 
data_phosphovanadylite-Ca 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H40 Al0.67 Ca O28 P2 V3.33' 
_chemical_formula_weight          778.13 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'V'  'V'   0.3005   0.5294 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Al'  'Al'   0.0645   0.0514 
 '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' 
 'Ca'  'Ca'   0.2262   0.3064 
 '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' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            ? 
_symmetry_space_group_name_H-M    I-43m 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 'y, z, x' 
 'z, x, y' 
 'y, -x, -z' 
 'z, -y, -x' 
 'x, -z, -y' 
 '-x, -y, z' 
 '-z, x, -y' 
 '-x, y, -z' 
 '-y, -z, x' 
 '-z, -x, y' 
 '-y, x, -z' 
 '-z, y, -x' 
 '-x, z, -y' 
 '-y, z, -x' 
 'z, y, x' 
 'x, z, y' 
 'y, x, z' 
 'y, -z, -x' 
 '-y, -x, z' 
 '-z, -y, x' 
 '-x, -z, y' 
 'x, -y, -z' 
 'z, -x, -y' 
 'x+1/2, y+1/2, z+1/2' 
 'y+1/2, z+1/2, x+1/2' 
 'z+1/2, x+1/2, y+1/2' 
 'y+1/2, -x+1/2, -z+1/2' 
 'z+1/2, -y+1/2, -x+1/2' 
 'x+1/2, -z+1/2, -y+1/2' 
 '-x+1/2, -y+1/2, z+1/2' 
 '-z+1/2, x+1/2, -y+1/2' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-y+1/2, -z+1/2, x+1/2' 
 '-z+1/2, -x+1/2, y+1/2' 
 '-y+1/2, x+1/2, -z+1/2' 
 '-z+1/2, y+1/2, -x+1/2' 
 '-x+1/2, z+1/2, -y+1/2' 
 '-y+1/2, z+1/2, -x+1/2' 
 'z+1/2, y+1/2, x+1/2' 
 'x+1/2, z+1/2, y+1/2' 
 'y+1/2, x+1/2, z+1/2' 
 'y+1/2, -z+1/2, -x+1/2' 
 '-y+1/2, -x+1/2, z+1/2' 
 '-z+1/2, -y+1/2, x+1/2' 
 '-x+1/2, -z+1/2, y+1/2' 
 'x+1/2, -y+1/2, -z+1/2' 
 'z+1/2, -x+1/2, -y+1/2' 
 
_cell_length_a                    15.441(11) 
_cell_length_b                    15.441(11) 
_cell_length_c                    15.441(11) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3681(5) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.07 
_exptl_crystal_size_mid           0.07 
_exptl_crystal_size_min           0.04 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.106 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2396 
_exptl_absorpt_coefficient_mu     1.716 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.8893 
_exptl_absorpt_correction_T_max   0.9345 
_exptl_absorpt_process_details    Higashi2001 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71075 
_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             1215 
_diffrn_reflns_av_R_equivalents   0.0679 
_diffrn_reflns_av_sigmaI/netI     0.0394 
_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        -8 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          3.23 
_diffrn_reflns_theta_max          15.92 
_reflns_number_total              188 
_reflns_number_gt                 171 
_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^)+(0.0240P)^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     mixed 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.05(13) 
_refine_ls_number_reflns          188 
_refine_ls_number_parameters      68 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0331 
_refine_ls_R_factor_gt            0.0272 
_refine_ls_wR_factor_ref          0.0560 
_refine_ls_wR_factor_gt           0.0534 
_refine_ls_goodness_of_fit_ref    1.174 
_refine_ls_restrained_S_all       1.174 
_refine_ls_shift/su_max           0.013 
_refine_ls_shift/su_mean          0.005 
 
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 
V V 0.42846(14) 0.42846(14) 0.0814(2) 0.0426(14) Uani 0.87 2 d SP . . 
Al Al 0.42846(14) 0.42846(14) 0.0814(2) 0.0426(14) Uani 0.13 2 d SP . . 
P P 0.2500 0.5000 0.0000 0.049(3) Uani 1 4 d S . . 
O1 O 0.4357(5) 0.3059(5) 0.0515(4) 0.042(2) Uani 1 1 d . . . 
O2 O 0.4214(5) 0.4214(5) 0.1866(7) 0.050(3) Uani 1 2 d S . . 
O3 O 0.5561(5) -0.5561(5) 0.0664(6) 0.043(3) Uani 1 2 d S . . 
Ca Ca 0.6590(12) -0.6590(12) 0.1605(19) 0.272(15) Uani 0.25 2 d SP . . 
OW1 O 0.6590(12) -0.6590(12) 0.1605(19) 0.272(15) Uani 0.61(5) 2 d SP . . 
OW2 O 0.2938(19) 0.2938(19) 0.2938(19) 0.194(17) Uani 1 6 d S . . 
OW3 O 0.3361(19) 0.452(2) 0.3361(19) 0.13(2) Uani 0.56(6) 2 d SP . . 
OW4 O 0.2451(9) 0.490(3) 0.2451(9) 0.221(14) Uani 1 2 d S . . 
OW5 O 0.345(5) 0.542(6) -0.542(6) 0.43(10) Uani 0.67(13) 2 d SP . . 
OW6 O 0.309(3) 0.691(3) -0.691(3) 0.44(15) Uani 0.54(13) 6 d SP . . 
OW7 O 0.295(11) 0.596(6) -0.596(6) 0.15(6) Uiso 0.20(9) 2 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 
V 0.0410(16) 0.0410(16) 0.046(3) -0.0005(15) -0.0005(15) 0.007(3) 
Al 0.0410(16) 0.0410(16) 0.046(3) -0.0005(15) -0.0005(15) 0.007(3) 
P 0.051(6) 0.048(4) 0.048(4) 0.000 0.000 0.000 
O1 0.035(6) 0.038(5) 0.053(6) -0.003(5) 0.016(5) -0.001(5) 
O2 0.046(5) 0.046(5) 0.059(10) -0.008(6) -0.008(6) -0.007(10) 
O3 0.044(5) 0.044(5) 0.041(8) -0.005(5) 0.005(5) 0.005(7) 
Ca 0.255(19) 0.255(19) 0.31(3) 0.128(14) -0.128(14) 0.01(2) 
OW1 0.255(19) 0.255(19) 0.31(3) 0.128(14) -0.128(14) 0.01(2) 
OW2 0.194(17) 0.194(17) 0.194(17) 0.05(2) 0.05(2) 0.05(2) 
OW3 0.11(2) 0.19(4) 0.11(2) -0.020(15) 0.06(2) -0.020(15) 
OW4 0.134(13) 0.40(4) 0.134(13) 0.009(16) 0.001(14) 0.009(16) 
OW5 0.15(5) 0.56(15) 0.56(15) 0.13(14) 0.11(5) -0.11(5) 
OW6 0.44(15) 0.44(15) 0.44(15) 0.21(7) -0.21(7) 0.21(7) 
 
_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 
V O2 1.631(11) . ? 
V O1 1.951(8) . ? 
V O1 1.951(8) 18 ? 
V O3 1.998(8) 7_655 ? 
V O3 1.998(8) 1_565 ? 
V O3 2.307(10) 4_665 ? 
P O1 1.537(7) 18 ? 
P O1 1.537(7) 34_554 ? 
P O1 1.537(7) 39 ? 
P O1 1.537(7) 4_565 ? 
O1 P 1.537(7) 35_554 ? 
O3 Al 1.998(8) 7_655 ? 
O3 V 1.998(8) 7_655 ? 
O3 Al 1.998(8) 1_545 ? 
O3 V 1.998(8) 1_545 ? 
O3 Al 2.307(10) 9_645 ? 
O3 V 2.307(10) 9_645 ? 
O3 Ca 2.676(18) . ? 
Ca OW6 2.40(3) 2 ? 
Ca OW7 2.50(18) 2 ? 
Ca OW4 2.99(4) 30_545 ? 
Ca OW2 3.03(4) 28_545 ? 
Ca Ca 3.94(3) 11_656 ? 
Ca Ca 3.94(3) 15_546 ? 
OW2 Ca 3.03(4) 36_445 ? 
OW2 Ca 3.03(4) 32_544 ? 
OW2 Ca 3.03(4) 30_454 ? 
OW4 Ca 2.99(4) 30_454 ? 
OW5 OW7 1.41(12) . ? 
OW5 OW5 1.8(3) 17_564 ? 
OW6 Ca 2.40(3) 7_654 ? 
OW6 Ca 2.40(3) 19_665 ? 
OW6 Ca 2.40(3) 3 ? 
OW7 Ca 2.50(18) 3 ? 
 
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 
O2 V O1 100.1(4) . . ? 
O2 V O1 100.1(4) . 18 ? 
O1 V O1 93.2(4) . 18 ? 
O2 V O3 100.9(4) . 7_655 ? 
O1 V O3 157.2(3) . 7_655 ? 
O1 V O3 91.8(4) 18 7_655 ? 
O2 V O3 100.9(4) . 1_565 ? 
O1 V O3 91.8(4) . 1_565 ? 
O1 V O3 157.2(3) 18 1_565 ? 
O3 V O3 75.6(5) 7_655 1_565 ? 
O2 V O3 177.0(5) . 4_665 ? 
O1 V O3 82.0(3) . 4_665 ? 
O1 V O3 82.0(3) 18 4_665 ? 
O3 V O3 76.7(4) 7_655 4_665 ? 
O3 V O3 76.7(4) 1_565 4_665 ? 
O1 P O1 108.4(3) 18 34_554 ? 
O1 P O1 108.4(3) 18 39 ? 
O1 P O1 111.7(5) 34_554 39 ? 
O1 P O1 111.7(5) 18 4_565 ? 
O1 P O1 108.4(3) 34_554 4_565 ? 
O1 P O1 108.4(3) 39 4_565 ? 
P O1 V 134.7(4) 35_554 . ? 
Al O3 V 0.00(12) 7_655 7_655 ? 
Al O3 Al 102.8(5) 7_655 1_545 ? 
V O3 Al 102.8(5) 7_655 1_545 ? 
Al O3 V 102.8(5) 7_655 1_545 ? 
V O3 V 102.8(5) 7_655 1_545 ? 
Al O3 V 0.00(14) 1_545 1_545 ? 
Al O3 Al 101.8(3) 7_655 9_645 ? 
V O3 Al 101.8(3) 7_655 9_645 ? 
Al O3 Al 101.8(3) 1_545 9_645 ? 
V O3 Al 101.8(3) 1_545 9_645 ? 
Al O3 V 101.8(3) 7_655 9_645 ? 
V O3 V 101.8(3) 7_655 9_645 ? 
Al O3 V 101.8(3) 1_545 9_645 ? 
V O3 V 101.8(3) 1_545 9_645 ? 
Al O3 V 0.00(11) 9_645 9_645 ? 
Al O3 Ca 116.8(5) 7_655 . ? 
V O3 Ca 116.8(5) 7_655 . ? 
Al O3 Ca 116.8(5) 1_545 . ? 
V O3 Ca 116.8(5) 1_545 . ? 
Al O3 Ca 114.5(9) 9_645 . ? 
V O3 Ca 114.5(9) 9_645 . ? 
OW6 Ca OW7 51(3) 2 2 ? 
OW6 Ca O3 140(2) 2 . ? 
OW7 Ca O3 89(3) 2 . ? 
OW6 Ca OW4 124(2) 2 30_545 ? 
OW7 Ca OW4 174(3) 2 30_545 ? 
O3 Ca OW4 96.1(8) . 30_545 ? 
OW6 Ca OW2 59(2) 2 28_545 ? 
OW7 Ca OW2 110(3) 2 28_545 ? 
O3 Ca OW2 160.6(18) . 28_545 ? 
OW4 Ca OW2 64.5(14) 30_545 28_545 ? 
OW6 Ca Ca 34.6(10) 2 11_656 ? 
OW7 Ca Ca 72(2) 2 11_656 ? 
O3 Ca Ca 143.5(4) . 11_656 ? 
OW4 Ca Ca 103.6(6) 30_545 11_656 ? 
OW2 Ca Ca 49.4(8) 28_545 11_656 ? 
OW6 Ca Ca 34.6(10) 2 15_546 ? 
OW7 Ca Ca 72(2) 2 15_546 ? 
O3 Ca Ca 143.5(4) . 15_546 ? 
OW4 Ca Ca 103.6(6) 30_545 15_546 ? 
OW2 Ca Ca 49.4(8) 28_545 15_546 ? 
Ca Ca Ca 60.001(1) 11_656 15_546 ? 
Ca OW2 Ca 81.2(16) 36_445 32_544 ? 
Ca OW2 Ca 81.2(16) 36_445 30_454 ? 
Ca OW2 Ca 81.2(16) 32_544 30_454 ? 
OW7 OW5 OW5 147(6) . 17_564 ? 
Ca OW6 Ca 111(2) 7_654 19_665 ? 
Ca OW6 Ca 111(2) 7_654 3 ? 
Ca OW6 Ca 111(2) 19_665 3 ? 
OW5 OW7 Ca 156(8) . 3 ? 
 
_diffrn_measured_fraction_theta_max    0.982 
_diffrn_reflns_theta_full              15.92 
_diffrn_measured_fraction_theta_full   0.982 
_refine_diff_density_max    0.162 
_refine_diff_density_min   -0.134 
_refine_diff_density_rms    0.041 
