data_global
_journal_coden_Cambridge 222
loop_
_publ_author_name
'Alberding, Brian'
'Chisholm, Malcolm'
'Gallucci, Judith'
'Reed, Carly'
'Turro, Claudia'
_publ_contact_author_name 'Chisholm, Malcolm'
_publ_contact_author_email chisholm@chemistry.ohio-state.edu
_publ_section_title
;
Concerning the Photophysical Properties of Re24+
and Re26+ Carboxylate Compounds.
;
_publ_requested_category FM
# Attachment '- crystalstructure.cif'
#\#CIF_1.1
# CIF produced by WinGX routine CIF_UPDATE
# Created on 2010-07-23 at 14:55:26
# Using CIFtbx version 2.6.2 16 Jun 1998
# Dictionary name : cif_core.dic
# Dictionary vers : 2.4
# Request file : c:\wingx\files\archive.reqdat
# CIF files read : shelxl scrals struct
#------------------ SECTION 1. GLOBAL INFORMATION ---------------------------#
data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 787576'
#TrackingRef '- crystalstructure.cif'
_audit_creation_date 2010-07-23T14:55:26-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.4
_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_name_common 'Chisholm 1708'
_chemical_formula_moiety 'C64 H52 Cl2 N2 O8 P4 Re2, 2(C4 H8 O)'
_chemical_formula_sum 'C72 H68 Cl2 N2 O10 P4 Re2'
_chemical_formula_weight 1688.46
_chemical_compound_source 'synthesis as described'
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M C2/c
_symmetry_space_group_name_Hall '-C 2yc'
_symmetry_Int_Tables_number 15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'
_cell_length_a 31.062(7)
_cell_length_b 10.454(3)
_cell_length_c 24.183(6)
_cell_angle_alpha 90
_cell_angle_beta 124.225(3)
_cell_angle_gamma 90
_cell_volume 6493(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 150(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_cell_measurement_wavelength 0.77490
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description blade
_exptl_crystal_colour orange-brown
_exptl_crystal_size_max 0.08
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.01
_exptl_crystal_density_diffrn 1.727
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3352
_exptl_special_details
;Intensity data were collected
at 150K on a D8 goniostat equipped with a Bruker APEXII CCD
detector at Beamline 11.3.1 at the Advanced Light Source
(Lawrence Berkeley National Laboratory) using synchrotron
radiation tuned to ?=0.7749 (1). A series of 7 second data
frames measured with a frame width of 0.2 degrees in omega were collected
to calculate a unit cell. For data collection, frames were measured
with a frame width of 0.3 degrees in omega and an exposure time of 7 seconds
per frame out to a maximum 2 theta value of about 58 degrees.
The data frames were collected using the program APEX2 and integrated
using the program SAINT within APEX2. The data were corrected for
absorption and beam corrections based on the multi-scan technique as
implemented in SADABS.
The rhenium complex contains a crystallographic two-fold rotation axis.
The asymmetric unit consists of half of the Re complex and one solvent
molecule of THF.
Crystallographic data were collected through the SCrALS program
(Service Crystallography at Advanced Light Source) at the Small-Crystal
Crystallography Beamline 11.3.1 (developed by the Experimental Systems
Group) at the Advanced Light Source (ALS). The ALS is supported by the
U.S. Department of Energy, Office of Energy Sciences Materials Sciences
Division, under contract DE-AC02-05CH11231 at Lawrence Berkeley National
Laboratory. We thank Dr. Jeanette Krause of the University of
Cincinnati for the data collection.
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 4.769
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.546
_exptl_absorpt_correction_T_max 0.746
_exptl_absorpt_process_details SADABS-2008/1
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_ambient_temperature 150(2)
_diffrn_radiation_wavelength 0.7749
_diffrn_radiation_type synchrotron
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_measurement_device_type 'Bruker APEXII'
_diffrn_measurement_method 'omega scans'
_diffrn_reflns_av_R_equivalents 0.1314
_diffrn_reflns_av_unetI/netI 0.0966
_diffrn_reflns_number 34819
_diffrn_reflns_limit_h_min -38
_diffrn_reflns_limit_h_max 38
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 3.97
_diffrn_reflns_theta_max 29.12
_diffrn_reflns_theta_full 29.12
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total 6692
_reflns_number_gt 4112
_reflns_threshold_expression >2\s(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection 'Bruker APEX2 v2008.5.0'
_computing_cell_refinement 'Bruker SAINT v7.56A'
_computing_data_reduction 'Bruker SAINT v7.56A'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material 'WinGX publication routines (Farrugia, 1999)'
#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_refine_special_details
;The hydrogen atoms were included in the model at calculated
positions using a riding model with U(H) = 1.2 * Ueq(attached atom).
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_number_reflns 6692
_refine_ls_number_parameters 415
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.104
_refine_ls_R_factor_gt 0.05
_refine_ls_wR_factor_ref 0.1197
_refine_ls_wR_factor_gt 0.1002
_refine_ls_goodness_of_fit_ref 0.971
_refine_ls_restrained_S_all 0.971
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0
_refine_diff_density_max 1.512
_refine_diff_density_min -2.242
_refine_diff_density_rms 0.167
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.004 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1704 0.1889 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0076 0.004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0133 0.0073 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1184 0.1127 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.4581 8.3324 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C1 C 0.9305(4) 0.9530(8) 0.2115(4) 0.029(2) Uani 1 1 d . . .
C2 C 0.8909(4) 1.0557(9) 0.1906(5) 0.035(2) Uani 1 1 d . . .
C3 C 0.8694(4) 1.0712(9) 0.2278(5) 0.037(2) Uani 1 1 d . . .
H3 H 0.8827 1.0235 0.2677 0.045 Uiso 1 1 calc R . .
C4 C 0.8279(4) 1.1573(9) 0.2061(5) 0.044(2) Uani 1 1 d . . .
H4 H 0.8144 1.1732 0.2322 0.053 Uiso 1 1 calc R . .
C5 C 0.8077(4) 1.2179(8) 0.1456(5) 0.037(2) Uani 1 1 d . . .
C6 C 0.8278(4) 1.2024(9) 0.1074(5) 0.041(2) Uani 1 1 d . . .
H6 H 0.8134 1.247 0.0664 0.049 Uiso 1 1 calc R . .
C7 C 0.8702(4) 1.1184(8) 0.1313(4) 0.032(2) Uani 1 1 d . . .
H7 H 0.8846 1.1053 0.1059 0.039 Uiso 1 1 calc R . .
C8 C 1.0784(4) 0.5115(8) 0.2992(4) 0.030(2) Uani 1 1 d . . .
H8A H 1.0568 0.4402 0.2977 0.037 Uiso 1 1 calc R . .
H8B H 1.1133 0.4771 0.3154 0.037 Uiso 1 1 calc R . .
C9 C 1.1053(3) 0.6053(8) 0.2102(4) 0.0277(18) Uani 1 1 d . . .
C10 C 1.1364(4) 0.5006(10) 0.2203(5) 0.041(2) Uani 1 1 d . . .
H10 H 1.1252 0.4164 0.2208 0.049 Uiso 1 1 calc R . .
C11 C 1.1849(4) 0.5208(11) 0.2296(5) 0.046(3) Uani 1 1 d . . .
H11 H 1.2073 0.4505 0.2386 0.055 Uiso 1 1 calc R . .
C12 C 1.1996(4) 0.6418(11) 0.2258(5) 0.045(3) Uani 1 1 d . . .
H12 H 1.2326 0.6553 0.2328 0.054 Uiso 1 1 calc R . .
C13 C 1.1673(4) 0.7439(12) 0.2119(5) 0.048(2) Uani 1 1 d . . .
H13 H 1.1775 0.8271 0.2077 0.058 Uiso 1 1 calc R . .
C14 C 1.1196(4) 0.7265(9) 0.2038(4) 0.038(2) Uani 1 1 d . . .
H14 H 1.0972 0.7972 0.194 0.046 Uiso 1 1 calc R . .
C15 C 1.0213(3) 0.4371(8) 0.1610(4) 0.0293(19) Uani 1 1 d . . .
C16 C 1.0179(4) 0.3158(9) 0.1823(5) 0.034(2) Uani 1 1 d . . .
H16 H 1.0288 0.3044 0.2274 0.041 Uiso 1 1 calc R . .
C17 C 0.9991(4) 0.2108(8) 0.1393(5) 0.037(2) Uani 1 1 d . . .
H17 H 0.9969 0.1293 0.155 0.044 Uiso 1 1 calc R . .
C18 C 0.9837(4) 0.2257(10) 0.0737(5) 0.046(3) Uani 1 1 d . . .
H18 H 0.9708 0.1546 0.0442 0.055 Uiso 1 1 calc R . .
C19 C 0.9871(4) 0.3464(9) 0.0512(5) 0.042(2) Uani 1 1 d . . .
H19 H 0.9768 0.3571 0.0063 0.05 Uiso 1 1 calc R . .
C20 C 1.0052(4) 0.4487(9) 0.0938(5) 0.040(2) Uani 1 1 d . . .
H20 H 1.007 0.53 0.0777 0.048 Uiso 1 1 calc R . .
C21 C 1.1063(3) 0.5414(8) 0.4328(4) 0.030(2) Uani 1 1 d . . .
C22 C 1.1159(4) 0.6038(9) 0.4906(5) 0.040(2) Uani 1 1 d . . .
H22 H 1.1085 0.6924 0.4889 0.048 Uiso 1 1 calc R . .
C23 C 1.1361(4) 0.5370(9) 0.5493(5) 0.048(3) Uani 1 1 d . . .
H23 H 1.1416 0.5791 0.5876 0.057 Uiso 1 1 calc R . .
C24 C 1.1482(4) 0.4090(10) 0.5526(5) 0.045(3) Uani 1 1 d . . .
H24 H 1.1631 0.3638 0.5936 0.055 Uiso 1 1 calc R . .
C25 C 1.1390(5) 0.3475(10) 0.4976(5) 0.050(3) Uani 1 1 d . . .
H25 H 1.1472 0.2592 0.4999 0.06 Uiso 1 1 calc R . .
C26 C 1.1175(4) 0.4141(9) 0.4374(5) 0.038(2) Uani 1 1 d . . .
H26 H 1.1106 0.3698 0.3989 0.046 Uiso 1 1 calc R . .
C27 C 1.1447(3) 0.7235(8) 0.3868(4) 0.030(2) Uani 1 1 d . . .
C28 C 1.1796(4) 0.6982(9) 0.3706(5) 0.035(2) Uani 1 1 d . . .
H28 H 1.1732 0.6287 0.3416 0.042 Uiso 1 1 calc R . .
C29 C 1.2239(4) 0.7719(10) 0.3955(5) 0.046(2) Uani 1 1 d . . .
H29 H 1.247 0.7546 0.3824 0.055 Uiso 1 1 calc R . .
C30 C 1.2345(4) 0.8708(10) 0.4394(5) 0.044(3) Uani 1 1 d . . .
H30 H 1.2646 0.9221 0.4563 0.053 Uiso 1 1 calc R . .
C31 C 1.2009(4) 0.8949(9) 0.4588(5) 0.044(3) Uani 1 1 d . . .
H31 H 1.2091 0.9596 0.4909 0.053 Uiso 1 1 calc R . .
C32 C 1.1554(4) 0.8249(8) 0.4316(4) 0.037(2) Uani 1 1 d . . .
H32 H 1.1315 0.845 0.443 0.044 Uiso 1 1 calc R . .
Cl Cl 1.01397(10) 0.8086(2) 0.40936(11) 0.0396(5) Uani 1 1 d . . .
N N 0.7629(3) 1.3023(8) 0.1207(5) 0.045(2) Uani 1 1 d . . .
O1 O 0.9454(3) 0.8944(6) 0.2642(3) 0.0332(15) Uani 1 1 d . . .
O2 O 0.9485(2) 0.9308(5) 0.1754(3) 0.0300(13) Uani 1 1 d . . .
O3 O 0.7422(3) 1.3072(7) 0.1510(4) 0.0496(18) Uani 1 1 d . . .
O4 O 0.7468(4) 1.3586(9) 0.0686(4) 0.075(3) Uani 1 1 d . . .
P1 P 1.04810(10) 0.5791(2) 0.21386(11) 0.0265(5) Uani 1 1 d . . .
P2 P 1.08451(9) 0.6343(2) 0.35683(11) 0.0266(5) Uani 1 1 d . . .
Re Re 1.006264(13) 0.75793(3) 0.302046(15) 0.02411(11) Uani 1 1 d . . .
O5 O 1.1593(3) -0.1538(8) 0.6482(4) 0.066(2) Uani 1 1 d . . .
C33 C 1.1037(4) -0.1668(11) 0.6102(6) 0.053(3) Uani 1 1 d . . .
H33A H 1.0921 -0.1875 0.6398 0.064 Uiso 1 1 calc R . .
H33B H 1.0918 -0.2352 0.5762 0.064 Uiso 1 1 calc R . .
C34 C 1.0830(4) -0.0386(10) 0.5772(5) 0.046(3) Uani 1 1 d . . .
H34A H 1.0485 -0.0474 0.5343 0.055 Uiso 1 1 calc R . .
H34B H 1.0798 0.0206 0.6067 0.055 Uiso 1 1 calc R . .
C35 C 1.1234(4) 0.0071(10) 0.5661(5) 0.048(3) Uani 1 1 d . . .
H35A H 1.1326 0.0976 0.5798 0.058 Uiso 1 1 calc R . .
H35B H 1.1108 -0.0012 0.5185 0.058 Uiso 1 1 calc R . .
C36 C 1.1696(4) -0.0797(11) 0.6097(6) 0.057(3) Uani 1 1 d . . .
H36A H 1.1756 -0.1351 0.5814 0.068 Uiso 1 1 calc R . .
H36B H 1.2013 -0.0279 0.6389 0.068 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.035(5) 0.022(4) 0.026(5) 0.003(4) 0.015(4) 0.008(4)
C2 0.043(6) 0.035(5) 0.034(5) 0.002(4) 0.026(5) 0.001(4)
C3 0.052(6) 0.038(5) 0.031(5) 0.002(4) 0.029(5) 0.007(5)
C4 0.050(7) 0.044(6) 0.045(6) 0.008(5) 0.030(5) 0.006(5)
C5 0.037(5) 0.036(5) 0.035(5) 0.002(4) 0.019(4) 0.003(4)
C6 0.050(6) 0.037(5) 0.045(6) 0.009(4) 0.032(5) 0.000(4)
C7 0.049(6) 0.028(5) 0.035(5) -0.003(4) 0.033(5) -0.002(4)
C8 0.037(6) 0.025(4) 0.032(5) -0.001(4) 0.022(5) -0.003(4)
C9 0.033(5) 0.032(5) 0.025(4) -0.002(4) 0.020(4) 0.000(4)
C10 0.035(6) 0.059(6) 0.036(5) 0.007(5) 0.025(5) 0.005(5)
C11 0.043(6) 0.067(7) 0.035(6) 0.009(5) 0.027(5) 0.021(5)
C12 0.033(6) 0.075(8) 0.037(6) 0.003(5) 0.025(5) -0.002(5)
C13 0.054(6) 0.059(6) 0.044(5) -0.002(6) 0.035(5) -0.011(7)
C14 0.039(5) 0.050(6) 0.031(5) -0.003(4) 0.022(4) -0.004(4)
C15 0.033(5) 0.034(5) 0.026(5) -0.009(4) 0.019(4) -0.002(4)
C16 0.034(5) 0.038(5) 0.036(5) -0.002(4) 0.023(5) 0.001(4)
C17 0.041(6) 0.028(5) 0.043(6) -0.004(4) 0.025(5) 0.000(4)
C18 0.049(6) 0.048(7) 0.048(6) -0.018(5) 0.032(5) 0.001(5)
C19 0.055(7) 0.044(6) 0.042(6) -0.010(5) 0.036(5) -0.003(5)
C20 0.056(7) 0.041(5) 0.039(6) -0.003(4) 0.037(5) 0.000(5)
C21 0.029(5) 0.036(5) 0.028(5) 0.011(4) 0.017(4) 0.005(4)
C22 0.052(6) 0.040(5) 0.032(5) 0.008(4) 0.026(5) 0.012(5)
C23 0.073(8) 0.044(6) 0.024(5) 0.009(4) 0.026(6) 0.012(5)
C24 0.061(7) 0.046(6) 0.028(5) 0.016(4) 0.024(5) 0.008(5)
C25 0.080(8) 0.037(5) 0.043(6) 0.018(5) 0.041(6) 0.016(5)
C26 0.045(6) 0.046(6) 0.025(5) 0.004(4) 0.020(5) 0.005(5)
C27 0.028(4) 0.036(5) 0.018(4) 0.002(3) 0.008(3) -0.003(4)
C28 0.034(5) 0.040(5) 0.032(5) 0.003(4) 0.019(4) 0.007(4)
C29 0.041(5) 0.062(7) 0.041(5) 0.003(5) 0.026(5) 0.000(5)
C30 0.034(6) 0.040(6) 0.039(6) 0.005(4) 0.009(5) -0.006(4)
C31 0.048(6) 0.040(6) 0.028(5) -0.003(4) 0.011(5) -0.004(5)
C32 0.045(6) 0.032(5) 0.027(5) -0.001(4) 0.017(5) 0.004(4)
Cl 0.0497(15) 0.0438(12) 0.0287(12) -0.0041(10) 0.0242(11) 0.0088(11)
N 0.053(6) 0.042(5) 0.055(6) 0.009(4) 0.040(5) 0.008(4)
O1 0.045(4) 0.032(3) 0.033(4) -0.007(3) 0.028(3) 0.002(3)
O2 0.034(4) 0.026(3) 0.029(3) -0.002(3) 0.017(3) -0.002(3)
O3 0.045(4) 0.053(4) 0.055(5) 0.006(4) 0.031(4) 0.011(3)
O4 0.092(7) 0.088(6) 0.072(6) 0.044(5) 0.061(6) 0.042(5)
P1 0.0348(13) 0.0286(11) 0.0237(12) -0.0017(9) 0.0211(11) -0.0006(10)
P2 0.0354(13) 0.0257(11) 0.0219(11) 0.0000(9) 0.0181(10) 0.0011(9)
Re 0.03145(17) 0.02450(17) 0.02093(15) -0.00027(19) 0.01750(13) 0.0010(2)
O5 0.056(5) 0.097(6) 0.052(5) 0.027(5) 0.035(4) 0.011(5)
C33 0.044(7) 0.070(8) 0.053(7) 0.002(6) 0.031(6) -0.001(6)
C34 0.049(7) 0.056(6) 0.040(6) 0.003(5) 0.030(5) 0.009(5)
C35 0.047(7) 0.052(6) 0.041(6) 0.001(5) 0.022(5) 0.000(5)
C36 0.051(7) 0.062(7) 0.064(8) 0.016(6) 0.037(6) -0.003(6)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_geom_special_details
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.245(10) . ?
C1 O2 1.296(10) . ?
C1 C2 1.492(12) . ?
C2 C7 1.365(12) . ?
C2 C3 1.398(12) . ?
C3 C4 1.409(13) . ?
C3 H3 0.95 . ?
C4 C5 1.380(13) . ?
C4 H4 0.95 . ?
C5 C6 1.384(13) . ?
C5 N 1.462(12) . ?
C6 C7 1.409(13) . ?
C6 H6 0.95 . ?
C7 H7 0.95 . ?
C8 P2 1.824(9) . ?
C8 P1 1.860(9) . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C9 C14 1.380(12) . ?
C9 C10 1.389(12) . ?
C9 P1 1.848(9) . ?
C10 C11 1.406(14) . ?
C10 H10 0.95 . ?
C11 C12 1.366(15) . ?
C11 H11 0.95 . ?
C12 C13 1.372(15) . ?
C12 H12 0.95 . ?
C13 C14 1.393(13) . ?
C13 H13 0.95 . ?
C14 H14 0.95 . ?
C15 C16 1.395(12) . ?
C15 C20 1.412(12) . ?
C15 P1 1.826(8) . ?
C16 C17 1.395(12) . ?
C16 H16 0.95 . ?
C17 C18 1.383(13) . ?
C17 H17 0.95 . ?
C18 C19 1.402(14) . ?
C18 H18 0.95 . ?
C19 C20 1.367(13) . ?
C19 H19 0.95 . ?
C20 H20 0.95 . ?
C21 C26 1.364(13) . ?
C21 C22 1.413(12) . ?
C21 P2 1.838(8) . ?
C22 C23 1.378(12) . ?
C22 H22 0.95 . ?
C23 C24 1.381(14) . ?
C23 H23 0.95 . ?
C24 C25 1.356(14) . ?
C24 H24 0.95 . ?
C25 C26 1.399(12) . ?
C25 H25 0.95 . ?
C26 H26 0.95 . ?
C27 C28 1.371(12) . ?
C27 C32 1.414(12) . ?
C27 P2 1.834(9) . ?
C28 C29 1.386(13) . ?
C28 H28 0.95 . ?
C29 C30 1.383(14) . ?
C29 H29 0.95 . ?
C30 C31 1.386(14) . ?
C30 H30 0.95 . ?
C31 C32 1.385(13) . ?
C31 H31 0.95 . ?
C32 H32 0.95 . ?
Cl Re 2.525(2) . ?
N O4 1.216(10) . ?
N O3 1.217(10) . ?
O1 Re 2.121(6) . ?
O2 Re 2.162(6) 6_756 ?
P1 Re 2.400(2) 6_756 ?
P2 Re 2.390(2) . ?
Re O2 2.162(6) 6_756 ?
Re Re 2.3208(9) 6_756 ?
Re P1 2.400(2) 6_756 ?
O5 C36 1.381(12) . ?
O5 C33 1.434(13) . ?
C33 C34 1.506(14) . ?
C33 H33A 0.99 . ?
C33 H33B 0.99 . ?
C34 C35 1.503(14) . ?
C34 H34A 0.99 . ?
C34 H34B 0.99 . ?
C35 C36 1.514(14) . ?
C35 H35A 0.99 . ?
C35 H35B 0.99 . ?
C36 H36A 0.99 . ?
C36 H36B 0.99 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O2 123.3(8) . . ?
O1 C1 C2 117.5(8) . . ?
O2 C1 C2 119.2(7) . . ?
C7 C2 C3 120.5(9) . . ?
C7 C2 C1 120.8(8) . . ?
C3 C2 C1 117.9(8) . . ?
C2 C3 C4 120.1(9) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 117.6(9) . . ?
C5 C4 H4 121.2 . . ?
C3 C4 H4 121.2 . . ?
C4 C5 C6 123.2(9) . . ?
C4 C5 N 118.2(9) . . ?
C6 C5 N 118.6(8) . . ?
C5 C6 C7 117.9(9) . . ?
C5 C6 H6 121 . . ?
C7 C6 H6 121 . . ?
C2 C7 C6 120.5(8) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
P2 C8 P1 110.5(5) . . ?
P2 C8 H8A 109.6 . . ?
P1 C8 H8A 109.6 . . ?
P2 C8 H8B 109.6 . . ?
P1 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
C14 C9 C10 120.5(8) . . ?
C14 C9 P1 121.3(7) . . ?
C10 C9 P1 117.9(7) . . ?
C9 C10 C11 119.1(9) . . ?
C9 C10 H10 120.5 . . ?
C11 C10 H10 120.5 . . ?
C12 C11 C10 119.9(10) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.6(9) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C14 120.5(10) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C9 C14 C13 119.2(10) . . ?
C9 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C16 C15 C20 116.9(8) . . ?
C16 C15 P1 125.5(7) . . ?
C20 C15 P1 117.6(7) . . ?
C15 C16 C17 121.8(8) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C18 C17 C16 119.8(9) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C17 C18 C19 119.6(9) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 120.1(9) . . ?
C20 C19 H19 120 . . ?
C18 C19 H19 120 . . ?
C19 C20 C15 122.0(9) . . ?
C19 C20 H20 119 . . ?
C15 C20 H20 119 . . ?
C26 C21 C22 117.9(8) . . ?
C26 C21 P2 122.0(7) . . ?
C22 C21 P2 119.9(7) . . ?
C23 C22 C21 120.4(9) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C22 C23 C24 120.1(9) . . ?
C22 C23 H23 119.9 . . ?
C24 C23 H23 119.9 . . ?
C25 C24 C23 120.2(9) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C24 C25 C26 119.9(9) . . ?
C24 C25 H25 120 . . ?
C26 C25 H25 120 . . ?
C21 C26 C25 121.4(9) . . ?
C21 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 C32 118.6(8) . . ?
C28 C27 P2 125.6(7) . . ?
C32 C27 P2 115.7(7) . . ?
C27 C28 C29 121.5(9) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C30 C29 C28 119.8(9) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C29 C30 C31 119.9(9) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C32 C31 C30 120.2(9) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C27 119.9(9) . . ?
C31 C32 H32 120 . . ?
C27 C32 H32 120 . . ?
O4 N O3 123.9(9) . . ?
O4 N C5 117.3(9) . . ?
O3 N C5 118.8(8) . . ?
C1 O1 Re 120.0(6) . . ?
C1 O2 Re 116.4(5) . 6_756 ?
C15 P1 C9 99.1(4) . . ?
C15 P1 C8 102.4(4) . . ?
C9 P1 C8 102.0(4) . . ?
C15 P1 Re 121.2(3) . 6_756 ?
C9 P1 Re 119.1(3) . 6_756 ?
C8 P1 Re 110.2(3) . 6_756 ?
C8 P2 C27 107.7(4) . . ?
C8 P2 C21 102.3(4) . . ?
C27 P2 C21 98.7(4) . . ?
C8 P2 Re 108.7(3) . . ?
C27 P2 Re 115.9(3) . . ?
C21 P2 Re 121.9(3) . . ?
O1 Re O2 80.9(2) . 6_756 ?
O1 Re Re 88.11(16) . 6_756 ?
O2 Re Re 87.87(15) 6_756 6_756 ?
O1 Re P2 169.93(17) . . ?
O2 Re P2 89.90(16) 6_756 . ?
Re Re P2 95.69(5) 6_756 . ?
O1 Re P1 94.50(18) . 6_756 ?
O2 Re P1 171.84(16) 6_756 6_756 ?
Re Re P1 98.77(5) 6_756 6_756 ?
P2 Re P1 94.13(8) . 6_756 ?
O1 Re Cl 81.30(16) . . ?
O2 Re Cl 83.83(16) 6_756 . ?
Re Re Cl 167.44(5) 6_756 . ?
P2 Re Cl 93.71(8) . . ?
P1 Re Cl 88.82(8) 6_756 . ?
C36 O5 C33 105.9(8) . . ?
O5 C33 C34 104.9(9) . . ?
O5 C33 H33A 110.8 . . ?
C34 C33 H33A 110.8 . . ?
O5 C33 H33B 110.8 . . ?
C34 C33 H33B 110.8 . . ?
H33A C33 H33B 108.8 . . ?
C35 C34 C33 103.0(8) . . ?
C35 C34 H34A 111.2 . . ?
C33 C34 H34A 111.2 . . ?
C35 C34 H34B 111.2 . . ?
C33 C34 H34B 111.2 . . ?
H34A C34 H34B 109.1 . . ?
C34 C35 C36 104.2(9) . . ?
C34 C35 H35A 110.9 . . ?
C36 C35 H35A 110.9 . . ?
C34 C35 H35B 110.9 . . ?
C36 C35 H35B 110.9 . . ?
H35A C35 H35B 108.9 . . ?
O5 C36 C35 108.5(9) . . ?
O5 C36 H36A 110 . . ?
C35 C36 H36A 110 . . ?
O5 C36 H36B 110 . . ?
C35 C36 H36B 110 . . ?
H36A C36 H36B 108.4 . . ?
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
O1 C1 C2 C7 -175.8(9) . . . . ?
O2 C1 C2 C7 5.7(13) . . . . ?
O1 C1 C2 C3 -6.0(13) . . . . ?
O2 C1 C2 C3 175.4(9) . . . . ?
C7 C2 C3 C4 -3.5(15) . . . . ?
C1 C2 C3 C4 -173.3(9) . . . . ?
C2 C3 C4 C5 4.2(14) . . . . ?
C3 C4 C5 C6 -3.2(15) . . . . ?
C3 C4 C5 N 176.8(9) . . . . ?
C4 C5 C6 C7 1.4(15) . . . . ?
N C5 C6 C7 -178.5(8) . . . . ?
C3 C2 C7 C6 1.7(14) . . . . ?
C1 C2 C7 C6 171.1(9) . . . . ?
C5 C6 C7 C2 -0.6(14) . . . . ?
C14 C9 C10 C11 5.4(13) . . . . ?
P1 C9 C10 C11 -168.8(7) . . . . ?
C9 C10 C11 C12 -2.9(14) . . . . ?
C10 C11 C12 C13 -1.0(15) . . . . ?
C11 C12 C13 C14 2.3(15) . . . . ?
C10 C9 C14 C13 -4.1(13) . . . . ?
P1 C9 C14 C13 169.9(7) . . . . ?
C12 C13 C14 C9 0.2(14) . . . . ?
C20 C15 C16 C17 -0.6(13) . . . . ?
P1 C15 C16 C17 -176.9(7) . . . . ?
C15 C16 C17 C18 0.6(14) . . . . ?
C16 C17 C18 C19 0.0(14) . . . . ?
C17 C18 C19 C20 -0.5(15) . . . . ?
C18 C19 C20 C15 0.4(15) . . . . ?
C16 C15 C20 C19 0.1(14) . . . . ?
P1 C15 C20 C19 176.7(8) . . . . ?
C26 C21 C22 C23 0.1(15) . . . . ?
P2 C21 C22 C23 -175.1(8) . . . . ?
C21 C22 C23 C24 1.6(17) . . . . ?
C22 C23 C24 C25 -1.9(18) . . . . ?
C23 C24 C25 C26 0.5(17) . . . . ?
C22 C21 C26 C25 -1.6(15) . . . . ?
P2 C21 C26 C25 173.5(8) . . . . ?
C24 C25 C26 C21 1.3(17) . . . . ?
C32 C27 C28 C29 -1.9(13) . . . . ?
P2 C27 C28 C29 179.5(7) . . . . ?
C27 C28 C29 C30 2.1(14) . . . . ?
C28 C29 C30 C31 0.6(15) . . . . ?
C29 C30 C31 C32 -3.5(15) . . . . ?
C30 C31 C32 C27 3.7(14) . . . . ?
C28 C27 C32 C31 -1.0(13) . . . . ?
P2 C27 C32 C31 177.7(7) . . . . ?
C4 C5 N O4 177.2(10) . . . . ?
C6 C5 N O4 -2.8(14) . . . . ?
C4 C5 N O3 -6.5(14) . . . . ?
C6 C5 N O3 173.4(9) . . . . ?
O2 C1 O1 Re 3.7(12) . . . . ?
C2 C1 O1 Re -174.8(6) . . . . ?
O1 C1 O2 Re 13.2(12) . . . 6_756 ?
C2 C1 O2 Re -168.3(6) . . . 6_756 ?
C16 C15 P1 C9 114.5(8) . . . . ?
C20 C15 P1 C9 -61.8(8) . . . . ?
C16 C15 P1 C8 9.9(9) . . . . ?
C20 C15 P1 C8 -166.3(7) . . . . ?
C16 C15 P1 Re -113.2(8) . . . 6_756 ?
C20 C15 P1 Re 70.5(8) . . . 6_756 ?
C14 C9 P1 C15 138.8(7) . . . . ?
C10 C9 P1 C15 -47.1(8) . . . . ?
C14 C9 P1 C8 -116.3(8) . . . . ?
C10 C9 P1 C8 57.8(8) . . . . ?
C14 C9 P1 Re 5.2(8) . . . 6_756 ?
C10 C9 P1 Re 179.3(6) . . . 6_756 ?
P2 C8 P1 C15 -157.0(5) . . . . ?
P2 C8 P1 C9 100.7(5) . . . . ?
P2 C8 P1 Re -26.7(5) . . . 6_756 ?
P1 C8 P2 C27 -84.0(5) . . . . ?
P1 C8 P2 C21 172.5(5) . . . . ?
P1 C8 P2 Re 42.3(5) . . . . ?
C28 C27 P2 C8 -2.4(9) . . . . ?
C32 C27 P2 C8 179.0(6) . . . . ?
C28 C27 P2 C21 103.6(8) . . . . ?
C32 C27 P2 C21 -75.0(7) . . . . ?
C28 C27 P2 Re -124.4(7) . . . . ?
C32 C27 P2 Re 57.0(7) . . . . ?
C26 C21 P2 C8 4.7(9) . . . . ?
C22 C21 P2 C8 179.7(8) . . . . ?
C26 C21 P2 C27 -105.7(8) . . . . ?
C22 C21 P2 C27 69.3(8) . . . . ?
C26 C21 P2 Re 126.3(7) . . . . ?
C22 C21 P2 Re -58.7(8) . . . . ?
C1 O1 Re O2 72.4(7) . . . 6_756 ?
C1 O1 Re Re -15.8(6) . . . 6_756 ?
C1 O1 Re P2 96.7(11) . . . . ?
C1 O1 Re P1 -114.4(6) . . . 6_756 ?
C1 O1 Re Cl 157.5(7) . . . . ?
C8 P2 Re O1 -149.8(10) . . . . ?
C27 P2 Re O1 -28.3(10) . . . . ?
C21 P2 Re O1 91.7(10) . . . . ?
C8 P2 Re O2 -125.9(3) . . . 6_756 ?
C27 P2 Re O2 -4.4(3) . . . 6_756 ?
C21 P2 Re O2 115.7(4) . . . 6_756 ?
C8 P2 Re Re -38.0(3) . . . 6_756 ?
C27 P2 Re Re 83.5(3) . . . 6_756 ?
C21 P2 Re Re -156.5(4) . . . 6_756 ?
C8 P2 Re P1 61.2(3) . . . 6_756 ?
C27 P2 Re P1 -177.3(3) . . . 6_756 ?
C21 P2 Re P1 -57.2(4) . . . 6_756 ?
C8 P2 Re Cl 150.3(3) . . . . ?
C27 P2 Re Cl -88.2(3) . . . . ?
C21 P2 Re Cl 31.9(4) . . . . ?
C36 O5 C33 C34 -37.9(11) . . . . ?
O5 C33 C34 C35 31.9(11) . . . . ?
C33 C34 C35 C36 -14.9(11) . . . . ?
C33 O5 C36 C35 28.2(12) . . . . ?
C34 C35 C36 O5 -7.5(13) . . . . ?
# END of CIF