data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Wang, Sue-Lein' _publ_contact_author_email slwang@mx.nthu.edu.tw _publ_section_title ; An Extraordinary Boron-Mediated 16R-Channel-Containing Trivalent Vanadium Phosphite with Unique Solid State Redox Property ; loop_ _publ_author_name 'Hui-Lin Huang' 'Sue-Lein Wang' # Attachment 'R2.cif.txt' data_VPO _database_code_depnum_ccdc_archive 'CCDC 774870' #TrackingRef 'R2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H81.86 B0.43 N3 O60.43 P16.57 V9' _chemical_formula_weight 2283.89 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' 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' V V 0.3005 0.5294 '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' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 13.4541(9) _cell_length_b 13.4541(9) _cell_length_c 27.755(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4350.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 15716 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour 'light green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 1.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.589 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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_reflns_number 29726 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.12 _reflns_number_total 3290 _reflns_number_gt 2993 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'SAINT V7.34A (Bruker AXS, 2006)' _computing_data_reduction 'SAINT V7.34A (Bruker AXS, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0623P)^2^+6.6215P] 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 3290 _refine_ls_number_parameters 134 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1174 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 V1 V 0.0000 0.0000 0.5000 0.0187(2) Uani 1 6 d S . . V2 V 0.14188(4) 0.43412(4) 0.473224(19) 0.02839(15) Uani 1 1 d . . . V3 V 0.0000 0.0000 0.33611(3) 0.0298(2) Uani 1 3 d S . . P1 P 0.02560(6) 0.18704(6) 0.41572(2) 0.02449(18) Uani 1 1 d . . . P2 P -0.12713(6) 0.36902(6) 0.46431(3) 0.02665(18) Uani 1 1 d . . . P3 P 0.19180(10) 0.06297(11) 0.2500 0.0345(3) Uani 1 2 d SD . . P4 P 0.3333 0.6667 0.41041(10) 0.0260(8) Uani 0.784(9) 3 d SP . 1 O9 O 0.2278(2) 0.5523(2) 0.42348(10) 0.0440(6) Uani 0.784(9) 1 d P . 1 H4 H 0.3333 0.6667 0.3644 0.050 Uiso 0.78 3 d SP . 1 B B 0.3333 0.6667 0.419(3) 0.0260(8) Uani 0.216(9) 3 d SP . 2 O9' O 0.2278(2) 0.5523(2) 0.42348(10) 0.0440(6) Uani 0.216(9) 1 d P . 2 O1 O -0.02643(16) 0.10887(16) 0.45959(7) 0.0255(4) Uani 1 1 d . . . O2 O 0.07122(19) 0.14026(18) 0.37740(7) 0.0335(5) Uani 1 1 d . . . O3 O 0.11973(18) 0.30721(17) 0.42953(8) 0.0333(5) Uani 1 1 d . . . O4 O -0.00149(17) 0.42734(19) 0.45040(9) 0.0376(5) Uani 1 1 d . . . O5 O -0.16654(19) 0.45285(19) 0.47659(9) 0.0396(5) Uani 1 1 d . . . O6 O -0.15193(17) 0.28152(18) 0.50400(9) 0.0382(5) Uani 1 1 d . . . O7 O 0.1419(2) 0.0764(3) 0.29531(9) 0.0539(7) Uani 1 1 d . A . O8 O 0.3226(9) 0.138(2) 0.2500 0.087(4) Uani 0.31(2) 1 d PD A 1 H7 H 0.3515 0.0966 0.2500 0.050 Uiso 0.31(2) 1 calc PR A 1 O8' O 0.3118(19) 0.169(3) 0.2500 0.087(4) Uani 0.19(2) 1 d PD A 2 H7' H 0.3064 0.2271 0.2500 0.050 Uiso 0.19(2) 1 calc PR A 2 O10 O 0.05342(17) 0.31066(17) 0.52658(8) 0.0317(4) Uani 1 1 d . . . H1 H -0.0634 0.1964 0.3966 0.050 Uiso 1 1 d . . . H2 H -0.1951 0.3081 0.4218 0.050 Uiso 1 1 d . . . H3 H 0.2001 -0.0425 0.2500 0.050 Uiso 1 2 d S . . H5 H 0.0598 0.2545 0.5272 0.050 Uiso 1 1 d . . . H6 H -0.0187 0.2811 0.5263 0.050 Uiso 1 1 d . . . 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 V1 0.0174(3) 0.0174(3) 0.0213(5) 0.000 0.000 0.00868(15) V2 0.0210(2) 0.0205(2) 0.0453(3) -0.00063(19) -0.00028(19) 0.01159(18) V3 0.0351(3) 0.0351(3) 0.0192(4) 0.000 0.000 0.01753(15) P1 0.0252(3) 0.0226(3) 0.0262(4) 0.0028(2) -0.0005(3) 0.0124(3) P2 0.0194(3) 0.0193(3) 0.0422(4) -0.0051(3) -0.0047(3) 0.0104(3) P3 0.0281(5) 0.0483(7) 0.0296(5) 0.000 0.000 0.0209(5) P4 0.0246(6) 0.0246(6) 0.0288(19) 0.000 0.000 0.0123(3) O9 0.0317(12) 0.0310(11) 0.0623(15) 0.0073(10) 0.0050(10) 0.0105(10) B 0.0246(6) 0.0246(6) 0.0288(19) 0.000 0.000 0.0123(3) O9' 0.0317(12) 0.0310(11) 0.0623(15) 0.0073(10) 0.0050(10) 0.0105(10) O1 0.0274(9) 0.0235(9) 0.0271(9) 0.0018(7) 0.0004(8) 0.0138(8) O2 0.0387(12) 0.0293(10) 0.0279(10) -0.0009(8) 0.0051(9) 0.0134(9) O3 0.0301(10) 0.0230(10) 0.0413(12) 0.0000(8) 0.0058(9) 0.0090(8) O4 0.0216(10) 0.0380(11) 0.0528(13) 0.0067(10) 0.0013(9) 0.0148(9) O5 0.0350(11) 0.0319(11) 0.0621(15) -0.0111(10) -0.0108(10) 0.0245(10) O6 0.0194(9) 0.0278(10) 0.0647(15) 0.0090(10) -0.0019(9) 0.0098(8) O7 0.0550(15) 0.0661(17) 0.0300(12) 0.0001(11) 0.0110(11) 0.0222(14) O8 0.049(4) 0.100(9) 0.126(5) 0.000 0.000 0.048(4) O8' 0.049(4) 0.100(9) 0.126(5) 0.000 0.000 0.048(4) O10 0.0271(10) 0.0266(10) 0.0429(12) -0.0003(8) -0.0002(8) 0.0145(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 V1 O1 2.0126(19) 8_556 ? V1 O1 2.0126(19) 2 ? V1 O1 2.0126(19) 9_556 ? V1 O1 2.0126(19) 7_556 ? V1 O1 2.0125(19) 3 ? V1 O1 2.0126(19) . ? V2 O5 1.964(2) 7_566 ? V2 O9 1.983(2) . ? V2 O6 1.986(2) 8_556 ? V2 O4 1.989(2) . ? V2 O3 1.991(2) . ? V2 O10 2.096(2) . ? V3 O2 1.996(2) 3 ? V3 O2 1.996(2) . ? V3 O2 1.996(2) 2 ? V3 O7 2.005(3) . ? V3 O7 2.005(3) 3 ? V3 O7 2.005(3) 2 ? P1 O2 1.513(2) . ? P1 O3 1.522(2) . ? P1 O1 1.531(2) . ? P1 H1 1.3719 . ? P2 O5 1.506(2) . ? P2 O4 1.515(2) . ? P2 O6 1.522(2) . ? P2 H2 1.4666 . ? P3 O7 1.478(2) 10_556 ? P3 O7 1.478(2) . ? P3 O8 1.529(10) . ? P3 O8' 1.529(18) . ? P3 H3 1.4781 . ? P4 O9 1.527(2) . ? P4 O9 1.527(2) 3_565 ? P4 O9 1.527(2) 2_665 ? P4 H4 1.2769 . ? B O9' 1.488(7) 3_565 ? B O9' 1.488(7) 2_665 ? B H4 1.5233 . ? O5 V2 1.964(2) 7_566 ? O6 V2 1.986(2) 9_556 ? O8 H7 0.8200 . ? O8' H7' 0.8200 . ? O10 H5 0.8021 . ? O10 H6 0.8449 . ? 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 V1 O1 180.00(10) 8_556 2 ? O1 V1 O1 91.96(8) 8_556 9_556 ? O1 V1 O1 88.04(8) 2 9_556 ? O1 V1 O1 91.96(8) 8_556 7_556 ? O1 V1 O1 88.04(8) 2 7_556 ? O1 V1 O1 91.96(8) 9_556 7_556 ? O1 V1 O1 88.04(8) 8_556 3 ? O1 V1 O1 91.96(8) 2 3 ? O1 V1 O1 180.00(9) 9_556 3 ? O1 V1 O1 88.04(8) 7_556 3 ? O1 V1 O1 88.04(8) 8_556 . ? O1 V1 O1 91.96(8) 2 . ? O1 V1 O1 88.04(8) 9_556 . ? O1 V1 O1 179.997(1) 7_556 . ? O1 V1 O1 91.96(8) 3 . ? O5 V2 O9 93.91(11) 7_566 . ? O5 V2 O6 89.07(9) 7_566 8_556 ? O9 V2 O6 92.95(10) . 8_556 ? O5 V2 O4 92.63(10) 7_566 . ? O9 V2 O4 88.77(10) . . ? O6 V2 O4 177.50(9) 8_556 . ? O5 V2 O3 172.11(10) 7_566 . ? O9 V2 O3 92.32(10) . . ? O6 V2 O3 85.78(9) 8_556 . ? O4 V2 O3 92.34(10) . . ? O5 V2 O10 85.51(10) 7_566 . ? O9 V2 O10 179.04(10) . . ? O6 V2 O10 86.28(9) 8_556 . ? O4 V2 O10 92.02(9) . . ? O3 V2 O10 88.20(9) . . ? O2 V3 O2 90.32(9) 3 . ? O2 V3 O2 90.32(9) 3 2 ? O2 V3 O2 90.32(9) . 2 ? O2 V3 O7 91.01(11) 3 . ? O2 V3 O7 87.46(10) . . ? O2 V3 O7 177.42(11) 2 . ? O2 V3 O7 87.47(10) 3 3 ? O2 V3 O7 177.42(11) . 3 ? O2 V3 O7 91.01(11) 2 3 ? O7 V3 O7 91.25(11) . 3 ? O2 V3 O7 177.42(11) 3 2 ? O2 V3 O7 91.01(11) . 2 ? O2 V3 O7 87.46(10) 2 2 ? O7 V3 O7 91.25(11) . 2 ? O7 V3 O7 91.25(11) 3 2 ? O2 P1 O3 108.88(12) . . ? O2 P1 O1 114.49(12) . . ? O3 P1 O1 112.41(12) . . ? O2 P1 H1 108.7 . . ? O3 P1 H1 107.5 . . ? O1 P1 H1 104.5 . . ? O5 P2 O4 112.91(13) . . ? O5 P2 O6 113.11(14) . . ? O4 P2 O6 109.95(12) . . ? O5 P2 H2 104.2 . . ? O4 P2 H2 107.9 . . ? O6 P2 H2 108.4 . . ? O7 P3 O7 116.6(2) 10_556 . ? O7 P3 O8 111.3(5) 10_556 . ? O7 P3 O8 111.3(5) . . ? O7 P3 O8' 102.6(8) 10_556 . ? O7 P3 O8' 102.6(8) . . ? O8 P3 O8' 19.1(10) . . ? O7 P3 H3 112.0 10_556 . ? O7 P3 H3 112.0 . . ? O8 P3 H3 91.0 . . ? O8' P3 H3 110.1 . . ? O9 P4 O9 114.54(11) . 3_565 ? O9 P4 O9 114.54(11) . 2_665 ? O9 P4 O9 114.54(11) 3_565 2_665 ? O9 P4 H4 103.7 . . ? O9 P4 H4 103.7 3_565 . ? O9 P4 H4 103.7 2_665 . ? P4 O9 V2 148.12(19) . . ? O9' B O9' 119.4(8) 3_565 2_665 ? O9' B H4 94.5 3_565 . ? O9' B H4 94.5 2_665 . ? P1 O1 V1 139.19(12) . . ? P1 O2 V3 133.93(13) . . ? P1 O3 V2 138.79(13) . . ? P2 O4 V2 138.42(15) . . ? P2 O5 V2 138.93(15) . 7_566 ? P2 O6 V2 134.34(13) . 9_556 ? P3 O7 V3 142.36(19) . . ? P3 O8 H7 109.5 . . ? P3 O8' H7' 109.5 . . ? V2 O10 H5 118.4 . . ? V2 O10 H6 115.5 . . ? H5 O10 H6 101.3 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.043 0.520 0.250 1014 231 ' ' 2 -0.033 0.450 0.750 1014 232 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.382 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.089