 
data_2009src1292
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C4 H8 La2 O13 P2, H2 O'
_chemical_formula_sum
 'C4 H10 La2 O14 P2'
_chemical_formula_weight          621.88
 
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'
 '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'
 'La'  'La'  -0.2871   2.4523
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Triclinic
_symmetry_space_group_name_H-M    P-1
_symmetry_space_group_name_hall   '-P 1'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.0460(3)
_cell_length_b                    9.0502(3)
_cell_length_c                    9.8341(3)
_cell_angle_alpha                 108.166(2)
_cell_angle_beta                  110.482(2)
_cell_angle_gamma                 91.492(2)
_cell_volume                      708.30(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     52289
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        plate
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.08
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.916
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              580
_exptl_absorpt_coefficient_mu     6.248
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6348
_exptl_absorpt_correction_T_max   0.8852
_exptl_absorpt_process_details    'SADABS 2007/2 (Sheldrick, G.M., 2007)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature           120(2)
_diffrn_radiation_wavelength           0.71073
_diffrn_radiation_type                      MoK\a
_diffrn_radiation_source                  'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator    'graphite'
_diffrn_measurement_device_type   'Bruker-Nonius Roper CCD camera on κ-goniostat'
_diffrn_measurement_method          'φ & ω scans'
_diffrn_detector_area_resol_mean   '9.091'
_diffrn_reflns_number             16163
_diffrn_reflns_av_R_equivalents   0.0406
_diffrn_reflns_av_sigmaI/netI     0.0323
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          3.14
_diffrn_reflns_theta_max          27.48
_reflns_number_total              3241
_reflns_number_gt                 2986
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        
'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
#Although determined using DirAx, the cell is refined in the HKL
#package during data reduction
_computing_data_reduction         
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'  
_computing_structure_solution     'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0311P)²+1.9552P] where P=(Fo²+2Fc²)/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        ?
_refine_ls_number_reflns          3241
_refine_ls_number_parameters      227
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0284
_refine_ls_R_factor_gt            0.0256
_refine_ls_wR_factor_ref          0.0638
_refine_ls_wR_factor_gt           0.0620
_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
La2 La 0.36798(2) 0.36501(2) 0.07777(2) 0.00674(7) Uani 1 1 d . . .
La1 La 0.56944(2) 0.21469(2) 0.48077(2) 0.00715(7) Uani 1 1 d . . .
P1 P 0.70806(11) 0.53300(10) 0.46265(10) 0.00752(18) Uani 1 1 d . . .
P2 P 0.57649(11) 0.18935(10) 0.81079(10) 0.00778(18) Uani 1 1 d . . .
C1 C 0.8411(4) 0.5185(4) 0.3585(4) 0.0088(7) Uani 1 1 d . . .
H4A H 0.9426 0.5894 0.4284 0.010(10) Uiso 1 1 calc R . .
H4B H 0.8657 0.4097 0.3311 0.018(12) Uiso 1 1 calc R . .
O2 O 0.5458(3) 0.4327(3) 0.3524(3) 0.0091(5) Uani 1 1 d . . .
O13 O 0.9735(4) 0.9017(3) 0.6763(4) 0.0189(6) Uani 1 1 d . . .
O11 O 0.7121(4) 0.1268(3) 0.2899(3) 0.0148(6) Uani 1 1 d . . .
O1 O 0.7793(3) 0.4566(3) 0.5846(3) 0.0093(5) Uani 1 1 d . . .
O3 O 0.6925(3) 0.7051(3) 0.5271(3) 0.0106(5) Uani 1 1 d . . .
O8 O 0.6378(3) 0.4906(3) 0.1152(3) 0.0103(5) Uani 1 1 d . . .
O6 O 0.4576(3) 0.1879(3) 0.8885(3) 0.0110(5) Uani 1 1 d . . .
O4 O 0.5140(3) 0.0693(3) 0.6443(3) 0.0101(5) Uani 1 1 d . . .
O7 O 0.8588(3) 0.6519(3) 0.1867(3) 0.0147(6) Uani 1 1 d . . .
O5 O 0.6239(3) 0.3463(3) 0.7974(3) 0.0109(5) Uani 1 1 d . . .
C3 C 0.7552(4) 0.1286(4) 0.9219(4) 0.0112(7) Uani 1 1 d . . .
H1A H 0.8390 0.1399 0.8811 0.027(13) Uiso 1 1 calc R . .
H1B H 0.7939 0.2009 1.0303 0.019(12) Uiso 1 1 calc R . .
C2 C 0.7766(4) 0.5589(4) 0.2135(4) 0.0096(7) Uani 1 1 d . . .
C4 C 0.7336(4) -0.0391(4) 0.9202(4) 0.0086(7) Uani 1 1 d . . .
O10 O 0.6227(3) -0.1402(3) 0.8083(3) 0.0129(5) Uani 1 1 d . . .
O9 O 0.8243(3) -0.0773(3) 1.0292(3) 0.0167(6) Uani 1 1 d . . .
O12 O 0.8478(3) 0.1600(4) 0.6229(3) 0.0152(6) Uani 1 1 d . . .
O17 O 0.0992(3) 0.4048(3) 0.1115(3) 0.0175(6) Uani 1 1 d . . .
H13A H 0.875(7) 0.844(6) 0.648(6) 0.028(14) Uiso 1 1 d . . .
H11B H 0.807(9) 0.129(8) 0.309(7) 0.047(19) Uiso 1 1 d . . .
H12A H 0.866(7) 0.065(8) 0.614(7) 0.046(18) Uiso 1 1 d . . .
H11A H 0.667(7) 0.030(7) 0.236(6) 0.030(15) Uiso 1 1 d . . .
H12B H 0.933(8) 0.227(8) 0.675(8) 0.051(19) Uiso 1 1 d . . .
H13B H 1.011(8) 0.915(8) 0.767(8) 0.049(19) Uiso 1 1 d . . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
La2 O6 2.440(3) 1_554 ?
La2 O2 2.477(2) . ?
La2 O5 2.503(2) 2_666 ?
La2 O8 2.520(3) . ?
La2 O17 2.586(3) . ?
La2 O10 2.602(3) 2_656 ?
La2 O8 2.607(3) 2_665 ?
La2 O7 2.645(3) 2_665 ?
La2 O9 2.772(3) 2_656 ?
La2 C2 3.008(3) 2_665 ?
La2 C4 3.075(3) 2_656 ?
La1 O4 2.443(2) 2_656 ?
La1 O3 2.479(3) 2_666 ?
La1 O4 2.534(2) . ?
La1 O1 2.544(3) . ?
La1 O12 2.563(3) . ?
La1 O11 2.577(3) . ?
La1 O10 2.616(3) 2_656 ?
La1 O2 2.630(2) . ?
La1 O5 2.818(2) . ?
La1 P1 3.1924(9) . ?
La1 P2 3.3030(9) . ?
P1 O3 1.519(3) . ?
P1 O1 1.527(2) . ?
P1 O2 1.535(3) . ?
P1 C1 1.817(4) . ?
P2 O6 1.523(3) . ?
P2 O5 1.531(3) . ?
P2 O4 1.546(3) . ?
P2 C3 1.815(4) . ?
C1 C2 1.504(5) . ?
C1 H4A 0.9900 . ?
C1 H4B 0.9900 . ?
O13 H13A 0.92(6) . ?
O13 H13B 0.80(7) . ?
O11 H11B 0.81(7) . ?
O11 H11A 0.87(6) . ?
O3 La1 2.479(3) 2_666 ?
O8 C2 1.277(4) . ?
O8 La2 2.607(3) 2_665 ?
O6 La2 2.440(3) 1_556 ?
O4 La1 2.443(2) 2_656 ?
O7 C2 1.255(5) . ?
O7 La2 2.645(3) 2_665 ?
O5 La2 2.503(2) 2_666 ?
C3 C4 1.520(5) . ?
C3 H1A 0.9900 . ?
C3 H1B 0.9900 . ?
C2 La2 3.008(3) 2_665 ?
C4 O9 1.253(4) . ?
C4 O10 1.268(4) . ?
C4 La2 3.075(3) 2_656 ?
O10 La2 2.602(3) 2_656 ?
O10 La1 2.616(3) 2_656 ?
O9 La2 2.772(3) 2_656 ?
O12 H12A 0.87(7) . ?
O12 H12B 0.85(7) . ?
 
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
O6 La2 O2 116.16(9) 1_554 . ?
O6 La2 O5 139.37(8) 1_554 2_666 ?
O2 La2 O5 73.82(8) . 2_666 ?
O6 La2 O8 72.22(8) 1_554 . ?
O2 La2 O8 71.41(8) . . ?
O5 La2 O8 74.93(8) 2_666 . ?
O6 La2 O17 136.51(9) 1_554 . ?
O2 La2 O17 99.23(9) . . ?
O5 La2 O17 72.35(9) 2_666 . ?
O8 La2 O17 147.28(9) . . ?
O6 La2 O10 86.34(8) 1_554 2_656 ?
O2 La2 O10 64.35(8) . 2_656 ?
O5 La2 O10 129.42(8) 2_666 2_656 ?
O8 La2 O10 114.31(8) . 2_656 ?
O17 La2 O10 87.17(9) . 2_656 ?
O6 La2 O8 74.67(8) 1_554 2_665 ?
O2 La2 O8 129.24(8) . 2_665 ?
O5 La2 O8 70.30(8) 2_666 2_665 ?
O8 La2 O8 65.46(9) . 2_665 ?
O17 La2 O8 102.67(9) . 2_665 ?
O10 La2 O8 160.21(8) 2_656 2_665 ?
O6 La2 O7 77.89(9) 1_554 2_665 ?
O2 La2 O7 165.78(9) . 2_665 ?
O5 La2 O7 94.14(8) 2_666 2_665 ?
O8 La2 O7 113.37(8) . 2_665 ?
O17 La2 O7 69.34(9) . 2_665 ?
O10 La2 O7 121.54(8) 2_656 2_665 ?
O8 La2 O7 49.57(8) 2_665 2_665 ?
O6 La2 O9 74.29(9) 1_554 2_656 ?
O2 La2 O9 111.05(8) . 2_656 ?
O5 La2 O9 142.03(9) 2_666 2_656 ?
O8 La2 O9 143.02(9) . 2_656 ?
O17 La2 O9 69.70(9) . 2_656 ?
O10 La2 O9 47.83(8) 2_656 2_656 ?
O8 La2 O9 119.40(8) 2_665 2_656 ?
O7 La2 O9 73.72(8) 2_665 2_656 ?
O6 La2 C2 73.95(9) 1_554 2_665 ?
O2 La2 C2 152.57(9) . 2_665 ?
O5 La2 C2 82.52(9) 2_666 2_665 ?
O8 La2 C2 89.38(9) . 2_665 ?
O17 La2 C2 86.32(9) . 2_665 ?
O10 La2 C2 143.05(9) 2_656 2_665 ?
O8 La2 C2 25.01(9) 2_665 2_665 ?
O7 La2 C2 24.59(9) 2_665 2_665 ?
O9 La2 C2 96.11(9) 2_656 2_665 ?
O6 La2 C4 77.19(9) 1_554 2_656 ?
O2 La2 C4 88.17(9) . 2_656 ?
O5 La2 C4 143.35(9) 2_666 2_656 ?
O8 La2 C4 129.62(9) . 2_656 ?
O17 La2 C4 79.67(9) . 2_656 ?
O10 La2 C4 24.00(9) 2_656 2_656 ?
O8 La2 C4 140.46(8) 2_665 2_656 ?
O7 La2 C4 97.69(9) 2_665 2_656 ?
O9 La2 C4 24.04(8) 2_656 2_656 ?
C2 La2 C4 119.26(9) 2_665 2_656 ?
O4 La1 O3 99.02(8) 2_656 2_666 ?
O4 La1 O4 63.98(9) 2_656 . ?
O3 La1 O4 81.19(8) 2_666 . ?
O4 La1 O1 150.35(8) 2_656 . ?
O3 La1 O1 110.13(8) 2_666 . ?
O4 La1 O1 124.65(8) . . ?
O4 La1 O12 88.24(9) 2_656 . ?
O3 La1 O12 152.04(9) 2_666 . ?
O4 La1 O12 77.85(9) . . ?
O1 La1 O12 68.59(9) . . ?
O4 La1 O11 74.33(9) 2_656 . ?
O3 La1 O11 137.11(9) 2_666 . ?
O4 La1 O11 127.93(9) . . ?
O1 La1 O11 80.52(9) . . ?
O12 La1 O11 70.84(9) . . ?
O4 La1 O10 68.15(8) 2_656 2_656 ?
O3 La1 O10 71.44(9) 2_666 2_656 ?
O4 La1 O10 119.17(8) . 2_656 ?
O1 La1 O10 115.66(8) . 2_656 ?
O12 La1 O10 135.53(9) . 2_656 ?
O11 La1 O10 66.78(9) . 2_656 ?
O4 La1 O2 128.64(8) 2_656 . ?
O3 La1 O2 77.21(8) 2_666 . ?
O4 La1 O2 156.45(8) . . ?
O1 La1 O2 56.56(8) . . ?
O12 La1 O2 118.81(9) . . ?
O11 La1 O2 75.25(9) . . ?
O10 La1 O2 62.12(8) 2_656 . ?
O4 La1 O5 117.90(8) 2_656 . ?
O3 La1 O5 78.11(8) 2_666 . ?
O4 La1 O5 54.20(8) . . ?
O1 La1 O5 74.76(7) . . ?
O12 La1 O5 74.67(8) . . ?
O11 La1 O5 143.00(9) . . ?
O10 La1 O5 149.55(8) 2_656 . ?
O2 La1 O5 111.38(7) . . ?
O4 La1 P1 146.95(6) 2_656 . ?
O3 La1 P1 95.20(6) 2_666 . ?
O4 La1 P1 148.27(6) . . ?
O1 La1 P1 28.07(6) . . ?
O12 La1 P1 93.00(7) . . ?
O11 La1 P1 74.94(7) . . ?
O10 La1 P1 88.69(6) 2_656 . ?
O2 La1 P1 28.55(6) . . ?
O5 La1 P1 94.13(5) . . ?
O4 La1 P2 90.38(6) 2_656 . ?
O3 La1 P2 80.37(6) 2_666 . ?
O4 La1 P2 26.81(6) . . ?
O1 La1 P2 99.46(6) . . ?
O12 La1 P2 72.57(7) . . ?
O11 La1 P2 140.54(7) . . ?
O10 La1 P2 140.57(6) 2_656 . ?
O2 La1 P2 137.29(6) . . ?
O5 La1 P2 27.53(5) . . ?
P1 La1 P2 121.46(2) . . ?
O4 La1 La1 32.64(6) 2_656 2_656 ?
O3 La1 La1 89.93(6) 2_666 2_656 ?
O4 La1 La1 31.34(6) . 2_656 ?
O1 La1 La1 147.59(5) . 2_656 ?
O12 La1 La1 81.71(7) . 2_656 ?
O11 La1 La1 102.28(7) . 2_656 ?
O10 La1 La1 94.43(6) 2_656 2_656 ?
O2 La1 La1 155.74(6) . 2_656 ?
O5 La1 La1 85.39(5) . 2_656 ?
P1 La1 La1 174.638(19) . 2_656 ?
P2 La1 La1 57.869(16) . 2_656 ?
O3 P1 O1 114.64(14) . . ?
O3 P1 O2 111.66(15) . . ?
O1 P1 O2 106.43(14) . . ?
O3 P1 C1 108.30(16) . . ?
O1 P1 C1 106.39(15) . . ?
O2 P1 C1 109.20(16) . . ?
O3 P1 La1 134.34(11) . . ?
O1 P1 La1 51.64(10) . . ?
O2 P1 La1 54.93(10) . . ?
C1 P1 La1 117.34(12) . . ?
O6 P2 O5 116.58(15) . . ?
O6 P2 O4 111.74(15) . . ?
O5 P2 O4 105.61(14) . . ?
O6 P2 C3 106.76(16) . . ?
O5 P2 C3 108.48(16) . . ?
O4 P2 C3 107.31(16) . . ?
O6 P2 La1 136.99(11) . . ?
O5 P2 La1 58.31(10) . . ?
O4 P2 La1 47.65(9) . . ?
C3 P2 La1 115.27(13) . . ?
C2 C1 P1 114.8(3) . . ?
C2 C1 H4A 108.6 . . ?
P1 C1 H4A 108.6 . . ?
C2 C1 H4B 108.6 . . ?
P1 C1 H4B 108.6 . . ?
H4A C1 H4B 107.5 . . ?
P1 O2 La2 137.75(14) . . ?
P1 O2 La1 96.52(12) . . ?
La2 O2 La1 118.74(10) . . ?
H13A O13 H13B 101(6) . . ?
La1 O11 H11B 128(5) . . ?
La1 O11 H11A 103(4) . . ?
H11B O11 H11A 107(6) . . ?
P1 O1 La1 100.29(12) . . ?
P1 O3 La1 120.84(14) . 2_666 ?
C2 O8 La2 145.3(2) . . ?
C2 O8 La2 95.3(2) . 2_665 ?
La2 O8 La2 114.54(9) . 2_665 ?
P2 O6 La2 140.31(15) . 1_556 ?
P2 O4 La1 137.15(14) . 2_656 ?
P2 O4 La1 105.55(12) . . ?
La1 O4 La1 116.02(9) 2_656 . ?
C2 O7 La2 94.1(2) . 2_665 ?
P2 O5 La2 139.92(14) . 2_666 ?
P2 O5 La1 94.16(11) . . ?
La2 O5 La1 121.16(9) 2_666 . ?
C4 C3 P2 114.9(3) . . ?
C4 C3 H1A 108.5 . . ?
P2 C3 H1A 108.5 . . ?
C4 C3 H1B 108.5 . . ?
P2 C3 H1B 108.5 . . ?
H1A C3 H1B 107.5 . . ?
O7 C2 O8 120.8(3) . . ?
O7 C2 C1 121.2(3) . . ?
O8 C2 C1 117.9(3) . . ?
O7 C2 La2 61.30(19) . 2_665 ?
O8 C2 La2 59.65(18) . 2_665 ?
C1 C2 La2 177.3(3) . 2_665 ?
O9 C4 O10 120.1(3) . . ?
O9 C4 C3 120.3(3) . . ?
O10 C4 C3 119.6(3) . . ?
O9 C4 La2 64.34(19) . 2_656 ?
O10 C4 La2 56.60(18) . 2_656 ?
C3 C4 La2 169.6(3) . 2_656 ?
C4 O10 La2 99.4(2) . 2_656 ?
C4 O10 La1 145.2(2) . 2_656 ?
La2 O10 La1 114.78(10) 2_656 2_656 ?
C4 O9 La2 91.6(2) . 2_656 ?
La1 O12 H12A 121(4) . . ?
La1 O12 H12B 127(4) . . ?
H12A O12 H12B 112(6) . . ?
 
_diffrn_measured_fraction_theta_max    0.998
_diffrn_reflns_theta_full              27.48
_diffrn_measured_fraction_theta_full   0.998
_refine_diff_density_max    1.240
_refine_diff_density_min   -1.535
_refine_diff_density_rms    0.191
