data_cemp_pr1 

_audit_update_record
;
2010-12-22 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97 


_chemical_name_mineral    'oxy-schorl'
_chemical_compound_source 'Pibyslavice, Czech Republic'
_chemical_formula_sum 
;
 Al6.80 B3 Ca0.02 F0.31 Fe1.96 H3.11 K0.01 
 Mg0.19 Mn0.01 Na0.59 O30.69 Si5.94 Ti0.09
;
_chemical_formula_weight          1016.33 
 
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' 
 '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' 
 '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' 
 'Mg'  'Mg'   0.0486   0.0363 
 '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' 
 'K'  'K'   0.2009   0.2494 
 '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                    15.9853(12) 
_cell_length_b                    15.9853(12) 
_cell_length_c                    7.1538(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      1583.1(2) 
_cell_formula_units_Z             3 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used   2936
_cell_measurement_theta_min     2.8470
_cell_measurement_theta_max     36.0482
 
_exptl_crystal_description        'elongated grain'
_exptl_crystal_colour             'brown'
_exptl_crystal_size_max           0.30 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.198 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1501 
_exptl_absorpt_coefficient_mu     2.199 
_exptl_absorpt_correction_T_min                   0.80567
_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            MoK\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             4166 
_diffrn_reflns_av_R_equivalents   0.0195 
_diffrn_reflns_av_sigmaI/netI     0.0279 
_diffrn_reflns_limit_h_min        -26 
_diffrn_reflns_limit_h_max        18 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        23 
_diffrn_reflns_limit_l_min        -8 
_diffrn_reflns_limit_l_max        11 
_diffrn_reflns_theta_min          3.21 
_diffrn_reflns_theta_max          36.07 
_reflns_number_total              1380 
_reflns_number_gt                 1285 
_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^)+(0.0207P)^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     refall 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00058(10) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.005(16) 
_refine_ls_number_reflns          1380 
_refine_ls_number_parameters      96 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0211 
_refine_ls_R_factor_gt            0.0191 
_refine_ls_wR_factor_ref          0.0401 
_refine_ls_wR_factor_gt           0.0398 
_refine_ls_goodness_of_fit_ref    0.976 
_refine_ls_restrained_S_all       0.976 
_refine_ls_shift/su_max           0.001 
_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 0.9019(5) 0.0266(11) Uani 0.676(10) 6 d SP . . 
YFE Fe 0.87496(3) 0.937481(16) 0.50264(6) 0.00869(12) Uani 0.621(4) 2 d SP . . 
YAL Al 0.87496(3) 0.937481(16) 0.50264(6) 0.00869(12) Uani 0.379(4) 2 d SP . . 
ZAL Al 0.70355(3) 0.63191(3) -0.14783(6) 0.00590(13) Uani 0.974(3) 1 d P . . 
ZFE Fe 0.70355(3) 0.63191(3) -0.14783(6) 0.00590(13) Uani 0.026(3) 1 d P . . 
Si Si 0.80806(3) 0.81008(3) 0.12963(6) 0.00569(10) Uani 1 1 d . . . 
O1 O 0.0000 0.0000 0.3485(5) 0.0363(9) Uani 0.69 6 d SP . . 
F F 0.0000 0.0000 0.3485(5) 0.0363(9) Uani 0.31 6 d SP . . 
O2 O 0.93822(6) 0.87643(12) 0.6435(3) 0.0151(4) Uani 1 2 d S . . 
O3 O 0.73144(14) 0.86572(7) 0.6201(2) 0.0123(3) Uani 1 2 d S . . 
O4 O 0.81267(12) 0.90634(6) 0.0387(2) 0.0103(3) Uani 1 2 d S . . 
O5 O 0.18631(12) 0.09316(6) 0.0618(2) 0.0104(3) Uani 1 2 d S . . 
O6 O 0.80182(8) 0.81238(8) 0.35415(17) 0.0089(2) Uani 1 1 d . . . 
O7 O 0.71481(8) 0.71419(8) 0.05039(16) 0.0086(2) Uani 1 1 d . . . 
O8 O 0.79017(8) 0.72936(8) -0.31139(16) 0.0097(2) Uani 1 1 d . . . 
B B 0.88991(10) 0.77981(19) 0.6753(4) 0.0076(4) Uani 1 2 d S . . 
H3 H 0.735(2) 0.8677(12) 0.732(5) 0.021(8) Uiso 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 0.0267(13) 0.0267(13) 0.0263(18) 0.000 0.000 0.0134(7) 
YFE 0.0087(2) 0.00611(15) 0.0121(2) -0.00108(7) -0.00216(15) 0.00433(10) 
YAL 0.0087(2) 0.00611(15) 0.0121(2) -0.00108(7) -0.00216(15) 0.00433(10) 
ZAL 0.0062(2) 0.0058(2) 0.0058(2) -0.00008(16) 0.00034(15) 0.00309(18) 
ZFE 0.0062(2) 0.0058(2) 0.0058(2) -0.00008(16) 0.00034(15) 0.00309(18) 
Si 0.0054(2) 0.00520(19) 0.0064(2) -0.00044(14) -0.00021(15) 0.00266(15) 
O1 0.0494(15) 0.0494(15) 0.0102(15) 0.000 0.000 0.0247(8) 
F 0.0494(15) 0.0494(15) 0.0102(15) 0.000 0.000 0.0247(8) 
O2 0.0207(7) 0.0069(7) 0.0132(8) 0.0008(6) 0.0004(3) 0.0035(4) 
O3 0.0213(9) 0.0123(6) 0.0063(7) 0.0004(3) 0.0007(6) 0.0107(4) 
O4 0.0145(8) 0.0074(5) 0.0114(8) 0.0006(3) 0.0011(6) 0.0072(4) 
O5 0.0149(8) 0.0082(5) 0.0105(7) 0.0006(3) 0.0012(6) 0.0075(4) 
O6 0.0090(5) 0.0103(5) 0.0070(5) -0.0009(4) -0.0003(4) 0.0047(4) 
O7 0.0088(5) 0.0068(5) 0.0082(5) -0.0008(4) -0.0009(4) 0.0024(4) 
O8 0.0075(5) 0.0115(5) 0.0111(5) 0.0021(4) 0.0010(4) 0.0054(5) 
B 0.0077(7) 0.0074(10) 0.0074(10) 0.0000(8) 0.0000(4) 0.0037(5) 
 
_geom_special_details 
;
All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'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 
Na O2 2.519(3) 1_445 y 
Na O2 2.519(3) 3_565 y 
Na O2 2.519(3) 2_655 y 
Na O4 2.772(2) 3_566 y 
Na O4 2.772(2) 1_446 y 
Na O4 2.772(2) 2_656 y 
Na O5 2.821(2) 2_556 y 
Na O5 2.821(2) 1_556 y 
Na O5 2.821(2) 3_556 y 
YFE O2 1.9941(12) . y 
YFE O2 1.9942(12) 3_675 y 
YFE O6 2.0387(13) 6_565 y 
YFE O6 2.0387(13) . y 
YFE O1 2.052(2) 1_665 y 
YFE O3 2.1572(19) . y 
ZAL O6 1.8615(13) 9_564 y 
ZAL O7 1.8804(12) . y 
ZAL O8 1.8857(12) . y 
ZAL O8 1.9264(12) 9_565 y 
ZAL O7 1.9589(12) 14_654 y 
ZAL O3 1.9814(9) 9_564 y 
Si O6 1.6108(13) . y 
Si O7 1.6149(11) . y 
Si O5 1.6253(7) 3_665 y 
Si O4 1.6380(8) . y 
B O2 1.357(3) . y 
B O8 1.3841(18) 1_556 y 
B O8 1.3841(18) 5_656 y 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              36.07 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    0.652 
_refine_diff_density_min   -0.495 
_refine_diff_density_rms    0.083

