data_3471_12

_publ_requested_journal          'Min. Mag.'
_publ_contact_author_name        'Fernando Camara'
_publ_contact_author_address     
;Dip. di Scienze Mineralogiche e Petrologiche
Universit\`a di degli Studi di Torino
Via Valperga Caluso, 35 - 10125 Torino, Italy
;
_publ_contact_author_email       fernando.camaraartigas@unito.it
_publ_contact_author_phone       +390116705132
_publ_contact_author_fax         
;+390116705128

;
loop_
_publ_author_name
_publ_author_address
'Camara, Fernando'
;Dip. di Scienze Mineralogiche e Petrologiche
Universit\`a di degli Studi di Torino
Via Valperga Caluso, 35 - 10125 Torino, Italy
;
'Sokolova, Elena'
;Dept. of Geological Sciences
University of Manitoba
Winnipeg, Manitoba R3T 2N2 Canada
;
'Hawthorne, Frank C.'
;Dept. of Geological Sciences
University of Manitoba
Winnipeg, Manitoba R3T 2N2 Canada
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        rinkite
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            
'Ca1.26 Ce0.13 Dy0 F0.99 Gd0.01 La0.04 Na0.68 Nb0.05 Nd0.06 O5.01 Pr0.01 Si1.33'
_chemical_melting_point          ?

_exptl_crystal_description       IRREGULAR
_exptl_crystal_colour            'light yelow'

_diffrn_ambient_temperature      298(2)
_chemical_formula_weight         262.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 '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           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.4235(10)
_cell_length_b                   5.7083(8)
_cell_length_c                   18.941(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.424(4)
_cell_angle_gamma                90.00
_cell_volume                     786.71(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3729
_cell_measurement_theta_min      4.388
_cell_measurement_theta_max      75.835
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             377
_exptl_absorpt_coefficient_mu    5.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.251 
_exptl_absorpt_correction_T_max  0.437 
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
; 
SADABS was used to perform the Absorption correction
Parameter refinement on 7837 reflections reduced R(int) from 0.0722 to 0.0263
Ratio of minimum to maximum apparent transmission: 0.676803
The given Tmax was generated using the SHELX SIZE command
Tmis was calculated as Tmin = relative-correction-factor * Tmax.
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source_type              SIEMENS
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER-AXS SMART APEX CCD'
_diffrn_measurement_method       \\w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10643
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.80
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1903
_reflns_number_gt                1489
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART,version 5.625'
_computing_cell_refinement       'SAINT version 6.45'
_computing_data_reduction        'SAINT version 6.45'
_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 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^)+(0.0907P)^2^+1.0617P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1903
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1384
_refine_ls_wR_factor_gt          0.1292
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
MCE Ce 0.09346(7) 0.66259(9) 0.19128(3) 0.0205(2) Uani 0.305(3) 1 d P . .
MCA Ca 0.09346(7) 0.66259(9) 0.19128(3) 0.0205(2) Uani 0.695(3) 1 d P . .
ACE Ce 0.59697(8) 0.66591(11) 0.19049(3) 0.0223(3) Uani 0.196(3) 1 d P . .
ACA Ca 0.59697(8) 0.66591(11) 0.19049(3) 0.0223(3) Uani 0.804(3) 1 d P . .
M1 Ti 0.0000 0.0000 0.0000 0.0269(4) Uani 1.100(6) 2 d SP . .
M2 Na 0.5000 0.0000 0.0000 0.0228(6) Uani 1 2 d S . .
M3 Ca 0.75492(16) 0.5009(2) 0.00095(7) 0.0388(6) Uani 0.830(7) 1 d P . .
Si1 Si 0.35087(17) 0.1560(2) 0.13998(7) 0.0175(3) Uani 1 1 d . . .
Si2 Si 0.78416(17) 0.1554(2) 0.13773(7) 0.0174(3) Uani 1 1 d . . .
O1 O 0.2179(5) 0.1496(6) 0.06081(18) 0.0311(8) Uani 1 1 d . . .
O2 O 0.8313(5) 0.1402(6) 0.05808(17) 0.0291(8) Uani 1 1 d . . .
O3 O 0.3376(5) 0.3977(7) 0.1827(2) 0.0317(9) Uani 1 1 d . . .
O4 O 0.8431(5) 0.3995(7) 0.1779(2) 0.0378(10) Uani 1 1 d . . .
O5 O 0.3336(5) 0.9349(7) 0.19092(18) 0.0292(9) Uani 1 1 d . . .
O6 O 0.8559(5) 0.9384(7) 0.19034(17) 0.0290(9) Uani 1 1 d . . .
O7 O 0.5579(5) 0.1403(7) 0.1209(2) 0.0377(9) Uani 1 1 d . . .
XM F 0.0313(5) 0.7041(6) 0.06004(18) 0.0354(11) Uani 0.950(10) 1 d P . .
F F 0.5296(6) 0.6575(5) 0.0612(2) 0.0469(9) Uani 1 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
MCE 0.0137(3) 0.0214(3) 0.0266(4) 0.00240(19) 0.0043(2) 0.00021(18)
MCA 0.0137(3) 0.0214(3) 0.0266(4) 0.00240(19) 0.0043(2) 0.00021(18)
ACE 0.0156(4) 0.0259(4) 0.0261(4) 0.0018(2) 0.0059(3) 0.0002(2)
ACA 0.0156(4) 0.0259(4) 0.0261(4) 0.0018(2) 0.0059(3) 0.0002(2)
M1 0.0108(5) 0.0422(7) 0.0287(7) -0.0211(5) 0.0059(4) -0.0044(5)
M2 0.0301(14) 0.0263(13) 0.0106(12) -0.0019(9) 0.0003(10) -0.0032(11)
M3 0.0300(9) 0.0287(8) 0.0590(12) 0.0137(7) 0.0121(7) 0.0020(6)
Si1 0.0146(6) 0.0202(6) 0.0173(6) -0.0003(4) 0.0022(4) -0.0002(5)
Si2 0.0154(6) 0.0207(6) 0.0164(6) -0.0005(4) 0.0042(4) -0.0004(5)
O1 0.0292(19) 0.0338(19) 0.0248(17) 0.0012(14) -0.0078(14) -0.0051(15)
O2 0.035(2) 0.0345(19) 0.0216(16) 0.0046(14) 0.0145(15) 0.0069(15)
O3 0.0247(19) 0.0293(19) 0.042(2) -0.0148(17) 0.0087(16) 0.0003(15)
O4 0.024(2) 0.033(2) 0.057(3) -0.024(2) 0.0105(18) -0.0073(16)
O5 0.031(2) 0.0283(19) 0.0279(19) 0.0067(14) 0.0046(16) -0.0049(15)
O6 0.031(2) 0.033(2) 0.0233(18) 0.0092(14) 0.0064(16) 0.0081(15)
O7 0.0152(16) 0.058(2) 0.041(2) -0.0109(18) 0.0079(15) -0.0024(17)
XM 0.035(2) 0.044(2) 0.0271(18) -0.0001(14) 0.0053(14) -0.0010(15)
F 0.061(2) 0.0415(19) 0.0363(19) 0.0018(14) 0.0050(17) 0.0008(17)

_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
MCE O6 2.361(4) 1_455 ?
MCE O4 2.364(4) 1_455 ?
MCE O5 2.366(4) . ?
MCE O3 2.390(4) . ?
MCE XM 2.448(3) . ?
MCE O6 2.544(4) 2_645 ?
MCE O4 2.780(5) 2_655 ?
MCE Si2 3.1858(14) 2_655 ?
MCE ACA 3.6828(8) 1_455 ?
MCE ACE 3.6828(8) 1_455 ?
MCE ACE 3.7408(8) . ?
ACE F 2.401(4) . ?
ACE O4 2.425(4) . ?
ACE O3 2.442(4) . ?
ACE O6 2.473(4) . ?
ACE O5 2.487(4) . ?
ACE O5 2.567(4) 2_645 ?
ACE O3 2.700(4) 2_655 ?
ACE Si1 3.1576(14) 2_655 ?
ACE Si2 3.3598(14) 1_565 ?
ACE Si1 3.3743(14) 1_565 ?
ACE Si2 3.4599(14) . ?
ACE Si1 3.4690(14) . ?
M1 O1 1.984(3) 3 ?
M1 O1 1.984(3) . ?
M1 O2 1.991(3) 3_655 ?
M1 O2 1.991(3) 1_455 ?
M1 XM 2.024(3) 3_565 ?
M1 XM 2.024(3) 1_545 ?
M1 M3 3.3822(12) 1_445 ?
M1 M3 3.3822(12) 3_665 ?
M1 M3 3.3911(12) 1_455 ?
M1 M3 3.3911(12) 3_655 ?
M1 M2 3.7118(5) . ?
M1 M2 3.7118(5) 1_455 ?
M2 F 2.261(3) 3_665 ?
M2 F 2.261(3) 1_545 ?
M2 O7 2.383(4) 3_655 ?
M2 O7 2.383(4) . ?
M2 O2 2.613(4) . ?
M2 O2 2.613(4) 3_655 ?
M2 O1 2.719(4) 3_655 ?
M2 O1 2.719(4) . ?
M2 Si2 3.1405(13) . ?
M2 Si2 3.1405(13) 3_655 ?
M2 Si1 3.1953(13) . ?
M2 Si1 3.1953(13) 3_655 ?
M3 O1 2.342(4) 3_665 ?
M3 O2 2.343(4) . ?
M3 F 2.378(4) . ?
M3 F 2.383(4) 3_665 ?
M3 XM 2.428(4) 1_655 ?
M3 XM 2.439(4) 3_665 ?
M3 Si2 3.2287(17) . ?
M3 Si1 3.2784(17) 3_665 ?
M3 M1 3.3823(12) 1_665 ?
M3 M1 3.3911(12) 1_655 ?
M3 M2 3.4182(12) 1_565 ?
Si1 O5 1.609(4) 1_545 ?
Si1 O1 1.624(3) . ?
Si1 O3 1.613(4) . ?
Si1 O7 1.650(4) . ?
Si1 ACA 3.1576(14) 2_645 ?
Si1 ACE 3.1576(14) 2_645 ?
Si1 M3 3.2783(17) 3_665 ?
Si1 ACE 3.3744(14) 1_545 ?
Si1 ACA 3.3744(14) 1_545 ?
Si2 O4 1.606(4) . ?
Si2 O2 1.617(3) . ?
Si2 O6 1.613(4) 1_545 ?
Si2 O7 1.649(3) . ?
Si2 MCA 3.1859(14) 2_645 ?
Si2 MCE 3.1859(14) 2_645 ?
Si2 ACA 3.3599(14) 1_545 ?
Si2 ACE 3.3599(14) 1_545 ?
O1 M3 2.341(4) 3_665 ?
O2 M1 1.991(3) 1_655 ?
O3 ACA 2.700(4) 2_645 ?
O3 ACE 2.700(4) 2_645 ?
O4 MCA 2.364(4) 1_655 ?
O4 MCE 2.364(4) 1_655 ?
O4 MCA 2.780(5) 2_645 ?
O4 MCE 2.780(5) 2_645 ?
O5 Si1 1.609(4) 1_565 ?
O5 ACE 2.567(4) 2_655 ?
O5 ACA 2.567(4) 2_655 ?
O6 Si2 1.613(4) 1_565 ?
O6 MCA 2.361(3) 1_655 ?
O6 MCE 2.361(3) 1_655 ?
O6 MCE 2.544(4) 2_655 ?
O6 MCA 2.544(4) 2_655 ?
O7 ACA 3.001(4) 1_545 ?
XM M1 2.024(3) 1_565 ?
XM M3 2.428(4) 1_455 ?
XM M3 2.439(4) 3_665 ?
F M2 2.261(3) 1_565 ?
F M3 2.383(4) 3_665 ?

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 MCE O4 81.53(14) 1_455 1_455 ?
O6 MCE O5 97.11(14) 1_455 . ?
O4 MCE O5 173.67(14) 1_455 . ?
O6 MCE O3 175.10(12) 1_455 . ?
O4 MCE O3 100.46(15) 1_455 . ?
O5 MCE O3 80.42(14) . . ?
O6 MCE XM 86.42(11) 1_455 . ?
O4 MCE XM 88.09(14) 1_455 . ?
O5 MCE XM 85.65(11) . . ?
O3 MCE XM 89.16(12) . . ?
O6 MCE O6 108.77(7) 1_455 2_645 ?
O4 MCE O6 75.55(14) 1_455 2_645 ?
O5 MCE O6 110.68(10) . 2_645 ?
O3 MCE O6 76.11(13) . 2_645 ?
XM MCE O6 155.33(11) . 2_645 ?
O6 MCE O4 71.14(11) 1_455 2_655 ?
O4 MCE O4 113.29(9) 1_455 2_655 ?
O5 MCE O4 71.83(11) . 2_655 ?
O3 MCE O4 111.80(10) . 2_655 ?
XM MCE O4 145.33(11) . 2_655 ?
O6 MCE O4 59.33(12) 2_645 2_655 ?
O6 MCE Si2 94.50(8) 1_455 2_655 ?
O4 MCE Si2 99.24(11) 1_455 2_655 ?
O5 MCE Si2 87.02(9) . 2_655 ?
O3 MCE Si2 89.62(9) . 2_655 ?
XM MCE Si2 172.67(9) . 2_655 ?
O5 MCE ACA 138.64(9) . 1_455 ?
O3 MCE ACA 140.77(9) . 1_455 ?
XM MCE ACA 90.47(9) . 1_455 ?
O6 MCE ACA 88.80(8) 2_645 1_455 ?
O4 MCE ACA 89.65(7) 2_655 1_455 ?
Si2 MCE ACA 95.04(3) 2_655 1_455 ?
O5 MCE ACE 138.64(9) . 1_455 ?
O3 MCE ACE 140.77(9) . 1_455 ?
XM MCE ACE 90.47(9) . 1_455 ?
O6 MCE ACE 88.80(8) 2_645 1_455 ?
O4 MCE ACE 89.65(7) 2_655 1_455 ?
Si2 MCE ACE 95.04(3) 2_655 1_455 ?
O6 MCE ACE 137.89(9) 1_455 . ?
O4 MCE ACE 140.16(10) 1_455 . ?
XM MCE ACE 89.02(9) . . ?
O6 MCE ACE 91.88(8) 2_645 . ?
O4 MCE ACE 90.46(7) 2_655 . ?
Si2 MCE ACE 85.42(3) 2_655 . ?
ACA MCE ACE 179.26(2) 1_455 . ?
ACE MCE ACE 179.26(2) 1_455 . ?
F ACE O4 84.04(14) . . ?
F ACE O3 85.61(13) . . ?
O4 ACE O3 101.62(14) . . ?
F ACE O6 90.94(12) . . ?
O4 ACE O6 78.07(13) . . ?
O3 ACE O6 176.55(12) . . ?
F ACE O5 90.60(12) . . ?
O4 ACE O5 174.58(13) . . ?
O3 ACE O5 77.07(13) . . ?
O6 ACE O5 102.90(13) . . ?
F ACE O5 147.92(11) . 2_645 ?
O4 ACE O5 74.89(13) . 2_645 ?
O3 ACE O5 75.52(12) . 2_645 ?
O6 ACE O5 107.62(10) . 2_645 ?
O5 ACE O5 109.63(7) . 2_645 ?
F ACE O3 151.80(11) . 2_655 ?
O4 ACE O3 112.85(11) . 2_655 ?
O3 ACE O3 111.20(8) . 2_655 ?
O6 ACE O3 71.93(11) . 2_655 ?
O5 ACE O3 72.40(11) . 2_655 ?
O5 ACE O3 60.27(12) 2_645 2_655 ?
F ACE Si1 174.65(11) . 2_655 ?
O4 ACE Si1 98.37(11) . 2_655 ?
O3 ACE Si1 89.22(9) . 2_655 ?
O6 ACE Si1 94.23(8) . 2_655 ?
O5 ACE Si1 86.90(8) . 2_655 ?
F ACE Si2 74.23(9) . 1_565 ?
O4 ACE Si2 97.37(11) . 1_565 ?
O3 ACE Si2 150.61(10) . 1_565 ?
O5 ACE Si2 81.90(8) . 1_565 ?
O5 ACE Si2 131.62(9) 2_645 1_565 ?
O3 ACE Si2 81.07(8) 2_655 1_565 ?
Si1 ACE Si2 110.04(4) 2_655 1_565 ?
F ACE Si1 74.67(9) . 1_565 ?
O4 ACE Si1 150.25(12) . 1_565 ?
O3 ACE Si1 97.27(10) . 1_565 ?
O6 ACE Si1 81.69(8) . 1_565 ?
O5 ACE Si1 132.65(8) 2_645 1_565 ?
O3 ACE Si1 80.67(8) 2_655 1_565 ?
Si1 ACE Si1 104.70(3) 2_655 1_565 ?
Si2 ACE Si1 57.23(3) 1_565 1_565 ?
F ACE Si2 72.72(9) . . ?
O3 ACE Si2 79.14(9) . . ?
O6 ACE Si2 99.94(9) . . ?
O5 ACE Si2 151.86(9) . . ?
O5 ACE Si2 78.32(8) 2_645 . ?
O3 ACE Si2 131.13(8) 2_655 . ?
Si1 ACE Si2 107.65(3) 2_655 . ?
Si2 ACE Si2 113.65(4) 1_565 . ?
Si1 ACE Si2 147.37(4) 1_565 . ?
F ACE Si1 73.13(9) . . ?
O4 ACE Si1 79.20(9) . . ?
O6 ACE Si1 153.43(9) . . ?
O5 ACE Si1 98.49(9) . . ?
O5 ACE Si1 79.27(8) 2_645 . ?
O3 ACE Si1 130.44(8) 2_655 . ?
Si1 ACE Si1 102.55(4) 2_655 . ?
Si2 ACE Si1 147.36(4) 1_565 . ?
Si1 ACE Si1 113.04(4) 1_565 . ?
Si2 ACE Si1 55.48(3) . . ?
O1 M1 O1 180.0 3 . ?
O1 M1 O2 92.07(16) 3 3_655 ?
O1 M1 O2 87.93(16) . 3_655 ?
O1 M1 O2 87.93(16) 3 1_455 ?
O1 M1 O2 92.07(16) . 1_455 ?
O2 M1 O2 180.00(17) 3_655 1_455 ?
O1 M1 XM 92.48(14) 3 3_565 ?
O1 M1 XM 87.52(14) . 3_565 ?
O2 M1 XM 92.28(14) 3_655 3_565 ?
O2 M1 XM 87.72(14) 1_455 3_565 ?
O1 M1 XM 87.52(14) 3 1_545 ?
O1 M1 XM 92.48(14) . 1_545 ?
O2 M1 XM 87.72(14) 3_655 1_545 ?
O2 M1 XM 92.28(14) 1_455 1_545 ?
XM M1 XM 180.00(19) 3_565 1_545 ?
O1 M1 M3 137.49(10) . 1_445 ?
O2 M1 M3 93.57(10) 3_655 1_445 ?
O2 M1 M3 86.43(10) 1_455 1_445 ?
XM M1 M3 134.75(10) 3_565 1_445 ?
XM M1 M3 45.25(10) 1_545 1_445 ?
O1 M1 M3 137.49(10) 3 3_665 ?
O2 M1 M3 86.43(10) 3_655 3_665 ?
O2 M1 M3 93.57(10) 1_455 3_665 ?
XM M1 M3 45.25(10) 3_565 3_665 ?
XM M1 M3 134.75(10) 1_545 3_665 ?
M3 M1 M3 180.00(4) 1_445 3_665 ?
O1 M1 M3 89.39(11) 3 1_455 ?
O1 M1 M3 90.61(10) . 1_455 ?
O2 M1 M3 137.61(10) 3_655 1_455 ?
XM M1 M3 45.34(10) 3_565 1_455 ?
XM M1 M3 134.66(10) 1_545 1_455 ?
M3 M1 M3 114.87(3) 1_445 1_455 ?
M3 M1 M3 65.13(3) 3_665 1_455 ?
O1 M1 M3 90.61(11) 3 3_655 ?
O1 M1 M3 89.39(10) . 3_655 ?
O2 M1 M3 137.61(10) 1_455 3_655 ?
XM M1 M3 134.66(10) 3_565 3_655 ?
XM M1 M3 45.34(10) 1_545 3_655 ?
M3 M1 M3 65.13(3) 1_445 3_655 ?
M3 M1 M3 114.87(3) 3_665 3_655 ?
M3 M1 M3 180.0 1_455 3_655 ?
O1 M1 M2 134.47(11) 3 . ?
O1 M1 M2 45.53(11) . . ?
O2 M1 M2 137.60(11) 1_455 . ?
XM M1 M2 90.20(10) 3_565 . ?
XM M1 M2 89.80(10) 1_545 . ?
M3 M1 M2 122.61(2) 1_445 . ?
M3 M1 M2 57.39(2) 3_665 . ?
M3 M1 M2 122.52(2) 1_455 . ?
M3 M1 M2 57.48(2) 3_655 . ?
O1 M1 M2 45.53(11) 3 1_455 ?
O1 M1 M2 134.47(11) . 1_455 ?
O2 M1 M2 137.60(11) 3_655 1_455 ?
XM M1 M2 89.80(10) 3_565 1_455 ?
XM M1 M2 90.20(10) 1_545 1_455 ?
M3 M1 M2 57.39(2) 1_445 1_455 ?
M3 M1 M2 122.61(2) 3_665 1_455 ?
M3 M1 M2 57.48(2) 1_455 1_455 ?
M3 M1 M2 122.52(2) 3_655 1_455 ?
M2 M1 M2 180.0 . 1_455 ?
F M2 F 180.00(19) 3_665 1_545 ?
F M2 O7 79.47(13) 3_665 3_655 ?
F M2 O7 100.53(13) 1_545 3_655 ?
F M2 O7 100.53(13) 3_665 . ?
F M2 O7 79.47(13) 1_545 . ?
O7 M2 O7 180.0 3_655 . ?
F M2 O2 86.49(13) 3_665 . ?
F M2 O2 93.51(13) 1_545 . ?
O7 M2 O2 118.89(10) 3_655 . ?
O7 M2 O2 61.11(10) . . ?
F M2 O2 93.51(13) 3_665 3_655 ?
F M2 O2 86.49(13) 1_545 3_655 ?
O7 M2 O2 61.11(10) 3_655 3_655 ?
O7 M2 O2 118.89(10) . 3_655 ?
O2 M2 O2 180.0 . 3_655 ?
F M2 O1 93.39(13) 3_665 3_655 ?
F M2 O1 86.61(13) 1_545 3_655 ?
O7 M2 O1 59.67(11) 3_655 3_655 ?
O7 M2 O1 120.33(11) . 3_655 ?
O2 M2 O1 62.29(10) . 3_655 ?
O2 M2 O1 117.71(10) 3_655 3_655 ?
F M2 O1 86.61(13) 3_665 . ?
F M2 O1 93.39(13) 1_545 . ?
O7 M2 O1 120.33(11) 3_655 . ?
O7 M2 O1 59.67(11) . . ?
O2 M2 O1 117.71(10) . . ?
O2 M2 O1 62.29(10) 3_655 . ?
O1 M2 O1 180.0 3_655 . ?
F M2 Si2 99.36(10) 3_665 . ?
F M2 Si2 80.64(10) 1_545 . ?
O7 M2 Si2 148.96(8) 3_655 . ?
O2 M2 Si2 149.05(7) 3_655 . ?
O1 M2 Si2 89.64(7) 3_655 . ?
O1 M2 Si2 90.36(7) . . ?
F M2 Si2 80.64(10) 3_665 3_655 ?
F M2 Si2 99.36(10) 1_545 3_655 ?
O7 M2 Si2 148.96(8) . 3_655 ?
O2 M2 Si2 149.05(7) . 3_655 ?
O1 M2 Si2 90.36(7) 3_655 3_655 ?
O1 M2 Si2 89.64(7) . 3_655 ?
Si2 M2 Si2 180.0 . 3_655 ?
F M2 Si1 99.79(10) 3_665 . ?
F M2 Si1 80.21(10) 1_545 . ?
O7 M2 Si1 149.84(8) 3_655 . ?
O2 M2 Si1 90.99(7) . . ?
O2 M2 Si1 89.01(7) 3_655 . ?
O1 M2 Si1 149.46(7) 3_655 . ?
Si2 M2 Si1 61.19(3) . . ?
Si2 M2 Si1 118.81(3) 3_655 . ?
F M2 Si1 80.21(10) 3_665 3_655 ?
F M2 Si1 99.79(10) 1_545 3_655 ?
O7 M2 Si1 149.84(8) . 3_655 ?
O2 M2 Si1 89.01(7) . 3_655 ?
O2 M2 Si1 90.99(7) 3_655 3_655 ?
O1 M2 Si1 149.46(7) . 3_655 ?
Si2 M2 Si1 118.81(3) . 3_655 ?
Si2 M2 Si1 61.19(3) 3_655 3_655 ?
Si1 M2 Si1 180.0 . 3_655 ?
O1 M3 O2 160.50(14) 3_665 . ?
O1 M3 F 93.32(13) 3_665 . ?
O2 M3 F 103.74(12) . . ?
O1 M3 F 103.41(12) 3_665 3_665 ?
O2 M3 F 90.25(13) . 3_665 ?
F M3 F 74.98(14) . 3_665 ?
O1 M3 XM 71.03(12) 3_665 1_655 ?
O2 M3 XM 95.84(13) . 1_655 ?
F M3 XM 102.11(13) . 1_655 ?
F M3 XM 173.75(11) 3_665 1_655 ?
O1 M3 XM 92.50(13) 3_665 3_665 ?
O2 M3 XM 71.12(11) . 3_665 ?
F M3 XM 173.27(12) . 3_665 ?
F M3 XM 100.37(13) 3_665 3_665 ?
XM M3 XM 82.98(12) 1_655 3_665 ?
O1 M3 Si2 157.30(10) 3_665 . ?
F M3 Si2 77.67(9) . . ?
F M3 Si2 94.41(9) 3_665 . ?
XM M3 Si2 90.32(9) 1_655 . ?
XM M3 Si2 98.07(9) 3_665 . ?
O2 M3 Si1 153.91(10) . 3_665 ?
F M3 Si1 95.07(9) . 3_665 ?
F M3 Si1 77.20(9) 3_665 3_665 ?
XM M3 Si1 97.71(9) 1_655 3_665 ?
XM M3 Si1 88.53(9) 3_665 3_665 ?
Si2 M3 Si1 170.20(5) . 3_665 ?
O2 M3 M1 131.42(10) . 1_665 ?
F M3 M1 96.68(9) . 1_665 ?
F M3 M1 137.90(9) 3_665 1_665 ?
XM M3 M1 90.03(9) 3_665 1_665 ?
Si2 M3 M1 124.61(5) . 1_665 ?
Si1 M3 M1 62.28(3) 3_665 1_665 ?
O1 M3 M1 128.06(10) 3_665 1_655 ?
F M3 M1 138.47(9) . 1_655 ?
F M3 M1 95.82(9) 3_665 1_655 ?
XM M3 M1 89.99(9) 1_655 1_655 ?
Si2 M3 M1 62.51(3) . 1_655 ?
Si1 M3 M1 122.80(5) 3_665 1_655 ?
M1 M3 M1 114.87(3) 1_665 1_655 ?
O1 M3 M2 52.38(9) 3_665 1_565 ?
O2 M3 M2 144.89(9) . 1_565 ?
F M3 M2 83.00(9) 3_665 1_565 ?
XM M3 M2 91.19(9) 1_655 1_565 ?
XM M3 M2 143.98(9) 3_665 1_565 ?
Si2 M3 M2 117.55(4) . 1_565 ?
Si1 M3 M2 56.95(3) 3_665 1_565 ?
M1 M3 M2 66.16(2) 1_665 1_565 ?
M1 M3 M2 178.81(4) 1_655 1_565 ?
O1 M3 M2 144.13(9) 3_665 . ?
O2 M3 M2 49.61(9) . . ?
F M3 M2 82.87(9) . . ?
XM M3 M2 144.70(9) 1_655 . ?
XM M3 M2 90.44(9) 3_665 . ?
Si2 M3 M2 56.21(3) . . ?
Si1 M3 M2 116.82(4) 3_665 . ?
M1 M3 M2 178.98(4) 1_665 . ?
M1 M3 M2 65.96(2) 1_655 . ?
M2 M3 M2 113.01(3) 1_565 . ?
O5 Si1 O1 115.48(19) 1_545 . ?
O5 Si1 O3 110.5(2) 1_545 . ?
O1 Si1 O3 113.4(2) . . ?
O5 Si1 O7 106.1(2) 1_545 . ?
O1 Si1 O7 102.6(2) . . ?
O3 Si1 O7 108.0(2) . . ?
O5 Si1 ACA 54.02(14) 1_545 2_645 ?
O1 Si1 ACA 150.34(15) . 2_645 ?
O3 Si1 ACA 58.77(15) . 2_645 ?
O7 Si1 ACA 106.97(14) . 2_645 ?
O5 Si1 ACE 54.02(14) 1_545 2_645 ?
O1 Si1 ACE 150.34(15) . 2_645 ?
O3 Si1 ACE 58.77(15) . 2_645 ?
O7 Si1 ACE 106.97(14) . 2_645 ?
O5 Si1 M2 111.16(14) 1_545 . ?
O1 Si1 M2 58.31(14) . . ?
O3 Si1 M2 136.11(15) . . ?
O7 Si1 M2 46.53(13) . . ?
ACA Si1 M2 148.86(4) 2_645 . ?
ACE Si1 M2 148.86(4) 2_645 . ?
O5 Si1 M3 157.25(14) 1_545 3_665 ?
O3 Si1 M3 82.47(15) . 3_665 ?
O7 Si1 M3 86.41(15) . 3_665 ?
ACA Si1 M3 141.13(5) 2_645 3_665 ?
ACE Si1 M3 141.13(5) 2_645 3_665 ?
M2 Si1 M3 63.73(3) . 3_665 ?
O1 Si1 ACE 116.05(14) . 1_545 ?
O3 Si1 ACE 130.57(15) . 1_545 ?
O7 Si1 ACE 62.71(15) . 1_545 ?
ACA Si1 ACE 77.06(3) 2_645 1_545 ?
ACE Si1 ACE 77.06(3) 2_645 1_545 ?
M2 Si1 ACE 75.36(3) . 1_545 ?
M3 Si1 ACE 139.04(5) 3_665 1_545 ?
O1 Si1 ACA 116.05(14) . 1_545 ?
O3 Si1 ACA 130.57(15) . 1_545 ?
O7 Si1 ACA 62.71(15) . 1_545 ?
ACA Si1 ACA 77.06(3) 2_645 1_545 ?
ACE Si1 ACA 77.06(3) 2_645 1_545 ?
M2 Si1 ACA 75.36(3) . 1_545 ?
M3 Si1 ACA 139.04(5) 3_665 1_545 ?
O5 Si1 ACE 126.35(14) 1_545 . ?
O1 Si1 ACE 117.65(13) . . ?
O7 Si1 ACE 69.11(14) . . ?
ACA Si1 ACE 75.68(3) 2_645 . ?
ACE Si1 ACE 75.68(3) 2_645 . ?
M2 Si1 ACE 102.27(3) . . ?
M3 Si1 ACE 75.61(4) 3_665 . ?
ACE Si1 ACE 113.04(4) 1_545 . ?
ACA Si1 ACE 113.04(4) 1_545 . ?
O4 Si2 O2 113.6(2) . . ?
O4 Si2 O6 110.4(2) . 1_545 ?
O2 Si2 O6 115.40(18) . 1_545 ?
O4 Si2 O7 108.0(2) . . ?
O2 Si2 O7 102.53(19) . . ?
O6 Si2 O7 106.2(2) 1_545 . ?
O4 Si2 M2 135.54(17) . . ?
O2 Si2 M2 56.20(14) . . ?
O6 Si2 M2 112.43(15) 1_545 . ?
O7 Si2 M2 48.20(13) . . ?
O4 Si2 MCA 60.73(17) . 2_645 ?
O2 Si2 MCA 151.43(14) . 2_645 ?
O6 Si2 MCA 52.34(14) 1_545 2_645 ?
O7 Si2 MCA 105.78(14) . 2_645 ?
M2 Si2 MCA 149.03(4) . 2_645 ?
O4 Si2 MCE 60.73(17) . 2_645 ?
O2 Si2 MCE 151.43(14) . 2_645 ?
O6 Si2 MCE 52.34(14) 1_545 2_645 ?
O7 Si2 MCE 105.78(14) . 2_645 ?
M2 Si2 MCE 149.03(4) . 2_645 ?
O4 Si2 M3 79.58(18) . . ?
O6 Si2 M3 157.88(14) 1_545 . ?
O7 Si2 M3 88.44(15) . . ?
M2 Si2 M3 65.08(3) . . ?
MCA Si2 M3 140.19(5) 2_645 . ?
MCE Si2 M3 140.19(5) 2_645 . ?
O4 Si2 ACA 132.09(17) . 1_545 ?
O2 Si2 ACA 114.29(14) . 1_545 ?
O7 Si2 ACA 63.15(15) . 1_545 ?
M2 Si2 ACA 76.28(3) . 1_545 ?
MCA Si2 ACA 76.10(3) 2_645 1_545 ?
MCE Si2 ACA 76.10(3) 2_645 1_545 ?
M3 Si2 ACA 141.32(5) . 1_545 ?
O4 Si2 ACE 132.09(17) . 1_545 ?
O2 Si2 ACE 114.29(14) . 1_545 ?
O7 Si2 ACE 63.15(15) . 1_545 ?
M2 Si2 ACE 76.28(3) . 1_545 ?
MCA Si2 ACE 76.10(3) 2_645 1_545 ?
MCE Si2 ACE 76.10(3) 2_645 1_545 ?
M3 Si2 ACE 141.32(5) . 1_545 ?
O2 Si2 ACE 119.23(13) . . ?
O6 Si2 ACE 124.81(14) 1_545 . ?
O7 Si2 ACE 69.40(14) . . ?
M2 Si2 ACE 103.64(4) . . ?
MCA Si2 ACE 75.26(3) 2_645 . ?
MCE Si2 ACE 75.26(3) 2_645 . ?
M3 Si2 ACE 75.54(4) . . ?
ACA Si2 ACE 113.65(4) 1_545 . ?
ACE Si2 ACE 113.65(4) 1_545 . ?
Si1 O1 M1 145.3(2) . . ?
Si1 O1 M3 110.22(17) . 3_665 ?
M1 O1 M3 102.57(14) . 3_665 ?
Si1 O1 M2 91.15(15) . . ?
M1 O1 M2 103.10(14) . . ?
M3 O1 M2 84.62(12) 3_665 . ?
Si2 O2 M1 144.4(2) . 1_655 ?
Si2 O2 M3 107.83(17) . . ?
M1 O2 M3 102.67(13) 1_655 . ?
Si2 O2 M2 92.85(15) . . ?
M1 O2 M2 106.68(14) 1_655 . ?
M3 O2 M2 87.32(12) . . ?
Si1 O3 MCE 134.26(19) . . ?
Si1 O3 ACE 116.16(17) . . ?
MCE O3 ACE 101.46(15) . . ?
Si1 O3 ACA 90.52(18) . 2_645 ?
MCE O3 ACA 104.77(13) . 2_645 ?
ACE O3 ACA 104.65(13) . 2_645 ?
Si1 O3 ACE 90.52(18) . 2_645 ?
MCE O3 ACE 104.77(13) . 2_645 ?
ACE O3 ACE 104.65(13) . 2_645 ?
Si2 O4 MCA 137.4(2) . 1_655 ?
Si2 O4 MCE 137.4(2) . 1_655 ?
Si2 O4 ACE 116.79(18) . . ?
MCA O4 ACE 100.54(15) 1_655 . ?
MCE O4 ACE 100.54(15) 1_655 . ?
Si2 O4 MCA 89.0(2) . 2_645 ?
MCA O4 MCA 102.88(14) 1_655 2_645 ?
MCE O4 MCA 102.88(14) 1_655 2_645 ?
ACE O4 MCA 102.45(14) . 2_645 ?
Si2 O4 MCE 89.0(2) . 2_645 ?
MCA O4 MCE 102.88(14) 1_655 2_645 ?
MCE O4 MCE 102.88(14) 1_655 2_645 ?
ACE O4 MCE 102.45(14) . 2_645 ?
Si1 O5 MCE 131.79(19) 1_565 . ?
Si1 O5 ACE 109.04(17) 1_565 . ?
MCE O5 ACE 100.81(14) . . ?
Si1 O5 ACE 95.50(17) 1_565 2_655 ?
MCE O5 ACE 110.84(13) . 2_655 ?
ACE O5 ACE 107.35(12) . 2_655 ?
Si1 O5 ACA 95.50(17) 1_565 2_655 ?
MCE O5 ACA 110.84(13) . 2_655 ?
ACE O5 ACA 107.35(12) . 2_655 ?
Si2 O6 MCA 132.20(19) 1_565 1_655 ?
Si2 O6 MCE 132.20(19) 1_565 1_655 ?
Si2 O6 ACE 108.79(17) 1_565 . ?
MCA O6 ACE 99.21(14) 1_655 . ?
MCE O6 ACE 99.21(14) 1_655 . ?
Si2 O6 MCE 97.54(18) 1_565 2_655 ?
MCA O6 MCE 110.43(13) 1_655 2_655 ?
MCE O6 MCE 110.43(13) 1_655 2_655 ?
ACE O6 MCE 107.12(12) . 2_655 ?
Si2 O6 MCA 97.54(18) 1_565 2_655 ?
MCA O6 MCA 110.43(13) 1_655 2_655 ?
MCE O6 MCA 110.43(13) 1_655 2_655 ?
ACE O6 MCA 107.12(12) . 2_655 ?
Si2 O7 Si1 155.8(3) . . ?
Si2 O7 M2 100.76(17) . . ?
Si1 O7 M2 103.31(17) . . ?
Si2 O7 ACA 87.50(16) . 1_545 ?
Si1 O7 ACA 88.04(16) . 1_545 ?
M2 O7 ACA 95.87(13) . 1_545 ?
M1 XM M3 98.46(14) 1_565 1_455 ?
M1 XM M3 98.48(14) 1_565 3_665 ?
M3 XM M3 97.02(12) 1_455 3_665 ?
M1 XM MCE 128.96(15) 1_565 . ?
M3 XM MCE 113.19(14) 1_455 . ?
M3 XM MCE 115.16(14) 3_665 . ?
M2 F M3 94.88(15) 1_565 . ?
M2 F M3 95.06(15) 1_565 3_665 ?
M3 F M3 105.02(14) . 3_665 ?
M2 F ACE 119.01(14) 1_565 . ?
M3 F ACE 118.21(17) . . ?
M3 F ACE 119.79(17) 3_665 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.162
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.315