refine_ls_number_reflns 2918 _refine_ls_number_parameters 64 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 3.9323 _pd_proc_2theta_range_max 109.9378 _pd_proc_2theta_range_inc 0.020054 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol EU1 0.3645(4) 0.5428(4) 0.33706(9) 0.01267 1.00000 Uiso EU P1 1.1018(7) 0.7274(8) 0.4186(3) 0.01267 1.00000 Uiso P P2 1.0111(8) 0.3944(8) 0.3092(3) 0.01267 1.00000 Uiso P O2 0.52802(20) 0.6103(20) 0.4347(8) 0.01267 1.00000 Uiso O C1 0.63355(9) 0.5647(5) 0.41096(11) 0.01267 1.00000 Uiso C O4 1.1619(18) 0.8658(7) 0.4121(7) 0.01267 1.00000 Uiso O O6 0.9259(12) 0.4510(13) 0.2555(7) 0.01267 1.00000 Uiso O O8 1.1570(9) 0.4406(14) 0.3056(7) 0.01267 1.00000 Uiso O O1 0.6244(4) 0.527(3) 0.3542(4) 0.01267 1.00000 Uiso O O7 1.0011(15) 0.2481(7) 0.3105(7) 0.01267 1.00000 Uiso O O5 1.2233(15) 0.6333(11) 0.4154(7) 0.01267 1.00000 Uiso O O1W 0.264(4) 0.693(4) 0.2524(7) 0.01267 1.00000 Uiso O O3 1.0457(18) 0.7188(13) 0.4899(6) 0.01267 1.00000 Uiso O H3 1.04679 0.79096 0.50764 0.01267 1.00000 Uiso H C2 0.77059(10) 0.5986(10) 0.4393(2) 0.01267 1.00000 Uiso C H2A 0.77542 0.67728 0.45344 0.01267 1.00000 Uiso H H2B 0.79512 0.53154 0.47131 0.01267 1.00000 Uiso H C3 0.955(3) 0.4534(16) 0.3883(5) 0.01267 1.00000 Uiso C H3A 0.91425 0.38798 0.41188 0.01267 1.00000 Uiso H H3B 1.04251 0.47609 0.41313 0.01267 1.00000 Uiso H N1 0.8702(12) 0.5791(8) 0.3819(6) 0.01267 1.00000 Uiso N H1 0.82100 0.55891 0.34473 0.01267 1.00000 Uiso H C4 0.9588(15) 0.6970(15) 0.3641(7) 0.01267 1.00000 Uiso C H4A 0.89331 0.77192 0.36777 0.01267 1.00000 Uiso H H4B 0.98563 0.69412 0.32095 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Eu1 O6 2.220(10) 8_556 ? Eu1 O5 2.329(10) 1_455 ? Eu1 O8 2.382(11) 1_455 ? Eu1 O4 2.397(10) 6_755 ? Eu1 O1W 2.534(10) . ? Eu1 O7 2.548(10) 6_765 ? Eu1 O1 2.589(11) . ? Eu1 O2 2.677(11) . ? Eu1 C1 3.073(19) . ? P1 O5 1.536(13) . ? P1 O4 1.556(12) . ? P1 O3 1.573(10) . ? P1 C4 1.827(16) . ? P2 O6 1.507(11) . ? P2 O7 1.518(11) . ? P2 O8 1.519(11) . ? P2 C3 1.835(17) . ? O2 C1 1.25(2) . ? C1 O1 1.240(15) . ? C1 C2 1.51(2) . ? O4 Eu1 2.397(10) 6_765 ? O6 Eu1 2.220(10) 8_656 ? O8 Eu1 2.382(11) 1_655 ? O7 Eu1 2.548(10) 6_755 ? O5 Eu1 2.329(10) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.54(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.54(2) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.54(2) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O6 Eu1 O5 158.6(4) 8_556 1_455 ? O6 Eu1 O8 78.8(4) 8_556 1_455 ? O5 Eu1 O8 81.7(3) 1_455 1_455 ? O6 Eu1 O4 105.3(4) 8_556 6_755 ? O5 Eu1 O4 78.1(4) 1_455 6_755 ? O8 Eu1 O4 75.5(4) 1_455 6_755 ? O6 Eu1 O1W 76.5(3) 8_556 . ? O5 Eu1 O1W 90.1(3) 1_455 . ? O8 Eu1 O1W 75.4(4) 1_455 . ? O4 Eu1 O1W 149.8(4) 6_755 . ? O6 Eu1 O7 91.5(4) 8_556 6_765 ? O5 Eu1 O7 97.2(4) 1_455 6_765 ? O8 Eu1 O7 138.6(4) 1_455 6_765 ? O4 Eu1 O7 145.2(4) 6_755 6_765 ? O1W Eu1 O7 63.2(4) . 6_765 ? O6 Eu1 O1 79.9(3) 8_556 . ? O5 Eu1 O1 121.5(3) 1_455 . ? O8 Eu1 O1 148.6(3) 1_455 . ? O4 Eu1 O1 88.3(4) 6_755 . ? O1W Eu1 O1 121.2(4) . . ? O7 Eu1 O1 64.5(4) 6_765 . ? O6 Eu1 O2 126.9(4) 8_556 . ? O5 Eu1 O2 74.5(3) 1_455 . ? O8 Eu1 O2 146.6(3) 1_455 . ? O4 Eu1 O2 76.9(4) 6_755 . ? O1W Eu1 O2 126.8(4) . . ? O7 Eu1 O2 68.6(4) 6_765 . ? O1 Eu1 O2 47.0(3) . . ? O6 Eu1 C1 103.2(4) 8_556 . ? O5 Eu1 C1 98.3(4) 1_455 . ? O8 Eu1 C1 155.0(4) 1_455 . ? O4 Eu1 C1 80.1(4) 6_755 . ? O1W Eu1 C1 129.5(4) . . ? O7 Eu1 C1 66.3(4) 6_765 . ? O1 Eu1 C1 23.4(3) . . ? O2 Eu1 C1 23.8(4) . . ? O5 P1 O4 106.3(6) . . ? O5 P1 O3 106.1(6) . . ? O4 P1 O3 105.7(7) . . ? O5 P1 C4 117.6(8) . . ? O4 P1 C4 113.1(8) . . ? O3 P1 C4 107.3(7) . . ? O6 P2 O7 111.3(7) . . ? O6 P2 O8 112.0(6) . . ? O7 P2 O8 111.8(7) . . ? O6 P2 C3 110.9(7) . . ? O7 P2 C3 107.2(8) . . ? O8 P2 C3 103.2(7) . . ? C1 O2 Eu1 96.2(10) . . ? O2 C1 O1 115.2(18) . . ? O2 C1 C2 120.4(12) . . ? O1 C1 C2 120.7(18) . . ? O2 C1 Eu1 60.0(9) . . ? O1 C1 Eu1 55.9(11) . . ? C2 C1 Eu1 168.8(11) . . ? P1 O4 Eu1 135.6(6) . 6_765 ? P2 O6 Eu1 161.6(7) . 8_656 ? P2 O8 Eu1 159.3(6) . 1_655 ? C1 O1 Eu1 100.8(12) . . ? P2 O7 Eu1 142.8(7) . 6_755 ? P1 O5 Eu1 138.6(5) . 1_655 ? P1 O3 H3 109.3 . . ? C1 C2 N1 103.7(11) . . ? C1 C2 H2A 111.0 . . ? N1 C2 H2A 111.0 . . ? C1 C2 H2B 111.1 . . ? N1 C2 H2B 111.0 . . ? H2A C2 H2B 109.0 . . ? N1 C3 P2 111.6(14) . . ? N1 C3 H3A 109.4 . . ? P2 C3 H3A 109.4 . . ? N1 C3 H3B 109.2 . . ? P2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C4 N1 C3 112.4(13) . . ? C4 N1 C2 116.0(12) . . ? C3 N1 C2 112.6(13) . . ? C4 N1 H1 104.8 . . ? C3 N1 H1 104.8 . . ? C2 N1 H1 105.0 . . ? N1 C4 P1 114.7(13) . . ? N1 C4 H4A 108.7 . . ? P1 C4 H4A 108.7 . . ? N1 C4 H4B 108.6 . . ? P1 C4 H4B 108.4 . . ? H4A C4 H4B 107.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Eu1 O2 C1 -4.5(13) 8_556 . . . ? O5 Eu1 O2 C1 176.1(12) 1_455 . . . ? O8 Eu1 O2 C1 130.0(10) 1_455 . . . ? O4 Eu1 O2 C1 95.0(11) 6_755 . . . ? O1W Eu1 O2 C1 -105.8(12) . . . . ? O7 Eu1 O2 C1 -79.5(11) 6_765 . . . ? O1 Eu1 O2 C1 -5.0(10) . . . . ? Eu1 O2 C1 O1 8.4(17) . . . . ? Eu1 O2 C1 C2 167.1(13) . . . . ? O6 Eu1 C1 O2 176.3(11) 8_556 . . . ? O5 Eu1 C1 O2 -3.8(12) 1_455 . . . ? O8 Eu1 C1 O2 -91.9(13) 1_455 . . . ? O4 Eu1 C1 O2 -80.1(11) 6_755 . . . ? O1W Eu1 C1 O2 93.1(12) . . . . ? O7 Eu1 C1 O2 90.5(11) 6_765 . . . ? O1 Eu1 C1 O2 170.8(18) . . . . ? O6 Eu1 C1 O1 5.6(11) 8_556 . . . ? O5 Eu1 C1 O1 -174.6(10) 1_455 . . . ? O8 Eu1 C1 O1 97.4(12) 1_455 . . . ? O4 Eu1 C1 O1 109.2(11) 6_755 . . . ? O1W Eu1 C1 O1 -77.6(11) . . . . ? O7 Eu1 C1 O1 -80.3(10) 6_765 . . . ? O2 Eu1 C1 O1 -170.8(18) . . . . ? O6 Eu1 C1 C2 81(6) 8_556 . . . ? O5 Eu1 C1 C2 -99(6) 1_455 . . . ? O8 Eu1 C1 C2 173(5) 1_455 . . . ? O4 Eu1 C1 C2 -175(6) 6_755 . . . ? O1W Eu1 C1 C2 -2(6) . . . . ? O7 Eu1 C1 C2 -5(6) 6_765 . . . ? O1 Eu1 C1 C2 76(5) . . . . ? O2 Eu1 C1 C2 -95(6) . . . . ? O5 P1 O4 Eu1 119.3(8) . . . 6_765 ? O3 P1 O4 Eu1 -128.2(8) . . . 6_765 ? C4 P1 O4 Eu1 -11.1(12) . . . 6_765 ? O7 P2 O6 Eu1 -105(2) . . . 8_656 ? O8 P2 O6 Eu1 21(2) . . . 8_656 ? C3 P2 O6 Eu1 135(2) . . . 8_656 ? O6 P2 O8 Eu1 118.5(18) . . . 1_655 ? O7 P2 O8 Eu1 -115.8(17) . . . 1_655 ? C3 P2 O8 Eu1 -1(2) . . . 1_655 ? O2 C1 O1 Eu1 -8.8(17) . . . . ? C2 C1 O1 Eu1 -167.4(13) . . . . ? O6 Eu1 O1 C1 -174.5(11) 8_556 . . . ? O5 Eu1 O1 C1 6.3(11) 1_455 . . . ? O8 Eu1 O1 C1 -126.5(10) 1_455 . . . ? O4 Eu1 O1 C1 -68.6(11) 6_755 . . . ? O1W Eu1 O1 C1 118.2(10) . . . . ? O7 Eu1 O1 C1 88.9(10) 6_765 . . . ? O2 Eu1 O1 C1 5.1(10) . . . . ? O6 P2 O7 Eu1 148.0(10) . . . 6_755 ? O8 P2 O7 Eu1 22.0(14) . . . 6_755 ? C3 P2 O7 Eu1 -90.5(13) . . . 6_755 ? O4 P1 O5 Eu1 -78.3(11) . . . 1_655 ? O3 P1 O5 Eu1 169.5(9) . . . 1_655 ? C4 P1 O5 Eu1 49.6(13) . . . 1_655 ? O2 C1 C2 N1 -155.1(16) . . . . ? O1 C1 C2 N1 2(2) . . . . ? Eu1 C1 C2 N1 -66(6) . . . . ? O6 P2 C3 N1 -19.9(14) . . . . ? O7 P2 C3 N1 -141.6(11) . . . . ? O8 P2 C3 N1 100.2(10) . . . . ? P2 C3 N1 C4 -72.1(16) . . . . ? P2 C3 N1 C2 154.7(11) . . . . ? C1 C2 N1 C4 124.0(15) . . . . ? C1 C2 N1 C3 -104.6(16) . . . . ? C3 N1 C4 P1 -54.9(19) . . . . ? C2 N1 C4 P1 76.6(18) . . . . ? O5 P1 C4 N1 72.5(14) . . . . ? O4 P1 C4 N1 -163.0(10) . . . . ? O3 P1 C4 N1 -46.9(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.59 2.36(2) 153.6 2_566 data_07 _database_code_depnum_ccdc_archive 'CCDC 705166' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '02 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Gd N O9 P2' _chemical_formula_sum 'C4 H10 Gd N O9 P2' _chemical_formula_weight 435.32 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source GD 25.07090 2.25341 19.07980 0.18195 13.85180 12.93310 3.54545 101.39799 2.41960 -9.24200 11.94600 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.28300 0.43400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.8093(7) _cell_length_b 10.2734(8) _cell_length_c 20.6812(11) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2084.1(2) _exptl_crystal_density_diffrn 2.775 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Glass slide ; _pd_spec_mount_mode Reflection _pd_spec_shape 'Flat sheet' #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; Conventional powder diffractometer instrument belonging to the University of Aveiro and located at the Central Analytical Laboratory ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source 'X-ray tube' _diffrn_radiation_type X-ray _diffrn_source_target Cu _diffrn_radiation_monochromator None _diffrn_measurement_method Bragg-Brentano _diffrn_detector_type 'X Celerator detector' _pd_meas_scan_method cont _pd_meas_special_details ; Data were collected in a continuous mode over the angular range 4-110. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 10472 _pd_meas_2theta_range_min 5.00000 _pd_meas_2theta_range_max 109.99271 _pd_meas_2theta_range_inc 0.010027 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function 'Fixed Points' _pd_proc_ls_pref_orient_corr ; Modified March's function along the [002] vector. G1 refined to about 0.591(1) which is consistent with the platy crystal habit of the material (as revealed by SEM pictures). ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 1.6068 _pd_proc_ls_prof_wR_factor 2.1493 _pd_proc_ls_prof_wR_expected 0.7213 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 19.3744 _pd_proc_ls_prof_cwR_factor 12.4783 _pd_proc_ls_prof_cwR_expected 4.1877 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 8.8790 _pd_proc_ls_prof_echi2 8.9216 # Items related to LS refinement _refine_ls_R_I_factor 9.9385 _refine_ls_number_reflns 2946 _refine_ls_number_parameters 64 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.9257 _pd_proc_2theta_range_max 109.9184 _pd_proc_2theta_range_inc 0.010027 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol GD1 0.3648(3) 0.5421(3) 0.33700(8) 0.01267 1.00000 Uiso GD P1 1.0862(7) 0.7294(7) 0.4168(3) 0.01267 1.00000 Uiso P P2 1.0216(7) 0.4045(7) 0.3056(3) 0.01267 1.00000 Uiso P O2 0.52985(17) 0.6122(13) 0.4286(7) 0.01267 1.00000 Uiso O C1 0.63565(9) 0.5594(3) 0.40885(10) 0.01267 1.00000 Uiso C O4 1.1481(17) 0.8673(7) 0.4179(6) 0.01267 1.00000 Uiso O O6 0.9299(11) 0.4749(12) 0.2587(6) 0.01267 1.00000 Uiso O O8 1.1662(8) 0.4460(13) 0.3051(6) 0.01267 1.00000 Uiso O O1 0.6247(4) 0.5175(19) 0.3529(3) 0.01267 1.00000 Uiso O O7 0.9965(13) 0.2610(7) 0.3068(6) 0.01267 1.00000 Uiso O O5 1.2045(14) 0.6322(10) 0.4112(6) 0.01267 1.00000 Uiso O O1W 0.258(3) 0.682(3) 0.2528(6) 0.01267 1.00000 Uiso O O3 1.0278(16) 0.7090(12) 0.4887(5) 0.01267 1.00000 Uiso O H3 1.03766 0.77876 0.51015 0.01267 1.00000 Uiso H C2 0.77294(9) 0.6010(7) 0.4346(2) 0.01267 1.00000 Uiso C H2A 0.77271 0.69596 0.44497 0.01267 1.00000 Uiso H H2B 0.79655 0.55722 0.47404 0.01267 1.00000 Uiso H C3 0.977(2) 0.4578(16) 0.3869(5) 0.01267 1.00000 Uiso C H3A 0.93988 0.39211 0.41229 0.01267 1.00000 Uiso H H3B 1.05697 0.49441 0.40841 0.01267 1.00000 Uiso H N1 0.8722(10) 0.5684(8) 0.3778(5) 0.01267 1.00000 Uiso N H1 0.81880 0.54958 0.34422 0.01267 1.00000 Uiso H C4 0.9550(15) 0.6910(14) 0.3576(6) 0.01267 1.00000 Uiso C H4A 0.89276 0.76797 0.35635 0.01267 1.00000 Uiso H H4B 0.99293 0.68195 0.31690 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Gd1 O6 2.1920(12) 8_556 ? Gd1 O8 2.2824(14) 1_455 ? Gd1 O5 2.3827(14) 1_455 ? Gd1 O4 2.4586(13) 6_755 ? Gd1 O1W 2.4865(13) . ? Gd1 O1 2.5816(14) . ? Gd1 O2 2.5912(15) . ? Gd1 O7 2.7008(15) 6_765 ? Gd1 C1 3.048(2) . ? P1 O5 1.5361(16) . ? P1 O4 1.5417(14) . ? P1 O3 1.6068(16) . ? P1 C4 1.8138(19) . ? P2 O8 1.4796(15) . ? P2 O7 1.4972(17) . ? P2 O6 1.5070(13) . ? P2 C3 1.822(2) . ? O2 C1 1.237(3) . ? C1 O1 1.238(2) . ? C1 C2 1.512(3) . ? O4 Gd1 2.4586(13) 6_765 ? O6 Gd1 2.1920(12) 8_656 ? O8 Gd1 2.2824(14) 1_655 ? O7 Gd1 2.7008(15) 6_755 ? O5 Gd1 2.3827(14) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.565(2) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.543(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.559(2) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O6 Gd1 O8 81.51(4) 8_556 1_455 ? O6 Gd1 O5 153.63(4) 8_556 1_455 ? O8 Gd1 O5 77.88(5) 1_455 1_455 ? O6 Gd1 O4 113.55(4) 8_556 6_755 ? O8 Gd1 O4 80.53(4) 1_455 6_755 ? O5 Gd1 O4 79.12(4) 1_455 6_755 ? O6 Gd1 O1W 70.88(5) 8_556 . ? O8 Gd1 O1W 71.86(5) 1_455 . ? O5 Gd1 O1W 87.07(4) 1_455 . ? O4 Gd1 O1W 151.19(5) 6_755 . ? O6 Gd1 O1 78.27(4) 8_556 . ? O8 Gd1 O1 146.91(4) 1_455 . ? O5 Gd1 O1 127.35(4) 1_455 . ? O4 Gd1 O1 83.89(4) 6_755 . ? O1W Gd1 O1 124.10(5) . . ? O6 Gd1 O2 124.37(5) 8_556 . ? O8 Gd1 O2 149.74(5) 1_455 . ? O5 Gd1 O2 80.48(4) 1_455 . ? O4 Gd1 O2 74.78(5) 6_755 . ? O1W Gd1 O2 127.90(6) . . ? O1 Gd1 O2 46.93(4) . . ? O6 Gd1 O7 84.61(4) 8_556 6_765 ? O8 Gd1 O7 136.44(4) 1_455 6_765 ? O5 Gd1 O7 99.15(5) 1_455 6_765 ? O4 Gd1 O7 142.31(4) 6_755 6_765 ? O1W Gd1 O7 64.57(5) . 6_765 ? O1 Gd1 O7 67.17(4) . 6_765 ? O2 Gd1 O7 67.88(5) . 6_765 ? O6 Gd1 C1 101.80(5) 8_556 . ? O8 Gd1 C1 155.49(5) 1_455 . ? O5 Gd1 C1 103.79(5) 1_455 . ? O4 Gd1 C1 75.89(5) 6_755 . ? O1W Gd1 C1 132.37(6) . . ? O1 Gd1 C1 23.59(4) . . ? O2 Gd1 C1 23.61(5) . . ? O7 Gd1 C1 67.93(5) 6_765 . ? O5 P1 O4 107.50(8) . . ? O5 P1 O3 104.74(8) . . ? O4 P1 O3 104.26(7) . . ? O5 P1 C4 109.96(10) . . ? O4 P1 C4 119.20(10) . . ? O3 P1 C4 110.14(8) . . ? O8 P2 O7 116.30(8) . . ? O8 P2 O6 115.43(7) . . ? O7 P2 O6 112.64(7) . . ? O8 P2 C3 98.48(9) . . ? O7 P2 C3 104.04(9) . . ? O6 P2 C3 107.80(9) . . ? C1 O2 Gd1 99.38(12) . . ? O2 C1 O1 112.66(17) . . ? O2 C1 C2 120.52(16) . . ? O1 C1 C2 120.38(17) . . ? O2 C1 Gd1 57.01(11) . . ? O1 C1 Gd1 56.56(10) . . ? C2 C1 Gd1 164.95(14) . . ? P1 O4 Gd1 129.85(7) . 6_765 ? P2 O6 Gd1 154.98(8) . 8_656 ? P2 O8 Gd1 160.18(8) . 1_655 ? C1 O1 Gd1 99.85(12) . . ? P2 O7 Gd1 137.73(8) . 6_755 ? P1 O5 Gd1 143.10(8) . 1_655 ? P1 O3 H3 109.5 . . ? C1 C2 N1 103.19(16) . . ? C1 C2 H2A 111.1 . . ? N1 C2 H2A 111.1 . . ? C1 C2 H2B 111.1 . . ? N1 C2 H2B 111.2 . . ? H2A C2 H2B 109.1 . . ? N1 C3 P2 105.62(14) . . ? N1 C3 H3A 110.6 . . ? P2 C3 H3A 110.5 . . ? N1 C3 H3B 110.7 . . ? P2 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? C3 N1 C4 106.03(17) . . ? C3 N1 C2 118.84(14) . . ? C4 N1 C2 110.72(15) . . ? C3 N1 H1 106.9 . . ? C4 N1 H1 106.9 . . ? C2 N1 H1 106.8 . . ? N1 C4 P1 111.42(12) . . ? N1 C4 H4A 109.2 . . ? P1 C4 H4A 109.3 . . ? N1 C4 H4B 109.4 . . ? P1 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Gd1 O2 C1 -18.88(15) 8_556 . . . ? O8 Gd1 O2 C1 125.95(14) 1_455 . . . ? O5 Gd1 O2 C1 170.74(14) 1_455 . . . ? O4 Gd1 O2 C1 89.52(13) 6_755 . . . ? O1W Gd1 O2 C1 -110.58(13) . . . . ? O1 Gd1 O2 C1 -6.40(11) . . . . ? O7 Gd1 O2 C1 -85.25(13) 6_765 . . . ? Gd1 O2 C1 O1 10.60(18) . . . . ? Gd1 O2 C1 C2 162.51(15) . . . . ? O6 Gd1 C1 O2 164.17(13) 8_556 . . . ? O8 Gd1 C1 O2 -100.39(16) 1_455 . . . ? O5 Gd1 C1 O2 -9.41(14) 1_455 . . . ? O4 Gd1 C1 O2 -84.22(13) 6_755 . . . ? O1W Gd1 C1 O2 89.37(14) . . . . ? O1 Gd1 C1 O2 168.3(2) . . . . ? O7 Gd1 C1 O2 85.02(13) 6_765 . . . ? O6 Gd1 C1 O1 -4.09(12) 8_556 . . . ? O8 Gd1 C1 O1 91.35(14) 1_455 . . . ? O5 Gd1 C1 O1 -177.67(11) 1_455 . . . ? O4 Gd1 C1 O1 107.52(12) 6_755 . . . ? O1W Gd1 C1 O1 -78.89(14) . . . . ? O2 Gd1 C1 O1 -168.3(2) . . . . ? O7 Gd1 C1 O1 -83.24(11) 6_765 . . . ? O6 Gd1 C1 C2 78.9(5) 8_556 . . . ? O8 Gd1 C1 C2 174.4(5) 1_455 . . . ? O5 Gd1 C1 C2 -94.7(5) 1_455 . . . ? O4 Gd1 C1 C2 -169.5(5) 6_755 . . . ? O1W Gd1 C1 C2 4.1(5) . . . . ? O1 Gd1 C1 C2 83.0(5) . . . . ? O2 Gd1 C1 C2 -85.3(5) . . . . ? O7 Gd1 C1 C2 -0.2(5) 6_765 . . . ? O5 P1 O4 Gd1 111.66(11) . . . 6_765 ? O3 P1 O4 Gd1 -137.52(9) . . . 6_765 ? C4 P1 O4 Gd1 -14.22(16) . . . 6_765 ? O8 P2 O6 Gd1 57.44(18) . . . 8_656 ? O7 P2 O6 Gd1 -79.43(17) . . . 8_656 ? C3 P2 O6 Gd1 166.36(17) . . . 8_656 ? O7 P2 O8 Gd1 -119.0(2) . . . 1_655 ? O6 P2 O8 Gd1 105.7(3) . . . 1_655 ? C3 P2 O8 Gd1 -8.7(3) . . . 1_655 ? O2 C1 O1 Gd1 -10.66(18) . . . . ? C2 C1 O1 Gd1 -162.61(17) . . . . ? O6 Gd1 O1 C1 175.91(12) 8_556 . . . ? O8 Gd1 O1 C1 -130.58(12) 1_455 . . . ? O5 Gd1 O1 C1 2.85(14) 1_455 . . . ? O4 Gd1 O1 C1 -68.45(11) 6_755 . . . ? O1W Gd1 O1 C1 118.90(12) . . . . ? O2 Gd1 O1 C1 6.40(11) . . . . ? O7 Gd1 O1 C1 86.87(11) 6_765 . . . ? O8 P2 O7 Gd1 18.87(13) . . . 6_755 ? O6 P2 O7 Gd1 155.35(9) . . . 6_755 ? C3 P2 O7 Gd1 -88.18(12) . . . 6_755 ? O4 P1 O5 Gd1 -76.42(15) . . . 1_655 ? O3 P1 O5 Gd1 173.09(13) . . . 1_655 ? C4 P1 O5 Gd1 54.78(15) . . . 1_655 ? O2 C1 C2 N1 -152.98(19) . . . . ? O1 C1 C2 N1 -3.2(2) . . . . ? Gd1 C1 C2 N1 -77.0(5) . . . . ? O8 P2 C3 N1 114.00(15) . . . . ? O7 P2 C3 N1 -126.05(14) . . . . ? O6 P2 C3 N1 -6.25(17) . . . . ? P2 C3 N1 C4 -77.37(15) . . . . ? P2 C3 N1 C2 157.29(15) . . . . ? C1 C2 N1 C3 -112.04(19) . . . . ? C1 C2 N1 C4 124.91(17) . . . . ? C3 N1 C4 P1 -56.42(17) . . . . ? C2 N1 C4 P1 73.76(18) . . . . ? O5 P1 C4 N1 74.52(16) . . . . ? O4 P1 C4 N1 -160.77(12) . . . . ? O3 P1 C4 N1 -40.41(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.72 2.514(2) 161.3 2_566 data_08 _database_code_depnum_ccdc_archive 'CCDC 705167' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '02 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 N O9 P2 Tb' _chemical_formula_sum 'C4 H10 N O9 P2 Tb' _chemical_formula_weight 436.99 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source TB 25.89760 2.24256 18.21850 0.19614 14.31670 12.66480 2.95354 115.36200 3.58224 -0.59100 4.15100 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.09000 0.09500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.00800 0.00600 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.00200 0.00200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.00400 0.00300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.6686(17) _cell_length_b 10.1018(18) _cell_length_c 20.359(4) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 1988.5(6) _exptl_crystal_density_diffrn 2.919 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Hilgenberg borosilicate glass capillary (ca. 0.4 mm of diameter) ; #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; MAR 345 Imaging Plate instrument belonging to the Swiss-Norwegian BM01a beam line (bending magnet source) at the European Synchrotron Radiation Facility (ESRF), Grenoble, France. ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source Synchrotron _diffrn_radiation_type X-ray _diffrn_radiation_monochromator 0.71013(1) _diffrn_measurement_method Debye-Scherrer _diffrn_detector 'Imaging Plate' _diffrn_detector_type 'MAR 345' _pd_meas_scan_method cont _pd_meas_special_details ; The powdered sample was slowly spun 180 degrees (in phi scanning mode) during data collection to improve powder averaging. Two-dimensional powder data was collected using a MAR2300 imaging plate detector and then integrated using the software Fit2D. The monochromatic wavelength (0.71013 A) and sample-to-detector distance (d of about 150 mm) were calibrated from an individual run using the standard LaB6. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 1257 _pd_meas_2theta_range_min 2.00000 _pd_meas_2theta_range_max 47.01253 _pd_meas_2theta_range_inc 0.035838 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Gaussian _pd_proc_ls_background_function 'Fixed points' _pd_proc_ls_pref_orient_corr ; None ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 6.1393 _pd_proc_ls_prof_wR_factor 7.7314 _pd_proc_ls_prof_wR_expected 1.5700 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 13.4505 _pd_proc_ls_prof_cwR_factor 14.7171 _pd_proc_ls_prof_cwR_expected 2.9886 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 24.2491 _pd_proc_ls_prof_echi2 24.2491 # Items related to LS refinement _refine_ls_R_I_factor 11.0170 _refine_ls_number_reflns 1917 _refine_ls_number_parameters 60 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0606 _pd_proc_2theta_range_max 47.0732 _pd_proc_2theta_range_inc 0.035838 _pd_proc_wavelength 0.710130 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol TB1 0.3637(4) 0.5420(4) 0.3367(2) 0.01267 1.00000 Uiso TB P1 1.0895(8) 0.7259(8) 0.4156(4) 0.01267 1.00000 Uiso P P2 1.0283(8) 0.3889(8) 0.3118(4) 0.01267 1.00000 Uiso P O2 0.5323(7) 0.614(4) 0.4250(9) 0.01267 1.00000 Uiso O C1 0.63979(10) 0.5733(4) 0.39840(14) 0.01267 1.00000 Uiso C O4 1.154(2) 0.8635(8) 0.4101(12) 0.01267 1.00000 Uiso O O6 0.9467(17) 0.4456(17) 0.2547(11) 0.01267 1.00000 Uiso O O8 1.1790(11) 0.4307(17) 0.3072(13) 0.01267 1.00000 Uiso O O1 0.6217(12) 0.487(2) 0.3557(12) 0.01267 1.00000 Uiso O O7 1.0153(18) 0.2394(10) 0.3131(14) 0.01267 1.00000 Uiso O O5 1.2019(19) 0.6214(11) 0.4104(11) 0.01267 1.00000 Uiso O O1W 0.246(5) 0.696(5) 0.258(2) 0.01267 0.88(4) Uiso O O3 1.018(2) 0.7130(14) 0.4823(10) 0.01267 1.00000 Uiso O H3 1.03646 0.77916 0.50572 0.01267 1.00000 Uiso H C2 0.77689(19) 0.5840(7) 0.4335(3) 0.01267 1.00000 Uiso C H2A 0.78277 0.67983 0.44998 0.01267 1.00000 Uiso H H2B 0.78278 0.52705 0.46465 0.01267 1.00000 Uiso H C3 0.981(2) 0.4636(19) 0.3897(5) 0.01267 1.00000 Uiso C H3A 0.93238 0.39480 0.41838 0.01267 1.00000 Uiso H H3B 1.05324 0.49698 0.41371 0.01267 1.00000 Uiso H N1 0.87062 0.57009 0.37176 0.01267 1.00000 Uiso N H1 0.82172 0.54530 0.33621 0.01267 1.00000 Uiso H C4 0.9434(18) 0.7046(15) 0.3599(10) 0.01267 1.00000 Uiso C H4A 0.88486 0.77388 0.36101 0.01267 1.00000 Uiso H H4B 0.98432 0.69942 0.31385 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Tb1 O8 2.193(2) 1_455 ? Tb1 O6 2.249(2) 8_556 ? Tb1 O5 2.310(2) 1_455 ? Tb1 O4 2.351(2) 6_755 ? Tb1 O7 2.358(2) 6_765 ? Tb1 O1W 2.499(2) . ? Tb1 O2 2.535(2) . ? Tb1 O1 2.589(3) . ? Tb1 C1 2.973(4) . ? P1 O5 1.517(3) . ? P1 O4 1.530(2) . ? P1 O3 1.530(2) . ? P1 C4 1.825(3) . ? P2 O7 1.522(2) . ? P2 O6 1.515(2) . ? P2 O8 1.520(2) . ? P2 C3 1.816(3) . ? O2 C1 1.237(5) . ? C1 O1 1.247(3) . ? C1 C2 1.504(5) . ? O4 Tb1 2.351(2) 6_765 ? O6 Tb1 2.249(2) 8_656 ? O8 Tb1 2.193(2) 1_655 ? O7 Tb1 2.358(2) 6_755 ? O5 Tb1 2.310(2) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.549(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.554(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.546(4) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O8 Tb1 O6 80.95(8) 1_455 8_556 ? O8 Tb1 O5 78.63(8) 1_455 1_455 ? O6 Tb1 O5 158.24(8) 8_556 1_455 ? O8 Tb1 O4 73.75(7) 1_455 6_755 ? O6 Tb1 O4 102.74(9) 8_556 6_755 ? O5 Tb1 O4 78.66(8) 1_455 6_755 ? O8 Tb1 O7 141.28(8) 1_455 6_765 ? O6 Tb1 O7 91.10(8) 8_556 6_765 ? O5 Tb1 O7 100.15(8) 1_455 6_765 ? O4 Tb1 O7 144.58(9) 6_755 6_765 ? O8 Tb1 O1W 76.85(8) 1_455 . ? O6 Tb1 O1W 84.47(9) 8_556 . ? O5 Tb1 O1W 83.65(8) 1_455 . ? O4 Tb1 O1W 148.07(8) 6_755 . ? O7 Tb1 O1W 64.65(8) 6_765 . ? O8 Tb1 O2 149.80(8) 1_455 . ? O6 Tb1 O2 118.76(9) 8_556 . ? O5 Tb1 O2 82.96(7) 1_455 . ? O4 Tb1 O2 79.32(7) 6_755 . ? O7 Tb1 O2 65.50(8) 6_765 . ? O1W Tb1 O2 124.72(8) . . ? O8 Tb1 O1 135.90(7) 1_455 . ? O6 Tb1 O1 71.80(7) 8_556 . ? O5 Tb1 O1 129.10(7) 1_455 . ? O4 Tb1 O1 79.19(8) 6_755 . ? O7 Tb1 O1 74.43(8) 6_765 . ? O1W Tb1 O1 131.93(7) . . ? O2 Tb1 O1 48.10(7) . . ? O8 Tb1 C1 154.60(7) 1_455 . ? O6 Tb1 C1 94.45(9) 8_556 . ? O5 Tb1 C1 107.23(9) 1_455 . ? O4 Tb1 C1 83.08(8) 6_755 . ? O7 Tb1 C1 63.24(8) 6_765 . ? O1W Tb1 C1 127.84(8) . . ? O2 Tb1 C1 24.32(9) . . ? O1 Tb1 C1 24.69(7) . . ? O5 P1 O4 109.39(12) . . ? O5 P1 O3 109.36(12) . . ? O4 P1 O3 108.87(13) . . ? O5 P1 C4 115.21(13) . . ? O4 P1 C4 112.41(14) . . ? O3 P1 C4 101.14(14) . . ? O7 P2 O6 110.14(14) . . ? O7 P2 O8 110.90(12) . . ? O6 P2 O8 110.39(14) . . ? O7 P2 C3 112.31(16) . . ? O6 P2 C3 112.36(13) . . ? O8 P2 C3 100.42(16) . . ? C1 O2 Tb1 98.1(2) . . ? O1 C1 O2 114.5(4) . . ? O1 C1 C2 119.7(3) . . ? O2 C1 C2 121.1(3) . . ? O1 C1 Tb1 60.2(2) . . ? O2 C1 Tb1 57.58(19) . . ? C2 C1 Tb1 176.4(2) . . ? P1 O4 Tb1 135.45(15) . 6_765 ? P2 O6 Tb1 169.46(14) . 8_656 ? P2 O8 Tb1 155.05(15) . 1_655 ? C1 O1 Tb1 95.1(2) . . ? P2 O7 Tb1 143.42(14) . 6_755 ? P1 O5 Tb1 140.62(14) . 1_655 ? P1 O3 H3 109.7 . . ? C1 C2 N1 97.5(3) . . ? C1 C2 H2A 112.4 . . ? N1 C2 H2A 112.5 . . ? C1 C2 H2B 111.9 . . ? N1 C2 H2B 112.2 . . ? H2A C2 H2B 109.9 . . ? N1 C3 P2 104.96(19) . . ? N1 C3 H3A 110.9 . . ? P2 C3 H3A 110.8 . . ? N1 C3 H3B 110.7 . . ? P2 C3 H3B 110.7 . . ? H3A C3 H3B 108.9 . . ? C4 N1 C2 108.5(2) . . ? C4 N1 C3 109.4(3) . . ? C2 N1 C3 105.7(2) . . ? C4 N1 H1 111.1 . . ? C2 N1 H1 111.0 . . ? C3 N1 H1 111.0 . . ? N1 C4 P1 111.0(2) . . ? N1 C4 H4A 109.3 . . ? P1 C4 H4A 109.4 . . ? N1 C4 H4B 109.6 . . ? P1 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Tb1 O2 C1 124.0(2) 1_455 . . . ? O6 Tb1 O2 C1 -1.9(2) 8_556 . . . ? O5 Tb1 O2 C1 176.58(19) 1_455 . . . ? O4 Tb1 O2 C1 96.85(18) 6_755 . . . ? O7 Tb1 O2 C1 -78.86(19) 6_765 . . . ? O1W Tb1 O2 C1 -106.20(18) . . . . ? O1 Tb1 O2 C1 11.86(16) . . . . ? Tb1 O2 C1 O1 -20.4(3) . . . . ? Tb1 O2 C1 C2 -176.1(2) . . . . ? O8 Tb1 C1 O1 55.1(3) 1_455 . . . ? O6 Tb1 C1 O1 -23.17(18) 8_556 . . . ? O5 Tb1 C1 O1 154.97(18) 1_455 . . . ? O4 Tb1 C1 O1 79.16(19) 6_755 . . . ? O7 Tb1 C1 O1 -112.15(19) 6_765 . . . ? O1W Tb1 C1 O1 -109.62(18) . . . . ? O2 Tb1 C1 O1 158.5(3) . . . . ? O8 Tb1 C1 O2 -103.5(3) 1_455 . . . ? O6 Tb1 C1 O2 178.31(18) 8_556 . . . ? O5 Tb1 C1 O2 -3.6(2) 1_455 . . . ? O4 Tb1 C1 O2 -79.37(18) 6_755 . . . ? O7 Tb1 C1 O2 89.32(18) 6_765 . . . ? O1W Tb1 C1 O2 91.9(2) . . . . ? O1 Tb1 C1 O2 -158.5(3) . . . . ? O8 Tb1 C1 C2 -34(4) 1_455 . . . ? O6 Tb1 C1 C2 -112(3) 8_556 . . . ? O5 Tb1 C1 C2 66(3) 1_455 . . . ? O4 Tb1 C1 C2 -10(3) 6_755 . . . ? O7 Tb1 C1 C2 159(3) 6_765 . . . ? O1W Tb1 C1 C2 162(3) . . . . ? O2 Tb1 C1 C2 70(3) . . . . ? O1 Tb1 C1 C2 -89(3) . . . . ? O5 P1 O4 Tb1 117.34(19) . . . 6_765 ? O3 P1 O4 Tb1 -123.20(19) . . . 6_765 ? C4 P1 O4 Tb1 -12.0(3) . . . 6_765 ? O7 P2 O6 Tb1 -116.8(8) . . . 8_656 ? O8 P2 O6 Tb1 6.0(9) . . . 8_656 ? C3 P2 O6 Tb1 117.2(8) . . . 8_656 ? O7 P2 O8 Tb1 -129.3(3) . . . 1_655 ? O6 P2 O8 Tb1 108.4(3) . . . 1_655 ? C3 P2 O8 Tb1 -10.4(3) . . . 1_655 ? O2 C1 O1 Tb1 19.9(3) . . . . ? C2 C1 O1 Tb1 175.9(2) . . . . ? O8 Tb1 O1 C1 -149.65(19) 1_455 . . . ? O6 Tb1 O1 C1 155.61(19) 8_556 . . . ? O5 Tb1 O1 C1 -31.4(2) 1_455 . . . ? O4 Tb1 O1 C1 -96.98(19) 6_755 . . . ? O7 Tb1 O1 C1 59.15(17) 6_765 . . . ? O1W Tb1 O1 C1 91.2(2) . . . . ? O2 Tb1 O1 C1 -11.69(18) . . . . ? O6 P2 O7 Tb1 144.6(2) . . . 6_755 ? O8 P2 O7 Tb1 22.2(3) . . . 6_755 ? C3 P2 O7 Tb1 -89.3(3) . . . 6_755 ? O4 P1 O5 Tb1 -63.6(3) . . . 1_655 ? O3 P1 O5 Tb1 177.25(19) . . . 1_655 ? C4 P1 O5 Tb1 64.2(3) . . . 1_655 ? O1 C1 C2 N1 44.8(3) . . . . ? O2 C1 C2 N1 -160.8(3) . . . . ? Tb1 C1 C2 N1 132(3) . . . . ? O7 P2 C3 N1 -127.1(2) . . . . ? O6 P2 C3 N1 -2.3(3) . . . . ? O8 P2 C3 N1 115.0(2) . . . . ? C1 C2 N1 C4 111.4(3) . . . . ? C1 C2 N1 C3 -131.4(2) . . . . ? P2 C3 N1 C4 -91.5(3) . . . . ? P2 C3 N1 C2 151.8(2) . . . . ? C2 N1 C4 P1 78.6(3) . . . . ? C3 N1 C4 P1 -36.3(3) . . . . ? O5 P1 C4 N1 59.9(3) . . . . ? O4 P1 C4 N1 -173.8(2) . . . . ? O3 P1 C4 N1 -57.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.80 2.575(3) 158.1 2_566 data_09 _database_code_depnum_ccdc_archive 'CCDC 705168' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '02 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Dy N O9 P2' _chemical_formula_sum 'C4 H10 Dy N O9 P2' _chemical_formula_weight 440.57 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source DY 26.50700 2.18020 17.63830 0.20217 14.55960 12.18990 2.96577 111.87400 4.29728 -10.42300 9.74800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.28300 0.43400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.7725(10) _cell_length_b 10.2143(11) _cell_length_c 20.6600(18) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2062.3(4) _exptl_crystal_density_diffrn 2.838 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Glass slide ; _pd_spec_mount_mode Reflection _pd_spec_shape 'Flat sheet' #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; Conventional powder diffractometer instrument belonging to the University of Aveiro and located at the Central Analytical Laboratory ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source 'X-ray tube' _diffrn_radiation_type X-ray _diffrn_source_target Cu _diffrn_radiation_monochromator None _diffrn_measurement_method Bragg-Brentano _diffrn_detector_type 'X Celerator detector' _pd_meas_scan_method cont _pd_meas_special_details ; Data were collected in a continuous mode over the angular range 4-110. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 8578 _pd_meas_2theta_range_min 4.00000 _pd_meas_2theta_range_max 90.00158 _pd_meas_2theta_range_inc 0.010027 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function 'Fixed Points' _pd_proc_ls_pref_orient_corr ; Modified March's function along the [002] vector. G1 refined to about 0.694(2) which is consistent with the platy crystal habit of the material (as revealed by SEM pictures). ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 1.6392 _pd_proc_ls_prof_wR_factor 2.2773 _pd_proc_ls_prof_wR_expected 0.7450 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 20.5880 _pd_proc_ls_prof_cwR_factor 15.6468 _pd_proc_ls_prof_cwR_expected 5.1190 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 9.3428 _pd_proc_ls_prof_echi2 9.4314 # Items related to LS refinement _refine_ls_R_I_factor 10.1911 _refine_ls_number_reflns 1936 _refine_ls_number_parameters 64 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 3.9377 _pd_proc_2theta_range_max 89.9393 _pd_proc_2theta_range_inc 0.010027 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol DY1 0.3666(3) 0.5409(3) 0.33719(10) 0.01267 1.00000 Uiso DY P1 1.0945(7) 0.7317(7) 0.4163(3) 0.01267 1.00000 Uiso P P2 1.0248(7) 0.4054(7) 0.3056(3) 0.01267 1.00000 Uiso P O2 0.53221(10) 0.6061(19) 0.4319(7) 0.01267 1.00000 Uiso O C1 0.63836(9) 0.5662(11) 0.4056(3) 0.01267 1.00000 Uiso C O4 1.1431(17) 0.8778(7) 0.4212(7) 0.01267 1.00000 Uiso O O6 0.9275(12) 0.4760(12) 0.2594(7) 0.01267 1.00000 Uiso O O8 1.1649(9) 0.4555(13) 0.3056(7) 0.01267 1.00000 Uiso O O1 0.6293(3) 0.5077(17) 0.3532(5) 0.01267 1.00000 Uiso O O7 1.0084(14) 0.2593(6) 0.2985(8) 0.01267 1.00000 Uiso O O5 1.2258(13) 0.6465(11) 0.4135(8) 0.01267 1.00000 Uiso O O1W 0.248(3) 0.650(3) 0.2458(9) 0.01267 1.00000 Uiso O O3 1.0330(16) 0.7031(12) 0.4867(6) 0.01267 1.00000 Uiso O H3 1.04580 0.78925 0.50341 0.01267 1.00000 Uiso H C2 0.77679(9) 0.6042(14) 0.4321(4) 0.01267 1.00000 Uiso C H2A 0.78071 0.69221 0.44436 0.01267 1.00000 Uiso H H2B 0.79443 0.54396 0.46798 0.01267 1.00000 Uiso H C3 0.970(2) 0.4542(16) 0.3866(5) 0.01267 1.00000 Uiso C H3A 0.90893 0.38016 0.40859 0.01267 1.00000 Uiso H H3B 1.03984 0.47084 0.41275 0.01267 1.00000 Uiso H N1 0.8737(11) 0.5735(8) 0.3740(5) 0.01267 1.00000 Uiso N H1 0.81554 0.55048 0.33733 0.01267 1.00000 Uiso H C4 0.9679(16) 0.6909(15) 0.3553(6) 0.01267 1.00000 Uiso C H4A 0.90118 0.76712 0.34657 0.01267 1.00000 Uiso H H4B 1.00414 0.67326 0.31064 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Dy1 O6 2.189(8) 8_556 ? Dy1 O8 2.255(9) 1_455 ? Dy1 O5 2.358(10) 1_455 ? Dy1 O4 2.412(7) 6_755 ? Dy1 O1W 2.482(9) . ? Dy1 O1 2.613(12) . ? Dy1 O2 2.627(8) . ? Dy1 O7 2.670(8) 6_765 ? Dy1 C1 3.015(14) . ? P1 O5 1.546(12) . ? P1 O4 1.563(9) . ? P1 O3 1.598(8) . ? P1 C4 1.821(11) . ? P2 O8 1.460(9) . ? P2 O7 1.503(10) . ? P2 O6 1.522(8) . ? P2 C3 1.825(12) . ? O2 C1 1.229(16) . ? C1 O1 1.241(11) . ? C1 C2 1.510(19) . ? O4 Dy1 2.412(7) 6_765 ? O6 Dy1 2.189(8) 8_656 ? O8 Dy1 2.255(9) 1_655 ? O7 Dy1 2.670(8) 6_755 ? O5 Dy1 2.358(9) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.566(17) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.561(17) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.554(14) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O6 Dy1 O8 81.9(2) 8_556 1_455 ? O6 Dy1 O5 155.5(3) 8_556 1_455 ? O8 Dy1 O5 81.9(3) 1_455 1_455 ? O6 Dy1 O4 117.3(2) 8_556 6_755 ? O8 Dy1 O4 84.7(3) 1_455 6_755 ? O5 Dy1 O4 79.3(3) 1_455 6_755 ? O6 Dy1 O1W 64.4(3) 8_556 . ? O8 Dy1 O1W 63.0(3) 1_455 . ? O5 Dy1 O1W 91.8(3) 1_455 . ? O4 Dy1 O1W 147.6(4) 6_755 . ? O6 Dy1 O1 78.9(2) 8_556 . ? O8 Dy1 O1 148.1(2) 1_455 . ? O5 Dy1 O1 123.2(3) 1_455 . ? O4 Dy1 O1 81.6(3) 6_755 . ? O1W Dy1 O1 127.8(3) . . ? O6 Dy1 O2 126.0(3) 8_556 . ? O8 Dy1 O2 148.5(3) 1_455 . ? O5 Dy1 O2 75.2(3) 1_455 . ? O4 Dy1 O2 70.1(3) 6_755 . ? O1W Dy1 O2 137.9(3) . . ? O1 Dy1 O2 48.0(3) . . ? O6 Dy1 O7 81.6(2) 8_556 6_765 ? O8 Dy1 O7 129.7(3) 1_455 6_765 ? O5 Dy1 O7 94.8(3) 1_455 6_765 ? O4 Dy1 O7 144.2(3) 6_755 6_765 ? O1W Dy1 O7 67.0(3) . 6_765 ? O1 Dy1 O7 72.2(3) . 6_765 ? O2 Dy1 O7 74.3(3) . 6_765 ? O6 Dy1 C1 102.4(3) 8_556 . ? O8 Dy1 C1 160.0(3) 1_455 . ? O5 Dy1 C1 99.1(3) 1_455 . ? O4 Dy1 C1 75.9(4) 6_755 . ? O1W Dy1 C1 136.6(4) . . ? O1 Dy1 C1 24.2(3) . . ? O2 Dy1 C1 23.9(3) . . ? O7 Dy1 C1 70.2(3) 6_765 . ? O5 P1 O4 106.7(6) . . ? O5 P1 O3 104.0(5) . . ? O4 P1 O3 103.0(6) . . ? O5 P1 C4 114.5(6) . . ? O4 P1 C4 117.9(6) . . ? O3 P1 C4 109.2(6) . . ? O8 P2 O7 116.7(5) . . ? O8 P2 O6 114.5(5) . . ? O7 P2 O6 110.2(5) . . ? O8 P2 C3 100.2(6) . . ? O7 P2 C3 108.8(6) . . ? O6 P2 C3 105.1(5) . . ? C1 O2 Dy1 96.0(8) . . ? O2 C1 O1 119.3(13) . . ? O2 C1 C2 120.8(9) . . ? O1 C1 C2 119.6(13) . . ? O2 C1 Dy1 60.1(7) . . ? O1 C1 Dy1 59.5(8) . . ? C2 C1 Dy1 168.9(9) . . ? P1 O4 Dy1 127.0(5) . 6_765 ? P2 O6 Dy1 152.0(5) . 8_656 ? P2 O8 Dy1 163.1(5) . 1_655 ? C1 O1 Dy1 96.4(9) . . ? P2 O7 Dy1 138.7(6) . 6_755 ? P1 O5 Dy1 139.8(5) . 1_655 ? P1 O3 H3 109.5 . . ? C1 C2 N1 102.6(10) . . ? C1 C2 H2A 111.5 . . ? N1 C2 H2A 111.1 . . ? C1 C2 H2B 110.9 . . ? N1 C2 H2B 111.4 . . ? H2A C2 H2B 109.2 . . ? N1 C3 P2 103.5(8) . . ? N1 C3 H3A 111.1 . . ? P2 C3 H3A 111.2 . . ? N1 C3 H3B 110.9 . . ? P2 C3 H3B 111.1 . . ? H3A C3 H3B 109.0 . . ? C3 N1 C4 107.3(12) . . ? C3 N1 C2 113.3(10) . . ? C4 N1 C2 112.8(8) . . ? C3 N1 H1 107.8 . . ? C4 N1 H1 107.7 . . ? C2 N1 H1 107.7 . . ? N1 C4 P1 114.0(8) . . ? N1 C4 H4A 109.2 . . ? P1 C4 H4A 108.8 . . ? N1 C4 H4B 108.5 . . ? P1 C4 H4B 108.5 . . ? H4A C4 H4B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Dy1 O2 C1 -9.7(9) 8_556 . . . ? O8 Dy1 O2 C1 139.1(7) 1_455 . . . ? O5 Dy1 O2 C1 -176.1(8) 1_455 . . . ? O4 Dy1 O2 C1 100.1(8) 6_755 . . . ? O1W Dy1 O2 C1 -100.1(9) . . . . ? O1 Dy1 O2 C1 3.3(7) . . . . ? O7 Dy1 O2 C1 -76.7(8) 6_765 . . . ? Dy1 O2 C1 O1 -6.0(12) . . . . ? Dy1 O2 C1 C2 167.1(10) . . . . ? O6 Dy1 C1 O2 172.0(8) 8_556 . . . ? O8 Dy1 C1 O2 -87.5(11) 1_455 . . . ? O5 Dy1 C1 O2 3.8(8) 1_455 . . . ? O4 Dy1 C1 O2 -72.7(8) 6_755 . . . ? O1W Dy1 C1 O2 106.3(9) . . . . ? O1 Dy1 C1 O2 -173.9(12) . . . . ? O7 Dy1 C1 O2 95.7(8) 6_765 . . . ? O6 Dy1 C1 O1 -14.1(6) 8_556 . . . ? O8 Dy1 C1 O1 86.4(11) 1_455 . . . ? O5 Dy1 C1 O1 177.7(6) 1_455 . . . ? O4 Dy1 C1 O1 101.2(6) 6_755 . . . ? O1W Dy1 C1 O1 -79.8(7) . . . . ? O2 Dy1 C1 O1 173.9(12) . . . . ? O7 Dy1 C1 O1 -90.4(7) 6_765 . . . ? O6 Dy1 C1 C2 74(5) 8_556 . . . ? O8 Dy1 C1 C2 175(4) 1_455 . . . ? O5 Dy1 C1 C2 -94(4) 1_455 . . . ? O4 Dy1 C1 C2 -170(5) 6_755 . . . ? O1W Dy1 C1 C2 9(5) . . . . ? O1 Dy1 C1 C2 88(5) . . . . ? O2 Dy1 C1 C2 -98(4) . . . . ? O7 Dy1 C1 C2 -2(4) 6_765 . . . ? O5 P1 O4 Dy1 106.7(7) . . . 6_765 ? O3 P1 O4 Dy1 -144.2(6) . . . 6_765 ? C4 P1 O4 Dy1 -23.9(12) . . . 6_765 ? O8 P2 O6 Dy1 59.9(9) . . . 8_656 ? O7 P2 O6 Dy1 -74.0(9) . . . 8_656 ? C3 P2 O6 Dy1 168.9(9) . . . 8_656 ? O7 P2 O8 Dy1 -106.4(17) . . . 1_655 ? O6 P2 O8 Dy1 122.7(18) . . . 1_655 ? C3 P2 O8 Dy1 10.7(18) . . . 1_655 ? O2 C1 O1 Dy1 6.0(12) . . . . ? C2 C1 O1 Dy1 -167.2(10) . . . . ? O6 Dy1 O1 C1 165.9(6) 8_556 . . . ? O8 Dy1 O1 C1 -139.8(6) 1_455 . . . ? O5 Dy1 O1 C1 -2.7(7) 1_455 . . . ? O4 Dy1 O1 C1 -74.0(6) 6_755 . . . ? O1W Dy1 O1 C1 121.1(6) . . . . ? O2 Dy1 O1 C1 -3.3(7) . . . . ? O7 Dy1 O1 C1 81.3(7) 6_765 . . . ? O8 P2 O7 Dy1 36.7(10) . . . 6_755 ? O6 P2 O7 Dy1 169.6(6) . . . 6_755 ? C3 P2 O7 Dy1 -75.6(9) . . . 6_755 ? O4 P1 O5 Dy1 -98.1(8) . . . 1_655 ? O3 P1 O5 Dy1 153.4(8) . . . 1_655 ? C4 P1 O5 Dy1 34.3(10) . . . 1_655 ? O2 C1 C2 N1 -163.3(13) . . . . ? O1 C1 C2 N1 9.9(14) . . . . ? Dy1 C1 C2 N1 -72(5) . . . . ? O8 P2 C3 N1 104.7(9) . . . . ? O7 P2 C3 N1 -132.3(8) . . . . ? O6 P2 C3 N1 -14.3(9) . . . . ? P2 C3 N1 C4 -73.8(9) . . . . ? P2 C3 N1 C2 161.0(8) . . . . ? C1 C2 N1 C3 -110.7(13) . . . . ? C1 C2 N1 C4 127.2(10) . . . . ? C3 N1 C4 P1 -57.6(11) . . . . ? C2 N1 C4 P1 67.9(14) . . . . ? O5 P1 C4 N1 82.4(10) . . . . ? O4 P1 C4 N1 -150.7(7) . . . . ? O3 P1 C4 N1 -33.7(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.77 2.578(14) 168.7 2_566 data_10 _database_code_depnum_ccdc_archive 'CCDC 705169' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '02 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Ho N O9 P2' _chemical_formula_sum 'C4 H10 Ho N O9 P2' _chemical_formula_weight 443.00 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source HO 26.90490 2.07051 17.29400 0.19794 14.55830 11.44070 3.63837 92.65660 4.56796 -12.25500 3.70400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.28300 0.43400 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.04700 0.03200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.01700 0.00900 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.02900 0.01800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.7409(6) _cell_length_b 10.1812(6) _cell_length_c 20.6262(13) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 2045.6(2) _exptl_crystal_density_diffrn 2.877 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Glass slide ; _pd_spec_mount_mode Reflection _pd_spec_shape 'Flat sheet' #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; Conventional powder diffractometer instrument belonging to the University of Aveiro and located at the Central Analytical Laboratory ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source 'X-ray tube' _diffrn_radiation_type X-ray _diffrn_source_target Cu _diffrn_radiation_monochromator None _diffrn_measurement_method Bragg-Brentano _diffrn_detector_type 'X Celerator detector' _pd_meas_scan_method cont _pd_meas_special_details ; Data were collected in a continuous mode over the angular range 4-110. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 9575 _pd_meas_2theta_range_min 4.00000 _pd_meas_2theta_range_max 99.99850 _pd_meas_2theta_range_inc 0.010027 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Pseudo-Voigt _pd_proc_ls_background_function 'Fixed Points' _pd_proc_ls_pref_orient_corr ; Modified March's function along the [002] vector. G1 refined to about 0.962(2) which is consistent with the platy crystal habit of the material (as revealed by SEM pictures). ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 3.3793 _pd_proc_ls_prof_wR_factor 4.5721 _pd_proc_ls_prof_wR_expected 0.8402 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 18.3812 _pd_proc_ls_prof_cwR_factor 15.8326 _pd_proc_ls_prof_cwR_expected 2.9095 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 29.6115 _pd_proc_ls_prof_echi2 30.2376 # Items related to LS refinement _refine_ls_R_I_factor 11.9288 _refine_ls_number_reflns 2289 _refine_ls_number_parameters 64 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 4.0575 _pd_proc_2theta_range_max 100.0560 _pd_proc_2theta_range_inc 0.010027 _pd_proc_wavelength 1.540560 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol HO1 0.3633(2) 0.5432(2) 0.33517(10) 0.01267 1.00000 Uiso HO P1 1.0958(7) 0.7262(6) 0.4116(3) 0.01267 1.00000 Uiso P P2 1.0272(6) 0.3870(6) 0.3021(3) 0.01267 1.00000 Uiso P O2 0.53078(11) 0.6022(13) 0.4373(3) 0.01267 1.00000 Uiso O C1 0.63544(8) 0.5764(7) 0.40557(19) 0.01267 1.00000 Uiso C O4 1.1339(15) 0.8705(6) 0.4021(6) 0.01267 1.00000 Uiso O O6 0.9238(10) 0.4573(10) 0.2607(7) 0.01267 1.00000 Uiso O O8 1.1654(8) 0.4381(11) 0.3053(7) 0.01267 1.00000 Uiso O O1 0.6210(3) 0.5127(12) 0.3548(4) 0.01267 1.00000 Uiso O O7 1.0041(12) 0.2429(6) 0.3037(7) 0.01267 1.00000 Uiso O O5 1.2102(12) 0.6295(9) 0.4027(7) 0.01267 1.00000 Uiso O O1W 0.2576(18) 0.6883(18) 0.2472(7) 0.01267 1.00000 Uiso O O3 1.0262(15) 0.7088(10) 0.4772(6) 0.01267 1.00000 Uiso O H3 1.03552 0.77593 0.49941 0.01267 1.00000 Uiso H C2 0.77609(10) 0.5944(12) 0.4350(3) 0.01267 1.00000 Uiso C H2A 0.77789 0.69609 0.44780 0.01267 1.00000 Uiso H H2B 0.79628 0.55315 0.47466 0.01267 1.00000 Uiso H C3 0.9659(18) 0.4431(13) 0.3814(5) 0.01267 1.00000 Uiso C H3A 0.91132 0.37679 0.40224 0.01267 1.00000 Uiso H H3B 1.03911 0.46641 0.40910 0.01267 1.00000 Uiso H N1 0.8718(11) 0.5657(8) 0.3750(5) 0.01267 1.00000 Uiso N H1 0.81129 0.55313 0.34383 0.01267 1.00000 Uiso H C4 0.9592(14) 0.6878(13) 0.3547(6) 0.01267 1.00000 Uiso C H4A 0.90271 0.76346 0.34871 0.01267 1.00000 Uiso H H4B 0.99988 0.66690 0.31295 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Ho1 O5 2.220(18) 1_455 ? Ho1 O4 2.242(15) 6_755 ? Ho1 O6 2.236(16) 8_556 ? Ho1 O8 2.283(14) 1_455 ? Ho1 O7 2.486(17) 6_765 ? Ho1 O1W 2.548(18) . ? Ho1 O1 2.556(14) . ? Ho1 O2 2.726(15) . ? P1 O5 1.504(19) . ? P1 O3 1.527(17) . ? P1 O4 1.517(16) . ? P1 C4 1.82(2) . ? P2 O8 1.453(17) . ? P2 O7 1.494(18) . ? P2 O6 1.505(17) . ? P2 C3 1.85(3) . ? O2 C1 1.26(3) . ? C1 O1 1.24(3) . ? C1 C2 1.50(4) . ? O4 Ho1 2.242(15) 6_765 ? O6 Ho1 2.236(16) 8_656 ? O8 Ho1 2.283(14) 1_655 ? O7 Ho1 2.486(17) 6_755 ? O5 Ho1 2.220(18) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.58(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.55(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.58(3) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O5 Ho1 O4 86.3(6) 1_455 6_755 ? O5 Ho1 O6 152.4(5) 1_455 8_556 ? O4 Ho1 O6 103.4(6) 6_755 8_556 ? O5 Ho1 O8 78.2(5) 1_455 1_455 ? O4 Ho1 O8 79.0(5) 6_755 1_455 ? O6 Ho1 O8 78.4(5) 8_556 1_455 ? O5 Ho1 O7 100.7(5) 1_455 6_765 ? O4 Ho1 O7 142.6(6) 6_755 6_765 ? O6 Ho1 O7 87.3(6) 8_556 6_765 ? O8 Ho1 O7 138.4(6) 1_455 6_765 ? O5 Ho1 O1W 87.0(6) 1_455 . ? O4 Ho1 O1W 153.8(6) 6_755 . ? O6 Ho1 O1W 72.9(6) 8_556 . ? O8 Ho1 O1W 74.9(6) 1_455 . ? O7 Ho1 O1W 63.6(6) 6_765 . ? O5 Ho1 O1 127.1(5) 1_455 . ? O4 Ho1 O1 78.1(5) 6_755 . ? O6 Ho1 O1 80.4(4) 8_556 . ? O8 Ho1 O1 144.1(6) 1_455 . ? O7 Ho1 O1 68.3(5) 6_765 . ? O1W Ho1 O1 125.3(5) . . ? O5 Ho1 O2 80.0(5) 1_455 . ? O4 Ho1 O2 72.0(5) 6_755 . ? O6 Ho1 O2 127.5(5) 8_556 . ? O8 Ho1 O2 144.5(5) 1_455 . ? O7 Ho1 O2 73.2(6) 6_765 . ? O1W Ho1 O2 131.4(6) . . ? O1 Ho1 O2 47.1(5) . . ? O5 P1 O3 111.2(11) . . ? O5 P1 O4 115.3(9) . . ? O3 P1 O4 109.7(9) . . ? O5 P1 C4 109.5(10) . . ? O3 P1 C4 102.9(11) . . ? O4 P1 C4 107.5(10) . . ? O8 P2 O7 119.7(10) . . ? O8 P2 O6 118.6(11) . . ? O7 P2 O6 112.5(9) . . ? O8 P2 C3 98.8(10) . . ? O7 P2 C3 103.5(13) . . ? O6 P2 C3 98.3(10) . . ? C1 O2 Ho1 92.8(16) . . ? O2 C1 O1 116(2) . . ? O2 C1 C2 121(2) . . ? O1 C1 C2 122.0(19) . . ? P1 O4 Ho1 147.1(10) . 6_765 ? P2 O6 Ho1 150.0(9) . 8_656 ? P2 O8 Ho1 164.7(10) . 1_655 ? C1 O1 Ho1 101.5(13) . . ? P2 O7 Ho1 137.0(8) . 6_755 ? P1 O5 Ho1 146.6(12) . 1_655 ? P1 O3 H3 109.4 . . ? C1 C2 N1 100(2) . . ? C1 C2 H2A 111.5 . . ? N1 C2 H2A 111.5 . . ? C1 C2 H2B 111.9 . . ? N1 C2 H2B 112.0 . . ? H2A C2 H2B 109.3 . . ? N1 C3 P2 110.6(16) . . ? N1 C3 H3A 109.6 . . ? P2 C3 H3A 109.5 . . ? N1 C3 H3B 109.9 . . ? P2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 N1 C4 110.2(15) . . ? C3 N1 C2 114.8(17) . . ? C4 N1 C2 111.8(16) . . ? C3 N1 H1 106.7 . . ? C4 N1 H1 106.1 . . ? C2 N1 H1 106.6 . . ? N1 C4 P1 113.3(17) . . ? N1 C4 H4A 109.1 . . ? P1 C4 H4A 109.1 . . ? N1 C4 H4B 108.6 . . ? P1 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Ho1 O2 C1 -171.1(14) 1_455 . . . ? O4 Ho1 O2 C1 99.5(14) 6_755 . . . ? O6 Ho1 O2 C1 6.3(16) 8_556 . . . ? O8 Ho1 O2 C1 136.1(13) 1_455 . . . ? O7 Ho1 O2 C1 -66.6(13) 6_765 . . . ? O1W Ho1 O2 C1 -94.2(14) . . . . ? O1 Ho1 O2 C1 9.1(11) . . . . ? Ho1 O2 C1 O1 -15(2) . . . . ? Ho1 O2 C1 C2 177(2) . . . . ? O5 P1 O4 Ho1 98.3(18) . . . 6_765 ? O3 P1 O4 Ho1 -135.3(16) . . . 6_765 ? C4 P1 O4 Ho1 -24.1(19) . . . 6_765 ? O8 P2 O6 Ho1 52(2) . . . 8_656 ? O7 P2 O6 Ho1 -95(2) . . . 8_656 ? C3 P2 O6 Ho1 157(2) . . . 8_656 ? O7 P2 O8 Ho1 -118(4) . . . 1_655 ? O6 P2 O8 Ho1 98(4) . . . 1_655 ? C3 P2 O8 Ho1 -6(4) . . . 1_655 ? O2 C1 O1 Ho1 17(2) . . . . ? C2 C1 O1 Ho1 -176(2) . . . . ? O5 Ho1 O1 C1 -9.7(16) 1_455 . . . ? O4 Ho1 O1 C1 -85.8(13) 6_755 . . . ? O6 Ho1 O1 C1 168.3(14) 8_556 . . . ? O8 Ho1 O1 C1 -137.1(13) 1_455 . . . ? O7 Ho1 O1 C1 77.4(14) 6_765 . . . ? O1W Ho1 O1 C1 107.3(14) . . . . ? O2 Ho1 O1 C1 -9.4(12) . . . . ? O8 P2 O7 Ho1 17(2) . . . 6_755 ? O6 P2 O7 Ho1 163.4(12) . . . 6_755 ? C3 P2 O7 Ho1 -91.5(16) . . . 6_755 ? O3 P1 O5 Ho1 170.3(15) . . . 1_655 ? O4 P1 O5 Ho1 -64.1(17) . . . 1_655 ? C4 P1 O5 Ho1 57.2(18) . . . 1_655 ? O2 C1 C2 N1 -174(2) . . . . ? O1 C1 C2 N1 20(3) . . . . ? O8 P2 C3 N1 103.3(16) . . . . ? O7 P2 C3 N1 -133.1(15) . . . . ? O6 P2 C3 N1 -17.5(18) . . . . ? P2 C3 N1 C4 -71(2) . . . . ? P2 C3 N1 C2 161.8(16) . . . . ? C1 C2 N1 C3 -116(2) . . . . ? C1 C2 N1 C4 117(2) . . . . ? C3 N1 C4 P1 -57(2) . . . . ? C2 N1 C4 P1 71.6(19) . . . . ? O5 P1 C4 N1 75.6(17) . . . . ? O3 P1 C4 N1 -42.7(16) . . . . ? O4 P1 C4 N1 -158.4(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.81 2.61(3) 164.1 2_566 data_11 _database_code_depnum_ccdc_archive 'CCDC 705170' #============================================================================= _audit_creation_method 'Manual editing plus fullprof.2k' _audit_creation_date '02 October 2008' #============================================================================= # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H10 Er N O9 P2' _chemical_formula_sum 'C4 H10 Er N O9 P2' _chemical_formula_weight 445.33 loop_ _atom_type_symbol _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source ER 27.65630 2.07356 16.42850 0.22354 14.97790 11.36040 2.98233 105.70300 5.92046 -0.72300 4.95800 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 P 6.43450 1.90670 4.17910 27.15700 1.78000 0.52600 1.49080 68.16450 1.11490 0.09000 0.09500 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 O 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080 0.00800 0.00600 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 C 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560 0.00200 0.00200 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 H 0.49300 10.51090 0.32291 26.12570 0.14019 3.14236 0.04081 57.79970 0.00304 0.00000 0.00000 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 N 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900 0.00400 0.00300 International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5 #============================================================================= # POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.6224(14) _cell_length_b 10.0504(15) _cell_length_c 20.334(3) _cell_angle_alpha 90.00000 _cell_angle_beta 90.00000 _cell_angle_gamma 90.00000 _cell_volume 1966.4(5) _exptl_crystal_density_diffrn 3.008 _cell_formula_units_Z 8 _cell_measurement_temperature 298 _cell_special_details ; ? ; _pd_spec_mounting ; Hilgenberg borosilicate glass capillary (ca. 0.4 mm of diameter) ; #============================================================================= # EXPERIMENTAL DATA _exptl_special_details ; ? ; _pd_instr_location ; MAR 345 Imaging Plate instrument belonging to the Swiss-Norwegian BM01a beam line (bending magnet source) at the European Synchrotron Radiation Facility (ESRF), Grenoble, France. ; _pd_calibration_special_details ; LaB6 standard ; _diffrn_ambient_temperature 298 _diffrn_source Synchrotron _diffrn_radiation_type X-ray _diffrn_radiation_monochromator 0.71013(1) _diffrn_measurement_method Debye-Scherrer _diffrn_detector 'Imaging Plate' _diffrn_detector_type 'MAR 345' _pd_meas_scan_method cont _pd_meas_special_details ; The powdered sample was slowly spun 180 degrees (in phi scanning mode) during data collection to improve powder averaging. Two-dimensional powder data was collected using a MAR2300 imaging plate detector and then integrated using the software Fit2D. The monochromatic wavelength (0.71013 A) and sample-to-detector distance (d of about 150 mm) were calibrated from an individual run using the standard LaB6. ; # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 1312 _pd_meas_2theta_range_min 2.02483 _pd_meas_2theta_range_max 49.00845 _pd_meas_2theta_range_inc 0.035838 #============================================================================= # REFINEMENT DATA _refine_special_details ; ? ; # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; ? ; # The next three items are given as text. _pd_proc_ls_profile_function Gaussian _pd_proc_ls_background_function 'Fixed points' _pd_proc_ls_pref_orient_corr ; None ; # The following profile R-factors are NOT CORRECTED for background # The sum is extended to all non-excluded points. # These are the current CIF standard _pd_proc_ls_prof_R_factor 5.5447 _pd_proc_ls_prof_wR_factor 7.1157 _pd_proc_ls_prof_wR_expected 1.4244 # The following profile R-factors are CORRECTED for background # The sum is extended to all non-excluded points. # These items are not in the current CIF standard, but are defined above _pd_proc_ls_prof_cR_factor 12.4685 _pd_proc_ls_prof_cwR_factor 13.6600 _pd_proc_ls_prof_cwR_expected 2.7344 # The following items are not in the CIF standard, but are defined above _pd_proc_ls_prof_chi2 24.9566 _pd_proc_ls_prof_echi2 24.9566 # Items related to LS refinement _refine_ls_R_I_factor 10.3520 _refine_ls_number_reflns 2062 _refine_ls_number_parameters 62 _refine_ls_number_restraints 27 # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0344 _pd_proc_2theta_range_max 49.0180 _pd_proc_2theta_range_inc 0.035838 _pd_proc_wavelength 0.710130 _pd_block_diffractogram_id ? # The id used for the block containing # the powder pattern profile (section 11) # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_structure_solution eXpo2004 _computing_structure_refinement FULLPROF _computing_molecular_graphics 'Crystal Impact Diamond 3.1f' _computing_publication_material ? #============================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_adp_type _atom_site_type_symbol ER1 0.3627(4) 0.5428(4) 0.33483(19) 0.01267 1.00000 Uiso ER P1 1.0943(8) 0.7288(8) 0.4133(4) 0.01267 1.00000 Uiso P P2 1.0247(8) 0.3793(8) 0.3071(4) 0.01267 1.00000 Uiso P O2 0.53039(11) 0.603(4) 0.4298(8) 0.01267 1.00000 Uiso O C1 0.63813(8) 0.5745(6) 0.39954(20) 0.01267 1.00000 Uiso C O4 1.143(2) 0.8731(7) 0.4058(11) 0.01267 1.00000 Uiso O O6 0.9351(16) 0.4452(14) 0.2542(12) 0.01267 1.00000 Uiso O O8 1.1724(11) 0.4319(14) 0.3030(12) 0.01267 1.00000 Uiso O O1 0.6269(5) 0.498(2) 0.3519(10) 0.01267 1.00000 Uiso O O7 1.0216(18) 0.2293(7) 0.2976(13) 0.01267 1.00000 Uiso O O5 1.2191(18) 0.6365(13) 0.4065(11) 0.01267 1.00000 Uiso O O1W 0.238(4) 0.681(4) 0.2514(17) 0.01267 1.00000 Uiso O O3 1.033(2) 0.7119(14) 0.4825(8) 0.01267 1.00000 Uiso O H3 1.04217 0.78399 0.50387 0.01267 1.00000 Uiso H C2 0.77875(10) 0.6010(12) 0.4298(4) 0.01267 1.00000 Uiso C H2A 0.78882 0.69222 0.44305 0.01267 1.00000 Uiso H H2B 0.79691 0.54368 0.46652 0.01267 1.00000 Uiso H C3 0.958(3) 0.4408(18) 0.3853(6) 0.01267 1.00000 Uiso C H3A 0.90021 0.37435 0.40567 0.01267 1.00000 Uiso H H3B 1.03287 0.46156 0.41445 0.01267 1.00000 Uiso H N1 0.8713(12) 0.5672(8) 0.3702(7) 0.01267 1.00000 Uiso N H1 0.81535 0.54910 0.33589 0.01267 1.00000 Uiso H C4 0.9657(18) 0.6851(18) 0.3508(7) 0.01267 1.00000 Uiso C H4A 0.90873 0.76120 0.34207 0.01267 1.00000 Uiso H H4B 1.01363 0.66278 0.31076 0.01267 1.00000 Uiso H # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. #============================================================================= # DISTANCES AND ANGLES / MOLECULAR GEOMETRY _geom_special_details ? 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 Er1 O6 2.173(2) 8_556 ? Er1 O5 2.219(3) 1_455 ? Er1 O4 2.234(2) 6_755 ? Er1 O8 2.240(2) 1_455 ? Er1 O7 2.309(3) 6_765 ? Er1 O1W 2.502(3) . ? Er1 O2 2.590(3) . ? Er1 O1 2.602(3) . ? Er1 C1 2.977(5) . ? P1 O5 1.523(3) . ? P1 O4 1.533(3) . ? P1 O3 1.534(3) . ? P1 C4 1.828(4) . ? P2 O8 1.518(2) . ? P2 O7 1.520(3) . ? P2 O6 1.529(2) . ? P2 C3 1.820(3) . ? O2 C1 1.242(5) . ? C1 O1 1.238(3) . ? C1 C2 1.508(6) . ? O4 Er1 2.234(2) 6_765 ? O6 Er1 2.173(2) 8_656 ? O8 Er1 2.240(2) 1_655 ? O7 Er1 2.309(3) 6_755 ? O5 Er1 2.219(3) 1_655 ? O3 H3 0.8200 . ? C2 N1 1.540(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N1 1.548(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.543(4) . ? N1 H1 0.9100 . ? C4 H4A 0.9700 . ? C4 H4B 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 O6 Er1 O5 159.81(9) 8_556 1_455 ? O6 Er1 O4 101.65(10) 8_556 6_755 ? O5 Er1 O4 83.41(9) 1_455 6_755 ? O6 Er1 O8 78.29(9) 8_556 1_455 ? O5 Er1 O8 83.82(10) 1_455 1_455 ? O4 Er1 O8 77.73(10) 6_755 1_455 ? O6 Er1 O7 86.50(10) 8_556 6_765 ? O5 Er1 O7 99.78(10) 1_455 6_765 ? O4 Er1 O7 147.42(11) 6_755 6_765 ? O8 Er1 O7 134.79(9) 1_455 6_765 ? O6 Er1 O1W 80.76(10) 8_556 . ? O5 Er1 O1W 84.84(8) 1_455 . ? O4 Er1 O1W 148.29(10) 6_755 . ? O8 Er1 O1W 71.78(7) 1_455 . ? O7 Er1 O1W 63.81(9) 6_765 . ? O6 Er1 O2 121.80(9) 8_556 . ? O5 Er1 O2 78.39(9) 1_455 . ? O4 Er1 O2 73.29(10) 6_755 . ? O8 Er1 O2 147.40(8) 1_455 . ? O7 Er1 O2 75.64(9) 6_765 . ? O1W Er1 O2 132.46(8) . . ? O6 Er1 O1 73.76(7) 8_556 . ? O5 Er1 O1 126.41(8) 1_455 . ? O4 Er1 O1 78.87(9) 6_755 . ? O8 Er1 O1 138.72(7) 1_455 . ? O7 Er1 O1 73.22(8) 6_765 . ? O1W Er1 O1 130.87(7) . . ? O2 Er1 O1 48.12(8) . . ? O6 Er1 C1 97.46(10) 8_556 . ? O5 Er1 C1 102.70(10) 1_455 . ? O4 Er1 C1 79.51(11) 6_755 . ? O8 Er1 C1 155.42(8) 1_455 . ? O7 Er1 C1 68.12(9) 6_765 . ? O1W Er1 C1 131.92(8) . . ? O2 Er1 C1 24.54(9) . . ? O1 Er1 C1 24.47(7) . . ? O5 P1 O4 109.03(18) . . ? O5 P1 O3 108.69(14) . . ? O4 P1 O3 108.31(14) . . ? O5 P1 C4 108.94(16) . . ? O4 P1 C4 111.36(15) . . ? O3 P1 C4 110.46(13) . . ? O8 P2 O7 110.87(15) . . ? O8 P2 O6 109.77(13) . . ? O7 P2 O6 109.27(15) . . ? O8 P2 C3 105.10(16) . . ? O7 P2 C3 116.10(18) . . ? O6 P2 C3 105.47(15) . . ? C1 O2 Er1 95.5(2) . . ? O1 C1 O2 117.2(4) . . ? O1 C1 C2 120.6(4) . . ? O2 C1 C2 120.3(3) . . ? O1 C1 Er1 60.6(2) . . ? O2 C1 Er1 60.0(2) . . ? C2 C1 Er1 175.6(2) . . ? P1 O4 Er1 141.23(15) . 6_765 ? P2 O6 Er1 164.16(15) . 8_656 ? P2 O8 Er1 157.29(14) . 1_655 ? C1 O1 Er1 95.0(3) . . ? P2 O7 Er1 139.03(16) . 6_755 ? P1 O5 Er1 144.07(15) . 1_655 ? P1 O3 H3 109.4 . . ? C1 C2 N1 99.2(3) . . ? C1 C2 H2A 112.0 . . ? N1 C2 H2A 112.0 . . ? C1 C2 H2B 111.9 . . ? N1 C2 H2B 111.8 . . ? H2A C2 H2B 109.6 . . ? N1 C3 P2 107.4(2) . . ? N1 C3 H3A 110.3 . . ? P2 C3 H3A 110.2 . . ? N1 C3 H3B 110.2 . . ? P2 C3 H3B 110.2 . . ? H3A C3 H3B 108.5 . . ? C2 N1 C4 111.9(3) . . ? C2 N1 C3 109.7(3) . . ? C4 N1 C3 111.3(3) . . ? C2 N1 H1 107.9 . . ? C4 N1 H1 108.0 . . ? C3 N1 H1 107.9 . . ? N1 C4 P1 113.8(2) . . ? N1 C4 H4A 108.8 . . ? P1 C4 H4A 108.8 . . ? N1 C4 H4B 108.8 . . ? P1 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Er1 O2 C1 8.0(3) 8_556 . . . ? O5 Er1 O2 C1 -172.0(2) 1_455 . . . ? O4 Er1 O2 C1 101.5(2) 6_755 . . . ? O8 Er1 O2 C1 129.7(2) 1_455 . . . ? O7 Er1 O2 C1 -68.6(2) 6_765 . . . ? O1W Er1 O2 C1 -100.2(2) . . . . ? O1 Er1 O2 C1 11.62(19) . . . . ? Er1 O2 C1 O1 -20.8(3) . . . . ? Er1 O2 C1 C2 174.9(3) . . . . ? O6 Er1 C1 O1 -14.38(18) 8_556 . . . ? O5 Er1 C1 O1 166.86(17) 1_455 . . . ? O4 Er1 C1 O1 86.15(16) 6_755 . . . ? O8 Er1 C1 O1 63.7(3) 1_455 . . . ? O7 Er1 C1 O1 -97.56(18) 6_765 . . . ? O1W Er1 C1 O1 -98.63(16) . . . . ? O2 Er1 C1 O1 158.8(3) . . . . ? O6 Er1 C1 O2 -173.2(2) 8_556 . . . ? O5 Er1 C1 O2 8.1(2) 1_455 . . . ? O4 Er1 C1 O2 -72.6(2) 6_755 . . . ? O8 Er1 C1 O2 -95.0(3) 1_455 . . . ? O7 Er1 C1 O2 103.7(3) 6_765 . . . ? O1W Er1 C1 O2 102.6(2) . . . . ? O1 Er1 C1 O2 -158.8(3) . . . . ? O6 Er1 C1 C2 92(3) 8_556 . . . ? O5 Er1 C1 C2 -86(3) 1_455 . . . ? O4 Er1 C1 C2 -167(3) 6_755 . . . ? O8 Er1 C1 C2 170(3) 1_455 . . . ? O7 Er1 C1 C2 9(3) 6_765 . . . ? O1W Er1 C1 C2 8(3) . . . . ? O2 Er1 C1 C2 -95(3) . . . . ? O1 Er1 C1 C2 107(3) . . . . ? O5 P1 O4 Er1 106.6(3) . . . 6_765 ? O3 P1 O4 Er1 -135.3(3) . . . 6_765 ? C4 P1 O4 Er1 -13.6(4) . . . 6_765 ? O8 P2 O6 Er1 27.6(7) . . . 8_656 ? O7 P2 O6 Er1 -94.1(7) . . . 8_656 ? C3 P2 O6 Er1 140.4(6) . . . 8_656 ? O7 P2 O8 Er1 -127.1(4) . . . 1_655 ? O6 P2 O8 Er1 112.1(4) . . . 1_655 ? C3 P2 O8 Er1 -0.9(4) . . . 1_655 ? O2 C1 O1 Er1 20.6(3) . . . . ? C2 C1 O1 Er1 -175.1(3) . . . . ? O6 Er1 O1 C1 165.14(18) 8_556 . . . ? O5 Er1 O1 C1 -16.0(2) 1_455 . . . ? O4 Er1 O1 C1 -89.10(17) 6_755 . . . ? O8 Er1 O1 C1 -145.57(17) 1_455 . . . ? O7 Er1 O1 C1 73.90(17) 6_765 . . . ? O1W Er1 O1 C1 103.39(17) . . . . ? O2 Er1 O1 C1 -11.65(19) . . . . ? O8 P2 O7 Er1 46.6(3) . . . 6_755 ? O6 P2 O7 Er1 167.7(2) . . . 6_755 ? C3 P2 O7 Er1 -73.2(3) . . . 6_755 ? O4 P1 O5 Er1 -77.8(3) . . . 1_655 ? O3 P1 O5 Er1 164.3(2) . . . 1_655 ? C4 P1 O5 Er1 43.9(3) . . . 1_655 ? O1 C1 C2 N1 23.8(4) . . . . ? O2 C1 C2 N1 -172.4(3) . . . . ? Er1 C1 C2 N1 -80(3) . . . . ? O8 P2 C3 N1 98.1(3) . . . . ? O7 P2 C3 N1 -139.0(2) . . . . ? O6 P2 C3 N1 -17.9(3) . . . . ? C1 C2 N1 C4 122.9(3) . . . . ? C1 C2 N1 C3 -113.0(3) . . . . ? P2 C3 N1 C2 163.8(2) . . . . ? P2 C3 N1 C4 -71.8(3) . . . . ? C2 N1 C4 P1 65.1(4) . . . . ? C3 N1 C4 P1 -58.1(3) . . . . ? O5 P1 C4 N1 82.6(3) . . . . ? O4 P1 C4 N1 -157.1(2) . . . . ? O3 P1 C4 N1 -36.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.82 1.79 2.577(4) 159.0 2_566 #============================================================================= # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./