 
data_cav_175
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'H3 Ca0.50 O5 Si2 V0.50'
_chemical_formula_weight          184.71
 
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                    9.4746(4)
_cell_length_b                    13.2620(5)
_cell_length_c                    9.6050(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1206.89(8)
_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     2.033
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              740
_exptl_absorpt_coefficient_mu     1.677
_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             7406
_diffrn_reflns_av_R_equivalents   0.0328
_diffrn_reflns_av_sigmaI/netI     0.0292
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        13
_diffrn_reflns_limit_k_min        -18
_diffrn_reflns_limit_k_max        18
_diffrn_reflns_limit_l_min        -7
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          2.62
_diffrn_reflns_theta_max          30.50
_reflns_number_total              1900
_reflns_number_gt                 1644
_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^)+(0.0516P)^2^+1.5350P] 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          1900
_refine_ls_number_parameters      102
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0361
_refine_ls_R_factor_gt            0.0287
_refine_ls_wR_factor_ref          0.0880
_refine_ls_wR_factor_gt           0.0821
_refine_ls_goodness_of_fit_ref    0.964
_refine_ls_restrained_S_all       0.964
_refine_ls_shift/su_max           0.356
_refine_ls_shift/su_mean          0.018
 
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 0.03479(5) 0.2500 0.09988(5) 0.01642(12) Uani 1 2 d S . .
Ca Ca -0.38889(6) 0.7500 -0.07578(6) 0.01849(14) Uani 1 2 d S . .
Si1 Si -0.19261(6) 0.52653(4) -0.08317(6) 0.01415(13) Uani 1 1 d . . .
Si2 Si -0.09206(6) 0.46155(4) 0.19910(5) 0.01366(13) Uani 1 1 d . . .
O1 O -0.18823(15) 0.64770(11) -0.07596(16) 0.0199(3) Uani 1 1 d . . .
O2 O -0.05978(17) 0.34527(11) 0.22691(16) 0.0218(3) Uani 1 1 d . . .
O3 O -0.20100(16) 0.47554(13) 0.07010(16) 0.0226(3) Uani 1 1 d . . .
O4 O -0.05458(16) 0.48034(11) -0.16282(16) 0.0196(3) Uani 1 1 d . . .
O5 O -0.33434(16) 0.48941(11) -0.16389(15) 0.0189(3) Uani 1 1 d . . .
O6 O -0.0552(3) 0.2500 -0.0398(3) 0.0337(6) Uani 1 2 d S . .
O7 O -0.430(2) 0.7778(16) 0.1679(16) 0.044(3) Uiso 0.162(12) 1 d P . .
O7A O -0.3625(16) 0.7750(11) 0.1759(12) 0.044(3) Uiso 0.203(10) 1 d P . .
O7B O -0.397(3) 0.810(2) 0.161(2) 0.044(3) Uiso 0.142(14) 1 d P . .
O8 O -0.6409(5) 0.7500 -0.0485(8) 0.121(2) Uani 1 2 d S . .
 
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 0.0140(2) 0.0168(2) 0.0185(2) 0.000 0.00103(17) 0.000
Ca 0.0163(3) 0.0197(3) 0.0194(3) 0.000 -0.0001(2) 0.000
Si1 0.0108(2) 0.0170(3) 0.0146(3) 0.00178(17) -0.00055(18) 0.00016(17)
Si2 0.0124(2) 0.0155(2) 0.0131(2) 0.00137(17) 0.00162(17) 0.00114(18)
O1 0.0153(6) 0.0172(7) 0.0272(8) -0.0011(6) 0.0017(5) -0.0002(5)
O2 0.0248(7) 0.0168(7) 0.0237(7) 0.0027(5) 0.0087(6) 0.0043(6)
O3 0.0180(7) 0.0328(9) 0.0169(7) 0.0063(6) -0.0025(5) -0.0008(6)
O4 0.0144(7) 0.0194(7) 0.0250(7) 0.0001(5) 0.0050(6) -0.0003(5)
O5 0.0158(7) 0.0220(7) 0.0190(7) 0.0037(5) -0.0051(5) -0.0018(5)
O6 0.0326(13) 0.0404(14) 0.0282(13) 0.000 -0.0086(11) 0.000
O8 0.035(2) 0.172(6) 0.157(6) 0.000 0.029(3) 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 1.590(3) . ?
V O2 1.9718(15) 7_565 ?
V O2 1.9718(15) . ?
V O1 2.0017(15) 5_565 ?
V O1 2.0017(15) 3_545 ?
V Ca 3.3629(8) 5_565 ?
V Ca 3.4082(8) 6_556 ?
Ca O7B 2.415(19) . ?
Ca O7B 2.415(19) 7_575 ?
Ca O2 2.3291(16) 4_464 ?
Ca O2 2.3291(16) 6_565 ?
Ca O1 2.3356(15) 7_575 ?
Ca O1 2.3356(15) . ?
Ca O7 2.402(15) . ?
Ca O7 2.402(15) 7_575 ?
Ca O8 2.402(5) . ?
Ca O7A 2.453(11) . ?
Ca O7A 2.453(11) 7_575 ?
Ca V 3.3629(8) 5_565 ?
Si1 O1 1.6090(16) . ?
Si1 O3 1.6220(16) . ?
Si1 O5 1.6269(15) . ?
Si1 O4 1.6343(15) . ?
Si2 O2 1.5947(16) . ?
Si2 O3 1.6233(16) . ?
Si2 O5 1.6251(15) 4_465 ?
Si2 O4 1.6265(16) 5_565 ?
Si2 Ca 3.5468(6) 6_556 ?
O1 V 2.0017(15) 5_565 ?
O2 Ca 2.3291(16) 6_556 ?
O4 Si2 1.6265(15) 5_565 ?
O5 Si2 1.6251(15) 4_464 ?
O7 O7A 0.65(2) . ?
O7 O7B 0.53(2) . ?
O7 O7 0.74(4) 7_575 ?
O7 O7A 0.954(17) 7_575 ?
O7 O7B 1.21(4) 7_575 ?
O7A O7A 0.66(3) 7_575 ?
O7A O7 0.954(17) 7_575 ?
O7A O7B 0.58(2) . ?
O7A O7B 1.18(4) 7_575 ?
O7B O7 1.21(4) 7_575 ?
O7B O7A 1.18(4) 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 106.17(9) . 7_565 ?
O6 V O2 106.17(9) . . ?
O2 V O2 79.70(9) 7_565 . ?
O6 V O1 107.02(9) . 5_565 ?
O2 V O1 146.65(7) 7_565 5_565 ?
O2 V O1 88.10(6) . 5_565 ?
O6 V O1 107.02(9) . 3_545 ?
O2 V O1 88.10(6) 7_565 3_545 ?
O2 V O1 146.65(7) . 3_545 ?
O1 V O1 85.34(9) 5_565 3_545 ?
O6 V Ca 118.49(10) . 5_565 ?
O2 V Ca 119.73(5) 7_565 5_565 ?
O2 V Ca 119.73(5) . 5_565 ?
O1 V Ca 42.91(4) 5_565 5_565 ?
O1 V Ca 42.91(4) 3_545 5_565 ?
O6 V Ca 123.63(11) . 6_556 ?
O2 V Ca 41.42(4) 7_565 6_556 ?
O2 V Ca 41.42(4) . 6_556 ?
O1 V Ca 113.55(5) 5_565 6_556 ?
O1 V Ca 113.55(5) 3_545 6_556 ?
Ca V Ca 117.876(18) 5_565 6_556 ?
O7B Ca O7B 38.4(15) . 7_575 ?
O7B Ca O2 160.0(7) . 4_464 ?
O7B Ca O2 125.6(7) 7_575 4_464 ?
O7B Ca O2 125.6(7) . 6_565 ?
O7B Ca O2 160.0(7) 7_575 6_565 ?
O2 Ca O2 65.71(8) 4_464 6_565 ?
O7B Ca O1 80.6(7) . 7_575 ?
O7B Ca O1 102.6(6) 7_575 7_575 ?
O2 Ca O1 118.98(6) 4_464 7_575 ?
O2 Ca O1 81.62(5) 6_565 7_575 ?
O7B Ca O1 102.6(6) . . ?
O7B Ca O1 80.6(7) 7_575 . ?
O2 Ca O1 81.62(5) 4_464 . ?
O2 Ca O1 118.98(6) 6_565 . ?
O1 Ca O1 71.02(7) 7_575 . ?
O7B Ca O7 12.7(5) . . ?
O7B Ca O7 29.0(11) 7_575 . ?
O2 Ca O7 147.3(6) 4_464 . ?
O2 Ca O7 132.5(4) 6_565 . ?
O1 Ca O7 92.6(6) 7_575 . ?
O1 Ca O7 102.9(4) . . ?
O7B Ca O7 29.0(11) . 7_575 ?
O7B Ca O7 12.7(5) 7_575 7_575 ?
O2 Ca O7 132.5(4) 4_464 7_575 ?
O2 Ca O7 147.3(6) 6_565 7_575 ?
O1 Ca O7 102.9(4) 7_575 7_575 ?
O1 Ca O7 92.6(6) . 7_575 ?
O7 Ca O7 17.7(10) . 7_575 ?
O7B Ca O8 82.2(6) . . ?
O7B Ca O8 82.2(6) 7_575 . ?
O2 Ca O8 83.17(16) 4_464 . ?
O2 Ca O8 83.17(16) 6_565 . ?
O1 Ca O8 144.02(5) 7_575 . ?
O1 Ca O8 144.02(5) . . ?
O7 Ca O8 74.4(5) . . ?
O7 Ca O8 74.4(5) 7_575 . ?
O7B Ca O7A 13.8(5) . . ?
O7B Ca O7A 28.1(9) 7_575 . ?
O2 Ca O7A 153.7(3) 4_464 . ?
O2 Ca O7A 138.6(4) 6_565 . ?
O1 Ca O7A 80.8(3) 7_575 . ?
O1 Ca O7A 89.8(4) . . ?
O7 Ca O7A 15.3(5) . . ?
O7 Ca O7A 22.6(4) 7_575 . ?
O8 Ca O7A 89.7(4) . . ?
O7B Ca O7A 28.1(9) . 7_575 ?
O7B Ca O7A 13.8(5) 7_575 7_575 ?
O2 Ca O7A 138.6(4) 4_464 7_575 ?
O2 Ca O7A 153.7(3) 6_565 7_575 ?
O1 Ca O7A 89.8(4) 7_575 7_575 ?
O1 Ca O7A 80.8(3) . 7_575 ?
O7 Ca O7A 22.6(4) . 7_575 ?
O7 Ca O7A 15.3(5) 7_575 7_575 ?
O8 Ca O7A 89.7(4) . 7_575 ?
O7A Ca O7A 15.5(7) . 7_575 ?
O7B Ca V 95.6(6) . 5_565 ?
O7B Ca V 95.6(6) 7_575 5_565 ?
O2 Ca V 98.76(4) 4_464 5_565 ?
O2 Ca V 98.76(4) 6_565 5_565 ?
O1 Ca V 35.70(4) 7_575 5_565 ?
O1 Ca V 35.70(4) . 5_565 ?
O7 Ca V 103.3(5) . 5_565 ?
O7 Ca V 103.3(5) 7_575 5_565 ?
O8 Ca V 177.69(18) . 5_565 ?
O7A Ca V 88.1(3) . 5_565 ?
O7A Ca V 88.1(3) 7_575 5_565 ?
O1 Si1 O3 112.25(9) . . ?
O1 Si1 O5 110.12(8) . . ?
O3 Si1 O5 105.42(8) . . ?
O1 Si1 O4 111.96(8) . . ?
O3 Si1 O4 107.93(8) . . ?
O5 Si1 O4 108.90(8) . . ?
O1 Si1 Ca 33.59(5) . . ?
O3 Si1 Ca 107.98(6) . . ?
O5 Si1 Ca 80.06(6) . . ?
O4 Si1 Ca 138.78(6) . . ?
O2 Si2 O3 111.12(9) . . ?
O2 Si2 O5 109.49(8) . 4_465 ?
O3 Si2 O5 107.43(8) . 4_465 ?
O2 Si2 O4 109.28(8) . 5_565 ?
O3 Si2 O4 108.99(8) . 5_565 ?
O5 Si2 O4 110.51(8) 4_465 5_565 ?
O2 Si2 Ca 30.98(6) . 6_556 ?
O3 Si2 Ca 121.56(6) . 6_556 ?
O5 Si2 Ca 78.52(6) 4_465 6_556 ?
O4 Si2 Ca 123.29(6) 5_565 6_556 ?
Si1 O1 V 133.68(9) . 5_565 ?
Si1 O1 Ca 124.00(8) . . ?
V O1 Ca 101.40(6) 5_565 . ?
Si2 O2 V 127.10(9) . . ?
Si2 O2 Ca 128.38(8) . 6_556 ?
V O2 Ca 104.52(6) . 6_556 ?
Si1 O3 Si2 135.18(10) . . ?
Si2 O4 Si1 127.32(10) 5_565 . ?
Si2 O5 Si1 128.24(10) 4_464 . ?
O7A O7 O7B 58(3) . . ?
O7A O7 O7 87(2) . 7_575 ?
O7B O7 O7 143(4) . 7_575 ?
O7A O7 O7A 44(2) . 7_575 ?
O7B O7 O7A 101(4) . 7_575 ?
O7 O7 O7A 42.8(17) 7_575 7_575 ?
O7A O7 O7B 72(3) . 7_575 ?
O7B O7 O7B 127(5) . 7_575 ?
O7 O7 O7B 15.5(15) 7_575 7_575 ?
O7A O7 O7B 28.4(14) 7_575 7_575 ?
O7A O7 Ca 86.8(18) . . ?
O7B O7 Ca 85(3) . . ?
O7 O7 Ca 81.2(5) 7_575 . ?
O7A O7 Ca 81.7(12) 7_575 . ?
O7B O7 Ca 76.1(13) 7_575 . ?
O7 O7A O7A 93(2) . 7_575 ?
O7 O7A O7 51(3) . 7_575 ?
O7A O7A O7 42.8(17) 7_575 7_575 ?
O7 O7A O7B 51(2) . . ?
O7A O7A O7B 142(3) 7_575 . ?
O7 O7A O7B 101(4) 7_575 . ?
O7 O7A O7B 76(3) . 7_575 ?
O7A O7A O7B 17.6(14) 7_575 7_575 ?
O7 O7A O7B 26.3(14) 7_575 7_575 ?
O7B O7A O7B 125(4) . 7_575 ?
O7 O7A Ca 77.9(17) . . ?
O7A O7A Ca 82.2(3) 7_575 . ?
O7 O7A Ca 75.7(12) 7_575 . ?
O7B O7A Ca 79(2) . . ?
O7B O7A Ca 74.2(11) 7_575 . ?
O7 O7B O7A 71(4) . . ?
O7 O7B O7 22(2) . 7_575 ?
O7A O7B O7 51(3) . 7_575 ?
O7 O7B O7A 52(3) . 7_575 ?
O7A O7B O7A 20.0(18) . 7_575 ?
O7 O7B O7A 31.6(18) 7_575 7_575 ?
O7 O7B Ca 82(3) . . ?
O7A O7B Ca 87(2) . . ?
O7 O7B Ca 74.9(14) 7_575 . ?
O7A O7B Ca 77.8(13) 7_575 . ?
 
_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              30.50
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    0.614
_refine_diff_density_min   -0.548
_refine_diff_density_rms    0.095
