# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1
#TrackingRef 'Combined CIFS bpxa -Khullar and Mandal.cif'

_chemical_name_systematic        ?
_chemical_name_common            '[Mn2(adc)2(bpma)2(H2O)2]'
_chemical_formula_moiety         'C34 H34 Mn2 N6 O10'
_chemical_formula_sum            'C34 H34 Mn2 N6 O10'
_chemical_formula_iupac          ?
_chemical_formula_weight         796.54

_chemical_melting_point          ?

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
'x-1/2, y, -z-1/2'

_cell_length_a                   14.0877(16)
_cell_length_b                   13.1032(14)
_cell_length_c                   19.028(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3512.5(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9964
_cell_measurement_theta_min      2.3773
_cell_measurement_theta_max      24.9660
_cell_measurement_temperature    296.(2)

_exptl_crystal_description       rectangular
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656

_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_absorpt_correction_T_min  0.6831
_exptl_absorpt_correction_T_max  0.7452

_exptl_special_details           
;
;

_diffrn_ambient_temperature      296.(2)

_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333


_diffrn_reflns_number            35676
_diffrn_reflns_av_R_equivalents  0.1295
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_theta_min         2.14
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_full        25.04
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_reflns_number_total             3111
_reflns_number_gt                2580
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1137
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_restrained_S_all      0.982
_refine_ls_number_reflns         3111
_refine_ls_number_parameters     242
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    undef
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0747P)²+0.5112P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.696
_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       'APEX2 (Bruker)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS)'
_computing_publication_material  'SHELXTL (Bruker AXS)'

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
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.13790(2) 0.00717(2) 0.316199(18) 0.03107(16) Uani d . 1 . .
O O1 0.03721(11) 0.12664(11) 0.31432(8) 0.0432(4) Uani d . 1 . .
O O2 -0.06718(16) 0.24946(16) 0.33366(11) 0.0930(8) Uani d . 1 . .
O O3 0.02638(11) 0.14986(13) 0.60244(9) 0.0555(5) Uani d . 1 . .
O O4 0.10766(10) -0.06343(10) 0.41654(7) 0.0382(4) Uani d . 1 . .
O O5 0.05387(12) -0.11904(12) 0.27291(10) 0.0500(4) Uani d . 1 . .
H H5A 0.023(2) -0.147(2) 0.3111(15) 0.075 Uiso d . 1 . .
H H5B 0.0551(19) -0.168(2) 0.2369(15) 0.075 Uiso d . 1 . .
N N1 0.27827(12) -0.07554(13) 0.28670(10) 0.0397(4) Uani d . 1 . .
N N2 0.25590(12) 0.08158(12) 0.38380(10) 0.0394(4) Uani d . 1 . .
N N3 0.17489(12) 0.05274(12) 0.20263(10) 0.0380(4) Uani d . 1 . .
C C1 0.28854(19) -0.17059(18) 0.32721(15) 0.0616(7) Uani d . 1 . .
H H1A 0.3429 -0.2076 0.3106 0.092 Uiso calc R 1 . .
H H1B 0.2327 -0.2117 0.3214 0.092 Uiso calc R 1 . .
H H1C 0.2967 -0.1545 0.3761 0.092 Uiso calc R 1 . .
C C2 0.35726(17) -0.00525(18) 0.30068(18) 0.0520(7) Uani d . 1 . .
H H2A 0.3609 0.0449 0.2633 0.062 Uiso calc R 1 . .
H H2B 0.4164 -0.0431 0.3013 0.062 Uiso calc R 1 . .
C C3 0.34436(15) 0.04848(16) 0.36998(13) 0.0442(6) Uani d . 1 . .
C C4 0.41882(17) 0.06545(18) 0.41591(15) 0.0598(7) Uani d . 1 . .
H H4 0.4788 0.0396 0.406 0.072 Uiso calc R 1 . .
C C5 0.40368(19) 0.12047(18) 0.47598(17) 0.0631(7) Uani d . 1 . .
H H5 0.4535 0.1338 0.5067 0.076 Uiso calc R 1 . .
C C6 0.31417(18) 0.15567(17) 0.49025(15) 0.0542(6) Uani d . 1 . .
H H6 0.3023 0.1938 0.5305 0.065 Uiso calc R 1 . .
C C7 0.24244(16) 0.13352(15) 0.44394(12) 0.0448(6) Uani d . 1 . .
H H7 0.1814 0.1555 0.4547 0.054 Uiso calc R 1 . .
C C8 0.27348(16) -0.09821(16) 0.21078(12) 0.0438(5) Uani d . 1 . .
H H8A 0.2305 -0.1549 0.2029 0.053 Uiso calc R 1 . .
H H8B 0.3358 -0.118 0.1941 0.053 Uiso calc R 1 . .
C C9 0.23958(16) -0.00670(13) 0.17034(13) 0.0363(5) Uani d . 1 . .
C C10 0.13978(14) 0.13215(15) 0.16639(13) 0.0399(5) Uani d . 1 . .
H H10 0.0952 0.1739 0.1881 0.048 Uiso calc R 1 . .
C C11 0.16657(16) 0.15471(16) 0.09881(13) 0.0462(6) Uani d . 1 . .
H H11 0.1397 0.2097 0.0752 0.055 Uiso calc R 1 . .
C C12 0.23367(16) 0.09489(17) 0.06657(13) 0.0494(6) Uani d . 1 . .
H H12 0.2533 0.1091 0.021 0.059 Uiso calc R 1 . .
C C13 0.27140(17) 0.01366(15) 0.10269(13) 0.0435(6) Uani d . 1 . .
H H13 0.3177 -0.0272 0.0821 0.052 Uiso calc R 1 . .
C C14 -0.01738(14) 0.17727(15) 0.35275(12) 0.0412(5) Uani d . 1 . .
C C15 -0.02220(14) 0.15116(13) 0.42746(12) 0.0369(5) Uani d . 1 . .
C C16 -0.02823(14) 0.13267(14) 0.48872(12) 0.0345(5) Uani d . 1 . .
C C17 -0.03689(14) 0.11365(13) 0.56417(12) 0.0339(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 O1 . 2.1129(14) ?
Mn1 O4 . 2.1638(14) ?
Mn1 O5 . 2.1942(16) ?
Mn1 N3 . 2.3016(18) ?
Mn1 N2 . 2.3170(18) ?
Mn1 N1 . 2.3238(16) ?
O1 C14 . 1.251(2) ?
O2 C14 . 1.232(2) ?
O3 C17 . 1.245(2) ?
O4 C17 5_556 1.250(2) ?
O5 H5A . 0.92(3) ?
O5 H5B . 0.94(3) ?
N1 C2 . 1.469(3) ?
N1 C1 . 1.472(3) ?
N1 C8 . 1.476(3) ?
N2 C7 . 1.345(3) ?
N2 C3 . 1.346(3) ?
N3 C10 . 1.343(3) ?
N3 C9 . 1.347(3) ?
C1 H1A . 0.96 ?
C1 H1B . 0.96 ?
C1 H1C . 0.96 ?
C2 C3 . 1.506(4) ?
C2 H2A . 0.97 ?
C2 H2B . 0.97 ?
C3 C4 . 1.383(3) ?
C4 C5 . 1.368(4) ?
C4 H4 . 0.93 ?
C5 C6 . 1.370(4) ?
C5 H5 . 0.93 ?
C6 C7 . 1.372(3) ?
C6 H6 . 0.93 ?
C7 H7 . 0.93 ?
C8 C9 . 1.503(3) ?
C8 H8A . 0.97 ?
C8 H8B . 0.97 ?
C9 C13 . 1.389(3) ?
C10 C11 . 1.372(3) ?
C10 H10 . 0.93 ?
C11 C12 . 1.373(3) ?
C11 H11 . 0.93 ?
C12 C13 . 1.374(3) ?
C12 H12 . 0.93 ?
C13 H13 . 0.93 ?
C14 C15 . 1.464(3) ?
C15 C16 . 1.194(3) ?
C16 C17 . 1.462(3) ?
C17 O4 5_556 1.250(2) ?

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
O1 Mn1 O4 . . 101.51(5) ?
O1 Mn1 O5 . . 100.95(6) ?
O4 Mn1 O5 . . 84.42(6) ?
O1 Mn1 N3 . . 86.78(6) ?
O4 Mn1 N3 . . 169.69(6) ?
O5 Mn1 N3 . . 88.01(7) ?
O1 Mn1 N2 . . 100.33(6) ?
O4 Mn1 N2 . . 80.29(6) ?
O5 Mn1 N2 . . 155.87(6) ?
N3 Mn1 N2 . . 104.45(6) ?
O1 Mn1 N1 . . 155.89(6) ?
O4 Mn1 N1 . . 100.44(6) ?
O5 Mn1 N1 . . 90.97(6) ?
N3 Mn1 N1 . . 72.64(6) ?
N2 Mn1 N1 . . 73.73(6) ?
C14 O1 Mn1 . . 142.70(14) ?
C17 O4 Mn1 5_556 . 129.89(14) ?
Mn1 O5 H5A . . 104.9(18) ?
Mn1 O5 H5B . . 141.1(17) ?
H5A O5 H5B . . 108.(2) ?
C2 N1 C1 . . 111.2(2) ?
C2 N1 C8 . . 109.76(19) ?
C1 N1 C8 . . 110.28(18) ?
C2 N1 Mn1 . . 107.97(13) ?
C1 N1 Mn1 . . 110.60(13) ?
C8 N1 Mn1 . . 106.93(12) ?
C7 N2 C3 . . 117.4(2) ?
C7 N2 Mn1 . . 125.75(14) ?
C3 N2 Mn1 . . 114.85(15) ?
C10 N3 C9 . . 117.58(19) ?
C10 N3 Mn1 . . 126.86(14) ?
C9 N3 Mn1 . . 115.56(14) ?
N1 C1 H1A . . 109.5 ?
N1 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
N1 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
N1 C2 C3 . . 111.1(2) ?
N1 C2 H2A . . 109.4 ?
C3 C2 H2A . . 109.4 ?
N1 C2 H2B . . 109.4 ?
C3 C2 H2B . . 109.4 ?
H2A C2 H2B . . 108.0 ?
N2 C3 C4 . . 121.8(2) ?
N2 C3 C2 . . 115.7(2) ?
C4 C3 C2 . . 122.5(2) ?
C5 C4 C3 . . 119.6(2) ?
C5 C4 H4 . . 120.2 ?
C3 C4 H4 . . 120.2 ?
C4 C5 C6 . . 119.1(2) ?
C4 C5 H5 . . 120.4 ?
C6 C5 H5 . . 120.4 ?
C5 C6 C7 . . 118.6(2) ?
C5 C6 H6 . . 120.7 ?
C7 C6 H6 . . 120.7 ?
N2 C7 C6 . . 123.4(2) ?
N2 C7 H7 . . 118.3 ?
C6 C7 H7 . . 118.3 ?
N1 C8 C9 . . 110.80(17) ?
N1 C8 H8A . . 109.5 ?
C9 C8 H8A . . 109.5 ?
N1 C8 H8B . . 109.5 ?
C9 C8 H8B . . 109.5 ?
H8A C8 H8B . . 108.1 ?
N3 C9 C13 . . 122.0(2) ?
N3 C9 C8 . . 116.3(2) ?
C13 C9 C8 . . 121.69(19) ?
N3 C10 C11 . . 123.2(2) ?
N3 C10 H10 . . 118.4 ?
C11 C10 H10 . . 118.4 ?
C10 C11 C12 . . 119.0(2) ?
C10 C11 H11 . . 120.5 ?
C12 C11 H11 . . 120.5 ?
C11 C12 C13 . . 119.0(2) ?
C11 C12 H12 . . 120.5 ?
C13 C12 H12 . . 120.5 ?
C12 C13 C9 . . 119.2(2) ?
C12 C13 H13 . . 120.4 ?
C9 C13 H13 . . 120.4 ?
O2 C14 O1 . . 125.8(2) ?
O2 C14 C15 . . 116.06(19) ?
O1 C14 C15 . . 118.17(17) ?
C16 C15 C14 . . 177.7(2) ?
C15 C16 C17 . . 178.0(2) ?
O3 C17 O4 . 5_556 126.9(2) ?
O3 C17 C16 . . 116.72(18) ?
O4 C17 C16 5_556 . 116.40(18) ?
_database_code_depnum_ccdc_archive 'CCDC 933166'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2
#TrackingRef 'Combined CIFS bpxa -Khullar and Mandal.cif'

_chemical_name_systematic        ?
_chemical_name_common            '[Mn2(adc)2(bpea)2]n'
_chemical_formula_moiety         'C36 H34 Mn2 N6 O8'
_chemical_formula_sum            'C36 H34 Mn2 N6 O8'
_chemical_formula_iupac          ?
_chemical_formula_weight         788.57

_chemical_melting_point          ?

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

_cell_length_a                   7.8454(3)
_cell_length_b                   22.3677(8)
_cell_length_c                   9.5853(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.491(2)
_cell_angle_gamma                90
_cell_volume                     1678.94(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1727
_cell_measurement_theta_min      2.3153
_cell_measurement_theta_max      23.5151
_cell_measurement_temperature    200.(2)

_exptl_crystal_description       'rod shaped'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             812

_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_absorpt_correction_T_min  0.6364
_exptl_absorpt_correction_T_max  0.7452

_exptl_special_details           
;
;

_diffrn_ambient_temperature      200.(2)

_diffrn_source                   'sealed tube'
_diffrn_source_type              'fine focus'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       'phi and omega scans'

_diffrn_detector_area_resol_mean 8.3333

_diffrn_reflns_number            15307
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_reflns_number_total             2974
_reflns_number_gt                2081
_reflns_threshold_expression     >2sigma(I)

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1076
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_restrained_S_all      0.974
_refine_ls_number_reflns         2974
_refine_ls_number_parameters     236
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    undef
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0550P)²+0.0000P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.357
_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       'APEX2 (Bruker)'
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS)'
_computing_publication_material  'SHELXTL (Bruker AXS)'

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
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn1 0.56764(6) 0.59717(2) 0.91323(5) 0.02035(17) Uani d . 1 . .
N N1 0.6920(4) 0.64811(11) 0.7295(3) 0.0237(6) Uani d . 1 . .
N N2 0.4280(3) 0.56346(11) 0.7158(3) 0.0237(6) Uani d . 1 . .
N N3 0.4260(4) 0.68588(11) 0.8832(2) 0.0236(6) Uani d . 1 . .
O O1 0.7339(3) 0.52144(10) 0.9052(2) 0.0318(6) Uani d . 1 . .
O O2 0.6153(3) 0.43344(11) 0.9515(2) 0.0387(7) Uani d . 1 . .
O O3 0.7241(3) 0.64013(10) 1.0700(2) 0.0328(6) Uani d . 1 . .
O O4 0.8271(4) 0.64689(12) 1.2903(2) 0.0477(8) Uani d . 1 . .
C C1 0.7349(4) 0.46617(15) 0.9169(3) 0.0239(8) Uani d . 1 . .
C C2 0.8934(4) 0.43510(14) 0.8868(3) 0.0229(8) Uani d . 1 . .
C C3 1.0195(5) 0.40753(14) 0.8631(3) 0.0235(7) Uani d . 1 . .
C C4 0.8311(4) 0.62933(14) 1.1699(3) 0.0246(8) Uani d . 1 . .
C C5 0.5938(5) 0.63854(15) 0.5941(3) 0.0296(9) Uani d . 1 . .
H H5A 0.6753 0.6305 0.5215 0.036 Uiso calc R 1 . .
H H5B 0.5323 0.6759 0.568 0.036 Uiso calc R 1 . .
C C6 0.8720(5) 0.62706(15) 0.7278(3) 0.0298(8) Uani d . 1 . .
H H6B 0.8706 0.5841 0.7032 0.036 Uiso calc R 1 . .
H H6A 0.9254 0.6306 0.8237 0.036 Uiso calc R 1 . .
C C7 0.9852(5) 0.65962(17) 0.6282(3) 0.0386(10) Uani d . 1 . .
H H7C 0.9388 0.6542 0.5318 0.058 Uiso calc R 1 . .
H H7B 1.1011 0.6432 0.638 0.058 Uiso calc R 1 . .
H H7A 0.9882 0.7023 0.6509 0.058 Uiso calc R 1 . .
C C8 0.6832(4) 0.71191(14) 0.7710(3) 0.0271(8) Uani d . 1 . .
H H8A 0.7158 0.7376 0.6928 0.033 Uiso calc R 1 . .
H H8B 0.7647 0.7194 0.8521 0.033 Uiso calc R 1 . .
C C9 0.5055(4) 0.72747(14) 0.8090(3) 0.0253(8) Uani d . 1 . .
C C10 0.4279(5) 0.78140(15) 0.7702(3) 0.0323(9) Uani d . 1 . .
H H10 0.4857 0.8099 0.7167 0.039 Uiso calc R 1 . .
C C11 0.2653(5) 0.79269(16) 0.8113(4) 0.0369(10) Uani d . 1 . .
H H11 0.2099 0.8293 0.7868 0.044 Uiso calc R 1 . .
C C12 0.1840(5) 0.75051(15) 0.8880(3) 0.0321(9) Uani d . 1 . .
H H12 0.0721 0.7575 0.917 0.038 Uiso calc R 1 . .
C C13 0.2687(4) 0.69757(15) 0.9220(3) 0.0284(8) Uani d . 1 . .
H H13 0.2127 0.6685 0.9751 0.034 Uiso calc R 1 . .
C C14 0.3109(5) 0.51998(15) 0.7132(3) 0.0310(9) Uani d . 1 . .
H H14 0.2866 0.5016 0.7991 0.037 Uiso calc R 1 . .
C C15 0.2237(5) 0.50049(16) 0.5926(3) 0.0337(9) Uani d . 1 . .
H H15 0.1385 0.4704 0.5953 0.04 Uiso calc R 1 . .
C C16 0.2639(5) 0.52606(15) 0.4678(4) 0.0329(9) Uani d . 1 . .
H H16 0.2068 0.5135 0.3825 0.039 Uiso calc R 1 . .
C C17 0.3866(4) 0.56960(14) 0.4676(3) 0.0277(8) Uani d . 1 . .
H H17 0.4169 0.587 0.3821 0.033 Uiso calc R 1 . .
C C18 0.4664(4) 0.58812(14) 0.5934(3) 0.0229(8) 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 O2 3_667 2.107(2) ?
Mn1 O3 . 2.113(2) ?
Mn1 O1 . 2.142(2) ?
Mn1 N2 . 2.258(3) ?
Mn1 N3 . 2.284(3) ?
Mn1 N1 . 2.358(3) ?
N1 C5 . 1.484(4) ?
N1 C8 . 1.484(4) ?
N1 C6 . 1.490(4) ?
N2 C14 . 1.337(4) ?
N2 C18 . 1.347(4) ?
N3 C13 . 1.336(4) ?
N3 C9 . 1.347(4) ?
O1 C1 . 1.241(4) ?
O2 C1 . 1.251(4) ?
O2 Mn1 3_667 2.107(2) ?
O3 C4 . 1.258(4) ?
O4 C4 . 1.222(4) ?
C1 C2 . 1.468(5) ?
C2 C3 . 1.199(4) ?
C3 C4 3_767 1.482(5) ?
C4 C3 3_767 1.482(5) ?
C5 C18 . 1.507(4) ?
C5 H5A . 0.99 ?
C5 H5B . 0.99 ?
C6 C7 . 1.527(5) ?
C6 H6B . 0.99 ?
C6 H6A . 0.99 ?
C7 H7C . 0.98 ?
C7 H7B . 0.98 ?
C7 H7A . 0.98 ?
C8 C9 . 1.503(5) ?
C8 H8A . 0.99 ?
C8 H8B . 0.99 ?
C9 C10 . 1.391(5) ?
C10 C11 . 1.381(5) ?
C10 H10 . 0.95 ?
C11 C12 . 1.376(5) ?
C11 H11 . 0.95 ?
C12 C13 . 1.387(5) ?
C12 H12 . 0.95 ?
C13 H13 . 0.95 ?
C14 C15 . 1.378(5) ?
C14 H14 . 0.95 ?
C15 C16 . 1.380(5) ?
C15 H15 . 0.95 ?
C16 C17 . 1.370(5) ?
C16 H16 . 0.95 ?
C17 C18 . 1.387(4) ?
C17 H17 . 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
O2 Mn1 O3 3_667 . 95.64(10) ?
O2 Mn1 O1 3_667 . 101.78(9) ?
O3 Mn1 O1 . . 93.24(9) ?
O2 Mn1 N2 3_667 . 95.37(10) ?
O3 Mn1 N2 . . 168.31(9) ?
O1 Mn1 N2 . . 88.36(9) ?
O2 Mn1 N3 3_667 . 90.88(10) ?
O3 Mn1 N3 . . 87.23(9) ?
O1 Mn1 N3 . . 167.21(9) ?
N2 Mn1 N3 . . 88.68(9) ?
O2 Mn1 N1 3_667 . 160.95(10) ?
O3 Mn1 N1 . . 93.58(9) ?
O1 Mn1 N1 . . 94.29(9) ?
N2 Mn1 N1 . . 74.75(9) ?
N3 Mn1 N1 . . 72.93(9) ?
C5 N1 C8 . . 110.1(3) ?
C5 N1 C6 . . 112.8(3) ?
C8 N1 C6 . . 111.5(3) ?
C5 N1 Mn1 . . 111.54(19) ?
C8 N1 Mn1 . . 103.65(18) ?
C6 N1 Mn1 . . 106.91(18) ?
C14 N2 C18 . . 118.2(3) ?
C14 N2 Mn1 . . 123.8(2) ?
C18 N2 Mn1 . . 118.1(2) ?
C13 N3 C9 . . 118.5(3) ?
C13 N3 Mn1 . . 125.8(2) ?
C9 N3 Mn1 . . 115.4(2) ?
C1 O1 Mn1 . . 141.7(2) ?
C1 O2 Mn1 . 3_667 154.7(2) ?
C4 O3 Mn1 . . 141.8(2) ?
O1 C1 O2 . . 127.3(3) ?
O1 C1 C2 . . 117.1(3) ?
O2 C1 C2 . . 115.7(3) ?
C3 C2 C1 . . 177.3(3) ?
C2 C3 C4 . 3_767 176.7(4) ?
O4 C4 O3 . . 127.1(3) ?
O4 C4 C3 . 3_767 116.5(3) ?
O3 C4 C3 . 3_767 116.4(3) ?
N1 C5 C18 . . 114.9(3) ?
N1 C5 H5A . . 108.5 ?
C18 C5 H5A . . 108.5 ?
N1 C5 H5B . . 108.5 ?
C18 C5 H5B . . 108.5 ?
H5A C5 H5B . . 107.5 ?
N1 C6 C7 . . 116.3(3) ?
N1 C6 H6B . . 108.2 ?
C7 C6 H6B . . 108.2 ?
N1 C6 H6A . . 108.2 ?
C7 C6 H6A . . 108.2 ?
H6B C6 H6A . . 107.4 ?
C6 C7 H7C . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7C C7 H7B . . 109.5 ?
C6 C7 H7A . . 109.5 ?
H7C C7 H7A . . 109.5 ?
H7B C7 H7A . . 109.5 ?
N1 C8 C9 . . 110.3(3) ?
N1 C8 H8A . . 109.6 ?
C9 C8 H8A . . 109.6 ?
N1 C8 H8B . . 109.6 ?
C9 C8 H8B . . 109.6 ?
H8A C8 H8B . . 108.1 ?
N3 C9 C10 . . 122.1(3) ?
N3 C9 C8 . . 115.7(3) ?
C10 C9 C8 . . 122.2(3) ?
C11 C10 C9 . . 118.6(3) ?
C11 C10 H10 . . 120.7 ?
C9 C10 H10 . . 120.7 ?
C12 C11 C10 . . 119.5(3) ?
C12 C11 H11 . . 120.2 ?
C10 C11 H11 . . 120.2 ?
C11 C12 C13 . . 118.7(3) ?
C11 C12 H12 . . 120.7 ?
C13 C12 H12 . . 120.7 ?
N3 C13 C12 . . 122.6(3) ?
N3 C13 H13 . . 118.7 ?
C12 C13 H13 . . 118.7 ?
N2 C14 C15 . . 123.4(3) ?
N2 C14 H14 . . 118.3 ?
C15 C14 H14 . . 118.3 ?
C14 C15 C16 . . 117.9(3) ?
C14 C15 H15 . . 121.0 ?
C16 C15 H15 . . 121.0 ?
C17 C16 C15 . . 119.5(3) ?
C17 C16 H16 . . 120.2 ?
C15 C16 H16 . . 120.2 ?
C16 C17 C18 . . 119.4(3) ?
C16 C17 H17 . . 120.3 ?
C18 C17 H17 . . 120.3 ?
N2 C18 C17 . . 121.4(3) ?
N2 C18 C5 . . 119.1(3) ?
C17 C18 C5 . . 119.4(3) ?

#===END



_database_code_depnum_ccdc_archive 'CCDC 933167'
