# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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. 
# 
#######################################################################

data_shelx
_audit_block_doi                 10.5517/ccdc.csd.cc1pdlwk
_database_code_depnum_ccdc_archive 'CCDC 1561249'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7CC05319C 2017
_audit_update_record             
;
2017-07-09 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Mn2MoN3
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Mn2 Mo N12 O5'
_chemical_formula_weight         562.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'y, -x, z'
'-x, -y, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'y, -x, -z'
'-y, x, -z'
'x, y, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'

_cell_length_a                   11.9694(3)
_cell_length_b                   11.9694(3)
_cell_length_c                   13.1021(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1877.09(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3958
_cell_measurement_theta_min      3.40
_cell_measurement_theta_max      28.22

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_F_000             1104
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.032
_shelx_estimated_absorpt_T_min   0.750
_shelx_estimated_absorpt_T_max   0.923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6652
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker PHOTON50 CMOS'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7342
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.404
_diffrn_reflns_theta_max         28.252
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             1220
_reflns_number_gt                1085
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0206P)²+3.9044P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1220
_refine_ls_number_parameters     93
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0476
_refine_ls_wR_factor_gt          0.0461
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mo1 Mo 0.5000 0.5000 0.74944(2) 0.00500(10) Uani 1 4 d S T P . .
Mn1 Mn 0.18837(3) 0.30822(3) 0.5000 0.00723(11) Uani 1 2 d S T P . .
O2 O 0.3921(4) 0.1152(3) 0.7066(3) 0.0195(9) Uani 0.75 1 d D . P . .
N5 N 0.404(3) 0.1179(19) 0.705(3) 0.072(10) Uani 0.25 1 d D U P . .
O1 O 0.29418(17) 0.15112(17) 0.5000 0.0193(4) Uani 1 2 d DS T P . .
N3 N 0.0829(2) 0.4530(2) 0.5000 0.0468(10) Uani 1 2 d S T P . .
C1 C 0.55033(14) 0.64146(15) 0.83937(15) 0.0105(4) Uani 1 1 d . . . . .
N1 N 0.58407(14) 0.71606(14) 0.88618(13) 0.0161(3) Uani 1 1 d . . . . .
C2 C 0.36734(14) 0.42506(14) 0.66144(15) 0.0103(3) Uani 1 1 d . . . . .
N4 N 0.0000 0.5000 0.5000 0.0142(6) Uani 1 4 d S T P . .
N2 N 0.29722(14) 0.37903(13) 0.61854(13) 0.0156(3) Uani 1 1 d . . . . .
H1B H 0.318(5) 0.140(5) 0.567(2) 0.18(3) Uiso 1 1 d D . . . .
H2A H 0.359(3) 0.166(3) 0.747(3) 0.092(15) Uiso 1 1 d D . . . .
H2B H 0.384(6) 0.043(2) 0.728(5) 0.19(3) Uiso 1 1 d D . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo1 0.00509(11) 0.00509(11) 0.00483(15) 0.000 0.000 0.000
Mn1 0.00704(18) 0.00730(18) 0.0074(2) 0.000 0.000 -0.00161(13)
O2 0.0228(13) 0.0181(14) 0.0177(15) -0.0067(9) 0.0018(10) 0.0032(9)
N5 0.074(11) 0.068(11) 0.072(11) -0.004(5) 0.003(5) 0.004(5)
O1 0.0147(10) 0.0126(9) 0.0307(13) 0.000 0.000 0.0020(7)
N3 0.0146(13) 0.0131(13) 0.113(3) 0.000 0.000 0.0054(11)
C1 0.0091(8) 0.0112(8) 0.0112(9) 0.0004(7) -0.0007(7) 0.0007(6)
N1 0.0180(8) 0.0155(8) 0.0147(9) -0.0031(6) -0.0020(7) -0.0039(6)
C2 0.0111(8) 0.0098(8) 0.0101(9) -0.0013(7) 0.0008(7) 0.0009(6)
N4 0.0168(16) 0.0096(14) 0.0163(17) 0.000 0.000 -0.0027(13)
N2 0.0148(7) 0.0176(8) 0.0143(9) -0.0029(6) -0.0008(6) -0.0026(6)

_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
Mo1 C1 2.1490(18) . ?
Mo1 C1 2.1490(18) 3_565 ?
Mo1 C1 2.1490(18) 4_665 ?
Mo1 C1 2.1490(18) 2_655 ?
Mo1 C2 2.1576(18) . ?
Mo1 C2 2.1576(18) 2_655 ?
Mo1 C2 2.1576(18) 4_665 ?
Mo1 C2 2.1576(18) 3_565 ?
Mn1 N3 2.144(3) . ?
Mn1 N2 2.1973(17) . ?
Mn1 N2 2.1974(17) 12_556 ?
Mn1 N1 2.2360(16) 5_444 ?
Mn1 N1 2.2360(16) 16_446 ?
Mn1 O1 2.267(2) . ?
O2 H2A 0.894(19) . ?
O2 H2B 0.912(19) . ?
N5 H2A 0.960(19) . ?
N5 H2B 0.977(19) . ?
O1 H1B 0.93(2) . ?
N3 N4 1.141(3) . ?
C1 N1 1.156(2) . ?
N1 Mn1 2.2360(16) 5 ?
C2 N2 1.151(2) . ?
N4 N3 1.141(3) 9_566 ?

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
C1 Mo1 C1 72.51(5) . 3_565 ?
C1 Mo1 C1 113.50(10) . 4_665 ?
C1 Mo1 C1 72.51(5) 3_565 4_665 ?
C1 Mo1 C1 72.51(5) . 2_655 ?
C1 Mo1 C1 113.50(10) 3_565 2_655 ?
C1 Mo1 C1 72.51(5) 4_665 2_655 ?
C1 Mo1 C2 145.78(6) . . ?
C1 Mo1 C2 139.14(6) 3_565 . ?
C1 Mo1 C2 76.06(7) 4_665 . ?
C1 Mo1 C2 80.19(7) 2_655 . ?
C1 Mo1 C2 139.14(6) . 2_655 ?
C1 Mo1 C2 76.06(7) 3_565 2_655 ?
C1 Mo1 C2 80.19(7) 4_665 2_655 ?
C1 Mo1 C2 145.78(6) 2_655 2_655 ?
C2 Mo1 C2 73.41(5) . 2_655 ?
C1 Mo1 C2 76.06(7) . 4_665 ?
C1 Mo1 C2 80.19(7) 3_565 4_665 ?
C1 Mo1 C2 145.78(6) 4_665 4_665 ?
C1 Mo1 C2 139.14(6) 2_655 4_665 ?
C2 Mo1 C2 115.40(10) . 4_665 ?
C2 Mo1 C2 73.41(5) 2_655 4_665 ?
C1 Mo1 C2 80.19(7) . 3_565 ?
C1 Mo1 C2 145.78(6) 3_565 3_565 ?
C1 Mo1 C2 139.14(6) 4_665 3_565 ?
C1 Mo1 C2 76.06(7) 2_655 3_565 ?
C2 Mo1 C2 73.41(5) . 3_565 ?
C2 Mo1 C2 115.40(10) 2_655 3_565 ?
C2 Mo1 C2 73.41(5) 4_665 3_565 ?
N3 Mn1 N2 92.13(7) . . ?
N3 Mn1 N2 92.13(7) . 12_556 ?
N2 Mn1 N2 89.96(9) . 12_556 ?
N3 Mn1 N1 94.02(7) . 5_444 ?
N2 Mn1 N1 173.13(6) . 5_444 ?
N2 Mn1 N1 92.86(6) 12_556 5_444 ?
N3 Mn1 N1 94.02(7) . 16_446 ?
N2 Mn1 N1 92.86(6) . 16_446 ?
N2 Mn1 N1 173.13(6) 12_556 16_446 ?
N1 Mn1 N1 83.67(9) 5_444 16_446 ?
N3 Mn1 O1 177.90(9) . . ?
N2 Mn1 O1 89.35(6) . . ?
N2 Mn1 O1 89.35(6) 12_556 . ?
N1 Mn1 O1 84.42(6) 5_444 . ?
N1 Mn1 O1 84.42(6) 16_446 . ?
H2A O2 H2B 114(5) . . ?
H2A N5 H2B 103(5) . . ?
Mn1 O1 H1B 107(4) . . ?
N4 N3 Mn1 155.6(2) . . ?
N1 C1 Mo1 175.82(16) . . ?
C1 N1 Mn1 158.42(15) . 5 ?
N2 C2 Mo1 175.51(17) . . ?
N3 N4 N3 180.0 . 9_566 ?
C2 N2 Mn1 164.26(16) . . ?


_refine_diff_density_max         0.641
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.076

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL GH084_0m_xprep_a.res in I4/m
CELL  0.71073  11.9694  11.9694  13.1021   90.000   90.000   90.000
ZERR     4.00   0.0003   0.0003   0.0004    0.000    0.000    0.000
LATT   2
SYMM  - Y,   X,   Z
SYMM    Y, - X,   Z
SYMM  - X, - Y,   Z
SFAC  C    H    N    MN   MO   O
UNIT  32 48 48 8 4 20
MERG   2
OMIT     0   4   0
OMIT     1   4   1
OMIT     1   1   4
OMIT     0   1   1
OMIT    -2   3   3
ISOR    0.001  0.005  N5
DFIX  0.950 0.020 O1 H1B
DFIX  0.950 0.020 O1 H1A
DFIX  1.500 0.020 H1B H1A
DFIX     0.950   0.020 H2A O2
DFIX     0.950   0.020 H2A N5
DFIX     0.950   0.020 H2B O2
DFIX     0.950   0.020 H2B N5
FMAP   2
PLAN   20
SIZE     0.040   0.040   0.150
ACTA
BOND   $H
CONF
LIST   6
L.S.  11
TEMP  -153.15
WGHT    0.020600    3.904400
EXTI    0.001861
FVAR       0.11126
MO1   5    0.500000    0.500000    0.749443    10.25000    0.00509    0.00509 =
         0.00483    0.00000    0.00000    0.00000
MN1   4    0.188373    0.308221    0.500000    10.50000    0.00704    0.00730 =
         0.00736    0.00000    0.00000   -0.00161
O2    6    0.392106    0.115210    0.706628    10.75000    0.02276    0.01811 =
         0.01771   -0.00667    0.00179    0.00320
N5    3    0.403955    0.117949    0.704508    10.25000    0.07404    0.06812 =
         0.07242   -0.00376    0.00339    0.00354
O1    6    0.294181    0.151122    0.500000    10.50000    0.01468    0.01257 =
         0.03067    0.00000    0.00000    0.00196
N3    3    0.082948    0.452990    0.500000    10.50000    0.01458    0.01306 =
         0.11268    0.00000    0.00000    0.00538
C1    1    0.550331    0.641462    0.839372    11.00000    0.00909    0.01119 =
         0.01117    0.00037   -0.00067    0.00068
N1    3    0.584069    0.716057    0.886177    11.00000    0.01801    0.01548 =
         0.01467   -0.00310   -0.00200   -0.00386
C2    1    0.367343    0.425062    0.661444    11.00000    0.01107    0.00984 =
         0.01009   -0.00126    0.00078    0.00087
N4    3    0.000000    0.500000    0.500000    10.25000    0.01679    0.00955 =
         0.01631    0.00000    0.00000   -0.00273
N2    3    0.297225    0.379034    0.618543    11.00000    0.01480    0.01764 =
         0.01428   -0.00288   -0.00083   -0.00259
H1B   2    0.317766    0.139799    0.566942    11.00000    0.17937
H2A   2    0.359432    0.165948    0.746821    11.00000    0.09161
H2B   2    0.383625    0.043174    0.727830    11.00000    0.18593
HKLF    4  1.0  1.00  0.00  0.00  0.00  1.00  0.00  0.00  0.00  1.00

REM  GH084_0m_xprep_a.res in I4/m
REM R1 =  0.0208 for    1085 Fo > 4sig(Fo)  and  0.0259 for all    1220 data
REM     93 parameters refined using     11 restraints

END

WGHT      0.0206      3.9093

REM Highest difference peak  0.641,  deepest hole -0.430,  1-sigma level  0.076
Q1    1   0.2608  0.0892  0.5000  10.50000  0.05    0.64
Q2    1   0.5000  0.5000  0.6886  10.25000  0.05    0.51
Q3    1   0.5000  0.5000  0.8089  10.25000  0.05    0.50
Q4    1   0.0657  0.4434  0.5369  11.00000  0.05    0.37
Q5    1   0.4652  0.1111  0.7248  11.00000  0.05    0.34
Q6    1   0.4345  0.4444  0.6839  11.00000  0.05    0.34
Q7    1   0.5894  0.6772  1.0000  10.50000  0.05    0.31
Q8    1   0.5409  0.5860  0.7871  11.00000  0.05    0.31
Q9    1   0.3964  0.1480  0.6431  11.00000  0.05    0.30
Q10   1   0.2108  0.3685  0.5000  10.50000  0.05    0.30
Q11   1   0.1735  0.5012  0.5000  10.50000  0.05    0.28
Q12   1   0.1306  0.3266  0.5000  10.50000  0.05    0.27
Q13   1   0.5000  0.5000  0.8781  10.25000  0.05    0.25
Q14   1   0.5000  0.5000  0.5000  10.12500  0.05    0.25
Q15   1   0.3234  0.3246  0.5000  10.50000  0.05    0.24
Q16   1   0.3268  0.1633  0.5521  11.00000  0.05    0.24
Q17   1   0.2540  0.3041  0.5169  11.00000  0.05    0.23
Q18   1   0.3927  0.4980  0.6683  11.00000  0.05    0.23
Q19   1   0.1779  0.2951  0.5600  11.00000  0.05    0.23
Q20   1   0.2456  0.4962  0.6920  11.00000  0.05    0.22
;
_shelx_res_checksum              37780

_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# 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. 
# 
#######################################################################

data_shelx_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc1pdlxl
_database_code_depnum_ccdc_archive 'CCDC 1561250'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C7CC05319C 2017
_audit_update_record             
;
2017-07-09 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Mn2NbN3
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H12 Mn2 N12 Nb O5'
_chemical_formula_weight         559.09

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'y, -x, z'
'-x, -y, z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'y, -x, -z'
'-y, x, -z'
'x, y, -z'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'

_cell_length_a                   12.0837(3)
_cell_length_b                   12.0837(3)
_cell_length_c                   13.3147(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1944.16(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    6965
_cell_measurement_theta_min      3.372
_cell_measurement_theta_max      27.63

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    1.907
_shelx_estimated_absorpt_T_min   0.555
_shelx_estimated_absorpt_T_max   0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5580
_exptl_absorpt_correction_T_max  0.8190
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'PHOTON50 CMOS'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9460
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.372
_diffrn_reflns_theta_max         27.632
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1188
_reflns_number_gt                1133
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+19.7916P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1188
_refine_ls_number_parameters     94
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0731
_refine_ls_wR_factor_gt          0.0723
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.241
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
Nb1 Nb 0.5000 0.5000 0.75123(4) 0.00800(13) Uani 1 4 d S T P . .
O1 O 0.3409(4) 0.2086(3) 0.5000 0.0355(9) Uani 1 2 d DS T P . .
Mn1 Mn 0.18617(6) 0.31776(6) 0.5000 0.01892(18) Uani 1 2 d S T P . .
N2 N 0.1162(3) 0.2100(3) 0.3834(2) 0.0291(7) Uani 1 1 d . . . . .
N1 N 0.2790(2) 0.4171(2) 0.6130(2) 0.0228(6) Uani 1 1 d . . . . .
N3 N 0.0462(5) 0.4227(6) 0.5000 0.072(2) Uani 1 2 d S T P . .
O2 O 0.3868(7) 0.1057(6) 0.2952(4) 0.0399(17) Uani 0.75 1 d D . P . .
N5 N 0.367(4) 0.107(5) 0.290(3) 0.12(2) Uani 0.25 1 d D . P . .
C2 C 0.0744(3) 0.1399(3) 0.3395(2) 0.0173(6) Uani 1 1 d . . . . .
C1 C 0.3522(3) 0.4483(2) 0.6601(2) 0.0156(6) Uani 1 1 d . . . . .
N4 N 0.0000 0.5000 0.5000 0.0320(15) Uani 1 4 d S T P . .
H1 H 0.345(12) 0.1293(7) 0.5000 0.27(10) Uiso 1 2 d DS . P . .
H2 H 0.411(5) 0.244(10) 0.5000 0.19(7) Uiso 1 2 d DS . P . .
H4 H 0.40(2) 0.16(3) 0.25(2) 1.2(7) Uiso 1 1 d D . . . .
H3 H 0.360(11) 0.131(14) 0.358(5) 0.30(9) Uiso 1 1 d D . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.00824(16) 0.00824(16) 0.0075(2) 0.000 0.000 0.000
O1 0.038(2) 0.024(2) 0.044(2) 0.000 0.000 0.0001(17)
Mn1 0.0243(4) 0.0236(4) 0.0088(3) 0.000 0.000 -0.0164(3)
N2 0.0401(18) 0.0274(16) 0.0197(15) -0.0013(13) -0.0054(13) -0.0156(14)
N1 0.0227(14) 0.0273(15) 0.0184(14) -0.0038(12) -0.0036(11) -0.0068(12)
N3 0.029(3) 0.057(4) 0.130(7) 0.000 0.000 0.003(3)
O2 0.039(4) 0.042(3) 0.038(3) 0.011(3) -0.019(3) -0.004(2)
N5 0.047(19) 0.17(4) 0.14(4) -0.08(3) 0.03(2) -0.04(2)
C2 0.0198(15) 0.0189(15) 0.0133(14) 0.0010(12) -0.0024(12) -0.0033(12)
C1 0.0167(14) 0.0169(14) 0.0133(14) -0.0028(11) 0.0007(12) -0.0017(11)
N4 0.039(4) 0.040(4) 0.017(3) 0.000 0.000 -0.026(4)

_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
Nb1 C2 2.247(3) 5 ?
Nb1 C2 2.247(3) 7 ?
Nb1 C2 2.247(3) 8 ?
Nb1 C2 2.247(3) 6 ?
Nb1 C1 2.247(3) 2_655 ?
Nb1 C1 2.247(3) 4_665 ?
Nb1 C1 2.247(3) 3_565 ?
Nb1 C1 2.247(3) . ?
O1 Mn1 2.288(4) . ?
O1 H1 0.960(5) . ?
O1 H2 0.950(5) . ?
Mn1 N3 2.115(7) . ?
Mn1 N2 2.195(3) . ?
Mn1 N2 2.195(3) 12_556 ?
Mn1 N1 2.228(3) . ?
Mn1 N1 2.228(3) 12_556 ?
N2 C2 1.147(4) . ?
N1 C1 1.148(4) . ?
N3 N4 1.088(7) . ?
O2 H4 0.951(15) . ?
O2 H3 0.948(15) . ?
N5 H4 0.949(15) . ?
N5 H3 0.95(2) . ?
C2 Nb1 2.247(3) 5_444 ?
N4 N3 1.088(7) 9_566 ?

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
C2 Nb1 C2 74.14(8) 5 7 ?
C2 Nb1 C2 116.96(16) 5 8 ?
C2 Nb1 C2 74.14(8) 7 8 ?
C2 Nb1 C2 74.14(8) 5 6 ?
C2 Nb1 C2 116.96(16) 7 6 ?
C2 Nb1 C2 74.14(8) 8 6 ?
C2 Nb1 C1 140.25(11) 5 2_655 ?
C2 Nb1 C1 75.80(11) 7 2_655 ?
C2 Nb1 C1 78.19(11) 8 2_655 ?
C2 Nb1 C1 144.05(11) 6 2_655 ?
C2 Nb1 C1 75.80(11) 5 4_665 ?
C2 Nb1 C1 78.19(11) 7 4_665 ?
C2 Nb1 C1 144.05(11) 8 4_665 ?
C2 Nb1 C1 140.25(11) 6 4_665 ?
C1 Nb1 C1 73.07(8) 2_655 4_665 ?
C2 Nb1 C1 78.19(11) 5 3_565 ?
C2 Nb1 C1 144.05(11) 7 3_565 ?
C2 Nb1 C1 140.25(11) 8 3_565 ?
C2 Nb1 C1 75.80(11) 6 3_565 ?
C1 Nb1 C1 114.68(16) 2_655 3_565 ?
C1 Nb1 C1 73.07(8) 4_665 3_565 ?
C2 Nb1 C1 144.05(11) 5 . ?
C2 Nb1 C1 140.25(11) 7 . ?
C2 Nb1 C1 75.80(11) 8 . ?
C2 Nb1 C1 78.19(11) 6 . ?
C1 Nb1 C1 73.07(8) 2_655 . ?
C1 Nb1 C1 114.68(16) 4_665 . ?
C1 Nb1 C1 73.07(8) 3_565 . ?
Mn1 O1 H1 128(8) . . ?
Mn1 O1 H2 118(8) . . ?
H1 O1 H2 114(4) . . ?
N3 Mn1 N2 92.73(17) . . ?
N3 Mn1 N2 92.73(17) . 12_556 ?
N2 Mn1 N2 90.02(16) . 12_556 ?
N3 Mn1 N1 94.59(17) . . ?
N2 Mn1 N1 172.29(13) . . ?
N2 Mn1 N1 92.04(11) 12_556 . ?
N3 Mn1 N1 94.59(17) . 12_556 ?
N2 Mn1 N1 92.04(11) . 12_556 ?
N2 Mn1 N1 172.29(13) 12_556 12_556 ?
N1 Mn1 N1 84.97(15) . 12_556 ?
N3 Mn1 O1 178.3(2) . . ?
N2 Mn1 O1 88.45(12) . . ?
N2 Mn1 O1 88.45(12) 12_556 . ?
N1 Mn1 O1 84.18(11) . . ?
N1 Mn1 O1 84.18(11) 12_556 . ?
C2 N2 Mn1 165.6(3) . . ?
C1 N1 Mn1 159.1(3) . . ?
N4 N3 Mn1 157.7(5) . . ?
H4 O2 H3 115(10) . . ?
H4 N5 H3 114(10) . . ?
N2 C2 Nb1 177.5(3) . 5_444 ?
N1 C1 Nb1 176.7(3) . . ?
N3 N4 N3 180.0 . 9_566 ?


_refine_diff_density_max         1.867
_refine_diff_density_min         -1.824
_refine_diff_density_rms         0.105

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL GH071A_4_xprep_a.res in I4/m
CELL  0.71073  12.0837  12.0837  13.3147   90.000   90.000   90.000
ZERR     4.00   0.0003   0.0003   0.0003    0.000    0.000    0.000
LATT   2
SYMM  - Y,   X,   Z
SYMM    Y, - X,   Z
SYMM  - X, - Y,   Z
SFAC  C    H    N    MN   NB   O
UNIT  32 48 48 8 4 20
MERG   2
OMIT     1   1   0
OMIT     0   0   2
OMIT     1   1   2
DFIX     0.950   0.005 O1 H1
DFIX     0.950   0.005 H2 O1
DANG     1.600   0.040 H1 O1 H1 H2
DFIX     0.950   0.020 O2 H3
DFIX     0.950   0.020 O2 H4
DFIX  0.950 0.020 N5 H4
DFIX     0.950   0.020 N5 H3
DFIX     0.950   0.020 O2 H3
DFIX     0.950   0.020 O2 H4
DFIX     0.950   0.020 N5 H4
FMAP   2
PLAN   20
SIZE     0.110   0.120   0.350
ACTA
BOND   $H
CONF
LIST   4
L.S.  31
TEMP  -103.25
WGHT    0.000000   19.791601
FVAR       0.10559
NB1   5    0.500000    0.500000    0.751229    10.25000    0.00824    0.00824 =
         0.00754    0.00000    0.00000    0.00000
O1    6    0.340936    0.208645    0.500000    10.50000    0.03820    0.02409 =
         0.04436    0.00000    0.00000    0.00013
MN1   4    0.186170    0.317763    0.500000    10.50000    0.02429    0.02364 =
         0.00883    0.00000    0.00000   -0.01636
N2    3    0.116225    0.210037    0.383394    11.00000    0.04014    0.02744 =
         0.01975   -0.00134   -0.00538   -0.01560
N1    3    0.279045    0.417050    0.613007    11.00000    0.02274    0.02731 =
         0.01842   -0.00383   -0.00363   -0.00681
N3    3    0.046155    0.422729    0.500000    10.50000    0.02864    0.05665 =
         0.12981    0.00000    0.00000    0.00251
O2    6    0.386819    0.105713    0.295212    10.75000    0.03928    0.04204 =
         0.03843    0.01055   -0.01891   -0.00375
N5    3    0.367177    0.107070    0.290156    10.25000    0.04682    0.17191 =
         0.14393   -0.07722    0.03029   -0.04375
C2    1    0.074444    0.139939    0.339455    11.00000    0.01979    0.01885 =
         0.01326    0.00102   -0.00240   -0.00333
C1    1    0.352201    0.448289    0.660141    11.00000    0.01669    0.01692 =
         0.01329   -0.00277    0.00073   -0.00170
N4    3    0.000000    0.500000    0.500000    10.25000    0.03926    0.03964 =
         0.01699    0.00000    0.00000   -0.02624
H1    2    0.344662    0.129292    0.500000    10.50000    0.27140
H2    2    0.411300    0.243701    0.500000    10.50000    0.18726
H4    2    0.395059    0.161794    0.245686    11.00000    1.23784
H3    2    0.359956    0.131055    0.358067    11.00000    0.30009
HKLF    4  1.0  1.00  0.00  0.00  0.00  1.00  0.00  0.00  0.00  1.00

REM  GH071A_4_xprep_a.res in I4/m
REM R1 =  0.0344 for    1133 Fo > 4sig(Fo)  and  0.0363 for all    1188 data
REM     94 parameters refined using     11 restraints

END

WGHT      0.0000     19.7921

REM Highest difference peak  1.867,  deepest hole -1.824,  1-sigma level  0.105
Q1    1   0.1475  0.3579  0.5000  10.50000  0.05    1.87
Q2    1   0.1721  0.2934  0.5000  10.50000  0.05    0.55
Q3    1   0.2100  0.3259  0.5000  10.50000  0.05    0.53
Q4    1   0.2663  0.1655  0.5000  10.50000  0.05    0.39
Q5    1   0.2774  0.2584  0.5000  10.50000  0.05    0.38
Q6    1   0.1331  0.4621  0.5000  10.50000  0.05    0.32
Q7    1   0.0704  0.4849  0.5000  10.50000  0.05    0.32
Q8    1   0.0597  0.2221  0.3794  11.00000  0.05    0.31
Q9    1   0.0203  0.1909  0.5000  10.50000  0.05    0.30
Q10   1   0.0424  0.1053  0.2849  11.00000  0.05    0.30
Q11   1   0.0750  0.4099  0.4612  11.00000  0.05    0.29
Q12   1   0.3472  0.1601  0.5529  11.00000  0.05    0.29
Q13   1   0.0673  0.2409  0.3823  11.00000  0.05    0.27
Q14   1   0.1171  0.5032  0.5300  11.00000  0.05    0.27
Q15   1   0.1017  0.4231  0.4660  11.00000  0.05    0.27
Q16   1   0.4413  0.1276  0.3230  11.00000  0.05    0.25
Q17   1   0.1146  0.1570  0.3829  11.00000  0.05    0.25
Q18   1   0.0222  0.3358  0.5000  10.50000  0.05    0.25
Q19   1   0.1189  0.1815  0.3311  11.00000  0.05    0.25
Q20   1   0.0631  0.0755  0.3065  11.00000  0.05    0.25
;
_shelx_res_checksum              48350

_exptl_crystal_preparation       ', Magnetic properties'
####################################################################### 
# 
# 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. 
# 
#######################################################################

data_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1835757'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT215_shelx               
;
PROBLEM: Disordered N10       has ADP max/min Ratio .....        5.0 Note
RESPONSE: The disordered N10 is the ammonium cation, with low occupancy.
;
# Added during the CSD deposition process: Sunday 08 April 2018 11:48 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Mn2NbCN
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 Mn4 N22 Nb2 O6'
_chemical_formula_weight         1025.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, -z+1/2'
'-x, -y, z'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'y, -x, z'
'-y, x, z'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'-x, y, z-1/2'
'x, y, -z'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'-y, x, -z'
'y, -x, -z'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, z'

_cell_length_a                   11.83052(9)
_cell_length_b                   11.83052(9)
_cell_length_c                   13.53251(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1894.03(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6874
_cell_measurement_theta_min      3.4370
_cell_measurement_theta_max      28.4300

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_F_000             984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.940
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_process_details   CrysAlisPro
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12366
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.010
_diffrn_reflns_theta_max         28.589
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             668
_reflns_number_gt                610
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0166P)²+8.2356P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         668
_refine_ls_number_parameters     54
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0241
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0561
_refine_ls_wR_factor_gt          0.0539
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_restrained_S_all      1.180
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Nb Nb 0.0000 0.0000 0.2500 0.00685(13) Uani 1 8 d S T P . .
Mn Mn -0.33174(4) 0.16826(4) 0.0000 0.00820(15) Uani 1 4 d S T P . .
N1 N -0.22611(16) 0.08555(17) 0.11467(14) 0.0204(4) Uani 1 1 d . . . . .
O1 O -0.189(2) 0.311(2) 0.0000 0.052(9) Uani 0.5 4 d S TU P . .
N10 N -0.198(3) 0.302(3) 0.0000 0.030(5) Uani 0.5 4 d S TU P . .
C1 C -0.14944(18) 0.05792(17) 0.16094(15) 0.0140(4) Uani 1 1 d . . . . .
C2 C -0.468(9) 0.032(9) 0.0000 0.019(11) Uani 0.5 4 d S TU P . .
N2 N -0.464(7) 0.036(7) 0.0000 0.012(9) Uani 0.5 4 d S TU P . .
O2 O -0.1165(6) 0.3835(6) -0.1979(7) 0.075(3) Uani 0.5 2 d S TU P A 1
N4 N -0.0540(14) 0.4460(14) -0.2342(17) 0.089(8) Uani 0.25 2 d S T P B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb 0.00717(16) 0.00717(16) 0.0062(2) 0.000 0.000 0.000
Mn 0.00784(19) 0.00784(19) 0.0089(3) 0.000 0.000 0.0006(2)
N1 0.0178(9) 0.0250(10) 0.0184(9) 0.0009(8) -0.0041(8) 0.0049(7)
O1 0.051(10) 0.051(10) 0.054(10) 0.000 0.000 -0.032(7)
N10 0.026(5) 0.026(5) 0.038(9) 0.000 0.000 -0.024(6)
C1 0.0154(10) 0.0138(10) 0.0127(9) 0.0004(8) -0.0004(8) -0.0007(7)
C2 0.018(12) 0.018(12) 0.021(14) 0.000 0.000 0.002(8)
N2 0.011(9) 0.011(9) 0.015(11) 0.000 0.000 0.002(7)
O2 0.077(3) 0.077(3) 0.072(5) -0.025(4) -0.025(4) 0.028(4)
N4 0.109(13) 0.109(13) 0.048(14) -0.012(11) -0.012(11) -0.004(13)

_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
Nb C1 2.247(2) 7 ?
Nb C1 2.247(2) 4 ?
Nb C1 2.247(2) 8 ?
Nb C1 2.247(2) 6 ?
Nb C1 2.247(2) 2 ?
Nb C1 2.247(2) 3 ?
Nb C1 2.247(2) 5 ?
Nb C1 2.247(2) . ?
Mn N10 2.23(4) . ?
Mn N2 2.21(11) . ?
Mn N1 2.2197(19) 32_455 ?
Mn N1 2.2197(19) 13_454 ?
Mn N1 2.2197(19) 19 ?
Mn N1 2.2197(19) . ?
Mn C2 2.27(15) . ?
Mn O1 2.38(4) . ?
N1 C1 1.150(3) . ?
C2 C2 1.1(3) 17_455 ?
C2 N2 1.15(4) 17_455 ?
N2 C2 1.15(4) 17_455 ?
N2 N2 1.2(2) 17_455 ?
N4 N4 1.35(4) 4_554 ?
N4 N4 1.35(4) 2_564 ?
N4 N4 1.81(5) 3_565 ?

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
C1 Nb C1 140.16(10) 7 4 ?
C1 Nb C1 144.48(10) 7 8 ?
C1 Nb C1 73.28(5) 4 8 ?
C1 Nb C1 115.12(11) 7 6 ?
C1 Nb C1 78.91(11) 4 6 ?
C1 Nb C1 76.21(11) 8 6 ?
C1 Nb C1 78.91(11) 7 2 ?
C1 Nb C1 115.12(11) 4 2 ?
C1 Nb C1 73.28(5) 8 2 ?
C1 Nb C1 140.16(10) 6 2 ?
C1 Nb C1 73.28(5) 7 3 ?
C1 Nb C1 76.21(11) 4 3 ?
C1 Nb C1 140.16(10) 8 3 ?
C1 Nb C1 73.28(5) 6 3 ?
C1 Nb C1 144.48(10) 2 3 ?
C1 Nb C1 76.21(11) 7 5 ?
C1 Nb C1 73.28(5) 4 5 ?
C1 Nb C1 115.12(11) 8 5 ?
C1 Nb C1 144.48(10) 6 5 ?
C1 Nb C1 73.28(5) 2 5 ?
C1 Nb C1 78.91(11) 3 5 ?
C1 Nb C1 73.27(5) 7 . ?
C1 Nb C1 144.48(10) 4 . ?
C1 Nb C1 78.91(11) 8 . ?
C1 Nb C1 73.28(5) 6 . ?
C1 Nb C1 76.21(11) 2 . ?
C1 Nb C1 115.12(11) 3 . ?
C1 Nb C1 140.16(10) 5 . ?
N10 Mn N2 180.0 . . ?
N10 Mn N1 85.05(5) . 32_455 ?
N2 Mn N1 94.95(5) . 32_455 ?
N10 Mn N1 85.05(5) . 13_454 ?
N2 Mn N1 94.95(5) . 13_454 ?
N1 Mn N1 88.71(10) 32_455 13_454 ?
N10 Mn N1 85.05(5) . 19 ?
N2 Mn N1 94.95(5) . 19 ?
N1 Mn N1 170.09(11) 32_455 19 ?
N1 Mn N1 90.44(10) 13_454 19 ?
N10 Mn N1 85.05(5) . . ?
N2 Mn N1 94.95(5) . . ?
N1 Mn N1 90.44(10) 32_455 . ?
N1 Mn N1 170.09(11) 13_454 . ?
N1 Mn N1 88.71(10) 19 . ?
N10 Mn C2 180.0 . . ?
N2 Mn C2 0.000(1) . . ?
N1 Mn C2 94.95(5) 32_455 . ?
N1 Mn C2 94.95(5) 13_454 . ?
N1 Mn C2 94.95(5) 19 . ?
N1 Mn C2 94.95(5) . . ?
N10 Mn O1 0.0 . . ?
N2 Mn O1 180.0 . . ?
N1 Mn O1 85.05(5) 32_455 . ?
N1 Mn O1 85.05(5) 13_454 . ?
N1 Mn O1 85.05(5) 19 . ?
N1 Mn O1 85.05(5) . . ?
C2 Mn O1 180(4) . . ?
C1 N1 Mn 161.86(18) . . ?
N1 C1 Nb 178.72(19) . . ?
C2 C2 N2 0.000(8) 17_455 17_455 ?
C2 C2 Mn 180.00(2) 17_455 . ?
N2 C2 Mn 180(6) 17_455 . ?
C2 N2 N2 0.000(4) 17_455 17_455 ?
C2 N2 Mn 180.0(13) 17_455 . ?
N2 N2 Mn 180.000(13) 17_455 . ?
N4 N4 N4 84.2(11) 4_554 2_564 ?
N4 N4 N4 47.9(6) 4_554 3_565 ?
N4 N4 N4 47.9(6) 2_564 3_565 ?

_refine_diff_density_max         0.496
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.079

_shelx_res_file                  
;

    shelx.res created by SHELXL-2014/7

TITL dp_g001_120
CELL  0.71073  11.8310  11.8310  13.5330   90.000   90.000   90.000
ZERR     2.00   0.0050   0.0050   0.0050    0.005    0.005    0.005
LATT   2
SYMM    X, - Y, 1/2 - Z
SYMM  - X, - Y,   Z
SYMM  - X,   Y, 1/2 - Z
SYMM    Y,   X, 1/2 - Z
SYMM    Y, - X,   Z
SYMM  - Y,   X,   Z
SYMM  - Y, - X, 1/2 - Z
SFAC  C    N    O    MN   NB
UNIT  36 44 12 8 4
MERG   2
ISOR  0.01 0.20 C2
ISOR  0.01 0.20 N2
ISOR  0.001 0.01 O2
ISOR  0.001 0.01 O1 N10
FMAP   2
PLAN   20
ACTA
L.S.  27
WGHT    0.016600    8.235600
FVAR       1.49000   2.45438
NB    5    0.000000    0.000000    0.250000    10.12500    0.00717    0.00717 =
         0.00621    0.00000    0.00000    0.00000
MN    4   -0.331740    0.168260    0.000000    10.25000    0.00784    0.00784 =
         0.00893    0.00000    0.00000    0.00064
N1    2   -0.226114    0.085549    0.114665    11.00000    0.01783    0.02501 =
         0.01841    0.00089   -0.00409    0.00487
O1    3   -0.189195    0.310805    0.000000    10.12500    0.05082    0.05082 =
         0.05389    0.00000    0.00000   -0.03180
N10   2   -0.198425    0.301575    0.000000    10.12500    0.02650    0.02650 =
         0.03812    0.00000    0.00000   -0.02412
C1    1   -0.149440    0.057924    0.160938    11.00000    0.01545    0.01380 =
         0.01272    0.00037   -0.00038   -0.00072
C2    1   -0.467537    0.032463    0.000000    10.12500    0.01781    0.01781 =
         0.02059    0.00000    0.00000    0.00164
N2    2   -0.464015    0.035985    0.000000    10.12500    0.01099    0.01099 =
         0.01525    0.00000    0.00000    0.00168
PART    1
O2    3   -0.116458    0.383542   -0.197916    10.25000    0.07698    0.07698 =
         0.07168   -0.02484   -0.02484    0.02781
PART    2
N4    2   -0.053994    0.446006   -0.234165    10.12500    0.10882    0.10882 =
         0.04847   -0.01202   -0.01202   -0.00390
HKLF    4

REM  dp_g001_120
REM R1 =  0.0199 for     610 Fo > 4sig(Fo)  and  0.0241 for all     668 data
REM     54 parameters refined using     30 restraints

END

WGHT      0.0171      8.3236

REM Highest difference peak  0.496,  deepest hole -0.481,  1-sigma level  0.079
Q1    1  -0.1320  0.2697  0.0000  10.50000  0.05    0.50
Q2    1  -0.2086  0.2914 -0.0412  10.50000  0.05    0.39
Q3    1  -0.1940  0.3603 -0.0524  11.00000  0.05    0.37
Q4    1  -0.1452  0.3283 -0.0562  11.00000  0.05    0.35
Q5    1  -0.4377  0.0901  0.0000  10.50000  0.05    0.30
Q6    1  -0.0797  0.0383  0.1863  11.00000  0.05    0.26
Q7    1  -0.1271  0.3729  0.0000  10.25000  0.05    0.24
Q8    1  -0.1478  0.3522 -0.1200  10.50000  0.05    0.23
Q9    1  -0.2706  0.0844  0.1155  11.00000  0.05    0.23
Q10   1  -0.1830  0.4433 -0.1991  11.00000  0.05    0.23
Q11   1  -0.3334  0.1666 -0.0312  10.50000  0.05    0.23
Q12   1  -0.1634  0.0776  0.1001  11.00000  0.05    0.22
Q13   1   0.0000  0.0000  0.1767  10.25000  0.05    0.22
Q14   1  -0.0793  0.4207 -0.2203  10.50000  0.05    0.21
Q15   1  -0.1140  0.3285 -0.2621  11.00000  0.05    0.21
Q16   1  -0.3287  0.1337  0.0000  10.50000  0.05    0.21
Q17   1  -0.4428  0.0259 -0.0305  11.00000  0.05    0.20
Q18   1   0.0000  0.0000  0.1044  10.25000  0.05    0.20
Q19   1  -0.2119  0.0860  0.1434  11.00000  0.05    0.19
Q20   1  -0.3004  0.1996  0.0000  10.25000  0.05    0.19
;
_shelx_res_checksum              28199

_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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. 
# 
#######################################################################

data_dp_dpp083
_database_code_depnum_ccdc_archive 'CCDC 1835756'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT306_dp_dpp083           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O2 Check
RESPONSE: The isolated oxygen atom is the crystallization water molecule. H-atoms could not be located.
;
# Added during the CSD deposition process: Sunday 08 April 2018 11:48 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Mn2Nbformate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H2 Mn4 N18 Nb2 O14'
_chemical_formula_weight         1099.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           108
_space_group_name_H-M_alt        'I 4 c m'
_space_group_name_Hall           'I 4 -2c'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, z+1/2'
'x, -y, z+1/2'
'y, x, z+1/2'
'-y, -x, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
'y+1/2, x+1/2, z+1'
'-y+1/2, -x+1/2, z+1'

_cell_length_a                   12.07320(10)
_cell_length_b                   12.07320(10)
_cell_length_c                   13.4352(3)
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 90.000(3)
_cell_angle_gamma                90.000(3)
_cell_volume                     1958.34(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6820
_cell_measurement_theta_min      3.0263
_cell_measurement_theta_max      28.6048

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_F_000             1060
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.895
_shelx_estimated_absorpt_T_min   0.833
_shelx_estimated_absorpt_T_max   0.911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   'Crysalis package'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12755
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.375
_diffrn_reflns_theta_max         28.288
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1265
_reflns_number_gt                1157
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.912
_reflns_Friedel_fraction_max     0.994
_reflns_Friedel_fraction_full    0.998

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0483P)²+2.2677P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1265
_refine_ls_number_parameters     81
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0296
_refine_ls_wR_factor_ref         0.0793
_refine_ls_wR_factor_gt          0.0756
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Nb Nb 0.5000 0.5000 0.12424(8) 0.01350(19) Uani 1 4 d S T P . .
Mn Mn 0.18312(5) 0.31688(5) -0.12802(13) 0.0217(2) Uani 1 2 d S T P . .
C1 C 0.3587(6) 0.4315(8) 0.0334(5) 0.0274(18) Uani 1 1 d . . . . .
N1 N 0.2899(6) 0.3934(6) -0.0129(6) 0.047(2) Uani 1 1 d . . . . .
C11 C 0.0000 0.5000 -0.1362(15) 0.046(4) Uani 1 4 d S T P . .
H11 H 0.0000 0.5000 -0.2054 0.055 Uiso 1 4 calc R U P . .
O2 O 0.6109(10) 0.1109(10) 0.1629(10) 0.097(5) Uani 1 2 d S T P . .
O12 O 0.0628(4) 0.4372(4) -0.0997(6) 0.064(2) Uani 1 2 d S T P . .
O1 O 0.3151(4) 0.1849(4) -0.1418(11) 0.086(4) Uani 1 2 d S T P . .
N2 N 0.4105(6) 0.2794(5) 0.2586(5) 0.0378(14) Uani 1 1 d . . . . .
C2 C 0.4433(7) 0.3521(6) 0.2127(6) 0.0260(16) Uani 1 1 d . . . . .
N11 N 0.3853(14) 0.1147(14) 0.062(4) 0.046(6) Uani 0.5 2 d S T P A 1
O11 O 0.387(3) 0.113(3) 0.078(4) 0.109(16) Uani 0.5 2 d S T P B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb 0.0135(2) 0.0135(2) 0.0136(3) 0.000 0.000 0.000
Mn 0.0232(3) 0.0232(3) 0.0188(4) 0.0011(6) -0.0011(6) -0.0089(3)
C1 0.029(4) 0.029(3) 0.024(4) -0.002(3) -0.004(3) -0.002(3)
N1 0.044(4) 0.057(4) 0.041(4) -0.004(3) -0.013(3) -0.021(3)
C11 0.050(4) 0.050(4) 0.037(9) 0.000 0.000 -0.019(5)
O2 0.089(6) 0.089(6) 0.114(14) 0.013(6) 0.013(6) 0.022(7)
O12 0.059(2) 0.059(2) 0.076(6) -0.009(2) 0.009(2) 0.023(4)
O1 0.095(4) 0.095(4) 0.067(9) 0.004(3) -0.004(3) 0.065(5)
N2 0.053(4) 0.032(3) 0.029(3) 0.005(2) 0.006(2) -0.012(3)
C2 0.031(4) 0.021(4) 0.026(3) -0.001(3) 0.007(3) -0.006(3)
N11 0.040(8) 0.040(8) 0.057(16) -0.010(6) 0.010(6) 0.014(10)
O11 0.14(2) 0.14(2) 0.06(2) -0.028(13) 0.028(13) -0.01(2)

_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
Nb C2 2.251(7) . ?
Nb C2 2.251(7) 2_665 ?
Nb C2 2.251(7) 3_655 ?
Nb C2 2.251(7) 4_565 ?
Nb C1 2.254(8) . ?
Nb C1 2.254(8) 3_655 ?
Nb C1 2.254(8) 2_665 ?
Nb C1 2.254(8) 4_565 ?
Mn O12 2.090(6) . ?
Mn N1 2.215(7) . ?
Mn N1 2.215(7) 16_554 ?
Mn N2 2.225(7) 10_554 ?
Mn N2 2.225(7) 7_554 ?
Mn O1 2.261(7) . ?
C1 N1 1.136(9) . ?
C11 O12 1.179(11) 2_565 ?
C11 O12 1.179(11) . ?
N2 C2 1.144(8) . ?
N2 Mn 2.225(7) 10 ?

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
C2 Nb C2 116.3(4) . 2_665 ?
C2 Nb C2 73.83(19) . 3_655 ?
C2 Nb C2 73.83(19) 2_665 3_655 ?
C2 Nb C2 73.83(19) . 4_565 ?
C2 Nb C2 73.83(19) 2_665 4_565 ?
C2 Nb C2 116.3(4) 3_655 4_565 ?
C2 Nb C1 76.38(16) . . ?
C2 Nb C1 143.78(18) 2_665 . ?
C2 Nb C1 140.72(18) 3_655 . ?
C2 Nb C1 78.31(17) 4_565 . ?
C2 Nb C1 78.30(17) . 3_655 ?
C2 Nb C1 140.72(18) 2_665 3_655 ?
C2 Nb C1 76.38(16) 3_655 3_655 ?
C2 Nb C1 143.78(18) 4_565 3_655 ?
C1 Nb C1 72.96(19) . 3_655 ?
C2 Nb C1 143.78(18) . 2_665 ?
C2 Nb C1 76.38(16) 2_665 2_665 ?
C2 Nb C1 78.31(17) 3_655 2_665 ?
C2 Nb C1 140.72(18) 4_565 2_665 ?
C1 Nb C1 114.5(4) . 2_665 ?
C1 Nb C1 72.96(19) 3_655 2_665 ?
C2 Nb C1 140.72(18) . 4_565 ?
C2 Nb C1 78.31(17) 2_665 4_565 ?
C2 Nb C1 143.78(18) 3_655 4_565 ?
C2 Nb C1 76.38(16) 4_565 4_565 ?
C1 Nb C1 72.96(19) . 4_565 ?
C1 Nb C1 114.5(4) 3_655 4_565 ?
C1 Nb C1 72.96(19) 2_665 4_565 ?
O12 Mn N1 89.3(3) . . ?
O12 Mn N1 89.3(3) . 16_554 ?
N1 Mn N1 89.9(4) . 16_554 ?
O12 Mn N2 97.8(2) . 10_554 ?
N1 Mn N2 172.6(2) . 10_554 ?
N1 Mn N2 87.82(15) 16_554 10_554 ?
O12 Mn N2 97.8(2) . 7_554 ?
N1 Mn N2 87.82(15) . 7_554 ?
N1 Mn N2 172.6(2) 16_554 7_554 ?
N2 Mn N2 93.5(4) 10_554 7_554 ?
O12 Mn O1 174.2(4) . . ?
N1 Mn O1 86.6(3) . . ?
N1 Mn O1 86.6(3) 16_554 . ?
N2 Mn O1 86.2(3) 10_554 . ?
N2 Mn O1 86.2(3) 7_554 . ?
N1 C1 Nb 177.4(7) . . ?
C1 N1 Mn 167.8(7) . . ?
O12 C11 O12 131(2) 2_565 . ?
C11 O12 Mn 144.9(11) . . ?
C2 N2 Mn 161.1(7) . 10 ?
N2 C2 Nb 177.1(8) . . ?

_refine_diff_density_max         1.182
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.093

_shelx_res_file                  
;

    dp_dpp083.res created by SHELXL-2014/7


TITL dp_dpp083 in I 4 c m
CELL  0.71073  12.0732  12.0732  13.4352   90.000   90.000   90.000
ZERR     2.00   0.0001   0.0001   0.0003    0.003    0.003    0.003
LATT  -2
SYMM  - X, - Y,   Z
SYMM  - Y,   X,   Z
SYMM    Y, - X,   Z
SYMM  - X,   Y, 1/2 + Z
SYMM    X, - Y, 1/2 + Z
SYMM    Y,   X, 1/2 + Z
SYMM  - Y, - X, 1/2 + Z
SFAC  C    H    N    O    MN   NB
UNIT 36 4 36 28 8 4
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
MERG   2
OMIT    -2.00  56.58
OMIT     0   0   2
OMIT     5   5   4
FMAP   2
PLAN   20
SIZE     0.05   0.05   0.10
ACTA
TWIN -1 0 0 0 -1 0 0 0 -1
BOND
L.S.  19
TEMP    20.00
WGHT    0.048300    2.267700
BASF   0.08241
FVAR       1.62541
NB    6    0.500000    0.500000    0.124237    10.25000    0.01347    0.01347 =
         0.01356    0.00000    0.00000    0.00000
MN    5    0.183119    0.316881   -0.128016    10.50000    0.02318    0.02318 =
         0.01878    0.00109   -0.00109   -0.00892
C1    1    0.358749    0.431491    0.033416    11.00000    0.02921    0.02930 =
         0.02381   -0.00155   -0.00366   -0.00181
N1    3    0.289923    0.393446   -0.012946    11.00000    0.04407    0.05656 =
         0.04080   -0.00428   -0.01270   -0.02115
C11   1    0.000000    0.500000   -0.136211    10.25000    0.04989    0.04989 =
         0.03709    0.00000    0.00000   -0.01905
AFIX  43
H11   2    0.000000    0.500000   -0.205432    10.25000   -1.20000
AFIX   0
O2    4    0.610919    0.110919    0.162854    10.50000    0.08859    0.08859 =
         0.11388    0.01346    0.01346    0.02178
O12   4    0.062791    0.437209   -0.099655    10.50000    0.05889    0.05889 =
         0.07570   -0.00864    0.00864    0.02302
O1    4    0.315093    0.184907   -0.141829    10.50000    0.09509    0.09509 =
         0.06732    0.00401   -0.00401    0.06453
N2    3    0.410484    0.279385    0.258554    11.00000    0.05311    0.03157 =
         0.02875    0.00515    0.00611   -0.01166
C2    1    0.443297    0.352149    0.212651    11.00000    0.03091    0.02130 =
         0.02593   -0.00067    0.00651   -0.00623
PART    1
N11   3    0.385350    0.114650    0.062027    10.25000    0.03992    0.03992 =
         0.05671   -0.00982    0.00982    0.01448
PART    2
O11   4    0.386533    0.113467    0.078198    10.25000    0.13590    0.13590 =
         0.05659   -0.02766    0.02766   -0.00847
HKLF    4

REM  dp_dpp083 in I 4 c m
REM R1 =  0.0296 for    1157 Fo > 4sig(Fo)  and  0.0339 for all    1265 data
REM     81 parameters refined using      1 restraints

END

WGHT      0.0483      2.2677

REM Highest difference peak  1.182,  deepest hole -0.689,  1-sigma level  0.093
Q1    1   0.1372  0.3628 -0.1249  10.50000  0.05    1.18
Q2    1   0.5661  0.5656  0.1248  11.00000  0.05    0.62
Q3    1   0.4242  0.4933  0.0544  11.00000  0.05    0.51
Q4    1   0.4967  0.4269  0.1931  11.00000  0.05    0.49
Q5    1   0.2523  0.2477 -0.1375  10.50000  0.05    0.40
Q6    1   0.3226  0.2363 -0.1015  11.00000  0.05    0.31
Q7    1   0.2981  0.2019 -0.0726  10.50000  0.05    0.30
Q8    1   0.3166  0.2220 -0.1707  11.00000  0.05    0.29
Q9    1   0.3506  0.1494 -0.1255  10.50000  0.05    0.28
Q10   1   0.2507  0.3172 -0.0595  11.00000  0.05    0.27
Q11   1   0.1515  0.2793 -0.0749  11.00000  0.05    0.25
Q12   1   0.4293  0.2404  0.2715  11.00000  0.05    0.25
Q13   1   0.1850  0.3738 -0.1874  11.00000  0.05    0.25
Q14   1   0.0658  0.4342 -0.1590  10.50000  0.05    0.25
Q15   1   0.1833  0.2487 -0.1947  11.00000  0.05    0.24
Q16   1   0.4466  0.3203 -0.1291  11.00000  0.05    0.24
Q17   1   0.3362  0.1638 -0.2044  10.50000  0.05    0.24
Q18   1   0.1223  0.3039 -0.0574  11.00000  0.05    0.23
Q19   1   0.4238  0.3020  0.2106  11.00000  0.05    0.23
Q20   1   0.5711  0.0711  0.2186  10.50000  0.05    0.23
;
_shelx_res_checksum              172

_chemical_properties_physical    Air-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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. 
# 
#######################################################################

data_MnMoform
_database_code_depnum_ccdc_archive 'CCDC 1835754'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT306_MnMoform            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O2 Check
RESPONSE: The isolated oxygen atom is the crystallization water molecule. H-atoms could not be located.
;
_vrf_PLAT430_MnMoform            
;
PROBLEM: Short Inter D...A Contact  O1       ..O2               2.82 Ang.
RESPONSE: The short distance is due to the stron H-bond. However, H-atoms could not be located.
;
_vrf_PLAT430_MnMoform_2          
;
PROBLEM: Short Inter D...A Contact  O2       ..N18              2.87 Ang.
RESPONSE: The short distance is due to the stron H-bond. However, H-atoms could not be located.
;
_vrf_PLAT430_MnMoform_3          
;
PROBLEM: Short Inter D...A Contact  O2       ..N18              2.87 Ang.
RESPONSE: The short distance is due to the stron H-bond. However, H-atoms could not be located.
;
# Added during the CSD deposition process: Sunday 08 April 2018 11:48 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Mn2Moformate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H2 Mn4 Mo2 N18 O14'
_chemical_formula_weight         1106.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           108
_space_group_name_H-M_alt        'I 4 c m'
_space_group_name_Hall           'I 4 -2c'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x, -y, z+1/2'
'-x, y, z+1/2'
'-y, -x, z+1/2'
'y, x, z+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, z+1'
'-x+1/2, y+1/2, z+1'
'-y+1/2, -x+1/2, z+1'
'y+1/2, x+1/2, z+1'

_cell_length_a                   11.8998(4)
_cell_length_b                   11.8998(4)
_cell_length_c                   13.2632(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1878.14(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4418
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      27.62

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_F_000             1064
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    2.034
_shelx_estimated_absorpt_T_min   0.823
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5759
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8QuestEco Photon50 CMOS'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6713
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.912
_diffrn_reflns_theta_max         27.627
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             1150
_reflns_number_gt                1071
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.914
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.998

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          'Refined as a 2-component inversion twin.,Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0183P)²+3.4386P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.48(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1150
_refine_ls_number_parameters     81
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0518
_refine_ls_wR_factor_gt          0.0503
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mo Mo 0.5000 0.5000 0.12401(8) 0.00931(14) Uani 1 4 d S T P . .
Mn Mn 0.18718(4) 0.31282(4) -0.12952(14) 0.01424(18) Uani 1 2 d S T P . .
C1 C 0.3668(6) 0.4321(7) 0.0338(6) 0.0193(15) Uani 1 1 d . . . . .
N11 N 0.2958(5) 0.3906(5) -0.0120(5) 0.0338(15) Uani 1 1 d . . . . .
C11 C 0.0000 0.5000 -0.1398(12) 0.033(3) Uani 1 4 d S T P . .
H11 H 0.0000 0.5000 -0.2099 0.040 Uiso 1 4 calc R U P . .
O2 O 0.3895(9) 0.1105(9) -0.3422(9) 0.086(4) Uani 1 2 d S T P . .
O12 O 0.0641(3) 0.4359(3) -0.0985(4) 0.0474(18) Uani 1 2 d S T P . .
O1 O 0.3192(3) 0.1808(3) -0.1490(8) 0.083(4) Uani 1 2 d S T P . .
N2 N 0.4130(5) 0.2818(5) 0.2567(5) 0.0332(14) Uani 1 1 d . . . . .
C2 C 0.4456(6) 0.3553(6) 0.2117(6) 0.0199(15) Uani 1 1 d . . . . .
N18 N 0.392(4) 0.108(4) 0.067(4) 0.18(3) Uani 0.5 2 d S T P A 1
O11 O 0.3848(9) 0.1152(9) 0.0669(16) 0.029(4) Uani 0.5 2 d S T P B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo 0.01019(17) 0.01019(17) 0.0075(3) 0.000 0.000 0.000
Mn 0.0146(2) 0.0146(2) 0.0134(4) 0.0002(6) -0.0002(6) -0.0025(3)
C1 0.016(3) 0.024(3) 0.018(3) 0.003(2) -0.001(3) 0.001(2)
N11 0.031(3) 0.039(3) 0.032(3) -0.002(3) -0.008(2) -0.012(2)
C11 0.035(3) 0.035(3) 0.030(9) 0.000 0.000 0.000(4)
O2 0.093(5) 0.093(5) 0.074(8) 0.005(5) -0.005(5) -0.010(6)
O12 0.045(2) 0.045(2) 0.053(5) -0.0019(16) 0.0019(16) 0.030(3)
O1 0.090(4) 0.090(4) 0.070(10) -0.002(2) 0.002(2) 0.067(4)
N2 0.044(3) 0.027(3) 0.028(3) 0.009(2) 0.008(2) -0.009(2)
C2 0.024(3) 0.019(3) 0.016(3) 0.001(2) 0.006(2) -0.003(2)
N18 0.21(3) 0.21(3) 0.13(5) -0.09(3) 0.09(3) -0.03(4)
O11 0.024(4) 0.024(4) 0.038(11) 0.000(5) 0.000(5) 0.005(5)

_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
Mo C1 2.144(8) 3_655 ?
Mo C1 2.144(8) 2_665 ?
Mo C1 2.144(8) 4_565 ?
Mo C1 2.144(8) . ?
Mo C2 2.176(7) . ?
Mo C2 2.176(7) 2_665 ?
Mo C2 2.176(7) 3_655 ?
Mo C2 2.176(7) 4_565 ?
Mn O12 2.112(5) . ?
Mn N11 2.226(7) 15_554 ?
Mn N11 2.226(7) . ?
Mn N2 2.229(7) 10_554 ?
Mn N2 2.229(7) 8_554 ?
Mn O1 2.237(6) . ?
C1 N11 1.152(9) . ?
C11 O12 1.209(9) 2_565 ?
C11 O12 1.209(9) . ?
N2 C2 1.128(9) . ?
N2 Mn 2.228(7) 10 ?

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
C1 Mo C1 71.8(2) 3_655 2_665 ?
C1 Mo C1 112.1(4) 3_655 4_565 ?
C1 Mo C1 71.8(2) 2_665 4_565 ?
C1 Mo C1 71.8(2) 3_655 . ?
C1 Mo C1 112.1(4) 2_665 . ?
C1 Mo C1 71.8(2) 4_565 . ?
C1 Mo C2 79.94(17) 3_655 . ?
C1 Mo C2 144.71(18) 2_665 . ?
C1 Mo C2 140.45(18) 4_565 . ?
C1 Mo C2 77.30(15) . . ?
C1 Mo C2 140.45(18) 3_655 2_665 ?
C1 Mo C2 77.30(15) 2_665 2_665 ?
C1 Mo C2 79.94(17) 4_565 2_665 ?
C1 Mo C2 144.71(18) . 2_665 ?
C2 Mo C2 115.4(4) . 2_665 ?
C1 Mo C2 77.30(15) 3_655 3_655 ?
C1 Mo C2 79.94(17) 2_665 3_655 ?
C1 Mo C2 144.71(18) 4_565 3_655 ?
C1 Mo C2 140.45(18) . 3_655 ?
C2 Mo C2 73.4(2) . 3_655 ?
C2 Mo C2 73.4(2) 2_665 3_655 ?
C1 Mo C2 144.71(18) 3_655 4_565 ?
C1 Mo C2 140.45(18) 2_665 4_565 ?
C1 Mo C2 77.30(15) 4_565 4_565 ?
C1 Mo C2 79.94(17) . 4_565 ?
C2 Mo C2 73.4(2) . 4_565 ?
C2 Mo C2 73.4(2) 2_665 4_565 ?
C2 Mo C2 115.4(4) 3_655 4_565 ?
O12 Mn N11 88.73(19) . 15_554 ?
O12 Mn N11 88.73(19) . . ?
N11 Mn N11 89.6(4) 15_554 . ?
O12 Mn N2 96.40(19) . 10_554 ?
N11 Mn N2 87.61(14) 15_554 10_554 ?
N11 Mn N2 174.1(2) . 10_554 ?
O12 Mn N2 96.40(19) . 8_554 ?
N11 Mn N2 174.1(2) 15_554 8_554 ?
N11 Mn N2 87.61(14) . 8_554 ?
N2 Mn N2 94.7(4) 10_554 8_554 ?
O12 Mn O1 175.4(3) . . ?
N11 Mn O1 88.0(3) 15_554 . ?
N11 Mn O1 88.0(3) . . ?
N2 Mn O1 86.7(2) 10_554 . ?
N2 Mn O1 86.7(2) 8_554 . ?
N11 C1 Mo 176.5(6) . . ?
C1 N11 Mn 166.7(6) . . ?
O12 C11 O12 126.1(14) 2_565 . ?
C11 O12 Mn 141.8(8) . . ?
C2 N2 Mn 159.1(6) . 10 ?
N2 C2 Mo 177.2(7) . . ?

_refine_diff_density_max         0.361
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.069

_shelx_res_file                  
;

    MnMoform.res created by SHELXL-2014/7


TITL GH083_xprep_b.res in I4cm
CELL  0.71073  11.8998  11.8998  13.2632   90.000   90.000   90.000
ZERR     2.00   0.0004   0.0004   0.0005    0.000    0.000    0.000
LATT  -2
SYMM  - X, - Y,   Z
SYMM  - Y,   X,   Z
SYMM    Y, - X,   Z
SYMM    X, - Y, 1/2 + Z
SYMM  - X,   Y, 1/2 + Z
SYMM  - Y, - X, 1/2 + Z
SYMM    Y,   X, 1/2 + Z
SFAC  C    H    N    O    MN   MO
UNIT 36 4 36 28 8 4
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
MERG   2
OMIT     0   4   0
OMIT     0   0   2
OMIT     0   2   0
TWIN
FMAP   2
PLAN   20
SIZE     0.050   0.050   0.100
ACTA
BOND
L.S.  19
TEMP    20.00
ACTA
WGHT    0.018300    3.438600
BASF   0.48372
FVAR       0.10705
MO    6    0.500000    0.500000    0.124015    10.25000    0.01019    0.01019 =
         0.00754    0.00000    0.00000    0.00000
MN    5    0.187180    0.312820   -0.129522    10.50000    0.01463    0.01463 =
         0.01345    0.00019   -0.00019   -0.00255
C1    1    0.366799    0.432142    0.033759    11.00000    0.01606    0.02414 =
         0.01767    0.00293   -0.00114    0.00126
N11   3    0.295780    0.390629   -0.012010    11.00000    0.03068    0.03875 =
         0.03200   -0.00215   -0.00805   -0.01193
C11   1    0.000000    0.500000   -0.139817    10.25000    0.03465    0.03465 =
         0.02951    0.00000    0.00000    0.00043
AFIX  43
H11   2    0.000000    0.500000   -0.209936    10.25000   -1.20000
AFIX   0
O2    4    0.389490    0.110510   -0.342178    10.50000    0.09253    0.09253 =
         0.07438    0.00543   -0.00543   -0.00957
O12   4    0.064058    0.435942   -0.098496    10.50000    0.04455    0.04455 =
         0.05319   -0.00186    0.00186    0.03024
O1    4    0.319227    0.180773   -0.148998    10.50000    0.08959    0.08959 =
         0.06958   -0.00240    0.00240    0.06748
N2    3    0.412989    0.281812    0.256702    11.00000    0.04380    0.02742 =
         0.02843    0.00860    0.00776   -0.00872
C2    1    0.445553    0.355274    0.211651    11.00000    0.02396    0.01935 =
         0.01626    0.00115    0.00640   -0.00310
PART    1
N18   3    0.391589    0.108411    0.066555    10.25000    0.21160    0.21160 =
         0.12805   -0.08852    0.08852   -0.03340
PART    2
O11   4    0.384759    0.115241    0.066913    10.25000    0.02418    0.02418 =
         0.03812   -0.00047    0.00047    0.00465
HKLF    4

REM  GH083_xprep_b.res in I4cm
REM R1 =  0.0230 for    1071 Fo > 4sig(Fo)  and  0.0268 for all    1150 data
REM     81 parameters refined using      1 restraints

END

WGHT      0.0183      3.4386

REM Highest difference peak  0.361,  deepest hole -0.403,  1-sigma level  0.069
Q1    1   0.3652  0.1968 -0.1255  11.00000  0.05    0.36
Q2    1   0.2729  0.1760 -0.1498  11.00000  0.05    0.33
Q3    1   0.3343  0.1850 -0.1792  11.00000  0.05    0.27
Q4    1   0.5000  0.5000  0.3377  10.25000  0.05    0.26
Q5    1   0.0792  0.4208 -0.1624  10.50000  0.05    0.26
Q6    1   0.2749  0.1761 -0.0977  11.00000  0.05    0.26
Q7    1   0.3092  0.1907 -0.3635  10.50000  0.05    0.25
Q8    1   0.2370  0.2630 -0.1227  10.50000  0.05    0.25
Q9    1   0.3438  0.1920 -0.0942  11.00000  0.05    0.24
Q10   1   0.4197  0.4811  0.0535  11.00000  0.05    0.23
Q11   1   0.3555  0.1445  0.1611  10.50000  0.05    0.23
Q12   1   0.5000  0.5000  0.1932  10.25000  0.05    0.23
Q13   1   0.4293  0.1383 -0.2847  11.00000  0.05    0.22
Q14   1   0.4609  0.4961 -0.1271  11.00000  0.05    0.22
Q15   1   0.0276  0.3654 -0.1407  11.00000  0.05    0.21
Q16   1   0.3574  0.1651 -0.4037  11.00000  0.05    0.21
Q17   1   0.2481  0.0776 -0.1776  11.00000  0.05    0.21
Q18   1   0.3165  0.0380  0.0953  11.00000  0.05    0.20
Q19   1   0.5000  0.5000  0.0486  10.25000  0.05    0.20
Q20   1   0.4350  0.2929  0.2031  11.00000  0.05    0.19
;
_shelx_res_checksum              6267

_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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. 
# 
#######################################################################

data_MnMoCN
_database_code_depnum_ccdc_archive 'CCDC 1835755'
_audit_update_record             
;
2018-04-08 deposited with the CCDC.
2018-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Mn2MoCN
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 Mn4 Mo2 N22 O6'
_chemical_formula_weight         1032.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -y, -z+1/2'
'-x, y, -z+1/2'
'y, x, -z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1/2, y+1/2, -z+1'
'y+1/2, x+1/2, -z+1'
'-y+1/2, -x+1/2, -z+1'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, y, z-1/2'
'x, -y, z-1/2'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'

_cell_length_a                   11.6902(4)
_cell_length_b                   11.6902(4)
_cell_length_c                   13.3582(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1825.54(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5404
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.49

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_F_000             988
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    2.072
_shelx_estimated_absorpt_T_min   0.733
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8QuestEco Photon 50 CMOS'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9757
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.050
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             592
_reflns_number_gt                541
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0110P)²+15.5588P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         592
_refine_ls_number_parameters     46
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0582
_refine_ls_wR_factor_gt          0.0550
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Mo Mo 0.0000 0.0000 0.2500 0.00441(15) Uani 1 8 d S T P . .
Mn Mn -0.32964(5) 0.17036(5) 0.0000 0.00603(18) Uani 1 4 d S T P . .
N1 N -0.2220(2) 0.0863(2) 0.11655(17) 0.0161(5) Uani 1 1 d . . . . .
O1 O -0.1922(3) 0.3078(3) 0.0000 0.0528(18) Uani 1 4 d S TU P A 1
C1 C -0.1437(2) 0.0569(2) 0.16216(19) 0.0102(5) Uani 1 1 d . . . . .
C2 C -0.468(6) 0.032(6) 0.0000 0.012(9) Uani 0.5 4 d S TU P A .
N2 N -0.462(5) 0.038(5) 0.0000 0.012(9) Uani 0.5 4 d S TU P A .
O2 O -0.1160(10) 0.3840(10) -0.1938(15) 0.019(3) Uiso 0.25 2 d S . P . .
N4 N -0.0954(15) 0.4046(15) -0.2184(11) 0.111(9) Uani 0.5 2 d S T P B 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mo 0.00447(18) 0.00447(18) 0.0043(3) 0.000 0.000 0.000
Mn 0.0057(2) 0.0057(2) 0.0067(3) 0.000 0.000 0.0007(3)
N1 0.0141(12) 0.0196(12) 0.0147(11) 0.0021(10) -0.0037(9) 0.0029(9)
O1 0.055(3) 0.055(3) 0.047(3) 0.000 0.000 -0.043(3)
C1 0.0098(12) 0.0104(12) 0.0105(12) -0.0004(9) 0.0005(10) -0.0004(9)
C2 0.010(9) 0.010(9) 0.017(12) 0.000 0.000 -0.002(7)
N2 0.010(10) 0.010(10) 0.016(10) 0.000 0.000 0.005(8)
N4 0.148(13) 0.148(13) 0.038(10) -0.043(9) -0.043(9) 0.093(14)

_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
Mo C1 2.154(3) 6 ?
Mo C1 2.154(3) 2 ?
Mo C1 2.154(3) 8 ?
Mo C1 2.154(3) 5 ?
Mo C1 2.154(3) 4 ?
Mo C1 2.154(3) 3 ?
Mo C1 2.154(3) 7 ?
Mo C1 2.154(3) . ?
Mn N2 2.19(8) . ?
Mn N1 2.230(2) 32_455 ?
Mn N1 2.230(2) 19 ?
Mn N1 2.230(2) 15_454 ?
Mn N1 2.230(2) . ?
Mn O1 2.271(5) . ?
Mn C2 2.29(9) . ?
N1 C1 1.152(3) . ?
C2 C2 1.04(19) 17_455 ?
C2 N2 1.15(3) 17_455 ?
N2 C2 1.15(3) 17_455 ?
N2 N2 1.25(15) 17_455 ?

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
C1 Mo C1 141.12(13) 6 2 ?
C1 Mo C1 72.75(6) 6 8 ?
C1 Mo C1 144.00(13) 2 8 ?
C1 Mo C1 114.00(13) 6 5 ?
C1 Mo C1 79.33(13) 2 5 ?
C1 Mo C1 72.75(6) 8 5 ?
C1 Mo C1 79.33(13) 6 4 ?
C1 Mo C1 114.00(13) 2 4 ?
C1 Mo C1 77.54(13) 8 4 ?
C1 Mo C1 141.12(13) 5 4 ?
C1 Mo C1 77.54(13) 6 3 ?
C1 Mo C1 72.75(6) 2 3 ?
C1 Mo C1 141.12(13) 8 3 ?
C1 Mo C1 144.00(13) 5 3 ?
C1 Mo C1 72.75(6) 4 3 ?
C1 Mo C1 72.75(6) 6 7 ?
C1 Mo C1 77.54(13) 2 7 ?
C1 Mo C1 114.00(13) 8 7 ?
C1 Mo C1 72.75(6) 5 7 ?
C1 Mo C1 144.00(13) 4 7 ?
C1 Mo C1 79.33(13) 3 7 ?
C1 Mo C1 144.00(13) 6 . ?
C1 Mo C1 72.75(6) 2 . ?
C1 Mo C1 79.32(13) 8 . ?
C1 Mo C1 77.54(13) 5 . ?
C1 Mo C1 72.75(6) 4 . ?
C1 Mo C1 114.00(13) 3 . ?
C1 Mo C1 141.12(13) 7 . ?
N2 Mn N1 95.02(7) . 32_455 ?
N2 Mn N1 95.02(7) . 19 ?
N1 Mn N1 169.95(13) 32_455 19 ?
N2 Mn N1 95.02(7) . 15_454 ?
N1 Mn N1 88.56(12) 32_455 15_454 ?
N1 Mn N1 90.56(12) 19 15_454 ?
N2 Mn N1 95.02(7) . . ?
N1 Mn N1 90.56(12) 32_455 . ?
N1 Mn N1 88.56(12) 19 . ?
N1 Mn N1 169.95(13) 15_454 . ?
N2 Mn O1 180(2) . . ?
N1 Mn O1 84.98(7) 32_455 . ?
N1 Mn O1 84.98(7) 19 . ?
N1 Mn O1 84.98(7) 15_454 . ?
N1 Mn O1 84.98(7) . . ?
N2 Mn C2 0(2) . . ?
N1 Mn C2 95.02(7) 32_455 . ?
N1 Mn C2 95.02(7) 19 . ?
N1 Mn C2 95.02(7) 15_454 . ?
N1 Mn C2 95.02(7) . . ?
O1 Mn C2 180(2) . . ?
C1 N1 Mn 161.6(2) . . ?
N1 C1 Mo 178.6(2) . . ?
C2 C2 N2 0.0(17) 17_455 17_455 ?
C2 C2 Mn 180(5) 17_455 . ?
N2 C2 Mn 180(3) 17_455 . ?
C2 N2 N2 0.0(15) 17_455 17_455 ?
C2 N2 Mn 180.0(14) 17_455 . ?
N2 N2 Mn 180(3) 17_455 . ?

_refine_diff_density_max         0.467
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.099

_shelx_res_file                  
;

    MnMoCN.res created by SHELXL-2014/7


TITL GH091_xprep-auto - I4mcm in I4/mcm #140
REM reset to I4/mcm #140
CELL 0.71073 11.6902 11.6902 13.3582 90 90 90
ZERR 2 0.0004 0.0004 0.0006 0 0 0
LATT 2
SYMM -Y,+X,+Z
SYMM -X,-Y,+Z
SYMM +Y,-X,+Z
SYMM +X,-Y,0.5-Z
SYMM -X,+Y,0.5-Z
SYMM +Y,+X,0.5-Z
SYMM -Y,-X,0.5-Z
SFAC C N O Mn Mo

UNIT 36 44 12 8 4
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
ISOR 0.01 0.2 C2
ISOR 0.01 0.2 N2
ISOR 0.02 0.2 O1
L.S. 20
PLAN  10
SIZE 0.03 0.04 0.16
TEMP -153.15
BOND
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%.\\GH091_xprep-auto%20-%20I4mcm_z%20insem%20Nb.hkl">
REM </olex2.extras>

WGHT    0.011000   15.558803
FVAR       0.09822
MO    5    0.000000    0.000000    0.250000    10.12500    0.00447    0.00447 =
         0.00431    0.00000    0.00000    0.00000
MN    4   -0.329635    0.170365    0.000000    10.25000    0.00572    0.00572 =
         0.00666    0.00000    0.00000    0.00066
N1    2   -0.221970    0.086325    0.116555    11.00000    0.01412    0.01958 =
         0.01468    0.00213   -0.00374    0.00292
PART 1
O1    3   -0.192246    0.307754    0.000000    10.25000    0.05543    0.05543 =
         0.04740    0.00000    0.00000   -0.04311
PART 0
C1    1   -0.143694    0.056948    0.162163    11.00000    0.00975    0.01040 =
         0.01049   -0.00044    0.00047   -0.00036
C2    1   -0.468433    0.031567    0.000000    10.12500    0.00983    0.00983 =
         0.01680    0.00000    0.00000   -0.00185
N2    2   -0.462217    0.037783    0.000000    10.12500    0.00954    0.00954 =
         0.01573    0.00000    0.00000    0.00466

O2    3   -0.116029    0.383971   -0.193832    10.12500    0.01874
PART 2
N4    2   -0.095378    0.404622   -0.218441    10.25000    0.14793    0.14793 =
         0.03798   -0.04311   -0.04311    0.09255
HKLF 4

REM  GH091_xprep-auto - I4mcm in I4/mcm #140
REM R1 =  0.0265 for     541 Fo > 4sig(Fo)  and  0.0316 for all     592 data
REM     46 parameters refined using     18 restraints

END

WGHT      0.0110     15.5592

REM Highest difference peak  0.467,  deepest hole -0.644,  1-sigma level  0.099
Q1    1  -0.1359  0.3641 -0.1609  10.50000  0.05    0.47
Q2    1   0.0000  0.4098 -0.2500  10.50000  0.05    0.38
Q3    1  -0.1731  0.3552  0.0594  11.00000  0.05    0.38
Q4    1  -0.1165  0.2650  0.0000  10.50000  0.05    0.36
Q5    1  -0.1544  0.0091  0.0000  10.50000  0.05    0.35
Q6    1  -0.1284  0.2324  0.0000  10.50000  0.05    0.34
Q7    1  -0.1883  0.3117 -0.2289  10.50000  0.05    0.33
Q8    1  -0.0601  0.0671  0.1887  11.00000  0.05    0.31
Q9    1   0.0281  0.0189  0.1607  11.00000  0.05    0.30
Q10   1  -0.2257  0.0521  0.1618  11.00000  0.05    0.29
;
_shelx_res_checksum              7953

_exptl_crystal_preparation       'Magnetic properties'
