# 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_a _database_code_depnum_ccdc_archive 'CCDC 888975' #TrackingRef '- Pb2NiP2O8.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ni O8 P2 Pb2 ' _chemical_formula_weight 663.03 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.2848(19) _cell_length_b 15.464(5) _cell_length_c 8.436(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.040(6) _cell_angle_gamma 90.00 _cell_volume 689.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1909 _cell_measurement_theta_min 3.5731 _cell_measurement_theta_max 27.4565 _exptl_crystal_description block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 286 _exptl_absorpt_coefficient_mu 12.974 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3570 _exptl_absorpt_correction_T_max 0.4234 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Mercury2 _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3389 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1151 _reflns_number_gt 1023 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0770P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0052(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1151 _refine_ls_number_parameters 120 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.067 _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 Pb1 Pb 0.25010(7) 0.49230(2) 0.82338(4) 0.0105(2) Uani 1 1 d . . . Pb2 Pb -0.26326(8) 0.76395(2) 0.31835(4) 0.0104(2) Uani 1 1 d . . . Ni1 Ni -0.7831(3) 0.63539(7) 0.47912(15) 0.0073(3) Uani 1 1 d . . . P1 P -0.7402(5) 0.66467(15) 0.0941(3) 0.0069(5) Uani 1 1 d . . . P2 P -0.2430(5) 0.92557(14) 0.0773(3) 0.0054(5) Uani 1 1 d . . . O1 O -0.4922(13) 0.6529(5) -0.0004(8) 0.0145(16) Uani 1 1 d U . . O2 O -0.6695(14) 0.6818(4) 0.2685(9) 0.0150(15) Uani 1 1 d U . . O3 O -0.8983(14) 0.7409(4) 0.0316(9) 0.0122(14) Uani 1 1 d U . . O4 O -0.8995(13) 0.5806(4) 0.0733(8) 0.0109(14) Uani 1 1 d U . . O5 O -0.3196(13) 1.0182(4) 0.1047(8) 0.0078(13) Uani 1 1 d U . . O6 O -0.1486(14) 0.9041(4) -0.0935(8) 0.0089(13) Uani 1 1 d U . . O7 O -0.0126(13) 0.9027(4) 0.1849(8) 0.0081(13) Uani 1 1 d U . . O8 O -0.4614(13) 0.8618(4) 0.1169(8) 0.0086(14) Uani 1 1 d U . . 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 Pb1 0.0170(3) 0.0072(3) 0.0073(3) 0.00006(11) 0.0008(2) -0.00075(12) Pb2 0.0188(3) 0.0055(3) 0.0068(3) 0.00155(11) 0.0022(2) 0.00148(12) Ni1 0.0138(7) 0.0032(6) 0.0049(6) 0.0005(4) 0.0011(5) -0.0004(4) P1 0.0137(13) 0.0032(10) 0.0039(11) 0.0011(8) 0.0029(9) -0.0006(9) P2 0.0101(13) 0.0030(10) 0.0032(11) 0.0007(8) 0.0024(9) -0.0002(9) O1 0.0148(18) 0.0140(18) 0.0146(18) 0.0003(10) 0.0014(10) -0.0003(10) O2 0.0158(17) 0.0147(17) 0.0145(17) 0.0002(10) -0.0003(10) -0.0011(10) O3 0.0126(17) 0.0115(16) 0.0125(17) 0.0006(10) -0.0002(10) -0.0004(10) O4 0.0113(16) 0.0106(16) 0.0109(16) -0.0002(10) 0.0000(10) 0.0003(10) O5 0.0084(15) 0.0070(15) 0.0079(15) -0.0008(10) -0.0003(10) 0.0004(10) O6 0.0098(16) 0.0091(16) 0.0079(16) 0.0000(10) 0.0000(10) 0.0001(10) O7 0.0085(16) 0.0080(15) 0.0079(15) 0.0003(10) -0.0003(10) 0.0000(10) O8 0.0089(16) 0.0082(16) 0.0088(16) 0.0010(10) 0.0000(10) -0.0011(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 Pb1 O4 2.338(7) 3_466 ? Pb1 O6 2.431(7) 2_545 ? Pb1 O7 2.435(7) 4_576 ? Pb1 O4 2.634(7) 1_656 ? Pb2 O1 2.336(7) 4_576 ? Pb2 O8 2.504(7) . ? Pb2 O2 2.529(8) . ? Pb2 O3 2.638(8) 4_676 ? Ni1 O2 2.009(7) . ? Ni1 O5 2.019(6) 2_445 ? Ni1 O3 2.056(7) 4_576 ? Ni1 O8 2.059(7) 4_576 ? Ni1 O6 2.116(7) 4_476 ? Ni1 O7 2.199(7) 4_476 ? Ni1 P2 2.736(3) 4_476 ? P1 O3 1.538(7) . ? P1 O2 1.540(8) . ? P1 O1 1.545(7) . ? P1 O4 1.559(7) . ? P2 O5 1.507(6) . ? P2 O8 1.555(7) . ? P2 O7 1.559(8) . ? P2 O6 1.561(7) . ? P2 Ni1 2.736(3) 4_675 ? O1 Pb2 2.336(7) 4_575 ? O3 Ni1 2.056(7) 4_575 ? O3 Pb2 2.638(8) 4_475 ? O4 Pb1 2.338(7) 3_466 ? O4 Pb1 2.634(7) 1_454 ? O5 Ni1 2.019(6) 2_455 ? O6 Ni1 2.116(7) 4_675 ? O6 Pb1 2.431(7) 2 ? O7 Ni1 2.199(7) 4_675 ? O7 Pb1 2.435(7) 4_575 ? O8 Ni1 2.059(7) 4_575 ? 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 Pb1 O6 81.5(2) 3_466 2_545 ? O4 Pb1 O7 92.8(2) 3_466 4_576 ? O6 Pb1 O7 82.3(2) 2_545 4_576 ? O4 Pb1 O4 73.3(2) 3_466 1_656 ? O6 Pb1 O4 149.7(2) 2_545 1_656 ? O7 Pb1 O4 82.3(2) 4_576 1_656 ? O1 Pb2 O8 84.0(2) 4_576 . ? O1 Pb2 O2 86.9(2) 4_576 . ? O8 Pb2 O2 80.6(2) . . ? O1 Pb2 O3 87.0(2) 4_576 4_676 ? O8 Pb2 O3 141.8(2) . 4_676 ? O2 Pb2 O3 136.0(2) . 4_676 ? O2 Ni1 O5 86.0(3) . 2_445 ? O2 Ni1 O3 86.9(3) . 4_576 ? O5 Ni1 O3 171.9(3) 2_445 4_576 ? O2 Ni1 O8 104.2(3) . 4_576 ? O5 Ni1 O8 89.7(3) 2_445 4_576 ? O3 Ni1 O8 95.9(3) 4_576 4_576 ? O2 Ni1 O6 96.9(3) . 4_476 ? O5 Ni1 O6 83.4(3) 2_445 4_476 ? O3 Ni1 O6 93.5(3) 4_576 4_476 ? O8 Ni1 O6 157.3(3) 4_576 4_476 ? O2 Ni1 O7 163.6(3) . 4_476 ? O5 Ni1 O7 100.7(2) 2_445 4_476 ? O3 Ni1 O7 85.1(3) 4_576 4_476 ? O8 Ni1 O7 90.9(3) 4_576 4_476 ? O6 Ni1 O7 69.4(3) 4_476 4_476 ? O2 Ni1 P2 131.1(2) . 4_476 ? O5 Ni1 P2 92.06(19) 2_445 4_476 ? O3 Ni1 P2 89.5(2) 4_576 4_476 ? O8 Ni1 P2 124.7(2) 4_576 4_476 ? O6 Ni1 P2 34.64(18) 4_476 4_476 ? O7 Ni1 P2 34.72(19) 4_476 4_476 ? O3 P1 O2 109.1(4) . . ? O3 P1 O1 111.9(4) . . ? O2 P1 O1 107.9(4) . . ? O3 P1 O4 107.9(4) . . ? O2 P1 O4 112.4(4) . . ? O1 P1 O4 107.6(4) . . ? O5 P2 O8 111.8(4) . . ? O5 P2 O7 109.7(4) . . ? O8 P2 O7 108.1(4) . . ? O5 P2 O6 115.5(4) . . ? O8 P2 O6 107.5(4) . . ? O7 P2 O6 103.9(4) . . ? O5 P2 Ni1 127.8(3) . 4_675 ? O8 P2 Ni1 120.4(3) . 4_675 ? O7 P2 Ni1 53.4(2) . 4_675 ? O6 P2 Ni1 50.4(3) . 4_675 ? P1 O1 Pb2 135.5(4) . 4_575 ? P1 O2 Ni1 135.3(4) . . ? P1 O2 Pb2 116.8(4) . . ? Ni1 O2 Pb2 106.6(3) . . ? P1 O3 Ni1 128.8(5) . 4_575 ? P1 O3 Pb2 127.5(4) . 4_475 ? Ni1 O3 Pb2 95.5(3) 4_575 4_475 ? P1 O4 Pb1 142.0(4) . 3_466 ? P1 O4 Pb1 111.1(3) . 1_454 ? Pb1 O4 Pb1 106.7(2) 3_466 1_454 ? P2 O5 Ni1 136.7(4) . 2_455 ? P2 O6 Ni1 94.9(3) . 4_675 ? P2 O6 Pb1 123.1(4) . 2 ? Ni1 O6 Pb1 126.4(3) 4_675 2 ? P2 O7 Ni1 91.8(3) . 4_675 ? P2 O7 Pb1 124.9(3) . 4_575 ? Ni1 O7 Pb1 104.0(3) 4_675 4_575 ? P2 O8 Ni1 118.5(4) . 4_575 ? P2 O8 Pb2 102.6(4) . . ? Ni1 O8 Pb2 137.8(3) 4_575 . ? _diffrn_measured_fraction_theta_max 0.730 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.730 _refine_diff_density_max 2.585 _refine_diff_density_min -2.389 _refine_diff_density_rms 0.433