#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:49:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179349 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/46/4324652.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4324652
loop_
_publ_author_name
'Qingxin Chu'
'Xiaofeng Wang'
'Xinhao Zhang'
'Qiliang Li'
'Xiaoyang Liu'
_publ_contact_author_address
;State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, Jilin
University, Changchun, 130012, China.
;
_publ_contact_author_email       liuxy@jlu.edu.cn
_publ_contact_author_fax         +86-431-85168316
_publ_contact_author_name        'Xiaoyang Liu'
_publ_contact_author_phone       +86-431-85168316
_publ_section_title
;
 Buckled Layers in K0.66Mn2O4.0.28H2O and K0.99Mn3O6.1.25H2O Synthesized
 at High Pressure: Implication for the Mechanism of Layer-to-Tunnel
 Transformation in Manganese Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2049
_journal_page_last               2051
_journal_paper_doi               10.1021/ic102282v
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'K1.39 Mn3 O6'
_chemical_formula_weight         315.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 126.908(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.259(4)
_cell_length_b                   2.8438(7)
_cell_length_c                   9.526(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     308.87(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1814
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    6.938
_exptl_absorpt_correction_T_max  0.9661
_exptl_absorpt_correction_T_min  0.5438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS,2008
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.389
_exptl_crystal_description       flake
_exptl_crystal_F_000             299
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0692P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1155
_reflns_number_gt                395
_reflns_number_total             519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102282v_si_002_1.cif
_cod_data_source_block           II
_cod_original_cell_volume        308.86(14)
_cod_database_code               4324652
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
K1 K -0.0772(2) 0.5000 0.3373(3) 0.0438(9) Uani 0.695(7) 2 d SP
Mn1 Mn -0.17584(6) 0.5000 0.66391(9) 0.0108(3) Uani 1 2 d S
Mn2 Mn 0.0000 0.0000 0.0000 0.0118(3) Uani 1 4 d S
O1 O -0.3371(3) 0.5000 0.4618(5) 0.0108(7) Uani 1 2 d S
O2 O 0.1927(3) 0.0000 0.2238(5) 0.0114(8) Uani 1 2 d S
O3 O 0.0111(3) 0.5000 0.1446(5) 0.0115(8) Uani 1 2 d S
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'
K K 0.2009 0.2494 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Mn1 O2 98.32(17) 5_566 5_556
O2 Mn1 O1 94.88(13) 5_566 .
O2 Mn1 O1 94.88(13) 5_556 .
O2 Mn1 O3 87.76(13) 5_566 5_566
O2 Mn1 O3 87.76(13) 5_556 5_566
O1 Mn1 O3 175.95(14) . 5_566
O2 Mn1 O1 177.40(11) 5_566 7_456
O2 Mn1 O1 83.63(13) 5_556 7_456
O1 Mn1 O1 83.20(14) . 7_456
O3 Mn1 O1 94.06(13) 5_566 7_456
O2 Mn1 O1 83.63(13) 5_566 7_466
O2 Mn1 O1 177.40(11) 5_556 7_466
O1 Mn1 O1 83.20(14) . 7_466
O3 Mn1 O1 94.06(14) 5_566 7_466
O1 Mn1 O1 94.38(16) 7_456 7_466
O2 Mn1 Mn1 139.16(9) 5_566 1_545
O2 Mn1 Mn1 40.84(9) 5_556 1_545
O1 Mn1 Mn1 90.000(1) . 1_545
O3 Mn1 Mn1 90.000(1) 5_566 1_545
O1 Mn1 Mn1 42.81(8) 7_456 1_545
O1 Mn1 Mn1 137.19(8) 7_466 1_545
O2 Mn1 Mn1 40.84(9) 5_566 1_565
O2 Mn1 Mn1 139.16(9) 5_556 1_565
O1 Mn1 Mn1 90.000(1) . 1_565
O3 Mn1 Mn1 90.000(1) 5_566 1_565
O1 Mn1 Mn1 137.19(8) 7_456 1_565
O1 Mn1 Mn1 42.81(8) 7_466 1_565
Mn1 Mn1 Mn1 180.00(7) 1_545 1_565
O2 Mn1 Mn1 136.73(12) 5_566 7_456
O2 Mn1 Mn1 88.97(10) 5_556 7_456
O1 Mn1 Mn1 41.87(8) . 7_456
O3 Mn1 Mn1 135.32(9) 5_566 7_456
O1 Mn1 Mn1 41.33(11) 7_456 7_456
O1 Mn1 Mn1 88.43(10) 7_466 7_456
Mn1 Mn1 Mn1 60.454(17) 1_545 7_456
Mn1 Mn1 Mn1 119.546(17) 1_565 7_456
O2 Mn1 Mn1 88.97(10) 5_566 7_466
O2 Mn1 Mn1 136.73(12) 5_556 7_466
O1 Mn1 Mn1 41.87(8) . 7_466
O3 Mn1 Mn1 135.32(9) 5_566 7_466
O1 Mn1 Mn1 88.43(10) 7_456 7_466
O1 Mn1 Mn1 41.33(11) 7_466 7_466
Mn1 Mn1 Mn1 119.546(17) 1_545 7_466
Mn1 Mn1 Mn1 60.454(17) 1_565 7_466
Mn1 Mn1 Mn1 59.09(3) 7_456 7_466
O2 Mn1 Mn2 48.82(11) 5_566 1_566
O2 Mn1 Mn2 93.56(10) 5_556 1_566
O1 Mn1 Mn2 143.60(7) . 1_566
O3 Mn1 Mn2 38.94(7) 5_566 1_566
O1 Mn1 Mn2 132.97(11) 7_456 1_566
O1 Mn1 Mn2 89.02(10) 7_466 1_566
Mn1 Mn1 Mn2 118.435(12) 1_545 1_566
Mn1 Mn1 Mn2 61.565(12) 1_565 1_566
Mn1 Mn1 Mn2 173.45(4) 7_456 1_566
Mn1 Mn1 Mn2 121.59(2) 7_466 1_566
O2 Mn1 Mn2 93.56(10) 5_566 1_556
O2 Mn1 Mn2 48.82(11) 5_556 1_556
O1 Mn1 Mn2 143.60(7) . 1_556
O3 Mn1 Mn2 38.94(7) 5_566 1_556
O1 Mn1 Mn2 89.02(10) 7_456 1_556
O1 Mn1 Mn2 132.97(11) 7_466 1_556
Mn1 Mn1 Mn2 61.565(12) 1_545 1_556
Mn1 Mn1 Mn2 118.435(12) 1_565 1_556
Mn1 Mn1 Mn2 121.59(2) 7_456 1_556
Mn1 Mn1 Mn2 173.45(4) 7_466 1_556
Mn2 Mn1 Mn2 56.87(2) 1_566 1_556
O3 Mn2 O3 180.0(2) 5 .
O3 Mn2 O3 95.64(16) 5 5_565
O3 Mn2 O3 84.36(16) . 5_565
O3 Mn2 O3 84.36(16) 5 1_545
O3 Mn2 O3 95.64(16) . 1_545
O3 Mn2 O3 180.0(2) 5_565 1_545
O3 Mn2 O2 101.99(12) 5 .
O3 Mn2 O2 78.01(12) . .
O3 Mn2 O2 101.99(12) 5_565 .
O3 Mn2 O2 78.01(12) 1_545 .
O3 Mn2 O2 78.01(12) 5 5
O3 Mn2 O2 101.99(12) . 5
O3 Mn2 O2 78.01(12) 5_565 5
O3 Mn2 O2 101.99(12) 1_545 5
O2 Mn2 O2 180.00(18) . 5
O3 Mn2 Mn2 137.82(8) 5 1_565
O3 Mn2 Mn2 42.18(8) . 1_565
O3 Mn2 Mn2 42.18(8) 5_565 1_565
O3 Mn2 Mn2 137.82(8) 1_545 1_565
O2 Mn2 Mn2 90.0 . 1_565
O2 Mn2 Mn2 90.0 5 1_565
O3 Mn2 Mn2 42.18(8) 5 1_545
O3 Mn2 Mn2 137.82(8) . 1_545
O3 Mn2 Mn2 137.82(8) 5_565 1_545
O3 Mn2 Mn2 42.18(8) 1_545 1_545
O2 Mn2 Mn2 90.0 . 1_545
O2 Mn2 Mn2 90.0 5 1_545
Mn2 Mn2 Mn2 180.0 1_565 1_545
O3 Mn2 Mn1 140.96(11) 5 5_566
O3 Mn2 Mn1 39.04(11) . 5_566
O3 Mn2 Mn1 94.07(9) 5_565 5_566
O3 Mn2 Mn1 85.93(9) 1_545 5_566
O2 Mn2 Mn1 38.97(6) . 5_566
O2 Mn2 Mn1 141.03(6) 5 5_566
Mn2 Mn2 Mn1 61.565(12) 1_565 5_566
Mn2 Mn2 Mn1 118.435(12) 1_545 5_566
O3 Mn2 Mn1 39.04(11) 5 1_544
O3 Mn2 Mn1 140.96(11) . 1_544
O3 Mn2 Mn1 85.93(9) 5_565 1_544
O3 Mn2 Mn1 94.07(9) 1_545 1_544
O2 Mn2 Mn1 141.03(6) . 1_544
O2 Mn2 Mn1 38.97(6) 5 1_544
Mn2 Mn2 Mn1 118.435(12) 1_565 1_544
Mn2 Mn2 Mn1 61.565(12) 1_545 1_544
Mn1 Mn2 Mn1 180.00(3) 5_566 1_544
O3 Mn2 Mn1 94.07(9) 5 5_556
O3 Mn2 Mn1 85.93(9) . 5_556
O3 Mn2 Mn1 140.96(11) 5_565 5_556
O3 Mn2 Mn1 39.04(11) 1_545 5_556
O2 Mn2 Mn1 38.97(6) . 5_556
O2 Mn2 Mn1 141.03(6) 5 5_556
Mn2 Mn2 Mn1 118.435(12) 1_565 5_556
Mn2 Mn2 Mn1 61.565(12) 1_545 5_556
Mn1 Mn2 Mn1 56.87(2) 5_566 5_556
Mn1 Mn2 Mn1 123.13(2) 1_544 5_556
O3 Mn2 Mn1 85.93(9) 5 1_554
O3 Mn2 Mn1 94.07(9) . 1_554
O3 Mn2 Mn1 39.04(11) 5_565 1_554
O3 Mn2 Mn1 140.96(11) 1_545 1_554
O2 Mn2 Mn1 141.03(6) . 1_554
O2 Mn2 Mn1 38.97(6) 5 1_554
Mn2 Mn2 Mn1 61.565(12) 1_565 1_554
Mn2 Mn2 Mn1 118.435(12) 1_545 1_554
Mn1 Mn2 Mn1 123.13(2) 5_566 1_554
Mn1 Mn2 Mn1 56.87(2) 1_544 1_554
Mn1 Mn2 Mn1 180.0 5_556 1_554
Mn1 O1 Mn1 96.80(14) . 7_456
Mn1 O1 Mn1 96.80(14) . 7_466
Mn1 O1 Mn1 94.38(16) 7_456 7_466
Mn1 O2 Mn1 98.32(17) 5_566 5_556
Mn1 O2 Mn2 92.20(13) 5_566 .
Mn1 O2 Mn2 92.20(13) 5_556 .
Mn2 O3 Mn2 95.64(16) . 1_565
Mn2 O3 Mn1 102.02(13) . 5_566
Mn2 O3 Mn1 102.02(13) 1_565 5_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 K1 2.502(5) 5_566
K1 O2 2.770(5) 3_455
K1 O3 2.781(4) .
K1 K1 2.8438(7) 1_545
K1 K1 2.8438(7) 1_565
K1 O1 3.160(4) 7_466
K1 O1 3.160(4) 7_456
K1 O1 3.205(4) 3
K1 O1 3.204(4) 3_545
Mn1 O2 1.880(2) 5_566
Mn1 O2 1.880(2) 5_556
Mn1 O1 1.918(4) .
Mn1 O3 1.923(4) 5_566
Mn1 O1 1.938(3) 7_456
Mn1 O1 1.938(3) 7_466
Mn1 Mn1 2.8438(7) 1_545
Mn1 Mn1 2.8438(7) 1_565
Mn1 Mn1 2.8834(14) 7_456
Mn1 Mn1 2.8834(14) 7_466
Mn1 Mn2 2.9862(10) 1_566
Mn1 Mn2 2.9862(10) 1_556
Mn2 O3 1.919(2) 5
Mn2 O3 1.919(2) .
Mn2 O3 1.919(2) 5_565
Mn2 O3 1.919(2) 1_545
Mn2 O2 2.249(4) .
Mn2 O2 2.249(4) 5
Mn2 Mn2 2.8438(7) 1_565
Mn2 Mn2 2.8438(7) 1_545
Mn2 Mn1 2.9862(10) 5_566
Mn2 Mn1 2.9862(10) 1_544
Mn2 Mn1 2.9862(10) 5_556
Mn2 Mn1 2.9862(10) 1_554
O1 Mn1 1.938(3) 7_456
O1 Mn1 1.938(3) 7_466
O1 K1 3.160(4) 7_466
O1 K1 3.160(4) 7_456
O1 K1 3.205(4) 3_445
O1 K1 3.205(4) 3_455
O2 Mn1 1.880(2) 5_566
O2 Mn1 1.880(2) 5_556
O2 K1 2.770(5) 3_545
O3 Mn2 1.919(2) 1_565
O3 Mn1 1.923(4) 5_566
