data_cemp_z1 
_audit_update_record
;
2011-11-29 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
? 
_chemical_name_mineral    'oxy-schorl'
_chemical_compound_source 'Zlat Idka, Slovakia'
_chemical_formula_sum
;
Al7.81 B3 Ca0.10 Cl0 F0.14 Fe1.11 H3.24 Mg0.57 Mn0.01 Na0.59 O30.86 Si5.51
;
_chemical_formula_weight          991.23 
 
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' 
 'Na'  'Na'   0.0362   0.0249 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Fe'  'Fe'   0.3463   0.8444 
 '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' 
 'Si'  'Si'   0.0817   0.0704 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Mg'  'Mg'   0.0486   0.0363 
 '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' 
 'Mn'  'Mn'   0.3368   0.7283 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            trigonal 
_symmetry_space_group_name_H-M    'R 3 m' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-y, -x, z' 
 '-x+y, y, z' 
 'x, x-y, z' 
 'x+2/3, y+1/3, z+1/3' 
 '-y+2/3, x-y+1/3, z+1/3' 
 '-x+y+2/3, -x+1/3, z+1/3' 
 '-y+2/3, -x+1/3, z+1/3' 
 '-x+y+2/3, y+1/3, z+1/3' 
 'x+2/3, x-y+1/3, z+1/3' 
 'x+1/3, y+2/3, z+2/3' 
 '-y+1/3, x-y+2/3, z+2/3' 
 '-x+y+1/3, -x+2/3, z+2/3' 
 '-y+1/3, -x+2/3, z+2/3' 
 '-x+y+1/3, y+2/3, z+2/3' 
 'x+1/3, x-y+2/3, z+2/3' 
 
_cell_length_a                    15.916(3) 
_cell_length_b                    15.916(3) 
_cell_length_c                    7.1071(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      1559.1(4) 
_cell_formula_units_Z             3 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     1225 
_cell_measurement_theta_min       3.2 
_cell_measurement_theta_max       36.1 
 
_exptl_crystal_description        'elongated grain' 
_exptl_crystal_colour             'brown'
_exptl_crystal_size_max           0.2 
_exptl_crystal_size_mid           0.1 
_exptl_crystal_size_min           0.1 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.167 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1468 
_exptl_absorpt_coefficient_mu     1.675 
_exptl_absorpt_correction_T_min   0.87503
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_source          'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator   'graphite'
_diffrn_measurement_device_type   'Kuma KM-4/Xcalibur-CCD(Sapphire2)'
_diffrn_measurement_method        '\w scans'
_diffrn_detector_area_resol_mean  8.4353
_diffrn_reflns_number             3174 
_diffrn_reflns_av_R_equivalents   0.0381 
_diffrn_reflns_av_sigmaI/netI     0.0780 
_diffrn_reflns_limit_h_min        -26 
_diffrn_reflns_limit_h_max        17 
_diffrn_reflns_limit_k_min        -17 
_diffrn_reflns_limit_k_max        26 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          3.22 
_diffrn_reflns_theta_max          36.05 
_reflns_number_total              1474 
_reflns_number_gt                 1111 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52
;
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52
;
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 2008)'
 
_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^)+(0.0284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_refine_ls_hydrogen_treatment     undef
_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    -0.15(7) 
_refine_ls_number_reflns          1474 
_refine_ls_number_parameters      92 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0514 
_refine_ls_R_factor_gt            0.0338 
_refine_ls_wR_factor_ref          0.0658 
_refine_ls_wR_factor_gt           0.0625 
_refine_ls_goodness_of_fit_ref    0.841 
_refine_ls_restrained_S_all       0.841 
_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 
Na Na 0.0000 0.0000 0.0825(5) 0.0229(12) Uani 0.859(14) 6 d SP . . 
YAL Al 0.12237(7) 0.06118(4) 0.50346(13) 0.0119(3) Uani 0.799(7) 2 d SP . . 
YFE Fe 0.12237(7) 0.06118(4) 0.50346(13) 0.0119(3) Uani 0.201(7) 2 d SP . . 
ZAL Al 0.29700(6) 0.36937(6) 1.14311(12) 0.0104(2) Uani 0.959(5) 1 d P . . 
Si Si 0.19214(5) 0.19002(5) 0.86941(10) 0.0080(2) Uani 0.899(5) 1 d P . . 
O1 O 0.0000 0.0000 0.6394(8) 0.0269(12) Uani 1 6 d S . . 
O2 O 0.06060(11) 0.1212(2) 0.3556(4) 0.0210(7) Uani 1 2 d S . . 
O3 O 0.2620(2) 0.13101(12) 0.3745(4) 0.0189(7) Uani 1 2 d S . . 
O4 O 0.1869(2) 0.09346(11) 0.9640(4) 0.0198(6) Uani 1 2 d S . . 
O5 O -0.1883(2) -0.09417(11) -0.0580(4) 0.0192(6) Uani 1 2 d S . . 
O6 O 0.19549(14) 0.18438(14) 0.6403(3) 0.0150(4) Uani 1 1 d . . . 
O7 O 0.28759(14) 0.28731(13) 0.9447(3) 0.0142(4) Uani 1 1 d . . . 
O8 O 0.20909(14) 0.26975(14) 1.3046(3) 0.0145(4) Uani 1 1 d . . . 
B B 0.10971(18) 0.2194(4) 0.3182(6) 0.0142(8) 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 
Na 0.0223(15) 0.0223(15) 0.024(2) 0.000 0.000 0.0111(8) 
YAL 0.0113(5) 0.0098(4) 0.0151(5) -0.00095(17) -0.0019(3) 0.0057(2) 
YFE 0.0113(5) 0.0098(4) 0.0151(5) -0.00095(17) -0.0019(3) 0.0057(2) 
ZAL 0.0113(4) 0.0109(4) 0.0098(4) -0.0004(3) 0.0001(3) 0.0060(3) 
Si 0.0081(4) 0.0082(4) 0.0076(3) -0.0008(3) -0.0002(3) 0.0041(3) 
O1 0.0314(19) 0.0314(19) 0.018(3) 0.000 0.000 0.0157(9) 
O2 0.0251(13) 0.0147(14) 0.0197(14) 0.0002(12) 0.0001(6) 0.0073(7) 
O3 0.0291(17) 0.0171(11) 0.0144(13) 0.0003(6) 0.0005(12) 0.0146(8) 
O4 0.0243(16) 0.0168(10) 0.0208(14) 0.0000(6) -0.0001(12) 0.0121(8) 
O5 0.0250(16) 0.0188(11) 0.0160(13) 0.0009(6) 0.0018(11) 0.0125(8) 
O6 0.0165(10) 0.0169(10) 0.0111(8) 0.0008(7) 0.0012(7) 0.0080(8) 
O7 0.0135(9) 0.0138(9) 0.0133(8) -0.0003(7) 0.0002(7) 0.0053(8) 
O8 0.0136(9) 0.0152(10) 0.0153(9) 0.0018(7) -0.0001(7) 0.0075(8) 
B 0.0172(16) 0.015(2) 0.0094(16) -0.0004(14) -0.0002(7) 0.0077(10) 
 
_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 
Na O2 2.561(4) 3 y 
Na O2 2.561(4) 2 y 
Na O2 2.561(4) . y 
Na O4 2.710(3) 1_554 y 
Na O4 2.710(3) 2_554 y 
Na O4 2.710(3) 3_554 y 
Na O5 2.781(3) 3 y
Na O5 2.781(3) 2 y 
Na O5 2.781(3) . y 
YAL O2 1.981(2) . y 
YAL O2 1.981(2) 3 y
YAL O6 1.965(2) 6 y 
YAL O6 1.965(2) . y 
YAL O1 1.944(3) . y
YAL O3 2.132(3) . y 
ZAL O6 1.869(2) 15 y 
ZAL O7 1.876(2) . y 
ZAL O8 1.889(2) . y 
ZAL O8 1.918(2) 15_554 y 
ZAL O7 1.925(2) 8 y 
ZAL O3 1.9890(15) 15 y 
Si O7 1.625(2) . y
Si O5 1.6298(12) 3_556 y
Si O6 1.633(2) . y
Si O4 1.6412(15) . y
B O2 1.380(6) . y
B O8 1.373(3) 1_554 y
B O8 1.373(3) 5_554 y 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              36.05 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    0.668 
_refine_diff_density_min   -0.384 
_refine_diff_density_rms    0.123

