# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author 'Dr. Simon M. Humphrey' _publ_contact_author_email smh@cm.utexas.edu loop_ _publ_author_name 'Ilich A. Ibarra' 'Kristina E. Tan' 'Vincent M. Lynch' 'Simon M. Humphrey' _publ_contact_author_name 'Dr. Simon M. Humphrey' data_sh11002 _database_code_depnum_ccdc_archive 'CCDC 849683' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'PCM-14 (180 K)' _chemical_melting_point ? _chemical_formula_moiety 'C22 H21 Ca O9 P, 2(H2 O)' _chemical_formula_sum 'C22 H25 Ca O11 P' _chemical_formula_weight 532.44 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 17.1078(9) _cell_length_b 17.1078(9) _cell_length_c 17.1078(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5007.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 2174 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 25.03 _exptl_crystal_description Shard _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.955 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 4088 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4088 _reflns_number_gt 2917 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0417P)^2^+5.4934P] 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_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -9(3) _refine_ls_number_reflns 4088 _refine_ls_number_parameters 126 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.032 _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 Ca1 Ca 0.66297(4) 0.33703(4) 0.83703(4) 0.0555(3) Uani 1 3 d S . . P1 P 0.54508(5) 0.04508(5) 0.45492(5) 0.0489(4) Uani 1 3 d S . . O1 O 0.6509(2) 0.33082(15) 0.70539(17) 0.1149(12) Uani 1 1 d . A . O2 O 0.65384(17) 0.39721(16) 0.59537(17) 0.0871(9) Uani 1 1 d . A . O3 O 0.6826(5) 0.3822(9) 0.9728(3) 0.052(4) Uani 0.47(2) 1 d PD A 1 H3A H 0.6445(15) 0.3590(18) 0.997(2) 0.078 Uiso 0.47(2) 1 d PD A 1 H4A H 0.7169(10) 0.3465(17) 0.980(2) 0.078 Uiso 0.47(2) 1 d PD A 1 O3' O 0.6727(4) 0.3282(11) 0.9691(4) 0.078(4) Uani 0.53(2) 1 d PD A 2 H3A' H 0.6445(15) 0.3590(18) 0.997(2) 0.117 Uiso 0.53 1 d PD A 2 H4A' H 0.7169(10) 0.3465(17) 0.980(2) 0.117 Uiso 0.53 1 d PD A 2 C1P C 0.4854(2) -0.0146(2) 0.5146(2) 0.073(2) Uani 1 3 d S . . H1P H 0.4728 -0.0551 0.4899 0.110 Uiso 1 1 calc R . . C7 C 0.6446(2) 0.3358(2) 0.6344(2) 0.0680(10) Uani 1 1 d . . . C2 C 0.57210(19) 0.13108(19) 0.5890(2) 0.0543(9) Uani 1 1 d . A . H2 H 0.5551 0.0862 0.6170 0.065 Uiso 1 1 calc R . . C4 C 0.6212(2) 0.2642(2) 0.5899(2) 0.0535(9) Uani 1 1 d . A . C6 C 0.5965(2) 0.1967(2) 0.46908(19) 0.0623(10) Uani 1 1 d . A . H6 H 0.5962 0.1974 0.4136 0.075 Uiso 1 1 calc R . . C1 C 0.57321(19) 0.13101(17) 0.50753(19) 0.0464(9) Uani 1 1 d . . . C5 C 0.6207(2) 0.2632(2) 0.5098(2) 0.0710(11) Uani 1 1 d . . . H5 H 0.6371 0.3082 0.4817 0.085 Uiso 1 1 calc R A . C3 C 0.5963(2) 0.1980(2) 0.6288(2) 0.0623(10) Uani 1 1 d . . . H3 H 0.5956 0.1981 0.6844 0.075 Uiso 1 1 calc R A . O100 O 0.5000 -0.2500 0.4709(3) 0.1351(18) Uani 1 2 d S . . O101 O 0.7040(3) 0.2040(3) 0.2960(3) 0.091(3) Uani 0.50 3 d SP . . 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 Ca1 0.0555(3) 0.0555(3) 0.0555(3) -0.0039(4) 0.0039(4) 0.0039(4) P1 0.0489(4) 0.0489(4) 0.0489(4) -0.0106(5) -0.0106(5) 0.0106(5) O1 0.213(4) 0.0669(19) 0.0646(19) -0.0281(15) -0.060(2) 0.022(2) O2 0.127(2) 0.0475(16) 0.0867(19) -0.0152(16) -0.0212(18) 0.0018(17) O3 0.052(4) 0.074(8) 0.030(3) 0.001(3) 0.008(2) -0.004(4) O3' 0.057(4) 0.110(10) 0.067(4) -0.010(4) 0.010(3) -0.015(4) C1P 0.073(2) 0.073(2) 0.073(2) -0.003(2) -0.003(2) 0.003(2) C7 0.088(3) 0.054(2) 0.062(2) -0.021(2) -0.029(2) 0.021(2) C2 0.059(2) 0.055(2) 0.049(2) -0.0070(17) -0.0075(17) 0.0156(16) C4 0.070(2) 0.042(2) 0.049(2) -0.0062(18) -0.0195(18) 0.0167(17) C6 0.097(3) 0.052(2) 0.038(2) -0.0132(17) -0.0158(19) 0.016(2) C1 0.060(2) 0.0367(18) 0.0425(19) -0.0086(15) -0.0154(15) 0.0208(16) C5 0.110(3) 0.043(2) 0.060(3) -0.0053(19) -0.016(2) 0.015(2) C3 0.079(3) 0.065(2) 0.043(2) -0.0236(19) -0.0135(19) 0.024(2) O100 0.124(4) 0.209(6) 0.072(3) 0.000 0.000 -0.006(4) O101 0.091(3) 0.091(3) 0.091(3) 0.012(3) 0.012(3) -0.012(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 Ca1 O1 2.264(3) . ? Ca1 O1 2.264(3) 7_665 ? Ca1 O1 2.264(3) 10_646 ? Ca1 O3' 2.271(6) 7_665 ? Ca1 O3' 2.271(6) 10_646 ? Ca1 O3' 2.271(6) . ? Ca1 O3 2.471(8) 10_646 ? Ca1 O3 2.471(8) . ? Ca1 O3 2.471(8) 7_665 ? Ca1 H3A 2.78(3) . ? Ca1 H4A 2.62(4) . ? Ca1 H3A' 2.78(3) . ? Ca1 H4A' 2.62(4) . ? P1 C1P 1.769(6) . ? P1 C1 1.790(3) . ? P1 C1 1.790(3) 8_645 ? P1 C1 1.790(3) 11_556 ? O1 C7 1.222(4) . ? O2 C7 1.256(5) . ? O3 H3A 0.867(18) . ? O3 H4A 0.856(18) . ? O3 H3A' 0.867(18) . ? O3 H4A' 0.856(18) . ? O3' H3A 0.857(18) . ? O3' H4A 0.838(18) . ? O3' H3A' 0.857(18) . ? O3' H4A' 0.838(18) . ? C1P H1P 0.8400 . ? C7 C4 1.497(5) . ? C2 C1 1.394(4) . ? C2 C3 1.395(4) . ? C2 H2 0.9500 . ? C4 C5 1.370(5) . ? C4 C3 1.380(5) . ? C6 C1 1.362(4) . ? C6 C5 1.397(5) . ? C6 H6 0.9500 . ? C5 H5 0.9500 . ? C3 H3 0.9500 . ? 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 O1 Ca1 O1 92.76(12) . 7_665 ? O1 Ca1 O1 92.76(12) . 10_646 ? O1 Ca1 O1 92.76(12) 7_665 10_646 ? O1 Ca1 O3' 80.8(5) . 7_665 ? O1 Ca1 O3' 173.4(5) 7_665 7_665 ? O1 Ca1 O3' 88.8(2) 10_646 7_665 ? O1 Ca1 O3' 88.84(19) . 10_646 ? O1 Ca1 O3' 80.8(5) 7_665 10_646 ? O1 Ca1 O3' 173.4(5) 10_646 10_646 ? O3' Ca1 O3' 97.7(4) 7_665 10_646 ? O1 Ca1 O3' 173.4(5) . . ? O1 Ca1 O3' 88.84(19) 7_665 . ? O1 Ca1 O3' 80.8(5) 10_646 . ? O3' Ca1 O3' 97.7(4) 7_665 . ? O3' Ca1 O3' 97.7(4) 10_646 . ? O1 Ca1 O3 83.14(19) . 10_646 ? O1 Ca1 O3 102.7(3) 7_665 10_646 ? O1 Ca1 O3 164.2(3) 10_646 10_646 ? O3' Ca1 O3 75.4(3) 7_665 10_646 ? O3' Ca1 O3 22.4(2) 10_646 10_646 ? O3' Ca1 O3 102.8(4) . 10_646 ? O1 Ca1 O3 164.2(3) . . ? O1 Ca1 O3 83.1(2) 7_665 . ? O1 Ca1 O3 102.7(3) 10_646 . ? O3' Ca1 O3 102.8(4) 7_665 . ? O3' Ca1 O3 75.4(3) 10_646 . ? O3' Ca1 O3 22.4(2) . . ? O3 Ca1 O3 82.9(3) 10_646 . ? O1 Ca1 O3 102.7(3) . 7_665 ? O1 Ca1 O3 164.2(3) 7_665 7_665 ? O1 Ca1 O3 83.1(2) 10_646 7_665 ? O3' Ca1 O3 22.4(2) 7_665 7_665 ? O3' Ca1 O3 102.8(4) 10_646 7_665 ? O3' Ca1 O3 75.4(3) . 7_665 ? O3 Ca1 O3 82.9(3) 10_646 7_665 ? O3 Ca1 O3 82.9(3) . 7_665 ? O1 Ca1 H3A 167.2(6) . . ? O1 Ca1 H3A 98.5(6) 7_665 . ? O1 Ca1 H3A 92.9(7) 10_646 . ? O3' Ca1 H3A 87.8(7) 7_665 . ? O3' Ca1 H3A 86.9(7) 10_646 . ? O3' Ca1 H3A 15.8(7) . . ? O3 Ca1 H3A 88.3(6) 10_646 . ? O3 Ca1 H3A 17.8(5) . . ? O3 Ca1 H3A 66.6(6) 7_665 . ? O1 Ca1 H4A 164.6(6) . . ? O1 Ca1 H4A 71.8(6) 7_665 . ? O1 Ca1 H4A 87.7(6) 10_646 . ? O3' Ca1 H4A 114.7(7) 7_665 . ? O3' Ca1 H4A 89.1(6) 10_646 . ? O3' Ca1 H4A 18.0(6) . . ? O3 Ca1 H4A 100.3(6) 10_646 . ? O3 Ca1 H4A 19.1(5) . . ? O3 Ca1 H4A 92.7(6) 7_665 . ? H3A Ca1 H4A 27.4(6) . . ? O1 Ca1 H3A' 167.2(6) . . ? O1 Ca1 H3A' 98.5(6) 7_665 . ? O1 Ca1 H3A' 92.9(7) 10_646 . ? O3' Ca1 H3A' 87.8(7) 7_665 . ? O3' Ca1 H3A' 86.9(7) 10_646 . ? O3' Ca1 H3A' 15.8(7) . . ? O3 Ca1 H3A' 88.3(6) 10_646 . ? O3 Ca1 H3A' 17.8(5) . . ? O3 Ca1 H3A' 66.6(6) 7_665 . ? H3A Ca1 H3A' 0.0(11) . . ? H4A Ca1 H3A' 27.4(6) . . ? O1 Ca1 H4A' 164.6(6) . . ? O1 Ca1 H4A' 71.8(6) 7_665 . ? O1 Ca1 H4A' 87.7(6) 10_646 . ? O3' Ca1 H4A' 114.7(7) 7_665 . ? O3' Ca1 H4A' 89.1(6) 10_646 . ? O3' Ca1 H4A' 18.0(6) . . ? O3 Ca1 H4A' 100.3(6) 10_646 . ? O3 Ca1 H4A' 19.1(5) . . ? O3 Ca1 H4A' 92.7(6) 7_665 . ? H3A Ca1 H4A' 27.4(6) . . ? H4A Ca1 H4A' 0.0(6) . . ? H3A' Ca1 H4A' 27.4(6) . . ? C1P P1 C1 109.82(12) . . ? C1P P1 C1 109.82(12) . 8_645 ? C1 P1 C1 109.12(12) . 8_645 ? C1P P1 C1 109.82(12) . 11_556 ? C1 P1 C1 109.12(12) . 11_556 ? C1 P1 C1 109.12(12) 8_645 11_556 ? C7 O1 Ca1 173.3(3) . . ? Ca1 O3 H3A 101(2) . . ? Ca1 O3 H4A 90(3) . . ? H3A O3 H4A 97(2) . . ? Ca1 O3 H3A' 101(2) . . ? H3A O3 H3A' 0(4) . . ? H4A O3 H3A' 97(2) . . ? Ca1 O3 H4A' 90(3) . . ? H3A O3 H4A' 97(2) . . ? H4A O3 H4A' 0(6) . . ? H3A' O3 H4A' 97(2) . . ? Ca1 O3' H3A 118(3) . . ? Ca1 O3' H4A 105(3) . . ? H3A O3' H4A 99(3) . . ? Ca1 O3' H3A' 118(3) . . ? H3A O3' H3A' 0(3) . . ? H4A O3' H3A' 99(3) . . ? Ca1 O3' H4A' 105(3) . . ? H3A O3' H4A' 99(3) . . ? H4A O3' H4A' 0(6) . . ? H3A' O3' H4A' 99(3) . . ? P1 C1P H1P 109.5 . . ? O1 C7 O2 125.1(3) . . ? O1 C7 C4 118.2(4) . . ? O2 C7 C4 116.6(3) . . ? C1 C2 C3 119.0(3) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C5 C4 C3 118.1(3) . . ? C5 C4 C7 121.3(3) . . ? C3 C4 C7 120.5(3) . . ? C1 C6 C5 121.2(3) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C1 C2 119.1(3) . . ? C6 C1 P1 120.9(2) . . ? C2 C1 P1 120.0(3) . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C4 C3 C2 121.9(3) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.176 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.048 data_sh11004 _database_code_depnum_ccdc_archive 'CCDC 849684' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'PCM-14 (375 K)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Ca O10.50 P' _chemical_formula_weight 524.44 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' 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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-x+1/2, y+1, -z+1' 'x+1, -y+1, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1, -x+1, -y+1/2' '-z+1, -x+1/2, y+1' '-z+1/2, x+1, -y+1' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1, -x+1' 'y+1, -z+1, -x+1/2' '-y+1, -z+1/2, x+1' _cell_length_a 17.124(2) _cell_length_b 17.124(2) _cell_length_c 17.124(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5020.9(10) _cell_formula_units_Z 8 _cell_measurement_temperature 375(2) _cell_measurement_reflns_used 2083 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 25.03 _exptl_crystal_description Shard _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 375(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 ? _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 2558 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0768 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 24.98 _reflns_number_total 1292 _reflns_number_gt 843 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0789P)^2^+0.9315P] 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_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(12) _refine_ls_number_reflns 1292 _refine_ls_number_parameters 112 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1597 _refine_ls_wR_factor_gt 0.1430 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.033 _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 Ca1 Ca 0.66382(7) 0.33618(7) 0.83618(7) 0.0685(6) Uani 1 3 d SD . . P1 P 0.54621(10) 0.04621(10) 0.45379(10) 0.0622(7) Uani 1 3 d S . . O1 O 0.6509(4) 0.3319(3) 0.7045(3) 0.124(2) Uani 1 1 d . . . O2 O 0.6565(4) 0.3977(3) 0.5946(3) 0.1108(18) Uani 1 1 d . . . O3 O 0.5287(3) 0.3231(3) 0.8558(7) 0.184(4) Uani 1 1 d D . . H3A H 0.5057(19) 0.2790(18) 0.854(7) 0.275 Uiso 1 1 d D . . H3B H 0.4952(13) 0.354(5) 0.836(7) 0.275 Uiso 1 1 d D . . O50 O 0.5000 0.2500 1.0281(5) 0.178(4) Uani 1 2 d S . . C1 C 0.5753(4) 0.1315(3) 0.5064(3) 0.0620(16) Uani 1 1 d . . . C1P C 0.4878(4) -0.0122(4) 0.5122(4) 0.085(3) Uani 1 3 d S . . H1P H 0.4505 0.0133 0.5281 0.127 Uiso 1 1 calc R . . C2 C 0.5987(4) 0.1981(4) 0.4683(3) 0.0775(18) Uani 1 1 d . . . H2 H 0.5985 0.1992 0.4140 0.093 Uiso 1 1 calc R . . C3 C 0.6224(4) 0.2634(3) 0.5089(4) 0.0811(19) Uani 1 1 d . . . H3 H 0.6383 0.3075 0.4815 0.097 Uiso 1 1 calc R . . C4 C 0.6230(4) 0.2644(3) 0.5891(4) 0.0720(17) Uani 1 1 d . . . C5 C 0.5983(4) 0.1978(4) 0.6286(3) 0.0780(18) Uani 1 1 d . . . H5 H 0.5984 0.1969 0.6829 0.094 Uiso 1 1 calc R . . C6 C 0.5731(4) 0.1322(3) 0.5868(3) 0.0733(17) Uani 1 1 d . . . H6 H 0.5547 0.0886 0.6136 0.088 Uiso 1 1 calc R . . C7 C 0.6469(4) 0.3373(5) 0.6344(5) 0.089(2) Uani 1 1 d . . . 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 Ca1 0.0685(6) 0.0685(6) 0.0685(6) -0.0041(6) 0.0041(6) 0.0041(6) P1 0.0622(7) 0.0622(7) 0.0622(7) -0.0126(8) -0.0126(8) 0.0126(8) O1 0.203(6) 0.090(4) 0.079(3) -0.031(3) -0.051(4) 0.021(4) O2 0.162(5) 0.063(3) 0.107(4) -0.015(3) -0.020(4) -0.004(3) O3 0.056(3) 0.079(3) 0.415(13) -0.032(6) -0.020(4) 0.014(2) O50 0.143(8) 0.285(15) 0.105(7) 0.000 0.000 -0.003(9) C1 0.077(4) 0.055(3) 0.054(3) -0.012(3) -0.015(3) 0.026(3) C1P 0.085(3) 0.085(3) 0.085(3) -0.007(4) -0.007(4) 0.007(4) C2 0.116(5) 0.067(4) 0.049(3) -0.009(3) -0.006(3) 0.016(4) C3 0.133(6) 0.052(3) 0.058(4) 0.000(3) -0.016(4) 0.011(4) C4 0.086(4) 0.060(4) 0.070(4) -0.011(3) -0.022(3) 0.021(3) C5 0.099(5) 0.081(4) 0.054(3) -0.018(3) -0.012(3) 0.013(4) C6 0.093(5) 0.057(3) 0.070(4) -0.013(3) -0.011(3) 0.016(3) C7 0.109(5) 0.070(4) 0.088(5) -0.030(4) -0.044(4) 0.034(4) _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 Ca1 O1 2.266(5) 7_665 ? Ca1 O1 2.266(5) . ? Ca1 O1 2.266(5) 10_646 ? Ca1 O3 2.348(5) 7_665 ? Ca1 O3 2.348(5) 10_646 ? Ca1 O3 2.348(5) . ? P1 C1P 1.733(12) . ? P1 C1 1.786(5) . ? P1 C1 1.786(5) 8_645 ? P1 C1 1.786(5) 11_556 ? O1 C7 1.206(9) . ? O2 C7 1.250(10) . ? O3 H3A 0.85(2) . ? O3 H3B 0.85(2) . ? C1 C2 1.374(9) . ? C1 C6 1.378(7) . ? C1P H1P 0.8200 . ? C2 C3 1.376(8) . ? C2 H2 0.9300 . ? C3 C4 1.374(8) . ? C3 H3 0.9300 . ? C4 C5 1.392(9) . ? C4 C7 1.524(8) . ? C5 C6 1.400(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? 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 O1 Ca1 O1 93.9(2) 7_665 . ? O1 Ca1 O1 93.9(2) 7_665 10_646 ? O1 Ca1 O1 93.9(2) . 10_646 ? O1 Ca1 O3 92.5(3) 7_665 7_665 ? O1 Ca1 O3 85.59(19) . 7_665 ? O1 Ca1 O3 173.7(3) 10_646 7_665 ? O1 Ca1 O3 85.59(19) 7_665 10_646 ? O1 Ca1 O3 173.7(3) . 10_646 ? O1 Ca1 O3 92.5(3) 10_646 10_646 ? O3 Ca1 O3 88.1(3) 7_665 10_646 ? O1 Ca1 O3 173.7(3) 7_665 . ? O1 Ca1 O3 92.5(3) . . ? O1 Ca1 O3 85.59(19) 10_646 . ? O3 Ca1 O3 88.1(3) 7_665 . ? O3 Ca1 O3 88.1(3) 10_646 . ? C1P P1 C1 110.0(2) . . ? C1P P1 C1 110.0(2) . 8_645 ? C1 P1 C1 109.0(2) . 8_645 ? C1P P1 C1 110.0(2) . 11_556 ? C1 P1 C1 109.0(2) . 11_556 ? C1 P1 C1 109.0(2) 8_645 11_556 ? C7 O1 Ca1 173.4(6) . . ? Ca1 O3 H3A 123(2) . . ? Ca1 O3 H3B 123(2) . . ? H3A O3 H3B 103(4) . . ? C2 C1 C6 118.3(5) . . ? C2 C1 P1 121.4(4) . . ? C6 C1 P1 120.2(5) . . ? P1 C1P H1P 109.5 . . ? C1 C2 C3 121.4(5) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 121.2(6) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C3 C4 C5 118.1(6) . . ? C3 C4 C7 121.5(6) . . ? C5 C4 C7 120.4(6) . . ? C4 C5 C6 120.3(6) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C1 C6 C5 120.6(6) . . ? C1 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? O1 C7 O2 126.8(6) . . ? O1 C7 C4 117.3(8) . . ? O2 C7 C4 115.8(6) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.474 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.042