#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/66/2236685.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2236685
loop_
_publ_author_name
'Sato, Mineo'
'Ishigaki, Tadashi'
'Uematsu, Kazuyoshi'
'Toda, Kenji'
'Okawa, Hirokazu'
_publ_section_title
;
 Redetermination of the low-temperature polymorph of Li₂MnSiO₄ from
 single-crystal X-ray data
;
_journal_coeditor_code           WM2658
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i68
_journal_page_last               i69
_journal_paper_doi               10.1107/S1600536812035040
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'Li2 Mn1 Si1 O4'
_chemical_formula_moiety         'Li2 Mn1 Si1 O4'
_chemical_formula_sum            'Li2 Mn O4 Si'
_chemical_formula_weight         160.91
_chemical_name_systematic
;
dilithium manganese(II) silicate
;
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3133(16)
_cell_length_b                   5.3677(14)
_cell_length_c                   4.9685(12)
_cell_measurement_reflns_used    1684
_cell_measurement_temperature    295
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     168.37(7)
_computing_cell_refinement       'CrystalClear (Rigaku, 2010)'
_computing_data_collection       'CrystalClear (Rigaku, 2010)'
_computing_data_reduction        'CrystalClear (Rigaku, 2010)'
_computing_molecular_graphics    'VESTA (Momma & Izumi, 2011)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      295
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Mercury375R
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1636
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.8
_exptl_absorpt_coefficient_mu    4.114
_exptl_absorpt_correction_T_max  0.477
_exptl_absorpt_correction_T_min  0.377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Rigaku, 1998)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    3.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             154
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.617
_refine_ls_abs_structure_details 'Flack (1983), 189 Friedel pairs'
_refine_ls_abs_structure_Flack   0.171(15)
_refine_ls_extinction_coef       0.392(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     45
_refine_ls_number_reflns         423
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0146
_refine_ls_R_factor_gt           0.0145
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0217P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0366
_refine_ls_wR_factor_ref         0.0366
_reflns_number_gt                419
_reflns_number_total             423
_reflns_threshold_expression     I>2σ(I)
_iucr_refine_instructions_details
;
TITL lms2
CELL  0.71069   6.3133   5.3677   4.9685   90.000   90.000   90.000
ZERR     2.00   0.0016   0.0014   0.0012    0.000    0.000    0.000
LATT  -1
SYMM  1/2 - X, - Y, 1/2 + Z
SYMM  - X,   Y,   Z
SYMM  1/2 + X, - Y, 1/2 + Z
SFAC  LI   O    SI   MN
UNIT  4    8    2    2
MERG   2
TWIN
FMAP   2
PLAN    5
ACTA
LIST   4
L.S.   4
WGHT    0.021700
EXTI    0.392339
BASF   0.17131
FVAR       6.46625
LI1   1    0.750281   -0.168755    0.994696    11.00000    0.00845    0.00606 =
         0.01247   -0.00172    0.00002   -0.00086
MN1   4    0.500000    0.331719    0.996800    10.50000    0.00548    0.00716 =
         0.00934    0.00001    0.00000    0.00000
SI1   3    1.000000    0.320904    0.985144    10.50000    0.00349    0.00284 =
         0.00418   -0.00032    0.00000    0.00000
O1    2    0.500000    0.686777    1.156932    10.50000    0.00748    0.00832 =
         0.00558   -0.00037    0.00000    0.00000
O2    2    0.500000    0.386691    0.580410    10.50000    0.00984    0.00477 =
         0.00958    0.00009    0.00000    0.00000
O3    2    0.788661    0.179922    1.097928    11.00000    0.00685    0.00670 =
         0.00887   -0.00001    0.00077   -0.00087
HKLF    4
REM  User-defined
REM R1 =  0.0145 for    419 Fo > 4sig(Fo)  and  0.0146 for all    423 data
REM     45 parameters refined using      1 restraints
END
WGHT      0.0217      0.0000
REM Highest difference peak  0.249,  deepest hole -0.617,  1-sigma level  0.093
Q1    1   0.7688  0.1785  0.8868  11.00000  0.05    0.23
Q2    1   0.5000  0.3559  0.3943  10.50000  0.05    0.18
Q3    1   0.3054  0.6627  1.2688  11.00000  0.05    0.16
Q4    1   0.2860  0.4475  0.7834  11.00000  0.05    0.16
Q5    1   0.8315  0.3174  1.2470  11.00000  0.05    0.16
;
_cod_data_source_file            wm2658.cif
_cod_data_source_block           I
_cod_database_code               2236685
_cod_database_fobs_code          2236685
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y, z'
'x+1/2, -y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Li Li1 0.7503(4) -0.1688(4) 0.995(5) 0.0090(7) Uani d . 1
Mn Mn1 0.5 0.33172(5) 0.9968 0.00733(15) Uani d S 1
Si Si1 1 0.32090(9) 0.9851(3) 0.00350(17) Uani d S 1
O O1 0.5 0.6868(3) 1.1569(5) 0.0071(5) Uani d S 1
O O2 0.5 0.3867(3) 0.5804(4) 0.0081(4) Uani d S 1
O O3 0.7887(2) 0.1799(2) 1.0979(4) 0.0075(3) Uani d . 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Li1 0.0084(17) 0.0061(15) 0.0125(15) -0.0009(7) 0.0000(14) -0.002(2)
Mn1 0.0055(2) 0.0072(2) 0.0093(2) 0 0 0.0000(2)
Si1 0.0035(3) 0.0028(3) 0.0042(4) 0 0 -0.0003(3)
O1 0.0075(9) 0.0083(8) 0.0056(11) 0 0 -0.0004(6)
O2 0.0098(8) 0.0048(7) 0.0096(10) 0 0 0.0001(7)
O3 0.0068(5) 0.0067(6) 0.0089(7) -0.0009(4) 0.0008(7) 0.0000(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Li1 O3 1_545 . 112.0(7) y
O1 Li1 O3 1_545 2_654 107.5(5) y
O3 Li1 O3 . 2_654 107.7(7) y
O1 Li1 O2 1_545 2_655 108.6(6) y
O3 Li1 O2 . 2_655 113.9(5) y
O3 Li1 O2 2_654 2_655 106.8(6) y
O3 Mn1 O3 3_655 . 124.58(8) y
O3 Mn1 O1 3_655 . 105.74(5) y
O3 Mn1 O1 . . 105.74(5) n
O3 Mn1 O2 3_655 . 107.31(6) y
O3 Mn1 O2 . . 107.31(6) n
O1 Mn1 O2 . . 104.54(8) y
O1 Si1 O3 2_664 . 109.35(10) y
O1 Si1 O3 2_664 3_755 109.35(10) n
O3 Si1 O3 . 3_755 109.58(13) y
O1 Si1 O2 2_664 2_665 108.23(13) y
O3 Si1 O2 . 2_665 110.16(10) y
O3 Si1 O2 3_755 2_665 110.16(10) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Li1 O1 1_545 1.936(10) y
Li1 O3 . 1.956(6) y
Li1 O3 2_654 1.99(2) y
Li1 O2 2_655 2.009(6) y
Mn1 O3 3_655 2.0585(16) y
Mn1 O3 . 2.0585(15) n
Mn1 O1 . 2.065(2) y
Mn1 O2 . 2.090(2) y
Si1 O1 2_664 1.631(3) y
Si1 O3 . 1.6331(17) y
Si1 O3 3_755 1.6331(17) n
Si1 O2 2_665 1.639(2) y
