 
data_cav_350
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'H1.50 Ca0.50 O5 Si2 V0.50'
_chemical_formula_weight          183.20
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 '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'
 'Si'  'Si'   0.0817   0.0704
 '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'
 'V'  'V'   0.3005   0.5294
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            ?
_symmetry_space_group_name_H-M    ?
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x, y+1/2, -z'
 '-x+1/2, -y, z+1/2'
 '-x, -y, -z'
 '-x-1/2, y-1/2, z-1/2'
 'x, -y-1/2, z'
 'x-1/2, y, -z-1/2'
 
_cell_length_a                    9.39(5)
_cell_length_b                    13.11(8)
_cell_length_c                    9.39(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1156(11)
_cell_formula_units_Z             8
_cell_measurement_temperature     296(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.105
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              728
_exptl_absorpt_coefficient_mu     1.749
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       296(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             4845
_diffrn_reflns_av_R_equivalents   0.0531
_diffrn_reflns_av_sigmaI/netI     0.0382
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_theta_min          2.67
_diffrn_reflns_theta_max          23.85
_reflns_number_total              916
_reflns_number_gt                 731
_reflns_threshold_expression      >2\s(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_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^ > 2\s(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^)+(0.1015P)^2^+5.6836P] 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_number_reflns          916
_refine_ls_number_parameters      95
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0783
_refine_ls_R_factor_gt            0.0593
_refine_ls_wR_factor_ref          0.1833
_refine_ls_wR_factor_gt           0.1683
_refine_ls_goodness_of_fit_ref    1.149
_refine_ls_restrained_S_all       1.149
_refine_ls_shift/su_max           0.000
_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
V V 0.0374(2) 0.2500 0.0993(2) 0.0323(6) Uani 1 2 d S . .
Ca Ca -0.3884(3) 0.7500 -0.0715(3) 0.0373(8) Uani 1 2 d S . .
Si1 Si -0.1968(2) 0.52399(16) -0.0781(2) 0.0256(6) Uani 1 1 d . . .
Si2 Si -0.0833(2) 0.46265(16) 0.2073(2) 0.0243(6) Uani 1 1 d . . .
O1 O -0.1921(6) 0.6461(4) -0.0706(7) 0.0373(15) Uani 1 1 d . . .
O2 O -0.0485(6) 0.3461(4) 0.2374(6) 0.0378(15) Uani 1 1 d . . .
O3 O -0.1946(6) 0.4739(5) 0.0777(6) 0.0366(15) Uani 1 1 d . . .
O4 O -0.0631(5) 0.4784(4) -0.1666(6) 0.0309(14) Uani 1 1 d . . .
O5 O -0.3434(6) 0.4873(4) -0.1524(6) 0.0310(14) Uani 1 1 d . . .
O6 O -0.0568(12) 0.2500 -0.0373(12) 0.061(3) Uani 1 2 d S . .
O7 O -0.517(6) 0.780(4) 0.134(6) 0.129(18) Uiso 0.25(3) 1 d P . .
O7B O -0.415(7) 0.782(4) 0.181(6) 0.129(18) Uiso 0.22(3) 1 d P . .
O8 O -0.590(9) 0.7500 0.018(10) 0.129(18) Uiso 0.24(4) 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 0.0308(12) 0.0317(11) 0.0343(13) 0.000 0.0063(10) 0.000
Ca 0.0358(14) 0.0357(14) 0.0405(17) 0.000 -0.0030(12) 0.000
Si1 0.0211(12) 0.0300(12) 0.0255(14) 0.0024(9) -0.0021(9) 0.0000(8)
Si2 0.0241(11) 0.0293(11) 0.0195(13) 0.0015(9) 0.0041(9) 0.0008(9)
O1 0.030(3) 0.033(3) 0.049(4) 0.001(3) 0.002(3) 0.000(2)
O2 0.048(4) 0.032(3) 0.033(4) 0.004(3) 0.016(3) 0.006(3)
O3 0.034(3) 0.054(4) 0.022(3) 0.007(3) -0.003(3) -0.002(3)
O4 0.023(3) 0.035(3) 0.035(3) 0.003(2) 0.003(3) 0.000(2)
O5 0.031(3) 0.038(3) 0.024(3) 0.008(2) -0.004(3) -0.001(2)
O6 0.067(7) 0.068(7) 0.048(7) 0.000 -0.010(6) 0.000
 
_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
V O6 1.559(13) . ?
V O2 1.980(9) . ?
V O2 1.980(9) 7_565 ?
V O1 2.009(10) 5_565 ?
V O1 2.009(10) 3_545 ?
V Ca 3.306(19) 5_565 ?
V Ca 3.394(17) 6_556 ?
Ca O8 2.07(8) . ?
Ca O2 2.271(11) 4_464 ?
Ca O2 2.271(11) 6_565 ?
Ca O1 2.292(11) 7_575 ?
Ca O1 2.292(11) . ?
Ca O7 2.31(5) . ?
Ca O7 2.31(5) 7_575 ?
Ca O7B 2.42(6) . ?
Ca O7B 2.42(6) 7_575 ?
Ca V 3.306(19) 5_565 ?
Ca V 3.394(17) 6_565 ?
Ca Si1 3.467(16) 7_575 ?
Si1 O1 1.603(11) . ?
Si1 O3 1.603(10) . ?
Si1 O5 1.617(9) . ?
Si1 O4 1.620(8) . ?
Si2 O2 1.588(10) . ?
Si2 O3 1.612(9) . ?
Si2 O4 1.623(9) 5_565 ?
Si2 O5 1.625(9) 4_465 ?
Si2 Ca 3.486(15) 6_556 ?
O1 V 2.009(10) 5_565 ?
O2 Ca 2.271(11) 6_556 ?
O4 Si2 1.623(9) 5_565 ?
O5 Si2 1.625(9) 4_464 ?
O7 O7 0.79(10) 7_575 ?
O7 O7B 1.05(6) . ?
O7 O7B 1.33(6) 7_575 ?
O7 O8 1.34(9) . ?
O7B O7B 0.83(11) 7_575 ?
O7B O7 1.33(6) 7_575 ?
O8 O7 1.34(9) 7_575 ?
 
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 V O2 108.0(5) . . ?
O6 V O2 108.0(5) . 7_565 ?
O2 V O2 79.0(5) . 7_565 ?
O6 V O1 107.4(4) . 5_565 ?
O2 V O1 87.2(4) . 5_565 ?
O2 V O1 144.5(3) 7_565 5_565 ?
O6 V O1 107.4(4) . 3_545 ?
O2 V O1 144.5(3) . 3_545 ?
O2 V O1 87.2(4) 7_565 3_545 ?
O1 V O1 85.3(6) 5_565 3_545 ?
O6 V Ca 120.0(5) . 5_565 ?
O2 V Ca 117.3(2) . 5_565 ?
O2 V Ca 117.3(2) 7_565 5_565 ?
O1 V Ca 43.0(3) 5_565 5_565 ?
O1 V Ca 43.0(3) 3_545 5_565 ?
O6 V Ca 121.1(6) . 6_556 ?
O2 V Ca 40.1(3) . 6_556 ?
O2 V Ca 40.1(3) 7_565 6_556 ?
O1 V Ca 114.9(2) 5_565 6_556 ?
O1 V Ca 114.9(2) 3_545 6_556 ?
Ca V Ca 118.88(16) 5_565 6_556 ?
O8 Ca O2 95(2) . 4_464 ?
O8 Ca O2 95(2) . 6_565 ?
O2 Ca O2 67.4(5) 4_464 6_565 ?
O8 Ca O1 137.1(13) . 7_575 ?
O2 Ca O1 122.9(3) 4_464 7_575 ?
O2 Ca O1 83.3(3) 6_565 7_575 ?
O8 Ca O1 137.1(13) . . ?
O2 Ca O1 83.3(3) 4_464 . ?
O2 Ca O1 122.9(3) 6_565 . ?
O1 Ca O1 72.9(5) 7_575 . ?
O8 Ca O7 35(2) . . ?
O2 Ca O7 128.2(16) 4_464 . ?
O2 Ca O7 115.4(15) 6_565 . ?
O1 Ca O7 108.4(15) 7_575 . ?
O1 Ca O7 121.2(15) . . ?
O8 Ca O7 35(2) . 7_575 ?
O2 Ca O7 115.4(15) 4_464 7_575 ?
O2 Ca O7 128.2(16) 6_565 7_575 ?
O1 Ca O7 121.2(15) 7_575 7_575 ?
O1 Ca O7 108.4(15) . 7_575 ?
O7 Ca O7 20(3) . 7_575 ?
O8 Ca O7B 60(3) . . ?
O2 Ca O7B 147.4(15) 4_464 . ?
O2 Ca O7B 130.7(15) 6_565 . ?
O1 Ca O7B 88.7(15) 7_575 . ?
O1 Ca O7B 100.4(15) . . ?
O7 Ca O7B 25.6(15) . . ?
O7 Ca O7B 32.6(16) 7_575 . ?
O8 Ca O7B 60(3) . 7_575 ?
O2 Ca O7B 130.7(14) 4_464 7_575 ?
O2 Ca O7B 147.4(15) 6_565 7_575 ?
O1 Ca O7B 100.4(15) 7_575 7_575 ?
O1 Ca O7B 88.7(15) . 7_575 ?
O7 Ca O7B 32.6(16) . 7_575 ?
O7 Ca O7B 25.6(15) 7_575 7_575 ?
O7B Ca O7B 20(3) . 7_575 ?
O8 Ca V 160(3) . 5_565 ?
O2 Ca V 101.4(2) 4_464 5_565 ?
O2 Ca V 101.4(2) 6_565 5_565 ?
O1 Ca V 36.7(3) 7_575 5_565 ?
O1 Ca V 36.7(3) . 5_565 ?
O7 Ca V 125.9(17) . 5_565 ?
O7 Ca V 125.9(17) 7_575 5_565 ?
O7B Ca V 100.4(16) . 5_565 ?
O7B Ca V 100.4(16) 7_575 5_565 ?
O8 Ca V 90(3) . 6_565 ?
O2 Ca V 34.2(2) 4_464 6_565 ?
O2 Ca V 34.2(2) 6_565 6_565 ?
O1 Ca V 109.6(2) 7_575 6_565 ?
O1 Ca V 109.6(2) . 6_565 ?
O7 Ca V 123.1(17) . 6_565 ?
O7 Ca V 123.1(17) 7_575 6_565 ?
O7B Ca V 148.2(16) . 6_565 ?
O7B Ca V 148.2(16) 7_575 6_565 ?
V Ca V 109.8(2) 5_565 6_565 ?
O8 Ca Si1 118.8(6) . 7_575 ?
O2 Ca Si1 126.5(3) 4_464 7_575 ?
O2 Ca Si1 69.4(3) 6_565 7_575 ?
O1 Ca Si1 22.31(14) 7_575 7_575 ?
O1 Ca Si1 95.2(5) . 7_575 ?
O7 Ca Si1 98.0(14) . 7_575 ?
O7 Ca Si1 115.6(13) 7_575 7_575 ?
O7B Ca Si1 85.6(14) . 7_575 ?
O7B Ca Si1 102.6(14) 7_575 7_575 ?
V Ca Si1 58.7(2) 5_565 7_575 ?
V Ca Si1 101.42(15) 6_565 7_575 ?
O1 Si1 O3 111.6(4) . . ?
O1 Si1 O5 109.8(3) . . ?
O3 Si1 O5 106.5(4) . . ?
O1 Si1 O4 111.7(3) . . ?
O3 Si1 O4 107.9(4) . . ?
O5 Si1 O4 109.2(5) . . ?
O1 Si1 Ca 32.9(3) . . ?
O3 Si1 Ca 109.9(3) . . ?
O5 Si1 Ca 79.6(4) . . ?
O4 Si1 Ca 136.6(2) . . ?
O2 Si2 O3 110.9(3) . . ?
O2 Si2 O4 109.0(4) . 5_565 ?
O3 Si2 O4 109.1(4) . 5_565 ?
O2 Si2 O5 109.3(4) . 4_465 ?
O3 Si2 O5 107.5(5) . 4_465 ?
O4 Si2 O5 111.0(4) 5_565 4_465 ?
O2 Si2 Ca 30.7(3) . 6_556 ?
O3 Si2 Ca 118.3(3) . 6_556 ?
O4 Si2 Ca 125.9(3) 5_565 6_556 ?
O5 Si2 Ca 78.9(4) 4_465 6_556 ?
Si1 O1 V 133.7(4) . 5_565 ?
Si1 O1 Ca 124.8(4) . . ?
V O1 Ca 100.3(5) 5_565 . ?
Si2 O2 V 125.4(4) . . ?
Si2 O2 Ca 128.4(3) . 6_556 ?
V O2 Ca 105.7(5) . 6_556 ?
Si1 O3 Si2 137.3(4) . . ?
Si1 O4 Si2 127.0(5) . 5_565 ?
Si1 O5 Si2 126.2(4) . 4_464 ?
O7 O7 O7B 91(5) 7_575 . ?
O7 O7 O7B 52(3) 7_575 7_575 ?
O7B O7 O7B 39(6) . 7_575 ?
O7 O7 O8 73(2) 7_575 . ?
O7B O7 O8 144(7) . . ?
O7B O7 O8 117(5) 7_575 . ?
O7 O7 Ca 80.1(13) 7_575 . ?
O7B O7 Ca 83(4) . . ?
O7B O7 Ca 78(4) 7_575 . ?
O8 O7 Ca 63(4) . . ?
O7B O7B O7 89(5) 7_575 . ?
O7B O7B O7 52(3) 7_575 7_575 ?
O7 O7B O7 37(5) . 7_575 ?
O7B O7B Ca 80.1(14) 7_575 . ?
O7 O7B Ca 71(4) . . ?
O7 O7B Ca 69(3) 7_575 . ?
O7 O8 O7 34(5) 7_575 . ?
O7 O8 Ca 82(5) 7_575 . ?
O7 O8 Ca 82(5) . . ?
 
_diffrn_measured_fraction_theta_max    0.976
_diffrn_reflns_theta_full              23.85
_diffrn_measured_fraction_theta_full   0.976
_refine_diff_density_max    0.790
_refine_diff_density_min   -0.779
_refine_diff_density_rms    0.155
