# 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_ReCl4CN2_50K
_database_code_depnum_ccdc_archive 'CCDC 1488917'
_audit_update_record             
;
2016-06-29 deposited with the CCDC.
2016-10-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H90 Cl4 N6 O2 Re'
_chemical_formula_weight         1039.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.4031(6)
_cell_length_b                   11.9265(7)
_cell_length_c                   11.9819(7)
_cell_angle_alpha                64.8219(16)
_cell_angle_beta                 75.0617(17)
_cell_angle_gamma                82.2082(17)
_cell_volume                     1299.34(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    50(2)
_cell_measurement_reflns_used    8821
_cell_measurement_theta_max      28.012
_cell_measurement_theta_min      2.466

_exptl_crystal_description       chip
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_F_000             543
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    2.581
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4567
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      50(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'I\mS microfocus source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       ω/2θ-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23134
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.466
_diffrn_reflns_theta_max         28.850
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6646
_reflns_number_gt                5558
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1105P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6646
_refine_ls_number_parameters     257
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0624
_refine_ls_wR_factor_ref         0.1708
_refine_ls_wR_factor_gt          0.1584
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re -0.5000 0.5000 0.5000 0.01422(14) Uani 1 2 d S . P . .
Cl1 Cl -0.43971(16) 0.70704(14) 0.40870(15) 0.0191(3) Uani 1 1 d . . . . .
Cl2 Cl -0.45060(15) 0.47603(14) 0.68725(14) 0.0175(3) Uani 1 1 d . . . . .
N1 N -0.1898(5) 0.4301(5) 0.3996(5) 0.0162(11) Uani 1 1 d . . . . .
C1 C -0.2978(5) 0.4524(5) 0.4337(5) 0.0078(11) Uani 1 1 d . . . . .
O1 O -0.0907(4) 1.0887(4) 0.1668(4) 0.0145(9) Uani 1 1 d . . . . .
N3 N -0.2779(6) 1.1253(5) 0.2943(5) 0.0197(12) Uani 1 1 d . . . . .
C18 C -0.3587(7) 1.0707(7) 0.2475(7) 0.0218(14) Uani 1 1 d . . . . .
H18A H -0.4347 1.1266 0.2239 0.033 Uiso 1 1 calc R U . . .
H18B H -0.3911 0.9907 0.3139 0.033 Uiso 1 1 calc R U . . .
H18C H -0.3045 1.0585 0.1733 0.033 Uiso 1 1 calc R U . . .
C19 C -0.3487(6) 1.1717(6) 0.3869(6) 0.0186(13) Uani 1 1 d . . . . .
H19A H -0.3905 1.1028 0.4640 0.028 Uiso 1 1 calc R U . . .
H19B H -0.4174 1.2324 0.3530 0.028 Uiso 1 1 calc R U . . .
H19C H -0.2864 1.2113 0.4069 0.028 Uiso 1 1 calc R U . . .
C20 C -0.1454(6) 1.1299(5) 0.2483(6) 0.0149(12) Uani 1 1 d . . . . .
C21 C -0.0631(7) 1.1861(7) 0.2979(7) 0.0214(14) Uani 1 1 d . . . . .
H21A H 0.0293 1.1921 0.2495 0.032 Uiso 1 1 calc R U . . .
H21B H -0.0659 1.1335 0.3873 0.032 Uiso 1 1 calc R U . . .
H21C H -0.0993 1.2690 0.2888 0.032 Uiso 1 1 calc R U . . .
N2 N 0.0402(5) 0.7485(4) 0.2438(4) 0.0093(9) Uani 1 1 d . . . . .
C2 C 0.1305(5) 0.8499(5) 0.2213(5) 0.0083(11) Uani 1 1 d . . . . .
H2A H 0.1873 0.8752 0.1349 0.010 Uiso 1 1 calc R U . . .
H2B H 0.0741 0.9228 0.2244 0.010 Uiso 1 1 calc R U . . .
C3 C 0.2195(6) 0.8161(5) 0.3130(5) 0.0103(11) Uani 1 1 d . . . . .
H3A H 0.2735 0.7405 0.3152 0.012 Uiso 1 1 calc R U . . .
H3B H 0.1647 0.7990 0.3992 0.012 Uiso 1 1 calc R U . . .
C4 C 0.3103(6) 0.9234(6) 0.2711(5) 0.0134(12) Uani 1 1 d . . . . .
H4A H 0.3536 0.9105 0.3403 0.016 Uiso 1 1 calc R U . . .
H4B H 0.2565 1.0016 0.2536 0.016 Uiso 1 1 calc R U . . .
C5 C 0.4169(6) 0.9346(6) 0.1529(6) 0.0178(13) Uani 1 1 d . . . . .
H5A H 0.3748 0.9569 0.0816 0.027 Uiso 1 1 calc R U . . .
H5B H 0.4659 0.8552 0.1678 0.027 Uiso 1 1 calc R U . . .
H5C H 0.4787 0.9990 0.1333 0.027 Uiso 1 1 calc R U . . .
C6 C 0.1192(6) 0.6402(5) 0.2242(6) 0.0117(11) Uani 1 1 d . . . . .
H6A H 0.0562 0.5782 0.2374 0.014 Uiso 1 1 calc R U . . .
H6B H 0.1723 0.6011 0.2897 0.014 Uiso 1 1 calc R U . . .
C7 C 0.2132(6) 0.6716(5) 0.0945(5) 0.0125(12) Uani 1 1 d . . . . .
H7A H 0.1655 0.7256 0.0277 0.015 Uiso 1 1 calc R U . . .
H7B H 0.2892 0.7176 0.0877 0.015 Uiso 1 1 calc R U . . .
C8 C 0.2646(6) 0.5550(6) 0.0743(6) 0.0160(13) Uani 1 1 d . . . . .
H8A H 0.1885 0.5091 0.0809 0.019 Uiso 1 1 calc R U . . .
H8B H 0.3120 0.5009 0.1412 0.019 Uiso 1 1 calc R U . . .
C9 C 0.3599(7) 0.5860(6) -0.0567(6) 0.0198(14) Uani 1 1 d . . . . .
H9A H 0.3129 0.6391 -0.1231 0.030 Uiso 1 1 calc R U . . .
H9B H 0.3908 0.5091 -0.0675 0.030 Uiso 1 1 calc R U . . .
H9C H 0.4365 0.6295 -0.0625 0.030 Uiso 1 1 calc R U . . .
C10 C -0.0494(6) 0.8096(5) 0.1499(5) 0.0102(11) Uani 1 1 d . . . . .
H10A H -0.1086 0.8713 0.1750 0.012 Uiso 1 1 calc R U . . .
H10B H 0.0076 0.8557 0.0657 0.012 Uiso 1 1 calc R U . . .
C11 C -0.1358(6) 0.7256(5) 0.1360(5) 0.0108(11) Uani 1 1 d . . . . .
H11A H -0.1915 0.6752 0.2194 0.013 Uiso 1 1 calc R U . . .
H11B H -0.0794 0.6688 0.1014 0.013 Uiso 1 1 calc R U . . .
C12 C -0.2241(6) 0.8085(6) 0.0455(6) 0.0134(12) Uani 1 1 d . . . . .
H12A H -0.2845 0.8604 0.0841 0.016 Uiso 1 1 calc R U . . .
H12B H -0.1674 0.8644 -0.0343 0.016 Uiso 1 1 calc R U . . .
C13 C -0.3060(7) 0.7321(6) 0.0167(6) 0.0197(14) Uani 1 1 d . . . . .
H13A H -0.3614 0.7876 -0.0410 0.030 Uiso 1 1 calc R U . . .
H13B H -0.3631 0.6775 0.0955 0.030 Uiso 1 1 calc R U . . .
H13C H -0.2463 0.6819 -0.0231 0.030 Uiso 1 1 calc R U . . .
C14 C -0.0398(6) 0.6959(5) 0.3790(5) 0.0107(11) Uani 1 1 d . . . . .
H14A H 0.0223 0.6505 0.4350 0.013 Uiso 1 1 calc R U . . .
H14B H -0.1012 0.6348 0.3873 0.013 Uiso 1 1 calc R U . . .
C15 C -0.1210(6) 0.7890(5) 0.4264(5) 0.0105(11) Uani 1 1 d . . . . .
H15A H -0.1917 0.8282 0.3789 0.013 Uiso 1 1 calc R U . . .
H15B H -0.0629 0.8549 0.4132 0.013 Uiso 1 1 calc R U . . .
C16 C -0.1832(6) 0.7222(6) 0.5670(5) 0.0141(12) Uani 1 1 d . U . . .
H16A H -0.1117 0.6853 0.6140 0.017 Uiso 1 1 calc R U . . .
H16B H -0.2377 0.6540 0.5797 0.017 Uiso 1 1 calc R U . . .
C17 C -0.2712(7) 0.8110(6) 0.6197(6) 0.0167(13) Uani 1 1 d . . . . .
H17A H -0.3502 0.8366 0.5836 0.025 Uiso 1 1 calc R U . . .
H17B H -0.2207 0.8841 0.5972 0.025 Uiso 1 1 calc R U . . .
H17C H -0.2986 0.7686 0.7120 0.025 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C1 2.140(5) . ?
Re1 C1 2.140(5) 2_466 ?
Re1 Cl2 2.3212(15) . ?
Re1 Cl2 2.3213(15) 2_466 ?
Re1 Cl1 2.3357(16) . ?
Re1 Cl1 2.3357(16) 2_466 ?
N1 C1 1.128(8) . ?
O1 C20 1.251(7) . ?
N3 C20 1.345(9) . ?
N3 C19 1.439(8) . ?
N3 C18 1.466(9) . ?
C20 C21 1.513(9) . ?
N2 C6 1.507(7) . ?
N2 C14 1.514(7) . ?
N2 C2 1.523(7) . ?
N2 C10 1.524(7) . ?
C2 C3 1.507(8) . ?
C3 C4 1.522(8) . ?
C4 C5 1.524(8) . ?
C6 C7 1.527(8) . ?
C7 C8 1.516(8) . ?
C8 C9 1.545(8) . ?
C10 C11 1.517(8) . ?
C11 C12 1.533(8) . ?
C12 C13 1.519(8) . ?
C14 C15 1.518(8) . ?
C15 C16 1.525(8) . ?
C16 C17 1.538(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 C1 180.0 . 2_466 ?
C1 Re1 Cl2 89.92(15) . . ?
C1 Re1 Cl2 90.08(15) 2_466 . ?
C1 Re1 Cl2 90.08(15) . 2_466 ?
C1 Re1 Cl2 89.92(15) 2_466 2_466 ?
Cl2 Re1 Cl2 180.00(7) . 2_466 ?
C1 Re1 Cl1 88.28(15) . . ?
C1 Re1 Cl1 91.72(15) 2_466 . ?
Cl2 Re1 Cl1 89.82(5) . . ?
Cl2 Re1 Cl1 90.19(5) 2_466 . ?
C1 Re1 Cl1 91.72(15) . 2_466 ?
C1 Re1 Cl1 88.28(15) 2_466 2_466 ?
Cl2 Re1 Cl1 90.19(5) . 2_466 ?
Cl2 Re1 Cl1 89.81(5) 2_466 2_466 ?
Cl1 Re1 Cl1 180.0 . 2_466 ?
N1 C1 Re1 177.8(5) . . ?
C20 N3 C19 124.8(6) . . ?
C20 N3 C18 118.9(5) . . ?
C19 N3 C18 116.3(5) . . ?
O1 C20 N3 121.2(6) . . ?
O1 C20 C21 120.4(6) . . ?
N3 C20 C21 118.4(6) . . ?
C6 N2 C14 105.6(4) . . ?
C6 N2 C2 111.6(4) . . ?
C14 N2 C2 111.3(4) . . ?
C6 N2 C10 111.4(4) . . ?
C14 N2 C10 111.7(4) . . ?
C2 N2 C10 105.5(4) . . ?
C3 C2 N2 115.8(5) . . ?
C2 C3 C4 109.0(5) . . ?
C3 C4 C5 111.6(5) . . ?
N2 C6 C7 115.3(5) . . ?
C8 C7 C6 110.9(5) . . ?
C7 C8 C9 111.2(5) . . ?
C11 C10 N2 117.3(5) . . ?
C10 C11 C12 107.5(5) . . ?
C13 C12 C11 111.4(5) . . ?
N2 C14 C15 116.2(5) . . ?
C14 C15 C16 109.0(5) . . ?
C15 C16 C17 111.5(5) . . ?

_refine_diff_density_max         4.422
_refine_diff_density_min         -1.982
_refine_diff_density_rms         0.248



