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

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



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



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


