# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_x
_database_code_depnum_ccdc_archive 'CCDC 1468795'
_audit_update_record             
;
2016-03-15 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;

_audit_creation_date             2016-03-14T17:39:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        ?
_chemical_name_common            Re-L0
_chemical_formula_moiety         'C23 H30 Cl N2 O9 P2 Re'
_chemical_formula_sum            'C23 H30 Cl N2 O9 P2 Re'
_chemical_formula_weight         762.08

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5189(8)
_cell_length_b                   12.2876(8)
_cell_length_c                   12.3796(8)
_cell_angle_alpha                60.874(7)
_cell_angle_beta                 71.142(7)
_cell_angle_gamma                72.476(6)
_cell_volume                     1426.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7099
_cell_measurement_theta_min      3.804
_cell_measurement_theta_max      27.86

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.1406
_exptl_crystal_size_mid          0.1214
_exptl_crystal_size_min          0.0799
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_F_000             752
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-16 -2 -7 0.037
16 3 8 0.0586
1 14 15 0.0537
0 -12 -16 0.0731
-4 8 -9 0.0311
5 -6 10 0.0429
9 11 -3 0.0457
-8 -7 7 0.0426
5 17 10 0.0476
-9 -16 -12 0.0704
-6 -12 -17 0.0612
-9 9 -5 0.0216
10 11 16 0.0608
-13 -3 5 0.0346

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.517
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.86999
_exptl_absorpt_correction_T_max  1
_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_detector_area_resol_mean 10.3385
_diffrn_orient_matrix_ub_11      0.0158571
_diffrn_orient_matrix_ub_12      -0.0579284
_diffrn_orient_matrix_ub_13      0.0516604
_diffrn_orient_matrix_ub_21      -0.0639815
_diffrn_orient_matrix_ub_22      -0.0047133
_diffrn_orient_matrix_ub_23      0.0250043
_diffrn_orient_matrix_ub_31      0.0045974
_diffrn_orient_matrix_ub_32      -0.0335407
_diffrn_orient_matrix_ub_33      -0.0347935
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_number            14520
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.416
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_number_total             5826
_reflns_number_gt                5136
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0267P)²+1.1045P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5826
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0654
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.137

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9866(4) 0.8275(4) 0.5677(5) 0.0258(10) Uani 1 d . .
C2 C 0.9311(4) 0.5915(5) 0.6714(4) 0.0270(10) Uani 1 d . .
C3 C 0.8454(5) 0.7266(5) 0.8047(5) 0.0295(11) Uani 1 d . .
C4 C 0.6936(4) 1.0091(4) 0.6580(4) 0.0230(10) Uani 1 d . .
H4 H 0.7168 0.9697 0.7357 0.028 Uiso 1 calc . .
C5 C 0.6324(4) 1.1326(4) 0.6176(4) 0.0221(10) Uani 1 d . .
H5 H 0.6145 1.1748 0.6678 0.026 Uiso 1 calc . .
C6 C 0.5975(4) 1.1940(4) 0.5016(4) 0.0199(9) Uani 1 d . .
C7 C 0.6219(4) 1.1242(4) 0.4334(4) 0.0199(9) Uani 1 d . .
H7 H 0.5974 1.1611 0.3567 0.024 Uiso 1 calc . .
C8 C 0.6825(4) 1.0000(4) 0.4796(4) 0.0181(9) Uani 1 d . .
C9 C 0.7131(4) 0.9190(4) 0.4132(4) 0.0165(9) Uani 1 d . .
C10 C 0.6652(4) 0.9515(4) 0.3099(4) 0.0207(9) Uani 1 d . .
H10 H 0.6112 1.0278 0.279 0.025 Uiso 1 calc . .
C11 C 0.6979(4) 0.8701(4) 0.2524(4) 0.0197(9) Uani 1 d . .
C12 C 0.7818(4) 0.7603(4) 0.2990(4) 0.0231(10) Uani 1 d . .
H12 H 0.8084 0.7052 0.2611 0.028 Uiso 1 calc . .
C13 C 0.8262(4) 0.7327(4) 0.4028(4) 0.0228(10) Uani 1 d . .
H13 H 0.8819 0.6578 0.4336 0.027 Uiso 1 calc . .
C14 C 0.5392(4) 1.3305(4) 0.4519(4) 0.0242(10) Uani 1 d . .
H14A H 0.489 1.3495 0.5224 0.029 Uiso 1 calc . .
H14B H 0.4844 1.3465 0.3987 0.029 Uiso 1 calc . .
C15 C 0.6451(4) 0.9011(4) 0.1421(4) 0.0245(10) Uani 1 d . .
H15A H 0.5551 0.9219 0.1647 0.029 Uiso 1 calc . .
H15B H 0.6646 0.826 0.1278 0.029 Uiso 1 calc . .
N1 N 0.7927(3) 0.8087(3) 0.4607(3) 0.0185(8) Uani 1 d . .
N2 N 0.7212(3) 0.9433(3) 0.5901(3) 0.0188(8) Uani 1 d . .
O1 O 1.0742(3) 0.8664(4) 0.5339(4) 0.0454(10) Uani 1 d . .
O2 O 0.9890(3) 0.4920(3) 0.6881(4) 0.0419(9) Uani 1 d . .
O3 O 0.8477(4) 0.7118(4) 0.9032(3) 0.0471(10) Uani 1 d . .
O4 O 0.5992(3) 1.5689(3) 0.3194(3) 0.0365(9) Uani 1 d . .
O5 O 0.7224(3) 1.3882(3) 0.2557(3) 0.0411(9) Uani 1 d . .
O6 O 0.7517(3) 1.3863(3) 0.4454(3) 0.0353(8) Uani 1 d . .
O7 O 0.6585(4) 1.1493(3) 0.0220(3) 0.0429(9) Uani 1 d . .
O8 O 0.8441(3) 1.0116(4) -0.0158(3) 0.0412(9) Uani 1 d . .
O9 O 0.6611(3) 1.0388(3) -0.1096(3) 0.0378(9) Uani 1 d . .
P1 P 0.65217(12) 1.43364(12) 0.36229(12) 0.0290(3) Uani 1 d . .
P2 P 0.70037(12) 1.02928(12) -0.00385(11) 0.0272(3) Uani 1 d . .
Cl1 Cl 0.63595(12) 0.67977(13) 0.72925(12) 0.0371(3) Uani 1 d . .
Re1 Re 0.83521(2) 0.75645(2) 0.64098(2) 0.02093(7) Uani 1 d . .
C18 C 0.7227(5) 1.4201(5) 0.5496(5) 0.0382(13) Uani 1 d . .
H18A H 0.6386 1.4084 0.5975 0.046 Uiso 1 calc . .
H18B H 0.7285 1.5082 0.5175 0.046 Uiso 1 calc . .
C19 C 0.8146(5) 1.3364(7) 0.6330(6) 0.0541(17) Uani 1 d . .
H19A H 0.797 1.3573 0.7026 0.081 Uiso 1 calc . .
H19B H 0.8975 1.349 0.5849 0.081 Uiso 1 calc . .
H19C H 0.8079 1.2495 0.6646 0.081 Uiso 1 calc . .
C21 C 0.9926(6) 0.9786(7) -0.1903(6) 0.063(2) Uani 1 d . .
H21A H 1.0509 0.9146 -0.2128 0.094 Uiso 1 calc . .
H21B H 1.0358 1.0419 -0.2051 0.094 Uiso 1 calc . .
H21C H 0.9307 1.017 -0.2409 0.094 Uiso 1 calc . .
C20 C 0.9310(6) 0.9201(7) -0.0536(6) 0.0578(17) Uani 1 d . .
H20A H 0.8883 0.8554 -0.0387 0.069 Uiso 1 calc . .
H20B H 0.9939 0.8797 -0.0028 0.069 Uiso 1 calc . .
C16 C 0.8220(6) 1.4407(7) 0.1575(5) 0.0586(18) Uani 1 d . .
H16A H 0.8979 1.409 0.1894 0.07 Uiso 1 calc . .
H16B H 0.8045 1.5321 0.1258 0.07 Uiso 1 calc . .
C17 C 0.8382(7) 1.4052(6) 0.0533(6) 0.0626(19) Uani 1 d . .
H17A H 0.9054 1.4413 -0.0142 0.094 Uiso 1 calc . .
H17B H 0.7628 1.4368 0.0222 0.094 Uiso 1 calc . .
H17C H 0.8569 1.3148 0.0849 0.094 Uiso 1 calc . .
C22 C 0.5396(7) 1.2329(8) -0.0031(10) 0.093(3) Uani 1 d . .
H22A H 0.5132 1.2192 -0.0618 0.111 Uiso 1 calc . .
H22B H 0.4773 1.2104 0.0752 0.111 Uiso 1 calc . .
C23 C 0.5446(9) 1.3601(8) -0.0530(9) 0.121(4) Uani 1 d . .
H23A H 0.4641 1.4095 -0.0673 0.182 Uiso 1 calc . .
H23B H 0.6046 1.3839 -0.1317 0.182 Uiso 1 calc . .
H23C H 0.5686 1.3751 0.0053 0.182 Uiso 1 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.115(5) . ?
C1 Re1 1.936(5) . ?
C2 O2 1.155(6) . ?
C2 Re1 1.910(5) . ?
C3 O3 1.151(6) . ?
C3 Re1 1.913(5) . ?
C4 N2 1.341(5) . ?
C4 C5 1.376(6) . ?
C5 C6 1.389(6) . ?
C6 C7 1.391(6) . ?
C6 C14 1.493(6) . ?
C7 C8 1.382(6) . ?
C8 N2 1.354(5) . ?
C8 C9 1.480(5) . ?
C9 N1 1.359(5) . ?
C9 C10 1.387(6) . ?
C10 C11 1.394(6) . ?
C11 C12 1.380(6) . ?
C11 C15 1.507(6) . ?
C12 C13 1.387(6) . ?
C13 N1 1.338(5) . ?
C14 P1 1.795(5) . ?
C15 P2 1.800(5) . ?
N1 Re1 2.181(3) . ?
N2 Re1 2.169(4) . ?
O4 P1 1.469(4) . ?
O5 C16 1.411(6) . ?
O5 P1 1.569(3) . ?
O6 C18 1.452(6) . ?
O6 P1 1.578(4) . ?
O7 C22 1.464(9) . ?
O7 P2 1.563(3) . ?
O8 C20 1.421(7) . ?
O8 P2 1.570(4) . ?
O9 P2 1.461(3) . ?
Cl1 Re1 2.4554(12) . ?
C18 C19 1.503(8) . ?
C21 C20 1.494(8) . ?
C16 C17 1.494(8) . ?
C22 C23 1.385(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Re1 175.0(4) . . ?
O2 C2 Re1 179.0(4) . . ?
O3 C3 Re1 177.6(5) . . ?
N2 C4 C5 122.7(4) . . ?
C4 C5 C6 119.8(4) . . ?
C5 C6 C7 117.4(4) . . ?
C5 C6 C14 120.6(4) . . ?
C7 C6 C14 121.9(4) . . ?
C8 C7 C6 120.1(4) . . ?
N2 C8 C7 121.8(4) . . ?
N2 C8 C9 114.4(4) . . ?
C7 C8 C9 123.8(4) . . ?
N1 C9 C10 121.6(4) . . ?
N1 C9 C8 115.1(4) . . ?
C10 C9 C8 123.3(4) . . ?
C9 C10 C11 120.1(4) . . ?
C12 C11 C10 117.6(4) . . ?
C12 C11 C15 120.9(4) . . ?
C10 C11 C15 121.4(4) . . ?
C11 C12 C13 119.6(4) . . ?
N1 C13 C12 123.1(4) . . ?
C6 C14 P1 112.7(3) . . ?
C11 C15 P2 115.2(3) . . ?
C13 N1 C9 117.8(4) . . ?
C13 N1 Re1 124.4(3) . . ?
C9 N1 Re1 117.1(2) . . ?
C4 N2 C8 118.1(4) . . ?
C4 N2 Re1 123.5(3) . . ?
C8 N2 Re1 118.3(3) . . ?
C16 O5 P1 124.2(3) . . ?
C18 O6 P1 119.1(3) . . ?
C22 O7 P2 120.5(4) . . ?
C20 O8 P2 121.8(4) . . ?
O4 P1 O5 116.1(2) . . ?
O4 P1 O6 114.2(2) . . ?
O5 P1 O6 103.2(2) . . ?
O4 P1 C14 114.4(2) . . ?
O5 P1 C14 101.10(19) . . ?
O6 P1 C14 106.2(2) . . ?
O9 P2 O7 116.3(2) . . ?
O9 P2 O8 117.00(19) . . ?
O7 P2 O8 98.1(2) . . ?
O9 P2 C15 111.3(2) . . ?
O7 P2 C15 106.3(2) . . ?
O8 P2 C15 106.5(2) . . ?
C2 Re1 C3 88.2(2) . . ?
C2 Re1 C1 90.25(19) . . ?
C3 Re1 C1 89.8(2) . . ?
C2 Re1 N2 173.87(16) . . ?
C3 Re1 N2 97.68(17) . . ?
C1 Re1 N2 91.45(16) . . ?
C2 Re1 N1 99.77(16) . . ?
C3 Re1 N1 170.36(17) . . ?
C1 Re1 N1 95.53(17) . . ?
N2 Re1 N1 74.21(12) . . ?
C2 Re1 Cl1 93.26(14) . . ?
C3 Re1 Cl1 90.92(15) . . ?
C1 Re1 Cl1 176.44(14) . . ?
N2 Re1 Cl1 85.00(9) . . ?
N1 Re1 Cl1 83.30(9) . . ?
O6 C18 C19 108.1(4) . . ?
O8 C20 C21 111.5(6) . . ?
O5 C16 C17 109.1(5) . . ?
C23 C22 O7 113.7(7) . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx_x
_database_code_depnum_ccdc_archive 'CCDC 1468796'
_audit_update_record             
;
2016-03-15 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;

_audit_creation_date             2016-03-14T18:29:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_chemical_name_common            Re-L0_OH
_chemical_formula_moiety         'C15 H14 Br N2 O9 P2 Re, 2(C H4 O)'
_chemical_formula_sum            'C17 H22 Br N2 O11 P2 Re'
_chemical_formula_weight         758.41

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.2650(2)
_cell_length_b                   14.0611(7)
_cell_length_c                   15.4117(6)
_cell_angle_alpha                68.954(4)
_cell_angle_beta                 82.163(3)
_cell_angle_gamma                81.699(4)
_cell_volume                     1248.56(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6926
_cell_measurement_theta_min      3.372
_cell_measurement_theta_max      76.058

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.1982
_exptl_crystal_size_mid          0.0398
_exptl_crystal_size_min          0.0396
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_F_000             732
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -5 -7 0.0322
3 5 7 0.0232
-3 2 7 0.1233
3 -2 -7 0.0671
-1 7 -2 0.0194
1 -7 2 0.0232
2 9 6 0.0396
-2 -9 -6 0.0396
3 6 4 0.0269
-3 -6 -4 0.0129
-1 5 -5 0.0239
1 -5 5 0.0156

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    13.134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.72504
_exptl_absorpt_correction_T_max  1
_exptl_crystal_description       fragment
_exptl_crystal_colour            orange

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_monochromator  mirror
_diffrn_detector_area_resol_mean 10.3385
_diffrn_orient_matrix_ub_11      0.1106051
_diffrn_orient_matrix_ub_12      0.0724913
_diffrn_orient_matrix_ub_13      0.0303715
_diffrn_orient_matrix_ub_21      -0.1075414
_diffrn_orient_matrix_ub_22      0.0929805
_diffrn_orient_matrix_ub_23      -0.0750587
_diffrn_orient_matrix_ub_31      -0.1961556
_diffrn_orient_matrix_ub_32      0.0053936
_diffrn_orient_matrix_ub_33      0.0707969
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_number            11751
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         7.432
_diffrn_reflns_theta_max         74.488
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_reflns_number_total             5093
_reflns_number_gt                4530
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0432P)²+2.2876P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5093
_refine_ls_number_parameters     333
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0871
_refine_ls_wR_factor_gt          0.0851
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.196
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.15

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1031(8) 0.7666(4) 0.1389(3) 0.0227(9) Uani 1 d . .
H1 H 0.1395 0.8296 0.0966 0.027 Uiso 1 calc . .
C2 C 0.2095(8) 0.7219(4) 0.2199(3) 0.0227(9) Uani 1 d . .
H2 H 0.3185 0.754 0.2301 0.027 Uiso 1 calc . .
C3 C 0.1529(8) 0.6296(4) 0.2852(3) 0.0231(10) Uani 1 d . .
C4 C -0.0055(8) 0.5828(4) 0.2654(3) 0.0223(9) Uani 1 d . .
H4 H -0.0465 0.5206 0.3077 0.027 Uiso 1 calc . .
C5 C -0.1035(8) 0.6289(4) 0.1820(3) 0.0212(9) Uani 1 d . .
C6 C -0.2743(8) 0.5850(4) 0.1562(3) 0.0187(9) Uani 1 d . .
C7 C -0.5461(8) 0.6159(4) 0.0581(3) 0.0209(9) Uani 1 d . .
H7 H -0.6245 0.6607 0.0099 0.025 Uiso 1 calc . .
C8 C -0.6037(8) 0.5162(4) 0.1025(3) 0.0222(10) Uani 1 d . .
H8 H -0.7201 0.4959 0.0844 0.027 Uiso 1 calc . .
C9 C -0.4870(8) 0.4479(4) 0.1734(3) 0.0228(10) Uani 1 d . .
C10 C -0.3192(9) 0.4838(4) 0.2008(4) 0.0242(10) Uani 1 d . .
H10 H -0.2382 0.4401 0.2486 0.029 Uiso 1 calc . .
C11 C -0.5321(9) 0.3378(4) 0.2135(4) 0.0249(10) Uani 1 d . .
H11A H -0.412 0.2971 0.1924 0.03 Uiso 1 calc . .
H11B H -0.6604 0.3312 0.1881 0.03 Uiso 1 calc . .
C12 C 0.2578(9) 0.5841(4) 0.3757(4) 0.0249(10) Uani 1 d . .
H12A H 0.4138 0.5836 0.3627 0.03 Uiso 1 calc . .
H12B H 0.2248 0.5138 0.4067 0.03 Uiso 1 calc . .
C13 C -0.4337(9) 0.8445(4) -0.0979(4) 0.0275(11) Uani 1 d . .
C14 C -0.0837(9) 0.9083(4) -0.0637(4) 0.0269(11) Uani 1 d . .
C17 C 0.6917(17) 0.8775(7) 0.3192(7) 0.069(3) Uani 1 d . .
H17A H 0.6702 0.9016 0.371 0.103 Uiso 1 calc . .
H17B H 0.6056 0.9223 0.2706 0.103 Uiso 1 calc . .
H17C H 0.8419 0.8768 0.2959 0.103 Uiso 1 calc . .
C18 C 0.061(2) 0.9199(13) 0.6683(17) 0.163(10) Uani 1 d . .
H18A H -0.0711 0.9453 0.6961 0.244 Uiso 1 calc . .
H18B H 0.1317 0.9764 0.6244 0.244 Uiso 1 calc . .
H18C H 0.1543 0.881 0.7161 0.244 Uiso 1 calc . .
N1 N -0.3811(7) 0.6492(3) 0.0829(3) 0.0208(8) Uani 1 d . .
N2 N -0.0514(6) 0.7208(3) 0.1204(3) 0.0176(7) Uani 1 d . .
O1 O 0.2861(8) 0.5993(3) 0.5399(3) 0.0348(9) Uani 1 d . .
H1A H 0.3199 0.6412 0.56 0.052 Uiso 1 calc . .
O2 O -0.0771(7) 0.6599(4) 0.4719(3) 0.0348(9) Uani 1 d . .
O3 O 0.2318(7) 0.7659(3) 0.4049(3) 0.0332(9) Uani 1 d . .
H3 H 0.3623 0.7631 0.389 0.05 Uiso 1 calc . .
O4 O -0.5435(7) 0.8739(3) -0.1559(3) 0.0377(9) Uani 1 d . .
O5 O 0.0123(8) 0.9775(3) -0.1014(3) 0.0396(10) Uani 1 d . .
O7 O -0.3718(7) 0.2847(3) 0.3813(3) 0.0362(9) Uani 1 d . .
O8 O -0.7708(7) 0.3533(3) 0.3622(3) 0.0355(9) Uani 1 d . .
H8A H -0.7952 0.3365 0.4191 0.053 Uiso 1 calc . .
O9 O -0.6288(7) 0.1738(3) 0.3657(3) 0.0353(9) Uani 1 d . .
H9 H -0.7587 0.1743 0.3629 0.053 Uiso 1 calc . .
O10 O 0.6285(8) 0.7766(4) 0.3489(4) 0.0473(11) Uani 1 d . .
H10A H 0.6938 0.7397 0.3938 0.071 Uiso 1 calc . .
O11 O 0.0136(11) 0.8576(6) 0.6225(7) 0.085(2) Uani 1 d . .
H11 H 0.0743 0.8752 0.5694 0.127 Uiso 1 calc . .
P1 P 0.1636(2) 0.65608(11) 0.45187(9) 0.0255(3) Uani 1 d . .
P2 P -0.5723(2) 0.28479(10) 0.33824(9) 0.0257(3) Uani 1 d . .
Br1A Br -0.00238(9) 0.67406(5) -0.07916(4) 0.0254(2) Uani 0.926(4) d A 1
C16A C -0.4189(16) 0.8740(7) 0.0654(6) 0.0248(18) Uani 0.926(4) d A 1
O6A O -0.5172(11) 0.9225(5) 0.1055(5) 0.0293(14) Uani 0.926(4) d A 1
Br1B Br -0.438(3) 0.8910(12) 0.0976(11) 0.033(3) Uani 0.074(4) d A 2
C16B C -0.046(13) 0.725(7) -0.079(6) 0.05(2) Uiso 0.074(4) d A 2
O6B O 0.045(10) 0.681(5) -0.122(5) 0.043(16) Uiso 0.074(4) d A 2
Re1 Re -0.24331(3) 0.79228(2) 0.00221(2) 0.01950(8) Uani 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.349(6) . ?
C1 C2 1.392(7) . ?
C2 C3 1.386(8) . ?
C3 C4 1.388(7) . ?
C3 C12 1.508(7) . ?
C4 C5 1.396(7) . ?
C5 N2 1.354(7) . ?
C5 C6 1.473(6) . ?
C6 N1 1.356(6) . ?
C6 C10 1.392(7) . ?
C7 N1 1.345(6) . ?
C7 C8 1.398(7) . ?
C8 C9 1.382(8) . ?
C9 C10 1.402(7) . ?
C9 C11 1.500(7) . ?
C11 P2 1.792(5) . ?
C12 P1 1.801(5) . ?
C13 O4 1.124(7) . ?
C13 Re1 1.943(5) . ?
C14 O5 1.146(7) . ?
C14 Re1 1.923(6) . ?
C17 O10 1.423(10) . ?
C18 O11 1.389(15) . ?
N1 Re1 2.179(4) . ?
N2 Re1 2.169(4) . ?
O1 P1 1.548(4) . ?
O2 P1 1.495(4) . ?
O3 P1 1.548(4) . ?
O7 P2 1.499(4) . ?
O8 P2 1.547(4) . ?
O9 P2 1.544(4) . ?
Br1A Re1 2.6213(7) . ?
C16A O6A 1.141(13) . ?
C16A Re1 1.905(11) . ?
Br1B Re1 2.463(19) . ?
C16B O6B 1.103(10) . ?
C16B Re1 2.022(10) . ?

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
N2 C1 C2 121.7(5) . . ?
C3 C2 C1 120.0(5) . . ?
C2 C3 C4 117.9(5) . . ?
C2 C3 C12 120.2(5) . . ?
C4 C3 C12 121.8(5) . . ?
C3 C4 C5 120.1(5) . . ?
N2 C5 C4 121.2(4) . . ?
N2 C5 C6 115.2(4) . . ?
C4 C5 C6 123.5(5) . . ?
N1 C6 C10 121.7(4) . . ?
N1 C6 C5 115.2(4) . . ?
C10 C6 C5 123.1(4) . . ?
N1 C7 C8 122.2(5) . . ?
C9 C8 C7 119.8(4) . . ?
C8 C9 C10 117.8(5) . . ?
C8 C9 C11 119.8(4) . . ?
C10 C9 C11 122.3(5) . . ?
C6 C10 C9 119.8(5) . . ?
C9 C11 P2 115.8(3) . . ?
C3 C12 P1 111.2(4) . . ?
O4 C13 Re1 179.4(5) . . ?
O5 C14 Re1 178.8(5) . . ?
C7 N1 C6 118.5(4) . . ?
C7 N1 Re1 124.4(3) . . ?
C6 N1 Re1 116.6(3) . . ?
C1 N2 C5 119.0(4) . . ?
C1 N2 Re1 123.4(3) . . ?
C5 N2 Re1 117.3(3) . . ?
O2 P1 O3 110.0(3) . . ?
O2 P1 O1 113.2(3) . . ?
O3 P1 O1 109.6(2) . . ?
O2 P1 C12 110.7(2) . . ?
O3 P1 C12 109.0(2) . . ?
O1 P1 C12 104.2(3) . . ?
O7 P2 O9 109.6(3) . . ?
O7 P2 O8 114.5(3) . . ?
O9 P2 O8 110.2(3) . . ?
O7 P2 C11 110.8(3) . . ?
O9 P2 C11 108.2(2) . . ?
O8 P2 C11 103.2(3) . . ?
O6A C16A Re1 177.2(7) . . ?
O6B C16B Re1 173(8) . . ?
C16A Re1 C14 88.0(3) . . ?
C16A Re1 C13 89.5(3) . . ?
C14 Re1 C13 87.2(2) . . ?
C14 Re1 C16B 84(3) . . ?
C13 Re1 C16B 87(3) . . ?
C16A Re1 N2 90.8(3) . . ?
C14 Re1 N2 98.74(18) . . ?
C13 Re1 N2 174.03(19) . . ?
C16B Re1 N2 93(3) . . ?
C16A Re1 N1 96.5(3) . . ?
C14 Re1 N1 172.05(19) . . ?
C13 Re1 N1 99.4(2) . . ?
C16B Re1 N1 91(3) . . ?
N2 Re1 N1 74.67(15) . . ?
C14 Re1 Br1B 87.7(3) . . ?
C13 Re1 Br1B 96.3(5) . . ?
C16B Re1 Br1B 171(3) . . ?
N2 Re1 Br1B 84.1(4) . . ?
N1 Re1 Br1B 95.9(3) . . ?
C16A Re1 Br1A 177.9(2) . . ?
C14 Re1 Br1A 93.67(16) . . ?
C13 Re1 Br1A 91.84(17) . . ?
N2 Re1 Br1A 87.70(11) . . ?
N1 Re1 Br1A 81.76(11) . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Re-L2
_database_code_depnum_ccdc_archive 'CCDC 1468797'
_audit_update_record             
;
2016-03-15 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;

_audit_creation_date             2016-03-14T16:58:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_chemical_name_common            Re-L2
_chemical_formula_moiety         'C39 H40 Cl N8 O9 P2 Re, C4 H8 O2'
_chemical_formula_sum            'C43 H48 Cl N8 O11 P2 Re'
_chemical_formula_weight         1136.48

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_Int_Tables_number      14
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  '-P 2ybc'
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                   10.6361(8)
_cell_length_b                   37.8192(14)
_cell_length_c                   11.9861(5)
_cell_angle_alpha                90
_cell_angle_beta                 105.124(5)
_cell_angle_gamma                90
_cell_volume                     4654.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5703
_cell_measurement_theta_min      3.342
_cell_measurement_theta_max      27.053

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.1197
_exptl_crystal_size_mid          0.0614
_exptl_crystal_size_min          0.0363
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_F_000             2288
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -51 -2 0.0082
-4 52 1 0.0263
6 -10 -16 0.0487
-2 -26 15 0.0323
13 0 4 0.0084
-13 -23 -2 0.0377
-8 -15 -11 0.0459

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.5315
_exptl_absorpt_correction_T_max  1
_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_detector_area_resol_mean 10.3385
_diffrn_orient_matrix_ub_11      -0.0206176
_diffrn_orient_matrix_ub_12      -0.0177243
_diffrn_orient_matrix_ub_13      -0.0127762
_diffrn_orient_matrix_ub_21      -0.0658749
_diffrn_orient_matrix_ub_22      0.0056097
_diffrn_orient_matrix_ub_23      -0.0141404
_diffrn_orient_matrix_ub_31      0.001641
_diffrn_orient_matrix_ub_32      0.0025263
_diffrn_orient_matrix_ub_33      -0.0582515
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0999
_diffrn_reflns_number            29297
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.522
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_number_total             9492
_reflns_number_gt                7123
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0440P)²+5.0930P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         9492
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1109
_refine_ls_wR_factor_gt          0.0998
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.132

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0493(6) 0.85911(15) 0.2226(5) 0.0301(13) Uani 1 d . .
C2 C -0.0193(6) 0.84139(17) 0.0059(5) 0.0318(14) Uani 1 d . .
C3 C -0.1992(7) 0.86785(16) 0.1071(5) 0.0355(15) Uani 1 d . .
C4 C -0.1583(6) 0.90840(16) -0.1702(4) 0.0308(14) Uani 1 d . .
H4 H -0.1483 0.8847 -0.187 0.037 Uiso 1 calc . .
C5 C -0.2057(6) 0.93115(15) -0.2608(4) 0.0291(13) Uani 1 d . .
H5 H -0.2258 0.923 -0.3366 0.035 Uiso 1 calc . .
C6 C -0.2231(6) 0.96632(15) -0.2375(4) 0.0297(13) Uani 1 d . .
C7 C -0.1897(6) 0.97716(15) -0.1224(4) 0.0280(13) Uani 1 d . .
H7 H -0.199 1.0007 -0.1039 0.034 Uiso 1 calc . .
C8 C -0.1429(6) 0.95278(14) -0.0363(4) 0.0283(13) Uani 1 d . .
C9 C -0.1053(6) 0.96256(14) 0.0882(4) 0.0261(13) Uani 1 d . .
C10 C -0.1206(6) 0.99637(15) 0.1278(4) 0.0275(13) Uani 1 d . .
H10 H -0.155 1.0143 0.0755 0.033 Uiso 1 calc . .
C11 C -0.0846(6) 1.00350(15) 0.2457(4) 0.0264(13) Uani 1 d . .
C12 C -0.0342(6) 0.97540(15) 0.3203(4) 0.0309(14) Uani 1 d . .
H12 H -0.0087 0.9791 0.3998 0.037 Uiso 1 calc . .
C13 C -0.0225(6) 0.94250(15) 0.2760(4) 0.0278(13) Uani 1 d . .
H13 H 0.0112 0.9243 0.3271 0.033 Uiso 1 calc . .
C14 C -0.0953(6) 1.03825(15) 0.2937(4) 0.0281(13) Uani 1 d . .
C15 C -0.2743(6) 0.99217(15) -0.3297(4) 0.0282(13) Uani 1 d . .
C16 C -0.2992(6) 1.02711(15) -0.3188(4) 0.0290(13) Uani 1 d . .
H16 H -0.2875 1.04 -0.2508 0.035 Uiso 1 calc . .
C17 C -0.1329(6) 1.07020(14) 0.2403(4) 0.0258(13) Uani 1 d . .
H17 H -0.16 1.0746 0.1613 0.031 Uiso 1 calc . .
C18 C -0.3891(6) 1.07364(15) -0.4662(4) 0.0286(13) Uani 1 d . .
C19 C -0.4561(6) 1.07939(16) -0.5806(5) 0.0342(14) Uani 1 d . .
H19 H -0.4714 1.0609 -0.6334 0.041 Uiso 1 calc . .
C20 C -0.5001(6) 1.11334(15) -0.6149(5) 0.0354(15) Uani 1 d . .
H20 H -0.5437 1.1175 -0.6918 0.042 Uiso 1 calc . .
C21 C -0.4803(6) 1.14098(16) -0.5372(5) 0.0353(14) Uani 1 d . .
C22 C -0.4113(7) 1.13457(16) -0.4240(5) 0.0371(15) Uani 1 d . .
H22 H -0.3951 1.1532 -0.3715 0.044 Uiso 1 calc . .
C23 C -0.3660(6) 1.10130(16) -0.3875(5) 0.0350(15) Uani 1 d . .
H23 H -0.3207 1.0974 -0.3109 0.042 Uiso 1 calc . .
C24 C -0.2270(7) 1.24161(15) 0.3257(5) 0.0376(15) Uani 1 d . .
H24A H -0.1477 1.2547 0.3288 0.045 Uiso 1 calc . .
H24B H -0.2533 1.247 0.3955 0.045 Uiso 1 calc . .
C25 C -0.1980(6) 1.20223(15) 0.3239(5) 0.0318(14) Uani 1 d . .
C26 C -0.1708(7) 1.18607(16) 0.2275(5) 0.0390(16) Uani 1 d . .
H26 H -0.1694 1.1995 0.1629 0.047 Uiso 1 calc . .
C27 C -0.1464(7) 1.15034(15) 0.2284(5) 0.0357(15) Uani 1 d . .
H27 H -0.1281 1.1397 0.1645 0.043 Uiso 1 calc . .
C28 C -0.1489(6) 1.13022(15) 0.3240(4) 0.0275(13) Uani 1 d . .
C29 C -0.1767(6) 1.14601(15) 0.4186(5) 0.0319(14) Uani 1 d . .
H29 H -0.1788 1.1325 0.4828 0.038 Uiso 1 calc . .
C30 C -0.2010(6) 1.18159(16) 0.4181(4) 0.0305(14) Uani 1 d . .
H30 H -0.2198 1.192 0.4822 0.037 Uiso 1 calc . .
C31 C -0.5298(6) 1.17768(16) -0.5749(5) 0.0373(15) Uani 1 d . .
H31A H -0.5095 1.1834 -0.6471 0.045 Uiso 1 calc . .
H31B H -0.4857 1.1947 -0.5173 0.045 Uiso 1 calc . .
C32 C -0.4525(8) 1.29958(19) 0.3324(6) 0.056(2) Uani 1 d . .
H32A H -0.4554 1.2774 0.372 0.067 Uiso 1 calc . .
H32B H -0.5409 1.3082 0.3037 0.067 Uiso 1 calc . .
C33 C -0.8602(8) 1.2345(2) -0.6606(8) 0.069(2) Uani 1 d . .
H33A H -0.8877 1.2409 -0.5922 0.083 Uiso 1 calc . .
H33B H -0.9183 1.2163 -0.7018 0.083 Uiso 1 calc . .
C34 C -0.5839(8) 1.2339(2) 0.1093(7) 0.062(2) Uani 1 d . .
H34A H -0.6394 1.2524 0.1266 0.075 Uiso 1 calc . .
H34B H -0.5605 1.2404 0.0389 0.075 Uiso 1 calc . .
C35 C -0.7483(12) 1.1179(3) -0.4045(9) 0.092(3) Uani 1 d . .
H35A H -0.8094 1.1014 -0.3878 0.138 Uiso 1 calc . .
H35B H -0.678 1.1214 -0.3366 0.138 Uiso 1 calc . .
H35C H -0.7146 1.1088 -0.4657 0.138 Uiso 1 calc . .
C36 C -0.8148(9) 1.1522(3) -0.4409(8) 0.077(3) Uani 1 d . .
H36A H -0.8874 1.1485 -0.5081 0.092 Uiso 1 calc . .
H36B H -0.849 1.1614 -0.3792 0.092 Uiso 1 calc . .
C37 C 0.5168(10) 0.9612(3) 0.1073(9) 0.078(3) Uani 1 d . .
C38 C -0.6530(9) 1.2003(2) 0.0935(7) 0.075(3) Uani 1 d . .
H38A H -0.7307 1.2023 0.0314 0.113 Uiso 1 calc . .
H38B H -0.6759 1.1941 0.1634 0.113 Uiso 1 calc . .
H38C H -0.598 1.1822 0.0754 0.113 Uiso 1 calc . .
C39 C -0.8652(10) 1.2658(2) -0.7355(8) 0.086(3) Uani 1 d . .
H39A H -0.9524 1.275 -0.7574 0.13 Uiso 1 calc . .
H39B H -0.8392 1.2592 -0.8035 0.13 Uiso 1 calc . .
H39C H -0.8071 1.2836 -0.6942 0.13 Uiso 1 calc . .
C40 C -0.3753(11) 1.3251(2) 0.4120(7) 0.086(3) Uani 1 d . .
H40A H -0.4134 1.3288 0.4754 0.129 Uiso 1 calc . .
H40B H -0.3732 1.3471 0.3726 0.129 Uiso 1 calc . .
H40C H -0.2881 1.3163 0.4408 0.129 Uiso 1 calc . .
C41 C 0.5077(10) 0.9371(3) -0.0821(7) 0.084(3) Uani 1 d . .
H41A H 0.438 0.9542 -0.1079 0.101 Uiso 1 calc . .
H41B H 0.5683 0.9396 -0.1296 0.101 Uiso 1 calc . .
C42 C 0.5977(10) 0.9628(3) 0.2291(8) 0.087(3) Uani 1 d . .
H42A H 0.679 0.9509 0.2351 0.131 Uiso 1 calc . .
H42B H 0.5522 0.9514 0.2787 0.131 Uiso 1 calc . .
H42C H 0.6139 0.987 0.2521 0.131 Uiso 1 calc . .
C43 C 0.4558(11) 0.9019(3) -0.0909(8) 0.095(3) Uani 1 d . .
H43A H 0.411 0.897 -0.1699 0.142 Uiso 1 calc . .
H43B H 0.3962 0.8998 -0.0434 0.142 Uiso 1 calc . .
H43C H 0.5257 0.8853 -0.0654 0.142 Uiso 1 calc . .
N1 N -0.1256(5) 0.91837(11) -0.0592(3) 0.0245(10) Uani 1 d . .
N2 N -0.0579(5) 0.93533(12) 0.1611(3) 0.0252(10) Uani 1 d . .
N3 N -0.3451(5) 1.03917(12) -0.4290(3) 0.0284(11) Uani 1 d . .
N4 N -0.3467(6) 1.01233(13) -0.5040(4) 0.0396(14) Uani 1 d . .
N5 N -0.3036(6) 0.98385(13) -0.4443(4) 0.0388(13) Uani 1 d . .
N6 N -0.0626(6) 1.04379(13) 0.4085(4) 0.0406(14) Uani 1 d . .
N7 N -0.0782(6) 1.07697(14) 0.4309(4) 0.0428(14) Uani 1 d . .
N8 N -0.1222(5) 1.09355(12) 0.3263(3) 0.0286(11) Uani 1 d . .
O1 O 0.0992(5) 0.84290(12) 0.3037(3) 0.0466(12) Uani 1 d . .
O2 O -0.0088(5) 0.81497(11) -0.0378(4) 0.0451(12) Uani 1 d . .
O3 O -0.2928(5) 0.85717(13) 0.1219(4) 0.0535(13) Uani 1 d . .
O4 O -0.7270(5) 1.22152(12) -0.6278(4) 0.0489(12) Uani 1 d . .
O5 O -0.7819(5) 1.15619(12) -0.6751(4) 0.0512(13) Uani 1 d . .
O6 O -0.7236(5) 1.17852(13) -0.4693(4) 0.0523(13) Uani 1 d . .
O7 O -0.3145(5) 1.25851(12) 0.0936(4) 0.0488(12) Uani 1 d . .
O8 O -0.3949(5) 1.29413(11) 0.2367(4) 0.0457(12) Uani 1 d . .
O9 O -0.4673(5) 1.23044(11) 0.2040(3) 0.0428(11) Uani 1 d . .
O10 O 0.5763(7) 0.94330(17) 0.0430(6) 0.0824(18) Uani 1 d . .
O11 O 0.4077(7) 0.9733(2) 0.0667(7) 0.112(3) Uani 1 d . .
P1 P -0.70220(18) 1.18112(4) -0.59367(14) 0.0397(4) Uani 1 d . .
P2 P -0.35153(19) 1.25644(4) 0.20346(13) 0.0371(4) Uani 1 d . .
Cl1 Cl 0.16898(14) 0.91183(4) 0.06391(10) 0.0291(3) Uani 1 d . .
Re1 Re -0.03688(2) 0.88458(2) 0.08632(2) 0.02610(9) Uani 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.155(7) . ?
C1 Re1 1.912(6) . ?
C2 O2 1.147(7) . ?
C2 Re1 1.931(6) . ?
C3 O3 1.131(8) . ?
C3 Re1 1.915(7) . ?
C4 N1 1.339(6) . ?
C4 C5 1.373(8) . ?
C5 C6 1.381(8) . ?
C6 C7 1.394(7) . ?
C6 C15 1.470(8) . ?
C7 C8 1.377(8) . ?
C8 N1 1.353(7) . ?
C8 C9 1.487(7) . ?
C9 N2 1.359(7) . ?
C9 C10 1.389(7) . ?
C10 C11 1.390(7) . ?
C11 C12 1.402(8) . ?
C11 C14 1.451(8) . ?
C12 C13 1.371(8) . ?
C13 N2 1.358(6) . ?
C14 N6 1.344(6) . ?
C14 C17 1.377(8) . ?
C15 N5 1.363(6) . ?
C15 C16 1.360(8) . ?
C16 N3 1.362(6) . ?
C17 N8 1.340(7) . ?
C18 C19 1.388(7) . ?
C18 C23 1.387(8) . ?
C18 N3 1.417(7) . ?
C19 C20 1.391(8) . ?
C20 C21 1.379(8) . ?
C21 C22 1.385(8) . ?
C21 C31 1.511(8) . ?
C22 C23 1.377(8) . ?
C24 C25 1.522(8) . ?
C24 P2 1.790(6) . ?
C25 C30 1.380(8) . ?
C25 C26 1.402(8) . ?
C26 C27 1.376(8) . ?
C27 C28 1.382(8) . ?
C28 C29 1.379(7) . ?
C28 N8 1.415(7) . ?
C29 C30 1.370(8) . ?
C31 P1 1.793(7) . ?
C32 O8 1.449(8) . ?
C32 C40 1.452(11) . ?
C33 O4 1.454(9) . ?
C33 C39 1.478(11) . ?
C34 C38 1.457(11) . ?
C34 O9 1.453(8) . ?
C35 C36 1.487(13) . ?
C36 O6 1.489(10) . ?
C37 O11 1.223(12) . ?
C37 O10 1.307(11) . ?
C37 C42 1.491(13) . ?
C41 C43 1.435(13) . ?
C41 O10 1.504(9) . ?
N1 Re1 2.169(4) . ?
N2 Re1 2.154(4) . ?
N3 N4 1.353(6) . ?
N4 N5 1.308(7) . ?
N6 N7 1.303(7) . ?
N7 N8 1.370(6) . ?
O4 P1 1.586(5) . ?
O5 P1 1.459(4) . ?
O6 P1 1.569(5) . ?
O7 P2 1.471(4) . ?
O8 P2 1.581(4) . ?
O9 P2 1.577(5) . ?
Cl1 Re1 2.4969(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 Re1 178.1(5) . . ?
O2 C2 Re1 177.2(5) . . ?
O3 C3 Re1 177.7(6) . . ?
N1 C4 C5 123.7(5) . . ?
C4 C5 C6 119.0(5) . . ?
C5 C6 C7 118.0(5) . . ?
C5 C6 C15 122.1(5) . . ?
C7 C6 C15 119.8(5) . . ?
C8 C7 C6 119.6(5) . . ?
N1 C8 C7 122.3(5) . . ?
N1 C8 C9 115.3(5) . . ?
C7 C8 C9 122.4(5) . . ?
N2 C9 C10 122.3(4) . . ?
N2 C9 C8 114.5(5) . . ?
C10 C9 C8 123.2(5) . . ?
C9 C10 C11 120.0(5) . . ?
C10 C11 C12 117.4(5) . . ?
C10 C11 C14 123.3(5) . . ?
C12 C11 C14 119.3(5) . . ?
C13 C12 C11 119.9(5) . . ?
N2 C13 C12 123.0(5) . . ?
N6 C14 C17 107.8(5) . . ?
N6 C14 C11 121.4(5) . . ?
C17 C14 C11 130.8(4) . . ?
N5 C15 C16 108.8(5) . . ?
N5 C15 C6 123.1(5) . . ?
C16 C15 C6 128.1(5) . . ?
N3 C16 C15 105.2(5) . . ?
N8 C17 C14 105.3(4) . . ?
C19 C18 C23 120.5(5) . . ?
C19 C18 N3 119.8(5) . . ?
C23 C18 N3 119.6(5) . . ?
C20 C19 C18 118.9(5) . . ?
C21 C20 C19 121.3(5) . . ?
C22 C21 C20 118.5(6) . . ?
C22 C21 C31 120.5(5) . . ?
C20 C21 C31 121.0(5) . . ?
C23 C22 C21 121.6(5) . . ?
C22 C23 C18 119.2(5) . . ?
C25 C24 P2 113.9(4) . . ?
C30 C25 C26 118.8(5) . . ?
C30 C25 C24 119.6(5) . . ?
C26 C25 C24 121.6(5) . . ?
C27 C26 C25 120.1(5) . . ?
C26 C27 C28 120.2(5) . . ?
C29 C28 C27 119.9(5) . . ?
C29 C28 N8 119.6(5) . . ?
C27 C28 N8 120.6(5) . . ?
C30 C29 C28 120.2(5) . . ?
C29 C30 C25 120.9(5) . . ?
C21 C31 P1 111.7(4) . . ?
O8 C32 C40 109.4(7) . . ?
O4 C33 C39 108.2(7) . . ?
C38 C34 O9 108.7(6) . . ?
O6 C36 C35 111.2(8) . . ?
O11 C37 O10 120.9(11) . . ?
O11 C37 C42 128.3(10) . . ?
O10 C37 C42 110.7(9) . . ?
C43 C41 O10 107.2(7) . . ?
C4 N1 C8 117.3(5) . . ?
C4 N1 Re1 125.4(4) . . ?
C8 N1 Re1 117.2(3) . . ?
C13 N2 C9 117.3(5) . . ?
C13 N2 Re1 124.7(4) . . ?
C9 N2 Re1 118.0(3) . . ?
N4 N3 C16 109.4(4) . . ?
N4 N3 C18 122.4(4) . . ?
C16 N3 C18 128.2(4) . . ?
N5 N4 N3 108.2(4) . . ?
N4 N5 C15 108.4(5) . . ?
N7 N6 C14 110.4(5) . . ?
N6 N7 N8 106.5(4) . . ?
C17 N8 N7 110.0(5) . . ?
C17 N8 C28 130.9(5) . . ?
N7 N8 C28 119.0(4) . . ?
C33 O4 P1 118.7(5) . . ?
C36 O6 P1 121.6(5) . . ?
C32 O8 P2 122.6(4) . . ?
C34 O9 P2 116.7(4) . . ?
C37 O10 C41 119.0(8) . . ?
O5 P1 O6 113.1(3) . . ?
O5 P1 O4 114.9(3) . . ?
O6 P1 O4 104.5(3) . . ?
O5 P1 C31 115.7(3) . . ?
O6 P1 C31 105.8(3) . . ?
O4 P1 C31 101.4(3) . . ?
O7 P2 O9 115.4(3) . . ?
O7 P2 O8 109.9(2) . . ?
O9 P2 O8 106.4(3) . . ?
O7 P2 C24 115.8(3) . . ?
O9 P2 C24 102.3(3) . . ?
O8 P2 C24 106.2(3) . . ?
C1 Re1 C3 88.3(3) . . ?
C1 Re1 C2 85.0(2) . . ?
C3 Re1 C2 89.6(3) . . ?
C1 Re1 N2 99.91(19) . . ?
C3 Re1 N2 92.6(2) . . ?
C2 Re1 N2 174.66(19) . . ?
C1 Re1 N1 174.10(19) . . ?
C3 Re1 N1 94.7(2) . . ?
C2 Re1 N1 100.11(19) . . ?
N2 Re1 N1 74.87(15) . . ?
C1 Re1 Cl1 93.53(19) . . ?
C3 Re1 Cl1 174.83(19) . . ?
C2 Re1 Cl1 95.37(18) . . ?
N2 Re1 Cl1 82.31(13) . . ?
N1 Re1 Cl1 83.12(13) . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Re-L1
_database_code_depnum_ccdc_archive 'CCDC 1468798'
_audit_update_record             
;
2016-03-15 deposited with the CCDC.
2016-04-28 downloaded from the CCDC.
;

_audit_creation_date             2016-03-14T16:24:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_chemical_name_common            Re-L1
_chemical_formula_moiety         'C35 H34 Cl N2 O9 P2 Re'
_chemical_formula_sum            'C35 H34 Cl N2 O9 P2 Re'
_chemical_formula_weight         910.23

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.7823(2)
_cell_length_b                   17.7372(3)
_cell_length_c                   26.8707(4)
_cell_angle_alpha                98.3880(10)
_cell_angle_beta                 90.293(2)
_cell_angle_gamma                99.121(2)
_cell_volume                     3621.54(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    17058
_cell_measurement_theta_min      3.449
_cell_measurement_theta_max      28.778

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_F_000             1808
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.90876
_exptl_absorpt_correction_T_max  1
_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_detector_area_resol_mean 10.3385
_diffrn_orient_matrix_ub_11      0.0072552
_diffrn_orient_matrix_ub_12      -0.0397391
_diffrn_orient_matrix_ub_13      -0.002649
_diffrn_orient_matrix_ub_21      -0.0843744
_diffrn_orient_matrix_ub_22      -0.0096489
_diffrn_orient_matrix_ub_23      -0.0115198
_diffrn_orient_matrix_ub_31      0.0368309
_diffrn_orient_matrix_ub_32      0.0022564
_diffrn_orient_matrix_ub_33      -0.0239335
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_number            38852
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.401
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_number_total             14784
_reflns_number_gt                12134
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_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)+(0.0293P)²+5.8282P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         14784
_refine_ls_number_parameters     901
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0357
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0746
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.106

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Re Re -1.0185 7.231 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3200(7) 0.2766(3) 0.14101(17) 0.0369(11) Uani 1 d . .
C2 C -0.0226(6) 0.2854(3) 0.14903(16) 0.0349(11) Uani 1 d . .
C3 C 0.1371(6) 0.2024(3) 0.20581(18) 0.0376(11) Uani 1 d . .
C4 C 0.5030(6) 0.1794(3) 0.52670(17) 0.0355(11) Uani 1 d . .
C5 C 0.1588(7) 0.1886(3) 0.52399(17) 0.0340(11) Uani 1 d . .
C6 C 0.3490(6) 0.2372(3) 0.60901(18) 0.0365(11) Uani 1 d . .
C7 C 0.3965(5) 0.4183(2) 0.43135(15) 0.0258(9) Uani 1 d . .
H7 H 0.373 0.4684 0.4329 0.031 Uiso 1 calc . .
C8 C 0.4730(6) 0.3845(2) 0.38869(15) 0.0278(9) Uani 1 d . .
C9 C 0.4978(6) 0.3083(2) 0.38817(15) 0.0283(9) Uani 1 d . .
H9 H 0.5418 0.282 0.3598 0.034 Uiso 1 calc . .
C10 C 0.4580(6) 0.2720(3) 0.42906(16) 0.0309(10) Uani 1 d . .
H10 H 0.4791 0.2216 0.4279 0.037 Uiso 1 calc . .
C11 C 0.3039(6) 0.0614(3) 0.13786(17) 0.0374(11) Uani 1 d . .
H11 H 0.3141 0.0786 0.1723 0.045 Uiso 1 calc . .
C12 C 0.3616(6) -0.0062(3) 0.11975(16) 0.0368(11) Uani 1 d . .
H12 H 0.4132 -0.0327 0.1416 0.044 Uiso 1 calc . .
C13 C 0.3431(6) -0.0357(2) 0.06829(15) 0.0284(9) Uani 1 d . .
C14 C 0.2713(5) 0.0097(2) 0.03790(15) 0.0266(9) Uani 1 d . .
H14 H 0.2574 -0.0068 0.0034 0.032 Uiso 1 calc . .
C15 C 0.2210(5) 0.0783(2) 0.05804(15) 0.0267(9) Uani 1 d . .
C16 C 0.1492(5) 0.1296(2) 0.02753(15) 0.0262(9) Uani 1 d . .
C17 C 0.1361(5) 0.1150(2) -0.02447(15) 0.0264(9) Uani 1 d . .
H17 H 0.1704 0.0705 -0.0414 0.032 Uiso 1 calc . .
C18 C 0.0718(5) 0.1665(2) -0.05190(15) 0.0251(9) Uani 1 d . .
C19 C 0.0247(6) 0.2319(2) -0.02374(16) 0.0311(10) Uani 1 d . .
H19 H -0.0181 0.2681 -0.04 0.037 Uiso 1 calc . .
C20 C 0.0408(6) 0.2433(2) 0.02761(16) 0.0303(10) Uani 1 d . .
H20 H 0.0082 0.2877 0.0453 0.036 Uiso 1 calc . .
C21 C 0.1426(6) 0.3816(2) 0.59080(16) 0.0311(10) Uani 1 d . .
H21 H 0.1163 0.3475 0.6139 0.037 Uiso 1 calc . .
C22 C 0.0819(6) 0.4502(3) 0.59896(16) 0.0312(10) Uani 1 d . .
H22 H 0.0121 0.4608 0.6263 0.037 Uiso 1 calc . .
C23 C 0.1236(5) 0.5046(2) 0.56659(15) 0.0256(9) Uani 1 d . .
C24 C 0.2163(5) 0.4808(2) 0.52441(15) 0.0255(9) Uani 1 d . .
H24 H 0.2437 0.514 0.5008 0.031 Uiso 1 calc . .
C25 C 0.2683(5) 0.4096(2) 0.51675(15) 0.0252(9) Uani 1 d . .
C26 C 0.3551(5) 0.3783(2) 0.47128(15) 0.0244(9) Uani 1 d . .
C27 C 0.0125(6) 0.6094(3) 0.62397(17) 0.0350(11) Uani 1 d . .
H27 H -0.0127 0.5756 0.6473 0.042 Uiso 1 calc . .
C28 C 0.0796(5) 0.5832(2) 0.57760(15) 0.0267(9) Uani 1 d . .
C29 C 0.1126(6) 0.6362(2) 0.54395(17) 0.0313(10) Uani 1 d . .
H29 H 0.1545 0.6205 0.5124 0.038 Uiso 1 calc . .
C30 C 0.0845(6) 0.7111(3) 0.55628(18) 0.0341(10) Uani 1 d . .
H30 H 0.1084 0.7451 0.533 0.041 Uiso 1 calc . .
C31 C 0.0215(6) 0.7371(3) 0.60251(18) 0.0335(10) Uani 1 d . .
C32 C -0.0166(6) 0.6843(3) 0.63559(18) 0.0389(11) Uani 1 d . .
H32 H -0.0632 0.6999 0.6665 0.047 Uiso 1 calc . .
C33 C -0.0011(7) 0.8211(3) 0.6170(2) 0.0464(13) Uani 1 d . .
C34 C 0.5336(6) 0.4288(3) 0.34732(15) 0.0291(10) Uani 1 d . .
C35 C 0.5098(6) 0.5049(3) 0.34858(17) 0.0368(11) Uani 1 d . .
H35 H 0.4443 0.5268 0.374 0.044 Uiso 1 calc . .
C36 C 0.5809(7) 0.5490(3) 0.31311(17) 0.0397(12) Uani 1 d . .
H36 H 0.5631 0.6 0.3151 0.048 Uiso 1 calc . .
C37 C 0.6777(7) 0.5180(3) 0.27496(18) 0.0424(12) Uani 1 d . .
C38 C 0.6938(7) 0.4413(3) 0.27176(19) 0.0472(13) Uani 1 d . .
H38 H 0.7521 0.4186 0.2449 0.057 Uiso 1 calc . .
C39 C 0.6250(7) 0.3971(3) 0.30759(18) 0.0416(12) Uani 1 d . .
H39 H 0.6402 0.3457 0.3049 0.05 Uiso 1 calc . .
C40 C 0.7677(8) 0.5673(3) 0.23746(19) 0.0505(14) Uani 1 d . .
C41 C 0.0507(5) 0.1510(2) -0.10722(16) 0.0268(9) Uani 1 d . .
C42 C -0.0045(6) 0.2041(3) -0.13452(17) 0.0367(11) Uani 1 d . .
H42 H -0.0222 0.2518 -0.1177 0.044 Uiso 1 calc . .
C43 C -0.0335(7) 0.1878(3) -0.18552(17) 0.0393(12) Uani 1 d . .
H43 H -0.0702 0.2246 -0.2027 0.047 Uiso 1 calc . .
C44 C -0.0087(6) 0.1166(3) -0.21217(16) 0.0329(10) Uani 1 d . .
C45 C 0.0791(6) 0.0810(3) -0.13430(17) 0.0366(11) Uani 1 d . .
H45 H 0.1199 0.045 -0.1173 0.044 Uiso 1 calc . .
C46 C 0.0483(7) 0.0639(3) -0.18540(17) 0.0401(12) Uani 1 d . .
H46 H 0.0661 0.0162 -0.2022 0.048 Uiso 1 calc . .
C47 C -0.0512(6) 0.0966(3) -0.26809(17) 0.0380(11) Uani 1 d . .
C48 C 0.3915(6) -0.1110(2) 0.04700(15) 0.0270(9) Uani 1 d . .
C49 C 0.4767(7) -0.2324(3) 0.05894(17) 0.0394(12) Uani 1 d . .
H49 H 0.5111 -0.2637 0.0808 0.047 Uiso 1 calc . .
C50 C 0.4420(6) -0.1609(3) 0.07782(17) 0.0366(11) Uani 1 d . .
H50 H 0.4523 -0.1449 0.1124 0.044 Uiso 1 calc . .
C51 C 0.4614(6) -0.2595(2) 0.00720(17) 0.0315(10) Uani 1 d . .
C52 C 0.4132(6) -0.2096(3) -0.02402(17) 0.0320(10) Uani 1 d . .
H52 H 0.4028 -0.2256 -0.0586 0.038 Uiso 1 calc . .
C53 C 0.3808(6) -0.1372(2) -0.00454(16) 0.0301(10) Uani 1 d . .
H53 H 0.3509 -0.1049 -0.0264 0.036 Uiso 1 calc . .
C54 C 0.4883(6) -0.3402(3) -0.01398(18) 0.0391(11) Uani 1 d . .
N1 N 0.2379(5) 0.36055(19) 0.55142(13) 0.0273(8) Uani 1 d . .
N2 N 0.3895(4) 0.30543(19) 0.47122(12) 0.0256(8) Uani 1 d . .
N3 N 0.2332(5) 0.1042(2) 0.10826(13) 0.0302(8) Uani 1 d . .
N4 N 0.1013(5) 0.19350(19) 0.05388(12) 0.0266(8) Uani 1 d . .
O1 O 0.4447(5) 0.3226(2) 0.14495(13) 0.0505(9) Uani 1 d . .
O2 O -0.1045(5) 0.3346(2) 0.15625(13) 0.0490(9) Uani 1 d . .
O3 O 0.1622(5) 0.2028(2) 0.24805(12) 0.0547(10) Uani 1 d . .
O4 O 0.5881(5) 0.1320(2) 0.51727(14) 0.0510(9) Uani 1 d . .
O5 O 0.0335(5) 0.1444(2) 0.51399(13) 0.0461(9) Uani 1 d . .
O6 O 0.3391(5) 0.2253(2) 0.64994(13) 0.0539(10) Uani 1 d . .
O7 O 0.3585(5) 0.8643(2) 0.62634(14) 0.0581(10) Uani 1 d . .
O8 O 0.1644(5) 0.9623(2) 0.65681(16) 0.0599(10) Uani 1 d . .
O9 O 0.1651(6) 0.8512(2) 0.70202(14) 0.0687(12) Uani 1 d . .
O10 O 1.0818(5) 0.5334(2) 0.26655(13) 0.0515(9) Uani 1 d . .
O11 O 1.0063(5) 0.6598(2) 0.30059(12) 0.0471(9) Uani 1 d . .
O12 O 1.0818(5) 0.6335(2) 0.20689(13) 0.0562(10) Uani 1 d . .
O13 O 0.3305(5) -0.4205(2) 0.05208(15) 0.0577(10) Uani 1 d . .
O14 O 0.1349(5) -0.3884(2) -0.01662(19) 0.0756(14) Uani 1 d . .
O15 O 0.3331(5) -0.48913(19) -0.03414(15) 0.0550(10) Uani 1 d . .
O16 O -0.3507(5) 0.0000(2) -0.24950(13) 0.0526(10) Uani 1 d . .
O17 O -0.3645(5) 0.1387(2) -0.26386(12) 0.0465(9) Uani 1 d . .
O18 O -0.3153(5) 0.0455(2) -0.33630(12) 0.0479(9) Uani 1 d . .
Cl1 Cl -0.16023(15) 0.10772(6) 0.12011(4) 0.0346(2) Uani 1 d . .
Cl2 Cl 0.63511(15) 0.35652(6) 0.56416(4) 0.0333(2) Uani 1 d . .
Re1 Re 0.11202(2) 0.20370(2) 0.13467(2) 0.02970(6) Uani 1 d . .
Re2 Re 0.36619(2) 0.26039(2) 0.54176(2) 0.02822(6) Uani 1 d . .
P1 P 0.9988(2) 0.60208(8) 0.25000(5) 0.0458(3) Uani 1 d . .
P2 P 0.19186(18) 0.87583(7) 0.65043(5) 0.0416(3) Uani 1 d . .
P3 P 0.30081(18) -0.40951(7) -0.00393(6) 0.0470(3) Uani 1 d . .
P4 P -0.28320(18) 0.06293(8) -0.27731(5) 0.0392(3) Uani 1 d . .
C68 C 1.1543(8) 0.7654(3) 0.3612(2) 0.0540(15) Uani 1 d . .
H68A H 1.2656 0.7946 0.3726 0.081 Uiso 1 calc . .
H68B H 1.1008 0.7411 0.3882 0.081 Uiso 1 calc . .
H68C H 1.0812 0.7993 0.3506 0.081 Uiso 1 calc . .
C67 C 1.1778(8) 0.7052(3) 0.3182(2) 0.0547(15) Uani 1 d . .
H67A H 1.2326 0.7295 0.2909 0.066 Uiso 1 calc . .
H67B H 1.2529 0.6713 0.3286 0.066 Uiso 1 calc . .
C61 C -0.2693(8) -0.0245(3) -0.36469(19) 0.0509(14) Uani 1 d . .
H61A H -0.3466 -0.0695 -0.3568 0.061 Uiso 1 calc . .
H61B H -0.1508 -0.0295 -0.3561 0.061 Uiso 1 calc . .
C70 C 1.1862(8) 0.4129(3) 0.2506(2) 0.0587(16) Uani 1 d . .
H70A H 1.242 0.3803 0.2263 0.088 Uiso 1 calc . .
H70B H 1.0737 0.3862 0.2575 0.088 Uiso 1 calc . .
H70C H 1.2561 0.4259 0.2811 0.088 Uiso 1 calc . .
C69 C 1.1659(9) 0.4846(3) 0.2302(2) 0.0598(16) Uani 1 d . .
H69A H 1.2792 0.5117 0.223 0.072 Uiso 1 calc . .
H69B H 1.0966 0.4718 0.1992 0.072 Uiso 1 calc . .
C65 C 0.2879(8) 0.8762(3) 0.7450(2) 0.0591(16) Uani 1 d . .
H65A H 0.2288 0.8996 0.7735 0.071 Uiso 1 calc . .
H65B H 0.3818 0.9146 0.7364 0.071 Uiso 1 calc . .
C57 C 0.2760(8) -0.5105(3) -0.0864(2) 0.0587(16) Uani 1 d . .
H57A H 0.3671 -0.4917 -0.1081 0.07 Uiso 1 calc . .
H57B H 0.1735 -0.4881 -0.0926 0.07 Uiso 1 calc . .
C66 C 0.3605(9) 0.8093(4) 0.7589(2) 0.0693(18) Uani 1 d . .
H66A H 0.4414 0.8265 0.7869 0.104 Uiso 1 calc . .
H66B H 0.4193 0.7863 0.7307 0.104 Uiso 1 calc . .
H66C H 0.2676 0.7719 0.7681 0.104 Uiso 1 calc . .
C58 C 0.2349(10) -0.5964(3) -0.0968(2) 0.072(2) Uani 1 d . .
H58A H 0.1972 -0.6122 -0.1314 0.107 Uiso 1 calc . .
H58B H 0.144 -0.6144 -0.0754 0.107 Uiso 1 calc . .
H58C H 0.3371 -0.618 -0.0905 0.107 Uiso 1 calc . .
C59 C -0.5300(7) 0.1401(4) -0.2411(2) 0.0609(16) Uani 1 d . .
H59A H -0.5461 0.1042 -0.2169 0.073 Uiso 1 calc . .
H59B H -0.6224 0.1247 -0.2667 0.073 Uiso 1 calc . .
C62 C -0.2861(9) -0.0189(4) -0.4197(2) 0.0703(19) Uani 1 d . .
H62A H -0.2563 -0.0646 -0.4393 0.105 Uiso 1 calc . .
H62B H -0.209 0.0256 -0.4272 0.105 Uiso 1 calc . .
H62C H -0.4039 -0.0143 -0.4279 0.105 Uiso 1 calc . .
C63 C 0.2576(9) 1.0197(4) 0.6260(3) 0.0703(18) Uani 1 d . .
H63A H 0.2313 1.0705 0.6386 0.084 Uiso 1 calc . .
H63B H 0.3821 1.0215 0.6301 0.084 Uiso 1 calc . .
C60 C -0.5367(9) 0.2198(4) -0.2155(2) 0.0698(18) Uani 1 d . .
H60A H -0.6473 0.2213 -0.2 0.105 Uiso 1 calc . .
H60B H -0.5218 0.255 -0.2397 0.105 Uiso 1 calc . .
H60C H -0.4453 0.2346 -0.1901 0.105 Uiso 1 calc . .
C64 C 0.2104(10) 1.0016(4) 0.5727(3) 0.086(2) Uani 1 d . .
H64A H 0.2735 1.0401 0.5551 0.129 Uiso 1 calc . .
H64B H 0.0877 1.0008 0.5681 0.129 Uiso 1 calc . .
H64C H 0.2389 0.9519 0.5596 0.129 Uiso 1 calc . .
C56 C 0.2201(11) -0.5319(5) 0.0904(3) 0.094(3) Uani 1 d . .
H56A H 0.1231 -0.5533 0.1087 0.141 Uiso 1 calc . .
H56B H 0.3248 -0.5253 0.1107 0.141 Uiso 1 calc . .
H56C H 0.2308 -0.5661 0.0599 0.141 Uiso 1 calc . .
C55 C 0.1940(12) -0.4628(6) 0.0793(5) 0.140(4) Uani 1 d . .
H55A H 0.1769 -0.4303 0.1105 0.168 Uiso 1 calc . .
H55B H 0.0865 -0.4708 0.0594 0.168 Uiso 1 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.158(6) . ?
C1 Re1 1.895(5) . ?
C2 O2 1.154(5) . ?
C2 Re1 1.916(5) . ?
C3 O3 1.149(5) . ?
C3 Re1 1.924(5) . ?
C4 O4 1.152(5) . ?
C4 Re2 1.918(5) . ?
C5 O5 1.154(6) . ?
C5 Re2 1.902(5) . ?
C6 O6 1.151(5) . ?
C6 Re2 1.911(5) . ?
C7 C26 1.382(6) . ?
C7 C8 1.396(6) . ?
C8 C9 1.393(6) . ?
C8 C34 1.489(6) . ?
C9 C10 1.366(6) . ?
C10 N2 1.353(5) . ?
C11 N3 1.348(5) . ?
C11 C12 1.371(6) . ?
C12 C13 1.403(6) . ?
C13 C14 1.399(6) . ?
C13 C48 1.480(6) . ?
C14 C15 1.374(6) . ?
C15 N3 1.358(5) . ?
C15 C16 1.479(6) . ?
C16 N4 1.351(5) . ?
C16 C17 1.384(6) . ?
C17 C18 1.402(6) . ?
C18 C19 1.390(6) . ?
C18 C41 1.475(6) . ?
C19 C20 1.367(6) . ?
C20 N4 1.346(5) . ?
C21 N1 1.338(5) . ?
C21 C22 1.363(6) . ?
C22 C23 1.394(6) . ?
C23 C24 1.396(6) . ?
C23 C28 1.477(6) . ?
C24 C25 1.375(6) . ?
C25 N1 1.361(5) . ?
C25 C26 1.478(6) . ?
C26 N2 1.361(5) . ?
C27 C32 1.375(6) . ?
C27 C28 1.398(6) . ?
C28 C29 1.393(6) . ?
C29 C30 1.374(6) . ?
C30 C31 1.381(6) . ?
C31 C32 1.383(6) . ?
C31 C33 1.521(6) . ?
C33 P2 1.810(5) . ?
C34 C39 1.386(6) . ?
C34 C35 1.387(6) . ?
C35 C36 1.383(6) . ?
C36 C37 1.376(7) . ?
C37 C38 1.377(7) . ?
C37 C40 1.529(7) . ?
C38 C39 1.385(7) . ?
C40 P1 1.819(6) . ?
C41 C42 1.391(6) . ?
C41 C45 1.394(6) . ?
C42 C43 1.368(6) . ?
C43 C44 1.401(6) . ?
C44 C46 1.383(6) . ?
C44 C47 1.515(6) . ?
C45 C46 1.374(6) . ?
C47 P4 1.813(5) . ?
C48 C53 1.393(6) . ?
C48 C50 1.394(6) . ?
C49 C50 1.364(6) . ?
C49 C51 1.401(6) . ?
C51 C52 1.394(6) . ?
C51 C54 1.508(6) . ?
C52 C53 1.377(6) . ?
C54 P3 1.802(5) . ?
N1 Re2 2.156(3) . ?
N2 Re2 2.159(3) . ?
N3 Re1 2.162(4) . ?
N4 Re1 2.152(3) . ?
O7 P2 1.482(4) . ?
O8 C63 1.506(7) . ?
O8 P2 1.566(4) . ?
O9 C65 1.466(6) . ?
O9 P2 1.519(4) . ?
O10 C69 1.438(6) . ?
O10 P1 1.583(4) . ?
O11 C67 1.482(7) . ?
O11 P1 1.573(4) . ?
O12 P1 1.466(3) . ?
O13 C55 1.463(8) . ?
O13 P3 1.566(4) . ?
O14 P3 1.453(4) . ?
O15 C57 1.447(6) . ?
O15 P3 1.580(4) . ?
O16 P4 1.464(4) . ?
O17 C59 1.430(6) . ?
O17 P4 1.572(4) . ?
O18 C61 1.456(6) . ?
O18 P4 1.581(3) . ?
Cl1 Re1 2.4888(11) . ?
Cl2 Re2 2.4912(11) . ?
C68 C67 1.488(8) . ?
C61 C62 1.503(7) . ?
C70 C69 1.486(8) . ?
C65 C66 1.485(8) . ?
C57 C58 1.490(7) . ?
C59 C60 1.489(8) . ?
C63 C64 1.453(9) . ?
C56 C55 1.347(10) . ?

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
O1 C1 Re1 178.3(4) . . ?
O2 C2 Re1 178.1(4) . . ?
O3 C3 Re1 176.1(4) . . ?
O4 C4 Re2 178.5(4) . . ?
O5 C5 Re2 178.7(4) . . ?
O6 C6 Re2 178.2(4) . . ?
C26 C7 C8 120.9(4) . . ?
C9 C8 C7 116.3(4) . . ?
C9 C8 C34 121.9(4) . . ?
C7 C8 C34 121.8(4) . . ?
C10 C9 C8 120.4(4) . . ?
N2 C10 C9 123.4(4) . . ?
N3 C11 C12 123.3(4) . . ?
C11 C12 C13 120.2(4) . . ?
C14 C13 C12 115.9(4) . . ?
C14 C13 C48 121.3(4) . . ?
C12 C13 C48 122.8(4) . . ?
C15 C14 C13 121.2(4) . . ?
N3 C15 C14 122.0(4) . . ?
N3 C15 C16 114.5(4) . . ?
C14 C15 C16 123.5(4) . . ?
N4 C16 C17 121.9(4) . . ?
N4 C16 C15 115.3(4) . . ?
C17 C16 C15 122.8(4) . . ?
C16 C17 C18 120.8(4) . . ?
C19 C18 C17 116.0(4) . . ?
C19 C18 C41 122.1(4) . . ?
C17 C18 C41 121.9(4) . . ?
C20 C19 C18 120.7(4) . . ?
N4 C20 C19 123.2(4) . . ?
N1 C21 C22 123.7(4) . . ?
C21 C22 C23 120.4(4) . . ?
C22 C23 C24 115.4(4) . . ?
C22 C23 C28 122.0(4) . . ?
C24 C23 C28 122.5(4) . . ?
C25 C24 C23 121.8(4) . . ?
N1 C25 C24 121.0(4) . . ?
N1 C25 C26 114.3(4) . . ?
C24 C25 C26 124.7(4) . . ?
N2 C26 C7 121.9(4) . . ?
N2 C26 C25 114.4(3) . . ?
C7 C26 C25 123.7(4) . . ?
C32 C27 C28 121.0(4) . . ?
C29 C28 C27 116.8(4) . . ?
C29 C28 C23 122.0(4) . . ?
C27 C28 C23 121.0(4) . . ?
C30 C29 C28 121.5(4) . . ?
C29 C30 C31 121.4(4) . . ?
C30 C31 C32 117.5(4) . . ?
C30 C31 C33 121.3(4) . . ?
C32 C31 C33 121.2(4) . . ?
C27 C32 C31 121.7(4) . . ?
C31 C33 P2 110.2(3) . . ?
C39 C34 C35 117.3(4) . . ?
C39 C34 C8 121.3(4) . . ?
C35 C34 C8 121.3(4) . . ?
C36 C35 C34 121.7(4) . . ?
C37 C36 C35 120.5(5) . . ?
C36 C37 C38 118.1(5) . . ?
C36 C37 C40 121.3(5) . . ?
C38 C37 C40 120.5(5) . . ?
C37 C38 C39 121.5(5) . . ?
C38 C39 C34 120.6(5) . . ?
C37 C40 P1 115.5(4) . . ?
C42 C41 C45 117.0(4) . . ?
C42 C41 C18 121.7(4) . . ?
C45 C41 C18 121.2(4) . . ?
C43 C42 C41 121.6(4) . . ?
C42 C43 C44 120.9(4) . . ?
C46 C44 C43 117.9(4) . . ?
C46 C44 C47 121.2(4) . . ?
C43 C44 C47 120.9(4) . . ?
C46 C45 C41 121.7(4) . . ?
C45 C46 C44 120.9(4) . . ?
C44 C47 P4 108.9(3) . . ?
C53 C48 C50 116.6(4) . . ?
C53 C48 C13 121.8(4) . . ?
C50 C48 C13 121.5(4) . . ?
C50 C49 C51 121.1(4) . . ?
C49 C50 C48 122.2(4) . . ?
C52 C51 C49 117.1(4) . . ?
C52 C51 C54 121.0(4) . . ?
C49 C51 C54 121.8(4) . . ?
C53 C52 C51 121.1(4) . . ?
C52 C53 C48 121.8(4) . . ?
C51 C54 P3 110.7(3) . . ?
C21 N1 C25 117.3(4) . . ?
C21 N1 Re2 125.3(3) . . ?
C25 N1 Re2 117.2(3) . . ?
C10 N2 C26 116.9(3) . . ?
C10 N2 Re2 125.4(3) . . ?
C26 N2 Re2 117.0(3) . . ?
C11 N3 C15 117.3(4) . . ?
C11 N3 Re1 125.4(3) . . ?
C15 N3 Re1 117.0(3) . . ?
C20 N4 C16 117.5(4) . . ?
C20 N4 Re1 125.1(3) . . ?
C16 N4 Re1 117.3(3) . . ?
C63 O8 P2 122.9(4) . . ?
C65 O9 P2 124.7(3) . . ?
C69 O10 P1 120.1(3) . . ?
C67 O11 P1 117.6(3) . . ?
C55 O13 P3 121.2(6) . . ?
C57 O15 P3 120.0(3) . . ?
C59 O17 P4 123.1(4) . . ?
C61 O18 P4 120.1(3) . . ?
C1 Re1 C2 90.4(2) . . ?
C1 Re1 C3 86.83(19) . . ?
C2 Re1 C3 89.09(19) . . ?
C1 Re1 N4 93.41(16) . . ?
C2 Re1 N4 97.89(16) . . ?
C3 Re1 N4 173.01(17) . . ?
C1 Re1 N3 96.08(17) . . ?
C2 Re1 N3 170.49(16) . . ?
C3 Re1 N3 98.20(17) . . ?
N4 Re1 N3 74.82(13) . . ?
C1 Re1 Cl1 176.15(13) . . ?
C2 Re1 Cl1 90.17(14) . . ?
C3 Re1 Cl1 96.99(15) . . ?
N4 Re1 Cl1 82.73(9) . . ?
N3 Re1 Cl1 82.92(10) . . ?
C5 Re2 C6 89.0(2) . . ?
C5 Re2 C4 90.4(2) . . ?
C6 Re2 C4 88.44(19) . . ?
C5 Re2 N1 94.88(16) . . ?
C6 Re2 N1 98.34(16) . . ?
C4 Re2 N1 171.45(16) . . ?
C5 Re2 N2 96.65(16) . . ?
C6 Re2 N2 170.92(16) . . ?
C4 Re2 N2 98.60(16) . . ?
N1 Re2 N2 74.15(13) . . ?
C5 Re2 Cl2 178.75(13) . . ?
C6 Re2 Cl2 91.82(15) . . ?
C4 Re2 Cl2 90.57(15) . . ?
N1 Re2 Cl2 84.05(10) . . ?
N2 Re2 Cl2 82.44(9) . . ?
O12 P1 O11 116.2(2) . . ?
O12 P1 O10 114.1(2) . . ?
O11 P1 O10 102.2(2) . . ?
O12 P1 C40 111.5(2) . . ?
O11 P1 C40 104.4(2) . . ?
O10 P1 C40 107.4(2) . . ?
O7 P2 O9 116.5(3) . . ?
O7 P2 O8 112.1(2) . . ?
O9 P2 O8 105.8(2) . . ?
O7 P2 C33 115.0(2) . . ?
O9 P2 C33 100.4(2) . . ?
O8 P2 C33 105.7(2) . . ?
O14 P3 O13 116.6(3) . . ?
O14 P3 O15 113.4(2) . . ?
O13 P3 O15 102.7(2) . . ?
O14 P3 C54 114.6(2) . . ?
O13 P3 C54 102.2(2) . . ?
O15 P3 C54 105.8(2) . . ?
O16 P4 O17 115.3(2) . . ?
O16 P4 O18 115.8(2) . . ?
O17 P4 O18 101.28(19) . . ?
O16 P4 C47 114.3(2) . . ?
O17 P4 C47 103.3(2) . . ?
O18 P4 C47 105.2(2) . . ?
O11 C67 C68 109.7(4) . . ?
O18 C61 C62 107.9(4) . . ?
O10 C69 C70 109.4(5) . . ?
O9 C65 C66 110.3(5) . . ?
O15 C57 C58 107.8(4) . . ?
O17 C59 C60 108.8(5) . . ?
C64 C63 O8 113.4(5) . . ?
C56 C55 O13 117.3(8) . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
