# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_x12012_0m
_database_code_depnum_ccdc_archive 'CCDC 1477963'
_audit_update_record             
;
2016-05-03 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;
_audit_creation_date             2016-04-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        H4Mn2V9O14
_chemical_formula_moiety         'Mn1.5 N O13 V4'
_chemical_formula_sum            'Mn1.50 N O13 V4'
_chemical_formula_weight         508.18
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_H-M_alt        'P 1 2/m 1'
_space_group_name_Hall           '-P 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'-x, -y, -z'
'x, -y, z'

_cell_length_a                   8.2011(2)
_cell_length_b                   3.52070(10)
_cell_length_c                   9.9129(3)
_cell_angle_alpha                90
_cell_angle_beta                 110.987(2)
_cell_angle_gamma                90
_cell_volume                     267.234(13)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7989
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      74.05
_cell_measurement_theta_min      2
_shelx_estimated_absorpt_T_max   0.931
_shelx_estimated_absorpt_T_min   0.272
_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_absorpt_special_details   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Bruker
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1208
_reflns_number_total             1530
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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)'
_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_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0362
_refine_ls_restrained_S_all      1.079
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 . .


_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
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 ?

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
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 ?

_olex2_submission_special_instructions 'No special instructions were received'
