Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jonna Jokiniemi' _publ_contact_author_email JONNA.JOKINIEMI@JOENSUU.FI _publ_section_title ; Structural study of alkaline earth metal complexes of (dichloromethylene)bisphosphonic acid P-morpholinium- and P-pyrrolidinium-P'-methyl esters ; loop_ _publ_author_name 'Jonna Jokiniemi' 'Markku Ahlgrena' 'Sirpa Peraniemi' 'Jouko J Vepsalainen' # Attachment 'CIF_B802668H' data_Structure(1) _database_code_depnum_ccdc_archive 'CCDC 673863' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H17 Cl2 Mg N O9 P2' _chemical_formula_sum 'C6 H17 Cl2 Mg N O9 P2' _chemical_formula_weight 404.36 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' Mg Mg 0.0486 0.0363 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.2714(6) _cell_length_b 7.4956(1) _cell_length_c 17.4303(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.970(1) _cell_angle_gamma 90.00 _cell_volume 3059.08(11) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.77 _cell_measurement_theta_max 27.45 _exptl_crystal_description diamond _exptl_crystal_colour colourles _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8703 _exptl_absorpt_correction_T_max 0.8703 _exptl_absorpt_process_details 'XPREP in SHELXTL (Bruker AXS, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method multi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20095 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3487 _reflns_number_gt 3136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect(Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0 (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0250P)^2^+5.5000P] 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 SHELXL _refine_ls_extinction_coef 0.00136(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3487 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0296 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _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 Cl1 Cl 0.339421(15) 0.03710(5) 0.07603(2) 0.01527(10) Uani 1 1 d . . . Cl2 Cl 0.327340(15) 0.33776(5) -0.03585(2) 0.01570(10) Uani 1 1 d . . . P1 P 0.436525(16) 0.13402(5) 0.04185(2) 0.00970(10) Uani 1 1 d . . . P2 P 0.400538(15) 0.37245(5) 0.15384(2) 0.00945(10) Uani 1 1 d . . . Mg1 Mg 0.5000 0.05840(9) 0.2500 0.01009(15) Uani 1 2 d S . . Mg2 Mg 0.5000 0.5000 0.0000 0.01064(15) Uani 1 2 d S . . O1 O 0.44228(5) -0.15222(14) 0.24069(7) 0.0140(2) Uani 1 1 d . . . H1A H 0.4515 -0.2170 0.2836 0.021 Uiso 1 1 d R . . H1B H 0.4339 -0.2302 0.2003 0.021 Uiso 1 1 d R . . O2 O 0.52796(5) 0.54606(14) 0.13530(7) 0.0138(2) Uani 1 1 d . . . H2C H 0.5463 0.4582 0.1655 0.021 Uiso 1 1 d R . . H2D H 0.4972 0.5412 0.1414 0.021 Uiso 1 1 d R . . O3 O 0.42650(5) 0.63687(14) -0.02408(7) 0.0153(2) Uani 1 1 d . . . H3C H 0.4134 0.5994 0.0081 0.023 Uiso 1 1 d R . . H3D H 0.4270 0.7539 -0.0207 0.036(6) Uiso 1 1 d R . . O4 O 0.26703(6) 0.59961(18) 0.21451(9) 0.0273(3) Uani 1 1 d . . . O11 O 0.47342(4) 0.03220(14) 0.12101(6) 0.0126(2) Uani 1 1 d . . . O12 O 0.46101(5) 0.28315(14) 0.01363(7) 0.0141(2) Uani 1 1 d . . . O13 O 0.40792(5) -0.00622(14) -0.03429(6) 0.0138(2) Uani 1 1 d . . . O21 O 0.43878(4) 0.26016(14) 0.22961(6) 0.0120(2) Uani 1 1 d . . . O22 O 0.42461(4) 0.53413(14) 0.13049(7) 0.0124(2) Uani 1 1 d . . . N2 N 0.34468(5) 0.43572(17) 0.16516(8) 0.0126(3) Uani 1 1 d . . . C1 C 0.37634(6) 0.2210(2) 0.05867(9) 0.0110(3) Uani 1 1 d . . . C2 C 0.30574(7) 0.5767(2) 0.11194(10) 0.0177(3) Uani 1 1 d . . . H2A H 0.2705 0.5225 0.0669 0.021 Uiso 1 1 calc R . . H2B H 0.3242 0.6467 0.0833 0.021 Uiso 1 1 calc R . . C3 C 0.29103(8) 0.6976(2) 0.16834(12) 0.0230(4) Uani 1 1 d . . . H3A H 0.3260 0.7598 0.2098 0.028 Uiso 1 1 calc R . . H3B H 0.2634 0.7890 0.1321 0.028 Uiso 1 1 calc R . . C5 C 0.30642(8) 0.4667(2) 0.26738(11) 0.0221(4) Uani 1 1 d . . . H5A H 0.2896 0.4014 0.2997 0.027 Uiso 1 1 calc R . . H5B H 0.3418 0.5254 0.3096 0.027 Uiso 1 1 calc R . . C6 C 0.32090(7) 0.3360(2) 0.21413(11) 0.0173(3) Uani 1 1 d . . . H6A H 0.3491 0.2479 0.2522 0.021 Uiso 1 1 calc R . . H6B H 0.2861 0.2710 0.1742 0.021 Uiso 1 1 calc R . . C13 C 0.38642(8) 0.0441(2) -0.12422(10) 0.0198(3) Uani 1 1 d . . . H13A H 0.3927 0.1720 -0.1281 0.030 Uiso 1 1 calc R . . H13B H 0.3455 0.0181 -0.1551 0.030 Uiso 1 1 calc R . . H13C H 0.4067 -0.0237 -0.1500 0.030 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 Cl1 0.01490(18) 0.01409(19) 0.01559(18) -0.00040(13) 0.00584(14) -0.00506(13) Cl2 0.01564(18) 0.01681(19) 0.01000(17) 0.00211(13) 0.00175(14) 0.00275(14) P1 0.01239(18) 0.00829(19) 0.00781(18) -0.00070(13) 0.00406(14) -0.00067(14) P2 0.00990(18) 0.00953(19) 0.00845(18) -0.00053(13) 0.00374(14) -0.00032(14) Mg1 0.0111(3) 0.0096(3) 0.0083(3) 0.000 0.0033(3) 0.000 Mg2 0.0129(3) 0.0094(3) 0.0096(3) 0.0003(3) 0.0051(3) -0.0003(3) O1 0.0184(5) 0.0120(5) 0.0103(5) -0.0003(4) 0.0055(4) -0.0019(4) O2 0.0148(5) 0.0145(5) 0.0119(5) 0.0006(4) 0.0059(4) -0.0002(4) O3 0.0184(5) 0.0108(5) 0.0186(6) 0.0020(4) 0.0101(5) 0.0009(4) O4 0.0286(7) 0.0279(7) 0.0379(7) 0.0057(6) 0.0258(6) 0.0080(6) O11 0.0147(5) 0.0134(5) 0.0094(5) 0.0007(4) 0.0050(4) 0.0019(4) O12 0.0189(5) 0.0106(5) 0.0151(5) -0.0004(4) 0.0097(4) -0.0013(4) O13 0.0212(5) 0.0098(5) 0.0082(5) -0.0010(4) 0.0048(4) -0.0009(4) O21 0.0123(5) 0.0122(5) 0.0094(5) -0.0003(4) 0.0030(4) 0.0012(4) O22 0.0150(5) 0.0108(5) 0.0131(5) -0.0012(4) 0.0078(4) -0.0019(4) N2 0.0125(6) 0.0137(6) 0.0127(6) 0.0033(5) 0.0068(5) 0.0021(5) C1 0.0111(7) 0.0110(7) 0.0086(6) 0.0017(5) 0.0023(5) -0.0013(5) C2 0.0157(7) 0.0202(8) 0.0159(7) 0.0038(6) 0.0061(6) 0.0065(6) C3 0.0280(9) 0.0197(9) 0.0289(9) 0.0040(7) 0.0195(8) 0.0079(7) C5 0.0280(9) 0.0231(9) 0.0240(9) 0.0009(7) 0.0194(8) -0.0004(7) C6 0.0180(7) 0.0168(8) 0.0217(8) 0.0017(6) 0.0131(7) -0.0020(6) C13 0.0293(9) 0.0182(8) 0.0084(7) -0.0015(6) 0.0054(6) 0.0002(7) _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 Cl1 C1 1.7884(15) . ? Cl2 C1 1.7926(14) . ? P1 O12 1.4807(11) . ? P1 O11 1.4875(11) . ? P1 O13 1.5895(11) . ? P1 C1 1.8525(15) . ? P2 O21 1.5028(11) . ? P2 O22 1.5058(11) . ? P2 N2 1.6370(13) . ? P2 C1 1.8674(15) . ? Mg1 O11 2.0389(10) . ? Mg1 O11 2.0389(10) 2_655 ? Mg1 O21 2.1170(12) 2_655 ? Mg1 O21 2.1170(12) . ? Mg1 O1 2.1436(12) . ? Mg1 O1 2.1436(12) 2_655 ? Mg2 O12 1.9920(11) 5_665 ? Mg2 O12 1.9921(11) . ? Mg2 O3 2.0548(11) 5_665 ? Mg2 O3 2.0549(11) . ? Mg2 O2 2.1562(10) . ? Mg2 O2 2.1563(10) 5_665 ? O1 H1A 0.8307 . ? O1 H1B 0.8630 . ? O2 H2C 0.8449 . ? O2 H2D 0.8616 . ? O3 H3C 0.8283 . ? O3 H3D 0.8792 . ? O4 C3 1.430(2) . ? O4 C5 1.431(2) . ? O13 C13 1.4545(18) . ? N2 C6 1.4702(19) . ? N2 C2 1.4705(19) . ? C2 C3 1.510(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 C6 1.512(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 P1 O11 119.81(6) . . ? O12 P1 O13 109.51(6) . . ? O11 P1 O13 107.31(6) . . ? O12 P1 C1 108.51(6) . . ? O11 P1 C1 106.12(6) . . ? O13 P1 C1 104.52(6) . . ? O21 P2 O22 119.54(6) . . ? O21 P2 N2 109.56(6) . . ? O22 P2 N2 107.98(6) . . ? O21 P2 C1 105.24(6) . . ? O22 P2 C1 105.35(6) . . ? N2 P2 C1 108.69(7) . . ? O11 Mg1 O11 168.94(7) . 2_655 ? O11 Mg1 O21 96.21(4) . 2_655 ? O11 Mg1 O21 91.69(4) 2_655 2_655 ? O11 Mg1 O21 91.69(4) . . ? O11 Mg1 O21 96.21(4) 2_655 . ? O21 Mg1 O21 88.82(6) 2_655 . ? O11 Mg1 O1 88.21(4) . . ? O11 Mg1 O1 83.64(4) 2_655 . ? O21 Mg1 O1 175.09(4) 2_655 . ? O21 Mg1 O1 93.21(4) . . ? O11 Mg1 O1 83.64(4) . 2_655 ? O11 Mg1 O1 88.22(4) 2_655 2_655 ? O21 Mg1 O1 93.20(4) 2_655 2_655 ? O21 Mg1 O1 175.08(4) . 2_655 ? O1 Mg1 O1 85.13(6) . 2_655 ? O12 Mg2 O12 180.0 5_665 . ? O12 Mg2 O3 86.87(4) 5_665 5_665 ? O12 Mg2 O3 93.13(4) . 5_665 ? O12 Mg2 O3 93.14(4) 5_665 . ? O12 Mg2 O3 86.87(4) . . ? O3 Mg2 O3 180.0 5_665 . ? O12 Mg2 O2 93.51(4) 5_665 . ? O12 Mg2 O2 86.49(4) . . ? O3 Mg2 O2 91.96(4) 5_665 . ? O3 Mg2 O2 88.05(4) . . ? O12 Mg2 O2 86.49(4) 5_665 5_665 ? O12 Mg2 O2 93.51(4) . 5_665 ? O3 Mg2 O2 88.04(4) 5_665 5_665 ? O3 Mg2 O2 91.95(4) . 5_665 ? O2 Mg2 O2 180.0 . 5_665 ? Mg1 O1 H1A 117.0 . . ? Mg1 O1 H1B 118.0 . . ? H1A O1 H1B 101.6 . . ? Mg2 O2 H2C 111.9 . . ? Mg2 O2 H2D 104.8 . . ? H2C O2 H2D 101.1 . . ? Mg2 O3 H3C 109.5 . . ? Mg2 O3 H3D 120.0 . . ? H3C O3 H3D 106.9 . . ? C3 O4 C5 110.20(13) . . ? P1 O11 Mg1 136.61(7) . . ? P1 O12 Mg2 168.51(7) . . ? C13 O13 P1 122.25(10) . . ? P2 O21 Mg1 134.57(6) . . ? C6 N2 C2 111.97(12) . . ? C6 N2 P2 124.26(11) . . ? C2 N2 P2 122.51(10) . . ? Cl1 C1 Cl2 108.25(7) . . ? Cl1 C1 P1 108.83(8) . . ? Cl2 C1 P1 109.58(8) . . ? Cl1 C1 P2 108.09(7) . . ? Cl2 C1 P2 109.45(8) . . ? P1 C1 P2 112.54(7) . . ? N2 C2 C3 109.31(13) . . ? N2 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? O4 C3 C2 111.49(14) . . ? O4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? O4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O4 C5 C6 111.44(14) . . ? O4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? O4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C5 108.57(13) . . ? N2 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? N2 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? O13 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 O1 H1A O2 0.83 2.18 2.9775(15) 161.0 2_645 O1 H1B O22 0.86 2.10 2.9365(15) 164.6 1_545 O2 H2D O22 0.86 1.83 2.6799(15) 168.3 . O3 H3C O22 0.83 2.08 2.8241(15) 150.0 . O3 H3C Cl2 0.83 2.82 3.3719(12) 125.4 . O3 H3D O13 0.88 1.85 2.7107(15) 164.8 1_565 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.460 _refine_diff_density_min -0.407 _refine_diff_density_rms 0.062 #===END==================================================================== data_Structure(2) _database_code_depnum_ccdc_archive 'CCDC 673864' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H15 Ba Cl2 N O8 P2' _chemical_formula_sum 'C6 H15 Ba Cl2 N O8 P2' _chemical_formula_weight 499.37 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6449(2) _cell_length_b 6.1356(1) _cell_length_c 28.8664(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.332(1) _cell_angle_gamma 90.00 _cell_volume 1514.96(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 26.0 _exptl_crystal_description neadle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 3.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5002 _exptl_absorpt_correction_T_max 0.8062 _exptl_absorpt_process_details 'XPREP in sSHELXTL (Bruker AXS, 1998' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method multi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12712 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2863 _reflns_number_gt 2629 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-200)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0 (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+2.0912P] 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 2863 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0202 _refine_ls_R_factor_gt 0.0170 _refine_ls_wR_factor_ref 0.0388 _refine_ls_wR_factor_gt 0.0377 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Ba1 Ba 0.159830(15) 0.18227(2) 0.046836(5) 0.00705(5) Uani 1 1 d . . . Cl1 Cl 0.01923(6) 0.35642(9) 0.14955(2) 0.01097(12) Uani 1 1 d . . . Cl2 Cl -0.03110(6) 0.80898(9) 0.174468(19) 0.01069(12) Uani 1 1 d . . . P1 P -0.09965(6) 0.66425(10) 0.07421(2) 0.00676(12) Uani 1 1 d . . . P2 P 0.24176(7) 0.69587(9) 0.12708(2) 0.00670(12) Uani 1 1 d . . . O1 O 0.45618(19) 0.2934(3) 0.03397(7) 0.0173(4) Uani 1 1 d . . . H1A H 0.5275 0.2565 0.0184 0.026 Uiso 1 1 d R . . H1B H 0.4954 0.3923 0.0518 0.026 Uiso 1 1 d R . . O2 O 0.28695(18) -0.2020(3) 0.01086(6) 0.0102(3) Uani 1 1 d . . . H2C H 0.2240 -0.2744 -0.0096 0.015 Uiso 1 1 d R . . H2D H 0.3055 -0.2814 0.0354 0.015 Uiso 1 1 d R . . O4 O 0.62222(19) 0.5878(3) 0.24195(6) 0.0159(4) Uani 1 1 d . . . O11 O -0.08471(18) 0.4613(3) 0.04639(6) 0.0109(3) Uani 1 1 d . . . O12 O -0.06351(18) 0.8736(3) 0.05123(6) 0.0099(3) Uani 1 1 d . . . O13 O -0.27083(18) 0.6676(3) 0.08775(6) 0.0107(3) Uani 1 1 d . . . O21 O 0.27943(18) 0.5437(3) 0.08933(6) 0.0093(3) Uani 1 1 d . . . O22 O 0.25142(17) 0.9352(3) 0.11915(5) 0.0091(3) Uani 1 1 d . . . N2 N 0.3463(2) 0.6296(3) 0.17684(7) 0.0100(4) Uani 1 1 d . . . C1 C 0.0318(3) 0.6353(4) 0.13102(8) 0.0077(5) Uani 1 1 d . . . C2 C 0.3819(3) 0.7837(4) 0.21584(8) 0.0110(5) Uani 1 1 d . . . H2A H 0.3325 0.7340 0.2429 0.013 Uiso 1 1 calc R . . H2B H 0.3395 0.9293 0.2063 0.013 Uiso 1 1 calc R . . C3 C 0.5570(3) 0.7977(4) 0.22970(9) 0.0130(5) Uani 1 1 d . . . H3A H 0.6050 0.8580 0.2033 0.016 Uiso 1 1 calc R . . H3B H 0.5812 0.8977 0.2567 0.016 Uiso 1 1 calc R . . C5 C 0.5912(3) 0.4410(4) 0.20317(9) 0.0150(5) Uani 1 1 d . . . H5A H 0.6379 0.2971 0.2122 0.018 Uiso 1 1 calc R . . H5B H 0.6406 0.4972 0.1767 0.018 Uiso 1 1 calc R . . C6 C 0.4164(3) 0.4147(4) 0.18775(9) 0.0121(5) Uani 1 1 d . . . H6A H 0.3976 0.3199 0.1597 0.015 Uiso 1 1 calc R . . H6B H 0.3678 0.3453 0.2131 0.015 Uiso 1 1 calc R . . C13 C -0.3528(3) 0.8719(4) 0.09201(9) 0.0156(5) Uani 1 1 d . . . H13A H -0.2776 0.9846 0.1043 0.023 Uiso 1 1 calc R . . H13B H -0.4299 0.8525 0.1134 0.023 Uiso 1 1 calc R . . H13C H -0.4062 0.9162 0.0612 0.023 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 Ba1 0.00811(8) 0.00647(7) 0.00663(7) -0.00035(5) 0.00126(5) 0.00022(5) Cl1 0.0133(3) 0.0087(3) 0.0107(3) 0.0028(2) 0.0012(2) -0.0006(2) Cl2 0.0128(3) 0.0123(3) 0.0074(3) -0.0023(2) 0.0030(2) 0.0019(2) P1 0.0053(3) 0.0089(3) 0.0060(3) 0.0000(2) 0.0004(2) 0.0003(2) P2 0.0065(3) 0.0075(3) 0.0057(3) -0.0004(2) -0.0006(2) -0.0001(2) O1 0.0145(9) 0.0151(9) 0.0244(10) -0.0055(8) 0.0100(8) -0.0015(7) O2 0.0107(8) 0.0108(8) 0.0087(8) -0.0010(7) -0.0003(6) -0.0003(7) O4 0.0134(8) 0.0163(9) 0.0157(9) -0.0001(8) -0.0056(7) 0.0010(7) O11 0.0091(8) 0.0128(8) 0.0100(8) -0.0033(7) -0.0013(6) 0.0021(7) O12 0.0092(8) 0.0124(8) 0.0078(8) 0.0022(7) 0.0000(6) -0.0008(7) O13 0.0071(8) 0.0119(8) 0.0135(8) 0.0012(7) 0.0029(6) 0.0017(7) O21 0.0092(8) 0.0086(8) 0.0102(8) -0.0012(7) 0.0018(6) -0.0005(7) O22 0.0095(8) 0.0085(8) 0.0088(8) 0.0010(7) -0.0010(6) -0.0006(7) N2 0.0119(10) 0.0081(10) 0.0082(9) -0.0005(8) -0.0043(8) 0.0024(8) C1 0.0115(11) 0.0072(11) 0.0049(10) -0.0013(9) 0.0028(9) 0.0012(9) C2 0.0107(11) 0.0145(12) 0.0067(11) -0.0019(10) -0.0023(9) -0.0001(10) C3 0.0122(12) 0.0137(12) 0.0121(12) -0.0011(10) -0.0015(9) -0.0014(10) C5 0.0143(12) 0.0134(12) 0.0161(12) 0.0005(11) -0.0019(10) 0.0016(10) C6 0.0144(12) 0.0070(11) 0.0134(12) 0.0025(10) -0.0031(9) 0.0002(10) C13 0.0116(12) 0.0157(12) 0.0198(13) 0.0016(11) 0.0032(10) 0.0073(10) _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 Ba1 O22 2.6085(15) 1_545 ? Ba1 O21 2.6689(16) . ? Ba1 O11 2.7188(16) . ? Ba1 O12 2.7205(16) 1_545 ? Ba1 O1 2.7280(17) . ? Ba1 O12 2.8532(16) 3_565 ? Ba1 O2 2.8591(16) . ? Cl1 C1 1.801(2) . ? Cl2 C1 1.789(2) . ? P1 O11 1.4975(17) . ? P1 O12 1.4993(17) . ? P1 O13 1.5844(16) . ? P1 C1 1.863(2) . ? P2 O22 1.4902(17) . ? P2 O21 1.5060(17) . ? P2 N2 1.6339(19) . ? P2 C1 1.872(2) . ? O1 H1A 0.8449 . ? O1 H1B 0.8355 . ? O2 H2C 0.8652 . ? O2 H2D 0.8566 . ? O4 C3 1.430(3) . ? O4 C5 1.431(3) . ? O12 Ba1 2.7205(16) 1_565 ? O12 Ba1 2.8534(16) 3_565 ? O13 C13 1.454(3) . ? O22 Ba1 2.6083(15) 1_565 ? N2 C6 1.466(3) . ? N2 C2 1.468(3) . ? C2 C3 1.511(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 C6 1.521(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O22 Ba1 O21 93.59(5) 1_545 . ? O22 Ba1 O11 121.02(5) 1_545 . ? O21 Ba1 O11 74.23(5) . . ? O22 Ba1 O12 72.14(5) 1_545 1_545 ? O21 Ba1 O12 141.92(5) . 1_545 ? O11 Ba1 O12 83.22(5) . 1_545 ? O22 Ba1 O1 94.13(5) 1_545 . ? O21 Ba1 O1 63.00(5) . . ? O11 Ba1 O1 125.94(5) . . ? O12 Ba1 O1 150.13(5) 1_545 . ? O22 Ba1 O12 137.33(5) 1_545 3_565 ? O21 Ba1 O12 126.43(5) . 3_565 ? O11 Ba1 O12 87.48(5) . 3_565 ? O12 Ba1 O12 81.70(5) 1_545 3_565 ? O1 Ba1 O12 92.28(5) . 3_565 ? O22 Ba1 O2 73.94(5) 1_545 . ? O21 Ba1 O2 135.10(4) . . ? O11 Ba1 O2 148.98(5) . . ? O12 Ba1 O2 75.86(5) 1_545 . ? O1 Ba1 O2 74.85(5) . . ? O12 Ba1 O2 67.22(5) 3_565 . ? O11 P1 O12 115.82(10) . . ? O11 P1 O13 107.41(9) . . ? O12 P1 O13 111.09(9) . . ? O11 P1 C1 107.68(10) . . ? O12 P1 C1 109.34(10) . . ? O13 P1 C1 104.87(10) . . ? O22 P2 O21 118.49(9) . . ? O22 P2 N2 110.13(10) . . ? O21 P2 N2 109.36(10) . . ? O22 P2 C1 106.33(10) . . ? O21 P2 C1 103.54(9) . . ? N2 P2 C1 108.35(10) . . ? Ba1 O1 H1A 141.0 . . ? Ba1 O1 H1B 113.8 . . ? H1A O1 H1B 105.1 . . ? Ba1 O2 H2C 115.7 . . ? Ba1 O2 H2D 101.8 . . ? H2C O2 H2D 107.2 . . ? C3 O4 C5 110.53(18) . . ? P1 O11 Ba1 130.43(8) . . ? P1 O12 Ba1 144.28(9) . 1_565 ? P1 O12 Ba1 106.64(8) . 3_565 ? Ba1 O12 Ba1 98.30(5) 1_565 3_565 ? C13 O13 P1 121.08(15) . . ? P2 O21 Ba1 137.54(9) . . ? P2 O22 Ba1 132.71(9) . 1_565 ? C6 N2 C2 112.35(18) . . ? C6 N2 P2 124.86(16) . . ? C2 N2 P2 122.79(16) . . ? Cl2 C1 Cl1 108.66(12) . . ? Cl2 C1 P1 110.58(12) . . ? Cl1 C1 P1 107.24(11) . . ? Cl2 C1 P2 108.68(12) . . ? Cl1 C1 P2 107.90(12) . . ? P1 C1 P2 113.63(12) . . ? N2 C2 C3 109.29(19) . . ? N2 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? N2 C2 H2B 109.8 . . ? C3 C2 H2B 109.8 . . ? H2A C2 H2B 108.3 . . ? O4 C3 C2 110.99(19) . . ? O4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? O4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O4 C5 C6 111.2(2) . . ? O4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? O4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C5 109.24(19) . . ? N2 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N2 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? O13 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? 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 O1 H1A O2 0.84 1.95 2.785(2) 170.9 3_655 O2 H2C O11 0.87 1.88 2.735(2) 171.3 3 O2 H2D O21 0.86 1.93 2.759(2) 162.7 1_545 _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.621 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.080 #===END========================================================================= data_Structure(3) _database_code_depnum_ccdc_archive 'CCDC 673865' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H29 Cl4 N2 O13.50 P4 Sr2' _chemical_formula_sum 'C12 H29 Cl4 N2 O13.50 P4 Sr2' _chemical_formula_weight 858.29 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sr Sr -1.5307 3.2498 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.1065(8) _cell_length_b 9.2205(4) _cell_length_c 28.5816(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.194(2) _cell_angle_gamma 90.00 _cell_volume 5816.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 26.00 _exptl_crystal_description diamond _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 4.317 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; The C41-C42, C42-C43, C43-C44, N4-C41, N4-C44, O33-C33, O33-C33', O2-H2B and O3-H3B bond distances were restrained using the DFIX command in SHELXL due to the relatively high thermal motions of these atoms. The anisotropic U-values of the atoms O3, C33 and C33' were restrainted to behave more isotropically using the ISOR command in SHELXL. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23619 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5672 _reflns_number_gt 4296 _reflns_threshold_expression >2sigma(I) _computing_data_collection collect _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0 (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0200P)^2^+40.0000P] 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 5672 _refine_ls_number_parameters 351 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.193 _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 Sr1 Sr 0.31944(2) 0.15917(6) 0.200928(17) 0.01688(13) Uani 1 1 d . . . Sr2 Sr 0.56980(2) -0.11445(6) 0.206660(16) 0.01476(13) Uani 1 1 d . . . Cl1 Cl 0.33364(6) -0.01978(15) 0.10525(4) 0.0212(3) Uani 1 1 d . . . Cl2 Cl 0.43747(6) -0.19040(16) 0.08011(5) 0.0260(3) Uani 1 1 d . . . Cl3 Cl 0.57939(6) -0.28801(17) 0.10374(5) 0.0269(3) Uani 1 1 d . . . Cl4 Cl 0.68522(6) -0.44654(17) 0.07508(5) 0.0278(3) Uani 1 1 d . . . P1 P 0.40261(6) -0.18425(15) 0.17987(5) 0.0158(3) Uani 1 1 d . . . P2 P 0.45684(6) 0.08690(15) 0.13385(5) 0.0160(3) Uani 1 1 d . . . P3 P 0.65583(6) -0.44363(16) 0.17564(5) 0.0176(3) Uani 1 1 d . . . P4 P 0.70093(6) -0.16653(16) 0.12757(5) 0.0175(3) Uani 1 1 d . . . O1 O 0.36224(17) 0.1341(4) 0.28700(12) 0.0223(9) Uani 1 1 d . . . H1A H 0.3286 0.1286 0.3084 0.033 Uiso 1 1 calc R . . H1B H 0.3877 0.2192 0.2959 0.033 Uiso 1 1 calc R . . O2 O 0.38215(19) 0.3934(4) 0.22326(13) 0.0322(10) Uani 1 1 d D . . H2A H 0.3739 0.4580 0.2030 0.048 Uiso 1 1 d R . . H2B H 0.4204 0.3963 0.2291 0.048 Uiso 1 1 d RD . . O3 O 0.2497(2) 0.2904(5) 0.25211(15) 0.0442(12) Uani 1 1 d DU . . H3A H 0.2696 0.3556 0.2671 0.066 Uiso 1 1 d R . . H3B H 0.2115 0.2863 0.2500 0.066 Uiso 1 1 d RD . . O4 O 0.5000 0.0704(6) 0.2500 0.0158(11) Uani 1 2 d S . . H4A H 0.5239 0.1324 0.2725 0.024 Uiso 1 1 d R . . O11 O 0.36303(15) -0.0992(4) 0.21111(11) 0.0178(8) Uani 1 1 d . . . O12 O 0.46451(15) -0.2151(4) 0.20055(12) 0.0204(8) Uani 1 1 d . . . O13 O 0.37340(17) -0.3334(4) 0.16445(13) 0.0245(9) Uani 1 1 d . . . O21 O 0.42767(15) 0.1658(4) 0.17294(12) 0.0189(8) Uani 1 1 d . . . O22 O 0.51988(15) 0.0310(4) 0.14172(11) 0.0171(8) Uani 1 1 d . . . O31 O 0.62118(17) -0.3588(4) 0.20978(13) 0.0271(9) Uani 1 1 d . . . O32 O 0.71994(16) -0.4831(4) 0.18888(12) 0.0225(9) Uani 1 1 d . . . O33 O 0.62155(18) -0.5918(4) 0.16253(14) 0.0324(10) Uani 1 1 d D . . O41 O 0.66902(16) -0.0888(4) 0.16521(12) 0.0225(9) Uani 1 1 d . . . O42 O 0.76532(15) -0.2119(4) 0.13589(12) 0.0184(8) Uani 1 1 d . . . N2 N 0.44954(19) 0.1868(5) 0.08676(15) 0.0216(11) Uani 1 1 d . . . N4 N 0.69281(18) -0.0747(5) 0.07920(15) 0.0306(13) Uani 1 1 d D . . C1 C 0.4087(2) -0.0786(6) 0.12505(17) 0.0165(11) Uani 1 1 d . . . C2 C 0.6566(2) -0.3372(6) 0.12066(18) 0.0182(12) Uani 1 1 d . . . C13 C 0.3110(3) -0.3545(8) 0.1495(3) 0.054(2) Uani 1 1 d . . . H13A H 0.2864 -0.2773 0.1624 0.081 Uiso 1 1 calc R . . H13B H 0.2973 -0.4488 0.1606 0.081 Uiso 1 1 calc R . . H13C H 0.3067 -0.3518 0.1152 0.081 Uiso 1 1 calc R . . C21 C 0.4861(3) 0.1738(7) 0.04543(19) 0.0307(15) Uani 1 1 d . . . H21A H 0.4692 0.0995 0.0234 0.037 Uiso 1 1 calc R . . H21B H 0.5287 0.1490 0.0546 0.037 Uiso 1 1 calc R . . C22 C 0.4813(3) 0.3248(8) 0.0241(2) 0.0405(17) Uani 1 1 d . . . H22A H 0.5125 0.3902 0.0386 0.049 Uiso 1 1 calc R . . H22B H 0.4860 0.3214 -0.0101 0.049 Uiso 1 1 calc R . . C23 C 0.4183(3) 0.3747(9) 0.0348(2) 0.053(2) Uani 1 1 d . . . H23A H 0.4159 0.4819 0.0352 0.064 Uiso 1 1 calc R . . H23B H 0.3877 0.3368 0.0113 0.064 Uiso 1 1 calc R . . C24 C 0.4085(3) 0.3138(7) 0.0822(2) 0.0369(16) Uani 1 1 d . . . H24A H 0.4189 0.3863 0.1069 0.044 Uiso 1 1 calc R . . H24B H 0.3658 0.2838 0.0846 0.044 Uiso 1 1 calc R . . C33 C 0.5540(4) -0.5945(11) 0.1652(3) 0.034(2) Uani 0.70 1 d PDU . . H33A H 0.5350 -0.5466 0.1375 0.052 Uiso 0.70 1 calc PR . . H33B H 0.5427 -0.5434 0.1935 0.052 Uiso 0.70 1 calc PR . . H33C H 0.5400 -0.6953 0.1663 0.052 Uiso 0.70 1 calc PR . . C33' C 0.5645(8) -0.618(3) 0.1401(8) 0.038(5) Uani 0.30 1 d PDU . . H33D H 0.5588 -0.7227 0.1358 0.057 Uiso 0.30 1 calc PR . . H33E H 0.5621 -0.5700 0.1095 0.057 Uiso 0.30 1 calc PR . . H33F H 0.5329 -0.5798 0.1594 0.057 Uiso 0.30 1 calc PR . . C41 C 0.7333(2) -0.0761(5) 0.04013(17) 0.0315(15) Uani 1 1 d D . . H41A H 0.7193 -0.1469 0.0159 0.038 Uiso 1 1 calc R . . H41B H 0.7753 -0.1008 0.0513 0.038 Uiso 1 1 calc R . . C42 C 0.7298(3) 0.0778(5) 0.0211(2) 0.0332(15) Uani 1 1 d D . . H42A H 0.7643 0.1361 0.0342 0.040 Uiso 1 1 calc R . . H42B H 0.7310 0.0772 -0.0135 0.040 Uiso 1 1 calc R . . C43 C 0.6703(3) 0.1408(7) 0.0358(3) 0.066(3) Uani 1 1 d D . . H43A H 0.6770 0.2375 0.0502 0.079 Uiso 1 1 calc R . . H43B H 0.6413 0.1510 0.0083 0.079 Uiso 1 1 calc R . . C44 C 0.6456(3) 0.0361(8) 0.0711(3) 0.078(3) Uani 1 1 d D . . H44A H 0.6074 -0.0086 0.0584 0.094 Uiso 1 1 calc R . . H44B H 0.6377 0.0869 0.1006 0.094 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 Sr1 0.0144(2) 0.0165(3) 0.0198(3) -0.0006(2) 0.00121(19) 0.0036(2) Sr2 0.0107(2) 0.0150(3) 0.0186(3) -0.0010(2) 0.00086(18) 0.0012(2) Cl1 0.0146(6) 0.0250(8) 0.0235(7) -0.0008(6) -0.0025(5) 0.0031(5) Cl2 0.0239(7) 0.0289(8) 0.0251(7) -0.0090(6) 0.0005(6) 0.0053(6) Cl3 0.0172(7) 0.0306(9) 0.0322(8) -0.0031(7) -0.0065(6) 0.0076(6) Cl4 0.0276(8) 0.0295(9) 0.0261(7) -0.0109(6) -0.0018(6) 0.0091(6) P1 0.0134(6) 0.0120(7) 0.0219(7) -0.0005(6) -0.0006(5) -0.0004(5) P2 0.0136(7) 0.0158(8) 0.0187(7) 0.0012(6) 0.0021(5) 0.0012(6) P3 0.0137(7) 0.0115(7) 0.0272(8) 0.0003(6) -0.0008(6) -0.0006(6) P4 0.0161(7) 0.0150(7) 0.0217(7) 0.0023(6) 0.0046(5) 0.0030(6) O1 0.026(2) 0.016(2) 0.024(2) -0.0023(17) -0.0008(16) -0.0013(17) O2 0.040(3) 0.020(2) 0.037(2) 0.0032(19) 0.0057(19) -0.004(2) O3 0.0413(14) 0.0461(15) 0.0452(14) -0.0058(9) 0.0015(9) 0.0015(9) O4 0.013(2) 0.018(3) 0.017(3) 0.000 0.000(2) 0.000 O11 0.0192(19) 0.015(2) 0.0187(18) 0.0021(16) 0.0007(14) 0.0015(16) O12 0.0135(18) 0.021(2) 0.026(2) 0.0057(17) -0.0012(15) -0.0007(16) O13 0.024(2) 0.016(2) 0.033(2) -0.0032(18) -0.0063(17) -0.0047(17) O21 0.0142(18) 0.016(2) 0.027(2) 0.0004(17) 0.0025(15) 0.0014(16) O22 0.0146(18) 0.018(2) 0.0183(18) 0.0005(16) 0.0014(14) -0.0010(16) O31 0.025(2) 0.021(2) 0.037(2) 0.0096(19) 0.0149(17) 0.0067(18) O32 0.0178(19) 0.023(2) 0.027(2) 0.0064(17) -0.0001(15) -0.0009(17) O33 0.033(2) 0.018(2) 0.044(2) 0.0038(19) -0.0164(19) -0.0084(19) O41 0.022(2) 0.015(2) 0.032(2) -0.0023(17) 0.0124(16) -0.0007(16) O42 0.0165(19) 0.016(2) 0.0230(19) 0.0031(16) 0.0022(15) 0.0025(15) N2 0.016(2) 0.026(3) 0.024(2) 0.008(2) 0.0060(18) 0.006(2) N4 0.020(3) 0.038(3) 0.035(3) 0.023(2) 0.010(2) 0.013(2) C1 0.011(2) 0.019(3) 0.020(3) -0.003(2) 0.000(2) 0.002(2) C2 0.013(3) 0.018(3) 0.024(3) -0.004(2) 0.000(2) 0.006(2) C13 0.043(4) 0.031(4) 0.085(6) 0.002(4) -0.032(4) -0.017(3) C21 0.034(3) 0.035(4) 0.023(3) 0.009(3) 0.007(3) 0.009(3) C22 0.050(4) 0.041(4) 0.032(3) 0.010(3) 0.014(3) 0.004(4) C23 0.065(5) 0.052(5) 0.044(4) 0.021(4) 0.017(4) 0.030(4) C24 0.030(3) 0.035(4) 0.046(4) 0.022(3) 0.004(3) 0.009(3) C33 0.034(2) 0.034(2) 0.035(2) 0.0002(10) 0.0010(10) -0.0007(10) C33' 0.038(5) 0.038(5) 0.038(5) 0.0000(10) 0.0019(11) -0.0001(10) C41 0.033(3) 0.037(4) 0.026(3) 0.007(3) 0.008(3) 0.004(3) C42 0.045(4) 0.028(4) 0.028(3) 0.009(3) 0.013(3) 0.002(3) C43 0.089(6) 0.040(5) 0.073(5) 0.029(4) 0.052(5) 0.033(5) C44 0.046(5) 0.085(7) 0.107(7) 0.077(6) 0.038(5) 0.045(5) _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 Sr1 O42 2.460(3) 3_455 ? Sr1 O3 2.496(4) . ? Sr1 O21 2.565(3) . ? Sr1 O32 2.568(4) 3_455 ? Sr1 O11 2.581(4) . ? Sr1 O1 2.596(3) . ? Sr1 O2 2.626(4) . ? Sr1 Cl1 3.2241(14) . ? Sr1 P4 3.6375(14) 3_455 ? Sr1 P1 3.7273(15) . ? Sr1 P2 3.7409(14) . ? Sr1 Sr2 4.3145(7) 2_655 ? Sr1 H3A 2.8820 . ? Sr2 O22 2.497(3) . ? Sr2 O12 2.503(3) . ? Sr2 O31 2.523(4) . ? Sr2 O41 2.561(3) . ? Sr2 O4 2.652(3) . ? Sr2 O11 2.713(3) 2_655 ? Sr2 O1 2.741(4) 2_655 ? Sr2 O12 2.948(4) 2_655 ? Sr2 P1 3.3291(14) 2_655 ? Sr2 Cl3 3.3658(15) . ? Sr2 P2 3.6652(14) . ? Sr2 P3 3.7153(15) . ? Cl1 C1 1.807(5) . ? Cl2 C1 1.791(5) . ? Cl3 C2 1.806(5) . ? Cl4 C2 1.790(5) . ? P1 O12 1.487(4) . ? P1 O11 1.505(4) . ? P1 O13 1.572(4) . ? P1 C1 1.856(5) . ? P1 Sr2 3.3292(14) 2_655 ? P2 O22 1.491(4) . ? P2 O21 1.508(4) . ? P2 N2 1.632(5) . ? P2 C1 1.869(5) . ? P3 O31 1.495(4) . ? P3 O32 1.492(4) . ? P3 O33 1.597(4) . ? P3 C2 1.854(5) . ? P4 O42 1.490(4) . ? P4 O41 1.501(4) . ? P4 N4 1.623(4) . ? P4 C2 1.858(6) . ? P4 Sr1 3.6374(14) 3_545 ? O1 Sr2 2.741(4) 2_655 ? O1 H1A 0.9900 . ? O1 H1B 0.9900 . ? O2 H2A 0.8445 . ? O2 H2B 0.8532 . ? O3 H3A 0.8466 . ? O3 H3B 0.8456 . ? O4 Sr2 2.652(3) 2_655 ? O4 H4A 0.9900 . ? O11 Sr2 2.713(3) 2_655 ? O12 Sr2 2.949(4) 2_655 ? O13 C13 1.434(7) . ? O32 Sr1 2.568(4) 3_545 ? O33 C33' 1.403(15) . ? O33 C33 1.501(9) . ? O42 Sr1 2.460(3) 3_545 ? N2 C21 1.473(7) . ? N2 C24 1.483(7) . ? N4 C44 1.4695(10) . ? N4 C41 1.4699(10) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C21 C22 1.521(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.514(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.493(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C33' H33D 0.9800 . ? C33' H33E 0.9800 . ? C33' H33F 0.9800 . ? C41 C42 1.5199(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.5196(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.5186(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 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 O42 Sr1 O3 85.32(13) 3_455 . ? O42 Sr1 O21 100.11(11) 3_455 . ? O3 Sr1 O21 142.01(14) . . ? O42 Sr1 O32 76.63(11) 3_455 3_455 ? O3 Sr1 O32 76.95(14) . 3_455 ? O21 Sr1 O32 141.00(12) . 3_455 ? O42 Sr1 O11 133.96(11) 3_455 . ? O3 Sr1 O11 128.35(13) . . ? O21 Sr1 O11 73.05(11) . . ? O32 Sr1 O11 81.66(11) 3_455 . ? O42 Sr1 O1 153.54(12) 3_455 . ? O3 Sr1 O1 72.08(13) . . ? O21 Sr1 O1 90.03(11) . . ? O32 Sr1 O1 110.23(11) 3_455 . ? O11 Sr1 O1 72.35(11) . . ? O42 Sr1 O2 90.81(13) 3_455 . ? O3 Sr1 O2 78.09(14) . . ? O21 Sr1 O2 64.35(12) . . ? O32 Sr1 O2 152.82(13) 3_455 . ? O11 Sr1 O2 122.91(12) . . ? O1 Sr1 O2 71.54(12) . . ? O42 Sr1 Cl1 70.88(9) 3_455 . ? O3 Sr1 Cl1 146.89(11) . . ? O21 Sr1 Cl1 67.12(8) . . ? O32 Sr1 Cl1 75.39(9) 3_455 . ? O11 Sr1 Cl1 64.52(8) . . ? O1 Sr1 Cl1 135.28(9) . . ? O2 Sr1 Cl1 123.51(9) . . ? O42 Sr1 P4 17.56(8) 3_455 3_455 ? O3 Sr1 P4 71.05(10) . 3_455 ? O21 Sr1 P4 117.64(8) . 3_455 ? O32 Sr1 P4 64.18(8) 3_455 3_455 ? O11 Sr1 P4 136.50(8) . 3_455 ? O1 Sr1 P4 142.97(9) . 3_455 ? O2 Sr1 P4 97.48(10) . 3_455 ? Cl1 Sr1 P4 80.69(3) . 3_455 ? O42 Sr1 P1 120.79(9) 3_455 . ? O3 Sr1 P1 146.39(11) . . ? O21 Sr1 P1 59.53(8) . . ? O32 Sr1 P1 88.32(9) 3_455 . ? O11 Sr1 P1 18.08(8) . . ? O1 Sr1 P1 85.43(8) . . ? O2 Sr1 P1 118.65(9) . . ? Cl1 Sr1 P1 49.91(3) . . ? P4 Sr1 P1 128.91(3) 3_455 . ? O42 Sr1 P2 94.20(8) 3_455 . ? O3 Sr1 P2 158.76(12) . . ? O21 Sr1 P2 17.54(8) . . ? O32 Sr1 P2 123.65(9) 3_455 . ? O11 Sr1 P2 65.46(8) . . ? O1 Sr1 P2 101.90(8) . . ? O2 Sr1 P2 80.69(9) . . ? Cl1 Sr1 P2 49.76(3) . . ? P4 Sr1 P2 111.26(3) 3_455 . ? P1 Sr1 P2 49.00(3) . . ? O42 Sr1 Sr2 168.70(8) 3_455 2_655 ? O3 Sr1 Sr2 105.82(10) . 2_655 ? O21 Sr1 Sr2 72.39(8) . 2_655 ? O32 Sr1 Sr2 103.65(8) 3_455 2_655 ? O11 Sr1 Sr2 36.43(7) . 2_655 ? O1 Sr1 Sr2 37.20(8) . 2_655 ? O2 Sr1 Sr2 93.34(9) . 2_655 ? Cl1 Sr1 Sr2 98.12(3) . 2_655 ? P4 Sr1 Sr2 167.74(3) 3_455 2_655 ? P1 Sr1 Sr2 48.23(2) . 2_655 ? P2 Sr1 Sr2 76.13(2) . 2_655 ? O42 Sr1 H3A 90.3 3_455 . ? O3 Sr1 H3A 16.2 . . ? O21 Sr1 H3A 125.9 . . ? O32 Sr1 H3A 93.1 3_455 . ? O11 Sr1 H3A 131.3 . . ? O1 Sr1 H3A 64.3 . . ? O2 Sr1 H3A 62.6 . . ? Cl1 Sr1 H3A 159.6 . . ? P4 Sr1 H3A 79.1 3_455 . ? P1 Sr1 H3A 148.2 . . ? P2 Sr1 H3A 143.1 . . ? Sr2 Sr1 H3A 101.0 2_655 . ? O22 Sr2 O12 77.09(11) . . ? O22 Sr2 O31 133.28(12) . . ? O12 Sr2 O31 94.95(13) . . ? O22 Sr2 O41 87.76(11) . . ? O12 Sr2 O41 144.99(12) . . ? O31 Sr2 O41 72.75(12) . . ? O22 Sr2 O4 75.96(9) . . ? O12 Sr2 O4 73.02(11) . . ? O31 Sr2 O4 146.10(11) . . ? O41 Sr2 O4 133.80(12) . . ? O22 Sr2 O11 144.51(11) . 2_655 ? O12 Sr2 O11 122.80(11) . 2_655 ? O31 Sr2 O11 77.98(12) . 2_655 ? O41 Sr2 O11 87.39(11) . 2_655 ? O4 Sr2 O11 82.35(8) . 2_655 ? O22 Sr2 O1 79.51(11) . 2_655 ? O12 Sr2 O1 144.98(12) . 2_655 ? O31 Sr2 O1 120.03(12) . 2_655 ? O41 Sr2 O1 58.19(11) . 2_655 ? O4 Sr2 O1 76.28(11) . 2_655 ? O11 Sr2 O1 68.15(10) 2_655 2_655 ? O22 Sr2 O12 135.45(10) . 2_655 ? O12 Sr2 O12 70.20(12) . 2_655 ? O31 Sr2 O12 79.91(11) . 2_655 ? O41 Sr2 O12 135.64(11) . 2_655 ? O4 Sr2 O12 66.22(10) . 2_655 ? O11 Sr2 O12 52.62(10) 2_655 2_655 ? O1 Sr2 O12 111.79(10) 2_655 2_655 ? O22 Sr2 P1 151.34(8) . 2_655 ? O12 Sr2 P1 96.63(8) . 2_655 ? O31 Sr2 P1 74.64(9) . 2_655 ? O41 Sr2 P1 110.69(9) . 2_655 ? O4 Sr2 P1 75.46(5) . 2_655 ? O11 Sr2 P1 26.41(8) 2_655 2_655 ? O1 Sr2 P1 91.56(8) 2_655 2_655 ? O12 Sr2 P1 26.53(7) 2_655 2_655 ? O22 Sr2 Cl3 69.66(8) . . ? O12 Sr2 Cl3 82.32(9) . . ? O31 Sr2 Cl3 63.65(9) . . ? O41 Sr2 Cl3 62.77(9) . . ? O4 Sr2 Cl3 141.30(3) . . ? O11 Sr2 Cl3 136.35(8) 2_655 . ? O1 Sr2 Cl3 113.23(8) 2_655 . ? O12 Sr2 Cl3 131.93(8) 2_655 . ? P1 Sr2 Cl3 137.94(4) 2_655 . ? O22 Sr2 P2 17.61(8) . . ? O12 Sr2 P2 63.05(9) . . ? O31 Sr2 P2 139.79(10) . . ? O41 Sr2 P2 105.33(9) . . ? O4 Sr2 P2 62.87(4) . . ? O11 Sr2 P2 142.04(8) 2_655 . ? O1 Sr2 P2 88.15(8) 2_655 . ? O12 Sr2 P2 117.96(7) 2_655 . ? P1 Sr2 P2 137.14(3) 2_655 . ? Cl3 Sr2 P2 79.55(3) . . ? O22 Sr2 P3 118.19(8) . . ? O12 Sr2 P3 99.60(9) . . ? O31 Sr2 P3 16.92(8) . . ? O41 Sr2 P3 60.15(9) . . ? O4 Sr2 P3 162.82(8) . . ? O11 Sr2 P3 89.21(8) 2_655 . ? O1 Sr2 P3 114.38(8) 2_655 . ? O12 Sr2 P3 96.79(8) 2_655 . ? P1 Sr2 P3 90.35(3) 2_655 . ? Cl3 Sr2 P3 49.08(3) . . ? P2 Sr2 P3 128.31(3) . . ? C1 Cl1 Sr1 91.10(16) . . ? C2 Cl3 Sr2 89.43(17) . . ? O12 P1 O11 114.6(2) . . ? O12 P1 O13 107.4(2) . . ? O11 P1 O13 112.2(2) . . ? O12 P1 C1 109.1(2) . . ? O11 P1 C1 107.4(2) . . ? O13 P1 C1 105.7(2) . . ? O12 P1 Sr2 62.31(15) . 2_655 ? O11 P1 Sr2 53.29(13) . 2_655 ? O13 P1 Sr2 119.49(15) . 2_655 ? C1 P1 Sr2 134.65(17) . 2_655 ? O12 P1 Sr1 123.33(16) . . ? O11 P1 Sr1 32.15(14) . . ? O13 P1 Sr1 126.15(15) . . ? C1 P1 Sr1 75.54(16) . . ? Sr2 P1 Sr1 75.15(3) 2_655 . ? O22 P2 O21 119.3(2) . . ? O22 P2 N2 111.6(2) . . ? O21 P2 N2 108.2(2) . . ? O22 P2 C1 105.0(2) . . ? O21 P2 C1 103.3(2) . . ? N2 P2 C1 108.7(2) . . ? O22 P2 Sr2 30.44(13) . . ? O21 P2 Sr2 97.45(14) . . ? N2 P2 Sr2 141.94(16) . . ? C1 P2 Sr2 91.57(16) . . ? O22 P2 Sr1 139.73(14) . . ? O21 P2 Sr1 30.83(14) . . ? N2 P2 Sr1 106.05(16) . . ? C1 P2 Sr1 75.06(16) . . ? Sr2 P2 Sr1 110.25(3) . . ? O31 P3 O32 118.4(2) . . ? O31 P3 O33 110.3(2) . . ? O32 P3 O33 106.4(2) . . ? O31 P3 C2 107.8(2) . . ? O32 P3 C2 106.9(2) . . ? O33 P3 C2 106.3(2) . . ? O31 P3 Sr2 29.43(15) . . ? O32 P3 Sr2 129.10(16) . . ? O33 P3 Sr2 120.84(16) . . ? C2 P3 Sr2 78.39(17) . . ? O42 P4 O41 120.2(2) . . ? O42 P4 N4 110.0(2) . . ? O41 P4 N4 109.1(2) . . ? O42 P4 C2 105.8(2) . . ? O41 P4 C2 102.4(2) . . ? N4 P4 C2 108.6(3) . . ? O42 P4 Sr1 29.88(14) . 3_545 ? O41 P4 Sr1 98.64(15) . 3_545 ? N4 P4 Sr1 139.79(15) . 3_545 ? C2 P4 Sr1 92.62(16) . 3_545 ? Sr1 O1 Sr2 107.86(12) . 2_655 ? Sr1 O1 H1A 110.1 . . ? Sr2 O1 H1A 110.1 2_655 . ? Sr1 O1 H1B 110.1 . . ? Sr2 O1 H1B 110.1 2_655 . ? H1A O1 H1B 108.4 . . ? Sr1 O2 H2A 108.8 . . ? Sr1 O2 H2B 125.3 . . ? H2A O2 H2B 106.6 . . ? Sr1 O3 H3A 108.7 . . ? Sr1 O3 H3B 125.8 . . ? H3A O3 H3B 123.8 . . ? Sr2 O4 Sr2 100.01(17) 2_655 . ? Sr2 O4 H4A 111.8 2_655 . ? Sr2 O4 H4A 111.8 . . ? P1 O11 Sr1 129.77(19) . . ? P1 O11 Sr2 100.30(16) . 2_655 ? Sr1 O11 Sr2 109.17(12) . 2_655 ? P1 O12 Sr2 142.0(2) . . ? P1 O12 Sr2 91.16(17) . 2_655 ? Sr2 O12 Sr2 96.04(11) . 2_655 ? C13 O13 P1 125.1(4) . . ? P2 O21 Sr1 131.6(2) . . ? P2 O22 Sr2 131.9(2) . . ? P3 O31 Sr2 133.6(2) . . ? P3 O32 Sr1 134.7(2) . 3_545 ? C33' O33 C33 31.6(9) . . ? C33' O33 P3 131.1(11) . . ? C33 O33 P3 117.6(5) . . ? P4 O41 Sr2 137.4(2) . . ? P4 O42 Sr1 132.6(2) . 3_545 ? C21 N2 C24 110.8(4) . . ? C21 N2 P2 125.6(4) . . ? C24 N2 P2 123.4(4) . . ? C44 N4 C41 110.1(4) . . ? C44 N4 P4 122.8(3) . . ? C41 N4 P4 126.8(3) . . ? Cl2 C1 Cl1 107.7(3) . . ? Cl2 C1 P1 110.4(3) . . ? Cl1 C1 P1 108.2(3) . . ? Cl2 C1 P2 110.1(3) . . ? Cl1 C1 P2 107.6(3) . . ? P1 C1 P2 112.5(3) . . ? Cl4 C2 Cl3 108.3(3) . . ? Cl4 C2 P4 110.4(3) . . ? Cl3 C2 P4 107.5(3) . . ? Cl4 C2 P3 109.8(3) . . ? Cl3 C2 P3 107.8(3) . . ? P4 C2 P3 112.8(3) . . ? O13 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C21 C22 102.5(5) . . ? N2 C21 H21A 111.3 . . ? C22 C21 H21A 111.3 . . ? N2 C21 H21B 111.3 . . ? C22 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C23 C22 C21 104.0(5) . . ? C23 C22 H22A 111.0 . . ? C21 C22 H22A 111.0 . . ? C23 C22 H22B 111.0 . . ? C21 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? C24 C23 C22 104.5(5) . . ? C24 C23 H23A 110.8 . . ? C22 C23 H23A 110.8 . . ? C24 C23 H23B 110.8 . . ? C22 C23 H23B 110.8 . . ? H23A C23 H23B 108.9 . . ? N2 C24 C23 104.9(5) . . ? N2 C24 H24A 110.8 . . ? C23 C24 H24A 110.8 . . ? N2 C24 H24B 110.8 . . ? C23 C24 H24B 110.8 . . ? H24A C24 H24B 108.8 . . ? O33 C33 H33A 109.5 . . ? O33 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O33 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O33 C33' H33D 109.5 . . ? O33 C33' H33E 109.5 . . ? H33D C33' H33E 109.5 . . ? O33 C33' H33F 109.5 . . ? H33D C33' H33F 109.5 . . ? H33E C33' H33F 109.5 . . ? N4 C41 C42 104.0(4) . . ? N4 C41 H41A 110.9 . . ? C42 C41 H41A 110.9 . . ? N4 C41 H41B 110.9 . . ? C42 C41 H41B 110.9 . . ? H41A C41 H41B 109.0 . . ? C43 C42 C41 106.6(4) . . ? C43 C42 H42A 110.4 . . ? C41 C42 H42A 110.4 . . ? C43 C42 H42B 110.4 . . ? C41 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C44 C43 C42 106.8(4) . . ? C44 C43 H43A 110.4 . . ? C42 C43 H43A 110.4 . . ? C44 C43 H43B 110.4 . . ? C42 C43 H43B 110.4 . . ? H43A C43 H43B 108.6 . . ? C43 C44 N4 105.6(4) . . ? C43 C44 H44A 110.6 . . ? N4 C44 H44A 110.6 . . ? C43 C44 H44B 110.6 . . ? N4 C44 H44B 110.6 . . ? H44A C44 H44B 108.8 . . ? 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 O1 H1B O33 0.99 2.13 2.922(5) 136.2 2_665 O2 H2A O13 0.84 2.22 3.028(6) 161.5 1_565 O3 H3B O11 0.85 2.29 2.940(6) 133.4 4 O3 H3B O31 0.85 2.62 3.324(6) 142.2 3_455 O4 H4A O21 0.99 1.87 2.791(4) 153.8 2_655 O1 H1A O41 0.99 2.14 2.583(5) 105.1 2_655 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.820 _refine_diff_density_min -0.857 _refine_diff_density_rms 0.140