# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Hu, Fei' 'Zhai, Quan-Guo' 'Li, Shuni' 'Jiang, Yucheng' 'Hu, Mancheng' _publ_contact_author_name 'Zhai, Quan-Guo' _publ_contact_author_email zhaiqg@snnu.edu.cn _publ_section_title ; Ionothermal synthesis of a new (4, 12)-connected heterometalic iodoplumbate with [Pb4(OH)4] cubane as jointing points of helices ; # Attachment '- 1.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 793574' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Br Cu H2 I2 O2 Pb2' _chemical_formula_sum 'Br Cu H2 I2 O2 Pb2' _chemical_formula_weight 845.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/acd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/4, x+3/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+1/4, -x+1/4, z+3/4' 'x, -y, -z+1/2' 'y+1/4, x+3/4, -z+3/4' '-x+1/2, y, -z' '-y+1/4, -x+1/4, -z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+3/4, x+5/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+3/4, -x+3/4, z+5/4' 'x+1/2, -y+1/2, -z+1' 'y+3/4, x+5/4, -z+5/4' '-x+1, y+1/2, -z+1/2' '-y+3/4, -x+3/4, -z+3/4' '-x, -y, -z' 'y-1/4, -x-3/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-1/4, x-1/4, -z-3/4' '-x, y, z-1/2' '-y-1/4, -x-3/4, z-3/4' 'x-1/2, -y, z' 'y-1/4, x-1/4, z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y+1/4, -x-1/4, -z+1/4' 'x, y+1/2, -z' '-y+1/4, x+1/4, -z-1/4' '-x+1/2, y+1/2, z' '-y+1/4, -x-1/4, z-1/4' 'x, -y+1/2, z+1/2' 'y+1/4, x+1/4, z+1/4' _cell_length_a 14.5579(14) _cell_length_b 14.5579(14) _cell_length_c 16.2961(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3453.7(6) _cell_formula_units_Z 16 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2071 _cell_measurement_theta_min 2.796 _cell_measurement_theta_max 26.891 _exptl_crystal_description polyhedron _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5632 _exptl_absorpt_coefficient_mu 53.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0246 _exptl_absorpt_correction_T_max 0.0376 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 8002 _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.02 _reflns_number_total 755 _reflns_number_gt 546 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1270P)^2^+634.1979P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 755 _refine_ls_number_parameters 38 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.2178 _refine_ls_wR_factor_gt 0.1995 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Pb1 Pb 0.09524(7) 0.15314(7) 0.95673(7) 0.0114(6) Uani 1 1 d . . . Cu1 Cu -0.1667(3) 0.0833(3) 1.1250 0.0209(13) Uani 1 2 d S . . Br1 Br -0.2500 0.0210(2) 1.0000 0.0093(9) Uani 1 2 d S . . I1 I 0.00302(16) 0.04702(16) 1.12310(12) 0.0266(8) Uani 1 1 d . . . O1 O 0.0706(13) 0.3201(13) 0.9399(11) 0.005(4) Uani 1 1 d . . . H1A H 0.1041 0.3531 0.9709 0.006 Uiso 1 1 d R . . 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 0.0106(8) 0.0092(8) 0.0143(8) 0.0030(4) -0.0037(4) 0.0075(4) Cu1 0.0208(19) 0.0208(19) 0.021(3) 0.0002(17) -0.0002(17) -0.001(2) Br1 0.0096(18) 0.0082(19) 0.0102(19) 0.000 -0.0046(15) 0.000 I1 0.0259(14) 0.0273(14) 0.0266(14) 0.0002(11) 0.0004(9) 0.0002(10) O1 0.005(9) 0.005(9) 0.005(9) 0.000(8) 0.000(8) 0.000(8) _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 O1 2.447(18) 18_567 ? Pb1 O1 2.461(18) 11_454 ? Pb1 O1 2.473(19) . ? Pb1 I1 3.397(2) . ? Cu1 I1 2.527(4) 14_446 ? Cu1 I1 2.527(4) . ? Cu1 Br1 2.538(4) . ? Cu1 Br1 2.538(4) 12_444 ? Br1 Cu1 2.538(4) 10_444 ? O1 Pb1 2.447(18) 28_557 ? O1 Pb1 2.461(18) 11_454 ? O1 H1A 0.8501 . ? 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 Pb1 O1 73.8(7) 18_567 11_454 ? O1 Pb1 O1 73.6(7) 18_567 . ? O1 Pb1 O1 72.0(7) 11_454 . ? O1 Pb1 I1 142.3(4) 18_567 . ? O1 Pb1 I1 76.9(5) 11_454 . ? O1 Pb1 I1 118.6(4) . . ? I1 Cu1 I1 114.1(2) 14_446 . ? I1 Cu1 Br1 105.02(9) 14_446 . ? I1 Cu1 Br1 112.51(6) . . ? I1 Cu1 Br1 112.51(6) 14_446 12_444 ? I1 Cu1 Br1 105.02(9) . 12_444 ? Br1 Cu1 Br1 107.7(2) . 12_444 ? Cu1 Br1 Cu1 138.2(2) . 10_444 ? Cu1 I1 Pb1 107.54(9) . . ? Pb1 O1 Pb1 103.8(7) 28_557 11_454 ? Pb1 O1 Pb1 103.4(7) 28_557 . ? Pb1 O1 Pb1 106.6(7) 11_454 . ? Pb1 O1 H1A 114.0 28_557 . ? Pb1 O1 H1A 114.0 11_454 . ? Pb1 O1 H1A 114.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I1 Cu1 Br1 Cu1 11.08(11) 14_446 . . 10_444 ? I1 Cu1 Br1 Cu1 -113.59(19) . . . 10_444 ? Br1 Cu1 Br1 Cu1 131.17(5) 12_444 . . 10_444 ? I1 Cu1 I1 Pb1 -56.88(6) 14_446 . . . ? Br1 Cu1 I1 Pb1 62.6(2) . . . . ? Br1 Cu1 I1 Pb1 179.46(10) 12_444 . . . ? O1 Pb1 I1 Cu1 -46.0(8) 18_567 . . . ? O1 Pb1 I1 Cu1 -6.5(5) 11_454 . . . ? O1 Pb1 I1 Cu1 54.2(5) . . . . ? O1 Pb1 O1 Pb1 -17.9(7) 18_567 . . 28_557 ? O1 Pb1 O1 Pb1 -95.8(5) 11_454 . . 28_557 ? I1 Pb1 O1 Pb1 -159.0(4) . . . 28_557 ? O1 Pb1 O1 Pb1 91.1(6) 18_567 . . 11_454 ? O1 Pb1 O1 Pb1 13.3(9) 11_454 . . 11_454 ? I1 Pb1 O1 Pb1 -50.0(8) . . . 11_454 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.588 _refine_diff_density_min -5.726 _refine_diff_density_rms 1.002