# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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data_2017_11_27_dt_js-375_n
_database_code_depnum_ccdc_archive 'CCDC 1867809'
_audit_update_record             
;
2018-09-14 deposited with the CCDC.
2018-11-23 downloaded from the CCDC.
;
_audit_creation_date             2018-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H15 N2 O7 Re'
_chemical_formula_sum            'C24 H15 N2 O7 Re'
_chemical_formula_weight         629.58
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
_chemical_oxdiff_usercomment     ?
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'

_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.
;
_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'
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                   10.7471(3)
_cell_length_b                   12.2015(3)
_cell_length_c                   16.6996(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.127(2)
_cell_angle_gamma                90
_cell_volume                     2188.32(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1510
_cell_measurement_theta_min      2.3100
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.603
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20546
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.068
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      ?
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0246823000
_diffrn_orient_matrix_UB_12      -0.0058170000
_diffrn_orient_matrix_UB_13      0.0385094000
_diffrn_orient_matrix_UB_21      0.0505806000
_diffrn_orient_matrix_UB_22      0.0307688000
_diffrn_orient_matrix_UB_23      0.0168414000
_diffrn_orient_matrix_UB_31      -0.0348626000
_diffrn_orient_matrix_UB_32      0.0488972000
_diffrn_orient_matrix_UB_33      -0.0059752000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5710
_reflns_number_total             6698
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.187
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6698
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0254
_refine_ls_restrained_S_all      1.084
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0172P)²+2.5677P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0555
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H,H,H,H) groups
2. Restrained distances
 C18-O6B \\sim O6B-O6A
 with sigma of 0.02
 O6B-C23B \\sim O6A-C23A
 with sigma of 0.02
 C23B-C24 \\sim C24-C23A
 with sigma of 0.02
 C23B-O7B \\sim C23A-O7A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C23B) \\sim Ueq, Uanis(O6B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Others
 Sof(C23B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(O6B)=Sof(O7B)=1-FVAR(1)
 Sof(C23A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(O6A)=Sof(O7A)=FVAR(1)
5.a Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C24(H24D,H24E,H24F)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C22(H22)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.5630(3) 0.2012(3) 0.18147(17) 0.0237(7) Uani 1 1 d . . . . .
C2 C 0.4710(3) 0.3970(2) 0.13579(16) 0.0168(6) Uani 1 1 d . . . . .
C3 C 0.7095(3) 0.3820(2) 0.18305(17) 0.0197(6) Uani 1 1 d . . . . .
C4 C 0.6709(3) 0.1929(2) 0.36892(18) 0.0205(6) Uani 1 1 d . . . . .
H4 H 0.6693 0.1373 0.3308 0.025 Uiso 1 1 calc R . . . .
C5 C 0.7079(3) 0.1672(3) 0.44751(18) 0.0236(7) Uani 1 1 d . . . . .
H5 H 0.7278 0.0953 0.4613 0.028 Uiso 1 1 calc R . . . .
C6 C 0.7150(3) 0.2481(3) 0.50443(17) 0.0236(7) Uani 1 1 d . . . . .
H6 H 0.7392 0.2317 0.5571 0.028 Uiso 1 1 calc R . . . .
C7 C 0.6849(3) 0.3562(3) 0.48203(16) 0.0196(6) Uani 1 1 d . . . . .
C8 C 0.6933(3) 0.4484(3) 0.53592(17) 0.0257(7) Uani 1 1 d . . . . .
H8 H 0.7199 0.4374 0.5889 0.031 Uiso 1 1 calc R . . . .
C9 C 0.6632(3) 0.5505(3) 0.51086(18) 0.0273(7) Uani 1 1 d . . . . .
H9 H 0.6715 0.6088 0.5465 0.033 Uiso 1 1 calc R . . . .
C10 C 0.6188(3) 0.5703(3) 0.43026(18) 0.0220(6) Uani 1 1 d . . . . .
C11 C 0.5831(3) 0.6743(3) 0.4014(2) 0.0268(7) Uani 1 1 d . . . . .
H11 H 0.5908 0.7356 0.4344 0.032 Uiso 1 1 calc R . . . .
C12 C 0.5372(3) 0.6846(3) 0.3246(2) 0.0280(7) Uani 1 1 d . . . . .
H12 H 0.5132 0.7530 0.3050 0.034 Uiso 1 1 calc R . . . .
C13 C 0.5262(3) 0.5926(3) 0.27549(18) 0.0232(6) Uani 1 1 d . . . . .
H13 H 0.4928 0.6008 0.2237 0.028 Uiso 1 1 calc R . . . .
C14 C 0.6076(3) 0.4818(2) 0.37667(15) 0.0154(5) Uani 1 1 d . . . . .
C15 C 0.6442(3) 0.3748(2) 0.40234(16) 0.0167(6) Uani 1 1 d . . . . .
C16 C 0.2841(3) 0.2991(2) 0.26743(15) 0.0143(5) Uani 1 1 d . . . . .
C17 C 0.1884(3) 0.2921(2) 0.33142(15) 0.0141(5) Uani 1 1 d . . . . .
C18 C 0.1876(3) 0.2032(3) 0.38188(19) 0.0230(7) Uani 1 1 d D . . . .
C19 C 0.1063(3) 0.1973(3) 0.44444(19) 0.0245(7) Uani 1 1 d . . . . .
H19 H 0.1063 0.1360 0.4776 0.029 Uiso 1 1 calc R . . . .
C20 C 0.0252(3) 0.2831(3) 0.45708(17) 0.0210(6) Uani 1 1 d . . . . .
H20 H -0.0274 0.2810 0.5000 0.025 Uiso 1 1 calc R . . . .
C21 C 0.0226(3) 0.3720(3) 0.40559(18) 0.0235(7) Uani 1 1 d . . . . .
H21 H -0.0334 0.4289 0.4129 0.028 Uiso 1 1 calc R . . . .
C22 C 0.1039(3) 0.3760(3) 0.34284(17) 0.0216(6) Uani 1 1 d . . . . .
H22 H 0.1017 0.4357 0.3081 0.026 Uiso 1 1 calc R . . . .
C23A C 0.3531(4) 0.0843(3) 0.41058(19) 0.0193(8) Uani 0.843(4) 1 d D . P A 1
C23B C 0.3210(16) 0.0722(13) 0.3516(8) 0.017(4) Uani 0.157(4) 1 d D U P A 2
C24 C 0.4255(3) -0.0096(3) 0.37720(18) 0.0235(7) Uani 1 1 d D . . . .
H24A H 0.3892 -0.0305 0.3261 0.035 Uiso 0.843(4) 1 calc R . P A 1
H24B H 0.5103 0.0126 0.3709 0.035 Uiso 0.843(4) 1 calc R . P A 1
H24C H 0.4233 -0.0707 0.4133 0.035 Uiso 0.843(4) 1 calc R . P A 1
H24D H 0.4595 0.0104 0.4291 0.035 Uiso 0.157(4) 1 calc R . P A 2
H24E H 0.3918 -0.0823 0.3793 0.035 Uiso 0.157(4) 1 calc R . P A 2
H24F H 0.4901 -0.0074 0.3390 0.035 Uiso 0.157(4) 1 calc R . P A 2
N1 N 0.6376(2) 0.29366(19) 0.34612(13) 0.0148(5) Uani 1 1 d . . . . .
N2 N 0.5617(2) 0.49352(19) 0.30011(13) 0.0157(5) Uani 1 1 d . . . . .
O1 O 0.5704(3) 0.1150(2) 0.15489(14) 0.0415(7) Uani 1 1 d . . . . .
O2 O 0.4224(2) 0.43025(18) 0.07805(11) 0.0235(5) Uani 1 1 d . . . . .
O3 O 0.7999(2) 0.41115(19) 0.15417(15) 0.0333(6) Uani 1 1 d . . . . .
O4 O 0.3954(2) 0.31550(18) 0.29693(11) 0.0196(4) Uani 1 1 d . . . . .
O5 O 0.2540(2) 0.2907(2) 0.19661(12) 0.0274(5) Uani 1 1 d . . . . .
O6A O 0.2594(2) 0.1130(2) 0.35866(13) 0.0173(6) Uani 0.843(4) 1 d D . P A 1
O6B O 0.2966(14) 0.1503(10) 0.4125(7) 0.021(3) Uani 0.157(4) 1 d D U P A 2
O7A O 0.3745(3) 0.1289(3) 0.47303(17) 0.0389(9) Uani 0.843(4) 1 d D . P A 1
O7B O 0.2616(13) 0.0660(11) 0.2877(7) 0.021(3) Uani 0.157(4) 1 d D . P A 2
Re1 Re 0.55734(2) 0.34301(2) 0.23030(2) 0.01306(4) 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
C1 O1 1.147(4) . ?
C1 Re1 1.914(3) . ?
C2 O2 1.153(3) . ?
C2 Re1 1.918(3) . ?
C3 O3 1.157(4) . ?
C3 Re1 1.903(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(4) . ?
C4 N1 1.332(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.370(4) . ?
C6 H6 0.9300 . ?
C6 C7 1.405(4) . ?
C7 C8 1.442(4) . ?
C7 C15 1.404(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.349(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.432(4) . ?
C10 C11 1.406(5) . ?
C10 C14 1.405(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.362(5) . ?
C12 H12 0.9300 . ?
C12 C13 1.392(4) . ?
C13 H13 0.9300 . ?
C13 N2 1.329(4) . ?
C14 C15 1.425(4) . ?
C14 N2 1.360(3) . ?
C15 N1 1.365(3) . ?
C16 C17 1.513(4) . ?
C16 O4 1.292(3) . ?
C16 O5 1.219(3) . ?
C17 C18 1.374(4) . ?
C17 C22 1.386(4) . ?
C18 C19 1.388(4) . ?
C18 O6A 1.407(4) . ?
C18 O6B 1.416(14) . ?
C19 H19 0.9300 . ?
C19 C20 1.383(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.384(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.390(4) . ?
C22 H22 0.9300 . ?
C23A C24 1.503(5) . ?
C23A O6A 1.350(4) . ?
C23A O7A 1.192(4) . ?
C23B C24 1.551(14) . ?
C23B O6B 1.426(14) . ?
C23B O7B 1.225(14) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24 H24D 0.9600 . ?
C24 H24E 0.9600 . ?
C24 H24F 0.9600 . ?
N1 Re1 2.173(2) . ?
N2 Re1 2.175(2) . ?
O4 Re1 2.127(2) . ?

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
O1 C1 Re1 176.9(3) . . ?
O2 C2 Re1 178.0(3) . . ?
O3 C3 Re1 176.5(3) . . ?
C5 C4 H4 118.6 . . ?
N1 C4 H4 118.6 . . ?
N1 C4 C5 122.8(3) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 120.5 . . ?
C5 C6 C7 119.0(3) . . ?
C7 C6 H6 120.5 . . ?
C6 C7 C8 123.9(3) . . ?
C15 C7 C6 117.7(3) . . ?
C15 C7 C8 118.4(3) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 C7 121.2(3) . . ?
C9 C8 H8 119.4 . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 121.0(3) . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 123.6(3) . . ?
C14 C10 C9 119.1(3) . . ?
C14 C10 C11 117.3(3) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.4(3) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.0(3) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 118.9 . . ?
N2 C13 C12 122.3(3) . . ?
N2 C13 H13 118.9 . . ?
C10 C14 C15 119.8(3) . . ?
N2 C14 C10 122.5(3) . . ?
N2 C14 C15 117.7(2) . . ?
C7 C15 C14 120.4(3) . . ?
N1 C15 C7 122.8(3) . . ?
N1 C15 C14 116.8(2) . . ?
O4 C16 C17 112.5(2) . . ?
O5 C16 C17 121.1(3) . . ?
O5 C16 O4 126.3(3) . . ?
C18 C17 C16 119.9(3) . . ?
C18 C17 C22 118.7(3) . . ?
C22 C17 C16 121.4(2) . . ?
C17 C18 C19 121.4(3) . . ?
C17 C18 O6A 115.6(3) . . ?
C17 C18 O6B 123.9(6) . . ?
C19 C18 O6A 122.3(3) . . ?
C19 C18 O6B 103.9(6) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.5(3) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 120.1 . . ?
C19 C20 C21 119.8(3) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C22 119.8(3) . . ?
C22 C21 H21 120.1 . . ?
C17 C22 C21 120.7(3) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
O6A C23A C24 110.1(3) . . ?
O7A C23A C24 125.9(4) . . ?
O7A C23A O6A 123.9(3) . . ?
O6B C23B C24 112.6(10) . . ?
O7B C23B C24 123.3(12) . . ?
O7B C23B O6B 124.0(14) . . ?
C23A C24 H24A 109.5 . . ?
C23A C24 H24B 109.5 . . ?
C23A C24 H24C 109.5 . . ?
C23B C24 H24D 109.5 . . ?
C23B C24 H24E 109.5 . . ?
C23B C24 H24F 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H24D C24 H24E 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
C4 N1 C15 117.8(2) . . ?
C4 N1 Re1 127.12(19) . . ?
C15 N1 Re1 114.84(19) . . ?
C13 N2 C14 118.4(2) . . ?
C13 N2 Re1 127.03(19) . . ?
C14 N2 Re1 114.54(18) . . ?
C16 O4 Re1 126.06(17) . . ?
C23A O6A C18 115.5(3) . . ?
C18 O6B C23B 102.6(10) . . ?
C1 Re1 C2 88.98(13) . . ?
C1 Re1 N1 96.37(11) . . ?
C1 Re1 N2 172.29(11) . . ?
C1 Re1 O4 96.89(11) . . ?
C2 Re1 N1 172.54(10) . . ?
C2 Re1 N2 98.69(10) . . ?
C2 Re1 O4 96.00(10) . . ?
C3 Re1 C1 90.44(13) . . ?
C3 Re1 C2 88.27(13) . . ?
C3 Re1 N1 96.86(11) . . ?
C3 Re1 N2 90.53(11) . . ?
C3 Re1 O4 171.56(10) . . ?
N1 Re1 N2 75.93(9) . . ?
O4 Re1 N1 78.24(8) . . ?
O4 Re1 N2 81.65(9) . . ?

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
C4 C5 C6 C7 -0.3(5) . . . . ?
C5 C4 N1 C15 2.0(5) . . . . ?
C5 C4 N1 Re1 -172.2(2) . . . . ?
C5 C6 C7 C8 -177.7(3) . . . . ?
C5 C6 C7 C15 2.5(5) . . . . ?
C6 C7 C8 C9 180.0(3) . . . . ?
C6 C7 C15 C14 177.5(3) . . . . ?
C6 C7 C15 N1 -2.7(5) . . . . ?
C7 C8 C9 C10 1.6(5) . . . . ?
C7 C15 N1 C4 0.4(4) . . . . ?
C7 C15 N1 Re1 175.3(2) . . . . ?
C8 C7 C15 C14 -2.4(4) . . . . ?
C8 C7 C15 N1 177.5(3) . . . . ?
C8 C9 C10 C11 178.3(3) . . . . ?
C8 C9 C10 C14 -0.5(5) . . . . ?
C9 C10 C11 C12 -177.4(3) . . . . ?
C9 C10 C14 C15 -2.0(5) . . . . ?
C9 C10 C14 N2 177.5(3) . . . . ?
C10 C11 C12 C13 -0.1(5) . . . . ?
C10 C14 C15 C7 3.5(4) . . . . ?
C10 C14 C15 N1 -176.4(3) . . . . ?
C10 C14 N2 C13 -0.1(4) . . . . ?
C10 C14 N2 Re1 179.2(2) . . . . ?
C11 C10 C14 C15 179.0(3) . . . . ?
C11 C10 C14 N2 -1.4(5) . . . . ?
C11 C12 C13 N2 -1.5(5) . . . . ?
C12 C13 N2 C14 1.6(5) . . . . ?
C12 C13 N2 Re1 -177.6(2) . . . . ?
C14 C10 C11 C12 1.5(5) . . . . ?
C14 C15 N1 C4 -179.7(3) . . . . ?
C14 C15 N1 Re1 -4.8(3) . . . . ?
C15 C7 C8 C9 -0.2(5) . . . . ?
C15 C14 N2 C13 179.4(3) . . . . ?
C15 C14 N2 Re1 -1.2(3) . . . . ?
C16 C17 C18 C19 175.9(3) . . . . ?
C16 C17 C18 O6A -13.6(4) . . . . ?
C16 C17 C18 O6B 37.5(7) . . . . ?
C16 C17 C22 C21 -175.3(3) . . . . ?
C17 C16 O4 Re1 -175.04(17) . . . . ?
C17 C18 C19 C20 -0.8(5) . . . . ?
C17 C18 O6A C23A 118.8(3) . . . . ?
C17 C18 O6B C23B -87.4(11) . . . . ?
C18 C17 C22 C21 2.0(5) . . . . ?
C18 C19 C20 C21 2.4(5) . . . . ?
C19 C18 O6A C23A -70.8(4) . . . . ?
C19 C18 O6B C23B 128.3(10) . . . . ?
C19 C20 C21 C22 -1.8(5) . . . . ?
C20 C21 C22 C17 -0.4(5) . . . . ?
C22 C17 C18 C19 -1.4(5) . . . . ?
C22 C17 C18 O6A 169.2(3) . . . . ?
C22 C17 C18 O6B -139.8(6) . . . . ?
C24 C23A O6A C18 -177.6(3) . . . . ?
C24 C23B O6B C18 -171.0(10) . . . . ?
N1 C4 C5 C6 -2.1(5) . . . . ?
N2 C14 C15 C7 -176.1(3) . . . . ?
N2 C14 C15 N1 4.1(4) . . . . ?
O4 C16 C17 C18 -69.9(3) . . . . ?
O4 C16 C17 C22 107.3(3) . . . . ?
O5 C16 C17 C18 110.8(3) . . . . ?
O5 C16 C17 C22 -72.0(4) . . . . ?
O5 C16 O4 Re1 4.2(4) . . . . ?
O6A C18 C19 C20 -170.7(3) . . . . ?
O6B C18 C19 C20 144.6(6) . . . . ?
O7A C23A O6A C18 1.5(5) . . . . ?
O7B C23B O6B C18 5(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.259
_oxdiff_exptl_absorpt_empirical_full_min 0.683

####################################################################### 
# 
# 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_2017_11_27_dt_js-376_n
_database_code_depnum_ccdc_archive 'CCDC 1867810'
_audit_update_record             
;
2018-09-14 deposited with the CCDC.
2018-11-23 downloaded from the CCDC.
;
_audit_creation_date             2018-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H25 N2 O5 Re'
_chemical_formula_sum            'C28 H25 N2 O5 Re'
_chemical_formula_weight         655.70
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C28 H25 N2 O5 Re'
_chemical_oxdiff_usercomment     ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'

_cell_length_a                   17.8677(5)
_cell_length_b                   12.9186(4)
_cell_length_c                   10.7310(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2477.00(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6340
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.7970
_cell_measurement_theta_min      1.9640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.948
_exptl_absorpt_correction_T_max  0.653
_exptl_absorpt_correction_T_min  0.338
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13281
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         1.898
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0026
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      ?
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0327950000
_diffrn_orient_matrix_UB_12      0.0305121000
_diffrn_orient_matrix_UB_13      -0.0057781000
_diffrn_orient_matrix_UB_21      0.0200538000
_diffrn_orient_matrix_UB_22      0.0440353000
_diffrn_orient_matrix_UB_23      0.0209764000
_diffrn_orient_matrix_UB_31      0.0098578000
_diffrn_orient_matrix_UB_32      0.0119927000
_diffrn_orient_matrix_UB_33      -0.0624452000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6959
_reflns_number_total             7563
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43c (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.488
_refine_diff_density_min         -1.760
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 
;
 Flack x determined using 2629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7563
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0443
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0150P)²+2.5982P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0795
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(1)
 Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C17(H17), C25A(H25A), C25B(H25B)
4.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C24(H24C,H24D)
4.c Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C27(H27D,H27E,H27F)
4.d Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C22(H22), C23(H23)
4.e Idealised Me refined as rotating group:
 C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.5714(5) 0.8249(7) 0.6928(8) 0.030(2) Uani 1 1 d . . . . .
C2 C 0.5394(5) 0.6442(8) 0.7973(10) 0.039(3) Uani 1 1 d . . . . .
C3 C 0.6499(4) 0.7553(6) 0.8904(7) 0.0176(16) Uani 1 1 d . . . . .
C4 C 0.7475(5) 0.8482(7) 0.5952(7) 0.0233(18) Uani 1 1 d . . . . .
H4 H 0.7114 0.8998 0.6023 0.028 Uiso 1 1 calc R . . . .
C5 C 0.8145(5) 0.8714(7) 0.5355(7) 0.0258(19) Uani 1 1 d . . . . .
H5 H 0.8227 0.9374 0.5037 0.031 Uiso 1 1 calc R . . . .
C6 C 0.8680(5) 0.7970(7) 0.5239(6) 0.0275(17) Uani 1 1 d . . . . .
H6 H 0.9128 0.8120 0.4835 0.033 Uiso 1 1 calc R . . . .
C7 C 0.8556(4) 0.6970(8) 0.5730(6) 0.0207(16) Uani 1 1 d . . . . .
C8 C 0.9075(5) 0.6133(8) 0.5641(8) 0.0266(19) Uani 1 1 d . . . . .
H8 H 0.9531 0.6242 0.5242 0.032 Uiso 1 1 calc R . . . .
C9 C 0.8928(5) 0.5194(7) 0.6113(8) 0.029(2) Uani 1 1 d . . . . .
H9 H 0.9275 0.4662 0.6028 0.035 Uiso 1 1 calc R . . . .
C10 C 0.8228(4) 0.5008(7) 0.6754(7) 0.0221(17) Uani 1 1 d . . . . .
C11 C 0.8053(4) 0.4059(6) 0.7308(8) 0.0261(17) Uani 1 1 d . . . . .
H11 H 0.8390 0.3511 0.7271 0.031 Uiso 1 1 calc R . . . .
C12 C 0.7381(5) 0.3944(6) 0.7904(7) 0.0241(18) Uani 1 1 d . . . . .
H12 H 0.7260 0.3317 0.8281 0.029 Uiso 1 1 calc R . . . .
C13 C 0.6872(5) 0.4777(6) 0.7944(7) 0.0220(17) Uani 1 1 d . . . . .
H13 H 0.6417 0.4690 0.8352 0.026 Uiso 1 1 calc R . . . .
C14 C 0.7697(4) 0.5799(6) 0.6829(7) 0.0170(15) Uani 1 1 d . . . . .
C15 C 0.7858(4) 0.6799(6) 0.6307(6) 0.0157(15) Uani 1 1 d . . . . .
C16 C 0.5911(4) 0.6722(6) 0.4496(7) 0.0184(17) Uani 1 1 d . . . . .
C17 C 0.5873(4) 0.6020(6) 0.3362(7) 0.0181(16) Uani 1 1 d . . . . .
H17 H 0.5684 0.5346 0.3642 0.022 Uiso 1 1 calc R . . . .
C18 C 0.6650(4) 0.5842(6) 0.2794(8) 0.0182(15) Uani 1 1 d . . . . .
C19 C 0.6740(5) 0.5178(7) 0.1780(7) 0.0264(18) Uani 1 1 d . . . . .
H19 H 0.6332 0.4801 0.1492 0.032 Uiso 1 1 calc R . . . .
C20 C 0.7427(5) 0.5069(7) 0.1195(7) 0.0236(18) Uani 1 1 d . . . . .
H20 H 0.7470 0.4623 0.0518 0.028 Uiso 1 1 calc R . . . .
C21 C 0.8052(4) 0.5612(6) 0.1600(7) 0.0191(16) Uani 1 1 d . . . . .
C22 C 0.7966(4) 0.6242(6) 0.2632(8) 0.0250(17) Uani 1 1 d . . . . .
H22 H 0.8380 0.6592 0.2944 0.030 Uiso 1 1 calc R . . . .
C23 C 0.7277(4) 0.6367(7) 0.3216(8) 0.0222(17) Uani 1 1 d . . . . .
H23 H 0.7236 0.6807 0.3898 0.027 Uiso 1 1 calc R . . . .
C24 C 0.8789(5) 0.5568(6) 0.0922(7) 0.0239(17) Uani 1 1 d . . . . .
H24A H 0.9172 0.5302 0.1477 0.029 Uiso 0.685(14) 1 calc R . P A 1
H24B H 0.8748 0.5100 0.0218 0.029 Uiso 0.685(14) 1 calc R . P A 1
H24C H 0.8921 0.4845 0.0819 0.029 Uiso 0.315(14) 1 calc R . P A 2
H24D H 0.9165 0.5877 0.1457 0.029 Uiso 0.315(14) 1 calc R . P A 2
C25A C 0.9009(6) 0.6614(9) 0.0474(10) 0.016(3) Uani 0.685(14) 1 d . . P A 1
H25A H 0.9050 0.7063 0.1206 0.019 Uiso 0.685(14) 1 calc R . P A 1
C25B C 0.8849(15) 0.612(2) -0.043(2) 0.031(8) Uani 0.315(14) 1 d . . P A 2
H25B H 0.8527 0.5697 -0.0968 0.037 Uiso 0.315(14) 1 calc R . P A 2
C26A C 0.9790(7) 0.6544(12) -0.0122(13) 0.032(3) Uani 0.685(14) 1 d . . P A 1
H26A H 1.0129 0.6216 0.0448 0.048 Uiso 0.685(14) 1 calc GR . P A 1
H26B H 0.9968 0.7228 -0.0311 0.048 Uiso 0.685(14) 1 calc GR . P A 1
H26C H 0.9762 0.6146 -0.0875 0.048 Uiso 0.685(14) 1 calc GR . P A 1
C26B C 0.9632(19) 0.601(3) -0.100(3) 0.041(9) Uani 0.315(14) 1 d . . P A 2
H26D H 0.9963 0.6505 -0.0617 0.061 Uiso 0.315(14) 1 calc GR . P A 2
H26E H 0.9606 0.6145 -0.1879 0.061 Uiso 0.315(14) 1 calc GR . P A 2
H26F H 0.9818 0.5326 -0.0861 0.061 Uiso 0.315(14) 1 calc GR . P A 2
C27 C 0.8500(6) 0.7127(9) -0.0418(8) 0.042(3) Uani 1 1 d . . . . .
H27A H 0.8699 0.7792 -0.0639 0.063 Uiso 0.685(14) 1 calc R . P A 1
H27B H 0.8453 0.6708 -0.1153 0.063 Uiso 0.685(14) 1 calc R . P A 1
H27C H 0.8016 0.7213 -0.0041 0.063 Uiso 0.685(14) 1 calc R . P A 1
H27D H 0.8015 0.7079 -0.0036 0.063 Uiso 0.315(14) 1 calc R . P A 2
H27E H 0.8806 0.7601 0.0046 0.063 Uiso 0.315(14) 1 calc R . P A 2
H27F H 0.8446 0.7371 -0.1258 0.063 Uiso 0.315(14) 1 calc R . P A 2
C28 C 0.5322(5) 0.6434(7) 0.2383(9) 0.030(2) Uani 1 1 d . . . . .
H28A H 0.5495 0.7091 0.2080 0.045 Uiso 1 1 calc GR . . . .
H28B H 0.4837 0.6517 0.2754 0.045 Uiso 1 1 calc GR . . . .
H28C H 0.5290 0.5954 0.1703 0.045 Uiso 1 1 calc GR . . . .
N1 N 0.7331(3) 0.7552(5) 0.6424(5) 0.0148(13) Uani 1 1 d . . . . .
N2 N 0.7025(3) 0.5690(4) 0.7414(6) 0.0162(13) Uani 1 1 d . . . . .
O1 O 0.5381(4) 0.8995(6) 0.6754(6) 0.045(2) Uani 1 1 d . . . . .
O2 O 0.4848(4) 0.6131(7) 0.8419(9) 0.068(3) Uani 1 1 d . U . . .
O3 O 0.6603(3) 0.7856(5) 0.9898(5) 0.0284(14) Uani 1 1 d . . . . .
O4 O 0.6132(3) 0.6263(4) 0.5501(5) 0.0224(12) Uani 1 1 d . . . . .
O5 O 0.5749(3) 0.7642(5) 0.4413(5) 0.0275(14) Uani 1 1 d . . . . .
Re1 Re 0.62828(2) 0.70150(2) 0.72720(3) 0.01835(7) 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
C1 O1 1.148(10) . ?
C1 Re1 1.926(9) . ?
C2 O2 1.158(11) . ?
C2 Re1 1.907(9) . ?
C3 O3 1.151(9) . ?
C3 Re1 1.923(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.390(12) . ?
C4 N1 1.330(10) . ?
C5 H5 0.9300 . ?
C5 C6 1.361(12) . ?
C6 H6 0.9300 . ?
C6 C7 1.413(12) . ?
C7 C8 1.429(12) . ?
C7 C15 1.411(10) . ?
C8 H8 0.9300 . ?
C8 C9 1.340(12) . ?
C9 H9 0.9300 . ?
C9 C10 1.447(11) . ?
C10 C11 1.397(12) . ?
C10 C14 1.397(11) . ?
C11 H11 0.9300 . ?
C11 C12 1.369(11) . ?
C12 H12 0.9300 . ?
C12 C13 1.409(11) . ?
C13 H13 0.9300 . ?
C13 N2 1.338(10) . ?
C14 C15 1.436(10) . ?
C14 N2 1.364(9) . ?
C15 N1 1.360(9) . ?
C16 C17 1.520(10) . ?
C16 O4 1.292(9) . ?
C16 O5 1.226(10) . ?
C17 H17 0.9800 . ?
C17 C18 1.535(10) . ?
C17 C28 1.536(11) . ?
C18 C19 1.395(11) . ?
C18 C23 1.384(11) . ?
C19 H19 0.9300 . ?
C19 C20 1.385(12) . ?
C20 H20 0.9300 . ?
C20 C21 1.389(11) . ?
C21 C22 1.383(10) . ?
C21 C24 1.505(11) . ?
C22 H22 0.9300 . ?
C22 C23 1.391(11) . ?
C23 H23 0.9300 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C24 H24D 0.9700 . ?
C24 C25A 1.487(13) . ?
C24 C25B 1.62(3) . ?
C25A H25A 0.9800 . ?
C25A C26A 1.538(16) . ?
C25A C27 1.478(14) . ?
C25B H25B 0.9800 . ?
C25B C26B 1.53(4) . ?
C25B C27 1.45(3) . ?
C26A H26A 0.9600 . ?
C26A H26B 0.9600 . ?
C26A H26C 0.9600 . ?
C26B H26D 0.9600 . ?
C26B H26E 0.9600 . ?
C26B H26F 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27 H27D 0.9600 . ?
C27 H27E 0.9600 . ?
C27 H27F 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
N1 Re1 2.194(6) . ?
N2 Re1 2.170(6) . ?
O4 Re1 2.152(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
O1 C1 Re1 178.1(7) . . ?
O2 C2 Re1 177.3(8) . . ?
O3 C3 Re1 177.2(7) . . ?
C5 C4 H4 118.8 . . ?
N1 C4 H4 118.8 . . ?
N1 C4 C5 122.5(8) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.7(8) . . ?
C6 C5 H5 120.1 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.1(8) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 C8 124.5(7) . . ?
C15 C7 C6 116.5(8) . . ?
C15 C7 C8 119.0(8) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 C7 122.2(8) . . ?
C9 C8 H8 118.9 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0(8) . . ?
C10 C9 H9 120.0 . . ?
C11 C10 C9 122.8(8) . . ?
C14 C10 C9 119.5(8) . . ?
C14 C10 C11 117.7(8) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.4(8) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 120.1 . . ?
C11 C12 C13 119.8(8) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 119.0 . . ?
N2 C13 C12 122.0(7) . . ?
N2 C13 H13 119.0 . . ?
C10 C14 C15 120.0(7) . . ?
N2 C14 C10 123.3(7) . . ?
N2 C14 C15 116.6(7) . . ?
C7 C15 C14 119.3(7) . . ?
N1 C15 C7 122.7(7) . . ?
N1 C15 C14 118.0(7) . . ?
O4 C16 C17 114.0(7) . . ?
O5 C16 C17 120.6(7) . . ?
O5 C16 O4 125.3(8) . . ?
C16 C17 H17 107.4 . . ?
C16 C17 C18 111.5(6) . . ?
C16 C17 C28 111.6(7) . . ?
C18 C17 H17 107.4 . . ?
C18 C17 C28 111.1(6) . . ?
C28 C17 H17 107.4 . . ?
C19 C18 C17 120.4(7) . . ?
C23 C18 C17 121.9(7) . . ?
C23 C18 C19 117.6(7) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 C18 121.2(8) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 119.3 . . ?
C19 C20 C21 121.3(7) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 C24 122.2(7) . . ?
C22 C21 C20 117.2(7) . . ?
C22 C21 C24 120.5(7) . . ?
C21 C22 H22 119.1 . . ?
C21 C22 C23 121.8(8) . . ?
C23 C22 H22 119.1 . . ?
C18 C23 C22 120.8(8) . . ?
C18 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
C21 C24 H24C 107.7 . . ?
C21 C24 H24D 107.7 . . ?
C21 C24 C25B 118.3(11) . . ?
H24A C24 H24B 108.1 . . ?
H24C C24 H24D 107.1 . . ?
C25A C24 C21 110.7(7) . . ?
C25A C24 H24A 109.5 . . ?
C25A C24 H24B 109.5 . . ?
C25B C24 H24C 107.7 . . ?
C25B C24 H24D 107.7 . . ?
C24 C25A H25A 107.4 . . ?
C24 C25A C26A 108.7(10) . . ?
C26A C25A H25A 107.4 . . ?
C27 C25A C24 117.0(10) . . ?
C27 C25A H25A 107.4 . . ?
C27 C25A C26A 108.4(9) . . ?
C24 C25B H25B 104.5 . . ?
C26B C25B C24 112(2) . . ?
C26B C25B H25B 104.5 . . ?
C27 C25B C24 111.2(17) . . ?
C27 C25B H25B 104.5 . . ?
C27 C25B C26B 118(3) . . ?
C25A C26A H26A 109.5 . . ?
C25A C26A H26B 109.5 . . ?
C25A C26A H26C 109.5 . . ?
H26A C26A H26B 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C25B C26B H26D 109.5 . . ?
C25B C26B H26E 109.5 . . ?
C25B C26B H26F 109.5 . . ?
H26D C26B H26E 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?
C25A C27 H27A 109.5 . . ?
C25A C27 H27B 109.5 . . ?
C25A C27 H27C 109.5 . . ?
C25B C27 H27D 109.5 . . ?
C25B C27 H27E 109.5 . . ?
C25B C27 H27F 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
H27D C27 H27E 109.5 . . ?
H27D C27 H27F 109.5 . . ?
H27E C27 H27F 109.5 . . ?
C17 C28 H28A 109.5 . . ?
C17 C28 H28B 109.5 . . ?
C17 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C4 N1 C15 118.5(7) . . ?
C4 N1 Re1 127.5(6) . . ?
C15 N1 Re1 113.8(5) . . ?
C13 N2 C14 117.8(6) . . ?
C13 N2 Re1 126.9(5) . . ?
C14 N2 Re1 115.2(5) . . ?
C16 O4 Re1 124.6(5) . . ?
C1 Re1 N1 96.2(3) . . ?
C1 Re1 N2 171.3(3) . . ?
C1 Re1 O4 97.9(3) . . ?
C2 Re1 C1 87.6(4) . . ?
C2 Re1 C3 87.0(4) . . ?
C2 Re1 N1 175.5(3) . . ?
C2 Re1 N2 100.1(3) . . ?
C2 Re1 O4 93.9(3) . . ?
C3 Re1 C1 89.0(3) . . ?
C3 Re1 N1 95.3(3) . . ?
C3 Re1 N2 95.6(3) . . ?
C3 Re1 O4 173.1(3) . . ?
N2 Re1 N1 76.0(2) . . ?
O4 Re1 N1 83.3(2) . . ?
O4 Re1 N2 77.4(2) . . ?

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
C4 C5 C6 C7 -0.5(11) . . . . ?
C5 C4 N1 C15 -0.6(11) . . . . ?
C5 C4 N1 Re1 -175.3(6) . . . . ?
C5 C6 C7 C8 179.0(7) . . . . ?
C5 C6 C7 C15 1.2(10) . . . . ?
C6 C7 C8 C9 -179.3(8) . . . . ?
C6 C7 C15 C14 -179.8(6) . . . . ?
C6 C7 C15 N1 -1.7(10) . . . . ?
C7 C8 C9 C10 -1.0(13) . . . . ?
C7 C15 N1 C4 1.4(10) . . . . ?
C7 C15 N1 Re1 176.8(5) . . . . ?
C8 C7 C15 C14 2.3(10) . . . . ?
C8 C7 C15 N1 -179.6(7) . . . . ?
C8 C9 C10 C11 -177.5(9) . . . . ?
C8 C9 C10 C14 2.8(12) . . . . ?
C9 C10 C11 C12 179.7(8) . . . . ?
C9 C10 C14 C15 -2.1(11) . . . . ?
C9 C10 C14 N2 180.0(7) . . . . ?
C10 C11 C12 C13 0.5(12) . . . . ?
C10 C14 C15 C7 -0.4(10) . . . . ?
C10 C14 C15 N1 -178.6(7) . . . . ?
C10 C14 N2 C13 0.2(11) . . . . ?
C10 C14 N2 Re1 -176.0(6) . . . . ?
C11 C10 C14 C15 178.2(7) . . . . ?
C11 C10 C14 N2 0.3(12) . . . . ?
C11 C12 C13 N2 0.0(12) . . . . ?
C12 C13 N2 C14 -0.4(11) . . . . ?
C12 C13 N2 Re1 175.4(6) . . . . ?
C14 C10 C11 C12 -0.6(12) . . . . ?
C14 C15 N1 C4 179.6(7) . . . . ?
C14 C15 N1 Re1 -5.1(8) . . . . ?
C15 C7 C8 C9 -1.6(12) . . . . ?
C15 C14 N2 C13 -177.8(6) . . . . ?
C15 C14 N2 Re1 6.0(8) . . . . ?
C16 C17 C18 C19 176.9(7) . . . . ?
C16 C17 C18 C23 -6.5(11) . . . . ?
C17 C16 O4 Re1 178.2(5) . . . . ?
C17 C18 C19 C20 175.0(8) . . . . ?
C17 C18 C23 C22 -175.7(8) . . . . ?
C18 C19 C20 C21 0.4(13) . . . . ?
C19 C18 C23 C22 0.9(12) . . . . ?
C19 C20 C21 C22 1.8(12) . . . . ?
C19 C20 C21 C24 -175.3(8) . . . . ?
C20 C21 C22 C23 -2.7(12) . . . . ?
C20 C21 C24 C25A 118.9(9) . . . . ?
C20 C21 C24 C25B 69.7(15) . . . . ?
C21 C22 C23 C18 1.3(13) . . . . ?
C21 C24 C25A C26A 175.7(8) . . . . ?
C21 C24 C25A C27 -61.1(11) . . . . ?
C21 C24 C25B C26B 180(2) . . . . ?
C21 C24 C25B C27 44(2) . . . . ?
C22 C21 C24 C25A -58.2(10) . . . . ?
C22 C21 C24 C25B -107.4(14) . . . . ?
C23 C18 C19 C20 -1.8(12) . . . . ?
C24 C21 C22 C23 174.6(8) . . . . ?
C28 C17 C18 C19 -57.9(10) . . . . ?
C28 C17 C18 C23 118.7(8) . . . . ?
N1 C4 C5 C6 0.1(12) . . . . ?
N2 C14 C15 C7 177.7(6) . . . . ?
N2 C14 C15 N1 -0.5(10) . . . . ?
O4 C16 C17 C18 -78.9(8) . . . . ?
O4 C16 C17 C28 156.1(7) . . . . ?
O5 C16 C17 C18 100.3(9) . . . . ?
O5 C16 C17 C28 -24.7(11) . . . . ?
O5 C16 O4 Re1 -0.9(11) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.236
_oxdiff_exptl_absorpt_empirical_full_min 0.749

####################################################################### 
# 
# 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_2018_04_10_dt_js-383_n
_database_code_depnum_ccdc_archive 'CCDC 1867811'
_audit_update_record             
;
2018-09-14 deposited with the CCDC.
2018-11-23 downloaded from the CCDC.
;
_audit_creation_date             2018-05-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H21 N2 O6 Re'
_chemical_formula_sum            'C29 H21 N2 O6 Re'
_chemical_formula_weight         679.68
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C29 H21 N2 O6 Re'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   6.16143(9)
_cell_length_b                   46.2179(6)
_cell_length_c                   9.40358(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2677.84(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    64485
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.6740
_cell_measurement_theta_min      3.7880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    9.260
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.209
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -55
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            90270
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.054
_diffrn_reflns_theta_max         67.054
_diffrn_reflns_theta_min         3.826
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2195
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      ?
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1421765000
_diffrn_orient_matrix_UB_12      0.0273873000
_diffrn_orient_matrix_UB_13      0.0071345000
_diffrn_orient_matrix_UB_21      -0.0228629000
_diffrn_orient_matrix_UB_22      -0.0038528000
_diffrn_orient_matrix_UB_23      0.1620311000
_diffrn_orient_matrix_UB_31      0.2043973000
_diffrn_orient_matrix_UB_32      0.0186223000
_diffrn_orient_matrix_UB_33      0.0229488000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.702
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4777
_reflns_number_total             4817
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.296
_refine_diff_density_min         -2.014
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details 
;
 Flack x determined using 1944 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4817
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0347
_refine_ls_restrained_S_all      1.191
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0089P)²+23.7585P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0771
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C29) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C17(H17)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C19(H19), C20(H20), C22(H22), C24(H24), C25(H25), C27(H27)
3.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.2788(16) 0.57984(19) 0.5601(10) 0.016(2) Uani 1 1 d . . . . .
C2 C 0.6695(18) 0.5515(2) 0.5804(11) 0.022(2) Uani 1 1 d . . . . .
C3 C 0.3386(14) 0.53554(18) 0.7404(9) 0.0142(19) Uani 1 1 d . U . . .
C4 C 0.1406(15) 0.61224(19) 0.8652(10) 0.0160(19) Uani 1 1 d . . . . .
H4 H 0.0650 0.6117 0.7796 0.019 Uiso 1 1 calc R . . . .
C5 C 0.0609(15) 0.62908(19) 0.9764(9) 0.017(2) Uani 1 1 d . . . . .
H5 H -0.0674 0.6394 0.9639 0.020 Uiso 1 1 calc R . . . .
C6 C 0.1674(15) 0.63075(19) 1.1029(11) 0.017(2) Uani 1 1 d . . . . .
H6 H 0.1138 0.6421 1.1768 0.021 Uiso 1 1 calc R . . . .
C7 C 0.3629(16) 0.61469(19) 1.1190(10) 0.0163(19) Uani 1 1 d . . . . .
C8 C 0.4852(18) 0.61410(18) 1.2500(8) 0.0204(19) Uani 1 1 d . . . . .
H8 H 0.4396 0.6252 1.3268 0.024 Uiso 1 1 calc R . . . .
C9 C 0.6646(15) 0.5976(2) 1.2624(9) 0.0164(19) Uani 1 1 d . . . . .
H9 H 0.7406 0.5974 1.3479 0.020 Uiso 1 1 calc R . . . .
C10 C 0.7402(15) 0.58022(19) 1.1455(10) 0.0162(19) Uani 1 1 d . . . . .
C11 C 0.9235(15) 0.56250(18) 1.1521(10) 0.018(2) Uani 1 1 d . . . . .
H11 H 1.0037 0.5612 1.2356 0.021 Uiso 1 1 calc R . . . .
C12 C 0.9840(17) 0.54708(18) 1.0340(9) 0.0199(18) Uani 1 1 d . . . . .
H12 H 1.1053 0.5351 1.0374 0.024 Uiso 1 1 calc R . . . .
C13 C 0.8640(15) 0.54932(19) 0.9088(10) 0.0140(18) Uani 1 1 d . . . . .
H13 H 0.9085 0.5388 0.8296 0.017 Uiso 1 1 calc R . . . .
C14 C 0.6261(14) 0.58096(18) 1.0170(9) 0.0113(17) Uani 1 1 d . U . . .
C15 C 0.4333(14) 0.59804(17) 1.0038(9) 0.0113(17) Uani 1 1 d . U . . .
C16 C 0.6103(16) 0.6326(2) 0.6236(11) 0.017(2) Uani 1 1 d . U . . .
C17 C 0.7890(18) 0.6550(2) 0.5994(10) 0.023(2) Uani 1 1 d . . . . .
H17 H 0.9245 0.6445 0.5826 0.027 Uiso 1 1 calc R . . . .
C18 C 0.8221(16) 0.67352(18) 0.7308(10) 0.0179(19) Uani 1 1 d . . . . .
C19 C 1.0244(18) 0.68822(18) 0.7450(8) 0.0193(19) Uani 1 1 d . . . . .
H19 H 1.1292 0.6862 0.6745 0.023 Uiso 1 1 calc R . . . .
C20 C 1.0670(16) 0.70536(18) 0.8611(10) 0.020(2) Uani 1 1 d . . . . .
H20 H 1.1995 0.7149 0.8674 0.024 Uiso 1 1 calc R . . . .
C21 C 0.9133(15) 0.70869(18) 0.9708(9) 0.0159(19) Uani 1 1 d . . . . .
C22 C 0.9579(16) 0.72517(18) 1.0953(8) 0.0160(19) Uani 1 1 d . . . . .
H22 H 1.0905 0.7346 1.1049 0.019 Uiso 1 1 calc R . . . .
C23 C 0.8080(16) 0.72712(18) 1.1993(11) 0.0190(19) Uani 1 1 d . . . . .
C24 C 0.6043(16) 0.7136(2) 1.1864(10) 0.020(2) Uani 1 1 d . . . . .
H24 H 0.5023 0.7155 1.2587 0.024 Uiso 1 1 calc R . . . .
C25 C 0.5558(16) 0.6977(2) 1.0673(10) 0.021(2) Uani 1 1 d . . . . .
H25 H 0.4203 0.6889 1.0590 0.026 Uiso 1 1 calc R . . . .
C26 C 0.7100(16) 0.69436(19) 0.9574(10) 0.017(2) Uani 1 1 d . . . . .
C27 C 0.6700(16) 0.67719(19) 0.8336(9) 0.0161(19) Uani 1 1 d . . . . .
H27 H 0.5356 0.6683 0.8232 0.019 Uiso 1 1 calc R . . . .
C28 C 1.046(2) 0.7521(2) 1.3577(11) 0.033(3) Uani 1 1 d . . . . .
H28A H 1.0467 0.7612 1.4495 0.049 Uiso 1 1 calc GR . . . .
H28B H 1.0885 0.7659 1.2867 0.049 Uiso 1 1 calc GR . . . .
H28C H 1.1463 0.7362 1.3577 0.049 Uiso 1 1 calc GR . . . .
C29 C 0.748(2) 0.6737(3) 0.4702(13) 0.038(3) Uani 1 1 d . U . . .
H29A H 0.7473 0.6618 0.3865 0.057 Uiso 1 1 calc GR . . . .
H29B H 0.8602 0.6880 0.4623 0.057 Uiso 1 1 calc GR . . . .
H29C H 0.6098 0.6831 0.4796 0.057 Uiso 1 1 calc GR . . . .
N1 N 0.3227(12) 0.59689(15) 0.8785(9) 0.0155(16) Uani 1 1 d . . . . .
N2 N 0.6885(12) 0.56585(15) 0.8984(8) 0.0134(16) Uani 1 1 d . . . . .
O1 O 0.1540(11) 0.58430(15) 0.4755(7) 0.0208(15) Uani 1 1 d . . . . .
O2 O 0.7891(12) 0.53987(15) 0.5033(8) 0.0257(16) Uani 1 1 d . U . . .
O3 O 0.2543(10) 0.51320(13) 0.7543(7) 0.0222(16) Uani 1 1 d . . . . .
O4 O 0.6754(10) 0.61007(12) 0.6923(7) 0.0164(14) Uani 1 1 d . . . . .
O5 O 0.4224(12) 0.63716(15) 0.5847(8) 0.0261(18) Uani 1 1 d . . . . .
O6 O 0.8332(13) 0.74173(14) 1.3270(7) 0.0243(17) Uani 1 1 d . . . . .
Re1 Re 0.48368(6) 0.57143(2) 0.71224(4) 0.01095(10) 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
C1 O1 1.125(11) . ?
C1 Re1 1.947(10) . ?
C2 O2 1.165(13) . ?
C2 Re1 1.923(11) . ?
C3 O3 1.163(11) . ?
C3 Re1 1.903(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.393(13) . ?
C4 N1 1.333(12) . ?
C5 H5 0.9300 . ?
C5 C6 1.361(14) . ?
C6 H6 0.9300 . ?
C6 C7 1.423(13) . ?
C7 C8 1.444(12) . ?
C7 C15 1.398(12) . ?
C8 H8 0.9300 . ?
C8 C9 1.348(14) . ?
C9 H9 0.9300 . ?
C9 C10 1.439(13) . ?
C10 C11 1.397(13) . ?
C10 C14 1.398(13) . ?
C11 H11 0.9300 . ?
C11 C12 1.371(13) . ?
C12 H12 0.9300 . ?
C12 C13 1.394(13) . ?
C13 H13 0.9300 . ?
C13 N2 1.328(12) . ?
C14 C15 1.432(12) . ?
C14 N2 1.370(11) . ?
C15 N1 1.363(12) . ?
C16 C17 1.530(14) . ?
C16 O4 1.289(11) . ?
C16 O5 1.232(12) . ?
C17 H17 0.9800 . ?
C17 C18 1.516(13) . ?
C17 C29 1.510(15) . ?
C18 C19 1.426(14) . ?
C18 C27 1.357(14) . ?
C19 H19 0.9300 . ?
C19 C20 1.375(12) . ?
C20 H20 0.9300 . ?
C20 C21 1.409(14) . ?
C21 C22 1.423(12) . ?
C21 C26 1.423(14) . ?
C22 H22 0.9300 . ?
C22 C23 1.348(14) . ?
C23 C24 1.407(14) . ?
C23 O6 1.386(11) . ?
C24 H24 0.9300 . ?
C24 C25 1.374(13) . ?
C25 H25 0.9300 . ?
C25 C26 1.412(14) . ?
C26 C27 1.431(13) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28 O6 1.426(14) . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
N1 Re1 2.194(8) . ?
N2 Re1 2.173(7) . ?
O4 Re1 2.149(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
O1 C1 Re1 177.3(9) . . ?
O2 C2 Re1 177.3(9) . . ?
O3 C3 Re1 177.8(8) . . ?
C5 C4 H4 119.2 . . ?
N1 C4 H4 119.2 . . ?
N1 C4 C5 121.6(9) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.2(9) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 120.9 . . ?
C5 C6 C7 118.1(9) . . ?
C7 C6 H6 120.9 . . ?
C6 C7 C8 122.8(9) . . ?
C15 C7 C6 117.9(9) . . ?
C15 C7 C8 119.3(8) . . ?
C7 C8 H8 119.6 . . ?
C9 C8 C7 120.8(8) . . ?
C9 C8 H8 119.6 . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 121.0(8) . . ?
C10 C9 H9 119.5 . . ?
C11 C10 C9 123.7(8) . . ?
C11 C10 C14 117.3(9) . . ?
C14 C10 C9 119.0(8) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.3(9) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 H12 120.0 . . ?
C11 C12 C13 120.1(9) . . ?
C13 C12 H12 120.0 . . ?
C12 C13 H13 118.8 . . ?
N2 C13 C12 122.5(9) . . ?
N2 C13 H13 118.8 . . ?
C10 C14 C15 120.4(8) . . ?
N2 C14 C10 123.3(8) . . ?
N2 C14 C15 116.3(8) . . ?
C7 C15 C14 119.6(8) . . ?
N1 C15 C7 122.4(8) . . ?
N1 C15 C14 117.9(8) . . ?
O4 C16 C17 113.5(8) . . ?
O5 C16 C17 121.1(9) . . ?
O5 C16 O4 125.4(9) . . ?
C16 C17 H17 107.3 . . ?
C18 C17 C16 110.9(8) . . ?
C18 C17 H17 107.3 . . ?
C29 C17 C16 112.6(9) . . ?
C29 C17 H17 107.3 . . ?
C29 C17 C18 110.9(8) . . ?
C19 C18 C17 117.5(9) . . ?
C27 C18 C17 123.9(9) . . ?
C27 C18 C19 118.5(8) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 C18 121.1(9) . . ?
C20 C19 H19 119.5 . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 121.1(9) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 C22 122.0(9) . . ?
C20 C21 C26 118.5(8) . . ?
C26 C21 C22 119.5(9) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.0(9) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 C24 121.3(9) . . ?
C22 C23 O6 125.7(9) . . ?
O6 C23 C24 113.0(9) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.2(9) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 119.7 . . ?
C24 C25 C26 120.5(9) . . ?
C26 C25 H25 119.7 . . ?
C21 C26 C27 118.8(9) . . ?
C25 C26 C21 118.5(9) . . ?
C25 C26 C27 122.7(9) . . ?
C18 C27 C26 122.0(9) . . ?
C18 C27 H27 119.0 . . ?
C26 C27 H27 119.0 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O6 C28 H28A 109.5 . . ?
O6 C28 H28B 109.5 . . ?
O6 C28 H28C 109.5 . . ?
C17 C29 H29A 109.5 . . ?
C17 C29 H29B 109.5 . . ?
C17 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C4 N1 C15 118.8(8) . . ?
C4 N1 Re1 126.8(7) . . ?
C15 N1 Re1 114.3(6) . . ?
C13 N2 C14 117.5(8) . . ?
C13 N2 Re1 126.9(6) . . ?
C14 N2 Re1 115.6(6) . . ?
C16 O4 Re1 122.9(6) . . ?
C23 O6 C28 116.3(8) . . ?
C1 Re1 N1 97.1(3) . . ?
C1 Re1 N2 172.7(3) . . ?
C1 Re1 O4 97.3(3) . . ?
C2 Re1 C1 90.5(4) . . ?
C2 Re1 N1 170.3(3) . . ?
C2 Re1 N2 96.7(4) . . ?
C2 Re1 O4 90.8(3) . . ?
C3 Re1 C1 88.4(4) . . ?
C3 Re1 C2 87.2(4) . . ?
C3 Re1 N1 99.0(3) . . ?
C3 Re1 N2 93.3(3) . . ?
C3 Re1 O4 174.1(3) . . ?
N2 Re1 N1 75.6(3) . . ?
O4 Re1 N1 82.2(3) . . ?
O4 Re1 N2 81.4(3) . . ?

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
C4 C5 C6 C7 -0.2(14) . . . . ?
C5 C4 N1 C15 -0.6(13) . . . . ?
C5 C4 N1 Re1 -175.9(6) . . . . ?
C5 C6 C7 C8 -177.9(8) . . . . ?
C5 C6 C7 C15 -0.3(13) . . . . ?
C6 C7 C8 C9 177.1(9) . . . . ?
C6 C7 C15 C14 -178.3(8) . . . . ?
C6 C7 C15 N1 0.4(13) . . . . ?
C7 C8 C9 C10 0.4(14) . . . . ?
C7 C15 N1 C4 0.1(13) . . . . ?
C7 C15 N1 Re1 175.9(6) . . . . ?
C8 C7 C15 C14 -0.7(12) . . . . ?
C8 C7 C15 N1 178.1(8) . . . . ?
C8 C9 C10 C11 -179.4(9) . . . . ?
C8 C9 C10 C14 0.8(13) . . . . ?
C9 C10 C11 C12 -179.1(8) . . . . ?
C9 C10 C14 C15 -2.0(12) . . . . ?
C9 C10 C14 N2 178.1(8) . . . . ?
C10 C11 C12 C13 0.4(14) . . . . ?
C10 C14 C15 C7 1.9(12) . . . . ?
C10 C14 C15 N1 -176.9(8) . . . . ?
C10 C14 N2 C13 1.4(12) . . . . ?
C10 C14 N2 Re1 -179.2(7) . . . . ?
C11 C10 C14 C15 178.3(8) . . . . ?
C11 C10 C14 N2 -1.6(13) . . . . ?
C11 C12 C13 N2 -0.7(14) . . . . ?
C12 C13 N2 C14 -0.3(13) . . . . ?
C12 C13 N2 Re1 -179.6(7) . . . . ?
C14 C10 C11 C12 0.6(13) . . . . ?
C14 C15 N1 C4 178.8(8) . . . . ?
C14 C15 N1 Re1 -5.3(9) . . . . ?
C15 C7 C8 C9 -0.5(13) . . . . ?
C15 C14 N2 C13 -178.5(7) . . . . ?
C15 C14 N2 Re1 0.9(9) . . . . ?
C16 C17 C18 C19 159.0(8) . . . . ?
C16 C17 C18 C27 -22.1(13) . . . . ?
C17 C16 O4 Re1 -168.9(6) . . . . ?
C17 C18 C19 C20 -179.9(8) . . . . ?
C17 C18 C27 C26 178.7(8) . . . . ?
C18 C19 C20 C21 0.8(13) . . . . ?
C19 C18 C27 C26 -2.5(13) . . . . ?
C19 C20 C21 C22 176.9(8) . . . . ?
C19 C20 C21 C26 -1.4(13) . . . . ?
C20 C21 C22 C23 -178.2(8) . . . . ?
C20 C21 C26 C25 180.0(8) . . . . ?
C20 C21 C26 C27 0.1(12) . . . . ?
C21 C22 C23 C24 -1.4(13) . . . . ?
C21 C22 C23 O6 178.1(8) . . . . ?
C21 C26 C27 C18 1.9(13) . . . . ?
C22 C21 C26 C25 1.7(12) . . . . ?
C22 C21 C26 C27 -178.2(8) . . . . ?
C22 C23 C24 C25 1.1(14) . . . . ?
C22 C23 O6 C28 -9.0(13) . . . . ?
C23 C24 C25 C26 0.6(13) . . . . ?
C24 C23 O6 C28 170.5(8) . . . . ?
C24 C25 C26 C21 -2.0(13) . . . . ?
C24 C25 C26 C27 177.9(8) . . . . ?
C25 C26 C27 C18 -178.0(8) . . . . ?
C26 C21 C22 C23 0.0(13) . . . . ?
C27 C18 C19 C20 1.2(13) . . . . ?
C29 C17 C18 C19 -75.0(12) . . . . ?
C29 C17 C18 C27 103.9(11) . . . . ?
N1 C4 C5 C6 0.6(14) . . . . ?
N2 C14 C15 C7 -178.2(8) . . . . ?
N2 C14 C15 N1 3.0(11) . . . . ?
O4 C16 C17 C18 -80.7(11) . . . . ?
O4 C16 C17 C29 154.2(9) . . . . ?
O5 C16 C17 C18 96.2(12) . . . . ?
O5 C16 C17 C29 -28.8(14) . . . . ?
O5 C16 O4 Re1 14.3(15) . . . . ?
O6 C23 C24 C25 -178.4(8) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.178 0.000 -0.252 114.7 50.4 ?
2 -0.230 0.320 0.361 18.7 3.5 ?
3 0.075 0.500 0.252 114.7 50.8 ?
4 0.230 0.680 0.361 18.7 3.1 ?
5 0.270 0.180 0.639 18.7 4.6 ?
6 0.730 0.820 0.639 18.7 2.5 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.986
_oxdiff_exptl_absorpt_empirical_full_min 0.551

