# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
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#  Bona fide researchers may freely download Mercury and enCIFer
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data_100611a_larry
_database_code_depnum_ccdc_archive 'CCDC 916504'
#TrackingRef '3.cif'
_audit_creation_date             2011-10-10
_audit_creation_method           
;
Olex2 1.1
(compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C22 H24 N4 O2 Re, C16 H36 N'
_chemical_formula_sum            'C38 H60 N5 O2 Re'
_chemical_formula_weight         805.11
_chemical_melting_point          ?
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'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   15.2908(4)
_cell_length_b                   12.3356(3)
_cell_length_c                   21.2687(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 101.227(2)
_cell_angle_gamma                90.00
_cell_volume                     3934.96(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8948
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.6718
_cell_measurement_theta_min      3.2745
_exptl_absorpt_coefficient_mu    6.316
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
?
;
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16058
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.28
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
1 omega -32.00 -5.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 86.0000 -153.0000 27
#__ type_ start__ end____ width___ exp.time_
2 omega -38.00 -4.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -87.0000 79.0000 34
#__ type_ start__ end____ width___ exp.time_
3 omega -15.00 18.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 86.0000 -87.0000 33
#__ type_ start__ end____ width___ exp.time_
4 omega -3.00 32.00 1.0000 8.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -87.0000 79.0000 35
#__ type_ start__ end____ width___ exp.time_
5 omega 35.00 110.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 77.0000 120.0000 75
#__ type_ start__ end____ width___ exp.time_
6 omega 77.00 122.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 125.0000 -180.0000 45
#__ type_ start__ end____ width___ exp.time_
7 omega -83.00 6.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- -64.0000 50.0000 30.0000 89
#__ type_ start__ end____ width___ exp.time_
8 omega -127.00 -65.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- -64.0000 -50.0000 -90.0000 62
#__ type_ start__ end____ width___ exp.time_
9 omega 41.00 68.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 0.0000 27
#__ type_ start__ end____ width___ exp.time_
10 omega 38.00 71.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 90.0000 33
#__ type_ start__ end____ width___ exp.time_
11 omega 46.00 74.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 -60.0000 28
#__ type_ start__ end____ width___ exp.time_
12 omega 44.00 72.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 30.0000 28
#__ type_ start__ end____ width___ exp.time_
13 omega 46.00 72.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 -90.0000 26
#__ type_ start__ end____ width___ exp.time_
14 omega 37.00 68.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -60.0000 31
#__ type_ start__ end____ width___ exp.time_
15 omega 37.00 62.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -120.0000 25
#__ type_ start__ end____ width___ exp.time_
16 omega 110.00 170.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 50.0000 120.0000 60
#__ type_ start__ end____ width___ exp.time_
17 omega 40.00 145.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -87.0000 -101.0000 105
#__ type_ start__ end____ width___ exp.time_
18 omega 37.00 62.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 60.0000 25
#__ type_ start__ end____ width___ exp.time_
19 omega 95.00 176.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 50.0000 30.0000 81
#__ type_ start__ end____ width___ exp.time_
20 omega 41.00 71.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -90.0000 30
#__ type_ start__ end____ width___ exp.time_
21 omega 42.00 81.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 60.0000 39
#__ type_ start__ end____ width___ exp.time_
22 omega 85.00 157.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 77.0000 60.0000 72
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0197710000
_diffrn_orient_matrix_UB_12      0.0928149000
_diffrn_orient_matrix_UB_13      0.0492690000
_diffrn_orient_matrix_UB_21      -0.0517963000
_diffrn_orient_matrix_UB_22      -0.0605943000
_diffrn_orient_matrix_UB_23      0.0444999000
_diffrn_orient_matrix_UB_31      0.0863443000
_diffrn_orient_matrix_UB_32      -0.0574798000
_diffrn_orient_matrix_UB_33      0.0325590000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                6575
_reflns_number_total             7017
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         3.449
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7017
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0267
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+2.7431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0753
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re -0.005055(7) -0.079581(8) 0.776764(5) 0.01839(6) Uani 1 1 d . . .
O1 O -0.16178(13) -0.18152(17) 0.68445(11) 0.0356(5) Uani 1 1 d . . .
O2 O -0.06564(15) -0.16721(19) 0.89563(10) 0.0373(5) Uani 1 1 d . . .
N1 N -0.09713(18) 0.1586(2) 0.78115(14) 0.0355(6) Uani 1 1 d . . .
N2 N 0.12087(16) -0.2906(2) 0.77225(12) 0.0293(5) Uani 1 1 d . . .
N3 N 0.05776(13) -0.00973(17) 0.70279(10) 0.0188(4) Uani 1 1 d . . .
N4 N 0.11791(14) -0.00333(17) 0.82720(10) 0.0208(4) Uani 1 1 d . . .
N5 N 0.88823(15) 0.48518(18) 0.81752(11) 0.0243(5) Uani 1 1 d . . .
C1 C -0.06674(19) 0.0732(2) 0.78013(14) 0.0246(6) Uani 1 1 d . . .
C2 C 0.07480(17) -0.2168(2) 0.77327(12) 0.0218(5) Uani 1 1 d . . .
C3 C -0.10294(18) -0.1430(2) 0.72129(14) 0.0250(6) Uani 1 1 d . . .
C4 C -0.04460(18) -0.1335(2) 0.84914(14) 0.0262(6) Uani 1 1 d . . .
C5 C 0.02213(17) -0.0111(2) 0.64054(12) 0.0232(5) Uani 1 1 d . . .
H5 H -0.0340 -0.0455 0.6272 0.028 Uiso 1 1 calc R . .
C6 C 0.06285(18) 0.0352(2) 0.59417(13) 0.0265(6) Uani 1 1 d . . .
H6 H 0.0341 0.0327 0.5504 0.032 Uiso 1 1 calc R . .
C7 C 0.14589(19) 0.0854(2) 0.61158(14) 0.0222(6) Uani 1 1 d . . .
C8 C 0.18295(18) 0.08690(19) 0.67710(13) 0.0201(5) Uani 1 1 d . . .
H8 H 0.2394 0.1201 0.6915 0.024 Uiso 1 1 calc R . .
C9 C 0.13835(16) 0.0404(2) 0.72158(12) 0.0187(5) Uani 1 1 d . . .
C10 C 0.17258(16) 0.0419(2) 0.79119(12) 0.0182(5) Uani 1 1 d . . .
C11 C 0.25426(19) 0.0865(2) 0.81927(14) 0.0210(6) Uani 1 1 d . . .
H11 H 0.2908 0.1184 0.7929 0.025 Uiso 1 1 calc R . .
C12 C 0.2834(2) 0.0850(2) 0.88550(15) 0.0250(6) Uani 1 1 d . . .
C13 C 0.2251(2) 0.0396(2) 0.92115(13) 0.0286(6) Uani 1 1 d . . .
H13 H 0.2410 0.0377 0.9666 0.034 Uiso 1 1 calc R . .
C14 C 0.14447(19) -0.0027(2) 0.89056(13) 0.0272(6) Uani 1 1 d . . .
H14 H 0.1060 -0.0329 0.9160 0.033 Uiso 1 1 calc R . .
C15 C 0.19469(19) 0.1372(2) 0.56283(13) 0.0282(6) Uani 1 1 d . . .
C16 C 0.1450(2) 0.1202(3) 0.49371(14) 0.0392(7) Uani 1 1 d . . .
H16A H 0.1399 0.0425 0.4844 0.059 Uiso 1 1 calc R . .
H16B H 0.1781 0.1553 0.4642 0.059 Uiso 1 1 calc R . .
H16C H 0.0853 0.1522 0.4883 0.059 Uiso 1 1 calc R . .
C17 C 0.2046(3) 0.2591(3) 0.57620(16) 0.0435(8) Uani 1 1 d . . .
H17A H 0.1455 0.2916 0.5734 0.065 Uiso 1 1 calc R . .
H17B H 0.2345 0.2930 0.5445 0.065 Uiso 1 1 calc R . .
H17C H 0.2401 0.2707 0.6193 0.065 Uiso 1 1 calc R . .
C18 C 0.2877(2) 0.0860(3) 0.57044(18) 0.0436(9) Uani 1 1 d . . .
H18A H 0.3219 0.1015 0.6134 0.065 Uiso 1 1 calc R . .
H18B H 0.3188 0.1165 0.5383 0.065 Uiso 1 1 calc R . .
H18C H 0.2818 0.0074 0.5644 0.065 Uiso 1 1 calc R . .
C19 C 0.3739(2) 0.1333(3) 0.91601(14) 0.0333(7) Uani 1 1 d . . .
C20 C 0.4469(2) 0.0881(3) 0.88307(18) 0.0479(10) Uani 1 1 d . . .
H20A H 0.4494 0.0090 0.8877 0.072 Uiso 1 1 calc R . .
H20B H 0.5046 0.1193 0.9030 0.072 Uiso 1 1 calc R . .
H20C H 0.4334 0.1070 0.8375 0.072 Uiso 1 1 calc R . .
C21 C 0.3682(3) 0.2559(3) 0.9069(2) 0.0551(10) Uani 1 1 d . . .
H21A H 0.3541 0.2728 0.8610 0.083 Uiso 1 1 calc R . .
H21B H 0.4256 0.2888 0.9261 0.083 Uiso 1 1 calc R . .
H21C H 0.3214 0.2849 0.9277 0.083 Uiso 1 1 calc R . .
C22 C 0.3985(3) 0.1062(4) 0.98739(16) 0.0473(9) Uani 1 1 d . . .
H22A H 0.3547 0.1387 1.0097 0.071 Uiso 1 1 calc R . .
H22B H 0.4579 0.1352 1.0051 0.071 Uiso 1 1 calc R . .
H22C H 0.3987 0.0274 0.9930 0.071 Uiso 1 1 calc R . .
C23 C 0.8586(2) 0.5896(2) 0.84486(16) 0.0286(6) Uani 1 1 d . . .
H23A H 0.8613 0.6489 0.8139 0.034 Uiso 1 1 calc R . .
H23B H 0.9014 0.6072 0.8848 0.034 Uiso 1 1 calc R . .
C24 C 0.7650(2) 0.5865(2) 0.85972(18) 0.0321(7) Uani 1 1 d . . .
H24A H 0.7230 0.5556 0.8227 0.039 Uiso 1 1 calc R . .
H24B H 0.7647 0.5394 0.8973 0.039 Uiso 1 1 calc R . .
C25 C 0.7348(2) 0.6997(3) 0.87353(19) 0.0412(8) Uani 1 1 d . . .
H25A H 0.7391 0.7477 0.8370 0.049 Uiso 1 1 calc R . .
H25B H 0.7750 0.7287 0.9120 0.049 Uiso 1 1 calc R . .
C26 C 0.6395(2) 0.7006(3) 0.8846(2) 0.0481(9) Uani 1 1 d . . .
H26A H 0.6002 0.6661 0.8482 0.072 Uiso 1 1 calc R . .
H26B H 0.6203 0.7756 0.8887 0.072 Uiso 1 1 calc R . .
H26C H 0.6365 0.6607 0.9239 0.072 Uiso 1 1 calc R . .
C27 C 0.98279(18) 0.5039(2) 0.80698(15) 0.0293(6) Uani 1 1 d . . .
H27A H 0.9841 0.5728 0.7833 0.035 Uiso 1 1 calc R . .
H27B H 1.0229 0.5123 0.8493 0.035 Uiso 1 1 calc R . .
C28 C 1.0188(2) 0.4138(2) 0.77031(18) 0.0342(7) Uani 1 1 d . . .
H28A H 1.0000 0.3427 0.7846 0.041 Uiso 1 1 calc R . .
H28B H 0.9939 0.4214 0.7239 0.041 Uiso 1 1 calc R . .
C29 C 1.1201(2) 0.4185(2) 0.78147(19) 0.0366(8) Uani 1 1 d . . .
H29A H 1.1388 0.4927 0.7723 0.044 Uiso 1 1 calc R . .
H29B H 1.1448 0.4025 0.8271 0.044 Uiso 1 1 calc R . .
C30 C 1.1573(2) 0.3393(3) 0.7401(2) 0.0481(9) Uani 1 1 d . . .
H30A H 1.1391 0.3604 0.6950 0.072 Uiso 1 1 calc R . .
H30B H 1.1346 0.2666 0.7462 0.072 Uiso 1 1 calc R . .
H30C H 1.2225 0.3391 0.7520 0.072 Uiso 1 1 calc R . .
C31 C 0.82680(18) 0.4564(2) 0.75433(13) 0.0241(5) Uani 1 1 d . . .
H31A H 0.8501 0.3905 0.7368 0.029 Uiso 1 1 calc R . .
H31B H 0.7671 0.4387 0.7630 0.029 Uiso 1 1 calc R . .
C32 C 0.8167(2) 0.5449(2) 0.70398(15) 0.0310(6) Uani 1 1 d . . .
H32A H 0.8763 0.5665 0.6967 0.037 Uiso 1 1 calc R . .
H32B H 0.7884 0.6092 0.7194 0.037 Uiso 1 1 calc R . .
C33 C 0.7600(2) 0.5054(2) 0.64136(15) 0.0342(7) Uani 1 1 d . . .
H33A H 0.7916 0.4458 0.6239 0.041 Uiso 1 1 calc R . .
H33B H 0.7031 0.4761 0.6498 0.041 Uiso 1 1 calc R . .
C34 C 0.7404(3) 0.5952(3) 0.59213(18) 0.0519(10) Uani 1 1 d . . .
H34A H 0.6995 0.5683 0.5540 0.078 Uiso 1 1 calc R . .
H34B H 0.7961 0.6189 0.5802 0.078 Uiso 1 1 calc R . .
H34C H 0.7129 0.6564 0.6103 0.078 Uiso 1 1 calc R . .
C35 C 0.88584(19) 0.3905(2) 0.86319(13) 0.0262(6) Uani 1 1 d . B .
H35A H 0.9092 0.3253 0.8449 0.031 Uiso 1 1 calc R . .
H35B H 0.8229 0.3758 0.8656 0.031 Uiso 1 1 calc R . .
C36 C 0.9389(2) 0.4075(3) 0.93124(16) 0.0389(8) Uani 1 1 d . . .
H36A H 0.9968 0.4416 0.9291 0.047 Uiso 0.45 1 calc PR A 1
H36B H 0.9058 0.4576 0.9545 0.047 Uiso 0.45 1 calc PR A 1
H36C H 0.9968 0.4416 0.9291 0.047 Uiso 0.55 1 calc PR A 2
H36D H 0.9058 0.4576 0.9545 0.047 Uiso 0.55 1 calc PR A 2
C37 C 0.9552(3) 0.3023(3) 0.96781(16) 0.0457(8) Uani 0.45 1 d PD B 1
H37A H 0.8960 0.2743 0.9721 0.055 Uiso 0.45 1 calc PR B 1
H37B H 0.9869 0.3212 1.0116 0.055 Uiso 0.45 1 calc PR B 1
C38 C 1.0056(12) 0.2072(12) 0.9459(9) 0.069(5) Uani 0.45 1 d PDU B 1
H38A H 0.9716 0.1785 0.9055 0.104 Uiso 0.45 1 calc PR B 1
H38B H 1.0132 0.1502 0.9787 0.104 Uiso 0.45 1 calc PR B 1
H38C H 1.0642 0.2318 0.9396 0.104 Uiso 0.45 1 calc PR B 1
C37A C 0.9552(3) 0.3023(3) 0.96781(16) 0.0457(8) Uani 0.55 1 d P B 2
H37C H 0.9022 0.2547 0.9578 0.055 Uiso 0.55 1 calc PR B 2
H37D H 0.9688 0.3161 1.0146 0.055 Uiso 0.55 1 calc PR B 2
C38A C 1.0367(9) 0.2488(10) 0.9456(8) 0.064(4) Uani 0.55 1 d PDU B 2
H38D H 1.0830 0.3036 0.9451 0.096 Uiso 0.55 1 calc PR B 2
H38E H 1.0177 0.2188 0.9025 0.096 Uiso 0.55 1 calc PR B 2
H38F H 1.0606 0.1906 0.9754 0.096 Uiso 0.55 1 calc PR B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.01572(9) 0.01533(9) 0.02528(9) 0.00062(4) 0.00684(5) -0.00026(4)
O1 0.0228(10) 0.0303(11) 0.0505(13) -0.0066(10) -0.0006(9) -0.0050(9)
O2 0.0389(12) 0.0419(13) 0.0339(11) 0.0076(10) 0.0137(9) -0.0062(10)
N1 0.0368(14) 0.0216(13) 0.0511(16) -0.0008(11) 0.0158(12) 0.0054(11)
N2 0.0257(12) 0.0247(13) 0.0377(13) -0.0005(10) 0.0065(10) 0.0045(10)
N3 0.0151(10) 0.0165(10) 0.0251(11) -0.0016(8) 0.0049(8) 0.0004(8)
N4 0.0214(10) 0.0181(11) 0.0239(11) 0.0024(8) 0.0070(8) 0.0001(8)
N5 0.0232(11) 0.0201(11) 0.0308(12) -0.0031(9) 0.0081(9) -0.0038(9)
C1 0.0203(14) 0.0249(15) 0.0302(15) -0.0012(10) 0.0088(11) -0.0022(10)
C2 0.0185(12) 0.0231(13) 0.0245(12) -0.0002(10) 0.0055(10) -0.0029(11)
C3 0.0211(13) 0.0172(12) 0.0396(15) 0.0044(11) 0.0133(12) 0.0038(10)
C4 0.0212(13) 0.0227(14) 0.0354(15) 0.0021(11) 0.0074(11) 0.0008(10)
C5 0.0193(12) 0.0265(14) 0.0237(13) -0.0007(11) 0.0035(10) -0.0077(10)
C6 0.0250(14) 0.0315(15) 0.0213(13) -0.0027(11) 0.0001(10) -0.0023(11)
C7 0.0216(14) 0.0215(14) 0.0238(14) 0.0009(10) 0.0051(11) 0.0019(10)
C8 0.0168(13) 0.0206(13) 0.0228(13) -0.0005(9) 0.0039(10) -0.0005(9)
C9 0.0166(12) 0.0159(12) 0.0236(12) -0.0006(10) 0.0035(9) 0.0022(10)
C10 0.0189(12) 0.0145(12) 0.0218(12) 0.0004(10) 0.0055(9) 0.0009(9)
C11 0.0212(14) 0.0197(13) 0.0223(13) -0.0008(9) 0.0049(11) -0.0015(9)
C12 0.0261(15) 0.0226(14) 0.0252(14) -0.0002(10) 0.0020(12) -0.0021(10)
C13 0.0363(16) 0.0290(15) 0.0198(13) 0.0020(11) 0.0037(11) -0.0026(12)
C14 0.0322(14) 0.0261(14) 0.0260(13) 0.0022(11) 0.0120(11) -0.0021(12)
C15 0.0298(14) 0.0338(16) 0.0216(13) 0.0014(11) 0.0065(11) -0.0054(12)
C16 0.0430(18) 0.051(2) 0.0232(14) 0.0032(14) 0.0066(13) -0.0114(16)
C17 0.066(2) 0.0350(18) 0.0315(16) 0.0043(14) 0.0128(15) -0.0155(16)
C18 0.0320(18) 0.068(3) 0.0349(18) 0.0080(15) 0.0158(14) -0.0011(15)
C19 0.0317(15) 0.0386(18) 0.0263(14) 0.0004(13) -0.0022(11) -0.0096(13)
C20 0.0264(17) 0.078(3) 0.0356(18) -0.0008(16) -0.0022(14) -0.0076(15)
C21 0.056(2) 0.039(2) 0.059(2) -0.0032(17) -0.0137(18) -0.0223(18)
C22 0.044(2) 0.065(2) 0.0280(17) -0.0002(16) -0.0053(14) -0.0137(18)
C23 0.0314(16) 0.0189(14) 0.0373(16) -0.0065(11) 0.0108(13) -0.0039(11)
C24 0.0310(17) 0.0260(16) 0.0417(19) -0.0061(12) 0.0128(14) -0.0026(11)
C25 0.0394(18) 0.0301(16) 0.058(2) -0.0132(15) 0.0194(15) -0.0046(14)
C26 0.044(2) 0.0407(19) 0.063(2) -0.0188(17) 0.0192(17) -0.0034(15)
C27 0.0244(14) 0.0239(14) 0.0421(16) -0.0037(12) 0.0128(12) -0.0074(11)
C28 0.0293(16) 0.0283(17) 0.050(2) -0.0043(13) 0.0191(14) -0.0041(12)
C29 0.0326(18) 0.0272(17) 0.052(2) 0.0000(13) 0.0137(15) 0.0015(12)
C30 0.045(2) 0.0357(19) 0.070(2) -0.0021(17) 0.0276(18) 0.0073(15)
C31 0.0223(13) 0.0214(13) 0.0293(14) -0.0034(11) 0.0066(11) -0.0044(11)
C32 0.0340(16) 0.0252(14) 0.0344(15) 0.0031(12) 0.0087(12) -0.0026(12)
C33 0.0426(17) 0.0295(16) 0.0321(15) -0.0012(12) 0.0110(13) 0.0010(13)
C34 0.081(3) 0.041(2) 0.0304(18) 0.0016(15) 0.0037(18) 0.0109(19)
C35 0.0277(14) 0.0232(13) 0.0282(14) -0.0003(12) 0.0070(11) -0.0033(11)
C36 0.0403(19) 0.0430(19) 0.0323(17) -0.0023(13) 0.0046(14) -0.0080(14)
C37 0.056(2) 0.048(2) 0.0308(16) -0.0024(15) 0.0018(15) 0.0152(17)
C38 0.101(13) 0.071(10) 0.033(5) 0.000(7) 0.008(7) 0.049(9)
C37A 0.056(2) 0.048(2) 0.0308(16) -0.0024(15) 0.0018(15) 0.0152(17)
C38A 0.077(8) 0.073(8) 0.042(5) 0.010(6) 0.009(5) 0.043(6)
_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 N3 2.175(2) . ?
Re1 N4 2.188(2) . ?
Re1 C1 2.115(3) . ?
Re1 C2 2.097(3) . ?
Re1 C3 1.886(3) . ?
Re1 C4 1.881(3) . ?
O1 C3 1.172(4) . ?
O2 C4 1.174(4) . ?
N1 C1 1.154(4) . ?
N2 C2 1.155(4) . ?
N3 C5 1.330(3) . ?
N3 C9 1.367(3) . ?
N4 C10 1.359(3) . ?
N4 C14 1.330(4) . ?
N5 C23 1.518(3) . ?
N5 C27 1.523(3) . ?
N5 C31 1.524(3) . ?
N5 C35 1.524(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.396(4) . ?
C7 C8 1.398(4) . ?
C7 C15 1.530(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.393(4) . ?
C9 C10 1.471(4) . ?
C10 C11 1.389(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.392(4) . ?
C12 C13 1.395(4) . ?
C12 C19 1.530(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.532(4) . ?
C15 C17 1.532(4) . ?
C15 C18 1.536(5) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.534(5) . ?
C19 C21 1.525(5) . ?
C19 C22 1.528(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.525(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.517(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.521(5) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.522(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.521(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.499(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.516(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.521(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.514(5) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.530(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 H36C 0.9900 . ?
C36 H36D 0.9900 . ?
C36 C37 1.508(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.525(13) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38A H38D 0.9800 . ?
C38A H38E 0.9800 . ?
C38A H38F 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
N3 Re1 N4 74.09(8) . . ?
C1 Re1 N3 86.22(10) . . ?
C1 Re1 N4 86.95(10) . . ?
C2 Re1 N3 87.24(9) . . ?
C2 Re1 N4 85.04(9) . . ?
C2 Re1 C1 170.80(10) . . ?
C3 Re1 N3 96.91(10) . . ?
C3 Re1 N4 170.69(10) . . ?
C3 Re1 C1 94.93(11) . . ?
C3 Re1 C2 92.28(11) . . ?
C4 Re1 N3 171.73(10) . . ?
C4 Re1 N4 97.66(10) . . ?
C4 Re1 C1 94.06(12) . . ?
C4 Re1 C2 91.48(11) . . ?
C4 Re1 C3 91.31(12) . . ?
C5 N3 Re1 124.21(17) . . ?
C5 N3 C9 117.9(2) . . ?
C9 N3 Re1 117.90(17) . . ?
C10 N4 Re1 117.68(17) . . ?
C14 N4 Re1 124.27(18) . . ?
C14 N4 C10 118.0(2) . . ?
C23 N5 C27 106.9(2) . . ?
C23 N5 C31 110.9(2) . . ?
C23 N5 C35 111.1(2) . . ?
C27 N5 C31 110.2(2) . . ?
C27 N5 C35 110.6(2) . . ?
C31 N5 C35 107.2(2) . . ?
N1 C1 Re1 176.9(3) . . ?
N2 C2 Re1 178.0(2) . . ?
O1 C3 Re1 176.8(2) . . ?
O2 C4 Re1 177.2(2) . . ?
N3 C5 H5 118.4 . . ?
N3 C5 C6 123.3(2) . . ?
C6 C5 H5 118.4 . . ?
C5 C6 H6 119.8 . . ?
C5 C6 C7 120.3(2) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C8 116.2(3) . . ?
C6 C7 C15 122.9(3) . . ?
C8 C7 C15 120.9(2) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 C7 121.0(2) . . ?
C9 C8 H8 119.5 . . ?
N3 C9 C8 121.4(2) . . ?
N3 C9 C10 115.0(2) . . ?
C8 C9 C10 123.6(2) . . ?
N4 C10 C9 115.2(2) . . ?
N4 C10 C11 121.4(2) . . ?
C11 C10 C9 123.5(2) . . ?
C10 C11 H11 119.5 . . ?
C10 C11 C12 120.9(3) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 C13 116.3(3) . . ?
C11 C12 C19 120.6(3) . . ?
C13 C12 C19 123.1(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
N4 C14 C13 123.3(3) . . ?
N4 C14 H14 118.4 . . ?
C13 C14 H14 118.4 . . ?
C7 C15 C16 112.2(2) . . ?
C7 C15 C17 109.1(2) . . ?
C7 C15 C18 108.7(2) . . ?
C16 C15 C17 109.0(3) . . ?
C16 C15 C18 108.7(3) . . ?
C17 C15 C18 109.1(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C12 C19 C20 110.1(3) . . ?
C21 C19 C12 108.0(3) . . ?
C21 C19 C20 109.3(3) . . ?
C21 C19 C22 109.9(3) . . ?
C22 C19 C12 111.3(3) . . ?
C22 C19 C20 108.3(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N5 C23 H23A 108.6 . . ?
N5 C23 H23B 108.6 . . ?
N5 C23 C24 114.9(2) . . ?
H23A C23 H23B 107.5 . . ?
C24 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
C25 C24 C23 110.5(2) . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
C24 C25 H25A 109.2 . . ?
C24 C25 H25B 109.2 . . ?
C24 C25 C26 111.9(3) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N5 C27 H27A 108.7 . . ?
N5 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
C28 C27 N5 114.4(2) . . ?
C28 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 108.1 . . ?
C29 C28 C27 110.6(3) . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C28 C29 H29A 109.2 . . ?
C28 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
C30 C29 C28 112.0(3) . . ?
C30 C29 H29A 109.2 . . ?
C30 C29 H29B 109.2 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 H31A 108.6 . . ?
N5 C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 N5 114.6(2) . . ?
C32 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 C33 110.5(2) . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 H32A 109.6 . . ?
C33 C32 H32B 109.5 . . ?
C32 C33 H33A 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 C32 111.9(3) . . ?
C34 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N5 C35 H35A 108.5 . . ?
N5 C35 H35B 108.5 . . ?
N5 C35 C36 115.1(2) . . ?
H35A C35 H35B 107.5 . . ?
C36 C35 H35A 108.5 . . ?
C36 C35 H35B 108.5 . . ?
C35 C36 H36A 109.2 . . ?
C35 C36 H36B 109.2 . . ?
C35 C36 H36C 109.2 . . ?
C35 C36 H36D 109.2 . . ?
H36A C36 H36B 107.9 . . ?
H36A C36 H36C 0.0 . . ?
H36A C36 H36D 107.9 . . ?
H36B C36 H36C 107.9 . . ?
H36B C36 H36D 0.0 . . ?
H36C C36 H36D 107.9 . . ?
C37 C36 C35 112.0(3) . . ?
C37 C36 H36A 109.2 . . ?
C37 C36 H36B 109.2 . . ?
C37 C36 H36C 109.2 . . ?
C37 C36 H36D 109.2 . . ?
C36 C37 H37A 106.5 . . ?
C36 C37 H37B 106.5 . . ?
C36 C37 C38 123.2(7) . . ?
H37A C37 H37B 106.5 . . ?
C38 C37 H37A 106.5 . . ?
C38 C37 H37B 106.5 . . ?
H38D C38A H38E 109.5 . . ?
H38D C38A H38F 109.5 . . ?
H38E C38A H38F 109.5 . . ?


data_100312a_larry
_database_code_depnum_ccdc_archive 'CCDC 916505'
#TrackingRef '4.cif'
_audit_creation_date             2012-12-08
_audit_creation_method           
;
Olex2 1.1
(compiled 2011.08.18 svn.r1932, GUI svn.r3819)
;
_chemical_name_common            ?
_chemical_name_systematic        
;
?
;
_chemical_formula_moiety         'C16 H8 N4 O2 Re, H2 O, C16 H36 N'
_chemical_formula_sum            'C32 H46 N5 O3 Re'
_chemical_formula_weight         734.94
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 S O2'
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'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 '-x, y+1/2, -z+1/2'
4 'x+1/2, -y+1/2, -z'
_cell_length_a                   9.9402(2)
_cell_length_b                   15.3605(2)
_cell_length_c                   21.5569(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3291.45(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9491
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.3329
_cell_measurement_theta_min      3.5302
_exptl_absorpt_coefficient_mu    7.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
?
;
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12936
_diffrn_reflns_theta_full        71.47
_diffrn_reflns_theta_max         71.47
_diffrn_reflns_theta_min         3.53
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
1 omega -13.00 14.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 -60.0000 27
#__ type_ start__ end____ width___ exp.time_
2 omega -19.00 29.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -99.0000 -180.0000 48
#__ type_ start__ end____ width___ exp.time_
3 omega 24.00 55.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 -60.0000 31
#__ type_ start__ end____ width___ exp.time_
4 omega -125.00 -25.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 -77.0000 60.0000 100
#__ type_ start__ end____ width___ exp.time_
5 omega 80.00 106.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 109.0000 35.0000 26
#__ type_ start__ end____ width___ exp.time_
6 omega 99.00 125.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 109.0000 59.0000 26
#__ type_ start__ end____ width___ exp.time_
7 omega 66.00 95.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 -125.0000 -90.0000 29
#__ type_ start__ end____ width___ exp.time_
8 omega 57.00 87.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -111.0000 30.0000 30
#__ type_ start__ end____ width___ exp.time_
9 omega 38.00 63.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -37.0000 -150.0000 25
#__ type_ start__ end____ width___ exp.time_
10 omega 49.00 79.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 30.0000 30
#__ type_ start__ end____ width___ exp.time_
11 omega 37.00 65.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -120.0000 28
#__ type_ start__ end____ width___ exp.time_
12 omega 43.00 69.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -25.0000 -150.0000 26
#__ type_ start__ end____ width___ exp.time_
13 omega 38.00 64.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -37.0000 -30.0000 26
#__ type_ start__ end____ width___ exp.time_
14 omega 40.00 68.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -37.0000 -60.0000 28
#__ type_ start__ end____ width___ exp.time_
15 omega 64.00 90.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -111.0000 90.0000 26
#__ type_ start__ end____ width___ exp.time_
16 omega 41.00 68.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -109.0000 143.0000 27
#__ type_ start__ end____ width___ exp.time_
17 omega 89.00 156.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 25.0000 0.0000 67
#__ type_ start__ end____ width___ exp.time_
18 omega -16.00 47.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -109.0000 120.0000 63
#__ type_ start__ end____ width___ exp.time_
19 omega -25.00 42.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -99.0000 -60.0000 67
#__ type_ start__ end____ width___ exp.time_
20 omega -125.00 -74.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 -157.0000 -120.0000 51
#__ type_ start__ end____ width___ exp.time_
21 omega -124.00 -34.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 -57.0000 -180.0000 90
#__ type_ start__ end____ width___ exp.time_
22 omega -124.00 -34.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- -55.0000 -57.0000 -90.0000 90
#__ type_ start__ end____ width___ exp.time_
23 omega 73.00 126.00 1.0000 24.0000
omega____ theta____ kappa____ phi______ frames
- 55.0000 125.0000 -90.0000 53
#__ type_ start__ end____ width___ exp.time_
24 omega 40.00 83.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -50.0000 150.0000 43
#__ type_ start__ end____ width___ exp.time_
25 omega 38.00 59.00 1.0000 48.0000
omega____ theta____ kappa____ phi______ frames
- 110.0000 -37.0000 0.0000 21
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0282515000
_diffrn_orient_matrix_UB_12      -0.0234082000
_diffrn_orient_matrix_UB_13      -0.0682869000
_diffrn_orient_matrix_UB_21      0.0271183000
_diffrn_orient_matrix_UB_22      0.0966556000
_diffrn_orient_matrix_UB_23      -0.0144047000
_diffrn_orient_matrix_UB_31      0.1498880000
_diffrn_orient_matrix_UB_32      -0.0130805000
_diffrn_orient_matrix_UB_33      0.0154787000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5631
_reflns_number_total             5694
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.022(11)
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         5694
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0297
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+3.6085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0847
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.33177(2) 0.971144(13) 0.446287(9) 0.02203(8) Uani 1 1 d . . .
O1 O 0.6157(4) 1.0371(3) 0.4723(2) 0.0489(11) Uani 1 1 d . . .
O2 O 0.2193(5) 1.1566(2) 0.4521(2) 0.0468(11) Uani 1 1 d . . .
O3 O 0.0570(4) 0.9531(3) 0.68394(17) 0.0396(10) Uani 1 1 d . . .
H3A H 0.0829 0.9776 0.7172 0.048 Uiso 1 1 d R . .
H3B H 0.1232 0.9505 0.6591 0.048 Uiso 1 1 d R . .
N1 N 0.2689(5) 0.9377(3) 0.5928(2) 0.0382(11) Uani 1 1 d . . .
N2 N 0.3766(6) 0.9674(3) 0.2979(2) 0.0452(13) Uani 1 1 d . . .
N3 N 0.3948(4) 0.8354(3) 0.43968(18) 0.0238(8) Uani 1 1 d . . .
N4 N 0.1464(4) 0.8982(3) 0.42550(17) 0.0231(8) Uani 1 1 d . . .
N5 N 0.4429(4) 0.7571(2) 0.16424(19) 0.0219(8) Uani 1 1 d . . .
C1 C 0.2899(4) 0.9510(3) 0.5415(2) 0.0215(9) Uani 1 1 d U . .
C2 C 0.3652(5) 0.9714(3) 0.3487(2) 0.0250(9) Uani 1 1 d . . .
C3 C 0.2608(6) 1.0857(4) 0.4491(3) 0.0335(11) Uani 1 1 d . . .
C4 C 0.5054(6) 1.0145(3) 0.4626(2) 0.0311(11) Uani 1 1 d . . .
C5 C 0.5217(5) 0.8060(4) 0.4452(3) 0.0312(10) Uani 1 1 d . . .
H5 H 0.5913 0.8465 0.4542 0.037 Uiso 1 1 calc R . .
C6 C 0.5547(6) 0.7187(4) 0.4382(3) 0.0389(13) Uani 1 1 d . . .
H6 H 0.6456 0.7005 0.4427 0.047 Uiso 1 1 calc R . .
C7 C 0.4573(6) 0.6588(4) 0.4248(3) 0.0372(13) Uani 1 1 d . . .
H7 H 0.4794 0.5990 0.4200 0.045 Uiso 1 1 calc R . .
C8 C 0.3231(7) 0.6877(3) 0.4181(2) 0.0322(11) Uani 1 1 d . . .
C9 C 0.2134(7) 0.6307(4) 0.4042(3) 0.0420(15) Uani 1 1 d . . .
H9 H 0.2300 0.5702 0.3990 0.050 Uiso 1 1 calc R . .
C10 C 0.0866(7) 0.6613(4) 0.3983(3) 0.0396(14) Uani 1 1 d . . .
H10 H 0.0155 0.6218 0.3897 0.048 Uiso 1 1 calc R . .
C11 C 0.0573(6) 0.7531(4) 0.4049(2) 0.0337(12) Uani 1 1 d . . .
C12 C -0.0714(6) 0.7892(4) 0.3992(3) 0.0368(13) Uani 1 1 d . . .
H12 H -0.1464 0.7529 0.3905 0.044 Uiso 1 1 calc R . .
C13 C -0.0885(6) 0.8765(5) 0.4062(3) 0.0392(14) Uani 1 1 d . . .
H13 H -0.1756 0.9015 0.4023 0.047 Uiso 1 1 calc R . .
C14 C 0.0236(5) 0.9301(3) 0.4193(2) 0.0301(11) Uani 1 1 d . . .
H14 H 0.0103 0.9910 0.4238 0.036 Uiso 1 1 calc R . .
C15 C 0.1644(6) 0.8109(3) 0.4183(2) 0.0250(9) Uani 1 1 d . . .
C16 C 0.2971(5) 0.7772(3) 0.4255(2) 0.0259(11) Uani 1 1 d . . .
C17 C 0.3906(5) 0.6644(3) 0.1570(2) 0.0250(10) Uani 1 1 d . . .
H17A H 0.3269 0.6633 0.1217 0.030 Uiso 1 1 calc R . .
H17B H 0.4673 0.6263 0.1460 0.030 Uiso 1 1 calc R . .
C18 C 0.3213(6) 0.6261(3) 0.2127(2) 0.0283(10) Uani 1 1 d . . .
H18A H 0.2469 0.6646 0.2261 0.034 Uiso 1 1 calc R . .
H18B H 0.3858 0.6204 0.2474 0.034 Uiso 1 1 calc R . .
C19 C 0.2657(6) 0.5362(4) 0.1951(3) 0.0373(12) Uani 1 1 d . . .
H19A H 0.1965 0.5431 0.1624 0.045 Uiso 1 1 calc R . .
H19B H 0.3394 0.5001 0.1779 0.045 Uiso 1 1 calc R . .
C20 C 0.2038(6) 0.4895(4) 0.2506(3) 0.0428(14) Uani 1 1 d . . .
H20A H 0.1778 0.4304 0.2385 0.064 Uiso 1 1 calc R . .
H20B H 0.1241 0.5215 0.2647 0.064 Uiso 1 1 calc R . .
H20C H 0.2698 0.4867 0.2843 0.064 Uiso 1 1 calc R . .
C21 C 0.3309(6) 0.8187(3) 0.1850(2) 0.0262(10) Uani 1 1 d . . .
H21A H 0.3009 0.8012 0.2270 0.031 Uiso 1 1 calc R . .
H21B H 0.3682 0.8783 0.1881 0.031 Uiso 1 1 calc R . .
C22 C 0.2095(5) 0.8210(4) 0.1426(3) 0.0326(12) Uani 1 1 d . . .
H22A H 0.1759 0.7610 0.1360 0.039 Uiso 1 1 calc R . .
H22B H 0.2360 0.8451 0.1018 0.039 Uiso 1 1 calc R . .
C23 C 0.0980(5) 0.8766(4) 0.1703(3) 0.0328(12) Uani 1 1 d . . .
H23A H 0.1326 0.9359 0.1785 0.039 Uiso 1 1 calc R . .
H23B H 0.0688 0.8511 0.2103 0.039 Uiso 1 1 calc R . .
C24 C -0.0226(6) 0.8820(4) 0.1260(3) 0.0426(14) Uani 1 1 d . . .
H24A H 0.0054 0.9096 0.0872 0.064 Uiso 1 1 calc R . .
H24B H -0.0942 0.9166 0.1453 0.064 Uiso 1 1 calc R . .
H24C H -0.0561 0.8232 0.1174 0.064 Uiso 1 1 calc R . .
C25 C 0.5530(5) 0.7602(3) 0.2131(2) 0.0263(10) Uani 1 1 d . . .
H25A H 0.5820 0.8215 0.2182 0.032 Uiso 1 1 calc R . .
H25B H 0.5143 0.7411 0.2532 0.032 Uiso 1 1 calc R . .
C26 C 0.6757(6) 0.7054(3) 0.1996(2) 0.0310(10) Uani 1 1 d . . .
H26A H 0.7155 0.7237 0.1596 0.037 Uiso 1 1 calc R . .
H26B H 0.6487 0.6435 0.1958 0.037 Uiso 1 1 calc R . .
C27 C 0.7805(6) 0.7145(4) 0.2510(3) 0.0381(13) Uani 1 1 d . . .
H27A H 0.8088 0.7762 0.2543 0.046 Uiso 1 1 calc R . .
H27B H 0.7403 0.6971 0.2912 0.046 Uiso 1 1 calc R . .
C28 C 0.9030(7) 0.6576(5) 0.2375(4) 0.0531(17) Uani 1 1 d . . .
H28A H 0.9417 0.6741 0.1974 0.080 Uiso 1 1 calc R . .
H28B H 0.8756 0.5964 0.2363 0.080 Uiso 1 1 calc R . .
H28C H 0.9704 0.6659 0.2702 0.080 Uiso 1 1 calc R . .
C29 C 0.4957(5) 0.7829(3) 0.1012(2) 0.0231(9) Uani 1 1 d . . .
H29A H 0.4187 0.7870 0.0722 0.028 Uiso 1 1 calc R . .
H29B H 0.5553 0.7360 0.0859 0.028 Uiso 1 1 calc R . .
C30 C 0.5737(5) 0.8691(3) 0.0989(2) 0.0275(10) Uani 1 1 d . . .
H30A H 0.5314 0.9117 0.1273 0.033 Uiso 1 1 calc R . .
H30B H 0.6673 0.8594 0.1129 0.033 Uiso 1 1 calc R . .
C31 C 0.5746(5) 0.9058(3) 0.0329(2) 0.0281(10) Uani 1 1 d . . .
H31A H 0.4824 0.9252 0.0224 0.034 Uiso 1 1 calc R . .
H31B H 0.6337 0.9576 0.0319 0.034 Uiso 1 1 calc R . .
C32 C 0.6219(6) 0.8419(4) -0.0164(3) 0.0342(12) Uani 1 1 d . . .
H32A H 0.6257 0.8714 -0.0567 0.051 Uiso 1 1 calc R . .
H32B H 0.5589 0.7930 -0.0188 0.051 Uiso 1 1 calc R . .
H32C H 0.7116 0.8203 -0.0056 0.051 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.02373(11) 0.02202(11) 0.02035(11) -0.00090(8) 0.00190(8) -0.00442(8)
O1 0.036(2) 0.069(3) 0.042(2) 0.000(2) -0.0058(18) -0.021(2)
O2 0.051(2) 0.0230(19) 0.066(3) -0.001(2) 0.020(2) -0.0029(17)
O3 0.039(2) 0.055(3) 0.0242(17) -0.0075(18) 0.0002(15) -0.003(2)
N1 0.046(3) 0.045(3) 0.024(2) -0.008(2) -0.001(2) -0.009(2)
N2 0.076(4) 0.031(2) 0.029(2) 0.002(2) -0.007(2) -0.008(3)
N3 0.031(2) 0.0230(19) 0.0175(18) 0.0015(16) 0.0022(17) 0.0016(16)
N4 0.021(2) 0.029(2) 0.0190(16) -0.0007(15) 0.0008(15) 0.0011(17)
N5 0.0219(18) 0.0194(18) 0.0245(19) -0.0044(16) -0.0010(16) -0.0008(15)
C1 0.0151(18) 0.028(2) 0.022(2) 0.0038(17) 0.0059(15) -0.0150(16)
C2 0.023(2) 0.029(2) 0.022(2) 0.000(2) 0.0007(16) -0.0060(19)
C3 0.036(3) 0.029(3) 0.035(3) -0.001(3) 0.007(3) -0.005(2)
C4 0.036(3) 0.033(3) 0.024(2) 0.003(2) 0.004(2) -0.014(2)
C5 0.025(2) 0.043(3) 0.025(2) 0.005(2) 0.004(2) 0.003(2)
C6 0.040(3) 0.046(3) 0.031(3) 0.010(3) 0.012(2) 0.021(3)
C7 0.048(3) 0.033(3) 0.031(3) 0.001(2) 0.012(2) 0.013(3)
C8 0.050(3) 0.025(2) 0.022(2) 0.0013(19) 0.010(2) 0.004(3)
C9 0.068(4) 0.023(3) 0.036(3) -0.003(2) 0.002(3) -0.003(3)
C10 0.058(4) 0.029(3) 0.032(3) -0.003(2) 0.002(3) -0.021(3)
C11 0.041(3) 0.036(3) 0.025(2) -0.001(2) 0.000(2) -0.012(2)
C12 0.032(3) 0.048(3) 0.030(3) 0.004(3) -0.003(2) -0.015(3)
C13 0.021(3) 0.061(4) 0.035(3) 0.007(3) -0.004(2) -0.005(3)
C14 0.032(3) 0.029(2) 0.030(2) 0.000(2) -0.002(2) 0.005(2)
C15 0.031(2) 0.028(2) 0.0167(19) -0.0013(18) 0.000(2) -0.007(2)
C16 0.036(3) 0.023(2) 0.018(2) 0.0002(18) 0.0042(18) 0.003(2)
C17 0.026(2) 0.020(2) 0.030(2) -0.0031(19) -0.003(2) -0.0026(19)
C18 0.026(2) 0.026(2) 0.033(2) 0.001(2) -0.002(2) -0.002(2)
C19 0.046(3) 0.024(2) 0.042(3) 0.001(2) -0.002(2) -0.004(2)
C20 0.037(3) 0.034(3) 0.057(4) 0.008(3) 0.012(3) -0.009(2)
C21 0.027(2) 0.022(2) 0.029(2) -0.0058(18) 0.002(2) 0.001(2)
C22 0.029(3) 0.035(3) 0.033(3) -0.005(2) -0.002(2) 0.006(2)
C23 0.026(3) 0.030(3) 0.042(3) -0.001(2) 0.005(2) 0.006(2)
C24 0.030(3) 0.048(3) 0.051(3) -0.001(3) 0.000(3) 0.003(3)
C25 0.026(2) 0.028(2) 0.025(2) -0.004(2) -0.0086(19) -0.007(2)
C26 0.031(3) 0.026(2) 0.035(3) 0.002(2) -0.008(2) 0.000(2)
C27 0.033(3) 0.037(3) 0.044(3) 0.004(3) -0.014(2) 0.001(2)
C28 0.039(3) 0.054(4) 0.066(4) 0.005(4) -0.024(3) 0.004(3)
C29 0.018(2) 0.027(2) 0.024(2) -0.0042(18) -0.0001(19) 0.002(2)
C30 0.021(2) 0.029(3) 0.032(3) -0.003(2) -0.002(2) -0.003(2)
C31 0.025(2) 0.027(2) 0.032(2) -0.001(2) 0.0061(19) 0.000(2)
C32 0.039(3) 0.029(3) 0.034(3) 0.000(2) 0.011(2) 0.002(2)
_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 N3 2.182(4) . ?
Re1 N4 2.203(4) . ?
Re1 C1 2.116(4) . ?
Re1 C2 2.129(4) . ?
Re1 C3 1.897(6) . ?
Re1 C4 1.883(6) . ?
O1 C4 1.168(7) . ?
O2 C3 1.166(7) . ?
O3 H3A 0.8503 . ?
O3 H3B 0.8501 . ?
N1 C1 1.144(7) . ?
N2 C2 1.103(7) . ?
N3 C5 1.346(7) . ?
N3 C16 1.355(7) . ?
N4 C14 1.322(7) . ?
N4 C15 1.361(6) . ?
N5 C17 1.524(6) . ?
N5 C21 1.528(6) . ?
N5 C25 1.520(6) . ?
N5 C29 1.510(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.389(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.367(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.413(9) . ?
C8 C9 1.430(9) . ?
C8 C16 1.409(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.351(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.448(9) . ?
C11 C12 1.399(9) . ?
C11 C15 1.415(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.361(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.414(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.425(8) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.504(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.535(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.525(8) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.514(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.521(7) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.534(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.511(7) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.528(7) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.527(9) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.535(7) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.529(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.521(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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
N3 Re1 N4 74.95(16) . . ?
C1 Re1 N3 88.86(17) . . ?
C1 Re1 N4 87.62(15) . . ?
C1 Re1 C2 171.33(19) . . ?
C2 Re1 N3 83.81(18) . . ?
C2 Re1 N4 86.01(16) . . ?
C3 Re1 N3 174.5(2) . . ?
C3 Re1 N4 99.7(2) . . ?
C3 Re1 C1 91.8(2) . . ?
C3 Re1 C2 95.1(2) . . ?
C4 Re1 N3 95.0(2) . . ?
C4 Re1 N4 169.9(2) . . ?
C4 Re1 C1 92.91(18) . . ?
C4 Re1 C2 92.34(18) . . ?
C4 Re1 C3 90.4(2) . . ?
H3A O3 H3B 108.5 . . ?
C5 N3 Re1 125.7(3) . . ?
C5 N3 C16 118.1(4) . . ?
C16 N3 Re1 116.1(3) . . ?
C14 N4 Re1 127.1(3) . . ?
C14 N4 C15 118.4(5) . . ?
C15 N4 Re1 114.5(4) . . ?
C17 N5 C21 111.1(4) . . ?
C25 N5 C17 110.3(4) . . ?
C25 N5 C21 107.6(4) . . ?
C29 N5 C17 105.8(4) . . ?
C29 N5 C21 110.7(4) . . ?
C29 N5 C25 111.4(4) . . ?
N1 C1 Re1 178.0(5) . . ?
N2 C2 Re1 175.5(5) . . ?
O2 C3 Re1 178.3(6) . . ?
O1 C4 Re1 176.4(5) . . ?
N3 C5 H5 118.8 . . ?
N3 C5 C6 122.4(5) . . ?
C6 C5 H5 118.8 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.4(5) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.7 . . ?
C6 C7 C8 118.6(5) . . ?
C8 C7 H7 120.7 . . ?
C7 C8 C9 123.3(5) . . ?
C16 C8 C7 117.9(6) . . ?
C16 C8 C9 118.8(6) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.2(5) . . ?
C10 C9 H9 119.4 . . ?
C9 C10 H10 119.4 . . ?
C9 C10 C11 121.2(6) . . ?
C11 C10 H10 119.4 . . ?
C12 C11 C10 124.1(5) . . ?
C12 C11 C15 117.2(5) . . ?
C15 C11 C10 118.6(6) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 C11 119.6(5) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 H13 120.1 . . ?
C12 C13 C14 119.8(6) . . ?
C14 C13 H13 120.1 . . ?
N4 C14 C13 122.1(5) . . ?
N4 C14 H14 118.9 . . ?
C13 C14 H14 118.9 . . ?
N4 C15 C11 122.8(5) . . ?
N4 C15 C16 117.8(5) . . ?
C11 C15 C16 119.4(5) . . ?
N3 C16 C8 122.6(5) . . ?
N3 C16 C15 116.7(4) . . ?
C8 C16 C15 120.8(5) . . ?
N5 C17 H17A 108.3 . . ?
N5 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C18 C17 N5 116.1(4) . . ?
C18 C17 H17A 108.3 . . ?
C18 C17 H17B 108.3 . . ?
C17 C18 H18A 110.0 . . ?
C17 C18 H18B 110.0 . . ?
C17 C18 C19 108.6(4) . . ?
H18A C18 H18B 108.3 . . ?
C19 C18 H18A 110.0 . . ?
C19 C18 H18B 110.0 . . ?
C18 C19 H19A 109.2 . . ?
C18 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 C18 111.9(5) . . ?
C20 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N5 C21 H21A 108.6 . . ?
N5 C21 H21B 108.6 . . ?
H21A C21 H21B 107.6 . . ?
C22 C21 N5 114.8(4) . . ?
C22 C21 H21A 108.6 . . ?
C22 C21 H21B 108.6 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 C23 110.9(4) . . ?
H22A C22 H22B 108.1 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 C24 110.8(5) . . ?
H23A C23 H23B 108.1 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N5 C25 H25A 108.4 . . ?
N5 C25 H25B 108.4 . . ?
H25A C25 H25B 107.5 . . ?
C26 C25 N5 115.4(4) . . ?
C26 C25 H25A 108.4 . . ?
C26 C25 H25B 108.4 . . ?
C25 C26 H26A 109.4 . . ?
C25 C26 H26B 109.4 . . ?
C25 C26 C27 111.0(4) . . ?
H26A C26 H26B 108.0 . . ?
C27 C26 H26A 109.4 . . ?
C27 C26 H26B 109.4 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C28 C27 C26 110.6(5) . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N5 C29 H29A 108.4 . . ?
N5 C29 H29B 108.4 . . ?
N5 C29 C30 115.6(4) . . ?
H29A C29 H29B 107.4 . . ?
C30 C29 H29A 108.4 . . ?
C30 C29 H29B 108.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 108.1 . . ?
C31 C30 C29 110.5(4) . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C30 C31 H31A 108.6 . . ?
C30 C31 H31B 108.6 . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 C30 114.5(4) . . ?
C32 C31 H31A 108.6 . . ?
C32 C31 H31B 108.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?