Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'J. Dilworth'
'Andrew R Cowley'
'Maria Salichou'

_publ_contact_author_name        J.Dilworth
_publ_contact_author_address     
;
Inorganic Chemical Laboratory
University of Oxford
South Parks Road
OXFORD
OX1 3QR
UNITED KINGDOM
;

_publ_contact_author_email       JON.DILWORTH@CHEMISTRY.OXFORD.AC.UK

_publ_requested_journal          'Dalton Transactions'

_publ_section_title              
;
Syntheses and structures of pyrazolylmethane complexes
of rhenium(III), (IV) and (V).
;

# Attachment 'Complex_3_Fig_3.cif'

data_arc1273
_database_code_depnum_ccdc_archive 'CCDC 629316'
#=============================================================
# Diffractometer details
#=============================================================
_diffrn_measurement_device_type  
;
Nonius KappaCCD
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
#=============================================================
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'

_chemical_name_systematic        # IUPAC name, in full
;
?
;
_chemical_melting_point          ?
_exptl_crystal_thermal_history   
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_special_details          
;
The hydrogen atom H1 was located in a difference Fourier map and its coordinates
and isotropic displacement parameter subsequently refined. All other hydrogen
atoms were positioned geometrically.
;
#=============================================================

_cell_length_a                   9.7300(3)
_cell_angle_alpha                90
_cell_length_b                   13.4343(5)
_cell_angle_beta                 95.9521(16)
_cell_length_c                   10.8514(4)
_cell_angle_gamma                90
_cell_volume                     1410.80(9)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Re ' -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417
52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            2
_chemical_formula_sum            ' C20 H20 Cl4 N12 O3 Re2 '
_chemical_formula_moiety         ' C20 H20 Cl4 N12 O3 Re2 '
_chemical_compound_source        
;
synthesis as described
;
_chemical_formula_weight         990.67

_cell_measurement_reflns_used    10485
_cell_measurement_theta_min      5
_cell_measurement_theta_max      28
_cell_measurement_temperature    150

_exptl_crystal_description       ' tablet '
_exptl_crystal_colour            ' dark blue '
_exptl_crystal_size_min          0.06
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_max          0.12

_exptl_crystal_density_diffrn    2.332
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             932
_exptl_absorpt_coefficient_mu    9.000

_diffrn_measurement_method       \w

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_T_max  0.58

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            10485
_reflns_number_total             3189
#3329 unique reflections including absences
_diffrn_reflns_av_R_equivalents  0.076

_diffrn_reflns_theta_min         5.126
_diffrn_reflns_theta_max         27.467
_diffrn_measured_fraction_theta_max 0.994

_diffrn_reflns_theta_full        27.467
_diffrn_measured_fraction_theta_full 0.994

_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              17
_reflns_limit_l_min              0
_reflns_limit_l_max              14

_refine_diff_density_min         -1.37
_refine_diff_density_max         1.18

_refine_ls_number_reflns         1832
_refine_ls_number_restraints     0
_refine_ls_number_parameters     191

#_refine_ls_R_factor_ref 0.0312
_refine_ls_wR_factor_ref         0.0311
_refine_ls_goodness_of_fit_ref   1.1131

#_reflns_number_all 3189
_refine_ls_R_factor_all          0.0781
_refine_ls_wR_factor_all         0.0703

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                1832
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_gt          0.0311

_refine_ls_shift/su_max          0.029903
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.176 0.0105 0.0190
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
Re1 Re 0.15885(3) 0.01486(2) 0.11982(3) 0.0238 1.0000 Uani .
Cl1 Cl 0.0936(2) -0.13706(17) 0.2136(2) 0.0351 1.0000 Uani .
Cl2 Cl 0.0156(2) 0.10905(17) 0.2463(2) 0.0326 1.0000 Uani .
O1 O 0.0000 0.0000 0.0000 0.0227 1.0000 Uani S
O2 O 0.3021(6) 0.0322(5) 0.2183(5) 0.0338 1.0000 Uani .
N1 N 0.2721(7) -0.0661(5) -0.0015(6) 0.0245 1.0000 Uani .
N2 N 0.3129(6) -0.0272(5) -0.1090(6) 0.0234 1.0000 Uani .
C1 C 0.3374(9) -0.1527(7) 0.0153(8) 0.0316 1.0000 Uani .
C2 C 0.4208(9) -0.1708(7) -0.0789(9) 0.0322 1.0000 Uani .
C3 C 0.3996(9) -0.0906(7) -0.1566(8) 0.0314 1.0000 Uani .
N3 N 0.2003(7) 0.1454(5) 0.0235(7) 0.0275 1.0000 Uani .
N4 N 0.2516(7) 0.1468(5) -0.0901(6) 0.0257 1.0000 Uani .
C4 C 0.2064(9) 0.2402(7) 0.0634(9) 0.0307 1.0000 Uani .
C5 C 0.2569(11) 0.3018(7) -0.0267(10) 0.0395 1.0000 Uani .
C6 C 0.2833(10) 0.2399(7) -0.1223(9) 0.0374 1.0000 Uani .
N5 N 0.4092(8) 0.1006(7) -0.3029(7) 0.0405 1.0000 Uani .
N6 N 0.2757(8) 0.0761(6) -0.2868(7) 0.0319 1.0000 Uani .
C7 C 0.4061(11) 0.1087(8) -0.4268(10) 0.0443 1.0000 Uani .
C8 C 0.2752(12) 0.0902(8) -0.4884(9) 0.0441 1.0000 Uani .
C9 C 0.1929(10) 0.0691(7) -0.3979(9) 0.0331 1.0000 Uani .
C10 C 0.2352(8) 0.0573(6) -0.1672(7) 0.0228 1.0000 Uani .
H1 H 0.145(8) 0.042(5) -0.179(6) 0.040(17) 1.0000 Uiso .
H11 H 0.3279 -0.1987 0.0863 0.0380 1.0000 Uiso .
H21 H 0.4822 -0.2294 -0.0881 0.0382 1.0000 Uiso .
H31 H 0.4422 -0.0809 -0.2358 0.0379 1.0000 Uiso .
H41 H 0.1791 0.2636 0.1449 0.0363 1.0000 Uiso .
H51 H 0.2707 0.3755 -0.0223 0.0477 1.0000 Uiso .
H61 H 0.3197 0.2605 -0.2013 0.0443 1.0000 Uiso .
H71 H 0.4886 0.1261 -0.4702 0.0542 1.0000 Uiso .
H81 H 0.2478 0.0922 -0.5798 0.0543 1.0000 Uiso .
H91 H 0.0924 0.0518 -0.4096 0.0394 1.0000 Uiso .
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 0.01958(15) 0.03231(17) 0.01989(15) 0.00029(17) 0.00405(10) 0.00084(18)
Cl1 0.0322(12) 0.0402(13) 0.0340(12) 0.0149(10) 0.0090(10) 0.0099(10)
Cl2 0.0293(11) 0.0375(12) 0.0326(12) -0.0107(9) 0.0113(9) -0.0016(9)
O1 0.018(4) 0.029(5) 0.023(4) 0.003(3) 0.008(3) -0.003(3)
O2 0.019(3) 0.057(4) 0.024(3) -0.005(3) -0.005(2) 0.000(3)
N1 0.020(4) 0.033(4) 0.021(4) 0.001(3) 0.001(3) 0.004(3)
N2 0.014(3) 0.037(4) 0.019(3) -0.001(3) 0.000(3) -0.001(3)
C1 0.031(5) 0.030(5) 0.034(5) 0.005(4) 0.005(4) 0.007(4)
C2 0.021(4) 0.041(5) 0.034(5) -0.005(4) -0.001(4) 0.010(4)
C3 0.025(5) 0.043(5) 0.027(5) -0.012(4) 0.007(4) 0.002(4)
N3 0.017(4) 0.040(4) 0.028(4) -0.003(3) 0.010(3) 0.001(3)
N4 0.029(4) 0.026(4) 0.024(4) -0.009(3) 0.012(3) -0.001(3)
C4 0.024(5) 0.028(5) 0.039(5) -0.007(4) -0.005(4) 0.004(4)
C5 0.042(6) 0.030(5) 0.047(6) -0.006(4) 0.009(5) 0.003(4)
C6 0.039(5) 0.034(5) 0.039(5) 0.009(4) 0.000(4) -0.009(4)
N5 0.023(4) 0.066(6) 0.035(5) 0.002(4) 0.014(3) -0.009(4)
N6 0.031(4) 0.042(5) 0.024(4) -0.006(3) 0.010(3) -0.006(3)
C7 0.045(6) 0.046(6) 0.044(6) -0.003(5) 0.016(5) -0.008(5)
C8 0.074(8) 0.036(5) 0.026(5) 0.001(4) 0.024(5) -0.006(5)
C9 0.036(6) 0.033(5) 0.030(5) -0.010(4) 0.001(4) -0.002(4)
C10 0.012(4) 0.034(4) 0.020(4) 0.004(3) -0.003(3) -0.004(3)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Re1 . Cl1 . 2.396(2) yes
Re1 . Cl2 . 2.413(2) yes
Re1 . O1 . 1.9242(3) yes
Re1 . O2 . 1.683(6) yes
Re1 . N1 . 2.105(7) yes
Re1 . N3 . 2.102(7) yes
N1 . N2 . 1.374(9) yes
N1 . C1 . 1.329(11) yes
N2 . C3 . 1.340(10) yes
N2 . C10 . 1.469(11) yes
C1 . C2 . 1.391(12) yes
C1 . H11 . 0.999 no
C2 . C3 . 1.371(13) yes
C2 . H21 . 1.000 no
C3 . H31 . 1.000 no
N3 . N4 . 1.378(9) yes
N3 . C4 . 1.344(11) yes
N4 . C6 . 1.343(11) yes
N4 . C10 . 1.464(11) yes
C4 . C5 . 1.408(13) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.374(14) yes
C5 . H51 . 1.000 no
C6 . H61 . 0.999 no
N5 . N6 . 1.368(10) yes
N5 . C7 . 1.347(12) yes
N6 . C9 . 1.382(12) yes
N6 . C10 . 1.418(10) yes
C7 . C8 . 1.397(15) yes
C7 . H71 . 1.000 no
C8 . C9 . 1.359(12) yes
C8 . H81 . 1.000 no
C9 . H91 . 1.000 no
C10 . H1 . 0.90(7) no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Re1 . Cl2 . 90.62(8) yes
Cl1 . Re1 . O1 . 88.22(6) yes
Cl2 . Re1 . O1 . 88.17(6) yes
Cl1 . Re1 . O2 . 95.0(2) yes
Cl2 . Re1 . O2 . 93.2(2) yes
O1 . Re1 . O2 . 176.5(2) yes
Cl1 . Re1 . N1 . 90.3(2) yes
Cl2 . Re1 . N1 . 175.72(19) yes
O1 . Re1 . N1 . 87.68(18) yes
O2 . Re1 . N1 . 90.9(3) yes
Cl1 . Re1 . N3 . 174.3(2) yes
Cl2 . Re1 . N3 . 89.83(18) yes
O1 . Re1 . N3 . 86.14(19) yes
O2 . Re1 . N3 . 90.7(3) yes
N1 . Re1 . N3 . 88.9(3) yes
Re1 . O1 . Re1 2_555 179.994 yes
Re1 . N1 . N2 . 123.4(5) yes
Re1 . N1 . C1 . 129.8(6) yes
N2 . N1 . C1 . 105.9(7) yes
N1 . N2 . C3 . 109.6(7) yes
N1 . N2 . C10 . 118.5(6) yes
C3 . N2 . C10 . 129.9(7) yes
N1 . C1 . C2 . 111.1(8) yes
N1 . C1 . H11 . 124.459 no
C2 . C1 . H11 . 124.462 no
C1 . C2 . C3 . 104.6(7) yes
C1 . C2 . H21 . 127.709 no
C3 . C2 . H21 . 127.678 no
N2 . C3 . C2 . 108.8(7) yes
N2 . C3 . H31 . 125.604 no
C2 . C3 . H31 . 125.560 no
Re1 . N3 . N4 . 124.2(5) yes
Re1 . N3 . C4 . 129.4(6) yes
N4 . N3 . C4 . 105.5(7) yes
N3 . N4 . C6 . 111.1(7) yes
N3 . N4 . C10 . 118.1(6) yes
C6 . N4 . C10 . 129.1(7) yes
N3 . C4 . C5 . 109.8(8) yes
N3 . C4 . H41 . 125.099 no
C5 . C4 . H41 . 125.051 no
C4 . C5 . C6 . 106.0(8) yes
C4 . C5 . H51 . 127.048 no
C6 . C5 . H51 . 126.964 no
N4 . C6 . C5 . 107.5(8) yes
N4 . C6 . H61 . 126.285 no
C5 . C6 . H61 . 126.193 no
N6 . N5 . C7 . 102.9(8) yes
N5 . N6 . C9 . 112.3(7) yes
N5 . N6 . C10 . 121.2(7) yes
C9 . N6 . C10 . 126.5(7) yes
N5 . C7 . C8 . 112.8(9) yes
N5 . C7 . H71 . 123.588 no
C8 . C7 . H71 . 123.591 no
C7 . C8 . C9 . 105.5(9) yes
C7 . C8 . H81 . 127.231 no
C9 . C8 . H81 . 127.224 no
N6 . C9 . C8 . 106.4(8) yes
N6 . C9 . H91 . 126.847 no
C8 . C9 . H91 . 126.779 no
N2 . C10 . N4 . 111.6(7) yes
N2 . C10 . N6 . 110.6(7) yes
N4 . C10 . N6 . 110.6(7) yes
N2 . C10 . H1 . 109(4) no
N4 . C10 . H1 . 109(4) no
N6 . C10 . H1 . 106(4) no

loop_
_geom_hbond_atom_site_label_d
_geom_hbond_atom_site_label_h
_geom_hbond_atom_site_label_a
_geom_hbond_site_symmetry_a
_geom_hbond_distance_dh
_geom_hbond_distance_ha
_geom_hbond_distance_da
_geom_hbond_angle_dha
_geom_hbond_publ_flag
C10 H1 Cl1 2_555 0.90(7) 2.64(7) 3.362(8) 137(5) yes
C10 H1 Cl2 2_555 0.90(7) 2.62(7) 3.354(9) 140(6) yes

# NB - bifurcated hydrogen bond

# Attachment 'Complex_4_Fig_4.cif'

data_ARC1138
_database_code_depnum_ccdc_archive 'CCDC 629317'
#=============================================================
# Diffractometer details
#=============================================================
_diffrn_measurement_device_type  
;
Nonius KappaCCD
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
#=============================================================
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'

_chemical_name_systematic        # IUPAC name, in full
;
?
;
_chemical_melting_point          ?
_exptl_crystal_thermal_history   
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
#=============================================================

_cell_length_a                   15.7338(2)
_cell_angle_alpha                90
_cell_length_b                   15.8808(2)
_cell_angle_beta                 106.5516(7)
_cell_length_c                   22.0122(3)
_cell_angle_gamma                90
_cell_volume                     5272.18(12)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Re ' -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417
52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            8
_chemical_formula_sum            ' C12 H12 Cl9 N6 O4 Re2 '
_chemical_formula_moiety         ' C10 H10 Cl3 N6 Re, O4 Re, 2(C H Cl3) '
_chemical_compound_source        
;
synthesis as described
;
_chemical_formula_weight         995.74

_cell_measurement_reflns_used    11977
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       ' block '
_exptl_crystal_colour            ' pale green '
_exptl_crystal_size_min          0.04
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_max          0.08

_exptl_crystal_density_diffrn    2.509
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             3688
_exptl_absorpt_coefficient_mu    10.120

_diffrn_measurement_method       \w

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_absorpt_correction_T_min  0.45
_exptl_absorpt_correction_T_max  0.67

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            52740
_reflns_number_total             11977

#12405 unique reflections including absences

_diffrn_reflns_av_R_equivalents  0.075

_diffrn_reflns_theta_min         5.107
_diffrn_reflns_theta_max         27.475
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        27.475
_diffrn_measured_fraction_theta_full 0.992

_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -20
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              20
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_refine_diff_density_min         -2.37
_refine_diff_density_max         7.46

_refine_ls_number_reflns         8182
_refine_ls_number_restraints     0
_refine_ls_number_parameters     595

#_refine_ls_R_factor_ref 0.0415
_refine_ls_wR_factor_ref         0.0489
_refine_ls_goodness_of_fit_ref   1.0792

#_reflns_number_all 11977
_refine_ls_R_factor_all          0.0640
_refine_ls_wR_factor_all         0.0697

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                8182
_refine_ls_R_factor_gt           0.0415
_refine_ls_wR_factor_gt          0.0489

_refine_ls_shift/su_max          0.003282
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.702 0.549 0.416
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
Re1 Re 0.643710(19) 0.22225(2) 0.759617(14) 0.0166 1.0000 Uani
Cl1 Cl 0.69732(14) 0.08628(12) 0.77227(11) 0.0267 1.0000 Uani
Cl2 Cl 0.70304(14) 0.25165(14) 0.67831(10) 0.0273 1.0000 Uani
Cl3 Cl 0.76338(14) 0.27402(14) 0.83621(11) 0.0287 1.0000 Uani
N1 N 0.5823(4) 0.3407(4) 0.7496(3) 0.0180 1.0000 Uani
N2 N 0.4963(4) 0.3493(4) 0.7480(3) 0.0135 1.0000 Uani
C1 C 0.6122(6) 0.4198(5) 0.7459(4) 0.0248 1.0000 Uani
C2 C 0.5431(6) 0.4769(5) 0.7405(4) 0.0264 1.0000 Uani
C3 C 0.4714(6) 0.4310(5) 0.7411(4) 0.0228 1.0000 Uani
N3 N 0.5696(4) 0.2017(4) 0.8248(3) 0.0185 1.0000 Uani
N4 N 0.4850(4) 0.2317(4) 0.8113(3) 0.0163 1.0000 Uani
C4 C 0.5855(6) 0.1595(6) 0.8789(4) 0.0308 1.0000 Uani
C5 C 0.5089(6) 0.1621(7) 0.9005(4) 0.0316 1.0000 Uani
C6 C 0.4473(6) 0.2073(6) 0.8568(4) 0.0265 1.0000 Uani
N5 N 0.5228(4) 0.1856(4) 0.6949(3) 0.0193 1.0000 Uani
N6 N 0.4442(4) 0.2172(4) 0.6999(3) 0.0185 1.0000 Uani
C7 C 0.5012(6) 0.1359(5) 0.6435(4) 0.0221 1.0000 Uani
C8 C 0.4087(6) 0.1355(6) 0.6163(4) 0.0305 1.0000 Uani
C9 C 0.3749(5) 0.1884(5) 0.6538(4) 0.0217 1.0000 Uani
C10 C 0.4454(5) 0.2739(5) 0.7513(4) 0.0181 1.0000 Uani
Re2 Re 0.149297(19) 0.40530(2) 0.259236(15) 0.0175 1.0000 Uani
Cl4 Cl 0.19796(14) 0.26775(13) 0.26367(11) 0.0286 1.0000 Uani
Cl5 Cl 0.20425(14) 0.44154(15) 0.17676(10) 0.0281 1.0000 Uani
Cl6 Cl 0.27296(14) 0.44844(14) 0.33567(10) 0.0275 1.0000 Uani
N7 N 0.0891(4) 0.5245(4) 0.2554(3) 0.0172 1.0000 Uani
N8 N 0.0031(4) 0.5309(4) 0.2567(3) 0.0173 1.0000 Uani
C11 C 0.1174(6) 0.6032(5) 0.2505(4) 0.0228 1.0000 Uani
C12 C 0.0484(6) 0.6599(6) 0.2491(4) 0.0262 1.0000 Uani
C13 C -0.0220(6) 0.6119(5) 0.2527(4) 0.0244 1.0000 Uani
N9 N 0.0807(4) 0.3822(4) 0.3276(3) 0.0193 1.0000 Uani
N10 N -0.0050(4) 0.4089(4) 0.3168(3) 0.0195 1.0000 Uani
C14 C 0.1005(7) 0.3434(7) 0.3837(5) 0.0367 1.0000 Uani
C15 C 0.0289(8) 0.3436(8) 0.4086(6) 0.0461 1.0000 Uani
C16 C -0.0372(7) 0.3864(7) 0.3648(5) 0.0342 1.0000 Uani
N11 N 0.0256(4) 0.3717(4) 0.1961(3) 0.0175 1.0000 Uani
N12 N -0.0520(4) 0.4021(4) 0.2051(3) 0.0188 1.0000 Uani
C17 C 0.0017(5) 0.3248(5) 0.1434(4) 0.0222 1.0000 Uani
C18 C -0.0909(6) 0.3255(5) 0.1190(4) 0.0246 1.0000 Uani
C19 C -0.1227(5) 0.3732(5) 0.1591(4) 0.0223 1.0000 Uani
C20 C -0.0465(5) 0.4558(5) 0.2600(4) 0.0183 1.0000 Uani
Re3 Re 0.70226(2) -0.07140(2) 0.633067(15) 0.0185 1.0000 Uani
O1 O 0.6503(5) -0.1212(4) 0.6812(3) 0.0341 1.0000 Uani
O2 O 0.8112(4) -0.0485(4) 0.6745(3) 0.0348 1.0000 Uani
O3 O 0.7045(5) -0.1355(5) 0.5716(4) 0.0421 1.0000 Uani
O4 O 0.6487(5) 0.0206(5) 0.6051(3) 0.0434 1.0000 Uani
Re4 Re 0.19048(2) 0.11467(2) 0.118951(15) 0.0188 1.0000 Uani
O5 O 0.1410(4) 0.0550(4) 0.1646(3) 0.0342 1.0000 Uani
O6 O 0.2994(4) 0.1369(5) 0.1598(3) 0.0349 1.0000 Uani
O7 O 0.1897(6) 0.0619(6) 0.0514(4) 0.0536 1.0000 Uani
O8 O 0.1328(6) 0.2064(5) 0.0975(4) 0.0509 1.0000 Uani
C21 C 0.6061(6) -0.1166(6) 0.9517(4) 0.0261 1.0000 Uani
Cl7 Cl 0.61578(16) -0.02235(15) 0.99562(12) 0.0351 1.0000 Uani
Cl8 Cl 0.65797(16) -0.19994(16) 1.00171(12) 0.0369 1.0000 Uani
Cl9 Cl 0.49324(16) -0.14161(18) 0.91642(11) 0.0375 1.0000 Uani
C22 C 0.6072(6) 0.3907(6) 0.9790(4) 0.0313 1.0000 Uani
Cl10 Cl 0.6011(3) 0.4135(2) 0.89943(13) 0.0582 1.0000 Uani
Cl11 Cl 0.50080(19) 0.3660(3) 0.98420(14) 0.0574 1.0000 Uani
Cl12 Cl 0.6797(2) 0.3079(2) 1.00758(17) 0.0591 1.0000 Uani
C23 C 0.1129(7) 0.0743(6) 0.4544(5) 0.0324 1.0000 Uani
Cl13 Cl 0.1149(2) 0.15809(17) 0.50666(13) 0.0445 1.0000 Uani
Cl14 Cl 0.1748(2) -0.01077(18) 0.49538(15) 0.0473 1.0000 Uani
Cl15 Cl 0.00386(18) 0.0426(2) 0.41522(14) 0.0469 1.0000 Uani
C24 C 0.1643(6) 0.5890(6) 0.4660(4) 0.0290 1.0000 Uani
Cl16 Cl 0.17234(18) 0.65541(19) 0.53120(12) 0.0433 1.0000 Uani
Cl17 Cl 0.05447(19) 0.5788(2) 0.41951(14) 0.0540 1.0000 Uani
Cl18 Cl 0.22979(18) 0.62890(16) 0.41961(11) 0.0362 1.0000 Uani
H11 H 0.6742 0.4350 0.7467 0.0318 1.0000 Uiso
H21 H 0.5462 0.5396 0.7369 0.0325 1.0000 Uiso
H31 H 0.4107 0.4533 0.7372 0.0264 1.0000 Uiso
H41 H 0.6423 0.1306 0.9009 0.0366 1.0000 Uiso
H51 H 0.5016 0.1358 0.9400 0.0408 1.0000 Uiso
H61 H 0.3856 0.2203 0.8580 0.0333 1.0000 Uiso
H71 H 0.5445 0.1038 0.6269 0.0253 1.0000 Uiso
H81 H 0.3745 0.1036 0.5779 0.0330 1.0000 Uiso
H91 H 0.3110 0.2024 0.6477 0.0242 1.0000 Uiso
H101 H 0.3830 0.2908 0.7478 0.0213 1.0000 Uiso
H111 H 0.1779 0.6189 0.2482 0.0285 1.0000 Uiso
H121 H 0.0504 0.7226 0.2461 0.0316 1.0000 Uiso
H131 H -0.0818 0.6334 0.2524 0.0292 1.0000 Uiso
H141 H 0.1594 0.3174 0.4050 0.0449 1.0000 Uiso
H151 H 0.0258 0.3183 0.4495 0.0594 1.0000 Uiso
H161 H -0.0981 0.3985 0.3681 0.0450 1.0000 Uiso
H171 H 0.0434 0.2941 0.1245 0.0268 1.0000 Uiso
H181 H -0.1267 0.2965 0.0797 0.0266 1.0000 Uiso
H191 H -0.1865 0.3847 0.1553 0.0236 1.0000 Uiso
H201 H -0.1074 0.4732 0.2605 0.0225 1.0000 Uiso
H211 H 0.6358 -0.1085 0.9176 0.0305 1.0000 Uiso
H221 H 0.6304 0.4413 1.0055 0.0369 1.0000 Uiso
H231 H 0.1403 0.0943 0.4212 0.0377 1.0000 Uiso
H241 H 0.1863 0.5320 0.4826 0.0344 1.0000 Uiso
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 0.01278(14) 0.01506(16) 0.02251(16) 0.00273(11) 0.00591(12) 0.00174(11)
Cl1 0.0243(10) 0.0144(9) 0.0413(12) 0.0040(8) 0.0090(9) 0.0063(7)
Cl2 0.0277(10) 0.0294(11) 0.0305(10) 0.0029(8) 0.0174(8) 0.0012(8)
Cl3 0.0194(9) 0.0306(11) 0.0324(11) 0.0042(8) 0.0018(8) -0.0036(8)
N1 0.017(3) 0.017(3) 0.020(3) 0.006(3) 0.005(3) 0.006(3)
N2 0.010(3) 0.011(3) 0.019(3) 0.000(2) 0.003(2) 0.002(2)
C1 0.031(5) 0.019(4) 0.030(4) 0.004(3) 0.017(4) 0.001(4)
C2 0.032(5) 0.010(4) 0.039(5) 0.002(3) 0.013(4) 0.008(3)
C3 0.023(4) 0.015(4) 0.029(4) 0.003(3) 0.003(3) 0.000(3)
N3 0.016(3) 0.015(3) 0.025(3) 0.002(3) 0.007(3) -0.002(3)
N4 0.012(3) 0.021(3) 0.016(3) 0.001(2) 0.006(2) 0.001(2)
C4 0.030(5) 0.033(5) 0.028(4) 0.006(4) 0.007(4) 0.006(4)
C5 0.029(5) 0.043(6) 0.029(5) 0.017(4) 0.020(4) 0.004(4)
C6 0.026(4) 0.032(5) 0.026(4) -0.001(4) 0.013(4) -0.007(4)
N5 0.016(3) 0.015(3) 0.028(4) 0.000(3) 0.008(3) 0.002(3)
N6 0.016(3) 0.016(3) 0.025(3) -0.001(3) 0.007(3) 0.003(3)
C7 0.026(4) 0.017(4) 0.021(4) -0.007(3) 0.002(3) 0.003(3)
C8 0.033(5) 0.028(5) 0.022(4) -0.004(3) -0.007(4) -0.004(4)
C9 0.016(4) 0.021(4) 0.023(4) 0.004(3) -0.001(3) -0.006(3)
C10 0.015(3) 0.017(4) 0.022(4) -0.002(3) 0.004(3) 0.003(3)
Re2 0.01199(14) 0.01545(16) 0.02446(16) -0.00019(11) 0.00444(12) 0.00200(11)
Cl4 0.0212(9) 0.0150(9) 0.0470(13) -0.0006(8) 0.0053(9) 0.0042(8)
Cl5 0.0248(10) 0.0312(11) 0.0317(11) -0.0027(9) 0.0133(8) -0.0011(9)
Cl6 0.0199(9) 0.0288(11) 0.0290(10) -0.0033(8) -0.0008(8) -0.0013(8)
N7 0.014(3) 0.011(3) 0.026(3) 0.000(3) 0.006(3) 0.005(2)
N8 0.011(3) 0.016(3) 0.025(3) -0.003(3) 0.006(3) -0.001(2)
C11 0.030(4) 0.012(4) 0.029(4) 0.002(3) 0.013(4) -0.002(3)
C12 0.027(4) 0.018(4) 0.035(5) -0.005(3) 0.010(4) -0.007(3)
C13 0.030(4) 0.020(4) 0.024(4) 0.000(3) 0.007(3) 0.007(4)
N9 0.017(3) 0.022(3) 0.023(3) 0.007(3) 0.012(3) 0.003(3)
N10 0.019(3) 0.021(4) 0.021(3) -0.001(3) 0.011(3) 0.002(3)
C14 0.039(5) 0.044(6) 0.030(5) 0.021(4) 0.013(4) 0.016(5)
C15 0.059(7) 0.043(6) 0.046(6) 0.028(5) 0.031(6) 0.016(5)
C16 0.045(6) 0.035(5) 0.033(5) 0.008(4) 0.027(4) 0.000(4)
N11 0.006(3) 0.022(3) 0.024(3) -0.002(3) 0.004(2) 0.003(2)
N12 0.019(3) 0.018(3) 0.022(3) -0.002(3) 0.009(3) 0.001(3)
C17 0.021(4) 0.017(4) 0.029(4) -0.002(3) 0.008(3) 0.003(3)
C18 0.026(4) 0.018(4) 0.022(4) -0.005(3) -0.005(3) -0.001(3)
C19 0.014(4) 0.016(4) 0.029(4) 0.005(3) -0.007(3) 0.000(3)
C20 0.013(3) 0.020(4) 0.024(4) 0.007(3) 0.007(3) 0.004(3)
Re3 0.01677(15) 0.01867(16) 0.02099(15) -0.00082(12) 0.00673(12) -0.00122(12)
O1 0.035(4) 0.030(4) 0.042(4) 0.009(3) 0.018(3) -0.001(3)
O2 0.026(3) 0.035(4) 0.039(4) 0.001(3) 0.002(3) -0.017(3)
O3 0.032(4) 0.052(5) 0.046(4) -0.026(4) 0.017(3) -0.012(3)
O4 0.054(5) 0.049(5) 0.033(4) 0.024(3) 0.022(3) 0.022(4)
Re4 0.01870(15) 0.01667(16) 0.02287(16) -0.00170(12) 0.00886(12) -0.00036(12)
O5 0.025(3) 0.038(4) 0.041(4) 0.014(3) 0.012(3) 0.000(3)
O6 0.028(3) 0.044(4) 0.030(3) 0.000(3) 0.002(3) -0.016(3)
O7 0.053(5) 0.062(6) 0.056(5) -0.034(4) 0.032(4) -0.016(4)
O8 0.062(5) 0.036(4) 0.067(5) 0.022(4) 0.038(4) 0.023(4)
C21 0.023(4) 0.028(5) 0.025(4) 0.000(3) 0.003(3) -0.003(4)
Cl7 0.0345(12) 0.0287(12) 0.0412(13) -0.0017(10) 0.0092(10) 0.0019(9)
Cl8 0.0351(12) 0.0302(12) 0.0389(12) 0.0019(10) 0.0002(10) 0.0042(10)
Cl9 0.0284(11) 0.0506(15) 0.0274(11) -0.0008(10) -0.0019(9) -0.0034(10)
C22 0.032(5) 0.037(5) 0.024(4) -0.001(4) 0.005(4) 0.004(4)
Cl10 0.099(3) 0.0492(17) 0.0262(12) -0.0051(11) 0.0183(14) -0.0206(17)
Cl11 0.0325(13) 0.098(3) 0.0409(15) -0.0151(15) 0.0095(12) -0.0061(15)
Cl12 0.0400(14) 0.0409(16) 0.076(2) 0.0032(14) -0.0161(14) 0.0103(12)
C23 0.031(5) 0.024(5) 0.039(5) 0.001(4) 0.005(4) 0.001(4)
Cl13 0.0586(16) 0.0325(13) 0.0421(14) -0.0057(11) 0.0137(12) 0.0070(12)
Cl14 0.0454(15) 0.0384(14) 0.0563(16) -0.0020(12) 0.0116(13) 0.0105(12)
Cl15 0.0336(13) 0.0614(18) 0.0424(14) -0.0059(12) 0.0056(11) -0.0027(12)
C24 0.027(4) 0.033(5) 0.026(4) 0.004(4) 0.006(4) -0.003(4)
Cl16 0.0444(14) 0.0597(17) 0.0295(11) -0.0131(11) 0.0163(10) -0.0166(13)
Cl17 0.0373(14) 0.067(2) 0.0455(15) -0.0048(14) -0.0088(12) -0.0127(13)
Cl18 0.0487(14) 0.0324(12) 0.0348(12) 0.0035(9) 0.0236(11) 0.0019(11)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Re1 . Cl1 . 2.306(2) yes
Re1 . Cl2 . 2.290(2) yes
Re1 . Cl3 . 2.292(2) yes
Re1 . N1 . 2.098(7) yes
Re1 . N3 . 2.116(7) yes
Re1 . N5 . 2.108(7) yes
N1 . N2 . 1.351(9) yes
N1 . C1 . 1.352(11) yes
N2 . C3 . 1.351(10) yes
N2 . C10 . 1.453(10) yes
C1 . C2 . 1.394(12) yes
C1 . H11 . 1.000 no
C2 . C3 . 1.347(12) yes
C2 . H21 . 1.000 no
C3 . H31 . 1.000 no
N3 . N4 . 1.363(9) yes
N3 . C4 . 1.327(11) yes
N4 . C6 . 1.358(10) yes
N4 . C10 . 1.454(10) yes
C4 . C5 . 1.415(13) yes
C4 . H41 . 1.000 no
C5 . C6 . 1.360(13) yes
C5 . H51 . 1.000 no
C6 . H61 . 1.000 no
N5 . N6 . 1.369(9) yes
N5 . C7 . 1.341(10) yes
N6 . C9 . 1.341(10) yes
N6 . C10 . 1.442(10) yes
C7 . C8 . 1.407(13) yes
C7 . H71 . 1.000 no
C8 . C9 . 1.386(13) yes
C8 . H81 . 1.000 no
C9 . H91 . 1.000 no
C10 . H101 . 1.000 no
Re2 . Cl4 . 2.308(2) yes
Re2 . Cl5 . 2.296(2) yes
Re2 . Cl6 . 2.285(2) yes
Re2 . N7 . 2.108(6) yes
Re2 . N9 . 2.119(6) yes
Re2 . N11 . 2.113(6) yes
N7 . N8 . 1.366(9) yes
N7 . C11 . 1.341(10) yes
N8 . C13 . 1.340(11) yes
N8 . C20 . 1.439(10) yes
C11 . C12 . 1.404(12) yes
C11 . H111 . 1.000 no
C12 . C13 . 1.365(13) yes
C12 . H121 . 1.000 no
C13 . H131 . 1.000 no
N9 . N10 . 1.369(9) yes
N9 . C14 . 1.335(11) yes
N10 . C16 . 1.343(11) yes
N10 . C20 . 1.441(10) yes
C14 . C15 . 1.386(15) yes
C14 . H141 . 1.000 no
C15 . C16 . 1.379(15) yes
C15 . H151 . 1.000 no
C16 . H161 . 1.000 no
N11 . N12 . 1.378(9) yes
N11 . C17 . 1.337(11) yes
N12 . C19 . 1.353(10) yes
N12 . C20 . 1.462(10) yes
C17 . C18 . 1.402(12) yes
C17 . H171 . 1.000 no
C18 . C19 . 1.362(13) yes
C18 . H181 . 1.000 no
C19 . H191 . 1.000 no
C20 . H201 . 1.000 no
Re3 . O1 . 1.706(6) yes
Re3 . O2 . 1.735(6) yes
Re3 . O3 . 1.703(7) yes
Re3 . O4 . 1.712(7) yes
Re4 . O5 . 1.720(6) yes
Re4 . O6 . 1.730(6) yes
Re4 . O7 . 1.705(7) yes
Re4 . O8 . 1.710(7) yes
C21 . Cl7 . 1.765(10) yes
C21 . Cl8 . 1.765(9) yes
C21 . Cl9 . 1.769(9) yes
C21 . H211 . 1.000 no
C22 . Cl10 . 1.763(10) yes
C22 . Cl11 . 1.755(10) yes
C22 . Cl12 . 1.736(10) yes
C22 . H221 . 1.000 no
C23 . Cl13 . 1.754(10) yes
C23 . Cl14 . 1.757(10) yes
C23 . Cl15 . 1.759(10) yes
C23 . H231 . 1.000 no
C24 . Cl16 . 1.756(10) yes
C24 . Cl17 . 1.747(10) yes
C24 . Cl18 . 1.763(9) yes
C24 . H241 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Re1 . Cl2 . 93.94(8) yes
Cl1 . Re1 . Cl3 . 92.95(8) yes
Cl2 . Re1 . Cl3 . 93.98(8) yes
Cl1 . Re1 . N1 . 173.82(19) yes
Cl2 . Re1 . N1 . 90.77(19) yes
Cl3 . Re1 . N1 . 90.72(19) yes
Cl1 . Re1 . N3 . 91.55(19) yes
Cl2 . Re1 . N3 . 170.87(19) yes
Cl3 . Re1 . N3 . 93.01(19) yes
N1 . Re1 . N3 . 83.3(3) yes
Cl1 . Re1 . N5 . 92.95(19) yes
Cl2 . Re1 . N5 . 91.02(19) yes
Cl3 . Re1 . N5 . 171.98(19) yes
N1 . Re1 . N5 . 82.9(3) yes
N3 . Re1 . N5 . 81.4(3) yes
Re1 . N1 . N2 . 121.4(5) yes
Re1 . N1 . C1 . 133.0(6) yes
N2 . N1 . C1 . 105.5(6) yes
N1 . N2 . C3 . 110.9(6) yes
N1 . N2 . C10 . 118.5(6) yes
C3 . N2 . C10 . 130.6(6) yes
N1 . C1 . C2 . 109.5(8) yes
N1 . C1 . H11 . 125.245 no
C2 . C1 . H11 . 125.251 no
C1 . C2 . C3 . 106.3(8) yes
C1 . C2 . H21 . 126.835 no
C3 . C2 . H21 . 126.845 no
N2 . C3 . C2 . 107.8(7) yes
N2 . C3 . H31 . 126.117 no
C2 . C3 . H31 . 126.121 no
Re1 . N3 . N4 . 119.4(5) yes
Re1 . N3 . C4 . 133.4(6) yes
N4 . N3 . C4 . 107.1(7) yes
N3 . N4 . C6 . 110.1(7) yes
N3 . N4 . C10 . 119.9(6) yes
C6 . N4 . C10 . 129.6(7) yes
N3 . C4 . C5 . 109.0(8) yes
N3 . C4 . H41 . 125.481 no
C5 . C4 . H41 . 125.475 no
C4 . C5 . C6 . 106.4(7) yes
C4 . C5 . H51 . 126.824 no
C6 . C5 . H51 . 126.825 no
N4 . C6 . C5 . 107.3(8) yes
N4 . C6 . H61 . 126.330 no
C5 . C6 . H61 . 126.323 no
Re1 . N5 . N6 . 120.4(5) yes
Re1 . N5 . C7 . 134.2(6) yes
N6 . N5 . C7 . 105.4(6) yes
N5 . N6 . C9 . 111.9(7) yes
N5 . N6 . C10 . 118.8(6) yes
C9 . N6 . C10 . 129.3(7) yes
N5 . C7 . C8 . 110.2(7) yes
N5 . C7 . H71 . 124.887 no
C8 . C7 . H71 . 124.900 no
C7 . C8 . C9 . 105.6(7) yes
C7 . C8 . H81 . 127.185 no
C9 . C8 . H81 . 127.198 no
N6 . C9 . C8 . 106.9(7) yes
N6 . C9 . H91 . 126.561 no
C8 . C9 . H91 . 126.556 no
N2 . C10 . N4 . 109.0(6) yes
N2 . C10 . N6 . 111.1(6) yes
N4 . C10 . N6 . 109.3(6) yes
N2 . C10 . H101 . 108.599 no
N4 . C10 . H101 . 110.466 no
N6 . C10 . H101 . 108.322 no
Cl4 . Re2 . Cl5 . 94.33(8) yes
Cl4 . Re2 . Cl6 . 92.87(8) yes
Cl5 . Re2 . Cl6 . 94.22(8) yes
Cl4 . Re2 . N7 . 172.68(19) yes
Cl5 . Re2 . N7 . 90.52(19) yes
Cl6 . Re2 . N7 . 92.24(19) yes
Cl4 . Re2 . N9 . 92.1(2) yes
Cl5 . Re2 . N9 . 171.12(19) yes
Cl6 . Re2 . N9 . 91.6(2) yes
N7 . Re2 . N9 . 82.5(3) yes
Cl4 . Re2 . N11 . 91.20(19) yes
Cl5 . Re2 . N11 . 91.54(19) yes
Cl6 . Re2 . N11 . 172.68(18) yes
N7 . Re2 . N11 . 83.2(3) yes
N9 . Re2 . N11 . 82.2(3) yes
Re2 . N7 . N8 . 120.2(5) yes
Re2 . N7 . C11 . 133.2(6) yes
N8 . N7 . C11 . 106.6(6) yes
N7 . N8 . C13 . 110.2(7) yes
N7 . N8 . C20 . 119.6(6) yes
C13 . N8 . C20 . 130.2(7) yes
N7 . C11 . C12 . 109.1(7) yes
N7 . C11 . H111 . 125.466 no
C12 . C11 . H111 . 125.466 no
C11 . C12 . C13 . 106.0(8) yes
C11 . C12 . H121 . 127.005 no
C13 . C12 . H121 . 127.015 no
N8 . C13 . C12 . 108.1(8) yes
N8 . C13 . H131 . 125.937 no
C12 . C13 . H131 . 125.921 no
Re2 . N9 . N10 . 119.9(5) yes
Re2 . N9 . C14 . 134.9(6) yes
N10 . N9 . C14 . 105.2(7) yes
N9 . N10 . C16 . 110.7(7) yes
N9 . N10 . C20 . 119.4(6) yes
C16 . N10 . C20 . 129.8(7) yes
N9 . C14 . C15 . 111.3(8) yes
N9 . C14 . H141 . 124.386 no
C15 . C14 . H141 . 124.347 no
C14 . C15 . C16 . 105.1(8) yes
C14 . C15 . H151 . 127.465 no
C16 . C15 . H151 . 127.456 no
N10 . C16 . C15 . 107.7(9) yes
N10 . C16 . H161 . 126.158 no
C15 . C16 . H161 . 126.160 no
Re2 . N11 . N12 . 120.3(5) yes
Re2 . N11 . C17 . 133.6(5) yes
N12 . N11 . C17 . 106.1(6) yes
N11 . N12 . C19 . 110.4(7) yes
N11 . N12 . C20 . 118.5(6) yes
C19 . N12 . C20 . 131.1(7) yes
N11 . C17 . C18 . 109.4(7) yes
N11 . C17 . H171 . 125.274 no
C18 . C17 . H171 . 125.289 no
C17 . C18 . C19 . 106.8(7) yes
C17 . C18 . H181 . 126.590 no
C19 . C18 . H181 . 126.590 no
N12 . C19 . C18 . 107.2(7) yes
N12 . C19 . H191 . 126.378 no
C18 . C19 . H191 . 126.378 no
N8 . C20 . N10 . 110.8(6) yes
N8 . C20 . N12 . 110.3(6) yes
N10 . C20 . N12 . 108.7(6) yes
N8 . C20 . H201 . 107.777 no
N10 . C20 . H201 . 109.368 no
N12 . C20 . H201 . 109.877 no
O1 . Re3 . O2 . 110.3(3) yes
O1 . Re3 . O3 . 109.8(4) yes
O2 . Re3 . O3 . 107.6(4) yes
O1 . Re3 . O4 . 110.2(3) yes
O2 . Re3 . O4 . 108.8(4) yes
O3 . Re3 . O4 . 110.2(4) yes
O5 . Re4 . O6 . 110.8(3) yes
O5 . Re4 . O7 . 110.3(4) yes
O6 . Re4 . O7 . 108.2(4) yes
O5 . Re4 . O8 . 109.7(3) yes
O6 . Re4 . O8 . 109.8(4) yes
O7 . Re4 . O8 . 107.9(5) yes
Cl7 . C21 . Cl8 . 110.0(5) yes
Cl7 . C21 . Cl9 . 110.5(5) yes
Cl8 . C21 . Cl9 . 109.5(5) yes
Cl7 . C21 . H211 . 108.427 no
Cl8 . C21 . H211 . 109.437 no
Cl9 . C21 . H211 . 108.940 no
Cl10 . C22 . Cl11 . 109.2(5) yes
Cl10 . C22 . Cl12 . 111.1(5) yes
Cl11 . C22 . Cl12 . 110.3(6) yes
Cl10 . C22 . H221 . 108.850 no
Cl11 . C22 . H221 . 109.691 no
Cl12 . C22 . H221 . 107.658 no
Cl13 . C23 . Cl14 . 110.0(6) yes
Cl13 . C23 . Cl15 . 111.8(6) yes
Cl14 . C23 . Cl15 . 110.6(5) yes
Cl13 . C23 . H231 . 107.891 no
Cl14 . C23 . H231 . 109.113 no
Cl15 . C23 . H231 . 107.268 no
Cl16 . C24 . Cl17 . 111.3(5) yes
Cl16 . C24 . Cl18 . 109.9(5) yes
Cl17 . C24 . Cl18 . 109.7(5) yes
Cl16 . C24 . H241 . 108.032 no
Cl17 . C24 . H241 . 108.191 no
Cl18 . C24 . H241 . 109.704 no

loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_site_symmetry_2
_geom_contact_distance
C3 O6 4_555 2.988(11)
C7 O4 . 3.251(10)
C10 O1 3_656 2.920(10)
C10 O6 4_555 2.950(10)
C13 O2 4_454 2.879(12)
C17 O8 . 3.163(10)
C20 O2 4_454 2.885(10)
C20 O5 3_555 2.975(10)

#these are likely to be C-H...O hydrogen bonds

# Attachment 'Complex_7a_Fig_7.cif'

data_arc1510
_database_code_depnum_ccdc_archive 'CCDC 629318'
#=============================================================
# Diffractometer details
#=============================================================
_diffrn_measurement_device_type  
;
Nonius KappaCCD
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
#=============================================================
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'

_chemical_name_systematic        # IUPAC name, in full
;
?
;
_chemical_melting_point          ?
_exptl_crystal_thermal_history   
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
#=============================================================

_cell_length_a                   11.7127(2)
_cell_angle_alpha                90
_cell_length_b                   16.3000(3)
_cell_angle_beta                 98.4918(7)
_cell_length_c                   18.0939(3)
_cell_angle_gamma                90
_cell_volume                     3416.56(10)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Re ' -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417
52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            4
_chemical_formula_sum            ' C36 H31 Cl2 N4 O7 Re '
_chemical_formula_moiety         ' C36 H31 Cl2 N4 O7 Re '
_chemical_compound_source        
;
synthesis as described
;
_chemical_formula_weight         888.77

_cell_measurement_reflns_used    30866
_cell_measurement_theta_min      5
_cell_measurement_theta_max      28
_cell_measurement_temperature    150

_exptl_crystal_description       ' tablet '
_exptl_crystal_colour            ' blue '
_exptl_crystal_size_min          0.06
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_max          0.14

_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    3.769

_diffrn_measurement_method       \w

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_T_max  0.80

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            30866
_reflns_number_total             7758
#8039 unique reflections including absences
_diffrn_reflns_av_R_equivalents  0.056

_diffrn_reflns_theta_min         5.119
_diffrn_reflns_theta_max         27.476
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.476
_diffrn_measured_fraction_theta_full 0.999

_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              21
_reflns_limit_l_min              0
_reflns_limit_l_max              23

_refine_diff_density_min         -1.41
_refine_diff_density_max         0.79

_refine_ls_number_reflns         5059
_refine_ls_number_restraints     0
_refine_ls_number_parameters     451

#_refine_ls_R_factor_ref 0.0324
_refine_ls_wR_factor_ref         0.0369
_refine_ls_goodness_of_fit_ref   1.0853

#_reflns_number_all 7758
_refine_ls_R_factor_all          0.0646
_refine_ls_wR_factor_all         0.0513

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                5059
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_gt          0.0369

_refine_ls_shift/su_max          0.001732
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.815 0.365 0.622
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
Re1 Re 0.224244(15) 0.546717(11) 0.207768(10) 0.0236 1.0000 Uani
Cl1 Cl 0.09141(10) 0.53105(8) 0.09916(7) 0.0340 1.0000 Uani
Cl2 Cl 0.13123(11) 0.43832(8) 0.25962(8) 0.0374 1.0000 Uani
O1 O 0.1715(3) 0.6267(2) 0.24906(19) 0.0273 1.0000 Uani
C1 C 0.4932(4) 0.5400(3) 0.1969(2) 0.0222 1.0000 Uani
C2 C 0.4364(4) 0.4592(3) 0.1656(2) 0.0258 1.0000 Uani
O2 O 0.4938(3) 0.4040(2) 0.1464(2) 0.0383 1.0000 Uani
O3 O 0.3254(3) 0.4599(2) 0.16486(19) 0.0277 1.0000 Uani
N1 N 0.4799(3) 0.5486(3) 0.2748(2) 0.0239 1.0000 Uani
N2 N 0.3714(3) 0.5436(3) 0.2950(2) 0.0253 1.0000 Uani
C3 C 0.3842(4) 0.5543(3) 0.3682(2) 0.0222 1.0000 Uani
C4 C 0.5015(4) 0.5655(3) 0.3960(3) 0.0292 1.0000 Uani
C5 C 0.5607(4) 0.5629(3) 0.3359(3) 0.0267 1.0000 Uani
C6 C 0.2884(4) 0.5614(3) 0.4139(3) 0.0279 1.0000 Uani
C7 C 0.2485(5) 0.4940(4) 0.4485(3) 0.0355 1.0000 Uani
C8 C 0.1678(5) 0.5036(4) 0.4975(3) 0.0452 1.0000 Uani
C9 C 0.1294(5) 0.5821(5) 0.5102(3) 0.0516 1.0000 Uani
C10 C 0.1670(4) 0.6501(4) 0.4760(3) 0.0378 1.0000 Uani
C11 C 0.2472(4) 0.6396(3) 0.4266(3) 0.0290 1.0000 Uani
O4 O 0.2924(3) 0.7025(2) 0.3906(2) 0.0345 1.0000 Uani
C12 C 0.2402(6) 0.7816(4) 0.3922(4) 0.0535 1.0000 Uani
C13 C 0.6837(4) 0.5828(4) 0.3340(3) 0.0358 1.0000 Uani
C14 C 0.7258(4) 0.6571(4) 0.3699(3) 0.0388 1.0000 Uani
C15 C 0.8393(6) 0.6803(5) 0.3716(4) 0.0536 1.0000 Uani
C16 C 0.9127(5) 0.6288(6) 0.3388(4) 0.0558 1.0000 Uani
C17 C 0.8743(5) 0.5572(5) 0.3044(3) 0.0510 1.0000 Uani
C18 C 0.7581(5) 0.5352(4) 0.3018(3) 0.0388 1.0000 Uani
O5 O 0.7132(4) 0.4632(3) 0.2703(2) 0.0466 1.0000 Uani
C19 C 0.7819(7) 0.4187(5) 0.2257(4) 0.0576 1.0000 Uani
N3 N 0.4422(3) 0.6100(2) 0.1539(2) 0.0214 1.0000 Uani
N4 N 0.3271(3) 0.6260(2) 0.1496(2) 0.0242 1.0000 Uani
C20 C 0.3081(4) 0.6970(3) 0.1128(3) 0.0247 1.0000 Uani
C21 C 0.4128(4) 0.7251(3) 0.0923(3) 0.0314 1.0000 Uani
C22 C 0.4967(4) 0.6695(3) 0.1202(3) 0.0267 1.0000 Uani
C23 C 0.1959(4) 0.7405(3) 0.1026(3) 0.0259 1.0000 Uani
C24 C 0.1692(4) 0.7913(3) 0.1601(3) 0.0324 1.0000 Uani
C25 C 0.0692(5) 0.8380(3) 0.1511(3) 0.0327 1.0000 Uani
C26 C -0.0038(4) 0.8342(3) 0.0844(3) 0.0338 1.0000 Uani
C27 C 0.0194(4) 0.7829(3) 0.0271(3) 0.0311 1.0000 Uani
C28 C 0.1198(4) 0.7360(3) 0.0364(3) 0.0300 1.0000 Uani
O6 O 0.1505(3) 0.6851(2) -0.0180(2) 0.0330 1.0000 Uani
C29 C 0.0593(5) 0.6576(4) -0.0742(3) 0.0445 1.0000 Uani
C30 C 0.6226(4) 0.6699(3) 0.1219(3) 0.0311 1.0000 Uani
C31 C 0.6868(4) 0.7317(3) 0.1606(3) 0.0361 1.0000 Uani
C32 C 0.8070(5) 0.7314(4) 0.1685(4) 0.0449 1.0000 Uani
C33 C 0.8625(4) 0.6699(4) 0.1355(4) 0.0393 1.0000 Uani
C34 C 0.8000(4) 0.6071(3) 0.0959(3) 0.0338 1.0000 Uani
C35 C 0.6796(4) 0.6058(3) 0.0894(3) 0.0310 1.0000 Uani
O7 O 0.6106(3) 0.5470(2) 0.0540(2) 0.0370 1.0000 Uani
C36 C 0.6643(5) 0.4798(5) 0.0216(4) 0.0505 1.0000 Uani
H11 H 0.5773 0.5384 0.1926 0.0269 1.0000 Uiso
H41 H 0.5355 0.5739 0.4495 0.0353 1.0000 Uiso
H71 H 0.2775 0.4380 0.4385 0.0435 1.0000 Uiso
H81 H 0.1384 0.4550 0.5228 0.0550 1.0000 Uiso
H91 H 0.0722 0.5894 0.5456 0.0628 1.0000 Uiso
H101 H 0.1377 0.7060 0.4862 0.0457 1.0000 Uiso
H121 H 0.2819 0.8215 0.3638 0.0630 1.0000 Uiso
H122 H 0.2449 0.8004 0.4452 0.0630 1.0000 Uiso
H123 H 0.1575 0.7783 0.3689 0.0630 1.0000 Uiso
H141 H 0.6724 0.6928 0.3940 0.0466 1.0000 Uiso
H151 H 0.8684 0.7328 0.3959 0.0637 1.0000 Uiso
H161 H 0.9955 0.6446 0.3405 0.0669 1.0000 Uiso
H171 H 0.9285 0.5210 0.2815 0.0615 1.0000 Uiso
H191 H 0.7399 0.3679 0.2062 0.0713 1.0000 Uiso
H192 H 0.8567 0.4032 0.2567 0.0713 1.0000 Uiso
H193 H 0.7974 0.4536 0.1828 0.0713 1.0000 Uiso
H211 H 0.4240 0.7758 0.0631 0.0380 1.0000 Uiso
H241 H 0.2230 0.7939 0.2084 0.0383 1.0000 Uiso
H251 H 0.0505 0.8739 0.1925 0.0396 1.0000 Uiso
H261 H -0.0750 0.8689 0.0770 0.0407 1.0000 Uiso
H271 H -0.0359 0.7796 -0.0205 0.0370 1.0000 Uiso
H291 H 0.0919 0.6212 -0.1104 0.0527 1.0000 Uiso
H292 H 0.0211 0.7060 -0.1013 0.0527 1.0000 Uiso
H293 H 0.0014 0.6263 -0.0500 0.0527 1.0000 Uiso
H311 H 0.6464 0.7772 0.1833 0.0437 1.0000 Uiso
H321 H 0.8525 0.7755 0.1979 0.0541 1.0000 Uiso
H331 H 0.9486 0.6703 0.1400 0.0478 1.0000 Uiso
H341 H 0.8413 0.5629 0.0722 0.0416 1.0000 Uiso
H361 H 0.6037 0.4412 -0.0026 0.0608 1.0000 Uiso
H362 H 0.7100 0.5010 -0.0169 0.0608 1.0000 Uiso
H363 H 0.7169 0.4502 0.0614 0.0608 1.0000 Uiso
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 0.01799(9) 0.02488(10) 0.02807(10) 0.00181(9) 0.00407(6) -0.00047(9)
Cl1 0.0244(5) 0.0389(7) 0.0366(6) -0.0031(5) -0.0022(5) -0.0047(5)
Cl2 0.0281(6) 0.0340(7) 0.0518(7) 0.0117(5) 0.0116(5) -0.0021(5)
O1 0.0206(15) 0.0302(18) 0.0324(17) 0.0007(14) 0.0079(13) 0.0008(13)
C1 0.0183(19) 0.025(2) 0.024(2) 0.0001(18) 0.0050(15) 0.0017(17)
C2 0.028(2) 0.024(2) 0.026(2) 0.0006(19) 0.0082(17) 0.000(2)
O2 0.0334(19) 0.033(2) 0.051(2) -0.0124(17) 0.0135(17) -0.0013(16)
O3 0.0265(16) 0.0247(16) 0.0333(17) -0.0045(14) 0.0089(13) -0.0024(14)
N1 0.0169(16) 0.0318(19) 0.0234(17) -0.0009(17) 0.0045(13) 0.0030(16)
N2 0.0206(17) 0.0265(19) 0.0289(18) -0.0029(17) 0.0041(14) 0.0021(16)
C3 0.021(2) 0.024(2) 0.0217(19) -0.0007(18) 0.0038(16) 0.0043(18)
C4 0.028(2) 0.033(3) 0.027(2) -0.0003(18) 0.0064(19) 0.0032(19)
C5 0.020(2) 0.029(3) 0.031(2) -0.0008(18) 0.0028(17) 0.0033(17)
C6 0.021(2) 0.036(3) 0.028(2) 0.0017(19) 0.0051(17) 0.0058(19)
C7 0.032(3) 0.044(3) 0.032(3) 0.005(2) 0.013(2) 0.006(2)
C8 0.030(3) 0.070(4) 0.038(3) 0.015(3) 0.011(2) -0.002(3)
C9 0.025(3) 0.094(5) 0.038(3) 0.002(3) 0.011(2) 0.007(3)
C10 0.025(2) 0.059(4) 0.031(3) -0.010(2) 0.007(2) 0.011(2)
C11 0.020(2) 0.040(3) 0.026(2) -0.006(2) -0.0005(17) 0.002(2)
O4 0.0323(19) 0.0328(19) 0.038(2) -0.0021(16) 0.0039(15) 0.0059(15)
C12 0.046(4) 0.037(3) 0.075(5) -0.005(3) -0.001(3) 0.011(3)
C13 0.021(2) 0.056(3) 0.029(2) 0.005(2) 0.0011(19) 0.000(2)
C14 0.025(2) 0.056(4) 0.035(3) -0.006(2) 0.004(2) -0.002(2)
C15 0.042(3) 0.074(5) 0.043(3) 0.001(3) 0.001(3) -0.019(3)
C16 0.027(3) 0.100(6) 0.040(3) 0.008(4) 0.005(2) -0.005(3)
C17 0.033(3) 0.084(5) 0.036(3) 0.012(3) 0.008(2) 0.008(3)
C18 0.029(3) 0.052(3) 0.035(3) -0.001(2) 0.003(2) 0.006(2)
O5 0.040(2) 0.057(3) 0.045(2) -0.006(2) 0.0128(18) 0.021(2)
C19 0.073(5) 0.051(4) 0.054(4) 0.005(3) 0.028(3) 0.022(4)
N3 0.0154(16) 0.0228(18) 0.0261(19) 0.0020(15) 0.0033(14) -0.0015(14)
N4 0.0177(17) 0.025(2) 0.030(2) -0.0013(16) 0.0036(15) 0.0006(15)
C20 0.019(2) 0.029(2) 0.026(2) 0.0013(18) 0.0018(17) -0.0004(18)
C21 0.025(2) 0.031(3) 0.038(3) 0.008(2) 0.007(2) -0.003(2)
C22 0.024(2) 0.030(2) 0.027(2) 0.0029(19) 0.0063(18) -0.0019(18)
C23 0.023(2) 0.026(2) 0.028(2) 0.0044(18) 0.0026(18) -0.0031(18)
C24 0.029(2) 0.026(2) 0.041(3) 0.000(2) 0.000(2) -0.0034(19)
C25 0.038(3) 0.021(2) 0.040(3) -0.003(2) 0.009(2) 0.002(2)
C26 0.024(2) 0.027(3) 0.051(3) 0.005(2) 0.006(2) 0.0029(19)
C27 0.026(2) 0.031(3) 0.035(3) 0.011(2) 0.002(2) -0.0034(19)
C28 0.026(2) 0.031(3) 0.033(2) 0.001(2) 0.0047(19) 0.000(2)
O6 0.0296(18) 0.041(2) 0.0283(17) -0.0055(15) 0.0033(14) 0.0007(15)
C29 0.037(3) 0.055(4) 0.040(3) -0.009(3) 0.000(2) -0.003(3)
C30 0.024(2) 0.037(3) 0.033(3) 0.008(2) 0.0088(19) 0.000(2)
C31 0.028(2) 0.032(3) 0.049(3) -0.002(2) 0.009(2) -0.005(2)
C32 0.027(3) 0.048(3) 0.061(4) -0.004(3) 0.009(2) -0.011(2)
C33 0.026(2) 0.036(3) 0.057(3) 0.009(2) 0.011(2) -0.004(2)
C34 0.030(2) 0.037(3) 0.037(3) 0.009(2) 0.013(2) 0.001(2)
C35 0.027(2) 0.039(3) 0.028(2) 0.005(2) 0.0069(19) -0.004(2)
O7 0.0252(16) 0.047(2) 0.041(2) -0.0146(18) 0.0104(14) -0.0024(16)
C36 0.038(3) 0.070(4) 0.044(3) -0.021(3) 0.007(3) 0.004(3)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Re1 . Cl1 . 2.3335(12) yes
Re1 . Cl2 . 2.3432(12) yes
Re1 . O1 . 1.666(3) yes
Re1 . O3 . 2.069(3) yes
Re1 . N2 . 2.159(4) yes
Re1 . N4 . 2.146(4) yes
C1 . C2 . 1.544(7) yes
C1 . N1 . 1.447(5) yes
C1 . N3 . 1.458(6) yes
C1 . H11 . 1.000 no
C2 . O2 . 1.206(6) yes
C2 . O3 . 1.298(6) yes
N1 . N2 . 1.376(5) yes
N1 . C5 . 1.366(6) yes
N2 . C3 . 1.322(6) yes
C3 . C4 . 1.403(6) yes
C3 . C6 . 1.493(6) yes
C4 . C5 . 1.374(7) yes
C4 . H41 . 1.000 no
C5 . C13 . 1.482(7) yes
C6 . C7 . 1.381(7) yes
C6 . C11 . 1.394(7) yes
C7 . C8 . 1.397(7) yes
C7 . H71 . 1.000 no
C8 . C9 . 1.387(11) yes
C8 . H81 . 1.000 no
C9 . C10 . 1.375(10) yes
C9 . H91 . 1.000 no
C10 . C11 . 1.400(7) yes
C10 . H101 . 1.000 no
C11 . O4 . 1.363(7) yes
O4 . C12 . 1.429(7) yes
C12 . H121 . 1.000 no
C12 . H122 . 1.000 no
C12 . H123 . 1.000 no
C13 . C14 . 1.428(8) yes
C13 . C18 . 1.360(8) yes
C14 . C15 . 1.377(8) yes
C14 . H141 . 1.000 no
C15 . C16 . 1.396(10) yes
C15 . H151 . 1.000 no
C16 . C17 . 1.366(11) yes
C16 . H161 . 1.000 no
C17 . C18 . 1.402(8) yes
C17 . H171 . 1.000 no
C18 . O5 . 1.374(7) yes
O5 . C19 . 1.420(7) yes
C19 . H191 . 1.000 no
C19 . H192 . 1.000 no
C19 . H193 . 1.000 no
N3 . N4 . 1.364(5) yes
N3 . C22 . 1.354(6) yes
N4 . C20 . 1.337(6) yes
C20 . C21 . 1.408(6) yes
C20 . C23 . 1.481(6) yes
C21 . C22 . 1.377(7) yes
C21 . H211 . 1.000 no
C22 . C30 . 1.471(7) yes
C23 . C24 . 1.400(7) yes
C23 . C28 . 1.386(7) yes
C24 . C25 . 1.387(7) yes
C24 . H241 . 1.000 no
C25 . C26 . 1.373(8) yes
C25 . H251 . 1.000 no
C26 . C27 . 1.389(8) yes
C26 . H261 . 1.000 no
C27 . C28 . 1.392(7) yes
C27 . H271 . 1.000 no
C28 . O6 . 1.375(6) yes
O6 . C29 . 1.433(6) yes
C29 . H291 . 1.000 no
C29 . H292 . 1.000 no
C29 . H293 . 1.000 no
C30 . C31 . 1.383(8) yes
C30 . C35 . 1.413(8) yes
C31 . C32 . 1.393(7) yes
C31 . H311 . 1.000 no
C32 . C33 . 1.378(9) yes
C32 . H321 . 1.000 no
C33 . C34 . 1.393(8) yes
C33 . H331 . 1.000 no
C34 . C35 . 1.398(7) yes
C34 . H341 . 1.000 no
C35 . O7 . 1.353(6) yes
O7 . C36 . 1.432(7) yes
C36 . H361 . 1.000 no
C36 . H362 . 1.000 no
C36 . H363 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Re1 . Cl2 . 87.88(5) yes
Cl1 . Re1 . O1 . 102.61(12) yes
Cl2 . Re1 . O1 . 100.70(12) yes
Cl1 . Re1 . O3 . 87.52(10) yes
Cl2 . Re1 . O3 . 87.73(10) yes
O1 . Re1 . O3 . 166.95(14) yes
Cl1 . Re1 . N2 . 166.98(11) yes
Cl2 . Re1 . N2 . 93.31(11) yes
O1 . Re1 . N2 . 89.93(15) yes
O3 . Re1 . N2 . 79.58(14) yes
Cl1 . Re1 . N4 . 90.34(11) yes
Cl2 . Re1 . N4 . 168.11(11) yes
O1 . Re1 . N4 . 91.16(15) yes
O3 . Re1 . N4 . 80.44(14) yes
N2 . Re1 . N4 . 85.83(15) yes
C2 . C1 . N1 . 109.7(4) yes
C2 . C1 . N3 . 110.6(4) yes
N1 . C1 . N3 . 110.5(4) yes
C2 . C1 . H11 . 108.925 no
N1 . C1 . H11 . 109.055 no
N3 . C1 . H11 . 108.080 no
C1 . C2 . O2 . 121.0(4) yes
C1 . C2 . O3 . 111.9(4) yes
O2 . C2 . O3 . 127.1(5) yes
Re1 . O3 . C2 . 129.1(3) yes
C1 . N1 . N2 . 119.3(3) yes
C1 . N1 . C5 . 130.1(4) yes
N2 . N1 . C5 . 110.6(4) yes
Re1 . N2 . N1 . 118.2(3) yes
Re1 . N2 . C3 . 133.6(3) yes
N1 . N2 . C3 . 106.6(3) yes
N2 . C3 . C4 . 109.7(4) yes
N2 . C3 . C6 . 125.5(4) yes
C4 . C3 . C6 . 124.6(4) yes
C3 . C4 . C5 . 107.1(4) yes
C3 . C4 . H41 . 126.455 no
C5 . C4 . H41 . 126.454 no
N1 . C5 . C4 . 106.0(4) yes
N1 . C5 . C13 . 125.3(4) yes
C4 . C5 . C13 . 128.2(5) yes
C3 . C6 . C7 . 121.5(4) yes
C3 . C6 . C11 . 118.0(4) yes
C7 . C6 . C11 . 120.3(5) yes
C6 . C7 . C8 . 120.4(5) yes
C6 . C7 . H71 . 119.817 no
C8 . C7 . H71 . 119.818 no
C7 . C8 . C9 . 118.3(6) yes
C7 . C8 . H81 . 120.828 no
C9 . C8 . H81 . 120.826 no
C8 . C9 . C10 . 122.4(5) yes
C8 . C9 . H91 . 118.782 no
C10 . C9 . H91 . 118.782 no
C9 . C10 . C11 . 118.6(6) yes
C9 . C10 . H101 . 120.679 no
C11 . C10 . H101 . 120.679 no
C6 . C11 . C10 . 119.9(5) yes
C6 . C11 . O4 . 116.1(4) yes
C10 . C11 . O4 . 123.9(5) yes
C11 . O4 . C12 . 118.1(4) yes
O4 . C12 . H121 . 109.467 no
O4 . C12 . H122 . 109.465 no
H121 . C12 . H122 . 109.477 no
O4 . C12 . H123 . 109.465 no
H121 . C12 . H123 . 109.478 no
H122 . C12 . H123 . 109.476 no
C5 . C13 . C14 . 116.5(5) yes
C5 . C13 . C18 . 124.9(5) yes
C14 . C13 . C18 . 118.6(5) yes
C13 . C14 . C15 . 120.7(5) yes
C13 . C14 . H141 . 119.656 no
C15 . C14 . H141 . 119.656 no
C14 . C15 . C16 . 118.6(6) yes
C14 . C15 . H151 . 120.706 no
C16 . C15 . H151 . 120.706 no
C15 . C16 . C17 . 121.7(6) yes
C15 . C16 . H161 . 119.149 no
C17 . C16 . H161 . 119.147 no
C16 . C17 . C18 . 119.1(6) yes
C16 . C17 . H171 . 120.461 no
C18 . C17 . H171 . 120.460 no
C13 . C18 . C17 . 121.3(6) yes
C13 . C18 . O5 . 115.8(5) yes
C17 . C18 . O5 . 122.8(5) yes
C18 . O5 . C19 . 117.3(5) yes
O5 . C19 . H191 . 109.466 no
O5 . C19 . H192 . 109.468 no
H191 . C19 . H192 . 109.476 no
O5 . C19 . H193 . 109.467 no
H191 . C19 . H193 . 109.474 no
H192 . C19 . H193 . 109.477 no
C1 . N3 . N4 . 120.2(3) yes
C1 . N3 . C22 . 128.1(4) yes
N4 . N3 . C22 . 111.4(4) yes
Re1 . N4 . N3 . 118.6(3) yes
Re1 . N4 . C20 . 134.6(3) yes
N3 . N4 . C20 . 106.5(4) yes
N4 . C20 . C21 . 109.0(4) yes
N4 . C20 . C23 . 123.7(4) yes
C21 . C20 . C23 . 127.0(4) yes
C20 . C21 . C22 . 106.9(4) yes
C20 . C21 . H211 . 126.529 no
C22 . C21 . H211 . 126.529 no
N3 . C22 . C21 . 106.1(4) yes
N3 . C22 . C30 . 122.1(4) yes
C21 . C22 . C30 . 131.6(4) yes
C20 . C23 . C24 . 118.9(4) yes
C20 . C23 . C28 . 121.8(4) yes
C24 . C23 . C28 . 119.2(5) yes
C23 . C24 . C25 . 121.0(5) yes
C23 . C24 . H241 . 119.498 no
C25 . C24 . H241 . 119.499 no
C24 . C25 . C26 . 119.0(5) yes
C24 . C25 . H251 . 120.524 no
C26 . C25 . H251 . 120.524 no
C25 . C26 . C27 . 121.2(5) yes
C25 . C26 . H261 . 119.407 no
C27 . C26 . H261 . 119.406 no
C26 . C27 . C28 . 119.7(5) yes
C26 . C27 . H271 . 120.149 no
C28 . C27 . H271 . 120.147 no
C23 . C28 . C27 . 119.9(5) yes
C23 . C28 . O6 . 116.6(4) yes
C27 . C28 . O6 . 123.4(5) yes
C28 . O6 . C29 . 116.8(4) yes
O6 . C29 . H291 . 109.465 no
O6 . C29 . H292 . 109.466 no
H291 . C29 . H292 . 109.476 no
O6 . C29 . H293 . 109.466 no
H291 . C29 . H293 . 109.476 no
H292 . C29 . H293 . 109.477 no
C22 . C30 . C31 . 118.8(5) yes
C22 . C30 . C35 . 121.4(5) yes
C31 . C30 . C35 . 119.6(5) yes
C30 . C31 . C32 . 121.0(5) yes
C30 . C31 . H311 . 119.520 no
C32 . C31 . H311 . 119.518 no
C31 . C32 . C33 . 119.5(5) yes
C31 . C32 . H321 . 120.260 no
C33 . C32 . H321 . 120.258 no
C32 . C33 . C34 . 120.8(5) yes
C32 . C33 . H331 . 119.624 no
C34 . C33 . H331 . 119.623 no
C33 . C34 . C35 . 120.1(5) yes
C33 . C34 . H341 . 119.975 no
C35 . C34 . H341 . 119.973 no
C30 . C35 . C34 . 119.1(5) yes
C30 . C35 . O7 . 115.8(4) yes
C34 . C35 . O7 . 125.1(5) yes
C35 . O7 . C36 . 118.0(4) yes
O7 . C36 . H361 . 109.467 no
O7 . C36 . H362 . 109.467 no
H361 . C36 . H362 . 109.476 no
O7 . C36 . H363 . 109.466 no
H361 . C36 . H363 . 109.475 no
H362 . C36 . H363 . 109.475 no

# Attachment 'Complex_10_Fig_9.cif'

data_arc1240
_database_code_depnum_ccdc_archive 'CCDC 629319'
#=============================================================
# Diffractometer details
#=============================================================
_diffrn_measurement_device_type  
;
Nonius KappaCCD
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
#=============================================================
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'

_chemical_name_systematic        # IUPAC name, in full
;
?
;
_chemical_melting_point          ?
_exptl_crystal_thermal_history   
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
#=============================================================

_cell_length_a                   15.2626(5)
_cell_angle_alpha                90
_cell_length_b                   10.7896(4)
_cell_angle_beta                 95.1189(17)
_cell_length_c                   8.5400(3)
_cell_angle_gamma                90
_cell_volume                     1400.74(9)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 1 2/m 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z
x,-y,z
-x+1/2,y+1/2,-z
x+1/2,-y+1/2,z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Re ' -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417
52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            2
_chemical_formula_sum            ' C18 H22 Cl4 N10 O3 Re2 '
_chemical_formula_moiety         ' C14 H16 Cl4 N8 O3 Re2, 2(C2 H3 N) '
_chemical_compound_source        
;
synthesis as described
;
_chemical_formula_weight         940.65

_cell_measurement_reflns_used    4815
_cell_measurement_theta_min      5
_cell_measurement_theta_max      28
_cell_measurement_temperature    150

_exptl_crystal_description       ' block '
_exptl_crystal_colour            ' dark blue '
_exptl_crystal_size_min          0.08
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_max          0.14

_exptl_crystal_density_diffrn    2.230
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             884
_exptl_absorpt_coefficient_mu    9.056

_diffrn_measurement_method       \w

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_T_max  0.48

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            4815
_reflns_number_total             1671
_diffrn_reflns_av_R_equivalents  0.037

_diffrn_reflns_theta_min         5.106
_diffrn_reflns_theta_max         27.477
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.477
_diffrn_measured_fraction_theta_full 0.999

_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              -19
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              13
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_refine_diff_density_min         -1.39
_refine_diff_density_max         0.85

_refine_ls_number_reflns         1421
_refine_ls_number_restraints     0
_refine_ls_number_parameters     101

#_refine_ls_R_factor_ref 0.0261
_refine_ls_wR_factor_ref         0.0290
_refine_ls_goodness_of_fit_ref   1.0971

#_reflns_number_all 1661
_refine_ls_R_factor_all          0.0340
_refine_ls_wR_factor_all         0.0394

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                1421
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_gt          0.0290

_refine_ls_shift/su_max          0.005716
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.250 0.0607 0.0376
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Re1 Re 0.377222(17) 0.5000 0.53223(3) 0.0118 1.0000 Uani S T
Cl1 Cl 0.40706(8) 0.34219(11) 0.72821(13) 0.0194 1.0000 Uani . .
O1 O 0.5000 0.5000 0.5000 0.0128 1.0000 Uani S T
O2 O 0.2671(3) 0.5000 0.5430(6) 0.0179 1.0000 Uani S T
N1 N 0.3644(3) 0.3636(4) 0.3566(4) 0.0146 1.0000 Uani . .
N2 N 0.3657(3) 0.3880(4) 0.2013(4) 0.0142 1.0000 Uani . .
C1 C 0.3392(3) 0.2456(4) 0.3669(6) 0.0172 1.0000 Uani . .
C2 C 0.3263(4) 0.1931(5) 0.2166(6) 0.0235 1.0000 Uani . .
C3 C 0.3449(3) 0.2845(5) 0.1148(6) 0.0194 1.0000 Uani . .
C4 C 0.4058(5) 0.5000 0.1460(8) 0.0162 1.0000 Uani S T
N3 N 0.1708(6) 0.5000 0.0944(10) 0.0466 1.0000 Uani S T
C5 C 0.1178(7) 0.5000 0.1822(12) 0.0389 1.0000 Uani S T
C6 C 0.0546(8) 0.5000 0.2998(17) 0.0600 1.0000 Uani S T
H1 H 0.471(6) 0.5000 0.185(10) 0.02(2) 1.0000 Uiso S .
H2 H 0.397(6) 0.5000 0.019(10) 0.02(2) 1.0000 Uiso S .
H11 H 0.3308 0.2012 0.4673 0.0210 1.0000 Uiso . .
H21 H 0.3074 0.1064 0.1896 0.0282 1.0000 Uiso . .
H31 H 0.3436 0.2769 -0.0021 0.0233 1.0000 Uiso . .
H61 H -0.0064 0.5000 0.2463 0.0741 1.0000 Uiso . .
H62 H 0.0634 0.5757 0.3670 0.0741 1.0000 Uiso . .
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 0.01210(14) 0.01350(14) 0.01015(13) 0.0000 0.00306(8) 0.0000
Cl1 0.0224(6) 0.0201(5) 0.0159(5) 0.0061(4) 0.0027(4) -0.0036(5)
O1 0.022(3) 0.010(3) 0.006(3) 0.0000 0.000(2) 0.0000
O2 0.019(2) 0.015(2) 0.019(2) 0.0000 -0.0004(19) 0.0000
N1 0.0177(19) 0.0145(19) 0.0118(17) -0.0002(15) 0.0033(15) 0.0004(16)
N2 0.0163(18) 0.015(2) 0.0111(17) -0.0020(15) 0.0008(14) -0.0001(16)
C1 0.021(2) 0.010(2) 0.021(2) 0.0004(18) 0.0058(18) -0.0032(18)
C2 0.030(3) 0.016(2) 0.025(3) -0.005(2) 0.003(2) -0.004(2)
C3 0.020(2) 0.018(2) 0.020(2) -0.004(2) 0.0018(18) -0.0010(19)
C4 0.019(3) 0.010(3) 0.019(3) 0.0000 0.004(3) 0.0000
N3 0.060(6) 0.044(5) 0.036(4) 0.0000 0.009(4) 0.0000
C5 0.045(5) 0.027(4) 0.044(5) 0.0000 -0.001(4) 0.0000
C6 0.054(7) 0.034(6) 0.097(10) 0.0000 0.037(7) 0.0000
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Re1 . Cl1 . 2.4025(11) yes
Re1 . Cl1 6_565 2.4025(11) yes
Re1 . O1 . 1.9182(3) yes
Re1 . O2 . 1.692(5) yes
Re1 . N1 . 2.098(4) yes
Re1 . N1 6_565 2.098(4) yes
N1 . N2 . 1.354(5) yes
N1 . C1 . 1.335(6) yes
N2 . C3 . 1.361(6) yes
N2 . C4 . 1.452(5) yes
C1 . C2 . 1.401(7) yes
C1 . H11 . 1.000 no
C2 . C3 . 1.361(7) yes
C2 . H21 . 1.000 no
C3 . H31 . 1.000 no
C4 . H1 . 1.02(9) no
C4 . H2 . 1.08(9) no
N3 . C5 . 1.150(13) yes
C5 . C6 . 1.454(15) yes
C6 . H61 . 1.000 no
C6 . H62 . 1.000 no
C6 . H62 6_565 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Re1 . Cl1 6_565 90.26(6) yes
Cl1 . Re1 . O1 . 88.46(3) yes
Cl1 6_565 Re1 . O1 . 88.46(3) yes
Cl1 . Re1 . O2 . 95.14(12) yes
Cl1 6_565 Re1 . O2 . 95.14(12) yes
O1 . Re1 . O2 . 174.89(16) yes
Cl1 . Re1 . N1 . 90.03(11) yes
Cl1 6_565 Re1 . N1 . 174.29(11) yes
O1 . Re1 . N1 . 85.85(11) yes
O2 . Re1 . N1 . 90.51(16) yes
Cl1 . Re1 . N1 6_565 174.29(11) yes
Cl1 6_565 Re1 . N1 6_565 90.03(11) yes
O1 . Re1 . N1 6_565 85.85(11) yes
O2 . Re1 . N1 6_565 90.51(16) yes
N1 . Re1 . N1 6_565 89.1(2) yes
Re1 . O1 . Re1 2_666 179.994 yes
Re1 . N1 . N2 . 123.7(3) yes
Re1 . N1 . C1 . 129.1(3) yes
N2 . N1 . C1 . 106.2(4) yes
N1 . N2 . C3 . 110.4(4) yes
N1 . N2 . C4 . 121.6(4) yes
C3 . N2 . C4 . 126.2(4) yes
N1 . C1 . C2 . 110.0(4) yes
N1 . C1 . H11 . 124.988 no
C2 . C1 . H11 . 124.987 no
C1 . C2 . C3 . 105.8(4) yes
C1 . C2 . H21 . 127.086 no
C3 . C2 . H21 . 127.086 no
N2 . C3 . C2 . 107.4(4) yes
N2 . C3 . H31 . 126.300 no
C2 . C3 . H31 . 126.300 no
N2 . C4 . N2 6_565 112.6(5) yes
N2 . C4 . H1 . 109(2) no
N2 6_565 C4 . H1 . 109(2) no
N2 . C4 . H2 . 108(2) no
N2 6_565 C4 . H2 . 108(2) no
H1 . C4 . H2 . 111(7) no
N3 . C5 . C6 . 177.0(12) yes
C5 . C6 . H61 . 109.467 no
C5 . C6 . H62 . 109.468 no
H61 . C6 . H62 . 109.474 no
C5 . C6 . H62 6_565 109.468 no
H61 . C6 . H62 6_565 109.474 no
H62 . C6 . H62 6_565 109.476 no

loop_
_geom_hbond_atom_site_label_d
_geom_hbond_atom_site_label_h
_geom_hbond_atom_site_label_a
_geom_hbond_site_symmetry_a
_geom_hbond_distance_dh
_geom_hbond_distance_ha
_geom_hbond_distance_da
_geom_hbond_angle_dha
_geom_hbond_publ_flag
C4 H1 Cl1 2_666 1.02(9) 2.58(7) 3.415(6) 138.7(13) yes
C4 H1 Cl1 5_656 1.02(9) 2.58(7) 3.415(6) 138.7(13) no

# Possible bifurcated hydrogen bond. Note that the geometry is constrained by
# space-group symmetry, i.e. the C and H atoms are assumed to lie exactly on
# the crystallographic mirror plane at y=0.5.