# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_PhaseI
_database_code_depnum_ccdc_archive 'CCDC 1939938'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2019-07-11 deposited with the CCDC.	2019-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H60 Mn2 N20'
_chemical_formula_weight         906.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.8900(18)
_cell_length_b                   17.0382(18)
_cell_length_c                   13.0657(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2424.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    375.00(10)
_cell_measurement_reflns_used    1578
_cell_measurement_theta_min      3.5870
_cell_measurement_theta_max      23.6180

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_F_000             956
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_min  0.95107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.962
_oxdiff_exptl_absorpt_empirical_full_max 1.062
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      375.00(10)
_diffrn_ambient_environment      air
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.6249
_diffrn_reflns_number            7967
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.713
_diffrn_reflns_theta_max         25.678
_diffrn_reflns_theta_full        25.678
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2384
_reflns_number_gt                1332
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1700P)²+0.1600P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2384
_refine_ls_number_parameters     149
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0826
_refine_ls_wR_factor_ref         0.3134
_refine_ls_wR_factor_gt          0.2659
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_restrained_S_all      1.203
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.500000 0.500000 0.500000 0.0557(5) Uani 1 2 d S . P . .
N1 N 0.5139(4) 0.3791(2) 0.5634(3) 0.0868(16) Uani 1 1 d . . . . .
N2A N 0.583(3) 0.250000 0.6297(12) 0.065(7) Uiso 0.41(4) 2 d S . P . .
N2B N 0.521(2) 0.250000 0.6469(12) 0.078(5) Uiso 0.59(4) 2 d S . P . .
N3 N 0.6003(4) 0.5456(3) 0.6368(4) 0.0894(15) Uani 1 1 d . . . . .
N4A N 0.6719(10) 0.5845(7) 0.8043(7) 0.0815(19) Uiso 0.555(16) 1 d . . P . .
N4B N 0.6395(13) 0.5543(9) 0.8245(9) 0.0815(19) Uiso 0.445(16) 1 d . . P . .
N5 N 0.8254(5) 0.5187(3) 0.9159(4) 0.0922(15) Uani 1 1 d . . . . .
C1 C 0.5282(5) 0.3175(3) 0.5942(4) 0.0763(15) Uani 1 1 d . . . . .
C2 C 0.6320(5) 0.5545(3) 0.7182(4) 0.0785(15) Uani 1 1 d . . . . .
C3 C 0.7512(6) 0.5407(3) 0.8639(4) 0.0823(15) Uani 1 1 d . . . . .
N6 N 0.6255(9) 0.250000 0.0060(8) 0.162(5) Uani 1 2 d DS T P . .
C4 C 0.7492(13) 0.2055(13) 0.000(2) 0.218(14) Uani 0.5 1 d D . P . .
C5 C 0.6123(19) 0.250000 0.1244(9) 0.286(13) Uani 1 2 d DS T P . .
C6 C 0.635(2) 0.250000 0.2339(11) 0.56(5) Uani 1 2 d DS T P . .
C7 C 0.554(2) 0.250000 0.3220(17) 0.291(18) Uani 1 2 d DS T P . .
C8 C 0.674(2) 0.250000 0.369(2) 0.261(12) Uani 1 2 d DS T P . .
C9 C 0.536(2) 0.1823(12) -0.0229(17) 0.227(10) Uiso 0.64(2) 1 d D . P . .
C10 C 0.6190(19) 0.1793(16) -0.068(3) 0.227(10) Uiso 0.36(2) 1 d D . P . .
C11 C 0.5201(15) 0.1338(11) -0.1130(15) 0.311(12) Uani 1 1 d D . . . .
C12 C 0.4264(15) 0.0781(9) -0.1435(13) 0.250(6) Uani 1 1 d D U . . .
C13A C 0.302(3) 0.049(5) -0.149(7) 0.221(7) Uiso 0.176(19) 1 d D . P . .
C13B C 0.3239(16) 0.1230(11) -0.1820(12) 0.221(7) Uiso 0.824(19) 1 d D . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N5 2.219(5) 6_557 ?
Mn1 N5 2.219(5) 2_664 ?
Mn1 N3 2.234(5) 5_666 ?
Mn1 N3 2.234(5) . ?
Mn1 N1 2.226(4) 5_666 ?
Mn1 N1 2.226(4) . ?


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
N5 Mn1 N5 180.0 6_557 2_664 ?
N5 Mn1 N3 91.56(17) 6_557 5_666 ?
N5 Mn1 N3 88.44(17) 2_664 5_666 ?
N5 Mn1 N3 88.44(17) 6_557 . ?
N5 Mn1 N3 91.56(17) 2_664 . ?
N3 Mn1 N3 180.0 5_666 . ?
N5 Mn1 N1 89.57(18) 6_557 5_666 ?
N5 Mn1 N1 90.43(18) 2_664 5_666 ?
N3 Mn1 N1 89.49(17) 5_666 5_666 ?
N3 Mn1 N1 90.52(17) . 5_666 ?
N5 Mn1 N1 90.43(18) 6_557 . ?
N5 Mn1 N1 89.57(18) 2_664 . ?
N3 Mn1 N1 90.51(17) 5_666 . ?
N3 Mn1 N1 89.48(17) . . ?
N1 Mn1 N1 180.0(2) 5_666 . ?
C1 N1 Mn1 175.9(5) . . ?
C1 N2A C1 113.6(15) 7_565 . ?
C1 N2B C1 117.8(13) 7_565 . ?
C2 N3 Mn1 161.9(5) . . ?
C2 N4A C3 118.7(8) . . ?
C3 N4B C2 115.8(10) . . ?
C3 N5 Mn1 165.1(5) . 2_665 ?


_refine_diff_density_max         0.654
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.089

####################################################################### 
# 
# 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_Phase_II
_database_code_depnum_ccdc_archive 'CCDC 1939939'
loop_
_audit_author_name
_audit_author_address
'Anna Gagor'
;ILT SR PAS Wroclaw Poland
Poland
;
_audit_update_record             
;
2019-07-11 deposited with the CCDC.	2019-08-01 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H60 Mn2 N20'
_chemical_formula_weight         906.94
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_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                   19.6529(13)
_cell_length_b                   13.2746(6)
_cell_length_c                   20.2864(13)
_cell_angle_alpha                90
_cell_angle_beta                 115.633(9)
_cell_angle_gamma                90
_cell_volume                     4771.5(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12929
_cell_measurement_temperature    290.00(12)
_cell_measurement_theta_max      29.4560
_cell_measurement_theta_min      3.2790
_exptl_absorpt_coefficient_mu    0.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1673
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40475
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.535
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      290.00(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6975
_reflns_number_total             9035
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    ?


_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none

_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         9035
_refine_ls_number_restraints     21

_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1148P)²+4.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_atom_sites_solution_hydrogens   geom




_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.2141
_refine_ls_wR_factor_gt          0.1933
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_restrained_S_all      1.176
_refine_ls_shift/su_max          0.024
_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
Mn1 Mn 0.52627(3) 0.24759(3) 0.75812(3) 0.03159(17) Uani 1 1 d . . . . .
Mn2 Mn 0.25622(3) 0.74185(3) 0.52303(3) 0.03048(17) Uani 1 1 d . . . . .
N1 N 0.2359(2) 0.7403(2) 0.62226(19) 0.0515(8) Uani 1 1 d . . . . .
N2 N 0.2008(2) 0.7125(3) 0.7222(2) 0.0643(10) Uani 1 1 d . . . . .
N3 N 0.0781(2) 0.7290(3) 0.7241(2) 0.0560(9) Uani 1 1 d . . . . .
N4 N 0.1739(2) 0.8644(3) 0.4741(2) 0.0569(9) Uani 1 1 d . . . . .
N5 N 0.0666(2) 0.9620(3) 0.3934(3) 0.0848(14) Uani 1 1 d . . . . .
N6 N 0.0617(2) 1.1132(3) 0.32438(19) 0.0563(8) Uani 1 1 d . . . . .
N7 N 0.35172(19) 0.8511(3) 0.57422(19) 0.0549(8) Uani 1 1 d . . . . .
N8 N 0.4655(2) 0.9526(3) 0.6194(2) 0.0642(10) Uani 1 1 d . . . . .
N9 N 0.4932(2) 1.1039(3) 0.6928(2) 0.0591(9) Uani 1 1 d . . . . .
N10 N 0.2682(2) 0.7480(3) 0.4182(2) 0.0552(9) Uani 1 1 d . . . . .
N11 N 0.2692(2) 0.7738(3) 0.29982(19) 0.0565(9) Uani 1 1 d . . . . .
N12 N 0.3725(2) 0.7525(2) 0.26534(19) 0.0508(8) Uani 1 1 d . . . . .
N13 N 0.3360(2) 0.6160(3) 0.5625(2) 0.0588(9) Uani 1 1 d . . . . .
N14 N 0.4095(9) 0.4694(10) 0.5694(6) 0.073(4) Uiso 0.400(19) 1 d . . P . .
N15 N 0.3708(5) 0.4378(6) 0.5622(4) 0.070(3) Uiso 0.600(19) 1 d . . P . .
N16 N 0.4606(2) 0.3388(3) 0.66210(19) 0.0575(9) Uani 1 1 d . . . . .
N17 N 0.5884(2) 0.1582(3) 0.85911(19) 0.0560(8) Uani 1 1 d . . . . .
N18 N 0.6324(3) 0.0545(3) 0.96877(19) 0.0690(11) Uani 1 1 d . . . . .
N19 N 0.66674(19) -0.1226(3) 0.9778(2) 0.0571(9) Uani 1 1 d . . . . .
C1 C 0.2724(2) 0.7579(3) 0.3646(2) 0.0415(8) Uani 1 1 d . . . . .
C2 C 0.3273(2) 0.7616(2) 0.2858(2) 0.0396(8) Uani 1 1 d . . . . .
C3 C 0.4037(2) 0.9014(3) 0.59753(19) 0.0422(8) Uani 1 1 d . . . . .
C4 C 0.47670(19) 1.0327(3) 0.65871(19) 0.0397(7) Uani 1 1 d . . . . .
C5 C 0.1267(2) 0.9138(3) 0.4354(2) 0.0471(9) Uani 1 1 d . . . . .
C6 C 0.0686(2) 1.0436(3) 0.3577(2) 0.0512(9) Uani 1 1 d . . . . .
C7 C 0.2143(2) 0.7278(3) 0.6661(2) 0.0412(8) Uani 1 1 d . . . . .
C8 C 0.1335(2) 0.7230(3) 0.7194(2) 0.0444(8) Uani 1 1 d . . . . .
C9 C 0.3612(3) 0.5394(4) 0.5685(3) 0.0758(15) Uani 1 1 d . . . . .
C10 C 0.4261(3) 0.3955(4) 0.6209(2) 0.0690(13) Uani 1 1 d . . . . .
C11 C 0.6096(2) 0.1055(3) 0.9085(2) 0.0465(8) Uani 1 1 d . . . . .
C12 C 0.6510(2) -0.0397(3) 0.97058(19) 0.0454(8) Uani 1 1 d . . . . .
N20 N 0.16769(17) 0.5743(2) 0.09607(17) 0.0467(7) Uani 1 1 d . . . . .
C13 C 0.1160(2) 0.4858(3) 0.0737(2) 0.0569(10) Uani 1 1 d . . . . .
H1 H 0.096906 0.474368 0.109387 0.085 Uiso 1 1 calc R U . . .
H2 H 0.143057 0.427345 0.070418 0.085 Uiso 1 1 calc R U . . .
H3 H 0.074672 0.498802 0.027000 0.085 Uiso 1 1 calc R U . . .
C14 C 0.2341(2) 0.5502(3) 0.1694(2) 0.0570(10) Uani 1 1 d . . . . .
H10 H 0.259644 0.491124 0.162907 0.068 Uiso 1 1 calc R U . . .
H11 H 0.269524 0.605801 0.182101 0.068 Uiso 1 1 calc R U . . .
C15 C 0.2159(3) 0.5311(3) 0.2330(2) 0.0576(10) Uani 1 1 d . . . . .
H6 H 0.195191 0.591985 0.243601 0.069 Uiso 1 1 calc R U . . .
H7 H 0.177869 0.478819 0.220011 0.069 Uiso 1 1 calc R U . . .
C16 C 0.2842(3) 0.4996(4) 0.3000(3) 0.0706(13) Uani 1 1 d . . . . .
H18 H 0.321098 0.553541 0.314133 0.085 Uiso 1 1 calc R U . . .
H19 H 0.306495 0.441118 0.288250 0.085 Uiso 1 1 calc R U . . .
C17 C 0.2671(4) 0.4742(4) 0.3643(3) 0.0859(16) Uani 1 1 d . . . . .
H23 H 0.233094 0.417962 0.351776 0.129 Uiso 1 1 calc R U . . .
H24 H 0.244234 0.531354 0.375722 0.129 Uiso 1 1 calc R U . . .
H25 H 0.313122 0.457275 0.405912 0.129 Uiso 1 1 calc R U . . .
C18 C 0.1273(2) 0.6667(3) 0.1022(2) 0.0550(10) Uani 1 1 d . . . . .
H4 H 0.163726 0.720916 0.121424 0.066 Uiso 1 1 calc R U . . .
H5 H 0.107239 0.653731 0.137489 0.066 Uiso 1 1 calc R U . . .
C19 C 0.0637(2) 0.7018(4) 0.0320(3) 0.0645(11) Uani 1 1 d . . . . .
H12 H 0.082848 0.711748 -0.004306 0.077 Uiso 1 1 calc R U . . .
H13 H 0.025494 0.649513 0.014067 0.077 Uiso 1 1 calc R U . . .
C20 C 0.0279(4) 0.7977(5) 0.0403(3) 0.0927(18) Uani 1 1 d . . . . .
H16 H 0.012189 0.788324 0.079130 0.111 Uiso 1 1 calc R U . . .
H17 H 0.066057 0.850095 0.056029 0.111 Uiso 1 1 calc R U . . .
C21 C -0.0365(3) 0.8336(5) -0.0239(3) 0.0922(18) Uani 1 1 d . . . . .
H20 H -0.035958 0.804057 -0.066854 0.138 Uiso 1 1 calc R U . . .
H21 H -0.034142 0.905577 -0.026645 0.138 Uiso 1 1 calc R U . . .
H22 H -0.082211 0.814778 -0.020737 0.138 Uiso 1 1 calc R U . . .
C22 C 0.1970(2) 0.5853(3) 0.0382(2) 0.0552(10) Uani 1 1 d . . . . .
H8 H 0.226802 0.526177 0.040182 0.066 Uiso 1 1 calc R U . . .
H9 H 0.154083 0.586098 -0.009454 0.066 Uiso 1 1 calc R U . . .
C23 C 0.2443(3) 0.6773(4) 0.0443(3) 0.0689(12) Uani 1 1 d . . . . .
H14 H 0.213762 0.737162 0.038009 0.083 Uiso 1 1 calc R U . . .
H15 H 0.285822 0.679742 0.092830 0.083 Uiso 1 1 calc R U . . .
C24 C 0.2749(4) 0.6772(6) -0.0113(3) 0.098(2) Uani 1 1 d . . . . .
H26 H 0.305496 0.737300 -0.003359 0.118 Uiso 1 1 calc R U . . .
H27 H 0.308660 0.619976 -0.000878 0.118 Uiso 1 1 calc R U . . .
C25 C 0.2264(5) 0.6736(9) -0.0844(4) 0.166(5) Uani 1 1 d . . . . .
H36A H 0.206008 0.606919 -0.096998 0.249 Uiso 1 1 calc R U . . .
H36B H 0.253234 0.690759 -0.112709 0.249 Uiso 1 1 calc R U . . .
H36C H 0.186011 0.720782 -0.094639 0.249 Uiso 1 1 calc R U . . .
N21 N 0.08808(19) 0.4018(3) 0.65852(18) 0.0693(11) Uani 1 1 d D . . . .
C26 C 0.0645(4) 0.4986(4) 0.6096(4) 0.109(2) Uani 1 1 d D . . . .
C27 C 0.1728(3) 0.3725(7) 0.6934(13) 0.113(9) Uiso 0.320(17) 1 d D . P . .
C28 C 0.1629(3) 0.4298(5) 0.7240(3) 0.059(2) Uiso 0.680(17) 1 d D . P . .
C29 C 0.2281(2) 0.4519(4) 0.7100(3) 0.0920(18) Uani 1 1 d D . . . .
C30 C 0.2999(5) 0.4615(18) 0.7070(8) 0.067(9) Uiso 0.182(13) 1 d D . P . .
C31 C 0.2939(3) 0.4850(5) 0.7760(3) 0.081(2) Uiso 0.818(13) 1 d D . P . .
C32 C 0.3613(3) 0.5105(6) 0.7676(4) 0.116(2) Uani 1 1 d D . . . .
C33 C 0.0987(3) 0.3166(4) 0.6133(3) 0.064(2) Uiso 0.760(13) 1 d D . P . .
C34 C 0.0258(7) 0.3707(9) 0.5838(6) 0.076(7) Uiso 0.240(13) 1 d D . P . .
C35 C 0.0320(3) 0.2746(4) 0.5547(3) 0.0854(17) Uani 1 1 d D . . . .
C36 C -0.0125(12) 0.2490(6) 0.4790(4) 0.068(8) Uiso 0.232(15) 1 d D . P . .
C37 C 0.0382(4) 0.1839(5) 0.5185(4) 0.089(3) Uiso 0.768(15) 1 d D . P . .
C38 C -0.0271(3) 0.1456(5) 0.4552(3) 0.0880(17) Uani 1 1 d D . . . .
C39 C 0.0256(4) 0.3886(6) 0.6799(4) 0.108(2) Uani 1 1 d . . . . .
C40 C 0.0272(4) 0.2888(5) 0.7196(3) 0.104(2) Uani 1 1 d D . . . .
C41 C 0.0164(9) 0.2043(13) 0.7593(12) 0.112(10) Uiso 0.313(19) 1 d D . P . .
C42 C -0.0412(5) 0.2736(7) 0.7301(6) 0.099(4) Uiso 0.687(19) 1 d D . P . .
C43 C -0.0529(8) 0.1824(7) 0.7641(5) 0.175(5) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N16 2.180(3) . ?
Mn1 N6 2.213(3) 4_676 ?
Mn1 N17 2.221(3) . ?
Mn1 N12 2.236(3) 3_666 ?
Mn1 N3 2.244(3) 2_546 ?
Mn1 N9 2.252(3) 1_545 ?
Mn2 N13 2.192(3) . ?
Mn2 N4 2.204(3) . ?
Mn2 N1 2.215(3) . ?
Mn2 N7 2.240(3) . ?
Mn2 N10 2.241(3) . ?
Mn2 N19 2.246(3) 4_565 ?
N1 C7 1.151(5) . ?
N2 C7 1.290(5) . ?
N2 C8 1.308(5) . ?
N3 C8 1.136(5) . ?
N4 C5 1.131(5) . ?
N5 C5 1.288(5) . ?
N5 C6 1.314(5) . ?
N6 C6 1.118(5) . ?
N7 C3 1.137(5) . ?
N8 C4 1.290(5) . ?
N8 C3 1.293(5) . ?
N9 C4 1.132(5) . ?
N10 C1 1.132(5) . ?
N11 C2 1.300(5) . ?
N11 C1 1.305(5) . ?
N12 C2 1.139(5) . ?
N13 C9 1.115(5) . ?
N14 N15 0.824(12) . ?
N14 C9 1.323(12) . ?
N14 C10 1.365(12) . ?
N15 C10 1.340(8) . ?
N15 C9 1.375(9) . ?
N16 C10 1.110(5) . ?
N17 C11 1.144(5) . ?
N18 C11 1.295(5) . ?
N18 C12 1.300(5) . ?
N19 C12 1.136(5) . ?
N20 C18 1.495(5) . ?
N20 C13 1.490(5) . ?
N20 C22 1.522(5) . ?
N20 C14 1.530(5) . ?
C13 H1 0.9600 . ?
C13 H2 0.9600 . ?
C13 H3 0.9600 . ?
C14 C15 1.501(6) . ?
C14 H10 0.9700 . ?
C14 H11 0.9700 . ?
C15 C16 1.498(7) . ?
C15 H6 0.9700 . ?
C15 H7 0.9700 . ?
C16 C17 1.519(7) . ?
C16 H18 0.9700 . ?
C16 H19 0.9700 . ?
C17 H23 0.9600 . ?
C17 H24 0.9600 . ?
C17 H25 0.9600 . ?
C18 C19 1.506(6) . ?
C18 H4 0.9700 . ?
C18 H5 0.9700 . ?
C19 C20 1.500(7) . ?
C19 H12 0.9700 . ?
C19 H13 0.9700 . ?
C20 C21 1.449(7) . ?
C20 H16 0.9700 . ?
C20 H17 0.9700 . ?
C21 H20 0.9600 . ?
C21 H21 0.9600 . ?
C21 H22 0.9600 . ?
C22 C23 1.506(6) . ?
C22 H8 0.9700 . ?
C22 H9 0.9700 . ?
C23 C24 1.491(7) . ?
C23 H14 0.9700 . ?
C23 H15 0.9700 . ?
C24 C25 1.374(9) . ?
C24 H26 0.9700 . ?
C24 H27 0.9700 . ?
C25 H36A 0.9600 . ?
C25 H36B 0.9600 . ?
C25 H36C 0.9600 . ?
N21 C39 1.479(7) . ?
N21 C33 1.526(4) . ?
N21 C34 1.536(5) . ?
N21 C28 1.541(4) . ?
N21 C27 1.550(5) . ?
N21 C26 1.567(4) . ?
C27 C29 1.445(5) . ?
C28 C29 1.458(4) . ?
C29 C30 1.445(5) . ?
C29 C31 1.471(5) . ?
C30 C32 1.451(5) . ?
C31 C32 1.446(5) . ?
C33 C35 1.447(4) . ?
C34 C35 1.433(5) . ?
C35 C37 1.442(4) . ?
C35 C36 1.440(5) . ?
C36 C38 1.442(5) . ?
C37 C38 1.458(5) . ?
C40 C41 1.450(5) . ?
C40 C42 1.463(5) . ?
C41 C42 1.377(19) . ?
C41 C43 1.436(5) . ?
C42 C43 1.461(5) . ?

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
N16 Mn1 N6 89.31(14) . 4_676 ?
N16 Mn1 N17 176.28(13) . . ?
N6 Mn1 N17 89.01(13) 4_676 . ?
N16 Mn1 N12 92.73(13) . 3_666 ?
N6 Mn1 N12 93.11(13) 4_676 3_666 ?
N17 Mn1 N12 90.68(13) . 3_666 ?
N16 Mn1 N3 88.58(14) . 2_546 ?
N6 Mn1 N3 93.67(13) 4_676 2_546 ?
N17 Mn1 N3 88.21(14) . 2_546 ?
N12 Mn1 N3 173.11(13) 3_666 2_546 ?
N16 Mn1 N9 92.08(13) . 1_545 ?
N6 Mn1 N9 178.41(14) 4_676 1_545 ?
N17 Mn1 N9 89.64(14) . 1_545 ?
N12 Mn1 N9 86.06(12) 3_666 1_545 ?
N3 Mn1 N9 87.13(13) 2_546 1_545 ?
N13 Mn2 N4 175.28(14) . . ?
N13 Mn2 N1 92.44(13) . . ?
N4 Mn2 N1 91.73(13) . . ?
N13 Mn2 N7 90.05(14) . . ?
N4 Mn2 N7 92.03(14) . . ?
N1 Mn2 N7 91.67(13) . . ?
N13 Mn2 N10 91.28(13) . . ?
N4 Mn2 N10 84.48(13) . . ?
N1 Mn2 N10 175.78(13) . . ?
N7 Mn2 N10 90.31(13) . . ?
N13 Mn2 N19 85.52(14) . 4_565 ?
N4 Mn2 N19 92.51(15) . 4_565 ?
N1 Mn2 N19 86.98(13) . 4_565 ?
N7 Mn2 N19 175.30(14) . 4_565 ?
N10 Mn2 N19 91.33(14) . 4_565 ?
C7 N1 Mn2 167.2(3) . . ?
C7 N2 C8 122.3(4) . . ?
C8 N3 Mn1 175.4(4) . 2_556 ?
C5 N4 Mn2 164.3(3) . . ?
C5 N5 C6 122.4(4) . . ?
C6 N6 Mn1 168.9(3) . 4_575 ?
C3 N7 Mn2 173.7(3) . . ?
C4 N8 C3 121.9(3) . . ?
C4 N9 Mn1 178.5(3) . 1_565 ?
C1 N10 Mn2 175.1(3) . . ?
C2 N11 C1 122.4(4) . . ?
C2 N12 Mn1 169.8(3) . 3_666 ?
C9 N13 Mn2 161.7(4) . . ?
C9 N14 C10 116.6(9) . . ?
C10 N15 C9 114.8(7) . . ?
C10 N16 Mn1 168.9(3) . . ?
C11 N17 Mn1 169.3(3) . . ?
C11 N18 C12 120.5(4) . . ?
C12 N19 Mn2 149.1(3) . 4_666 ?
N10 C1 N11 173.3(4) . . ?
N12 C2 N11 172.2(4) . . ?
N7 C3 N8 173.3(4) . . ?
N9 C4 N8 173.1(4) . . ?
N4 C5 N5 171.9(4) . . ?
N6 C6 N5 172.2(4) . . ?
N1 C7 N2 171.2(4) . . ?
N3 C8 N2 173.1(4) . . ?
N13 C9 N14 157.7(9) . . ?
N13 C9 N15 163.1(7) . . ?



_refine_diff_density_max         1.300
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.080

