# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_LiCu2[BP2O8(OH)2] _database_code_depnum_ccdc_archive 'CCDC 902700' #TrackingRef '- LiCuBPO.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum ' B Cu2 H2 Li O10 P2' _chemical_formula_weight 368.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li -0.0003 0.0001 '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' B B 0.0013 0.0007 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) 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' _cell_length_a 5.3195(10) _cell_length_b 7.9352(15) _cell_length_c 17.464(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 737.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1828 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.32 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 3.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 6.248 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5399 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.32 _reflns_number_total 1828 _reflns_number_gt 1770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0216P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0098(7) _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 0.010(11) _refine_ls_number_reflns 1828 _refine_ls_number_parameters 146 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0178 _refine_ls_R_factor_gt 0.0172 _refine_ls_wR_factor_ref 0.0470 _refine_ls_wR_factor_gt 0.0468 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.054 _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 Cu1 Cu 0.94901(7) 0.16076(4) 0.980387(18) 0.01017(9) Uani 1 1 d . . . Cu2 Cu 0.96428(6) 0.82686(4) 0.843381(18) 0.00882(9) Uani 1 1 d . . . P2 P 0.93942(13) 0.49164(7) 1.09308(4) 0.00584(14) Uani 1 1 d . . . P1 P 0.74605(12) 0.46396(8) 0.88132(4) 0.00662(14) Uani 1 1 d . . . B1 B 0.7181(5) 0.5885(4) 0.73572(17) 0.0071(5) Uani 1 1 d . . . Li1 Li 0.7423(9) -0.1352(6) 1.0471(3) 0.0154(10) Uani 1 1 d . . . O4 O 0.8720(3) 0.2932(2) 0.89209(11) 0.0093(4) Uani 1 1 d . . . O3 O 0.9329(3) 0.6080(2) 0.89349(11) 0.0105(4) Uani 1 1 d . . . O2 O 1.0292(3) 1.0420(2) 0.79291(10) 0.0094(4) Uani 1 1 d . . . H2 H 0.9676 1.1168 0.8140 0.014 Uiso 1 1 d R . . O1 O 1.0161(3) 0.0164(2) 1.06674(11) 0.0112(4) Uani 1 1 d . . . O5 O 0.6984(3) -0.0348(2) 0.93987(11) 0.0097(4) Uani 1 1 d . . . O6 O 0.8166(3) 0.3483(2) 1.04792(11) 0.0094(4) Uani 1 1 d . . . O8 O 0.7253(3) 0.7594(2) 0.76470(11) 0.0100(4) Uani 1 1 d D . . H8 H 0.6249 0.8355 0.7398 0.015 Uiso 1 1 d RD . . O9 O 0.9789(3) 0.4310(2) 1.17737(10) 0.0080(4) Uani 1 1 d . . . O10 O 0.6488(3) 0.4676(2) 0.79633(11) 0.0101(4) Uani 1 1 d . . . O7A O 0.7666(3) 0.6466(2) 1.09244(11) 0.0106(4) 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 Cu1 0.01115(15) 0.01127(15) 0.00808(16) 0.00282(13) -0.00072(13) 0.00162(14) Cu2 0.00928(15) 0.00790(15) 0.00928(16) 0.00110(12) -0.00286(12) -0.00230(14) P2 0.0060(3) 0.0065(3) 0.0050(3) 0.0001(2) 0.0011(2) 0.0007(2) P1 0.0074(3) 0.0071(3) 0.0053(3) 0.0011(3) -0.0001(3) -0.0006(2) B1 0.0093(13) 0.0100(13) 0.0019(12) 0.0006(11) -0.0007(11) 0.0012(11) Li1 0.012(2) 0.017(3) 0.017(2) 0.004(2) -0.001(2) -0.0038(18) O4 0.0124(8) 0.0093(9) 0.0063(9) 0.0006(7) -0.0008(7) 0.0025(7) O3 0.0113(8) 0.0090(8) 0.0113(9) 0.0023(7) -0.0053(8) -0.0029(7) O2 0.0088(8) 0.0088(8) 0.0105(9) -0.0012(7) 0.0024(8) 0.0012(7) O1 0.0117(9) 0.0129(8) 0.0089(9) 0.0045(7) -0.0034(8) -0.0016(8) O5 0.0095(8) 0.0084(9) 0.0112(10) 0.0021(8) -0.0038(8) -0.0012(7) O6 0.0081(8) 0.0112(9) 0.0088(9) -0.0026(8) -0.0008(7) -0.0006(7) O8 0.0106(9) 0.0074(8) 0.0120(10) -0.0012(8) -0.0046(8) 0.0024(7) O9 0.0062(8) 0.0116(8) 0.0064(8) 0.0000(7) 0.0023(7) 0.0016(7) O10 0.0137(8) 0.0113(9) 0.0052(9) 0.0031(8) -0.0035(7) -0.0044(7) O7A 0.0107(8) 0.0083(9) 0.0129(9) 0.0017(8) 0.0037(8) 0.0033(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 Cu1 O4 1.9107(19) . ? Cu1 O1 1.9271(18) . ? Cu1 O6 2.0184(17) 4_557 ? Cu1 O6 2.0253(19) . ? Cu1 O5 2.1646(18) . ? Cu1 Li1 2.843(5) . ? Cu2 O8 1.9469(19) . ? Cu2 O3 1.9521(18) . ? Cu2 O2 1.9524(18) . ? Cu2 O7A 1.9716(18) 4_567 ? Cu2 Li1 2.856(5) 4_557 ? P2 O6 1.5303(19) . ? P2 O5 1.5315(18) 4_557 ? P2 O7A 1.5351(19) . ? P2 O9 1.5628(19) . ? P1 O4 1.5231(18) . ? P1 O3 1.5292(19) . ? P1 O1 1.5308(19) 4_457 ? P1 O10 1.572(2) . ? B1 O8 1.448(3) . ? B1 O9 1.470(3) 2_664 ? B1 O10 1.475(3) . ? B1 O2 1.481(3) 3_746 ? Li1 O7A 1.908(5) 1_545 ? Li1 O1 1.920(5) . ? Li1 O3 1.957(5) 4_457 ? Li1 O5 2.049(5) . ? Li1 Cu2 2.856(5) 4_457 ? O3 Li1 1.957(5) 4_557 ? O2 B1 1.481(3) 3_756 ? O1 P1 1.5308(19) 4_557 ? O5 P2 1.5315(18) 4_457 ? O6 Cu1 2.0184(17) 4_457 ? O9 B1 1.470(3) 2_665 ? O7A Li1 1.908(5) 1_565 ? O7A Cu2 1.9716(18) 4_467 ? 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 O4 Cu1 O1 176.66(8) . . ? O4 Cu1 O6 91.69(8) . 4_557 ? O1 Cu1 O6 89.49(8) . 4_557 ? O4 Cu1 O6 89.50(8) . . ? O1 Cu1 O6 92.60(8) . . ? O6 Cu1 O6 120.38(7) 4_557 . ? O4 Cu1 O5 89.92(8) . . ? O1 Cu1 O5 86.78(7) . . ? O6 Cu1 O5 119.42(8) 4_557 . ? O6 Cu1 O5 120.19(7) . . ? O4 Cu1 Li1 134.63(12) . . ? O1 Cu1 Li1 42.25(12) . . ? O6 Cu1 Li1 116.46(11) 4_557 . ? O6 Cu1 Li1 103.52(12) . . ? O5 Cu1 Li1 45.87(12) . . ? O8 Cu2 O3 90.91(8) . . ? O8 Cu2 O2 92.13(8) . . ? O3 Cu2 O2 174.70(8) . . ? O8 Cu2 O7A 164.42(8) . 4_567 ? O3 Cu2 O7A 84.84(8) . 4_567 ? O2 Cu2 O7A 91.08(8) . 4_567 ? O8 Cu2 Li1 131.63(12) . 4_557 ? O3 Cu2 Li1 43.15(11) . 4_557 ? O2 Cu2 Li1 132.56(12) . 4_557 ? O7A Cu2 Li1 41.75(11) 4_567 4_557 ? O6 P2 O5 110.87(11) . 4_557 ? O6 P2 O7A 109.62(11) . . ? O5 P2 O7A 110.91(10) 4_557 . ? O6 P2 O9 108.31(10) . . ? O5 P2 O9 107.56(11) 4_557 . ? O7A P2 O9 109.50(10) . . ? O4 P1 O3 111.19(10) . . ? O4 P1 O1 111.65(10) . 4_457 ? O3 P1 O1 111.16(11) . 4_457 ? O4 P1 O10 106.12(11) . . ? O3 P1 O10 109.35(10) . . ? O1 P1 O10 107.14(11) 4_457 . ? O8 B1 O9 111.1(2) . 2_664 ? O8 B1 O10 111.4(2) . . ? O9 B1 O10 104.5(2) 2_664 . ? O8 B1 O2 109.1(2) . 3_746 ? O9 B1 O2 112.8(2) 2_664 3_746 ? O10 B1 O2 107.9(2) . 3_746 ? O7A Li1 O1 116.3(3) 1_545 . ? O7A Li1 O3 86.4(2) 1_545 4_457 ? O1 Li1 O3 118.3(3) . 4_457 ? O7A Li1 O5 137.7(3) 1_545 . ? O1 Li1 O5 90.3(2) . . ? O3 Li1 O5 110.2(2) 4_457 . ? O7A Li1 Cu1 153.3(2) 1_545 . ? O1 Li1 Cu1 42.44(11) . . ? O3 Li1 Cu1 116.8(2) 4_457 . ? O5 Li1 Cu1 49.31(12) . . ? O7A Li1 Cu2 43.47(11) 1_545 4_457 ? O1 Li1 Cu2 127.4(2) . 4_457 ? O3 Li1 Cu2 43.00(11) 4_457 4_457 ? O5 Li1 Cu2 139.5(2) . 4_457 ? Cu1 Li1 Cu2 156.2(2) . 4_457 ? P1 O4 Cu1 133.10(12) . . ? P1 O3 Cu2 131.16(11) . . ? P1 O3 Li1 134.64(18) . 4_557 ? Cu2 O3 Li1 93.85(17) . 4_557 ? B1 O2 Cu2 122.06(16) 3_756 . ? P1 O1 Li1 140.86(19) 4_557 . ? P1 O1 Cu1 123.45(11) 4_557 . ? Li1 O1 Cu1 95.31(17) . . ? P2 O5 Li1 122.21(18) 4_457 . ? P2 O5 Cu1 121.11(11) 4_457 . ? Li1 O5 Cu1 84.82(15) . . ? P2 O6 Cu1 124.49(11) . 4_457 ? P2 O6 Cu1 134.25(11) . . ? Cu1 O6 Cu1 99.67(8) 4_457 . ? B1 O8 Cu2 121.43(16) . . ? B1 O9 P2 126.13(16) 2_665 . ? B1 O10 P1 127.39(17) . . ? P2 O7A Li1 140.39(19) . 1_565 ? P2 O7A Cu2 124.75(11) . 4_467 ? Li1 O7A Cu2 94.78(17) 1_565 4_467 ? 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 O2 H2 O4 0.77 2.02 2.770(3) 164.3 1_565 O8 H8 O10 0.92 1.90 2.797(3) 165.3 3_656 O8 H8 O9 0.92 2.47 2.962(3) 113.5 4_467 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.322 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.085