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

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#
#                 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.
#
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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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#  from this site to visualise CIF-encoded structures and 
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data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H19 N O5 P Re'
_chemical_melting_point          ?

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         654.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_int_tables_number      14


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

_cell_length_a                   9.9334(15)
_cell_length_b                   29.643(4)
_cell_length_c                   8.6911(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.9850(10)
_cell_angle_gamma                90.00
_cell_volume                     2389.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9974
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.5
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_absorpt_coefficient_mu    5.192
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            27882
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         27.49
_reflns_number_total             5484
_reflns_number_gt                4914
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0128P)²+1.9811P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5484
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0429
_refine_ls_wR_factor_gt          0.0414
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.574112(10) 0.080567(3) 0.708363(12) 0.01669(4) Uani 1 1 d . . .
P1 P 0.40469(7) 0.12455(2) 0.80450(8) 0.01615(13) Uani 1 1 d . . .
O1 O 0.66363(19) 0.14431(6) 0.6783(2) 0.0230(4) Uani 1 1 d . . .
O2 O 0.8428(2) 0.19349(7) 0.7895(3) 0.0353(5) Uani 1 1 d . . .
O3 O 0.3329(2) 0.07512(8) 0.3686(2) 0.0381(5) Uani 1 1 d . . .
O4 O 0.4786(2) -0.00968(7) 0.8080(3) 0.0332(5) Uani 1 1 d . . .
O5 O 0.7473(2) 0.02476(8) 0.5430(3) 0.0425(6) Uani 1 1 d . . .
N1 N 0.7451(2) 0.09396(7) 0.9466(2) 0.0171(4) Uani 1 1 d . . .
C1 C 0.7786(3) 0.06831(9) 1.0837(3) 0.0227(6) Uani 1 1 d . . .
H1 H 0.7319 0.0401 1.0780 0.027 Uiso 1 1 calc R . .
C2 C 0.8792(3) 0.08224(10) 1.2318(3) 0.0273(6) Uani 1 1 d . . .
H2 H 0.8998 0.0639 1.3270 0.033 Uiso 1 1 calc R . .
C3 C 0.9497(3) 0.12285(10) 1.2415(4) 0.0315(7) Uani 1 1 d . . .
H3 H 1.0186 0.1329 1.3430 0.038 Uiso 1 1 calc R . .
C4 C 0.9181(3) 0.14852(10) 1.1008(3) 0.0277(6) Uani 1 1 d . . .
H4 H 0.9659 0.1764 1.1035 0.033 Uiso 1 1 calc R . .
C5 C 0.8157(3) 0.13319(9) 0.9556(3) 0.0200(5) Uani 1 1 d . . .
C6 C 0.7740(3) 0.16006(9) 0.7973(3) 0.0225(6) Uani 1 1 d . . .
C7 C 0.4933(3) 0.15691(9) 0.9909(3) 0.0180(5) Uani 1 1 d . . .
C8 C 0.5233(3) 0.20264(9) 0.9783(3) 0.0248(6) Uani 1 1 d . . .
H8 H 0.4881 0.2171 0.8739 0.030 Uiso 1 1 calc R . .
C9 C 0.6043(3) 0.22697(10) 1.1173(4) 0.0349(7) Uani 1 1 d . . .
H9 H 0.6247 0.2579 1.1079 0.042 Uiso 1 1 calc R . .
C10 C 0.6552(3) 0.20591(11) 1.2697(4) 0.0347(7) Uani 1 1 d . . .
H10 H 0.7106 0.2225 1.3648 0.042 Uiso 1 1 calc R . .
C11 C 0.6257(3) 0.16065(11) 1.2840(3) 0.0311(7) Uani 1 1 d . . .
H11 H 0.6593 0.1465 1.3890 0.037 Uiso 1 1 calc R . .
C12 C 0.5472(3) 0.13603(10) 1.1450(3) 0.0237(6) Uani 1 1 d . . .
H12 H 0.5300 0.1048 1.1548 0.028 Uiso 1 1 calc R . .
C13 C 0.2902(3) 0.16543(9) 0.6580(3) 0.0192(5) Uani 1 1 d . . .
C14 C 0.3291(3) 0.18289(9) 0.5306(3) 0.0262(6) Uani 1 1 d . . .
H14 H 0.4160 0.1734 0.5182 0.031 Uiso 1 1 calc R . .
C15 C 0.2401(3) 0.21428(10) 0.4216(4) 0.0319(7) Uani 1 1 d . . .
H15 H 0.2670 0.2263 0.3354 0.038 Uiso 1 1 calc R . .
C16 C 0.1126(3) 0.22814(10) 0.4380(4) 0.0297(7) Uani 1 1 d . . .
H16 H 0.0523 0.2495 0.3633 0.036 Uiso 1 1 calc R . .
C17 C 0.0739(3) 0.21069(9) 0.5641(3) 0.0272(6) Uani 1 1 d . . .
H17 H -0.0135 0.2201 0.5755 0.033 Uiso 1 1 calc R . .
C18 C 0.1610(3) 0.17977(9) 0.6732(3) 0.0228(6) Uani 1 1 d . . .
H18 H 0.1334 0.1681 0.7592 0.027 Uiso 1 1 calc R . .
C19 C 0.2675(3) 0.08953(8) 0.8387(3) 0.0187(5) Uani 1 1 d . . .
C20 C 0.1889(3) 0.06128(9) 0.7097(3) 0.0223(6) Uani 1 1 d . . .
H20 H 0.2137 0.0594 0.6140 0.027 Uiso 1 1 calc R . .
C21 C 0.0752(3) 0.03604(10) 0.7193(3) 0.0249(6) Uani 1 1 d . . .
H21 H 0.0204 0.0177 0.6289 0.030 Uiso 1 1 calc R . .
C22 C 0.0410(3) 0.03740(10) 0.8601(3) 0.0251(6) Uani 1 1 d . . .
H22 H -0.0366 0.0198 0.8668 0.030 Uiso 1 1 calc R . .
C23 C 0.1193(3) 0.06430(10) 0.9903(3) 0.0262(6) Uani 1 1 d . . .
H23 H 0.0972 0.0646 1.0880 0.031 Uiso 1 1 calc R . .
C24 C 0.2313(3) 0.09115(9) 0.9796(3) 0.0237(6) Uani 1 1 d . . .
H24 H 0.2828 0.1105 1.0683 0.028 Uiso 1 1 calc R . .
C25 C 0.4237(3) 0.07717(9) 0.4965(3) 0.0237(6) Uani 1 1 d . . .
C26 C 0.5115(3) 0.02437(9) 0.7675(3) 0.0222(6) Uani 1 1 d . . .
C27 C 0.6913(3) 0.04623(10) 0.6120(3) 0.0261(6) 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
Re1 C26 1.912(3) . ?
Re1 C25 1.914(3) . ?
Re1 C27 1.947(3) . ?
Re1 O1 2.1439(18) . ?
Re1 N1 2.193(2) . ?
Re1 P1 2.4975(7) . ?
P1 C7 1.816(3) . ?
P1 C19 1.820(3) . ?
P1 C13 1.829(3) . ?
O1 C6 1.295(3) . ?
O2 C6 1.219(3) . ?
O3 C25 1.155(3) . ?
O4 C26 1.154(3) . ?
O5 C27 1.145(3) . ?
N1 C5 1.346(3) . ?
N1 C1 1.351(3) . ?
C1 C2 1.380(4) . ?
C1 H1 0.9500 . ?
C2 C3 1.380(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.513(4) . ?
C7 C12 1.397(4) . ?
C7 C8 1.401(4) . ?
C8 C9 1.390(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.388(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.387(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.396(4) . ?
C13 C18 1.402(4) . ?
C14 C15 1.395(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.379(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.394(4) . ?
C19 C24 1.394(4) . ?
C20 C21 1.382(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.375(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.398(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?

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
C26 Re1 C25 89.76(11) . . ?
C26 Re1 C27 87.84(11) . . ?
C25 Re1 C27 86.53(11) . . ?
C26 Re1 O1 171.84(9) . . ?
C25 Re1 O1 98.28(10) . . ?
C27 Re1 O1 94.03(10) . . ?
C26 Re1 N1 96.92(9) . . ?
C25 Re1 N1 172.57(10) . . ?
C27 Re1 N1 96.92(10) . . ?
O1 Re1 N1 74.98(7) . . ?
C26 Re1 P1 92.40(8) . . ?
C25 Re1 P1 87.83(8) . . ?
C27 Re1 P1 174.35(8) . . ?
O1 Re1 P1 86.52(5) . . ?
N1 Re1 P1 88.65(6) . . ?
C7 P1 C19 107.89(12) . . ?
C7 P1 C13 104.65(12) . . ?
C19 P1 C13 100.15(12) . . ?
C7 P1 Re1 113.89(8) . . ?
C19 P1 Re1 113.00(9) . . ?
C13 P1 Re1 116.00(9) . . ?
C6 O1 Re1 119.33(16) . . ?
C5 N1 C1 118.5(2) . . ?
C5 N1 Re1 114.99(16) . . ?
C1 N1 Re1 126.43(18) . . ?
N1 C1 C2 121.5(3) . . ?
N1 C1 H1 119.3 . . ?
C2 C1 H1 119.3 . . ?
C1 C2 C3 120.0(3) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 118.6(3) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 119.2(3) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 122.3(2) . . ?
N1 C5 C6 115.8(2) . . ?
C4 C5 C6 121.9(2) . . ?
O2 C6 O1 125.4(3) . . ?
O2 C6 C5 120.1(2) . . ?
O1 C6 C5 114.4(2) . . ?
C12 C7 C8 119.0(2) . . ?
C12 C7 P1 121.2(2) . . ?
C8 C7 P1 119.34(19) . . ?
C9 C8 C7 120.5(3) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C8 119.8(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 120.3(3) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C7 120.3(3) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
C14 C13 C18 119.0(2) . . ?
C14 C13 P1 121.2(2) . . ?
C18 C13 P1 119.8(2) . . ?
C15 C14 C13 119.9(3) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C16 C15 C14 120.5(3) . . ?
C16 C15 H15 119.7 . . ?
C14 C15 H15 119.7 . . ?
C17 C16 C15 119.6(3) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C18 C17 C16 120.6(3) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C17 C18 C13 120.5(3) . . ?
C17 C18 H18 119.8 . . ?
C13 C18 H18 119.8 . . ?
C20 C19 C24 118.8(2) . . ?
C20 C19 P1 116.58(19) . . ?
C24 C19 P1 124.6(2) . . ?
C21 C20 C19 120.7(2) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C20 C21 C22 120.2(3) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C23 C22 C21 119.9(3) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.3(3) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C19 C24 C23 120.0(3) . . ?
C19 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
O3 C25 Re1 180.0(3) . . ?
O4 C26 Re1 177.4(2) . . ?
O5 C27 Re1 173.0(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C26 Re1 P1 C7 109.44(12) . . . . ?
C25 Re1 P1 C7 -160.90(12) . . . . ?
C27 Re1 P1 C7 -158.3(9) . . . . ?
O1 Re1 P1 C7 -62.47(11) . . . . ?
N1 Re1 P1 C7 12.56(11) . . . . ?
C26 Re1 P1 C19 -14.14(12) . . . . ?
C25 Re1 P1 C19 75.53(12) . . . . ?
C27 Re1 P1 C19 78.2(9) . . . . ?
O1 Re1 P1 C19 173.96(10) . . . . ?
N1 Re1 P1 C19 -111.01(11) . . . . ?
C26 Re1 P1 C13 -128.98(12) . . . . ?
C25 Re1 P1 C13 -39.32(12) . . . . ?
C27 Re1 P1 C13 -36.7(9) . . . . ?
O1 Re1 P1 C13 59.11(10) . . . . ?
N1 Re1 P1 C13 134.14(11) . . . . ?
C26 Re1 O1 C6 11.0(7) . . . . ?
C25 Re1 O1 C6 -179.1(2) . . . . ?
C27 Re1 O1 C6 -92.1(2) . . . . ?
N1 Re1 O1 C6 4.02(18) . . . . ?
P1 Re1 O1 C6 93.56(19) . . . . ?
C26 Re1 N1 C5 -178.41(19) . . . . ?
C25 Re1 N1 C5 -24.4(8) . . . . ?
C27 Re1 N1 C5 92.94(19) . . . . ?
O1 Re1 N1 C5 0.61(17) . . . . ?
P1 Re1 N1 C5 -86.15(17) . . . . ?
C26 Re1 N1 C1 -2.6(2) . . . . ?
C25 Re1 N1 C1 151.4(7) . . . . ?
C27 Re1 N1 C1 -91.2(2) . . . . ?
O1 Re1 N1 C1 176.4(2) . . . . ?
P1 Re1 N1 C1 89.7(2) . . . . ?
C5 N1 C1 C2 2.1(4) . . . . ?
Re1 N1 C1 C2 -173.5(2) . . . . ?
N1 C1 C2 C3 -1.0(4) . . . . ?
C1 C2 C3 C4 -0.5(4) . . . . ?
C2 C3 C4 C5 0.9(4) . . . . ?
C1 N1 C5 C4 -1.7(4) . . . . ?
Re1 N1 C5 C4 174.4(2) . . . . ?
C1 N1 C5 C6 179.4(2) . . . . ?
Re1 N1 C5 C6 -4.4(3) . . . . ?
C3 C4 C5 N1 0.2(4) . . . . ?
C3 C4 C5 C6 179.0(3) . . . . ?
Re1 O1 C6 O2 172.6(2) . . . . ?
Re1 O1 C6 C5 -7.4(3) . . . . ?
N1 C5 C6 O2 -172.2(3) . . . . ?
C4 C5 C6 O2 8.9(4) . . . . ?
N1 C5 C6 O1 7.8(3) . . . . ?
C4 C5 C6 O1 -171.1(2) . . . . ?
C19 P1 C7 C12 50.6(2) . . . . ?
C13 P1 C7 C12 156.6(2) . . . . ?
Re1 P1 C7 C12 -75.7(2) . . . . ?
C19 P1 C7 C8 -137.0(2) . . . . ?
C13 P1 C7 C8 -31.0(2) . . . . ?
Re1 P1 C7 C8 96.7(2) . . . . ?
C12 C7 C8 C9 -0.6(4) . . . . ?
P1 C7 C8 C9 -173.2(2) . . . . ?
C7 C8 C9 C10 -0.3(4) . . . . ?
C8 C9 C10 C11 0.0(5) . . . . ?
C9 C10 C11 C12 1.2(5) . . . . ?
C10 C11 C12 C7 -2.1(4) . . . . ?
C8 C7 C12 C11 1.9(4) . . . . ?
P1 C7 C12 C11 174.2(2) . . . . ?
C7 P1 C13 C14 103.8(2) . . . . ?
C19 P1 C13 C14 -144.5(2) . . . . ?
Re1 P1 C13 C14 -22.6(2) . . . . ?
C7 P1 C13 C18 -76.0(2) . . . . ?
C19 P1 C13 C18 35.6(2) . . . . ?
Re1 P1 C13 C18 157.57(18) . . . . ?
C18 C13 C14 C15 0.4(4) . . . . ?
P1 C13 C14 C15 -179.5(2) . . . . ?
C13 C14 C15 C16 -0.4(4) . . . . ?
C14 C15 C16 C17 0.2(4) . . . . ?
C15 C16 C17 C18 0.1(4) . . . . ?
C16 C17 C18 C13 -0.1(4) . . . . ?
C14 C13 C18 C17 -0.1(4) . . . . ?
P1 C13 C18 C17 179.7(2) . . . . ?
C7 P1 C19 C20 -178.8(2) . . . . ?
C13 P1 C19 C20 72.1(2) . . . . ?
Re1 P1 C19 C20 -51.9(2) . . . . ?
C7 P1 C19 C24 5.1(3) . . . . ?
C13 P1 C19 C24 -104.1(2) . . . . ?
Re1 P1 C19 C24 131.9(2) . . . . ?
C24 C19 C20 C21 1.4(4) . . . . ?
P1 C19 C20 C21 -175.0(2) . . . . ?
C19 C20 C21 C22 -2.1(4) . . . . ?
C20 C21 C22 C23 0.6(4) . . . . ?
C21 C22 C23 C24 1.6(4) . . . . ?
C20 C19 C24 C23 0.8(4) . . . . ?
P1 C19 C24 C23 176.9(2) . . . . ?
C22 C23 C24 C19 -2.3(4) . . . . ?
C26 Re1 C25 O3 30(100) . . . . ?
C27 Re1 C25 O3 118(100) . . . . ?
O1 Re1 C25 O3 -148(100) . . . . ?
N1 Re1 C25 O3 -124(100) . . . . ?
P1 Re1 C25 O3 -62(100) . . . . ?
C25 Re1 C26 O4 164(5) . . . . ?
C27 Re1 C26 O4 77(5) . . . . ?
O1 Re1 C26 O4 -26(6) . . . . ?
N1 Re1 C26 O4 -20(5) . . . . ?
P1 Re1 C26 O4 -108(5) . . . . ?
C26 Re1 C27 O5 71(2) . . . . ?
C25 Re1 C27 O5 -19(2) . . . . ?
O1 Re1 C27 O5 -117(2) . . . . ?
N1 Re1 C27 O5 167(2) . . . . ?
P1 Re1 C27 O5 -22(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.088
_database_code_depnum_ccdc_archive 'CCDC 983202'
#######################################################################
#
#                 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_3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H36 Cl6 N O4 P2 Re'
_chemical_melting_point          ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         1127.60

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'
Cl Cl 0.1484 0.1585 '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'
Re Re -1.0185 7.2310 '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'
_symmetry_int_tables_number      2


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

_cell_length_a                   10.8612(3)
_cell_length_b                   14.6446(5)
_cell_length_c                   15.5216(5)
_cell_angle_alpha                77.9590(10)
_cell_angle_beta                 82.0390(10)
_cell_angle_gamma                72.2150(10)
_cell_volume                     2291.70(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9885
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.6
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1116
_exptl_absorpt_coefficient_mu    3.115
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.40
_exptl_absorpt_correction_T_max  0.51
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            21139
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.82
_diffrn_reflns_theta_max         27.61
_reflns_number_total             10429
_reflns_number_gt                9683
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0261P)²+1.3662P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10429
_refine_ls_number_parameters     541
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0569
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.272614(9) 0.353801(7) 0.648618(6) 0.01655(3) Uani 1 1 d . . .
Cl1 Cl 0.44791(17) 0.08084(9) 1.09615(8) 0.0944(5) Uani 1 1 d . . .
Cl2 Cl 0.34203(10) 0.28766(8) 1.04118(6) 0.0566(2) Uani 1 1 d . . .
Cl3 Cl 0.57724(10) 0.18452(9) 0.95053(9) 0.0721(3) Uani 1 1 d . . .
Cl4 Cl 0.10109(16) 0.01522(8) 1.08507(10) 0.1012(5) Uani 1 1 d . . .
Cl5 Cl -0.13019(9) 0.17033(8) 1.04536(6) 0.0583(2) Uani 1 1 d . . .
Cl6 Cl 0.05472(11) 0.19335(7) 1.14956(6) 0.0560(2) Uani 1 1 d . . .
P1 P 0.37510(6) 0.20817(4) 0.58598(4) 0.01754(12) Uani 1 1 d . . .
P2 P 0.18205(6) 0.49118(4) 0.72365(4) 0.01800(12) Uani 1 1 d . . .
O2 O 0.29768(17) 0.26537(13) 0.77934(11) 0.0213(4) Uani 1 1 d . . .
O3 O 0.2098(2) 0.17910(15) 0.89309(12) 0.0327(5) Uani 1 1 d . . .
O4 O 0.1840(2) 0.47371(15) 0.47135(13) 0.0381(5) Uani 1 1 d . . .
O5 O 0.5313(2) 0.40324(17) 0.60595(14) 0.0395(5) Uani 1 1 d . . .
N1 N 0.0948(2) 0.31068(15) 0.68751(13) 0.0193(4) Uani 1 1 d . . .
C1 C 0.2069(3) 0.22925(18) 0.81850(16) 0.0226(5) Uani 1 1 d . . .
C2 C 0.0897(3) 0.25328(19) 0.76790(16) 0.0223(5) Uani 1 1 d . . .
C3 C -0.0180(3) 0.2213(2) 0.80054(18) 0.0340(7) Uani 1 1 d . . .
H3 H -0.0186 0.1795 0.8563 0.041 Uiso 1 1 calc R . .
C4 C -0.1248(3) 0.2504(2) 0.7515(2) 0.0376(7) Uani 1 1 d . . .
H4 H -0.1999 0.2299 0.7733 0.045 Uiso 1 1 calc R . .
C5 C -0.1201(3) 0.3096(2) 0.67046(19) 0.0321(6) Uani 1 1 d . . .
H5 H -0.1925 0.3311 0.6358 0.039 Uiso 1 1 calc R . .
C6 C -0.0093(3) 0.3375(2) 0.63989(17) 0.0257(5) Uani 1 1 d . . .
H6 H -0.0062 0.3771 0.5832 0.031 Uiso 1 1 calc R . .
C7 C 0.2963(2) 0.11080(18) 0.62058(16) 0.0214(5) Uani 1 1 d . . .
C8 C 0.1720(3) 0.1254(2) 0.59457(16) 0.0245(5) Uani 1 1 d . . .
H8 H 0.1336 0.1824 0.5544 0.029 Uiso 1 1 calc R . .
C9 C 0.1051(3) 0.0572(2) 0.62719(18) 0.0335(6) Uani 1 1 d . . .
H9 H 0.0205 0.0683 0.6098 0.040 Uiso 1 1 calc R . .
C10 C 0.1599(3) -0.0269(2) 0.6848(2) 0.0421(8) Uani 1 1 d . . .
H10 H 0.1133 -0.0734 0.7069 0.051 Uiso 1 1 calc R . .
C11 C 0.2823(4) -0.0427(3) 0.7099(3) 0.0532(10) Uani 1 1 d . . .
H11 H 0.3210 -0.1008 0.7487 0.064 Uiso 1 1 calc R . .
C12 C 0.3501(3) 0.0262(2) 0.6786(2) 0.0398(7) Uani 1 1 d . . .
H12 H 0.4340 0.0150 0.6972 0.048 Uiso 1 1 calc R . .
C13 C 0.3929(2) 0.22778(18) 0.46537(15) 0.0205(5) Uani 1 1 d . . .
C14 C 0.4411(3) 0.3048(2) 0.42131(17) 0.0275(6) Uani 1 1 d . . .
H14 H 0.4642 0.3440 0.4543 0.033 Uiso 1 1 calc R . .
C15 C 0.4554(3) 0.3244(2) 0.32963(18) 0.0348(7) Uani 1 1 d . . .
H15 H 0.4895 0.3763 0.3002 0.042 Uiso 1 1 calc R . .
C16 C 0.4204(3) 0.2689(2) 0.28145(18) 0.0376(7) Uani 1 1 d . . .
H16 H 0.4288 0.2832 0.2187 0.045 Uiso 1 1 calc R . .
C17 C 0.3730(3) 0.1925(2) 0.32374(18) 0.0369(7) Uani 1 1 d . . .
H17 H 0.3487 0.1545 0.2901 0.044 Uiso 1 1 calc R . .
C18 C 0.3608(3) 0.1709(2) 0.41560(17) 0.0284(6) Uani 1 1 d . . .
H18 H 0.3303 0.1171 0.4444 0.034 Uiso 1 1 calc R . .
C19 C 0.5397(2) 0.14415(17) 0.61681(16) 0.0197(5) Uani 1 1 d . . .
C20 C 0.5690(3) 0.1405(2) 0.70263(17) 0.0266(5) Uani 1 1 d . . .
H20 H 0.5073 0.1779 0.7409 0.032 Uiso 1 1 calc R . .
C21 C 0.6877(3) 0.0827(2) 0.73214(18) 0.0296(6) Uani 1 1 d . . .
H21 H 0.7061 0.0796 0.7909 0.036 Uiso 1 1 calc R . .
C22 C 0.7792(3) 0.02953(19) 0.67659(19) 0.0286(6) Uani 1 1 d . . .
H22 H 0.8601 -0.0103 0.6972 0.034 Uiso 1 1 calc R . .
C23 C 0.7527(3) 0.03452(19) 0.59074(19) 0.0282(6) Uani 1 1 d . . .
H23 H 0.8164 -0.0009 0.5521 0.034 Uiso 1 1 calc R . .
C24 C 0.6335(2) 0.09100(18) 0.56076(17) 0.0230(5) Uani 1 1 d . . .
H24 H 0.6156 0.0935 0.5020 0.028 Uiso 1 1 calc R . .
C25 C 0.0402(2) 0.48145(18) 0.79868(16) 0.0207(5) Uani 1 1 d . . .
C26 C -0.0804(3) 0.50010(19) 0.76586(17) 0.0253(5) Uani 1 1 d . . .
H26 H -0.0906 0.5245 0.7048 0.030 Uiso 1 1 calc R . .
C27 C -0.1849(3) 0.4832(2) 0.82197(19) 0.0325(6) Uani 1 1 d . . .
H27 H -0.2669 0.4973 0.7995 0.039 Uiso 1 1 calc R . .
C28 C -0.1702(3) 0.4460(2) 0.91045(19) 0.0354(7) Uani 1 1 d . . .
H28 H -0.2423 0.4346 0.9486 0.042 Uiso 1 1 calc R . .
C29 C -0.0513(3) 0.4252(2) 0.94381(18) 0.0314(6) Uani 1 1 d . . .
H29 H -0.0414 0.3985 1.0046 0.038 Uiso 1 1 calc R . .
C30 C 0.0536(3) 0.44325(19) 0.88856(16) 0.0252(5) Uani 1 1 d . . .
H30 H 0.1351 0.4296 0.9118 0.030 Uiso 1 1 calc R . .
C31 C 0.1341(2) 0.61201(18) 0.65481(16) 0.0208(5) Uani 1 1 d . . .
C32 C 0.0206(3) 0.68374(19) 0.67125(17) 0.0266(5) Uani 1 1 d . . .
H32 H -0.0424 0.6688 0.7164 0.032 Uiso 1 1 calc R . .
C33 C -0.0016(3) 0.7770(2) 0.6224(2) 0.0334(6) Uani 1 1 d . . .
H33 H -0.0802 0.8254 0.6338 0.040 Uiso 1 1 calc R . .
C34 C 0.0895(3) 0.8000(2) 0.55733(18) 0.0332(6) Uani 1 1 d . . .
H34 H 0.0749 0.8645 0.5250 0.040 Uiso 1 1 calc R . .
C35 C 0.2027(3) 0.7287(2) 0.53922(18) 0.0325(6) Uani 1 1 d . . .
H35 H 0.2653 0.7442 0.4940 0.039 Uiso 1 1 calc R . .
C36 C 0.2243(3) 0.6352(2) 0.58678(17) 0.0269(6) Uani 1 1 d . . .
H36 H 0.3010 0.5862 0.5732 0.032 Uiso 1 1 calc R . .
C37 C 0.2915(2) 0.51117(19) 0.79377(15) 0.0209(5) Uani 1 1 d . . .
C38 C 0.2675(3) 0.6018(2) 0.81855(17) 0.0276(6) Uani 1 1 d . . .
H38 H 0.1918 0.6526 0.8017 0.033 Uiso 1 1 calc R . .
C39 C 0.3535(3) 0.6179(2) 0.86761(18) 0.0303(6) Uani 1 1 d . . .
H39 H 0.3364 0.6797 0.8844 0.036 Uiso 1 1 calc R . .
C40 C 0.4642(3) 0.5447(2) 0.89236(16) 0.0285(6) Uani 1 1 d . . .
H40 H 0.5241 0.5566 0.9247 0.034 Uiso 1 1 calc R . .
C41 C 0.4873(3) 0.4542(2) 0.86993(18) 0.0310(6) Uani 1 1 d . . .
H41 H 0.5621 0.4032 0.8883 0.037 Uiso 1 1 calc R . .
C42 C 0.4015(3) 0.4373(2) 0.82053(17) 0.0261(5) Uani 1 1 d . . .
H42 H 0.4182 0.3750 0.8050 0.031 Uiso 1 1 calc R . .
C43 C 0.2206(3) 0.42864(19) 0.53847(17) 0.0244(5) Uani 1 1 d . . .
C44 C 0.4327(2) 0.38464(19) 0.62298(16) 0.0234(5) Uani 1 1 d . . .
C45 C 0.4262(4) 0.1769(3) 1.0058(2) 0.0464(8) Uani 1 1 d . . .
H45 H 0.3737 0.1647 0.9636 0.056 Uiso 1 1 calc R . .
C46 C 0.0348(3) 0.1404(2) 1.06273(19) 0.0393(7) Uani 1 1 d . . .
H46 H 0.0814 0.1669 1.0076 0.047 Uiso 1 1 calc R . .


_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
Re1 C43 1.884(3) . ?
Re1 C44 1.897(3) . ?
Re1 O2 2.1701(16) . ?
Re1 N1 2.181(2) . ?
Re1 P2 2.4130(6) . ?
Re1 P1 2.4182(6) . ?
Cl1 C45 1.752(4) . ?
Cl2 C45 1.759(4) . ?
Cl3 C45 1.767(4) . ?
Cl4 C46 1.731(3) . ?
Cl5 C46 1.756(3) . ?
Cl6 C46 1.756(3) . ?
P1 C19 1.825(3) . ?
P1 C13 1.826(2) . ?
P1 C7 1.831(2) . ?
P2 C25 1.822(2) . ?
P2 C31 1.829(2) . ?
P2 C37 1.840(3) . ?
O2 C1 1.281(3) . ?
O3 C1 1.234(3) . ?
O4 C43 1.161(3) . ?
O5 C44 1.167(3) . ?
N1 C6 1.348(3) . ?
N1 C2 1.356(3) . ?
C1 C2 1.500(4) . ?
C2 C3 1.384(4) . ?
C3 C4 1.383(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.388(4) . ?
C7 C8 1.404(4) . ?
C8 C9 1.383(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.383(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.375(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.394(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.390(4) . ?
C13 C14 1.398(3) . ?
C14 C15 1.388(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.374(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.391(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.397(3) . ?
C19 C20 1.399(4) . ?
C20 C21 1.387(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.381(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.384(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.389(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.399(4) . ?
C25 C30 1.400(3) . ?
C26 C27 1.384(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.380(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.381(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.386(4) . ?
C31 C36 1.399(3) . ?
C32 C33 1.384(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.378(4) . ?
C33 H33 0.9500 . ?
C34 C35 1.386(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.380(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.390(4) . ?
C37 C38 1.397(4) . ?
C38 C39 1.384(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.382(4) . ?
C39 H39 0.9500 . ?
C40 C41 1.380(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.391(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C45 H45 1.0000 . ?
C46 H46 1.0000 . ?

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
C43 Re1 C44 88.96(11) . . ?
C43 Re1 O2 169.83(9) . . ?
C44 Re1 O2 101.16(9) . . ?
C43 Re1 N1 95.56(9) . . ?
C44 Re1 N1 175.46(9) . . ?
O2 Re1 N1 74.33(7) . . ?
C43 Re1 P2 92.73(8) . . ?
C44 Re1 P2 90.69(8) . . ?
O2 Re1 P2 86.16(5) . . ?
N1 Re1 P2 89.55(5) . . ?
C43 Re1 P1 92.67(8) . . ?
C44 Re1 P1 87.88(8) . . ?
O2 Re1 P1 88.79(5) . . ?
N1 Re1 P1 91.46(6) . . ?
P2 Re1 P1 174.39(2) . . ?
C19 P1 C13 103.43(11) . . ?
C19 P1 C7 101.05(11) . . ?
C13 P1 C7 105.87(11) . . ?
C19 P1 Re1 114.81(8) . . ?
C13 P1 Re1 114.84(8) . . ?
C7 P1 Re1 115.23(8) . . ?
C25 P2 C31 105.64(11) . . ?
C25 P2 C37 103.75(11) . . ?
C31 P2 C37 100.03(11) . . ?
C25 P2 Re1 113.15(8) . . ?
C31 P2 Re1 117.23(8) . . ?
C37 P2 Re1 115.35(9) . . ?
C1 O2 Re1 119.15(16) . . ?
C6 N1 C2 118.2(2) . . ?
C6 N1 Re1 125.94(16) . . ?
C2 N1 Re1 115.86(16) . . ?
O3 C1 O2 124.7(2) . . ?
O3 C1 C2 119.9(2) . . ?
O2 C1 C2 115.4(2) . . ?
N1 C2 C3 121.6(2) . . ?
N1 C2 C1 115.3(2) . . ?
C3 C2 C1 123.1(2) . . ?
C4 C3 C2 119.6(3) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C5 C4 C3 118.8(3) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 119.4(3) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
N1 C6 C5 122.4(2) . . ?
N1 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C12 C7 C8 118.3(2) . . ?
C12 C7 P1 122.1(2) . . ?
C8 C7 P1 119.29(19) . . ?
C9 C8 C7 120.3(3) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C8 120.8(3) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 119.5(3) . . ?
C11 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C10 C11 C12 120.4(3) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C7 C12 C11 120.7(3) . . ?
C7 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C18 C13 C14 118.7(2) . . ?
C18 C13 P1 123.71(19) . . ?
C14 C13 P1 117.60(19) . . ?
C15 C14 C13 120.5(3) . . ?
C15 C14 H14 119.7 . . ?
C13 C14 H14 119.7 . . ?
C16 C15 C14 120.0(3) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C16 C17 120.3(3) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C16 C17 C18 120.2(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C13 C18 C17 120.3(3) . . ?
C13 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C24 C19 C20 118.8(2) . . ?
C24 C19 P1 122.29(19) . . ?
C20 C19 P1 118.60(19) . . ?
C21 C20 C19 120.3(3) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C21 C22 C23 119.8(3) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C22 C23 C24 120.4(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C19 120.2(2) . . ?
C23 C24 H24 119.9 . . ?
C19 C24 H24 119.9 . . ?
C26 C25 C30 118.8(2) . . ?
C26 C25 P2 120.49(18) . . ?
C30 C25 P2 120.2(2) . . ?
C27 C26 C25 120.3(2) . . ?
C27 C26 H26 119.8 . . ?
C25 C26 H26 119.8 . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 120.4(3) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.8 . . ?
C28 C29 C30 120.0(3) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 C25 120.3(3) . . ?
C29 C30 H30 119.8 . . ?
C25 C30 H30 119.8 . . ?
C32 C31 C36 118.7(2) . . ?
C32 C31 P2 124.03(19) . . ?
C36 C31 P2 116.9(2) . . ?
C33 C32 C31 120.5(2) . . ?
C33 C32 H32 119.7 . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C32 120.4(3) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.8(2) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C36 C35 C34 120.0(3) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 120.5(3) . . ?
C35 C36 H36 119.8 . . ?
C31 C36 H36 119.8 . . ?
C42 C37 C38 119.0(2) . . ?
C42 C37 P2 120.5(2) . . ?
C38 C37 P2 120.5(2) . . ?
C39 C38 C37 120.3(3) . . ?
C39 C38 H38 119.9 . . ?
C37 C38 H38 119.9 . . ?
C40 C39 C38 120.4(3) . . ?
C40 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
C41 C40 C39 119.8(3) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C40 C41 C42 120.2(3) . . ?
C40 C41 H41 119.9 . . ?
C42 C41 H41 119.9 . . ?
C37 C42 C41 120.3(3) . . ?
C37 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
O4 C43 Re1 177.2(2) . . ?
O5 C44 Re1 179.0(2) . . ?
Cl1 C45 Cl2 110.20(19) . . ?
Cl1 C45 Cl3 110.7(2) . . ?
Cl2 C45 Cl3 109.79(19) . . ?
Cl1 C45 H45 108.7 . . ?
Cl2 C45 H45 108.7 . . ?
Cl3 C45 H45 108.7 . . ?
Cl4 C46 Cl6 110.48(18) . . ?
Cl4 C46 Cl5 110.5(2) . . ?
Cl6 C46 Cl5 110.29(17) . . ?
Cl4 C46 H46 108.5 . . ?
Cl6 C46 H46 108.5 . . ?
Cl5 C46 H46 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C43 Re1 P1 C19 130.98(11) . . . . ?
C44 Re1 P1 C19 42.13(11) . . . . ?
O2 Re1 P1 C19 -59.09(9) . . . . ?
N1 Re1 P1 C19 -133.38(10) . . . . ?
P2 Re1 P1 C19 -33.1(2) . . . . ?
C43 Re1 P1 C13 11.25(12) . . . . ?
C44 Re1 P1 C13 -77.61(12) . . . . ?
O2 Re1 P1 C13 -178.83(10) . . . . ?
N1 Re1 P1 C13 106.88(10) . . . . ?
P2 Re1 P1 C13 -152.9(2) . . . . ?
C43 Re1 P1 C7 -112.20(12) . . . . ?
C44 Re1 P1 C7 158.95(12) . . . . ?
O2 Re1 P1 C7 57.73(10) . . . . ?
N1 Re1 P1 C7 -16.56(11) . . . . ?
P2 Re1 P1 C7 83.7(2) . . . . ?
C43 Re1 P2 C25 110.68(12) . . . . ?
C44 Re1 P2 C25 -160.33(12) . . . . ?
O2 Re1 P2 C25 -59.19(10) . . . . ?
N1 Re1 P2 C25 15.14(11) . . . . ?
P1 Re1 P2 C25 -85.2(2) . . . . ?
C43 Re1 P2 C31 -12.66(12) . . . . ?
C44 Re1 P2 C31 76.33(12) . . . . ?
O2 Re1 P2 C31 177.47(10) . . . . ?
N1 Re1 P2 C31 -108.20(11) . . . . ?
P1 Re1 P2 C31 151.4(2) . . . . ?
C43 Re1 P2 C37 -130.07(11) . . . . ?
C44 Re1 P2 C37 -41.09(11) . . . . ?
O2 Re1 P2 C37 60.06(9) . . . . ?
N1 Re1 P2 C37 134.38(10) . . . . ?
P1 Re1 P2 C37 34.0(2) . . . . ?
C43 Re1 O2 C1 7.0(6) . . . . ?
C44 Re1 O2 C1 -179.01(18) . . . . ?
N1 Re1 O2 C1 0.44(17) . . . . ?
P2 Re1 O2 C1 91.05(17) . . . . ?
P1 Re1 O2 C1 -91.41(17) . . . . ?
C43 Re1 N1 C6 -0.9(2) . . . . ?
C44 Re1 N1 C6 -175.2(11) . . . . ?
O2 Re1 N1 C6 177.9(2) . . . . ?
P2 Re1 N1 C6 91.8(2) . . . . ?
P1 Re1 N1 C6 -93.7(2) . . . . ?
C43 Re1 N1 C2 -179.50(18) . . . . ?
C44 Re1 N1 C2 6.2(12) . . . . ?
O2 Re1 N1 C2 -0.66(17) . . . . ?
P2 Re1 N1 C2 -86.80(17) . . . . ?
P1 Re1 N1 C2 87.68(17) . . . . ?
Re1 O2 C1 O3 -179.0(2) . . . . ?
Re1 O2 C1 C2 -0.2(3) . . . . ?
C6 N1 C2 C3 1.0(4) . . . . ?
Re1 N1 C2 C3 179.7(2) . . . . ?
C6 N1 C2 C1 -177.9(2) . . . . ?
Re1 N1 C2 C1 0.8(3) . . . . ?
O3 C1 C2 N1 178.5(2) . . . . ?
O2 C1 C2 N1 -0.4(3) . . . . ?
O3 C1 C2 C3 -0.4(4) . . . . ?
O2 C1 C2 C3 -179.3(3) . . . . ?
N1 C2 C3 C4 -1.9(4) . . . . ?
C1 C2 C3 C4 177.0(3) . . . . ?
C2 C3 C4 C5 1.0(5) . . . . ?
C3 C4 C5 C6 0.6(5) . . . . ?
C2 N1 C6 C5 0.7(4) . . . . ?
Re1 N1 C6 C5 -177.8(2) . . . . ?
C4 C5 C6 N1 -1.5(4) . . . . ?
C19 P1 C7 C12 17.0(3) . . . . ?
C13 P1 C7 C12 124.6(2) . . . . ?
Re1 P1 C7 C12 -107.3(2) . . . . ?
C19 P1 C7 C8 -169.1(2) . . . . ?
C13 P1 C7 C8 -61.5(2) . . . . ?
Re1 P1 C7 C8 66.5(2) . . . . ?
C12 C7 C8 C9 0.7(4) . . . . ?
P1 C7 C8 C9 -173.4(2) . . . . ?
C7 C8 C9 C10 -0.9(4) . . . . ?
C8 C9 C10 C11 0.0(5) . . . . ?
C9 C10 C11 C12 1.0(6) . . . . ?
C8 C7 C12 C11 0.3(5) . . . . ?
P1 C7 C12 C11 174.2(3) . . . . ?
C10 C11 C12 C7 -1.2(6) . . . . ?
C19 P1 C13 C18 100.9(2) . . . . ?
C7 P1 C13 C18 -5.0(3) . . . . ?
Re1 P1 C13 C18 -133.3(2) . . . . ?
C19 P1 C13 C14 -79.4(2) . . . . ?
C7 P1 C13 C14 174.7(2) . . . . ?
Re1 P1 C13 C14 46.4(2) . . . . ?
C18 C13 C14 C15 0.5(4) . . . . ?
P1 C13 C14 C15 -179.2(2) . . . . ?
C13 C14 C15 C16 1.0(5) . . . . ?
C14 C15 C16 C17 -1.1(5) . . . . ?
C15 C16 C17 C18 -0.2(5) . . . . ?
C14 C13 C18 C17 -1.9(4) . . . . ?
P1 C13 C18 C17 177.8(2) . . . . ?
C16 C17 C18 C13 1.7(5) . . . . ?
C13 P1 C19 C24 -23.3(2) . . . . ?
C7 P1 C19 C24 86.1(2) . . . . ?
Re1 P1 C19 C24 -149.21(17) . . . . ?
C13 P1 C19 C20 162.9(2) . . . . ?
C7 P1 C19 C20 -87.6(2) . . . . ?
Re1 P1 C19 C20 37.0(2) . . . . ?
C24 C19 C20 C21 -2.0(4) . . . . ?
P1 C19 C20 C21 171.9(2) . . . . ?
C19 C20 C21 C22 1.3(4) . . . . ?
C20 C21 C22 C23 0.4(4) . . . . ?
C21 C22 C23 C24 -1.4(4) . . . . ?
C22 C23 C24 C19 0.7(4) . . . . ?
C20 C19 C24 C23 1.0(4) . . . . ?
P1 C19 C24 C23 -172.70(19) . . . . ?
C31 P2 C25 C26 52.6(2) . . . . ?
C37 P2 C25 C26 157.3(2) . . . . ?
Re1 P2 C25 C26 -76.9(2) . . . . ?
C31 P2 C25 C30 -135.6(2) . . . . ?
C37 P2 C25 C30 -30.9(2) . . . . ?
Re1 P2 C25 C30 94.9(2) . . . . ?
C30 C25 C26 C27 1.6(4) . . . . ?
P2 C25 C26 C27 173.5(2) . . . . ?
C25 C26 C27 C28 -1.3(4) . . . . ?
C26 C27 C28 C29 0.0(5) . . . . ?
C27 C28 C29 C30 1.1(5) . . . . ?
C28 C29 C30 C25 -0.8(4) . . . . ?
C26 C25 C30 C29 -0.5(4) . . . . ?
P2 C25 C30 C29 -172.5(2) . . . . ?
C25 P2 C31 C32 10.6(3) . . . . ?
C37 P2 C31 C32 -96.9(2) . . . . ?
Re1 P2 C31 C32 137.7(2) . . . . ?
C25 P2 C31 C36 -175.7(2) . . . . ?
C37 P2 C31 C36 76.8(2) . . . . ?
Re1 P2 C31 C36 -48.6(2) . . . . ?
C36 C31 C32 C33 -1.3(4) . . . . ?
P2 C31 C32 C33 172.3(2) . . . . ?
C31 C32 C33 C34 -0.7(4) . . . . ?
C32 C33 C34 C35 1.6(5) . . . . ?
C33 C34 C35 C36 -0.6(4) . . . . ?
C34 C35 C36 C31 -1.5(4) . . . . ?
C32 C31 C36 C35 2.4(4) . . . . ?
P2 C31 C36 C35 -171.7(2) . . . . ?
C25 P2 C37 C42 106.8(2) . . . . ?
C31 P2 C37 C42 -144.2(2) . . . . ?
Re1 P2 C37 C42 -17.5(2) . . . . ?
C25 P2 C37 C38 -75.3(2) . . . . ?
C31 P2 C37 C38 33.7(2) . . . . ?
Re1 P2 C37 C38 160.40(17) . . . . ?
C42 C37 C38 C39 1.2(4) . . . . ?
P2 C37 C38 C39 -176.8(2) . . . . ?
C37 C38 C39 C40 0.2(4) . . . . ?
C38 C39 C40 C41 -1.6(4) . . . . ?
C39 C40 C41 C42 1.7(4) . . . . ?
C38 C37 C42 C41 -1.1(4) . . . . ?
P2 C37 C42 C41 176.9(2) . . . . ?
C40 C41 C42 C37 -0.3(4) . . . . ?
C44 Re1 C43 O4 178(100) . . . . ?
O2 Re1 C43 O4 -8(5) . . . . ?
N1 Re1 C43 O4 -1(5) . . . . ?
P2 Re1 C43 O4 -91(5) . . . . ?
P1 Re1 C43 O4 90(5) . . . . ?
C43 Re1 C44 O5 -48(14) . . . . ?
O2 Re1 C44 O5 133(14) . . . . ?
N1 Re1 C44 O5 127(14) . . . . ?
P2 Re1 C44 O5 -141(14) . . . . ?
P1 Re1 C44 O5 45(14) . . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.61
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 983203'
#######################################################################
#
#                 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_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C13 H10 N3 O6 Re, C3 H6 O'
_chemical_formula_sum            'C16 H16 N3 O7 Re'
_chemical_melting_point          ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless

_diffrn_ambient_temperature      173(2)
_chemical_formula_weight         548.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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'
_symmetry_int_tables_number      2


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

_cell_length_a                   8.6015(9)
_cell_length_b                   10.2481(11)
_cell_length_c                   11.3012(12)
_cell_angle_alpha                88.9500(10)
_cell_angle_beta                 74.7110(10)
_cell_angle_gamma                86.0810(10)
_cell_volume                     958.69(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    7987
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.6
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    6.380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_T_max  0.45
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0.0
_diffrn_reflns_number            11290
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.87
_diffrn_reflns_theta_max         27.56
_reflns_number_total             4355
_reflns_number_gt                4134
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0200P)²+0.2585P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4355
_refine_ls_number_parameters     248
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_ref         0.0404
_refine_ls_wR_factor_gt          0.0398
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.084153(10) 0.070407(9) 0.208889(8) 0.02048(4) Uani 1 1 d . . .
O1 O 0.1242(2) -0.04832(17) 0.35947(16) 0.0241(4) Uani 1 1 d . . .
O2 O 0.2658(2) -0.07605(17) 0.49878(16) 0.0276(4) Uani 1 1 d . . .
O3 O -0.2315(2) -0.0499(2) 0.2045(2) 0.0413(5) Uani 1 1 d . . .
O4 O 0.0391(3) 0.2665(2) 0.0117(2) 0.0422(5) Uani 1 1 d . . .
O5 O 0.2725(3) -0.1213(2) 0.0103(2) 0.0465(6) Uani 1 1 d . . .
O6 O -0.0239(2) 0.19670(17) 0.36531(17) 0.0285(4) Uani 1 1 d . . .
O7 O -0.1063(3) 0.4520(2) 0.3864(2) 0.0569(7) Uani 1 1 d . . .
N1 N 0.2980(2) 0.1396(2) 0.24464(19) 0.0222(4) Uani 1 1 d . . .
N2 N 0.3981(3) 0.2294(2) 0.1953(2) 0.0254(5) Uani 1 1 d . . .
N3 N 0.5046(2) 0.2282(2) 0.2638(2) 0.0244(4) Uani 1 1 d . . .
C1 C 0.4732(3) 0.1397(2) 0.3553(2) 0.0251(5) Uani 1 1 d . . .
H1 H 0.5311 0.1209 0.4152 0.030 Uiso 1 1 calc R . .
C2 C 0.3386(3) 0.0829(2) 0.3425(2) 0.0223(5) Uani 1 1 d . . .
C3 C 0.2367(3) -0.0211(2) 0.4072(2) 0.0223(5) Uani 1 1 d . . .
C4 C 0.6374(3) 0.3163(3) 0.2307(3) 0.0325(6) Uani 1 1 d . . .
H4A H 0.7071 0.2926 0.1482 0.039 Uiso 1 1 calc R . .
H4B H 0.7041 0.3045 0.2899 0.039 Uiso 1 1 calc R . .
C5 C 0.5767(3) 0.4577(3) 0.2304(3) 0.0274(5) Uani 1 1 d . . .
C6 C 0.4789(4) 0.5160(3) 0.3360(3) 0.0460(8) Uani 1 1 d . . .
H6 H 0.4479 0.4663 0.4092 0.055 Uiso 1 1 calc R . .
C7 C 0.4261(5) 0.6475(3) 0.3353(3) 0.0582(10) Uani 1 1 d . . .
H7 H 0.3601 0.6874 0.4083 0.070 Uiso 1 1 calc R . .
C8 C 0.4687(5) 0.7193(3) 0.2300(4) 0.0529(9) Uani 1 1 d . . .
H8 H 0.4329 0.8091 0.2303 0.064 Uiso 1 1 calc R . .
C9 C 0.5626(4) 0.6626(3) 0.1243(3) 0.0528(9) Uani 1 1 d . . .
H9 H 0.5915 0.7124 0.0509 0.063 Uiso 1 1 calc R . .
C10 C 0.6159(4) 0.5304(3) 0.1254(3) 0.0446(8) Uani 1 1 d . . .
H10 H 0.6805 0.4906 0.0519 0.054 Uiso 1 1 calc R . .
C11 C -0.1133(3) -0.0050(3) 0.2056(2) 0.0278(5) Uani 1 1 d . . .
C12 C 0.0560(3) 0.1916(3) 0.0859(3) 0.0286(6) Uani 1 1 d . . .
C13 C 0.1996(3) -0.0480(3) 0.0843(3) 0.0300(6) Uani 1 1 d . . .
C14 C -0.1250(6) 0.6808(3) 0.3748(5) 0.0791(14) Uani 1 1 d . . .
H14A H -0.1956 0.6745 0.4581 0.119 Uiso 1 1 calc R . .
H14B H -0.1883 0.7166 0.3198 0.119 Uiso 1 1 calc R . .
H14C H -0.0387 0.7384 0.3749 0.119 Uiso 1 1 calc R . .
C15 C -0.0532(4) 0.5488(3) 0.3317(3) 0.0437(8) Uani 1 1 d . . .
C16 C 0.0793(5) 0.5373(4) 0.2169(4) 0.0731(13) Uani 1 1 d . . .
H16A H 0.1316 0.4488 0.2105 0.110 Uiso 1 1 calc R . .
H16B H 0.1588 0.6010 0.2181 0.110 Uiso 1 1 calc R . .
H16C H 0.0348 0.5545 0.1463 0.110 Uiso 1 1 calc R . .
H2O H -0.1036 0.1610 0.4143 0.049(10) Uiso 1 1 d R . .
H1O H -0.0394 0.2843 0.3681 0.064(12) Uiso 1 1 d R . .


_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
Re1 C13 1.898(3) . ?
Re1 C12 1.899(3) . ?
Re1 C11 1.923(3) . ?
Re1 N1 2.152(2) . ?
Re1 O1 2.1612(17) . ?
Re1 O6 2.1719(18) . ?
O1 C3 1.274(3) . ?
O2 C3 1.244(3) . ?
O3 C11 1.147(3) . ?
O4 C12 1.157(3) . ?
O5 C13 1.157(3) . ?
O6 H2O 0.8588 . ?
O6 H1O 0.8985 . ?
O7 C15 1.210(4) . ?
N1 N2 1.316(3) . ?
N1 C2 1.355(3) . ?
N2 N3 1.345(3) . ?
N3 C1 1.348(3) . ?
N3 C4 1.471(3) . ?
C1 C2 1.372(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.483(3) . ?
C4 C5 1.507(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C10 1.366(4) . ?
C5 C6 1.385(4) . ?
C6 C7 1.393(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.366(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.367(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.402(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C14 C15 1.483(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.484(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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
C13 Re1 C12 89.38(12) . . ?
C13 Re1 C11 89.48(11) . . ?
C12 Re1 C11 89.76(11) . . ?
C13 Re1 N1 94.38(10) . . ?
C12 Re1 N1 99.73(9) . . ?
C11 Re1 N1 169.77(9) . . ?
C13 Re1 O1 95.29(9) . . ?
C12 Re1 O1 173.25(9) . . ?
C11 Re1 O1 95.15(9) . . ?
N1 Re1 O1 75.09(7) . . ?
C13 Re1 O6 172.08(9) . . ?
C12 Re1 O6 96.82(10) . . ?
C11 Re1 O6 95.44(9) . . ?
N1 Re1 O6 79.76(7) . . ?
O1 Re1 O6 78.13(7) . . ?
C3 O1 Re1 118.59(15) . . ?
Re1 O6 H2O 110.5 . . ?
Re1 O6 H1O 129.2 . . ?
H2O O6 H1O 110.8 . . ?
N2 N1 C2 110.9(2) . . ?
N2 N1 Re1 134.59(16) . . ?
C2 N1 Re1 114.41(16) . . ?
N1 N2 N3 105.0(2) . . ?
N2 N3 C1 112.3(2) . . ?
N2 N3 C4 119.0(2) . . ?
C1 N3 C4 128.7(2) . . ?
N3 C1 C2 104.4(2) . . ?
N3 C1 H1 127.8 . . ?
C2 C1 H1 127.8 . . ?
N1 C2 C1 107.4(2) . . ?
N1 C2 C3 117.0(2) . . ?
C1 C2 C3 135.6(2) . . ?
O2 C3 O1 125.0(2) . . ?
O2 C3 C2 120.4(2) . . ?
O1 C3 C2 114.5(2) . . ?
N3 C4 C5 112.1(2) . . ?
N3 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N3 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C10 C5 C6 118.8(3) . . ?
C10 C5 C4 120.5(3) . . ?
C6 C5 C4 120.7(3) . . ?
C5 C6 C7 120.2(3) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 120.2(3) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 120.4(3) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C8 C9 C10 119.3(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C5 C10 C9 121.1(3) . . ?
C5 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
O3 C11 Re1 179.5(3) . . ?
O4 C12 Re1 179.3(3) . . ?
O5 C13 Re1 178.2(2) . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 C14 120.5(4) . . ?
O7 C15 C16 120.6(3) . . ?
C14 C15 C16 118.8(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 Re1 O1 C3 98.93(19) . . . . ?
C12 Re1 O1 C3 -34.6(8) . . . . ?
C11 Re1 O1 C3 -171.12(18) . . . . ?
N1 Re1 O1 C3 5.79(17) . . . . ?
O6 Re1 O1 C3 -76.62(17) . . . . ?
C13 Re1 N1 N2 84.4(2) . . . . ?
C12 Re1 N1 N2 -5.7(3) . . . . ?
C11 Re1 N1 N2 -163.6(5) . . . . ?
O1 Re1 N1 N2 178.8(2) . . . . ?
O6 Re1 N1 N2 -100.9(2) . . . . ?
C13 Re1 N1 C2 -98.43(18) . . . . ?
C12 Re1 N1 C2 171.46(18) . . . . ?
C11 Re1 N1 C2 13.5(6) . . . . ?
O1 Re1 N1 C2 -4.11(16) . . . . ?
O6 Re1 N1 C2 76.21(17) . . . . ?
C2 N1 N2 N3 0.3(3) . . . . ?
Re1 N1 N2 N3 177.54(17) . . . . ?
N1 N2 N3 C1 -0.1(3) . . . . ?
N1 N2 N3 C4 178.4(2) . . . . ?
N2 N3 C1 C2 -0.1(3) . . . . ?
C4 N3 C1 C2 -178.5(2) . . . . ?
N2 N1 C2 C1 -0.4(3) . . . . ?
Re1 N1 C2 C1 -178.21(16) . . . . ?
N2 N1 C2 C3 -179.6(2) . . . . ?
Re1 N1 C2 C3 2.6(3) . . . . ?
N3 C1 C2 N1 0.3(3) . . . . ?
N3 C1 C2 C3 179.3(3) . . . . ?
Re1 O1 C3 O2 175.21(18) . . . . ?
Re1 O1 C3 C2 -6.1(3) . . . . ?
N1 C2 C3 O2 -179.0(2) . . . . ?
C1 C2 C3 O2 2.1(4) . . . . ?
N1 C2 C3 O1 2.3(3) . . . . ?
C1 C2 C3 O1 -176.7(3) . . . . ?
N2 N3 C4 C5 58.3(3) . . . . ?
C1 N3 C4 C5 -123.4(3) . . . . ?
N3 C4 C5 C10 -119.2(3) . . . . ?
N3 C4 C5 C6 60.3(4) . . . . ?
C10 C5 C6 C7 -1.8(5) . . . . ?
C4 C5 C6 C7 178.7(3) . . . . ?
C5 C6 C7 C8 0.8(6) . . . . ?
C6 C7 C8 C9 0.4(6) . . . . ?
C7 C8 C9 C10 -0.6(6) . . . . ?
C6 C5 C10 C9 1.7(5) . . . . ?
C4 C5 C10 C9 -178.9(3) . . . . ?
C8 C9 C10 C5 -0.5(6) . . . . ?
C13 Re1 C11 O3 144(30) . . . . ?
C12 Re1 C11 O3 -127(30) . . . . ?
N1 Re1 C11 O3 31(30) . . . . ?
O1 Re1 C11 O3 48(30) . . . . ?
O6 Re1 C11 O3 -30(30) . . . . ?
C13 Re1 C12 O4 -141(20) . . . . ?
C11 Re1 C12 O4 129(20) . . . . ?
N1 Re1 C12 O4 -47(20) . . . . ?
O1 Re1 C12 O4 -8(20) . . . . ?
O6 Re1 C12 O4 34(20) . . . . ?
C12 Re1 C13 O5 147(9) . . . . ?
C11 Re1 C13 O5 -124(9) . . . . ?
N1 Re1 C13 O5 47(9) . . . . ?
O1 Re1 C13 O5 -28(9) . . . . ?
O6 Re1 C13 O5 5(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O6 H2O O2 0.86 1.75 2.610(3) 173.6 2_556
O6 H1O O7 0.90 1.77 2.662(3) 169.8 .

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.097
_database_code_depnum_ccdc_archive 'CCDC 983204'
#######################################################################
#
#                 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_6

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C31 H23 N3 O5 P Re, C2 H6 O'
_chemical_formula_sum            'C33 H29 N3 O6 P Re'
_chemical_melting_point          ?

_exptl_crystal_description       Plate
_exptl_crystal_colour            Colourless

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         780.76

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 '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                   10.1876(14)
_cell_length_b                   10.5072(14)
_cell_length_c                   15.090(2)
_cell_angle_alpha                86.0620(10)
_cell_angle_beta                 70.4170(10)
_cell_angle_gamma                86.9510(10)
_cell_volume                     1517.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9981
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.4
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_F_000             772
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    4.107
_shelx_estimated_absorpt_T_min   0.233
_shelx_estimated_absorpt_T_max   0.494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.33
_exptl_absorpt_correction_T_max  0.49
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'normal focus tube'

_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16777
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.434
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6183
_reflns_number_gt                6078
_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       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0114P)²+1.3047P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6183
_refine_ls_number_parameters     402
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0141
_refine_ls_wR_factor_ref         0.0339
_refine_ls_wR_factor_gt          0.0338
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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
Re1 Re 0.44638(2) 0.42086(2) 0.28775(2) 0.00876(3) Uani 1 1 d . . . . .
P1 P 0.39757(5) 0.25602(4) 0.19110(3) 0.00901(9) Uani 1 1 d . . . . .
O1 O 0.61298(13) 0.28740(12) 0.29837(9) 0.0115(3) Uani 1 1 d . . . . .
N1 N 0.35217(16) 0.29831(14) 0.41118(11) 0.0104(3) Uani 1 1 d . . . . .
C1 C 0.58668(19) 0.20449(17) 0.36841(13) 0.0111(4) Uani 1 1 d . . . . .
O2 O 0.67240(14) 0.12796(13) 0.38530(10) 0.0146(3) Uani 1 1 d . . . . .
N2 N 0.22521(16) 0.28970(15) 0.47192(11) 0.0116(3) Uani 1 1 d . . . . .
C2 C 0.43914(19) 0.20715(17) 0.43169(13) 0.0105(4) Uani 1 1 d . . . . .
O3 O 0.53417(16) 0.60869(14) 0.40587(11) 0.0211(3) Uani 1 1 d . . . . .
N3 N 0.23314(16) 0.19098(15) 0.53179(11) 0.0114(3) Uani 1 1 d . . . . .
C3 C 0.36224(19) 0.13735(18) 0.51016(13) 0.0119(4) Uani 1 1 d . . . . .
H3 H 0.3930 0.0671 0.5421 0.014 Uiso 1 1 calc R U . . .
O4 O 0.61070(16) 0.56689(15) 0.10364(10) 0.0237(3) Uani 1 1 d . . . . .
C4 C 0.10725(19) 0.15521(19) 0.61108(13) 0.0147(4) Uani 1 1 d . . . . .
H4A H 0.0888 0.0642 0.6087 0.018 Uiso 1 1 calc R U . . .
H4B H 0.0259 0.2069 0.6056 0.018 Uiso 1 1 calc R U . . .
O5 O 0.18903(15) 0.59342(14) 0.30039(10) 0.0211(3) Uani 1 1 d . . . . .
C5 C 0.12639(19) 0.17694(19) 0.70391(13) 0.0135(4) Uani 1 1 d . . . . .
C6 C 0.1328(2) 0.0745(2) 0.76584(14) 0.0170(4) Uani 1 1 d . . . . .
H6 H 0.1224 -0.0099 0.7507 0.020 Uiso 1 1 calc R U . . .
C7 C 0.1542(2) 0.0952(2) 0.85006(14) 0.0209(4) Uani 1 1 d . . . . .
H7 H 0.1561 0.0252 0.8930 0.025 Uiso 1 1 calc R U . . .
C8 C 0.1729(2) 0.2176(2) 0.87140(15) 0.0226(5) Uani 1 1 d . . . . .
H8 H 0.1907 0.2313 0.9278 0.027 Uiso 1 1 calc R U . . .
C9 C 0.1655(2) 0.3201(2) 0.81007(16) 0.0224(5) Uani 1 1 d . . . . .
H9 H 0.1770 0.4042 0.8251 0.027 Uiso 1 1 calc R U . . .
C10 C 0.1414(2) 0.3006(2) 0.72706(15) 0.0183(4) Uani 1 1 d . . . . .
H10 H 0.1351 0.3713 0.6858 0.022 Uiso 1 1 calc R U . . .
C11 C 0.37392(19) 0.09952(17) 0.25416(13) 0.0102(4) Uani 1 1 d . . . . .
C12 C 0.48788(19) 0.01450(18) 0.24193(13) 0.0128(4) Uani 1 1 d . . . . .
H12 H 0.5741 0.0327 0.1941 0.015 Uiso 1 1 calc R U . . .
C13 C 0.4761(2) -0.09688(18) 0.29938(14) 0.0152(4) Uani 1 1 d . . . . .
H13 H 0.5540 -0.1544 0.2905 0.018 Uiso 1 1 calc R U . . .
C14 C 0.3508(2) -0.12377(18) 0.36950(14) 0.0154(4) Uani 1 1 d . . . . .
H14 H 0.3430 -0.1992 0.4092 0.019 Uiso 1 1 calc R U . . .
C15 C 0.2362(2) -0.04002(18) 0.38171(14) 0.0145(4) Uani 1 1 d . . . . .
H15 H 0.1502 -0.0591 0.4294 0.017 Uiso 1 1 calc R U . . .
C16 C 0.24690(19) 0.07120(18) 0.32475(13) 0.0120(4) Uani 1 1 d . . . . .
H16 H 0.1684 0.1280 0.3335 0.014 Uiso 1 1 calc R U . . .
C17 C 0.24554(19) 0.29113(18) 0.15434(13) 0.0112(4) Uani 1 1 d . . . . .
C18 C 0.1494(2) 0.20004(18) 0.15554(13) 0.0139(4) Uani 1 1 d . . . . .
H18 H 0.1637 0.1135 0.1737 0.017 Uiso 1 1 calc R U . . .
C19 C 0.0332(2) 0.23632(19) 0.13010(14) 0.0159(4) Uani 1 1 d . . . . .
H19 H -0.0326 0.1746 0.1319 0.019 Uiso 1 1 calc R U . . .
C20 C 0.0128(2) 0.36224(19) 0.10210(14) 0.0160(4) Uani 1 1 d . . . . .
H20 H -0.0680 0.3869 0.0862 0.019 Uiso 1 1 calc R U . . .
C21 C 0.1102(2) 0.45200(19) 0.09723(14) 0.0155(4) Uani 1 1 d . . . . .
H21 H 0.0976 0.5376 0.0761 0.019 Uiso 1 1 calc R U . . .
C22 C 0.2260(2) 0.41697(18) 0.12329(13) 0.0133(4) Uani 1 1 d . . . . .
H22 H 0.2924 0.4788 0.1200 0.016 Uiso 1 1 calc R U . . .
C23 C 0.53918(19) 0.22896(17) 0.08050(13) 0.0114(4) Uani 1 1 d . . . . .
C24 C 0.5120(2) 0.1991(2) -0.00007(15) 0.0196(4) Uani 1 1 d . . . . .
H24 H 0.4184 0.1926 0.0019 0.024 Uiso 1 1 calc R U . . .
C25 C 0.6209(2) 0.1786(2) -0.08334(15) 0.0252(5) Uani 1 1 d . . . . .
H25 H 0.6014 0.1594 -0.1382 0.030 Uiso 1 1 calc R U . . .
C26 C 0.7581(2) 0.1863(2) -0.08641(14) 0.0198(4) Uani 1 1 d . . . . .
H26 H 0.8326 0.1724 -0.1433 0.024 Uiso 1 1 calc R U . . .
C27 C 0.7857(2) 0.21448(19) -0.00628(14) 0.0158(4) Uani 1 1 d . . . . .
H27 H 0.8796 0.2183 -0.0081 0.019 Uiso 1 1 calc R U . . .
C28 C 0.6777(2) 0.23722(18) 0.07671(14) 0.0139(4) Uani 1 1 d . . . . .
H28 H 0.6977 0.2584 0.1309 0.017 Uiso 1 1 calc R U . . .
C29 C 0.5000(2) 0.53914(18) 0.36288(14) 0.0144(4) Uani 1 1 d . . . . .
C30 C 0.5498(2) 0.51252(18) 0.17278(14) 0.0148(4) Uani 1 1 d . . . . .
C31 C 0.2860(2) 0.52812(18) 0.29418(13) 0.0141(4) Uani 1 1 d . . . . .
O1S O 0.93003(16) 0.18861(14) 0.39043(12) 0.0223(3) Uani 1 1 d . . . . .
H1OS H 0.861(3) 0.177(2) 0.3879(19) 0.025(7) Uiso 1 1 d . . . . .
C1S C 0.8592(3) 0.3957(2) 0.45648(17) 0.0321(6) Uani 1 1 d . . . . .
H1S1 H 0.7617 0.3906 0.4603 0.048 Uiso 1 1 calc R U . . .
H1S2 H 0.8857 0.4852 0.4472 0.048 Uiso 1 1 calc R U . . .
H1S3 H 0.8706 0.3589 0.5150 0.048 Uiso 1 1 calc R U . . .
C2S C 0.9504(2) 0.32293(19) 0.37540(15) 0.0192(4) Uani 1 1 d . . . . .
H2S1 H 0.9303 0.3536 0.3176 0.023 Uiso 1 1 calc R U . . .
H2S2 H 1.0492 0.3397 0.3655 0.023 Uiso 1 1 calc R U . . .


_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
Re1 C31 1.913(2) . ?
Re1 C30 1.924(2) . ?
Re1 C29 1.951(2) . ?
Re1 N1 2.1570(15) . ?
Re1 O1 2.1843(13) . ?
Re1 P1 2.5098(5) . ?
P1 C17 1.8247(19) . ?
P1 C11 1.8279(19) . ?
P1 C23 1.8316(19) . ?
O1 C1 1.287(2) . ?
N1 N2 1.314(2) . ?
N1 C2 1.360(2) . ?
C1 O2 1.233(2) . ?
C1 C2 1.486(3) . ?
N2 N3 1.345(2) . ?
C2 C3 1.369(3) . ?
O3 C29 1.149(2) . ?
N3 C3 1.346(2) . ?
N3 C4 1.476(2) . ?
C3 H3 0.9500 . ?
O4 C30 1.150(2) . ?
C4 C5 1.511(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
O5 C31 1.154(2) . ?
C5 C6 1.390(3) . ?
C5 C10 1.397(3) . ?
C6 C7 1.393(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.385(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.387(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.385(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.396(3) . ?
C11 C16 1.404(3) . ?
C12 C13 1.393(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.386(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.392(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.399(3) . ?
C17 C18 1.400(3) . ?
C18 C19 1.390(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.387(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.386(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.389(3) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.393(3) . ?
C23 C28 1.400(3) . ?
C24 C25 1.390(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.390(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.388(3) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
O1S C2S 1.429(2) . ?
O1S H1OS 0.74(3) . ?
C1S C2S 1.495(3) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?

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
C31 Re1 C30 89.51(8) . . ?
C31 Re1 C29 89.44(8) . . ?
C30 Re1 C29 91.34(8) . . ?
C31 Re1 N1 97.85(7) . . ?
C30 Re1 N1 172.28(7) . . ?
C29 Re1 N1 91.07(7) . . ?
C31 Re1 O1 172.47(6) . . ?
C30 Re1 O1 97.99(7) . . ?
C29 Re1 O1 89.79(7) . . ?
N1 Re1 O1 74.68(5) . . ?
C31 Re1 P1 96.01(6) . . ?
C30 Re1 P1 88.82(6) . . ?
C29 Re1 P1 174.56(6) . . ?
N1 Re1 P1 88.10(4) . . ?
O1 Re1 P1 84.80(4) . . ?
C17 P1 C11 107.32(8) . . ?
C17 P1 C23 103.76(9) . . ?
C11 P1 C23 104.28(8) . . ?
C17 P1 Re1 115.22(6) . . ?
C11 P1 Re1 111.16(6) . . ?
C23 P1 Re1 114.19(6) . . ?
C1 O1 Re1 118.77(11) . . ?
N2 N1 C2 110.91(15) . . ?
N2 N1 Re1 133.83(12) . . ?
C2 N1 Re1 115.24(12) . . ?
O2 C1 O1 125.42(17) . . ?
O2 C1 C2 120.40(17) . . ?
O1 C1 C2 114.18(16) . . ?
N1 N2 N3 104.77(14) . . ?
N1 C2 C3 107.40(16) . . ?
N1 C2 C1 117.06(16) . . ?
C3 C2 C1 135.54(17) . . ?
N2 N3 C3 112.68(15) . . ?
N2 N3 C4 119.31(15) . . ?
C3 N3 C4 128.00(16) . . ?
N3 C3 C2 104.23(16) . . ?
N3 C3 H3 127.9 . . ?
C2 C3 H3 127.9 . . ?
N3 C4 C5 110.45(15) . . ?
N3 C4 H4A 109.6 . . ?
C5 C4 H4A 109.6 . . ?
N3 C4 H4B 109.6 . . ?
C5 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 C10 119.40(19) . . ?
C6 C5 C4 120.57(18) . . ?
C10 C5 C4 120.01(18) . . ?
C5 C6 C7 120.12(19) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C8 C7 C6 120.2(2) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C9 119.8(2) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 120.4(2) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C5 120.1(2) . . ?
C9 C10 H10 120.0 . . ?
C5 C10 H10 120.0 . . ?
C12 C11 C16 119.23(17) . . ?
C12 C11 P1 119.88(14) . . ?
C16 C11 P1 120.27(14) . . ?
C13 C12 C11 120.46(17) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 120.05(18) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 119.88(18) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 120.50(18) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C11 119.88(17) . . ?
C15 C16 H16 120.1 . . ?
C11 C16 H16 120.1 . . ?
C22 C17 C18 119.12(17) . . ?
C22 C17 P1 117.04(14) . . ?
C18 C17 P1 123.83(14) . . ?
C19 C18 C17 119.98(18) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C18 120.34(18) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C21 C20 C19 120.03(18) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 120.06(18) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C17 120.38(18) . . ?
C21 C22 H22 119.8 . . ?
C17 C22 H22 119.8 . . ?
C24 C23 C28 119.10(18) . . ?
C24 C23 P1 121.31(15) . . ?
C28 C23 P1 119.58(14) . . ?
C25 C24 C23 120.50(19) . . ?
C25 C24 H24 119.7 . . ?
C23 C24 H24 119.7 . . ?
C26 C25 C24 120.0(2) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C25 119.70(19) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C26 C27 C28 120.64(19) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
C27 C28 C23 119.99(18) . . ?
C27 C28 H28 120.0 . . ?
C23 C28 H28 120.0 . . ?
O3 C29 Re1 178.63(18) . . ?
O4 C30 Re1 179.29(18) . . ?
O5 C31 Re1 178.24(17) . . ?
C2S O1S H1OS 107(2) . . ?
C2S C1S H1S1 109.5 . . ?
C2S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
C2S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
O1S C2S C1S 112.27(18) . . ?
O1S C2S H2S1 109.2 . . ?
C1S C2S H2S1 109.2 . . ?
O1S C2S H2S2 109.2 . . ?
C1S C2S H2S2 109.2 . . ?
H2S1 C2S H2S2 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 O1 C1 O2 -176.35(14) . . . . ?
Re1 O1 C1 C2 3.2(2) . . . . ?
C2 N1 N2 N3 0.07(19) . . . . ?
Re1 N1 N2 N3 178.41(12) . . . . ?
N2 N1 C2 C3 -0.2(2) . . . . ?
Re1 N1 C2 C3 -178.85(12) . . . . ?
N2 N1 C2 C1 179.62(15) . . . . ?
Re1 N1 C2 C1 0.9(2) . . . . ?
O2 C1 C2 N1 176.84(16) . . . . ?
O1 C1 C2 N1 -2.7(2) . . . . ?
O2 C1 C2 C3 -3.5(3) . . . . ?
O1 C1 C2 C3 177.0(2) . . . . ?
N1 N2 N3 C3 0.1(2) . . . . ?
N1 N2 N3 C4 179.21(15) . . . . ?
N2 N3 C3 C2 -0.2(2) . . . . ?
C4 N3 C3 C2 -179.22(17) . . . . ?
N1 C2 C3 N3 0.2(2) . . . . ?
C1 C2 C3 N3 -179.5(2) . . . . ?
N2 N3 C4 C5 -114.85(18) . . . . ?
C3 N3 C4 C5 64.1(2) . . . . ?
N3 C4 C5 C6 -113.47(19) . . . . ?
N3 C4 C5 C10 64.9(2) . . . . ?
C10 C5 C6 C7 -0.1(3) . . . . ?
C4 C5 C6 C7 178.24(18) . . . . ?
C5 C6 C7 C8 -1.7(3) . . . . ?
C6 C7 C8 C9 2.2(3) . . . . ?
C7 C8 C9 C10 -0.9(3) . . . . ?
C8 C9 C10 C5 -0.9(3) . . . . ?
C6 C5 C10 C9 1.4(3) . . . . ?
C4 C5 C10 C9 -176.98(18) . . . . ?
C17 P1 C11 C12 141.15(15) . . . . ?
C23 P1 C11 C12 31.48(17) . . . . ?
Re1 P1 C11 C12 -92.03(15) . . . . ?
C17 P1 C11 C16 -48.02(17) . . . . ?
C23 P1 C11 C16 -157.69(15) . . . . ?
Re1 P1 C11 C16 78.81(15) . . . . ?
C16 C11 C12 C13 -0.3(3) . . . . ?
P1 C11 C12 C13 170.59(15) . . . . ?
C11 C12 C13 C14 -0.2(3) . . . . ?
C12 C13 C14 C15 0.7(3) . . . . ?
C13 C14 C15 C16 -0.7(3) . . . . ?
C14 C15 C16 C11 0.1(3) . . . . ?
C12 C11 C16 C15 0.4(3) . . . . ?
P1 C11 C16 C15 -170.50(14) . . . . ?
C11 P1 C17 C22 166.27(14) . . . . ?
C23 P1 C17 C22 -83.70(16) . . . . ?
Re1 P1 C17 C22 41.88(16) . . . . ?
C11 P1 C17 C18 -13.82(18) . . . . ?
C23 P1 C17 C18 96.20(17) . . . . ?
Re1 P1 C17 C18 -138.22(14) . . . . ?
C22 C17 C18 C19 -2.8(3) . . . . ?
P1 C17 C18 C19 177.25(15) . . . . ?
C17 C18 C19 C20 1.0(3) . . . . ?
C18 C19 C20 C21 1.5(3) . . . . ?
C19 C20 C21 C22 -2.1(3) . . . . ?
C20 C21 C22 C17 0.2(3) . . . . ?
C18 C17 C22 C21 2.3(3) . . . . ?
P1 C17 C22 C21 -177.79(15) . . . . ?
C17 P1 C23 C24 -19.73(18) . . . . ?
C11 P1 C23 C24 92.52(17) . . . . ?
Re1 P1 C23 C24 -145.96(15) . . . . ?
C17 P1 C23 C28 160.85(15) . . . . ?
C11 P1 C23 C28 -86.90(16) . . . . ?
Re1 P1 C23 C28 34.62(17) . . . . ?
C28 C23 C24 C25 -0.5(3) . . . . ?
P1 C23 C24 C25 -179.88(17) . . . . ?
C23 C24 C25 C26 0.8(3) . . . . ?
C24 C25 C26 C27 0.0(3) . . . . ?
C25 C26 C27 C28 -1.1(3) . . . . ?
C26 C27 C28 C23 1.4(3) . . . . ?
C24 C23 C28 C27 -0.7(3) . . . . ?
P1 C23 C28 C27 178.78(15) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1OS O2 0.74(3) 2.03(3) 2.761(2) 175(3) .

_refine_diff_density_max         0.875
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.067

_shelxl_version_number           2013-4

_diffrn_standards_decay_%        0.0
_symmetry_cell_setting           ?
_symmetry_space_group_name_h-m   ?
_symmetry_int_tables_number      ?

_chemical_absolute_configuration rmad
_database_code_depnum_ccdc_archive 'CCDC 983205'
#######################################################################
#
#                 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_7

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C48 H38 N3 O4 P2 Re, C H Cl3'
_chemical_formula_sum            'C49 H39 Cl3 N3 O4 P2 Re'
_chemical_melting_point          ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1088.32

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'
Cl Cl 0.1484 0.1585 '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'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.1322(6)
_cell_length_b                   12.2900(4)
_cell_length_c                   21.1693(8)
_cell_angle_alpha                90
_cell_angle_beta                 100.7630(10)
_cell_angle_gamma                90
_cell_volume                     4378.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7115
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      27.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_F_000             2168
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.081
_shelx_estimated_absorpt_T_min   0.578
_shelx_estimated_absorpt_T_max   0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_process_details   
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 Göttingen, Germany).
;

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?

_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31375
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.210
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8949
_reflns_number_gt                7317
_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       'APEX2 (Bruker AXS, 2008)'
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

_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)+(0.0183P)²+1.5352P] 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         8949
_refine_ls_number_parameters     559
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0587
_refine_ls_wR_factor_gt          0.0537
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Re1 Re 0.22049(2) 0.54483(2) 0.34856(2) 0.00974(5) Uani 1 1 d . . . . .
P1 P 0.21268(5) 0.73554(7) 0.31970(4) 0.0108(2) Uani 1 1 d . . . . .
O1 O 0.26824(13) 0.59092(18) 0.44865(11) 0.0131(5) Uani 1 1 d . . . . .
N1 N 0.34900(16) 0.5378(2) 0.35894(13) 0.0104(6) Uani 1 1 d . . . . .
C1 C 0.3441(2) 0.5843(3) 0.46963(18) 0.0143(8) Uani 1 1 d . . . . .
P2 P 0.22100(5) 0.35918(7) 0.38838(4) 0.0110(2) Uani 1 1 d . . . . .
O2 O 0.37772(14) 0.59713(18) 0.52613(11) 0.0164(6) Uani 1 1 d . . . . .
N2 N 0.39753(16) 0.5090(2) 0.32003(14) 0.0140(7) Uani 1 1 d . . . . .
C2 C 0.39036(19) 0.5574(2) 0.41927(16) 0.0110(7) Uani 1 1 d . . . . .
O3 O 0.04252(14) 0.55209(19) 0.35190(12) 0.0224(6) Uani 1 1 d . . . . .
N3 N 0.47126(16) 0.5102(2) 0.35721(14) 0.0140(7) Uani 1 1 d . . . . .
C3 C 0.4696(2) 0.5393(3) 0.41827(17) 0.0138(8) Uani 1 1 d . . . . .
H3 H 0.5133 0.5459 0.4530 0.017 Uiso 1 1 calc R U . . .
O4 O 0.17929(14) 0.47916(19) 0.20722(12) 0.0192(6) Uani 1 1 d . . . . .
C4 C 0.5400(2) 0.4785(3) 0.32870(18) 0.0166(8) Uani 1 1 d . . . . .
H4A H 0.5208 0.4480 0.2853 0.020 Uiso 1 1 calc R U . . .
H4B H 0.5702 0.4208 0.3554 0.020 Uiso 1 1 calc R U . . .
C5 C 0.5945(2) 0.5732(3) 0.32357(17) 0.0141(8) Uani 1 1 d . . . . .
C6 C 0.6692(2) 0.5779(3) 0.36230(18) 0.0184(8) Uani 1 1 d . . . . .
H6 H 0.6862 0.5206 0.3918 0.022 Uiso 1 1 calc R U . . .
C7 C 0.7191(2) 0.6652(3) 0.35851(19) 0.0249(9) Uani 1 1 d . . . . .
H7 H 0.7708 0.6661 0.3842 0.030 Uiso 1 1 calc R U . . .
C8 C 0.6941(2) 0.7507(3) 0.31757(19) 0.0265(10) Uani 1 1 d . . . . .
H8 H 0.7280 0.8114 0.3158 0.032 Uiso 1 1 calc R U . . .
C9 C 0.6194(2) 0.7478(3) 0.27907(19) 0.0250(9) Uani 1 1 d . . . . .
H9 H 0.6018 0.8071 0.2512 0.030 Uiso 1 1 calc R U . . .
C10 C 0.5699(2) 0.6587(3) 0.28090(18) 0.0208(9) Uani 1 1 d . . . . .
H10 H 0.5195 0.6559 0.2532 0.025 Uiso 1 1 calc R U . . .
C11 C 0.3030(2) 0.8182(3) 0.34188(16) 0.0122(8) Uani 1 1 d . . . . .
C12 C 0.3078(2) 0.9053(3) 0.38561(17) 0.0158(8) Uani 1 1 d . . . . .
H12 H 0.2628 0.9241 0.4036 0.019 Uiso 1 1 calc R U . . .
C13 C 0.3775(2) 0.9637(3) 0.40262(18) 0.0185(8) Uani 1 1 d . . . . .
H13 H 0.3798 1.0219 0.4325 0.022 Uiso 1 1 calc R U . . .
C14 C 0.4437(2) 0.9392(3) 0.37710(17) 0.0186(9) Uani 1 1 d . . . . .
H14 H 0.4910 0.9807 0.3885 0.022 Uiso 1 1 calc R U . . .
C15 C 0.4400(2) 0.8525(3) 0.33419(18) 0.0181(8) Uani 1 1 d . . . . .
H15 H 0.4853 0.8348 0.3163 0.022 Uiso 1 1 calc R U . . .
C16 C 0.3708(2) 0.7913(3) 0.31719(17) 0.0163(8) Uani 1 1 d . . . . .
H16 H 0.3697 0.7312 0.2888 0.020 Uiso 1 1 calc R U . . .
C17 C 0.1769(2) 0.7625(3) 0.23409(16) 0.0128(8) Uani 1 1 d . . . . .
C18 C 0.2160(2) 0.8258(3) 0.19516(17) 0.0158(8) Uani 1 1 d . . . . .
H18 H 0.2664 0.8562 0.2126 0.019 Uiso 1 1 calc R U . . .
C19 C 0.1821(2) 0.8453(3) 0.13087(18) 0.0209(9) Uani 1 1 d . . . . .
H19 H 0.2101 0.8871 0.1046 0.025 Uiso 1 1 calc R U . . .
C20 C 0.1076(2) 0.8036(3) 0.10543(18) 0.0225(9) Uani 1 1 d . . . . .
H20 H 0.0838 0.8187 0.0621 0.027 Uiso 1 1 calc R U . . .
C21 C 0.0680(2) 0.7398(3) 0.14333(18) 0.0213(9) Uani 1 1 d . . . . .
H21 H 0.0171 0.7109 0.1259 0.026 Uiso 1 1 calc R U . . .
C22 C 0.1029(2) 0.7182(3) 0.20680(17) 0.0173(8) Uani 1 1 d . . . . .
H22 H 0.0761 0.6727 0.2321 0.021 Uiso 1 1 calc R U . . .
C23 C 0.14142(19) 0.8135(3) 0.35679(17) 0.0121(8) Uani 1 1 d . . . . .
C24 C 0.0901(2) 0.8899(3) 0.32276(18) 0.0164(8) Uani 1 1 d . . . . .
H24 H 0.0877 0.8984 0.2778 0.020 Uiso 1 1 calc R U . . .
C25 C 0.0424(2) 0.9537(3) 0.35404(18) 0.0195(8) Uani 1 1 d . . . . .
H25 H 0.0067 1.0044 0.3301 0.023 Uiso 1 1 calc R U . . .
C26 C 0.0462(2) 0.9445(3) 0.41892(19) 0.0214(9) Uani 1 1 d . . . . .
H26 H 0.0147 0.9904 0.4402 0.026 Uiso 1 1 calc R U . . .
C27 C 0.0963(2) 0.8676(3) 0.45367(18) 0.0202(9) Uani 1 1 d . . . . .
H27 H 0.0984 0.8603 0.4986 0.024 Uiso 1 1 calc R U . . .
C28 C 0.1433(2) 0.8016(3) 0.42281(18) 0.0165(8) Uani 1 1 d . . . . .
H28 H 0.1768 0.7483 0.4466 0.020 Uiso 1 1 calc R U . . .
C29 C 0.31778(19) 0.3041(3) 0.42710(17) 0.0114(8) Uani 1 1 d . . . . .
C30 C 0.3360(2) 0.2834(3) 0.49279(17) 0.0164(8) Uani 1 1 d . . . . .
H30 H 0.2971 0.2948 0.5187 0.020 Uiso 1 1 calc R U . . .
C31 C 0.4115(2) 0.2457(3) 0.52070(19) 0.0228(9) Uani 1 1 d . . . . .
H31 H 0.4236 0.2311 0.5655 0.027 Uiso 1 1 calc R U . . .
C32 C 0.4689(2) 0.2297(3) 0.48357(19) 0.0202(9) Uani 1 1 d . . . . .
H32 H 0.5204 0.2049 0.5028 0.024 Uiso 1 1 calc R U . . .
C33 C 0.4507(2) 0.2498(3) 0.41822(18) 0.0179(8) Uani 1 1 d . . . . .
H33 H 0.4897 0.2380 0.3924 0.021 Uiso 1 1 calc R U . . .
C34 C 0.3761(2) 0.2872(3) 0.39016(18) 0.0161(8) Uani 1 1 d . . . . .
H34 H 0.3644 0.3016 0.3453 0.019 Uiso 1 1 calc R U . . .
C35 C 0.15973(19) 0.3372(3) 0.44947(16) 0.0123(8) Uani 1 1 d . . . . .
C36 C 0.1349(2) 0.4241(3) 0.48350(17) 0.0151(8) Uani 1 1 d . . . . .
H36 H 0.1497 0.4963 0.4749 0.018 Uiso 1 1 calc R U . . .
C37 C 0.0890(2) 0.4057(3) 0.52964(17) 0.0173(8) Uani 1 1 d . . . . .
H37 H 0.0713 0.4656 0.5516 0.021 Uiso 1 1 calc R U . . .
C38 C 0.0685(2) 0.3008(3) 0.54406(17) 0.0189(9) Uani 1 1 d . . . . .
H38 H 0.0371 0.2886 0.5759 0.023 Uiso 1 1 calc R U . . .
C39 C 0.0942(2) 0.2136(3) 0.51169(18) 0.0207(9) Uani 1 1 d . . . . .
H39 H 0.0811 0.1414 0.5220 0.025 Uiso 1 1 calc R U . . .
C40 C 0.1387(2) 0.2311(3) 0.46457(17) 0.0160(8) Uani 1 1 d . . . . .
H40 H 0.1552 0.1709 0.4422 0.019 Uiso 1 1 calc R U . . .
C41 C 0.1840(2) 0.2572(3) 0.32684(16) 0.0124(8) Uani 1 1 d . . . . .
C42 C 0.1141(2) 0.2798(3) 0.28290(16) 0.0140(8) Uani 1 1 d . . . . .
H42 H 0.0855 0.3447 0.2872 0.017 Uiso 1 1 calc R U . . .
C43 C 0.0864(2) 0.2078(3) 0.23304(17) 0.0172(8) Uani 1 1 d . . . . .
H43 H 0.0391 0.2242 0.2033 0.021 Uiso 1 1 calc R U . . .
C44 C 0.1273(2) 0.1124(3) 0.22659(17) 0.0168(8) Uani 1 1 d . . . . .
H44 H 0.1089 0.0640 0.1920 0.020 Uiso 1 1 calc R U . . .
C45 C 0.1950(2) 0.0884(3) 0.27082(17) 0.0173(8) Uani 1 1 d . . . . .
H45 H 0.2228 0.0226 0.2668 0.021 Uiso 1 1 calc R U . . .
C46 C 0.2230(2) 0.1592(3) 0.32110(17) 0.0162(8) Uani 1 1 d . . . . .
H46 H 0.2690 0.1407 0.3517 0.019 Uiso 1 1 calc R U . . .
C47 C 0.1106(2) 0.5502(3) 0.35079(16) 0.0148(8) Uani 1 1 d . . . . .
C48 C 0.1944(2) 0.5032(3) 0.26177(18) 0.0143(8) Uani 1 1 d . . . . .
Cl1S Cl 0.27369(8) 1.02893(8) 0.55338(5) 0.0449(3) Uani 1 1 d . . . . .
C1S C 0.2872(2) 0.9142(3) 0.60424(17) 0.0206(9) Uani 1 1 d . . . . .
H1S H 0.2346 0.8946 0.6152 0.025 Uiso 1 1 calc R U . . .
Cl2S Cl 0.35350(6) 0.94524(8) 0.67642(5) 0.0278(2) Uani 1 1 d . . . . .
Cl3S Cl 0.32159(6) 0.80216(8) 0.56597(5) 0.0258(2) 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
Re1 C48 1.879(4) . ?
Re1 C47 1.892(4) . ?
Re1 N1 2.173(3) . ?
Re1 O1 2.198(2) . ?
Re1 P1 2.4196(9) . ?
Re1 P2 2.4318(9) . ?
P1 C17 1.832(4) . ?
P1 C11 1.838(3) . ?
P1 C23 1.839(4) . ?
O1 C1 1.295(4) . ?
N1 N2 1.323(4) . ?
N1 C2 1.361(4) . ?
C1 O2 1.237(4) . ?
C1 C2 1.480(5) . ?
P2 C35 1.832(4) . ?
P2 C41 1.833(3) . ?
P2 C29 1.836(3) . ?
N2 N3 1.358(3) . ?
C2 C3 1.379(5) . ?
O3 C47 1.172(4) . ?
N3 C3 1.347(4) . ?
N3 C4 1.472(4) . ?
C3 H3 0.9500 . ?
O4 C48 1.173(4) . ?
C4 C5 1.509(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.386(4) . ?
C5 C10 1.398(5) . ?
C6 C7 1.383(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.379(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.390(5) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C16 1.400(5) . ?
C11 C12 1.407(5) . ?
C12 C13 1.382(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.395(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.393(5) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C18 1.392(5) . ?
C17 C22 1.402(4) . ?
C18 C19 1.397(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.388(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.386(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.393(4) . ?
C23 C28 1.400(5) . ?
C24 C25 1.386(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.367(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.391(5) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(5) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.391(5) . ?
C29 C34 1.394(5) . ?
C30 C31 1.397(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.383(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.382(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.385(4) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.399(5) . ?
C35 C40 1.405(4) . ?
C36 C37 1.383(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.386(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.387(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.381(5) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 C46 1.395(5) . ?
C41 C42 1.399(4) . ?
C42 C43 1.391(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.387(5) . ?
C43 H43 0.9500 . ?
C44 C45 1.380(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.389(5) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
Cl1S C1S 1.763(4) . ?
C1S Cl3S 1.754(4) . ?
C1S Cl2S 1.767(3) . ?
C1S H1S 1.0000 . ?

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
C48 Re1 C47 88.73(15) . . ?
C48 Re1 N1 98.01(13) . . ?
C47 Re1 N1 172.90(13) . . ?
C48 Re1 O1 172.06(12) . . ?
C47 Re1 O1 99.20(12) . . ?
N1 Re1 O1 74.05(9) . . ?
C48 Re1 P1 91.44(10) . . ?
C47 Re1 P1 87.96(10) . . ?
N1 Re1 P1 94.10(7) . . ?
O1 Re1 P1 89.25(6) . . ?
C48 Re1 P2 93.90(10) . . ?
C47 Re1 P2 87.88(10) . . ?
N1 Re1 P2 89.40(7) . . ?
O1 Re1 P2 86.05(6) . . ?
P1 Re1 P2 173.15(3) . . ?
C17 P1 C11 105.23(16) . . ?
C17 P1 C23 101.66(15) . . ?
C11 P1 C23 101.38(15) . . ?
C17 P1 Re1 114.70(11) . . ?
C11 P1 Re1 117.84(11) . . ?
C23 P1 Re1 113.98(11) . . ?
C1 O1 Re1 118.9(2) . . ?
N2 N1 C2 110.7(3) . . ?
N2 N1 Re1 133.7(2) . . ?
C2 N1 Re1 115.3(2) . . ?
O2 C1 O1 125.5(3) . . ?
O2 C1 C2 120.6(3) . . ?
O1 C1 C2 113.9(3) . . ?
C35 P2 C41 103.47(15) . . ?
C35 P2 C29 102.65(15) . . ?
C41 P2 C29 103.22(15) . . ?
C35 P2 Re1 114.71(11) . . ?
C41 P2 Re1 114.62(11) . . ?
C29 P2 Re1 116.44(11) . . ?
N1 N2 N3 105.1(3) . . ?
N1 C2 C3 107.4(3) . . ?
N1 C2 C1 117.4(3) . . ?
C3 C2 C1 135.1(3) . . ?
C3 N3 N2 112.0(3) . . ?
C3 N3 C4 128.8(3) . . ?
N2 N3 C4 119.2(3) . . ?
N3 C3 C2 104.8(3) . . ?
N3 C3 H3 127.6 . . ?
C2 C3 H3 127.6 . . ?
N3 C4 C5 112.2(3) . . ?
N3 C4 H4A 109.2 . . ?
C5 C4 H4A 109.2 . . ?
N3 C4 H4B 109.2 . . ?
C5 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C10 118.9(3) . . ?
C6 C5 C4 120.4(3) . . ?
C10 C5 C4 120.7(3) . . ?
C7 C6 C5 120.7(3) . . ?
C7 C6 H6 119.6 . . ?
C5 C6 H6 119.6 . . ?
C8 C7 C6 120.3(4) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 119.7(4) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C9 C10 120.3(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C5 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C5 C10 H10 120.0 . . ?
C16 C11 C12 118.4(3) . . ?
C16 C11 P1 119.4(3) . . ?
C12 C11 P1 122.1(3) . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C14 C13 C12 121.3(3) . . ?
C14 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
C13 C14 C15 118.8(3) . . ?
C13 C14 H14 120.6 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 120.9(3) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 C11 120.1(3) . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
C18 C17 C22 118.1(3) . . ?
C18 C17 P1 125.3(3) . . ?
C22 C17 P1 116.6(3) . . ?
C17 C18 C19 121.0(3) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C20 C19 C18 120.0(4) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 120.0(3) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C17 121.1(3) . . ?
C21 C22 H22 119.5 . . ?
C17 C22 H22 119.5 . . ?
C24 C23 C28 118.8(3) . . ?
C24 C23 P1 122.4(3) . . ?
C28 C23 P1 118.6(3) . . ?
C25 C24 C23 120.4(3) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C26 C25 C24 120.7(3) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C27 119.7(4) . . ?
C25 C26 H26 120.1 . . ?
C27 C26 H26 120.1 . . ?
C28 C27 C26 120.2(4) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C23 120.1(3) . . ?
C27 C28 H28 120.0 . . ?
C23 C28 H28 120.0 . . ?
C30 C29 C34 118.9(3) . . ?
C30 C29 P2 122.0(3) . . ?
C34 C29 P2 119.1(3) . . ?
C29 C30 C31 120.1(4) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C32 C31 C30 120.5(3) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C31 119.5(3) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C32 C33 C34 120.4(4) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C33 C34 C29 120.7(3) . . ?
C33 C34 H34 119.7 . . ?
C29 C34 H34 119.7 . . ?
C36 C35 C40 118.5(3) . . ?
C36 C35 P2 121.3(3) . . ?
C40 C35 P2 120.2(3) . . ?
C37 C36 C35 120.4(3) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 H36 119.8 . . ?
C36 C37 C38 120.6(3) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C37 C38 C39 119.6(4) . . ?
C37 C38 H38 120.2 . . ?
C39 C38 H38 120.2 . . ?
C40 C39 C38 120.4(3) . . ?
C40 C39 H39 119.8 . . ?
C38 C39 H39 119.8 . . ?
C39 C40 C35 120.6(3) . . ?
C39 C40 H40 119.7 . . ?
C35 C40 H40 119.7 . . ?
C46 C41 C42 118.5(3) . . ?
C46 C41 P2 123.0(3) . . ?
C42 C41 P2 118.4(3) . . ?
C43 C42 C41 120.5(3) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C44 C43 C42 120.3(3) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C45 C44 C43 119.4(3) . . ?
C45 C44 H44 120.3 . . ?
C43 C44 H44 120.3 . . ?
C44 C45 C46 120.8(3) . . ?
C44 C45 H45 119.6 . . ?
C46 C45 H45 119.6 . . ?
C45 C46 C41 120.4(3) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
O3 C47 Re1 179.1(3) . . ?
O4 C48 Re1 178.4(3) . . ?
Cl3S C1S Cl1S 111.3(2) . . ?
Cl3S C1S Cl2S 110.58(19) . . ?
Cl1S C1S Cl2S 110.2(2) . . ?
Cl3S C1S H1S 108.2 . . ?
Cl1S C1S H1S 108.2 . . ?
Cl2S C1S H1S 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 O1 C1 O2 -172.4(3) . . . . ?
Re1 O1 C1 C2 6.7(4) . . . . ?
C2 N1 N2 N3 0.3(3) . . . . ?
Re1 N1 N2 N3 -173.0(2) . . . . ?
N2 N1 C2 C3 -0.3(4) . . . . ?
Re1 N1 C2 C3 174.3(2) . . . . ?
N2 N1 C2 C1 -176.5(3) . . . . ?
Re1 N1 C2 C1 -1.9(4) . . . . ?
O2 C1 C2 N1 176.0(3) . . . . ?
O1 C1 C2 N1 -3.1(4) . . . . ?
O2 C1 C2 C3 1.2(6) . . . . ?
O1 C1 C2 C3 -177.9(3) . . . . ?
N1 N2 N3 C3 -0.1(4) . . . . ?
N1 N2 N3 C4 178.3(3) . . . . ?
N2 N3 C3 C2 -0.1(4) . . . . ?
C4 N3 C3 C2 -178.3(3) . . . . ?
N1 C2 C3 N3 0.2(4) . . . . ?
C1 C2 C3 N3 175.4(3) . . . . ?
C3 N3 C4 C5 -69.9(4) . . . . ?
N2 N3 C4 C5 112.0(3) . . . . ?
N3 C4 C5 C6 110.2(4) . . . . ?
N3 C4 C5 C10 -68.3(4) . . . . ?
C10 C5 C6 C7 -0.6(5) . . . . ?
C4 C5 C6 C7 -179.1(3) . . . . ?
C5 C6 C7 C8 2.2(6) . . . . ?
C6 C7 C8 C9 -1.5(6) . . . . ?
C7 C8 C9 C10 -0.8(6) . . . . ?
C8 C9 C10 C5 2.4(6) . . . . ?
C6 C5 C10 C9 -1.7(5) . . . . ?
C4 C5 C10 C9 176.8(3) . . . . ?
C17 P1 C11 C16 -68.5(3) . . . . ?
C23 P1 C11 C16 -174.1(3) . . . . ?
Re1 P1 C11 C16 60.8(3) . . . . ?
C17 P1 C11 C12 114.7(3) . . . . ?
C23 P1 C11 C12 9.1(3) . . . . ?
Re1 P1 C11 C12 -116.0(3) . . . . ?
C16 C11 C12 C13 1.2(5) . . . . ?
P1 C11 C12 C13 178.1(3) . . . . ?
C11 C12 C13 C14 0.5(5) . . . . ?
C12 C13 C14 C15 -1.1(5) . . . . ?
C13 C14 C15 C16 0.0(5) . . . . ?
C14 C15 C16 C11 1.7(5) . . . . ?
C12 C11 C16 C15 -2.3(5) . . . . ?
P1 C11 C16 C15 -179.2(3) . . . . ?
C11 P1 C17 C18 4.8(3) . . . . ?
C23 P1 C17 C18 110.2(3) . . . . ?
Re1 P1 C17 C18 -126.3(3) . . . . ?
C11 P1 C17 C22 -173.0(3) . . . . ?
C23 P1 C17 C22 -67.6(3) . . . . ?
Re1 P1 C17 C22 55.9(3) . . . . ?
C22 C17 C18 C19 0.5(5) . . . . ?
P1 C17 C18 C19 -177.3(3) . . . . ?
C17 C18 C19 C20 1.6(5) . . . . ?
C18 C19 C20 C21 -2.0(5) . . . . ?
C19 C20 C21 C22 0.3(6) . . . . ?
C20 C21 C22 C17 1.8(5) . . . . ?
C18 C17 C22 C21 -2.2(5) . . . . ?
P1 C17 C22 C21 175.8(3) . . . . ?
C17 P1 C23 C24 -13.3(3) . . . . ?
C11 P1 C23 C24 95.1(3) . . . . ?
Re1 P1 C23 C24 -137.2(2) . . . . ?
C17 P1 C23 C28 171.9(3) . . . . ?
C11 P1 C23 C28 -79.7(3) . . . . ?
Re1 P1 C23 C28 47.9(3) . . . . ?
C28 C23 C24 C25 0.7(5) . . . . ?
P1 C23 C24 C25 -174.2(3) . . . . ?
C23 C24 C25 C26 1.5(5) . . . . ?
C24 C25 C26 C27 -2.3(5) . . . . ?
C25 C26 C27 C28 1.0(5) . . . . ?
C26 C27 C28 C23 1.1(5) . . . . ?
C24 C23 C28 C27 -1.9(5) . . . . ?
P1 C23 C28 C27 173.1(3) . . . . ?
C35 P2 C29 C30 -15.5(3) . . . . ?
C41 P2 C29 C30 -122.8(3) . . . . ?
Re1 P2 C29 C30 110.7(3) . . . . ?
C35 P2 C29 C34 167.6(3) . . . . ?
C41 P2 C29 C34 60.2(3) . . . . ?
Re1 P2 C29 C34 -66.3(3) . . . . ?
C34 C29 C30 C31 -0.4(5) . . . . ?
P2 C29 C30 C31 -177.3(3) . . . . ?
C29 C30 C31 C32 0.6(5) . . . . ?
C30 C31 C32 C33 -0.8(5) . . . . ?
C31 C32 C33 C34 0.9(5) . . . . ?
C32 C33 C34 C29 -0.7(5) . . . . ?
C30 C29 C34 C33 0.4(5) . . . . ?
P2 C29 C34 C33 177.5(3) . . . . ?
C41 P2 C35 C36 -143.7(3) . . . . ?
C29 P2 C35 C36 109.2(3) . . . . ?
Re1 P2 C35 C36 -18.1(3) . . . . ?
C41 P2 C35 C40 38.4(3) . . . . ?
C29 P2 C35 C40 -68.8(3) . . . . ?
Re1 P2 C35 C40 164.0(2) . . . . ?
C40 C35 C36 C37 -1.7(5) . . . . ?
P2 C35 C36 C37 -179.7(2) . . . . ?
C35 C36 C37 C38 1.7(5) . . . . ?
C36 C37 C38 C39 -0.2(5) . . . . ?
C37 C38 C39 C40 -1.1(5) . . . . ?
C38 C39 C40 C35 1.1(5) . . . . ?
C36 C35 C40 C39 0.3(5) . . . . ?
P2 C35 C40 C39 178.4(3) . . . . ?
C35 P2 C41 C46 -100.9(3) . . . . ?
C29 P2 C41 C46 5.8(3) . . . . ?
Re1 P2 C41 C46 133.5(3) . . . . ?
C35 P2 C41 C42 80.3(3) . . . . ?
C29 P2 C41 C42 -173.0(3) . . . . ?
Re1 P2 C41 C42 -45.3(3) . . . . ?
C46 C41 C42 C43 -2.7(5) . . . . ?
P2 C41 C42 C43 176.1(3) . . . . ?
C41 C42 C43 C44 0.5(5) . . . . ?
C42 C43 C44 C45 1.3(5) . . . . ?
C43 C44 C45 C46 -0.8(5) . . . . ?
C44 C45 C46 C41 -1.5(6) . . . . ?
C42 C41 C46 C45 3.2(5) . . . . ?
P2 C41 C46 C45 -175.6(3) . . . . ?

_refine_diff_density_max         0.753
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.122

_shelxl_version_number           2013-4

_diffrn_standards_decay_%        0.0
_symmetry_cell_setting           ?
_symmetry_space_group_name_h-m   ?
_symmetry_int_tables_number      ?

_chemical_absolute_configuration rmad

_database_code_depnum_ccdc_archive 'CCDC 983206'
