#------------------------------------------------------------------------------
#$Date: 2016-08-26 17:04:42 +0300 (Fri, 26 Aug 2016) $
#$Revision: 186028 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/91/7119176.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_7119176
loop_
_publ_author_name
'Martin K. Dufficy'
'Lan Luo'
'Peter S. Fedkiw'
'Paul A. Maggard'
_publ_section_title
;
 Vacancy-induced manganese vanadates and their potential application to
 Li-ion batteries
;
_journal_name_full               Chem.Commun.
_journal_page_first              7509
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'Mn1.5 N O13 V4'
_chemical_formula_sum            'Mn1.5 N O13 V4'
_chemical_formula_weight         508.18
_chemical_name_systematic        H4Mn2V9O14
_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_Hall           '-P 2y'
_space_group_name_H-M_alt        'P 1 2/m 1'
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 1'
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-03 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.987(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   8.2011(2)
_cell_length_b                   3.52070(10)
_cell_length_c                   9.9129(3)
_cell_measurement_reflns_used    7989
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      74.05
_cell_measurement_theta_min      2
_cell_volume                     267.234(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Bruker
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7789
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.026
_diffrn_reflns_theta_min         2.200
_exptl_absorpt_coefficient_mu    5.154
_exptl_absorpt_correction_T_max  0.7477
_exptl_absorpt_correction_T_min  0.6266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    3.158
_exptl_crystal_description       needle
_exptl_crystal_F_000             240
_exptl_crystal_preparation       Hydrothermal
_exptl_crystal_recrystallization_method needle
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.014
_exptl_crystal_size_min          0.014
_refine_diff_density_max         1.057
_refine_diff_density_min         -1.795
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         1530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0500P)²+0.3970P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1208
_reflns_number_total             1530
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc02249a2.cif
_cod_data_source_block           x12012_0m
_cod_original_formula_sum        'Mn1.50 N O13 V4'
_cod_database_code               7119176
_shelxl_version_number           2014/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.272
_olex2_refinement_description
;
1. Shared sites
{O7, N}
2. Uiso/Uaniso restraints and constraints
Uanis(O7) = Uanis(N)
3. Others
 Fixed Sof: Mn1(0.125) O7(0.25) N(0.25)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'-x, -y, -z'
'x, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn2 Mn 1.0000 1.0000 0.5000 0.00993(15) Uani 1 4 d S T P . .
V2 V 0.24408(7) 0.5000 0.33108(6) 0.00820(12) Uani 1 2 d S T P . .
V1 V 0.54180(7) 1.0000 0.30765(6) 0.00853(12) Uani 1 2 d S T P . .
O4 O 0.5095(3) 0.5000 0.3547(3) 0.0126(4) Uani 1 2 d S T P . .
O5 O 0.7558(3) 1.0000 0.3422(3) 0.0130(4) Uani 1 2 d S T P . .
O3 O 0.3245(3) 0.0000 0.3776(3) 0.0103(4) Uani 1 2 d S T P . .
O2 O 0.0796(3) 0.5000 0.3989(3) 0.0113(4) Uani 1 2 d S T P . .
O1 O 0.1455(3) 0.5000 0.1581(3) 0.0151(5) Uani 1 2 d S T P . .
O6 O 0.4559(4) 1.0000 0.1293(3) 0.0210(6) Uani 1 2 d S T P . .
Mn1 Mn 0.5000 0.5000 0.0000 0.0165(3) Uani 0.5 4 d S T P . .
O7 O 0.7769(4) 0.5000 0.0998(4) 0.0261(7) Uani 0.5 2 d S T P . .
N N 0.7769(4) 0.5000 0.0998(4) 0.0261(7) Uani 0.5 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
V V 0.3005 0.5294 '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
O5 Mn2 O5 180.0 3_776 .
O5 Mn2 O2 88.84(8) . 3_676
O5 Mn2 O2 91.16(8) 3_776 3_676
O5 Mn2 O2 91.16(8) . 1_665
O5 Mn2 O2 91.16(8) 3_776 3_666
O5 Mn2 O2 88.84(8) 3_776 1_655
O5 Mn2 O2 88.84(8) . 3_666
O5 Mn2 O2 91.16(8) . 1_655
O5 Mn2 O2 88.84(8) 3_776 1_665
O2 Mn2 O2 103.88(9) 1_655 1_665
O2 Mn2 O2 103.88(9) 3_676 3_666
O2 Mn2 O2 76.12(9) 1_655 3_666
O2 Mn2 O2 180.0 1_665 3_666
O2 Mn2 O2 76.12(9) 3_676 1_665
O2 Mn2 O2 180.0 3_676 1_655
V1 V2 V1 69.572(16) . 1_545
O4 V2 V1 36.24(2) . .
O4 V2 V1 36.24(2) . 1_545
O3 V2 V1 42.78(7) 1_565 .
O3 V2 V1 109.59(7) . .
O3 V2 V1 42.78(7) . 1_545
O3 V2 V1 109.59(7) 1_565 1_545
O3 V2 O4 73.40(7) 1_565 .
O3 V2 O4 73.40(7) . .
O3 V2 O3 139.15(14) 1_565 .
O2 V2 V1 141.90(4) . 1_545
O2 V2 V1 141.90(4) . .
O2 V2 O4 152.49(12) . .
O2 V2 O3 99.25(8) . .
O2 V2 O3 99.25(8) . 1_565
O1 V2 V1 91.65(8) . 1_545
O1 V2 V1 91.65(8) . .
O1 V2 O4 102.88(12) . .
O1 V2 O3 105.02(8) . .
O1 V2 O3 105.02(8) . 1_565
O1 V2 O2 104.63(13) . .
V2 V1 V2 69.573(16) 1_565 .
O4 V1 V2 41.85(7) 1_565 1_565
O4 V1 V2 109.43(7) 1_565 .
O4 V1 V2 109.43(7) . 1_565
O4 V1 V2 41.86(7) . .
O4 V1 O4 141.57(15) . 1_565
O4 V1 O3 73.03(7) . 1_565
O4 V1 O3 73.03(7) 1_565 1_565
O5 V1 V2 142.14(4) . 1_565
O5 V1 V2 142.14(4) . .
O5 V1 O4 100.52(8) . 1_565
O5 V1 O4 100.52(8) . .
O5 V1 O3 151.24(12) . 1_565
O3 V1 V2 36.78(2) 1_565 .
O3 V1 V2 36.78(2) 1_565 1_565
O6 V1 V2 92.00(8) . 1_565
O6 V1 V2 92.00(8) . .
O6 V1 O4 102.91(9) . .
O6 V1 O4 102.91(9) . 1_565
O6 V1 O5 103.56(14) . .
O6 V1 O3 105.20(12) . 1_565
V1 O4 V2 101.90(8) . .
V1 O4 V2 101.90(8) 1_545 .
V1 O4 V1 141.57(15) . 1_545
V1 O5 Mn2 145.73(16) . .
V2 O3 V2 139.15(14) 1_545 .
V2 O3 V1 100.44(8) 1_545 1_545
V2 O3 V1 100.44(8) . 1_545
Mn2 O2 Mn2 103.88(9) 1_455 1_445
V2 O2 Mn2 125.08(6) . 1_455
V2 O2 Mn2 125.08(6) . 1_445
V1 O6 Mn1 120.56(8) . 1_565
V1 O6 Mn1 120.56(8) . .
Mn1 O6 Mn1 101.00(10) . 1_565
O6 Mn1 O6 101.00(10) 3_665 3_675
O6 Mn1 O6 180.0 3_665 .
O6 Mn1 O6 101.00(10) 1_545 .
O6 Mn1 O6 180.0 1_545 3_675
O6 Mn1 O6 79.00(10) 3_675 .
O6 Mn1 O6 79.00(10) 3_665 1_545
O7 Mn1 O6 95.54(9) . 1_545
O7 Mn1 O6 84.46(9) 3_665 .
O7 Mn1 O6 84.46(9) 3_665 1_545
O7 Mn1 O6 84.46(9) . 3_675
O7 Mn1 O6 95.54(9) . .
O7 Mn1 O6 95.54(9) 3_665 3_675
O7 Mn1 O6 84.46(9) . 3_665
O7 Mn1 O6 95.54(9) 3_665 3_665
O7 Mn1 O7 180.0 . 3_665
O7 Mn1 N 180.0 . 3_665
N Mn1 O6 95.54(9) 3_665 3_665
N Mn1 O6 84.46(9) 3_665 .
N Mn1 O6 84.46(9) 3_665 1_545
N Mn1 O6 95.54(9) 3_665 3_675
N Mn1 O7 0.0 3_665 3_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn2 O5 2.053(2) 3_776
Mn2 O5 2.053(2) .
Mn2 O2 2.2358(14) 1_655
Mn2 O2 2.2358(14) 1_665
Mn2 O2 2.2358(14) 3_666
Mn2 O2 2.2358(14) 3_676
V2 V1 3.0856(6) 1_545
V2 V1 3.0855(6) .
V2 O4 2.104(2) .
V2 O3 1.8784(8) .
V2 O3 1.8784(8) 1_565
V2 O2 1.709(2) .
V2 O1 1.613(3) .
V1 V2 3.0855(6) 1_565
V1 O4 1.8642(8) 1_565
V1 O4 1.8642(8) .
V1 O5 1.663(2) .
V1 O3 2.131(2) 1_565
V1 O6 1.652(3) .
O4 V1 1.8642(8) 1_545
O3 V2 1.8784(8) 1_545
O3 V1 2.131(2) 1_545
O2 Mn2 2.2358(14) 1_455
O2 Mn2 2.2358(14) 1_445
O6 Mn1 2.2813(17) .
O6 Mn1 2.2813(17) 1_565
Mn1 O6 2.2813(17) 3_665
Mn1 O6 2.2813(17) 3_675
Mn1 O6 2.2813(17) 1_545
Mn1 O7 2.127(3) 3_665
Mn1 O7 2.127(3) .
Mn1 N 2.127(3) 3_665
