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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_3c

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 iodo(pentacarbonyl)rhenium(I)
;
_chemical_name_common            3c
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C5 I O5 Re'
_chemical_formula_weight         453.16

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4740 1.8120 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0180 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_H-M_alt        'C m c m'
_space_group_name_Hall           '-C 2c 2'

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

_cell_length_a                   7.6549(7)
_cell_length_b                   11.1028(11)
_cell_length_c                   10.9893(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     933.99(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.223
_exptl_crystal_F_000             792
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    16.296
_exptl_transmission_factor_min   0.3741
_exptl_transmission_factor_max   0.7457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
 multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5114
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.232
_diffrn_reflns_theta_max         28.126
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             628
_reflns_number_gt                621
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0111P)²+1.6455P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0089(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         628
_refine_ls_number_parameters     36
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0165
_refine_ls_wR_factor_ref         0.0390
_refine_ls_wR_factor_gt          0.0389
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_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 0.0000 0.36007(2) 0.2500 0.03742(14) Uani 1 4 d S T P . .
I1 I 0.0000 0.61305(4) 0.2500 0.05038(15) Uani 1 4 d S T P . .
O1 O 0.0000 0.0834(5) 0.2500 0.0712(17) Uani 1 4 d S T P . .
O2 O 0.2959(4) 0.3741(2) 0.4470(3) 0.0678(8) Uani 1 1 d . . . . .
C1 C 0.0000 0.1860(7) 0.2500 0.0481(15) Uani 1 4 d S T P . .
C2 C 0.1890(5) 0.3675(3) 0.3771(4) 0.0473(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C1 1.933(7) . ?
Re1 C2 2.013(4) 4 ?
Re1 C2 2.013(4) 11 ?
Re1 C2 2.013(4) 10_556 ?
Re1 C2 2.013(4) . ?
Re1 I1 2.8088(5) . ?
O1 C1 1.139(10) . ?
O2 C2 1.125(5) . ?

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 92.34(8) . 4 ?
C1 Re1 C2 92.34(8) . 11 ?
C2 Re1 C2 87.9(2) 4 11 ?
C1 Re1 C2 92.34(8) . 10_556 ?
C2 Re1 C2 91.9(2) 4 10_556 ?
C2 Re1 C2 175.32(17) 11 10_556 ?
C1 Re1 C2 92.34(8) . . ?
C2 Re1 C2 175.32(17) 4 . ?
C2 Re1 C2 91.9(2) 11 . ?
C2 Re1 C2 87.9(2) 10_556 . ?
C1 Re1 I1 180.0 . . ?
C2 Re1 I1 87.66(8) 4 . ?
C2 Re1 I1 87.66(8) 11 . ?
C2 Re1 I1 87.66(8) 10_556 . ?
C2 Re1 I1 87.66(8) . . ?
O1 C1 Re1 180.0 . . ?
O2 C2 Re1 178.4(3) . . ?

_refine_diff_density_max         1.401
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.133

_shelxl_version_number           2014-3

_database_code_depnum_ccdc_archive 'CCDC 997709'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4b

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
bromo(pentacarbonyl)manganese(I)
;
_chemical_name_common            4b
_chemical_melting_point          ?
_chemical_formula_moiety         'C5 Br1 Mn1 O5'
_chemical_formula_sum            'C5 Br Mn O5'
_chemical_formula_weight         274.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3370 0.7280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2900 2.4600 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

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

_cell_length_a                   11.7723(15)
_cell_length_b                   11.5071(15)
_cell_length_c                   6.1089(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     827.54(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.206
_exptl_crystal_F_000             520
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    6.400
_exptl_transmission_factor_min   0.4520
_exptl_transmission_factor_max   0.7456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8552
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         3.461
_diffrn_reflns_theta_max         27.682
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1001
_reflns_number_gt                860
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0433P)²+0.3796P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1001
_refine_ls_number_parameters     61
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0749
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_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
Mn1 Mn 0.12192(4) 0.2500 0.05306(9) 0.03063(18) Uani 1 2 d S T P . .
Br1 Br 0.24874(3) 0.2500 0.38213(7) 0.04418(17) Uani 1 2 d S T P . .
C1 C 0.2167(2) 0.3651(2) -0.0655(5) 0.0389(6) Uani 1 1 d . . . . .
C2 C 0.0363(2) 0.3672(2) 0.1902(5) 0.0386(6) Uani 1 1 d . . . . .
O3 O -0.0288(3) 0.2500 -0.3323(6) 0.0584(8) Uani 1 2 d S T P . .
O1 O 0.2735(2) 0.4351(2) -0.1341(4) 0.0605(7) Uani 1 1 d . . . . .
O2 O -0.01253(18) 0.4398(2) 0.2671(4) 0.0623(7) Uani 1 1 d . . . . .
C3 C 0.0298(4) 0.2500 -0.1844(7) 0.0390(8) Uani 1 2 d S T P . .


_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
Mn1 C3 1.811(4) . ?
Mn1 C1 1.878(3) 7_565 ?
Mn1 C1 1.878(3) . ?
Mn1 C2 1.880(3) 7_565 ?
Mn1 C2 1.880(3) . ?
Mn1 Br1 2.5041(7) . ?
C1 O1 1.127(4) . ?
C2 O2 1.118(3) . ?
O3 C3 1.137(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
C3 Mn1 C1 92.70(13) . 7_565 ?
C3 Mn1 C1 92.70(13) . . ?
C1 Mn1 C1 89.75(18) 7_565 . ?
C3 Mn1 C2 92.05(12) . 7_565 ?
C1 Mn1 C2 89.11(12) 7_565 7_565 ?
C1 Mn1 C2 175.16(13) . 7_565 ?
C3 Mn1 C2 92.05(12) . . ?
C1 Mn1 C2 175.16(13) 7_565 . ?
C1 Mn1 C2 89.11(12) . . ?
C2 Mn1 C2 91.64(18) 7_565 . ?
C3 Mn1 Br1 179.82(13) . . ?
C1 Mn1 Br1 87.43(9) 7_565 . ?
C1 Mn1 Br1 87.43(9) . . ?
C2 Mn1 Br1 87.82(9) 7_565 . ?
C2 Mn1 Br1 87.82(9) . . ?
O1 C1 Mn1 179.0(3) . . ?
O2 C2 Mn1 177.4(3) . . ?
O3 C3 Mn1 179.4(4) . . ?

_refine_diff_density_max         1.118
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.083

_shelxl_version_number           2014-3

_database_code_depnum_ccdc_archive 'CCDC 997710'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_7

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 bis(1,10-phenanthroline)di(carbonyl)rhenium(I) perrhenate(VII)
 acetonitrile solvate 1/1
;
_chemical_name_common            7
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H19 N5 O6 Re2'
_chemical_formula_weight         893.88

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   12.6739(6)
_cell_length_b                   11.2202(6)
_cell_length_c                   19.9289(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.7190(10)
_cell_angle_gamma                90
_cell_volume                     2741.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.166
_exptl_crystal_F_000             1680
_exptl_transmission_factor_min   0.4113
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    8.877
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   
;
 multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30845
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.727
_diffrn_reflns_theta_max         28.178
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6452
_reflns_number_gt                5139
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014 (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)+(0.0240P)²+5.9870P] 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         6452
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0648
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.70467(2) 0.66659(2) 0.01269(2) 0.02977(6) Uani 1 1 d . . . . .
Re2 Re 0.81937(2) 0.97274(3) -0.19315(2) 0.05957(9) Uani 1 1 d . . . . .
O1 O 0.6668(4) 0.4039(3) 0.0364(2) 0.0571(11) Uani 1 1 d . . . . .
O2 O 0.5419(4) 0.6444(4) -0.1288(2) 0.0585(11) Uani 1 1 d . . . . .
O3 O 0.7275(5) 0.8900(7) -0.1634(3) 0.115(2) Uani 1 1 d . . . . .
O4 O 0.9247(4) 1.0119(5) -0.1255(3) 0.0893(17) Uani 1 1 d . . . . .
O5 O 0.8620(6) 0.8981(10) -0.2512(5) 0.194(5) Uani 1 1 d . . . . .
O6 O 0.7506(7) 1.0968(7) -0.2283(4) 0.146(3) Uani 1 1 d . . . . .
N1 N 0.5893(3) 0.7229(4) 0.0669(2) 0.0357(10) Uani 1 1 d . . . . .
N2 N 0.7205(3) 0.8607(4) 0.0149(2) 0.0354(10) Uani 1 1 d . . . . .
N3 N 0.8395(4) 0.6823(3) 0.1049(2) 0.0350(9) Uani 1 1 d . . . . .
N4 N 0.8442(3) 0.6491(3) -0.0269(2) 0.0331(9) Uani 1 1 d . . . . .
N5 N 0.6756(10) 0.7566(12) 0.2943(6) 0.140(4) Uani 1 1 d . . . . .
C1 C 0.7897(5) 0.9267(5) -0.0085(3) 0.0443(13) Uani 1 1 d . . . . .
H1 H 0.8364 0.8892 -0.0311 0.053 Uiso 1 1 calc R U . . .
C2 C 0.7959(6) 1.0509(5) -0.0008(3) 0.0570(16) Uani 1 1 d . . . . .
H2 H 0.8465 1.0945 -0.0173 0.068 Uiso 1 1 calc R U . . .
C3 C 0.7267(6) 1.1068(5) 0.0313(3) 0.0580(17) Uani 1 1 d . . . . .
H3 H 0.7286 1.1893 0.0356 0.070 Uiso 1 1 calc R U . . .
C4 C 0.6534(5) 1.0409(5) 0.0574(3) 0.0440(13) Uani 1 1 d . . . . .
C5 C 0.6532(4) 0.9161(5) 0.0493(2) 0.0352(11) Uani 1 1 d . . . . .
C6 C 0.5786(5) 1.0914(6) 0.0929(3) 0.0595(18) Uani 1 1 d . . . . .
H6 H 0.5763 1.1736 0.0983 0.071 Uiso 1 1 calc R U . . .
C7 C 0.5117(5) 1.0215(6) 0.1183(3) 0.0607(19) Uani 1 1 d . . . . .
H7 H 0.4637 1.0571 0.1406 0.073 Uiso 1 1 calc R U . . .
C8 C 0.5116(5) 0.8940(6) 0.1123(3) 0.0487(15) Uani 1 1 d . . . . .
C9 C 0.5832(4) 0.8435(5) 0.0765(2) 0.0363(11) Uani 1 1 d . . . . .
C10 C 0.4532(5) 0.6983(7) 0.1302(3) 0.0609(18) Uani 1 1 d . . . . .
H10 H 0.4107 0.6467 0.1488 0.073 Uiso 1 1 calc R U . . .
C11 C 0.5249(5) 0.6530(6) 0.0935(3) 0.0480(14) Uani 1 1 d . . . . .
H11 H 0.5277 0.5710 0.0873 0.058 Uiso 1 1 calc R U . . .
C12 C 0.4459(5) 0.8177(7) 0.1388(3) 0.0618(19) Uani 1 1 d . . . . .
H12 H 0.3972 0.8482 0.1623 0.074 Uiso 1 1 calc R U . . .
C13 C 0.6832(4) 0.5031(5) 0.0253(3) 0.0394(12) Uani 1 1 d . . . . .
C14 C 0.6024(4) 0.6551(4) -0.0742(3) 0.0363(11) Uani 1 1 d . . . . .
C15 C 0.9400(4) 0.6774(4) 0.0919(2) 0.0321(10) Uani 1 1 d . . . . .
C16 C 1.0374(4) 0.6916(5) 0.1437(3) 0.0406(12) Uani 1 1 d . . . . .
C17 C 1.1380(5) 0.6842(5) 0.1244(3) 0.0495(15) Uani 1 1 d . . . . .
H17 H 1.2032 0.6925 0.1584 0.059 Uiso 1 1 calc R U . . .
C18 C 1.1407(5) 0.6655(5) 0.0583(3) 0.0474(14) Uani 1 1 d . . . . .
H18 H 1.2078 0.6594 0.0478 0.057 Uiso 1 1 calc R U . . .
C19 C 1.0433(4) 0.6547(4) 0.0037(3) 0.0388(12) Uani 1 1 d . . . . .
C20 C 0.9431(4) 0.6602(4) 0.0209(3) 0.0338(11) Uani 1 1 d . . . . .
C21 C 0.8349(5) 0.7012(5) 0.1697(3) 0.0488(14) Uani 1 1 d . . . . .
H21 H 0.7668 0.7051 0.1792 0.059 Uiso 1 1 calc R U . . .
C22 C 0.9279(5) 0.7158(6) 0.2244(3) 0.0560(16) Uani 1 1 d . . . . .
H22 H 0.9214 0.7282 0.2693 0.067 Uiso 1 1 calc R U . . .
C23 C 1.0287(5) 0.7115(6) 0.2113(3) 0.0505(15) Uani 1 1 d . . . . .
H23 H 1.0912 0.7217 0.2472 0.061 Uiso 1 1 calc R U . . .
C24 C 1.0420(5) 0.6406(5) -0.0659(3) 0.0461(14) Uani 1 1 d . . . . .
H24 H 1.1070 0.6370 -0.0794 0.055 Uiso 1 1 calc R U . . .
C25 C 0.8471(5) 0.6357(5) -0.0935(3) 0.0418(13) Uani 1 1 d . . . . .
H25 H 0.7814 0.6285 -0.1271 0.050 Uiso 1 1 calc R U . . .
C26 C 0.9437(5) 0.6320(5) -0.1144(3) 0.0487(14) Uani 1 1 d . . . . .
H26 H 0.9417 0.6237 -0.1612 0.058 Uiso 1 1 calc R U . . .
C27 C 0.6566(10) 0.6581(15) 0.2895(6) 0.111(4) Uani 1 1 d . . . . .
C28 C 0.6330(10) 0.5328(13) 0.2823(7) 0.144(5) Uani 1 1 d . . . . .
H28A H 0.6294 0.5006 0.3264 0.215 Uiso 1 1 calc R U . . .
H28B H 0.6894 0.4930 0.2667 0.215 Uiso 1 1 calc R U . . .
H28C H 0.5642 0.5210 0.2491 0.215 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 C13 1.881(6) . ?
Re1 C14 1.886(5) . ?
Re1 N4 2.121(4) . ?
Re1 N1 2.122(4) . ?
Re1 N3 2.175(4) . ?
Re1 N2 2.187(4) . ?
Re2 O5 1.627(6) . ?
Re2 O4 1.696(5) . ?
Re2 O6 1.697(7) . ?
Re2 O3 1.709(6) . ?
O1 C13 1.164(6) . ?
O2 C14 1.166(6) . ?
N1 C11 1.335(7) . ?
N1 C9 1.372(6) . ?
N2 C1 1.321(7) . ?
N2 C5 1.370(6) . ?
N3 C21 1.324(7) . ?
N3 C15 1.365(6) . ?
N4 C25 1.346(6) . ?
N4 C20 1.373(6) . ?
N5 C27 1.130(15) . ?
C1 C2 1.402(8) . ?
C2 C3 1.361(9) . ?
C3 C4 1.389(9) . ?
C4 C5 1.410(7) . ?
C4 C6 1.435(8) . ?
C5 C9 1.410(7) . ?
C6 C7 1.346(10) . ?
C7 C8 1.436(9) . ?
C8 C12 1.389(9) . ?
C8 C9 1.408(7) . ?
C10 C12 1.356(9) . ?
C10 C11 1.400(9) . ?
C15 C16 1.402(7) . ?
C15 C20 1.437(7) . ?
C16 C23 1.397(8) . ?
C16 C17 1.424(8) . ?
C17 C18 1.343(8) . ?
C18 C19 1.428(8) . ?
C19 C24 1.393(8) . ?
C19 C20 1.399(7) . ?
C21 C22 1.397(8) . ?
C22 C23 1.368(8) . ?
C24 C26 1.372(8) . ?
C25 C26 1.391(8) . ?
C27 C28 1.437(16) . ?

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 C14 88.1(2) . . ?
C13 Re1 N4 97.02(19) . . ?
C14 Re1 N4 95.50(19) . . ?
C13 Re1 N1 94.6(2) . . ?
C14 Re1 N1 94.94(19) . . ?
N4 Re1 N1 164.59(15) . . ?
C13 Re1 N3 94.34(19) . . ?
C14 Re1 N3 172.11(19) . . ?
N4 Re1 N3 76.77(16) . . ?
N1 Re1 N3 92.35(15) . . ?
C13 Re1 N2 169.89(19) . . ?
C14 Re1 N2 97.17(18) . . ?
N4 Re1 N2 91.09(15) . . ?
N1 Re1 N2 76.36(16) . . ?
N3 Re1 N2 81.60(15) . . ?
O5 Re2 O4 111.2(3) . . ?
O5 Re2 O6 111.0(5) . . ?
O4 Re2 O6 109.5(3) . . ?
O5 Re2 O3 110.2(4) . . ?
O4 Re2 O3 109.5(3) . . ?
O6 Re2 O3 105.4(4) . . ?
C11 N1 C9 117.5(5) . . ?
C11 N1 Re1 126.6(4) . . ?
C9 N1 Re1 115.8(3) . . ?
C1 N2 C5 118.4(5) . . ?
C1 N2 Re1 128.1(4) . . ?
C5 N2 Re1 113.4(3) . . ?
C21 N3 C15 117.8(5) . . ?
C21 N3 Re1 128.0(4) . . ?
C15 N3 Re1 114.0(3) . . ?
C25 N4 C20 116.5(4) . . ?
C25 N4 Re1 127.7(4) . . ?
C20 N4 Re1 115.7(3) . . ?
N2 C1 C2 122.8(5) . . ?
C3 C2 C1 119.0(6) . . ?
C2 C3 C4 120.2(6) . . ?
C3 C4 C5 117.8(5) . . ?
C3 C4 C6 124.3(6) . . ?
C5 C4 C6 117.8(6) . . ?
N2 C5 C4 121.7(5) . . ?
N2 C5 C9 117.5(5) . . ?
C4 C5 C9 120.8(5) . . ?
C7 C6 C4 120.9(6) . . ?
C6 C7 C8 122.4(6) . . ?
C12 C8 C9 118.1(6) . . ?
C12 C8 C7 124.8(6) . . ?
C9 C8 C7 117.1(6) . . ?
N1 C9 C8 122.3(5) . . ?
N1 C9 C5 116.9(4) . . ?
C8 C9 C5 120.8(5) . . ?
C12 C10 C11 120.0(6) . . ?
N1 C11 C10 122.5(6) . . ?
C10 C12 C8 119.6(6) . . ?
O1 C13 Re1 175.6(5) . . ?
O2 C14 Re1 177.2(5) . . ?
N3 C15 C16 123.0(5) . . ?
N3 C15 C20 116.9(4) . . ?
C16 C15 C20 120.1(5) . . ?
C23 C16 C15 117.2(5) . . ?
C23 C16 C17 124.3(5) . . ?
C15 C16 C17 118.4(5) . . ?
C18 C17 C16 121.3(5) . . ?
C17 C18 C19 121.9(5) . . ?
C24 C19 C20 117.9(5) . . ?
C24 C19 C18 123.9(5) . . ?
C20 C19 C18 118.2(5) . . ?
N4 C20 C19 123.5(5) . . ?
N4 C20 C15 116.6(4) . . ?
C19 C20 C15 120.0(5) . . ?
N3 C21 C22 122.8(6) . . ?
C23 C22 C21 119.4(5) . . ?
C22 C23 C16 119.7(5) . . ?
C26 C24 C19 119.2(5) . . ?
N4 C25 C26 123.0(5) . . ?
C24 C26 C25 119.9(5) . . ?
N5 C27 C28 178.9(16) . . ?

_refine_diff_density_max         1.556
_refine_diff_density_min         -1.865
_refine_diff_density_rms         0.132

_shelxl_version_number           2014-3

_database_code_depnum_ccdc_archive 'CCDC 997711'
