 
data_miguelromeroite 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'H20 As8 Mn10 O40' 
_chemical_formula_weight          1808.92 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'As'  'As'   0.0499   2.0058 
 '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' 
 'O'  'O'   0.0106   0.0060 
 '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            ? 
_symmetry_space_group_name_H-M    ? 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
 
_cell_length_a                    18.0300(10) 
_cell_length_b                    9.2715(5) 
_cell_length_c                    9.7756(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  96.266(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      1624.38(15) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.24 
_exptl_crystal_size_mid           0.19 
_exptl_crystal_size_min           0.17 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     3.698 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1708 
_exptl_absorpt_coefficient_mu     11.977 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   0.1612 
_exptl_absorpt_correction_T_max   0.2353 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71075 
_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             16656 
_diffrn_reflns_av_R_equivalents   0.0434 
_diffrn_reflns_av_sigmaI/netI     0.0236 
_diffrn_reflns_limit_h_min        -22 
_diffrn_reflns_limit_h_max        23 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        12 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          3.16 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              1863 
_reflns_number_gt                 1781 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_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)+(0.0466P)²+50.0010P] where P=(Fo²+2Fc²)/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          1863 
_refine_ls_number_parameters      153 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.0402 
_refine_ls_R_factor_gt            0.0383 
_refine_ls_wR_factor_ref          0.0990 
_refine_ls_wR_factor_gt           0.0977 
_refine_ls_goodness_of_fit_ref    1.044 
_refine_ls_restrained_S_all       1.042 
_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 
Mn1 Mn 0.5000 0.39422(14) 0.7500 0.0134(3) Uani 1 2 d S . . 
Mn2 Mn 0.31499(4) 0.08719(8) 0.18801(8) 0.00553(18) Uani 1 1 d . . . 
Mn3 Mn 0.32573(5) 0.47138(10) 0.13764(9) 0.0116(2) Uani 1 1 d . . . 
As1 As 0.41668(3) 0.31557(6) 0.41075(6) 0.01243(17) Uani 1 1 d . . . 
As2 As 0.66118(3) 0.23631(6) 0.62399(6) 0.01146(16) Uani 1 1 d . . . 
O1 O 0.4242(3) 0.4383(5) 0.2882(4) 0.0190(9) Uani 1 1 d . . . 
O2 O 0.3388(3) 0.2224(5) 0.3621(5) 0.0194(9) Uani 1 1 d . . . 
O3 O 0.4153(3) 0.3919(5) 0.5667(5) 0.0196(9) Uani 1 1 d . . . 
O4 O 0.6650(2) 0.2579(5) 0.4519(4) 0.0153(9) Uani 1 1 d . . . 
O5 O 0.7070(2) 0.0866(5) 0.6782(5) 0.0160(9) Uani 1 1 d . . . 
O6 O 0.7036(2) 0.3773(5) 0.7080(5) 0.0164(9) Uani 1 1 d . . . 
O7 O 0.5704(2) 0.2280(5) 0.6561(5) 0.0167(9) Uani 1 1 d . . . 
OH O 0.4902(3) 0.1977(5) 0.4214(5) 0.0233(10) Uani 1 1 d D . . 
OW1 O 0.2418(3) 0.4236(5) 0.4706(5) 0.0197(9) Uani 1 1 d D . . 
OW2 O 0.5840(3) 0.0058(6) 0.8411(5) 0.0260(11) Uani 1 1 d D . . 
HOH H 0.508(5) 0.221(10) 0.508(5) 0.04(3) Uiso 1 1 d D . . 
HW1A H 0.210(4) 0.378(8) 0.521(8) 0.04(3) Uiso 1 1 d D . . 
HW1B H 0.260(6) 0.357(8) 0.416(9) 0.06(3) Uiso 1 1 d D . . 
HW2A H 0.571(4) 0.082(6) 0.787(7) 0.02(2) Uiso 1 1 d D . . 
HW2B H 0.546(4) -0.056(9) 0.836(13) 0.09(5) Uiso 1 1 d 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 
Mn1 O1 2.128(5) 5_666 ? 
Mn1 O1 2.128(5) 6_566 ? 
Mn1 O3 2.224(4) . ? 
Mn1 O3 2.224(4) 2_656 ? 
Mn1 O7 2.255(4) . ? 
Mn1 O7 2.255(4) 2_656 ? 
Mn2 OW2 2.063(5) 5_656 ? 
Mn2 O6 2.066(4) 8_455 ? 
Mn2 O2 2.120(5) . ? 
Mn2 O5 2.140(4) 5_656 ? 
Mn2 O4 2.148(4) 2_655 ? 
Mn2 OW1 2.325(5) 4_545 ? 
Mn3 O6 2.168(4) 5_666 ? 
Mn3 O4 2.178(4) 2_655 ? 
Mn3 O1 2.201(5) . ? 
Mn3 O3 2.222(5) 6_565 ? 
Mn3 O5 2.283(4) 8_455 ? 
Mn3 OW1 2.316(5) 6_565 ? 
As1 O1 1.669(4) . ? 
As1 O2 1.673(5) . ? 
As1 O3 1.684(4) . ? 
As1 OH 1.713(5) . ? 
As1 HOH 2.02(9) . ? 
As2 O5 1.672(4) . ? 
As2 O6 1.682(4) . ? 
As2 O7 1.701(4) . ? 
As2 O4 1.703(4) . ? 
O1 Mn1 2.128(5) 5_666 ? 
O2 OW1 2.840(7) . ? 
O3 Mn3 2.222(5) 6_566 ? 
O4 Mn2 2.148(4) 2_655 ? 
O4 Mn3 2.178(4) 2_655 ? 
O5 Mn2 2.140(4) 5_656 ? 
O5 Mn3 2.283(4) 8_556 ? 
O6 Mn2 2.066(4) 8_556 ? 
O6 Mn3 2.168(4) 5_666 ? 
O7 OH 2.591(7) . ? 
O7 OW2 2.735(7) . ? 
OH HOH 0.90(3) . ? 
OW1 Mn3 2.316(5) 6_566 ? 
OW1 Mn2 2.325(5) 4 ? 
OW1 O2 2.672(6) 7_556 ? 
OW1 HW1A 0.90(3) . ? 
OW1 HW1B 0.90(3) . ? 
OW2 Mn2 2.063(5) 5_656 ? 
OW2 OH 2.706(7) 6_556 ? 
OW2 HW2A 0.90(3) . ? 
OW2 HW2B 0.89(3) . ? 
 
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 
O1 Mn1 O1 86.3(3) 5_666 6_566 ? 
O1 Mn1 O3 105.27(17) 5_666 . ? 
O1 Mn1 O3 75.57(17) 6_566 . ? 
O1 Mn1 O3 75.57(17) 5_666 2_656 ? 
O1 Mn1 O3 105.27(17) 6_566 2_656 ? 
O3 Mn1 O3 178.9(3) . 2_656 ? 
O1 Mn1 O7 91.51(17) 5_666 . ? 
O1 Mn1 O7 166.17(16) 6_566 . ? 
O3 Mn1 O7 91.91(16) . . ? 
O3 Mn1 O7 87.33(17) 2_656 . ? 
O1 Mn1 O7 166.17(16) 5_666 2_656 ? 
O1 Mn1 O7 91.51(17) 6_566 2_656 ? 
O3 Mn1 O7 87.33(17) . 2_656 ? 
O3 Mn1 O7 91.91(16) 2_656 2_656 ? 
O7 Mn1 O7 93.8(2) . 2_656 ? 
OW2 Mn2 O6 164.1(2) 5_656 8_455 ? 
OW2 Mn2 O2 104.7(2) 5_656 . ? 
O6 Mn2 O2 86.79(18) 8_455 . ? 
OW2 Mn2 O5 89.72(18) 5_656 5_656 ? 
O6 Mn2 O5 79.34(17) 8_455 5_656 ? 
O2 Mn2 O5 89.39(18) . 5_656 ? 
OW2 Mn2 O4 90.46(18) 5_656 2_655 ? 
O6 Mn2 O4 100.09(17) 8_455 2_655 ? 
O2 Mn2 O4 92.42(17) . 2_655 ? 
O5 Mn2 O4 178.07(17) 5_656 2_655 ? 
OW2 Mn2 OW1 88.09(19) 5_656 4_545 ? 
O6 Mn2 OW1 78.73(17) 8_455 4_545 ? 
O2 Mn2 OW1 163.15(17) . 4_545 ? 
O5 Mn2 OW1 79.57(17) 5_656 4_545 ? 
O4 Mn2 OW1 98.52(16) 2_655 4_545 ? 
O6 Mn3 O4 154.56(17) 5_666 2_655 ? 
O6 Mn3 O1 82.22(17) 5_666 . ? 
O4 Mn3 O1 92.91(17) 2_655 . ? 
O6 Mn3 O3 95.08(17) 5_666 6_565 ? 
O4 Mn3 O3 107.65(17) 2_655 6_565 ? 
O1 Mn3 O3 74.17(17) . 6_565 ? 
O6 Mn3 O5 74.17(16) 5_666 8_455 ? 
O4 Mn3 O5 88.28(16) 2_655 8_455 ? 
O1 Mn3 O5 123.68(17) . 8_455 ? 
O3 Mn3 O5 156.24(17) 6_565 8_455 ? 
O6 Mn3 OW1 91.66(17) 5_666 6_565 ? 
O4 Mn3 OW1 99.86(16) 2_655 6_565 ? 
O1 Mn3 OW1 161.34(17) . 6_565 ? 
O3 Mn3 OW1 88.93(16) 6_565 6_565 ? 
O5 Mn3 OW1 70.65(16) 8_455 6_565 ? 
O1 As1 O2 106.3(2) . . ? 
O1 As1 O3 112.0(2) . . ? 
O2 As1 O3 112.3(2) . . ? 
O1 As1 OH 110.8(2) . . ? 
O2 As1 OH 107.9(2) . . ? 
O3 As1 OH 107.5(2) . . ? 
O1 As1 HOH 121(3) . . ? 
O2 As1 HOH 122(3) . . ? 
O3 As1 HOH 81.2(17) . . ? 
OH As1 HOH 26.4(17) . . ? 
O5 As2 O6 107.9(2) . . ? 
O5 As2 O7 110.9(2) . . ? 
O6 As2 O7 109.9(2) . . ? 
O5 As2 O4 109.8(2) . . ? 
O6 As2 O4 109.0(2) . . ? 
O7 As2 O4 109.4(2) . . ? 
As1 O1 Mn1 136.7(3) . 5_666 ? 
As1 O1 Mn3 116.9(2) . . ? 
Mn1 O1 Mn3 105.53(18) 5_666 . ? 
As1 O2 Mn2 128.6(3) . . ? 
As1 O2 OW1 95.0(2) . . ? 
Mn2 O2 OW1 127.5(2) . . ? 
As1 O3 Mn3 127.3(2) . 6_566 ? 
As1 O3 Mn1 131.1(2) . . ? 
Mn3 O3 Mn1 101.64(18) 6_566 . ? 
As2 O4 Mn2 124.8(2) . 2_655 ? 
As2 O4 Mn3 121.1(2) . 2_655 ? 
Mn2 O4 Mn3 112.84(19) 2_655 2_655 ? 
As2 O5 Mn2 134.5(2) . 5_656 ? 
As2 O5 Mn3 125.5(2) . 8_556 ? 
Mn2 O5 Mn3 99.71(17) 5_656 8_556 ? 
As2 O6 Mn2 118.2(2) . 8_556 ? 
As2 O6 Mn3 135.3(2) . 5_666 ? 
Mn2 O6 Mn3 106.03(19) 8_556 5_666 ? 
As2 O7 Mn1 129.8(2) . . ? 
As2 O7 OH 107.3(2) . . ? 
Mn1 O7 OH 98.63(19) . . ? 
As2 O7 OW2 97.9(2) . . ? 
Mn1 O7 OW2 105.0(2) . . ? 
OH O7 OW2 120.3(2) . . ? 
As1 OH O7 109.8(2) . . ? 
As1 OH HOH 96(6) . . ? 
O7 OH HOH 14(6) . . ? 
Mn3 OW1 Mn2 113.7(2) 6_566 4 ? 
Mn3 OW1 O2 97.97(19) 6_566 7_556 ? 
Mn2 OW1 O2 120.6(2) 4 7_556 ? 
Mn3 OW1 O2 99.09(19) 6_566 . ? 
Mn2 OW1 O2 115.07(19) 4 . ? 
O2 OW1 O2 107.09(19) 7_556 . ? 
Mn3 OW1 HW1A 103(6) 6_566 . ? 
Mn2 OW1 HW1A 115(6) 4 . ? 
O2 OW1 HW1A 6(6) 7_556 . ? 
O2 OW1 HW1A 110(6) . . ? 
Mn3 OW1 HW1B 117(7) 6_566 . ? 
Mn2 OW1 HW1B 102(7) 4 . ? 
O2 OW1 HW1B 106(6) 7_556 . ? 
O2 OW1 HW1B 18(7) . . ? 
HW1A OW1 HW1B 107(4) . . ? 
Mn2 OW2 OH 109.7(2) 5_656 6_556 ? 
Mn2 OW2 O7 103.9(2) 5_656 . ? 
OH OW2 O7 134.7(2) 6_556 . ? 
Mn2 OW2 HW2A 115(5) 5_656 . ? 
OH OW2 HW2A 126(5) 6_556 . ? 
O7 OW2 HW2A 11(5) . . ? 
Mn2 OW2 HW2B 114(8) 5_656 . ? 
OH OW2 HW2B 21(7) 6_556 . ? 
O7 OW2 HW2B 116(6) . . ? 
HW2A OW2 HW2B 109(5) . . ? 
 
_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    2.351 
_refine_diff_density_min   -1.154 
_refine_diff_density_rms    0.223 
