#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:39:18 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179071 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/33/4303366.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_4303366
loop_
_publ_author_name
'Siu-Tung Lam'
'Nianyong Zhu'
'Vivian Wing-Wah Yam'
_publ_section_title
;
Synthesis and Characterization of Luminescent Rhenium(I) Tricarbonyl
Diimine Complexes with a Triarylboron Moiety and the Study of Their
Fluoride Ion-Binding Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9664
_journal_page_last               9670
_journal_paper_doi               10.1021/ic900803a
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C53 H50 B N2 O3 Re'
_chemical_formula_sum            'C53 H50 B N2 O3 Re'
_chemical_formula_weight         959.96
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.81(2)
_cell_angle_beta                 98.15(2)
_cell_angle_gamma                92.75(2)
_cell_formula_units_Z            2
_cell_length_a                   9.463(2)
_cell_length_b                   13.821(2)
_cell_length_c                   20.383(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2500.6(9)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker Smart CCD 1000'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15223
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    2.470
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.676319
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.200
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         9170
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1566P)²+8.4711P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2051
_refine_ls_wR_factor_ref         0.2172
_reflns_number_gt                7707
_reflns_number_total             9170
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900803a_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2500.6(8)
_cod_database_code               4303366
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
C4 C 0.7075(9) 0.2530(6) 0.6427(4) 0.0548(17) Uani 1 1 d . . .
C5 C 0.6385(8) 0.2362(6) 0.6831(4) 0.0532(17) Uani 1 1 d . A .
C6 C 0.5495(7) 0.2220(5) 0.7317(3) 0.0481(15) Uani 1 1 d . . .
C7 C 0.5797(8) 0.1527(6) 0.7684(4) 0.0519(16) Uani 1 1 d . A .
C8 C 0.4918(8) 0.1399(6) 0.8146(4) 0.0559(17) Uani 1 1 d . . .
C9 C 0.3754(8) 0.2003(6) 0.8294(4) 0.0508(16) Uani 1 1 d . A .
C10 C 0.3473(8) 0.2726(6) 0.7932(4) 0.0506(16) Uani 1 1 d . . .
C11 C 0.4330(8) 0.2820(6) 0.7441(4) 0.0495(15) Uani 1 1 d . A .
B1 B 0.2736(9) 0.1837(7) 0.8797(4) 0.0522(18) Uani 1 1 d . . .
C12 C 0.2506(8) 0.2776(6) 0.9462(4) 0.0529(16) Uani 1 1 d . A .
C13 C 0.3691(9) 0.3358(6) 0.9930(4) 0.062(2) Uani 1 1 d . . .
C14 C 0.3510(10) 0.4132(6) 1.0524(4) 0.064(2) Uani 1 1 d . A .
C15 C 0.2091(10) 0.4302(6) 1.0665(5) 0.065(2) Uani 1 1 d . . .
C16 C 0.0899(9) 0.3752(6) 1.0195(4) 0.0579(18) Uani 1 1 d . A .
C17 C 0.1111(9) 0.2983(6) 0.9597(4) 0.0558(17) Uani 1 1 d . . .
C18 C 0.1918(13) 0.5076(7) 1.1301(5) 0.078(3) Uani 1 1 d . A .
C19 C 0.1796(16) 0.5669(9) 1.1803(7) 0.107(4) Uani 1 1 d . . .
H19 H 0.1695 0.6160 1.2219 0.128 Uiso 1 1 calc R A .
C20 C 0.1942(8) 0.0739(6) 0.8677(4) 0.0526(16) Uani 1 1 d . A .
C21 C 0.2005(9) 0.0317(6) 0.9235(4) 0.0580(18) Uani 1 1 d . . .
C22 C 0.1250(11) -0.0625(6) 0.9133(4) 0.065(2) Uani 1 1 d . A .
C23 C 0.0455(12) -0.1143(7) 0.8485(5) 0.072(2) Uani 1 1 d . . .
C24 C 0.0367(10) -0.0747(6) 0.7920(4) 0.0622(19) Uani 1 1 d . A .
C25 C 0.1122(8) 0.0185(6) 0.8024(4) 0.0529(16) Uani 1 1 d . . .
C26 C -0.0341(16) -0.2134(9) 0.8382(7) 0.102(4) Uani 1 1 d . A .
C27 C -0.090(2) -0.2890(13) 0.8299(9) 0.156(9) Uani 1 1 d . . .
H27 H -0.1372 -0.3528 0.8228 0.187 Uiso 1 1 calc R A .
C28 C 0.7065(9) 0.0911(8) 0.7556(5) 0.070(2) Uani 1 1 d . . .
H28A H 0.7790 0.1130 0.7965 0.105 Uiso 1 1 calc R A .
H28B H 0.7448 0.1013 0.7168 0.105 Uiso 1 1 calc R . .
H28C H 0.6762 0.0200 0.7453 0.105 Uiso 1 1 calc R . .
C29 C 0.5281(11) 0.0662(8) 0.8560(6) 0.079(3) Uani 1 1 d . A .
H29A H 0.5417 0.0010 0.8245 0.118 Uiso 1 1 calc R . .
H29B H 0.4509 0.0585 0.8804 0.118 Uiso 1 1 calc R . .
H29C H 0.6146 0.0930 0.8890 0.118 Uiso 1 1 calc R . .
C30 C 0.2218(9) 0.3339(7) 0.8034(4) 0.0607(19) Uani 1 1 d . A .
H30A H 0.2541 0.4018 0.8338 0.091 Uiso 1 1 calc R . .
H30B H 0.1550 0.3024 0.8238 0.091 Uiso 1 1 calc R . .
H30C H 0.1757 0.3369 0.7590 0.091 Uiso 1 1 calc R . .
C31 C 0.4029(11) 0.3558(7) 0.7037(5) 0.067(2) Uani 1 1 d . . .
H31A H 0.3068 0.3746 0.7058 0.101 Uiso 1 1 calc R A .
H31B H 0.4130 0.3241 0.6558 0.101 Uiso 1 1 calc R . .
H31C H 0.4695 0.4158 0.7237 0.101 Uiso 1 1 calc R . .
C32 C 0.5228(11) 0.3152(9) 0.9832(6) 0.085(3) Uani 1 1 d . A .
H32A H 0.5783 0.3784 0.9897 0.127 Uiso 1 1 calc R . .
H32B H 0.5230 0.2700 0.9369 0.127 Uiso 1 1 calc R . .
H32C H 0.5639 0.2843 1.0168 0.127 Uiso 1 1 calc R . .
C33 C 0.4788(13) 0.4785(8) 1.1052(6) 0.091(3) Uani 1 1 d . . .
H33A H 0.5231 0.4391 1.1324 0.137 Uiso 1 1 calc R A .
H33B H 0.4455 0.5378 1.1355 0.137 Uiso 1 1 calc R . .
H33C H 0.5474 0.4995 1.0805 0.137 Uiso 1 1 calc R . .
C34 C -0.0573(11) 0.3977(7) 1.0347(6) 0.077(2) Uani 1 1 d . . .
H34A H -0.1267 0.3646 0.9936 0.116 Uiso 1 1 calc R A .
H34B H -0.0632 0.4701 1.0482 0.116 Uiso 1 1 calc R . .
H34C H -0.0765 0.3729 1.0720 0.116 Uiso 1 1 calc R . .
C35 C -0.0206(9) 0.2431(6) 0.9081(4) 0.0584(18) Uani 1 1 d . A .
H35A H -0.0582 0.1881 0.9221 0.088 Uiso 1 1 calc R . .
H35B H 0.0046 0.2163 0.8625 0.088 Uiso 1 1 calc R . .
H35C H -0.0920 0.2899 0.9070 0.088 Uiso 1 1 calc R . .
C36 C 0.2927(12) 0.0833(8) 0.9934(5) 0.079(3) Uani 1 1 d . A .
H36A H 0.2327 0.1070 1.0281 0.119 Uiso 1 1 calc R . .
H36B H 0.3514 0.1402 0.9908 0.119 Uiso 1 1 calc R . .
H36C H 0.3530 0.0355 1.0058 0.119 Uiso 1 1 calc R . .
C37 C 0.1313(15) -0.1084(8) 0.9720(5) 0.091(3) Uani 1 1 d . . .
H37A H 0.0720 -0.1721 0.9562 0.137 Uiso 1 1 calc R A .
H37B H 0.0973 -0.0624 1.0109 0.137 Uiso 1 1 calc R . .
H37C H 0.2285 -0.1200 0.9861 0.137 Uiso 1 1 calc R . .
C38 C -0.0515(13) -0.1353(8) 0.7224(6) 0.089(3) Uani 1 1 d . . .
H38A H -0.1358 -0.1020 0.7140 0.133 Uiso 1 1 calc R A .
H38B H -0.0793 -0.2028 0.7229 0.133 Uiso 1 1 calc R . .
H38C H 0.0044 -0.1397 0.6860 0.133 Uiso 1 1 calc R . .
C39 C 0.1039(11) 0.0601(7) 0.7415(4) 0.069(2) Uani 1 1 d . A .
H39A H 0.0430 0.0133 0.7015 0.104 Uiso 1 1 calc R . .
H39B H 0.1983 0.0683 0.7305 0.104 Uiso 1 1 calc R . .
H39C H 0.0653 0.1250 0.7536 0.104 Uiso 1 1 calc R . .
C1 C 0.8815(13) 0.3412(11) 0.4964(6) 0.049(3) Uiso 0.609(10) 1 d PD A 1
C2 C 0.9340(17) 0.4051(13) 0.6393(8) 0.074(4) Uiso 0.609(10) 1 d PD A 1
O1 O 0.9240(15) 0.3742(12) 0.4558(7) 0.091(4) Uiso 0.609(10) 1 d PD A 1
O2 O 1.0114(19) 0.4697(13) 0.6834(8) 0.120(5) Uiso 0.609(10) 1 d PD A 1
C3 C 0.9729(16) 0.2256(13) 0.5862(9) 0.075(4) Uiso 0.609(10) 1 d PD A 1
O3 O 1.0738(15) 0.1851(12) 0.6003(9) 0.111(5) Uiso 0.609(10) 1 d PD A 1
N1 N 0.6604(11) 0.1797(8) 0.4930(4) 0.071(4) Uani 0.609(10) 1 d PG A 1
C41 C 0.6937(15) 0.0817(10) 0.4601(5) 0.109(8) Uani 0.609(10) 1 d PGD A 1
C42 C 0.585(2) 0.0050(8) 0.4240(5) 0.153(15) Uani 0.609(10) 1 d PG A 1
H42 H 0.6070 -0.0606 0.4020 0.183 Uiso 0.609(10) 1 calc PR A 1
C43 C 0.4423(18) 0.0263(11) 0.4208(6) 0.128(16) Uani 0.609(10) 1 d PG A 1
H43 H 0.3693 -0.0250 0.3967 0.153 Uiso 0.609(10) 1 calc PR A 1
C44 C 0.4089(12) 0.1244(13) 0.4538(6) 0.139(11) Uani 0.609(10) 1 d PGD A 1
C45 C 0.5180(12) 0.2011(9) 0.4899(5) 0.080(6) Uani 0.609(10) 1 d PGD A 1
N2 N 0.6120(9) 0.3699(9) 0.5552(5) 0.063(4) Uani 0.609(10) 1 d PG A 1
C46 C 0.4948(11) 0.2995(8) 0.5203(5) 0.062(4) Uani 0.609(10) 1 d PGD A 1
C47 C 0.3572(9) 0.3306(13) 0.5173(6) 0.109(9) Uani 0.609(10) 1 d PGD A 1
C48 C 0.3368(13) 0.4321(14) 0.5492(7) 0.118(11) Uani 0.609(10) 1 d PG A 1
H48 H 0.2447 0.4529 0.5472 0.142 Uiso 0.609(10) 1 calc PR A 1
C49 C 0.4540(18) 0.5025(10) 0.5841(7) 0.117(10) Uani 0.609(10) 1 d PG A 1
H49 H 0.4404 0.5704 0.6054 0.141 Uiso 0.609(10) 1 calc PR A 1
C50 C 0.5916(15) 0.4714(8) 0.5871(6) 0.090(6) Uani 0.609(10) 1 d PGD A 1
C40 C 0.841(3) 0.063(2) 0.4575(15) 0.158(14) Uani 0.609(10) 1 d PD A 1
H40A H 0.9016 0.1230 0.4858 0.237 Uiso 0.609(10) 1 calc PR A 1
H40B H 0.8572 0.0462 0.4101 0.237 Uiso 0.609(10) 1 calc PR A 1
H40C H 0.8616 0.0071 0.4748 0.237 Uiso 0.609(10) 1 calc PR A 1
C51 C 0.708(4) 0.5475(17) 0.6244(13) 0.160(17) Uani 0.609(10) 1 d PD A 1
H51A H 0.7965 0.5167 0.6235 0.239 Uiso 0.609(10) 1 calc PR A 1
H51B H 0.6937 0.5766 0.6719 0.239 Uiso 0.609(10) 1 calc PR A 1
H51C H 0.7106 0.6001 0.6028 0.239 Uiso 0.609(10) 1 calc PR A 1
C52 C 0.270(2) 0.158(3) 0.4515(10) 0.19(2) Uani 0.609(10) 1 d PD A 1
H52 H 0.1930 0.1100 0.4280 0.227 Uiso 0.609(10) 1 calc PR A 1
C53 C 0.239(2) 0.260(2) 0.4823(8) 0.13(2) Uani 0.609(10) 1 d PD A 1
H53 H 0.1462 0.2783 0.4795 0.158 Uiso 0.609(10) 1 calc PR A 1
Re1 Re 0.8123(3) 0.2979(2) 0.56867(16) 0.0549(4) Uani 0.609(10) 1 d PD A 1
Re1' Re 0.7990(6) 0.2790(6) 0.5584(4) 0.0853(16) Uani 0.389(10) 1 d PD A 2
O1' O 0.902(2) 0.3193(18) 0.4309(9) 0.084(5) Uiso 0.389(10) 1 d PD A 2
O2' O 1.052(2) 0.419(2) 0.6624(13) 0.118(8) Uiso 0.389(10) 1 d PD A 2
C2' C 0.956(2) 0.364(2) 0.6233(14) 0.080(7) Uiso 0.389(10) 1 d PD A 2
C1' C 0.857(3) 0.294(2) 0.4749(12) 0.077(7) Uiso 0.389(10) 1 d PD A 2
C3' C 0.924(2) 0.1738(15) 0.5541(12) 0.063(5) Uiso 0.389(10) 1 d PD A 2
O3' O 1.011(2) 0.1217(17) 0.5667(14) 0.110(7) Uiso 0.389(10) 1 d PD A 2
N1' N 0.6068(18) 0.1936(14) 0.4912(8) 0.074(8) Uiso 0.389(10) 1 d PG A 2
C41' C 0.595(2) 0.0911(15) 0.4516(10) 0.081(8) Uiso 0.389(10) 1 d PGD A 2
C42' C 0.461(3) 0.0389(11) 0.4216(9) 0.118(19) Uiso 0.389(10) 1 d PG A 2
H42' H 0.4531 -0.0297 0.3952 0.142 Uiso 0.389(10) 1 calc PR A 2
C43' C 0.338(2) 0.0893(15) 0.4312(10) 0.113(14) Uiso 0.389(10) 1 d PG A 2
H43' H 0.2482 0.0543 0.4111 0.136 Uiso 0.389(10) 1 calc PR A 2
C44' C 0.3496(19) 0.1918(15) 0.4707(10) 0.075(7) Uiso 0.389(10) 1 d PGD A 2
C45' C 0.484(2) 0.2440(11) 0.5007(8) 0.082(12) Uiso 0.389(10) 1 d PGD A 2
N2' N 0.6386(15) 0.3963(12) 0.5666(9) 0.048(5) Uiso 0.389(10) 1 d PG A 2
C46' C 0.5027(18) 0.3470(9) 0.5363(7) 0.044(5) Uiso 0.389(10) 1 d PGD A 2
C47' C 0.3830(14) 0.4015(12) 0.5428(9) 0.068(7) Uiso 0.389(10) 1 d PGD A 2
C48' C 0.3991(17) 0.5053(12) 0.5795(10) 0.071(7) Uiso 0.389(10) 1 d PG A 2
H48' H 0.3190 0.5418 0.5838 0.085 Uiso 0.389(10) 1 calc PR A 2
C49' C 0.535(2) 0.5546(9) 0.6098(11) 0.078(7) Uiso 0.389(10) 1 d PG A 2
H49' H 0.5458 0.6241 0.6344 0.094 Uiso 0.389(10) 1 calc PR A 2
C50' C 0.6547(15) 0.5001(12) 0.6033(12) 0.085(11) Uiso 0.389(10) 1 d PGD A 2
C40' C 0.721(4) 0.046(3) 0.432(2) 0.107(11) Uiso 0.389(10) 1 d PD A 2
H40D H 0.8036 0.0925 0.4563 0.161 Uiso 0.389(10) 1 calc PR A 2
H40E H 0.7171 0.0327 0.3822 0.161 Uiso 0.389(10) 1 calc PR A 2
H40F H 0.7259 -0.0163 0.4424 0.161 Uiso 0.389(10) 1 calc PR A 2
C51' C 0.795(3) 0.552(4) 0.618(3) 0.121(15) Uiso 0.389(10) 1 d PD A 2
H51D H 0.8642 0.5027 0.6099 0.181 Uiso 0.389(10) 1 calc PR A 2
H51E H 0.8146 0.5943 0.6661 0.181 Uiso 0.389(10) 1 calc PR A 2
H51F H 0.8010 0.5935 0.5884 0.181 Uiso 0.389(10) 1 calc PR A 2
C52' C 0.229(3) 0.244(2) 0.4762(14) 0.098(16) Uiso 0.389(10) 1 d PD A 2
H52' H 0.1379 0.2106 0.4566 0.117 Uiso 0.389(10) 1 calc PR A 2
C53' C 0.250(3) 0.346(2) 0.5120(11) 0.093(10) Uiso 0.389(10) 1 d PD A 2
H53' H 0.1695 0.3822 0.5160 0.112 Uiso 0.389(10) 1 calc PR A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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
C5 C4 Re1 172.3(7) . . ?
C5 C4 Re1' 170.5(7) . . ?
Re1 C4 Re1' 7.8(3) . . ?
C4 C5 C6 175.9(9) . . ?
C7 C6 C11 119.9(6) . . ?
C7 C6 C5 121.0(7) . . ?
C11 C6 C5 119.1(7) . . ?
C8 C7 C6 119.9(7) . . ?
C8 C7 C28 121.0(7) . . ?
C6 C7 C28 119.1(7) . . ?
C7 C8 C9 121.6(7) . . ?
C7 C8 C29 119.4(8) . . ?
C9 C8 C29 118.7(8) . . ?
C8 C9 C10 118.2(7) . . ?
C8 C9 B1 121.6(6) . . ?
C10 C9 B1 120.0(7) . . ?
C11 C10 C9 119.8(7) . . ?
C11 C10 C30 119.4(6) . . ?
C9 C10 C30 120.7(7) . . ?
C10 C11 C6 120.4(6) . . ?
C10 C11 C31 120.8(7) . . ?
C6 C11 C31 118.7(7) . . ?
C9 B1 C20 120.9(7) . . ?
C9 B1 C12 120.1(6) . . ?
C20 B1 C12 119.0(6) . . ?
C13 C12 C17 119.4(8) . . ?
C13 C12 B1 120.2(7) . . ?
C17 C12 B1 120.3(7) . . ?
C14 C13 C12 120.8(8) . . ?
C14 C13 C32 116.9(8) . . ?
C12 C13 C32 122.3(8) . . ?
C13 C14 C15 118.8(7) . . ?
C13 C14 C33 122.3(9) . . ?
C15 C14 C33 118.8(9) . . ?
C16 C15 C14 121.1(8) . . ?
C16 C15 C18 120.5(9) . . ?
C14 C15 C18 118.4(8) . . ?
C15 C16 C17 118.8(8) . . ?
C15 C16 C34 119.6(8) . . ?
C17 C16 C34 121.6(8) . . ?
C16 C17 C12 120.9(7) . . ?
C16 C17 C35 117.4(8) . . ?
C12 C17 C35 121.5(7) . . ?
C19 C18 C15 178.7(13) . . ?
C18 C19 H19 180.0 . . ?
C25 C20 C21 118.8(7) . . ?
C25 C20 B1 120.6(6) . . ?
C21 C20 B1 120.5(7) . . ?
C22 C21 C20 120.1(7) . . ?
C22 C21 C36 118.0(7) . . ?
C20 C21 C36 121.9(7) . . ?
C23 C22 C21 119.4(7) . . ?
C23 C22 C37 120.0(8) . . ?
C21 C22 C37 120.6(8) . . ?
C22 C23 C24 122.1(8) . . ?
C22 C23 C26 119.1(9) . . ?
C24 C23 C26 118.9(9) . . ?
C25 C24 C23 118.3(8) . . ?
C25 C24 C38 122.2(8) . . ?
C23 C24 C38 119.5(8) . . ?
C24 C25 C20 121.3(7) . . ?
C24 C25 C39 118.1(7) . . ?
C20 C25 C39 120.5(7) . . ?
C27 C26 C23 178(2) . . ?
C26 C27 H27 180.0 . . ?
C7 C28 H28A 109.5 . . ?
C7 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C7 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C8 C29 H29A 109.5 . . ?
C8 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C8 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C10 C30 H30A 109.5 . . ?
C10 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C10 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C11 C31 H31A 109.5 . . ?
C11 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C11 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C13 C32 H32A 109.5 . . ?
C13 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C13 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C14 C33 H33A 109.5 . . ?
C14 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C14 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C16 C34 H34A 109.5 . . ?
C16 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C16 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C17 C35 H35A 109.5 . . ?
C17 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C17 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C21 C36 H36A 109.5 . . ?
C21 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C21 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C22 C37 H37A 109.5 . . ?
C22 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C22 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C24 C38 H38A 109.5 . . ?
C24 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C24 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C25 C39 H39A 109.5 . . ?
C25 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C25 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O1 C1 Re1 175.3(14) . . ?
O2 C2 Re1 178.4(18) . . ?
O3 C3 Re1 176.4(18) . . ?
C41 N1 C45 120.0 . . ?
C41 N1 Re1 123.9(6) . . ?
C45 N1 Re1 114.8(6) . . ?
N1 C41 C42 120.0 . . ?
N1 C41 C40 119.5(13) . . ?
C42 C41 C40 120.2(13) . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C44 C43 C42 120.0 . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 120.0 . . ?
C43 C44 C52 126.0(16) . . ?
C45 C44 C52 113.9(16) . . ?
C46 C45 C44 123.6(9) . . ?
C46 C45 N1 116.3(9) . . ?
C44 C45 N1 120.0 . . ?
C46 N2 C50 120.0 . . ?
C46 N2 Re1 113.0(6) . . ?
C50 N2 Re1 126.2(6) . . ?
C45 C46 N2 118.7(9) . . ?
C45 C46 C47 121.3(9) . . ?
N2 C46 C47 120.0 . . ?
C46 C47 C48 120.0 . . ?
C46 C47 C53 120.0(15) . . ?
C48 C47 C53 120.0(15) . . ?
C47 C48 C49 120.0 . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C50 C49 C48 120.0 . . ?
C50 C49 H49 120.0 . . ?
C48 C49 H49 120.0 . . ?
C49 C50 N2 120.0 . . ?
C49 C50 C51 117.2(15) . . ?
N2 C50 C51 122.7(15) . . ?
C41 C40 H40A 109.5 . . ?
C41 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C41 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C53 C52 C44 125(3) . . ?
C53 C52 H52 117.5 . . ?
C44 C52 H52 117.5 . . ?
C47 C53 C52 116(2) . . ?
C47 C53 H53 121.9 . . ?
C52 C53 H53 121.9 . . ?
C3 Re1 C2 79.9(8) . . ?
C3 Re1 C1 95.8(6) . . ?
C2 Re1 C1 90.8(7) . . ?
C3 Re1 C4 91.3(6) . . ?
C2 Re1 C4 93.3(6) . . ?
C1 Re1 C4 172.3(4) . . ?
C3 Re1 N1 103.1(7) . . ?
C2 Re1 N1 175.5(7) . . ?
C1 Re1 N1 92.3(5) . . ?
C4 Re1 N1 83.3(3) . . ?
C3 Re1 N2 172.6(6) . . ?
C2 Re1 N2 102.4(7) . . ?
C1 Re1 N2 91.2(4) . . ?
C4 Re1 N2 81.5(3) . . ?
N1 Re1 N2 74.2(5) . . ?
C3' Re1' C2' 83.8(12) . . ?
C3' Re1' C1' 88.9(11) . . ?
C2' Re1' C1' 97.0(13) . . ?
C3' Re1' C4 93.3(7) . . ?
C2' Re1' C4 90.5(10) . . ?
C1' Re1' C4 172.3(10) . . ?
C3' Re1' N1' 101.4(9) . . ?
C2' Re1' N1' 174.0(11) . . ?
C1' Re1' N1' 86.1(10) . . ?
C4 Re1' N1' 86.2(5) . . ?
C3' Re1' N2' 175.5(9) . . ?
C2' Re1' N2' 98.3(11) . . ?
C1' Re1' N2' 94.8(10) . . ?
C4 Re1' N2' 82.7(5) . . ?
N1' Re1' N2' 76.2(7) . . ?
O2' C2' Re1' 178(3) . . ?
O1' C1' Re1' 169(3) . . ?
O3' C3' Re1' 165(2) . . ?
C41' N1' C45' 120.0 . . ?
C41' N1' Re1' 125.2(10) . . ?
C45' N1' Re1' 113.7(10) . . ?
C42' C41' N1' 120.0 . . ?
C42' C41' C40' 120(2) . . ?
N1' C41' C40' 119(2) . . ?
C41' C42' C43' 120.0 . . ?
C41' C42' H42' 120.0 . . ?
C43' C42' H42' 120.0 . . ?
C44' C43' C42' 120.0 . . ?
C44' C43' H43' 120.0 . . ?
C42' C43' H43' 120.0 . . ?
C52' C44' C43' 120(2) . . ?
C52' C44' C45' 120(2) . . ?
C43' C44' C45' 120.0 . . ?
C46' C45' C44' 122.6(15) . . ?
C46' C45' N1' 117.3(15) . . ?
C44' C45' N1' 120.0 . . ?
C46' N2' C50' 120.0 . . ?
C46' N2' Re1' 109.2(9) . . ?
C50' N2' Re1' 130.2(9) . . ?
C45' C46' N2' 121.0(14) . . ?
C45' C46' C47' 119.0(14) . . ?
N2' C46' C47' 120.0 . . ?
C48' C47' C46' 120.0 . . ?
C48' C47' C53' 123.4(18) . . ?
C46' C47' C53' 116.6(18) . . ?
C47' C48' C49' 120.0 . . ?
C47' C48' H48' 120.0 . . ?
C49' C48' H48' 120.0 . . ?
C48' C49' C50' 120.0 . . ?
C48' C49' H49' 120.0 . . ?
C50' C49' H49' 120.0 . . ?
C49' C50' N2' 120.0 . . ?
C49' C50' C51' 121(2) . . ?
N2' C50' C51' 118(2) . . ?
C41' C40' H40D 109.5 . . ?
C41' C40' H40E 109.5 . . ?
H40D C40' H40E 109.5 . . ?
C41' C40' H40F 109.5 . . ?
H40D C40' H40F 109.5 . . ?
H40E C40' H40F 109.5 . . ?
C50' C51' H51D 109.5 . . ?
C50' C51' H51E 109.5 . . ?
H51D C51' H51E 109.5 . . ?
C50' C51' H51F 109.5 . . ?
H51D C51' H51F 109.5 . . ?
H51E C51' H51F 109.5 . . ?
C44' C52' C53' 117(3) . . ?
C44' C52' H52' 121.7 . . ?
C53' C52' H52' 121.7 . . ?
C52' C53' C47' 125(3) . . ?
C52' C53' H53' 117.3 . . ?
C47' C53' H53' 117.3 . . ?
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
C4 C5 1.187(11) . ?
C4 Re1 2.142(8) . ?
C4 Re1' 2.147(9) . ?
C5 C6 1.439(10) . ?
C6 C7 1.402(10) . ?
C6 C11 1.416(11) . ?
C7 C8 1.384(11) . ?
C7 C28 1.511(11) . ?
C8 C9 1.424(11) . ?
C8 C29 1.531(11) . ?
C9 C10 1.426(10) . ?
C9 B1 1.562(11) . ?
C10 C11 1.404(10) . ?
C10 C30 1.493(11) . ?
C11 C31 1.510(10) . ?
B1 C20 1.593(11) . ?
B1 C12 1.613(12) . ?
C12 C13 1.398(11) . ?
C12 C17 1.411(12) . ?
C13 C14 1.387(13) . ?
C13 C32 1.525(14) . ?
C14 C15 1.428(14) . ?
C14 C33 1.538(12) . ?
C15 C16 1.391(12) . ?
C15 C18 1.443(13) . ?
C16 C17 1.398(12) . ?
C16 C34 1.496(13) . ?
C17 C35 1.512(11) . ?
C18 C19 1.124(17) . ?
C19 H19 0.9300 . ?
C20 C25 1.409(11) . ?
C20 C21 1.424(10) . ?
C21 C22 1.396(12) . ?
C21 C36 1.505(12) . ?
C22 C23 1.382(13) . ?
C22 C37 1.513(11) . ?
C23 C24 1.413(12) . ?
C23 C26 1.472(13) . ?
C24 C25 1.384(11) . ?
C24 C38 1.511(13) . ?
C25 C39 1.514(10) . ?
C26 C27 1.102(17) . ?
C27 H27 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C1 O1 1.167(12) . ?
C1 Re1 1.932(10) . ?
C2 O2 1.183(14) . ?
C2 Re1 1.911(12) . ?
C3 O3 1.175(13) . ?
C3 Re1 1.909(11) . ?
N1 C41 1.3900 . ?
N1 C45 1.3900 . ?
N1 Re1 2.172(9) . ?
C41 C42 1.3900 . ?
C41 C40 1.43(2) . ?
C42 C43 1.3900 . ?
C42 H42 0.9300 . ?
C43 C44 1.3900 . ?
C43 H43 0.9300 . ?
C44 C45 1.3900 . ?
C44 C52 1.415(17) . ?
C45 C46 1.354(15) . ?
N2 C46 1.3900 . ?
N2 C50 1.3900 . ?
N2 Re1 2.203(8) . ?
C46 C47 1.3900 . ?
C47 C48 1.3900 . ?
C47 C53 1.397(17) . ?
C48 C49 1.3900 . ?
C48 H48 0.9300 . ?
C49 C50 1.3900 . ?
C49 H49 0.9300 . ?
C50 C51 1.43(2) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 C53 1.413(19) . ?
C52 H52 0.9300 . ?
C53 H53 0.9300 . ?
Re1' C3' 1.911(13) . ?
Re1' C2' 1.917(13) . ?
Re1' C1' 1.924(13) . ?
Re1' N1' 2.162(18) . ?
Re1' N2' 2.259(14) . ?
O1' C1' 1.181(15) . ?
O2' C2' 1.175(15) . ?
C3' O3' 1.171(15) . ?
N1' C41' 1.3900 . ?
N1' C45' 1.3900 . ?
C41' C42' 1.3900 . ?
C41' C40' 1.42(2) . ?
C42' C43' 1.3900 . ?
C42' H42' 0.9300 . ?
C43' C44' 1.3900 . ?
C43' H43' 0.9300 . ?
C44' C52' 1.375(19) . ?
C44' C45' 1.3900 . ?
C45' C46' 1.375(18) . ?
N2' C46' 1.3900 . ?
N2' C50' 1.3900 . ?
C46' C47' 1.3900 . ?
C47' C48' 1.3900 . ?
C47' C53' 1.393(19) . ?
C48' C49' 1.3900 . ?
C48' H48' 0.9300 . ?
C49' C50' 1.3900 . ?
C49' H49' 0.9300 . ?
C50' C51' 1.42(2) . ?
C40' H40D 0.9600 . ?
C40' H40E 0.9600 . ?
C40' H40F 0.9600 . ?
C51' H51D 0.9600 . ?
C51' H51E 0.9600 . ?
C51' H51F 0.9600 . ?
C52' C53' 1.38(2) . ?
C52' H52' 0.9300 . ?
C53' H53' 0.9300 . ?
