 
data_esp2 


_symmetry_space_group_name_hall   '-P 2yb'
#Added by publCIF




_audit_update_record
;
2009-12-01 # Formatted by publCIF
;
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             Esperite 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'Ca1.87 Cr0.02 Fe0.07 Mn0.04 O12 Pb Si3 Zn3' 
_chemical_formula_weight          761.67 
 
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' 
 'Zn'  'Zn'   0.2839   1.4301 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Pb'  'Pb'  -3.3944  10.1111 
 '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' 
 'Mn'  'Mn'   0.3368   0.7283 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cr'  'Cr'   0.3209   0.6236 
 '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 1 21/n 1' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x-1/2, -y-1/2, z-1/2' 
 
_cell_length_a                    8.7889(2) 
_cell_length_b                    8.2685(2) 
_cell_length_c                    15.2535(3) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.0500(10) 
_cell_angle_gamma                 90.00 
_cell_volume                      1108.49(4) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     9164 
_cell_measurement_theta_min       2.67 
_cell_measurement_theta_max       40.8 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.07 
_exptl_crystal_size_mid           0.06 
_exptl_crystal_size_min           0.06 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     4.564 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1403 
_exptl_absorpt_coefficient_mu     22.961 
_exptl_absorpt_correction_type    multi-scan 
_exptl_absorpt_correction_T_min   0.2963 
_exptl_absorpt_correction_T_max   0.3396 
_exptl_absorpt_process_details    '(TWINABS; Sheldrick, 2008)'
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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   'Apex 2 CCD area detector'
_diffrn_measurement_method        'Phi and omega scan' 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             24487 
_diffrn_reflns_av_R_equivalents   0.0321 
_diffrn_reflns_av_sigmaI/netI     0.0334 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -28 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          2.67 
_diffrn_reflns_theta_max          40.81 
_reflns_number_total              7025 
_reflns_number_gt                 5935 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Bruker APEX2 (Bruker, 2003)'
_computing_cell_refinement        'SAINT (Bruker, 2005)'
_computing_data_reduction         SAINT 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 2008)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)' 
_computing_molecular_graphics     'XtalDraw (Downs & Hall-Wallace, 2003)' 
_computing_publication_material   'SHELXTL (Bruker, 1997)' 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0182P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.00065(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          7025 
_refine_ls_number_parameters      191 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0307 
_refine_ls_R_factor_gt            0.0222 
_refine_ls_wR_factor_ref          0.0461 
_refine_ls_wR_factor_gt           0.0441 
_refine_ls_goodness_of_fit_ref    1.001 
_refine_ls_restrained_S_all       1.001 
_refine_ls_shift/su_max           0.002 
_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_symetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Pb Pb 0.245756(8) 0.055200(9) 0.250826(5) 0.00928(2) Uani 1 1 d . . . 
Ca1 Ca 0.73827(4) 0.46078(5) 0.07414(3) 0.00779(6) Uani 1 1 d . . . 
Ca2 Ca 0.76071(4) 0.03835(5) 0.08855(3) 0.00768(6) Uani 1 1 d . . . 
Zn1 Zn 0.57626(3) 0.33526(3) 0.243382(15) 0.00795(4) Uani 1 1 d . . . 
Zn2 Zn 0.07422(3) 0.33879(3) 0.090376(15) 0.00789(4) Uani 1 1 d . . . 
Zn3 Zn 0.09274(3) 0.33936(3) 0.416260(15) 0.00797(4) Uani 1 1 d . . . 
Si1 Si 0.91112(6) 0.22833(7) 0.26527(4) 0.00588(9) Uani 1 1 d . . . 
Si2 Si 0.43933(6) 0.22969(7) 0.41207(4) 0.00581(9) Uani 1 1 d . . . 
Si3 Si 0.39507(6) 0.22585(7) 0.07455(4) 0.00596(9) Uani 1 1 d . . . 
O1 O 0.40952(16) 0.22951(18) 0.18190(9) 0.0094(2) Uani 1 1 d . . . 
O2 O 0.43393(16) 0.73658(18) 0.29470(10) 0.0093(2) Uani 1 1 d . . . 
O3 O 0.26983(16) 0.23027(18) 0.36612(10) 0.0095(2) Uani 1 1 d . . . 
O4 O 0.76842(16) 0.25032(18) 0.19791(9) 0.0087(2) Uani 1 1 d . . . 
O5 O 0.91245(16) 0.24224(18) 0.01701(9) 0.0082(2) Uani 1 1 d . . . 
O6 O 0.56548(16) 0.25408(18) 0.03459(9) 0.0086(2) Uani 1 1 d . . . 
O7 O 0.54635(17) 0.36723(18) 0.36778(9) 0.0097(2) Uani 1 1 d . . . 
O8 O 0.27624(16) 0.36327(18) 0.04170(10) 0.0099(2) Uani 1 1 d . . . 
O9 O 0.91472(16) 0.36442(17) 0.34199(10) 0.0097(2) Uani 1 1 d . . . 
O10 O 0.58887(18) 0.55191(16) 0.18814(10) 0.0115(3) Uani 1 1 d . . . 
O11 O -0.01719(16) 0.55450(16) 0.10598(10) 0.0102(3) Uani 1 1 d . . . 
O12 O 0.17231(17) 0.55078(16) 0.45324(10) 0.0103(3) Uani 1 1 d . . . 
 
 
_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 
Pb O2 2.2855(14) 2_545 ? 
Pb O3 2.2875(14) . ? 
Pb O1 2.2928(14) . ? 
Pb O10 3.0857(15) 2_545 ? 
Pb O2 3.1815(15) 1_545 ? 
Pb O1 3.1890(15) 2_545 ? 
Pb O12 3.1958(15) 2_545 ? 
Pb O3 3.2278(16) 2_545 ? 
Pb O11 3.2331(16) 2_545 ? 
Ca1 O8 2.2922(15) 3_665 ? 
Ca1 O10 2.3065(15) . ? 
Ca1 O11 2.3354(15) 1_655 ? 
Ca1 O6 2.3642(15) . ? 
Ca1 O5 2.5240(15) . ? 
Ca1 O4 2.5811(15) . ? 
Ca2 O7 2.3063(15) 2_645 ? 
Ca2 O12 2.3245(16) 4_665 ? 
Ca2 O9 2.3602(14) 2_645 ? 
Ca2 O5 2.4113(14) . ? 
Ca2 O4 2.4206(15) . ? 
Ca2 O6 2.6079(15) . ? 
Zn1 O7 1.9341(14) . ? 
Zn1 O1 1.9467(15) . ? 
Zn1 O4 1.9567(14) . ? 
Zn1 O10 1.9828(14) . ? 
Zn2 O8 1.9358(14) . ? 
Zn2 O2 1.9474(14) 2_545 ? 
Zn2 O11 1.9707(14) . ? 
Zn2 O5 1.9769(14) 1_455 ? 
Zn3 O9 1.9419(15) 1_455 ? 
Zn3 O3 1.9553(14) . ? 
Zn3 O12 1.9654(14) . ? 
Zn3 O6 1.9781(14) 4_566 ? 
Si1 O10 1.6226(15) 2_645 ? 
Si1 O9 1.6238(15) . ? 
Si1 O4 1.6308(15) . ? 
Si1 O2 1.6426(15) 2_645 ? 
Si2 O7 1.6234(15) . ? 
Si2 O11 1.6256(15) 2_545 ? 
Si2 O5 1.6348(15) 4_566 ? 
Si2 O3 1.6458(15) . ? 
Si3 O12 1.6203(15) 2_545 ? 
Si3 O8 1.6223(15) . ? 
Si3 O6 1.6342(14) . ? 
Si3 O1 1.6426(15) . ? 

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 
O7 Zn1 O1 115.55(6) . . ? 
O7 Zn1 O4 120.99(6) . . ? 
O1 Zn1 O4 108.52(6) . . ? 
O7 Zn1 O10 107.52(6) . . ? 
O1 Zn1 O10 104.09(7) . . ? 
O4 Zn1 O10 97.19(6) . . ? 
O8 Zn2 O2 115.17(6) . 2_545 ? 
O8 Zn2 O11 109.02(6) . . ? 
O2 Zn2 O11 105.58(6) 2_545 . ? 
O8 Zn2 O5 118.98(6) . 1_455 ? 
O2 Zn2 O5 107.90(6) 2_545 1_455 ? 
O11 Zn2 O5 98.10(6) . 1_455 ? 
O9 Zn3 O3 117.54(6) 1_455 . ? 
O9 Zn3 O12 111.03(6) 1_455 . ? 
O3 Zn3 O12 103.85(6) . . ? 
O9 Zn3 O6 118.40(6) 1_455 4_566 ? 
O3 Zn3 O6 105.89(6) . 4_566 ? 
O12 Zn3 O6 97.41(6) . 4_566 ? 
O10 Si1 O9 107.89(8) 2_645 . ? 
O10 Si1 O4 112.08(8) 2_645 . ? 
O9 Si1 O4 113.03(8) . . ? 
O10 Si1 O2 106.35(8) 2_645 2_645 ? 
O9 Si1 O2 110.92(8) . 2_645 ? 
O4 Si1 O2 106.39(8) . 2_645 ? 
O7 Si2 O11 108.03(8) . 2_545 ? 
O7 Si2 O5 113.09(8) . 4_566 ? 
O11 Si2 O5 110.71(8) 2_545 4_566 ? 
O7 Si2 O3 110.20(8) . . ? 
O11 Si2 O3 108.16(8) 2_545 . ? 
O5 Si2 O3 106.56(8) 4_566 . ? 
O12 Si3 O8 108.05(8) 2_545 . ? 
O12 Si3 O6 111.40(8) 2_545 . ? 
O8 Si3 O6 112.00(8) . . ? 
O12 Si3 O1 107.76(8) 2_545 . ? 
O8 Si3 O1 110.13(8) . . ? 
O6 Si3 O1 107.42(8) . . ? 
 
_diffrn_measured_fraction_theta_max    0.972 
_diffrn_reflns_theta_full              40.81 
_diffrn_measured_fraction_theta_full   0.972 
_refine_diff_density_max    3.290 
_refine_diff_density_min   -1.234 
_refine_diff_density_rms    0.239 
