# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2014

#===============================================================================
 
data_YMnO3_200K 

#===============================================================================

# SUBMISSION DETAILS
 
_publ_contact_author_name           'Stefan G. Ebbinghaus'
_publ_contact_author_address  
;
 Institut für Chemie
 Martin-Luther-Universität Halle-Wittenberg
 Kurt-Mothes-Straße 2
 D-06120 Halle(Saale)
 GERMANY
;
 
_publ_contact_author_email  'stefan.ebbinghaus@chemie.uni-halle.de'
_publ_contact_author_fax    '+49-345-55-27028'
_publ_contact_author_phone  '+49-345-55-25870'
 

#==========================================================================
 
_audit_creation_method            SHELXL-97 
_chemical_name_common             ?
_chemical_formula_sum          'Mn1 O3 Y1' 
_chemical_formula_moiety     'Mn O3 Y'
_chemical_formula_weight          191.85 
 
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' 
 'Mn'  'Mn'   0.3368   0.7283 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Y'  'Y'  -2.7962   3.5667 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting                  Hexagonal
_symmetry_space_group_name_Hall      'P 6c -2'
_symmetry_space_group_name_H-M       'P 63 c m'
_symmetry_Int_Tables_number                185
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-y, x-y, z' 
 '-x+y, -x, z' 
 '-x, -y, z+1/2' 
 'y, -x+y, z+1/2' 
 'x-y, x, z+1/2' 
 '-y, -x, z+1/2' 
 '-x+y, y, z+1/2' 
 'x, x-y, z+1/2' 
 'y, x, z' 
 'x-y, -y, z' 
 '-x, -x+y, z' 
 
_cell_length_a                    6.1545(3) 
_cell_length_b                    6.1545(3) 
_cell_length_c                    11.4533(10) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      375.70(4) 
_cell_formula_units_Z             6 
_cell_measurement_temperature     200(2) 
_cell_measurement_reflns_used    8458
_cell_measurement_theta_min      5.23
_cell_measurement_theta_max      34.21
 
_exptl_crystal_description       'plate'
_exptl_crystal_colour            'black'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn     5.088 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              528 
_exptl_absorpt_coefficient_mu     27.816 
_exptl_absorpt_correction_type   'numerical from crystal shape'
_exptl_absorpt_correction_T_min  0.0290
_exptl_absorpt_correction_T_max  0.3157
_exptl_absorpt_process_details    
;
 Meulenaer, J. de & Tompa, H. (1965). Acta Cryst. 19, 1014-1018.
; 
loop_
    _exptl_crystal_face_index_h
    _exptl_crystal_face_index_k
    _exptl_crystal_face_index_l
    _exptl_crystal_face_perp_dist
 -22 -18 -30  0.0186
  30  24  24  0.0229
  11  -8  30  0.0737
  -4   3 -30  0.0813
  13  -2 -30  0.1412
 -19  30  26  0.1576
 
_diffrn_measurement_device         '2-circle goniometer'
_diffrn_measurement_device_type    'STOE IPDS 2T'
_diffrn_detector                   'image plate (34 cm diameter)'
_diffrn_detector_type              'STOE'
_diffrn_detector_area_resol_mean   6.67
_diffrn_source_voltage             50
_diffrn_source_current             35
_diffrn_radiation_monochromator    'plane graphite'
_diffrn_radiation_collimation      '0.5 mm diameter, monocapillary'
_diffrn_measurement_method         'rotation method'
_diffrn_measurement_details
; 
360 frames, detector distance = 65 mm
;
_diffrn_ambient_temperature       200(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 

_diffrn_reflns_number             8956 
_diffrn_reflns_av_R_equivalents   0.1067 
_diffrn_reflns_av_sigmaI/netI     0.0362 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        9 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        9 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          5.23 
_diffrn_reflns_theta_max          33.96 
_reflns_number_total              578 
_reflns_number_gt                 422 
_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)' 
 
_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)+(0.0195P)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        0.0241(12) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.0(3) 
_refine_ls_number_reflns          578 
_refine_ls_number_parameters      33 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0299 
_refine_ls_R_factor_gt            0.0176 
_refine_ls_wR_factor_ref          0.0398 
_refine_ls_wR_factor_gt           0.0386 
_refine_ls_goodness_of_fit_ref    0.958 
_refine_ls_restrained_S_all       0.957 
_refine_ls_shift/su_max           0.004 
_refine_ls_shift/su_mean          0.002 
 
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 
Y1 Y 0.0000 0.0000 0.27675(8) 0.0038(2) Uani 1 6 d S . . 
Y2 Y 0.3333 0.6667 0.2357 0.00479(15) Uani 1 3 d S . . 
Mn Mn 0.3336(11) 0.3336(11) 0.00331(11) 0.00402(10) Uani 1 2 d S . . 
O1 O 0.0000 0.0000 -0.0183(11) 0.0046(14) Uani 1 6 d S . . 
O2 O 0.3333 0.6667 0.0229(7) 0.0104(16) Uani 1 3 d S . . 
O3 O 0.3075(16) 0.3075(16) 0.1662(5) 0.0071(15) Uani 1 2 d S . . 
O4 O 0.3585(16) 0.3585(16) -0.1598(4) 0.0044(13) Uani 1 2 d S . . 
 
 
_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 
Y1 O3 2.277(10) 3 ? 
Y1 O3 2.277(10) 2 ? 
Y1 O3 2.277(10) . ? 
Y1 O4 2.323(9) 4 ? 
Y1 O4 2.323(9) 6 ? 
Y1 O4 2.323(9) 5 ? 
Y1 O1 2.348(12) 4 ? 
Y1 Mn 3.309(4) 6 ? 
Y1 Mn 3.309(4) 5 ? 
Y1 Mn 3.309(4) 4 ? 
Y1 Y2 3.5843(2) 10_455 ? 
Y1 Y2 3.5843(2) 1_545 ? 
Y2 O3 2.279(9) 3_565 ? 
Y2 O3 2.279(9) 2_665 ? 
Y2 O3 2.279(9) . ? 
Y2 O4 2.312(8) 5_565 ? 
Y2 O4 2.312(8) 6 ? 
Y2 O4 2.312(8) 4_665 ? 
Y2 O2 2.438(8) . ? 
Y2 Mn 3.360(4) 3_565 ? 
Y2 Mn 3.360(4) . ? 
Y2 Mn 3.360(4) 2_665 ? 
Y2 Y2 3.55330(17) 10_455 ? 
Y2 Y2 3.55330(17) 10_565 ? 
Mn O3 1.872(6) . ? 
Mn O4 1.875(5) . ? 
Mn O2 2.063(6) 10 ? 
Mn O2 2.063(6) . ? 
Mn O1 2.068(7) . ? 
Mn Y1 3.309(4) 4_554 ? 
Mn Y2 3.360(4) 10 ? 
O1 Mn 2.068(7) 3 ? 
O1 Mn 2.068(7) 2 ? 
O1 Y1 2.348(12) 4_554 ? 
O2 Mn 2.063(6) 3_565 ? 
O2 Mn 2.063(6) 2_665 ? 
O3 Y2 2.279(9) 10 ? 
O4 Y2 2.312(8) 7_664 ? 
O4 Y2 2.312(8) 4_664 ? 
O4 Y1 2.323(9) 4_554 ? 
 
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 
O3 Y1 O3 92.1(2) 3 2 ? 
O3 Y1 O3 92.1(2) 3 . ? 
O3 Y1 O3 92.1(2) 2 . ? 
O3 Y1 O4 77.25(11) 3 4 ? 
O3 Y1 O4 77.25(12) 2 4 ? 
O3 Y1 O4 164.4(2) . 4 ? 
O3 Y1 O4 164.4(2) 3 6 ? 
O3 Y1 O4 77.25(11) 2 6 ? 
O3 Y1 O4 77.25(12) . 6 ? 
O4 Y1 O4 110.69(13) 4 6 ? 
O3 Y1 O4 77.25(11) 3 5 ? 
O3 Y1 O4 164.4(2) 2 5 ? 
O3 Y1 O4 77.25(11) . 5 ? 
O4 Y1 O4 110.69(13) 4 5 ? 
O4 Y1 O4 110.69(13) 6 5 ? 
O3 Y1 O1 123.80(16) 3 4 ? 
O3 Y1 O1 123.80(16) 2 4 ? 
O3 Y1 O1 123.80(16) . 4 ? 
O4 Y1 O1 71.77(14) 4 4 ? 
O4 Y1 O1 71.77(14) 6 4 ? 
O4 Y1 O1 71.77(14) 5 4 ? 
O3 Y1 Mn 162.2(2) 3 6 ? 
O3 Y1 Mn 100.28(14) 2 6 ? 
O3 Y1 Mn 100.28(14) . 6 ? 
O4 Y1 Mn 92.83(13) 4 6 ? 
O4 Y1 Mn 33.42(17) 6 6 ? 
O4 Y1 Mn 92.83(13) 5 6 ? 
O1 Y1 Mn 38.35(9) 4 6 ? 
O3 Y1 Mn 100.28(14) 3 5 ? 
O3 Y1 Mn 162.2(2) 2 5 ? 
O3 Y1 Mn 100.28(14) . 5 ? 
O4 Y1 Mn 92.83(13) 4 5 ? 
O4 Y1 Mn 92.83(13) 6 5 ? 
O4 Y1 Mn 33.42(17) 5 5 ? 
O1 Y1 Mn 38.35(9) 4 5 ? 
Mn Y1 Mn 65.01(15) 6 5 ? 
O3 Y1 Mn 100.28(14) 3 4 ? 
O3 Y1 Mn 100.28(14) 2 4 ? 
O3 Y1 Mn 162.2(2) . 4 ? 
O4 Y1 Mn 33.42(17) 4 4 ? 
O4 Y1 Mn 92.83(13) 6 4 ? 
O4 Y1 Mn 92.83(13) 5 4 ? 
O1 Y1 Mn 38.35(9) 4 4 ? 
Mn Y1 Mn 65.01(15) 6 4 ? 
Mn Y1 Mn 65.01(15) 5 4 ? 
O3 Y1 Y2 129.83(13) 3 10_455 ? 
O3 Y1 Y2 38.15(10) 2 10_455 ? 
O3 Y1 Y2 85.82(2) . 10_455 ? 
O4 Y1 Y2 92.350(16) 4 10_455 ? 
O4 Y1 Y2 39.24(8) 6 10_455 ? 
O4 Y1 Y2 148.93(4) 5 10_455 ? 
O1 Y1 Y2 97.535(15) 4 10_455 ? 
Mn Y1 Y2 64.54(8) 6 10_455 ? 
Mn Y1 Y2 129.46(8) 5 10_455 ? 
Mn Y1 Y2 95.903(13) 4 10_455 ? 
O3 Y1 Y2 38.15(10) 3 1_545 ? 
O3 Y1 Y2 129.83(13) 2 1_545 ? 
O3 Y1 Y2 85.82(2) . 1_545 ? 
O4 Y1 Y2 92.351(16) 4 1_545 ? 
O4 Y1 Y2 148.92(4) 6 1_545 ? 
O4 Y1 Y2 39.24(8) 5 1_545 ? 
O1 Y1 Y2 97.535(15) 4 1_545 ? 
Mn Y1 Y2 129.46(8) 6 1_545 ? 
Mn Y1 Y2 64.54(8) 5 1_545 ? 
Mn Y1 Y2 95.903(13) 4 1_545 ? 
Y2 Y1 Y2 164.93(3) 10_455 1_545 ? 
O3 Y2 O3 108.47(16) 3_565 2_665 ? 
O3 Y2 O3 108.47(16) 3_565 . ? 
O3 Y2 O3 108.47(16) 2_665 . ? 
O3 Y2 O4 77.4(4) 3_565 5_565 ? 
O3 Y2 O4 77.2(3) 2_665 5_565 ? 
O3 Y2 O4 169.3(2) . 5_565 ? 
O3 Y2 O4 77.2(3) 3_565 6 ? 
O3 Y2 O4 169.3(2) 2_665 6 ? 
O3 Y2 O4 77.4(4) . 6 ? 
O4 Y2 O4 95.64(16) 5_565 6 ? 
O3 Y2 O4 169.3(2) 3_565 4_665 ? 
O3 Y2 O4 77.4(4) 2_665 4_665 ? 
O3 Y2 O4 77.2(2) . 4_665 ? 
O4 Y2 O4 95.64(16) 5_565 4_665 ? 
O4 Y2 O4 95.64(16) 6 4_665 ? 
O3 Y2 O2 69.54(15) 3_565 . ? 
O3 Y2 O2 69.54(15) 2_665 . ? 
O3 Y2 O2 69.54(15) . . ? 
O4 Y2 O2 121.16(12) 5_565 . ? 
O4 Y2 O2 121.16(12) 6 . ? 
O4 Y2 O2 121.16(12) 4_665 . ? 
O3 Y2 Mn 32.06(17) 3_565 3_565 ? 
O3 Y2 Mn 92.3(2) 2_665 3_565 ? 
O3 Y2 Mn 88.63(17) . 3_565 ? 
O4 Y2 Mn 100.4(2) 5_565 3_565 ? 
O4 Y2 Mn 96.80(11) 6 3_565 ? 
O4 Y2 Mn 158.58(13) 4_665 3_565 ? 
O2 Y2 Mn 37.61(5) . 3_565 ? 
O3 Y2 Mn 92.3(2) 3_565 . ? 
O3 Y2 Mn 88.63(17) 2_665 . ? 
O3 Y2 Mn 32.06(17) . . ? 
O4 Y2 Mn 158.58(13) 5_565 . ? 
O4 Y2 Mn 100.4(2) 6 . ? 
O4 Y2 Mn 96.80(11) 4_665 . ? 
O2 Y2 Mn 37.61(5) . . ? 
Mn Y2 Mn 63.81(8) 3_565 . ? 
O3 Y2 Mn 88.63(17) 3_565 2_665 ? 
O3 Y2 Mn 32.06(17) 2_665 2_665 ? 
O3 Y2 Mn 92.3(2) . 2_665 ? 
O4 Y2 Mn 96.80(11) 5_565 2_665 ? 
O4 Y2 Mn 158.58(13) 6 2_665 ? 
O4 Y2 Mn 100.4(2) 4_665 2_665 ? 
O2 Y2 Mn 37.61(5) . 2_665 ? 
Mn Y2 Mn 63.81(8) 3_565 2_665 ? 
Mn Y2 Mn 63.81(8) . 2_665 ? 
O3 Y2 Y2 38.79(16) 3_565 10_455 ? 
O3 Y2 Y2 147.1(2) 2_665 10_455 ? 
O3 Y2 Y2 86.5(2) . 10_455 ? 
O4 Y2 Y2 93.3(2) 5_565 10_455 ? 
O4 Y2 Y2 39.79(13) 6 10_455 ? 
O4 Y2 Y2 135.3(2) 4_665 10_455 ? 
O2 Y2 Y2 90.000(1) . 10_455 ? 
Mn Y2 Y2 58.08(2) 3_565 10_455 ? 
Mn Y2 Y2 90.02(10) . 10_455 ? 
Mn Y2 Y2 121.89(10) 2_665 10_455 ? 
O3 Y2 Y2 86.5(2) 3_565 10_565 ? 
O3 Y2 Y2 38.79(16) 2_665 10_565 ? 
O3 Y2 Y2 147.1(2) . 10_565 ? 
O4 Y2 Y2 39.79(13) 5_565 10_565 ? 
O4 Y2 Y2 135.3(2) 6 10_565 ? 
O4 Y2 Y2 93.3(2) 4_665 10_565 ? 
O2 Y2 Y2 90.0 . 10_565 ? 
Mn Y2 Y2 90.02(10) 3_565 10_565 ? 
Mn Y2 Y2 121.89(10) . 10_565 ? 
Mn Y2 Y2 58.08(2) 2_665 10_565 ? 
Y2 Y2 Y2 120.0 10_455 10_565 ? 
O3 Mn O4 179.8(9) . . ? 
O3 Mn O2 86.2(3) . 10 ? 
O4 Mn O2 93.9(3) . 10 ? 
O3 Mn O2 86.2(3) . . ? 
O4 Mn O2 93.9(3) . . ? 
O2 Mn O2 118.9(3) 10 . ? 
O3 Mn O1 91.9(5) . . ? 
O4 Mn O1 87.8(5) . . ? 
O2 Mn O1 120.4(2) 10 . ? 
O2 Mn O1 120.4(2) . . ? 
O3 Mn Y1 136.7(5) . 4_554 ? 
O4 Mn Y1 43.0(3) . 4_554 ? 
O2 Mn Y1 113.16(18) 10 4_554 ? 
O2 Mn Y1 113.16(18) . 4_554 ? 
O1 Mn Y1 44.8(3) . 4_554 ? 
O3 Mn Y2 40.27(19) . . ? 
O4 Mn Y2 139.9(3) . . ? 
O2 Mn Y2 102.6(2) 10 . ? 
O2 Mn Y2 46.2(2) . . ? 
O1 Mn Y2 113.4(3) . . ? 
Y1 Mn Y2 144.13(11) 4_554 . ? 
O3 Mn Y2 40.27(19) . 10 ? 
O4 Mn Y2 139.9(3) . 10 ? 
O2 Mn Y2 46.2(2) 10 10 ? 
O2 Mn Y2 102.6(2) . 10 ? 
O1 Mn Y2 113.4(3) . 10 ? 
Y1 Mn Y2 144.13(11) 4_554 10 ? 
Y2 Mn Y2 63.84(5) . 10 ? 
Mn O1 Mn 118.59(14) . 3 ? 
Mn O1 Mn 118.59(14) . 2 ? 
Mn O1 Mn 118.59(14) 3 2 ? 
Mn O1 Y1 96.9(3) . 4_554 ? 
Mn O1 Y1 96.9(3) 3 4_554 ? 
Mn O1 Y1 96.9(3) 2 4_554 ? 
Mn O2 Mn 118.84(8) 3_565 2_665 ? 
Mn O2 Mn 118.84(8) 3_565 . ? 
Mn O2 Mn 118.84(8) 2_665 . ? 
Mn O2 Y2 96.2(2) 3_565 . ? 
Mn O2 Y2 96.2(2) 2_665 . ? 
Mn O2 Y2 96.2(2) . . ? 
Mn O3 Y1 128.7(5) . . ? 
Mn O3 Y2 107.7(3) . 10 ? 
Y1 O3 Y2 103.7(2) . 10 ? 
Mn O3 Y2 107.7(3) . . ? 
Y1 O3 Y2 103.7(2) . . ? 
Y2 O3 Y2 102.4(3) 10 . ? 
Mn O4 Y2 123.1(2) . 7_664 ? 
Mn O4 Y2 123.1(2) . 4_664 ? 
Y2 O4 Y2 100.4(3) 7_664 4_664 ? 
Mn O4 Y1 103.5(5) . 4_554 ? 
Y2 O4 Y1 101.3(2) 7_664 4_554 ? 
Y2 O4 Y1 101.3(2) 4_664 4_554 ? 
 
_diffrn_measured_fraction_theta_max    0.990 
_diffrn_reflns_theta_full              33.96 
_diffrn_measured_fraction_theta_full   0.990 
_refine_diff_density_max    0.555 
_refine_diff_density_min   -1.003 
_refine_diff_density_rms    0.165 


# start Validation Reply Form
_vrf_PLAT926_YMnO3_200K
;
PROBLEM: Reported and Calculated   R1 Differ by -0.0084 Check 
RESPONSE: The difference between reported and calculated R1 results from 
the inability of CheckCIF to handle the racemic twinning.
;
_vrf_PLAT927_YMnO3_200K
;
PROBLEM: Reported and Calculated  wR2 Differ by  -0.0252 Check 
RESPONSE: The difference between reported and calculated wR2 results from 
the inability of CheckCIF to handle the racemic twinning.
;
_vrf_PLAT928_YMnO3_200K
;
PROBLEM: Reported and Calculated    S value   Differ by -0.607       
RESPONSE: The difference between reported and calculated S results from 
the inability of CheckCIF to handle the racemic twinning.
;
# end Validation Reply Form