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

#######################################################################
#
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#                                CCDC 
# 
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# 
#  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.
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#  fide research purposes only. It may contain copyright material
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data_cmpd16c

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H29 Mn N2 O3 P, P F6, C H2 Cl2'
_chemical_formula_sum            'C22 H31 Cl2 F6 Mn N2 O3 P2'
_chemical_formula_weight         673.27

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   14.2290(2)
_cell_length_b                   14.4430(3)
_cell_length_c                   16.8230(4)
_cell_angle_alpha                72.1450(10)
_cell_angle_beta                 73.3360(10)
_cell_angle_gamma                72.4180(10)
_cell_volume                     3064.40(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8990
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      27.55

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7476
_exptl_absorpt_correction_T_max  0.8930
_exptl_absorpt_process_details   Denzo/Scalepack

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(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  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21717
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.23
_diffrn_reflns_theta_max         27.55
_reflns_number_total             13925
_reflns_number_gt                8990
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXs-97
_computing_structure_refinement  SHELXL-97

_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.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0839P)²+4.1706P] where P=(Fo²+2Fc²)/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     SHELXL
_refine_ls_extinction_coef       0.0056(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13925
_refine_ls_number_parameters     761
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.1930
_refine_ls_wR_factor_gt          0.1680
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.003
_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
C1 C 0.3364(3) 0.9111(3) 0.1298(3) 0.0318(9) Uani 1 1 d . A 1
H1 H 0.3391 0.9810 0.0961 0.038 Uiso 1 1 calc R A 1
C2 C 0.2382(3) 0.8912(3) 0.1274(3) 0.0309(9) Uani 1 1 d . A 1
H2 H 0.2335 0.9089 0.0662 0.037 Uiso 1 1 calc R A 1
C3 C 0.1462(3) 0.9551(3) 0.1738(3) 0.0389(10) Uani 1 1 d . A 1
H3A H 0.0854 0.9334 0.1768 0.047 Uiso 1 1 calc R A 1
H3B H 0.1382 1.0257 0.1409 0.047 Uiso 1 1 calc R A 1
C4 C 0.1546(3) 0.9476(3) 0.2651(3) 0.0459(12) Uani 1 1 d . A 1
H4A H 0.0971 0.9960 0.2906 0.055 Uiso 1 1 calc R A 1
H4B H 0.1512 0.8796 0.3009 0.055 Uiso 1 1 calc R A 1
C5 C 0.2540(3) 0.9696(3) 0.2641(3) 0.0416(10) Uani 1 1 d . A 1
H5A H 0.2542 1.0400 0.2334 0.050 Uiso 1 1 calc R A 1
H5B H 0.2593 0.9606 0.3236 0.050 Uiso 1 1 calc R A 1
C6 C 0.3439(3) 0.9007(3) 0.2210(3) 0.0367(10) Uani 1 1 d . A 1
H6A H 0.3465 0.8306 0.2540 0.044 Uiso 1 1 calc R A 1
H6B H 0.4068 0.9175 0.2199 0.044 Uiso 1 1 calc R A 1
C7 C 0.3556(3) 0.5823(3) 0.1385(3) 0.0365(10) Uani 1 1 d . A 1
C8 C 0.5185(3) 0.6441(3) 0.0656(3) 0.0354(10) Uani 1 1 d . A 1
C9 C 0.4327(3) 0.6582(3) 0.2145(3) 0.0366(10) Uani 1 1 d . A 1
C10 C 0.2168(3) 0.7761(3) -0.0228(3) 0.0333(9) Uani 1 1 d . A 1
C11 C 0.1737(3) 0.8707(3) -0.0665(3) 0.0443(11) Uani 1 1 d . A 1
H11 H 0.2152 0.9154 -0.1005 0.053 Uiso 1 1 calc R A 1
C12 C 0.0699(4) 0.9006(4) -0.0608(4) 0.0558(14) Uani 1 1 d . A 1
H12 H 0.0409 0.9660 -0.0902 0.067 Uiso 1 1 calc R A 1
C13 C 0.0088(4) 0.8364(4) -0.0131(4) 0.0585(14) Uani 1 1 d . A 1
H13 H -0.0618 0.8567 -0.0103 0.070 Uiso 1 1 calc R A 1
C14 C 0.0512(3) 0.7427(4) 0.0305(3) 0.0538(13) Uani 1 1 d . A 1
H14 H 0.0093 0.6981 0.0638 0.065 Uiso 1 1 calc R A 1
C15 C 0.1538(3) 0.7123(3) 0.0266(3) 0.0404(10) Uani 1 1 d . A 1
H15 H 0.1817 0.6476 0.0579 0.048 Uiso 1 1 calc R A 1
C16 C 0.4094(3) 0.8260(3) -0.1100(3) 0.0363(10) Uani 1 1 d . A 1
H16A H 0.3895 0.8310 -0.1632 0.044 Uiso 1 1 calc R A 1
H16B H 0.3845 0.8926 -0.0969 0.044 Uiso 1 1 calc R A 1
C17 C 0.5227(3) 0.7961(4) -0.1235(3) 0.0404(10) Uani 1 1 d . A 1
H17 H 0.5560 0.7339 -0.1381 0.049 Uiso 1 1 calc R A 1
C18 C 0.5784(4) 0.8486(4) -0.1169(3) 0.0500(12) Uani 1 1 d . A 1
H18A H 0.5480 0.9112 -0.1024 0.060 Uiso 1 1 calc R A 1
H18B H 0.6497 0.8245 -0.1264 0.060 Uiso 1 1 calc R A 1
C19 C 0.3897(3) 0.6227(3) -0.0657(3) 0.0400(10) Uani 1 1 d . A 1
H19A H 0.4637 0.5970 -0.0722 0.048 Uiso 1 1 calc R A 1
H19B H 0.3574 0.5700 -0.0240 0.048 Uiso 1 1 calc R A 1
C20 C 0.3639(4) 0.6404(4) -0.1493(3) 0.0497(12) Uani 1 1 d . A 1
H20 H 0.2944 0.6559 -0.1503 0.060 Uiso 1 1 calc R A 1
C21 C 0.4290(5) 0.6363(5) -0.2214(4) 0.0705(17) Uani 1 1 d . A 1
H21A H 0.4992 0.6210 -0.2230 0.085 Uiso 1 1 calc R A 1
H21B H 0.4062 0.6486 -0.2723 0.085 Uiso 1 1 calc R A 1
C22 C 0.7642(3) 0.5943(3) 0.3602(3) 0.0354(10) Uani 1 1 d . B 1
H22 H 0.7263 0.5845 0.4211 0.042 Uiso 1 1 calc R B 1
C23 C 0.8763(3) 0.5652(3) 0.3593(3) 0.0407(11) Uani 1 1 d . B 1
H23 H 0.8922 0.4965 0.3971 0.049 Uiso 1 1 calc R B 1
C24 C 0.9416(3) 0.5633(4) 0.2708(3) 0.0496(12) Uani 1 1 d . B 1
H24A H 1.0137 0.5400 0.2741 0.059 Uiso 1 1 calc R B 1
H24B H 0.9311 0.6317 0.2331 0.059 Uiso 1 1 calc R B 1
C25 C 0.9139(4) 0.4931(4) 0.2340(4) 0.0628(15) Uani 1 1 d . B 1
H25A H 0.9557 0.4933 0.1757 0.075 Uiso 1 1 calc R B 1
H25B H 0.9292 0.4241 0.2698 0.075 Uiso 1 1 calc R B 1
C26 C 0.8028(4) 0.5240(4) 0.2301(3) 0.0541(13) Uani 1 1 d . B 1
H26A H 0.7888 0.5902 0.1896 0.065 Uiso 1 1 calc R B 1
H26B H 0.7870 0.4749 0.2088 0.065 Uiso 1 1 calc R B 1
C27 C 0.7356(3) 0.5297(3) 0.3179(3) 0.0443(11) Uani 1 1 d . B 1
H27A H 0.7407 0.4613 0.3552 0.053 Uiso 1 1 calc R B 1
H27B H 0.6646 0.5578 0.3121 0.053 Uiso 1 1 calc R B 1
C28 C 0.7351(4) 0.9051(4) 0.3177(3) 0.0454(11) Uani 1 1 d . B 1
C29 C 0.9014(4) 0.8058(4) 0.2572(3) 0.0471(12) Uani 1 1 d . B 1
C30 C 0.8783(4) 0.8423(4) 0.3968(3) 0.0517(13) Uani 1 1 d . B 1
C31 C 0.5813(3) 0.7328(3) 0.4943(3) 0.0340(9) Uani 1 1 d . B 1
C32 C 0.5619(3) 0.6419(3) 0.5474(3) 0.0386(10) Uani 1 1 d . B 1
H32 H 0.6035 0.6024 0.5867 0.046 Uiso 1 1 calc R B 1
C33 C 0.4813(4) 0.6094(4) 0.5424(3) 0.0492(12) Uani 1 1 d . B 1
H33 H 0.4679 0.5479 0.5789 0.059 Uiso 1 1 calc R B 1
C34 C 0.4211(4) 0.6654(5) 0.4854(4) 0.0577(14) Uani 1 1 d . B 1
H34 H 0.3673 0.6419 0.4815 0.069 Uiso 1 1 calc R B 1
C35 C 0.4391(4) 0.7565(4) 0.4335(3) 0.0540(13) Uani 1 1 d . B 1
H35 H 0.3961 0.7964 0.3953 0.065 Uiso 1 1 calc R B 1
C36 C 0.5189(3) 0.7894(4) 0.4369(3) 0.0430(11) Uani 1 1 d . B 1
H36 H 0.5317 0.8509 0.4000 0.052 Uiso 1 1 calc R B 1
C37 C 0.6366(4) 0.8986(3) 0.5137(3) 0.0427(11) Uani 1 1 d . B 1
H37A H 0.6916 0.9249 0.5170 0.051 Uiso 1 1 calc R B 1
H37B H 0.6065 0.9443 0.4653 0.051 Uiso 1 1 calc R B 1
C38 C 0.5578(4) 0.9007(4) 0.5942(3) 0.0454(11) Uani 1 1 d . B 1
H38 H 0.5006 0.8763 0.6002 0.055 Uiso 1 1 calc R B 1
C39 C 0.5618(5) 0.9338(4) 0.6570(4) 0.0612(14) Uani 1 1 d . B 1
H39A H 0.6179 0.9589 0.6532 0.073 Uiso 1 1 calc R B 1
H39B H 0.5086 0.9329 0.7064 0.073 Uiso 1 1 calc R B 1
C40 C 0.7346(3) 0.6965(4) 0.5884(3) 0.0438(11) Uani 1 1 d D B 1
H40A H 0.6795 0.7094 0.6380 0.053 Uiso 1 1 calc R B 1
H40B H 0.7468 0.6252 0.5885 0.053 Uiso 1 1 calc R B 1
C41 C 0.8291(10) 0.7133(12) 0.6001(15) 0.060(5) Uani 0.587(16) 1 d PD B 1
H41A H 0.8922 0.6879 0.5662 0.072 Uiso 0.587(16) 1 calc PR B 1
C42 C 0.8276(10) 0.7620(11) 0.6557(8) 0.091(5) Uani 0.587(16) 1 d PD B 1
H42A H 0.7653 0.7880 0.6903 0.109 Uiso 0.587(16) 1 calc PR B 1
H42B H 0.8889 0.7708 0.6611 0.109 Uiso 0.587(16) 1 calc PR B 1
C41A C 0.8102(13) 0.7426(14) 0.6003(18) 0.043(5) Uani 0.413(16) 1 d PD B 2
H41B H 0.7953 0.8115 0.5997 0.051 Uiso 0.413(16) 1 calc PR B 2
C42A C 0.8978(13) 0.6818(13) 0.6114(11) 0.083(6) Uani 0.413(16) 1 d PD B 2
H42C H 0.9103 0.6133 0.6116 0.099 Uiso 0.413(16) 1 calc PR B 2
H42D H 0.9485 0.7065 0.6193 0.099 Uiso 0.413(16) 1 calc PR B 2
F1 F 0.2503(3) 0.5602(3) 0.3288(2) 0.0837(11) Uani 1 1 d . C 1
F2 F 0.1071(3) 0.6797(3) 0.3284(3) 0.1054(17) Uani 1 1 d . C 1
F3 F 0.1110(2) 0.5350(2) 0.4314(2) 0.0621(9) Uani 1 1 d . C 1
F4 F 0.0993(3) 0.6764(3) 0.4627(3) 0.1041(15) Uani 1 1 d . C 1
F5 F 0.2437(2) 0.5576(2) 0.4630(2) 0.0703(10) Uani 1 1 d . C 1
F6 F 0.23924(19) 0.7034(2) 0.36094(18) 0.0516(7) Uani 1 1 d . C 1
F7 F 0.6392(2) 0.7713(2) 0.1055(3) 0.0881(13) Uani 1 1 d . D 1
F8 F 0.59495(18) 0.94001(19) 0.06104(18) 0.0476(7) Uani 1 1 d . D 1
F9 F 0.7442(3) 0.8502(3) -0.0035(2) 0.0713(9) Uani 1 1 d . D 1
F10 F 0.7440(2) 0.9459(2) 0.0766(3) 0.0755(11) Uani 1 1 d . D 1
F11 F 0.78683(18) 0.7779(2) 0.12376(17) 0.0463(7) Uani 1 1 d . D 1
F12 F 0.6395(2) 0.8665(3) 0.1869(2) 0.0859(12) Uani 1 1 d . D 1
Mn1 Mn 0.39112(4) 0.69931(4) 0.11251(4) 0.02935(18) Uani 1 1 d . A 1
Mn2 Mn 0.81040(5) 0.78344(5) 0.35828(4) 0.03732(19) Uani 1 1 d . B 1
N1 N 0.4205(2) 0.8406(2) 0.0876(2) 0.0317(8) Uani 1 1 d . A 1
H1A H 0.4779 0.8331 0.1061 0.038 Uiso 1 1 calc R A 1
H1B H 0.4327 0.8674 0.0295 0.038 Uiso 1 1 calc R A 1
N2 N 0.2472(2) 0.7807(2) 0.1609(2) 0.0294(7) Uani 1 1 d . A 1
H2A H 0.1991 0.7630 0.1456 0.035 Uiso 1 1 calc R A 1
H2B H 0.2354 0.7649 0.2196 0.035 Uiso 1 1 calc R A 1
N3 N 0.7394(3) 0.7036(3) 0.3180(2) 0.0354(8) Uani 1 1 d . B 1
H3C H 0.6707 0.7284 0.3308 0.042 Uiso 1 1 calc R B 1
H3D H 0.7598 0.7123 0.2596 0.042 Uiso 1 1 calc R B 1
N4 N 0.8948(3) 0.6364(3) 0.3980(2) 0.0414(9) Uani 1 1 d . B 1
H4C H 0.9624 0.6359 0.3825 0.050 Uiso 1 1 calc R B 1
H4D H 0.8779 0.6157 0.4566 0.050 Uiso 1 1 calc R B 1
O1 O 0.3368(3) 0.5056(2) 0.1552(2) 0.0529(9) Uani 1 1 d . A 1
O2 O 0.6003(2) 0.6066(2) 0.0385(2) 0.0488(8) Uani 1 1 d . A 1
O3 O 0.4662(2) 0.6227(3) 0.2737(2) 0.0502(8) Uani 1 1 d . A 1
O4 O 0.6931(3) 0.9847(3) 0.2896(2) 0.0613(10) Uani 1 1 d . B 1
O5 O 0.9578(3) 0.8308(3) 0.1954(2) 0.0630(10) Uani 1 1 d . B 1
O6 O 0.9215(3) 0.8838(3) 0.4164(3) 0.0708(11) Uani 1 1 d . B 1
P1 P 0.35084(7) 0.73441(8) -0.02163(7) 0.0296(2) Uani 1 1 d . A 1
P2 P 0.69188(8) 0.77425(8) 0.49002(7) 0.0350(3) Uani 1 1 d . B 1
P3 P 0.17545(8) 0.61927(9) 0.39649(8) 0.0410(3) Uani 1 1 d . C 1
P4 P 0.69100(8) 0.85893(8) 0.09233(7) 0.0325(3) Uani 1 1 d . D 1
Cl1 Cl 0.1337(2) 0.5010(3) 0.9976(3) 0.0828(11) Uani 0.667(7) 1 d PDU E 1
Cl2 Cl 0.1744(4) 0.3519(5) 1.1381(3) 0.172(3) Uani 0.667(7) 1 d PDU E 1
C43 C 0.1548(8) 0.3693(3) 1.0346(4) 0.079(3) Uani 0.667(7) 1 d PDU E 1
H43A H 0.2150 0.3350 0.9984 0.095 Uiso 0.667(7) 1 calc PR E 1
H43B H 0.0955 0.3455 1.0372 0.095 Uiso 0.667(7) 1 calc PR E 1
Cl1A Cl 0.1167(11) 0.4647(8) 1.0047(7) 0.159(5) Uani 0.333(7) 1 d PDU E 2
Cl2A Cl 0.1148(6) 0.2939(6) 1.1293(4) 0.116(3) Uani 0.333(7) 1 d PDU E 2
C43A C 0.1982(9) 0.3477(13) 1.0386(14) 0.114(6) Uani 0.333(7) 1 d PDU E 2
H43C H 0.2571 0.3553 1.0541 0.136 Uiso 0.333(7) 1 calc PR E 2
H43D H 0.2218 0.3084 0.9947 0.136 Uiso 0.333(7) 1 calc PR E 2
Cl3 Cl 0.7327(6) 0.1600(7) 0.3755(6) 0.183(4) Uani 0.463(7) 1 d PDU F 1
Cl4 Cl 0.8997(8) 0.2315(7) 0.2295(7) 0.214(4) Uani 0.463(7) 1 d PDU F 1
C44 C 0.8308(10) 0.1389(10) 0.2858(8) 0.102(5) Uani 0.463(7) 1 d PDU F 1
H44A H 0.8797 0.0761 0.3053 0.122 Uiso 0.463(7) 1 calc PR F 1
H44B H 0.8011 0.1268 0.2445 0.122 Uiso 0.463(7) 1 calc PR F 1
Cl3A Cl 0.8617(15) 0.0950(14) 0.4886(10) 0.430(10) Uani 0.537(7) 1 d PDU F 2
Cl4A Cl 0.8992(12) 0.1915(11) 0.3215(10) 0.351(7) Uani 0.537(7) 1 d PDU F 2
C44A C 0.7966(10) 0.161(3) 0.4051(14) 0.245(10) Uani 0.537(7) 1 d PDU F 2
H44C H 0.7460 0.2214 0.4184 0.294 Uiso 0.537(7) 1 calc PR F 2
H44D H 0.7634 0.1180 0.3918 0.294 Uiso 0.537(7) 1 calc PR F 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.481(5) . ?
C1 C2 1.524(5) . ?
C1 C6 1.527(6) . ?
C2 N2 1.500(5) . ?
C2 C3 1.516(6) . ?
C3 C4 1.542(7) . ?
C4 C5 1.535(6) . ?
C5 C6 1.515(6) . ?
C7 O1 1.149(5) . ?
C7 Mn1 1.800(4) . ?
C8 O2 1.150(5) . ?
C8 Mn1 1.799(4) . ?
C9 O3 1.139(5) . ?
C9 Mn1 1.841(5) . ?
C10 C11 1.385(6) . ?
C10 C15 1.395(6) . ?
C10 P1 1.823(4) . ?
C11 C12 1.391(6) . ?
C12 C13 1.374(7) . ?
C13 C14 1.373(7) . ?
C14 C15 1.380(6) . ?
C16 C17 1.505(6) . ?
C16 P1 1.845(4) . ?
C17 C18 1.298(6) . ?
C19 C20 1.481(7) . ?
C19 P1 1.849(4) . ?
C20 C21 1.304(8) . ?
C22 N3 1.497(5) . ?
C22 C23 1.519(6) . ?
C22 C27 1.531(6) . ?
C23 N4 1.490(6) . ?
C23 C24 1.515(7) . ?
C24 C25 1.528(8) . ?
C25 C26 1.523(8) . ?
C26 C27 1.522(7) . ?
C28 O4 1.148(6) . ?
C28 Mn2 1.802(5) . ?
C29 O5 1.148(5) . ?
C29 Mn2 1.824(5) . ?
C30 O6 1.144(6) . ?
C30 Mn2 1.808(6) . ?
C31 C32 1.399(6) . ?
C31 C36 1.399(6) . ?
C31 P2 1.821(4) . ?
C32 C33 1.397(6) . ?
C33 C34 1.373(8) . ?
C34 C35 1.390(8) . ?
C35 C36 1.378(6) . ?
C37 C38 1.491(7) . ?
C37 P2 1.846(5) . ?
C38 C39 1.308(7) . ?
C40 C41 1.512(9) . ?
C40 P2 1.842(4) . ?
C41 C42 1.324(10) . ?
C41A C42A 1.316(10) . ?
F1 P3 1.584(4) . ?
F2 P3 1.591(3) . ?
F3 P3 1.610(3) . ?
F4 P3 1.558(4) . ?
F5 P3 1.574(3) . ?
F6 P3 1.603(3) . ?
F7 P4 1.579(3) . ?
F8 P4 1.607(3) . ?
F9 P4 1.598(3) . ?
F10 P4 1.572(3) . ?
F11 P4 1.606(3) . ?
F12 P4 1.571(3) . ?
Mn1 N1 2.099(3) . ?
Mn1 N2 2.101(3) . ?
Mn1 P1 2.3543(13) . ?
Mn2 N3 2.094(4) . ?
Mn2 N4 2.109(4) . ?
Mn2 P2 2.3632(13) . ?
Cl1 C43 1.7697(11) . ?
Cl2 C43 1.7703(11) . ?
Cl1A C43A 1.7698(11) . ?
Cl2A C43A 1.7699(11) . ?
Cl3 C44 1.7701(11) . ?
Cl4 C44 1.7695(11) . ?
Cl3A C44A 1.7698(11) . ?
Cl4A C44A 1.7701(11) . ?

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
N1 C1 C2 107.5(3) . . ?
N1 C1 C6 111.7(3) . . ?
C2 C1 C6 111.8(3) . . ?
N2 C2 C3 114.4(3) . . ?
N2 C2 C1 106.9(3) . . ?
C3 C2 C1 112.4(3) . . ?
C2 C3 C4 112.1(3) . . ?
C5 C4 C3 111.0(4) . . ?
C6 C5 C4 111.1(4) . . ?
C5 C6 C1 110.5(4) . . ?
O1 C7 Mn1 177.3(4) . . ?
O2 C8 Mn1 177.4(4) . . ?
O3 C9 Mn1 171.4(4) . . ?
C11 C10 C15 118.4(4) . . ?
C11 C10 P1 122.9(3) . . ?
C15 C10 P1 118.6(3) . . ?
C10 C11 C12 120.3(4) . . ?
C13 C12 C11 120.7(5) . . ?
C14 C13 C12 119.2(4) . . ?
C13 C14 C15 120.8(4) . . ?
C14 C15 C10 120.5(4) . . ?
C17 C16 P1 111.3(3) . . ?
C18 C17 C16 125.1(5) . . ?
C20 C19 P1 114.6(3) . . ?
C21 C20 C19 125.2(5) . . ?
N3 C22 C23 106.6(3) . . ?
N3 C22 C27 113.2(4) . . ?
C23 C22 C27 112.0(4) . . ?
N4 C23 C24 112.9(4) . . ?
N4 C23 C22 106.6(4) . . ?
C24 C23 C22 112.8(4) . . ?
C23 C24 C25 109.5(4) . . ?
C26 C25 C24 111.9(4) . . ?
C27 C26 C25 111.0(4) . . ?
C26 C27 C22 112.7(4) . . ?
O4 C28 Mn2 175.4(4) . . ?
O5 C29 Mn2 171.7(5) . . ?
O6 C30 Mn2 175.8(5) . . ?
C32 C31 C36 118.9(4) . . ?
C32 C31 P2 122.1(3) . . ?
C36 C31 P2 118.7(3) . . ?
C33 C32 C31 119.8(4) . . ?
C34 C33 C32 120.7(5) . . ?
C33 C34 C35 119.7(4) . . ?
C36 C35 C34 120.4(5) . . ?
C35 C36 C31 120.5(4) . . ?
C38 C37 P2 115.3(3) . . ?
C39 C38 C37 124.7(5) . . ?
C41 C40 P2 115.2(9) . . ?
C42 C41 C40 122.8(13) . . ?
C8 Mn1 C7 91.31(19) . . ?
C8 Mn1 C9 86.44(19) . . ?
C7 Mn1 C9 88.29(19) . . ?
C8 Mn1 N1 93.41(16) . . ?
C7 Mn1 N1 175.27(16) . . ?
C9 Mn1 N1 91.61(17) . . ?
C8 Mn1 N2 172.98(16) . . ?
C7 Mn1 N2 95.60(16) . . ?
C9 Mn1 N2 94.98(16) . . ?
N1 Mn1 N2 79.70(12) . . ?
C8 Mn1 P1 88.10(14) . . ?
C7 Mn1 P1 87.90(14) . . ?
C9 Mn1 P1 173.27(14) . . ?
N1 Mn1 P1 92.65(10) . . ?
N2 Mn1 P1 90.92(10) . . ?
C28 Mn2 C30 89.3(2) . . ?
C28 Mn2 C29 86.4(2) . . ?
C30 Mn2 C29 85.8(2) . . ?
C28 Mn2 N3 95.54(18) . . ?
C30 Mn2 N3 175.15(19) . . ?
C29 Mn2 N3 94.53(19) . . ?
C28 Mn2 N4 174.9(2) . . ?
C30 Mn2 N4 95.47(19) . . ?
C29 Mn2 N4 92.15(19) . . ?
N3 Mn2 N4 79.68(14) . . ?
C28 Mn2 P2 88.91(15) . . ?
C30 Mn2 P2 89.01(16) . . ?
C29 Mn2 P2 173.02(16) . . ?
N3 Mn2 P2 91.03(10) . . ?
N4 Mn2 P2 93.00(11) . . ?
C1 N1 Mn1 113.0(2) . . ?
C2 N2 Mn1 111.3(2) . . ?
C22 N3 Mn2 111.4(3) . . ?
C23 N4 Mn2 111.8(3) . . ?
C10 P1 C16 104.62(19) . . ?
C10 P1 C19 102.1(2) . . ?
C16 P1 C19 102.4(2) . . ?
C10 P1 Mn1 115.76(14) . . ?
C16 P1 Mn1 117.48(15) . . ?
C19 P1 Mn1 112.53(15) . . ?
C31 P2 C40 103.84(19) . . ?
C31 P2 C37 102.8(2) . . ?
C40 P2 C37 103.1(2) . . ?
C31 P2 Mn2 114.97(14) . . ?
C40 P2 Mn2 118.76(16) . . ?
C37 P2 Mn2 111.51(15) . . ?
F4 P3 F5 91.5(2) . . ?
F4 P3 F1 178.3(2) . . ?
F5 P3 F1 89.4(2) . . ?
F4 P3 F2 89.5(3) . . ?
F5 P3 F2 178.8(3) . . ?
F1 P3 F2 89.6(3) . . ?
F4 P3 F6 91.81(19) . . ?
F5 P3 F6 91.18(15) . . ?
F1 P3 F6 89.54(17) . . ?
F2 P3 F6 89.39(16) . . ?
F4 P3 F3 88.35(19) . . ?
F5 P3 F3 89.28(16) . . ?
F1 P3 F3 90.29(18) . . ?
F2 P3 F3 90.15(16) . . ?
F6 P3 F3 179.51(18) . . ?
F12 P4 F10 92.0(2) . . ?
F12 P4 F7 89.6(2) . . ?
F10 P4 F7 178.4(2) . . ?
F12 P4 F9 179.4(2) . . ?
F10 P4 F9 88.2(2) . . ?
F7 P4 F9 90.3(2) . . ?
F12 P4 F11 90.56(16) . . ?
F10 P4 F11 90.47(16) . . ?
F7 P4 F11 89.51(15) . . ?
F9 P4 F11 88.88(16) . . ?
F12 P4 F8 89.33(16) . . ?
F10 P4 F8 89.55(16) . . ?
F7 P4 F8 90.47(15) . . ?
F9 P4 F8 91.22(16) . . ?
F11 P4 F8 179.9(2) . . ?
Cl1 C43 Cl2 101.1(2) . . ?
Cl1A C43A Cl2A 99.7(3) . . ?
Cl4 C44 Cl3 119.2(8) . . ?
Cl3A C44A Cl4A 99.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.090
_database_code_depnum_ccdc_archive 'CCDC 1015695'
#######################################################################
#
#                 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_shelx_cmpd7

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H34 F I Mn O4 P3'
_chemical_formula_weight         776.34

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'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

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

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

_cell_length_a                   35.176(5)
_cell_length_b                   10.9232(15)
_cell_length_c                   20.217(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.514(9)
_cell_angle_gamma                90
_cell_volume                     7122.9(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2895
_cell_measurement_theta_min      1.09
_cell_measurement_theta_max      21.029

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_F_000             3120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.410
_shelx_estimated_absorpt_T_min   0.602
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_process_details   Sadabs/Denzo


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9674
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_av_R_equivalents  0.0992
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.098
_diffrn_reflns_theta_max         21.029
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measured_fraction_theta_full 0.579
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_Laue_measured_fraction_full 0.579
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.579
_reflns_number_total             3944
_reflns_number_gt                2895
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'COLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0903P)²+213.1648P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3944
_refine_ls_number_parameters     540
_refine_ls_number_restraints     567
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0821
_refine_ls_wR_factor_ref         0.2248
_refine_ls_wR_factor_gt          0.1991
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4162(4) -0.1314(14) 0.3264(7) 0.044(4) Uani 1 1 d . . . . .
C2 C 0.4090(4) -0.1960(14) 0.3800(8) 0.046(4) Uani 1 1 d . . . . .
C3 C 0.4354(5) -0.2920(16) 0.4152(8) 0.059(5) Uani 1 1 d . . . . .
H3 H 0.4309 -0.3357 0.4521 0.071 Uiso 1 1 calc R U . . .
C4 C 0.4679(5) -0.3244(17) 0.3973(9) 0.063(5) Uani 1 1 d . . . . .
H4 H 0.4853 -0.3914 0.4205 0.075 Uiso 1 1 calc R U . . .
C5 C 0.4750(5) -0.2570(19) 0.3441(9) 0.067(5) Uani 1 1 d . . . . .
H5 H 0.4982 -0.2765 0.3331 0.080 Uiso 1 1 calc R U . . .
C6 C 0.4495(5) -0.1650(15) 0.3085(8) 0.055(4) Uani 1 1 d . . . . .
H6 H 0.4540 -0.1227 0.2712 0.066 Uiso 1 1 calc R U . . .
C7 C 0.4051(8) -0.057(2) 0.4856(7) 0.045(4) Uani 0.5 1 d D U P . .
H7 H 0.4317 -0.0425 0.4800 0.054 Uiso 0.5 1 calc R U P . .
C8 C 0.4141(9) -0.1305(17) 0.5552(11) 0.046(4) Uani 0.5 1 d D U P . .
H8A H 0.4251 -0.2124 0.5513 0.056 Uiso 0.5 1 calc R U P . .
H8B H 0.3883 -0.1414 0.5632 0.056 Uiso 0.5 1 calc R U P . .
C9 C 0.4464(7) -0.059(2) 0.6187(8) 0.046(4) Uani 0.5 1 d D U P . .
H9A H 0.4540 -0.1065 0.6639 0.055 Uiso 0.5 1 calc R U P . .
H9B H 0.4717 -0.0453 0.6097 0.055 Uiso 0.5 1 calc R U P . .
C10 C 0.4271(8) 0.064(2) 0.6254(7) 0.047(4) Uani 0.5 1 d D U P . .
H10A H 0.4011 0.0504 0.6324 0.056 Uiso 0.5 1 calc R U P . .
H10B H 0.4465 0.1101 0.6676 0.056 Uiso 0.5 1 calc R U P . .
C11 C 0.4180(9) 0.1383(17) 0.5560(11) 0.047(4) Uani 0.5 1 d D U P . .
H11A H 0.4066 0.2197 0.5600 0.056 Uiso 0.5 1 calc R U P . .
H11B H 0.4438 0.1507 0.5485 0.056 Uiso 0.5 1 calc R U P . .
C12 C 0.3863(7) 0.067(2) 0.4920(8) 0.045(4) Uani 0.5 1 d D U P . .
H12 H 0.3616 0.0511 0.5032 0.054 Uiso 0.5 1 calc R U P . .
C13 C 0.3438(5) -0.2735(15) 0.4212(9) 0.057(4) Uani 1 1 d . U . . .
H13A H 0.3308 -0.3212 0.3768 0.085 Uiso 1 1 calc R U . . .
H13B H 0.3226 -0.2484 0.4386 0.085 Uiso 1 1 calc R U . . .
H13C H 0.3647 -0.3237 0.4581 0.085 Uiso 1 1 calc R U . . .
C14 C 0.3726(7) 0.0000 0.1911(9) 0.053(6) Uani 1 2 d DS TU P . .
C15 C 0.3674(6) -0.1114(12) 0.1551(8) 0.082(6) Uani 1 1 d D U . . .
H15 H 0.3708 -0.1862 0.1808 0.098 Uiso 0.5 1 calc R U P . .
C16 C 0.3569(7) -0.1118(12) 0.0805(8) 0.120(8) Uani 1 1 d D U . . .
H16 H 0.3527 -0.1865 0.0545 0.144 Uiso 1 1 calc R U . . .
C17 C 0.3529(10) 0.0000 0.0459(11) 0.118(12) Uani 1 2 d DS TU P . .
H17 H 0.3470 0.0000 -0.0042 0.141 Uiso 1 2 calc R U P . .
C18 C 0.2923(8) 0.0000 0.3600(14) 0.070(7) Uani 1 2 d S TU P . .
C19 C 0.3049(4) -0.1238(15) 0.2590(7) 0.043(4) Uani 1 1 d . U . . .
C20 C 0.4089(4) 0.6971(15) 0.8794(7) 0.047(4) Uani 1 1 d . U . . .
C21 C 0.3923(4) 0.6319(13) 0.9211(7) 0.039(4) Uani 1 1 d . U . . .
C22 C 0.4023(4) 0.6630(15) 0.9934(8) 0.051(4) Uani 1 1 d . U . . .
H22 H 0.3917 0.6176 1.0223 0.061 Uiso 1 1 calc R U . . .
C23 C 0.4288(5) 0.7651(15) 1.0217(9) 0.055(4) Uani 1 1 d . U . . .
H23 H 0.4354 0.7908 1.0699 0.066 Uiso 1 1 calc R U . . .
C24 C 0.4447(5) 0.8251(17) 0.9812(9) 0.065(5) Uani 1 1 d . U . . .
H24 H 0.4636 0.8899 1.0024 0.078 Uiso 1 1 calc R U . . .
C25 C 0.4346(5) 0.7970(16) 0.9102(8) 0.057(4) Uani 1 1 d . U . . .
H25 H 0.4451 0.8452 0.8822 0.069 Uiso 1 1 calc R U . . .
C26 C 0.4482(5) 0.558(2) 0.8184(16) 0.042(5) Uani 0.5 1 d D U P . .
H26 H 0.4581 0.5411 0.8712 0.050 Uiso 0.5 1 calc R U P . .
C27 C 0.4826(7) 0.6303(19) 0.8063(18) 0.043(5) Uani 0.5 1 d D U P . .
H27A H 0.4869 0.7105 0.8310 0.051 Uiso 0.5 1 calc R U P . .
H27B H 0.4747 0.6447 0.7541 0.051 Uiso 0.5 1 calc R U P . .
C28 C 0.5228(4) 0.554(2) 0.8374(14) 0.042(5) Uani 0.5 1 d D U P . .
H28A H 0.5460 0.5993 0.8326 0.051 Uiso 0.5 1 calc R U P . .
H28B H 0.5303 0.5369 0.8892 0.051 Uiso 0.5 1 calc R U P . .
C29 C 0.5153(6) 0.433(2) 0.7951(15) 0.044(5) Uani 0.5 1 d D U P . .
H29A H 0.5066 0.4500 0.7430 0.053 Uiso 0.5 1 calc R U P . .
H29B H 0.5413 0.3844 0.8117 0.053 Uiso 0.5 1 calc R U P . .
C30 C 0.4813(6) 0.3605(16) 0.8076(18) 0.044(5) Uani 0.5 1 d D U P . .
H30A H 0.4770 0.2808 0.7823 0.053 Uiso 0.5 1 calc R U P . .
H30B H 0.4899 0.3446 0.8597 0.053 Uiso 0.5 1 calc R U P . .
C31 C 0.4409(5) 0.435(2) 0.7788(14) 0.042(5) Uani 0.5 1 d D U P . .
H31 H 0.4332 0.4507 0.7263 0.050 Uiso 0.5 1 calc R U P . .
C32 C 0.3931(6) 0.7704(16) 0.7339(9) 0.071(5) Uani 1 1 d . U . . .
H32A H 0.3658 0.8086 0.7210 0.106 Uiso 1 1 calc R U . . .
H32B H 0.3964 0.7453 0.6899 0.106 Uiso 1 1 calc R U . . .
H32C H 0.4148 0.8292 0.7606 0.106 Uiso 1 1 calc R U . . .
C33 C 0.3174(6) 0.5000 0.9088(12) 0.056(6) Uani 1 2 d DS TU P . .
C34 C 0.2999(4) 0.6110(11) 0.9153(9) 0.064(5) Uani 1 1 d D U . . .
H34 H 0.3106 0.6856 0.9056 0.077 Uiso 0.5 1 calc R U P . .
C35 C 0.2665(5) 0.6119(12) 0.9364(11) 0.107(7) Uani 1 1 d D U . . .
H35 H 0.2559 0.6866 0.9463 0.128 Uiso 1 1 calc R U . . .
C36 C 0.2493(7) 0.5000 0.9424(15) 0.091(9) Uani 1 2 d DS TU P . .
H36 H 0.2247 0.5000 0.9510 0.110 Uiso 1 2 calc R U P . .
C37 C 0.3360(8) 0.5000 0.6648(15) 0.069(7) Uani 1 2 d S TU P . .
C38 C 0.3071(4) 0.3769(14) 0.7419(7) 0.039(4) Uani 1 1 d . U . . .
O1 O 0.2695(5) 0.0000 0.3883(9) 0.073(5) Uani 1 2 d S TU P . .
O2 O 0.2905(3) -0.2072(11) 0.2208(6) 0.067(3) Uani 1 1 d . U . . .
O3 O 0.3280(6) 0.5000 0.6046(10) 0.093(6) Uani 1 2 d S TU P . .
O4 O 0.2843(3) 0.2968(11) 0.7335(6) 0.065(3) Uani 1 1 d . U . . .
F1 F 0.3641(7) -0.2183(16) 0.1850(12) 0.106(7) Uani 0.5 1 d D U P . .
F2 F 0.3110(6) 0.7211(14) 0.9005(11) 0.088(6) Uani 0.5 1 d D U P . .
P1 P 0.38347(16) 0.0000 0.2874(3) 0.0417(15) Uani 1 2 d S T P . .
P2 P 0.36813(12) -0.1392(4) 0.4033(2) 0.0444(11) Uani 1 1 d . . . . .
P3 P 0.39706(12) 0.6386(4) 0.7892(2) 0.0455(11) Uani 1 1 d . . . . .
P4 P 0.35975(16) 0.5000 0.8780(3) 0.0398(14) Uani 1 2 d S T P . .
Mn1 Mn 0.32949(9) 0.0000 0.32049(16) 0.0422(9) Uani 1 2 d S T P . .
Mn2 Mn 0.34441(9) 0.5000 0.75899(15) 0.0409(9) Uani 1 2 d S T P . .
I1 I 0.50392(4) 0.0000 0.82999(7) 0.0452(5) Uani 1 2 d S T P . .
I2 I 0.42646(4) 0.5000 0.57634(7) 0.0491(5) Uani 1 2 d S T P . .
C39 C 0.3125(10) 0.5000 0.1403(18) 0.17(2) Uani 1 2 d S T P . .
H39A H 0.2990 0.5000 0.0875 0.256 Uiso 1 2 calc R U P . .
H39B H 0.3042 0.5733 0.1592 0.256 Uiso 0.5 1 calc R U P . .
H39C H 0.3042 0.4267 0.1592 0.256 Uiso 0.5 1 calc R U P . .
C40 C 0.3590(8) 0.5000 0.1634(15) 0.065(7) Uani 1 2 d S T P . .
C41 C 0.3837(9) 0.5000 0.2393(15) 0.102(10) Uani 1 2 d S T P . .
H41A H 0.4131 0.5000 0.2477 0.153 Uiso 1 2 calc R U P . .
H41B H 0.3775 0.4267 0.2612 0.153 Uiso 0.5 1 calc R U P . .
H41C H 0.3775 0.5733 0.2612 0.153 Uiso 0.5 1 calc R U P . .
O5 O 0.3725(7) 0.5000 0.1189(12) 0.148(12) Uani 1 2 d S T P . .
C42 C 0.3428(18) 0.0000 0.853(4) 0.056(11) Uani 0.25 2 d DS TU P A 1
H42A H 0.3699 0.0000 0.8502 0.084 Uiso 0.25 2 calc R U P A 1
H42B H 0.3402 -0.0733 0.8790 0.084 Uiso 0.125 1 calc R U P A 1
H42C H 0.3402 0.0733 0.8790 0.084 Uiso 0.125 1 calc R U P A 1
C43 C 0.3085(17) 0.0000 0.777(3) 0.054(9) Uani 0.25 2 d DS TU P A 1
C44 C 0.2646(15) 0.0000 0.775(4) 0.038(11) Uani 0.25 2 d DS TU P A 1
H44A H 0.2443 0.0000 0.7250 0.057 Uiso 0.25 2 calc R U P A 1
H44B H 0.2606 0.0733 0.7998 0.057 Uiso 0.125 1 calc R U P A 1
H44C H 0.2606 -0.0733 0.7998 0.057 Uiso 0.125 1 calc R U P A 1
O6 O 0.3138(18) 0.0000 0.721(3) 0.057(10) Uani 0.25 2 d DS TU P A 1
C42A C 0.2911(16) 0.1142(5) 0.867(3) 0.070(13) Uani 0.25 1 d D U P B 2
H42D H 0.2942 0.1773 0.8352 0.105 Uiso 0.25 1 calc R U P B 2
H42E H 0.3069 0.1379 0.9175 0.105 Uiso 0.25 1 calc R U P B 2
H42F H 0.2618 0.1053 0.8583 0.105 Uiso 0.25 1 calc R U P B 2
C43A C 0.3066(14) 0.0000 0.853(2) 0.057(9) Uani 0.25 2 d DS TU P B 2
O6A O 0.3350(16) 0.0000 0.832(3) 0.057(10) Uani 0.25 2 d DS TU P B 2
C45 C 0.2764(18) 0.1168(10) 0.550(3) 0.067(10) Uani 0.25 1 d D U P C 1
H45A H 0.2989 0.1771 0.5649 0.101 Uiso 0.25 1 calc R U P C 1
H45B H 0.2539 0.1463 0.5627 0.101 Uiso 0.25 1 calc R U P C 1
H45C H 0.2658 0.1051 0.4975 0.101 Uiso 0.25 1 calc R U P C 1
C46 C 0.2920(15) 0.0000 0.586(3) 0.069(9) Uani 0.25 2 d DS TU P C 1
O7 O 0.3186(18) 0.0000 0.648(3) 0.072(9) Uani 0.25 2 d DS TU P C 1
C45A C 0.2607(17) 0.1164(10) 0.565(4) 0.066(11) Uani 0.25 1 d D U P D 2
H45D H 0.2800 0.1855 0.5783 0.100 Uiso 0.25 1 calc R U P D 2
H45E H 0.2475 0.1108 0.5998 0.100 Uiso 0.25 1 calc R U P D 2
H45F H 0.2394 0.1289 0.5167 0.100 Uiso 0.25 1 calc R U P D 2
C46A C 0.284(2) 0.0000 0.567(5) 0.069(9) Uani 0.25 2 d DS TU P D 2
O7A O 0.3178(16) 0.0000 0.563(4) 0.077(10) Uani 0.25 2 d DS TU P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.40(2) . ?
C1 C6 1.40(2) . ?
C1 P1 1.812(15) . ?
C2 C3 1.39(2) . ?
C2 P2 1.794(15) . ?
C3 C4 1.38(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.40(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.35(2) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.538(10) . ?
C7 C8 1.540(10) . ?
C7 P2 1.881(17) . ?
C7 H7 1.0000 . ?
C8 C9 1.542(10) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.540(10) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.538(10) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.537(10) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 P2 1.823(17) 6 ?
C12 H12 1.0000 . ?
C13 P2 1.806(15) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.391(9) 6 ?
C14 C15 1.391(9) . ?
C14 P1 1.829(17) . ?
C15 C16 1.403(9) . ?
C15 H15 0.9500 . ?
C16 C17 1.387(10) . ?
C16 H16 0.9500 . ?
C17 C16 1.387(10) 6 ?
C17 H17 0.9500 . ?
C18 O1 1.16(3) . ?
C18 Mn1 1.79(3) . ?
C19 O2 1.172(17) . ?
C19 Mn1 1.806(16) . ?
C20 C25 1.40(2) . ?
C20 C21 1.396(19) . ?
C20 P3 1.816(15) . ?
C21 C22 1.403(19) . ?
C21 P4 1.830(14) . ?
C22 C23 1.42(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.33(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.37(2) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C31 1.539(10) . ?
C26 C27 1.542(10) . ?
C26 P3 1.874(16) . ?
C26 H26 1.0000 . ?
C27 C28 1.544(10) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.537(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.536(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.534(10) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 P3 1.823(19) 6_565 ?
C31 H31 1.0000 . ?
C32 P3 1.794(17) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.388(9) . ?
C33 C34 1.388(9) 6_565 ?
C33 P4 1.830(17) . ?
C34 C35 1.402(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(10) . ?
C35 H35 0.9500 . ?
C36 C35 1.390(10) 6_565 ?
C36 H36 0.9500 . ?
C37 O3 1.13(3) . ?
C37 Mn2 1.81(3) . ?
C38 O4 1.155(16) . ?
C38 Mn2 1.812(16) . ?
P1 C1 1.812(15) 6 ?
P1 Mn1 2.251(6) . ?
P2 C12 1.823(17) 6 ?
P2 Mn1 2.269(4) . ?
P3 C31 1.823(19) 6_565 ?
P3 Mn2 2.279(4) . ?
P4 C21 1.830(14) 6_565 ?
P4 Mn2 2.246(6) . ?
Mn1 C19 1.806(16) 6 ?
Mn1 P2 2.269(4) 6 ?
Mn2 C38 1.812(16) 6_565 ?
Mn2 P3 2.279(4) 6_565 ?
C39 C40 1.51(4) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 O5 1.17(3) . ?
C40 C41 1.43(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.53(2) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 O6 1.22(2) . ?
C43 C44 1.53(2) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C42A C43A 1.432(11) . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 0.9800 . ?
C43A O6A 1.233(11) . ?
C43A C42A 1.432(11) 6 ?
C45 C46 1.47(2) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 O7 1.22(2) . ?
C46 C45 1.47(2) 6 ?
C45A C46A 1.502(14) . ?
C45A H45D 0.9800 . ?
C45A H45E 0.9800 . ?
C45A H45F 0.9800 . ?
C46A O7A 1.23(2) . ?
C46A C45A 1.502(14) 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
C2 C1 C6 119.7(14) . . ?
C2 C1 P1 117.1(12) . . ?
C6 C1 P1 123.1(12) . . ?
C3 C2 C1 119.0(14) . . ?
C3 C2 P2 124.5(13) . . ?
C1 C2 P2 116.2(11) . . ?
C4 C3 C2 120.9(17) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 119.2(16) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 120.9(16) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C1 120.3(16) . . ?
C5 C6 H6 119.9 . . ?
C1 C6 H6 119.9 . . ?
C12 C7 C8 108.8(9) . . ?
C12 C7 P2 109.2(14) . . ?
C8 C7 P2 112.1(15) . . ?
C12 C7 H7 108.9 . . ?
C8 C7 H7 108.9 . . ?
P2 C7 H7 108.9 . . ?
C7 C8 C9 108.2(9) . . ?
C7 C8 H8A 110.1 . . ?
C9 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
C9 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C10 C9 C8 108.2(9) . . ?
C10 C9 H9A 110.1 . . ?
C8 C9 H9A 110.1 . . ?
C10 C9 H9B 110.1 . . ?
C8 C9 H9B 110.1 . . ?
H9A C9 H9B 108.4 . . ?
C11 C10 C9 108.6(9) . . ?
C11 C10 H10A 110.0 . . ?
C9 C10 H10A 110.0 . . ?
C11 C10 H10B 110.0 . . ?
C9 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
C12 C11 C10 108.7(9) . . ?
C12 C11 H11A 110.0 . . ?
C10 C11 H11A 110.0 . . ?
C12 C11 H11B 110.0 . . ?
C10 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
C11 C12 C7 109.0(9) . . ?
C11 C12 P2 117.6(15) . 6 ?
C7 C12 P2 106.9(13) . 6 ?
C11 C12 H12 107.7 . . ?
C7 C12 H12 107.7 . . ?
P2 C12 H12 107.7 6 . ?
P2 C13 H13A 109.5 . . ?
P2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
P2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 C15 122.0(15) 6 . ?
C15 C14 P1 118.9(7) 6 . ?
C15 C14 P1 118.9(7) . . ?
C14 C15 C16 119.2(10) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
C17 C16 C15 118.0(11) . . ?
C17 C16 H16 121.0 . . ?
C15 C16 H16 121.0 . . ?
C16 C17 C16 123.5(16) . 6 ?
C16 C17 H17 118.2 . . ?
C16 C17 H17 118.2 6 . ?
O1 C18 Mn1 177(2) . . ?
O2 C19 Mn1 177.0(13) . . ?
C25 C20 C21 118.8(13) . . ?
C25 C20 P3 124.9(12) . . ?
C21 C20 P3 116.2(11) . . ?
C20 C21 C22 121.0(13) . . ?
C20 C21 P4 116.6(10) . . ?
C22 C21 P4 122.3(11) . . ?
C21 C22 C23 117.5(14) . . ?
C21 C22 H22 121.3 . . ?
C23 C22 H22 121.3 . . ?
C24 C23 C22 120.5(15) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 122.6(17) . . ?
C23 C24 H24 118.7 . . ?
C25 C24 H24 118.7 . . ?
C24 C25 C20 119.6(16) . . ?
C24 C25 H25 120.2 . . ?
C20 C25 H25 120.2 . . ?
C31 C26 C27 110.1(16) . . ?
C31 C26 P3 107.9(13) . . ?
C27 C26 P3 115.3(15) . . ?
C31 C26 H26 107.7 . . ?
C27 C26 H26 107.7 . . ?
P3 C26 H26 107.7 . . ?
C26 C27 C28 108.0(9) . . ?
C26 C27 H27A 110.1 . . ?
C28 C27 H27A 110.1 . . ?
C26 C27 H27B 110.1 . . ?
C28 C27 H27B 110.1 . . ?
H27A C27 H27B 108.4 . . ?
C29 C28 C27 108.2(9) . . ?
C29 C28 H28A 110.1 . . ?
C27 C28 H28A 110.1 . . ?
C29 C28 H28B 110.1 . . ?
C27 C28 H28B 110.1 . . ?
H28A C28 H28B 108.4 . . ?
C30 C29 C28 108.8(10) . . ?
C30 C29 H29A 109.9 . . ?
C28 C29 H29A 109.9 . . ?
C30 C29 H29B 109.9 . . ?
C28 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
C31 C30 C29 109.3(9) . . ?
C31 C30 H30A 109.8 . . ?
C29 C30 H30A 109.8 . . ?
C31 C30 H30B 109.8 . . ?
C29 C30 H30B 109.8 . . ?
H30A C30 H30B 108.3 . . ?
C30 C31 C26 109.2(9) . . ?
C30 C31 P3 115.1(16) . 6_565 ?
C26 C31 P3 107.4(14) . 6_565 ?
C30 C31 H31 108.3 . . ?
C26 C31 H31 108.3 . . ?
P3 C31 H31 108.3 6_565 . ?
P3 C32 H32A 109.5 . . ?
P3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
P3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C34 121.6(14) . 6_565 ?
C34 C33 P4 118.9(7) . . ?
C34 C33 P4 118.9(7) 6_565 . ?
C33 C34 C35 119.5(10) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C36 C35 C34 117.8(10) . . ?
C36 C35 H35 121.1 . . ?
C34 C35 H35 121.1 . . ?
C35 C36 C35 123.2(15) 6_565 . ?
C35 C36 H36 118.4 6_565 . ?
C35 C36 H36 118.4 . . ?
O3 C37 Mn2 175(2) . . ?
O4 C38 Mn2 177.4(13) . . ?
C1 P1 C1 104.7(9) 6 . ?
C1 P1 C14 106.8(6) 6 . ?
C1 P1 C14 106.8(6) . . ?
C1 P1 Mn1 109.6(5) 6 . ?
C1 P1 Mn1 109.6(5) . . ?
C14 P1 Mn1 118.3(7) . . ?
C2 P2 C13 105.4(7) . . ?
C2 P2 C12 113.8(10) . 6 ?
C13 P2 C12 99.3(9) . 6 ?
C2 P2 C7 93.1(9) . . ?
C13 P2 C7 115.3(9) . . ?
C12 P2 C7 22.7(8) 6 . ?
C2 P2 Mn1 110.2(5) . . ?
C13 P2 Mn1 120.0(5) . . ?
C12 P2 Mn1 108.1(8) 6 . ?
C7 P2 Mn1 109.4(7) . . ?
C32 P3 C20 105.8(8) . . ?
C32 P3 C31 98.0(10) . 6_565 ?
C20 P3 C31 113.9(10) . 6_565 ?
C32 P3 C26 113.5(10) . . ?
C20 P3 C26 92.4(10) . . ?
C31 P3 C26 23.0(8) 6_565 . ?
C32 P3 Mn2 120.9(6) . . ?
C20 P3 Mn2 109.8(5) . . ?
C31 P3 Mn2 108.2(8) 6_565 . ?
C26 P3 Mn2 110.5(7) . . ?
C33 P4 C21 106.2(6) . 6_565 ?
C33 P4 C21 106.2(6) . . ?
C21 P4 C21 103.8(9) 6_565 . ?
C33 P4 Mn2 119.0(7) . . ?
C21 P4 Mn2 110.3(5) 6_565 . ?
C21 P4 Mn2 110.3(5) . . ?
C18 Mn1 C19 94.2(7) . . ?
C18 Mn1 C19 94.2(7) . 6 ?
C19 Mn1 C19 96.9(9) . 6 ?
C18 Mn1 P1 171.6(8) . . ?
C19 Mn1 P1 91.4(5) . . ?
C19 Mn1 P1 91.4(5) 6 . ?
C18 Mn1 P2 90.0(6) . 6 ?
C19 Mn1 P2 172.2(5) . 6 ?
C19 Mn1 P2 89.3(5) 6 6 ?
P1 Mn1 P2 83.78(16) . 6 ?
C18 Mn1 P2 90.0(6) . . ?
C19 Mn1 P2 89.3(5) . . ?
C19 Mn1 P2 172.2(5) 6 . ?
P1 Mn1 P2 83.78(16) . . ?
P2 Mn1 P2 84.1(2) 6 . ?
C37 Mn2 C38 89.9(7) . . ?
C37 Mn2 C38 89.9(7) . 6_565 ?
C38 Mn2 C38 95.8(9) . 6_565 ?
C37 Mn2 P4 175.9(8) . . ?
C38 Mn2 P4 92.9(4) . . ?
C38 Mn2 P4 92.9(4) 6_565 . ?
C37 Mn2 P3 93.2(6) . 6_565 ?
C38 Mn2 P3 90.4(4) . 6_565 ?
C38 Mn2 P3 173.1(5) 6_565 6_565 ?
P4 Mn2 P3 83.71(16) . 6_565 ?
C37 Mn2 P3 93.2(6) . . ?
C38 Mn2 P3 173.1(5) . . ?
C38 Mn2 P3 90.4(4) 6_565 . ?
P4 Mn2 P3 83.71(16) . . ?
P3 Mn2 P3 83.3(2) 6_565 . ?
C40 C39 H39A 109.5 . . ?
C40 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C40 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O5 C40 C41 124(3) . . ?
O5 C40 C39 119(3) . . ?
C41 C40 C39 117(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 H42A 109.5 . . ?
C43 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C43 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
O6 C43 C42 126(5) . . ?
O6 C43 C44 120(5) . . ?
C42 C43 C44 114(2) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C43A C42A H42D 109.5 . . ?
C43A C42A H42E 109.5 . . ?
H42D C42A H42E 109.5 . . ?
C43A C42A H42F 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
O6A C43A C42A 119.4(9) . 6 ?
O6A C43A C42A 119.4(9) . . ?
C42A C43A C42A 121.1(17) 6 . ?
C46 C45 H45A 109.5 . . ?
C46 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C46 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O7 C46 C45 119.5(15) . 6 ?
O7 C46 C45 119.5(15) . . ?
C45 C46 C45 121(3) 6 . ?
C46A C45A H45D 109.5 . . ?
C46A C45A H45E 109.5 . . ?
H45D C45A H45E 109.5 . . ?
C46A C45A H45F 109.5 . . ?
H45D C45A H45F 109.5 . . ?
H45E C45A H45F 109.5 . . ?
O7A C46A C45A 122.0(12) . 6 ?
O7A C46A C45A 122.0(12) . . ?
C45A C46A C45A 116(2) 6 . ?

_refine_diff_density_max         1.892
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.153

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1015696'
#######################################################################
#
#                 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_shelx_cmpd1

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 B Cu F4 P4'
_chemical_formula_weight         446.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
C C 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.7911(5)
_cell_length_b                   8.9433(3)
_cell_length_c                   12.8881(6)
_cell_angle_alpha                80.312(3)
_cell_angle_beta                 83.702(2)
_cell_angle_gamma                88.708(3)
_cell_volume                     992.79(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2872
_cell_measurement_theta_min      2.331
_cell_measurement_theta_max      27.487


_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_F_000             460
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.448
_shelx_estimated_absorpt_T_min   0.869
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.869
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_process_details   Denzo/Scalepack

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6956
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.331
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4487
_reflns_number_gt                2872
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXs-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0931P)²+1.2089P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.070(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4487
_refine_ls_number_parameters     246
_refine_ls_number_restraints     254
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1971
_refine_ls_wR_factor_gt          0.1678
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1747(6) 0.1378(6) 0.7104(4) 0.0549(13) Uani 1 1 d . . . . .
H1 H 0.1594 0.2475 0.7156 0.066 Uiso 1 1 calc R U . . .
C2 C 0.3471(6) 0.1089(6) 0.6940(4) 0.0573(13) Uani 1 1 d . . . . .
H2 H 0.3632 -0.0021 0.6937 0.069 Uiso 1 1 calc R U . . .
C3 C 0.4276(8) 0.1511(7) 0.7869(5) 0.0705(17) Uani 1 1 d . . . . .
H3A H 0.5380 0.1261 0.7773 0.085 Uiso 1 1 calc R U . . .
H3B H 0.4171 0.2613 0.7879 0.085 Uiso 1 1 calc R U . . .
C4 C 0.3525(9) 0.0607(8) 0.8925(5) 0.084(2) Uani 1 1 d . . . . .
H4A H 0.3740 -0.0488 0.8939 0.101 Uiso 1 1 calc R U . . .
H4B H 0.3987 0.0921 0.9521 0.101 Uiso 1 1 calc R U . . .
C5 C 0.1836(8) 0.0850(9) 0.9070(5) 0.084(2) Uani 1 1 d . . . . .
H5A H 0.1621 0.1925 0.9130 0.101 Uiso 1 1 calc R U . . .
H5B H 0.1401 0.0214 0.9736 0.101 Uiso 1 1 calc R U . . .
C6 C 0.1071(8) 0.0453(7) 0.8153(4) 0.0660(15) Uani 1 1 d . . . . .
H6A H -0.0041 0.0660 0.8263 0.079 Uiso 1 1 calc R U . . .
H6B H 0.1212 -0.0642 0.8127 0.079 Uiso 1 1 calc R U . . .
C7 C 0.2462(9) 0.4924(7) 0.2502(5) 0.0778(19) Uani 1 1 d . . . . .
H7 H 0.3591 0.5074 0.2470 0.093 Uiso 1 1 calc R U . . .
C8 C 0.2328(9) 0.3566(8) 0.2044(5) 0.082(2) Uani 1 1 d . . . . .
H8 H 0.1198 0.3450 0.2053 0.098 Uiso 1 1 calc R U . . .
C9 C 0.2908(9) 0.3696(10) 0.0879(5) 0.091(2) Uani 1 1 d . . . . .
H9A H 0.4039 0.3616 0.0808 0.109 Uiso 1 1 calc R U . . .
H9B H 0.2508 0.2834 0.0601 0.109 Uiso 1 1 calc R U . . .
C10 C 0.2462(14) 0.5129(16) 0.0227(7) 0.137(4) Uani 1 1 d . . . . .
H10A H 0.3138 0.5270 -0.0448 0.164 Uiso 1 1 calc R U . . .
H10B H 0.1406 0.5012 0.0055 0.164 Uiso 1 1 calc R U . . .
C11 C 0.2515(17) 0.6460(14) 0.0670(8) 0.163(5) Uani 1 1 d . . . . .
H11A H 0.1929 0.7259 0.0252 0.196 Uiso 1 1 calc R U . . .
H11B H 0.3593 0.6798 0.0585 0.196 Uiso 1 1 calc R U . . .
C12 C 0.1908(8) 0.6354(7) 0.1820(5) 0.0787(19) Uani 1 1 d . . . . .
H12A H 0.0775 0.6357 0.1885 0.094 Uiso 1 1 calc R U . . .
H12B H 0.2240 0.7256 0.2087 0.094 Uiso 1 1 calc R U . . .
B1 B 0.7350(9) 0.3719(9) 0.3089(6) 0.0511(17) Uani 0.720(5) 1 d D U P A 1
F1 F 0.6019(7) 0.4280(9) 0.3512(7) 0.126(2) Uani 0.720(5) 1 d D U P A 1
F2 F 0.6898(10) 0.2849(8) 0.2438(5) 0.127(2) Uani 0.720(5) 1 d D U P A 1
F3 F 0.8145(7) 0.4920(6) 0.2524(5) 0.104(2) Uani 0.720(5) 1 d D U P A 1
F4 F 0.8060(9) 0.3015(9) 0.3881(6) 0.129(2) Uani 0.720(5) 1 d D U P A 1
B1A B 0.733(5) 0.378(5) 0.306(3) 0.082(3) Uani 0.280(5) 1 d . U P A 2
F1A F 0.8466(15) 0.3197(17) 0.2460(11) 0.101(4) Uani 0.280(5) 1 d D U P A 2
F2A F 0.6104(14) 0.403(2) 0.2660(14) 0.108(4) Uani 0.280(5) 1 d D U P A 2
F3A F 0.709(2) 0.2520(15) 0.3870(11) 0.117(4) Uani 0.280(5) 1 d D U P A 2
F4A F 0.7846(19) 0.4789(16) 0.3528(14) 0.118(4) Uani 0.280(5) 1 d D U P A 2
P1 P 0.08759(16) 0.10323(14) 0.59331(10) 0.0488(4) Uani 1 1 d . . . . .
H1A H -0.0180 0.1442 0.5937 0.059 Uiso 1 1 calc R U . . .
H1B H 0.0852 -0.0066 0.5904 0.059 Uiso 1 1 calc R U . . .
P2 P 0.43227(17) 0.21323(17) 0.56299(13) 0.0618(4) Uani 1 1 d . . . . .
H2A H 0.5216 0.1574 0.5346 0.074 Uiso 1 1 calc R U . . .
H2B H 0.4654 0.3159 0.5697 0.074 Uiso 1 1 calc R U . . .
P3 P 0.18028(16) 0.47027(14) 0.39030(11) 0.0509(4) Uani 1 1 d . . . . .
H3C H 0.0684 0.4870 0.4015 0.061 Uiso 1 1 calc R U . . .
H3D H 0.2325 0.5427 0.4246 0.061 Uiso 1 1 calc R U . . .
P4 P 0.28880(17) 0.18333(16) 0.28892(12) 0.0583(4) Uani 1 1 d . . . . .
H4C H 0.3987 0.1611 0.2722 0.070 Uiso 1 1 calc R U . . .
H4D H 0.2282 0.0960 0.2787 0.070 Uiso 1 1 calc R U . . .
Cu1 Cu 0.24185(7) 0.22741(7) 0.45582(5) 0.0517(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.528(8) . ?
C1 C2 1.529(8) . ?
C1 P1 1.838(5) . ?
C2 C3 1.558(7) . ?
C2 P2 1.872(6) . ?
C3 C4 1.549(10) . ?
C4 C5 1.492(10) . ?
C5 C6 1.517(8) . ?
C7 C8 1.449(9) . ?
C7 C12 1.527(8) . ?
C7 P3 1.814(6) . ?
C8 C9 1.518(9) . ?
C8 P4 1.829(7) . ?
C9 C10 1.479(13) . ?
C10 C11 1.408(15) . ?
C11 C12 1.508(11) . ?
B1 F4 1.317(8) . ?
B1 F2 1.331(8) . ?
B1 F3 1.353(8) . ?
B1 F1 1.358(8) . ?
B1A F2A 1.25(5) . ?
B1A F4A 1.28(4) . ?
B1A F1A 1.34(5) . ?
B1A F3A 1.40(5) . ?
P1 Cu1 2.2563(15) . ?
P2 Cu1 2.2726(15) . ?
P3 Cu1 2.2701(14) . ?
P4 Cu1 2.2440(16) . ?

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
C6 C1 C2 109.7(4) . . ?
C6 C1 P1 115.0(4) . . ?
C2 C1 P1 109.2(4) . . ?
C1 C2 C3 110.9(5) . . ?
C1 C2 P2 110.9(3) . . ?
C3 C2 P2 111.5(4) . . ?
C4 C3 C2 108.9(5) . . ?
C5 C4 C3 112.2(5) . . ?
C4 C5 C6 111.6(6) . . ?
C5 C6 C1 110.9(6) . . ?
C8 C7 C12 113.2(6) . . ?
C8 C7 P3 114.2(5) . . ?
C12 C7 P3 115.5(5) . . ?
C7 C8 C9 115.6(6) . . ?
C7 C8 P4 113.5(4) . . ?
C9 C8 P4 115.4(5) . . ?
C10 C9 C8 113.7(8) . . ?
C11 C10 C9 117.0(8) . . ?
C10 C11 C12 116.7(9) . . ?
C11 C12 C7 112.3(6) . . ?
F4 B1 F2 115.9(7) . . ?
F4 B1 F3 112.7(7) . . ?
F2 B1 F3 109.9(7) . . ?
F4 B1 F1 107.3(7) . . ?
F2 B1 F1 103.6(7) . . ?
F3 B1 F1 106.6(7) . . ?
F2A B1A F4A 119(4) . . ?
F2A B1A F1A 115(3) . . ?
F4A B1A F1A 111(3) . . ?
F2A B1A F3A 107(3) . . ?
F4A B1A F3A 104(3) . . ?
F1A B1A F3A 98(3) . . ?
C1 P1 Cu1 103.92(19) . . ?
C2 P2 Cu1 105.09(17) . . ?
C7 P3 Cu1 104.5(2) . . ?
C8 P4 Cu1 105.9(2) . . ?
P4 Cu1 P1 129.89(5) . . ?
P4 Cu1 P3 88.64(5) . . ?
P1 Cu1 P3 117.96(6) . . ?
P4 Cu1 P2 120.97(6) . . ?
P1 Cu1 P2 88.83(6) . . ?
P3 Cu1 P2 112.55(6) . . ?

_refine_diff_density_max         0.777
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.090

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1015697'
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#                                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.
#
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#  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
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#  data retrieval see:
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data_shelx_cmpd2

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H50 Ag3 P10, 3(C F3 O3 S)'
_chemical_formula_sum            'C33 H50 Ag3 F9 O9 P10 S3'
_chemical_formula_weight         1491.22

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'
Ag Ag -0.8971 1.1015 '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'
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 21/m'
_space_group_name_Hall           '-P 2yb'

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

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

_cell_length_a                   9.8754(3)
_cell_length_b                   23.0437(9)
_cell_length_c                   13.1527(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.030(2)
_cell_angle_gamma                90
_cell_volume                     2956.01(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4542
_cell_measurement_theta_min      2.088
_cell_measurement_theta_max      25.242

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_F_000             1480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.430
_shelx_estimated_absorpt_T_min   0.674
_shelx_estimated_absorpt_T_max   0.870
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6735
_exptl_absorpt_correction_T_max  0.8702
_exptl_absorpt_process_details   Denzo/Scalepack

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11498
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.088
_diffrn_reflns_theta_max         27.463
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6912
_reflns_number_gt                4542
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXs-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1027P)²+12.2417P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0094(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6912
_refine_ls_number_parameters     433
_refine_ls_number_restraints     638
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.0749
_refine_ls_wR_factor_ref         0.2190
_refine_ls_wR_factor_gt          0.1911
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.057
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8745(6) 0.3714(3) 0.1673(5) 0.0384(14) Uani 1 1 d . . . . .
H1 H 0.8481 0.3304 0.1492 0.046 Uiso 1 1 calc R U . . .
C2 C 0.8068(7) 0.3883(3) 0.2601(5) 0.0462(16) Uani 1 1 d . . . . .
H2A H 0.8284 0.4293 0.2783 0.055 Uiso 1 1 calc R U . . .
H2B H 0.7060 0.3848 0.2416 0.055 Uiso 1 1 calc R U . . .
C3 C 0.8562(9) 0.3499(4) 0.3527(5) 0.0565(19) Uani 1 1 d . . . . .
H3A H 0.8294 0.3092 0.3363 0.068 Uiso 1 1 calc R U . . .
H3B H 0.8123 0.3624 0.4118 0.068 Uiso 1 1 calc R U . . .
C4 C 1.0115(9) 0.3538(4) 0.3817(6) 0.058(2) Uani 1 1 d . . . . .
H4A H 1.0374 0.3939 0.4037 0.069 Uiso 1 1 calc R U . . .
H4B H 1.0422 0.3276 0.4403 0.069 Uiso 1 1 calc R U . . .
C5 C 1.0829(9) 0.3373(4) 0.2917(6) 0.060(2) Uani 1 1 d . . . . .
H5A H 1.0667 0.2957 0.2758 0.071 Uiso 1 1 calc R U . . .
H5B H 1.1829 0.3431 0.3114 0.071 Uiso 1 1 calc R U . . .
C6 C 1.0319(7) 0.3734(3) 0.1950(5) 0.0425(15) Uani 1 1 d . . . . .
H6 H 1.0612 0.4146 0.2081 0.051 Uiso 1 1 calc R U . . .
C7 C 0.7856(10) 0.2686(6) -0.2127(9) 0.052(4) Uani 0.5 1 d D . P . .
H7 H 0.7856 0.3119 -0.2150 0.063 Uiso 0.5 1 calc R U P . .
C8 C 0.9154(12) 0.2500 -0.2545(7) 0.100(6) Uani 1 2 d DS T P . .
H8 H 0.8995 0.2074 -0.2486 0.120 Uiso 0.5 1 calc R U P . .
C9 C 0.9090(14) 0.2500 -0.3719(7) 0.074(4) Uani 1 2 d DS T P . .
H9A H 0.9808 0.2234 -0.3889 0.089 Uiso 0.5 1 calc R U P . .
H9B H 0.9327 0.2895 -0.3931 0.089 Uiso 0.5 1 calc R U P . .
C10 C 0.7721(15) 0.2325(9) -0.4371(12) 0.095(9) Uani 0.5 1 d D . P . .
H10A H 0.7696 0.2493 -0.5067 0.114 Uiso 1 2 calc R U P . .
H10B H 0.7718 0.1898 -0.4448 0.114 Uiso 0.5 1 calc R U P . .
C11 C 0.639(2) 0.2500 -0.3983(8) 0.155(9) Uani 1 2 d DS TU P . .
H11A H 0.5656 0.2229 -0.4272 0.186 Uiso 0.5 1 calc R U P . .
H11B H 0.6125 0.2893 -0.4243 0.186 Uiso 0.5 1 calc R U P . .
C12 C 0.6514(12) 0.2500 -0.2804(8) 0.072(4) Uani 1 2 d DS T P . .
H12A H 0.6303 0.2102 -0.2594 0.087 Uiso 0.5 1 calc R U P . .
H12B H 0.5779 0.2755 -0.2626 0.087 Uiso 0.5 1 calc R U P . .
C13 C 0.5903(9) 0.5359(4) 0.2755(6) 0.069(2) Uani 1 1 d . . . . .
H13 H 0.6882 0.5259 0.2726 0.083 Uiso 1 1 calc R U . . .
C14 C 0.5678(9) 0.5983(4) 0.2402(7) 0.071(2) Uani 1 1 d . . . . .
H14 H 0.4699 0.6080 0.2437 0.085 Uiso 1 1 calc R U . . .
C15 C 0.6543(9) 0.6377(5) 0.3135(8) 0.083(3) Uani 1 1 d . . . . .
H15A H 0.6349 0.6783 0.2912 0.100 Uiso 1 1 calc R U . . .
H15B H 0.7519 0.6299 0.3095 0.100 Uiso 1 1 calc R U . . .
C16 C 0.6331(14) 0.6319(6) 0.4254(9) 0.107(4) Uani 1 1 d . . . . .
H16A H 0.6979 0.6576 0.4695 0.128 Uiso 1 1 calc R U . . .
H16B H 0.5386 0.6438 0.4323 0.128 Uiso 1 1 calc R U . . .
C17 C 0.6565(15) 0.5702(6) 0.4587(9) 0.102(4) Uani 1 1 d . . . . .
H17A H 0.6358 0.5658 0.5295 0.122 Uiso 1 1 calc R U . . .
H17B H 0.7542 0.5603 0.4597 0.122 Uiso 1 1 calc R U . . .
C18 C 0.5669(11) 0.5283(5) 0.3870(7) 0.081(3) Uani 1 1 d . . . . .
H18A H 0.5889 0.4879 0.4093 0.097 Uiso 1 1 calc R U . . .
H18B H 0.4692 0.5354 0.3915 0.097 Uiso 1 1 calc R U . . .
Ag1 Ag 1.04195(8) 0.2500 0.00814(6) 0.0501(3) Uani 1 2 d S T P . .
Ag2 Ag 0.55636(6) 0.43717(3) 0.03818(5) 0.0645(3) Uani 1 1 d . . . . .
P1 P 0.80393(18) 0.41715(9) 0.05644(14) 0.0456(5) Uani 1 1 d . . . . .
P2 P 1.11561(19) 0.34417(9) 0.08925(15) 0.0478(5) Uani 1 1 d . . . . .
P3 P 1.0777(3) 0.2500 -0.1779(2) 0.0529(7) Uani 1 2 d S T P . .
P4 P 0.7911(3) 0.2500 -0.0777(2) 0.0507(7) Uani 1 2 d S T P . .
P5 P 0.4785(2) 0.48273(11) 0.1890(2) 0.0695(7) Uani 1 1 d . . . . .
P6 P 0.5934(2) 0.60877(12) 0.10495(17) 0.0679(7) Uani 1 1 d . . . . .
C19 C 0.9250(7) 0.4470(3) -0.3563(5) 0.065(3) Uani 0.636(7) 1 d D U P A 1
F1 F 0.9577(13) 0.3980(4) -0.3981(6) 0.097(4) Uani 0.636(7) 1 d D U P A 1
F2 F 1.0214(9) 0.4851(3) -0.3660(6) 0.101(3) Uani 0.636(7) 1 d D U P A 1
F3 F 0.8096(8) 0.4659(7) -0.4094(7) 0.160(6) Uani 0.636(7) 1 d D U P A 1
O1 O 1.0345(7) 0.4082(5) -0.1803(7) 0.095(4) Uani 0.636(7) 1 d D U P A 1
O2 O 0.7900(6) 0.3992(3) -0.2275(6) 0.059(2) Uani 0.636(7) 1 d D U P A 1
O3 O 0.8898(12) 0.4931(3) -0.1853(9) 0.102(6) Uani 0.636(7) 1 d D U P A 1
S1 S 0.9083(4) 0.43551(17) -0.2218(3) 0.0520(11) Uani 0.636(7) 1 d D U P A 1
C19A C 0.8876(11) 0.4440(5) -0.3473(7) 0.073(5) Uani 0.364(7) 1 d D U P A 2
F1A F 0.9684(17) 0.4192(9) -0.4052(8) 0.122(8) Uani 0.364(7) 1 d D U P A 2
F2A F 0.7718(12) 0.4145(6) -0.3594(11) 0.120(7) Uani 0.364(7) 1 d D U P A 2
F3A F 0.859(2) 0.4967(5) -0.3831(10) 0.106(7) Uani 0.364(7) 1 d D U P A 2
O1A O 0.9764(15) 0.3863(3) -0.1839(10) 0.078(6) Uani 0.364(7) 1 d D U P A 2
O2A O 1.0969(8) 0.4732(5) -0.2167(9) 0.069(5) Uani 0.364(7) 1 d D U P A 2
O3A O 0.8742(11) 0.4799(6) -0.1649(10) 0.047(4) Uani 0.364(7) 1 d D U P A 2
S1A S 0.9680(6) 0.4460(3) -0.2130(5) 0.0500(18) Uani 0.364(7) 1 d D U P A 2
C20 C 0.4827(6) 0.2500 0.2559(5) 0.065(3) Uani 0.791(11) 2 d DS TU P B 1
F4 F 0.5304(8) 0.2956(4) 0.3130(6) 0.137(4) Uani 0.791(11) 1 d D U P B 1
F5 F 0.3490(5) 0.2500 0.2565(5) 0.051(2) Uani 0.791(11) 2 d DS TU P B 1
O4 O 0.6792(5) 0.2500 0.1501(6) 0.052(2) Uani 0.791(11) 2 d DS TU P B 1
O5 O 0.4776(10) 0.3049(4) 0.0897(8) 0.160(5) Uani 0.791(11) 1 d D U P B 1
S2 S 0.5319(3) 0.2500 0.1333(2) 0.0793(11) Uani 0.791(11) 2 d DS TU P B 1
C20A C 0.4827(6) 0.2500 0.2559(5) 0.065(3) Uani 0.209(11) 2 d DS TU P B 2
F4A F 0.3701(14) 0.2743(12) 0.2682(9) 0.090(8) Uani 0.209(11) 1 d D U P B 2
F5A F 0.5748(12) 0.2500 0.3350(5) 0.034(6) Uani 0.209(11) 2 d DS TU P B 2
O4A O 0.4120(11) 0.2500 0.0589(7) 0.041(7) Uani 0.209(11) 2 d DS TU P B 2
O5A O 0.623(2) 0.2978(9) 0.1305(8) 0.175(13) Uani 0.209(11) 1 d D U P B 2
S2A S 0.5319(3) 0.2500 0.1333(2) 0.0793(11) Uani 0.209(11) 2 d DS TU P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.531(9) . ?
C1 C6 1.540(9) . ?
C1 P1 1.844(6) . ?
C2 C3 1.523(10) . ?
C3 C4 1.523(12) . ?
C4 C5 1.518(11) . ?
C5 C6 1.536(10) . ?
C6 P2 1.853(7) . ?
C7 C8 1.532(5) . ?
C7 C12 1.537(5) . ?
C7 P4 1.818(13) . ?
C8 C9 1.536(5) . ?
C8 P3 1.754(13) . ?
C9 C10 1.537(5) . ?
C10 C11 1.534(5) . ?
C11 C12 1.537(5) . ?
C13 C14 1.516(14) . ?
C13 C18 1.530(12) . ?
C13 P5 1.903(10) . ?
C14 C15 1.492(14) . ?
C14 P6 1.852(9) . ?
C15 C16 1.524(14) . ?
C16 C17 1.495(17) . ?
C17 C18 1.531(16) . ?
Ag1 P2 2.477(2) . ?
Ag1 P2 2.477(2) 4_565 ?
Ag1 P3 2.526(3) . ?
Ag1 P4 2.556(3) . ?
Ag2 P6 2.445(3) 3_665 ?
Ag2 P1 2.4623(19) . ?
Ag2 P5 2.471(3) . ?
Ag2 Ag2 3.2068(14) 3_665 ?
P4 C7 1.818(13) 4_565 ?
P6 Ag2 2.445(3) 3_665 ?
C19 F3 1.314(5) . ?
C19 F2 1.316(5) . ?
C19 F1 1.319(5) . ?
C19 S1 1.822(7) . ?
O1 S1 1.425(5) . ?
O2 S1 1.429(5) . ?
O3 S1 1.433(5) . ?
C19A F1A 1.317(6) . ?
C19A F3A 1.317(6) . ?
C19A F2A 1.319(6) . ?
C19A S1A 1.820(8) . ?
O1A S1A 1.427(5) . ?
O2A S1A 1.427(5) . ?
O3A S1A 1.434(5) . ?
C20 F5 1.321(5) . ?
C20 F4 1.334(5) 4_565 ?
C20 F4 1.334(5) . ?
C20 S2 1.756(6) . ?
O4 S2 1.437(5) . ?
O5 S2 1.455(5) . ?
S2 O5 1.455(5) 4_565 ?
F4A F4A 1.12(5) 4_565 ?

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 C1 C6 110.7(5) . . ?
C2 C1 P1 109.1(5) . . ?
C6 C1 P1 114.4(5) . . ?
C3 C2 C1 111.4(6) . . ?
C2 C3 C4 110.4(6) . . ?
C5 C4 C3 111.3(6) . . ?
C4 C5 C6 112.2(6) . . ?
C5 C6 C1 111.6(6) . . ?
C5 C6 P2 107.3(5) . . ?
C1 C6 P2 111.3(4) . . ?
C8 C7 C12 114.1(10) . . ?
C8 C7 P4 112.7(7) . . ?
C12 C7 P4 113.0(8) . . ?
C7 C8 C9 117.1(10) . . ?
C7 C8 P3 122.3(7) . . ?
C9 C8 P3 117.8(8) . . ?
C8 C9 C10 117.1(11) . . ?
C11 C10 C9 117.9(15) . . ?
C10 C11 C12 113.7(14) . . ?
C11 C12 C7 120.5(12) . . ?
C14 C13 C18 111.4(9) . . ?
C14 C13 P5 112.6(6) . . ?
C18 C13 P5 109.8(7) . . ?
C15 C14 C13 109.7(7) . . ?
C15 C14 P6 113.0(6) . . ?
C13 C14 P6 112.5(7) . . ?
C14 C15 C16 114.8(8) . . ?
C17 C16 C15 109.1(11) . . ?
C16 C17 C18 111.9(9) . . ?
C13 C18 C17 111.0(8) . . ?
P2 Ag1 P2 122.39(10) . 4_565 ?
P2 Ag1 P3 109.94(6) . . ?
P2 Ag1 P3 109.94(6) 4_565 . ?
P2 Ag1 P4 112.90(5) . . ?
P2 Ag1 P4 112.90(5) 4_565 . ?
P3 Ag1 P4 81.08(10) . . ?
P6 Ag2 P1 117.73(8) 3_665 . ?
P6 Ag2 P5 125.11(9) 3_665 . ?
P1 Ag2 P5 115.51(8) . . ?
P6 Ag2 Ag2 90.66(7) 3_665 3_665 ?
P1 Ag2 Ag2 119.36(6) . 3_665 ?
P5 Ag2 Ag2 74.41(6) . 3_665 ?
C1 P1 Ag2 115.5(2) . . ?
C6 P2 Ag1 120.4(2) . . ?
C8 P3 Ag1 107.6(3) . . ?
C7 P4 C7 27.2(8) 4_565 . ?
C7 P4 Ag1 108.0(3) 4_565 . ?
C7 P4 Ag1 108.0(3) . . ?
C13 P5 Ag2 121.9(3) . . ?
C14 P6 Ag2 121.7(3) . 3_665 ?
F3 C19 F2 107.9(5) . . ?
F3 C19 F1 108.1(6) . . ?
F2 C19 F1 107.6(5) . . ?
F3 C19 S1 111.2(5) . . ?
F2 C19 S1 111.6(5) . . ?
F1 C19 S1 110.3(4) . . ?
O1 S1 O2 114.9(4) . . ?
O1 S1 O3 115.5(5) . . ?
O2 S1 O3 114.4(4) . . ?
O1 S1 C19 103.2(4) . . ?
O2 S1 C19 103.4(3) . . ?
O3 S1 C19 103.1(4) . . ?
F1A C19A F3A 108.0(6) . . ?
F1A C19A F2A 107.4(6) . . ?
F3A C19A F2A 107.3(6) . . ?
F1A C19A S1A 111.1(5) . . ?
F3A C19A S1A 111.2(5) . . ?
F2A C19A S1A 111.6(5) . . ?
O2A S1A O1A 114.8(5) . . ?
O2A S1A O3A 114.6(5) . . ?
O1A S1A O3A 115.0(5) . . ?
O2A S1A C19A 103.5(4) . . ?
O1A S1A C19A 103.5(5) . . ?
O3A S1A C19A 103.2(5) . . ?
F5 C20 F4 105.2(4) . 4_565 ?
F5 C20 F4 105.2(4) . . ?
F4 C20 F4 103.9(12) 4_565 . ?
F5 C20 S2 115.2(5) . . ?
F4 C20 S2 113.2(4) 4_565 . ?
F4 C20 S2 113.2(4) . . ?
O4 S2 O5 111.2(4) . 4_565 ?
O4 S2 O5 111.2(4) . . ?
O5 S2 O5 120.6(11) 4_565 . ?
O4 S2 C20 106.2(4) . . ?
O5 S2 C20 102.9(4) 4_565 . ?
O5 S2 C20 102.9(4) . . ?

_refine_diff_density_max         2.068
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.142

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1015698'
#######################################################################
#
#                 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_shelx_cmpd10

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H31 F9 Fe P4'
_chemical_formula_weight         730.27

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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

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

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

_cell_length_a                   13.02100(10)
_cell_length_b                   15.2570(2)
_cell_length_c                   30.5590(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6070.89(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5784
_cell_measurement_theta_min      2.869
_cell_measurement_theta_max      25.242

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_F_000             2976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.784
_shelx_estimated_absorpt_T_min   0.745
_shelx_estimated_absorpt_T_max   0.926
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_process_details   Sadabs/Denzo

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13105
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.869
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             6923
_reflns_number_gt                5784
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'cOLLECT,Nonius BV, 1997-2001'
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_reduction        DENZO/SCALEPACK
_computing_structure_solution    SHELXs-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0233P)²+10.4241P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6923
_refine_ls_number_parameters     508
_refine_ls_number_restraints     630
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1140
_refine_ls_wR_factor_gt          0.1095
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_restrained_S_all      1.148
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0247(2) -0.03489(19) 0.59659(9) 0.0266(6) Uani 1 1 d . . . A 1
C2 C -0.0606(2) -0.1191(2) 0.60515(10) 0.0318(7) Uani 1 1 d . . . A 1
C3 C -0.0021(3) -0.1935(2) 0.60087(11) 0.0362(7) Uani 1 1 d . . . A 1
H3 H -0.0300 -0.2495 0.6074 0.043 Uiso 1 1 calc R U . A 1
C4 C 0.0987(3) -0.1847(2) 0.58670(11) 0.0379(8) Uani 1 1 d . . . A 1
H4 H 0.1409 -0.2351 0.5834 0.045 Uiso 1 1 calc R U . A 1
C5 C 0.1375(2) -0.1025(2) 0.57740(11) 0.0371(7) Uani 1 1 d . . . A 1
H5 H 0.2062 -0.0966 0.5673 0.045 Uiso 1 1 calc R U . A 1
C6 C 0.0769(2) -0.0289(2) 0.58270(11) 0.0319(7) Uani 1 1 d . . . A 1
H6 H 0.1054 0.0272 0.5767 0.038 Uiso 1 1 calc R U . A 1
C7 C -0.2073(2) 0.0470(2) 0.56467(9) 0.0273(6) Uani 1 1 d . . . A 1
C8 C -0.2875(2) 0.1068(2) 0.56120(10) 0.0313(7) Uani 1 1 d . . . A 1
C9 C -0.3657(2) 0.1008(2) 0.53101(10) 0.0357(7) Uani 1 1 d . . . A 1
H9 H -0.4192 0.1431 0.5302 0.043 Uiso 1 1 calc R U . A 1
C10 C -0.3637(2) 0.0312(2) 0.50190(10) 0.0367(7) Uani 1 1 d . . . A 1
H10 H -0.4166 0.0253 0.4807 0.044 Uiso 1 1 calc R U . A 1
C11 C -0.2856(2) -0.0292(2) 0.50356(10) 0.0353(7) Uani 1 1 d . . . A 1
H11 H -0.2845 -0.0766 0.4834 0.042 Uiso 1 1 calc R U . A 1
C12 C -0.2080(2) -0.0215(2) 0.53460(10) 0.0306(6) Uani 1 1 d . . . A 1
H12 H -0.1544 -0.0638 0.5353 0.037 Uiso 1 1 calc R U . A 1
C13 C -0.1661(2) 0.0401(2) 0.65676(9) 0.0284(6) Uani 1 1 d . . . A 1
C14 C -0.1079(2) 0.0237(2) 0.69391(10) 0.0317(7) Uani 1 1 d . . . A 1
C15 C -0.1473(3) 0.0117(2) 0.73506(10) 0.0365(7) Uani 1 1 d . . . A 1
H15 H -0.1033 0.0022 0.7594 0.044 Uiso 1 1 calc R U . A 1
C16 C -0.2525(3) 0.0137(2) 0.74012(11) 0.0412(8) Uani 1 1 d . . . A 1
H16 H -0.2822 0.0054 0.7682 0.049 Uiso 1 1 calc R U . A 1
C17 C -0.3147(3) 0.0280(2) 0.70408(11) 0.0399(8) Uani 1 1 d . . . A 1
H17 H -0.3871 0.0294 0.7077 0.048 Uiso 1 1 calc R U . A 1
C18 C -0.2728(2) 0.0403(2) 0.66284(10) 0.0346(7) Uani 1 1 d . . . A 1
H18 H -0.3168 0.0490 0.6384 0.042 Uiso 1 1 calc R U . A 1
C19 C -0.0848(3) 0.2282(2) 0.53468(11) 0.0441(8) Uani 1 1 d . . . A 1
H19 H -0.1543 0.2211 0.5260 0.053 Uiso 1 1 calc R U . A 1
C20 C -0.0045(3) 0.1661(2) 0.52936(11) 0.0459(9) Uani 1 1 d . . . A 1
H20 H -0.0110 0.1098 0.5163 0.055 Uiso 1 1 calc R U . A 1
C21 C 0.0861(3) 0.2022(2) 0.54670(12) 0.0454(9) Uani 1 1 d . . . A 1
H21 H 0.1516 0.1748 0.5474 0.054 Uiso 1 1 calc R U . A 1
C22 C 0.0623(3) 0.2868(2) 0.56293(12) 0.0442(9) Uani 1 1 d . . . A 1
H22 H 0.1090 0.3260 0.5766 0.053 Uiso 1 1 calc R U . A 1
C23 C -0.0418(3) 0.3025(2) 0.55531(12) 0.0443(9) Uani 1 1 d . . . A 1
H23 H -0.0779 0.3545 0.5628 0.053 Uiso 1 1 calc R U . A 1
C24 C -0.0415(4) 0.2825(4) 0.69584(17) 0.0331(18) Uani 0.590(6) 1 d D U P A 1
H24 H -0.0063 0.3397 0.6904 0.040 Uiso 0.590(6) 1 calc R U P A 1
C25 C 0.0441(4) 0.2136(3) 0.70098(13) 0.0294(14) Uani 0.590(6) 1 d D U P A 1
H25 H 0.0107 0.1603 0.7137 0.035 Uiso 0.590(6) 1 calc R U P A 1
C26 C 0.1196(3) 0.2473(4) 0.73592(17) 0.046(2) Uani 0.590(6) 1 d D U P A 1
H26A H 0.1767 0.2051 0.7396 0.055 Uiso 0.590(6) 1 calc R U P A 1
H26B H 0.1489 0.3042 0.7266 0.055 Uiso 0.590(6) 1 calc R U P A 1
C27 C 0.0620(5) 0.2583(4) 0.77957(14) 0.048(2) Uani 0.590(6) 1 d D U P A 1
H27A H 0.0338 0.2010 0.7890 0.058 Uiso 0.590(6) 1 calc R U P A 1
H27B H 0.1102 0.2789 0.8024 0.058 Uiso 0.590(6) 1 calc R U P A 1
C28 C -0.0260(5) 0.3248(4) 0.77435(18) 0.056(2) Uani 0.590(6) 1 d D U P A 1
H28A H 0.0023 0.3828 0.7663 0.068 Uiso 0.590(6) 1 calc R U P A 1
H28B H -0.0633 0.3310 0.8024 0.068 Uiso 0.590(6) 1 calc R U P A 1
C29 C -0.1003(6) 0.2930(5) 0.7385(3) 0.036(2) Uani 0.590(6) 1 d D U P A 1
H29A H -0.1310 0.2362 0.7471 0.043 Uiso 0.590(6) 1 calc R U P A 1
H29B H -0.1564 0.3361 0.7346 0.043 Uiso 0.590(6) 1 calc R U P A 1
C24A C -0.0467(5) 0.2492(6) 0.69944(18) 0.032(2) Uani 0.410(6) 1 d D U P A 2
H24A H -0.0648 0.1900 0.7112 0.038 Uiso 0.410(6) 1 calc R U P A 2
C25A C 0.0708(5) 0.2491(4) 0.69419(16) 0.043(2) Uani 0.410(6) 1 d D U P A 2
H25A H 0.0957 0.3101 0.6885 0.052 Uiso 0.410(6) 1 calc R U P A 2
C26A C 0.1194(5) 0.2138(5) 0.7366(2) 0.039(3) Uani 0.410(6) 1 d D U P A 2
H26C H 0.1948 0.2095 0.7332 0.047 Uiso 0.410(6) 1 calc R U P A 2
H26D H 0.0922 0.1547 0.7432 0.047 Uiso 0.410(6) 1 calc R U P A 2
C27A C 0.0928(6) 0.2774(6) 0.7741(2) 0.049(3) Uani 0.410(6) 1 d D U P A 2
H27C H 0.1242 0.2566 0.8017 0.059 Uiso 0.410(6) 1 calc R U P A 2
H27D H 0.1203 0.3364 0.7675 0.059 Uiso 0.410(6) 1 calc R U P A 2
C28A C -0.0247(6) 0.2819(6) 0.77915(18) 0.054(3) Uani 0.410(6) 1 d D U P A 2
H28C H -0.0429 0.3226 0.8032 0.064 Uiso 0.410(6) 1 calc R U P A 2
H28D H -0.0521 0.2231 0.7865 0.064 Uiso 0.410(6) 1 calc R U P A 2
C29A C -0.0724(7) 0.3140(8) 0.7359(3) 0.040(3) Uani 0.410(6) 1 d D U P A 2
H29C H -0.1478 0.3190 0.7391 0.047 Uiso 0.410(6) 1 calc R U P A 2
H29D H -0.0448 0.3727 0.7285 0.047 Uiso 0.410(6) 1 calc R U P A 2
F1 F -0.15985(14) -0.12936(12) 0.61805(7) 0.0416(5) Uani 1 1 d . . . A 1
F2 F -0.29019(14) 0.17636(13) 0.58909(6) 0.0412(5) Uani 1 1 d . . . A 1
F3 F -0.00366(14) 0.01926(13) 0.68927(6) 0.0408(5) Uani 1 1 d . . . A 1
Fe1 Fe -0.02445(3) 0.19236(3) 0.59570(2) 0.02760(13) Uani 0.590(6) 1 d . . P A
1
P1 P -0.10252(5) 0.06420(5) 0.60436(2) 0.02481(17) Uani 1 1 d . . . A 1
P2 P -0.11385(6) 0.25802(6) 0.64670(3) 0.0354(2) Uani 0.590(6) 1 d D . P A 1
H2A H -0.1416 0.3134 0.6347 0.042 Uiso 0.590(6) 1 calc R U P A 1
H2B H -0.1729 0.2203 0.6546 0.042 Uiso 0.590(6) 1 calc R U P A 1
P3 P 0.09426(6) 0.18037(5) 0.64635(3) 0.0337(2) Uani 0.590(6) 1 d D . P A 1
H3A H 0.1184 0.1189 0.6477 0.040 Uiso 0.590(6) 1 calc R U P A 1
H3B H 0.1536 0.2179 0.6386 0.040 Uiso 0.590(6) 1 calc R U P A 1
Fe1A Fe -0.02445(3) 0.19236(3) 0.59570(2) 0.02760(13) Uani 0.410(6) 1 d . . P A
2
P2A P -0.11385(6) 0.25802(6) 0.64670(3) 0.0354(2) Uani 0.410(6) 1 d D . P A 2
H2A1 H -0.1232 0.3206 0.6390 0.042 Uiso 0.410(6) 1 calc R U P A 2
H2A2 H -0.1826 0.2306 0.6490 0.042 Uiso 0.410(6) 1 calc R U P A 2
P3A P 0.09426(6) 0.18037(5) 0.64635(3) 0.0337(2) Uani 0.410(6) 1 d D . P A 2
H3A1 H 0.0983 0.1184 0.6558 0.040 Uiso 0.410(6) 1 calc R U P A 2
H3A2 H 0.1615 0.1964 0.6335 0.040 Uiso 0.410(6) 1 calc R U P A 2
P4 P -0.6118(4) 0.0451(3) 0.63283(16) 0.0287(8) Uani 0.554(7) 1 d D U P B 1
F4 F -0.5390(5) -0.0036(5) 0.6662(2) 0.067(3) Uani 0.554(7) 1 d D U P B 1
F5 F -0.6310(5) 0.1197(4) 0.6673(2) 0.0650(19) Uani 0.554(7) 1 d D U P B 1
F6 F -0.7067(3) -0.0053(3) 0.65228(17) 0.0625(16) Uani 0.554(7) 1 d D U P B 1
F7 F -0.6853(4) 0.0929(4) 0.59930(17) 0.0622(16) Uani 0.554(7) 1 d D U P B 1
F8 F -0.5950(5) -0.0305(3) 0.59871(14) 0.071(2) Uani 0.554(7) 1 d D U P B 1
F9 F -0.5178(4) 0.0958(4) 0.6137(2) 0.0715(19) Uani 0.554(7) 1 d D U P B 1
P4A P -0.5884(5) 0.0396(4) 0.6292(2) 0.0332(12) Uani 0.446(7) 1 d D U P B 2
F4A F -0.5495(7) -0.0198(6) 0.6680(2) 0.047(2) Uani 0.446(7) 1 d D U P B 2
F5A F -0.6625(5) 0.0886(6) 0.6615(3) 0.080(3) Uani 0.446(7) 1 d D U P B 2
F6A F -0.6746(5) -0.0276(4) 0.6181(3) 0.094(3) Uani 0.446(7) 1 d D U P B 2
F7A F -0.6252(8) 0.1003(4) 0.5906(2) 0.087(3) Uani 0.446(7) 1 d D U P B 2
F8A F -0.5131(6) -0.0099(3) 0.59746(17) 0.065(2) Uani 0.446(7) 1 d D U P B 2
F9A F -0.5010(4) 0.1073(3) 0.6402(3) 0.0592(19) Uani 0.446(7) 1 d D U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.392(4) . ?
C1 C6 1.393(4) . ?
C1 P1 1.835(3) . ?
C2 F1 1.360(3) . ?
C2 C3 1.373(4) . ?
C3 C4 1.389(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.382(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.390(4) . ?
C7 C12 1.392(4) . ?
C7 P1 1.845(3) . ?
C8 F2 1.362(3) . ?
C8 C9 1.377(4) . ?
C9 C10 1.386(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.388(4) . ?
C13 C18 1.401(4) . ?
C13 P1 1.840(3) . ?
C14 F3 1.366(4) . ?
C14 C15 1.370(4) . ?
C15 C16 1.379(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.384(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.386(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C23 1.412(5) . ?
C19 C20 1.420(5) . ?
C19 Fe1 2.096(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.406(5) . ?
C20 Fe1 2.083(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.417(5) . ?
C21 Fe1 2.083(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.396(5) . ?
C22 Fe1 2.087(3) . ?
C22 H22 0.9500 . ?
C23 Fe1 2.097(3) . ?
C23 H23 0.9500 . ?
C24 C29 1.520(11) . ?
C24 C25 1.5396(10) . ?
C24 P2 1.811(3) . ?
C24 H24 1.0000 . ?
C25 C26 1.5401(10) . ?
C25 P3 1.863(4) . ?
C25 H25 1.0000 . ?
C26 C27 1.5395(10) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.5391(10) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.5396(10) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C24A C29A 1.528(16) . ?
C24A C25A 1.5396(10) . ?
C24A H24A 1.0000 . ?
C25A C26A 1.5399(10) . ?
C25A H25A 1.0000 . ?
C26A C27A 1.5399(10) . ?
C26A H26C 0.9900 . ?
C26A H26D 0.9900 . ?
C27A C28A 1.5396(10) . ?
C27A H27C 0.9900 . ?
C27A H27D 0.9900 . ?
C28A C29A 1.5397(10) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
Fe1 P2 2.1880(9) . ?
Fe1 P3 2.1950(9) . ?
Fe1 P1 2.2195(8) . ?
P2 H2A 0.9900 . ?
P2 H2B 0.9900 . ?
P3 H3A 0.9900 . ?
P3 H3B 0.9900 . ?
P4 F9 1.562(5) . ?
P4 F8 1.570(5) . ?
P4 F5 1.571(6) . ?
P4 F6 1.571(5) . ?
P4 F4 1.577(6) . ?
P4 F7 1.582(6) . ?
P4A F6A 1.557(6) . ?
P4A F5A 1.570(6) . ?
P4A F8A 1.572(6) . ?
P4A F7A 1.574(7) . ?
P4A F9A 1.574(6) . ?
P4A F4A 1.575(7) . ?

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 C1 C6 115.9(3) . . ?
C2 C1 P1 123.4(2) . . ?
C6 C1 P1 120.7(2) . . ?
F1 C2 C3 117.3(3) . . ?
F1 C2 C1 118.7(3) . . ?
C3 C2 C1 124.0(3) . . ?
C2 C3 C4 118.3(3) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 119.8(3) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 120.3(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C1 121.6(3) . . ?
C5 C6 H6 119.2 . . ?
C1 C6 H6 119.2 . . ?
C8 C7 C12 115.9(3) . . ?
C8 C7 P1 120.9(2) . . ?
C12 C7 P1 123.0(2) . . ?
F2 C8 C9 116.8(3) . . ?
F2 C8 C7 118.9(3) . . ?
C9 C8 C7 124.3(3) . . ?
C8 C9 C10 117.8(3) . . ?
C8 C9 H9 121.1 . . ?
C10 C9 H9 121.1 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 121.2(3) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?
C14 C13 C18 115.7(3) . . ?
C14 C13 P1 120.1(2) . . ?
C18 C13 P1 124.1(2) . . ?
F3 C14 C15 117.4(3) . . ?
F3 C14 C13 117.8(3) . . ?
C15 C14 C13 124.8(3) . . ?
C14 C15 C16 118.1(3) . . ?
C14 C15 H15 120.9 . . ?
C16 C15 H15 120.9 . . ?
C15 C16 C17 119.7(3) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C16 C17 C18 121.0(3) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C17 C18 C13 120.7(3) . . ?
C17 C18 H18 119.7 . . ?
C13 C18 H18 119.7 . . ?
C23 C19 C20 107.2(3) . . ?
C23 C19 Fe1 70.4(2) . . ?
C20 C19 Fe1 69.6(2) . . ?
C23 C19 H19 126.4 . . ?
C20 C19 H19 126.4 . . ?
Fe1 C19 H19 125.2 . . ?
C21 C20 C19 108.2(3) . . ?
C21 C20 Fe1 70.3(2) . . ?
C19 C20 Fe1 70.6(2) . . ?
C21 C20 H20 125.9 . . ?
C19 C20 H20 125.9 . . ?
Fe1 C20 H20 124.8 . . ?
C20 C21 C22 107.8(3) . . ?
C20 C21 Fe1 70.3(2) . . ?
C22 C21 Fe1 70.3(2) . . ?
C20 C21 H21 126.1 . . ?
C22 C21 H21 126.1 . . ?
Fe1 C21 H21 124.9 . . ?
C23 C22 C21 108.1(3) . . ?
C23 C22 Fe1 70.89(19) . . ?
C21 C22 Fe1 69.98(18) . . ?
C23 C22 H22 126.0 . . ?
C21 C22 H22 126.0 . . ?
Fe1 C22 H22 124.8 . . ?
C22 C23 C19 108.8(3) . . ?
C22 C23 Fe1 70.12(19) . . ?
C19 C23 Fe1 70.29(19) . . ?
C22 C23 H23 125.6 . . ?
C19 C23 H23 125.6 . . ?
Fe1 C23 H23 125.6 . . ?
C29 C24 C25 110.4(5) . . ?
C29 C24 P2 118.1(4) . . ?
C25 C24 P2 108.7(3) . . ?
C29 C24 H24 106.3 . . ?
C25 C24 H24 106.3 . . ?
P2 C24 H24 106.3 . . ?
C24 C25 C26 107.8(3) . . ?
C24 C25 P3 110.4(3) . . ?
C26 C25 P3 119.2(3) . . ?
C24 C25 H25 106.2 . . ?
C26 C25 H25 106.2 . . ?
P3 C25 H25 106.2 . . ?
C27 C26 C25 109.0(3) . . ?
C27 C26 H26A 109.9 . . ?
C25 C26 H26A 109.9 . . ?
C27 C26 H26B 109.9 . . ?
C25 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
C28 C27 C26 110.2(3) . . ?
C28 C27 H27A 109.6 . . ?
C26 C27 H27A 109.6 . . ?
C28 C27 H27B 109.6 . . ?
C26 C27 H27B 109.6 . . ?
H27A C27 H27B 108.1 . . ?
C27 C28 C29 109.5(3) . . ?
C27 C28 H28A 109.8 . . ?
C29 C28 H28A 109.8 . . ?
C27 C28 H28B 109.8 . . ?
C29 C28 H28B 109.8 . . ?
H28A C28 H28B 108.2 . . ?
C24 C29 C28 109.1(6) . . ?
C24 C29 H29A 109.9 . . ?
C28 C29 H29A 109.9 . . ?
C24 C29 H29B 109.9 . . ?
C28 C29 H29B 109.9 . . ?
H29A C29 H29B 108.3 . . ?
C29A C24A C25A 107.0(6) . . ?
C29A C24A H24A 105.7 . . ?
C25A C24A H24A 105.7 . . ?
C24A C25A C26A 108.7(3) . . ?
C24A C25A H25A 109.9 . . ?
C26A C25A H25A 109.9 . . ?
C25A C26A C27A 108.3(3) . . ?
C25A C26A H26C 110.0 . . ?
C27A C26A H26C 110.0 . . ?
C25A C26A H26D 110.0 . . ?
C27A C26A H26D 110.0 . . ?
H26C C26A H26D 108.4 . . ?
C28A C27A C26A 109.0(3) . . ?
C28A C27A H27C 109.9 . . ?
C26A C27A H27C 109.9 . . ?
C28A C27A H27D 109.9 . . ?
C26A C27A H27D 109.9 . . ?
H27C C27A H27D 108.3 . . ?
C27A C28A C29A 109.2(3) . . ?
C27A C28A H28C 109.8 . . ?
C29A C28A H28C 109.8 . . ?
C27A C28A H28D 109.8 . . ?
C29A C28A H28D 109.8 . . ?
H28C C28A H28D 108.3 . . ?
C24A C29A C28A 109.4(8) . . ?
C24A C29A H29C 109.8 . . ?
C28A C29A H29C 109.8 . . ?
C24A C29A H29D 109.8 . . ?
C28A C29A H29D 109.8 . . ?
H29C C29A H29D 108.2 . . ?
C21 Fe1 C20 39.46(15) . . ?
C21 Fe1 C22 39.72(14) . . ?
C20 Fe1 C22 66.32(14) . . ?
C21 Fe1 C19 66.45(15) . . ?
C20 Fe1 C19 39.73(15) . . ?
C22 Fe1 C19 66.16(15) . . ?
C21 Fe1 C23 66.01(15) . . ?
C20 Fe1 C23 66.09(14) . . ?
C22 Fe1 C23 38.99(15) . . ?
C19 Fe1 C23 39.36(14) . . ?
C21 Fe1 P2 147.86(10) . . ?
C20 Fe1 P2 147.96(12) . . ?
C22 Fe1 P2 108.28(11) . . ?
C19 Fe1 P2 108.35(11) . . ?
C23 Fe1 P2 89.72(11) . . ?
C21 Fe1 P3 91.50(12) . . ?
C20 Fe1 P3 125.63(12) . . ?
C22 Fe1 P3 90.84(11) . . ?
C19 Fe1 P3 155.91(11) . . ?
C23 Fe1 P3 123.91(11) . . ?
P2 Fe1 P3 84.87(3) . . ?
C21 Fe1 P1 117.77(10) . . ?
C20 Fe1 P1 90.20(10) . . ?
C22 Fe1 P1 155.97(11) . . ?
C19 Fe1 P1 99.45(10) . . ?
C23 Fe1 P1 136.59(11) . . ?
P2 Fe1 P1 94.29(4) . . ?
P3 Fe1 P1 99.50(3) . . ?
C1 P1 C13 101.32(14) . . ?
C1 P1 C7 101.93(13) . . ?
C13 P1 C7 102.17(13) . . ?
C1 P1 Fe1 117.21(10) . . ?
C13 P1 Fe1 119.08(10) . . ?
C7 P1 Fe1 112.68(10) . . ?
C24 P2 Fe1 114.08(18) . . ?
C24 P2 H2A 108.7 . . ?
Fe1 P2 H2A 108.7 . . ?
C24 P2 H2B 108.7 . . ?
Fe1 P2 H2B 108.7 . . ?
H2A P2 H2B 107.6 . . ?
C25 P3 Fe1 111.23(15) . . ?
C25 P3 H3A 109.4 . . ?
Fe1 P3 H3A 109.4 . . ?
C25 P3 H3B 109.4 . . ?
Fe1 P3 H3B 109.4 . . ?
H3A P3 H3B 108.0 . . ?
F9 P4 F8 90.4(4) . . ?
F9 P4 F5 91.0(4) . . ?
F8 P4 F5 178.6(5) . . ?
F9 P4 F6 179.5(5) . . ?
F8 P4 F6 90.1(4) . . ?
F5 P4 F6 88.6(3) . . ?
F9 P4 F4 90.3(4) . . ?
F8 P4 F4 90.0(4) . . ?
F5 P4 F4 90.2(4) . . ?
F6 P4 F4 89.9(4) . . ?
F9 P4 F7 90.1(3) . . ?
F8 P4 F7 89.6(3) . . ?
F5 P4 F7 90.1(4) . . ?
F6 P4 F7 89.7(3) . . ?
F4 P4 F7 179.4(5) . . ?
F6A P4A F5A 90.5(5) . . ?
F6A P4A F8A 90.0(4) . . ?
F5A P4A F8A 179.1(5) . . ?
F6A P4A F7A 90.3(4) . . ?
F5A P4A F7A 90.2(4) . . ?
F8A P4A F7A 90.6(4) . . ?
F6A P4A F9A 179.7(6) . . ?
F5A P4A F9A 89.8(4) . . ?
F8A P4A F9A 89.8(4) . . ?
F7A P4A F9A 89.6(4) . . ?
F6A P4A F4A 91.0(5) . . ?
F5A P4A F4A 89.9(4) . . ?
F8A P4A F4A 89.3(4) . . ?
F7A P4A F4A 178.7(6) . . ?
F9A P4A F4A 89.1(4) . . ?

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.066

_shelxl_version_number           2013-4

_database_code_depnum_ccdc_archive 'CCDC 1015699'
