# 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_1 _database_code_depnum_ccdc_archive 'CCDC 926783' #TrackingRef '18057_web_deposit_cif_file_0_YingWang_1361952742.RbPbBP2O8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B O8 P2 Pb Rb' _chemical_formula_weight 493.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Rb Rb -0.9393 2.9676 '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 Tetragonal _symmetry_space_group_name_H-M I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 7.213(3) _cell_length_b 7.213(3) _cell_length_c 13.987(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 727.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 905 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 26.33 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.126 _exptl_crystal_size_mid 0.112 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 4.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 30.276 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.2768 _exptl_absorpt_correction_T_max 0.6521 _exptl_absorpt_process_details Face-indexed _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 2118 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.58 _reflns_number_total 428 _reflns_number_gt 400 _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^)+(0.0330P)^2^+6.8689P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens ? _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0061(8) _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 0.02(4) _refine_ls_number_reflns 428 _refine_ls_number_parameters 32 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0762 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.217 _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 Rb1 Rb 0.63600(10) 0.7500 0.1250 0.0264(4) Uani 0.50 2 d SP . . Pb1 Pb 0.63600(10) 0.7500 0.1250 0.0264(4) Uani 0.50 2 d SP . . B1 B 1.0000 0.0000 0.0000 0.045(3) Uani 1 4 d SU . . P1 P 0.8432(6) 0.2500 0.1250 0.0329(10) Uani 1 2 d SU . . O1 O 0.7274(17) 0.3925(13) 0.0768(8) 0.055(2) Uani 1 1 d U . . O2 O 0.9914(16) 0.1613(14) 0.0570(7) 0.049(2) 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 Rb1 0.0240(5) 0.0273(5) 0.0279(5) 0.0008(3) 0.000 0.000 Pb1 0.0240(5) 0.0273(5) 0.0279(5) 0.0008(3) 0.000 0.000 B1 0.046(4) 0.046(4) 0.042(6) 0.000 0.000 0.000 P1 0.045(2) 0.0265(18) 0.0275(19) -0.0115(17) 0.000 0.000 O1 0.062(5) 0.046(4) 0.058(4) 0.001(3) -0.016(4) -0.006(4) O2 0.055(4) 0.046(4) 0.046(4) -0.012(3) 0.007(3) -0.006(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 Rb1 O1 2.746(11) . ? Rb1 O1 2.746(11) 14_464 ? Rb1 O1 2.835(11) 4_655 ? Rb1 O1 2.835(11) 15_564 ? Rb1 O1 2.895(12) 2_665 ? Rb1 O1 2.895(12) 13_554 ? Rb1 O2 2.922(12) 13_654 ? Rb1 O2 2.922(12) 2_765 ? Rb1 O2 3.414(11) 15_564 ? Rb1 O2 3.414(11) 4_655 ? Rb1 P1 3.457(5) 2_665 ? B1 O2 1.412(10) . ? B1 O2 1.412(10) 4_645 ? B1 O2 1.412(10) 2_755 ? B1 O2 1.412(10) 3_665 ? P1 O1 1.486(11) 14_454 ? P1 O1 1.486(11) . ? P1 O2 1.567(11) 14_454 ? P1 O2 1.567(11) . ? O1 Rb1 2.835(11) 3_565 ? O1 Rb1 2.895(12) 2_665 ? O2 Rb1 2.922(12) 2_765 ? O2 Rb1 3.414(11) 3_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 O1 Rb1 O1 152.2(5) . 14_464 ? O1 Rb1 O1 73.7(3) . 4_655 ? O1 Rb1 O1 108.4(3) 14_464 4_655 ? O1 Rb1 O1 108.4(3) . 15_564 ? O1 Rb1 O1 73.7(3) 14_464 15_564 ? O1 Rb1 O1 171.7(4) 4_655 15_564 ? O1 Rb1 O1 80.0(4) . 2_665 ? O1 Rb1 O1 127.4(3) 14_464 2_665 ? O1 Rb1 O1 71.5(3) 4_655 2_665 ? O1 Rb1 O1 100.8(3) 15_564 2_665 ? O1 Rb1 O1 127.4(3) . 13_554 ? O1 Rb1 O1 80.0(4) 14_464 13_554 ? O1 Rb1 O1 100.8(3) 4_655 13_554 ? O1 Rb1 O1 71.5(3) 15_564 13_554 ? O1 Rb1 O1 50.2(4) 2_665 13_554 ? O1 Rb1 O2 69.7(3) . 13_654 ? O1 Rb1 O2 84.6(3) 14_464 13_654 ? O1 Rb1 O2 112.2(3) 4_655 13_654 ? O1 Rb1 O2 75.8(3) 15_564 13_654 ? O1 Rb1 O2 146.2(3) 2_665 13_654 ? O1 Rb1 O2 146.6(3) 13_554 13_654 ? O1 Rb1 O2 84.6(3) . 2_765 ? O1 Rb1 O2 69.7(3) 14_464 2_765 ? O1 Rb1 O2 75.8(3) 4_655 2_765 ? O1 Rb1 O2 112.2(3) 15_564 2_765 ? O1 Rb1 O2 146.6(3) 2_665 2_765 ? O1 Rb1 O2 146.2(3) 13_554 2_765 ? O2 Rb1 O2 46.2(4) 13_654 2_765 ? O1 Rb1 O2 66.5(3) . 15_564 ? O1 Rb1 O2 101.1(3) 14_464 15_564 ? O1 Rb1 O2 138.1(3) 4_655 15_564 ? O1 Rb1 O2 47.0(3) 15_564 15_564 ? O1 Rb1 O2 112.4(3) 2_665 15_564 ? O1 Rb1 O2 113.3(3) 13_554 15_564 ? O2 Rb1 O2 41.5(3) 13_654 15_564 ? O2 Rb1 O2 87.73(18) 2_765 15_564 ? O1 Rb1 O2 101.1(3) . 4_655 ? O1 Rb1 O2 66.5(3) 14_464 4_655 ? O1 Rb1 O2 47.0(3) 4_655 4_655 ? O1 Rb1 O2 138.1(3) 15_564 4_655 ? O1 Rb1 O2 113.3(3) 2_665 4_655 ? O1 Rb1 O2 112.4(3) 13_554 4_655 ? O2 Rb1 O2 87.73(18) 13_654 4_655 ? O2 Rb1 O2 41.5(3) 2_765 4_655 ? O2 Rb1 O2 129.3(3) 15_564 4_655 ? O1 Rb1 P1 103.9(2) . 2_665 ? O1 Rb1 P1 103.9(2) 14_464 2_665 ? O1 Rb1 P1 85.84(19) 4_655 2_665 ? O1 Rb1 P1 85.84(19) 15_564 2_665 ? O1 Rb1 P1 25.1(2) 2_665 2_665 ? O1 Rb1 P1 25.1(2) 13_554 2_665 ? O2 Rb1 P1 156.90(19) 13_654 2_665 ? O2 Rb1 P1 156.90(19) 2_765 2_665 ? O2 Rb1 P1 115.37(17) 15_564 2_665 ? O2 Rb1 P1 115.37(17) 4_655 2_665 ? O1 Rb1 B1 58.6(2) . 13_654 ? O1 Rb1 B1 100.1(2) 14_464 13_654 ? O1 Rb1 B1 120.2(2) 4_655 13_654 ? O1 Rb1 B1 66.5(2) 15_564 13_654 ? O1 Rb1 B1 126.2(2) 2_665 13_654 ? O1 Rb1 B1 135.9(2) 13_554 13_654 ? O2 Rb1 B1 21.57(19) 13_654 13_654 ? O2 Rb1 B1 66.46(19) 2_765 13_654 ? O2 Rb1 B1 22.84(16) 15_564 13_654 ? O2 Rb1 B1 107.61(17) 4_655 13_654 ? P1 Rb1 B1 136.270(13) 2_665 13_654 ? O2 B1 O2 108.6(4) . 4_645 ? O2 B1 O2 111.2(8) . 2_755 ? O2 B1 O2 108.6(4) 4_645 2_755 ? O2 B1 O2 108.6(4) . 3_665 ? O2 B1 O2 111.2(8) 4_645 3_665 ? O2 B1 O2 108.6(4) 2_755 3_665 ? O2 B1 Rb1 96.1(4) . 1_545 ? O2 B1 Rb1 69.8(4) 4_645 1_545 ? O2 B1 Rb1 49.5(5) 2_755 1_545 ? O2 B1 Rb1 152.7(5) 3_665 1_545 ? O2 B1 Rb1 69.8(4) . 3_565 ? O2 B1 Rb1 49.5(5) 4_645 3_565 ? O2 B1 Rb1 152.7(5) 2_755 3_565 ? O2 B1 Rb1 96.1(4) 3_665 3_565 ? Rb1 B1 Rb1 103.387(17) 1_545 3_565 ? O2 B1 Rb1 49.5(5) . 2_765 ? O2 B1 Rb1 152.7(5) 4_645 2_765 ? O2 B1 Rb1 96.0(4) 2_755 2_765 ? O2 B1 Rb1 69.8(4) 3_665 2_765 ? Rb1 B1 Rb1 122.48(4) 1_545 2_765 ? Rb1 B1 Rb1 103.387(17) 3_565 2_765 ? O2 B1 Rb1 152.7(5) . 4_745 ? O2 B1 Rb1 96.1(4) 4_645 4_745 ? O2 B1 Rb1 69.8(4) 2_755 4_745 ? O2 B1 Rb1 49.5(5) 3_665 4_745 ? Rb1 B1 Rb1 103.387(17) 1_545 4_745 ? Rb1 B1 Rb1 122.48(4) 3_565 4_745 ? Rb1 B1 Rb1 103.387(17) 2_765 4_745 ? O1 P1 O1 111.6(9) 14_454 . ? O1 P1 O2 113.0(6) 14_454 14_454 ? O1 P1 O2 112.1(5) . 14_454 ? O1 P1 O2 112.1(5) 14_454 . ? O1 P1 O2 113.0(6) . . ? O2 P1 O2 94.0(8) 14_454 . ? O1 P1 Rb1 55.8(5) 14_454 2_665 ? O1 P1 Rb1 55.8(5) . 2_665 ? O2 P1 Rb1 133.0(4) 14_454 2_665 ? O2 P1 Rb1 133.0(4) . 2_665 ? O1 P1 Rb1 119.1(5) 14_454 3_565 ? O1 P1 Rb1 46.1(4) . 3_565 ? O2 P1 Rb1 127.9(4) 14_454 3_565 ? O2 P1 Rb1 68.7(4) . 3_565 ? Rb1 P1 Rb1 79.40(7) 2_665 3_565 ? O1 P1 Rb1 46.1(4) 14_454 12_645 ? O1 P1 Rb1 119.1(5) . 12_645 ? O2 P1 Rb1 68.7(4) 14_454 12_645 ? O2 P1 Rb1 127.9(4) . 12_645 ? Rb1 P1 Rb1 79.40(7) 2_665 12_645 ? Rb1 P1 Rb1 158.80(13) 3_565 12_645 ? O1 P1 Rb1 124.2(5) 14_454 2_765 ? O1 P1 Rb1 124.2(5) . 2_765 ? O2 P1 Rb1 47.0(4) 14_454 2_765 ? O2 P1 Rb1 47.0(4) . 2_765 ? Rb1 P1 Rb1 180.0 2_665 2_765 ? Rb1 P1 Rb1 100.60(7) 3_565 2_765 ? Rb1 P1 Rb1 100.60(7) 12_645 2_765 ? O1 P1 Rb1 31.3(4) 14_454 1_545 ? O1 P1 Rb1 115.1(4) . 1_545 ? O2 P1 Rb1 129.7(4) 14_454 1_545 ? O2 P1 Rb1 83.3(4) . 1_545 ? Rb1 P1 Rb1 67.49(6) 2_665 1_545 ? Rb1 P1 Rb1 97.90(4) 3_565 1_545 ? Rb1 P1 Rb1 73.84(3) 12_645 1_545 ? Rb1 P1 Rb1 112.51(6) 2_765 1_545 ? P1 O1 Rb1 132.3(6) . . ? P1 O1 Rb1 111.7(6) . 3_565 ? Rb1 O1 Rb1 109.0(3) . 3_565 ? P1 O1 Rb1 99.1(5) . 2_665 ? Rb1 O1 Rb1 93.4(4) . 2_665 ? Rb1 O1 Rb1 105.0(3) 3_565 2_665 ? B1 O2 P1 135.2(8) . . ? B1 O2 Rb1 108.9(6) . 2_765 ? P1 O2 Rb1 109.9(5) . 2_765 ? B1 O2 Rb1 87.4(5) . 3_565 ? P1 O2 Rb1 86.0(4) . 3_565 ? Rb1 O2 Rb1 128.2(4) 2_765 3_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.056 _refine_diff_density_min -1.260 _refine_diff_density_rms 0.234