# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 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_xsc1263a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H9 Br Mn N3 O3'
_chemical_formula_weight         402.09

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.8523(5)
_cell_length_b                   24.8560(15)
_cell_length_c                   7.1018(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.4880(10)
_cell_angle_gamma                90.00
_cell_volume                     1490.40(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9084
_cell_measurement_theta_min      2.412
_cell_measurement_theta_max      28.254

_exptl_crystal_description       block
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    3.581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4548
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            16746
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         28.26
_reflns_number_total             3668
_reflns_number_gt                3353
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker, 2012)'
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.4268P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3668
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0215
_refine_ls_wR_factor_ref         0.0566
_refine_ls_wR_factor_gt          0.0551
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.37969(2) 0.381128(9) 1.09818(3) 0.02998(7) Uani 1 1 d . . .
Br Br 0.27742(2) 0.420920(7) 0.75607(2) 0.04097(6) Uani 1 1 d . . .
O1 O 0.5165(2) 0.33421(6) 1.4923(2) 0.0676(4) Uani 1 1 d . . .
O2 O 0.69846(17) 0.42415(7) 1.1399(3) 0.0763(5) Uani 1 1 d . . .
O3 O 0.47772(17) 0.28725(6) 0.9074(2) 0.0581(4) Uani 1 1 d . . .
N1 N 0.29685(15) 0.44755(5) 1.19749(19) 0.0318(3) Uani 1 1 d . . .
N2 N 0.06505(15) 0.39529(5) 1.1250(2) 0.0340(3) Uani 1 1 d . . .
N3 N 0.15443(14) 0.36101(5) 1.07801(18) 0.0293(2) Uani 1 1 d . . .
C1 C 0.4598(2) 0.35183(6) 1.3404(3) 0.0402(4) Uani 1 1 d . . .
C2 C 0.5742(2) 0.40858(7) 1.1210(3) 0.0438(4) Uani 1 1 d . . .
C3 C 0.43530(18) 0.32236(7) 0.9808(3) 0.0386(3) Uani 1 1 d . . .
C4 C 0.3705(2) 0.49445(6) 1.2593(3) 0.0396(3) Uani 1 1 d . . .
H4A H 0.4757 0.4984 1.2621 0.048 Uiso 1 1 calc R . .
C5 C 0.2957(2) 0.53704(7) 1.3190(3) 0.0467(4) Uani 1 1 d . . .
H5A H 0.3505 0.5689 1.3610 0.056 Uiso 1 1 calc R . .
C6 C 0.1404(2) 0.53241(7) 1.3163(3) 0.0446(4) Uani 1 1 d . . .
H6A H 0.0891 0.5608 1.3566 0.054 Uiso 1 1 calc R . .
C7 C 0.0619(2) 0.48454(7) 1.2521(3) 0.0406(4) Uani 1 1 d . . .
H7A H -0.0432 0.4800 1.2484 0.049 Uiso 1 1 calc R . .
C8 C 0.14390(18) 0.44365(6) 1.1936(2) 0.0323(3) Uani 1 1 d . . .
C9 C 0.07302(17) 0.31165(6) 1.0035(2) 0.0301(3) Uani 1 1 d . . .
C10 C -0.08449(19) 0.31249(7) 0.8885(2) 0.0373(3) Uani 1 1 d . . .
H10A H -0.1383 0.3450 0.8568 0.045 Uiso 1 1 calc R . .
C11 C -0.1606(2) 0.26439(8) 0.8217(3) 0.0452(4) Uani 1 1 d . . .
H11A H -0.2653 0.2645 0.7418 0.054 Uiso 1 1 calc R . .
C12 C -0.0815(2) 0.21628(7) 0.8734(3) 0.0474(4) Uani 1 1 d . . .
H12A H -0.1335 0.1841 0.8290 0.057 Uiso 1 1 calc R . .
C13 C 0.0741(2) 0.21554(7) 0.9905(3) 0.0430(4) Uani 1 1 d . . .
H13A H 0.1260 0.1829 1.0267 0.052 Uiso 1 1 calc R . .
C14 C 0.15347(19) 0.26347(6) 1.0545(2) 0.0352(3) Uani 1 1 d . . .
H14A H 0.2593 0.2632 1.1306 0.042 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn 0.02320(11) 0.02863(12) 0.03681(12) 0.00111(8) 0.00703(9) 0.00034(8)
Br 0.04020(10) 0.04212(10) 0.04038(10) 0.00646(6) 0.01177(7) 0.00053(6)
O1 0.0865(11) 0.0541(8) 0.0472(8) 0.0078(7) -0.0027(7) 0.0113(8)
O2 0.0339(7) 0.0744(11) 0.1215(15) -0.0082(10) 0.0244(8) -0.0143(7)
O3 0.0544(8) 0.0474(8) 0.0780(10) -0.0115(7) 0.0281(7) 0.0075(6)
N1 0.0299(6) 0.0285(6) 0.0351(6) 0.0005(5) 0.0067(5) -0.0009(5)
N2 0.0296(6) 0.0321(6) 0.0413(7) -0.0012(5) 0.0123(5) -0.0014(5)
N3 0.0274(6) 0.0292(6) 0.0309(6) 0.0033(5) 0.0081(5) -0.0010(5)
C1 0.0385(8) 0.0308(8) 0.0464(9) -0.0026(7) 0.0054(7) 0.0021(6)
C2 0.0317(8) 0.0390(9) 0.0595(11) -0.0012(8) 0.0119(7) 0.0014(7)
C3 0.0288(7) 0.0379(8) 0.0481(9) 0.0016(7) 0.0102(7) -0.0001(6)
C4 0.0334(8) 0.0345(8) 0.0480(9) -0.0018(7) 0.0077(7) -0.0054(6)
C5 0.0497(10) 0.0328(8) 0.0521(10) -0.0077(7) 0.0070(8) -0.0053(7)
C6 0.0479(9) 0.0346(8) 0.0498(10) -0.0063(7) 0.0124(8) 0.0050(7)
C7 0.0356(8) 0.0402(9) 0.0465(9) -0.0027(7) 0.0130(7) 0.0034(7)
C8 0.0307(7) 0.0309(7) 0.0343(7) 0.0008(6) 0.0083(6) 0.0002(6)
C9 0.0326(7) 0.0305(7) 0.0293(7) 0.0004(5) 0.0122(6) -0.0050(5)
C10 0.0340(8) 0.0409(8) 0.0357(8) 0.0016(6) 0.0086(6) -0.0033(6)
C11 0.0393(9) 0.0550(11) 0.0406(9) -0.0075(8) 0.0112(7) -0.0155(8)
C12 0.0579(11) 0.0427(9) 0.0485(10) -0.0123(8) 0.0262(8) -0.0216(8)
C13 0.0585(11) 0.0317(8) 0.0463(9) -0.0004(7) 0.0271(8) -0.0034(7)
C14 0.0378(8) 0.0341(8) 0.0355(8) 0.0022(6) 0.0138(6) -0.0015(6)

_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
Mn C1 1.8054(18) . y
Mn C2 1.8139(18) . y
Mn C3 1.8215(17) . y
Mn N1 2.0179(13) . y
Mn N3 2.0187(12) . y
Mn Br 2.5256(3) . y
O1 C1 1.132(2) . ?
O2 C2 1.135(2) . ?
O3 C3 1.136(2) . ?
N1 C4 1.3436(19) . ?
N1 C8 1.349(2) . ?
N2 N3 1.2735(18) . ?
N2 C8 1.4019(19) . ?
N3 C9 1.4407(18) . ?
C4 C5 1.381(2) . ?
C5 C6 1.374(3) . ?
C6 C7 1.384(2) . ?
C7 C8 1.383(2) . ?
C9 C14 1.385(2) . ?
C9 C10 1.388(2) . ?
C10 C11 1.384(2) . ?
C11 C12 1.379(3) . ?
C12 C13 1.379(3) . ?
C13 C14 1.388(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Mn C2 88.62(8) . . y
C1 Mn C3 91.70(8) . . y
C2 Mn C3 87.86(8) . . y
C1 Mn N1 94.42(6) . . y
C2 Mn N1 95.51(7) . . y
C3 Mn N1 173.08(6) . . y
C1 Mn N3 93.70(7) . . y
C2 Mn N3 172.15(7) . . y
C3 Mn N3 99.55(6) . . y
N1 Mn N3 76.85(5) . . y
C1 Mn Br 177.71(6) . . y
C2 Mn Br 89.71(6) . . y
C3 Mn Br 86.67(5) . . y
N1 Mn Br 87.30(4) . . y
N3 Mn Br 88.16(3) . . y
C4 N1 C8 117.05(13) . . ?
C4 N1 Mn 129.22(11) . . ?
C8 N1 Mn 113.69(10) . . ?
N3 N2 C8 112.39(12) . . ?
N2 N3 C9 112.60(12) . . ?
N2 N3 Mn 119.60(10) . . ?
C9 N3 Mn 127.69(10) . . ?
O1 C1 Mn 176.96(18) . . ?
O2 C2 Mn 177.37(19) . . ?
O3 C3 Mn 176.02(15) . . ?
N1 C4 C5 122.32(16) . . ?
C6 C5 C4 120.11(16) . . ?
C5 C6 C7 118.52(16) . . ?
C8 C7 C6 118.30(16) . . ?
N1 C8 C7 123.69(14) . . ?
N1 C8 N2 117.42(13) . . ?
C7 C8 N2 118.89(14) . . ?
C14 C9 C10 120.90(14) . . ?
C14 C9 N3 118.63(13) . . ?
C10 C9 N3 120.43(13) . . ?
C11 C10 C9 119.20(16) . . ?
C12 C11 C10 120.15(16) . . ?
C11 C12 C13 120.49(16) . . ?
C12 C13 C14 120.09(16) . . ?
C9 C14 C13 119.13(15) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.26
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.051
_database_code_depnum_ccdc_archive 'CCDC 956964'
#######################################################################
#
#                 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_xsc1267b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H24 Cl Mn N3 O7 P'
_chemical_formula_weight         683.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   11.090(4)
_cell_length_b                   12.173(4)
_cell_length_c                   22.935(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.670(9)
_cell_angle_gamma                90.00
_cell_volume                     3095.9(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1400
_exptl_absorpt_coefficient_mu    0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5802
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26098
_diffrn_reflns_av_R_equivalents  0.1476
_diffrn_reflns_av_sigmaI/netI    0.3230
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         27.90
_reflns_number_total             6382
_reflns_number_gt                2857
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 (Bruker, 2012)'
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6382
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1963
_refine_ls_R_factor_gt           0.0970
_refine_ls_wR_factor_ref         0.3401
_refine_ls_wR_factor_gt          0.2281
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_restrained_S_all      0.984
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.18361(10) 0.30982(7) 0.06418(5) 0.0354(4) Uani 1 1 d . . .
P P 0.33583(16) 0.27254(13) 0.13572(9) 0.0348(5) Uani 1 1 d . . .
Cl1 Cl 0.61802(18) 0.27861(16) 0.32951(10) 0.0515(6) Uani 1 1 d . . .
O1 O 0.0030(6) 0.3750(5) -0.0244(3) 0.068(2) Uani 1 1 d . . .
O2 O 0.2653(7) 0.5409(5) 0.0566(4) 0.076(2) Uani 1 1 d . . .
O3 O 0.3650(6) 0.2479(5) -0.0263(3) 0.0575(16) Uani 1 1 d . . .
N1 N 0.0576(5) 0.3471(5) 0.1258(3) 0.0354(13) Uani 1 1 d . . .
N2 N 0.0284(6) 0.1570(5) 0.1224(4) 0.053(2) Uani 1 1 d . . .
N3 N 0.1055(6) 0.1627(5) 0.0817(4) 0.0470(19) Uani 1 1 d . . .
C1 C 0.0735(7) 0.3464(6) 0.0081(4) 0.052(2) Uani 1 1 d . . .
C3 C 0.2937(7) 0.2686(5) 0.0077(4) 0.0397(17) Uani 1 1 d . . .
C4 C 0.0223(8) 0.4464(6) 0.1456(4) 0.050(2) Uani 1 1 d . . .
H4 H 0.0603 0.5087 0.1311 0.060 Uiso 1 1 calc R . .
C5 C -0.0673(9) 0.4599(7) 0.1861(5) 0.063(3) Uani 1 1 d . . .
H5 H -0.0894 0.5297 0.1986 0.076 Uiso 1 1 calc R . .
C6 C -0.1237(9) 0.3675(8) 0.2078(5) 0.068(3) Uani 1 1 d . . .
H6 H -0.1839 0.3749 0.2355 0.081 Uiso 1 1 calc R . .
C7 C -0.0916(8) 0.2664(8) 0.1890(5) 0.059(2) Uani 1 1 d . . .
H7 H -0.1282 0.2033 0.2032 0.071 Uiso 1 1 calc R . .
C8 C -0.0008(7) 0.2606(6) 0.1471(4) 0.047(2) Uani 1 1 d . . .
C9 C 0.1284(7) 0.0589(6) 0.0549(4) 0.047(2) Uani 1 1 d . . .
C10 C 0.1273(7) -0.0358(6) 0.0905(4) 0.048(2) Uani 1 1 d . . .
H10 H 0.1110 -0.0324 0.1301 0.057 Uiso 1 1 calc R . .
C11 C 0.1528(9) -0.1358(6) 0.0620(5) 0.057(2) Uani 1 1 d . . .
H11 H 0.1535 -0.2007 0.0834 0.069 Uiso 1 1 calc R . .
C12 C 0.1765(10) -0.1396(7) 0.0034(6) 0.079(4) Uani 1 1 d . . .
H12 H 0.1952 -0.2063 -0.0141 0.094 Uiso 1 1 calc R . .
C13 C 0.1727(8) -0.0458(7) -0.0290(5) 0.057(2) Uani 1 1 d . . .
H13 H 0.1864 -0.0502 -0.0689 0.069 Uiso 1 1 calc R . .
C14 C 0.1492(7) 0.0549(6) -0.0048(4) 0.056(3) Uani 1 1 d . . .
H14 H 0.1473 0.1183 -0.0275 0.067 Uiso 1 1 calc R . .
C15 C 0.4507(7) 0.3793(5) 0.1401(4) 0.0394(17) Uani 1 1 d . . .
C16 C 0.4927(8) 0.4224(6) 0.1927(4) 0.054(2) Uani 1 1 d . . .
H16 H 0.4615 0.3996 0.2282 0.064 Uiso 1 1 calc R . .
C17 C 0.5830(8) 0.5007(7) 0.1901(5) 0.058(2) Uani 1 1 d . . .
H17 H 0.6119 0.5304 0.2249 0.070 Uiso 1 1 calc R . .
C18 C 0.6323(9) 0.5370(8) 0.1387(6) 0.079(4) Uani 1 1 d . . .
H18 H 0.6882 0.5940 0.1391 0.095 Uiso 1 1 calc R . .
C19 C 0.5990(11) 0.4894(11) 0.0877(6) 0.104(5) Uani 1 1 d . . .
H19 H 0.6374 0.5074 0.0531 0.124 Uiso 1 1 calc R . .
C20 C 0.5056(9) 0.4127(8) 0.0883(5) 0.067(3) Uani 1 1 d . . .
H20 H 0.4790 0.3826 0.0531 0.080 Uiso 1 1 calc R . .
C21 C 0.4313(6) 0.1500(5) 0.1293(3) 0.0366(16) Uani 1 1 d . . .
C22 C 0.5260(7) 0.1375(6) 0.1688(4) 0.0432(18) Uani 1 1 d . . .
H22 H 0.5389 0.1896 0.1979 0.052 Uiso 1 1 calc R . .
C23 C 0.6008(7) 0.0477(6) 0.1647(4) 0.049(2) Uani 1 1 d . . .
H23 H 0.6634 0.0396 0.1917 0.059 Uiso 1 1 calc R . .
C24 C 0.5858(8) -0.0294(7) 0.1224(4) 0.054(2) Uani 1 1 d . . .
H24 H 0.6374 -0.0895 0.1206 0.065 Uiso 1 1 calc R . .
C25 C 0.4937(7) -0.0177(6) 0.0825(4) 0.0467(19) Uani 1 1 d . . .
H25 H 0.4831 -0.0692 0.0530 0.056 Uiso 1 1 calc R . .
C26 C 0.4159(7) 0.0721(5) 0.0864(3) 0.0390(16) Uani 1 1 d . . .
H26 H 0.3528 0.0794 0.0597 0.047 Uiso 1 1 calc R . .
C27 C 0.2689(6) 0.2646(5) 0.2082(3) 0.0360(16) Uani 1 1 d . . .
C28 C 0.2230(8) 0.3589(6) 0.2347(4) 0.054(3) Uani 1 1 d . . .
H28 H 0.2317 0.4264 0.2163 0.065 Uiso 1 1 calc R . .
C29 C 0.1647(9) 0.3542(7) 0.2881(4) 0.057(2) Uani 1 1 d . . .
H29 H 0.1362 0.4182 0.3052 0.068 Uiso 1 1 calc R . .
C30 C 0.1494(10) 0.2547(8) 0.3153(5) 0.068(3) Uani 1 1 d . . .
H30 H 0.1103 0.2508 0.3508 0.082 Uiso 1 1 calc R . .
C31 C 0.1916(10) 0.1630(7) 0.2899(5) 0.070(3) Uani 1 1 d . . .
H31 H 0.1795 0.0958 0.3082 0.085 Uiso 1 1 calc R . .
C32 C 0.2540(9) 0.1653(6) 0.2361(4) 0.053(2) Uani 1 1 d . . .
H32 H 0.2842 0.1009 0.2200 0.064 Uiso 1 1 calc R . .
C2 C 0.2366(7) 0.4492(6) 0.0611(4) 0.0450(19) Uani 1 1 d . . .
O5 O 0.6883(7) 0.2218(6) 0.2871(4) 0.074(2) Uani 1 1 d . . .
O7 O 0.6338(9) 0.3934(6) 0.3228(5) 0.100(3) Uani 1 1 d . . .
O6 O 0.4966(6) 0.2516(8) 0.3212(5) 0.099(3) Uani 1 1 d . . .
O4 O 0.6557(9) 0.2482(7) 0.3860(4) 0.100(3) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn 0.0360(6) 0.0266(5) 0.0433(7) 0.0028(4) -0.0098(5) -0.0003(4)
P 0.0355(9) 0.0242(7) 0.0446(11) 0.0016(7) -0.0111(8) -0.0021(6)
Cl1 0.0501(11) 0.0466(10) 0.0574(14) -0.0030(9) -0.0182(10) 0.0005(8)
O1 0.075(4) 0.065(4) 0.063(4) 0.007(3) -0.033(4) 0.016(3)
O2 0.084(5) 0.034(3) 0.110(6) 0.011(3) -0.020(4) -0.012(3)
O3 0.062(4) 0.054(3) 0.057(4) -0.001(3) -0.010(3) -0.002(3)
N1 0.034(3) 0.035(3) 0.037(3) 0.000(2) -0.005(3) 0.005(2)
N2 0.037(4) 0.040(3) 0.082(6) 0.005(3) -0.018(4) -0.004(3)
N3 0.034(3) 0.032(3) 0.074(5) 0.001(3) -0.024(4) -0.001(2)
C1 0.050(5) 0.036(3) 0.072(6) -0.014(4) -0.013(4) 0.006(3)
C3 0.045(4) 0.032(3) 0.042(5) -0.006(3) -0.007(4) -0.001(3)
C4 0.056(5) 0.034(3) 0.060(6) 0.009(3) -0.006(4) 0.013(3)
C5 0.060(5) 0.044(4) 0.086(7) -0.006(4) -0.004(5) 0.015(4)
C6 0.049(5) 0.058(5) 0.096(8) 0.007(5) 0.017(5) 0.008(4)
C7 0.044(5) 0.057(5) 0.077(7) 0.004(5) 0.005(5) -0.005(4)
C8 0.036(4) 0.037(3) 0.067(6) -0.001(4) -0.013(4) 0.002(3)
C9 0.042(4) 0.033(3) 0.066(6) -0.001(3) -0.026(4) -0.003(3)
C10 0.045(4) 0.039(4) 0.059(5) -0.001(3) -0.009(4) -0.002(3)
C11 0.065(6) 0.036(4) 0.071(7) 0.000(4) -0.007(5) 0.002(3)
C12 0.065(6) 0.042(5) 0.128(12) -0.019(6) -0.018(7) -0.004(4)
C13 0.053(5) 0.054(5) 0.064(6) -0.023(4) 0.000(4) -0.009(4)
C14 0.044(4) 0.039(4) 0.083(7) -0.006(4) -0.029(5) -0.011(3)
C15 0.042(4) 0.031(3) 0.045(5) 0.000(3) -0.003(3) -0.002(3)
C16 0.055(5) 0.043(4) 0.062(6) -0.006(4) -0.019(4) -0.005(3)
C17 0.051(5) 0.055(5) 0.069(6) -0.014(5) -0.013(5) -0.006(4)
C18 0.056(6) 0.060(5) 0.121(10) 0.018(6) -0.024(7) -0.025(4)
C19 0.088(8) 0.101(9) 0.121(11) 0.053(8) -0.033(8) -0.061(7)
C20 0.067(6) 0.077(6) 0.056(6) 0.016(5) -0.012(5) -0.030(5)
C21 0.034(3) 0.032(3) 0.044(4) -0.003(3) -0.005(3) 0.001(3)
C22 0.035(4) 0.044(4) 0.051(5) -0.003(3) -0.004(3) 0.003(3)
C23 0.042(4) 0.051(4) 0.054(5) 0.000(4) -0.012(4) 0.010(3)
C24 0.049(5) 0.045(4) 0.069(6) 0.001(4) -0.010(4) 0.012(3)
C25 0.048(4) 0.037(3) 0.055(5) -0.001(3) -0.007(4) 0.004(3)
C26 0.040(4) 0.039(3) 0.038(4) 0.000(3) -0.002(3) -0.001(3)
C27 0.035(3) 0.029(3) 0.044(4) 0.001(3) -0.009(3) -0.002(2)
C28 0.067(5) 0.027(3) 0.069(6) 0.000(3) -0.029(5) 0.001(3)
C29 0.077(6) 0.042(4) 0.052(6) -0.008(4) -0.010(5) 0.000(4)
C30 0.080(7) 0.060(5) 0.064(6) 0.011(5) -0.007(6) -0.012(5)
C31 0.085(7) 0.035(4) 0.091(8) 0.005(4) 0.001(7) 0.000(4)
C32 0.069(6) 0.031(3) 0.059(6) 0.004(3) 0.001(5) 0.005(3)
C2 0.042(4) 0.040(4) 0.052(5) -0.006(3) -0.004(4) 0.006(3)
O5 0.077(5) 0.069(4) 0.078(5) -0.018(4) 0.003(4) 0.004(3)
O7 0.106(6) 0.045(4) 0.148(8) 0.001(4) -0.023(6) -0.001(4)
O6 0.041(4) 0.126(7) 0.129(8) -0.038(6) -0.019(5) -0.007(4)
O4 0.120(7) 0.108(7) 0.070(5) 0.003(5) -0.041(5) 0.023(5)

_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
Mn C2 1.797(8) . y
Mn C1 1.818(8) . y
Mn C3 1.859(10) . y
Mn N3 2.031(6) . y
Mn N1 2.050(7) . y
Mn P 2.3839(19) . y
P C15 1.822(7) . ?
P C27 1.830(9) . ?
P C21 1.836(7) . ?
Cl1 O6 1.397(7) . ?
Cl1 O4 1.406(8) . ?
Cl1 O7 1.417(7) . ?
Cl1 O5 1.431(8) . ?
O1 C1 1.130(9) . ?
O2 C2 1.165(9) . ?
O3 C3 1.145(11) . ?
N1 C8 1.332(10) . ?
N1 C4 1.350(9) . ?
N2 N3 1.275(11) . ?
N2 C8 1.421(10) . ?
N3 C9 1.429(10) . ?
C4 C5 1.379(14) . ?
C5 C6 1.382(14) . ?
C6 C7 1.354(14) . ?
C7 C8 1.401(14) . ?
C9 C14 1.394(14) . ?
C9 C10 1.411(11) . ?
C10 C11 1.412(12) . ?
C11 C12 1.372(17) . ?
C12 C13 1.364(14) . ?
C13 C14 1.373(11) . ?
C15 C16 1.392(11) . ?
C15 C20 1.401(13) . ?
C16 C17 1.384(12) . ?
C17 C18 1.378(16) . ?
C18 C19 1.353(18) . ?
C19 C20 1.395(13) . ?
C21 C26 1.375(10) . ?
C21 C22 1.387(9) . ?
C22 C23 1.376(10) . ?
C23 C24 1.359(12) . ?
C24 C25 1.371(10) . ?
C25 C26 1.395(10) . ?
C27 C32 1.380(10) . ?
C27 C28 1.397(11) . ?
C28 C29 1.392(14) . ?
C29 C30 1.374(13) . ?
C30 C31 1.345(15) . ?
C31 C32 1.422(15) . ?

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
C2 Mn C1 87.6(3) . . y
C2 Mn C3 90.6(4) . . y
C1 Mn C3 90.8(4) . . y
C2 Mn N3 168.6(4) . . y
C1 Mn N3 94.1(3) . . y
C3 Mn N3 100.7(3) . . y
C2 Mn N1 92.5(3) . . y
C1 Mn N1 88.6(4) . . y
C3 Mn N1 176.9(3) . . y
N3 Mn N1 76.3(3) . . y
C2 Mn P 88.7(2) . . y
C1 Mn P 176.1(3) . . y
C3 Mn P 87.8(2) . . y
N3 Mn P 89.78(16) . . y
N1 Mn P 92.87(16) . . y
C15 P C27 106.2(3) . . ?
C15 P C21 100.4(3) . . ?
C27 P C21 105.7(3) . . ?
C15 P Mn 113.0(2) . . ?
C27 P Mn 110.1(2) . . ?
C21 P Mn 120.3(2) . . ?
O6 Cl1 O4 109.8(7) . . ?
O6 Cl1 O7 109.7(6) . . ?
O4 Cl1 O7 108.9(6) . . ?
O6 Cl1 O5 109.0(5) . . ?
O4 Cl1 O5 109.9(5) . . ?
O7 Cl1 O5 109.5(6) . . ?
C8 N1 C4 116.1(8) . . ?
C8 N1 Mn 114.6(5) . . ?
C4 N1 Mn 129.2(6) . . ?
N3 N2 C8 113.7(7) . . ?
N2 N3 C9 113.0(7) . . ?
N2 N3 Mn 118.9(5) . . ?
C9 N3 Mn 128.0(7) . . ?
O1 C1 Mn 175.3(8) . . ?
O3 C3 Mn 176.5(6) . . ?
N1 C4 C5 123.2(8) . . ?
C4 C5 C6 118.6(9) . . ?
C7 C6 C5 120.2(11) . . ?
C6 C7 C8 117.3(9) . . ?
N1 C8 C7 124.6(7) . . ?
N1 C8 N2 116.2(8) . . ?
C7 C8 N2 119.1(8) . . ?
C14 C9 C10 122.9(7) . . ?
C14 C9 N3 119.0(7) . . ?
C10 C9 N3 118.1(8) . . ?
C9 C10 C11 115.7(9) . . ?
C12 C11 C10 121.6(8) . . ?
C13 C12 C11 120.1(9) . . ?
C12 C13 C14 122.1(11) . . ?
C13 C14 C9 117.6(8) . . ?
C16 C15 C20 118.8(7) . . ?
C16 C15 P 122.9(7) . . ?
C20 C15 P 118.1(6) . . ?
C17 C16 C15 117.2(9) . . ?
C18 C17 C16 123.5(9) . . ?
C19 C18 C17 119.7(9) . . ?
C18 C19 C20 118.2(12) . . ?
C19 C20 C15 122.2(10) . . ?
C26 C21 C22 118.5(6) . . ?
C26 C21 P 123.4(5) . . ?
C22 C21 P 118.0(5) . . ?
C23 C22 C21 119.7(7) . . ?
C24 C23 C22 121.9(7) . . ?
C23 C24 C25 119.2(7) . . ?
C24 C25 C26 119.6(7) . . ?
C21 C26 C25 121.0(6) . . ?
C32 C27 C28 118.1(9) . . ?
C32 C27 P 121.3(6) . . ?
C28 C27 P 120.4(6) . . ?
C29 C28 C27 121.7(7) . . ?
C30 C29 C28 119.7(9) . . ?
C31 C30 C29 119.4(12) . . ?
C30 C31 C32 122.3(9) . . ?
C27 C32 C31 118.8(8) . . ?
O2 C2 Mn 175.7(7) . . ?

_diffrn_measured_fraction_theta_max 0.862
_diffrn_reflns_theta_full        27.90
_diffrn_measured_fraction_theta_full 0.862
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.142
_database_code_depnum_ccdc_archive 'CCDC 956965'