Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_junk _database_code_CSD 156617 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Choudhury, Amitava' 'Natarajan, Srinivasan' 'Neeraj, S.' 'Rao, C. N. R.' _publ_contact_author_name 'Prof C N R Rao' _publ_contact_author_address ; Chemistry & Physics of Materials Unit Jawaharlal Nehru Centre for Advanced Scientific Research Jaakur P.O. Bangalore 560 064 INDIA ; _publ_contact_author_email 'CNRRAO@JNCASR.AC.IN' _publ_section_title ; An Open-framework Zincoborate formed by Zn6B12O24 Clusters ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'H2.24 B2 O5.12 Zn1' _chemical_formula_weight 171.14 _chemical_melting_point ? _chemical_compound_source ? 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+1/3' 'x-y+2/3, -y+1/3, -z+1/3' '-x+2/3, -x+y+1/3, -z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+2/3' 'x-y+1/3, -y+2/3, -z+2/3' '-x+1/3, -x+y+2/3, -z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 11.4101(6) _cell_length_b 11.4101(6) _cell_length_c 17.1556(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1934.3(2) _cell_formula_units_Z 36 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1575 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description Rod _exptl_crystal_colour White _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.610 _exptl_crystal_density_method ? _exptl_crystal_F_000 1457 _exptl_absorpt_coefficient_mu 5.620 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.622389 _exptl_absorpt_correction_T_max 1.000000 _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 'Siemens CCD-diffractometer' _diffrn_measurement_method '\W' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2759 _diffrn_reflns_av_R_equivalents 0.1015 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 23.28 _reflns_number_total 371 _reflns_number_observed 306 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART(Siemens,1996)' _computing_cell_refinement 'SAINT(Siemens,1996)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL v5.0' _computing_publication_material 'SHELXTL v5.0' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0347P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 371 _refine_ls_number_parameters 49 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_obs 0.0300 _refine_ls_wR_factor_all 0.0757 _refine_ls_wR_factor_obs 0.0692 _refine_ls_goodness_of_fit_all 1.089 _refine_ls_goodness_of_fit_obs 1.114 _refine_ls_restrained_S_all 1.089 _refine_ls_restrained_S_obs 1.114 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Zn1 Zn 0.23547(4) 0.76453(4) 0.01308(4) 0.0177(4) Uani 1 d S . B1 B 0.4737(4) 0.9474(8) -0.0818(4) 0.013(2) Uani 1 d S . B2 B 0.1063(6) 0.6667 0.1667 0.011(2) Uani 1 d S . O1 O 0.2299(2) 0.7701(2) 0.1267(2) 0.0112(11) Uani 1 d S . O2 O 0.4225(2) 0.8450(4) -0.0272(2) 0.0127(11) Uani 1 d S . O3 O 0.1456(3) 0.8544(3) -0.0412(3) 0.048(2) Uani 1 d S . O4 O 0.3946(3) 0.9979(3) -0.1077(2) 0.0124(8) Uani 1 d . . O100 O 0.0000 1.0000 -0.1319(19) 0.071(15) Uani 0.36(3) d SP . 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 Zn1 0.0145(4) 0.0145(4) 0.0178(5) -0.0023(2) 0.0023(2) 0.0027(4) B1 0.015(3) 0.010(4) 0.013(4) -0.006(4) -0.003(2) 0.005(2) B2 0.011(3) 0.014(5) 0.007(4) -0.001(3) -0.001(2) 0.007(2) O1 0.010(2) 0.010(2) 0.010(2) -0.0008(9) 0.0008(9) 0.003(2) O2 0.013(2) 0.008(2) 0.015(2) 0.004(2) 0.0020(10) 0.0041(12) O3 0.032(3) 0.032(3) 0.063(4) 0.017(2) -0.017(2) 0.004(3) O4 0.009(2) 0.013(2) 0.016(2) 0.004(2) 0.0001(14) 0.006(2) O100 0.074(20) 0.074(20) 0.065(25) 0.000 0.000 0.037(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 Zn1 O1 1.953(4) . ? Zn1 O2 1.979(2) . ? Zn1 O2 1.979(2) 2_665 ? Zn1 O3 2.004(6) . ? B1 O4 1.365(5) 23 ? B1 O4 1.365(5) . ? B1 O2 1.378(9) . ? B2 O4 1.477(5) 30_465 ? B2 O4 1.477(5) 20_455 ? B2 O1 1.479(5) . ? B2 O1 1.479(5) 27 ? O1 B2 1.479(5) 26_455 ? O2 Zn1 1.979(2) 3_565 ? O4 B2 1.477(5) 21_665 ? 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 Zn1 O2 112.24(13) . . ? O1 Zn1 O2 112.24(13) . 2_665 ? O2 Zn1 O2 100.9(2) . 2_665 ? O1 Zn1 O3 114.5(2) . . ? O2 Zn1 O3 108.0(2) . . ? O2 Zn1 O3 108.0(2) 2_665 . ? O4 B1 O4 121.4(6) 23 . ? O4 B1 O2 119.3(3) 23 . ? O4 B1 O2 119.3(3) . . ? O4 B2 O4 107.4(5) 30_465 20_455 ? O4 B2 O1 110.7(2) 30_465 . ? O4 B2 O1 107.7(2) 20_455 . ? O4 B2 O1 107.7(2) 30_465 27 ? O4 B2 O1 110.7(2) 20_455 27 ? O1 B2 O1 112.6(6) . 27 ? B2 O1 B2 122.3(3) 26_455 . ? B2 O1 Zn1 118.0(2) 26_455 . ? B2 O1 Zn1 118.0(2) . . ? B1 O2 Zn1 122.15(10) . . ? B1 O2 Zn1 122.15(10) . 3_565 ? Zn1 O2 Zn1 115.7(2) . 3_565 ? B1 O4 B2 123.4(4) . 21_665 ? _refine_diff_density_max 0.971 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.302