# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jihong Yu' _publ_contact_author_email JIHONG@JLU.EDU.CN _publ_section_title ; Spontaneous Crystallization of a New Chiral Open-Framework Borophosphate in the Ionothermal System ; loop_ _publ_author_name 'Jihong Yu.' 'Yi Li.' 'Hongzhu Xing.' 'Ruren Xu.' 'Jin Xu.' 'Weiting Yang.' ; Enbo Zhu ; # Attachment 'B919933K_725136.cif' data_JIS-2 _database_code_depnum_ccdc_archive 'CCDC 725136' #TrackingRef 'B919933K_725136.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'B H9 N2 O8 P2' _chemical_formula_weight 237.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P41212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 7.2392(10) _cell_length_b 7.2392(10) _cell_length_c 14.870(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 779.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7327 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 27.41 _exptl_crystal_description octahedral _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7670 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0110 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.41 _reflns_number_total 893 _reflns_number_gt 879 _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^)+(0.0371P)^2^+0.2180P] 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 none _refine_ls_extinction_coef ? _chemical_absolute_configuration ad _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(13) _refine_ls_number_reflns 893 _refine_ls_number_parameters 80 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.153 _refine_ls_shift/su_mean 0.058 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 B B 0.71259(11) 0.28741(11) 0.2500 0.0067(2) Uani 1 2 d S . . N N 0.36616(10) 0.03753(10) 0.07956(5) 0.01932(17) Uani 1 1 d . . . O1 O 0.99543(8) 0.21504(8) 0.09208(4) 0.01873(13) Uani 1 1 d . . . O2 O 0.98783(8) -0.08751(8) 0.17468(3) 0.01831(13) Uani 1 1 d . . . O3 O 0.76926(7) -0.03342(7) 0.04559(3) 0.00969(11) Uani 1 1 d . . . O4 O 0.71633(7) 0.13030(7) 0.18708(3) 0.01014(11) Uani 1 1 d . . . P1 P 0.87463(2) 0.06037(2) 0.124227(11) 0.00846(4) Uani 1 1 d . . . H1 H 0.4325(17) 0.1364(17) 0.0824(8) 0.037(3) Uiso 1 1 d . . . H2 H 0.4233(18) -0.0542(18) 0.1036(9) 0.053(4) Uiso 1 1 d . . . H3 H 0.3297(17) 0.0204(17) 0.0258(8) 0.033(3) Uiso 1 1 d . . . H4 H 0.2805(19) 0.0586(17) 0.1090(9) 0.046(4) Uiso 1 1 d . . . H5 H 1.020(4) -0.051(4) 0.2238(13) 0.041(8) Uiso 0.50 1 d P A -1 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 B 0.0072(3) 0.0072(3) 0.0056(4) 0.0007(3) 0.0007(3) 0.0002(4) N 0.0149(3) 0.0182(3) 0.0249(3) 0.0025(3) -0.0011(3) 0.0011(3) O1 0.0176(3) 0.0188(3) 0.0198(2) -0.0070(2) 0.0060(2) -0.0076(2) O2 0.0214(3) 0.0199(3) 0.0136(2) -0.0082(2) -0.0091(2) 0.0104(2) O3 0.0115(2) 0.0087(2) 0.0088(2) -0.00402(18) -0.00197(18) 0.00124(19) O4 0.0091(2) 0.0117(2) 0.0096(2) -0.00463(19) 0.00209(19) -0.00079(19) P1 0.00762(7) 0.00996(7) 0.00780(7) -0.00423(7) -0.00012(6) 0.00072(6) _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 B O3 1.4694(8) 5_655 ? B O3 1.4695(8) 3_545 ? B O4 1.4730(8) . ? B O4 1.4730(8) 8_665 ? N H1 0.863(12) . ? N H2 0.860(13) . ? N H3 0.851(11) . ? N H4 0.775(14) . ? O1 P1 1.4990(6) . ? O2 P1 1.5428(6) . ? O2 H5 0.81(2) . ? O3 B 1.4695(8) 4_554 ? O3 P1 1.5525(6) . ? O4 P1 1.5631(6) . ? 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 O3 B O3 111.76(8) 5_655 3_545 ? O3 B O4 112.76(3) 5_655 . ? O3 B O4 103.90(3) 3_545 . ? O3 B O4 103.90(3) 5_655 8_665 ? O3 B O4 112.76(3) 3_545 8_665 ? O4 B O4 112.03(8) . 8_665 ? H1 N H2 110.7(12) . . ? H1 N H3 109.8(12) . . ? H2 N H3 115.3(12) . . ? H1 N H4 104.7(12) . . ? H2 N H4 107.5(13) . . ? H3 N H4 108.2(13) . . ? P1 O2 H5 111.4(18) . . ? B O3 P1 133.59(4) 4_554 . ? B O4 P1 130.04(4) . . ? O1 P1 O2 111.32(3) . . ? O1 P1 O3 111.91(3) . . ? O2 P1 O3 108.89(3) . . ? O1 P1 O4 112.12(3) . . ? O2 P1 O4 108.87(3) . . ? O3 P1 O4 103.40(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.311 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.059