# 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_17RPA005
_database_code_depnum_ccdc_archive 'CCDC 1828961'
_audit_update_record             
;
2018-03-12 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            DS-504
_chemical_formula_moiety         'C21 H16 Mn N3 O4'
_chemical_formula_sum            'C21 H16 Mn N3 O4'
_chemical_formula_iupac          ?
_chemical_formula_weight         429.31

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.9527(3)
_cell_length_b                   9.7141(3)
_cell_length_c                   14.9863(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.3930(10)
_cell_angle_gamma                90
_cell_volume                     1885.08(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9976
_cell_measurement_theta_min      2.9354
_cell_measurement_theta_max      33.2558
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear orange'
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.217
_exptl_crystal_size_min          0.186
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880

_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_T_max  0.88

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'SIEMENS KFN MO 2K-90'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker AXS X8 APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            61294
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         36.40
_diffrn_reflns_theta_full        36.40
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24

_refine_special_details          
;
;

_reflns_number_total             9171
_reflns_number_gt                6335
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0411
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.1042
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_number_reflns         9171
_refine_ls_number_parameters     263
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0394P)²+0.7632P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.796
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'Bruker APEX2 software'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 807)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.49760(2) 0.16806(2) 0.32173(2) 0.01384(5) Uani d . . . 1 . .
N N1 0.71473(8) 0.18649(11) 0.23546(7) 0.0161(2) Uani d . . . 1 . .
C C2 0.61645(9) 0.17685(12) 0.23094(8) 0.0146(2) Uani d . . . 1 . .
O O3 0.57395(7) 0.17761(10) 0.14534(6) 0.01770(18) Uani d . . . 1 . .
C C10 0.64498(10) 0.17849(14) 0.07314(8) 0.0191(2) Uani d . . . 1 . .
H H10A 0.606289 0.179687 0.016132 0.029 Uiso calc U . R 1 . .
H H10B 0.688273 0.095831 0.076428 0.029 Uiso calc U . R 1 . .
H H10C 0.688795 0.260562 0.077641 0.029 Uiso calc U . R 1 . .
C C11 0.77411(9) 0.18364(13) 0.31453(8) 0.0153(2) Uani d . . . 1 . .
C C12 0.79541(10) 0.06024(14) 0.35948(9) 0.0176(2) Uani d . . . 1 . .
H H12 0.765052 -0.023227 0.338767 0.021 Uiso calc U . R 1 . .
C C13 0.86090(10) 0.05947(14) 0.43437(9) 0.0194(2) Uani d . . . 1 . .
H H13 0.874469 -0.02478 0.464639 0.023 Uiso calc U . R 1 . .
C C14 0.90667(10) 0.17962(14) 0.46554(9) 0.0195(2) Uani d . . . 1 . .
H H14 0.950321 0.178367 0.517403 0.023 Uiso calc U . R 1 . .
C C15 0.88790(10) 0.30219(14) 0.41989(9) 0.0186(2) Uani d . . . 1 . .
H H15 0.919722 0.384902 0.440268 0.022 Uiso calc U . R 1 . .
C C16 0.82284(10) 0.30449(13) 0.34462(9) 0.0171(2) Uani d . . . 1 . .
H H16 0.811385 0.388462 0.31343 0.021 Uiso calc U . R 1 . .
C C4 0.42231(11) 0.07399(15) 0.23966(9) 0.0205(2) Uani d . . . 1 . .
O O5 0.37267(9) 0.00892(12) 0.19059(8) 0.0311(2) Uani d . . . 1 . .
C C6 0.54156(10) 0.00471(14) 0.36387(9) 0.0189(2) Uani d . . . 1 . .
O O7 0.56483(9) -0.10283(11) 0.38992(8) 0.0279(2) Uani d . . . 1 . .
C C8 0.38631(10) 0.16654(14) 0.39439(9) 0.0196(2) Uani d . . . 1 . .
O O9 0.31399(8) 0.16092(13) 0.43710(8) 0.0303(2) Uani d . . . 1 . .
N N21 0.57905(8) 0.28729(11) 0.41099(7) 0.01511(19) Uani d . . . 1 . .
C C22 0.57573(9) 0.42488(13) 0.39658(8) 0.0153(2) Uani d . . . 1 . .
C C23 0.62129(10) 0.51824(14) 0.45625(9) 0.0199(2) Uani d . . . 1 . .
H H23 0.618136 0.61431 0.444649 0.024 Uiso calc U . R 1 . .
C C24 0.67091(10) 0.46950(16) 0.53222(9) 0.0227(3) Uani d . . . 1 . .
H H24 0.702628 0.531384 0.573607 0.027 Uiso calc U . R 1 . .
C C25 0.67385(10) 0.32903(16) 0.54730(9) 0.0213(3) Uani d . . . 1 . .
H H25 0.707007 0.293198 0.599559 0.026 Uiso calc U . R 1 . .
C C26 0.62795(10) 0.24144(15) 0.48541(9) 0.0183(2) Uani d . . . 1 . .
H H26 0.63107 0.145054 0.495845 0.022 Uiso calc U . R 1 . .
N N31 0.46577(8) 0.36058(11) 0.27502(7) 0.01557(19) Uani d . . . 1 . .
C C32 0.51476(9) 0.46642(13) 0.31723(8) 0.0158(2) Uani d . . . 1 . .
C C33 0.50424(11) 0.60116(14) 0.28832(10) 0.0220(3) Uani d . . . 1 . .
H H33 0.541797 0.672798 0.317558 0.026 Uiso calc U . R 1 . .
C C34 0.43890(12) 0.63082(16) 0.21680(10) 0.0266(3) Uani d . . . 1 . .
H H34 0.429704 0.722903 0.1968 0.032 Uiso calc U . R 1 . .
C C35 0.38708(11) 0.52332(16) 0.17488(10) 0.0259(3) Uani d . . . 1 . .
H H35 0.340669 0.540766 0.126126 0.031 Uiso calc U . R 1 . .
C C36 0.40354(10) 0.39058(15) 0.20465(9) 0.0209(3) Uani d . . . 1 . .
H H36 0.369433 0.317248 0.174101 0.025 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 C6 . 1.7954(14) ?
Mn1 C4 . 1.8000(14) ?
Mn1 C8 . 1.8277(14) ?
Mn1 N31 . 2.0355(11) ?
Mn1 N21 . 2.0434(11) ?
Mn1 C2 . 2.0809(12) ?
N1 C2 . 1.2767(16) ?
N1 C11 . 1.3972(16) ?
C2 O3 . 1.3836(15) ?
O3 C10 . 1.4371(15) ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
C11 C12 . 1.3992(18) ?
C11 C16 . 1.4022(18) ?
C12 C13 . 1.3904(18) ?
C12 H12 . 0.95 ?
C13 C14 . 1.3851(19) ?
C13 H13 . 0.95 ?
C14 C15 . 1.3917(19) ?
C14 H14 . 0.95 ?
C15 C16 . 1.3917(18) ?
C15 H15 . 0.95 ?
C16 H16 . 0.95 ?
C4 O5 . 1.1536(17) ?
C6 O7 . 1.1527(17) ?
C8 O9 . 1.1486(17) ?
N21 C26 . 1.3449(17) ?
N21 C22 . 1.3544(17) ?
C22 C23 . 1.3945(18) ?
C22 C32 . 1.4680(18) ?
C23 C24 . 1.378(2) ?
C23 H23 . 0.95 ?
C24 C25 . 1.384(2) ?
C24 H24 . 0.95 ?
C25 C26 . 1.3824(19) ?
C25 H25 . 0.95 ?
C26 H26 . 0.95 ?
N31 C36 . 1.3436(17) ?
N31 C32 . 1.3566(17) ?
C32 C33 . 1.3844(19) ?
C33 C34 . 1.380(2) ?
C33 H33 . 0.95 ?
C34 C35 . 1.384(2) ?
C34 H34 . 0.95 ?
C35 C36 . 1.379(2) ?
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 Mn1 C4 . . 87.34(6) ?
C6 Mn1 C8 . . 91.79(6) ?
C4 Mn1 C8 . . 88.91(6) ?
C6 Mn1 N31 . . 173.13(5) ?
C4 Mn1 N31 . . 97.45(6) ?
C8 Mn1 N31 . . 93.22(5) ?
C6 Mn1 N21 . . 96.68(5) ?
C4 Mn1 N21 . . 175.98(6) ?
C8 Mn1 N21 . . 90.95(5) ?
N31 Mn1 N21 . . 78.55(4) ?
C6 Mn1 C2 . . 91.89(5) ?
C4 Mn1 C2 . . 88.35(6) ?
C8 Mn1 C2 . . 175.31(6) ?
N31 Mn1 C2 . . 83.36(4) ?
N21 Mn1 C2 . . 91.51(4) ?
C2 N1 C11 . . 124.83(11) ?
N1 C2 O3 . . 114.99(11) ?
N1 C2 Mn1 . . 136.13(10) ?
O3 C2 Mn1 . . 108.82(8) ?
C2 O3 C10 . . 116.78(10) ?
O3 C10 H10A . . 109.5 ?
O3 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
O3 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
N1 C11 C12 . . 121.56(11) ?
N1 C11 C16 . . 119.36(11) ?
C12 C11 C16 . . 118.72(11) ?
C13 C12 C11 . . 120.17(12) ?
C13 C12 H12 . . 119.9 ?
C11 C12 H12 . . 119.9 ?
C14 C13 C12 . . 121.02(12) ?
C14 C13 H13 . . 119.5 ?
C12 C13 H13 . . 119.5 ?
C13 C14 C15 . . 119.14(12) ?
C13 C14 H14 . . 120.4 ?
C15 C14 H14 . . 120.4 ?
C14 C15 C16 . . 120.48(12) ?
C14 C15 H15 . . 119.8 ?
C16 C15 H15 . . 119.8 ?
C15 C16 C11 . . 120.41(12) ?
C15 C16 H16 . . 119.8 ?
C11 C16 H16 . . 119.8 ?
O5 C4 Mn1 . . 176.38(13) ?
O7 C6 Mn1 . . 176.49(12) ?
O9 C8 Mn1 . . 176.51(12) ?
C26 N21 C22 . . 118.13(11) ?
C26 N21 Mn1 . . 125.48(9) ?
C22 N21 Mn1 . . 116.17(8) ?
N21 C22 C23 . . 121.89(12) ?
N21 C22 C32 . . 114.51(11) ?
C23 C22 C32 . . 123.48(12) ?
C24 C23 C22 . . 119.21(13) ?
C24 C23 H23 . . 120.4 ?
C22 C23 H23 . . 120.4 ?
C23 C24 C25 . . 118.97(13) ?
C23 C24 H24 . . 120.5 ?
C25 C24 H24 . . 120.5 ?
C26 C25 C24 . . 119.19(13) ?
C26 C25 H25 . . 120.4 ?
C24 C25 H25 . . 120.4 ?
N21 C26 C25 . . 122.60(13) ?
N21 C26 H26 . . 118.7 ?
C25 C26 H26 . . 118.7 ?
C36 N31 C32 . . 117.80(12) ?
C36 N31 Mn1 . . 125.58(10) ?
C32 N31 Mn1 . . 116.58(8) ?
N31 C32 C33 . . 121.96(12) ?
N31 C32 C22 . . 113.94(11) ?
C33 C32 C22 . . 124.08(12) ?
C34 C33 C32 . . 119.62(14) ?
C34 C33 H33 . . 120.2 ?
C32 C33 H33 . . 120.2 ?
C33 C34 C35 . . 118.47(14) ?
C33 C34 H34 . . 120.8 ?
C35 C34 H34 . . 120.8 ?
C36 C35 C34 . . 119.28(14) ?
C36 C35 H35 . . 120.4 ?
C34 C35 H35 . . 120.4 ?
N31 C36 C35 . . 122.80(14) ?
N31 C36 H36 . . 118.6 ?
C35 C36 H36 . . 118.6 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C11 N1 C2 O3 . . . . -177.98(11) ?
C11 N1 C2 Mn1 . . . . 5.3(2) ?
N1 C2 O3 C10 . . . . 4.56(16) ?
Mn1 C2 O3 C10 . . . . -177.85(8) ?
C2 N1 C11 C12 . . . . 77.49(17) ?
C2 N1 C11 C16 . . . . -109.52(15) ?
N1 C11 C12 C13 . . . . 175.29(12) ?
C16 C11 C12 C13 . . . . 2.26(19) ?
C11 C12 C13 C14 . . . . -0.4(2) ?
C12 C13 C14 C15 . . . . -1.2(2) ?
C13 C14 C15 C16 . . . . 0.9(2) ?
C14 C15 C16 C11 . . . . 1.0(2) ?
N1 C11 C16 C15 . . . . -175.70(12) ?
C12 C11 C16 C15 . . . . -2.51(19) ?
C26 N21 C22 C23 . . . . 0.07(17) ?
Mn1 N21 C22 C23 . . . . 174.98(9) ?
C26 N21 C22 C32 . . . . -175.91(10) ?
Mn1 N21 C22 C32 . . . . -0.99(13) ?
N21 C22 C23 C24 . . . . -0.18(18) ?
C32 C22 C23 C24 . . . . 175.43(12) ?
C22 C23 C24 C25 . . . . -0.20(19) ?
C23 C24 C25 C26 . . . . 0.68(19) ?
C22 N21 C26 C25 . . . . 0.43(18) ?
Mn1 N21 C26 C25 . . . . -173.96(10) ?
C24 C25 C26 N21 . . . . -0.8(2) ?
C36 N31 C32 C33 . . . . -1.75(18) ?
Mn1 N31 C32 C33 . . . . 176.07(10) ?
C36 N31 C32 C22 . . . . 176.31(11) ?
Mn1 N31 C32 C22 . . . . -5.86(13) ?
N21 C22 C32 N31 . . . . 4.44(15) ?
C23 C22 C32 N31 . . . . -171.47(11) ?
N21 C22 C32 C33 . . . . -177.55(11) ?
C23 C22 C32 C33 . . . . 6.55(19) ?
N31 C32 C33 C34 . . . . 2.8(2) ?
C22 C32 C33 C34 . . . . -175.11(12) ?
C32 C33 C34 C35 . . . . -1.2(2) ?
C33 C34 C35 C36 . . . . -1.1(2) ?
C32 N31 C36 C35 . . . . -0.73(19) ?
Mn1 N31 C36 C35 . . . . -178.33(10) ?
C34 C35 C36 N31 . . . . 2.2(2) ?

####################################################################### 
# 
# 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_17RPA008
_database_code_depnum_ccdc_archive 'CCDC 1828962'
_audit_update_record             
;
2018-03-12 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            'DS-511.2 - 17RPA008'
_chemical_formula_moiety         'C21 H17 Mn N3 O4, B F4, C H2 Cl2'
_chemical_formula_sum            'C22 H19 B Cl2 F4 Mn N3 O4'
_chemical_formula_iupac          ?
_chemical_formula_weight         602.05

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2025(2)
_cell_length_b                   10.5656(2)
_cell_length_c                   15.3399(4)
_cell_angle_alpha                80.5480(10)
_cell_angle_beta                 78.2160(10)
_cell_angle_gamma                87.4530(10)
_cell_volume                     1283.65(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7187
_cell_measurement_theta_min      2.2032
_cell_measurement_theta_max      26.7006
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608

_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.94

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'SIEMENS KFN MO 2K-90'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker AXS X8 APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            25396
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_full        27.15
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19

_refine_special_details          
;
;

_reflns_number_total             5683
_reflns_number_gt                4516
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1007
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.058
_refine_ls_number_reflns         5683
_refine_ls_number_parameters     409
_refine_ls_number_restraints     409
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0407P)²+1.2839P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.548
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn01 0.33856(4) 0.71124(3) 0.33786(2) 0.01365(10) Uani d . . . 1.0 . .
N N1 0.1778(2) 0.73756(18) 0.24504(12) 0.0153(4) Uani d . . . 1.0 . .
C C2 0.1738(3) 0.8358(2) 0.18512(16) 0.0195(5) Uani d . . . 1.0 . .
H H2 0.106061 0.835997 0.14174 0.023 Uiso calc U . R 1.0 . .
O O3 0.2635(2) 0.93783(16) 0.18289(11) 0.0226(4) Uani d . . . 1.0 . .
C C4 0.3285(3) 0.8793(2) 0.35190(15) 0.0200(5) Uani d . . . 1.0 . .
O O5 0.3198(3) 0.98262(17) 0.36611(12) 0.0312(4) Uani d . . . 1.0 . .
C C6 0.1698(3) 0.6856(2) 0.43430(16) 0.0187(5) Uani d . . . 1.0 . .
O O7 0.0662(2) 0.67303(18) 0.49812(11) 0.0273(4) Uani d . . . 1.0 . .
C C8 0.4845(3) 0.6790(2) 0.41277(15) 0.0196(5) Uani d . . . 1.0 . .
O O9 0.5757(2) 0.65655(19) 0.46060(12) 0.0299(4) Uani d . . . 1.0 . .
C C10 0.2545(4) 1.0443(3) 0.11140(19) 0.0367(7) Uani d . . . 1.0 . .
H H10A 0.329903 1.027884 0.055929 0.055 Uiso calc U . R 1.0 . .
H H10B 0.287273 1.123223 0.128683 0.055 Uiso calc U . R 1.0 . .
H H10C 0.140191 1.053758 0.101155 0.055 Uiso calc U . R 1.0 . .
C C11 0.0789(3) 0.6311(2) 0.23840(15) 0.0166(5) Uani d . . . 1.0 . .
C C12 -0.0562(3) 0.5915(2) 0.30687(16) 0.0202(5) Uani d . . . 1.0 . .
H H12 -0.089485 0.638421 0.355455 0.024 Uiso calc U . R 1.0 . .
C C13 -0.1424(3) 0.4825(2) 0.30376(17) 0.0242(5) Uani d . . . 1.0 . .
H H13 -0.235185 0.455077 0.350319 0.029 Uiso calc U . R 1.0 . .
C C14 -0.0937(3) 0.4137(3) 0.23295(18) 0.0262(6) Uani d . . . 1.0 . .
H H14 -0.15082 0.33781 0.231964 0.031 Uiso calc U . R 1.0 . .
C C15 0.0383(3) 0.4557(2) 0.16380(18) 0.0243(5) Uani d . . . 1.0 . .
H H15 0.069824 0.409723 0.114554 0.029 Uiso calc U . R 1.0 . .
C C16 0.1250(3) 0.5645(2) 0.16604(16) 0.0201(5) Uani d . . . 1.0 . .
H H16 0.215262 0.593419 0.118344 0.024 Uiso calc U . R 1.0 . .
N N21 0.3605(2) 0.52619(18) 0.31395(12) 0.0140(4) Uani d . . . 1.0 . .
C C22 0.4683(3) 0.5054(2) 0.23797(14) 0.0145(4) Uani d . . . 1.0 . .
C C23 0.4889(3) 0.3854(2) 0.21154(16) 0.0183(5) Uani d . . . 1.0 . .
H H23 0.564912 0.373301 0.157771 0.022 Uiso calc U . R 1.0 . .
C C24 0.3978(3) 0.2835(2) 0.26430(17) 0.0210(5) Uani d . . . 1.0 . .
H H24 0.410242 0.200501 0.247376 0.025 Uiso calc U . R 1.0 . .
C C25 0.2879(3) 0.3045(2) 0.34233(16) 0.0204(5) Uani d . . . 1.0 . .
H H25 0.22435 0.235982 0.380017 0.024 Uiso calc U . R 1.0 . .
C C26 0.2726(3) 0.4262(2) 0.36420(15) 0.0175(5) Uani d . . . 1.0 . .
H H26 0.196225 0.440147 0.41738 0.021 Uiso calc U . R 1.0 . .
N N31 0.5286(2) 0.72687(18) 0.22684(12) 0.0147(4) Uani d . . . 1.0 . .
C C32 0.5646(3) 0.6191(2) 0.18909(15) 0.0148(4) Uani d . . . 1.0 . .
C C33 0.6885(3) 0.6155(2) 0.11305(15) 0.0180(5) Uani d . . . 1.0 . .
H H33 0.708986 0.53955 0.086653 0.022 Uiso calc U . R 1.0 . .
C C34 0.7818(3) 0.7243(2) 0.07627(15) 0.0199(5) Uani d . . . 1.0 . .
H H34 0.86873 0.723504 0.024838 0.024 Uiso calc U . R 1.0 . .
C C35 0.7473(3) 0.8344(2) 0.11518(16) 0.0195(5) Uani d . . . 1.0 . .
H H35 0.810449 0.909848 0.091255 0.023 Uiso calc U . R 1.0 . .
C C36 0.6191(3) 0.8322(2) 0.18945(15) 0.0174(5) Uani d . . . 1.0 . .
H H36 0.593832 0.908325 0.215204 0.021 Uiso calc U . R 1.0 . .
B B40A 0.7604(7) 0.1927(6) 0.0622(4) 0.0271(10) Uani d U P D 0.791(7) A 1
F F41A 0.8142(8) 0.3185(5) 0.0559(6) 0.0259(10) Uani d U P D 0.791(7) A 1
F F42A 0.8947(11) 0.1208(12) 0.0237(6) 0.0251(13) Uani d U P D 0.791(7) A 1
F F43A 0.6352(3) 0.1922(3) 0.0135(3) 0.0577(11) Uani d U P D 0.791(7) A 1
F F44A 0.7021(6) 0.1397(3) 0.1503(2) 0.0623(13) Uani d U P D 0.791(7) A 1
B B40B 0.784(3) 0.188(3) 0.0750(15) 0.032(3) Uani d U P D 0.209(7) A 2
F F41B 0.810(2) 0.1395(10) 0.1619(6) 0.050(3) Uani d U P D 0.209(7) A 2
F F42B 0.6209(11) 0.1596(10) 0.0767(11) 0.049(3) Uani d U P D 0.209(7) A 2
F F43B 0.782(4) 0.320(2) 0.057(3) 0.036(4) Uani d U P D 0.209(7) A 2
F F44B 0.892(5) 0.129(5) 0.014(2) 0.027(4) Uani d U P D 0.209(7) A 2
Cl Cl51 0.6618(2) 0.1515(2) 0.40740(13) 0.0203(9) Uani d U P D 0.574(17) B 1
C C50 0.8399(12) 0.0813(8) 0.3513(8) 0.058(3) Uani d U P D 0.574(17) B 1
H H50A 0.850155 0.109756 0.285622 0.069 Uiso calc U P R 0.574(17) B 1
H H50B 0.938203 0.113196 0.368936 0.069 Uiso calc U P R 0.574(17) B 1
Cl Cl52 0.8444(6) -0.0827(5) 0.3716(7) 0.0955(15) Uani d U P D 0.574(17) B 1
Cl Cl61 0.6655(8) 0.1444(7) 0.4089(5) 0.108(3) Uani d U P D 0.426(17) B 2
C C60 0.8622(18) 0.0838(13) 0.3802(13) 0.078(4) Uani d U P D 0.426(17) B 2
H H60A 0.903877 0.111032 0.314755 0.094 Uiso calc U P R 0.426(17) B 2
H H60B 0.935994 0.121023 0.412714 0.094 Uiso calc U P R 0.426(17) B 2
Cl Cl62 0.8747(12) -0.0788(7) 0.4036(6) 0.084(2) Uani d U P D 0.426(17) B 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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn01 C6 . 1.801(2) ?
Mn01 C8 . 1.807(2) ?
Mn01 C4 . 1.820(3) ?
Mn01 N21 . 2.0413(19) ?
Mn01 N31 . 2.0501(18) ?
Mn01 N1 . 2.1087(19) ?
N1 C2 . 1.273(3) ?
N1 C11 . 1.444(3) ?
C2 O3 . 1.323(3) ?
C2 H2 . 0.95 ?
O3 C10 . 1.447(3) ?
C4 O5 . 1.144(3) ?
C6 O7 . 1.151(3) ?
C8 O9 . 1.143(3) ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
C11 C12 . 1.389(3) ?
C11 C16 . 1.390(3) ?
C12 C13 . 1.390(3) ?
C12 H12 . 0.95 ?
C13 C14 . 1.388(4) ?
C13 H13 . 0.95 ?
C14 C15 . 1.383(4) ?
C14 H14 . 0.95 ?
C15 C16 . 1.387(3) ?
C15 H15 . 0.95 ?
C16 H16 . 0.95 ?
N21 C26 . 1.343(3) ?
N21 C22 . 1.354(3) ?
C22 C23 . 1.387(3) ?
C22 C32 . 1.476(3) ?
C23 C24 . 1.382(3) ?
C23 H23 . 0.95 ?
C24 C25 . 1.387(3) ?
C24 H24 . 0.95 ?
C25 C26 . 1.376(3) ?
C25 H25 . 0.95 ?
C26 H26 . 0.95 ?
N31 C36 . 1.345(3) ?
N31 C32 . 1.354(3) ?
C32 C33 . 1.386(3) ?
C33 C34 . 1.384(3) ?
C33 H33 . 0.95 ?
C34 C35 . 1.385(3) ?
C34 H34 . 0.95 ?
C35 C36 . 1.381(3) ?
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
B40A F44A . 1.371(6) ?
B40A F43A . 1.388(6) ?
B40A F42A . 1.395(7) ?
B40A F41A . 1.401(7) ?
B40B F44B . 1.37(2) ?
B40B F42B . 1.375(19) ?
B40B F43B . 1.381(19) ?
B40B F41B . 1.404(18) ?
Cl51 C50 . 1.740(7) ?
C50 Cl52 . 1.709(8) ?
C50 H50A . 0.99 ?
C50 H50B . 0.99 ?
Cl61 C60 . 1.708(13) ?
C60 Cl62 . 1.699(12) ?
C60 H60A . 0.99 ?
C60 H60B . 0.99 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C6 Mn01 C8 . . 89.21(10) ?
C6 Mn01 C4 . . 86.84(10) ?
C8 Mn01 C4 . . 90.09(11) ?
C6 Mn01 N21 . . 96.96(9) ?
C8 Mn01 N21 . . 90.65(9) ?
C4 Mn01 N21 . . 176.14(9) ?
C6 Mn01 N31 . . 175.82(9) ?
C8 Mn01 N31 . . 91.34(9) ?
C4 Mn01 N31 . . 97.29(9) ?
N21 Mn01 N31 . . 78.90(7) ?
C6 Mn01 N1 . . 93.36(9) ?
C8 Mn01 N1 . . 175.53(9) ?
C4 Mn01 N1 . . 93.70(9) ?
N21 Mn01 N1 . . 85.41(7) ?
N31 Mn01 N1 . . 85.83(7) ?
C2 N1 C11 . . 115.04(19) ?
C2 N1 Mn01 . . 125.32(16) ?
C11 N1 Mn01 . . 119.06(14) ?
N1 C2 O3 . . 120.4(2) ?
N1 C2 H2 . . 119.8 ?
O3 C2 H2 . . 119.8 ?
C2 O3 C10 . . 116.80(19) ?
O5 C4 Mn01 . . 175.9(2) ?
O7 C6 Mn01 . . 176.5(2) ?
O9 C8 Mn01 . . 178.9(2) ?
O3 C10 H10A . . 109.5 ?
O3 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
O3 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C12 C11 C16 . . 120.3(2) ?
C12 C11 N1 . . 119.8(2) ?
C16 C11 N1 . . 119.8(2) ?
C11 C12 C13 . . 119.5(2) ?
C11 C12 H12 . . 120.3 ?
C13 C12 H12 . . 120.3 ?
C14 C13 C12 . . 120.3(2) ?
C14 C13 H13 . . 119.9 ?
C12 C13 H13 . . 119.9 ?
C15 C14 C13 . . 119.9(2) ?
C15 C14 H14 . . 120.1 ?
C13 C14 H14 . . 120.1 ?
C14 C15 C16 . . 120.3(2) ?
C14 C15 H15 . . 119.8 ?
C16 C15 H15 . . 119.8 ?
C15 C16 C11 . . 119.7(2) ?
C15 C16 H16 . . 120.2 ?
C11 C16 H16 . . 120.2 ?
C26 N21 C22 . . 117.97(19) ?
C26 N21 Mn01 . . 125.87(15) ?
C22 N21 Mn01 . . 116.08(14) ?
N21 C22 C23 . . 121.9(2) ?
N21 C22 C32 . . 114.28(19) ?
C23 C22 C32 . . 123.8(2) ?
C24 C23 C22 . . 119.3(2) ?
C24 C23 H23 . . 120.4 ?
C22 C23 H23 . . 120.4 ?
C23 C24 C25 . . 118.9(2) ?
C23 C24 H24 . . 120.6 ?
C25 C24 H24 . . 120.6 ?
C26 C25 C24 . . 118.8(2) ?
C26 C25 H25 . . 120.6 ?
C24 C25 H25 . . 120.6 ?
N21 C26 C25 . . 123.1(2) ?
N21 C26 H26 . . 118.4 ?
C25 C26 H26 . . 118.4 ?
C36 N31 C32 . . 118.12(19) ?
C36 N31 Mn01 . . 126.32(15) ?
C32 N31 Mn01 . . 115.56(14) ?
N31 C32 C33 . . 122.2(2) ?
N31 C32 C22 . . 114.75(19) ?
C33 C32 C22 . . 123.0(2) ?
C34 C33 C32 . . 118.9(2) ?
C34 C33 H33 . . 120.6 ?
C32 C33 H33 . . 120.6 ?
C33 C34 C35 . . 119.3(2) ?
C33 C34 H34 . . 120.3 ?
C35 C34 H34 . . 120.3 ?
C36 C35 C34 . . 118.7(2) ?
C36 C35 H35 . . 120.7 ?
C34 C35 H35 . . 120.7 ?
N31 C36 C35 . . 122.8(2) ?
N31 C36 H36 . . 118.6 ?
C35 C36 H36 . . 118.6 ?
F44A B40A F43A . . 109.4(5) ?
F44A B40A F42A . . 110.3(6) ?
F43A B40A F42A . . 108.1(6) ?
F44A B40A F41A . . 111.0(6) ?
F43A B40A F41A . . 109.8(5) ?
F42A B40A F41A . . 108.1(7) ?
F44B B40B F42B . . 112.(2) ?
F44B B40B F43B . . 115.(3) ?
F42B B40B F43B . . 102.1(19) ?
F44B B40B F41B . . 109.(2) ?
F42B B40B F41B . . 105.1(17) ?
F43B B40B F41B . . 113.(2) ?
Cl52 C50 Cl51 . . 114.9(6) ?
Cl52 C50 H50A . . 108.5 ?
Cl51 C50 H50A . . 108.5 ?
Cl52 C50 H50B . . 108.5 ?
Cl51 C50 H50B . . 108.5 ?
H50A C50 H50B . . 107.5 ?
Cl62 C60 Cl61 . . 113.9(9) ?
Cl62 C60 H60A . . 108.8 ?
Cl61 C60 H60A . . 108.8 ?
Cl62 C60 H60B . . 108.8 ?
Cl61 C60 H60B . . 108.8 ?
H60A C60 H60B . . 107.7 ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C11 N1 C2 O3 . . . . -178.0(2) ?
Mn01 N1 C2 O3 . . . . -6.9(3) ?
N1 C2 O3 C10 . . . . 178.7(2) ?
C2 N1 C11 C12 . . . . -115.6(2) ?
Mn01 N1 C11 C12 . . . . 72.7(2) ?
C2 N1 C11 C16 . . . . 68.0(3) ?
Mn01 N1 C11 C16 . . . . -103.7(2) ?
C16 C11 C12 C13 . . . . 1.7(3) ?
N1 C11 C12 C13 . . . . -174.7(2) ?
C11 C12 C13 C14 . . . . 0.2(4) ?
C12 C13 C14 C15 . . . . -1.9(4) ?
C13 C14 C15 C16 . . . . 1.6(4) ?
C14 C15 C16 C11 . . . . 0.3(4) ?
C12 C11 C16 C15 . . . . -2.0(3) ?
N1 C11 C16 C15 . . . . 174.5(2) ?
C26 N21 C22 C23 . . . . 0.1(3) ?
Mn01 N21 C22 C23 . . . . -176.83(16) ?
C26 N21 C22 C32 . . . . -177.51(19) ?
Mn01 N21 C22 C32 . . . . 5.5(2) ?
N21 C22 C23 C24 . . . . -0.3(3) ?
C32 C22 C23 C24 . . . . 177.1(2) ?
C22 C23 C24 C25 . . . . 0.1(3) ?
C23 C24 C25 C26 . . . . 0.4(3) ?
C22 N21 C26 C25 . . . . 0.4(3) ?
Mn01 N21 C26 C25 . . . . 177.03(17) ?
C24 C25 C26 N21 . . . . -0.7(4) ?
C36 N31 C32 C33 . . . . -1.2(3) ?
Mn01 N31 C32 C33 . . . . 179.17(17) ?
C36 N31 C32 C22 . . . . 175.68(19) ?
Mn01 N31 C32 C22 . . . . -3.9(2) ?
N21 C22 C32 N31 . . . . -1.0(3) ?
C23 C22 C32 N31 . . . . -178.6(2) ?
N21 C22 C32 C33 . . . . 175.8(2) ?
C23 C22 C32 C33 . . . . -1.7(3) ?
N31 C32 C33 C34 . . . . 2.1(3) ?
C22 C32 C33 C34 . . . . -174.5(2) ?
C32 C33 C34 C35 . . . . -1.2(3) ?
C33 C34 C35 C36 . . . . -0.5(3) ?
C32 N31 C36 C35 . . . . -0.6(3) ?
Mn01 N31 C36 C35 . . . . 178.97(17) ?
C34 C35 C36 N31 . . . . 1.5(3) ?

####################################################################### 
# 
# 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_17RPA007B
_database_code_depnum_ccdc_archive 'CCDC 1828964'
_audit_update_record             
;
2018-03-12 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            'DS-506.2 - 17RPA007B'
_chemical_formula_moiety         'C21 H17 Mn N3 O4, B F4'
_chemical_formula_sum            'C21 H17 B F4 Mn N3 O4'
_chemical_formula_iupac          ?
_chemical_formula_weight         517.12

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   31.9054(5)
_cell_length_b                   6.91700(10)
_cell_length_c                   20.7312(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.0868(8)
_cell_angle_gamma                90
_cell_volume                     4456.34(12)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9909
_cell_measurement_theta_min      2.6430
_cell_measurement_theta_max      24.1688
_cell_measurement_temperature    250.(2)

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_size_max          0.418
_exptl_crystal_size_mid          0.308
_exptl_crystal_size_min          0.148
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2096

_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.81
_exptl_absorpt_correction_T_max  0.91

_exptl_special_details           
;
;

_diffrn_ambient_temperature      250.(2)

_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'SIEMENS KFN MO 2K-90'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker AXS X8 APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            74079
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_theta_min         2.02
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_full        27.14
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26

_refine_special_details          
;
;

_reflns_number_total             4916
_reflns_number_gt                3907
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0904
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.039
_refine_ls_number_reflns         4916
_refine_ls_number_parameters     404
_refine_ls_number_restraints     493
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0384P)²+4.8258P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.239
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_computing_data_collection       'Bruker APEX3 software'
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 833)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.33977(2) 0.44748(4) 0.47778(2) 0.03093(9) Uani d . . . 1.0 . .
N N1 0.38553(6) 0.2810(3) 0.37364(8) 0.0505(5) Uani d . . . 1.0 . .
H H1 0.4058(8) 0.227(4) 0.3640(12) 0.061 Uiso d U . . 1.0 . .
C C2 0.38591(6) 0.3278(3) 0.43501(9) 0.0382(4) Uani d . . . 1.0 . .
O O3 0.42252(4) 0.2938(2) 0.47859(6) 0.0474(4) Uani d . . . 1.0 . .
C C10 0.46198(7) 0.2466(5) 0.45829(11) 0.0609(7) Uani d . . . 1.0 . .
H H10A 0.459675 0.117896 0.439257 0.091 Uiso calc U . R 1.0 . .
H H10B 0.486006 0.250917 0.496497 0.091 Uiso calc U . R 1.0 . .
H H10C 0.466615 0.339569 0.425567 0.091 Uiso calc U . R 1.0 . .
C C11 0.35075(6) 0.3141(4) 0.31676(9) 0.0414(5) Uani d . . . 1.0 . .
C C12 0.34748(7) 0.4890(4) 0.28520(11) 0.0547(6) Uani d . . . 1.0 . .
H H12 0.367378 0.587914 0.300919 0.066 Uiso calc U . R 1.0 . .
C C13 0.31450(8) 0.5188(4) 0.22980(12) 0.0603(7) Uani d . . . 1.0 . .
H H13 0.311942 0.638809 0.208006 0.072 Uiso calc U . R 1.0 . .
C C14 0.28587(7) 0.3758(4) 0.20679(10) 0.0530(6) Uani d . . . 1.0 . .
H H14 0.263352 0.397814 0.169575 0.064 Uiso calc U . R 1.0 . .
C C15 0.28972(8) 0.2009(4) 0.23746(11) 0.0580(7) Uani d . . . 1.0 . .
H H15 0.270039 0.101755 0.221038 0.07 Uiso calc U . R 1.0 . .
C C16 0.32274(8) 0.1679(4) 0.29321(10) 0.0526(6) Uani d . . . 1.0 . .
H H16 0.325658 0.046707 0.314245 0.063 Uiso calc U . R 1.0 . .
C C4 0.32832(7) 0.6466(4) 0.42089(11) 0.0470(5) Uani d . . . 1.0 . .
O O5 0.31891(7) 0.7786(3) 0.38789(10) 0.0785(6) Uani d . . . 1.0 . .
C C6 0.29582(7) 0.3158(3) 0.42639(10) 0.0424(5) Uani d . . . 1.0 . .
O O7 0.26529(5) 0.2442(3) 0.39582(8) 0.0673(5) Uani d . . . 1.0 . .
C C8 0.29976(6) 0.5459(3) 0.51940(9) 0.0367(4) Uani d . . . 1.0 . .
O O9 0.27289(5) 0.6017(3) 0.54226(8) 0.0572(4) Uani d . . . 1.0 . .
N N21 0.35464(5) 0.2499(2) 0.55300(7) 0.0305(3) Uani d . . . 1.0 . .
C C22 0.38601(6) 0.3039(3) 0.60575(8) 0.0322(4) Uani d . . . 1.0 . .
C C23 0.39632(7) 0.1921(3) 0.66247(9) 0.0447(5) Uani d . . . 1.0 . .
H H23 0.418732 0.229895 0.697987 0.054 Uiso calc U . R 1.0 . .
C C24 0.37369(8) 0.0257(4) 0.66661(11) 0.0520(6) Uani d . . . 1.0 . .
H H24 0.380114 -0.050567 0.705135 0.062 Uiso calc U . R 1.0 . .
C C25 0.34155(8) -0.0279(3) 0.61375(11) 0.0495(5) Uani d . . . 1.0 . .
H H25 0.325423 -0.140559 0.61575 0.059 Uiso calc U . R 1.0 . .
C C26 0.33323(7) 0.0853(3) 0.55776(10) 0.0408(5) Uani d . . . 1.0 . .
H H26 0.311648 0.045903 0.521325 0.049 Uiso calc U . R 1.0 . .
N N31 0.38975(5) 0.5827(2) 0.54115(8) 0.0328(3) Uani d . . . 1.0 . .
C C32 0.40650(6) 0.4886(3) 0.59811(9) 0.0338(4) Uani d . . . 1.0 . .
C C33 0.44066(7) 0.5641(4) 0.64521(11) 0.0486(5) Uani d . . . 1.0 . .
H H33 0.451888 0.496578 0.684686 0.058 Uiso calc U . R 1.0 . .
C C34 0.45779(7) 0.7397(4) 0.63308(13) 0.0570(6) Uani d . . . 1.0 . .
H H34 0.480723 0.794039 0.664431 0.068 Uiso calc U . R 1.0 . .
C C35 0.44111(7) 0.8343(4) 0.57497(13) 0.0536(6) Uani d . . . 1.0 . .
H H35 0.452555 0.953721 0.565801 0.064 Uiso calc U . R 1.0 . .
C C36 0.40737(7) 0.7522(3) 0.53018(11) 0.0438(5) Uani d . . . 1.0 . .
H H36 0.39619 0.817597 0.490232 0.053 Uiso calc U . R 1.0 . .
B B1A 0.4560(2) -0.2124(12) 0.3496(4) 0.0371(15) Uani d U P D 0.606(3) A 1
F F1A 0.4536(4) -0.3537(15) 0.3032(5) 0.081(2) Uani d U P D 0.606(3) A 1
F F2A 0.4398(2) -0.2702(8) 0.4025(2) 0.1058(15) Uani d U P D 0.606(3) A 1
F F3A 0.4332(2) -0.0537(9) 0.3195(3) 0.092(2) Uani d U P D 0.606(3) A 1
F F4A 0.49793(19) -0.1669(13) 0.3714(3) 0.090(2) Uani d U P D 0.606(3) A 1
B B1B 0.4531(5) -0.195(2) 0.3466(8) 0.047(3) Uani d U P D 0.315(3) B 2
F F1B 0.4470(7) -0.352(2) 0.3062(10) 0.065(3) Uani d U P D 0.315(3) B 2
F F2B 0.4182(3) -0.1934(16) 0.3766(5) 0.104(3) Uani d U P D 0.315(3) B 2
F F3B 0.4483(4) -0.0099(18) 0.3152(7) 0.078(3) Uani d U P D 0.315(3) B 2
F F4B 0.4907(4) -0.187(3) 0.3916(6) 0.089(4) Uani d U P D 0.315(3) B 2
B B1C 0.4554(8) -0.206(4) 0.3431(12) 0.063(4) Uani d U P D 0.079(2) C 3
F F1C 0.4521(14) -0.397(4) 0.3267(15) 0.080(7) Uani d U P D 0.079(2) C 3
F F2C 0.4710(11) -0.195(5) 0.4104(10) 0.084(6) Uani d U P D 0.079(2) C 3
F F3C 0.4147(8) -0.120(5) 0.3352(15) 0.074(6) Uani d U P D 0.079(2) C 3
F F4C 0.4801(9) -0.113(4) 0.3086(12) 0.096(5) Uani d U P D 0.079(2) C 3


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 C4 . 1.796(2) ?
Mn1 C6 . 1.804(2) ?
Mn1 C8 . 1.826(2) ?
Mn1 N21 . 2.0470(15) ?
Mn1 N31 . 2.0481(16) ?
Mn1 C2 . 2.057(2) ?
N1 C2 . 1.310(2) ?
N1 C11 . 1.443(2) ?
N1 H1 . 0.81(3) ?
C2 O3 . 1.326(2) ?
O3 C10 . 1.452(2) ?
C10 H10A . 0.97 ?
C10 H10B . 0.97 ?
C10 H10C . 0.97 ?
C11 C16 . 1.365(3) ?
C11 C12 . 1.368(3) ?
C12 C13 . 1.386(3) ?
C12 H12 . 0.94 ?
C13 C14 . 1.357(4) ?
C13 H13 . 0.94 ?
C14 C15 . 1.359(4) ?
C14 H14 . 0.94 ?
C15 C16 . 1.395(3) ?
C15 H15 . 0.94 ?
C16 H16 . 0.94 ?
C4 O5 . 1.140(3) ?
C6 O7 . 1.147(3) ?
C8 O9 . 1.137(2) ?
N21 C26 . 1.342(2) ?
N21 C22 . 1.357(2) ?
C22 C23 . 1.384(3) ?
C22 C32 . 1.460(3) ?
C23 C24 . 1.372(3) ?
C23 H23 . 0.94 ?
C24 C25 . 1.371(3) ?
C24 H24 . 0.94 ?
C25 C26 . 1.375(3) ?
C25 H25 . 0.94 ?
C26 H26 . 0.94 ?
N31 C36 . 1.342(3) ?
N31 C32 . 1.348(2) ?
C32 C33 . 1.390(3) ?
C33 C34 . 1.378(3) ?
C33 H33 . 0.94 ?
C34 C35 . 1.368(4) ?
C34 H34 . 0.94 ?
C35 C36 . 1.375(3) ?
C35 H35 . 0.94 ?
C36 H36 . 0.94 ?
B1A F4A . 1.348(7) ?
B1A F1A . 1.361(7) ?
B1A F2A . 1.374(7) ?
B1A F3A . 1.386(7) ?
B1B F4B . 1.342(14) ?
B1B F1B . 1.362(13) ?
B1B F2B . 1.393(14) ?
B1B F3B . 1.426(14) ?
B1C F4C . 1.343(17) ?
B1C F1C . 1.358(17) ?
B1C F2C . 1.373(18) ?
B1C F3C . 1.404(17) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C4 Mn1 C6 . . 89.08(10) ?
C4 Mn1 C8 . . 87.96(9) ?
C6 Mn1 C8 . . 86.24(9) ?
C4 Mn1 N21 . . 171.83(9) ?
C6 Mn1 N21 . . 97.35(8) ?
C8 Mn1 N21 . . 87.44(7) ?
C4 Mn1 N31 . . 94.82(9) ?
C6 Mn1 N31 . . 176.00(8) ?
C8 Mn1 N31 . . 93.03(7) ?
N21 Mn1 N31 . . 78.69(6) ?
C4 Mn1 C2 . . 94.84(9) ?
C6 Mn1 C2 . . 94.51(9) ?
C8 Mn1 C2 . . 177.11(8) ?
N21 Mn1 C2 . . 89.69(7) ?
N31 Mn1 C2 . . 86.03(7) ?
C2 N1 C11 . . 126.21(18) ?
C2 N1 H1 . . 121.3(18) ?
C11 N1 H1 . . 112.4(18) ?
N1 C2 O3 . . 115.52(17) ?
N1 C2 Mn1 . . 131.91(14) ?
O3 C2 Mn1 . . 112.57(13) ?
C2 O3 C10 . . 122.02(15) ?
O3 C10 H10A . . 109.5 ?
O3 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
O3 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C16 C11 C12 . . 120.75(19) ?
C16 C11 N1 . . 119.7(2) ?
C12 C11 N1 . . 119.5(2) ?
C11 C12 C13 . . 119.3(2) ?
C11 C12 H12 . . 120.4 ?
C13 C12 H12 . . 120.4 ?
C14 C13 C12 . . 120.5(2) ?
C14 C13 H13 . . 119.8 ?
C12 C13 H13 . . 119.8 ?
C13 C14 C15 . . 120.1(2) ?
C13 C14 H14 . . 119.9 ?
C15 C14 H14 . . 119.9 ?
C14 C15 C16 . . 120.3(2) ?
C14 C15 H15 . . 119.9 ?
C16 C15 H15 . . 119.9 ?
C11 C16 C15 . . 119.1(2) ?
C11 C16 H16 . . 120.5 ?
C15 C16 H16 . . 120.5 ?
O5 C4 Mn1 . . 174.4(2) ?
O7 C6 Mn1 . . 173.4(2) ?
O9 C8 Mn1 . . 175.62(18) ?
C26 N21 C22 . . 117.97(16) ?
C26 N21 Mn1 . . 126.02(13) ?
C22 N21 Mn1 . . 115.55(12) ?
N21 C22 C23 . . 121.39(19) ?
N21 C22 C32 . . 114.86(16) ?
C23 C22 C32 . . 123.73(18) ?
C24 C23 C22 . . 119.7(2) ?
C24 C23 H23 . . 120.2 ?
C22 C23 H23 . . 120.2 ?
C25 C24 C23 . . 119.0(2) ?
C25 C24 H24 . . 120.5 ?
C23 C24 H24 . . 120.5 ?
C24 C25 C26 . . 119.2(2) ?
C24 C25 H25 . . 120.4 ?
C26 C25 H25 . . 120.4 ?
N21 C26 C25 . . 122.7(2) ?
N21 C26 H26 . . 118.6 ?
C25 C26 H26 . . 118.6 ?
C36 N31 C32 . . 118.18(17) ?
C36 N31 Mn1 . . 125.84(14) ?
C32 N31 Mn1 . . 115.96(13) ?
N31 C32 C33 . . 121.72(19) ?
N31 C32 C22 . . 114.77(16) ?
C33 C32 C22 . . 123.50(18) ?
C34 C33 C32 . . 118.9(2) ?
C34 C33 H33 . . 120.5 ?
C32 C33 H33 . . 120.5 ?
C35 C34 C33 . . 119.4(2) ?
C35 C34 H34 . . 120.3 ?
C33 C34 H34 . . 120.3 ?
C34 C35 C36 . . 119.1(2) ?
C34 C35 H35 . . 120.4 ?
C36 C35 H35 . . 120.4 ?
N31 C36 C35 . . 122.7(2) ?
N31 C36 H36 . . 118.7 ?
C35 C36 H36 . . 118.7 ?
F4A B1A F1A . . 107.4(7) ?
F4A B1A F2A . . 108.9(6) ?
F1A B1A F2A . . 112.5(7) ?
F4A B1A F3A . . 110.3(7) ?
F1A B1A F3A . . 108.1(7) ?
F2A B1A F3A . . 109.6(6) ?
F4B B1B F1B . . 116.2(15) ?
F4B B1B F2B . . 111.6(13) ?
F1B B1B F2B . . 105.1(13) ?
F4B B1B F3B . . 105.6(13) ?
F1B B1B F3B . . 116.8(15) ?
F2B B1B F3B . . 100.6(11) ?
F4C B1C F1C . . 111.(2) ?
F4C B1C F2C . . 113.(2) ?
F1C B1C F2C . . 107.(2) ?
F4C B1C F3C . . 112.(2) ?
F1C B1C F3C . . 111.(2) ?
F2C B1C F3C . . 102.0(19) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C11 N1 C2 O3 . . . . -176.0(2) ?
C11 N1 C2 Mn1 . . . . 3.7(4) ?
N1 C2 O3 C10 . . . . 12.4(3) ?
Mn1 C2 O3 C10 . . . . -167.42(19) ?
C2 N1 C11 C16 . . . . -98.2(3) ?
C2 N1 C11 C12 . . . . 84.9(3) ?
C16 C11 C12 C13 . . . . 1.9(4) ?
N1 C11 C12 C13 . . . . 178.7(2) ?
C11 C12 C13 C14 . . . . -0.4(4) ?
C12 C13 C14 C15 . . . . -0.9(4) ?
C13 C14 C15 C16 . . . . 0.8(4) ?
C12 C11 C16 C15 . . . . -2.0(3) ?
N1 C11 C16 C15 . . . . -178.87(19) ?
C14 C15 C16 C11 . . . . 0.7(4) ?
C26 N21 C22 C23 . . . . 1.1(3) ?
Mn1 N21 C22 C23 . . . . 173.82(15) ?
C26 N21 C22 C32 . . . . -177.31(16) ?
Mn1 N21 C22 C32 . . . . -4.6(2) ?
N21 C22 C23 C24 . . . . -1.9(3) ?
C32 C22 C23 C24 . . . . 176.35(19) ?
C22 C23 C24 C25 . . . . 0.9(3) ?
C23 C24 C25 C26 . . . . 0.8(4) ?
C22 N21 C26 C25 . . . . 0.7(3) ?
Mn1 N21 C26 C25 . . . . -171.20(16) ?
C24 C25 C26 N21 . . . . -1.6(3) ?
C36 N31 C32 C33 . . . . 0.9(3) ?
Mn1 N31 C32 C33 . . . . 179.69(15) ?
C36 N31 C32 C22 . . . . -179.02(16) ?
Mn1 N31 C32 C22 . . . . -0.3(2) ?
N21 C22 C32 N31 . . . . 3.2(2) ?
C23 C22 C32 N31 . . . . -175.18(18) ?
N21 C22 C32 C33 . . . . -176.76(18) ?
C23 C22 C32 C33 . . . . 4.9(3) ?
N31 C32 C33 C34 . . . . -0.1(3) ?
C22 C32 C33 C34 . . . . 179.84(19) ?
C32 C33 C34 C35 . . . . -0.6(3) ?
C33 C34 C35 C36 . . . . 0.4(4) ?
C32 N31 C36 C35 . . . . -1.1(3) ?
Mn1 N31 C36 C35 . . . . -179.71(16) ?
C34 C35 C36 N31 . . . . 0.4(3) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 F3A . 0.81(3) 2.40(3) 3.115(6) 148.(2) ?
N1 H1 F3B . 0.81(3) 2.48(3) 3.260(15) 161.(2) ?
N1 H1 F3C . 0.81(3) 2.51(4) 3.09(3) 130.(2) ?

####################################################################### 
# 
# 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_17RPA004
_database_code_depnum_ccdc_archive 'CCDC 1828963'
_audit_update_record             
;
2018-03-12 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            DS-478
_chemical_formula_moiety         'C22 H20 Mn N4 O3, Cl O4'
_chemical_formula_sum            'C22 H20 Cl Mn N4 O7'
_chemical_formula_iupac          ?
_chemical_formula_weight         542.81

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.2177(2)
_cell_length_b                   19.8711(4)
_cell_length_c                   11.7872(2)
_cell_angle_alpha                90
_cell_angle_beta                 116.3700(10)
_cell_angle_gamma                90
_cell_volume                     2354.06(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8709
_cell_measurement_theta_min      2.1839
_cell_measurement_theta_max      25.3692
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       'elongated prism'
_exptl_crystal_colour            'clear pale yellow'
_exptl_crystal_size_max          0.505
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.098
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112

_exptl_absorpt_coefficient_mu    0.725
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.93

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'SIEMENS KFN MO 2K-90'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'κ--geometry diffractometer'
_diffrn_measurement_method       'φ or ω oscillation scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            76486
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         31.55
_diffrn_reflns_theta_full        31.55
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17

_refine_special_details          
;
;

_reflns_number_total             7858
_reflns_number_gt                5268
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1200
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_number_reflns         7858
_refine_ls_number_parameters     320
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0517P)²+0.7299P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.589
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
Cl Cl 0.1484 0.1585 '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'

_computing_data_collection       'Bruker APEX2 software'
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 807)'
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.14673(3) 0.17061(2) 0.62950(3) 0.01812(8) Uani d . . . 1 . .
N N1 0.34778(15) 0.16537(8) 0.67470(14) 0.0194(3) Uani d . . . 1 . .
C C2 0.39423(19) 0.19037(10) 0.60102(17) 0.0199(4) Uani d . . . 1 . .
H H2 0.332063 0.213168 0.527747 0.024 Uiso calc U . R 1 . .
N N3 0.51903(17) 0.18788(9) 0.61589(16) 0.0224(3) Uani d . . . 1 . .
H H3 0.575(2) 0.1622(12) 0.673(2) 0.027 Uiso d U . . 1 . .
C C4 0.1404(2) 0.25931(11) 0.59289(18) 0.0232(4) Uani d . . . 1 . .
O O5 0.13670(17) 0.31632(8) 0.57667(15) 0.0342(4) Uani d . . . 1 . .
C C6 0.44386(19) 0.12912(11) 0.78697(18) 0.0253(4) Uani d . . . 1 . .
H H6A 0.464236 0.085426 0.761168 0.038 Uiso calc U . R 1 . .
H H6B 0.405598 0.122168 0.846366 0.038 Uiso calc U . R 1 . .
H H6C 0.525726 0.155623 0.828147 0.038 Uiso calc U . R 1 . .
C C7 0.5497(2) 0.20907(11) 0.51338(19) 0.0253(4) Uani d . . . 1 . .
H H7A 0.64748 0.211636 0.545359 0.03 Uiso calc U . R 1 . .
H H7B 0.512841 0.254622 0.484849 0.03 Uiso calc U . R 1 . .
C C8 0.4929(2) 0.16091(12) 0.4012(2) 0.0274(4) Uani d . . . 1 . .
C C9 0.5006(3) 0.09160(13) 0.4178(2) 0.0363(5) Uani d . . . 1 . .
H H9 0.543096 0.073608 0.501043 0.044 Uiso calc U . R 1 . .
C C10 0.4484(3) 0.04892(14) 0.3171(3) 0.0427(6) Uani d . . . 1 . .
H H10 0.453265 0.001705 0.331108 0.051 Uiso calc U . R 1 . .
C C11 0.3882(3) 0.07356(17) 0.1943(3) 0.0511(7) Uani d . . . 1 . .
H H11 0.354431 0.043844 0.123815 0.061 Uiso calc U . R 1 . .
C C13 0.4299(3) 0.18567(15) 0.2789(2) 0.0441(6) Uani d . . . 1 . .
H H13 0.421932 0.232914 0.265213 0.053 Uiso calc U . R 1 . .
C C12 0.3787(3) 0.14273(17) 0.1771(3) 0.0554(8) Uani d . . . 1 . .
H H12 0.336208 0.160658 0.093758 0.067 Uiso calc U . R 1 . .
C C24 -0.0284(2) 0.17257(10) 0.58995(18) 0.0239(4) Uani d . . . 1 . .
O O25 -0.13869(15) 0.17519(8) 0.56603(15) 0.0340(4) Uani d . . . 1 . .
C C26 0.1861(2) 0.19589(11) 0.78928(19) 0.0250(4) Uani d . . . 1 . .
O O27 0.21158(17) 0.21489(9) 0.88913(14) 0.0395(4) Uani d . . . 1 . .
N N31 0.11347(15) 0.13469(8) 0.45512(14) 0.0184(3) Uani d . . . 1 . .
C C32 0.14162(17) 0.06852(9) 0.45266(17) 0.0183(4) Uani d . . . 1 . .
C C33 0.13702(19) 0.03799(11) 0.34490(19) 0.0245(4) Uani d . . . 1 . .
H H33 0.159013 -0.008254 0.346062 0.029 Uiso calc U . R 1 . .
C C34 0.1001(2) 0.07557(12) 0.2361(2) 0.0292(5) Uani d . . . 1 . .
H H34 0.097021 0.055675 0.16154 0.035 Uiso calc U . R 1 . .
C C35 0.0678(2) 0.14261(11) 0.23718(19) 0.0288(5) Uani d . . . 1 . .
H H35 0.039887 0.169252 0.162832 0.035 Uiso calc U . R 1 . .
C C36 0.0768(2) 0.17017(10) 0.34823(18) 0.0243(4) Uani d . . . 1 . .
H H36 0.055938 0.21647 0.348829 0.029 Uiso calc U . R 1 . .
N N41 0.16216(15) 0.06919(8) 0.66282(15) 0.0204(3) Uani d . . . 1 . .
C C42 0.17307(18) 0.03204(10) 0.57160(18) 0.0199(4) Uani d . . . 1 . .
C C43 0.2076(2) -0.03540(11) 0.5891(2) 0.0274(4) Uani d . . . 1 . .
H H43 0.216459 -0.060404 0.524564 0.033 Uiso calc U . R 1 . .
C C44 0.2292(2) -0.06582(12) 0.7026(2) 0.0348(5) Uani d . . . 1 . .
H H44 0.255455 -0.111687 0.7176 0.042 Uiso calc U . R 1 . .
C C45 0.2121(2) -0.02909(12) 0.7928(2) 0.0349(5) Uani d . . . 1 . .
H H45 0.223191 -0.04962 0.869616 0.042 Uiso calc U . R 1 . .
C C46 0.17877(19) 0.03805(11) 0.77046(19) 0.0268(4) Uani d . . . 1 . .
H H46 0.167062 0.063283 0.833237 0.032 Uiso calc U . R 1 . .
Cl Cl1 0.83871(5) 0.11247(3) 0.87043(4) 0.02448(11) Uani d . . . 1 . .
O O1 0.74636(15) 0.09668(8) 0.74148(14) 0.0341(4) Uani d . . . 1 . .
O O2 0.79597(17) 0.17372(9) 0.90583(18) 0.0452(5) Uani d . . . 1 . .
O O3 0.96903(16) 0.12144(10) 0.88046(18) 0.0444(4) Uani d . . . 1 . .
O O4 0.8387(2) 0.05835(10) 0.95030(17) 0.0547(5) Uani d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 C26 . 1.804(2) ?
Mn1 C24 . 1.806(2) ?
Mn1 C4 . 1.808(2) ?
Mn1 N41 . 2.0459(17) ?
Mn1 N31 . 2.0476(15) ?
Mn1 N1 . 2.0769(16) ?
N1 C2 . 1.294(2) ?
N1 C6 . 1.471(2) ?
C2 N3 . 1.332(2) ?
C2 H2 . 0.95 ?
N3 C7 . 1.458(2) ?
N3 H3 . 0.85(2) ?
C4 O5 . 1.147(2) ?
C6 H6A . 0.98 ?
C6 H6B . 0.98 ?
C6 H6C . 0.98 ?
C7 C8 . 1.524(3) ?
C7 H7A . 0.99 ?
C7 H7B . 0.99 ?
C8 C13 . 1.384(3) ?
C8 C9 . 1.388(3) ?
C9 C10 . 1.362(3) ?
C9 H9 . 0.95 ?
C10 C11 . 1.387(4) ?
C10 H10 . 0.95 ?
C11 C12 . 1.387(4) ?
C11 H11 . 0.95 ?
C13 C12 . 1.373(4) ?
C13 H13 . 0.95 ?
C12 H12 . 0.95 ?
C24 O25 . 1.142(2) ?
C26 O27 . 1.145(2) ?
N31 C36 . 1.339(2) ?
N31 C32 . 1.356(2) ?
C32 C33 . 1.388(3) ?
C32 C42 . 1.475(3) ?
C33 C34 . 1.379(3) ?
C33 H33 . 0.95 ?
C34 C35 . 1.382(3) ?
C34 H34 . 0.95 ?
C35 C36 . 1.381(3) ?
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
N41 C46 . 1.348(2) ?
N41 C42 . 1.354(2) ?
C42 C43 . 1.385(3) ?
C43 C44 . 1.387(3) ?
C43 H43 . 0.95 ?
C44 C45 . 1.371(4) ?
C44 H44 . 0.95 ?
C45 C46 . 1.379(3) ?
C45 H45 . 0.95 ?
C46 H46 . 0.95 ?
Cl1 O3 . 1.4246(17) ?
Cl1 O4 . 1.4294(18) ?
Cl1 O2 . 1.4362(17) ?
Cl1 O1 . 1.4433(15) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C26 Mn1 C24 . . 89.83(9) ?
C26 Mn1 C4 . . 86.75(9) ?
C24 Mn1 C4 . . 89.69(9) ?
C26 Mn1 N41 . . 96.50(8) ?
C24 Mn1 N41 . . 93.46(8) ?
C4 Mn1 N41 . . 175.47(8) ?
C26 Mn1 N31 . . 174.81(8) ?
C24 Mn1 N31 . . 93.21(8) ?
C4 Mn1 N31 . . 97.46(7) ?
N41 Mn1 N31 . . 79.13(6) ?
C26 Mn1 N1 . . 90.69(8) ?
C24 Mn1 N1 . . 178.36(8) ?
C4 Mn1 N1 . . 91.89(8) ?
N41 Mn1 N1 . . 84.93(6) ?
N31 Mn1 N1 . . 86.15(6) ?
C2 N1 C6 . . 116.05(16) ?
C2 N1 Mn1 . . 121.58(13) ?
C6 N1 Mn1 . . 122.24(12) ?
N1 C2 N3 . . 127.61(18) ?
N1 C2 H2 . . 116.2 ?
N3 C2 H2 . . 116.2 ?
C2 N3 C7 . . 120.09(17) ?
C2 N3 H3 . . 119.4(16) ?
C7 N3 H3 . . 117.3(16) ?
O5 C4 Mn1 . . 175.87(18) ?
N1 C6 H6A . . 109.5 ?
N1 C6 H6B . . 109.5 ?
H6A C6 H6B . . 109.5 ?
N1 C6 H6C . . 109.5 ?
H6A C6 H6C . . 109.5 ?
H6B C6 H6C . . 109.5 ?
N3 C7 C8 . . 112.08(17) ?
N3 C7 H7A . . 109.2 ?
C8 C7 H7A . . 109.2 ?
N3 C7 H7B . . 109.2 ?
C8 C7 H7B . . 109.2 ?
H7A C7 H7B . . 107.9 ?
C13 C8 C9 . . 118.1(2) ?
C13 C8 C7 . . 120.3(2) ?
C9 C8 C7 . . 121.66(19) ?
C10 C9 C8 . . 121.3(2) ?
C10 C9 H9 . . 119.4 ?
C8 C9 H9 . . 119.4 ?
C9 C10 C11 . . 120.8(3) ?
C9 C10 H10 . . 119.6 ?
C11 C10 H10 . . 119.6 ?
C10 C11 C12 . . 118.2(3) ?
C10 C11 H11 . . 120.9 ?
C12 C11 H11 . . 120.9 ?
C12 C13 C8 . . 120.8(3) ?
C12 C13 H13 . . 119.6 ?
C8 C13 H13 . . 119.6 ?
C13 C12 C11 . . 120.9(3) ?
C13 C12 H12 . . 119.6 ?
C11 C12 H12 . . 119.6 ?
O25 C24 Mn1 . . 178.51(19) ?
O27 C26 Mn1 . . 176.9(2) ?
C36 N31 C32 . . 117.89(16) ?
C36 N31 Mn1 . . 127.14(13) ?
C32 N31 Mn1 . . 114.79(12) ?
N31 C32 C33 . . 121.96(18) ?
N31 C32 C42 . . 114.58(16) ?
C33 C32 C42 . . 123.44(18) ?
C34 C33 C32 . . 119.23(19) ?
C34 C33 H33 . . 120.4 ?
C32 C33 H33 . . 120.4 ?
C33 C34 C35 . . 119.00(19) ?
C33 C34 H34 . . 120.5 ?
C35 C34 H34 . . 120.5 ?
C36 C35 C34 . . 118.82(19) ?
C36 C35 H35 . . 120.6 ?
C34 C35 H35 . . 120.6 ?
N31 C36 C35 . . 123.07(19) ?
N31 C36 H36 . . 118.5 ?
C35 C36 H36 . . 118.5 ?
C46 N41 C42 . . 118.28(18) ?
C46 N41 Mn1 . . 126.68(15) ?
C42 N41 Mn1 . . 114.49(13) ?
N41 C42 C43 . . 121.83(18) ?
N41 C42 C32 . . 114.77(17) ?
C43 C42 C32 . . 123.37(18) ?
C42 C43 C44 . . 118.9(2) ?
C42 C43 H43 . . 120.6 ?
C44 C43 H43 . . 120.6 ?
C45 C44 C43 . . 119.4(2) ?
C45 C44 H44 . . 120.3 ?
C43 C44 H44 . . 120.3 ?
C44 C45 C46 . . 119.1(2) ?
C44 C45 H45 . . 120.4 ?
C46 C45 H45 . . 120.4 ?
N41 C46 C45 . . 122.4(2) ?
N41 C46 H46 . . 118.8 ?
C45 C46 H46 . . 118.8 ?
O3 Cl1 O4 . . 109.87(12) ?
O3 Cl1 O2 . . 109.42(11) ?
O4 Cl1 O2 . . 110.39(13) ?
O3 Cl1 O1 . . 110.17(11) ?
O4 Cl1 O1 . . 108.66(11) ?
O2 Cl1 O1 . . 108.31(10) ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C6 N1 C2 N3 . . . . -1.0(3) ?
Mn1 N1 C2 N3 . . . . -176.84(16) ?
N1 C2 N3 C7 . . . . 169.93(19) ?
C2 N3 C7 C8 . . . . -68.8(2) ?
N3 C7 C8 C13 . . . . 136.2(2) ?
N3 C7 C8 C9 . . . . -42.9(3) ?
C13 C8 C9 C10 . . . . 0.3(4) ?
C7 C8 C9 C10 . . . . 179.4(2) ?
C8 C9 C10 C11 . . . . 1.4(4) ?
C9 C10 C11 C12 . . . . -2.1(4) ?
C9 C8 C13 C12 . . . . -1.1(4) ?
C7 C8 C13 C12 . . . . 179.8(2) ?
C8 C13 C12 C11 . . . . 0.3(5) ?
C10 C11 C12 C13 . . . . 1.3(4) ?
C36 N31 C32 C33 . . . . 1.9(3) ?
Mn1 N31 C32 C33 . . . . -173.57(14) ?
C36 N31 C32 C42 . . . . -176.37(16) ?
Mn1 N31 C32 C42 . . . . 8.17(19) ?
N31 C32 C33 C34 . . . . -1.3(3) ?
C42 C32 C33 C34 . . . . 176.76(18) ?
C32 C33 C34 C35 . . . . -0.5(3) ?
C33 C34 C35 C36 . . . . 1.6(3) ?
C32 N31 C36 C35 . . . . -0.7(3) ?
Mn1 N31 C36 C35 . . . . 174.17(16) ?
C34 C35 C36 N31 . . . . -1.1(3) ?
C46 N41 C42 C43 . . . . -3.6(3) ?
Mn1 N41 C42 C43 . . . . 168.44(15) ?
C46 N41 C42 C32 . . . . 174.73(16) ?
Mn1 N41 C42 C32 . . . . -13.2(2) ?
N31 C32 C42 N41 . . . . 3.4(2) ?
C33 C32 C42 N41 . . . . -174.87(17) ?
N31 C32 C42 C43 . . . . -178.35(17) ?
C33 C32 C42 C43 . . . . 3.4(3) ?
N41 C42 C43 C44 . . . . 1.2(3) ?
C32 C42 C43 C44 . . . . -176.94(18) ?
C42 C43 C44 C45 . . . . 1.8(3) ?
C43 C44 C45 C46 . . . . -2.4(3) ?
C42 N41 C46 C45 . . . . 3.0(3) ?
Mn1 N41 C46 C45 . . . . -167.95(16) ?
C44 C45 C46 N41 . . . . 0.0(3) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N3 H3 O1 . 0.85(2) 2.16(2) 2.937(2) 151.(2) ?

