data_CORALLOITE _publ_contact_author ; Athos Maria Callegari ; _publ_contact_author_email ; callegari@crystal.unipv.it ; loop_ _publ_author_name _publ_author_address ; Callegari A.M.' ; ; Dip.to di Scienze della Terra e dell'Ambiente, University of Pavia, Pavia, Italy ; ; Boiocchi M. ; ; Centro Grandi Strumenti, University of Pavia, Pavia, Italy ; ; Ciriotti M. E. ; ; Associazione micromineralogica italiana, Devesi-Cirie, Italy ; ; Balestra C. ; ; Associazione micromineralogica italiana, Millesimo, Italy ; _audit_creation_method 'manually entered' _chemical_name_systematic ; ? ; _chemical_name_common 'CORALLOITE' _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_formula_moiety 'As2 H10 Mn3 O14' _chemical_formula_sum 'As2 H10 Mn3 O14' _chemical_formula_weight 548.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 5.5828(7) _cell_length_b 9.7660(7) _cell_length_c 5.5455(13) _cell_angle_alpha 94.467(2) _cell_angle_beta 111.348(3) _cell_angle_gamma 93.850(2) _cell_volume 279.26(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1682 _cell_measurement_theta_min 4 _cell_measurement_theta_max 29 _exptl_crystal_description 'irreglular' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 263 _exptl_absorpt_coefficient_mu 9.296 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Axs Smart-Apex CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4874 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 30.05 _reflns_number_total 3092 _reflns_number_gt 2641 _reflns_threshold_expression >3\s(I) _computing_data_collection 'SMART (Bruker-Axs Inc)' _computing_cell_refinement 'SAINT (Bruker-Axs Inc)' _computing_data_reduction 'SAINT (Bruker-Axs Inc)' _computing_structure_refinement ; ORFLS (Busing et al., 1962), locally modified' ; _refine_special_details ; Refinement of F against reflections with F > 3sigma(F). The threshold expression (_gt) of F > 3sigma(F) corresponds to the cutoff used to discriminate between observed and unobserved reflections for refinement. The use of unitary weigth produces unusual values for the calculated weighted wR-factor (similar to R) and for the goodness of fit statistic. Positions for H atoms bonded to oxygens of water molecules and OH groups were not determined. The origin of unit cell was fixed by keeping the M1 atom site at 0,0,0. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.058(18) _refine_ls_number_reflns 3092 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0471 _refine_ls_wR_factor_gt 0.0413 _refine_ls_restrained_S_all 1.205 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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_posn _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.0643(4) 0.1933(2) 0.5121(4) 0.011(1) Uani 1 1 d . . . As2 As -0.0661(4) 0.8037(2) 0.4850(4) 0.012(1) Uani 1 1 d . . . M1 Mn 0.0000 0.0000 0.0000 0.011(1) Uani 1 1 d S . . M2 Mn 0.5006(5) 0.0047(3) 0.4997(5) 0.011(1) Uani 1 1 d . . . M3 Mn 0.1697(4) 0.5046(2) 0.3445(4) 0.017(1) Uani 1 1 d . . . O1 O -0.0734(13) 0.1508(7) 0.1866(13) 0.011(2) Uani 1 1 d . . . O2 O 0.0608(14) 0.8431(8) 0.8123(14) 0.016(2) Uani 1 1 d . . . O3 O -0.1079(14) 0.1081(8) 0.6569(14) 0.017(3) Uani 1 1 d . . . O4 O 0.1118(13) 0.8912(7) 0.3496(14) 0.015(2) Uani 1 1 d . . . O5 O 0.3748(14) 0.1571(7) 0.6328(15) 0.016(2) Uani 1 1 d . . . O6 O 0.6282(13) 0.8512(7) 0.3668(13) 0.013(2) Uani 1 1 d . . . O7 O 0.0459(13) 0.3631(7) 0.5591(14) 0.016(2) Uani 1 1 d . . . O8 O -0.0853(12) 0.6376(8) 0.4180(15) 0.021(2) Uani 1 1 d . . . OH1 O 0.3683(12) 0.0667(7) 0.1556(13) 0.012(2) Uani 1 1 d . . . OH2 O 0.6237(13) 0.9414(7) -0.1536(14) 0.013(2) Uani 1 1 d . . . OW1 O 0.4615(15) 0.3745(9) 0.2708(19) 0.035(3) Uani 1 1 d . . . OW2 O 0.2816(12) 0.6416(6) 0.1007(12) 0.019(2) Uani 1 1 d . . . OW3 O -0.1225(12) 0.4105(7) -0.0471(13) 0.024(2) Uani 1 1 d . . . OW4 O 0.4961(15) 0.6011(9) 0.7240(17) 0.035(3) 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 As1 0.0100(4) 0.0126(4) 0.0120(5) 0.0014(4) 0.0061(4) 0.0029(4) As2 0.0100(4) 0.0138(4) 0.0141(5) 0.0011(4) 0.0064(4) 0.0029(3) M1 0.0084(4) 0.0146(4) 0.0117(4) 0.0010(3) 0.0044(3) 0.0034(3) M2 0.0081(4) 0.0143(4) 0.0107(4) 0.0008(3) 0.0042(3) 0.0037(3) M3 0.0175(5) 0.0165(5) 0.0193(6) 0.0022(4) 0.0104(5) 0.0033(4) O1 0.0133(3) 0.0120(3) 0.0084(3) -0.0003(2) 0.0026(3) 0.0078(2) O2 0.0128(3) 0.0242(4) 0.0141(4) 0.0031(3) 0.0077(3) 0.0066(3) O3 0.0138(4) 0.0223(4) 0.0147(4) 0.0004(3) 0.0080(3) -0.0039(3) O4 0.0100(3) 0.0172(4) 0.0190(4) 0.0039(3) 0.0079(3) 0.0004(3) O5 0.0153(4) 0.0156(3) 0.0176(4) -0.0012(3) 0.0054(3) 0.0047(3) O6 0.0053(3) 0.0205(3) 0.0101(3) -0.0031(3) 0.0012(3) 0.0050(2) O7 0.0261(3) 0.0083(3) 0.0222(3) 0.0082(3) 0.0160(3) 0.0024(2) O8 0.0083(2) 0.0225(4) 0.0301(4) -0.0030(3) 0.0061(3) 0.0040(2) OH1 0.0078(3) 0.0207(3) 0.0099(3) -0.0015(2) 0.0058(3) 0.0015(2) OH2 0.0077(3) 0.0188(3) 0.0136(3) 0.0058(3) 0.0042(3) 0.0032(2) OW1 0.0307(4) 0.0383(4) 0.0492(5) 0.0208(4) 0.0259(4) 0.0150(3) OW2 0.0170(3) 0.0204(3) 0.0179(3) 0.0028(2) 0.0053(2) 0.0029(2) OW3 0.0220(3) 0.0241(3) 0.0281(3) -0.0048(3) 0.0131(3) 0.0021(2) OW4 0.0298(4) 0.0409(4) 0.0313(4) -0.0012(4) 0.0104(4) -0.0036(3) _geom_special_details ; All s.u.'s are estimated using the full covariance matrix. ; 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 As1 O7 1.674(7) . ? As1 O3 1.679(7) . ? As1 O1 1.689(7) . ? As1 O5 1.689(7) . ? As2 O8 1.622(7) . ? As2 O4 1.676(7) . ? As2 O2 1.692(7) . ? As2 O6 1.702(7) 1_455 ? M1 O1 1.886(6) . ? M1 O2 1.904(7) 1_544 ? M1 OH1 1.959(7) . ? M1 OH2 1.981(7) 1_445 ? M1 O3 2.159(7) 1_554 ? M1 O4 2.192(7) 1_545 ? M2 O5 1.897(7) . ? M2 O6 1.911(6) 1_545 ? M2 OH1 1.941(7) . ? M2 OH2 1.957(7) 1_546 ? M2 O3 2.176(7) 1_655 ? M2 O4 2.203(7) 1_545 ? M3 O8 2.114(6) . ? M3 O7 2.128(6) . ? M3 OW2 2.189(6) . ? M3 OW1 2.262(8) . ? M3 OW3 2.265(7) . ? M3 OW4 2.304(8) . ? 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 As1 O3 109.4(3) . . ? O7 As1 O1 105.4(3) . . ? O3 As1 O1 109.2(3) . . ? O7 As1 O5 110.8(3) . . ? O3 As1 O5 109.9(4) . . ? O1 As1 O5 111.9(3) . . ? O8 As2 O4 113.0(4) . . ? O8 As2 O2 108.9(4) . . ? O4 As2 O2 109.7(3) . . ? O8 As2 O6 107.6(3) . 1_455 ? O4 As2 O6 108.3(3) . 1_455 ? O2 As2 O6 109.2(3) . 1_455 ? O1 M1 O2 177.4(4) . 1_544 ? O1 M1 OH1 89.6(3) . . ? O2 M1 OH1 92.7(3) 1_544 . ? O1 M1 OH2 87.9(3) . 1_445 ? O2 M1 OH2 89.9(3) 1_544 1_445 ? OH1 M1 OH2 177.3(4) . 1_445 ? O1 M1 O3 90.0(3) . 1_554 ? O2 M1 O3 90.9(3) 1_544 1_554 ? OH1 M1 O3 99.1(3) . 1_554 ? OH2 M1 O3 79.9(3) 1_445 1_554 ? O1 M1 O4 89.9(3) . 1_545 ? O2 M1 O4 89.3(3) 1_544 1_545 ? OH1 M1 O4 80.5(3) . 1_545 ? OH2 M1 O4 100.5(3) 1_445 1_545 ? O3 M1 O4 179.6(3) 1_554 1_545 ? O5 M2 O6 179.8(4) . 1_545 ? O5 M2 OH1 89.8(3) . . ? O6 M2 OH1 90.3(3) 1_545 . ? O5 M2 OH2 89.4(3) . 1_546 ? O6 M2 OH2 90.4(3) 1_545 1_546 ? OH1 M2 OH2 178.3(3) . 1_546 ? O5 M2 O3 91.2(3) . 1_655 ? O6 M2 O3 88.7(3) 1_545 1_655 ? OH1 M2 O3 101.5(3) . 1_655 ? OH2 M2 O3 80.0(3) 1_546 1_655 ? O5 M2 O4 90.6(3) . 1_545 ? O6 M2 O4 89.5(3) 1_545 1_545 ? OH1 M2 O4 80.6(3) . 1_545 ? OH2 M2 O4 97.9(3) 1_546 1_545 ? O3 M2 O4 177.2(4) 1_655 1_545 ? O8 M3 O7 86.9(3) . . ? O8 M3 OW2 94.1(3) . . ? O7 M3 OW2 176.3(3) . . ? O8 M3 OW1 176.2(3) . . ? O7 M3 OW1 96.0(3) . . ? OW2 M3 OW1 83.3(3) . . ? O8 M3 OW3 94.0(3) . . ? O7 M3 OW3 94.4(3) . . ? OW2 M3 OW3 82.0(3) . . ? OW1 M3 OW3 88.2(3) . . ? O8 M3 OW4 90.0(3) . . ? O7 M3 OW4 89.6(3) . . ? OW2 M3 OW4 94.0(3) . . ? OW1 M3 OW4 87.5(3) . . ? OW3 M3 OW4 174.4(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.126 _refine_diff_density_min -0.795 _refine_diff_density_rms 0.194