#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:36:26 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180147 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/44/7104489.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7104489
loop_
_publ_author_name
'Nieto, Sonia'
'Pérez, Julio'
'Riera, Lucía'
'Riera, Víctor'
'Miguel, Daniel'
_publ_section_title
;
 Metal complexes with two different hydrogen-bond donor ligands as
 anion hosts.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3279
_journal_page_last               3281
_journal_paper_doi               10.1039/b823460d
_journal_volume                  34
_journal_year                    2009
_chemical_formula_sum            'C18.88 H24 Cl0.25 N7 O6 Re'
_chemical_formula_weight         640.01
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.678(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.1425(2)
_cell_length_b                   18.6344(3)
_cell_length_c                   19.2945(3)
_cell_measurement_reflns_used    12678
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5472
_cell_measurement_theta_min      2.7142
_cell_volume                     5838.83(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29294
_diffrn_reflns_theta_full        73.82
_diffrn_reflns_theta_max         73.82
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    8.486
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.791
_refine_diff_density_min         -2.494
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         11272
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0773
_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/[σ²(Fo²)+(0.0728P)²+65.3035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2221
_reflns_number_gt                8936
_reflns_number_total             11272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b823460d.txt
_cod_data_source_block           Compound_2NO3_(lr296x)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to 'constr'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7104489
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
C92 C 0.079(2) -0.121(3) -0.012(3) 0.18(2) Uiso 0.50 1 d PD . .
H92A H 0.0952 -0.0830 -0.0372 0.269 Uiso 0.50 1 calc PR . .
H92B H 0.0724 -0.1646 -0.0396 0.269 Uiso 0.50 1 calc PR . .
H92C H 0.1203 -0.1281 0.0351 0.269 Uiso 0.50 1 calc PR . .
C93 C -0.001(2) -0.10251(9) 0.000(2) 0.101(10) Uiso 0.50 1 d PD . .
H93A H 0.0043 -0.1078 0.0510 0.122 Uiso 0.50 1 calc PR . .
H93B H -0.0434 -0.1357 -0.0279 0.122 Uiso 0.50 1 calc PR . .
C94 C -0.028(2) -0.0274(6) -0.024(2) 0.41(8) Uiso 0.50 1 d PD . .
H94A H -0.0280 -0.0206 -0.0740 0.491 Uiso 0.50 1 calc PR . .
H94B H -0.0835 -0.0201 -0.0233 0.491 Uiso 0.50 1 calc PR . .
Re1 Re 0.02939(4) 0.02845(4) 0.73379(3) 0.0673(2) Uani 1 1 d . . .
Re2 Re 0.52849(3) 0.92165(3) 0.72384(3) 0.05937(19) Uani 1 1 d . . .
O1 O -0.0237(10) -0.0928(8) 0.8131(6) 0.126(6) Uani 1 1 d . . .
O2 O -0.0643(8) 0.1262(8) 0.8077(6) 0.107(4) Uani 1 1 d . . .
O3 O 0.1852(6) 0.0377(6) 0.8674(5) 0.084(3) Uani 1 1 d . . .
O4 O 0.3878(10) 0.9235(11) 0.5791(8) 0.181(9) Uani 1 1 d . . .
O5 O 0.4259(7) 0.8062(7) 0.7654(9) 0.120(5) Uani 1 1 d . . .
O6 O 0.4341(7) 1.0265(7) 0.7912(6) 0.103(4) Uani 1 1 d . . .
O7 O 0.9502(7) 0.7935(7) 0.6881(5) 0.102(4) Uani 1 1 d . . .
O8 O 0.9110(10) 0.7819(8) 0.5706(5) 0.141(6) Uani 1 1 d . . .
O9 O 0.8731(6) 0.7048(5) 0.6352(4) 0.069(2) Uani 1 1 d . . .
O10 O 0.5618(6) 0.6859(5) 0.7951(5) 0.075(2) Uani 1 1 d . . .
O11 O 0.6915(6) 0.6739(6) 0.8488(7) 0.091(3) Uani 1 1 d . . .
O12 O 0.6087(7) 0.5990(5) 0.8735(5) 0.078(3) Uani 1 1 d . . .
N1 N 0.0634(5) 0.1180(6) 0.6739(5) 0.057(2) Uani 1 1 d . . .
N2 N 0.1010(6) 0.1758(6) 0.7128(5) 0.058(2) Uani 1 1 d . . .
H011 H 0.1106 0.1807 0.7591 0.070 Uiso 1 1 calc R . .
N3 N 0.0975(7) -0.0443(7) 0.6817(6) 0.071(3) Uani 1 1 d . . .
N4 N 0.0725(11) -0.1100(9) 0.6611(8) 0.117(6) Uani 1 1 d . . .
H026 H 0.0266 -0.1274 0.6624 0.141 Uiso 1 1 calc R . .
N5 N -0.0838(7) 0.0221(9) 0.6383(6) 0.084(4) Uani 1 1 d . . .
N6 N -0.2170(10) -0.1046(12) 0.5116(7) 0.147(8) Uani 1 1 d . . .
H03A H -0.2605 -0.1034 0.4739 0.177 Uiso 1 1 calc R . .
H03B H -0.1944 -0.1451 0.5279 0.177 Uiso 1 1 calc R . .
N7 N 0.5910(6) 0.8471(5) 0.6694(5) 0.054(2) Uani 1 1 d . . .
N8 N 0.6131(6) 0.7800(5) 0.6927(5) 0.054(2) Uani 1 1 d . . .
H008 H 0.6079 0.7629 0.7324 0.064 Uiso 1 1 calc R . .
N9 N 0.6010(8) 1.0055(6) 0.6963(7) 0.076(3) Uani 1 1 d . . .
N10 N 0.5614(9) 1.0678(6) 0.6629(7) 0.084(4) Uani 1 1 d . . .
H035 H 0.5095 1.0755 0.6530 0.101 Uiso 1 1 calc R . .
N11 N 0.6291(6) 0.9168(6) 0.8302(5) 0.062(3) Uani 1 1 d . . .
N12 N 0.7461(8) 0.7865(8) 0.9636(6) 0.094(4) Uani 1 1 d . . .
H03G H 0.7835 0.7861 1.0058 0.113 Uiso 1 1 calc R . .
H03H H 0.7261 0.7468 0.9426 0.113 Uiso 1 1 calc R . .
N13 N 0.9121(8) 0.7582(8) 0.6315(6) 0.087(4) Uani 1 1 d . . .
N14 N 0.6194(7) 0.6534(6) 0.8383(6) 0.065(3) Uani 1 1 d . . .
C1 C -0.0030(11) -0.0519(10) 0.7829(8) 0.090(5) Uani 1 1 d . . .
C2 C -0.0283(9) 0.0921(13) 0.7800(7) 0.101(7) Uani 1 1 d . . .
C3 C 0.1263(9) 0.0356(8) 0.8167(7) 0.070(4) Uani 1 1 d . . .
C4 C 0.4422(12) 0.9262(11) 0.6347(9) 0.106(6) Uani 1 1 d . . .
C5 C 0.4675(9) 0.8492(8) 0.7499(9) 0.078(4) Uani 1 1 d . . .
C6 C 0.4719(8) 0.9875(7) 0.7681(7) 0.063(3) Uani 1 1 d . . .
C11 C 0.0612(8) 0.1320(8) 0.6055(6) 0.067(4) Uani 1 1 d . . .
C12 C 0.0958(8) 0.1966(8) 0.6010(7) 0.071(4) Uani 1 1 d . . .
H022 H 0.1010 0.2178 0.5590 0.086 Uiso 1 1 calc R . .
C13 C 0.1216(6) 0.2246(7) 0.6707(6) 0.055(3) Uani 1 1 d . . .
C14 C 0.0292(10) 0.0786(10) 0.5442(8) 0.091(5) Uani 1 1 d . . .
H04A H 0.0742 0.0510 0.5389 0.137 Uiso 1 1 calc R . .
H04B H 0.0024 0.1037 0.4995 0.137 Uiso 1 1 calc R . .
H04C H -0.0095 0.0471 0.5553 0.137 Uiso 1 1 calc R . .
C15 C 0.1644(8) 0.2924(7) 0.6995(7) 0.066(3) Uani 1 1 d . . .
H02A H 0.1545 0.3047 0.7443 0.099 Uiso 1 1 calc R . .
H02B H 0.1440 0.3300 0.6644 0.099 Uiso 1 1 calc R . .
H02C H 0.2225 0.2866 0.7087 0.099 Uiso 1 1 calc R . .
C21 C 0.1261(16) -0.1461(12) 0.6383(13) 0.133(9) Uani 1 1 d . . .
C22 C 0.1915(13) -0.1030(10) 0.6453(11) 0.114(7) Uani 1 1 d . . .
H061 H 0.2394 -0.1141 0.6348 0.136 Uiso 1 1 calc R . .
C23 C 0.1712(9) -0.0369(10) 0.6722(8) 0.088(5) Uani 1 1 d . . .
C24 C 0.1122(17) -0.2201(12) 0.6124(19) 0.196(15) Uani 1 1 d . . .
H07A H 0.0913 -0.2475 0.6447 0.294 Uiso 1 1 calc R . .
H07B H 0.1633 -0.2406 0.6115 0.294 Uiso 1 1 calc R . .
H07C H 0.0731 -0.2209 0.5640 0.294 Uiso 1 1 calc R . .
C25 C 0.2234(9) 0.0279(9) 0.6894(11) 0.096(5) Uani 1 1 d . . .
H05A H 0.1991 0.0648 0.6544 0.144 Uiso 1 1 calc R . .
H05B H 0.2772 0.0166 0.6872 0.144 Uiso 1 1 calc R . .
H05C H 0.2278 0.0443 0.7376 0.144 Uiso 1 1 calc R . .
C34 C -0.1220(10) 0.0853(14) 0.6113(9) 0.107(7) Uani 1 1 d . . .
H50 H -0.1013 0.1287 0.6334 0.129 Uiso 1 1 calc R . .
C35 C -0.1931(11) 0.0834(17) 0.5496(11) 0.142(10) Uani 1 1 d . . .
H053 H -0.2207 0.1256 0.5304 0.170 Uiso 1 1 calc R . .
C36 C -0.2211(11) 0.0179(17) 0.5179(10) 0.114(8) Uani 1 1 d . . .
H041 H -0.2674 0.0170 0.4763 0.136 Uiso 1 1 calc R . .
C37 C -0.1848(11) -0.0443(15) 0.5445(10) 0.106(7) Uani 1 1 d . . .
C38 C -0.1145(9) -0.0405(10) 0.6068(7) 0.082(5) Uani 1 1 d . . .
H034 H -0.0883 -0.0829 0.6270 0.099 Uiso 1 1 calc R . .
C41 C 0.6444(7) 0.7417(6) 0.6479(7) 0.057(3) Uani 1 1 d . . .
C42 C 0.6432(9) 0.7888(8) 0.5924(7) 0.073(4) Uani 1 1 d . . .
H42 H 0.6614 0.7795 0.5528 0.088 Uiso 1 1 calc R . .
C43 C 0.6096(10) 0.8523(8) 0.6069(8) 0.077(4) Uani 1 1 d . . .
C44 C 0.6745(9) 0.6660(7) 0.6642(9) 0.077(4) Uani 1 1 d . . .
H03D H 0.7002 0.6604 0.7160 0.116 Uiso 1 1 calc R . .
H03E H 0.7138 0.6557 0.6396 0.116 Uiso 1 1 calc R . .
H03F H 0.6289 0.6336 0.6475 0.116 Uiso 1 1 calc R . .
C45 C 0.5964(15) 0.9186(10) 0.5598(9) 0.124(8) Uani 1 1 d . . .
H05D H 0.5403 0.9340 0.5481 0.185 Uiso 1 1 calc R . .
H05E H 0.6083 0.9080 0.5156 0.185 Uiso 1 1 calc R . .
H05F H 0.6324 0.9561 0.5859 0.185 Uiso 1 1 calc R . .
C51 C 0.6134(15) 1.1140(10) 0.6480(12) 0.122(8) Uani 1 1 d . . .
C52 C 0.6875(15) 1.0832(10) 0.6733(14) 0.132(9) Uani 1 1 d . . .
H056 H 0.7358 1.1033 0.6700 0.158 Uiso 1 1 calc R . .
C53 C 0.6831(11) 1.0177(10) 0.7048(11) 0.101(6) Uani 1 1 d . . .
C54 C 0.5799(17) 1.1813(11) 0.6068(14) 0.162(12) Uani 1 1 d . . .
H04D H 0.5415 1.1692 0.5599 0.242 Uiso 1 1 calc R . .
H04E H 0.6243 1.2089 0.6002 0.242 Uiso 1 1 calc R . .
H04F H 0.5524 1.2090 0.6340 0.242 Uiso 1 1 calc R . .
C55 C 0.7486(11) 0.9626(10) 0.7365(12) 0.110(6) Uani 1 1 d . . .
H06A H 0.7761 0.9515 0.7016 0.165 Uiso 1 1 calc R . .
H06B H 0.7239 0.9199 0.7480 0.165 Uiso 1 1 calc R . .
H06C H 0.7878 0.9813 0.7803 0.165 Uiso 1 1 calc R . .
C61 C 0.6610(10) 0.9780(9) 0.8651(9) 0.089(5) Uani 1 1 d . . .
H048 H 0.6426 1.0220 0.8432 0.107 Uiso 1 1 calc R . .
C62 C 0.7195(13) 0.9759(12) 0.9316(11) 0.122(7) Uani 1 1 d . . .
H046 H 0.7388 1.0187 0.9559 0.146 Uiso 1 1 calc R . .
C63 C 0.7515(5) 0.9113(5) 0.9644(4) 0.124(8) Uani 1 1 d . . .
H52 H 0.7941 0.9104 1.0087 0.148 Uiso 1 1 calc R . .
C64 C 0.7189(5) 0.8497(5) 0.9302(4) 0.073(4) Uani 1 1 d R . .
C65 C 0.6580(5) 0.8558(5) 0.8642(4) 0.060(3) Uani 1 1 d R . .
H023 H 0.6348 0.8135 0.8410 0.071 Uiso 1 1 d R . .
Cl91 Cl 0.5960(16) 0.2635(15) 0.9199(12) 0.161(11) Uani 0.25 1 d PG . .
Cl92 Cl 0.6849(16) 0.1696(11) 0.8573(18) 0.177(13) Uani 0.25 1 d PG . .
C90 C 0.5950(19) 0.1770(16) 0.883(3) 0.081(17) Uani 0.25 1 d PG . .
H90A H 0.5948 0.1407 0.9187 0.097 Uiso 0.25 1 d PG . .
H90B H 0.5464 0.1706 0.8403 0.097 Uiso 0.25 1 d PG . .
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C93 C92 H92A 109.5 . . ?
C93 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C93 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C92 C93 C94 112.1(2) . . ?
C92 C93 H93A 109.2 . . ?
C94 C93 H93A 109.2 . . ?
C92 C93 H93B 109.2 . . ?
C94 C93 H93B 109.2 . . ?
H93A C93 H93B 107.9 . . ?
C94 C94 C93 112.1(2) 3 . ?
C94 C94 H94A 109.2 3 . ?
C93 C94 H94A 109.2 . . ?
C94 C94 H94B 109.2 3 . ?
C93 C94 H94B 109.2 . . ?
H94A C94 H94B 107.9 . . ?
C3 Re1 C2 90.4(6) . . ?
C3 Re1 C1 87.3(6) . . ?
C2 Re1 C1 88.8(8) . . ?
C3 Re1 N5 178.9(6) . . ?
C2 Re1 N5 88.6(6) . . ?
C1 Re1 N5 93.1(6) . . ?
C3 Re1 N1 94.7(5) . . ?
C2 Re1 N1 92.2(6) . . ?
C1 Re1 N1 177.8(5) . . ?
N5 Re1 N1 85.0(4) . . ?
C3 Re1 N3 88.8(5) . . ?
C2 Re1 N3 179.2(5) . . ?
C1 Re1 N3 91.4(6) . . ?
N5 Re1 N3 92.2(4) . . ?
N1 Re1 N3 87.7(4) . . ?
C5 Re2 C4 86.3(9) . . ?
C5 Re2 C6 86.4(6) . . ?
C4 Re2 C6 90.9(7) . . ?
C5 Re2 N9 178.6(6) . . ?
C4 Re2 N9 95.1(8) . . ?
C6 Re2 N9 93.4(5) . . ?
C5 Re2 N7 94.1(5) . . ?
C4 Re2 N7 87.3(6) . . ?
C6 Re2 N7 178.1(5) . . ?
N9 Re2 N7 86.2(4) . . ?
C5 Re2 N11 93.3(6) . . ?
C4 Re2 N11 179.0(6) . . ?
C6 Re2 N11 88.2(5) . . ?
N9 Re2 N11 85.4(5) . . ?
N7 Re2 N11 93.6(3) . . ?
C11 N1 N2 104.5(10) . . ?
C11 N1 Re1 137.4(9) . . ?
N2 N1 Re1 118.1(7) . . ?
C13 N2 N1 112.1(9) . . ?
C13 N2 H011 123.9 . . ?
N1 N2 H011 123.9 . . ?
N4 N3 C23 106.5(14) . . ?
N4 N3 Re1 122.3(9) . . ?
C23 N3 Re1 130.7(11) . . ?
N3 N4 C21 112.4(14) . . ?
N3 N4 H026 123.8 . . ?
C21 N4 H026 123.8 . . ?
C38 N5 C34 120.4(15) . . ?
C38 N5 Re1 122.4(13) . . ?
C34 N5 Re1 117.2(11) . . ?
C37 N6 H03A 120.0 . . ?
C37 N6 H03B 120.0 . . ?
H03A N6 H03B 120.0 . . ?
N8 N7 C43 104.2(10) . . ?
N8 N7 Re2 123.6(7) . . ?
C43 N7 Re2 132.0(9) . . ?
N7 N8 C41 113.8(9) . . ?
N7 N8 H008 123.1 . . ?
C41 N8 H008 123.1 . . ?
C53 N9 N10 104.1(12) . . ?
C53 N9 Re2 137.1(10) . . ?
N10 N9 Re2 118.7(9) . . ?
C51 N10 N9 112.1(14) . . ?
C51 N10 H035 123.9 . . ?
N9 N10 H035 123.9 . . ?
C65 N11 C61 116.8(11) . . ?
C65 N11 Re2 123.3(8) . . ?
C61 N11 Re2 119.8(10) . . ?
C64 N12 H03G 120.0 . . ?
C64 N12 H03H 120.0 . . ?
H03G N12 H03H 120.0 . . ?
O9 N13 O8 120.2(11) . . ?
O9 N13 O7 121.2(11) . . ?
O8 N13 O7 118.4(12) . . ?
O10 N14 O11 119.9(11) . . ?
O10 N14 O12 122.3(11) . . ?
O11 N14 O12 117.8(12) . . ?
O1 C1 Re1 174.3(18) . . ?
O2 C2 Re1 176.4(17) . . ?
O3 C3 Re1 177.9(13) . . ?
O4 C4 Re2 175(2) . . ?
O5 C5 Re2 176.5(12) . . ?
O6 C6 Re2 176.1(13) . . ?
N1 C11 C12 111.3(11) . . ?
N1 C11 C14 122.3(13) . . ?
C12 C11 C14 126.3(12) . . ?
C11 C12 C13 106.5(11) . . ?
C11 C12 H022 126.8 . . ?
C13 C12 H022 126.8 . . ?
N2 C13 C12 105.7(11) . . ?
N2 C13 C15 123.2(10) . . ?
C12 C13 C15 131.1(12) . . ?
C11 C14 H04A 109.5 . . ?
C11 C14 H04B 109.5 . . ?
H04A C14 H04B 109.5 . . ?
C11 C14 H04C 109.5 . . ?
H04A C14 H04C 109.5 . . ?
H04B C14 H04C 109.5 . . ?
C13 C15 H02A 109.5 . . ?
C13 C15 H02B 109.5 . . ?
H02A C15 H02B 109.5 . . ?
C13 C15 H02C 109.5 . . ?
H02A C15 H02C 109.5 . . ?
H02B C15 H02C 109.5 . . ?
N4 C21 C22 107.9(17) . . ?
N4 C21 C24 122.8(19) . . ?
C22 C21 C24 129(2) . . ?
C21 C22 C23 104.9(17) . . ?
C21 C22 H061 127.5 . . ?
C23 C22 H061 127.5 . . ?
N3 C23 C22 108.2(15) . . ?
N3 C23 C25 125.7(16) . . ?
C22 C23 C25 126.1(15) . . ?
C21 C24 H07A 109.5 . . ?
C21 C24 H07B 109.5 . . ?
H07A C24 H07B 109.5 . . ?
C21 C24 H07C 109.5 . . ?
H07A C24 H07C 109.5 . . ?
H07B C24 H07C 109.5 . . ?
C23 C25 H05A 109.5 . . ?
C23 C25 H05B 109.5 . . ?
H05A C25 H05B 109.5 . . ?
C23 C25 H05C 109.5 . . ?
H05A C25 H05C 109.5 . . ?
H05B C25 H05C 109.5 . . ?
N5 C34 C35 119(2) . . ?
N5 C34 H50 120.6 . . ?
C35 C34 H50 120.6 . . ?
C36 C35 C34 119(2) . . ?
C36 C35 H053 120.6 . . ?
C34 C35 H053 120.6 . . ?
C37 C36 C35 123.0(19) . . ?
C37 C36 H041 118.5 . . ?
C35 C36 H041 118.5 . . ?
N6 C37 C36 119(2) . . ?
N6 C37 C38 124(3) . . ?
C36 C37 C38 117(2) . . ?
N5 C38 C37 122.4(19) . . ?
N5 C38 H034 118.8 . . ?
C37 C38 H034 118.8 . . ?
N8 C41 C42 104.5(10) . . ?
N8 C41 C44 122.7(11) . . ?
C42 C41 C44 132.8(12) . . ?
C41 C42 C43 106.9(12) . . ?
C41 C42 H42 126.5 . . ?
C43 C42 H42 126.5 . . ?
N7 C43 C42 110.6(13) . . ?
N7 C43 C45 124.5(13) . . ?
C42 C43 C45 124.9(14) . . ?
C41 C44 H03D 109.5 . . ?
C41 C44 H03E 109.5 . . ?
H03D C44 H03E 109.5 . . ?
C41 C44 H03F 109.5 . . ?
H03D C44 H03F 109.5 . . ?
H03E C44 H03F 109.5 . . ?
C43 C45 H05D 109.5 . . ?
C43 C45 H05E 109.5 . . ?
H05D C45 H05E 109.5 . . ?
C43 C45 H05F 109.5 . . ?
H05D C45 H05F 109.5 . . ?
H05E C45 H05F 109.5 . . ?
N10 C51 C52 105.4(16) . . ?
N10 C51 C54 119(2) . . ?
C52 C51 C54 135(2) . . ?
C51 C52 C53 111.2(18) . . ?
C51 C52 H056 124.4 . . ?
C53 C52 H056 124.4 . . ?
C52 C53 N9 107.0(16) . . ?
C52 C53 C55 130.3(17) . . ?
N9 C53 C55 122.4(16) . . ?
C51 C54 H04D 109.5 . . ?
C51 C54 H04E 109.5 . . ?
H04D C54 H04E 109.5 . . ?
C51 C54 H04F 109.5 . . ?
H04D C54 H04F 109.5 . . ?
H04E C54 H04F 109.5 . . ?
C53 C55 H06A 109.5 . . ?
C53 C55 H06B 109.5 . . ?
H06A C55 H06B 109.5 . . ?
C53 C55 H06C 109.5 . . ?
H06A C55 H06C 109.5 . . ?
H06B C55 H06C 109.5 . . ?
N11 C61 C62 120.5(17) . . ?
N11 C61 H048 119.7 . . ?
C62 C61 H048 119.7 . . ?
C61 C62 C63 121.5(16) . . ?
C61 C62 H046 119.3 . . ?
C63 C62 H046 119.3 . . ?
C64 C63 C62 118.2(9) . . ?
C64 C63 H52 120.9 . . ?
C62 C63 H52 120.9 . . ?
N12 C64 C63 118.7(8) . . ?
N12 C64 C65 124.1(8) . . ?
C63 C64 C65 117.1 . . ?
N11 C65 C64 125.8(6) . . ?
N11 C65 H023 116.9 . . ?
C64 C65 H023 117.3 . . ?
Cl91 C90 Cl92 106.8 . . ?
Cl91 C90 H90A 110.4 . . ?
Cl92 C90 H90A 110.4 . . ?
Cl91 C90 H90B 110.4 . . ?
Cl92 C90 H90B 110.4 . . ?
H90A C90 H90B 108.6 . . ?
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
C92 C93 1.498(2) . ?
C92 H92A 0.9600 . ?
C92 H92B 0.9600 . ?
C92 H92C 0.9600 . ?
C93 C94 1.498(2) . ?
C93 H93A 0.9700 . ?
C93 H93B 0.9700 . ?
C94 C94 1.498(2) 3 ?
C94 H94A 0.9700 . ?
C94 H94B 0.9700 . ?
Re1 C3 1.907(14) . ?
Re1 C2 1.936(19) . ?
Re1 C1 1.945(17) . ?
Re1 N5 2.210(12) . ?
Re1 N1 2.211(10) . ?
Re1 N3 2.228(12) . ?
Re2 C5 1.872(16) . ?
Re2 C4 1.877(16) . ?
Re2 C6 1.926(12) . ?
Re2 N9 2.166(12) . ?
Re2 N7 2.215(9) . ?
Re2 N11 2.220(10) . ?
O1 C1 1.086(17) . ?
O2 C2 1.13(2) . ?
O3 C3 1.159(16) . ?
O4 C4 1.18(2) . ?
O5 C5 1.174(18) . ?
O6 C6 1.152(15) . ?
O7 N13 1.263(14) . ?
O8 N13 1.249(14) . ?
O9 N13 1.213(14) . ?
O10 N14 1.230(14) . ?
O11 N14 1.246(14) . ?
O12 N14 1.266(13) . ?
N1 C11 1.335(14) . ?
N1 N2 1.353(14) . ?
N2 C13 1.340(15) . ?
N2 H011 0.8600 . ?
N3 N4 1.315(18) . ?
N3 C23 1.340(18) . ?
N4 C21 1.32(3) . ?
N4 H026 0.8600 . ?
N5 C38 1.342(19) . ?
N5 C34 1.37(2) . ?
N6 C37 1.32(3) . ?
N6 H03A 0.8600 . ?
N6 H03B 0.8600 . ?
N7 N8 1.340(12) . ?
N7 C43 1.346(16) . ?
N8 C41 1.357(14) . ?
N8 H008 0.8600 . ?
N9 C53 1.38(2) . ?
N9 N10 1.394(14) . ?
N10 C51 1.34(2) . ?
N10 H035 0.8600 . ?
N11 C65 1.326(13) . ?
N11 C61 1.348(18) . ?
N12 C64 1.350(15) . ?
N12 H03G 0.8600 . ?
N12 H03H 0.8600 . ?
C11 C12 1.358(19) . ?
C11 C14 1.508(18) . ?
C12 C13 1.377(17) . ?
C12 H022 0.9300 . ?
C13 C15 1.478(18) . ?
C14 H04A 0.9600 . ?
C14 H04B 0.9600 . ?
C14 H04C 0.9600 . ?
C15 H02A 0.9600 . ?
C15 H02B 0.9600 . ?
C15 H02C 0.9600 . ?
C21 C22 1.35(2) . ?
C21 C24 1.46(3) . ?
C22 C23 1.42(2) . ?
C22 H061 0.9300 . ?
C23 C25 1.48(2) . ?
C24 H07A 0.9600 . ?
C24 H07B 0.9600 . ?
C24 H07C 0.9600 . ?
C25 H05A 0.9600 . ?
C25 H05B 0.9600 . ?
C25 H05C 0.9600 . ?
C34 C35 1.41(2) . ?
C34 H50 0.9300 . ?
C35 C36 1.38(3) . ?
C35 H053 0.9300 . ?
C36 C37 1.34(3) . ?
C36 H041 0.9300 . ?
C37 C38 1.41(2) . ?
C38 H034 0.9300 . ?
C41 C42 1.378(18) . ?
C41 C44 1.501(17) . ?
C42 C43 1.384(19) . ?
C42 H42 0.9300 . ?
C43 C45 1.51(2) . ?
C44 H03D 0.9600 . ?
C44 H03E 0.9600 . ?
C44 H03F 0.9600 . ?
C45 H05D 0.9600 . ?
C45 H05E 0.9600 . ?
C45 H05F 0.9600 . ?
C51 C52 1.34(3) . ?
C51 C54 1.50(2) . ?
C52 C53 1.37(2) . ?
C52 H056 0.9300 . ?
C53 C55 1.50(2) . ?
C54 H04D 0.9600 . ?
C54 H04E 0.9600 . ?
C54 H04F 0.9600 . ?
C55 H06A 0.9600 . ?
C55 H06B 0.9600 . ?
C55 H06C 0.9600 . ?
C61 C62 1.35(2) . ?
C61 H048 0.9300 . ?
C62 C63 1.39(2) . ?
C62 H046 0.9300 . ?
C63 C64 1.3539 . ?
C63 H52 0.9300 . ?
C64 C65 1.3675 . ?
C65 H023 0.9300 . ?
Cl91 C90 1.7637 . ?
Cl92 C90 1.7656 . ?
C90 H90A 0.9700 . ?
C90 H90B 0.9700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N12 H03H O11 0.86 2.19 2.98(2) 152.2 .
N10 H035 O12 0.86 1.97 2.832(17) 176.1 2_656
N8 H008 O10 0.86 2.18 2.978(13) 153.8 .
N6 H03B O8 0.86 2.20 3.00(3) 154.0 1_445
N4 H026 O7 0.86 2.13 2.933(16) 154.8 1_445
N2 H011 O9 0.86 2.02 2.874(12) 172.7 2_646
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C92 C93 C94 C94 -68(7) . . . 3 ?
C3 Re1 N1 C11 137.5(13) . . . . ?
C2 Re1 N1 C11 -131.9(13) . . . . ?
N5 Re1 N1 C11 -43.6(13) . . . . ?
N3 Re1 N1 C11 48.8(12) . . . . ?
C3 Re1 N1 N2 -38.1(9) . . . . ?
C2 Re1 N1 N2 52.4(9) . . . . ?
N5 Re1 N1 N2 140.8(8) . . . . ?
N3 Re1 N1 N2 -126.8(8) . . . . ?
C11 N1 N2 C13 0.2(13) . . . . ?
Re1 N1 N2 C13 177.1(7) . . . . ?
C3 Re1 N3 N4 121.5(13) . . . . ?
C1 Re1 N3 N4 34.2(13) . . . . ?
N5 Re1 N3 N4 -58.9(13) . . . . ?
N1 Re1 N3 N4 -143.8(12) . . . . ?
C3 Re1 N3 C23 -50.1(14) . . . . ?
C1 Re1 N3 C23 -137.4(14) . . . . ?
N5 Re1 N3 C23 129.5(14) . . . . ?
N1 Re1 N3 C23 44.6(14) . . . . ?
C23 N3 N4 C21 0(2) . . . . ?
Re1 N3 N4 C21 -173.7(15) . . . . ?
C2 Re1 N5 C38 -132.5(11) . . . . ?
C1 Re1 N5 C38 -43.8(11) . . . . ?
N1 Re1 N5 C38 135.2(10) . . . . ?
N3 Re1 N5 C38 47.7(10) . . . . ?
C2 Re1 N5 C34 48.1(11) . . . . ?
C1 Re1 N5 C34 136.8(11) . . . . ?
N1 Re1 N5 C34 -44.2(10) . . . . ?
N3 Re1 N5 C34 -131.7(10) . . . . ?
C5 Re2 N7 N8 -35.1(10) . . . . ?
C4 Re2 N7 N8 -121.2(11) . . . . ?
N9 Re2 N7 N8 143.5(9) . . . . ?
N11 Re2 N7 N8 58.4(9) . . . . ?
C5 Re2 N7 C43 138.9(13) . . . . ?
C4 Re2 N7 C43 52.8(14) . . . . ?
N9 Re2 N7 C43 -42.5(13) . . . . ?
N11 Re2 N7 C43 -127.6(13) . . . . ?
C43 N7 N8 C41 -0.5(14) . . . . ?
Re2 N7 N8 C41 174.9(8) . . . . ?
C4 Re2 N9 C53 -138.7(18) . . . . ?
C6 Re2 N9 C53 130.0(18) . . . . ?
N7 Re2 N9 C53 -51.8(17) . . . . ?
N11 Re2 N9 C53 42.1(17) . . . . ?
C4 Re2 N9 N10 44.0(11) . . . . ?
C6 Re2 N9 N10 -47.3(11) . . . . ?
N7 Re2 N9 N10 130.9(10) . . . . ?
N11 Re2 N9 N10 -135.2(10) . . . . ?
C53 N9 N10 C51 3.0(19) . . . . ?
Re2 N9 N10 C51 -178.9(12) . . . . ?
C5 Re2 N11 C65 41.0(9) . . . . ?
C6 Re2 N11 C65 127.2(9) . . . . ?
N9 Re2 N11 C65 -139.2(8) . . . . ?
N7 Re2 N11 C65 -53.3(8) . . . . ?
C5 Re2 N11 C61 -135.7(12) . . . . ?
C6 Re2 N11 C61 -49.5(12) . . . . ?
N9 Re2 N11 C61 44.1(11) . . . . ?
N7 Re2 N11 C61 130.0(11) . . . . ?
N2 N1 C11 C12 -0.4(15) . . . . ?
Re1 N1 C11 C12 -176.4(9) . . . . ?
N2 N1 C11 C14 175.7(13) . . . . ?
Re1 N1 C11 C14 0(2) . . . . ?
N1 C11 C12 C13 0.4(16) . . . . ?
C14 C11 C12 C13 -175.5(14) . . . . ?
N1 N2 C13 C12 0.0(13) . . . . ?
N1 N2 C13 C15 -179.2(10) . . . . ?
C11 C12 C13 N2 -0.3(15) . . . . ?
C11 C12 C13 C15 178.9(13) . . . . ?
N3 N4 C21 C22 1(3) . . . . ?
N3 N4 C21 C24 -180(2) . . . . ?
N4 C21 C22 C23 -2(3) . . . . ?
C24 C21 C22 C23 179(3) . . . . ?
N4 N3 C23 C22 -0.8(19) . . . . ?
Re1 N3 C23 C22 171.7(12) . . . . ?
N4 N3 C23 C25 -178.9(17) . . . . ?
Re1 N3 C23 C25 -6(2) . . . . ?
C21 C22 C23 N3 2(2) . . . . ?
C21 C22 C23 C25 180(2) . . . . ?
C38 N5 C34 C35 -1(2) . . . . ?
Re1 N5 C34 C35 178.6(12) . . . . ?
N5 C34 C35 C36 -1(3) . . . . ?
C34 C35 C36 C37 2(3) . . . . ?
C35 C36 C37 N6 178.5(17) . . . . ?
C35 C36 C37 C38 -1(3) . . . . ?
C34 N5 C38 C37 2(2) . . . . ?
Re1 N5 C38 C37 -177.6(10) . . . . ?
N6 C37 C38 N5 179.8(14) . . . . ?
C36 C37 C38 N5 -1(2) . . . . ?
N7 N8 C41 C42 1.0(14) . . . . ?
N7 N8 C41 C44 178.8(11) . . . . ?
N8 C41 C42 C43 -1.0(15) . . . . ?
C44 C41 C42 C43 -178.5(15) . . . . ?
N8 N7 C43 C42 -0.2(16) . . . . ?
Re2 N7 C43 C42 -175.0(9) . . . . ?
N8 N7 C43 C45 -179.6(17) . . . . ?
Re2 N7 C43 C45 6(2) . . . . ?
C41 C42 C43 N7 0.8(18) . . . . ?
C41 C42 C43 C45 -179.8(17) . . . . ?
N9 N10 C51 C52 -2(2) . . . . ?
N9 N10 C51 C54 175.4(17) . . . . ?
N10 C51 C52 C53 -1(3) . . . . ?
C54 C51 C52 C53 -177(3) . . . . ?
C51 C52 C53 N9 2(3) . . . . ?
C51 C52 C53 C55 176(2) . . . . ?
N10 N9 C53 C52 -3(2) . . . . ?
Re2 N9 C53 C52 179.3(14) . . . . ?
N10 N9 C53 C55 -177.7(17) . . . . ?
Re2 N9 C53 C55 5(3) . . . . ?
C65 N11 C61 C62 0(2) . . . . ?
Re2 N11 C61 C62 176.8(15) . . . . ?
N11 C61 C62 C63 3(3) . . . . ?
C61 C62 C63 C64 -4(2) . . . . ?
C62 C63 C64 N12 -176.2(14) . . . . ?
C62 C63 C64 C65 1.9(11) . . . . ?
C61 N11 C65 C64 -2.2(14) . . . . ?
Re2 N11 C65 C64 -179.0(3) . . . . ?
N12 C64 C65 N11 179.3(12) . . . . ?
C63 C64 C65 N11 1.3(7) . . . . ?
