# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Jose R. Garcia' _publ_contact_author_address ; Quimica Organica e Inorganica Universidad de Oviedo Julian Claveria, 8 Oviedo 33006 SPAIN ; _publ_contact_author_email JRGM@UNIOVI.ES _publ_section_title ; Crystal structure and photoluminescent properties of lanthanide diphosphonates ; _publ_author_address ; Departamento de Qu\'imica F\'isica y Anal\'itica Facultad de Qu\'imica Universidad de Oviedo Juli\'an Claver\'ia, 8 33006 Oviedo Spain ; _publ_requested_category FM loop_ _publ_author_name 'Jose Garcia' 'Luis D. Carlos' 'Santiago Garcia-Granda' 'Feng-Yi Liu' 'Laura Roces' 'Joao Rocha' ; R.A.S.Ferreira ; data_la01 _database_code_depnum_ccdc_archive 'CCDC 639249' _audit_creation_date 2007-05-09T11:19:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (NH3(CH2)4NH3)La(hedpH)(hedpH2) _chemical_formula_moiety 'C4 H11 La O14 P4, C4 H14 N2' _chemical_formula_sum 'C8 H25 La N2 O14 P4' _chemical_formula_weight 636.09 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.215(1) _cell_length_b 10.697(1) _cell_length_c 10.722(1) _cell_angle_alpha 67.49(1) _cell_angle_beta 89.98(1) _cell_angle_gamma 68.65(1) _cell_volume 994.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2932 _cell_measurement_theta_min 2.209 _cell_measurement_theta_max 70.076 _cell_measurement_wavelength 1.54184 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colrless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 20.339 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_absorpt_correction_T_min 0.2234 _exptl_absorpt_correction_T_max 0.6658 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.104008 _diffrn_orient_matrix_ub_12 -0.57759E-1 _diffrn_orient_matrix_ub_13 0.355618E-1 _diffrn_orient_matrix_ub_21 -0.142265E-1 _diffrn_orient_matrix_ub_22 0.157321E-1 _diffrn_orient_matrix_ub_23 0.857973E-1 _diffrn_orient_matrix_ub_31 -0.174353E-1 _diffrn_orient_matrix_ub_32 -0.925025E-1 _diffrn_orient_matrix_ub_33 0.424591E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_unetI/netI 0.0546 _diffrn_reflns_number 11560 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.52 _diffrn_reflns_theta_max 70 _diffrn_reflns_theta_full 70 _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.976 _reflns_number_total 3680 _reflns_number_gt 3633 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor )' _computing_structure_solution ; Patterson methods using DIRDIF-99 (Beurskens et al., 1999) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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 'w=1/[\s^2^(Fo^2^)+(0.1113P)^2^+2.7943P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3680 _refine_ls_number_parameters 271 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1363 _refine_ls_wR_factor_gt 0.1358 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.48 _refine_diff_density_min -1.48 _refine_diff_density_rms 0.22 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' La La -1.4094 9.0376 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.47513(3) 0.24280(3) 0.98648(3) 0.01838(16) Uani 1 1 d . . . P1 P 0.55364(14) -0.11683(15) 1.28129(14) 0.0200(3) Uani 1 1 d . . . P2 P 0.25439(14) 0.02413(15) 1.12525(14) 0.0200(3) Uani 1 1 d . . . P3 P 0.76530(14) 0.37400(15) 1.05636(15) 0.0211(3) Uani 1 1 d . . . P4 P 0.62933(16) 0.51541(16) 0.75375(15) 0.0245(3) Uani 1 1 d . . . O1 O 0.5741(4) 0.0227(5) 1.2018(4) 0.0277(9) Uani 1 1 d . . . O2 O 0.5989(4) -0.2313(5) 1.2232(4) 0.0269(9) Uani 1 1 d . . . O3 O 0.6364(5) -0.1810(5) 1.4300(4) 0.0295(9) Uani 1 1 d . . . H1 H 0.6032 -0.2353 1.4837 0.044 Uiso 1 1 calc RD . . O4 O 0.2849(4) 0.1605(5) 1.0502(4) 0.0299(9) Uani 1 1 d . . . O5 O 0.2999(4) -0.0874(5) 1.0605(4) 0.0281(9) Uani 1 1 d . . . O6 O 0.0988(4) 0.0600(5) 1.1447(5) 0.0296(10) Uani 1 1 d . . . O7 O 0.3527(5) -0.2165(5) 1.3639(4) 0.0287(9) Uani 1 1 d . . . H2 H 0.3777 -0.2638 1.3172 0.043 Uiso 1 1 calc R . . O8 O 0.6681(5) 0.2891(5) 1.0875(4) 0.0299(9) Uani 1 1 d . . . O9 O 0.7021(5) 0.5159(5) 1.0730(5) 0.0314(9) Uani 1 1 d . . . O10 O 0.9113(4) 0.2813(5) 1.1486(5) 0.0321(10) Uani 1 1 d . . . H3 H 0.9576 0.2169 1.1237 0.048 Uiso 1 1 calc RD . . O11 O 0.5470(4) 0.4181(5) 0.7807(4) 0.0278(9) Uani 1 1 d . . . O12 O 0.5451(5) 0.6574(5) 0.7806(5) 0.0370(11) Uani 1 1 d . . . H4 H 0.4764 0.6488 0.8170 0.055 Uiso 1 1 calc R . . O13 O 0.6669(5) 0.5634(5) 0.6117(4) 0.0333(10) Uani 1 1 d . . . O14 O 0.8608(5) 0.2725(5) 0.8644(5) 0.0324(10) Uani 1 1 d . . . H5 H 0.8139 0.2226 0.8946 0.049 Uiso 1 1 calc R . . C1 C 0.3645(6) -0.0752(6) 1.2958(6) 0.0208(11) Uani 1 1 d . . . C2 C 0.3149(8) 0.0099(9) 1.3850(8) 0.0375(16) Uani 1 1 d . . . H6 H 0.2143 0.0370 1.3844 0.056 Uiso 1 1 calc R . . H7 H 0.3348 0.0970 1.3498 0.056 Uiso 1 1 calc R . . H8 H 0.3644 -0.0510 1.4770 0.056 Uiso 1 1 calc R . . C3 C 0.7953(6) 0.4109(7) 0.8777(7) 0.0266(12) Uani 1 1 d . . . C4 C 0.8989(8) 0.4880(9) 0.8420(8) 0.0370(16) Uani 1 1 d . . . H9 H 0.9863 0.4284 0.9056 0.056 Uiso 1 1 calc R . . H10 H 0.8575 0.5819 0.8471 0.056 Uiso 1 1 calc R . . H11 H 0.9179 0.5022 0.7510 0.056 Uiso 1 1 calc R . . C5 C 0.8873(7) -0.0549(8) 1.3369(7) 0.0354(14) Uani 1 1 d . . . H12 H 0.8038 -0.0724 1.3677 0.042 Uiso 1 1 calc R . . H13 H 0.8737 0.0430 1.3275 0.042 Uiso 1 1 calc R . . C6 C 1.0167(7) -0.1664(8) 1.4439(7) 0.0356(14) Uani 1 1 d . . . H14 H 1.0099 -0.1449 1.5243 0.043 Uiso 1 1 calc R . . H15 H 1.1011 -0.1556 1.4085 0.043 Uiso 1 1 calc R . . C7 C 1.0344(7) -0.3263(8) 1.4867(8) 0.0387(16) Uani 1 1 d . . . H16 H 0.9450 -0.3344 1.5091 0.046 Uiso 1 1 calc R . . H17 H 1.0563 -0.3531 1.4101 0.046 Uiso 1 1 calc R . . C8 C 1.1515(7) -0.4341(8) 1.6092(7) 0.0372(15) Uani 1 1 d . . . H18 H 1.1342 -0.4030 1.6837 0.045 Uiso 1 1 calc R . . H19 H 1.1488 -0.5309 1.6398 0.045 Uiso 1 1 calc R . . N1 N 0.8999(6) -0.0612(7) 1.2005(6) 0.0376(13) Uani 1 1 d . . . H20 H 0.9618 -0.0233 1.1621 0.056 Uiso 1 1 calc R . . H21 H 0.8152 -0.0097 1.1471 0.056 Uiso 1 1 calc R . . H22 H 0.9303 -0.1545 1.2111 0.056 Uiso 1 1 calc R . . N2 N 1.2949(5) -0.4437(6) 1.5755(6) 0.0317(11) Uani 1 1 d . . . H23 H 1.3174 -0.4869 1.5177 0.048 Uiso 1 1 calc R . . H24 H 1.3589 -0.4963 1.6517 0.048 Uiso 1 1 calc R . . H25 H 1.2943 -0.3535 1.5368 0.048 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 0.0188(2) 0.0185(2) 0.0179(2) -0.00778(15) 0.00305(14) -0.00704(15) P1 0.0201(6) 0.0240(7) 0.0166(7) -0.0079(5) 0.0017(5) -0.0099(5) P2 0.0181(7) 0.0225(7) 0.0212(7) -0.0111(6) 0.0055(5) -0.0078(5) P3 0.0205(7) 0.0223(7) 0.0226(7) -0.0128(6) 0.0046(5) -0.0069(5) P4 0.0295(7) 0.0250(7) 0.0208(7) -0.0089(6) 0.0063(6) -0.0133(6) O1 0.028(2) 0.031(2) 0.020(2) -0.0017(17) 0.0027(16) -0.0155(18) O2 0.0220(19) 0.036(2) 0.026(2) -0.0189(19) 0.0039(16) -0.0078(17) O3 0.039(2) 0.034(2) 0.017(2) -0.0061(18) -0.0017(17) -0.0203(19) O4 0.026(2) 0.032(2) 0.028(2) -0.0043(18) 0.0025(17) -0.0153(18) O5 0.025(2) 0.034(2) 0.024(2) -0.0174(18) 0.0004(16) -0.0047(17) O6 0.020(2) 0.026(2) 0.041(3) -0.014(2) 0.0078(18) -0.0078(17) O7 0.036(2) 0.028(2) 0.025(2) -0.0100(18) 0.0098(17) -0.0177(18) O8 0.035(2) 0.031(2) 0.029(2) -0.0134(19) 0.0059(18) -0.0186(19) O9 0.032(2) 0.027(2) 0.037(2) -0.0189(19) 0.0065(18) -0.0089(18) O10 0.025(2) 0.038(2) 0.031(2) -0.022(2) -0.0004(17) -0.0023(18) O11 0.028(2) 0.032(2) 0.026(2) -0.0112(18) 0.0029(17) -0.0140(18) O12 0.033(2) 0.033(2) 0.047(3) -0.019(2) 0.012(2) -0.012(2) O13 0.042(3) 0.036(2) 0.020(2) -0.0063(19) 0.0072(18) -0.018(2) O14 0.032(2) 0.036(2) 0.037(3) -0.024(2) 0.0123(19) -0.0119(19) C1 0.026(3) 0.023(3) 0.017(3) -0.010(2) 0.007(2) -0.011(2) C2 0.041(4) 0.051(4) 0.038(4) -0.031(3) 0.018(3) -0.025(3) C3 0.021(3) 0.027(3) 0.033(3) -0.014(3) 0.006(2) -0.008(2) C4 0.039(4) 0.050(4) 0.037(4) -0.025(3) 0.015(3) -0.027(3) C5 0.028(3) 0.042(4) 0.033(4) -0.012(3) 0.003(3) -0.014(3) C6 0.034(3) 0.041(4) 0.034(4) -0.017(3) 0.003(3) -0.016(3) C7 0.027(3) 0.045(4) 0.041(4) -0.014(3) 0.002(3) -0.014(3) C8 0.036(4) 0.041(4) 0.028(3) -0.008(3) 0.006(3) -0.015(3) N1 0.036(3) 0.040(3) 0.033(3) -0.012(3) 0.004(2) -0.014(2) N2 0.026(3) 0.026(3) 0.031(3) -0.005(2) -0.006(2) -0.004(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O9 2.384(4) 2_667 yes La1 O4 2.408(4) . yes La1 O2 2.434(4) 2_657 yes La1 O1 2.450(4) . yes La1 O5 2.481(4) 2_657 yes La1 O8 2.535(4) . yes La1 O11 2.600(4) . yes P1 O1 1.500(4) . yes P1 O2 1.507(4) . yes P1 O3 1.571(4) . yes P1 C1 1.839(6) . yes P2 O4 1.518(4) . yes P2 O6 1.528(4) . yes P2 O5 1.534(4) . yes P2 C1 1.838(6) . yes P3 O9 1.499(4) . yes P3 O8 1.532(4) . yes P3 O10 1.536(4) . yes P3 C3 1.852(7) . yes P4 O13 1.509(5) . yes P4 O11 1.510(4) . yes P4 O12 1.585(5) . yes P4 C3 1.837(6) . yes O2 La1 2.434(4) 2_657 yes O3 H1 0.8200 . yes O5 La1 2.481(4) 2_657 yes O7 C1 1.457(7) . yes O7 H2 0.8200 . yes O9 La1 2.384(4) 2_667 yes O10 H3 0.8200 . yes O12 H4 0.8200 . yes O14 C3 1.450(7) . yes O14 H5 0.8200 . yes C1 C2 1.527(8) . yes C2 H6 0.9600 . yes C2 H7 0.9600 . yes C2 H8 0.9600 . yes C3 C4 1.530(9) . yes C4 H9 0.9600 . yes C4 H10 0.9600 . yes C4 H11 0.9600 . yes C5 N1 1.493(9) . yes C5 C6 1.513(9) . yes C5 H12 0.9700 . yes C5 H13 0.9700 . yes C6 C7 1.530(10) . yes C6 H14 0.9700 . yes C6 H15 0.9700 . yes C7 C8 1.524(9) . yes C7 H16 0.9700 . yes C7 H17 0.9700 . yes C8 N2 1.485(9) . yes C8 H18 0.9700 . yes C8 H19 0.9700 . yes N1 H20 0.8900 . yes N1 H21 0.8900 . yes N1 H22 0.8900 . yes N2 H23 0.8900 . yes N2 H24 0.8900 . yes N2 H25 0.8900 . yes 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 O9 La1 O4 85.46(15) 2_667 . yes O9 La1 O2 93.30(15) 2_667 2_657 yes O4 La1 O2 79.20(15) . 2_657 yes O9 La1 O1 133.54(15) 2_667 . yes O4 La1 O1 73.94(14) . . yes O2 La1 O1 121.84(15) 2_657 . yes O9 La1 O5 147.10(15) 2_667 2_657 yes O4 La1 O5 122.03(15) . 2_657 yes O2 La1 O5 76.51(13) 2_657 2_657 yes O1 La1 O5 75.92(14) . 2_657 yes O9 La1 O8 94.83(15) 2_667 . yes O4 La1 O8 140.99(15) . . yes O2 La1 O8 139.48(14) 2_657 . yes O1 La1 O8 78.08(14) . . yes O5 La1 O8 75.29(14) 2_657 . yes O9 La1 O11 73.75(15) 2_667 . yes O4 La1 O11 141.66(14) . . yes O2 La1 O11 70.45(14) 2_657 . yes O1 La1 O11 142.61(13) . . yes O5 La1 O11 73.36(14) 2_657 . yes O8 La1 O11 73.95(13) . . yes O1 P1 O2 116.2(3) . . yes O1 P1 O3 106.4(2) . . yes O2 P1 O3 110.7(2) . . yes O1 P1 C1 110.0(2) . . yes O2 P1 C1 106.3(2) . . yes O3 P1 C1 107.0(3) . . yes O4 P2 O6 113.0(2) . . yes O4 P2 O5 113.9(3) . . yes O6 P2 O5 109.5(2) . . yes O4 P2 C1 107.6(2) . . yes O6 P2 C1 107.8(3) . . yes O5 P2 C1 104.4(2) . . yes O9 P3 O8 112.6(3) . . yes O9 P3 O10 108.4(3) . . yes O8 P3 O10 111.3(3) . . yes O9 P3 C3 110.0(3) . . yes O8 P3 C3 107.0(3) . . yes O10 P3 C3 107.4(3) . . yes O13 P4 O11 114.2(3) . . yes O13 P4 O12 108.7(3) . . yes O11 P4 O12 111.1(3) . . yes O13 P4 C3 108.4(3) . . yes O11 P4 C3 107.5(3) . . yes O12 P4 C3 106.7(3) . . yes P1 O1 La1 139.9(2) . . yes P1 O2 La1 135.1(2) . 2_657 yes P1 O3 H1 109.5 . . yes P2 O4 La1 143.0(3) . . yes P2 O5 La1 137.2(2) . 2_657 yes C1 O7 H2 109.5 . . yes P3 O8 La1 145.2(3) . . yes P3 O9 La1 152.5(3) . 2_667 yes P3 O10 H3 109.5 . . yes P4 O11 La1 139.2(2) . . yes P4 O12 H4 109.5 . . yes C3 O14 H5 109.5 . . yes O7 C1 C2 107.7(5) . . yes O7 C1 P2 109.2(4) . . yes C2 C1 P2 111.5(4) . . yes O7 C1 P1 106.3(4) . . yes C2 C1 P1 111.5(4) . . yes P2 C1 P1 110.5(3) . . yes C1 C2 H6 109.5 . . yes C1 C2 H7 109.5 . . yes H6 C2 H7 109.5 . . yes C1 C2 H8 109.5 . . yes H6 C2 H8 109.5 . . yes H7 C2 H8 109.5 . . yes O14 C3 C4 107.2(5) . . yes O14 C3 P4 105.7(4) . . yes C4 C3 P4 111.4(5) . . yes O14 C3 P3 109.4(4) . . yes C4 C3 P3 109.9(4) . . yes P4 C3 P3 113.0(3) . . yes C3 C4 H9 109.5 . . yes C3 C4 H10 109.5 . . yes H9 C4 H10 109.5 . . yes C3 C4 H11 109.5 . . yes H9 C4 H11 109.5 . . yes H10 C4 H11 109.5 . . yes N1 C5 C6 112.9(6) . . yes N1 C5 H12 109.0 . . yes C6 C5 H12 109.0 . . yes N1 C5 H13 109.0 . . yes C6 C5 H13 109.0 . . yes H12 C5 H13 107.8 . . yes C5 C6 C7 114.1(6) . . yes C5 C6 H14 108.7 . . yes C7 C6 H14 108.7 . . yes C5 C6 H15 108.7 . . yes C7 C6 H15 108.7 . . yes H14 C6 H15 107.6 . . yes C8 C7 C6 112.9(6) . . yes C8 C7 H16 109.0 . . yes C6 C7 H16 109.0 . . yes C8 C7 H17 109.0 . . yes C6 C7 H17 109.0 . . yes H16 C7 H17 107.8 . . yes N2 C8 C7 111.9(5) . . yes N2 C8 H18 109.2 . . yes C7 C8 H18 109.2 . . yes N2 C8 H19 109.2 . . yes C7 C8 H19 109.2 . . yes H18 C8 H19 107.9 . . yes C5 N1 H20 109.5 . . yes C5 N1 H21 109.5 . . yes H20 N1 H21 109.5 . . yes C5 N1 H22 109.5 . . yes H20 N1 H22 109.5 . . yes H21 N1 H22 109.5 . . yes C8 N2 H23 109.5 . . yes C8 N2 H24 109.5 . . yes H23 N2 H24 109.5 . . yes C8 N2 H25 109.5 . . yes H23 N2 H25 109.5 . . yes H24 N2 H25 109.5 . . yes 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 O2 P1 O1 La1 70.8(4) . . . . yes O3 P1 O1 La1 -165.5(4) . . . . yes C1 P1 O1 La1 -50.0(5) . . . . yes O9 La1 O1 P1 94.7(4) 2_667 . . . yes O4 La1 O1 P1 27.5(4) . . . . yes O2 La1 O1 P1 -38.4(5) 2_657 . . . yes O5 La1 O1 P1 -102.4(4) 2_657 . . . yes O8 La1 O1 P1 -180.0(4) . . . . yes O11 La1 O1 P1 -137.9(3) . . . . yes O1 P1 O2 La1 -62.9(4) . . . 2_657 yes O3 P1 O2 La1 175.7(3) . . . 2_657 yes C1 P1 O2 La1 59.9(4) . . . 2_657 yes O6 P2 O4 La1 170.6(4) . . . . yes O5 P2 O4 La1 -63.5(5) . . . . yes C1 P2 O4 La1 51.7(5) . . . . yes O9 La1 O4 P2 -167.5(5) 2_667 . . . yes O2 La1 O4 P2 98.3(5) 2_657 . . . yes O1 La1 O4 P2 -29.6(4) . . . . yes O5 La1 O4 P2 31.8(5) 2_657 . . . yes O8 La1 O4 P2 -75.4(5) . . . . yes O11 La1 O4 P2 136.1(4) . . . . yes O4 P2 O5 La1 62.4(4) . . . 2_657 yes O6 P2 O5 La1 -169.9(3) . . . 2_657 yes C1 P2 O5 La1 -54.7(4) . . . 2_657 yes O9 P3 O8 La1 93.2(5) . . . . yes O10 P3 O8 La1 -144.9(4) . . . . yes C3 P3 O8 La1 -27.8(5) . . . . yes O9 La1 O8 P3 -67.5(5) 2_667 . . . yes O4 La1 O8 P3 -156.2(4) . . . . yes O2 La1 O8 P3 33.3(6) 2_657 . . . yes O1 La1 O8 P3 159.0(5) . . . . yes O5 La1 O8 P3 80.6(5) 2_657 . . . yes O11 La1 O8 P3 4.0(4) . . . . yes O8 P3 O9 La1 -63.1(6) . . . 2_667 yes O10 P3 O9 La1 173.3(5) . . . 2_667 yes C3 P3 O9 La1 56.1(6) . . . 2_667 yes O13 P4 O11 La1 165.1(3) . . . . yes O12 P4 O11 La1 -71.5(4) . . . . yes C3 P4 O11 La1 44.8(4) . . . . yes O9 La1 O11 P4 86.2(4) 2_667 . . . yes O4 La1 O11 P4 146.1(3) . . . . yes O2 La1 O11 P4 -174.2(4) 2_657 . . . yes O1 La1 O11 P4 -56.9(5) . . . . yes O5 La1 O11 P4 -92.9(4) 2_657 . . . yes O8 La1 O11 P4 -13.9(4) . . . . yes O4 P2 C1 O7 -172.4(3) . . . . yes O6 P2 C1 O7 65.4(4) . . . . yes O5 P2 C1 O7 -51.0(4) . . . . yes O4 P2 C1 C2 68.8(5) . . . . yes O6 P2 C1 C2 -53.4(5) . . . . yes O5 P2 C1 C2 -169.8(4) . . . . yes O4 P2 C1 P1 -55.8(3) . . . . yes O6 P2 C1 P1 -178.0(3) . . . . yes O5 P2 C1 P1 65.6(3) . . . . yes O1 P1 C1 O7 175.4(3) . . . . yes O2 P1 C1 O7 48.9(4) . . . . yes O3 P1 C1 O7 -69.5(4) . . . . yes O1 P1 C1 C2 -67.5(5) . . . . yes O2 P1 C1 C2 165.9(4) . . . . yes O3 P1 C1 C2 47.6(5) . . . . yes O1 P1 C1 P2 57.1(3) . . . . yes O2 P1 C1 P2 -69.5(3) . . . . yes O3 P1 C1 P2 172.2(3) . . . . yes O13 P4 C3 O14 -70.8(4) . . . . yes O11 P4 C3 O14 53.1(4) . . . . yes O12 P4 C3 O14 172.2(4) . . . . yes O13 P4 C3 C4 45.3(5) . . . . yes O11 P4 C3 C4 169.2(4) . . . . yes O12 P4 C3 C4 -71.6(5) . . . . yes O13 P4 C3 P3 169.6(3) . . . . yes O11 P4 C3 P3 -66.5(4) . . . . yes O12 P4 C3 P3 52.7(4) . . . . yes O9 P3 C3 O14 178.1(4) . . . . yes O8 P3 C3 O14 -59.3(4) . . . . yes O10 P3 C3 O14 60.3(4) . . . . yes O9 P3 C3 C4 60.6(5) . . . . yes O8 P3 C3 C4 -176.7(4) . . . . yes O10 P3 C3 C4 -57.1(5) . . . . yes O9 P3 C3 P4 -64.5(4) . . . . yes O8 P3 C3 P4 58.2(4) . . . . yes O10 P3 C3 P4 177.8(3) . . . . yes N1 C5 C6 C7 -69.0(8) . . . . yes C5 C6 C7 C8 -171.2(6) . . . . yes C6 C7 C8 N2 -67.1(8) . . . . yes 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 O10 H3 O6 0.82 1.70 2.459(6) 152.6 1_655 O3 H1 O13 0.82 1.91 2.583(6) 138.2 1_546 O12 H4 O8 0.82 1.86 2.604(6) 149.5 2_667 O14 H5 O5 0.82 2.09 2.900(7) 169.4 2_657 O7 H2 O11 0.82 2.20 3.009(6) 171.9 2_657 N1 H20 O6 0.89 1.89 2.736(7) 158.6 1_655 N1 H21 O5 0.89 2.18 2.960(7) 145.8 2_657 N1 H22 O14 0.89 2.37 2.957(7) 123.6 2_757 N2 H23 O13 0.89 1.84 2.724(7) 170.8 2_757 N2 H24 O11 0.89 2.05 2.898(7) 159.4 1_646 N2 H25 O7 0.89 2.12 2.867(7) 141.1 1_655