# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_re2anth
_database_code_depnum_ccdc_archive 'CCDC 1581215'
_audit_update_record             
;
2017-10-20 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Anthracenyldirheniumoctacarbonylhydride
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H10 O8 Re2'
_chemical_formula_weight         774.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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)/c

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

_cell_length_a                   13.5703(6)
_cell_length_b                   13.8800(6)
_cell_length_c                   11.6405(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.1290(10)
_cell_angle_gamma                90.00
_cell_volume                     2183.78(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9645
_cell_measurement_theta_min      2.653
_cell_measurement_theta_max      27.662

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    11.122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3050
_exptl_absorpt_correction_T_max  0.7314
_exptl_absorpt_process_details   '(SADABS, Bruker, 2016)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Incoatec microfocus source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 QUEST diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            99717
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         27.77
_reflns_number_total             5151
_reflns_number_gt                4128
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1990)'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'

_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)+(0.0137P)²+3.3632P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5151
_refine_ls_number_parameters     293
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0421
_refine_ls_wR_factor_gt          0.0385
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_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 0.190638(11) 0.635032(11) 0.306112(12) 0.03595(5) Uani 1 1 d . . .
Re2 Re 0.175991(12) 0.425677(13) 0.380894(14) 0.04607(5) Uani 1 1 d . . .
O15 O 0.3867(2) 0.6655(2) 0.4646(3) 0.0579(8) Uani 1 1 d . . .
O16 O 0.2458(2) 0.7974(2) 0.1448(3) 0.0624(8) Uani 1 1 d . . .
O17 O 0.0863(3) 0.7802(3) 0.4519(3) 0.0776(10) Uani 1 1 d . . .
O18 O -0.0077(2) 0.6215(3) 0.1497(3) 0.0698(10) Uani 1 1 d . . .
O25 O 0.3876(3) 0.4384(3) 0.5082(4) 0.0851(11) Uani 1 1 d . . .
O26 O 0.2198(3) 0.2163(3) 0.3174(4) 0.0865(12) Uani 1 1 d . . .
O27 O 0.0987(3) 0.3768(4) 0.6155(4) 0.1233(18) Uani 1 1 d . . .
O28 O -0.0431(3) 0.4010(3) 0.2806(4) 0.0931(13) Uani 1 1 d . . .
C1 C 0.3137(3) 0.5280(3) 0.2091(3) 0.0359(8) Uani 1 1 d . . .
H1 H 0.3529 0.5410 0.2770 0.043 Uiso 1 1 calc R . .
C2 C 0.2241(3) 0.4812(3) 0.2175(3) 0.0397(9) Uani 1 1 d . . .
C3 C 0.1670(3) 0.4634(3) 0.1060(3) 0.0458(10) Uani 1 1 d . . .
H3 H 0.1057 0.4335 0.1059 0.055 Uiso 1 1 calc R . .
C4 C 0.1992(3) 0.4884(3) 0.0049(3) 0.0465(10) Uani 1 1 d . . .
H4 H 0.1605 0.4732 -0.0626 0.056 Uiso 1 1 calc R . .
C5 C 0.4558(4) 0.6320(3) -0.2182(4) 0.0589(12) Uani 1 1 d . . .
H5 H 0.4188 0.6191 -0.2875 0.071 Uiso 1 1 calc R . .
C6 C 0.5447(4) 0.6752(4) -0.2193(5) 0.0675(14) Uani 1 1 d . . .
H6 H 0.5676 0.6925 -0.2894 0.081 Uiso 1 1 calc R . .
C7 C 0.6033(4) 0.6946(3) -0.1164(5) 0.0634(13) Uani 1 1 d . . .
H7 H 0.6647 0.7240 -0.1189 0.076 Uiso 1 1 calc R . .
C8 C 0.5709(3) 0.6706(3) -0.0135(4) 0.0522(11) Uani 1 1 d . . .
H8 H 0.6103 0.6835 0.0543 0.063 Uiso 1 1 calc R . .
C9 C 0.4408(3) 0.6010(3) 0.0968(3) 0.0392(9) Uani 1 1 d . . .
H9 H 0.4791 0.6142 0.1652 0.047 Uiso 1 1 calc R . .
C10 C 0.3261(3) 0.5621(3) -0.1075(3) 0.0454(10) Uani 1 1 d . . .
H10 H 0.2874 0.5490 -0.1758 0.054 Uiso 1 1 calc R . .
C11 C 0.3498(3) 0.5575(2) 0.1014(3) 0.0340(8) Uani 1 1 d . . .
C12 C 0.2909(3) 0.5374(3) -0.0033(3) 0.0394(9) Uani 1 1 d . . .
C13 C 0.4768(3) 0.6258(3) -0.0080(3) 0.0402(9) Uani 1 1 d . . .
C14 C 0.4180(3) 0.6060(3) -0.1125(3) 0.0450(10) Uani 1 1 d . . .
C15 C 0.3160(3) 0.6537(3) 0.4079(3) 0.0400(9) Uani 1 1 d . . .
C16 C 0.2273(3) 0.7362(3) 0.2043(3) 0.0421(9) Uani 1 1 d . . .
C17 C 0.1254(3) 0.7266(3) 0.3977(4) 0.0517(11) Uani 1 1 d . . .
C18 C 0.0638(3) 0.6225(3) 0.2060(4) 0.0463(10) Uani 1 1 d . . .
C25 C 0.3118(4) 0.4357(3) 0.4600(4) 0.0539(11) Uani 1 1 d . . .
C26 C 0.2024(3) 0.2940(4) 0.3425(4) 0.0602(12) Uani 1 1 d . . .
C27 C 0.1273(4) 0.3937(4) 0.5296(5) 0.0749(15) Uani 1 1 d . . .
C28 C 0.0370(4) 0.4122(4) 0.3134(4) 0.0600(12) Uani 1 1 d . . .
H2 H 0.145(3) 0.546(3) 0.406(4) 0.081(15) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C17 1.925(5) . ?
Re1 C16 1.931(4) . ?
Re1 C18 1.998(4) . ?
Re1 C15 2.002(4) . ?
Re1 C2 2.431(4) . ?
Re1 C1 2.571(3) . ?
Re1 Re2 3.0450(3) . ?
Re1 H2 1.84(5) . ?
Re2 C26 1.922(6) . ?
Re2 C27 1.958(5) . ?
Re2 C28 1.986(5) . ?
Re2 C25 1.989(5) . ?
Re2 C2 2.205(4) . ?
Re2 H2 1.76(5) . ?
O15 C15 1.127(4) . ?
O16 C16 1.138(5) . ?
O17 C17 1.137(5) . ?
O18 C18 1.121(5) . ?
O25 C25 1.128(5) . ?
O26 C26 1.148(6) . ?
O27 C27 1.129(5) . ?
O28 C28 1.130(5) . ?
C1 C2 1.389(5) . ?
C1 C11 1.446(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.472(5) . ?
C3 C4 1.337(5) . ?
C3 H3 0.9300 . ?
C4 C12 1.429(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.348(7) . ?
C5 C14 1.421(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.403(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.354(6) . ?
C7 H7 0.9300 . ?
C8 C13 1.427(5) . ?
C8 H8 0.9300 . ?
C9 C11 1.380(5) . ?
C9 C13 1.396(5) . ?
C9 H9 0.9300 . ?
C10 C12 1.386(5) . ?
C10 C14 1.395(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.423(5) . ?
C13 C14 1.421(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
C17 Re1 C16 90.92(17) . . ?
C17 Re1 C18 88.04(17) . . ?
C16 Re1 C18 87.76(16) . . ?
C17 Re1 C15 89.72(16) . . ?
C16 Re1 C15 90.97(15) . . ?
C18 Re1 C15 177.41(16) . . ?
C17 Re1 C2 158.06(16) . . ?
C16 Re1 C2 108.05(14) . . ?
C18 Re1 C2 81.95(15) . . ?
C15 Re1 C2 100.59(14) . . ?
C17 Re1 C1 166.91(15) . . ?
C16 Re1 C1 86.42(14) . . ?
C18 Re1 C1 104.64(14) . . ?
C15 Re1 C1 77.52(13) . . ?
C2 Re1 C1 32.08(11) . . ?
C17 Re1 Re2 115.29(13) . . ?
C16 Re1 Re2 153.67(11) . . ?
C18 Re1 Re2 90.51(12) . . ?
C15 Re1 Re2 91.62(11) . . ?
C2 Re1 Re2 45.80(9) . . ?
C1 Re1 Re2 68.62(8) . . ?
C17 Re1 H2 83.9(14) . . ?
C16 Re1 H2 174.2(14) . . ?
C18 Re1 H2 89.5(14) . . ?
C15 Re1 H2 91.6(14) . . ?
C2 Re1 H2 76.5(14) . . ?
C1 Re1 H2 99.2(14) . . ?
Re2 Re1 H2 31.4(14) . . ?
C26 Re2 C27 94.3(2) . . ?
C26 Re2 C28 90.5(2) . . ?
C27 Re2 C28 86.9(2) . . ?
C26 Re2 C25 89.39(19) . . ?
C27 Re2 C25 88.7(2) . . ?
C28 Re2 C25 175.57(18) . . ?
C26 Re2 C2 93.23(17) . . ?
C27 Re2 C2 172.4(2) . . ?
C28 Re2 C2 92.06(16) . . ?
C25 Re2 C2 92.37(16) . . ?
C26 Re2 Re1 145.32(14) . . ?
C27 Re2 Re1 120.32(18) . . ?
C28 Re2 Re1 93.49(14) . . ?
C25 Re2 Re1 89.11(12) . . ?
C2 Re2 Re1 52.24(10) . . ?
C26 Re2 H2 175.5(15) . . ?
C27 Re2 H2 87.9(15) . . ?
C28 Re2 H2 85.7(15) . . ?
C25 Re2 H2 94.6(15) . . ?
C2 Re2 H2 84.5(15) . . ?
Re1 Re2 H2 33.0(15) . . ?
C2 C1 C11 124.1(3) . . ?
C2 C1 Re1 68.4(2) . . ?
C11 C1 Re1 120.0(2) . . ?
C2 C1 H1 118.0 . . ?
C11 C1 H1 118.0 . . ?
Re1 C1 H1 81.9 . . ?
C1 C2 C3 114.3(3) . . ?
C1 C2 Re2 123.6(3) . . ?
C3 C2 Re2 121.9(3) . . ?
C1 C2 Re1 79.5(2) . . ?
C3 C2 Re1 114.7(3) . . ?
Re2 C2 Re1 81.97(12) . . ?
C4 C3 C2 123.0(4) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C12 122.5(4) . . ?
C3 C4 H4 118.7 . . ?
C12 C4 H4 118.7 . . ?
C6 C5 C14 120.9(5) . . ?
C6 C5 H5 119.5 . . ?
C14 C5 H5 119.5 . . ?
C5 C6 C7 121.1(4) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 120.2(4) . . ?
C8 C7 H7 119.9 . . ?
C6 C7 H7 119.9 . . ?
C7 C8 C13 120.7(5) . . ?
C7 C8 H8 119.7 . . ?
C13 C8 H8 119.7 . . ?
C11 C9 C13 121.7(4) . . ?
C11 C9 H9 119.1 . . ?
C13 C9 H9 119.1 . . ?
C12 C10 C14 121.6(4) . . ?
C12 C10 H10 119.2 . . ?
C14 C10 H10 119.2 . . ?
C9 C11 C12 119.2(3) . . ?
C9 C11 C1 122.1(3) . . ?
C12 C11 C1 118.6(3) . . ?
C10 C12 C11 119.4(3) . . ?
C10 C12 C4 123.1(4) . . ?
C11 C12 C4 117.5(3) . . ?
C9 C13 C14 119.2(3) . . ?
C9 C13 C8 122.1(4) . . ?
C14 C13 C8 118.8(4) . . ?
C10 C14 C5 122.8(4) . . ?
C10 C14 C13 119.0(3) . . ?
C5 C14 C13 118.3(4) . . ?
O15 C15 Re1 179.1(4) . . ?
O16 C16 Re1 177.6(4) . . ?
O17 C17 Re1 179.4(4) . . ?
O18 C18 Re1 175.7(4) . . ?
O25 C25 Re2 177.0(4) . . ?
O26 C26 Re2 178.1(5) . . ?
O27 C27 Re2 178.8(6) . . ?
O28 C28 Re2 175.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.77
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.064
_refine_diff_density_min         -1.003
_refine_diff_density_rms         0.109
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane'
####################################################################### 
# 
# 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_p21n
_database_code_depnum_ccdc_archive 'CCDC 1581216'
_audit_update_record             
;
2017-10-20 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'anthrceneyl bis(dirheniumoctacarbonylhydride)'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H10 O16 Re4'
_chemical_formula_weight         1371.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   9.3222(4)
_cell_length_b                   17.8131(8)
_cell_length_c                   21.1743(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.8010(10)
_cell_angle_gamma                90.00
_cell_volume                     3441.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    294(2)
_cell_measurement_reflns_used    8070
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.26

_exptl_crystal_description       rectangular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2472
_exptl_absorpt_coefficient_mu    14.094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.35076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      294(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  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            46257
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         28.33
_reflns_number_total             8551
_reflns_number_gt                7409
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'

_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)+(0.0409P)²+3.0261P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8551
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0985
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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 1.01293(3) 0.865075(15) 0.290103(13) 0.04756(8) Uani 1 1 d . . .
Re2 Re 0.95391(3) 0.704871(16) 0.329814(12) 0.04547(8) Uani 1 1 d . . .
Re3 Re 0.96657(3) 0.615217(14) 0.114568(11) 0.03961(8) Uani 1 1 d . . .
Re4 Re 1.24633(3) 0.687745(14) 0.090084(12) 0.04043(8) Uani 1 1 d . . .
O15 O 1.3248(7) 0.8269(5) 0.2653(4) 0.094(2) Uani 1 1 d . . .
O16 O 1.0029(9) 0.9943(4) 0.1922(3) 0.090(2) Uani 1 1 d . . .
O17 O 1.1758(10) 0.9623(5) 0.4017(4) 0.114(3) Uani 1 1 d . . .
O18 O 0.7157(8) 0.9214(4) 0.3203(4) 0.105(3) Uani 1 1 d . . .
O25 O 1.2881(8) 0.6724(5) 0.3472(4) 0.108(3) Uani 1 1 d . . .
O26 O 0.8756(10) 0.5388(4) 0.3035(4) 0.100(2) Uani 1 1 d . . .
O27 O 0.9671(10) 0.6836(5) 0.4763(3) 0.105(3) Uani 1 1 d . . .
O28 O 0.6195(7) 0.7393(5) 0.3049(3) 0.091(2) Uani 1 1 d . . .
O35 O 1.1350(7) 0.5146(4) 0.2260(3) 0.0778(17) Uani 1 1 d . . .
O36 O 0.6880(6) 0.6110(4) 0.1710(3) 0.0830(19) Uani 1 1 d . . .
O37 O 0.8812(9) 0.4662(4) 0.0448(3) 0.096(2) Uani 1 1 d . . .
O38 O 0.7876(8) 0.6931(4) -0.0092(3) 0.091(2) Uani 1 1 d . . .
O45 O 1.4124(6) 0.6270(4) 0.2229(3) 0.0770(18) Uani 1 1 d . . .
O46 O 1.4750(8) 0.6014(5) 0.0303(4) 0.101(2) Uani 1 1 d . . .
O47 O 1.4326(8) 0.8307(4) 0.1185(3) 0.0817(18) Uani 1 1 d . . .
O48 O 1.1205(9) 0.7182(4) -0.0554(3) 0.096(2) Uani 1 1 d . . .
C1 C 0.8517(7) 0.7977(3) 0.1988(3) 0.0397(13) Uani 1 1 d . . .
H1 H 0.7760 0.8139 0.2179 0.048 Uiso 1 1 calc R . .
C2 C 0.9508(7) 0.7462(3) 0.2315(3) 0.0379(12) Uani 1 1 d . . .
C3 C 1.0569(6) 0.7186(3) 0.1939(3) 0.0351(11) Uani 1 1 d . . .
H3 H 1.1207 0.6813 0.2133 0.042 Uiso 1 1 calc R . .
C4 C 1.0735(6) 0.7417(3) 0.1325(3) 0.0352(11) Uani 1 1 d . . .
C5 C 0.9047(9) 0.9322(4) -0.0387(3) 0.0580(18) Uani 1 1 d . . .
H5 H 0.9800 0.9183 -0.0591 0.070 Uiso 1 1 calc R . .
C6 C 0.8087(10) 0.9864(5) -0.0652(4) 0.068(2) Uani 1 1 d . . .
H6 H 0.8145 1.0073 -0.1048 0.082 Uiso 1 1 calc R . .
C7 C 0.7004(11) 1.0108(6) -0.0324(5) 0.081(3) Uani 1 1 d . . .
H7 H 0.6377 1.0496 -0.0495 0.097 Uiso 1 1 calc R . .
C8 C 0.6864(9) 0.9784(5) 0.0238(4) 0.068(2) Uani 1 1 d . . .
H8 H 0.6144 0.9954 0.0449 0.082 Uiso 1 1 calc R . .
C9 C 0.7663(7) 0.8828(4) 0.1081(3) 0.0487(15) Uani 1 1 d . . .
H9 H 0.6906 0.8968 0.1283 0.058 Uiso 1 1 calc R . .
C10 C 0.9907(7) 0.8402(4) 0.0485(3) 0.0435(13) Uani 1 1 d . . .
H10 H 1.0690 0.8277 0.0295 0.052 Uiso 1 1 calc R . .
C11 C 0.8607(7) 0.8276(4) 0.1355(3) 0.0403(13) Uani 1 1 d . . .
C12 C 0.9747(7) 0.8028(3) 0.1046(3) 0.0376(12) Uani 1 1 d . . .
C13 C 0.7792(8) 0.9193(4) 0.0507(3) 0.0519(16) Uani 1 1 d . . .
C14 C 0.8918(8) 0.8967(4) 0.0196(3) 0.0497(15) Uani 1 1 d . . .
C15 C 1.2096(9) 0.8369(5) 0.2741(4) 0.063(2) Uani 1 1 d . . .
C16 C 1.0074(9) 0.9461(4) 0.2287(4) 0.0601(19) Uani 1 1 d . . .
C17 C 1.1130(11) 0.9264(5) 0.3608(4) 0.072(2) Uani 1 1 d . . .
C18 C 0.8224(11) 0.8998(5) 0.3087(4) 0.071(2) Uani 1 1 d . . .
C25 C 1.1666(10) 0.6826(5) 0.3413(4) 0.068(2) Uani 1 1 d . . .
C26 C 0.9039(10) 0.6006(5) 0.3119(4) 0.065(2) Uani 1 1 d . . .
C27 C 0.9630(11) 0.6898(5) 0.4225(4) 0.066(2) Uani 1 1 d . . .
C28 C 0.7407(10) 0.7274(5) 0.3143(4) 0.0603(19) Uani 1 1 d . . .
C35 C 1.0756(8) 0.5526(4) 0.1872(4) 0.0520(16) Uani 1 1 d . . .
C36 C 0.7917(8) 0.6130(4) 0.1503(4) 0.0530(17) Uani 1 1 d . . .
C37 C 0.9107(10) 0.5218(4) 0.0704(4) 0.063(2) Uani 1 1 d . . .
C38 C 0.8532(8) 0.6679(4) 0.0363(4) 0.0564(18) Uani 1 1 d . . .
C45 C 1.3488(7) 0.6501(4) 0.1764(4) 0.0505(16) Uani 1 1 d . . .
C46 C 1.3914(9) 0.6321(5) 0.0527(4) 0.062(2) Uani 1 1 d . . .
C47 C 1.3650(8) 0.7770(4) 0.1060(3) 0.0535(17) Uani 1 1 d . . .
C48 C 1.1594(9) 0.7107(4) -0.0019(4) 0.0577(18) Uani 1 1 d . . .
H2 H 1.005(8) 0.790(4) 0.354(4) 0.06(2) Uiso 1 1 d . . .
H4 H 1.123(7) 0.609(4) 0.077(3) 0.042(17) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C17 1.932(8) . ?
Re1 C16 1.936(8) . ?
Re1 C18 1.994(9) . ?
Re1 C15 1.995(9) . ?
Re1 C2 2.463(6) . ?
Re1 C1 2.500(6) . ?
Re1 Re2 3.0566(4) . ?
Re1 H2 1.92(7) . ?
Re2 C26 1.935(9) . ?
Re2 C27 1.965(8) . ?
Re2 C28 1.987(9) . ?
Re2 C25 1.988(9) . ?
Re2 C2 2.202(6) . ?
Re2 H2 1.65(8) . ?
Re3 C37 1.927(8) . ?
Re3 C36 1.933(7) . ?
Re3 C35 2.001(8) . ?
Re3 C38 2.007(8) . ?
Re3 C4 2.462(6) . ?
Re3 C3 2.519(6) . ?
Re3 Re4 3.0484(3) . ?
Re3 H4 1.81(6) . ?
Re4 C47 1.927(8) . ?
Re4 C46 1.968(7) . ?
Re4 C48 1.993(8) . ?
Re4 C45 1.997(8) . ?
Re4 C4 2.217(5) . ?
Re4 H4 1.80(6) . ?
O15 C15 1.141(10) . ?
O16 C16 1.151(9) . ?
O17 C17 1.139(10) . ?
O18 C18 1.139(10) . ?
O25 C25 1.129(10) . ?
O26 C26 1.137(10) . ?
O27 C27 1.137(9) . ?
O28 C28 1.127(10) . ?
O35 C35 1.119(9) . ?
O36 C36 1.141(8) . ?
O37 C37 1.136(9) . ?
O38 C38 1.124(9) . ?
O45 C45 1.119(9) . ?
O46 C46 1.133(9) . ?
O47 C47 1.147(9) . ?
O48 C48 1.124(9) . ?
C1 C2 1.383(9) . ?
C1 C11 1.459(8) . ?
C1 H1 0.9300 . ?
C2 C3 1.474(8) . ?
C3 C4 1.403(8) . ?
C3 H3 0.9300 . ?
C4 C12 1.470(8) . ?
C5 C6 1.358(11) . ?
C5 C14 1.414(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.406(14) . ?
C6 H6 0.9300 . ?
C7 C8 1.352(12) . ?
C7 H7 0.9300 . ?
C8 C13 1.407(10) . ?
C8 H8 0.9300 . ?
C9 C11 1.367(9) . ?
C9 C13 1.406(10) . ?
C9 H9 0.9300 . ?
C10 C12 1.395(8) . ?
C10 C14 1.416(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.428(8) . ?
C13 C14 1.407(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
C17 Re1 C16 92.3(3) . . ?
C17 Re1 C18 88.9(4) . . ?
C16 Re1 C18 89.9(4) . . ?
C17 Re1 C15 87.7(4) . . ?
C16 Re1 C15 88.5(4) . . ?
C18 Re1 C15 176.1(4) . . ?
C17 Re1 C2 154.6(3) . . ?
C16 Re1 C2 109.4(3) . . ?
C18 Re1 C2 103.8(3) . . ?
C15 Re1 C2 80.1(3) . . ?
C17 Re1 C1 171.6(3) . . ?
C16 Re1 C1 84.8(3) . . ?
C18 Re1 C1 83.3(3) . . ?
C15 Re1 C1 100.1(3) . . ?
C2 Re1 C1 32.4(2) . . ?
C17 Re1 Re2 113.6(3) . . ?
C16 Re1 Re2 154.1(2) . . ?
C18 Re1 Re2 91.0(3) . . ?
C15 Re1 Re2 92.0(3) . . ?
C2 Re1 Re2 45.47(13) . . ?
C1 Re1 Re2 69.56(14) . . ?
C17 Re1 H2 86(2) . . ?
C16 Re1 H2 174(2) . . ?
C18 Re1 H2 85(2) . . ?
C15 Re1 H2 97(2) . . ?
C2 Re1 H2 74(2) . . ?
C1 Re1 H2 96(2) . . ?
Re2 Re1 H2 28(2) . . ?
C26 Re2 C27 91.4(3) . . ?
C26 Re2 C28 88.2(4) . . ?
C27 Re2 C28 91.8(3) . . ?
C26 Re2 C25 91.5(4) . . ?
C27 Re2 C25 90.7(4) . . ?
C28 Re2 C25 177.5(3) . . ?
C26 Re2 C2 100.3(3) . . ?
C27 Re2 C2 168.2(3) . . ?
C28 Re2 C2 87.5(3) . . ?
C25 Re2 C2 90.1(3) . . ?
C26 Re2 Re1 153.2(2) . . ?
C27 Re2 Re1 115.4(3) . . ?
C28 Re2 Re1 89.8(3) . . ?
C25 Re2 Re1 89.4(3) . . ?
C2 Re2 Re1 52.88(16) . . ?
C26 Re2 H2 173(3) . . ?
C27 Re2 H2 82(3) . . ?
C28 Re2 H2 95(3) . . ?
C25 Re2 H2 86(3) . . ?
C2 Re2 H2 86(3) . . ?
Re1 Re2 H2 34(3) . . ?
C37 Re3 C36 90.4(3) . . ?
C37 Re3 C35 86.3(3) . . ?
C36 Re3 C35 91.4(3) . . ?
C37 Re3 C38 87.6(3) . . ?
C36 Re3 C38 89.4(3) . . ?
C35 Re3 C38 173.9(3) . . ?
C37 Re3 C4 157.7(3) . . ?
C36 Re3 C4 107.8(3) . . ?
C35 Re3 C4 105.4(3) . . ?
C38 Re3 C4 80.1(3) . . ?
C37 Re3 C3 167.2(3) . . ?
C36 Re3 C3 87.0(3) . . ?
C35 Re3 C3 81.2(2) . . ?
C38 Re3 C3 104.9(3) . . ?
C4 Re3 C3 32.70(17) . . ?
C37 Re3 Re4 116.0(2) . . ?
C36 Re3 Re4 153.5(2) . . ?
C35 Re3 Re4 92.8(2) . . ?
C38 Re3 Re4 89.2(2) . . ?
C4 Re3 Re4 45.94(13) . . ?
C3 Re3 Re4 67.83(12) . . ?
C37 Re3 H4 84(2) . . ?
C36 Re3 H4 174(2) . . ?
C35 Re3 H4 89(2) . . ?
C38 Re3 H4 90(2) . . ?
C4 Re3 H4 78(2) . . ?
C3 Re3 H4 99(2) . . ?
Re4 Re3 H4 32(2) . . ?
C47 Re4 C46 93.9(3) . . ?
C47 Re4 C48 96.1(3) . . ?
C46 Re4 C48 83.5(4) . . ?
C47 Re4 C45 88.1(3) . . ?
C46 Re4 C45 87.6(3) . . ?
C48 Re4 C45 170.4(3) . . ?
C47 Re4 C4 90.6(3) . . ?
C46 Re4 C4 175.4(3) . . ?
C48 Re4 C4 97.0(3) . . ?
C45 Re4 C4 91.5(2) . . ?
C47 Re4 Re3 143.2(2) . . ?
C46 Re4 Re3 122.5(2) . . ?
C48 Re4 Re3 93.6(2) . . ?
C45 Re4 Re3 88.16(19) . . ?
C4 Re4 Re3 52.94(14) . . ?
C47 Re4 H4 175(2) . . ?
C46 Re4 H4 91(2) . . ?
C48 Re4 H4 83(2) . . ?
C45 Re4 H4 93(2) . . ?
C4 Re4 H4 85(2) . . ?
Re3 Re4 H4 32(2) . . ?
C2 C1 C11 123.0(5) . . ?
C2 C1 Re1 72.4(4) . . ?
C11 C1 Re1 113.3(4) . . ?
C2 C1 H1 118.5 . . ?
C11 C1 H1 118.5 . . ?
Re1 C1 H1 84.4 . . ?
C1 C2 C3 113.8(5) . . ?
C1 C2 Re2 125.0(4) . . ?
C3 C2 Re2 121.2(4) . . ?
C1 C2 Re1 75.3(4) . . ?
C3 C2 Re1 116.3(4) . . ?
Re2 C2 Re1 81.65(18) . . ?
C4 C3 C2 128.1(5) . . ?
C4 C3 Re3 71.4(3) . . ?
C2 C3 Re3 115.7(4) . . ?
C4 C3 H3 116.0 . . ?
C2 C3 H3 116.0 . . ?
Re3 C3 H3 82.5 . . ?
C3 C4 C12 114.2(5) . . ?
C3 C4 Re4 118.4(4) . . ?
C12 C4 Re4 127.3(4) . . ?
C3 C4 Re3 75.9(3) . . ?
C12 C4 Re3 114.5(4) . . ?
Re4 C4 Re3 81.12(18) . . ?
C6 C5 C14 120.8(8) . . ?
C6 C5 H5 119.6 . . ?
C14 C5 H5 119.6 . . ?
C5 C6 C7 119.6(8) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C8 C7 C6 120.8(8) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C8 C13 120.9(9) . . ?
C7 C8 H8 119.6 . . ?
C13 C8 H8 119.6 . . ?
C11 C9 C13 122.6(7) . . ?
C11 C9 H9 118.7 . . ?
C13 C9 H9 118.7 . . ?
C12 C10 C14 122.2(6) . . ?
C12 C10 H10 118.9 . . ?
C14 C10 H10 118.9 . . ?
C9 C11 C12 120.1(6) . . ?
C9 C11 C1 120.0(6) . . ?
C12 C11 C1 119.7(6) . . ?
C10 C12 C11 117.6(6) . . ?
C10 C12 C4 121.9(5) . . ?
C11 C12 C4 120.6(5) . . ?
C9 C13 C14 118.4(6) . . ?
C9 C13 C8 122.8(7) . . ?
C14 C13 C8 118.8(7) . . ?
C13 C14 C5 119.0(7) . . ?
C13 C14 C10 118.9(6) . . ?
C5 C14 C10 122.0(7) . . ?
O15 C15 Re1 174.3(8) . . ?
O16 C16 Re1 179.5(8) . . ?
O17 C17 Re1 177.9(10) . . ?
O18 C18 Re1 177.9(9) . . ?
O25 C25 Re2 177.7(9) . . ?
O26 C26 Re2 177.7(8) . . ?
O27 C27 Re2 177.7(8) . . ?
O28 C28 Re2 179.0(9) . . ?
O35 C35 Re3 176.6(7) . . ?
O36 C36 Re3 179.2(8) . . ?
O37 C37 Re3 178.3(9) . . ?
O38 C38 Re3 175.7(7) . . ?
O45 C45 Re4 175.8(7) . . ?
O46 C46 Re4 178.4(9) . . ?
O47 C47 Re4 176.3(7) . . ?
O48 C48 Re4 172.6(8) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.33
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.486
_refine_diff_density_min         -2.291
_refine_diff_density_rms         0.211
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane'
####################################################################### 
# 
# 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_p-1
_database_code_depnum_ccdc_archive 'CCDC 1581217'
_audit_update_record             
;
2017-10-20 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H6 O16 Re4'
_chemical_formula_weight         1271.07

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

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   8.8829(3)
_cell_length_b                   11.4074(4)
_cell_length_c                   15.4729(5)
_cell_angle_alpha                86.5200(10)
_cell_angle_beta                 80.1800(10)
_cell_angle_gamma                67.4180(10)
_cell_volume                     1426.44(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    301(2)
_cell_measurement_reflns_used    9824
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      28.31

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.959
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1132
_exptl_absorpt_coefficient_mu    16.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2545
_exptl_absorpt_correction_T_max  0.4604
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      301(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  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        <1
_diffrn_reflns_number            69210
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.34
_diffrn_reflns_theta_max         28.36
_reflns_number_total             7112
_reflns_number_gt                6110
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'

_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)+(0.0187P)²+1.4999P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7112
_refine_ls_number_parameters     387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0444
_refine_ls_wR_factor_gt          0.0422
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_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 0.711573(18) 0.424582(14) 0.336036(9) 0.03353(4) Uani 1 1 d . . .
Re2 Re 0.713675(19) 0.390888(15) 0.144686(10) 0.03859(5) Uani 1 1 d . . .
Re3 Re 0.86204(2) -0.106747(16) 0.332971(12) 0.04795(5) Uani 1 1 d . . .
Re4 Re 0.61851(2) -0.054343(16) 0.206931(11) 0.04278(5) Uani 1 1 d . . .
O11 O 1.0469(5) 0.4592(4) 0.3094(3) 0.0852(12) Uani 1 1 d . . .
O12 O 0.5524(5) 0.6951(4) 0.4145(3) 0.0801(12) Uani 1 1 d . . .
O13 O 0.7964(5) 0.2939(5) 0.5103(3) 0.0979(15) Uani 1 1 d . . .
O14 O 0.3636(4) 0.4111(4) 0.3877(2) 0.0709(10) Uani 1 1 d . . .
O21 O 1.0416(5) 0.4380(4) 0.0913(3) 0.0822(12) Uani 1 1 d . . .
O22 O 0.5654(5) 0.6196(4) 0.0303(3) 0.0818(12) Uani 1 1 d . . .
O23 O 0.8048(5) 0.2038(4) -0.0084(3) 0.0904(13) Uani 1 1 d . . .
O24 O 0.3664(5) 0.3724(4) 0.1794(2) 0.0763(11) Uani 1 1 d . . .
O31 O 0.5975(7) 0.0891(5) 0.4674(3) 0.1055(16) Uani 1 1 d . . .
O32 O 1.1250(6) -0.0354(5) 0.3968(3) 0.1044(16) Uani 1 1 d . . .
O33 O 0.8726(5) -0.3025(4) 0.4777(3) 0.0928(14) Uani 1 1 d . . .
O34 O 1.1382(6) -0.3287(4) 0.2202(4) 0.1051(16) Uani 1 1 d . . .
O41 O 0.3301(5) 0.1329(4) 0.3368(3) 0.0841(12) Uani 1 1 d . . .
O42 O 0.4646(8) 0.1156(4) 0.0583(3) 0.1168(19) Uani 1 1 d . . .
O43 O 0.4026(5) -0.2127(4) 0.2132(3) 0.0884(13) Uani 1 1 d . . .
O44 O 0.8681(6) -0.2490(5) 0.0677(4) 0.122(2) Uani 1 1 d . . .
C1 C 0.8192(4) 0.2442(3) 0.2595(2) 0.0349(8) Uani 1 1 d . . .
C2 C 0.7295(5) 0.1666(4) 0.2555(2) 0.0363(8) Uani 1 1 d . . .
H2 H 0.6195 0.1988 0.2821 0.044 Uiso 1 1 calc R . .
C3 C 0.7876(5) 0.0449(4) 0.2156(2) 0.0374(8) Uani 1 1 d . . .
C4 C 0.9548(5) 0.0024(4) 0.1754(3) 0.0489(10) Uani 1 1 d . . .
H4 H 1.0013 -0.0753 0.1462 0.059 Uiso 1 1 calc R . .
C5 C 1.0527(5) 0.0723(4) 0.1777(4) 0.0646(14) Uani 1 1 d . . .
H5 H 1.1631 0.0395 0.1518 0.077 Uiso 1 1 calc R . .
C6 C 0.9875(5) 0.1887(4) 0.2176(3) 0.0516(11) Uani 1 1 d . . .
H6 H 1.0554 0.2337 0.2175 0.062 Uiso 1 1 calc R . .
C11 C 0.9275(6) 0.4454(5) 0.3158(3) 0.0514(11) Uani 1 1 d . . .
C12 C 0.6112(6) 0.5951(4) 0.3875(3) 0.0487(10) Uani 1 1 d . . .
C13 C 0.7660(6) 0.3428(5) 0.4457(3) 0.0550(12) Uani 1 1 d . . .
C14 C 0.4894(5) 0.4142(4) 0.3664(3) 0.0417(9) Uani 1 1 d . . .
C21 C 0.9264(6) 0.4176(5) 0.1126(3) 0.0542(11) Uani 1 1 d . . .
C22 C 0.6212(6) 0.5332(5) 0.0723(3) 0.0528(11) Uani 1 1 d . . .
C23 C 0.7721(6) 0.2738(5) 0.0474(3) 0.0566(12) Uani 1 1 d . . .
C24 C 0.4914(6) 0.3777(4) 0.1697(3) 0.0496(10) Uani 1 1 d . . .
C31 C 0.6910(8) 0.0208(5) 0.4166(4) 0.0675(14) Uani 1 1 d . . .
C32 C 1.0294(7) -0.0639(5) 0.3745(4) 0.0696(15) Uani 1 1 d . . .
C33 C 0.8701(6) -0.2293(5) 0.4240(4) 0.0613(13) Uani 1 1 d . . .
C34 C 1.0365(7) -0.2457(5) 0.2585(4) 0.0663(14) Uani 1 1 d . . .
C41 C 0.4387(6) 0.0658(4) 0.2914(3) 0.0521(11) Uani 1 1 d . . .
C42 C 0.5225(7) 0.0517(5) 0.1129(4) 0.0669(14) Uani 1 1 d . . .
C43 C 0.4815(6) -0.1547(4) 0.2113(3) 0.0568(12) Uani 1 1 d . . .
C44 C 0.7815(7) -0.1775(6) 0.1200(4) 0.0720(15) Uani 1 1 d . . .
H1 H 0.640(6) 0.511(5) 0.237(3) 0.078(16) Uiso 1 1 d . . .
H3 H 0.701(6) -0.152(5) 0.290(3) 0.076(16) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C13 1.929(5) . ?
Re1 C12 1.956(5) . ?
Re1 C11 1.992(4) . ?
Re1 C14 1.997(4) . ?
Re1 C1 2.224(4) . ?
Re1 Re2 3.0046(2) . ?
Re1 H1 1.85(5) . ?
Re2 C22 1.906(5) . ?
Re2 C23 1.940(5) . ?
Re2 C21 2.004(5) . ?
Re2 C24 2.008(5) . ?
Re2 C1 2.417(4) . ?
Re2 H1 1.89(5) . ?
Re3 C33 1.914(5) . ?
Re3 C32 1.945(5) . ?
Re3 C31 1.990(6) . ?
Re3 C34 1.991(6) . ?
Re3 C3 2.424(4) . ?
Re3 Re4 3.0240(2) . ?
Re3 H3 1.92(5) . ?
Re4 C42 1.930(6) . ?
Re4 C43 1.957(5) . ?
Re4 C44 1.971(5) . ?
Re4 C41 1.991(5) . ?
Re4 C3 2.224(4) . ?
Re4 H3 1.72(5) . ?
O11 C11 1.118(5) . ?
O12 C12 1.129(5) . ?
O13 C13 1.138(5) . ?
O14 C14 1.124(5) . ?
O21 C21 1.126(6) . ?
O22 C22 1.139(5) . ?
O23 C23 1.136(5) . ?
O24 C24 1.119(5) . ?
O31 C31 1.126(7) . ?
O32 C32 1.128(6) . ?
O33 C33 1.139(6) . ?
O34 C34 1.138(6) . ?
O41 C41 1.130(5) . ?
O42 C42 1.138(6) . ?
O43 C43 1.131(5) . ?
O44 C44 1.139(6) . ?
C1 C2 1.410(5) . ?
C1 C6 1.431(5) . ?
C2 C3 1.421(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.413(5) . ?
C4 C5 1.393(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.367(6) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 Re1 C12 93.8(2) . . ?
C13 Re1 C11 88.49(19) . . ?
C12 Re1 C11 88.02(18) . . ?
C13 Re1 C14 88.99(17) . . ?
C12 Re1 C14 87.36(17) . . ?
C11 Re1 C14 174.58(17) . . ?
C13 Re1 C1 94.23(18) . . ?
C12 Re1 C1 171.94(16) . . ?
C11 Re1 C1 91.63(16) . . ?
C14 Re1 C1 93.34(15) . . ?
C13 Re1 Re2 146.66(16) . . ?
C12 Re1 Re2 119.48(13) . . ?
C11 Re1 Re2 93.95(13) . . ?
C14 Re1 Re2 90.79(11) . . ?
C1 Re1 Re2 52.51(9) . . ?
C13 Re1 H1 174.7(15) . . ?
C12 Re1 H1 82.7(16) . . ?
C11 Re1 H1 95.4(16) . . ?
C14 Re1 H1 86.9(16) . . ?
C1 Re1 H1 89.3(16) . . ?
Re2 Re1 H1 36.8(16) . . ?
C22 Re2 C23 91.7(2) . . ?
C22 Re2 C21 86.7(2) . . ?
C23 Re2 C21 91.5(2) . . ?
C22 Re2 C24 88.02(19) . . ?
C23 Re2 C24 88.56(19) . . ?
C21 Re2 C24 174.74(18) . . ?
C22 Re2 C1 167.90(17) . . ?
C23 Re2 C1 100.34(17) . . ?
C21 Re2 C1 91.74(16) . . ?
C24 Re2 C1 93.42(15) . . ?
C22 Re2 Re1 121.07(14) . . ?
C23 Re2 Re1 147.22(15) . . ?
C21 Re2 Re1 91.06(13) . . ?
C24 Re2 Re1 91.71(12) . . ?
C1 Re2 Re1 46.91(9) . . ?
C22 Re2 H1 85.2(15) . . ?
C23 Re2 H1 175.4(16) . . ?
C21 Re2 H1 91.6(15) . . ?
C24 Re2 H1 88.0(15) . . ?
C1 Re2 H1 82.9(15) . . ?
Re1 Re2 H1 36.0(15) . . ?
C33 Re3 C32 91.6(2) . . ?
C33 Re3 C31 87.0(2) . . ?
C32 Re3 C31 88.7(2) . . ?
C33 Re3 C34 87.7(2) . . ?
C32 Re3 C34 90.6(2) . . ?
C31 Re3 C34 174.7(2) . . ?
C33 Re3 C3 165.92(17) . . ?
C32 Re3 C3 101.75(17) . . ?
C31 Re3 C3 88.91(17) . . ?
C34 Re3 C3 96.42(18) . . ?
C33 Re3 Re4 119.92(14) . . ?
C32 Re3 Re4 148.34(14) . . ?
C31 Re3 Re4 90.23(15) . . ?
C34 Re3 Re4 93.10(17) . . ?
C3 Re3 Re4 46.60(9) . . ?
C33 Re3 H3 88.5(15) . . ?
C32 Re3 H3 178.8(15) . . ?
C31 Re3 H3 92.5(15) . . ?
C34 Re3 H3 88.1(15) . . ?
C3 Re3 H3 78.3(15) . . ?
Re4 Re3 H3 31.7(15) . . ?
C42 Re4 C43 93.6(2) . . ?
C42 Re4 C44 89.7(3) . . ?
C43 Re4 C44 87.6(2) . . ?
C42 Re4 C41 88.4(2) . . ?
C43 Re4 C41 87.80(19) . . ?
C44 Re4 C41 174.93(19) . . ?
C42 Re4 C3 93.51(18) . . ?
C43 Re4 C3 172.90(18) . . ?
C44 Re4 C3 92.52(18) . . ?
C41 Re4 C3 92.30(15) . . ?
C42 Re4 Re3 145.84(16) . . ?
C43 Re4 Re3 120.55(15) . . ?
C44 Re4 Re3 92.73(17) . . ?
C41 Re4 Re3 91.46(13) . . ?
C3 Re4 Re3 52.35(10) . . ?
C42 Re4 H3 178.2(17) . . ?
C43 Re4 H3 84.6(17) . . ?
C44 Re4 H3 90.0(16) . . ?
C41 Re4 H3 91.7(16) . . ?
C3 Re4 H3 88.3(17) . . ?
Re3 Re4 H3 36.0(17) . . ?
C2 C1 C6 113.2(3) . . ?
C2 C1 Re1 122.0(3) . . ?
C6 C1 Re1 124.6(3) . . ?
C2 C1 Re2 98.0(2) . . ?
C6 C1 Re2 97.8(3) . . ?
Re1 C1 Re2 80.58(11) . . ?
C1 C2 C3 127.6(3) . . ?
C1 C2 H2 116.2 . . ?
C3 C2 H2 116.2 . . ?
C4 C3 C2 113.3(3) . . ?
C4 C3 Re4 124.8(3) . . ?
C2 C3 Re4 121.6(3) . . ?
C4 C3 Re3 90.3(3) . . ?
C2 C3 Re3 105.6(2) . . ?
Re4 C3 Re3 81.05(12) . . ?
C5 C4 C3 122.6(4) . . ?
C5 C4 H4 118.7 . . ?
C3 C4 H4 118.7 . . ?
C6 C5 C4 120.4(4) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C5 C6 C1 122.8(4) . . ?
C5 C6 H6 118.6 . . ?
C1 C6 H6 118.6 . . ?
O11 C11 Re1 175.8(4) . . ?
O12 C12 Re1 177.7(4) . . ?
O13 C13 Re1 179.1(4) . . ?
O14 C14 Re1 176.3(4) . . ?
O21 C21 Re2 176.0(4) . . ?
O22 C22 Re2 178.8(4) . . ?
O23 C23 Re2 178.6(5) . . ?
O24 C24 Re2 176.4(4) . . ?
O31 C31 Re3 176.5(5) . . ?
O32 C32 Re3 177.6(5) . . ?
O33 C33 Re3 178.8(4) . . ?
O34 C34 Re3 176.2(5) . . ?
O41 C41 Re4 175.9(4) . . ?
O42 C42 Re4 179.0(6) . . ?
O43 C43 Re4 179.6(5) . . ?
O44 C44 Re4 175.9(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.36
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.580
_refine_diff_density_rms         0.152
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: hexane'
