# Electronic Supplementary Material (ESI) for ChemComm.
# 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
_database_code_depnum_ccdc_archive 'CCDC 853881'
_audit_update_record             
;
2016-09-16 deposited with the CCDC.
2016-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C41 H32 Br N3 O6 Re'
_chemical_formula_weight         928.81

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   c2/c

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

_cell_length_a                   19.79(4)
_cell_length_b                   14.87(3)
_cell_length_c                   25.04(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.33(3)
_cell_angle_gamma                90.00
_cell_volume                     7252(24)
_cell_formula_units_Z            8
_cell_measurement_temperature    446(2)
_cell_measurement_reflns_used    29476
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      25.00

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3656
_exptl_absorpt_coefficient_mu    4.506
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6614
_exptl_absorpt_correction_T_max  0.8061
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      446(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29476
_diffrn_reflns_av_R_equivalents  0.1071
_diffrn_reflns_av_sigmaI/netI    0.0616
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.17
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6366
_reflns_number_gt                5633
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0166P)²+20.2855P] 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         6366
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0939
_refine_ls_wR_factor_gt          0.0898
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.860702(10) 0.047097(15) 1.163506(9) 0.04133(9) Uani 1 1 d . . .
Br1 Br 0.74318(5) 0.73978(5) 0.83414(3) 0.0803(3) Uani 1 1 d . . .
N1 N 0.8035(2) 0.1666(3) 1.12390(18) 0.0403(10) Uani 1 1 d . . .
O3 O 0.9215(3) 0.1548(3) 1.2654(2) 0.0858(16) Uani 1 1 d . . .
C3 C 0.8989(3) 0.1154(4) 1.2271(3) 0.0566(16) Uani 1 1 d . . .
C2 C 0.8994(3) -0.0585(5) 1.2006(3) 0.0627(17) Uani 1 1 d . . .
N3 N 0.7564(2) 0.0417(3) 1.18535(18) 0.0380(10) Uani 1 1 d . . .
O2 O 0.9258(3) -0.1202(4) 1.2241(3) 0.0971(19) Uani 1 1 d . . .
N2 N 0.8022(2) -0.0327(3) 1.09550(19) 0.0414(11) Uani 1 1 d . . .
O1 O 1.0010(2) 0.0740(4) 1.1295(2) 0.0860(16) Uani 1 1 d . . .
C1 C 0.9471(3) 0.0644(4) 1.1412(3) 0.0604(16) Uani 1 1 d . . .
O4 O 0.4953(3) -0.0324(3) 1.3644(3) 0.0866(18) Uani 1 1 d . . .
C29 C 0.8298(3) -0.0782(4) 1.0540(3) 0.0494(14) Uani 1 1 d . . .
O5 O 0.5120(2) -0.1734(3) 1.34052(19) 0.0616(12) Uani 1 1 d . . .
C28 C 0.9014(4) -0.0886(5) 1.0609(4) 0.083(2) Uani 1 1 d . . .
H28A H 0.9292 -0.0688 1.0927 0.099 Uiso 1 1 calc R . .
O6 O 0.9437(3) 0.3585(5) 0.8554(4) 0.126(3) Uani 1 1 d . . .
C27 C 0.9303(5) -0.1282(6) 1.0207(5) 0.100(3) Uani 1 1 d . . .
H27A H 0.9778 -0.1340 1.0253 0.119 Uiso 1 1 calc R . .
C26 C 0.8897(6) -0.1596(6) 0.9734(4) 0.097(3) Uani 1 1 d . . .
H26A H 0.9098 -0.1843 0.9459 0.117 Uiso 1 1 calc R . .
C25 C 0.8195(5) -0.1539(5) 0.9675(3) 0.079(2) Uani 1 1 d . . .
H25A H 0.7921 -0.1766 0.9364 0.094 Uiso 1 1 calc R . .
C24 C 0.7884(3) -0.1137(3) 1.0084(2) 0.0516(15) Uani 1 1 d . . .
C23 C 0.7140(4) -0.1074(4) 1.0028(2) 0.0524(15) Uani 1 1 d . . .
C22 C 0.6677(4) -0.1393(4) 0.9575(3) 0.0699(19) Uani 1 1 d . . .
H22A H 0.6844 -0.1656 0.9287 0.084 Uiso 1 1 calc R . .
C21 C 0.5985(5) -0.1318(5) 0.9554(3) 0.081(2) Uani 1 1 d . . .
H21A H 0.5685 -0.1526 0.9251 0.097 Uiso 1 1 calc R . .
C20 C 0.5722(4) -0.0931(5) 0.9982(3) 0.072(2) Uani 1 1 d . . .
H20A H 0.5250 -0.0884 0.9961 0.086 Uiso 1 1 calc R . .
C19 C 0.6159(3) -0.0620(4) 1.0434(3) 0.0516(14) Uani 1 1 d . . .
H19A H 0.5981 -0.0364 1.0718 0.062 Uiso 1 1 calc R . .
C18 C 0.6878(3) -0.0689(3) 1.0468(2) 0.0439(13) Uani 1 1 d . . .
C30 C 0.7349(3) -0.0339(3) 1.0925(2) 0.0375(11) Uani 1 1 d . . .
C31 C 0.7056(3) 0.0030(4) 1.1398(2) 0.0437(12) Uani 1 1 d . . .
H31A H 0.6725 0.0493 1.1262 0.052 Uiso 1 1 calc R . .
H31B H 0.6810 -0.0450 1.1542 0.052 Uiso 1 1 calc R . .
C4 C 0.8219(3) 0.2169(4) 1.0810(2) 0.0444(13) Uani 1 1 d . . .
C6 C 0.8849(3) 0.2283(5) 1.0070(3) 0.0682(19) Uani 1 1 d . . .
H6A H 0.9127 0.2019 0.9851 0.082 Uiso 1 1 calc R . .
C7 C 0.8643(4) 0.3170(5) 0.9985(3) 0.072(2) Uani 1 1 d . . .
H7A H 0.8799 0.3513 0.9721 0.087 Uiso 1 1 calc R . .
C8 C 0.8210(4) 0.3530(4) 1.0290(3) 0.0660(18) Uani 1 1 d . . .
H8A H 0.8071 0.4124 1.0227 0.079 Uiso 1 1 calc R . .
C9 C 0.7965(3) 0.3045(4) 1.0697(2) 0.0477(13) Uani 1 1 d . . .
C10 C 0.7453(3) 0.3384(4) 1.0994(2) 0.0512(14) Uani 1 1 d . . .
C11 C 0.7145(4) 0.4243(4) 1.0901(3) 0.0696(19) Uani 1 1 d . . .
H11A H 0.7297 0.4636 1.0660 0.084 Uiso 1 1 calc R . .
C12 C 0.6625(4) 0.4503(4) 1.1162(3) 0.073(2) Uani 1 1 d . . .
H12A H 0.6420 0.5062 1.1087 0.087 Uiso 1 1 calc R . .
C13 C 0.6401(4) 0.3938(4) 1.1539(3) 0.0688(19) Uani 1 1 d . . .
H13A H 0.6042 0.4117 1.1710 0.083 Uiso 1 1 calc R . .
C14 C 0.6710(3) 0.3118(4) 1.1660(3) 0.0539(15) Uani 1 1 d . . .
H14A H 0.6574 0.2754 1.1923 0.065 Uiso 1 1 calc R . .
C15 C 0.7226(3) 0.2831(3) 1.1388(2) 0.0421(12) Uani 1 1 d . . .
C16 C 0.7556(3) 0.1962(3) 1.1500(2) 0.0396(12) Uani 1 1 d . . .
C17 C 0.7371(3) 0.1368(3) 1.1942(2) 0.0421(12) Uani 1 1 d . . .
H17A H 0.7612 0.1573 1.2293 0.051 Uiso 1 1 calc R . .
H17B H 0.6882 0.1406 1.1941 0.051 Uiso 1 1 calc R . .
C32 C 0.7589(3) -0.0117(4) 1.2371(2) 0.0476(13) Uani 1 1 d . . .
H32A H 0.7921 0.0171 1.2651 0.057 Uiso 1 1 calc R . .
H32B H 0.7769 -0.0708 1.2312 0.057 Uiso 1 1 calc R . .
C33 C 0.6932(3) -0.0251(3) 1.2598(2) 0.0434(13) Uani 1 1 d . . .
C34 C 0.6691(4) 0.0377(4) 1.2926(3) 0.0597(17) Uani 1 1 d . . .
H34A H 0.6897 0.0940 1.2977 0.072 Uiso 1 1 calc R . .
C35 C 0.6143(4) 0.0171(4) 1.3179(3) 0.0626(18) Uani 1 1 d . . .
H35A H 0.5988 0.0599 1.3399 0.075 Uiso 1 1 calc R . .
C36 C 0.5825(3) -0.0652(4) 1.3112(2) 0.0458(13) Uani 1 1 d . . .
C37 C 0.6049(3) -0.1274(4) 1.2773(2) 0.0537(15) Uani 1 1 d . . .
H37A H 0.5828 -0.1827 1.2713 0.064 Uiso 1 1 calc R . .
C38 C 0.6604(3) -0.1078(4) 1.2522(2) 0.0525(15) Uani 1 1 d . . .
H38A H 0.6758 -0.1506 1.2301 0.063 Uiso 1 1 calc R . .
C39 C 0.5260(3) -0.0854(4) 1.3416(3) 0.0559(15) Uani 1 1 d . . .
C40 C 0.4589(4) -0.2031(5) 1.3699(3) 0.074(2) Uani 1 1 d . . .
H40B H 0.4534 -0.2670 1.3662 0.111 Uiso 1 1 calc R . .
H40C H 0.4163 -0.1740 1.3552 0.111 Uiso 1 1 calc R . .
H40D H 0.4720 -0.1878 1.4075 0.111 Uiso 1 1 calc R . .
C41 C 0.9790(8) 0.2999(11) 0.8212(8) 0.230(10) Uani 1 1 d . . .
H41A H 1.0269 0.2960 0.8367 0.345 Uiso 1 1 calc R . .
H41B H 0.9739 0.3247 0.7853 0.345 Uiso 1 1 calc R . .
H41C H 0.9590 0.2409 0.8193 0.345 Uiso 1 1 calc R . .
C5 C 0.8642(3) 0.1788(4) 1.0480(2) 0.0532(15) Uani 1 1 d . . .
H5A H 0.8785 0.1195 1.0537 0.064 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 C1 1.909(8) . ?
Re1 C2 1.913(7) . ?
Re1 C3 1.925(7) . ?
Re1 N2 2.223(5) . ?
Re1 N3 2.231(6) . ?
Re1 N1 2.240(5) . ?
N1 C16 1.319(7) . ?
N1 C4 1.408(7) . ?
O3 C3 1.144(8) . ?
C2 O2 1.162(8) . ?
N3 C17 1.492(7) . ?
N3 C31 1.494(7) . ?
N3 C32 1.514(7) . ?
N2 C30 1.320(7) . ?
N2 C29 1.429(7) . ?
O1 C1 1.165(8) . ?
O4 C39 1.200(7) . ?
C29 C24 1.385(9) . ?
C29 C28 1.404(10) . ?
O5 C39 1.338(7) . ?
O5 C40 1.454(7) . ?
C28 C27 1.378(10) . ?
O6 C41 1.482(16) . ?
C27 C26 1.389(13) . ?
C26 C25 1.372(13) . ?
C25 C24 1.418(8) . ?
C24 C23 1.457(10) . ?
C23 C22 1.408(9) . ?
C23 C18 1.418(8) . ?
C22 C21 1.366(11) . ?
C21 C20 1.396(11) . ?
C20 C19 1.375(9) . ?
C19 C18 1.415(9) . ?
C18 C30 1.439(8) . ?
C30 C31 1.510(7) . ?
C4 C5 1.398(8) . ?
C4 C9 1.407(8) . ?
C6 C5 1.384(9) . ?
C6 C7 1.386(10) . ?
C7 C8 1.356(10) . ?
C8 C9 1.405(8) . ?
C9 C10 1.452(8) . ?
C10 C11 1.416(8) . ?
C10 C15 1.416(8) . ?
C11 C12 1.369(10) . ?
C12 C13 1.395(10) . ?
C13 C14 1.373(9) . ?
C14 C15 1.394(8) . ?
C15 C16 1.452(7) . ?
C16 C17 1.513(7) . ?
C32 C33 1.523(8) . ?
C33 C34 1.385(8) . ?
C33 C38 1.386(8) . ?
C34 C35 1.385(9) . ?
C35 C36 1.373(8) . ?
C36 C37 1.380(7) . ?
C36 C39 1.491(8) . ?
C37 C38 1.392(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Re1 C2 87.2(3) . . ?
C1 Re1 C3 86.0(3) . . ?
C2 Re1 C3 88.1(3) . . ?
C1 Re1 N2 102.7(3) . . ?
C2 Re1 N2 92.4(3) . . ?
C3 Re1 N2 171.3(2) . . ?
C1 Re1 N3 173.6(2) . . ?
C2 Re1 N3 99.2(2) . . ?
C3 Re1 N3 93.4(2) . . ?
N2 Re1 N3 77.92(19) . . ?
C1 Re1 N1 99.9(3) . . ?
C2 Re1 N1 173.0(2) . . ?
C3 Re1 N1 92.3(2) . . ?
N2 Re1 N1 86.09(19) . . ?
N3 Re1 N1 73.79(17) . . ?
C16 N1 C4 120.4(4) . . ?
C16 N1 Re1 113.4(4) . . ?
C4 N1 Re1 125.5(4) . . ?
O3 C3 Re1 178.9(6) . . ?
O2 C2 Re1 176.7(7) . . ?
C17 N3 C31 109.0(4) . . ?
C17 N3 C32 109.9(4) . . ?
C31 N3 C32 111.5(4) . . ?
C17 N3 Re1 105.9(3) . . ?
C31 N3 Re1 110.6(3) . . ?
C32 N3 Re1 109.8(3) . . ?
C30 N2 C29 117.8(5) . . ?
C30 N2 Re1 115.6(3) . . ?
C29 N2 Re1 126.6(4) . . ?
O1 C1 Re1 177.6(7) . . ?
C24 C29 C28 119.7(6) . . ?
C24 C29 N2 122.2(5) . . ?
C28 C29 N2 118.1(6) . . ?
C39 O5 C40 117.0(5) . . ?
C27 C28 C29 119.9(8) . . ?
C28 C27 C26 121.0(8) . . ?
C25 C26 C27 119.3(7) . . ?
C26 C25 C24 120.8(8) . . ?
C29 C24 C25 119.1(7) . . ?
C29 C24 C23 119.5(5) . . ?
C25 C24 C23 121.4(7) . . ?
C22 C23 C18 119.1(6) . . ?
C22 C23 C24 123.8(6) . . ?
C18 C23 C24 117.1(6) . . ?
C21 C22 C23 120.4(6) . . ?
C22 C21 C20 120.9(7) . . ?
C19 C20 C21 120.3(7) . . ?
C20 C19 C18 120.1(6) . . ?
C19 C18 C23 119.1(6) . . ?
C19 C18 C30 121.5(5) . . ?
C23 C18 C30 119.3(6) . . ?
N2 C30 C18 123.6(5) . . ?
N2 C30 C31 118.4(5) . . ?
C18 C30 C31 118.0(5) . . ?
N3 C31 C30 116.0(5) . . ?
C5 C4 C9 119.1(5) . . ?
C5 C4 N1 119.9(5) . . ?
C9 C4 N1 121.0(5) . . ?
C5 C6 C7 120.2(7) . . ?
C8 C7 C6 119.2(6) . . ?
C7 C8 C9 122.7(6) . . ?
C8 C9 C4 117.7(6) . . ?
C8 C9 C10 123.9(5) . . ?
C4 C9 C10 118.4(5) . . ?
C11 C10 C15 117.3(6) . . ?
C11 C10 C9 123.3(6) . . ?
C15 C10 C9 119.4(5) . . ?
C12 C11 C10 120.9(7) . . ?
C11 C12 C13 120.7(6) . . ?
C14 C13 C12 120.0(7) . . ?
C13 C14 C15 120.1(6) . . ?
C14 C15 C10 120.9(5) . . ?
C14 C15 C16 121.5(5) . . ?
C10 C15 C16 117.6(5) . . ?
N1 C16 C15 122.7(5) . . ?
N1 C16 C17 117.2(4) . . ?
C15 C16 C17 120.1(5) . . ?
N3 C17 C16 110.1(4) . . ?
N3 C32 C33 119.2(5) . . ?
C34 C33 C38 118.4(5) . . ?
C34 C33 C32 122.8(5) . . ?
C38 C33 C32 118.4(5) . . ?
C35 C34 C33 120.2(5) . . ?
C36 C35 C34 121.4(5) . . ?
C35 C36 C37 118.8(5) . . ?
C35 C36 C39 119.1(5) . . ?
C37 C36 C39 122.1(5) . . ?
C36 C37 C38 120.2(5) . . ?
C33 C38 C37 120.9(5) . . ?
O4 C39 O5 122.0(6) . . ?
O4 C39 C36 126.9(5) . . ?
O5 C39 C36 111.0(5) . . ?
C6 C5 C4 120.8(6) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.734
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.095
####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 853882'
_audit_update_record             
;
2016-09-16 deposited with the CCDC.
2016-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H33 Br N3 O7 Re'
_chemical_formula_weight         909.78

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   13.791(2)
_cell_length_b                   13.5301(15)
_cell_length_c                   20.451(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.728(6)
_cell_angle_gamma                90.00
_cell_volume                     3614.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6350
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      25.00

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1792
_exptl_absorpt_coefficient_mu    4.521
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4650
_exptl_absorpt_correction_T_max  0.6606
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            29677
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6350
_reflns_number_gt                5163
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0594P)²+3.8330P] 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         6350
_refine_ls_number_parameters     453
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0533
_refine_ls_wR_factor_ref         0.1423
_refine_ls_wR_factor_gt          0.1322
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.62710(2) 0.19706(2) 0.843475(15) 0.04568(14) Uani 1 1 d . . .
Br1 Br 0.81322(9) -0.12481(8) 0.87733(6) 0.0866(3) Uani 1 1 d . . .
N1 N 0.7176(5) 0.3333(5) 0.8859(3) 0.0449(14) Uani 1 1 d . . .
O1 O 0.4234(6) 0.2418(8) 0.8673(4) 0.103(3) Uani 1 1 d . . .
C1 C 0.5013(8) 0.2251(9) 0.8615(5) 0.073(3) Uani 1 1 d . . .
O2 O 0.5310(6) -0.0062(5) 0.7975(4) 0.090(2) Uani 1 1 d . . .
N2 N 0.7326(5) 0.1358(5) 0.9419(3) 0.0497(15) Uani 1 1 d . . .
C2 C 0.5693(7) 0.0704(7) 0.8133(4) 0.060(2) Uani 1 1 d . . .
O3 O 0.5019(5) 0.2759(5) 0.7003(3) 0.0681(16) Uani 1 1 d . . .
N3 N 0.7712(5) 0.1815(5) 0.8171(3) 0.0436(14) Uani 1 1 d . . .
C3 C 0.5520(6) 0.2479(6) 0.7541(5) 0.0526(19) Uani 1 1 d . . .
O4 O 1.1877(6) 0.0012(6) 0.7059(4) 0.096(2) Uani 1 1 d . . .
C4 C 0.7010(6) 0.3993(6) 0.9366(4) 0.0523(19) Uani 1 1 d . . .
O5 O 1.1724(6) 0.1611(7) 0.6759(5) 0.096(2) Uani 1 1 d . . .
C5 C 0.6319(8) 0.3748(7) 0.9696(5) 0.071(3) Uani 1 1 d . . .
H5A H 0.5978 0.3146 0.9593 0.085 Uiso 1 1 calc R . .
O6 O 0.818(5) -0.1952(18) 1.0230(17) 0.44(4) Uani 1 1 d . . .
C6 C 0.6111(9) 0.4361(8) 1.0176(5) 0.082(3) Uani 1 1 d . . .
H6A H 0.5647 0.4176 1.0398 0.098 Uiso 1 1 calc R . .
O7 O 0.4189(16) -0.261(2) 0.6298(18) 0.310(14) Uani 1 1 d . . .
C7 C 0.6614(10) 0.5259(9) 1.0313(6) 0.091(3) Uani 1 1 d . . .
H7A H 0.6454 0.5704 1.0610 0.110 Uiso 1 1 calc R . .
C8 C 0.7346(8) 0.5504(8) 1.0020(5) 0.078(3) Uani 1 1 d . . .
H8A H 0.7695 0.6100 1.0141 0.094 Uiso 1 1 calc R . .
C9 C 0.7583(7) 0.4884(6) 0.9545(4) 0.058(2) Uani 1 1 d . . .
C10 C 0.8385(6) 0.5082(6) 0.9263(4) 0.055(2) Uani 1 1 d . . .
C11 C 0.9016(8) 0.5929(7) 0.9435(5) 0.073(3) Uani 1 1 d . . .
H11A H 0.8887 0.6401 0.9728 0.088 Uiso 1 1 calc R . .
C12 C 0.9795(8) 0.6070(8) 0.9187(5) 0.079(3) Uani 1 1 d . . .
H12A H 1.0190 0.6640 0.9302 0.094 Uiso 1 1 calc R . .
C13 C 1.0010(8) 0.5375(8) 0.8764(6) 0.081(3) Uani 1 1 d . . .
H13A H 1.0567 0.5473 0.8608 0.097 Uiso 1 1 calc R . .
C14 C 0.9420(7) 0.4533(7) 0.8563(5) 0.068(2) Uani 1 1 d . . .
H14A H 0.9567 0.4076 0.8268 0.082 Uiso 1 1 calc R . .
C15 C 0.8591(6) 0.4380(6) 0.8814(4) 0.0496(18) Uani 1 1 d . . .
C16 C 0.7918(6) 0.3530(6) 0.8615(4) 0.0465(17) Uani 1 1 d . . .
C17 C 0.8046(6) 0.2844(5) 0.8077(4) 0.0471(18) Uani 1 1 d . . .
H17A H 0.8760 0.2835 0.8100 0.057 Uiso 1 1 calc R . .
H17B H 0.7647 0.3084 0.7624 0.057 Uiso 1 1 calc R . .
C18 C 0.353(2) -0.228(4) 0.664(2) 0.46(5) Uani 1 1 d . . .
H18A H 0.3609 -0.2671 0.7041 0.696 Uiso 1 1 calc R . .
H18B H 0.2833 -0.2330 0.6333 0.696 Uiso 1 1 calc R . .
H18C H 0.3677 -0.1599 0.6767 0.696 Uiso 1 1 calc R . .
C19 C 0.723(6) -0.171(3) 1.025(4) 0.47(5) Uani 1 1 d . . .
H19A H 0.7289 -0.1397 1.0681 0.700 Uiso 1 1 calc R . .
H19B H 0.6825 -0.2300 1.0203 0.700 Uiso 1 1 calc R . .
H19C H 0.6905 -0.1267 0.9877 0.700 Uiso 1 1 calc R . .
C20 C 0.9115(7) 0.1085(6) 1.0029(5) 0.064(2) Uani 1 1 d . . .
H20A H 0.9781 0.1060 1.0013 0.077 Uiso 1 1 calc R . .
C21 C 0.8919(8) 0.0918(8) 1.0636(5) 0.078(3) Uani 1 1 d . . .
H21A H 0.9454 0.0804 1.1042 0.093 Uiso 1 1 calc R . .
C22 C 0.7910(8) 0.0921(7) 1.0639(4) 0.068(2) Uani 1 1 d . . .
C23 C 0.7662(10) 0.0714(10) 1.1240(5) 0.094(4) Uani 1 1 d . . .
H23A H 0.8185 0.0569 1.1646 0.113 Uiso 1 1 calc R . .
C24 C 0.6674(11) 0.0720(10) 1.1242(6) 0.104(4) Uani 1 1 d . . .
H24A H 0.6531 0.0600 1.1649 0.125 Uiso 1 1 calc R . .
C25 C 0.5881(10) 0.0905(8) 1.0634(6) 0.088(3) Uani 1 1 d . . .
H25A H 0.5207 0.0891 1.0633 0.105 Uiso 1 1 calc R . .
C26 C 0.6088(8) 0.1109(7) 1.0031(5) 0.069(3) Uani 1 1 d . . .
H26A H 0.5551 0.1225 0.9626 0.082 Uiso 1 1 calc R . .
C27 C 0.7097(7) 0.1143(6) 1.0020(4) 0.057(2) Uani 1 1 d . . .
C28 C 1.1390(7) 0.0774(9) 0.6947(5) 0.071(3) Uani 1 1 d . . .
C29 C 1.2764(9) 0.1609(12) 0.6729(9) 0.126(5) Uani 1 1 d . . .
H29A H 1.2923 0.2249 0.6588 0.188 Uiso 1 1 calc R . .
H29B H 1.2822 0.1121 0.6403 0.188 Uiso 1 1 calc R . .
H29C H 1.3234 0.1455 0.7177 0.188 Uiso 1 1 calc R . .
C30 C 0.8291(6) 0.1294(5) 0.9431(4) 0.0502(18) Uani 1 1 d . . .
C31 C 0.8527(6) 0.1342(6) 0.8765(4) 0.0496(18) Uani 1 1 d . . .
H31A H 0.8643 0.0675 0.8632 0.059 Uiso 1 1 calc R . .
H31B H 0.9160 0.1707 0.8844 0.059 Uiso 1 1 calc R . .
C32 C 0.7557(6) 0.1228(7) 0.7509(4) 0.055(2) Uani 1 1 d . . .
H32A H 0.7291 0.0580 0.7562 0.066 Uiso 1 1 calc R . .
H32B H 0.7046 0.1561 0.7134 0.066 Uiso 1 1 calc R . .
C33 C 0.8520(6) 0.1097(6) 0.7312(4) 0.0492(18) Uani 1 1 d . . .
C34 C 0.8852(8) 0.1830(7) 0.6954(5) 0.065(2) Uani 1 1 d . . .
H34A H 0.8461 0.2397 0.6808 0.078 Uiso 1 1 calc R . .
C35 C 0.9755(7) 0.1713(7) 0.6818(5) 0.062(2) Uani 1 1 d . . .
H35A H 0.9980 0.2216 0.6592 0.075 Uiso 1 1 calc R . .
C36 C 1.0335(6) 0.0875(7) 0.7007(4) 0.0536(19) Uani 1 1 d . . .
C37 C 0.9955(7) 0.0103(7) 0.7290(4) 0.059(2) Uani 1 1 d . . .
H37A H 1.0304 -0.0496 0.7374 0.071 Uiso 1 1 calc R . .
C38 C 0.9058(6) 0.0210(6) 0.7452(4) 0.0520(19) Uani 1 1 d . . .
H38A H 0.8816 -0.0310 0.7653 0.062 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 C2 1.907(9) . ?
Re1 C3 1.917(9) . ?
Re1 C1 1.924(10) . ?
Re1 N3 2.230(6) . ?
Re1 N2 2.230(6) . ?
Re1 N1 2.239(6) . ?
N1 C16 1.301(10) . ?
N1 C4 1.442(10) . ?
O1 C1 1.140(11) . ?
O2 C2 1.162(10) . ?
N2 C30 1.326(10) . ?
N2 C27 1.394(10) . ?
O3 C3 1.159(10) . ?
N3 C17 1.498(9) . ?
N3 C31 1.506(9) . ?
N3 C32 1.525(9) . ?
O4 C28 1.211(12) . ?
C4 C5 1.373(12) . ?
C4 C9 1.423(12) . ?
O5 C28 1.326(13) . ?
O5 C29 1.455(12) . ?
C5 C6 1.383(12) . ?
O6 C19 1.37(8) . ?
C6 C7 1.383(15) . ?
O7 C18 1.39(5) . ?
C7 C8 1.369(15) . ?
C8 C9 1.401(12) . ?
C9 C10 1.426(12) . ?
C10 C15 1.414(11) . ?
C10 C11 1.414(12) . ?
C11 C12 1.341(14) . ?
C12 C13 1.375(15) . ?
C13 C14 1.384(13) . ?
C14 C15 1.410(12) . ?
C15 C16 1.452(11) . ?
C16 C17 1.493(10) . ?
C20 C21 1.372(13) . ?
C20 C30 1.405(12) . ?
C21 C22 1.393(14) . ?
C22 C23 1.404(13) . ?
C22 C27 1.427(12) . ?
C23 C24 1.364(17) . ?
C24 C25 1.389(16) . ?
C25 C26 1.381(13) . ?
C26 C27 1.399(13) . ?
C28 C36 1.506(11) . ?
C30 C31 1.501(11) . ?
C32 C33 1.517(10) . ?
C33 C38 1.392(11) . ?
C33 C34 1.394(12) . ?
C34 C35 1.369(13) . ?
C35 C36 1.370(12) . ?
C36 C37 1.376(12) . ?
C37 C38 1.387(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
C2 Re1 C3 88.4(4) . . ?
C2 Re1 C1 86.0(4) . . ?
C3 Re1 C1 82.4(4) . . ?
C2 Re1 N3 98.6(3) . . ?
C3 Re1 N3 93.1(3) . . ?
C1 Re1 N3 173.5(4) . . ?
C2 Re1 N2 92.4(3) . . ?
C3 Re1 N2 172.1(3) . . ?
C1 Re1 N2 105.5(3) . . ?
N3 Re1 N2 79.0(2) . . ?
C2 Re1 N1 171.2(3) . . ?
C3 Re1 N1 97.9(3) . . ?
C1 Re1 N1 100.9(4) . . ?
N3 Re1 N1 75.1(2) . . ?
N2 Re1 N1 80.5(2) . . ?
C16 N1 C4 118.4(7) . . ?
C16 N1 Re1 115.4(5) . . ?
C4 N1 Re1 126.2(5) . . ?
O1 C1 Re1 175.2(9) . . ?
C30 N2 C27 118.7(7) . . ?
C30 N2 Re1 113.6(5) . . ?
C27 N2 Re1 127.4(6) . . ?
O2 C2 Re1 176.2(8) . . ?
C17 N3 C31 108.5(6) . . ?
C17 N3 C32 109.3(6) . . ?
C31 N3 C32 110.5(6) . . ?
C17 N3 Re1 106.2(4) . . ?
C31 N3 Re1 109.7(4) . . ?
C32 N3 Re1 112.5(4) . . ?
O3 C3 Re1 176.2(7) . . ?
C5 C4 C9 119.6(8) . . ?
C5 C4 N1 120.0(8) . . ?
C9 C4 N1 120.3(7) . . ?
C28 O5 C29 116.7(10) . . ?
C4 C5 C6 122.6(10) . . ?
C7 C6 C5 117.8(10) . . ?
C8 C7 C6 121.1(10) . . ?
C7 C8 C9 121.9(10) . . ?
C8 C9 C4 116.8(9) . . ?
C8 C9 C10 123.5(8) . . ?
C4 C9 C10 119.7(7) . . ?
C15 C10 C11 118.1(8) . . ?
C15 C10 C9 118.7(7) . . ?
C11 C10 C9 123.2(8) . . ?
C12 C11 C10 121.7(10) . . ?
C11 C12 C13 120.2(10) . . ?
C12 C13 C14 121.6(10) . . ?
C13 C14 C15 118.8(9) . . ?
C14 C15 C10 119.6(7) . . ?
C14 C15 C16 122.4(8) . . ?
C10 C15 C16 118.0(7) . . ?
N1 C16 C15 124.5(7) . . ?
N1 C16 C17 116.7(7) . . ?
C15 C16 C17 118.8(7) . . ?
C16 C17 N3 111.6(6) . . ?
C21 C20 C30 118.8(9) . . ?
C20 C21 C22 119.4(8) . . ?
C21 C22 C23 121.8(9) . . ?
C21 C22 C27 119.8(8) . . ?
C23 C22 C27 118.4(10) . . ?
C24 C23 C22 121.7(10) . . ?
C23 C24 C25 119.9(10) . . ?
C26 C25 C24 120.4(11) . . ?
C25 C26 C27 120.8(10) . . ?
N2 C27 C26 121.8(8) . . ?
N2 C27 C22 119.4(8) . . ?
C26 C27 C22 118.7(8) . . ?
O4 C28 O5 124.0(9) . . ?
O4 C28 C36 123.6(10) . . ?
O5 C28 C36 112.4(9) . . ?
N2 C30 C20 123.8(8) . . ?
N2 C30 C31 119.3(7) . . ?
C20 C30 C31 116.6(7) . . ?
C30 C31 N3 115.2(6) . . ?
C33 C32 N3 114.3(6) . . ?
C38 C33 C34 118.6(7) . . ?
C38 C33 C32 120.0(7) . . ?
C34 C33 C32 121.3(7) . . ?
C35 C34 C33 119.9(8) . . ?
C34 C35 C36 121.6(9) . . ?
C35 C36 C37 118.7(8) . . ?
C35 C36 C28 123.0(9) . . ?
C37 C36 C28 118.2(8) . . ?
C36 C37 C38 120.6(8) . . ?
C37 C38 C33 119.9(8) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.198
_refine_diff_density_min         -1.610
_refine_diff_density_rms         0.128
####################################################################### 
# 
# 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_exp_1900ac1s
_database_code_depnum_ccdc_archive 'CCDC 853883'
_audit_update_record             
;
2016-09-16 deposited with the CCDC.
2016-12-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H31 Br N3 O7 Re'
_chemical_formula_weight         859.73

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'
Br Br -0.2901 2.4595 '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   P2(1)/n

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

_cell_length_a                   14.2253(4)
_cell_length_b                   13.4844(3)
_cell_length_c                   19.7773(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.927(3)
_cell_angle_gamma                90.00
_cell_volume                     3566.54(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    6249
_cell_measurement_theta_min      3.05
_cell_measurement_theta_max      25.00

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1688
_exptl_absorpt_coefficient_mu    4.575
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3607
_exptl_absorpt_correction_T_max  0.8035
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Xcalibur2'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19688
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6249
_reflns_number_gt                5355
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0411P)²+1.6483P] 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         6249
_refine_ls_number_parameters     417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0834
_refine_ls_wR_factor_gt          0.0788
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.957200(12) 0.819414(13) 0.240370(9) 0.01864(8) Uani 1 1 d . . .
N1 N 0.9656(3) 0.6743(3) 0.2996(2) 0.0207(8) Uani 1 1 d . . .
O1 O 1.1142(3) 0.8051(3) 0.1661(2) 0.0414(9) Uani 1 1 d . . .
C1 C 1.0569(4) 0.8076(3) 0.1956(3) 0.0275(11) Uani 1 1 d . . .
Br1 Br 0.57646(4) 0.64936(4) 0.15146(3) 0.03765(14) Uani 1 1 d . . .
N2 N 1.0538(3) 0.8597(3) 0.3476(2) 0.0208(8) Uani 1 1 d . . .
O2 O 0.9380(2) 1.0307(3) 0.17997(18) 0.0342(8) Uani 1 1 d . . .
C2 C 0.9440(3) 0.9520(4) 0.2031(2) 0.0253(10) Uani 1 1 d . . .
N3 N 0.8462(3) 0.8372(3) 0.29600(19) 0.0175(8) Uani 1 1 d . . .
O3 O 0.8082(3) 0.7576(2) 0.09343(18) 0.0353(8) Uani 1 1 d . . .
C3 C 0.8621(4) 0.7786(3) 0.1495(3) 0.0253(10) Uani 1 1 d . . .
O4 O 0.3887(3) 0.9140(3) 0.3797(2) 0.0496(10) Uani 1 1 d . . .
C4 C 1.0412(3) 0.6013(3) 0.3146(2) 0.0270(11) Uani 1 1 d . . .
O5 O 0.4614(3) 1.0628(3) 0.4107(2) 0.0401(9) Uani 1 1 d . . .
C5 C 1.1183(4) 0.6108(4) 0.2866(3) 0.0388(13) Uani 1 1 d . . .
H5A H 1.1188 0.6663 0.2572 0.047 Uiso 1 1 calc R . .
O6 O 0.3614(5) 0.5869(6) 0.1837(4) 0.125(2) Uani 1 1 d . . .
C6 C 1.1932(4) 0.5424(4) 0.3004(3) 0.0455(14) Uani 1 1 d . . .
H6A H 1.2454 0.5509 0.2812 0.055 Uiso 1 1 calc R . .
O7 O 0.3846(3) 0.7304(3) 0.0124(2) 0.0563(11) Uani 1 1 d . . .
C7 C 1.1927(4) 0.4602(4) 0.3428(3) 0.0475(15) Uani 1 1 d . . .
H7A H 1.2451 0.4127 0.3528 0.057 Uiso 1 1 calc R . .
C8 C 1.1169(4) 0.4472(4) 0.3702(3) 0.0412(14) Uani 1 1 d . . .
H8A H 1.1167 0.3902 0.3984 0.049 Uiso 1 1 calc R . .
C9 C 1.0397(4) 0.5172(3) 0.3570(2) 0.0269(11) Uani 1 1 d . . .
C10 C 0.9599(3) 0.5045(3) 0.3855(2) 0.0259(10) Uani 1 1 d . . .
C11 C 0.9518(4) 0.4223(4) 0.4272(3) 0.0372(13) Uani 1 1 d . . .
H11A H 1.0009 0.3714 0.4374 0.045 Uiso 1 1 calc R . .
C12 C 0.8743(4) 0.4147(4) 0.4531(3) 0.0423(14) Uani 1 1 d . . .
H12A H 0.8707 0.3591 0.4816 0.051 Uiso 1 1 calc R . .
C13 C 0.8008(4) 0.4877(4) 0.4383(3) 0.0361(12) Uani 1 1 d . . .
H13A H 0.7471 0.4815 0.4563 0.043 Uiso 1 1 calc R . .
C14 C 0.8062(4) 0.5681(4) 0.3978(3) 0.0300(11) Uani 1 1 d . . .
H14A H 0.7559 0.6178 0.3877 0.036 Uiso 1 1 calc R . .
C15 C 0.8868(3) 0.5785(3) 0.3706(2) 0.0234(10) Uani 1 1 d . . .
C16 C 0.8934(3) 0.6613(3) 0.3270(2) 0.0224(10) Uani 1 1 d . . .
C17 C 0.8105(3) 0.7375(3) 0.3066(3) 0.0233(10) Uani 1 1 d . . .
H17A H 0.7578 0.7163 0.2617 0.028 Uiso 1 1 calc R . .
H17B H 0.7805 0.7407 0.3449 0.028 Uiso 1 1 calc R . .
C18 C 0.6792(3) 0.9159(3) 0.2888(2) 0.0222(10) Uani 1 1 d . . .
C19 C 0.6810(3) 1.0040(3) 0.3260(2) 0.0210(9) Uani 1 1 d . . .
H19A H 0.7317 1.0516 0.3300 0.025 Uiso 1 1 calc R . .
C20 C 0.6091(3) 1.0224(3) 0.3573(2) 0.0239(10) Uani 1 1 d . . .
H20A H 0.6112 1.0825 0.3828 0.029 Uiso 1 1 calc R . .
C21 C 0.5338(3) 0.9535(3) 0.3515(2) 0.0250(10) Uani 1 1 d . . .
C22 C 0.5319(4) 0.8663(4) 0.3143(3) 0.0338(12) Uani 1 1 d . . .
H22A H 0.4814 0.8184 0.3106 0.041 Uiso 1 1 calc R . .
C23 C 0.6035(4) 0.8480(4) 0.2823(3) 0.0325(12) Uani 1 1 d . . .
H23A H 0.6005 0.7886 0.2558 0.039 Uiso 1 1 calc R . .
C24 C 0.4546(4) 0.9722(4) 0.3818(3) 0.0341(12) Uani 1 1 d . . .
C25 C 0.3828(4) 1.0890(5) 0.4394(4) 0.0513(16) Uani 1 1 d . . .
H25A H 0.3944 1.1563 0.4592 0.077 Uiso 1 1 calc R . .
H25B H 0.3836 1.0422 0.4775 0.077 Uiso 1 1 calc R . .
H25C H 0.3177 1.0861 0.4008 0.077 Uiso 1 1 calc R . .
C26 C 1.1555(3) 0.8599(3) 0.3718(2) 0.0243(10) Uani 1 1 d . . .
H26A H 1.1888 0.8502 0.3381 0.029 Uiso 1 1 calc R . .
C27 C 1.2114(3) 0.8734(4) 0.4422(3) 0.0299(11) Uani 1 1 d . . .
H27A H 1.2823 0.8713 0.4576 0.036 Uiso 1 1 calc R . .
C28 C 1.1627(3) 0.8903(3) 0.4909(3) 0.0276(11) Uani 1 1 d . . .
H28A H 1.2000 0.9010 0.5403 0.033 Uiso 1 1 calc R . .
C29 C 1.0588(3) 0.8916(3) 0.4670(2) 0.0230(10) Uani 1 1 d . . .
H29A H 1.0242 0.9026 0.4998 0.028 Uiso 1 1 calc R . .
C30 C 1.0068(3) 0.8765(3) 0.3953(2) 0.0177(9) Uani 1 1 d . . .
C31 C 0.8955(3) 0.8887(3) 0.3663(2) 0.0208(10) Uani 1 1 d . . .
H31A H 0.8796 0.9603 0.3601 0.025 Uiso 1 1 calc R . .
H31B H 0.8672 0.8625 0.4021 0.025 Uiso 1 1 calc R . .
C32 C 0.7558(3) 0.8984(4) 0.2528(2) 0.0232(10) Uani 1 1 d . . .
H32A H 0.7796 0.9635 0.2420 0.028 Uiso 1 1 calc R . .
H32B H 0.7225 0.8645 0.2063 0.028 Uiso 1 1 calc R . .
C33 C 0.3554(8) 0.6760(6) 0.2130(7) 0.115(4) Uani 1 1 d . . .
H33A H 0.3986 0.6763 0.2636 0.173 Uiso 1 1 calc R . .
H33B H 0.2861 0.6884 0.2098 0.173 Uiso 1 1 calc R . .
H33C H 0.3770 0.7280 0.1869 0.173 Uiso 1 1 calc R . .
C34 C 0.2902(6) 0.6995(5) 0.0121(5) 0.076(3) Uani 1 1 d . . .
H34A H 0.2965 0.6354 0.0367 0.114 Uiso 1 1 calc R . .
H34B H 0.2449 0.6927 -0.0377 0.114 Uiso 1 1 calc R . .
H34C H 0.2633 0.7488 0.0371 0.114 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 C1 1.918(5) . ?
Re1 C2 1.919(5) . ?
Re1 C3 1.925(5) . ?
Re1 N2 2.166(4) . ?
Re1 N3 2.224(4) . ?
Re1 N1 2.263(4) . ?
N1 C16 1.326(6) . ?
N1 C4 1.412(6) . ?
O1 C1 1.154(6) . ?
N2 C30 1.349(5) . ?
N2 C26 1.359(5) . ?
O2 C2 1.147(5) . ?
N3 C17 1.477(5) . ?
N3 C31 1.498(5) . ?
N3 C32 1.522(5) . ?
O3 C3 1.148(6) . ?
O4 C24 1.212(6) . ?
C4 C5 1.391(7) . ?
C4 C9 1.415(7) . ?
O5 C24 1.339(6) . ?
O5 C25 1.460(6) . ?
C5 C6 1.365(7) . ?
O6 C33 1.350(10) . ?
C6 C7 1.392(8) . ?
O7 C34 1.403(7) . ?
C7 C8 1.373(8) . ?
C8 C9 1.403(7) . ?
C9 C10 1.440(7) . ?
C10 C15 1.398(6) . ?
C10 C11 1.409(7) . ?
C11 C12 1.370(8) . ?
C12 C13 1.393(8) . ?
C13 C14 1.366(7) . ?
C14 C15 1.430(6) . ?
C15 C16 1.434(6) . ?
C16 C17 1.511(6) . ?
C18 C23 1.385(6) . ?
C18 C19 1.393(6) . ?
C18 C32 1.510(6) . ?
C19 C20 1.385(6) . ?
C20 C21 1.394(6) . ?
C21 C22 1.382(7) . ?
C21 C24 1.467(7) . ?
C22 C23 1.393(7) . ?
C26 C27 1.360(6) . ?
C27 C28 1.384(7) . ?
C28 C29 1.391(6) . ?
C29 C30 1.373(6) . ?
C30 C31 1.497(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Re1 C2 83.76(19) . . ?
C1 Re1 C3 86.6(2) . . ?
C2 Re1 C3 87.84(19) . . ?
C1 Re1 N2 98.66(17) . . ?
C2 Re1 N2 95.08(16) . . ?
C3 Re1 N2 174.23(16) . . ?
C1 Re1 N3 177.52(16) . . ?
C2 Re1 N3 95.53(16) . . ?
C3 Re1 N3 95.77(16) . . ?
N2 Re1 N3 79.01(13) . . ?
C1 Re1 N1 104.48(17) . . ?
C2 Re1 N1 170.31(17) . . ?
C3 Re1 N1 97.60(16) . . ?
N2 Re1 N1 78.83(13) . . ?
N3 Re1 N1 76.01(13) . . ?
C16 N1 C4 117.6(4) . . ?
C16 N1 Re1 114.5(3) . . ?
C4 N1 Re1 127.8(3) . . ?
O1 C1 Re1 176.0(4) . . ?
C30 N2 C26 118.4(4) . . ?
C30 N2 Re1 115.2(3) . . ?
C26 N2 Re1 126.1(3) . . ?
O2 C2 Re1 178.1(4) . . ?
C17 N3 C31 111.4(3) . . ?
C17 N3 C32 108.0(3) . . ?
C31 N3 C32 108.0(3) . . ?
C17 N3 Re1 107.9(3) . . ?
C31 N3 Re1 108.8(2) . . ?
C32 N3 Re1 112.7(3) . . ?
O3 C3 Re1 176.0(4) . . ?
C5 C4 N1 120.0(4) . . ?
C5 C4 C9 118.8(4) . . ?
N1 C4 C9 121.2(4) . . ?
C24 O5 C25 115.7(4) . . ?
C6 C5 C4 121.8(5) . . ?
C5 C6 C7 119.7(5) . . ?
C8 C7 C6 120.3(5) . . ?
C7 C8 C9 120.8(5) . . ?
C8 C9 C4 118.7(5) . . ?
C8 C9 C10 121.2(5) . . ?
C4 C9 C10 120.0(4) . . ?
C15 C10 C11 118.8(5) . . ?
C15 C10 C9 117.5(4) . . ?
C11 C10 C9 123.7(4) . . ?
C12 C11 C10 121.0(5) . . ?
C11 C12 C13 120.8(5) . . ?
C14 C13 C12 119.7(5) . . ?
C13 C14 C15 120.7(5) . . ?
C10 C15 C14 119.0(4) . . ?
C10 C15 C16 119.1(4) . . ?
C14 C15 C16 121.9(4) . . ?
N1 C16 C15 124.6(4) . . ?
N1 C16 C17 116.3(4) . . ?
C15 C16 C17 119.0(4) . . ?
N3 C17 C16 112.5(4) . . ?
C23 C18 C19 119.1(4) . . ?
C23 C18 C32 121.1(4) . . ?
C19 C18 C32 119.8(4) . . ?
C20 C19 C18 120.4(4) . . ?
C19 C20 C21 120.5(4) . . ?
C22 C21 C20 119.1(4) . . ?
C22 C21 C24 119.0(4) . . ?
C20 C21 C24 121.9(4) . . ?
C21 C22 C23 120.5(5) . . ?
C18 C23 C22 120.5(5) . . ?
O4 C24 O5 123.2(5) . . ?
O4 C24 C21 124.6(5) . . ?
O5 C24 C21 112.2(4) . . ?
N2 C26 C27 122.8(4) . . ?
C26 C27 C28 118.5(4) . . ?
C27 C28 C29 119.4(4) . . ?
C30 C29 C28 119.0(4) . . ?
N2 C30 C29 121.8(4) . . ?
N2 C30 C31 117.5(4) . . ?
C29 C30 C31 120.4(4) . . ?
C30 C31 N3 113.9(3) . . ?
C18 C32 N3 115.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.708
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.133
