# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_pcobcm _database_code_depnum_ccdc_archive 'CCDC 917976' #TrackingRef 'PrCOB.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B3 Ca4 O10 Pr' _chemical_formula_weight 493.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'Cm ' _symmetry_space_group_name_Hall 'c -2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' _cell_length_a 8.1772(12) _cell_length_b 16.157(2) _cell_length_c 3.6286(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.3990(10) _cell_angle_gamma 90.00 _cell_volume 469.95(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2097 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 7.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5887 _exptl_absorpt_correction_T_max 0.6649 _exptl_absorpt_process_details 'APEX2 Software Suite (Bruker,2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2727 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1085 _reflns_number_gt 1078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0051(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.032(12) _refine_ls_number_reflns 1085 _refine_ls_number_parameters 89 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0153 _refine_ls_R_factor_gt 0.0152 _refine_ls_wR_factor_ref 0.0305 _refine_ls_wR_factor_gt 0.0305 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.956 _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 Pr1 Pr 0.35930(3) 0.5000 0.15353(4) 0.00844(9) Uani 1 2 d S . . Ca1 Ca 0.62839(9) 0.31870(5) -0.18394(19) 0.00985(17) Uani 1 1 d . . . Ca2 Ca 0.00405(9) 0.38629(4) 0.48584(19) 0.00660(17) Uani 1 1 d . . . O1 O 0.5686(6) 0.5000 -0.2363(14) 0.0139(12) Uani 1 2 d S . . O5 O 0.3290(3) 0.23041(16) 0.4338(7) 0.0132(6) Uani 1 1 d . . . O6 O 0.6613(3) 0.16988(16) 0.0449(7) 0.0119(6) Uani 1 1 d . . . B1 B 0.3146(5) 0.3057(3) 0.2408(12) 0.0073(8) Uani 1 1 d . . . O3 O 0.8276(3) 0.57392(16) -0.0899(7) 0.0114(6) Uani 1 1 d . . . O2 O 0.1843(6) 0.5000 0.5679(13) 0.0055(9) Uani 1 2 d S . . O4 O 0.4554(3) 0.35415(17) 0.2405(8) 0.0111(6) Uani 1 1 d . . . B2 B 0.7427(7) 0.5000 -0.1379(16) 0.0077(12) Uani 1 2 d S . . 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 Pr1 0.00650(14) 0.01361(16) 0.00519(13) 0.000 0.00110(9) 0.000 Ca1 0.0095(4) 0.0131(4) 0.0073(4) 0.0006(3) 0.0025(3) 0.0010(3) Ca2 0.0069(4) 0.0069(4) 0.0058(3) -0.0002(3) 0.0008(3) 0.0000(3) O1 0.005(2) 0.030(3) 0.008(2) 0.000 0.0035(18) 0.000 O5 0.0167(14) 0.0097(14) 0.0152(14) 0.0057(11) 0.0084(11) 0.0034(11) O6 0.0102(15) 0.0165(15) 0.0087(13) 0.0000(11) 0.0014(12) -0.0055(12) B1 0.010(2) 0.007(2) 0.005(2) -0.0043(16) 0.0025(16) 0.0011(17) O3 0.0133(14) 0.0076(14) 0.0128(14) 0.0005(11) 0.0015(11) -0.0035(11) O2 0.004(2) 0.004(2) 0.008(2) 0.000 -0.0010(16) 0.000 O4 0.0108(15) 0.0105(14) 0.0121(14) -0.0002(12) 0.0026(12) -0.0018(12) B2 0.003(3) 0.017(3) 0.004(3) 0.000 0.001(2) 0.000 _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 Pr1 O2 2.271(5) . ? Pr1 O2 2.316(5) 1_554 ? Pr1 O1 2.427(5) . ? Pr1 O4 2.484(3) 2_565 ? Pr1 O4 2.484(3) . ? Pr1 O1 2.517(5) 1_556 ? Pr1 Pr1 3.6286(5) 1_554 ? Pr1 Pr1 3.6286(5) 1_556 ? Pr1 Ca2 3.8279(8) 2_565 ? Pr1 Ca2 3.8279(8) . ? Pr1 Ca2 3.8603(8) 1_554 ? Pr1 Ca2 3.8603(8) 2_564 ? Ca1 O4 2.350(3) 1_554 ? Ca1 O3 2.358(3) 2_565 ? Ca1 O4 2.359(3) . ? Ca1 O5 2.479(3) 4_554 ? Ca1 O6 2.541(3) . ? Ca1 O5 2.625(3) 4 ? Ca1 B1 2.794(4) 4 ? Ca1 O5 2.935(3) 1_554 ? Ca1 O1 2.9697(12) . ? Ca1 B1 2.978(4) 1_554 ? Ca1 B2 3.0693(19) . ? Ca1 B1 3.251(4) . ? Ca2 O2 2.337(3) . ? Ca2 O5 2.353(3) 4_455 ? Ca2 O6 2.358(3) 4_456 ? Ca2 O3 2.381(3) 2_465 ? Ca2 O3 2.396(3) 2_466 ? Ca2 O6 2.419(3) 4_455 ? Ca2 B1 3.135(4) . ? Ca2 Ca1 3.5997(11) 4_456 ? Ca2 Ca2 3.6286(5) 1_556 ? Ca2 Ca2 3.6286(5) 1_554 ? Ca2 Ca2 3.6743(15) 2_565 ? Ca2 Ca1 3.6769(11) 1_456 ? O1 B2 1.397(7) . ? O1 Pr1 2.517(5) 1_554 ? O1 Ca1 2.9697(12) 2_565 ? O5 B1 1.397(5) . ? O5 Ca2 2.353(3) 4 ? O5 Ca1 2.479(3) 4_456 ? O5 Ca1 2.625(3) 4_455 ? O5 Ca1 2.935(3) 1_556 ? O6 B1 1.371(5) 4 ? O6 Ca2 2.358(3) 4_554 ? O6 Ca2 2.419(3) 4 ? B1 O6 1.371(5) 4_455 ? B1 O4 1.392(5) . ? B1 Ca1 2.794(4) 4_455 ? B1 Ca1 2.978(4) 1_556 ? O3 B2 1.375(4) . ? O3 Ca1 2.358(3) 2_565 ? O3 Ca2 2.381(3) 2_665 ? O3 Ca2 2.396(3) 2_664 ? O2 Pr1 2.316(5) 1_556 ? O2 Ca2 2.337(3) 2_565 ? O4 Ca1 2.350(3) 1_556 ? B2 O3 1.375(4) 2_565 ? B2 Ca1 3.0692(19) 2_565 ? 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 O2 Pr1 O2 104.56(19) . 1_554 ? O2 Pr1 O1 174.4(2) . . ? O2 Pr1 O1 81.04(17) 1_554 . ? O2 Pr1 O4 98.09(7) . 2_565 ? O2 Pr1 O4 103.84(7) 1_554 2_565 ? O1 Pr1 O4 80.34(7) . 2_565 ? O2 Pr1 O4 98.09(7) . . ? O2 Pr1 O4 103.84(7) 1_554 . ? O1 Pr1 O4 80.34(7) . . ? O4 Pr1 O4 143.07(13) 2_565 . ? O2 Pr1 O1 79.96(17) . 1_556 ? O2 Pr1 O1 175.5(2) 1_554 1_556 ? O1 Pr1 O1 94.44(17) . 1_556 ? O4 Pr1 O1 75.24(7) 2_565 1_556 ? O4 Pr1 O1 75.24(7) . 1_556 ? O2 Pr1 Pr1 141.85(12) . 1_554 ? O2 Pr1 Pr1 37.29(12) 1_554 1_554 ? O1 Pr1 Pr1 43.75(12) . 1_554 ? O4 Pr1 Pr1 93.70(6) 2_565 1_554 ? O4 Pr1 Pr1 93.70(6) . 1_554 ? O1 Pr1 Pr1 138.19(11) 1_556 1_554 ? O2 Pr1 Pr1 38.15(12) . 1_556 ? O2 Pr1 Pr1 142.71(12) 1_554 1_556 ? O1 Pr1 Pr1 136.25(12) . 1_556 ? O4 Pr1 Pr1 86.30(6) 2_565 1_556 ? O4 Pr1 Pr1 86.30(6) . 1_556 ? O1 Pr1 Pr1 41.81(11) 1_556 1_556 ? Pr1 Pr1 Pr1 180.000(17) 1_554 1_556 ? O2 Pr1 Ca2 34.39(6) . 2_565 ? O2 Pr1 Ca2 85.37(11) 1_554 2_565 ? O1 Pr1 Ca2 148.25(5) . 2_565 ? O4 Pr1 Ca2 75.25(6) 2_565 2_565 ? O4 Pr1 Ca2 130.99(6) . 2_565 ? O1 Pr1 Ca2 98.59(10) 1_556 2_565 ? Pr1 Pr1 Ca2 117.710(11) 1_554 2_565 ? Pr1 Pr1 Ca2 62.290(11) 1_556 2_565 ? O2 Pr1 Ca2 34.39(6) . . ? O2 Pr1 Ca2 85.37(11) 1_554 . ? O1 Pr1 Ca2 148.25(5) . . ? O4 Pr1 Ca2 130.99(6) 2_565 . ? O4 Pr1 Ca2 75.25(6) . . ? O1 Pr1 Ca2 98.59(10) 1_556 . ? Pr1 Pr1 Ca2 117.710(11) 1_554 . ? Pr1 Pr1 Ca2 62.290(11) 1_556 . ? Ca2 Pr1 Ca2 57.36(2) 2_565 . ? O2 Pr1 Ca2 85.47(11) . 1_554 ? O2 Pr1 Ca2 34.11(6) 1_554 1_554 ? O1 Pr1 Ca2 99.45(10) . 1_554 ? O4 Pr1 Ca2 135.32(6) 2_565 1_554 ? O4 Pr1 Ca2 78.94(6) . 1_554 ? O1 Pr1 Ca2 148.08(5) 1_556 1_554 ? Pr1 Pr1 Ca2 61.387(12) 1_554 1_554 ? Pr1 Pr1 Ca2 118.613(13) 1_556 1_554 ? Ca2 Pr1 Ca2 84.39(2) 2_565 1_554 ? Ca2 Pr1 Ca2 56.323(13) . 1_554 ? O2 Pr1 Ca2 85.47(11) . 2_564 ? O2 Pr1 Ca2 34.11(6) 1_554 2_564 ? O1 Pr1 Ca2 99.45(10) . 2_564 ? O4 Pr1 Ca2 78.94(6) 2_565 2_564 ? O4 Pr1 Ca2 135.32(6) . 2_564 ? O1 Pr1 Ca2 148.08(5) 1_556 2_564 ? Pr1 Pr1 Ca2 61.387(12) 1_554 2_564 ? Pr1 Pr1 Ca2 118.613(13) 1_556 2_564 ? Ca2 Pr1 Ca2 56.323(13) 2_565 2_564 ? Ca2 Pr1 Ca2 84.39(2) . 2_564 ? Ca2 Pr1 Ca2 56.84(2) 1_554 2_564 ? O4 Ca1 O3 103.10(10) 1_554 2_565 ? O4 Ca1 O4 100.82(11) 1_554 . ? O3 Ca1 O4 102.32(10) 2_565 . ? O4 Ca1 O5 85.95(9) 1_554 4_554 ? O3 Ca1 O5 78.57(9) 2_565 4_554 ? O4 Ca1 O5 172.69(10) . 4_554 ? O4 Ca1 O6 121.83(9) 1_554 . ? O3 Ca1 O6 128.56(9) 2_565 . ? O4 Ca1 O6 93.15(10) . . ? O5 Ca1 O6 80.84(9) 4_554 . ? O4 Ca1 O5 175.76(9) 1_554 4 ? O3 Ca1 O5 78.56(9) 2_565 4 ? O4 Ca1 O5 82.53(9) . 4 ? O5 Ca1 O5 90.59(9) 4_554 4 ? O6 Ca1 O5 55.03(8) . 4 ? O4 Ca1 B1 146.33(12) 1_554 4 ? O3 Ca1 B1 99.43(12) 2_565 4 ? O4 Ca1 B1 98.41(11) . 4 ? O5 Ca1 B1 74.31(11) 4_554 4 ? O6 Ca1 B1 29.29(10) . 4 ? O5 Ca1 B1 29.67(10) 4 4 ? O4 Ca1 O5 53.05(8) 1_554 1_554 ? O3 Ca1 O5 156.07(8) 2_565 1_554 ? O4 Ca1 O5 82.80(9) . 1_554 ? O5 Ca1 O5 99.34(7) 4_554 1_554 ? O6 Ca1 O5 73.69(8) . 1_554 ? O5 Ca1 O5 125.37(6) 4 1_554 ? B1 Ca1 O5 102.94(10) 4 1_554 ? O4 Ca1 O1 68.91(12) 1_554 . ? O3 Ca1 O1 51.96(11) 2_565 . ? O4 Ca1 O1 71.93(12) . . ? O5 Ca1 O1 113.50(12) 4_554 . ? O6 Ca1 O1 163.72(12) . . ? O5 Ca1 O1 114.84(11) 4 . ? B1 Ca1 O1 144.08(13) 4 . ? O5 Ca1 O1 109.74(11) 1_554 . ? O4 Ca1 B1 27.17(11) 1_554 1_554 ? O3 Ca1 B1 128.92(11) 2_565 1_554 ? O4 Ca1 B1 85.98(11) . 1_554 ? O5 Ca1 B1 99.14(10) 4_554 1_554 ? O6 Ca1 B1 100.56(10) . 1_554 ? O5 Ca1 B1 152.08(11) 4 1_554 ? B1 Ca1 B1 129.50(7) 4 1_554 ? O5 Ca1 B1 27.32(10) 1_554 1_554 ? O1 Ca1 B1 85.21(13) . 1_554 ? O4 Ca1 B2 86.51(12) 1_554 . ? O3 Ca1 B2 25.28(12) 2_565 . ? O4 Ca1 B2 87.03(12) . . ? O5 Ca1 B2 96.20(12) 4_554 . ? O6 Ca1 B2 150.92(12) . . ? O5 Ca1 B2 96.31(12) 4 . ? B1 Ca1 B2 121.98(13) 4 . ? O5 Ca1 B2 134.93(11) 1_554 . ? O1 Ca1 B2 26.69(14) . . ? B1 Ca1 B2 108.44(13) 1_554 . ? O4 Ca1 B1 92.53(10) 1_554 . ? O3 Ca1 B1 124.51(10) 2_565 . ? O4 Ca1 B1 22.26(9) . . ? O5 Ca1 B1 156.39(10) 4_554 . ? O6 Ca1 B1 80.01(10) . . ? O5 Ca1 B1 89.67(10) 4 . ? B1 Ca1 B1 95.00(11) 4 . ? O5 Ca1 B1 61.94(9) 1_554 . ? O1 Ca1 B1 87.63(12) . . ? B1 Ca1 B1 71.11(9) 1_554 . ? B2 Ca1 B1 107.23(13) . . ? O2 Ca2 O5 177.12(14) . 4_455 ? O2 Ca2 O6 88.28(12) . 4_456 ? O5 Ca2 O6 88.88(10) 4_455 4_456 ? O2 Ca2 O3 99.03(13) . 2_465 ? O5 Ca2 O3 83.82(9) 4_455 2_465 ? O6 Ca2 O3 172.58(10) 4_456 2_465 ? O2 Ca2 O3 98.73(13) . 2_466 ? O5 Ca2 O3 80.36(9) 4_455 2_466 ? O6 Ca2 O3 81.13(9) 4_456 2_466 ? O3 Ca2 O3 98.86(10) 2_465 2_466 ? O2 Ca2 O6 88.56(13) . 4_455 ? O5 Ca2 O6 92.34(9) 4_455 4_455 ? O6 Ca2 O6 98.85(9) 4_456 4_455 ? O3 Ca2 O6 80.21(9) 2_465 4_455 ? O3 Ca2 O6 172.70(10) 2_466 4_455 ? O2 Ca2 B1 80.61(12) . . ? O5 Ca2 B1 99.12(10) 4_455 . ? O6 Ca2 B1 75.50(11) 4_456 . ? O3 Ca2 B1 104.33(10) 2_465 . ? O3 Ca2 B1 156.63(11) 2_466 . ? O6 Ca2 B1 24.51(10) 4_455 . ? O2 Ca2 Ca1 123.46(10) . 4_456 ? O5 Ca2 Ca1 54.31(7) 4_455 4_456 ? O6 Ca2 Ca1 44.72(7) 4_456 4_456 ? O3 Ca2 Ca1 128.53(7) 2_465 4_456 ? O3 Ca2 Ca1 101.50(7) 2_466 4_456 ? O6 Ca2 Ca1 73.91(6) 4_455 4_456 ? B1 Ca2 Ca1 61.37(8) . 4_456 ? O2 Ca2 Ca2 89.85(12) . 1_556 ? O5 Ca2 Ca2 87.71(6) 4_455 1_556 ? O6 Ca2 Ca2 41.20(6) 4_456 1_556 ? O3 Ca2 Ca2 139.27(6) 2_465 1_556 ? O3 Ca2 Ca2 40.41(6) 2_466 1_556 ? O6 Ca2 Ca2 140.04(6) 4_455 1_556 ? B1 Ca2 Ca2 116.34(8) . 1_556 ? Ca1 Ca2 Ca2 73.916(16) 4_456 1_556 ? O2 Ca2 Ca2 90.15(12) . 1_554 ? O5 Ca2 Ca2 92.29(6) 4_455 1_554 ? O6 Ca2 Ca2 138.80(6) 4_456 1_554 ? O3 Ca2 Ca2 40.73(6) 2_465 1_554 ? O3 Ca2 Ca2 139.59(6) 2_466 1_554 ? O6 Ca2 Ca2 39.96(6) 4_455 1_554 ? B1 Ca2 Ca2 63.66(8) . 1_554 ? Ca1 Ca2 Ca2 106.084(16) 4_456 1_554 ? Ca2 Ca2 Ca2 180.00(5) 1_556 1_554 ? O2 Ca2 Ca2 38.18(9) . 2_565 ? O5 Ca2 Ca2 143.28(7) 4_455 2_565 ? O6 Ca2 Ca2 112.63(7) 4_456 2_565 ? O3 Ca2 Ca2 74.33(6) 2_465 2_565 ? O3 Ca2 Ca2 74.44(6) 2_466 2_565 ? O6 Ca2 Ca2 112.04(7) 4_455 2_565 ? B1 Ca2 Ca2 114.54(8) . 2_565 ? Ca1 Ca2 Ca2 156.941(16) 4_456 2_565 ? Ca2 Ca2 Ca2 90.0 1_556 2_565 ? Ca2 Ca2 Ca2 90.0 1_554 2_565 ? O2 Ca2 Ca1 137.59(11) . 1_456 ? O5 Ca2 Ca1 41.73(6) 4_455 1_456 ? O6 Ca2 Ca1 87.37(7) 4_456 1_456 ? O3 Ca2 Ca1 88.04(7) 2_465 1_456 ? O3 Ca2 Ca1 38.97(6) 2_466 1_456 ? O6 Ca2 Ca1 133.77(7) 4_455 1_456 ? B1 Ca2 Ca1 138.14(8) . 1_456 ? Ca1 Ca2 Ca1 79.48(2) 4_456 1_456 ? Ca2 Ca2 Ca1 60.594(16) 1_556 1_456 ? Ca2 Ca2 Ca1 119.406(16) 1_554 1_456 ? Ca2 Ca2 Ca1 107.278(16) 2_565 1_456 ? B2 O1 Pr1 130.6(4) . . ? B2 O1 Pr1 134.9(4) . 1_554 ? Pr1 O1 Pr1 94.44(17) . 1_554 ? B2 O1 Ca1 80.63(10) . 2_565 ? Pr1 O1 Ca1 95.09(10) . 2_565 ? Pr1 O1 Ca1 97.53(10) 1_554 2_565 ? B2 O1 Ca1 80.63(10) . . ? Pr1 O1 Ca1 95.09(10) . . ? Pr1 O1 Ca1 97.53(10) 1_554 . ? Ca1 O1 Ca1 161.08(19) 2_565 . ? B1 O5 Ca2 136.7(2) . 4 ? B1 O5 Ca1 124.1(2) . 4_456 ? Ca2 O5 Ca1 99.09(9) 4 4_456 ? B1 O5 Ca1 81.9(2) . 4_455 ? Ca2 O5 Ca1 95.39(9) 4 4_455 ? Ca1 O5 Ca1 90.59(9) 4_456 4_455 ? B1 O5 Ca1 78.1(2) . 1_556 ? Ca2 O5 Ca1 85.06(8) 4 1_556 ? Ca1 O5 Ca1 118.27(10) 4_456 1_556 ? Ca1 O5 Ca1 150.78(10) 4_455 1_556 ? B1 O6 Ca2 147.6(3) 4 4_554 ? B1 O6 Ca2 108.4(2) 4 4 ? Ca2 O6 Ca2 98.85(9) 4_554 4 ? B1 O6 Ca1 85.6(2) 4 . ? Ca2 O6 Ca1 94.50(9) 4_554 . ? Ca2 O6 Ca1 122.37(11) 4 . ? O6 B1 O4 120.6(4) 4_455 . ? O6 B1 O5 119.2(3) 4_455 . ? O4 B1 O5 120.2(3) . . ? O6 B1 Ca1 65.1(2) 4_455 4_455 ? O4 B1 Ca1 139.9(3) . 4_455 ? O5 B1 Ca1 68.5(2) . 4_455 ? O6 B1 Ca1 156.3(3) 4_455 1_556 ? O4 B1 Ca1 50.41(18) . 1_556 ? O5 B1 Ca1 74.6(2) . 1_556 ? Ca1 B1 Ca1 137.52(16) 4_455 1_556 ? O6 B1 Ca2 47.06(17) 4_455 . ? O4 B1 Ca2 118.9(2) . . ? O5 B1 Ca2 102.2(2) . . ? Ca1 B1 Ca2 94.11(12) 4_455 . ? Ca1 B1 Ca2 113.95(13) 1_556 . ? O6 B1 Ca1 117.5(3) 4_455 . ? O4 B1 Ca1 39.92(16) . . ? O5 B1 Ca1 107.3(2) . . ? Ca1 B1 Ca1 100.38(12) 4_455 . ? Ca1 B1 Ca1 71.11(9) 1_556 . ? Ca2 B1 Ca1 150.14(15) . . ? B2 O3 Ca1 107.7(3) . 2_565 ? B2 O3 Ca2 123.3(3) . 2_665 ? Ca1 O3 Ca2 102.11(10) 2_565 2_665 ? B2 O3 Ca2 120.3(3) . 2_664 ? Ca1 O3 Ca2 101.31(10) 2_565 2_664 ? Ca2 O3 Ca2 98.86(10) 2_665 2_664 ? Pr1 O2 Pr1 104.56(18) . 1_556 ? Pr1 O2 Ca2 112.31(14) . . ? Pr1 O2 Ca2 112.13(14) 1_556 . ? Pr1 O2 Ca2 112.31(14) . 2_565 ? Pr1 O2 Ca2 112.13(14) 1_556 2_565 ? Ca2 O2 Ca2 103.64(18) . 2_565 ? B1 O4 Ca1 102.4(2) . 1_556 ? B1 O4 Ca1 117.8(2) . . ? Ca1 O4 Ca1 100.82(11) 1_556 . ? B1 O4 Pr1 107.0(2) . . ? Ca1 O4 Pr1 117.63(11) 1_556 . ? Ca1 O4 Pr1 111.28(11) . . ? O3 B2 O3 120.5(5) . 2_565 ? O3 B2 O1 119.7(2) . . ? O3 B2 O1 119.7(2) 2_565 . ? O3 B2 Ca1 167.5(3) . . ? O3 B2 Ca1 47.07(16) 2_565 . ? O1 B2 Ca1 72.68(10) . . ? O3 B2 Ca1 47.07(16) . 2_565 ? O3 B2 Ca1 167.5(3) 2_565 2_565 ? O1 B2 Ca1 72.68(10) . 2_565 ? Ca1 B2 Ca1 145.3(2) . 2_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.526 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.095