# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_MB2-82
_database_code_depnum_ccdc_archive 'CCDC 1587398'
_audit_update_record             
;
2017-11-24 deposited with the CCDC.
2018-02-23 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         'C37 H28 N4'
_chemical_formula_sum            'C37 H28 N4'
_chemical_formula_weight         528.63

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_H-M_alt        'P -4'
_space_group_name_Hall           'P -4'

_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'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'

_cell_length_a                   18.3763(10)
_cell_length_b                   18.3763(10)
_cell_length_c                   4.4365(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1498.15(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3343
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      24.74

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_F_000             556
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.070
_shelx_estimated_absorpt_T_min   0.996
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.996
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2626
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         2.478
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_full        25.009
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             2542
_reflns_number_gt                2216
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0173P)²+0.5852P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   3(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2542
_refine_ls_number_parameters     187
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1427
_refine_ls_wR_factor_gt          0.1371
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
N1 N -0.2312(2) -0.19005(19) 0.2245(9) 0.0614(11) Uani 1 1 d . . . . .
N2 N -0.1289(2) -0.2124(2) -0.0422(12) 0.0722(13) Uani 1 1 d . . . . .
C1 C -0.2337(3) -0.4372(2) -0.4870(10) 0.0564(12) Uani 1 1 d . . . . .
H1 H -0.1901 -0.4489 -0.5914 0.068 Uiso 1 1 calc R U . . .
C2 C -0.2921(3) -0.4815(3) -0.5185(11) 0.0601(14) Uani 1 1 d . . . . .
H2 H -0.2894 -0.5229 -0.6464 0.072 Uiso 1 1 calc R U . . .
C3 C -0.3572(3) -0.4659(2) -0.3597(11) 0.0572(12) Uani 1 1 d . . . . .
H3 H -0.3981 -0.4972 -0.3781 0.069 Uiso 1 1 calc R U . . .
C4 C -0.3608(3) -0.4061(2) -0.1817(9) 0.0482(10) Uani 1 1 d . . . . .
H4 H -0.4050 -0.3958 -0.0790 0.058 Uiso 1 1 calc R U . . .
C5 C -0.3012(2) -0.3584(2) -0.1433(9) 0.0446(10) Uani 1 1 d . . . . .
C6 C -0.2352(2) -0.3739(2) -0.3037(9) 0.0476(10) Uani 1 1 d . . . . .
C7 C -0.1748(2) -0.3278(2) -0.2753(11) 0.0538(12) Uani 1 1 d . . . . .
H7 H -0.1308 -0.3386 -0.3784 0.065 Uiso 1 1 calc R U . . .
C8 C -0.1798(2) -0.2671(2) -0.0974(12) 0.0586(13) Uani 1 1 d . . . . .
C9 C -0.2455(2) -0.2526(2) 0.0669(10) 0.0501(11) Uani 1 1 d . . . . .
C10 C -0.3052(3) -0.2969(2) 0.0443(9) 0.0474(10) Uani 1 1 d . . . . .
H10 H -0.3485 -0.2863 0.1532 0.057 Uiso 1 1 calc R U . . .
C11 C -0.1629(3) -0.1685(3) 0.1442(15) 0.0745(16) Uani 1 1 d . . . . .
H11 H -0.1414 -0.1249 0.2177 0.089 Uiso 1 1 calc R U . . .
C12 C -0.2821(3) -0.1489(2) 0.4162(11) 0.0616(13) Uani 1 1 d . . . . .
H12A H -0.2546 -0.1128 0.5360 0.074 Uiso 1 1 calc R U . . .
H12B H -0.3062 -0.1828 0.5585 0.074 Uiso 1 1 calc R U . . .
C13 C -0.3393(2) -0.1102(2) 0.2331(8) 0.0441(10) Uani 1 1 d . . . . .
C14 C -0.3218(2) -0.0462(2) 0.0824(11) 0.0505(11) Uani 1 1 d . . . . .
H14 H -0.2743 -0.0265 0.0998 0.061 Uiso 1 1 calc R U . . .
C15 C -0.3734(2) -0.0111(2) -0.0931(10) 0.0499(11) Uani 1 1 d . . . . .
H15 H -0.3608 0.0322 -0.1974 0.060 Uiso 1 1 calc R U . . .
C16 C -0.4425(2) -0.0385(2) -0.1172(8) 0.0420(10) Uani 1 1 d . . . . .
C17 C -0.4605(2) -0.10108(19) 0.0365(8) 0.0394(9) Uani 1 1 d . . . . .
H17 H -0.5086 -0.1198 0.0240 0.047 Uiso 1 1 calc R U . . .
C18 C -0.4092(2) -0.1367(2) 0.2085(9) 0.0435(10) Uani 1 1 d . . . . .
H18 H -0.4221 -0.1802 0.3114 0.052 Uiso 1 1 calc R U . . .
C19 C -0.5000 0.0000 -0.3044(12) 0.0543(17) Uani 1 2 d S T P . .
H19A H -0.4758 0.0361 -0.4361 0.065 Uiso 0.5 1 calc R U P . .
H19B H -0.5242 -0.0361 -0.4361 0.065 Uiso 0.5 1 calc R U 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
N1 C11 1.363(7) . ?
N1 C9 1.370(5) . ?
N1 C12 1.474(6) . ?
N2 C11 1.313(7) . ?
N2 C8 1.395(6) . ?
C1 C2 1.354(7) . ?
C1 C6 1.419(6) . ?
C1 H1 0.9500 . ?
C2 C3 1.418(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.355(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.414(6) . ?
C4 H4 0.9500 . ?
C5 C10 1.405(5) . ?
C5 C6 1.435(6) . ?
C6 C7 1.400(6) . ?
C7 C8 1.371(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.434(6) . ?
C9 C10 1.371(6) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.506(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C18 1.377(6) . ?
C13 C14 1.390(6) . ?
C14 C15 1.386(6) . ?
C14 H14 0.9500 . ?
C15 C16 1.370(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.377(5) . ?
C16 C19 1.519(5) . ?
C17 C18 1.379(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C16 1.519(5) 3_455 ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?

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
C11 N1 C9 106.7(4) . . ?
C11 N1 C12 125.9(4) . . ?
C9 N1 C12 127.0(4) . . ?
C11 N2 C8 103.6(5) . . ?
C2 C1 C6 122.5(5) . . ?
C2 C1 H1 118.8 . . ?
C6 C1 H1 118.8 . . ?
C1 C2 C3 119.7(4) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 119.7(5) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 122.4(4) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C10 C5 C4 121.9(4) . . ?
C10 C5 C6 119.9(4) . . ?
C4 C5 C6 118.2(4) . . ?
C7 C6 C1 122.1(4) . . ?
C7 C6 C5 120.3(4) . . ?
C1 C6 C5 117.6(4) . . ?
C8 C7 C6 119.4(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 N2 130.0(5) . . ?
C7 C8 C9 120.0(4) . . ?
N2 C8 C9 109.9(4) . . ?
N1 C9 C10 133.6(4) . . ?
N1 C9 C8 104.7(4) . . ?
C10 C9 C8 121.7(4) . . ?
C9 C10 C5 118.6(4) . . ?
C9 C10 H10 120.7 . . ?
C5 C10 H10 120.7 . . ?
N2 C11 N1 115.0(5) . . ?
N2 C11 H11 122.5 . . ?
N1 C11 H11 122.5 . . ?
N1 C12 C13 112.0(4) . . ?
N1 C12 H12A 109.2 . . ?
C13 C12 H12A 109.2 . . ?
N1 C12 H12B 109.2 . . ?
C13 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C18 C13 C14 118.4(4) . . ?
C18 C13 C12 121.7(4) . . ?
C14 C13 C12 119.9(4) . . ?
C15 C14 C13 120.4(4) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C16 C15 C14 120.5(4) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C15 C16 C17 119.3(4) . . ?
C15 C16 C19 121.1(3) . . ?
C17 C16 C19 119.5(4) . . ?
C16 C17 C18 120.4(4) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 120.9(4) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C16 C19 C16 113.7(4) 3_455 . ?
C16 C19 H19A 108.8 3_455 . ?
C16 C19 H19A 108.8 . . ?
C16 C19 H19B 108.8 3_455 . ?
C16 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -1.3(7) . . . . ?
C1 C2 C3 C4 1.1(6) . . . . ?
C2 C3 C4 C5 -1.0(6) . . . . ?
C3 C4 C5 C10 -179.3(4) . . . . ?
C3 C4 C5 C6 1.0(6) . . . . ?
C2 C1 C6 C7 -179.2(4) . . . . ?
C2 C1 C6 C5 1.4(6) . . . . ?
C10 C5 C6 C7 -0.3(6) . . . . ?
C4 C5 C6 C7 179.4(4) . . . . ?
C10 C5 C6 C1 179.2(3) . . . . ?
C4 C5 C6 C1 -1.2(5) . . . . ?
C1 C6 C7 C8 179.3(4) . . . . ?
C5 C6 C7 C8 -1.3(6) . . . . ?
C6 C7 C8 N2 -177.6(5) . . . . ?
C6 C7 C8 C9 2.4(6) . . . . ?
C11 N2 C8 C7 -179.9(5) . . . . ?
C11 N2 C8 C9 0.1(5) . . . . ?
C11 N1 C9 C10 -176.9(5) . . . . ?
C12 N1 C9 C10 -3.5(7) . . . . ?
C11 N1 C9 C8 2.6(5) . . . . ?
C12 N1 C9 C8 176.1(4) . . . . ?
C7 C8 C9 N1 178.3(4) . . . . ?
N2 C8 C9 N1 -1.7(5) . . . . ?
C7 C8 C9 C10 -2.1(6) . . . . ?
N2 C8 C9 C10 177.9(4) . . . . ?
N1 C9 C10 C5 -180.0(4) . . . . ?
C8 C9 C10 C5 0.6(6) . . . . ?
C4 C5 C10 C9 -179.1(4) . . . . ?
C6 C5 C10 C9 0.6(5) . . . . ?
C8 N2 C11 N1 1.7(6) . . . . ?
C9 N1 C11 N2 -2.9(6) . . . . ?
C12 N1 C11 N2 -176.4(4) . . . . ?
C11 N1 C12 C13 101.1(5) . . . . ?
C9 N1 C12 C13 -71.2(6) . . . . ?
N1 C12 C13 C18 102.3(5) . . . . ?
N1 C12 C13 C14 -77.3(5) . . . . ?
C18 C13 C14 C15 -1.3(6) . . . . ?
C12 C13 C14 C15 178.3(4) . . . . ?
C13 C14 C15 C16 0.9(6) . . . . ?
C14 C15 C16 C17 0.5(6) . . . . ?
C14 C15 C16 C19 179.0(4) . . . . ?
C15 C16 C17 C18 -1.3(5) . . . . ?
C19 C16 C17 C18 -179.8(3) . . . . ?
C14 C13 C18 C17 0.5(6) . . . . ?
C12 C13 C18 C17 -179.1(4) . . . . ?
C16 C17 C18 C13 0.8(6) . . . . ?
C15 C16 C19 C16 -106.6(4) . . . 3_455 ?
C17 C16 C19 C16 71.9(3) . . . 3_455 ?

_refine_diff_density_max         0.164
_refine_diff_density_min         -0.144
_refine_diff_density_rms         0.034



####################################################################### 
# 
# 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_MS-248
_database_code_depnum_ccdc_archive 'CCDC 1587407'
_audit_update_record             
;
2017-11-25 deposited with the CCDC.
2018-02-23 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         'C56 H36 Cl2 N4 O10 Re2'
_chemical_formula_sum            'C56 H36 Cl2 N4 O10 Re2'
_chemical_formula_weight         1368.19

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      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'I 2/m'
_space_group_name_Hall           '-I 2y'

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

_cell_length_a                   12.1045(5)
_cell_length_b                   21.3981(10)
_cell_length_c                   20.7916(10)
_cell_angle_alpha                90
_cell_angle_beta                 90.132(3)
_cell_angle_gamma                90
_cell_volume                     5385.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9641
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      31.14

_exptl_crystal_description       needle
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_F_000             2656
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    4.652
_shelx_estimated_absorpt_T_min   0.707
_shelx_estimated_absorpt_T_max   0.768
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.707
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            61157
_diffrn_reflns_av_unetI/netI     0.0816
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.722
_diffrn_reflns_theta_max         35.032
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.622
_diffrn_measured_fraction_theta_full 0.586
_diffrn_reflns_Laue_measured_fraction_max 0.622
_diffrn_reflns_Laue_measured_fraction_full 0.586
_diffrn_reflns_point_group_measured_fraction_max 0.622
_diffrn_reflns_point_group_measured_fraction_full 0.586
_reflns_number_total             7548
_reflns_number_gt                4671
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0485P)²+19.4222P] 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         7548
_refine_ls_number_parameters     352
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1244
_refine_ls_wR_factor_gt          0.1136
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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 0.71007(2) 0.18994(2) 0.01593(2) 0.03363(8) Uani 1 1 d . . . . .
Cl1 Cl 0.93001(16) 0.0000 -0.06587(11) 0.0570(6) Uani 1 2 d S T P . .
Cl2 Cl 0.49041(12) 0.0000 0.10088(8) 0.0290(3) Uani 1 2 d S T P . .
O1 O 0.8051(3) 0.1095(2) -0.01211(18) 0.0383(8) Uani 1 1 d . . . . .
O2 O 0.6189(3) 0.11017(16) 0.04894(17) 0.0292(6) Uani 1 1 d . . . . .
O5 O 0.5956(4) 0.1971(2) -0.1164(2) 0.0440(10) Uani 1 1 d . . . . .
O3 O 0.8717(5) 0.2856(3) -0.0373(3) 0.0733(18) Uani 1 1 d . . . . .
O4 O 0.5636(4) 0.29592(19) 0.0663(2) 0.0448(10) Uani 1 1 d . . . . .
N1 N 0.9266(3) 0.19722(18) 0.1822(2) 0.0278(8) Uani 1 1 d . . . . .
N2 N 0.7946(4) 0.1828(2) 0.1082(2) 0.0329(9) Uani 1 1 d . . . . .
C1 C 0.8153(6) 0.0000 -0.0176(3) 0.0352(15) Uani 1 2 d S T P . .
C2 C 0.7674(4) 0.0555(3) 0.0000(3) 0.0373(11) Uani 1 1 d . . . . .
C3 C 0.6588(4) 0.0572(2) 0.0392(2) 0.0289(9) Uani 1 1 d . . . . .
C4 C 0.6119(5) 0.0000 0.0571(3) 0.0278(12) Uani 1 2 d S T P . .
C5 C 0.6346(5) 0.1933(2) -0.0671(3) 0.0332(11) Uani 1 1 d . . . . .
C6 C 0.8113(5) 0.2511(3) -0.0162(3) 0.0487(16) Uani 1 1 d . . . . .
C7 C 0.6177(5) 0.2563(3) 0.0471(3) 0.0382(12) Uani 1 1 d . . . . .
C8 C 0.8986(4) 0.1988(3) 0.1208(3) 0.0338(10) Uani 1 1 d . . . . .
H8 H 0.9490 0.2105 0.0880 0.041 Uiso 1 1 calc R U . . .
C9 C 0.8329(4) 0.18004(19) 0.2166(2) 0.0236(8) Uani 1 1 d . . . . .
C10 C 0.7494(4) 0.1706(2) 0.1688(2) 0.0272(8) Uani 1 1 d . . . . .
C11 C 0.6433(4) 0.1547(2) 0.1873(2) 0.0284(9) Uani 1 1 d . . . . .
H11 H 0.5867 0.1491 0.1561 0.034 Uiso 1 1 calc R U . . .
C12 C 0.6212(4) 0.1472(2) 0.2529(2) 0.0269(9) Uani 1 1 d . . . . .
C13 C 0.7067(4) 0.1564(2) 0.3005(2) 0.0279(9) Uani 1 1 d . . . . .
C14 C 0.8145(4) 0.1726(2) 0.2812(2) 0.0261(8) Uani 1 1 d . . . . .
H14 H 0.8721 0.1781 0.3117 0.031 Uiso 1 1 calc R U . . .
C15 C 0.6790(4) 0.1480(2) 0.3660(3) 0.0338(10) Uani 1 1 d . . . . .
H15 H 0.7347 0.1536 0.3978 0.041 Uiso 1 1 calc R U . . .
C16 C 0.5742(4) 0.1320(3) 0.3852(3) 0.0385(11) Uani 1 1 d . . . . .
H16 H 0.5577 0.1275 0.4296 0.046 Uiso 1 1 calc R U . . .
C17 C 0.4907(4) 0.1224(3) 0.3382(3) 0.0369(10) Uani 1 1 d . . . . .
H17 H 0.4183 0.1109 0.3511 0.044 Uiso 1 1 calc R U . . .
C18 C 0.5147(4) 0.1295(2) 0.2741(3) 0.0318(9) Uani 1 1 d . . . . .
H18 H 0.4582 0.1225 0.2432 0.038 Uiso 1 1 calc R U . . .
C19 C 1.0343(4) 0.2158(2) 0.2101(3) 0.0298(9) Uani 1 1 d . . . . .
H19A H 1.0213 0.2386 0.2508 0.036 Uiso 1 1 calc R U . . .
H19B H 1.0719 0.2447 0.1801 0.036 Uiso 1 1 calc R U . . .
C20 C 1.1621(5) 0.1314(2) 0.1721(3) 0.0388(11) Uani 1 1 d . . . . .
H20 H 1.1506 0.1461 0.1295 0.047 Uiso 1 1 calc R U . . .
C21 C 1.2322(5) 0.0808(2) 0.1830(3) 0.0400(12) Uani 1 1 d . . . . .
H21 H 1.2691 0.0615 0.1479 0.048 Uiso 1 1 calc R U . . .
C22 C 1.2480(4) 0.0585(2) 0.2450(3) 0.0381(12) Uani 1 1 d . . . . .
C23 C 1.3192(6) 0.0000 0.2558(5) 0.045(2) Uani 1 2 d S T P . .
H23A H 1.3821 0.0000 0.2255 0.054 Uiso 1 2 calc R U P . .
H23B H 1.3490 0.0000 0.3002 0.054 Uiso 1 2 calc R U P . .
C24 C 1.1959(5) 0.0880(3) 0.2958(3) 0.0448(13) Uani 1 1 d . . . . .
H24 H 1.2074 0.0732 0.3384 0.054 Uiso 1 1 calc R U . . .
C25 C 1.1264(4) 0.1393(3) 0.2853(3) 0.0394(11) Uani 1 1 d . . . . .
H25 H 1.0915 0.1593 0.3206 0.047 Uiso 1 1 calc R U . . .
C26 C 1.1087(4) 0.1608(2) 0.2232(3) 0.0301(9) Uani 1 1 d . . . . .
C27 C 0.9452(14) 0.0000 0.2214(11) 0.127(10) Uani 1 2 d DS T P . .
H27 H 1.0158 0.0000 0.2016 0.152 Uiso 1 2 calc R U P . .
C28 C 0.8558(10) 0.0000 0.1898(14) 0.137(12) Uani 1 2 d DS T P . .
H28 H 0.8610 0.0000 0.1442 0.165 Uiso 1 2 calc R U P . .
C29 C 0.7483(11) 0.0000 0.2170(11) 0.091(6) Uani 1 2 d DS T P . .
H29 H 0.6851 0.0000 0.1898 0.109 Uiso 1 2 calc R U P . .
C30 C 0.7371(12) 0.0000 0.2764(14) 0.099(7) Uani 1 2 d S T P . .
H30 H 0.6653 0.0000 0.2947 0.118 Uiso 1 2 calc R U P . .
C31 C 0.8301(10) 0.0000 0.3162(9) 0.071(3) Uani 1 2 d S T P . .
C32 C 0.9312(9) 0.0000 0.2874(7) 0.064(3) Uani 1 2 d DS T P . .
H32 H 0.9951 0.0000 0.3140 0.077 Uiso 1 2 calc R U P . .
C33 C 0.831(3) 0.0000 0.371(2) 0.22(2) Uani 1 2 d S T P . .
H33A H 0.7553 0.0000 0.3876 0.326 Uiso 1 2 calc R U P . .
H33B H 0.8698 -0.0374 0.3869 0.326 Uiso 0.5 1 calc R U P . .
H33C H 0.8698 0.0374 0.3869 0.326 Uiso 0.5 1 calc R U 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
Re1 C6 1.914(5) . ?
Re1 C7 1.921(7) . ?
Re1 C5 1.952(5) . ?
Re1 O2 2.146(3) . ?
Re1 O1 2.151(4) . ?
Re1 N2 2.177(4) . ?
Cl1 C1 1.716(7) . ?
Cl2 C4 1.731(7) . ?
O1 C2 1.268(7) . ?
O2 C3 1.249(6) . ?
O5 C5 1.132(7) . ?
O3 C6 1.130(7) . ?
O4 C7 1.143(8) . ?
N1 C8 1.320(8) . ?
N1 C9 1.392(6) . ?
N1 C19 1.480(6) . ?
N2 C8 1.329(6) . ?
N2 C10 1.401(7) . ?
C1 C2 1.372(7) 6 ?
C1 C2 1.372(7) . ?
C2 C3 1.549(7) . ?
C3 C4 1.399(6) . ?
C4 C3 1.399(6) 6 ?
C8 H8 0.9500 . ?
C9 C14 1.372(7) . ?
C9 C10 1.429(6) . ?
C10 C11 1.383(6) . ?
C11 C12 1.401(7) . ?
C11 H11 0.9500 . ?
C12 C18 1.414(6) . ?
C12 C13 1.443(6) . ?
C13 C14 1.409(7) . ?
C13 C15 1.416(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.373(7) . ?
C15 H15 0.9500 . ?
C16 C17 1.419(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.372(8) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C26 1.507(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C26 1.393(8) . ?
C20 C21 1.394(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.388(9) . ?
C21 H21 0.9500 . ?
C22 C24 1.383(9) . ?
C22 C23 1.536(6) . ?
C23 C22 1.536(6) 6 ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.400(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(8) . ?
C25 H25 0.9500 . ?
C27 C28 1.27(3) . ?
C27 C32 1.383(17) . ?
C27 H27 0.9500 . ?
C28 C29 1.419(17) . ?
C28 H28 0.9500 . ?
C29 C30 1.24(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.40(2) . ?
C30 H30 0.9500 . ?
C31 C33 1.15(4) . ?
C31 C32 1.36(2) . ?
C32 H32 0.9500 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

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
C6 Re1 C7 89.2(3) . . ?
C6 Re1 C5 88.0(2) . . ?
C7 Re1 C5 90.0(2) . . ?
C6 Re1 O2 170.2(3) . . ?
C7 Re1 O2 100.39(19) . . ?
C5 Re1 O2 94.15(17) . . ?
C6 Re1 O1 96.2(3) . . ?
C7 Re1 O1 174.19(19) . . ?
C5 Re1 O1 92.26(19) . . ?
O2 Re1 O1 74.11(14) . . ?
C6 Re1 N2 93.2(2) . . ?
C7 Re1 N2 91.60(19) . . ?
C5 Re1 N2 178.06(19) . . ?
O2 Re1 N2 84.44(14) . . ?
O1 Re1 N2 86.07(16) . . ?
C2 O1 Re1 118.8(4) . . ?
C3 O2 Re1 118.1(3) . . ?
C8 N1 C9 107.2(4) . . ?
C8 N1 C19 126.7(5) . . ?
C9 N1 C19 125.9(4) . . ?
C8 N2 C10 104.0(4) . . ?
C8 N2 Re1 126.8(4) . . ?
C10 N2 Re1 128.5(3) . . ?
C2 C1 C2 120.0(7) 6 . ?
C2 C1 Cl1 119.9(4) 6 . ?
C2 C1 Cl1 119.9(4) . . ?
O1 C2 C1 125.7(5) . . ?
O1 C2 C3 113.0(5) . . ?
C1 C2 C3 121.3(5) . . ?
O2 C3 C4 126.4(5) . . ?
O2 C3 C2 115.7(4) . . ?
C4 C3 C2 117.7(5) . . ?
C3 C4 C3 121.9(6) . 6 ?
C3 C4 Cl2 119.0(3) . . ?
C3 C4 Cl2 119.0(3) 6 . ?
O5 C5 Re1 176.2(5) . . ?
O3 C6 Re1 177.3(7) . . ?
O4 C7 Re1 179.2(4) . . ?
N1 C8 N2 115.2(5) . . ?
N1 C8 H8 122.4 . . ?
N2 C8 H8 122.4 . . ?
C14 C9 N1 131.9(4) . . ?
C14 C9 C10 123.2(4) . . ?
N1 C9 C10 104.8(4) . . ?
C11 C10 N2 131.3(4) . . ?
C11 C10 C9 119.9(4) . . ?
N2 C10 C9 108.8(4) . . ?
C10 C11 C12 118.5(4) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C11 C12 C18 120.7(4) . . ?
C11 C12 C13 120.9(4) . . ?
C18 C12 C13 118.4(4) . . ?
C14 C13 C15 121.8(4) . . ?
C14 C13 C12 120.1(4) . . ?
C15 C13 C12 118.1(4) . . ?
C9 C14 C13 117.4(4) . . ?
C9 C14 H14 121.3 . . ?
C13 C14 H14 121.3 . . ?
C16 C15 C13 122.1(5) . . ?
C16 C15 H15 118.9 . . ?
C13 C15 H15 118.9 . . ?
C15 C16 C17 119.6(5) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 120.0(5) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C12 121.8(4) . . ?
C17 C18 H18 119.1 . . ?
C12 C18 H18 119.1 . . ?
N1 C19 C26 112.7(4) . . ?
N1 C19 H19A 109.0 . . ?
C26 C19 H19A 109.0 . . ?
N1 C19 H19B 109.0 . . ?
C26 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C26 C20 C21 120.7(5) . . ?
C26 C20 H20 119.7 . . ?
C21 C20 H20 119.7 . . ?
C22 C21 C20 120.0(5) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C24 C22 C21 119.4(5) . . ?
C24 C22 C23 121.1(6) . . ?
C21 C22 C23 119.5(6) . . ?
C22 C23 C22 109.2(5) 6 . ?
C22 C23 H23A 109.8 6 . ?
C22 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 6 . ?
C22 C23 H23B 109.8 . . ?
H23A C23 H23B 108.3 . . ?
C22 C24 C25 120.9(6) . . ?
C22 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C26 C25 C24 119.8(6) . . ?
C26 C25 H25 120.1 . . ?
C24 C25 H25 120.1 . . ?
C25 C26 C20 119.3(5) . . ?
C25 C26 C19 121.2(5) . . ?
C20 C26 C19 119.5(5) . . ?
C28 C27 C32 114.1(19) . . ?
C28 C27 H27 122.9 . . ?
C32 C27 H27 122.9 . . ?
C27 C28 C29 125(2) . . ?
C27 C28 H28 117.4 . . ?
C29 C28 H28 117.4 . . ?
C30 C29 C28 119.8(16) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 120.0(18) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C33 C31 C32 115(2) . . ?
C33 C31 C30 127(3) . . ?
C32 C31 C30 117.5(17) . . ?
C31 C32 C27 123.2(13) . . ?
C31 C32 H32 118.4 . . ?
C27 C32 H32 118.4 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 O1 C2 C1 176.6(5) . . . . ?
Re1 O1 C2 C3 -4.6(5) . . . . ?
C2 C1 C2 O1 178.3(4) 6 . . . ?
Cl1 C1 C2 O1 -5.9(9) . . . . ?
C2 C1 C2 C3 -0.5(10) 6 . . . ?
Cl1 C1 C2 C3 175.3(4) . . . . ?
Re1 O2 C3 C4 179.9(4) . . . . ?
Re1 O2 C3 C2 -3.8(5) . . . . ?
O1 C2 C3 O2 5.5(6) . . . . ?
C1 C2 C3 O2 -175.6(5) . . . . ?
O1 C2 C3 C4 -177.8(5) . . . . ?
C1 C2 C3 C4 1.0(8) . . . . ?
O2 C3 C4 C3 174.5(3) . . . 6 ?
C2 C3 C4 C3 -1.7(9) . . . 6 ?
O2 C3 C4 Cl2 -3.7(8) . . . . ?
C2 C3 C4 Cl2 -179.9(4) . . . . ?
C9 N1 C8 N2 -1.6(6) . . . . ?
C19 N1 C8 N2 -176.6(4) . . . . ?
C10 N2 C8 N1 1.3(6) . . . . ?
Re1 N2 C8 N1 172.0(4) . . . . ?
C8 N1 C9 C14 -178.5(5) . . . . ?
C19 N1 C9 C14 -3.5(8) . . . . ?
C8 N1 C9 C10 1.2(5) . . . . ?
C19 N1 C9 C10 176.2(4) . . . . ?
C8 N2 C10 C11 176.7(6) . . . . ?
Re1 N2 C10 C11 6.3(8) . . . . ?
C8 N2 C10 C9 -0.4(6) . . . . ?
Re1 N2 C10 C9 -170.9(3) . . . . ?
C14 C9 C10 C11 1.7(7) . . . . ?
N1 C9 C10 C11 -178.0(4) . . . . ?
C14 C9 C10 N2 179.3(4) . . . . ?
N1 C9 C10 N2 -0.5(5) . . . . ?
N2 C10 C11 C12 -178.0(5) . . . . ?
C9 C10 C11 C12 -1.1(7) . . . . ?
C10 C11 C12 C18 -178.5(4) . . . . ?
C10 C11 C12 C13 0.6(7) . . . . ?
C11 C12 C13 C14 -0.6(7) . . . . ?
C18 C12 C13 C14 178.5(4) . . . . ?
C11 C12 C13 C15 -179.9(4) . . . . ?
C18 C12 C13 C15 -0.8(7) . . . . ?
N1 C9 C14 C13 178.0(4) . . . . ?
C10 C9 C14 C13 -1.7(7) . . . . ?
C15 C13 C14 C9 -179.6(5) . . . . ?
C12 C13 C14 C9 1.1(7) . . . . ?
C14 C13 C15 C16 -179.8(5) . . . . ?
C12 C13 C15 C16 -0.5(8) . . . . ?
C13 C15 C16 C17 1.2(9) . . . . ?
C15 C16 C17 C18 -0.7(9) . . . . ?
C16 C17 C18 C12 -0.7(9) . . . . ?
C11 C12 C18 C17 -179.5(5) . . . . ?
C13 C12 C18 C17 1.4(7) . . . . ?
C8 N1 C19 C26 -99.0(6) . . . . ?
C9 N1 C19 C26 87.0(6) . . . . ?
C26 C20 C21 C22 1.0(8) . . . . ?
C20 C21 C22 C24 -1.6(8) . . . . ?
C20 C21 C22 C23 175.9(5) . . . . ?
C24 C22 C23 C22 94.0(8) . . . 6 ?
C21 C22 C23 C22 -83.4(8) . . . 6 ?
C21 C22 C24 C25 0.9(8) . . . . ?
C23 C22 C24 C25 -176.6(5) . . . . ?
C22 C24 C25 C26 0.5(9) . . . . ?
C24 C25 C26 C20 -1.1(8) . . . . ?
C24 C25 C26 C19 179.9(5) . . . . ?
C21 C20 C26 C25 0.3(8) . . . . ?
C21 C20 C26 C19 179.4(5) . . . . ?
N1 C19 C26 C25 -105.5(6) . . . . ?
N1 C19 C26 C20 75.5(6) . . . . ?
C32 C27 C28 C29 0.000(2) . . . . ?
C27 C28 C29 C30 0.000(2) . . . . ?
C28 C29 C30 C31 0.000(3) . . . . ?
C29 C30 C31 C33 180.000(4) . . . . ?
C29 C30 C31 C32 0.000(2) . . . . ?
C33 C31 C32 C27 180.000(2) . . . . ?
C30 C31 C32 C27 0.000(2) . . . . ?
C28 C27 C32 C31 0.000(2) . . . . ?

_refine_diff_density_max         1.529
_refine_diff_density_min         -2.266
_refine_diff_density_rms         0.122



####################################################################### 
# 
# 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_MB2-121
_database_code_depnum_ccdc_archive 'CCDC 1587399'
_audit_update_record             
;
2017-11-24 deposited with the CCDC.
2018-02-23 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         'C29 H24 N4'
_chemical_formula_sum            'C29 H24 N4'
_chemical_formula_weight         428.52

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -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, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   12.8628(5)
_cell_length_b                   30.2997(10)
_cell_length_c                   5.5303(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2155.37(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9013
_cell_measurement_theta_min      2.56
_cell_measurement_theta_max      25.64

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             904
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.079
_shelx_estimated_absorpt_T_min   0.994
_shelx_estimated_absorpt_T_max   0.996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.994
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17499
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.564
_diffrn_reflns_theta_max         25.645
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             3942
_reflns_number_gt                3698
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+0.4234P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3942
_refine_ls_number_parameters     299
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0716
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_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
N3 N -0.05526(13) -0.24004(5) 0.0343(3) 0.0184(4) Uani 1 1 d . . . . .
N1 N -0.76486(13) -0.40755(5) 0.4007(3) 0.0201(4) Uani 1 1 d . . . . .
N2 N -0.84613(14) -0.34932(6) 0.2341(4) 0.0240(4) Uani 1 1 d . . . . .
N4 N -0.10740(14) -0.18128(5) -0.1826(4) 0.0233(4) Uani 1 1 d . . . . .
C9 C -0.58176(16) -0.43271(6) 0.3991(4) 0.0177(4) Uani 1 1 d . . . . .
C19 C -0.11358(15) -0.31487(6) 0.1659(4) 0.0157(4) Uani 1 1 d . . . . .
C25 C 0.01788(15) -0.23502(6) -0.1473(4) 0.0167(4) Uani 1 1 d . . . . .
C5 C -0.87309(16) -0.38772(7) 0.1087(4) 0.0204(5) Uani 1 1 d . . . . .
C21 C -0.16370(16) -0.38834(6) 0.2900(4) 0.0196(4) Uani 1 1 d . . . . .
H21 H -0.1608 -0.4115 0.4054 0.023 Uiso 1 1 calc R U . . .
C16 C -0.22219(15) -0.39382(6) 0.0803(4) 0.0169(4) Uani 1 1 d . . . . .
C14 C -0.49883(16) -0.45663(6) 0.4962(4) 0.0192(4) Uani 1 1 d . . . . .
H14 H -0.5079 -0.4723 0.6435 0.023 Uiso 1 1 calc R U . . .
C24 C -0.01539(16) -0.19793(6) -0.2800(4) 0.0183(5) Uani 1 1 d . . . . .
C17 C -0.22583(16) -0.35929(6) -0.0841(4) 0.0182(4) Uani 1 1 d . . . . .
H17 H -0.2658 -0.3624 -0.2275 0.022 Uiso 1 1 calc R U . . .
C18 C -0.17183(16) -0.32019(6) -0.0423(4) 0.0178(4) Uani 1 1 d . . . . .
H18 H -0.1750 -0.2970 -0.1577 0.021 Uiso 1 1 calc R U . . .
C10 C -0.56598(16) -0.41059(6) 0.1808(4) 0.0178(4) Uani 1 1 d . . . . .
H10 H -0.6215 -0.3944 0.1100 0.021 Uiso 1 1 calc R U . . .
C6 C -0.82289(16) -0.42445(7) 0.2111(4) 0.0187(4) Uani 1 1 d . . . . .
C11 C -0.47035(16) -0.41191(6) 0.0664(4) 0.0180(4) Uani 1 1 d . . . . .
H11 H -0.4611 -0.3964 -0.0812 0.022 Uiso 1 1 calc R U . . .
C29 C 0.04326(17) -0.18334(6) -0.4774(4) 0.0226(5) Uani 1 1 d . . . . .
H29 H 0.0228 -0.1582 -0.5682 0.027 Uiso 1 1 calc R U . . .
C7 C -0.78254(16) -0.36302(7) 0.4020(4) 0.0226(5) Uani 1 1 d . . . . .
H7 H -0.7511 -0.3437 0.5158 0.027 Uiso 1 1 calc R U . . .
C23 C -0.12666(17) -0.20724(6) 0.0017(4) 0.0212(5) Uani 1 1 d . . . . .
H23 H -0.1854 -0.2035 0.1040 0.025 Uiso 1 1 calc R U . . .
C26 C 0.10694(16) -0.25890(6) -0.2054(4) 0.0198(5) Uani 1 1 d . . . . .
H26 H 0.1281 -0.2839 -0.1146 0.024 Uiso 1 1 calc R U . . .
C12 C -0.38767(16) -0.43549(6) 0.1630(4) 0.0170(4) Uani 1 1 d . . . . .
C13 C -0.40321(16) -0.45776(6) 0.3798(4) 0.0199(5) Uani 1 1 d . . . . .
H13 H -0.3476 -0.4740 0.4494 0.024 Uiso 1 1 calc R U . . .
C20 C -0.10974(16) -0.34954(6) 0.3328(4) 0.0190(4) Uani 1 1 d . . . . .
H20 H -0.0699 -0.3465 0.4764 0.023 Uiso 1 1 calc R U . . .
C22 C -0.05407(17) -0.27306(6) 0.2252(4) 0.0206(5) Uani 1 1 d . . . . .
H22A H -0.0839 -0.2599 0.3735 0.025 Uiso 1 1 calc R U . . .
H22B H 0.0190 -0.2810 0.2605 0.025 Uiso 1 1 calc R U . . .
C15 C -0.28295(16) -0.43597(6) 0.0377(4) 0.0209(5) Uani 1 1 d . . . . .
H15A H -0.2936 -0.4400 -0.1382 0.025 Uiso 1 1 calc R U . . .
H15B H -0.2419 -0.4614 0.0978 0.025 Uiso 1 1 calc R U . . .
C28 C 0.13196(18) -0.20676(7) -0.5360(4) 0.0245(5) Uani 1 1 d . . . . .
H28 H 0.1730 -0.1974 -0.6693 0.029 Uiso 1 1 calc R U . . .
C2 C -0.90331(17) -0.47207(7) -0.0703(4) 0.0266(5) Uani 1 1 d . . . . .
H2 H -0.9154 -0.5007 -0.1344 0.032 Uiso 1 1 calc R U . . .
C27 C 0.16282(17) -0.24401(7) -0.4034(4) 0.0240(5) Uani 1 1 d . . . . .
H27 H 0.2238 -0.2595 -0.4507 0.029 Uiso 1 1 calc R U . . .
C3 C -0.95289(17) -0.43566(7) -0.1763(5) 0.0282(5) Uani 1 1 d . . . . .
H3 H -0.9970 -0.4402 -0.3119 0.034 Uiso 1 1 calc R U . . .
C8 C -0.68368(16) -0.42986(7) 0.5366(4) 0.0236(5) Uani 1 1 d . . . . .
H8A H -0.7073 -0.4601 0.5770 0.028 Uiso 1 1 calc R U . . .
H8B H -0.6719 -0.4139 0.6903 0.028 Uiso 1 1 calc R U . . .
C1 C -0.83741(17) -0.46727(7) 0.1247(4) 0.0237(5) Uani 1 1 d . . . . .
H1 H -0.8036 -0.4919 0.1966 0.028 Uiso 1 1 calc R U . . .
C4 C -0.93913(17) -0.39344(7) -0.0879(4) 0.0259(5) Uani 1 1 d . . . . .
H4 H -0.9738 -0.3690 -0.1593 0.031 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
N3 C23 1.365(3) . ?
N3 C25 1.384(3) . ?
N3 C22 1.454(3) . ?
N1 C7 1.368(3) . ?
N1 C6 1.385(3) . ?
N1 C8 1.453(3) . ?
N2 C7 1.305(3) . ?
N2 C5 1.398(3) . ?
N4 C23 1.311(3) . ?
N4 C24 1.395(3) . ?
C9 C10 1.396(3) . ?
C9 C14 1.397(3) . ?
C9 C8 1.518(3) . ?
C19 C18 1.383(3) . ?
C19 C20 1.399(3) . ?
C19 C22 1.516(3) . ?
C25 C26 1.393(3) . ?
C25 C24 1.409(3) . ?
C5 C4 1.391(3) . ?
C5 C6 1.406(3) . ?
C21 C20 1.385(3) . ?
C21 C16 1.392(3) . ?
C21 H21 0.9500 . ?
C16 C17 1.387(3) . ?
C16 C15 1.516(3) . ?
C14 C13 1.389(3) . ?
C14 H14 0.9500 . ?
C24 C29 1.399(3) . ?
C17 C18 1.392(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C6 C1 1.395(3) . ?
C11 C12 1.388(3) . ?
C11 H11 0.9500 . ?
C29 C28 1.382(3) . ?
C29 H29 0.9500 . ?
C7 H7 0.9500 . ?
C23 H23 0.9500 . ?
C26 C27 1.385(3) . ?
C26 H26 0.9500 . ?
C12 C13 1.390(3) . ?
C12 C15 1.515(3) . ?
C13 H13 0.9500 . ?
C20 H20 0.9500 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C28 C27 1.403(3) . ?
C28 H28 0.9500 . ?
C2 C1 1.380(3) . ?
C2 C3 1.402(3) . ?
C2 H2 0.9500 . ?
C27 H27 0.9500 . ?
C3 C4 1.381(3) . ?
C3 H3 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C1 H1 0.9500 . ?
C4 H4 0.9500 . ?

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
C23 N3 C25 106.34(17) . . ?
C23 N3 C22 127.14(19) . . ?
C25 N3 C22 126.50(17) . . ?
C7 N1 C6 106.21(18) . . ?
C7 N1 C8 125.12(19) . . ?
C6 N1 C8 127.34(18) . . ?
C7 N2 C5 104.09(17) . . ?
C23 N4 C24 104.10(17) . . ?
C10 C9 C14 118.1(2) . . ?
C10 C9 C8 122.11(19) . . ?
C14 C9 C8 119.76(19) . . ?
C18 C19 C20 118.74(18) . . ?
C18 C19 C22 123.42(18) . . ?
C20 C19 C22 117.84(19) . . ?
N3 C25 C26 132.02(19) . . ?
N3 C25 C24 105.02(17) . . ?
C26 C25 C24 122.96(19) . . ?
C4 C5 N2 130.01(19) . . ?
C4 C5 C6 119.78(19) . . ?
N2 C5 C6 110.20(19) . . ?
C20 C21 C16 120.94(19) . . ?
C20 C21 H21 119.5 . . ?
C16 C21 H21 119.5 . . ?
C17 C16 C21 118.31(18) . . ?
C17 C16 C15 121.10(19) . . ?
C21 C16 C15 120.57(18) . . ?
C13 C14 C9 120.72(19) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
N4 C24 C29 130.14(19) . . ?
N4 C24 C25 110.19(18) . . ?
C29 C24 C25 119.67(19) . . ?
C16 C17 C18 121.1(2) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 120.48(19) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C11 C10 C9 120.72(19) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
N1 C6 C1 132.5(2) . . ?
N1 C6 C5 105.04(17) . . ?
C1 C6 C5 122.5(2) . . ?
C10 C11 C12 121.34(19) . . ?
C10 C11 H11 119.3 . . ?
C12 C11 H11 119.3 . . ?
C28 C29 C24 117.77(19) . . ?
C28 C29 H29 121.1 . . ?
C24 C29 H29 121.1 . . ?
N2 C7 N1 114.5(2) . . ?
N2 C7 H7 122.8 . . ?
N1 C7 H7 122.8 . . ?
N4 C23 N3 114.3(2) . . ?
N4 C23 H23 122.8 . . ?
N3 C23 H23 122.8 . . ?
C27 C26 C25 116.12(19) . . ?
C27 C26 H26 121.9 . . ?
C25 C26 H26 121.9 . . ?
C11 C12 C13 118.1(2) . . ?
C11 C12 C15 120.69(19) . . ?
C13 C12 C15 121.17(19) . . ?
C14 C13 C12 121.01(19) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C21 C20 C19 120.4(2) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
N3 C22 C19 114.38(17) . . ?
N3 C22 H22A 108.7 . . ?
C19 C22 H22A 108.7 . . ?
N3 C22 H22B 108.7 . . ?
C19 C22 H22B 108.7 . . ?
H22A C22 H22B 107.6 . . ?
C12 C15 C16 112.29(16) . . ?
C12 C15 H15A 109.1 . . ?
C16 C15 H15A 109.1 . . ?
C12 C15 H15B 109.1 . . ?
C16 C15 H15B 109.1 . . ?
H15A C15 H15B 107.9 . . ?
C29 C28 C27 121.6(2) . . ?
C29 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
C1 C2 C3 121.5(2) . . ?
C1 C2 H2 119.2 . . ?
C3 C2 H2 119.2 . . ?
C26 C27 C28 121.9(2) . . ?
C26 C27 H27 119.1 . . ?
C28 C27 H27 119.1 . . ?
C4 C3 C2 121.5(2) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
N1 C8 C9 112.82(18) . . ?
N1 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
N1 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C2 C1 C6 116.6(2) . . ?
C2 C1 H1 121.7 . . ?
C6 C1 H1 121.7 . . ?
C3 C4 C5 118.1(2) . . ?
C3 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C23 N3 C25 C26 -179.3(2) . . . . ?
C22 N3 C25 C26 2.3(3) . . . . ?
C23 N3 C25 C24 0.5(2) . . . . ?
C22 N3 C25 C24 -177.95(17) . . . . ?
C7 N2 C5 C4 179.6(2) . . . . ?
C7 N2 C5 C6 0.2(2) . . . . ?
C20 C21 C16 C17 -0.5(3) . . . . ?
C20 C21 C16 C15 -178.60(19) . . . . ?
C10 C9 C14 C13 0.8(3) . . . . ?
C8 C9 C14 C13 -176.59(18) . . . . ?
C23 N4 C24 C29 -179.1(2) . . . . ?
C23 N4 C24 C25 0.7(2) . . . . ?
N3 C25 C24 N4 -0.8(2) . . . . ?
C26 C25 C24 N4 179.03(19) . . . . ?
N3 C25 C24 C29 179.07(18) . . . . ?
C26 C25 C24 C29 -1.1(3) . . . . ?
C21 C16 C17 C18 0.5(3) . . . . ?
C15 C16 C17 C18 178.57(19) . . . . ?
C20 C19 C18 C17 0.2(3) . . . . ?
C22 C19 C18 C17 -179.12(19) . . . . ?
C16 C17 C18 C19 -0.4(3) . . . . ?
C14 C9 C10 C11 -0.9(3) . . . . ?
C8 C9 C10 C11 176.48(19) . . . . ?
C7 N1 C6 C1 -178.7(2) . . . . ?
C8 N1 C6 C1 14.1(4) . . . . ?
C7 N1 C6 C5 -0.1(2) . . . . ?
C8 N1 C6 C5 -167.34(19) . . . . ?
C4 C5 C6 N1 -179.53(19) . . . . ?
N2 C5 C6 N1 -0.1(2) . . . . ?
C4 C5 C6 C1 -0.8(3) . . . . ?
N2 C5 C6 C1 178.7(2) . . . . ?
C9 C10 C11 C12 0.6(3) . . . . ?
N4 C24 C29 C28 -179.3(2) . . . . ?
C25 C24 C29 C28 0.9(3) . . . . ?
C5 N2 C7 N1 -0.3(3) . . . . ?
C6 N1 C7 N2 0.2(2) . . . . ?
C8 N1 C7 N2 167.9(2) . . . . ?
C24 N4 C23 N3 -0.4(2) . . . . ?
C25 N3 C23 N4 -0.1(2) . . . . ?
C22 N3 C23 N4 178.37(18) . . . . ?
N3 C25 C26 C27 -179.9(2) . . . . ?
C24 C25 C26 C27 0.4(3) . . . . ?
C10 C11 C12 C13 -0.3(3) . . . . ?
C10 C11 C12 C15 -178.95(17) . . . . ?
C9 C14 C13 C12 -0.6(3) . . . . ?
C11 C12 C13 C14 0.3(3) . . . . ?
C15 C12 C13 C14 178.90(18) . . . . ?
C16 C21 C20 C19 0.4(3) . . . . ?
C18 C19 C20 C21 -0.2(3) . . . . ?
C22 C19 C20 C21 179.13(19) . . . . ?
C23 N3 C22 C19 89.3(2) . . . . ?
C25 N3 C22 C19 -92.6(2) . . . . ?
C18 C19 C22 N3 -5.3(3) . . . . ?
C20 C19 C22 N3 175.37(18) . . . . ?
C11 C12 C15 C16 77.5(2) . . . . ?
C13 C12 C15 C16 -101.1(2) . . . . ?
C17 C16 C15 C12 -94.8(2) . . . . ?
C21 C16 C15 C12 83.2(2) . . . . ?
C24 C29 C28 C27 0.1(3) . . . . ?
C25 C26 C27 C28 0.6(3) . . . . ?
C29 C28 C27 C26 -0.8(3) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
C7 N1 C8 C9 -88.4(3) . . . . ?
C6 N1 C8 C9 76.6(2) . . . . ?
C10 C9 C8 N1 8.4(3) . . . . ?
C14 C9 C8 N1 -174.32(17) . . . . ?
C3 C2 C1 C6 0.1(3) . . . . ?
N1 C6 C1 C2 179.1(2) . . . . ?
C5 C6 C1 C2 0.7(3) . . . . ?
C2 C3 C4 C5 0.9(3) . . . . ?
N2 C5 C4 C3 -179.4(2) . . . . ?
C6 C5 C4 C3 -0.1(3) . . . . ?

_refine_diff_density_max         0.123
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.035

####################################################################### 
# 
# 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_MB2-85
_database_code_depnum_ccdc_archive 'CCDC 1587406'
_audit_update_record             
;
2017-11-24 deposited with the CCDC.
2018-02-23 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         'C68 H42 N4 O10 Re2'
_chemical_formula_sum            'C68 H42 N4 O10 Re2'
_chemical_formula_weight         1447.45

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      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                   14.5376(8)
_cell_length_b                   14.8971(8)
_cell_length_c                   15.5162(8)
_cell_angle_alpha                109.772(2)
_cell_angle_beta                 110.734(2)
_cell_angle_gamma                101.320(2)
_cell_volume                     2760.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9540
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      25.74

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.450
_shelx_estimated_absorpt_T_min   0.746
_shelx_estimated_absorpt_T_max   0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  0.808
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            76040
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0407
_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       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.188
_diffrn_reflns_theta_max         25.787
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             10501
_reflns_number_gt                9337
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0478P)²+61.0624P] 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         10501
_refine_ls_number_parameters     757
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0516
_refine_ls_wR_factor_ref         0.1345
_refine_ls_wR_factor_gt          0.1286
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.022
_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
C1 C 0.0233(7) 0.7714(7) 0.1514(7) 0.034(2) Uani 1 1 d . . . . .
H1 H 0.0747 0.8217 0.1513 0.041 Uiso 1 1 calc R U . . .
C2 C -0.0613(8) 0.7913(8) 0.1602(8) 0.040(2) Uani 1 1 d . . . . .
H2 H -0.0678 0.8551 0.1665 0.048 Uiso 1 1 calc R U . . .
C3 C -0.1396(7) 0.7180(8) 0.1601(8) 0.045(3) Uani 1 1 d . . . . .
H3 H -0.1978 0.7332 0.1672 0.055 Uiso 1 1 calc R U . . .
C4 C -0.1318(7) 0.6258(8) 0.1500(8) 0.041(2) Uani 1 1 d . . . . .
H4 H -0.1852 0.5769 0.1495 0.049 Uiso 1 1 calc R U . . .
C5 C -0.0448(6) 0.6016(7) 0.1403(7) 0.0301(19) Uani 1 1 d . . . . .
C6 C 0.0360(6) 0.6778(7) 0.1424(6) 0.0280(18) Uani 1 1 d . . . . .
C7 C 0.1247(6) 0.6582(7) 0.1369(7) 0.0264(17) Uani 1 1 d . . . . .
H7 H 0.1780 0.7077 0.1380 0.032 Uiso 1 1 calc R U . . .
C8 C -0.0361(6) 0.5069(7) 0.1310(7) 0.0293(18) Uani 1 1 d . . . . .
H8 H -0.0892 0.4557 0.1282 0.035 Uiso 1 1 calc R U . . .
C9 C 0.1333(6) 0.5656(6) 0.1300(6) 0.0251(17) Uani 1 1 d . . . . .
C10 C 0.0526(6) 0.4915(6) 0.1262(6) 0.0254(17) Uani 1 1 d . . . . .
C11 C 0.1792(6) 0.4340(6) 0.1177(6) 0.0260(17) Uani 1 1 d . . . . .
H11 H 0.2183 0.3899 0.1132 0.031 Uiso 1 1 calc R U . . .
C12 C 0.0231(7) 0.3096(6) 0.1057(7) 0.0304(19) Uani 1 1 d . . . . .
H12A H 0.0462 0.2559 0.0713 0.036 Uiso 1 1 calc R U . . .
H12B H -0.0525 0.2914 0.0608 0.036 Uiso 1 1 calc R U . . .
C13 C 0.0358(7) 0.3106(6) 0.2073(8) 0.031(2) Uani 1 1 d . . . . .
C14 C -0.0447(8) 0.3129(9) 0.2352(10) 0.050(3) Uani 1 1 d . . . . .
H14 H -0.1086 0.3144 0.1908 0.059 Uiso 1 1 calc R U . . .
C15 C -0.0316(9) 0.3130(10) 0.3291(11) 0.056(3) Uani 1 1 d . . . . .
H15 H -0.0873 0.3146 0.3473 0.067 Uiso 1 1 calc R U . . .
C16 C 0.0585(8) 0.3108(7) 0.3954(8) 0.037(2) Uani 1 1 d . . . . .
C17 C 0.1378(8) 0.3046(8) 0.3646(8) 0.041(2) Uani 1 1 d . . . . .
H17 H 0.2003 0.3001 0.4078 0.050 Uiso 1 1 calc R U . . .
C18 C 0.1265(7) 0.3050(8) 0.2724(8) 0.039(2) Uani 1 1 d . . . . .
H18 H 0.1816 0.3013 0.2535 0.046 Uiso 1 1 calc R U . . .
C19 C 0.0763(8) 0.3101(9) 0.4993(9) 0.048(3) Uani 1 1 d . . . . .
H19A H 0.0112 0.3087 0.5068 0.058 Uiso 1 1 calc R U . . .
H19B H 0.0877 0.2463 0.4976 0.058 Uiso 1 1 calc R U . . .
C20 C 0.1669(8) 0.3988(7) 0.5920(8) 0.037(2) Uani 1 1 d . . . . .
C21 C 0.1659(10) 0.4950(11) 0.6247(14) 0.094(6) Uani 1 1 d . . . . .
H21 H 0.1053 0.5070 0.5887 0.113 Uiso 1 1 calc R U . . .
C22 C 0.2530(11) 0.5775(10) 0.7109(14) 0.094(6) Uani 1 1 d . . . . .
H22 H 0.2512 0.6447 0.7307 0.112 Uiso 1 1 calc R U . . .
C23 C 0.3384(7) 0.5625(7) 0.7654(8) 0.0309(19) Uani 1 1 d . . . . .
C24 C 0.3384(12) 0.4666(9) 0.7352(10) 0.064(4) Uani 1 1 d . . . . .
H24 H 0.3974 0.4544 0.7741 0.077 Uiso 1 1 calc R U . . .
C25 C 0.2555(12) 0.3860(10) 0.6496(10) 0.066(4) Uani 1 1 d . . . . .
H25 H 0.2594 0.3196 0.6296 0.079 Uiso 1 1 calc R U . . .
C26 C 0.4317(7) 0.6496(7) 0.8624(8) 0.035(2) Uani 1 1 d . . . . .
H26A H 0.4085 0.6736 0.9161 0.042 Uiso 1 1 calc R U . . .
H26B H 0.4873 0.6226 0.8879 0.042 Uiso 1 1 calc R U . . .
C27 C 0.5176(6) 0.8899(7) 0.8459(6) 0.0259(18) Uani 1 1 d . . . . .
C28 C 0.5602(6) 0.7542(6) 0.8287(7) 0.0260(17) Uani 1 1 d . . . . .
H28 H 0.5941 0.7062 0.8165 0.031 Uiso 1 1 calc R U . . .
C29 C 0.5121(6) 0.9817(7) 0.8541(7) 0.0267(17) Uani 1 1 d . . . . .
H29 H 0.5621 1.0277 0.8481 0.032 Uiso 1 1 calc R U . . .
C30 C 0.4466(6) 0.8211(7) 0.8589(7) 0.0270(18) Uani 1 1 d . . . . .
C31 C 0.3652(7) 0.8444(8) 0.8765(7) 0.036(2) Uani 1 1 d . . . . .
H31 H 0.3168 0.7985 0.8842 0.043 Uiso 1 1 calc R U . . .
C32 C 0.3569(7) 0.9384(9) 0.8826(7) 0.036(2) Uani 1 1 d . . . . .
C33 C 0.4298(7) 1.0071(8) 0.8720(6) 0.031(2) Uani 1 1 d . . . . .
C34 C 0.4205(8) 1.1030(8) 0.8800(8) 0.039(2) Uani 1 1 d . . . . .
H34 H 0.4704 1.1503 0.8752 0.047 Uiso 1 1 calc R U . . .
C35 C 0.3388(9) 1.1260(10) 0.8946(8) 0.047(3) Uani 1 1 d . . . . .
H35 H 0.3321 1.1895 0.8994 0.056 Uiso 1 1 calc R U . . .
C36 C 0.2645(10) 1.0570(11) 0.9026(9) 0.055(3) Uani 1 1 d . . . . .
H36 H 0.2085 1.0748 0.9126 0.066 Uiso 1 1 calc R U . . .
C37 C 0.2714(9) 0.9655(10) 0.8962(8) 0.048(3) Uani 1 1 d . . . . .
H37 H 0.2200 0.9195 0.9007 0.058 Uiso 1 1 calc R U . . .
C38 C 0.8239(7) 0.9409(6) 0.7554(7) 0.0259(17) Uani 1 1 d . . . . .
C39 C 0.8201(7) 0.8869(7) 0.9004(7) 0.0286(18) Uani 1 1 d . . . . .
C40 C 0.7651(7) 1.0413(8) 0.8913(7) 0.032(2) Uani 1 1 d . . . . .
C41 C 0.5937(6) 0.7142(6) 0.5826(7) 0.0232(16) Uani 1 1 d . . . . .
C42 C 0.5843(7) 0.6132(6) 0.5218(7) 0.0270(18) Uani 1 1 d . . . . .
H42 H 0.6200 0.5786 0.5555 0.032 Uiso 1 1 calc R U . . .
C43 C 0.5270(7) 0.5651(6) 0.4190(7) 0.0289(18) Uani 1 1 d . . . . .
H43 H 0.5244 0.4983 0.3824 0.035 Uiso 1 1 calc R U . . .
C44 C 0.4695(6) 0.6118(6) 0.3628(7) 0.0235(17) Uani 1 1 d . . . . .
C45 C 0.5355(6) 0.7632(6) 0.5318(7) 0.0225(16) Uani 1 1 d . . . . .
C46 C 0.4725(6) 0.7104(6) 0.4197(6) 0.0215(16) Uani 1 1 d . . . . .
C47 C 0.4076(6) 0.7563(6) 0.3691(6) 0.0220(16) Uani 1 1 d . . . . .
C48 C 0.3926(6) 0.8463(6) 0.4312(6) 0.0228(16) Uani 1 1 d . . . . .
C49 C 0.4555(6) 0.8981(6) 0.5373(7) 0.0240(17) Uani 1 1 d . . . . .
C50 C 0.5348(6) 0.8601(6) 0.5889(6) 0.0224(16) Uani 1 1 d . . . . .
C51 C 0.4441(7) 0.9863(6) 0.5941(7) 0.0268(17) Uani 1 1 d . . . . .
H51 H 0.4889 1.0232 0.6661 0.032 Uiso 1 1 calc R U . . .
C52 C 0.3686(7) 1.0211(7) 0.5474(7) 0.0308(19) Uani 1 1 d . . . . .
H52 H 0.3604 1.0805 0.5872 0.037 Uiso 1 1 calc R U . . .
C53 C 0.3044(7) 0.9677(7) 0.4409(7) 0.0298(19) Uani 1 1 d . . . . .
H53 H 0.2519 0.9909 0.4086 0.036 Uiso 1 1 calc R U . . .
C54 C 0.3164(6) 0.8827(7) 0.3827(7) 0.0291(18) Uani 1 1 d . . . . .
H54 H 0.2739 0.8483 0.3102 0.035 Uiso 1 1 calc R U . . .
C55 C 0.5105(7) 0.6881(7) 0.1915(7) 0.0295(19) Uani 1 1 d . . . . .
C56 C 0.3775(6) 0.5017(7) 0.0494(7) 0.0309(19) Uani 1 1 d . . . . .
C57 C 0.3158(6) 0.6586(7) 0.0512(7) 0.0286(19) Uani 1 1 d . . . . .
C58 C 0.292(2) 0.5783(17) 0.484(3) 0.207(19) Uani 1 1 d . . . . .
H58A H 0.3501 0.5939 0.5495 0.311 Uiso 1 1 calc R U . . .
H58B H 0.2366 0.5138 0.4598 0.311 Uiso 1 1 calc R U . . .
H58C H 0.3190 0.5721 0.4327 0.311 Uiso 1 1 calc R U . . .
C59 C 0.2523(15) 0.6561(13) 0.4956(16) 0.086(5) Uani 1 1 d . . . . .
C60 C 0.1687(14) 0.6458(14) 0.4080(12) 0.083(5) Uani 1 1 d . . . . .
H60 H 0.1401 0.5871 0.3439 0.099 Uiso 1 1 calc R U . . .
C61 C 0.1302(12) 0.7227(15) 0.4179(12) 0.077(5) Uani 1 1 d . . . . .
H61 H 0.0743 0.7150 0.3576 0.093 Uiso 1 1 calc R U . . .
C62 C 0.1635(13) 0.8101(16) 0.5060(16) 0.089(6) Uani 1 1 d . . . . .
H62 H 0.1339 0.8619 0.5084 0.107 Uiso 1 1 calc R U . . .
C63 C 0.2390(13) 0.8156(11) 0.5856(14) 0.074(4) Uani 1 1 d . . . . .
H63 H 0.2622 0.8728 0.6495 0.088 Uiso 1 1 calc R U . . .
C64 C 0.2882(10) 0.7468(11) 0.5860(10) 0.064(4) Uani 1 1 d . . . . .
H64 H 0.3468 0.7598 0.6472 0.077 Uiso 1 1 calc R U . . .
N1 N 0.0833(5) 0.4078(5) 0.1166(5) 0.0252(15) Uani 1 1 d . . . . .
N2 N 0.2119(5) 0.5264(5) 0.1256(5) 0.0250(14) Uani 1 1 d . . . . .
N3 N 0.4775(6) 0.7374(6) 0.8481(6) 0.0310(16) Uani 1 1 d . . . . .
N4 N 0.5908(5) 0.8442(6) 0.8280(5) 0.0253(15) Uani 1 1 d . . . . .
O1 O 0.8873(5) 0.9605(5) 0.7329(5) 0.0382(15) Uani 1 1 d . . . . .
O2 O 0.7944(5) 1.1277(5) 0.9478(5) 0.0351(14) Uani 1 1 d . . . . .
O3 O 0.8835(5) 0.8791(6) 0.9654(5) 0.0381(15) Uani 1 1 d . . . . .
O4 O 0.5939(4) 0.9169(4) 0.6832(4) 0.0245(12) Uani 1 1 d . . . . .
O5 O 0.6532(4) 0.7503(4) 0.6802(4) 0.0251(12) Uani 1 1 d . . . . .
O6 O 0.3598(4) 0.7234(4) 0.2717(4) 0.0255(12) Uani 1 1 d . . . . .
O7 O 0.4200(4) 0.5575(4) 0.2641(5) 0.0271(12) Uani 1 1 d . . . . .
O8 O 0.5976(5) 0.7339(5) 0.2159(6) 0.0385(16) Uani 1 1 d . . . . .
O9 O 0.2844(5) 0.6873(5) -0.0092(5) 0.0342(14) Uani 1 1 d . . . . .
O10 O 0.3877(5) 0.4369(5) -0.0087(5) 0.0376(15) Uani 1 1 d . . . . .
Re1 Re 0.71720(2) 0.90245(2) 0.79520(2) 0.02080(10) Uani 1 1 d . . . . .
Re2 Re 0.36869(2) 0.61013(2) 0.15190(2) 0.02212(10) Uani 1 1 d . . . . .
C66 C 0.0244(14) 0.0248(12) 0.4429(15) 0.075(4) Uani 1 1 d . U . . .
C65 C 0.1595(13) 0.0816(16) 0.6262(17) 0.119(7) Uani 1 1 d . U . . .
C67 C 0.129(2) 0.0738(19) 0.520(2) 0.135(8) Uani 1 1 d . U . . .
C68 C -0.063(2) -0.025(2) 0.413(3) 0.227(16) Uani 1 1 d . 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
C1 C2 1.361(13) . ?
C1 C6 1.409(13) . ?
C1 H1 0.9500 . ?
C2 C3 1.413(16) . ?
C2 H2 0.9500 . ?
C3 C4 1.361(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.425(12) . ?
C4 H4 0.9500 . ?
C5 C8 1.405(13) . ?
C5 C6 1.446(13) . ?
C6 C7 1.402(12) . ?
C7 C9 1.382(12) . ?
C7 H7 0.9500 . ?
C8 C10 1.377(12) . ?
C8 H8 0.9500 . ?
C9 N2 1.394(10) . ?
C9 C10 1.412(12) . ?
C10 N1 1.384(11) . ?
C11 N2 1.313(11) . ?
C11 N1 1.365(10) . ?
C11 H11 0.9500 . ?
C12 N1 1.470(11) . ?
C12 C13 1.515(14) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.387(13) . ?
C13 C18 1.387(14) . ?
C14 C15 1.401(17) . ?
C14 H14 0.9500 . ?
C15 C16 1.364(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.403(14) . ?
C16 C19 1.544(15) . ?
C17 C18 1.383(15) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.497(14) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.354(16) . ?
C20 C25 1.375(16) . ?
C21 C22 1.407(19) . ?
C21 H21 0.9500 . ?
C22 C23 1.342(15) . ?
C22 H22 0.9500 . ?
C23 C24 1.345(14) . ?
C23 C26 1.527(13) . ?
C24 C25 1.370(18) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 N3 1.472(10) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C29 1.351(12) . ?
C27 C30 1.424(11) . ?
C27 N4 1.428(11) . ?
C28 N4 1.333(11) . ?
C28 N3 1.337(11) . ?
C28 H28 0.9500 . ?
C29 C33 1.413(12) . ?
C29 H29 0.9500 . ?
C30 N3 1.384(12) . ?
C30 C31 1.387(13) . ?
C31 C32 1.402(15) . ?
C31 H31 0.9500 . ?
C32 C33 1.417(14) . ?
C32 C37 1.441(13) . ?
C33 C34 1.429(14) . ?
C34 C35 1.370(14) . ?
C34 H34 0.9500 . ?
C35 C36 1.408(18) . ?
C35 H35 0.9500 . ?
C36 C37 1.360(17) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 O1 1.117(10) . ?
C38 Re1 1.919(8) . ?
C39 O3 1.158(11) . ?
C39 Re1 1.903(9) . ?
C40 O2 1.168(12) . ?
C40 Re1 1.897(10) . ?
C41 O5 1.293(10) . ?
C41 C45 1.424(11) . ?
C41 C42 1.429(12) . ?
C42 C43 1.343(13) . ?
C42 H42 0.9500 . ?
C43 C44 1.437(11) . ?
C43 H43 0.9500 . ?
C44 O7 1.292(10) . ?
C44 C46 1.418(11) . ?
C45 C50 1.420(11) . ?
C45 C46 1.466(12) . ?
C46 C47 1.437(11) . ?
C47 O6 1.277(10) . ?
C47 C48 1.472(12) . ?
C48 C49 1.392(12) . ?
C48 C54 1.418(11) . ?
C49 C51 1.392(12) . ?
C49 C50 1.482(11) . ?
C50 O4 1.257(10) . ?
C51 C52 1.382(12) . ?
C51 H51 0.9500 . ?
C52 C53 1.401(13) . ?
C52 H52 0.9500 . ?
C53 C54 1.368(13) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 O8 1.165(11) . ?
C55 Re2 1.912(9) . ?
C56 O10 1.153(11) . ?
C56 Re2 1.908(9) . ?
C57 O9 1.148(11) . ?
C57 Re2 1.919(9) . ?
C58 C59 1.38(3) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C60 1.40(3) . ?
C59 C64 1.41(2) . ?
C60 C61 1.36(2) . ?
C60 H60 0.9500 . ?
C61 C62 1.37(2) . ?
C61 H61 0.9500 . ?
C62 C63 1.29(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.36(2) . ?
C63 H63 0.9500 . ?
C64 H64 0.9500 . ?
N2 Re2 2.190(7) . ?
N4 Re1 2.173(7) . ?
O4 Re1 2.116(5) . ?
O5 Re1 2.109(6) . ?
O6 Re2 2.110(6) . ?
O7 Re2 2.107(6) . ?
C66 C67 1.40(3) . ?
C66 C68 1.17(3) . ?
C65 C68 1.28(3) 2_556 ?
C65 C67 1.51(4) . ?
C68 C65 1.28(3) 2_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 C6 121.3(9) . . ?
C2 C1 H1 119.3 . . ?
C6 C1 H1 119.3 . . ?
C1 C2 C3 120.8(9) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 C2 120.2(9) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.9(10) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C8 C5 C4 121.0(9) . . ?
C8 C5 C6 120.5(8) . . ?
C4 C5 C6 118.5(9) . . ?
C7 C6 C1 121.7(8) . . ?
C7 C6 C5 120.1(8) . . ?
C1 C6 C5 118.3(8) . . ?
C9 C7 C6 118.8(8) . . ?
C9 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C10 C8 C5 117.2(8) . . ?
C10 C8 H8 121.4 . . ?
C5 C8 H8 121.4 . . ?
C7 C9 N2 131.4(8) . . ?
C7 C9 C10 120.2(7) . . ?
N2 C9 C10 108.4(7) . . ?
C8 C10 N1 130.8(8) . . ?
C8 C10 C9 123.2(8) . . ?
N1 C10 C9 106.0(7) . . ?
N2 C11 N1 113.0(7) . . ?
N2 C11 H11 123.5 . . ?
N1 C11 H11 123.5 . . ?
N1 C12 C13 113.4(7) . . ?
N1 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 . . ?
N1 C12 H12B 108.9 . . ?
C13 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C14 C13 C18 118.5(10) . . ?
C14 C13 C12 120.7(9) . . ?
C18 C13 C12 120.7(8) . . ?
C13 C14 C15 119.8(10) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 122.3(9) . . ?
C16 C15 H15 118.8 . . ?
C14 C15 H15 118.8 . . ?
C15 C16 C17 117.4(10) . . ?
C15 C16 C19 124.1(9) . . ?
C17 C16 C19 118.4(9) . . ?
C18 C17 C16 121.1(10) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C17 C18 C13 120.8(9) . . ?
C17 C18 H18 119.6 . . ?
C13 C18 H18 119.6 . . ?
C20 C19 C16 115.1(8) . . ?
C20 C19 H19A 108.5 . . ?
C16 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C16 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C21 C20 C25 116.4(10) . . ?
C21 C20 C19 122.3(11) . . ?
C25 C20 C19 121.2(10) . . ?
C20 C21 C22 121.3(11) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C23 C22 C21 120.7(11) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 118.1(11) . . ?
C22 C23 C26 122.0(9) . . ?
C24 C23 C26 119.8(9) . . ?
C23 C24 C25 121.7(12) . . ?
C23 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
C20 C25 C24 121.6(11) . . ?
C20 C25 H25 119.2 . . ?
C24 C25 H25 119.2 . . ?
N3 C26 C23 114.5(7) . . ?
N3 C26 H26A 108.6 . . ?
C23 C26 H26A 108.6 . . ?
N3 C26 H26B 108.6 . . ?
C23 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C29 C27 C30 122.4(8) . . ?
C29 C27 N4 130.1(8) . . ?
C30 C27 N4 107.4(7) . . ?
N4 C28 N3 114.0(8) . . ?
N4 C28 H28 123.0 . . ?
N3 C28 H28 123.0 . . ?
C27 C29 C33 117.9(8) . . ?
C27 C29 H29 121.1 . . ?
C33 C29 H29 121.1 . . ?
N3 C30 C31 133.0(8) . . ?
N3 C30 C27 106.2(7) . . ?
C31 C30 C27 120.7(8) . . ?
C30 C31 C32 117.5(8) . . ?
C30 C31 H31 121.2 . . ?
C32 C31 H31 121.2 . . ?
C31 C32 C33 121.1(8) . . ?
C31 C32 C37 120.4(10) . . ?
C33 C32 C37 118.5(10) . . ?
C29 C33 C32 120.4(9) . . ?
C29 C33 C34 119.7(9) . . ?
C32 C33 C34 119.9(8) . . ?
C35 C34 C33 119.4(10) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C34 C35 C36 121.0(10) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
C37 C36 C35 121.2(10) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 C32 119.9(11) . . ?
C36 C37 H37 120.0 . . ?
C32 C37 H37 120.0 . . ?
O1 C38 Re1 177.4(7) . . ?
O3 C39 Re1 178.9(9) . . ?
O2 C40 Re1 177.6(8) . . ?
O5 C41 C45 126.8(8) . . ?
O5 C41 C42 115.0(7) . . ?
C45 C41 C42 118.1(8) . . ?
C43 C42 C41 122.6(8) . . ?
C43 C42 H42 118.7 . . ?
C41 C42 H42 118.7 . . ?
C42 C43 C44 122.0(8) . . ?
C42 C43 H43 119.0 . . ?
C44 C43 H43 119.0 . . ?
O7 C44 C46 127.2(7) . . ?
O7 C44 C43 115.0(7) . . ?
C46 C44 C43 117.8(8) . . ?
C50 C45 C41 120.8(8) . . ?
C50 C45 C46 120.1(7) . . ?
C41 C45 C46 119.1(7) . . ?
C44 C46 C47 120.3(7) . . ?
C44 C46 C45 120.3(7) . . ?
C47 C46 C45 119.2(7) . . ?
O6 C47 C46 124.3(7) . . ?
O6 C47 C48 116.3(7) . . ?
C46 C47 C48 119.4(7) . . ?
C49 C48 C54 119.8(8) . . ?
C49 C48 C47 120.2(7) . . ?
C54 C48 C47 120.0(8) . . ?
C51 C49 C48 119.4(7) . . ?
C51 C49 C50 120.4(8) . . ?
C48 C49 C50 120.2(7) . . ?
O4 C50 C45 125.4(7) . . ?
O4 C50 C49 115.4(7) . . ?
C45 C50 C49 119.2(7) . . ?
C52 C51 C49 121.0(8) . . ?
C52 C51 H51 119.5 . . ?
C49 C51 H51 119.5 . . ?
C51 C52 C53 119.3(8) . . ?
C51 C52 H52 120.4 . . ?
C53 C52 H52 120.4 . . ?
C54 C53 C52 120.9(8) . . ?
C54 C53 H53 119.6 . . ?
C52 C53 H53 119.6 . . ?
C53 C54 C48 119.6(8) . . ?
C53 C54 H54 120.2 . . ?
C48 C54 H54 120.2 . . ?
O8 C55 Re2 178.5(7) . . ?
O10 C56 Re2 176.5(7) . . ?
O9 C57 Re2 179.7(8) . . ?
C59 C58 H58A 109.5 . . ?
C59 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C59 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C58 C59 C60 117(2) . . ?
C58 C59 C64 127(2) . . ?
C60 C59 C64 115.9(16) . . ?
C61 C60 C59 117.6(16) . . ?
C61 C60 H60 121.2 . . ?
C59 C60 H60 121.2 . . ?
C60 C61 C62 126.7(18) . . ?
C60 C61 H61 116.6 . . ?
C62 C61 H61 116.6 . . ?
C63 C62 C61 113.7(19) . . ?
C63 C62 H62 123.2 . . ?
C61 C62 H62 123.2 . . ?
C62 C63 C64 125.9(18) . . ?
C62 C63 H63 117.1 . . ?
C64 C63 H63 117.1 . . ?
C63 C64 C59 120.0(15) . . ?
C63 C64 H64 120.0 . . ?
C59 C64 H64 120.0 . . ?
C11 N1 C10 106.6(7) . . ?
C11 N1 C12 127.0(7) . . ?
C10 N1 C12 126.4(7) . . ?
C11 N2 C9 106.0(7) . . ?
C11 N2 Re2 126.5(5) . . ?
C9 N2 Re2 126.8(6) . . ?
C28 N3 C30 107.6(7) . . ?
C28 N3 C26 126.5(8) . . ?
C30 N3 C26 125.8(8) . . ?
C28 N4 C27 104.7(7) . . ?
C28 N4 Re1 127.1(6) . . ?
C27 N4 Re1 128.0(6) . . ?
C50 O4 Re1 132.3(5) . . ?
C41 O5 Re1 128.9(5) . . ?
C47 O6 Re2 131.0(5) . . ?
C44 O7 Re2 127.1(5) . . ?
C40 Re1 C39 86.7(4) . . ?
C40 Re1 C38 88.2(4) . . ?
C39 Re1 C38 87.7(4) . . ?
C40 Re1 O5 175.1(3) . . ?
C39 Re1 O5 98.0(3) . . ?
C38 Re1 O5 92.8(3) . . ?
C40 Re1 O4 93.1(3) . . ?
C39 Re1 O4 175.2(3) . . ?
C38 Re1 O4 97.1(3) . . ?
O5 Re1 O4 82.1(2) . . ?
C40 Re1 N4 97.3(3) . . ?
C39 Re1 N4 93.3(3) . . ?
C38 Re1 N4 174.4(3) . . ?
O5 Re1 N4 81.6(3) . . ?
O4 Re1 N4 82.0(2) . . ?
C56 Re2 C55 88.0(4) . . ?
C56 Re2 C57 88.0(4) . . ?
C55 Re2 C57 90.8(3) . . ?
C56 Re2 O7 94.0(3) . . ?
C55 Re2 O7 91.6(3) . . ?
C57 Re2 O7 177.0(3) . . ?
C56 Re2 O6 175.6(3) . . ?
C55 Re2 O6 93.2(3) . . ?
C57 Re2 O6 96.2(3) . . ?
O7 Re2 O6 81.8(2) . . ?
C56 Re2 N2 96.6(3) . . ?
C55 Re2 N2 173.4(3) . . ?
C57 Re2 N2 94.2(3) . . ?
O7 Re2 N2 83.3(2) . . ?
O6 Re2 N2 81.9(2) . . ?
C67 C66 C68 150(3) . . ?
C68 C65 C67 83(3) 2_556 . ?
C66 C67 C65 122(2) . . ?
C66 C68 C65 176(5) . 2_556 ?

_refine_diff_density_max         7.201
_refine_diff_density_min         -2.090
_refine_diff_density_rms         0.207

