# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Andrew Hallett'
_publ_contact_author_email       hallettaj@cardiff.ac.uk

_publ_section_title              
;
The co-ordination chemistry of tris
(3,5-dimethylpyrazolyl)methane manganese carbonyl complexes:
synthetic, electrochemical and DFT studies
;
_publ_author_name                A.Hallett

# Attachment '- Hallett_cifs.cif'

data_2+
_database_code_depnum_ccdc_archive 'CCDC 822692'
#TrackingRef '- Hallett_cifs.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H31 Mn N6 O2 P1, F6 P'
_chemical_formula_sum            'C21 H31 F6 Mn N6 O2 P2'
_chemical_formula_weight         630.40

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'
P P 0.1023 0.0942 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121
_symmetry_space_group_name_Hall  'P 2ab 2ac'

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

_cell_length_a                   12.6906(7)
_cell_length_b                   12.9537(7)
_cell_length_c                   17.4956(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2876.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1919
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      17.26

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.025
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1296
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_process_details   'SADABS V2.05'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.5
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13045
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         23.26
_reflns_number_total             4118
_reflns_number_gt                3402
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0675P)^2^+0.9669P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_number_reflns         4118
_refine_ls_number_parameters     353
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.1575
_refine_ls_wR_factor_gt          0.1493
_refine_ls_goodness_of_fit_ref   1.151
_refine_ls_restrained_S_all      1.164
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn -0.00693(7) 0.75816(6) 0.13140(5) 0.0565(3) Uani 1 1 d . . .
P1 P 0.12508(17) 0.87766(16) 0.11790(14) 0.0766(6) Uani 1 1 d . . .
O2 O -0.1734(5) 0.9132(4) 0.1197(4) 0.108(2) Uani 1 1 d . . .
O1 O -0.0241(5) 0.8120(5) 0.2933(3) 0.120(2) Uani 1 1 d . . .
N1 N -0.1082(4) 0.6335(4) 0.1297(4) 0.0581(14) Uani 1 1 d . . .
N4 N -0.0816(4) 0.5501(4) 0.0861(3) 0.0482(13) Uani 1 1 d . . .
N2 N 0.1031(4) 0.6362(4) 0.1478(3) 0.0559(15) Uani 1 1 d . . .
N5 N 0.1056(4) 0.5610(4) 0.0946(3) 0.0568(14) Uani 1 1 d . . .
N3 N -0.0056(4) 0.7312(3) 0.0125(3) 0.0581(12) Uani 1 1 d . . .
N6 N 0.0150(4) 0.6325(3) -0.0120(3) 0.0514(12) Uani 1 1 d . . .
C16 C -0.2012(5) 0.6120(6) 0.1595(4) 0.0637(19) Uani 1 1 d . . .
C17 C -0.2332(5) 0.5129(6) 0.1372(4) 0.0674(19) Uani 1 1 d . . .
H2 H -0.2950 0.4793 0.1513 0.081 Uiso 1 1 calc R . .
C18 C -0.1556(6) 0.4753(6) 0.0905(4) 0.067(2) Uani 1 1 d . . .
C19 C -0.2579(6) 0.6824(7) 0.2117(5) 0.096(3) Uani 1 1 d . . .
H4A H -0.2839 0.6441 0.2547 0.144 Uiso 1 1 calc R . .
H4B H -0.3159 0.7135 0.1851 0.144 Uiso 1 1 calc R . .
H4C H -0.2107 0.7353 0.2292 0.144 Uiso 1 1 calc R . .
C20 C -0.1477(6) 0.3734(6) 0.0513(5) 0.082(2) Uani 1 1 d . . .
H5A H -0.1533 0.3831 -0.0029 0.124 Uiso 1 1 calc R . .
H5B H -0.2037 0.3293 0.0685 0.124 Uiso 1 1 calc R . .
H5C H -0.0811 0.3422 0.0631 0.124 Uiso 1 1 calc R . .
C21 C 0.1733(5) 0.6035(5) 0.2006(4) 0.0624(17) Uani 1 1 d . . .
C7 C 0.2171(6) 0.5109(6) 0.1790(5) 0.075(2) Uani 1 1 d . . .
H7 H 0.2679 0.4745 0.2062 0.090 Uiso 1 1 calc R . .
C8 C 0.1736(5) 0.4811(5) 0.1111(4) 0.0604(19) Uani 1 1 d . . .
C9 C 0.1930(6) 0.6558(7) 0.2753(4) 0.090(2) Uani 1 1 d . . .
H9A H 0.1609 0.7229 0.2749 0.135 Uiso 1 1 calc R . .
H9B H 0.2675 0.6629 0.2832 0.135 Uiso 1 1 calc R . .
H9C H 0.1633 0.6153 0.3159 0.135 Uiso 1 1 calc R . .
C10 C 0.1891(6) 0.3884(6) 0.0621(5) 0.085(2) Uani 1 1 d . . .
H10A H 0.2399 0.3435 0.0854 0.128 Uiso 1 1 calc R . .
H10B H 0.2141 0.4094 0.0127 0.128 Uiso 1 1 calc R . .
H10C H 0.1234 0.3526 0.0565 0.128 Uiso 1 1 calc R . .
C11 C -0.0219(6) 0.7845(5) -0.0520(4) 0.0646(18) Uani 1 1 d . . .
C12 C -0.0101(6) 0.7224(5) -0.1146(3) 0.0680(17) Uani 1 1 d . . .
H12 H -0.0165 0.7428 -0.1653 0.082 Uiso 1 1 calc R . .
C13 C 0.0124(6) 0.6258(5) -0.0897(3) 0.0625(16) Uani 1 1 d . . .
C14 C -0.0511(8) 0.8950(6) -0.0538(5) 0.104(3) Uani 1 1 d . . .
H14A H -0.1254 0.9015 -0.0628 0.156 Uiso 1 1 calc R . .
H14B H -0.0131 0.9290 -0.0940 0.156 Uiso 1 1 calc R . .
H14C H -0.0336 0.9263 -0.0057 0.156 Uiso 1 1 calc R . .
C15 C 0.0355(7) 0.5267(6) -0.1308(4) 0.090(3) Uani 1 1 d . . .
H15A H 0.1039 0.5020 -0.1161 0.136 Uiso 1 1 calc R . .
H15B H 0.0342 0.5385 -0.1849 0.136 Uiso 1 1 calc R . .
H15C H -0.0167 0.4761 -0.1176 0.136 Uiso 1 1 calc R . .
C3 C 0.0178(4) 0.5516(4) 0.0435(3) 0.0496(14) Uani 1 1 d . . .
H16 H 0.0244 0.4858 0.0162 0.060 Uiso 1 1 calc R . .
C2 C -0.1067(7) 0.8513(6) 0.1223(5) 0.079(2) Uani 1 1 d . . .
C1 C -0.0147(6) 0.7867(6) 0.2293(5) 0.082(2) Uani 1 1 d . . .
C6 C 0.2288(7) 0.8817(7) 0.1900(5) 0.104(3) Uani 1 1 d . . .
H19A H 0.2818 0.9305 0.1748 0.156 Uiso 1 1 calc R . .
H19B H 0.2599 0.8145 0.1949 0.156 Uiso 1 1 calc R . .
H19C H 0.1993 0.9023 0.2381 0.156 Uiso 1 1 calc R . .
C4 C 0.0887(10) 1.0110(6) 0.1195(8) 0.172(6) Uani 1 1 d . . .
H20A H 0.0596 1.0279 0.1685 0.258 Uiso 1 1 calc R . .
H20B H 0.0372 1.0239 0.0805 0.258 Uiso 1 1 calc R . .
H20C H 0.1499 1.0528 0.1103 0.258 Uiso 1 1 calc R . .
C5 C 0.2090(8) 0.8581(9) 0.0342(5) 0.135(4) Uani 1 1 d . . .
H21A H 0.1721 0.8800 -0.0109 0.203 Uiso 1 1 calc R . .
H21B H 0.2266 0.7863 0.0298 0.203 Uiso 1 1 calc R . .
H21C H 0.2724 0.8979 0.0397 0.203 Uiso 1 1 calc R . .
P2 P 0.49684(18) 0.78826(14) 0.36607(12) 0.0779(6) Uani 1 1 d D . .
F1 F 0.4354(8) 0.7172(6) 0.4191(4) 0.205(4) Uani 1 1 d D . .
F2 F 0.5673(6) 0.8500(6) 0.3134(4) 0.187(3) Uani 1 1 d D . .
F3 F 0.4035(7) 0.8434(8) 0.3401(9) 0.317(7) Uani 1 1 d D . .
F4 F 0.5217(11) 0.8588(5) 0.4306(4) 0.268(6) Uani 1 1 d D . .
F5 F 0.5919(7) 0.7200(6) 0.3823(5) 0.200(4) Uani 1 1 d D . .
F6 F 0.4736(5) 0.7101(4) 0.2993(3) 0.144(2) Uani 1 1 d 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
Mn1 0.0526(5) 0.0595(5) 0.0574(6) -0.0035(4) 0.0033(5) 0.0044(5)
P1 0.0819(13) 0.0652(11) 0.0827(16) -0.0012(12) 0.0006(13) -0.0148(10)
O2 0.099(4) 0.083(4) 0.142(6) 0.000(4) 0.004(4) 0.040(3)
O1 0.113(5) 0.178(6) 0.067(3) -0.040(4) 0.007(4) 0.019(5)
N1 0.044(3) 0.067(3) 0.064(4) 0.005(3) 0.010(3) 0.000(3)
N4 0.040(3) 0.053(3) 0.051(3) 0.007(3) 0.008(2) 0.000(3)
N2 0.051(3) 0.059(3) 0.058(4) -0.004(3) 0.007(3) -0.004(3)
N5 0.045(3) 0.064(3) 0.061(4) 0.006(3) -0.003(3) 0.007(3)
N3 0.064(3) 0.053(3) 0.057(3) 0.001(2) -0.002(3) 0.012(3)
N6 0.055(3) 0.048(3) 0.051(3) 0.006(2) 0.002(3) -0.001(3)
C16 0.043(4) 0.098(5) 0.051(4) 0.012(4) 0.008(3) 0.008(4)
C17 0.051(4) 0.081(5) 0.071(5) 0.013(4) -0.004(4) -0.011(4)
C18 0.059(4) 0.076(5) 0.065(5) 0.015(4) -0.003(4) -0.008(4)
C19 0.070(5) 0.124(7) 0.095(6) -0.006(5) 0.029(5) 0.011(5)
C20 0.078(5) 0.071(5) 0.097(6) 0.006(5) -0.004(5) -0.016(4)
C21 0.057(4) 0.067(4) 0.063(4) 0.007(4) -0.012(4) 0.001(3)
C7 0.064(5) 0.082(5) 0.080(6) 0.022(4) -0.012(4) 0.010(4)
C8 0.043(4) 0.059(4) 0.079(5) 0.018(4) 0.009(4) 0.010(3)
C9 0.083(6) 0.109(6) 0.079(5) -0.002(5) -0.021(5) -0.003(5)
C10 0.083(6) 0.076(5) 0.097(6) -0.007(5) -0.006(5) 0.020(4)
C11 0.075(5) 0.057(4) 0.062(4) 0.015(3) -0.006(4) 0.004(3)
C12 0.079(4) 0.074(4) 0.051(4) 0.020(3) -0.010(4) -0.013(4)
C13 0.069(4) 0.070(4) 0.049(3) 0.001(3) 0.002(4) -0.006(4)
C14 0.141(8) 0.071(5) 0.099(7) 0.022(5) 0.000(6) 0.014(5)
C15 0.123(8) 0.086(5) 0.062(5) -0.011(4) 0.017(5) -0.003(5)
C3 0.044(3) 0.056(3) 0.049(3) -0.002(3) 0.003(3) 0.000(3)
C2 0.095(6) 0.074(5) 0.069(5) -0.009(4) -0.011(5) 0.006(4)
C1 0.059(4) 0.101(5) 0.085(5) -0.019(4) 0.009(4) -0.001(5)
C6 0.098(6) 0.120(6) 0.094(6) -0.012(6) -0.012(5) -0.036(6)
C4 0.159(11) 0.063(5) 0.293(19) 0.002(9) -0.033(12) -0.018(6)
C5 0.135(8) 0.180(10) 0.090(7) 0.008(7) 0.041(6) -0.076(8)
P2 0.0758(12) 0.0716(10) 0.0862(13) 0.0157(10) -0.0109(15) -0.0113(12)
F1 0.311(10) 0.166(6) 0.137(5) -0.006(5) 0.107(6) -0.106(6)
F2 0.207(7) 0.204(7) 0.152(6) 0.081(5) -0.024(5) -0.118(6)
F3 0.156(7) 0.252(10) 0.54(2) -0.023(14) -0.081(10) 0.146(8)
F4 0.54(2) 0.136(5) 0.132(6) -0.064(5) 0.065(10) -0.122(10)
F5 0.184(7) 0.189(7) 0.227(9) -0.024(7) -0.088(7) 0.049(6)
F6 0.184(6) 0.149(4) 0.098(4) 0.006(3) -0.016(4) -0.068(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
Mn1 C1 1.755(8) . ?
Mn1 C2 1.756(8) . ?
Mn1 N1 2.064(5) . ?
Mn1 N3 2.110(5) . ?
Mn1 N2 2.129(5) . ?
Mn1 P1 2.293(2) . ?
P1 C4 1.788(9) . ?
P1 C6 1.823(9) . ?
P1 C5 1.829(9) . ?
O2 C2 1.167(9) . ?
O1 C1 1.173(8) . ?
N1 C16 1.321(8) . ?
N1 N4 1.364(7) . ?
N4 C18 1.351(8) . ?
N4 C3 1.465(7) . ?
N2 N5 1.348(7) . ?
N2 C21 1.351(8) . ?
N5 C8 1.378(8) . ?
N5 C3 1.435(7) . ?
N3 C11 1.339(7) . ?
N3 N6 1.373(6) . ?
N6 C13 1.362(7) . ?
N6 C3 1.428(7) . ?
C16 C17 1.402(9) . ?
C16 C19 1.477(9) . ?
C17 C18 1.369(10) . ?
C17 H2 0.9300 . ?
C18 C20 1.491(10) . ?
C19 H4A 0.9600 . ?
C19 H4B 0.9600 . ?
C19 H4C 0.9600 . ?
C20 H5A 0.9600 . ?
C20 H5B 0.9600 . ?
C20 H5C 0.9600 . ?
C21 C7 1.374(10) . ?
C21 C9 1.494(10) . ?
C7 C8 1.366(10) . ?
C7 H7 0.9300 . ?
C8 C10 1.488(9) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.367(9) . ?
C11 C14 1.479(9) . ?
C12 C13 1.355(8) . ?
C12 H12 0.9300 . ?
C13 C15 1.500(9) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C3 H16 0.9800 . ?
C6 H19A 0.9600 . ?
C6 H19B 0.9600 . ?
C6 H19C 0.9600 . ?
C4 H20A 0.9600 . ?
C4 H20B 0.9600 . ?
C4 H20C 0.9600 . ?
C5 H21A 0.9600 . ?
C5 H21B 0.9600 . ?
C5 H21C 0.9600 . ?
P2 F3 1.456(7) . ?
P2 F4 1.487(6) . ?
P2 F2 1.513(6) . ?
P2 F1 1.521(6) . ?
P2 F5 1.522(7) . ?
P2 F6 1.573(6) . ?

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 Mn1 C2 84.4(4) . . ?
C1 Mn1 N1 98.3(3) . . ?
C2 Mn1 N1 95.0(3) . . ?
C1 Mn1 N3 176.2(3) . . ?
C2 Mn1 N3 91.8(3) . . ?
N1 Mn1 N3 82.0(2) . . ?
C1 Mn1 N2 93.5(3) . . ?
C2 Mn1 N2 174.5(3) . . ?
N1 Mn1 N2 80.19(18) . . ?
N3 Mn1 N2 90.3(2) . . ?
C1 Mn1 P1 90.0(3) . . ?
C2 Mn1 P1 93.1(3) . . ?
N1 Mn1 P1 168.96(17) . . ?
N3 Mn1 P1 90.25(16) . . ?
N2 Mn1 P1 92.05(15) . . ?
C4 P1 C6 98.5(5) . . ?
C4 P1 C5 107.2(6) . . ?
C6 P1 C5 97.9(5) . . ?
C4 P1 Mn1 117.5(4) . . ?
C6 P1 Mn1 118.4(3) . . ?
C5 P1 Mn1 114.5(3) . . ?
C16 N1 N4 106.0(5) . . ?
C16 N1 Mn1 135.7(5) . . ?
N4 N1 Mn1 118.3(4) . . ?
C18 N4 N1 111.4(5) . . ?
C18 N4 C3 129.5(6) . . ?
N1 N4 C3 119.1(5) . . ?
N5 N2 C21 103.3(5) . . ?
N5 N2 Mn1 117.3(4) . . ?
C21 N2 Mn1 139.3(5) . . ?
N2 N5 C8 114.3(6) . . ?
N2 N5 C3 118.3(5) . . ?
C8 N5 C3 123.6(6) . . ?
C11 N3 N6 104.3(5) . . ?
C11 N3 Mn1 138.1(4) . . ?
N6 N3 Mn1 117.6(3) . . ?
C13 N6 N3 111.4(5) . . ?
C13 N6 C3 129.2(5) . . ?
N3 N6 C3 118.4(4) . . ?
N1 C16 C17 110.0(6) . . ?
N1 C16 C19 123.3(7) . . ?
C17 C16 C19 126.6(7) . . ?
C18 C17 C16 106.5(6) . . ?
C18 C17 H2 126.8 . . ?
C16 C17 H2 126.8 . . ?
N4 C18 C17 106.2(6) . . ?
N4 C18 C20 124.2(7) . . ?
C17 C18 C20 129.6(7) . . ?
C16 C19 H4A 109.5 . . ?
C16 C19 H4B 109.5 . . ?
H4A C19 H4B 109.5 . . ?
C16 C19 H4C 109.5 . . ?
H4A C19 H4C 109.5 . . ?
H4B C19 H4C 109.5 . . ?
C18 C20 H5A 109.5 . . ?
C18 C20 H5B 109.5 . . ?
H5A C20 H5B 109.5 . . ?
C18 C20 H5C 109.5 . . ?
H5A C20 H5C 109.5 . . ?
H5B C20 H5C 109.5 . . ?
N2 C21 C7 110.6(7) . . ?
N2 C21 C9 124.5(6) . . ?
C7 C21 C9 124.7(7) . . ?
C8 C7 C21 108.8(7) . . ?
C8 C7 H7 125.6 . . ?
C21 C7 H7 125.6 . . ?
C7 C8 N5 102.9(6) . . ?
C7 C8 C10 132.5(7) . . ?
N5 C8 C10 124.6(7) . . ?
C21 C9 H9A 109.5 . . ?
C21 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C21 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 C12 110.7(5) . . ?
N3 C11 C14 123.8(7) . . ?
C12 C11 C14 125.5(7) . . ?
C13 C12 C11 108.0(5) . . ?
C13 C12 H12 126.0 . . ?
C11 C12 H12 126.0 . . ?
C12 C13 N6 105.5(5) . . ?
C12 C13 C15 132.6(6) . . ?
N6 C13 C15 121.9(6) . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N6 C3 N5 112.3(5) . . ?
N6 C3 N4 109.5(5) . . ?
N5 C3 N4 110.7(4) . . ?
N6 C3 H16 108.1 . . ?
N5 C3 H16 108.1 . . ?
N4 C3 H16 108.1 . . ?
O2 C2 Mn1 177.1(9) . . ?
O1 C1 Mn1 175.1(8) . . ?
P1 C6 H19A 109.5 . . ?
P1 C6 H19B 109.5 . . ?
H19A C6 H19B 109.5 . . ?
P1 C6 H19C 109.5 . . ?
H19A C6 H19C 109.5 . . ?
H19B C6 H19C 109.5 . . ?
P1 C4 H20A 109.5 . . ?
P1 C4 H20B 109.5 . . ?
H20A C4 H20B 109.5 . . ?
P1 C4 H20C 109.5 . . ?
H20A C4 H20C 109.5 . . ?
H20B C4 H20C 109.5 . . ?
P1 C5 H21A 109.5 . . ?
P1 C5 H21B 109.5 . . ?
H21A C5 H21B 109.5 . . ?
P1 C5 H21C 109.5 . . ?
H21A C5 H21C 109.5 . . ?
H21B C5 H21C 109.5 . . ?
F3 P2 F4 96.2(7) . . ?
F3 P2 F2 91.8(7) . . ?
F4 P2 F2 90.7(5) . . ?
F3 P2 F1 94.0(7) . . ?
F4 P2 F1 91.0(5) . . ?
F2 P2 F1 173.7(5) . . ?
F3 P2 F5 171.0(6) . . ?
F4 P2 F5 92.7(6) . . ?
F2 P2 F5 87.3(5) . . ?
F1 P2 F5 86.6(5) . . ?
F3 P2 F6 86.1(6) . . ?
F4 P2 F6 177.6(5) . . ?
F2 P2 F6 89.9(4) . . ?
F1 P2 F6 88.1(4) . . ?
F5 P2 F6 85.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 Mn1 P1 C4 -74.8(6) . . . . ?
C2 Mn1 P1 C4 9.6(6) . . . . ?
N1 Mn1 P1 C4 146.7(11) . . . . ?
N3 Mn1 P1 C4 101.4(6) . . . . ?
N2 Mn1 P1 C4 -168.3(6) . . . . ?
C1 Mn1 P1 C6 43.3(5) . . . . ?
C2 Mn1 P1 C6 127.7(5) . . . . ?
N1 Mn1 P1 C6 -95.2(11) . . . . ?
N3 Mn1 P1 C6 -140.5(4) . . . . ?
N2 Mn1 P1 C6 -50.2(4) . . . . ?
C1 Mn1 P1 C5 158.0(5) . . . . ?
C2 Mn1 P1 C5 -117.5(5) . . . . ?
N1 Mn1 P1 C5 19.5(11) . . . . ?
N3 Mn1 P1 C5 -25.8(4) . . . . ?
N2 Mn1 P1 C5 64.5(4) . . . . ?
C1 Mn1 N1 C16 44.2(7) . . . . ?
C2 Mn1 N1 C16 -40.9(7) . . . . ?
N3 Mn1 N1 C16 -132.0(7) . . . . ?
N2 Mn1 N1 C16 136.4(7) . . . . ?
P1 Mn1 N1 C16 -177.8(6) . . . . ?
C1 Mn1 N1 N4 -139.0(5) . . . . ?
C2 Mn1 N1 N4 135.9(6) . . . . ?
N3 Mn1 N1 N4 44.8(4) . . . . ?
N2 Mn1 N1 N4 -46.8(4) . . . . ?
P1 Mn1 N1 N4 -1.0(13) . . . . ?
C16 N1 N4 C18 -2.1(7) . . . . ?
Mn1 N1 N4 C18 -179.7(4) . . . . ?
C16 N1 N4 C3 178.6(5) . . . . ?
Mn1 N1 N4 C3 0.9(7) . . . . ?
C1 Mn1 N2 N5 154.4(5) . . . . ?
C2 Mn1 N2 N5 86(4) . . . . ?
N1 Mn1 N2 N5 56.6(4) . . . . ?
N3 Mn1 N2 N5 -25.3(4) . . . . ?
P1 Mn1 N2 N5 -115.5(4) . . . . ?
C1 Mn1 N2 C21 -20.5(7) . . . . ?
C2 Mn1 N2 C21 -89(4) . . . . ?
N1 Mn1 N2 C21 -118.3(7) . . . . ?
N3 Mn1 N2 C21 159.9(7) . . . . ?
P1 Mn1 N2 C21 69.6(7) . . . . ?
C21 N2 N5 C8 0.5(7) . . . . ?
Mn1 N2 N5 C8 -176.0(4) . . . . ?
C21 N2 N5 C3 159.5(5) . . . . ?
Mn1 N2 N5 C3 -17.0(7) . . . . ?
C1 Mn1 N3 C11 32(5) . . . . ?
C2 Mn1 N3 C11 32.2(8) . . . . ?
N1 Mn1 N3 C11 127.0(7) . . . . ?
N2 Mn1 N3 C11 -153.0(7) . . . . ?
P1 Mn1 N3 C11 -60.9(7) . . . . ?
C1 Mn1 N3 N6 -146(4) . . . . ?
C2 Mn1 N3 N6 -146.0(5) . . . . ?
N1 Mn1 N3 N6 -51.2(5) . . . . ?
N2 Mn1 N3 N6 28.9(5) . . . . ?
P1 Mn1 N3 N6 120.9(4) . . . . ?
C11 N3 N6 C13 0.7(7) . . . . ?
Mn1 N3 N6 C13 179.4(4) . . . . ?
C11 N3 N6 C3 -169.1(5) . . . . ?
Mn1 N3 N6 C3 9.6(7) . . . . ?
N4 N1 C16 C17 1.9(7) . . . . ?
Mn1 N1 C16 C17 179.0(5) . . . . ?
N4 N1 C16 C19 179.2(6) . . . . ?
Mn1 N1 C16 C19 -3.8(11) . . . . ?
N1 C16 C17 C18 -1.2(8) . . . . ?
C19 C16 C17 C18 -178.3(7) . . . . ?
N1 N4 C18 C17 1.3(7) . . . . ?
C3 N4 C18 C17 -179.4(6) . . . . ?
N1 N4 C18 C20 -178.0(7) . . . . ?
C3 N4 C18 C20 1.2(11) . . . . ?
C16 C17 C18 N4 -0.1(8) . . . . ?
C16 C17 C18 C20 179.2(7) . . . . ?
N5 N2 C21 C7 0.2(7) . . . . ?
Mn1 N2 C21 C7 175.5(5) . . . . ?
N5 N2 C21 C9 -174.5(6) . . . . ?
Mn1 N2 C21 C9 0.8(11) . . . . ?
N2 C21 C7 C8 -0.9(9) . . . . ?
C9 C21 C7 C8 173.8(7) . . . . ?
C21 C7 C8 N5 1.1(8) . . . . ?
C21 C7 C8 C10 -178.8(7) . . . . ?
N2 N5 C8 C7 -1.1(7) . . . . ?
C3 N5 C8 C7 -158.8(6) . . . . ?
N2 N5 C8 C10 178.9(6) . . . . ?
C3 N5 C8 C10 21.2(10) . . . . ?
N6 N3 C11 C12 -1.1(8) . . . . ?
Mn1 N3 C11 C12 -179.5(5) . . . . ?
N6 N3 C11 C14 177.6(7) . . . . ?
Mn1 N3 C11 C14 -0.7(12) . . . . ?
N3 C11 C12 C13 1.2(9) . . . . ?
C14 C11 C12 C13 -177.5(8) . . . . ?
C11 C12 C13 N6 -0.8(9) . . . . ?
C11 C12 C13 C15 -178.5(8) . . . . ?
N3 N6 C13 C12 0.1(8) . . . . ?
C3 N6 C13 C12 168.4(6) . . . . ?
N3 N6 C13 C15 178.1(7) . . . . ?
C3 N6 C13 C15 -13.5(11) . . . . ?
C13 N6 C3 N5 124.5(7) . . . . ?
N3 N6 C3 N5 -67.8(7) . . . . ?
C13 N6 C3 N4 -112.1(7) . . . . ?
N3 N6 C3 N4 55.5(7) . . . . ?
N2 N5 C3 N6 72.8(6) . . . . ?
C8 N5 C3 N6 -130.3(6) . . . . ?
N2 N5 C3 N4 -49.9(7) . . . . ?
C8 N5 C3 N4 107.0(6) . . . . ?
C18 N4 C3 N6 117.5(7) . . . . ?
N1 N4 C3 N6 -63.3(6) . . . . ?
C18 N4 C3 N5 -118.2(7) . . . . ?
N1 N4 C3 N5 61.1(7) . . . . ?
C1 Mn1 C2 O2 -10(14) . . . . ?
N1 Mn1 C2 O2 88(14) . . . . ?
N3 Mn1 C2 O2 170(14) . . . . ?
N2 Mn1 C2 O2 59(15) . . . . ?
P1 Mn1 C2 O2 -99(14) . . . . ?
C2 Mn1 C1 O1 -14(8) . . . . ?
N1 Mn1 C1 O1 -108(9) . . . . ?
N3 Mn1 C1 O1 -14(12) . . . . ?
N2 Mn1 C1 O1 171(9) . . . . ?
P1 Mn1 C1 O1 79(9) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        23.26
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.059

data_6+
_database_code_depnum_ccdc_archive 'CCDC 822693'
#TrackingRef '- Hallett_cifs.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C25 H31 Cl4 F6 Mn N7 O2 P'
_chemical_formula_weight         803.28

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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                   12.5498(18)
_cell_length_b                   14.150(2)
_cell_length_c                   19.981(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.070(3)
_cell_angle_gamma                90.00
_cell_volume                     3493.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    56
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1632
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.771248
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'Siemens CCD area detector'
_diffrn_measurement_method       '\w scans with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            18345
_diffrn_reflns_av_R_equivalents  0.0839
_diffrn_reflns_av_sigmaI/netI    0.1045
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6145
_reflns_number_gt                3302
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0815P)^2^+0.6691P] 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         6145
_refine_ls_number_parameters     458
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.1772
_refine_ls_wR_factor_gt          0.1434
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.006
_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
Mn1 Mn 1.55768(6) 1.05858(5) 1.19865(4) 0.0271(2) Uani 1 1 d . . .
N4 N 1.7546(3) 1.0366(3) 1.3037(2) 0.0313(11) Uani 1 1 d . . .
N1 N 1.7029(3) 1.0983(3) 1.2557(2) 0.0317(11) Uani 1 1 d . . .
N5 N 1.7036(3) 0.8949(3) 1.2433(2) 0.0306(10) Uani 1 1 d . . .
N2 N 1.6378(3) 0.9326(3) 1.1870(2) 0.0294(10) Uani 1 1 d . . .
N6 N 1.6050(3) 0.9485(3) 1.3276(2) 0.0280(10) Uani 1 1 d . . .
N3 N 1.5255(3) 1.0001(3) 1.2881(2) 0.0270(10) Uani 1 1 d . . .
O2 O 1.4526(3) 1.2395(3) 1.2181(2) 0.0483(11) Uani 1 1 d . . .
O1 O 1.5990(3) 1.1491(3) 1.0734(2) 0.0522(12) Uani 1 1 d . . .
C22 C 1.9233(5) 1.0169(4) 1.3912(3) 0.0499(17) Uani 1 1 d . . .
H1A H 1.8824 0.9965 1.4262 0.075 Uiso 1 1 calc R . .
H1B H 1.9835 1.0574 1.4118 0.075 Uiso 1 1 calc R . .
H1C H 1.9516 0.9613 1.3709 0.075 Uiso 1 1 calc R . .
C23 C 1.8502(4) 1.0711(4) 1.3372(3) 0.0347(13) Uani 1 1 d . . .
C24 C 1.8595(4) 1.1591(4) 1.3105(3) 0.0404(15) Uani 1 1 d . . .
H3A H 1.9176 1.2020 1.3234 0.048 Uiso 1 1 calc R . .
C4 C 1.7680(4) 1.1746(4) 1.2606(3) 0.0333(13) Uani 1 1 d . . .
C5 C 1.7435(5) 1.2579(4) 1.2152(3) 0.0436(15) Uani 1 1 d . . .
H5A H 1.6659 1.2716 1.2086 0.065 Uiso 1 1 calc R . .
H5B H 1.7643 1.2442 1.1712 0.065 Uiso 1 1 calc R . .
H5C H 1.7843 1.3127 1.2359 0.065 Uiso 1 1 calc R . .
C6 C 1.8364(5) 0.7637(4) 1.2780(3) 0.0479(16) Uani 1 1 d . . .
H6A H 1.7990 0.7410 1.3140 0.072 Uiso 1 1 calc R . .
H6B H 1.8966 0.8049 1.2977 0.072 Uiso 1 1 calc R . .
H6C H 1.8646 0.7096 1.2558 0.072 Uiso 1 1 calc R . .
C7 C 1.7591(4) 0.8178(4) 1.2268(3) 0.0337(13) Uani 1 1 d . . .
C8 C 1.7266(4) 0.8046(4) 1.1585(3) 0.0391(14) Uani 1 1 d . . .
H8A H 1.7501 0.7557 1.1319 0.047 Uiso 1 1 calc R . .
C9 C 1.6521(4) 0.8762(4) 1.1349(3) 0.0338(13) Uani 1 1 d . . .
C10 C 1.5954(5) 0.8920(5) 1.0647(3) 0.0520(17) Uani 1 1 d . . .
H10A H 1.6061 0.9576 1.0515 0.078 Uiso 1 1 calc R . .
H10B H 1.5180 0.8798 1.0621 0.078 Uiso 1 1 calc R . .
H10C H 1.6246 0.8492 1.0339 0.078 Uiso 1 1 calc R . .
C11 C 1.6416(5) 0.8545(4) 1.4364(3) 0.0486(16) Uani 1 1 d . . .
H11A H 1.6747 0.8034 1.4140 0.073 Uiso 1 1 calc R . .
H11B H 1.5977 0.8275 1.4676 0.073 Uiso 1 1 calc R . .
H11C H 1.6986 0.8943 1.4618 0.073 Uiso 1 1 calc R . .
C12 C 1.5712(4) 0.9130(4) 1.3838(3) 0.0338(13) Uani 1 1 d . . .
C13 C 1.4669(4) 0.9435(4) 1.3802(3) 0.0370(14) Uani 1 1 d . . .
H13A H 1.4208 0.9306 1.4120 0.044 Uiso 1 1 calc R . .
C14 C 1.4409(4) 0.9973(4) 1.3209(3) 0.0312(13) Uani 1 1 d . . .
C15 C 1.3359(4) 1.0464(4) 1.2953(3) 0.0424(15) Uani 1 1 d . . .
H15A H 1.3490 1.1142 1.2909 0.064 Uiso 1 1 calc R . .
H15B H 1.2862 1.0365 1.3274 0.064 Uiso 1 1 calc R . .
H15C H 1.3039 1.0205 1.2508 0.064 Uiso 1 1 calc R . .
N7 N 1.4190(3) 0.9948(3) 1.1500(2) 0.0289(10) Uani 1 1 d . . .
C16 C 1.3968(4) 0.9037(4) 1.1626(3) 0.0337(13) Uani 1 1 d . . .
H16A H 1.4465 0.8701 1.1954 0.040 Uiso 1 1 calc R . .
C17 C 1.3054(4) 0.8571(4) 1.1299(3) 0.0395(14) Uani 1 1 d . . .
H17A H 1.2937 0.7928 1.1402 0.047 Uiso 1 1 calc R . .
C18 C 1.2320(5) 0.9038(4) 1.0831(3) 0.0456(16) Uani 1 1 d . . .
H18A H 1.1688 0.8727 1.0603 0.055 Uiso 1 1 calc R . .
C19 C 1.2517(5) 0.9974(4) 1.0693(3) 0.0426(15) Uani 1 1 d . . .
H19A H 1.2022 1.0318 1.0368 0.051 Uiso 1 1 calc R . .
C20 C 1.3441(4) 1.0399(4) 1.1035(3) 0.0341(13) Uani 1 1 d . . .
H20A H 1.3563 1.1044 1.0940 0.041 Uiso 1 1 calc R . .
C1 C 1.5856(4) 1.1100(4) 1.1226(3) 0.0334(13) Uani 1 1 d . . .
C2 C 1.4931(4) 1.1656(4) 1.2114(3) 0.0324(13) Uani 1 1 d . . .
C3 C 1.7098(4) 0.9425(4) 1.3074(2) 0.0275(12) Uani 1 1 d . . .
H24A H 1.7591 0.9057 1.3427 0.033 Uiso 1 1 calc R . .
P1 P 0.92600(15) 0.76369(13) 1.00659(12) 0.0671(7) Uani 1 1 d . . .
F3 F 0.9674(3) 0.8657(3) 0.9953(3) 0.1049(17) Uani 1 1 d . A .
F5 F 0.8820(5) 0.6649(4) 1.0289(5) 0.195(4) Uani 1 1 d . A .
F1 F 0.8046(6) 0.8029(4) 1.0061(4) 0.062(2) Uani 0.661(10) 1 d P A 1
F2 F 1.0432(13) 0.7191(11) 1.0220(8) 0.093(5) Uani 0.661(10) 1 d P A 1
F4 F 0.8986(6) 0.7154(10) 0.9413(4) 0.131(5) Uani 0.661(10) 1 d P A 1
F6 F 0.9505(6) 0.7902(5) 1.0909(3) 0.087(3) Uani 0.661(10) 1 d P A 1
F1' F 0.852(2) 0.794(3) 1.0366(12) 0.231(18) Uani 0.339(10) 1 d P A 2
F2' F 1.0110(17) 0.7699(13) 0.9377(8) 0.143(8) Uani 0.339(10) 1 d P A 2
F4' F 0.8400(14) 0.7959(10) 0.9339(7) 0.092(6) Uani 0.339(10) 1 d P A 2
F6' F 1.0303(17) 0.7422(16) 1.0466(13) 0.074(9) Uani 0.339(10) 1 d P A 2
C99 C 1.7369(6) 1.1734(5) 1.5061(4) 0.078(2) Uani 1 1 d . . .
H99A H 1.7157 1.2234 1.5358 0.093 Uiso 1 1 calc R . .
H99B H 1.7910 1.2006 1.4809 0.093 Uiso 1 1 calc R . .
Cl1 Cl 1.62368(18) 1.13831(15) 1.44832(10) 0.0860(7) Uani 1 1 d . . .
Cl2 Cl 1.79688(17) 1.07903(16) 1.55710(13) 0.0975(8) Uani 1 1 d . . .
C98 C 1.9873(6) 1.0123(6) 1.1386(4) 0.084(3) Uani 1 1 d . . .
H98A H 2.0331 1.0645 1.1267 0.100 Uiso 1 1 calc R . .
H98B H 1.9924 0.9594 1.1069 0.100 Uiso 1 1 calc R . .
Cl3 Cl 2.03718(19) 0.97474(19) 1.22246(12) 0.1037(8) Uani 1 1 d . . .
Cl4 Cl 1.85548(16) 1.05008(18) 1.12816(11) 0.0938(7) 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
Mn1 0.0284(5) 0.0284(5) 0.0230(4) 0.0025(4) 0.0006(3) -0.0016(4)
N4 0.023(2) 0.044(3) 0.025(2) -0.001(2) 0.0005(19) 0.000(2)
N1 0.035(3) 0.035(3) 0.023(2) -0.002(2) -0.0005(19) 0.001(2)
N5 0.029(3) 0.033(3) 0.029(3) 0.000(2) 0.003(2) 0.001(2)
N2 0.030(2) 0.034(3) 0.023(2) 0.003(2) 0.0015(18) 0.001(2)
N6 0.024(2) 0.033(3) 0.027(2) 0.001(2) 0.0036(18) 0.003(2)
N3 0.024(2) 0.033(3) 0.023(2) 0.0043(19) -0.0001(19) 0.005(2)
O2 0.054(3) 0.032(2) 0.059(3) -0.001(2) 0.011(2) 0.004(2)
O1 0.063(3) 0.058(3) 0.033(2) 0.017(2) 0.001(2) -0.017(2)
C22 0.039(4) 0.059(4) 0.045(4) -0.006(3) -0.009(3) 0.001(3)
C23 0.028(3) 0.045(4) 0.029(3) -0.011(3) 0.001(2) -0.002(3)
C24 0.034(3) 0.048(4) 0.037(3) -0.008(3) 0.002(3) -0.011(3)
C4 0.033(3) 0.034(3) 0.033(3) -0.008(3) 0.007(3) -0.007(3)
C5 0.050(4) 0.036(3) 0.044(4) 0.001(3) 0.005(3) -0.015(3)
C6 0.046(4) 0.046(4) 0.049(4) 0.003(3) 0.002(3) 0.015(3)
C7 0.034(3) 0.034(3) 0.034(3) -0.001(3) 0.008(3) 0.003(3)
C8 0.048(4) 0.038(3) 0.035(3) -0.007(3) 0.018(3) 0.006(3)
C9 0.041(3) 0.037(3) 0.023(3) -0.004(3) 0.007(2) -0.002(3)
C10 0.064(4) 0.060(4) 0.031(4) -0.008(3) 0.004(3) 0.000(4)
C11 0.047(4) 0.062(4) 0.037(4) 0.021(3) 0.010(3) 0.002(3)
C12 0.037(3) 0.037(3) 0.027(3) 0.007(2) 0.004(2) 0.000(3)
C13 0.039(3) 0.044(3) 0.031(3) 0.008(3) 0.014(2) 0.003(3)
C14 0.033(3) 0.034(3) 0.027(3) 0.000(2) 0.006(2) -0.003(3)
C15 0.035(3) 0.049(4) 0.045(4) 0.008(3) 0.011(3) 0.011(3)
N7 0.032(3) 0.029(3) 0.024(2) 0.001(2) 0.0026(19) 0.003(2)
C16 0.037(3) 0.034(3) 0.027(3) 0.003(3) -0.002(2) -0.004(3)
C17 0.043(4) 0.038(3) 0.037(3) -0.004(3) 0.004(3) -0.009(3)
C18 0.035(4) 0.056(4) 0.041(4) -0.007(3) -0.009(3) -0.006(3)
C19 0.040(4) 0.043(4) 0.040(4) 0.005(3) -0.007(3) -0.001(3)
C20 0.035(3) 0.033(3) 0.032(3) 0.009(3) -0.001(3) 0.002(3)
C1 0.028(3) 0.030(3) 0.038(4) 0.000(3) -0.004(3) -0.004(2)
C2 0.035(3) 0.034(3) 0.027(3) 0.007(3) 0.001(2) -0.005(3)
C3 0.028(3) 0.033(3) 0.019(3) -0.001(2) -0.001(2) 0.003(3)
P1 0.0424(11) 0.0442(12) 0.1004(17) -0.0262(11) -0.0269(11) 0.0082(9)
F3 0.057(3) 0.098(4) 0.147(5) 0.047(3) -0.018(3) -0.010(3)
F5 0.088(4) 0.077(4) 0.374(12) 0.046(5) -0.081(6) -0.013(3)
F1 0.044(4) 0.046(4) 0.094(7) 0.002(3) 0.005(4) 0.001(3)
F2 0.048(5) 0.106(8) 0.125(11) -0.009(6) 0.014(6) 0.031(5)
F4 0.066(5) 0.260(14) 0.075(6) -0.121(8) 0.033(4) -0.049(7)
F6 0.067(5) 0.128(6) 0.060(4) -0.030(4) -0.009(4) 0.007(4)
F1' 0.13(2) 0.50(5) 0.09(2) -0.02(2) 0.099(19) 0.09(2)
F2' 0.21(2) 0.166(17) 0.066(11) 0.009(10) 0.069(12) 0.011(15)
F4' 0.107(12) 0.091(11) 0.057(9) -0.029(8) -0.042(8) 0.010(9)
F6' 0.031(11) 0.079(15) 0.097(18) 0.064(15) -0.026(11) -0.015(11)
C99 0.070(5) 0.051(5) 0.121(7) 0.008(4) 0.040(5) 0.002(4)
Cl1 0.1094(17) 0.0800(14) 0.0721(14) -0.0110(11) 0.0256(12) -0.0286(13)
Cl2 0.0748(14) 0.0922(16) 0.140(2) 0.0455(15) 0.0590(14) 0.0230(12)
C98 0.057(5) 0.134(8) 0.063(5) -0.017(5) 0.020(4) 0.002(5)
Cl3 0.0932(17) 0.141(2) 0.0734(15) 0.0018(14) 0.0050(12) 0.0130(15)
Cl4 0.0550(12) 0.130(2) 0.0976(17) -0.0282(14) 0.0163(11) 0.0098(12)

_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 C2 1.757(6) . ?
Mn1 C1 1.774(6) . ?
Mn1 N7 2.048(4) . ?
Mn1 N1 2.052(4) . ?
Mn1 N3 2.072(4) . ?
Mn1 N2 2.079(4) . ?
N4 C23 1.358(6) . ?
N4 N1 1.372(5) . ?
N4 C3 1.453(6) . ?
N1 C4 1.347(6) . ?
N5 C7 1.366(6) . ?
N5 N2 1.381(5) . ?
N5 C3 1.436(6) . ?
N2 C9 1.349(6) . ?
N6 C12 1.365(6) . ?
N6 N3 1.369(5) . ?
N6 C3 1.445(6) . ?
N3 C14 1.343(6) . ?
O2 C2 1.180(6) . ?
O1 C1 1.166(6) . ?
C22 C23 1.498(7) . ?
C23 C24 1.368(8) . ?
C24 C4 1.400(7) . ?
C4 C5 1.486(7) . ?
C6 C7 1.493(7) . ?
C7 C8 1.366(7) . ?
C8 C9 1.404(7) . ?
C9 C10 1.474(7) . ?
C11 C12 1.498(7) . ?
C12 C13 1.368(7) . ?
C13 C14 1.398(7) . ?
C14 C15 1.497(7) . ?
N7 C16 1.351(6) . ?
N7 C20 1.360(6) . ?
C16 C17 1.384(7) . ?
C17 C18 1.363(7) . ?
C18 C19 1.384(8) . ?
C19 C20 1.378(7) . ?
P1 F1' 1.269(18) . ?
P1 F6' 1.44(2) . ?
P1 F4 1.460(6) . ?
P1 F3 1.564(5) . ?
P1 F2 1.580(15) . ?
P1 F5 1.595(6) . ?
P1 F1 1.620(7) . ?
P1 F6 1.701(6) . ?
P1 F4' 1.713(12) . ?
P1 F2' 1.884(16) . ?
C99 Cl1 1.739(8) . ?
C99 Cl2 1.766(7) . ?
C98 Cl4 1.716(7) . ?
C98 Cl3 1.766(8) . ?

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 Mn1 C1 86.3(2) . . ?
C2 Mn1 N7 94.2(2) . . ?
C1 Mn1 N7 93.0(2) . . ?
C2 Mn1 N1 94.1(2) . . ?
C1 Mn1 N1 94.3(2) . . ?
N7 Mn1 N1 169.31(17) . . ?
C2 Mn1 N3 93.1(2) . . ?
C1 Mn1 N3 179.3(2) . . ?
N7 Mn1 N3 87.48(16) . . ?
N1 Mn1 N3 85.31(16) . . ?
C2 Mn1 N2 177.9(2) . . ?
C1 Mn1 N2 94.8(2) . . ?
N7 Mn1 N2 87.53(16) . . ?
N1 Mn1 N2 84.07(16) . . ?
N3 Mn1 N2 85.70(16) . . ?
C23 N4 N1 112.7(4) . . ?
C23 N4 C3 128.4(4) . . ?
N1 N4 C3 118.6(4) . . ?
C4 N1 N4 104.6(4) . . ?
C4 N1 Mn1 136.7(4) . . ?
N4 N1 Mn1 118.7(3) . . ?
C7 N5 N2 111.6(4) . . ?
C7 N5 C3 129.8(4) . . ?
N2 N5 C3 118.4(4) . . ?
C9 N2 N5 105.0(4) . . ?
C9 N2 Mn1 136.5(3) . . ?
N5 N2 Mn1 118.2(3) . . ?
C12 N6 N3 111.8(4) . . ?
C12 N6 C3 129.6(4) . . ?
N3 N6 C3 118.5(4) . . ?
C14 N3 N6 105.2(4) . . ?
C14 N3 Mn1 136.3(3) . . ?
N6 N3 Mn1 118.5(3) . . ?
N4 C23 C24 105.2(5) . . ?
N4 C23 C22 123.2(5) . . ?
C24 C23 C22 131.6(5) . . ?
C23 C24 C4 107.8(5) . . ?
N1 C4 C24 109.7(5) . . ?
N1 C4 C5 122.3(5) . . ?
C24 C4 C5 127.9(5) . . ?
C8 C7 N5 106.0(5) . . ?
C8 C7 C6 131.2(5) . . ?
N5 C7 C6 122.8(5) . . ?
C7 C8 C9 107.6(5) . . ?
N2 C9 C8 109.8(4) . . ?
N2 C9 C10 122.5(5) . . ?
C8 C9 C10 127.7(5) . . ?
N6 C12 C13 105.8(4) . . ?
N6 C12 C11 123.4(5) . . ?
C13 C12 C11 130.8(5) . . ?
C12 C13 C14 107.3(5) . . ?
N3 C14 C13 110.0(5) . . ?
N3 C14 C15 122.9(5) . . ?
C13 C14 C15 127.1(5) . . ?
C16 N7 C20 115.8(4) . . ?
C16 N7 Mn1 121.2(3) . . ?
C20 N7 Mn1 123.1(3) . . ?
N7 C16 C17 123.2(5) . . ?
C18 C17 C16 119.8(5) . . ?
C17 C18 C19 118.5(5) . . ?
C20 C19 C18 118.9(5) . . ?
N7 C20 C19 123.7(5) . . ?
O1 C1 Mn1 175.1(5) . . ?
O2 C2 Mn1 176.9(5) . . ?
N5 C3 N6 111.5(4) . . ?
N5 C3 N4 110.2(4) . . ?
N6 C3 N4 109.9(4) . . ?
F1' P1 F6' 118.8(18) . . ?
F1' P1 F4 120.2(14) . . ?
F6' P1 F4 116.5(13) . . ?
F1' P1 F3 92.6(17) . . ?
F6' P1 F3 89.0(8) . . ?
F4 P1 F3 109.6(6) . . ?
F1' P1 F2 141.2(15) . . ?
F6' P1 F2 23.7(14) . . ?
F4 P1 F2 93.1(7) . . ?
F3 P1 F2 94.3(7) . . ?
F1' P1 F5 81.2(16) . . ?
F6' P1 F5 89.2(8) . . ?
F4 P1 F5 78.5(6) . . ?
F3 P1 F5 171.7(5) . . ?
F2 P1 F5 87.2(7) . . ?
F1' P1 F1 28.1(13) . . ?
F6' P1 F1 146.9(12) . . ?
F4 P1 F1 94.6(4) . . ?
F3 P1 F1 91.1(3) . . ?
F2 P1 F1 168.6(7) . . ?
F5 P1 F1 86.0(3) . . ?
F1' P1 F6 58.5(13) . . ?
F6' P1 F6 60.5(11) . . ?
F4 P1 F6 164.2(7) . . ?
F3 P1 F6 86.2(3) . . ?
F2 P1 F6 83.9(6) . . ?
F5 P1 F6 85.9(5) . . ?
F1 P1 F6 86.4(4) . . ?
F1' P1 F4' 84.5(13) . . ?
F6' P1 F4' 154.5(12) . . ?
F4 P1 F4' 49.6(5) . . ?
F3 P1 F4' 78.9(5) . . ?
F2 P1 F4' 134.3(9) . . ?
F5 P1 F4' 105.8(6) . . ?
F1 P1 F4' 56.7(7) . . ?
F6 P1 F4' 139.4(7) . . ?
F1' P1 F2' 152.3(16) . . ?
F6' P1 F2' 80.8(11) . . ?
F4 P1 F2' 56.2(6) . . ?
F3 P1 F2' 66.8(6) . . ?
F2 P1 F2' 62.3(8) . . ?
F5 P1 F2' 120.8(7) . . ?
F1 P1 F2' 129.2(7) . . ?
F6 P1 F2' 133.3(7) . . ?
F4' P1 F2' 73.9(9) . . ?
Cl1 C99 Cl2 112.5(4) . . ?
Cl4 C98 Cl3 112.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.083