# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_s
_database_code_depnum_ccdc_archive 'CCDC 1909095'
loop_
_audit_author_name
_audit_author_address
'Jun Qian'
;Jiangsu university
China
;
_audit_update_record             
;
2019-04-10 deposited with the CCDC.	2019-06-21 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            'C33 H16 Mn2 N17 O6 W'
_chemical_formula_weight         1040.36

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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'
'-x, -y, z'
'y, -x, z'
'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, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-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'

_cell_length_a                   14.470(2)
_cell_length_b                   14.470(2)
_cell_length_c                   28.017(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5866(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2880
_cell_measurement_theta_min      2.8154
_cell_measurement_theta_max      28.7858

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_F_000             2020
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_exptl_absorpt_coefficient_mu    2.425
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7368
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.169
_diffrn_reflns_theta_max         26.003
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             2880
_reflns_number_gt                2651
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_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)+(0.0742P)²+40.3077P] 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_number_reflns         2880
_refine_ls_number_parameters     139
_refine_ls_number_restraints     228
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1438
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_restrained_S_all      1.409
_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
W1 W 0.0000 0.0000 0.31522(2) 0.01974(18) Uani 1 4 d S TU P . .
Mn1 Mn 0.2500 0.2500 0.2500 0.0394(4) Uani 1 2 d S . P . .
O1 O 0.1525(7) 0.3593(7) 0.2713(4) 0.117(3) Uani 1 1 d . . . . .
O2 O 0.1251(5) 0.2210(5) 0.0000 0.0360(15) Uani 1 2 d S T P . .
N1 N 0.0000 0.0000 0.1960(4) 0.039(2) Uani 1 4 d S TU P . .
N2 N 0.1591(6) 0.1468(6) 0.2790(2) 0.0626(16) Uani 1 1 d . U . . .
N3 N 0.1832(5) 0.2362(5) 0.1761(2) 0.0443(14) Uani 1 1 d . U . . .
N4 N -0.0101(4) 0.1731(5) 0.0249(2) 0.0423(14) Uani 1 1 d . U . . .
N5 N 0.0151(10) 0.1831(9) 0.3913(4) 0.120(3) Uani 1 1 d . U . . .
C1 C 0.1034(5) 0.0953(5) 0.2929(3) 0.0422(15) Uani 1 1 d . U . . .
C2 C 0.0000 0.0000 0.2376(4) 0.028(2) Uani 1 4 d S TU P . .
C3 C 0.2276(6) 0.2667(7) 0.1375(3) 0.0566(17) Uani 1 1 d . U . . .
H3 H 0.2841 0.2963 0.1413 0.068 Uiso 1 1 calc R U . . .
C4 C 0.1918(6) 0.2556(7) 0.0920(3) 0.0567(17) Uani 1 1 d . U . . .
H4 H 0.2248 0.2770 0.0657 0.068 Uiso 1 1 calc R U . . .
C5 C 0.1033(5) 0.1941(6) 0.1696(3) 0.0445(14) Uani 1 1 d . U . . .
H5 H 0.0715 0.1726 0.1962 0.053 Uiso 1 1 calc R U . . .
C6 C 0.0645(5) 0.1806(6) 0.1248(2) 0.0468(15) Uani 1 1 d . U . . .
H6 H 0.0088 0.1491 0.1218 0.056 Uiso 1 1 calc R U . . .
C7 C 0.1080(5) 0.2134(5) 0.0856(2) 0.0375(13) Uani 1 1 d . U . . .
C8 C 0.0703(5) 0.2005(5) 0.0378(2) 0.0367(13) Uani 1 1 d . U . . .
C9 C 0.0141(6) 0.1105(5) 0.3655(3) 0.0438(10) Uani 1 1 d . U . . .


_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
W1 C1 2.129(7) 3 ?
W1 C1 2.129(7) 4 ?
W1 C1 2.129(7) 2 ?
W1 C1 2.129(7) . ?
W1 C9 2.140(7) . ?
W1 C9 2.140(7) 4 ?
W1 C9 2.140(7) 3 ?
W1 C9 2.140(7) 2 ?
W1 C2 2.175(12) . ?
Mn1 N2 2.149(7) . ?
Mn1 N2 2.149(7) 13 ?
Mn1 O1 2.202(9) 13 ?
Mn1 O1 2.202(9) . ?
Mn1 N3 2.294(6) 13 ?
Mn1 N3 2.294(6) . ?
O2 C8 1.356(7) . ?
O2 C8 1.356(7) 11 ?
N1 C2 1.165(17) . ?
N2 C1 1.165(10) . ?
N3 C5 1.319(9) . ?
N3 C3 1.333(10) . ?
N4 C8 1.281(9) . ?
N4 N4 1.396(11) 11 ?
N5 C9 1.276(13) . ?
C3 C4 1.386(11) . ?
C3 H3 0.9300 . ?
C4 C7 1.370(10) . ?
C4 H4 0.9300 . ?
C5 C6 1.388(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.352(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.457(9) . ?

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 W1 C1 85.05(11) 3 4 ?
C1 W1 C1 85.05(11) 3 2 ?
C1 W1 C1 145.8(4) 4 2 ?
C1 W1 C1 145.8(4) 3 . ?
C1 W1 C1 85.05(11) 4 . ?
C1 W1 C1 85.05(11) 2 . ?
C1 W1 C9 138.1(3) 3 . ?
C1 W1 C9 131.0(3) 4 . ?
C1 W1 C9 74.3(3) 2 . ?
C1 W1 C9 69.0(3) . . ?
C1 W1 C9 131.0(3) 3 4 ?
C1 W1 C9 69.0(3) 4 4 ?
C1 W1 C9 138.1(3) 2 4 ?
C1 W1 C9 74.3(3) . 4 ?
C9 W1 C9 64.4(2) . 4 ?
C1 W1 C9 69.0(3) 3 3 ?
C1 W1 C9 74.3(3) 4 3 ?
C1 W1 C9 131.0(3) 2 3 ?
C1 W1 C9 138.1(3) . 3 ?
C9 W1 C9 97.7(4) . 3 ?
C9 W1 C9 64.4(2) 4 3 ?
C1 W1 C9 74.3(3) 3 2 ?
C1 W1 C9 138.1(3) 4 2 ?
C1 W1 C9 69.0(3) 2 2 ?
C1 W1 C9 131.0(3) . 2 ?
C9 W1 C9 64.4(2) . 2 ?
C9 W1 C9 97.7(4) 4 2 ?
C9 W1 C9 64.4(2) 3 2 ?
C1 W1 C2 72.92(19) 3 . ?
C1 W1 C2 72.92(19) 4 . ?
C1 W1 C2 72.92(19) 2 . ?
C1 W1 C2 72.92(19) . . ?
C9 W1 C2 131.1(2) . . ?
C9 W1 C2 131.1(2) 4 . ?
C9 W1 C2 131.1(2) 3 . ?
C9 W1 C2 131.1(2) 2 . ?
N2 Mn1 N2 180.0 . 13 ?
N2 Mn1 O1 89.7(4) . 13 ?
N2 Mn1 O1 90.3(4) 13 13 ?
N2 Mn1 O1 90.3(4) . . ?
N2 Mn1 O1 89.7(4) 13 . ?
O1 Mn1 O1 180.0 13 . ?
N2 Mn1 N3 88.7(2) . 13 ?
N2 Mn1 N3 91.3(2) 13 13 ?
O1 Mn1 N3 92.1(3) 13 13 ?
O1 Mn1 N3 87.9(3) . 13 ?
N2 Mn1 N3 91.3(2) . . ?
N2 Mn1 N3 88.7(2) 13 . ?
O1 Mn1 N3 87.9(3) 13 . ?
O1 Mn1 N3 92.1(3) . . ?
N3 Mn1 N3 180.0 13 . ?
C8 O2 C8 102.8(7) . 11 ?
C1 N2 Mn1 173.9(8) . . ?
C5 N3 C3 117.5(6) . . ?
C5 N3 Mn1 122.3(5) . . ?
C3 N3 Mn1 120.0(5) . . ?
C8 N4 N4 106.4(4) . 11 ?
N2 C1 W1 177.5(6) . . ?
N1 C2 W1 180.0 . . ?
N3 C3 C4 121.9(7) . . ?
N3 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C7 C4 C3 120.2(7) . . ?
C7 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
N3 C5 C6 123.0(7) . . ?
N3 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C7 C6 C5 119.8(6) . . ?
C7 C6 H6 120.1 . . ?
C5 C6 H6 120.1 . . ?
C6 C7 C4 117.5(6) . . ?
C6 C7 C8 121.8(6) . . ?
C4 C7 C8 120.6(6) . . ?
N4 C8 O2 112.2(6) . . ?
N4 C8 C7 129.7(6) . . ?
O2 C8 C7 118.1(6) . . ?
N5 C9 W1 171.6(8) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N3 C3 C4 0.3(14) . . . . ?
Mn1 N3 C3 C4 176.8(8) . . . . ?
N3 C3 C4 C7 0.8(16) . . . . ?
C3 N3 C5 C6 0.1(14) . . . . ?
Mn1 N3 C5 C6 -176.2(7) . . . . ?
N3 C5 C6 C7 -1.7(14) . . . . ?
C5 C6 C7 C4 2.8(13) . . . . ?
C5 C6 C7 C8 179.7(8) . . . . ?
C3 C4 C7 C6 -2.4(14) . . . . ?
C3 C4 C7 C8 -179.4(9) . . . . ?
N4 N4 C8 O2 1.1(7) 11 . . . ?
N4 N4 C8 C7 -180.0(7) 11 . . . ?
C8 O2 C8 N4 -1.7(11) 11 . . . ?
C8 O2 C8 C7 179.2(4) 11 . . . ?
C6 C7 C8 N4 12.3(13) . . . . ?
C4 C7 C8 N4 -170.8(9) . . . . ?
C6 C7 C8 O2 -168.8(8) . . . . ?
C4 C7 C8 O2 8.1(12) . . . . ?

_refine_diff_density_max         1.487
_refine_diff_density_min         -3.213
_refine_diff_density_rms         0.169



####################################################################### 
# 
# 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_a_sq_s
_audit_block_doi                 10.5517/cczth4d
_database_code_depnum_ccdc_archive 'CCDC 918224'
loop_
_audit_author_name
_audit_author_address
'Jun Qian'
;Jiangsu university
China
;
_audit_update_record             
;
2019-04-10 deposited with the CCDC.	2019-06-21 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            'C45 H44 Mn2 Mo N21 O10'
_chemical_formula_weight         1244.83

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'
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'
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'
H H 0.0000 0.0000 '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'
'-x, -y, z'
'y, -x, z'
'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, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-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'

_cell_length_a                   14.450(2)
_cell_length_b                   14.450(2)
_cell_length_c                   28.044(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5856(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3030
_cell_measurement_theta_min      3.172
_cell_measurement_theta_max      26.363

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             2595
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.710
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_process_details   'SADABS(Bruker, 2002)'
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11222
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         3.172
_diffrn_reflns_theta_max         26.363
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             3030
_reflns_number_gt                2841
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    SHELXL
_computing_publication_material  SHELXL
_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)+(0.1134P)²+15.4149P] 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_number_reflns         3030
_refine_ls_number_parameters     296
_refine_ls_number_restraints     333
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1879
_refine_ls_wR_factor_gt          0.1840
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.002
_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 0.0000 0.0000 0.31542(2) 0.0259(2) Uani 1 4 d S T P . .
Mn1 Mn 0.2500 0.2500 0.2500 0.0477(3) Uani 1 2 d S . P . .
C1 C 0.0000 0.0000 0.2375(3) 0.0313(15) Uani 1 4 d S T P . .
N1 N 0.0000 0.0000 0.1960(2) 0.0329(13) Uani 1 4 d S T P . .
C2 C 0.0876(15) 0.1115(14) 0.2914(9) 0.039(3) Uani 0.59(3) 1 d . U P A 1
N2 N 0.1346(11) 0.1692(11) 0.2774(4) 0.044(3) Uani 0.59(3) 1 d . U P A 1
C2' C 0.106(2) 0.092(2) 0.2948(12) 0.040(3) Uani 0.41(3) 1 d . U P A 2
N2' N 0.1651(15) 0.1409(14) 0.2817(6) 0.042(3) Uani 0.41(3) 1 d . U P A 2
C3 C -0.1170(13) -0.0062(18) 0.3634(7) 0.079(4) Uani 0.457(3) 1 d . U P B 1
N3 N -0.1787(10) -0.0136(12) 0.3885(5) 0.100(4) Uani 0.457(3) 1 d . U P B 1
C3' C -0.075(2) 0.047(3) 0.3744(9) 0.081(4) Uani 0.299(3) 1 d . U P A 2
N3' N -0.1243(15) 0.0627(18) 0.4075(7) 0.092(4) Uani 0.299(3) 1 d . U P A 2
C3'' C -0.094(3) -0.040(4) 0.3710(14) 0.080(4) Uani 0.244(3) 1 d . U P A 3
N3'' N -0.1337(19) -0.069(2) 0.4043(8) 0.088(5) Uani 0.244(3) 1 d . U P A 3
O1 O 0.2182(3) 0.1267(3) 0.0000 0.0386(9) Uani 1 2 d S T P . .
N4 N 0.2338(3) 0.1848(3) 0.17631(13) 0.0505(10) Uani 1 1 d . . . . .
N5 N 0.1723(3) -0.0102(3) 0.02515(12) 0.0487(9) Uani 1 1 d . . . . .
C5 C 0.2626(5) 0.2287(4) 0.13749(19) 0.0742(18) Uani 1 1 d . U . . .
H5 H 0.2919 0.2855 0.1413 0.089 Uiso 1 1 calc R U . . .
C6 C 0.2517(5) 0.1949(4) 0.09182(17) 0.0718(18) Uani 1 1 d . U . . .
H6 H 0.2712 0.2293 0.0657 0.086 Uiso 1 1 calc R U . . .
C7 C 0.2112(3) 0.1092(3) 0.08560(13) 0.0390(9) Uani 1 1 d . . . . .
C8 C 0.1811(3) 0.0633(3) 0.12527(15) 0.0505(12) Uani 1 1 d . . . . .
H8 H 0.1524 0.0059 0.1224 0.061 Uiso 1 1 calc R U . . .
C9 C 0.1935(4) 0.1030(4) 0.16952(16) 0.0544(13) Uani 1 1 d . . . . .
H9 H 0.1725 0.0707 0.1961 0.065 Uiso 1 1 calc R U . . .
C10 C 0.1991(3) 0.0713(3) 0.03790(13) 0.0360(9) Uani 1 1 d . . . . .
O2A O 0.3639(16) 0.1538(14) 0.2659(6) 0.105(4) Uani 0.571(8) 1 d . U P A 1
C1A C 0.4189(14) 0.1216(14) 0.3802(8) 0.177(3) Uani 0.571(8) 1 d D U P A 1
H1AA H 0.4285 0.1366 0.3472 0.265 Uiso 0.571(8) 1 calc R U P A 1
H1AB H 0.4755 0.0985 0.3936 0.265 Uiso 0.571(8) 1 calc R U P A 1
H1AC H 0.4001 0.1762 0.3971 0.265 Uiso 0.571(8) 1 calc R U P A 1
C2A C 0.2983(15) 0.0435(15) 0.4311(6) 0.180(4) Uani 0.571(8) 1 d D U P A 1
H2AA H 0.3363 0.0091 0.4529 0.270 Uiso 0.571(8) 1 calc R U P A 1
H2AB H 0.2399 0.0126 0.4273 0.270 Uiso 0.571(8) 1 calc R U P A 1
H2AC H 0.2882 0.1046 0.4435 0.270 Uiso 0.571(8) 1 calc R U P A 1
N1A N 0.3456(10) 0.0498(10) 0.3842(6) 0.176(4) Uani 0.571(8) 1 d D U P A 1
C3A C 0.3234(14) -0.0008(16) 0.3508(7) 0.174(3) Uani 0.571(8) 1 d D U P A 1
H3A H 0.2747 -0.0419 0.3554 0.209 Uiso 0.571(8) 1 calc R U P A 1
O1A O 0.3640(11) 0.0000(12) 0.3096(5) 0.157(5) Uani 0.571(8) 1 d D U P A 1
C1B C 0.4818(19) 0.103(2) 0.3253(12) 0.176(4) Uani 0.429(8) 1 d D U P A 2
H1BA H 0.5137 0.0993 0.2953 0.263 Uiso 0.429(8) 1 calc R U P A 2
H1BB H 0.5200 0.0767 0.3499 0.263 Uiso 0.429(8) 1 calc R U P A 2
H1BC H 0.4686 0.1662 0.3327 0.263 Uiso 0.429(8) 1 calc R U P A 2
C2B C 0.382(2) -0.0375(18) 0.3508(11) 0.176(3) Uani 0.429(8) 1 d D U P A 2
H2BA H 0.3190 -0.0585 0.3489 0.264 Uiso 0.429(8) 1 calc R U P A 2
H2BB H 0.3975 -0.0252 0.3835 0.264 Uiso 0.429(8) 1 calc R U P A 2
H2BC H 0.4224 -0.0844 0.3384 0.264 Uiso 0.429(8) 1 calc R U P A 2
N1B N 0.3927(17) 0.0492(15) 0.3221(8) 0.174(4) Uani 0.429(8) 1 d D U P A 2
C3B C 0.331(2) 0.079(2) 0.2961(10) 0.174(3) Uani 0.429(8) 1 d D U P A 2
H3B H 0.2742 0.0495 0.2933 0.209 Uiso 0.429(8) 1 calc R U P A 2
O1B O 0.350(3) 0.154(3) 0.2729(12) 0.147(5) Uani 0.429(8) 1 d D U P A 2
O2B O 0.380(2) 0.112(2) 0.4578(10) 0.253(9) Uiso 0.429(8) 1 d . U P A 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
Mo1 C3' 2.09(3) . ?
Mo1 C3' 2.09(3) 4 ?
Mo1 C3' 2.09(3) 3 ?
Mo1 C3' 2.09(3) 2 ?
Mo1 C2' 2.11(4) 3 ?
Mo1 C2' 2.11(4) 4 ?
Mo1 C2' 2.11(4) 2 ?
Mo1 C2' 2.11(4) . ?
Mo1 C3'' 2.15(4) 3 ?
Mo1 C3'' 2.15(4) 4 ?
Mo1 C3'' 2.15(4) 2 ?
Mo1 C3'' 2.15(4) . ?
Mn1 O1B 2.10(4) 13 ?
Mn1 O1B 2.10(4) . ?
Mn1 N2 2.177(12) 13 ?
Mn1 N2 2.177(12) . ?
Mn1 N2' 2.186(18) . ?
Mn1 N2' 2.186(18) 13 ?
Mn1 O2A 2.200(17) . ?
Mn1 O2A 2.200(17) 13 ?
Mn1 N4 2.284(4) 13 ?
Mn1 N4 2.284(3) . ?
C1 N1 1.166(10) . ?
C2 N2 1.144(18) . ?
C2' N2' 1.16(3) . ?
C3 N3 1.14(2) . ?
C3' N3' 1.19(3) . ?
C3' C3' 1.81(3) 4 ?
C3' C3' 1.81(3) 2 ?
C3'' N3'' 1.17(4) . ?
O1 C10 1.359(4) 11 ?
O1 C10 1.359(4) . ?
N4 C5 1.327(6) . ?
N4 C9 1.331(6) . ?
N5 C10 1.290(5) . ?
N5 N5 1.411(7) 11 ?
C5 C6 1.380(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.379(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.367(6) . ?
C7 C10 1.456(5) . ?
C8 C9 1.379(6) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C1A N1A 1.488(9) . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?
C2A N1A 1.486(16) . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
N1A C3A 1.23(2) . ?
C3A O1A 1.298(10) . ?
C3A H3A 0.9300 . ?
C1B N1B 1.504(17) . ?
C1B H1BA 0.9600 . ?
C1B H1BB 0.9600 . ?
C1B H1BC 0.9600 . ?
C2B N1B 1.498(17) . ?
C2B H2BA 0.9600 . ?
C2B H2BB 0.9600 . ?
C2B H2BC 0.9600 . ?
N1B C3B 1.23(3) . ?
C3B O1B 1.29(2) . ?
C3B H3B 0.9300 . ?

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' 51.3(8) . 4 ?
C3' Mo1 C3' 75.5(14) . 3 ?
C3' Mo1 C3' 51.3(8) 4 3 ?
C3' Mo1 C3' 51.3(8) . 2 ?
C3' Mo1 C3' 75.5(14) 4 2 ?
C3' Mo1 C3' 51.3(8) 3 2 ?
C3' Mo1 C2' 92.7(16) . 3 ?
C3' Mo1 C2' 141.3(12) 4 3 ?
C3' Mo1 C2' 112.7(17) 3 3 ?
C3' Mo1 C2' 69.6(12) 2 3 ?
C3' Mo1 C2' 141.3(12) . 4 ?
C3' Mo1 C2' 112.7(17) 4 4 ?
C3' Mo1 C2' 69.6(12) 3 4 ?
C3' Mo1 C2' 92.7(16) 2 4 ?
C2' Mo1 C2' 85.7(5) 3 4 ?
C3' Mo1 C2' 69.6(12) . 2 ?
C3' Mo1 C2' 92.7(16) 4 2 ?
C3' Mo1 C2' 141.3(12) 3 2 ?
C3' Mo1 C2' 112.7(17) 2 2 ?
C2' Mo1 C2' 85.7(5) 3 2 ?
C2' Mo1 C2' 148.3(18) 4 2 ?
C3' Mo1 C2' 112.7(17) . . ?
C3' Mo1 C2' 69.6(12) 4 . ?
C3' Mo1 C2' 92.7(16) 3 . ?
C3' Mo1 C2' 141.3(12) 2 . ?
C2' Mo1 C2' 148.3(18) 3 . ?
C2' Mo1 C2' 85.7(5) 4 . ?
C2' Mo1 C2' 85.7(5) 2 . ?
C3'' Mo1 C3'' 58.2(14) 3 4 ?
C3'' Mo1 C3'' 58.2(14) 3 2 ?
C3'' Mo1 C3'' 87(2) 4 2 ?
C3'' Mo1 C3'' 87(2) 3 . ?
C3'' Mo1 C3'' 58.2(14) 4 . ?
C3'' Mo1 C3'' 58.2(14) 2 . ?
O1B Mn1 O1B 180.0 13 . ?
N2 Mn1 N2 180.0 13 . ?
O1B Mn1 N2' 102.4(13) 13 . ?
O1B Mn1 N2' 77.6(13) . . ?
O1B Mn1 N2' 77.6(13) 13 13 ?
O1B Mn1 N2' 102.4(13) . 13 ?
N2' Mn1 N2' 180.0 . 13 ?
N2 Mn1 O2A 80.6(8) 13 . ?
N2 Mn1 O2A 99.4(8) . . ?
N2 Mn1 O2A 99.4(8) 13 13 ?
N2 Mn1 O2A 80.6(8) . 13 ?
O2A Mn1 O2A 180.0 . 13 ?
O1B Mn1 N4 94.2(10) 13 13 ?
O1B Mn1 N4 85.8(10) . 13 ?
N2 Mn1 N4 91.1(3) 13 13 ?
N2 Mn1 N4 88.9(3) . 13 ?
N2' Mn1 N4 89.3(4) . 13 ?
N2' Mn1 N4 90.7(4) 13 13 ?
O2A Mn1 N4 90.0(5) . 13 ?
O2A Mn1 N4 90.0(5) 13 13 ?
O1B Mn1 N4 85.8(10) 13 . ?
O1B Mn1 N4 94.2(10) . . ?
N2 Mn1 N4 88.9(3) 13 . ?
N2 Mn1 N4 91.1(3) . . ?
N2' Mn1 N4 90.7(4) . . ?
N2' Mn1 N4 89.3(4) 13 . ?
O2A Mn1 N4 90.0(5) . . ?
O2A Mn1 N4 90.0(5) 13 . ?
N4 Mn1 N4 180.0 13 . ?
N1 C1 Mo1 180.0 . . ?
N2 C2 Mo1 178.0(16) . . ?
C2 N2 Mn1 165.1(11) . . ?
N2' C2' Mo1 177(2) . . ?
C2' N2' Mn1 167.0(16) . . ?
N3 C3 Mo1 177(2) . . ?
N3' C3' C3' 123(3) . 4 ?
N3' C3' C3' 108(4) . 2 ?
C3' C3' C3' 90.001(4) 4 2 ?
N3' C3' Mo1 171(4) . . ?
C3' C3' Mo1 64.3(4) 4 . ?
C3' C3' Mo1 64.3(4) 2 . ?
N3'' C3'' Mo1 170(4) . . ?
C10 O1 C10 102.9(4) 11 . ?
C5 N4 C9 116.4(4) . . ?
C5 N4 Mn1 120.9(3) . . ?
C9 N4 Mn1 122.7(3) . . ?
C10 N5 N5 106.1(2) . 11 ?
N4 C5 C6 123.8(4) . . ?
N4 C5 H5 118.1 . . ?
C6 C5 H5 118.1 . . ?
C7 C6 C5 118.9(4) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
C8 C7 C6 117.9(4) . . ?
C8 C7 C10 121.7(4) . . ?
C6 C7 C10 120.3(4) . . ?
C7 C8 C9 119.3(4) . . ?
C7 C8 H8 120.3 . . ?
C9 C8 H8 120.3 . . ?
N4 C9 C8 123.7(4) . . ?
N4 C9 H9 118.2 . . ?
C8 C9 H9 118.2 . . ?
N5 C10 O1 112.5(3) . . ?
N5 C10 C7 129.4(4) . . ?
O1 C10 C7 118.2(3) . . ?
N1A C1A H1AA 109.5 . . ?
N1A C1A H1AB 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
N1A C1A H1AC 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
N1A C2A H2AA 109.5 . . ?
N1A C2A H2AB 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
N1A C2A H2AC 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C3A N1A C2A 121.2(11) . . ?
C3A N1A C1A 122.9(14) . . ?
C2A N1A C1A 115.9(14) . . ?
N1A C3A O1A 123.7(19) . . ?
N1A C3A H3A 118.1 . . ?
O1A C3A H3A 118.1 . . ?
N1B C1B H1BA 109.5 . . ?
N1B C1B H1BB 109.5 . . ?
H1BA C1B H1BB 109.5 . . ?
N1B C1B H1BC 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
N1B C2B H2BA 109.5 . . ?
N1B C2B H2BB 109.5 . . ?
H2BA C2B H2BB 109.5 . . ?
N1B C2B H2BC 109.5 . . ?
H2BA C2B H2BC 109.5 . . ?
H2BB C2B H2BC 109.5 . . ?
C3B N1B C2B 122(2) . . ?
C3B N1B C1B 118(2) . . ?
C2B N1B C1B 119(2) . . ?
N1B C3B O1B 116(3) . . ?
N1B C3B H3B 121.9 . . ?
O1B C3B H3B 121.9 . . ?
C3B O1B Mn1 124(3) . . ?

_refine_diff_density_max         0.657
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.103



