# 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_MnMo3-Pypz
_database_code_depnum_ccdc_archive 'CCDC 1835917'
_audit_update_record             
;
2018-04-28 deposited with the CCDC.
2018-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?a
_chemical_formula_sum            'C17 H12 Mn2 Mo N11 O'
_chemical_formula_weight         592.20

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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   24.605(11)
_cell_length_b                   7.246(3)
_cell_length_c                   12.402(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.546(6)
_cell_angle_gamma                90
_cell_volume                     2130.2(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1591
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      26.16

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   0.695?
_exptl_transmission_factor_max   0.726
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.782
_shelx_estimated_absorpt_T_min   0.706
_shelx_estimated_absorpt_T_max   0.740
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'sealed tube'
_diffrn_measurement_method       'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean '\f and \w scans'
_diffrn_reflns_number            8312
_diffrn_reflns_av_unetI/netI     0.0939
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.704
_diffrn_reflns_theta_max         26.275
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2321
_reflns_number_gt                1897
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0683P)²+5.4499P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2321
_refine_ls_number_parameters     178
_refine_ls_number_restraints     222
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0548
_refine_ls_wR_factor_ref         0.1504
_refine_ls_wR_factor_gt          0.1420
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.073
_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 0.10555(2) 0.0000 0.29733(5) 0.0136(2) Uani 1 2 d S T P . .
O1 O -0.0360(3) 0.5000 0.1507(5) 0.0357(14) Uani 1 2 d DS TU P . .
H1 H -0.0248 0.5744 0.2036 0.043 Uiso 1 1 d DR U . . .
N1 N 0.1827(3) 0.0000 0.5614(6) 0.0231(14) Uani 1 2 d S TU P . .
C1 C 0.1551(3) 0.0000 0.4712(6) 0.0204(14) Uani 1 2 d S TU P . .
Mn1 Mn 0.23997(5) 0.0000 0.72707(9) 0.0169(3) Uani 1 2 d S TU P . .
C4 C 0.1729(2) 0.1846(7) 0.2913(4) 0.0200(10) Uani 1 1 d . U . . .
Mn2 Mn 0.0000 0.5000 0.5000 0.0190(4) Uani 1 4 d S TU P . .
N3 N 0.0552(2) 0.2844(6) 0.0916(4) 0.0351(12) Uani 1 1 d . U . . .
C3 C 0.0721(2) 0.1772(7) 0.1603(4) 0.0227(11) Uani 1 1 d . U . . .
Mn3 Mn 0.0000 0.5000 0.0000 0.0184(4) Uani 1 4 d DS TU P . .
N2 N 0.0293(2) 0.2927(6) 0.3992(4) 0.0284(10) Uani 1 1 d . U . . .
C2 C 0.0565(2) 0.1947(7) 0.3626(4) 0.0214(10) Uani 1 1 d . U . . .
N5 N -0.0935(3) 0.5000 0.3873(7) 0.0384(17) Uani 1 2 d S TU P . .
C13 C -0.1327(4) 0.5000 0.4170(7) 0.0312(18) Uani 1 2 d S TU P . .
N6 N 0.1670(3) 0.0000 0.7971(7) 0.0360(18) Uani 1 2 d S T P . .
C14 C -0.1809(4) 0.5000 0.4649(8) 0.036(2) Uani 1 2 d S TU P . .
H14A H -0.1699 0.4463 0.5383 0.054 Uiso 0.5 1 calc R U P . .
H14B H -0.2111 0.4292 0.4179 0.054 Uiso 0.5 1 calc R U P . .
H14C H -0.1933 0.6245 0.4699 0.054 Uiso 0.5 1 calc R U P . .
N7 N 0.2737(4) 0.0000 0.9150(6) 0.043(2) Uani 1 2 d S T P . .
C12 C 0.1117(4) 0.0000 0.7395(8) 0.0398(17) Uani 1 2 d S TU P . .
H12 H 0.1016 0.0000 0.6617 0.048 Uiso 1 2 calc R U P . .
N8 N 0.3250(4) 0.0000 0.9846(7) 0.055(3) Uani 1 2 d S T P . .
H8 H 0.3553 0.0000 0.9626 0.066 Uiso 1 2 calc R U P . .
C11 C 0.0725(4) 0.0000 0.7928(8) 0.0375(17) Uani 1 2 d S TU P . .
H11 H 0.0347 0.0000 0.7528 0.045 Uiso 1 2 calc R U P . .
C10 C 0.0872(5) 0.0000 0.9092(9) 0.053(2) Uani 1 2 d S TU P . .
H10 H 0.0584 0.0000 0.9449 0.063 Uiso 1 2 calc R U P . .
C9 C 0.1414(5) 0.0000 0.9734(10) 0.0525(19) Uani 1 2 d S TU P . .
H9 H 0.1518 0.0000 1.0513 0.063 Uiso 1 2 calc R U P . .
C8 C 0.1789(4) 0.0000 0.9093(9) 0.0412(16) Uani 1 2 d S TU P . .
C7 C 0.2378(5) 0.0000 0.9745(8) 0.0469(18) Uani 1 2 d DS TU P . .
C6 C 0.2702(5) 0.0000 1.0946(9) 0.052(2) Uani 1 2 d DS TU P . .
H6 H 0.2558 0.0000 1.1568 0.062 Uiso 1 2 calc R U P . .
C5 C 0.3252(4) 0.0000 1.0935(8) 0.0419(19) Uani 1 2 d S TU P . .
H5 H 0.3565 0.0000 1.1552 0.050 Uiso 1 2 calc R U P . .
N4 N 0.2102(2) 0.2757(6) 0.2899(4) 0.0277(11) Uani 1 1 d . . . . .


_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 C3 2.113(5) . ?
Mo1 C3 2.113(5) 6 ?
Mo1 C4 2.147(5) . ?
Mo1 C4 2.147(5) 6 ?
Mo1 C2 2.150(5) . ?
Mo1 C2 2.150(5) 6 ?
Mo1 C1 2.174(8) . ?
O1 Mn3 2.274(6) . ?
O1 H1 0.8362 . ?
N1 C1 1.143(10) . ?
N1 Mn1 2.158(7) . ?
Mn1 N4 2.080(5) 7_556 ?
Mn1 N4 2.080(5) 4_546 ?
Mn1 N6 2.195(7) . ?
Mn1 N7 2.255(8) . ?
C4 N4 1.134(7) . ?
Mn2 N2 2.196(4) 5_566 ?
Mn2 N2 2.196(4) 6_565 ?
Mn2 N2 2.196(4) 2_556 ?
Mn2 N2 2.196(4) . ?
Mn2 N5 2.350(8) . ?
Mn2 N5 2.350(8) 5_566 ?
N3 C3 1.145(7) . ?
N3 Mn3 2.180(5) . ?
Mn3 N3 2.180(5) 6_565 ?
Mn3 N3 2.180(5) 2 ?
Mn3 N3 2.180(5) 5_565 ?
Mn3 O1 2.273(6) 5_565 ?
N2 C2 1.151(7) . ?
N5 C13 1.121(12) . ?
C13 C14 1.462(12) . ?
N6 C8 1.343(13) . ?
N6 C12 1.356(13) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
N7 C7 1.294(13) . ?
N7 N8 1.326(12) . ?
C12 C11 1.306(13) . ?
C12 H12 0.9300 . ?
N8 C5 1.350(12) . ?
N8 H8 0.8600 . ?
C11 C10 1.391(14) . ?
C11 H11 0.9300 . ?
C10 C9 1.359(16) . ?
C10 H10 0.9300 . ?
C9 C8 1.371(14) . ?
C9 H9 0.9300 . ?
C8 C7 1.457(15) . ?
C7 C6 1.489(13) . ?
C6 C5 1.356(15) . ?
C6 H6 0.9300 . ?
C5 H5 0.9300 . ?
N4 Mn1 2.081(5) 7_556 ?

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
C3 Mo1 C3 74.9(3) . 6 ?
C3 Mo1 C4 74.4(2) . . ?
C3 Mo1 C4 119.2(2) 6 . ?
C3 Mo1 C4 119.2(2) . 6 ?
C3 Mo1 C4 74.4(2) 6 6 ?
C4 Mo1 C4 77.1(3) . 6 ?
C3 Mo1 C2 76.5(2) . . ?
C3 Mo1 C2 124.4(2) 6 . ?
C4 Mo1 C2 96.91(19) . . ?
C4 Mo1 C2 159.7(2) 6 . ?
C3 Mo1 C2 124.4(2) . 6 ?
C3 Mo1 C2 76.5(2) 6 6 ?
C4 Mo1 C2 159.7(2) . 6 ?
C4 Mo1 C2 96.91(19) 6 6 ?
C2 Mo1 C2 82.0(3) . 6 ?
C3 Mo1 C1 142.34(14) . . ?
C3 Mo1 C1 142.34(14) 6 . ?
C4 Mo1 C1 78.6(2) . . ?
C4 Mo1 C1 78.6(2) 6 . ?
C2 Mo1 C1 81.3(2) . . ?
C2 Mo1 C1 81.3(2) 6 . ?
Mn3 O1 H1 121.7 . . ?
C1 N1 Mn1 175.9(6) . . ?
N1 C1 Mo1 177.7(7) . . ?
N4 Mn1 N4 102.7(3) 7_556 4_546 ?
N4 Mn1 N1 98.96(17) 7_556 . ?
N4 Mn1 N1 98.96(17) 4_546 . ?
N4 Mn1 N6 127.40(14) 7_556 . ?
N4 Mn1 N6 127.40(14) 4_546 . ?
N1 Mn1 N6 89.0(3) . . ?
N4 Mn1 N7 92.4(2) 7_556 . ?
N4 Mn1 N7 92.4(2) 4_546 . ?
N1 Mn1 N7 161.8(3) . . ?
N6 Mn1 N7 72.8(3) . . ?
N4 C4 Mo1 176.8(4) . . ?
N2 Mn2 N2 93.7(2) 5_566 6_565 ?
N2 Mn2 N2 86.3(2) 5_566 2_556 ?
N2 Mn2 N2 180.0(2) 6_565 2_556 ?
N2 Mn2 N2 180.0 5_566 . ?
N2 Mn2 N2 86.3(2) 6_565 . ?
N2 Mn2 N2 93.7(2) 2_556 . ?
N2 Mn2 N5 85.45(19) 5_566 . ?
N2 Mn2 N5 94.55(19) 6_565 . ?
N2 Mn2 N5 85.45(19) 2_556 . ?
N2 Mn2 N5 94.55(19) . . ?
N2 Mn2 N5 94.55(19) 5_566 5_566 ?
N2 Mn2 N5 85.45(19) 6_565 5_566 ?
N2 Mn2 N5 94.55(19) 2_556 5_566 ?
N2 Mn2 N5 85.45(19) . 5_566 ?
N5 Mn2 N5 180.0 . 5_566 ?
C3 N3 Mn3 157.7(5) . . ?
N3 C3 Mo1 174.7(5) . . ?
N3 Mn3 N3 180.0(3) 6_565 2 ?
N3 Mn3 N3 88.4(3) 6_565 5_565 ?
N3 Mn3 N3 91.6(3) 2 5_565 ?
N3 Mn3 N3 91.6(3) 6_565 . ?
N3 Mn3 N3 88.4(3) 2 . ?
N3 Mn3 N3 180.0 5_565 . ?
N3 Mn3 O1 95.89(18) 6_565 5_565 ?
N3 Mn3 O1 84.11(18) 2 5_565 ?
N3 Mn3 O1 84.11(18) 5_565 5_565 ?
N3 Mn3 O1 95.89(18) . 5_565 ?
N3 Mn3 O1 84.11(18) 6_565 . ?
N3 Mn3 O1 95.89(18) 2 . ?
N3 Mn3 O1 95.89(18) 5_565 . ?
N3 Mn3 O1 84.11(18) . . ?
O1 Mn3 O1 180.0 5_565 . ?
C2 N2 Mn2 164.1(5) . . ?
N2 C2 Mo1 177.1(5) . . ?
C13 N5 Mn2 126.6(7) . . ?
N5 C13 C14 175.4(10) . . ?
C8 N6 C12 117.1(7) . . ?
C8 N6 Mn1 115.7(6) . . ?
C12 N6 Mn1 127.1(6) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C7 N7 N8 107.8(8) . . ?
C7 N7 Mn1 118.1(7) . . ?
N8 N7 Mn1 134.1(6) . . ?
C11 C12 N6 120.3(9) . . ?
C11 C12 H12 119.8 . . ?
N6 C12 H12 119.8 . . ?
N7 N8 C5 113.4(8) . . ?
N7 N8 H8 123.3 . . ?
C5 N8 H8 123.3 . . ?
C12 C11 C10 120.3(10) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C9 C10 C11 123.3(11) . . ?
C9 C10 H10 118.4 . . ?
C11 C10 H10 118.4 . . ?
C10 C9 C8 111.6(11) . . ?
C10 C9 H9 124.2 . . ?
C8 C9 H9 124.2 . . ?
N6 C8 C9 127.4(11) . . ?
N6 C8 C7 119.0(8) . . ?
C9 C8 C7 113.6(10) . . ?
N7 C7 C8 114.3(9) . . ?
N7 C7 C6 107.8(10) . . ?
C8 C7 C6 137.9(10) . . ?
C5 C6 C7 105.0(10) . . ?
C5 C6 H6 127.5 . . ?
C7 C6 H6 127.5 . . ?
N8 C5 C6 106.0(10) . . ?
N8 C5 H5 127.0 . . ?
C6 C5 H5 127.0 . . ?
C4 N4 Mn1 163.2(4) . 7_556 ?

_refine_diff_density_max         2.688
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.199

####################################################################### 
# 
# 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__MnMoPyim
_database_code_depnum_ccdc_archive 'CCDC 1835919'
_audit_update_record             
;
2018-04-28 deposited with the CCDC.
2018-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H12 Mn2 Mo N11 O'
_chemical_formula_weight         592.20

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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   24.2785(11)
_cell_length_b                   7.2502(3)
_cell_length_c                   12.4353(6)
_cell_angle_alpha                90
_cell_angle_beta                 103.2990(10)
_cell_angle_gamma                90
_cell_volume                     2130.21(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    5194
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    1.782
_shelx_estimated_absorpt_T_min   0.635
_shelx_estimated_absorpt_T_max   0.695
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_T_max  0.676
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9229
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.672
_diffrn_reflns_theta_max         27.102
_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             2531
_reflns_number_gt                2229
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0217P)²+3.7294P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2531
_refine_ls_number_parameters     178
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0554
_refine_ls_wR_factor_gt          0.0534
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.044
_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
Mo1 Mo 0.39309(2) 0.0000 0.21013(2) 0.01372(8) Uani 1 2 d S TU P . .
Mn1 Mn 0.26911(2) 0.0000 -0.21712(4) 0.01898(11) Uani 1 2 d S T P . .
Mn2 Mn 0.5000 0.5000 0.0000 0.02253(16) Uani 1 4 d S TU P . .
Mn3 Mn 0.5000 0.5000 0.5000 0.02234(16) Uani 1 4 d S T P . .
C1 C 0.34732(13) 0.0000 0.0373(3) 0.0225(7) Uani 1 2 d S T P . .
N1 N 0.32069(12) 0.0000 -0.0516(2) 0.0308(7) Uani 1 2 d S T P . .
N7 N 0.34541(12) 0.0000 -0.2796(2) 0.0342(7) Uani 1 2 d S T P . .
C3 C 0.42459(9) 0.1777(3) 0.34648(18) 0.0234(5) Uani 1 1 d . . . . .
N3 N 0.44209(9) 0.2798(3) 0.41756(16) 0.0322(5) Uani 1 1 d . . . . .
C2 C 0.44378(9) 0.1947(3) 0.14270(19) 0.0245(5) Uani 1 1 d . U . . .
O1 O 0.53171(11) 0.5000 0.3411(2) 0.0422(7) Uani 1 2 d DS T P . .
H1 H 0.5246 0.5878 0.2978 0.051 Uiso 1 1 d DR U . . .
N6 N 0.23944(11) 0.0000 -0.4056(2) 0.0279(6) Uani 1 2 d S T P . .
N2 N 0.47067(9) 0.2929(3) 0.10297(18) 0.0352(5) Uani 1 1 d . U . . .
C11 C 0.28098(14) 0.0000 -0.4608(3) 0.0283(7) Uani 1 2 d S T P . .
N8 N 0.38763(14) 0.0000 -0.4173(3) 0.0543(10) Uani 1 2 d S T P . .
H8 H 0.3926 0.0000 -0.4835 0.065 Uiso 1 2 calc R U P . .
C7 C 0.18627(16) 0.0000 -0.4647(3) 0.0411(10) Uani 1 2 d S T P . .
H7 H 0.1569 0.0000 -0.4282 0.049 Uiso 1 2 calc R U P . .
C12 C 0.33756(14) 0.0000 -0.3886(3) 0.0302(8) Uani 1 2 d S T P . .
C5 C 0.63307(19) 0.5000 0.0770(3) 0.0457(10) Uani 1 2 d S TU P . .
N5 N 0.59236(15) 0.5000 0.1126(3) 0.0590(10) Uani 1 2 d S TU P . .
C13 C 0.42965(16) 0.0000 -0.3211(4) 0.0620(14) Uani 1 2 d S T P . .
H13 H 0.4685 0.0000 -0.3154 0.074 Uiso 1 2 calc R U P . .
C14 C 0.40318(16) 0.0000 -0.2378(4) 0.0523(12) Uani 1 2 d S T P . .
H14 H 0.4210 0.0000 -0.1631 0.063 Uiso 1 2 calc R U P . .
C6 C 0.68151(18) 0.5000 0.0299(4) 0.0463(10) Uani 1 2 d S TU P . .
H6A H 0.6711 0.4524 -0.0441 0.069 Uiso 0.5 1 calc R U P . .
H6B H 0.7105 0.4239 0.0737 0.069 Uiso 0.5 1 calc R U P . .
H6C H 0.6954 0.6237 0.0284 0.069 Uiso 0.5 1 calc R U P . .
C10 C 0.27041(18) 0.0000 -0.5737(3) 0.0450(10) Uani 1 2 d S T P . .
H10 H 0.3000 0.0000 -0.6098 0.054 Uiso 1 2 calc R U P . .
C8 C 0.17355(18) 0.0000 -0.5782(4) 0.0518(12) Uani 1 2 d S T P . .
H8A H 0.1360 0.0000 -0.6178 0.062 Uiso 1 2 calc R U P . .
C9 C 0.2159(2) 0.0000 -0.6319(3) 0.0557(13) Uani 1 2 d S T P . .
H9 H 0.2077 0.0000 -0.7087 0.067 Uiso 1 2 calc R U P . .
C4 C 0.32454(9) 0.1864(3) 0.21162(17) 0.0227(5) Uani 1 1 d . U . . .
N4 N 0.28555(8) 0.2794(3) 0.20744(17) 0.0309(5) Uani 1 1 d . . . . .


_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 C3 2.127(2) 6 ?
Mo1 C3 2.127(2) . ?
Mo1 C4 2.147(2) 6 ?
Mo1 C4 2.147(2) . ?
Mo1 C2 2.164(2) 6 ?
Mo1 C2 2.164(2) . ?
Mo1 C1 2.180(3) . ?
Mn1 N4 2.099(2) 4_545 ?
Mn1 N4 2.099(2) 7 ?
Mn1 N1 2.149(3) . ?
Mn1 N7 2.168(3) . ?
Mn1 N6 2.288(3) . ?
Mn2 N2 2.196(2) . ?
Mn2 N2 2.196(2) 6_565 ?
Mn2 N2 2.196(2) 2_655 ?
Mn2 N2 2.196(2) 5_665 ?
Mn2 N5 2.355(4) . ?
Mn2 N5 2.355(4) 5_665 ?
Mn3 N3 2.216(2) . ?
Mn3 N3 2.216(2) 5_666 ?
Mn3 N3 2.216(2) 6_565 ?
Mn3 N3 2.216(2) 2_656 ?
Mn3 O1 2.279(3) 5_666 ?
Mn3 O1 2.279(3) . ?
C1 N1 1.146(4) . ?
N7 C12 1.324(4) . ?
N7 C14 1.379(5) . ?
C3 N3 1.156(3) . ?
C2 N2 1.151(3) . ?
O1 H1 0.8260 . ?
N6 C7 1.331(4) . ?
N6 C11 1.344(4) . ?
C11 C10 1.369(5) . ?
C11 C12 1.458(5) . ?
N8 C12 1.343(5) . ?
N8 C13 1.382(6) . ?
N8 H8 0.8600 . ?
C7 C8 1.374(6) . ?
C7 H7 0.9300 . ?
C5 N5 1.172(6) . ?
C5 C6 1.430(6) . ?
C13 C14 1.339(6) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C10 C9 1.354(6) . ?
C10 H10 0.9300 . ?
C8 C9 1.349(6) . ?
C8 H8A 0.9300 . ?
C9 H9 0.9300 . ?
C4 N4 1.154(3) . ?
N4 Mn1 2.099(2) 7 ?

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
C3 Mo1 C3 74.58(12) 6 . ?
C3 Mo1 C4 75.47(8) 6 6 ?
C3 Mo1 C4 120.77(9) . 6 ?
C3 Mo1 C4 120.78(9) 6 . ?
C3 Mo1 C4 75.47(8) . . ?
C4 Mo1 C4 78.00(12) 6 . ?
C3 Mo1 C2 77.38(8) 6 6 ?
C3 Mo1 C2 124.87(9) . 6 ?
C4 Mo1 C2 95.96(9) 6 6 ?
C4 Mo1 C2 157.62(8) . 6 ?
C3 Mo1 C2 124.87(8) 6 . ?
C3 Mo1 C2 77.38(8) . . ?
C4 Mo1 C2 157.62(8) 6 . ?
C4 Mo1 C2 95.97(9) . . ?
C2 Mo1 C2 81.40(12) 6 . ?
C3 Mo1 C1 142.56(6) 6 . ?
C3 Mo1 C1 142.56(6) . . ?
C4 Mo1 C1 77.77(8) 6 . ?
C4 Mo1 C1 77.77(8) . . ?
C2 Mo1 C1 79.89(8) 6 . ?
C2 Mo1 C1 79.89(8) . . ?
N4 Mn1 N4 99.27(12) 4_545 7 ?
N4 Mn1 N1 100.48(8) 4_545 . ?
N4 Mn1 N1 100.48(8) 7 . ?
N4 Mn1 N7 128.62(6) 4_545 . ?
N4 Mn1 N7 128.62(6) 7 . ?
N1 Mn1 N7 89.17(11) . . ?
N4 Mn1 N6 90.26(7) 4_545 . ?
N4 Mn1 N6 90.26(7) 7 . ?
N1 Mn1 N6 163.29(11) . . ?
N7 Mn1 N6 74.12(10) . . ?
N2 Mn2 N2 86.29(12) . 6_565 ?
N2 Mn2 N2 93.71(12) . 2_655 ?
N2 Mn2 N2 180.00(11) 6_565 2_655 ?
N2 Mn2 N2 180.00(10) . 5_665 ?
N2 Mn2 N2 93.71(12) 6_565 5_665 ?
N2 Mn2 N2 86.29(12) 2_655 5_665 ?
N2 Mn2 N5 92.60(9) . . ?
N2 Mn2 N5 92.60(9) 6_565 . ?
N2 Mn2 N5 87.40(9) 2_655 . ?
N2 Mn2 N5 87.40(9) 5_665 . ?
N2 Mn2 N5 87.40(9) . 5_665 ?
N2 Mn2 N5 87.40(9) 6_565 5_665 ?
N2 Mn2 N5 92.60(9) 2_655 5_665 ?
N2 Mn2 N5 92.60(9) 5_665 5_665 ?
N5 Mn2 N5 180.0 . 5_665 ?
N3 Mn3 N3 180.0 . 5_666 ?
N3 Mn3 N3 92.14(11) . 6_565 ?
N3 Mn3 N3 87.86(11) 5_666 6_565 ?
N3 Mn3 N3 87.86(11) . 2_656 ?
N3 Mn3 N3 92.14(11) 5_666 2_656 ?
N3 Mn3 N3 180.00(10) 6_565 2_656 ?
N3 Mn3 O1 95.52(7) . 5_666 ?
N3 Mn3 O1 84.48(7) 5_666 5_666 ?
N3 Mn3 O1 95.52(7) 6_565 5_666 ?
N3 Mn3 O1 84.48(7) 2_656 5_666 ?
N3 Mn3 O1 84.48(7) . . ?
N3 Mn3 O1 95.52(7) 5_666 . ?
N3 Mn3 O1 84.48(7) 6_565 . ?
N3 Mn3 O1 95.52(7) 2_656 . ?
O1 Mn3 O1 180.0 5_666 . ?
N1 C1 Mo1 176.4(3) . . ?
C1 N1 Mn1 178.8(3) . . ?
C12 N7 C14 106.3(3) . . ?
C12 N7 Mn1 115.7(2) . . ?
C14 N7 Mn1 138.1(3) . . ?
N3 C3 Mo1 177.2(2) . . ?
C3 N3 Mn3 153.8(2) . . ?
N2 C2 Mo1 176.9(2) . . ?
Mn3 O1 H1 120.3 . . ?
C7 N6 C11 117.7(3) . . ?
C7 N6 Mn1 127.1(3) . . ?
C11 N6 Mn1 115.3(2) . . ?
C2 N2 Mn2 164.8(2) . . ?
N6 C11 C10 122.6(3) . . ?
N6 C11 C12 113.4(3) . . ?
C10 C11 C12 124.0(3) . . ?
C12 N8 C13 107.6(3) . . ?
C12 N8 H8 126.2 . . ?
C13 N8 H8 126.2 . . ?
N6 C7 C8 121.9(4) . . ?
N6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
N7 C12 N8 110.2(3) . . ?
N7 C12 C11 121.6(3) . . ?
N8 C12 C11 128.2(3) . . ?
N5 C5 C6 178.0(5) . . ?
C5 N5 Mn2 123.1(3) . . ?
C14 C13 N8 106.2(3) . . ?
C14 C13 H13 126.9 . . ?
N8 C13 H13 126.9 . . ?
C13 C14 N7 109.6(4) . . ?
C13 C14 H14 125.2 . . ?
N7 C14 H14 125.2 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C9 C10 C11 118.6(4) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C9 C8 C7 119.4(4) . . ?
C9 C8 H8A 120.3 . . ?
C7 C8 H8A 120.3 . . ?
C8 C9 C10 119.9(4) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N4 C4 Mo1 175.6(2) . . ?
C4 N4 Mn1 165.0(2) . 7 ?

_refine_diff_density_max         0.353
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.072

####################################################################### 
# 
# 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_MnMo1-Pypz
_database_code_depnum_ccdc_archive 'CCDC 1835918'
_audit_update_record             
;
2018-04-28 deposited with the CCDC.
2018-05-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     'Sheldrick, 2014'
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H12 Mn2 Mo N11 O'
_chemical_formula_weight         592.20

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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   24.442(6)
_cell_length_b                   7.2801(16)
_cell_length_c                   12.456(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.200(3)
_cell_angle_gamma                90
_cell_volume                     2148.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2403
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      27.38

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_F_000             1164
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.767
_shelx_estimated_absorpt_T_min   0.708
_shelx_estimated_absorpt_T_max   0.742
_exptl_absorpt_correction_type   multi-Scan
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_process_details   'SADABS: Bruker, 2000'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7334
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.686
_diffrn_reflns_theta_max         27.592
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2678
_reflns_number_gt                2264
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0406P)²+8.2808P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2678
_refine_ls_number_parameters     182
_refine_ls_number_restraints     158
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0852
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.070
_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 0.39410(2) 0.0000 0.20712(3) 0.01148(11) Uani 1 2 d S T P . .
Mn1 Mn 0.26520(3) 0.0000 -0.21990(5) 0.01515(17) Uani 1 2 d S T P . .
Mn2 Mn 0.5000 0.5000 0.0000 0.0160(2) Uani 1 4 d S TU P . .
Mn3 Mn 0.5000 0.5000 0.5000 0.0163(2) Uani 1 4 d S T P . .
N7 N 0.2381(2) 0.0000 -0.4068(3) 0.0276(10) Uani 1 2 d S T P . .
C3 C 0.42636(14) 0.1783(4) 0.3432(3) 0.0174(6) Uani 1 1 d . U . . .
C2 C 0.44318(14) 0.1950(5) 0.1391(3) 0.0192(6) Uani 1 1 d . U . . .
N6 N 0.3417(2) 0.0000 -0.2803(4) 0.0331(11) Uani 1 2 d S T P . .
C4 C 0.32612(14) 0.1846(5) 0.2107(3) 0.0179(6) Uani 1 1 d . U . . .
N1 N 0.31907(17) 0.0000 -0.0553(3) 0.0209(9) Uani 1 2 d S T P . .
C10 C 0.2784(3) 0.0000 -0.4595(5) 0.0366(9) Uani 1 2 d S TU P . .
C14 C 0.1855(3) 0.0000 -0.4701(5) 0.0404(11) Uani 1 2 d S TU P . .
H14 H 0.1552 0.0000 -0.4373 0.048 Uiso 1 2 calc R U P . .
N8 N 0.3354(2) 0.0000 -0.3913(4) 0.0344(11) Uani 1 2 d S T P . .
C8 C 0.4296(3) 0.0000 -0.3128(5) 0.0416(12) Uani 1 2 d S TU P . .
H8 H 0.4687 0.0000 -0.3005 0.050 Uiso 1 2 calc R U P . .
C13 C 0.1758(3) 0.0000 -0.5833(5) 0.0445(12) Uani 1 2 d S TU P . .
H13 H 0.1389 0.0000 -0.6269 0.053 Uiso 1 2 calc R U P . .
C9 C 0.3877(3) 0.0000 -0.4171(6) 0.0452(11) Uani 1 2 d S TU P . .
H9 H 0.3944 0.0000 -0.4875 0.054 Uiso 1 2 calc R U P . .
C7 C 0.3973(3) 0.0000 -0.2346(5) 0.0401(12) Uani 1 2 d S TU P . .
H7 H 0.4128 0.0000 -0.1585 0.048 Uiso 1 2 calc R U P . .
C11 C 0.2718(3) 0.0000 -0.5729(5) 0.0470(11) Uani 1 2 d S TU P . .
H11 H 0.3021 0.0000 -0.6057 0.056 Uiso 1 2 calc R U P . .
C12 C 0.2186(3) 0.0000 -0.6304(6) 0.0506(12) Uani 1 2 d S TU P . .
H12 H 0.2111 0.0000 -0.7073 0.061 Uiso 1 2 calc R U P . .
N2 N 0.47035(13) 0.2931(4) 0.1008(2) 0.0258(7) Uani 1 1 d . U . . .
N3 N 0.44383(13) 0.2826(4) 0.4129(2) 0.0246(7) Uani 1 1 d . . . . .
O1 O 0.53467(18) 0.5000 0.3442(3) 0.0312(9) Uani 1 2 d DS T P . .
C1 C 0.3463(2) 0.0000 0.0345(4) 0.0183(9) Uani 1 2 d S TU P . .
C5 C 0.6338(2) 0.5000 0.0780(5) 0.0321(12) Uani 1 2 d S TU P . .
N5 N 0.5931(2) 0.5000 0.1121(4) 0.0394(12) Uani 1 2 d S TU P . .
C6 C 0.6811(2) 0.5000 0.0312(5) 0.0308(12) Uani 1 2 d S TU P . .
H6A H 0.7108 0.5726 0.0764 0.046 Uiso 0.5 1 calc R U P . .
H6B H 0.6705 0.5511 -0.0420 0.046 Uiso 0.5 1 calc R U P . .
H6C H 0.6941 0.3763 0.0275 0.046 Uiso 0.5 1 calc R U P . .
N4 N 0.28783(12) 0.2783(4) 0.2092(2) 0.0235(6) Uani 1 1 d . . . . .
H1 H 0.528(3) 0.600(5) 0.311(5) 0.11(3) Uiso 1 1 d D . . . .


_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 C3 2.127(3) 6 ?
Mo1 C3 2.127(3) . ?
Mo1 C4 2.146(3) . ?
Mo1 C4 2.146(3) 6 ?
Mo1 C2 2.161(3) 6 ?
Mo1 C2 2.161(3) . ?
Mo1 C1 2.181(5) . ?
Mn1 N4 2.095(3) 4_545 ?
Mn1 N4 2.095(3) 7 ?
Mn1 N1 2.148(4) . ?
Mn1 N6 2.180(5) . ?
Mn1 N7 2.259(4) . ?
Mn2 N2 2.195(3) 6_565 ?
Mn2 N2 2.195(3) 2_655 ?
Mn2 N2 2.195(3) 5_665 ?
Mn2 N2 2.195(3) . ?
Mn2 N5 2.360(5) 5_665 ?
Mn2 N5 2.360(5) . ?
Mn3 N3 2.199(3) 5_666 ?
Mn3 N3 2.199(3) 6_565 ?
Mn3 N3 2.199(3) 2_656 ?
Mn3 N3 2.199(3) . ?
Mn3 O1 2.301(4) 5_666 ?
Mn3 O1 2.301(4) . ?
N7 C10 1.311(8) . ?
N7 C14 1.333(8) . ?
C3 N3 1.154(4) . ?
C2 N2 1.154(4) . ?
N6 C7 1.337(8) . ?
N6 N8 1.354(7) . ?
C4 N4 1.154(4) . ?
N1 C1 1.152(6) . ?
C10 C11 1.382(9) . ?
C10 N8 1.443(8) . ?
C14 C13 1.371(8) . ?
C14 H14 0.9300 . ?
N8 C9 1.393(8) . ?
C8 C7 1.398(9) . ?
C8 C9 1.444(9) . ?
C8 H8 0.9300 . ?
C13 C12 1.321(10) . ?
C13 H13 0.9300 . ?
C9 H9 0.9300 . ?
C7 H7 0.9300 . ?
C11 C12 1.322(10) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
O1 H1 0.83(2) . ?
C5 N5 1.173(8) . ?
C5 C6 1.417(8) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N4 Mn1 2.095(3) 7 ?

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
C3 Mo1 C3 75.20(17) 6 . ?
C3 Mo1 C4 120.20(12) 6 . ?
C3 Mo1 C4 74.86(12) . . ?
C3 Mo1 C4 74.86(12) 6 6 ?
C3 Mo1 C4 120.20(12) . 6 ?
C4 Mo1 C4 77.54(18) . 6 ?
C3 Mo1 C2 77.22(12) 6 6 ?
C3 Mo1 C2 125.47(13) . 6 ?
C4 Mo1 C2 157.91(12) . 6 ?
C4 Mo1 C2 95.97(13) 6 6 ?
C3 Mo1 C2 125.47(13) 6 . ?
C3 Mo1 C2 77.22(12) . . ?
C4 Mo1 C2 95.97(13) . . ?
C4 Mo1 C2 157.91(12) 6 . ?
C2 Mo1 C2 82.11(17) 6 . ?
C3 Mo1 C1 142.19(9) 6 . ?
C3 Mo1 C1 142.19(9) . . ?
C4 Mo1 C1 77.91(13) . . ?
C4 Mo1 C1 77.91(13) 6 . ?
C2 Mo1 C1 80.09(13) 6 . ?
C2 Mo1 C1 80.09(13) . . ?
N4 Mn1 N4 100.81(17) 4_545 7 ?
N4 Mn1 N1 100.54(11) 4_545 . ?
N4 Mn1 N1 100.54(11) 7 . ?
N4 Mn1 N6 128.21(9) 4_545 . ?
N4 Mn1 N6 128.21(9) 7 . ?
N1 Mn1 N6 87.28(17) . . ?
N4 Mn1 N7 92.07(11) 4_545 . ?
N4 Mn1 N7 92.07(11) 7 . ?
N1 Mn1 N7 160.07(17) . . ?
N6 Mn1 N7 72.79(18) . . ?
N2 Mn2 N2 180.00(16) 6_565 2_655 ?
N2 Mn2 N2 93.33(16) 6_565 5_665 ?
N2 Mn2 N2 86.67(16) 2_655 5_665 ?
N2 Mn2 N2 86.67(16) 6_565 . ?
N2 Mn2 N2 93.33(16) 2_655 . ?
N2 Mn2 N2 180.0 5_665 . ?
N2 Mn2 N5 86.15(13) 6_565 5_665 ?
N2 Mn2 N5 93.85(13) 2_655 5_665 ?
N2 Mn2 N5 93.85(13) 5_665 5_665 ?
N2 Mn2 N5 86.15(13) . 5_665 ?
N2 Mn2 N5 93.85(13) 6_565 . ?
N2 Mn2 N5 86.15(13) 2_655 . ?
N2 Mn2 N5 86.15(13) 5_665 . ?
N2 Mn2 N5 93.85(13) . . ?
N5 Mn2 N5 180.0 5_665 . ?
N3 Mn3 N3 87.93(15) 5_666 6_565 ?
N3 Mn3 N3 92.07(15) 5_666 2_656 ?
N3 Mn3 N3 180.00(14) 6_565 2_656 ?
N3 Mn3 N3 180.0 5_666 . ?
N3 Mn3 N3 92.07(16) 6_565 . ?
N3 Mn3 N3 87.93(16) 2_656 . ?
N3 Mn3 O1 84.17(11) 5_666 5_666 ?
N3 Mn3 O1 95.83(11) 6_565 5_666 ?
N3 Mn3 O1 84.17(11) 2_656 5_666 ?
N3 Mn3 O1 95.83(11) . 5_666 ?
N3 Mn3 O1 95.83(11) 5_666 . ?
N3 Mn3 O1 84.17(11) 6_565 . ?
N3 Mn3 O1 95.83(11) 2_656 . ?
N3 Mn3 O1 84.17(11) . . ?
O1 Mn3 O1 180.0 5_666 . ?
C10 N7 C14 116.0(5) . . ?
C10 N7 Mn1 116.7(4) . . ?
C14 N7 Mn1 127.3(4) . . ?
N3 C3 Mo1 176.3(3) . . ?
N2 C2 Mo1 177.1(3) . . ?
C7 N6 N8 106.5(5) . . ?
C7 N6 Mn1 136.1(4) . . ?
N8 N6 Mn1 117.4(4) . . ?
N4 C4 Mo1 176.7(3) . . ?
C1 N1 Mn1 177.6(4) . . ?
N7 C10 C11 126.8(6) . . ?
N7 C10 N8 116.2(5) . . ?
C11 C10 N8 117.0(6) . . ?
N7 C14 C13 120.5(6) . . ?
N7 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
N6 N8 C9 110.8(5) . . ?
N6 N8 C10 116.9(5) . . ?
C9 N8 C10 132.3(5) . . ?
C7 C8 C9 103.2(6) . . ?
C7 C8 H8 128.4 . . ?
C9 C8 H8 128.4 . . ?
C12 C13 C14 120.1(7) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
N8 C9 C8 106.3(5) . . ?
N8 C9 H9 126.8 . . ?
C8 C9 H9 126.8 . . ?
N6 C7 C8 113.1(6) . . ?
N6 C7 H7 123.4 . . ?
C8 C7 H7 123.4 . . ?
C12 C11 C10 114.0(7) . . ?
C12 C11 H11 123.0 . . ?
C10 C11 H11 123.0 . . ?
C13 C12 C11 122.7(7) . . ?
C13 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C2 N2 Mn2 164.7(3) . . ?
C3 N3 Mn3 156.3(3) . . ?
Mn3 O1 H1 110(5) . . ?
N1 C1 Mo1 177.2(4) . . ?
N5 C5 C6 177.0(6) . . ?
C5 N5 Mn2 124.4(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 N4 Mn1 165.0(3) . 7 ?

_refine_diff_density_max         1.610
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.114

