# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 182/1632

 
# Supplementary material for C.-Y. Chen, F.-R. Lo, H.-M. Kao and K.-H. Lii
# Correspondence author:
# K.-H. Lii, Department of Chemistry, National Central University, Chungli,
# Taiwan 320, e-mail: liikh@cc.ncu.edu.tw, fax: 886-3-4227664
#
data_GaPO
 
_audit_creation_method            SHELXTL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      
[Ga4(C10H9N2)2(PO4)(H0.5PO4)2(HPO4)2(H2PO4)2(H2O)2].H2O
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C20 H31 Ga4 N4 O31 P7' 
_chemical_formula_weight          1319.16 
_chemical_melting_point           ? 
_chemical_compound_source         'hydrothermal synthesis '
 
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' 
 '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' 
 'Ga'  'Ga'   0.2307   1.6083 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    C2/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    26.4161(6) 
_cell_length_b                    8.04160(10) 
_cell_length_c                    20.3515(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  111.1940(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      4030.81(13) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     7407 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        plate 
_exptl_crystal_colour             colorless 
_exptl_crystal_size_max           0.135  
_exptl_crystal_size_mid           0.063  
_exptl_crystal_size_min           0.027  
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.174 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2624 
_exptl_absorpt_coefficient_mu     3.037 
_exptl_absorpt_correction_type    'empirical (SADABS program)' 
_exptl_absorpt_correction_T_min   0.815 
_exptl_absorpt_correction_T_max   0.922 
 
_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 Smart CCD '
_diffrn_measurement_method        ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             11223 
_diffrn_reflns_av_R_equivalents   0.0564 
_diffrn_reflns_av_sigmaI/netI     0.0789 
_diffrn_reflns_limit_h_min        -32 
_diffrn_reflns_limit_h_max        33 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        25 
_diffrn_reflns_theta_min          1.65 
_diffrn_reflns_theta_max          28.03 
_reflns_number_total              4388 
_reflns_number_observed           3120 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXTL (Sheldrick, 1998)' 
_computing_structure_refinement   'SHELXTL (Sheldrick, 1998)' 
_computing_molecular_graphics     ATOMS 
_computing_publication_material   ? 
 
_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^)+(0.0153P)^2^+13.4357P] 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     difmap 
_refine_ls_extinction_method      SHELXTL 
_refine_ls_extinction_coef        0.00044(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          4388 
_refine_ls_number_parameters      356 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0803 
_refine_ls_R_factor_obs           0.0429 
_refine_ls_wR_factor_all          0.0903 
_refine_ls_wR_factor_obs          0.0776 
_refine_ls_goodness_of_fit_all    1.068 
_refine_ls_goodness_of_fit_obs    1.108 
_refine_ls_restrained_S_all       1.068 
_refine_ls_restrained_S_obs       1.108 
_refine_ls_shift/esd_max          -0.074 
_refine_ls_shift/esd_mean         0.004 
 
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 
Ga1 Ga 0.02224(2) 0.61417(6) 0.40892(3) 0.01300(14) Uani 1 d . . 
Ga2 Ga 0.09780(2) 0.33717(7) 0.21707(3) 0.01544(15) Uani 1 d . . 
P1 P 0.0000 0.4461(2) 0.2500 0.0126(4) Uani 1 d S . 
P2 P -0.10875(5) 0.6823(2) 0.33873(7) 0.0165(3) Uani 1 d . . 
P3 P 0.20837(5) 0.1602(2) 0.27033(7) 0.0185(3) Uani 1 d . . 
P4 P -0.02116(5) 0.26295(15) 0.44064(6) 0.0122(3) Uani 1 d . . 
O1 O 0.00747(13) 0.5551(4) 0.3128(2) 0.0216(8) Uani 1 d . . 
O2 O -0.04924(12) 0.3279(4) 0.2376(2) 0.0218(8) Uani 1 d . . 
O3 O -0.14946(14) 0.6848(5) 0.3749(2) 0.0305(9) Uani 1 d . . 
O4 O -0.05332(12) 0.6568(4) 0.3933(2) 0.0232(8) Uani 1 d . . 
O5 O -0.1104(2) 0.8483(5) 0.3000(2) 0.0333(10) Uani 1 d . . 
O6 O -0.12318(13) 0.5466(4) 0.2816(2) 0.0246(8) Uani 1 d . . 
O7 O 0.15296(12) 0.2107(4) 0.2739(2) 0.0201(8) Uani 1 d . . 
O8 O 0.25203(13) 0.2010(5) 0.3404(2) 0.0299(9) Uani 1 d . . 
O9 O 0.2174(2) 0.2618(6) 0.2102(2) 0.0350(11) Uani 1 d . . 
O10 O 0.20592(14) -0.0215(4) 0.2515(2) 0.0381(10) Uani 1 d . . 
O11 O 0.00719(12) 0.0896(4) 0.4551(2) 0.0168(7) Uani 1 d . . 
O12 O 0.02055(12) 0.3851(4) 0.4360(2) 0.0178(7) Uani 1 d . . 
O13 O -0.04409(12) 0.2976(4) 0.4974(2) 0.0164(7) Uani 1 d . . 
O14 O -0.06978(12) 0.2472(4) 0.3702(2) 0.0219(8) Uani 1 d . . 
O15 O 0.03038(15) 0.8498(5) 0.3766(2) 0.0226(8) Uani 1 d . . 
N1 N 0.10581(15) 0.5892(5) 0.4300(2) 0.0158(9) Uani 1 d . . 
N2 N 0.3829(2) 0.4258(6) 0.5102(3) 0.0346(12) Uani 1 d . . 
C1 C 0.1835(2) 0.5902(8) 0.3965(3) 0.0299(13) Uani 1 d . . 
C2 C 0.1291(2) 0.6166(7) 0.3826(3) 0.0254(12) Uani 1 d . . 
C3 C 0.1380(2) 0.5393(7) 0.4938(3) 0.0262(13) Uani 1 d . . 
C4 C 0.1929(2) 0.5134(8) 0.5122(3) 0.0313(14) Uani 1 d . . 
C5 C 0.2171(2) 0.5367(6) 0.4631(3) 0.0213(11) Uani 1 d . . 
C6 C 0.2760(2) 0.5008(6) 0.4803(3) 0.0219(11) Uani 1 d . . 
C7 C 0.3024(2) 0.5494(8) 0.4357(3) 0.0294(13) Uani 1 d . . 
C8 C 0.3561(2) 0.5099(7) 0.4515(3) 0.0298(13) Uani 1 d . . 
C9 C 0.3589(2) 0.3787(9) 0.5556(3) 0.039(2) Uani 1 d . . 
C10 C 0.3054(2) 0.4136(8) 0.5413(3) 0.0319(14) Uani 1 d . . 
OW O 0.0347(3) 0.9662(10) 0.2545(4) 0.034(2) Uiso 0.50 d P . 
H3O H -0.1895(31) 0.6807(91) 0.3537(39) 0.088(26) Uiso 1 d . . 
H5O H -0.1382(27) 0.8887(89) 0.2837(36) 0.060(25) Uiso 1 d . . 
H9O H 0.2370(26) 0.3245(83) 0.2278(35) 0.047(23) Uiso 1 d . . 
H11O H 0.0000 0.0000 0.5000 0.069(30) Uiso 1 d S . 
H1C H 0.1979(21) 0.6159(66) 0.3648(28) 0.032(15) Uiso 1 d . . 
H2C H 0.1034(23) 0.6521(70) 0.3361(31) 0.045(17) Uiso 1 d . . 
H3C H 0.1220(19) 0.5180(60) 0.5293(25) 0.024(14) Uiso 1 d . . 
H4C H 0.2121(22) 0.4835(69) 0.5581(30) 0.040(17) Uiso 1 d . . 
H7C H 0.2843(20) 0.5935(64) 0.3949(27) 0.023(15) Uiso 1 d . . 
H8C H 0.3763(23) 0.5481(75) 0.4196(31) 0.051(18) Uiso 1 d . . 
H9C H 0.3795(22) 0.3219(71) 0.5929(30) 0.038(17) Uiso 1 d . . 
H10C H 0.2922(22) 0.3760(69) 0.5714(29) 0.035(17) Uiso 1 d . . 
H15A H 0.0186(21) 0.9288(72) 0.3936(29) 0.030(17) Uiso 1 d . . 
H15B H 0.0161(24) 0.8816(74) 0.3355(33) 0.041(19) Uiso 1 d . . 
H2N H 0.4271(35) 0.4025(103) 0.5204(42) 0.110(29) Uiso 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 
Ga1 0.0119(3) 0.0152(3) 0.0121(3) -0.0012(2) 0.0047(2) -0.0005(2) 
Ga2 0.0131(3) 0.0192(3) 0.0129(3) 0.0005(2) 0.0034(2) 0.0014(2) 
P1 0.0114(8) 0.0165(9) 0.0104(9) 0.000 0.0046(7) 0.000 
P2 0.0133(6) 0.0187(7) 0.0167(7) 0.0001(5) 0.0042(5) 0.0022(5) 
P3 0.0120(6) 0.0200(7) 0.0224(7) -0.0023(5) 0.0049(5) 0.0000(5) 
P4 0.0123(6) 0.0139(6) 0.0104(6) 0.0001(5) 0.0041(5) 0.0006(5) 
O1 0.020(2) 0.031(2) 0.011(2) -0.0060(15) 0.0034(14) -0.002(2) 
O2 0.018(2) 0.023(2) 0.029(2) -0.006(2) 0.014(2) -0.0070(15) 
O3 0.015(2) 0.053(3) 0.025(2) 0.000(2) 0.010(2) 0.004(2) 
O4 0.012(2) 0.037(2) 0.019(2) -0.005(2) 0.0037(14) 0.004(2) 
O5 0.028(2) 0.023(2) 0.047(3) 0.009(2) 0.011(2) 0.003(2) 
O6 0.022(2) 0.026(2) 0.020(2) -0.004(2) 0.000(2) 0.006(2) 
O7 0.014(2) 0.027(2) 0.019(2) 0.0031(14) 0.0053(14) 0.0066(14) 
O8 0.015(2) 0.049(3) 0.021(2) -0.001(2) 0.0009(15) -0.002(2) 
O9 0.040(2) 0.045(3) 0.021(2) -0.004(2) 0.012(2) -0.015(2) 
O10 0.025(2) 0.019(2) 0.071(3) -0.013(2) 0.017(2) 0.001(2) 
O11 0.020(2) 0.013(2) 0.020(2) 0.0034(13) 0.0109(15) 0.0050(14) 
O12 0.017(2) 0.015(2) 0.024(2) 0.0013(14) 0.0102(14) -0.0033(14) 
O13 0.013(2) 0.023(2) 0.013(2) -0.0048(13) 0.0053(13) -0.0022(14) 
O14 0.022(2) 0.029(2) 0.012(2) 0.0005(14) 0.0020(14) -0.005(2) 
O15 0.033(2) 0.019(2) 0.016(2) 0.001(2) 0.010(2) 0.002(2) 
N1 0.017(2) 0.014(2) 0.017(2) -0.001(2) 0.006(2) -0.001(2) 
N2 0.015(2) 0.047(3) 0.043(3) -0.010(2) 0.012(2) -0.002(2) 
C1 0.022(3) 0.047(4) 0.025(3) 0.008(3) 0.014(2) 0.000(3) 
C2 0.020(3) 0.041(4) 0.016(3) 0.005(2) 0.009(2) 0.004(2) 
C3 0.017(3) 0.044(4) 0.023(3) 0.009(2) 0.014(2) 0.004(2) 
C4 0.023(3) 0.050(4) 0.021(3) 0.011(3) 0.008(2) 0.006(3) 
C5 0.016(2) 0.028(3) 0.021(3) 0.000(2) 0.007(2) 0.000(2) 
C6 0.019(3) 0.025(3) 0.024(3) -0.003(2) 0.010(2) -0.001(2) 
C7 0.024(3) 0.041(4) 0.025(3) 0.001(3) 0.011(3) -0.002(3) 
C8 0.021(3) 0.039(4) 0.035(3) -0.009(3) 0.017(3) -0.007(3) 
C9 0.022(3) 0.052(4) 0.036(4) 0.005(3) 0.001(3) 0.012(3) 
C10 0.023(3) 0.042(4) 0.032(3) 0.005(3) 0.012(3) 0.003(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 
Ga1 O1 1.912(3) . ? 
Ga1 O13 1.918(3) 5_566 ? 
Ga1 O12 1.928(3) . ? 
Ga1 O4 1.935(3) . ? 
Ga1 O15 2.043(4) . ? 
Ga1 N1 2.101(4) . ? 
Ga2 O14 1.810(3) 2 ? 
Ga2 O6 1.810(3) 2 ? 
Ga2 O7 1.810(3) . ? 
Ga2 O2 1.832(3) 2 ? 
P1 O1 1.503(3) . ? 
P1 O1 1.503(3) 2 ? 
P1 O2 1.556(3) 2 ? 
P1 O2 1.556(3) . ? 
P2 O4 1.498(3) . ? 
P2 O3 1.508(3) . ? 
P2 O6 1.538(3) . ? 
P2 O5 1.543(4) . ? 
P3 O10 1.506(4) . ? 
P3 O8 1.511(4) . ? 
P3 O7 1.546(3) . ? 
P3 O9 1.559(4) . ? 
P4 O12 1.504(3) . ? 
P4 O13 1.511(3) . ? 
P4 O14 1.546(3) . ? 
P4 O11 1.559(3) . ? 
O2 Ga2 1.832(3) 2 ? 
O6 Ga2 1.810(3) 2 ? 
O13 Ga1 1.918(3) 5_566 ? 
O14 Ga2 1.810(3) 2 ? 
N1 C3 1.331(6) . ? 
N1 C2 1.335(6) . ? 
N2 C8 1.332(7) . ? 
N2 C9 1.350(8) . ? 
C1 C2 1.377(7) . ? 
C1 C5 1.394(7) . ? 
C3 C4 1.378(7) . ? 
C4 C5 1.378(7) . ? 
C5 C6 1.493(6) . ? 
C6 C7 1.388(7) . ? 
C6 C10 1.393(7) . ? 
C7 C8 1.373(7) . ? 
C9 C10 1.365(7) . ? 
OW OW 1.777(14) 2 ? 
 
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 Ga1 O13 170.56(14) . 5_566 ? 
O1 Ga1 O12 92.21(14) . . ? 
O13 Ga1 O12 95.66(14) 5_566 . ? 
O1 Ga1 O4 93.41(13) . . ? 
O13 Ga1 O4 91.11(13) 5_566 . ? 
O12 Ga1 O4 95.00(14) . . ? 
O1 Ga1 O15 84.7(2) . . ? 
O13 Ga1 O15 87.02(15) 5_566 . ? 
O12 Ga1 O15 174.02(14) . . ? 
O4 Ga1 O15 90.29(15) . . ? 
O1 Ga1 N1 89.73(14) . . ? 
O13 Ga1 N1 85.21(14) 5_566 . ? 
O12 Ga1 N1 88.95(14) . . ? 
O4 Ga1 N1 174.85(15) . . ? 
O15 Ga1 N1 85.93(15) . . ? 
O14 Ga2 O6 113.9(2) 2 2 ? 
O14 Ga2 O7 110.57(15) 2 . ? 
O6 Ga2 O7 107.76(15) 2 . ? 
O14 Ga2 O2 111.41(15) 2 2 ? 
O6 Ga2 O2 110.7(2) 2 2 ? 
O7 Ga2 O2 101.77(14) . 2 ? 
O1 P1 O1 108.6(3) . 2 ? 
O1 P1 O2 111.9(2) . 2 ? 
O1 P1 O2 109.8(2) 2 2 ? 
O1 P1 O2 109.8(2) . . ? 
O1 P1 O2 111.9(2) 2 . ? 
O2 P1 O2 104.7(3) 2 . ? 
O4 P2 O3 108.5(2) . . ? 
O4 P2 O6 111.9(2) . . ? 
O3 P2 O6 110.7(2) . . ? 
O4 P2 O5 109.7(2) . . ? 
O3 P2 O5 110.1(2) . . ? 
O6 P2 O5 105.9(2) . . ? 
O10 P3 O8 113.5(2) . . ? 
O10 P3 O7 108.2(2) . . ? 
O8 P3 O7 108.1(2) . . ? 
O10 P3 O9 108.3(2) . . ? 
O8 P3 O9 110.2(2) . . ? 
O7 P3 O9 108.3(2) . . ? 
O12 P4 O13 115.6(2) . . ? 
O12 P4 O14 112.2(2) . . ? 
O13 P4 O14 107.2(2) . . ? 
O12 P4 O11 106.4(2) . . ? 
O13 P4 O11 108.6(2) . . ? 
O14 P4 O11 106.4(2) . . ? 
P1 O1 Ga1 158.5(2) . . ? 
P1 O2 Ga2 126.2(2) . 2 ? 
P2 O4 Ga1 145.0(2) . . ? 
P2 O6 Ga2 131.3(2) . 2 ? 
P3 O7 Ga2 132.4(2) . . ? 
P4 O12 Ga1 137.3(2) . . ? 
P4 O13 Ga1 140.2(2) . 5_566 ? 
P4 O14 Ga2 141.7(2) . 2 ? 
C3 N1 C2 117.1(4) . . ? 
C3 N1 Ga1 118.7(3) . . ? 
C2 N1 Ga1 124.2(3) . . ? 
C8 N2 C9 121.8(5) . . ? 
C2 C1 C5 119.7(5) . . ? 
N1 C2 C1 123.1(5) . . ? 
N1 C3 C4 123.3(5) . . ? 
C3 C4 C5 120.1(5) . . ? 
C4 C5 C1 116.6(5) . . ? 
C4 C5 C6 121.3(5) . . ? 
C1 C5 C6 122.0(4) . . ? 
C7 C6 C10 118.3(5) . . ? 
C7 C6 C5 121.3(5) . . ? 
C10 C6 C5 120.3(4) . . ? 
C8 C7 C6 120.2(5) . . ? 
N2 C8 C7 119.8(5) . . ? 
N2 C9 C10 120.2(6) . . ? 
C9 C10 C6 119.6(5) . . ? 
 
_refine_diff_density_max    0.686 
_refine_diff_density_min   -0.591 
_refine_diff_density_rms    0.141 
#===END