#------------------------------------------------------------------------------
#$Date: 2016-06-20 12:08:03 +0300 (Mon, 20 Jun 2016) $
#$Revision: 183806 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/89/4308953.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_4308953
loop_
_publ_author_name
'Lihui Wei'
'John Babich'
'William C. Eckelman'
'Jon Zubieta'
_publ_contact_author_address
;Dept. of Chemistry
Syracuse University
CST 1-014
Syracuse, NY 13244
;
_publ_contact_author_email       jazubiet@syr.edu
_publ_contact_author_fax         (315)443-4070
_publ_contact_author_name        'Jon Zubieta'
_publ_contact_author_phone       (315)443-2925
_publ_section_title
;
Rhenium Tricarbonyl Core Complexes of Thymidine and Uridine Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2198
_journal_page_last               2209
_journal_paper_doi               10.1021/ic048301n
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C66 H58 Br2 F6 N10 Na O18 P Re2'
_chemical_formula_weight         1979.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 112.422(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   24.618(3)
_cell_length_b                   11.4787(11)
_cell_length_c                   15.5902(15)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.41
_cell_volume                     4072.5(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Platform w/ APEX CCD detector'
_diffrn_measurement_method       'Phi and omega scan'
_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  0.0645
_diffrn_reflns_av_sigmaI/netI    0.1025
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21671
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    4.057
_exptl_absorpt_correction_T_max  0.7929
_exptl_absorpt_correction_T_min  0.4975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 97)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.305
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9982
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0579
_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)+(0.0762P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                8350
_reflns_number_total             9982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048301nsi20041203_114219.cif
_cod_data_source_block           c2
_cod_original_cell_volume        4072.5(7)
_cod_original_formula_sum        'C33 H29 Br F3 N5 Na0.50 O9 P0.50 Re'
_cod_database_code               4308953
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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.799091(14) 0.07573(3) 0.86256(2) 0.01570(9) Uani 1 1 d . . .
Br1 Br 0.84282(5) 0.98281(9) 0.49549(8) 0.0277(3) Uani 1 1 d . . .
N1 N 0.7741(4) -0.0745(7) 0.7638(6) 0.0160(17) Uani 1 1 d . . .
N2 N 0.7103(4) 0.1500(7) 0.7912(6) 0.0217(18) Uani 1 1 d . . .
N3 N 0.7986(4) 0.1550(7) 0.7315(6) 0.0172(16) Uani 1 1 d . . .
N4 N 0.8889(4) 0.5536(7) 0.6641(6) 0.025(2) Uani 1 1 d . . .
N5 N 0.8805(5) 0.7513(8) 0.6373(7) 0.027(3) Uani 1 1 d . . .
H5A H 0.8715 0.8083 0.5987 0.032 Uiso 1 1 calc R . .
O1 O 0.7911(4) -0.0180(8) 1.0419(5) 0.0346(19) Uani 1 1 d . . .
O2 O 0.9268(3) -0.0056(7) 0.9491(5) 0.0331(18) Uani 1 1 d . . .
O3 O 0.8287(4) 0.3015(8) 0.9746(6) 0.046(2) Uani 1 1 d . . .
O4 O 0.8478(3) 0.3677(6) 0.6588(6) 0.0280(17) Uani 1 1 d . . .
O5 O 0.9250(4) 0.2145(7) 0.5634(6) 0.037(2) Uani 1 1 d . . .
H5 H 0.8934 0.2332 0.5232 0.055 Uiso 1 1 calc R . .
O6 O 0.8573(5) 0.6256(7) 0.5164(6) 0.043(2) Uani 1 1 d . . .
O7 O 0.9052(4) 0.8838(7) 0.7525(6) 0.036(2) Uani 1 1 d . . .
C1 C 0.7936(5) 0.0158(9) 0.9725(7) 0.022(2) Uani 1 1 d . . .
C2 C 0.8775(5) 0.0280(9) 0.9148(7) 0.019(2) Uani 1 1 d . . .
C3 C 0.8200(5) 0.2167(10) 0.9338(8) 0.025(2) Uani 1 1 d . . .
C4 C 0.7630(4) 0.0804(13) 0.6491(6) 0.0230(18) Uani 1 1 d . . .
H4A H 0.7802 0.0842 0.6026 0.028 Uiso 1 1 calc R . .
H4B H 0.7233 0.1106 0.6217 0.028 Uiso 1 1 calc R . .
C5 C 0.7612(4) -0.0462(8) 0.6779(7) 0.0163(19) Uani 1 1 d . . .
C6 C 0.7424(5) -0.1276(9) 0.6039(7) 0.023(2) Uani 1 1 d . . .
H6 H 0.7313 -0.1029 0.5428 0.027 Uiso 1 1 calc R . .
C7 C 0.7409(5) -0.2453(9) 0.6246(8) 0.028(2) Uani 1 1 d . . .
H7 H 0.7292 -0.3006 0.5775 0.034 Uiso 1 1 calc R . .
C8 C 0.7568(5) -0.2781(8) 0.7152(8) 0.023(2) Uani 1 1 d . . .
C9 C 0.7733(4) -0.1915(8) 0.7866(7) 0.019(2) Uani 1 1 d . . .
C10 C 0.7922(5) -0.2280(9) 0.8801(8) 0.027(2) Uani 1 1 d . . .
H10 H 0.8045 -0.1732 0.9276 0.032 Uiso 1 1 calc R . .
C11 C 0.7923(6) -0.3457(11) 0.9012(9) 0.041(3) Uani 1 1 d . . .
H11 H 0.8044 -0.3700 0.9626 0.049 Uiso 1 1 calc R . .
C12 C 0.7746(5) -0.4253(15) 0.8308(7) 0.034(2) Uani 1 1 d . . .
H12 H 0.7733 -0.5033 0.8462 0.041 Uiso 1 1 calc R . .
C13 C 0.7594(5) -0.3987(8) 0.7434(8) 0.030(3) Uani 1 1 d . . .
H13 H 0.7501 -0.4575 0.6990 0.036 Uiso 1 1 calc R . .
C14 C 0.7631(5) 0.2667(9) 0.7204(8) 0.023(2) Uani 1 1 d . . .
H14A H 0.7873 0.3261 0.7617 0.028 Uiso 1 1 calc R . .
H14B H 0.7511 0.2949 0.6572 0.028 Uiso 1 1 calc R . .
C15 C 0.7097(5) 0.2446(8) 0.7426(7) 0.021(2) Uani 1 1 d . . .
C16 C 0.6619(5) 0.3243(10) 0.7115(9) 0.033(3) Uani 1 1 d . . .
H16 H 0.6627 0.3882 0.6753 0.040 Uiso 1 1 calc R . .
C17 C 0.6152(5) 0.3054(11) 0.7357(10) 0.037(3) Uani 1 1 d . . .
H17 H 0.5848 0.3594 0.7196 0.045 Uiso 1 1 calc R . .
C18 C 0.6129(5) 0.2042(10) 0.7852(8) 0.028(2) Uani 1 1 d . . .
C19 C 0.6591(5) 0.1254(9) 0.8087(7) 0.022(2) Uani 1 1 d . . .
C20 C 0.6555(5) 0.0191(9) 0.8513(8) 0.021(2) Uani 1 1 d . . .
H20 H 0.6856 -0.0355 0.8647 0.026 Uiso 1 1 calc R . .
C21 C 0.6083(5) -0.0032(9) 0.8727(8) 0.026(2) Uani 1 1 d . . .
H21 H 0.6055 -0.0737 0.9001 0.031 Uiso 1 1 calc R . .
C22 C 0.5626(4) 0.0814(14) 0.8531(8) 0.037(3) Uani 1 1 d . . .
H22 H 0.5311 0.0678 0.8708 0.044 Uiso 1 1 calc R . .
C23 C 0.5651(5) 0.1787(11) 0.8097(9) 0.035(3) Uani 1 1 d . . .
H23 H 0.5344 0.2318 0.7951 0.042 Uiso 1 1 calc R . .
C24 C 0.8569(4) 0.1780(10) 0.7328(7) 0.023(2) Uani 1 1 d . . .
H24A H 0.8763 0.1036 0.7366 0.028 Uiso 1 1 calc R . .
H24B H 0.8787 0.2200 0.7895 0.028 Uiso 1 1 calc R . .
C25 C 0.8626(5) 0.2458(9) 0.6526(8) 0.023(2) Uani 1 1 d . . .
H25 H 0.8353 0.2133 0.5939 0.027 Uiso 1 1 calc R . .
C26 C 0.9253(5) 0.2435(9) 0.6531(9) 0.029(3) Uani 1 1 d . . .
H26 H 0.9504 0.1898 0.7006 0.035 Uiso 1 1 calc R . .
C27 C 0.9472(5) 0.3679(9) 0.6742(8) 0.025(2) Uani 1 1 d . . .
H27A H 0.9739 0.3882 0.6442 0.030 Uiso 1 1 calc R . .
H27B H 0.9662 0.3817 0.7405 0.030 Uiso 1 1 calc R . .
C28 C 0.8882(6) 0.4336(11) 0.6313(10) 0.028(3) Uani 1 1 d . . .
H28 H 0.8750 0.4332 0.5636 0.033 Uiso 1 1 calc R . .
C29 C 0.8746(5) 0.6415(8) 0.5999(8) 0.026(2) Uani 1 1 d . . .
C30 C 0.8991(6) 0.7802(10) 0.7296(8) 0.031(3) Uani 1 1 d . . .
C31 C 0.9133(5) 0.6825(9) 0.7927(8) 0.025(2) Uani 1 1 d . . .
C32 C 0.9064(4) 0.5800(15) 0.7575(6) 0.0242(18) Uani 1 1 d . . .
H32 H 0.9137 0.5177 0.7984 0.029 Uiso 1 1 calc R . .
C33 C 0.9341(7) 0.7093(12) 0.8922(9) 0.040(3) Uani 1 1 d . . .
H33A H 0.9068 0.7608 0.9033 0.060 Uiso 1 1 calc R . .
H33B H 0.9719 0.7460 0.9118 0.060 Uiso 1 1 calc R . .
H33C H 0.9372 0.6385 0.9265 0.060 Uiso 1 1 calc R . .
Na1 Na 1.0000 0.2313(6) 0.5000 0.050(2) Uani 1 2 d S . .
P1 P 1.0000 0.3287(4) 1.0000 0.0275(9) Uani 1 2 d S . .
F1 F 1.0097(6) 0.3395(13) 0.9074(8) 0.102(4) Uani 1 1 d . . .
F2 F 0.9494(7) 0.2426(16) 0.9579(11) 0.139(7) Uani 1 1 d . . .
F3 F 0.9500(11) 0.4235(17) 0.9618(15) 0.232(13) Uani 1 1 d . . .
O8 O 0.9477(9) 0.083(3) 0.406(2) 0.29(2) Uani 1 1 d . . .
O9 O 0.979(6) 0.435(2) 0.483(10) 0.57(7) Uani 1 1 d . . .
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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
Na Na 0.0362 0.0249 '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
C2 Re1 C1 85.3(4) . . ?
C2 Re1 C3 89.5(4) . . ?
C1 Re1 C3 83.0(5) . . ?
C2 Re1 N2 172.4(4) . . ?
C1 Re1 N2 101.3(4) . . ?
C3 Re1 N2 87.8(4) . . ?
C2 Re1 N3 99.4(4) . . ?
C1 Re1 N3 175.1(4) . . ?
C3 Re1 N3 95.3(4) . . ?
N2 Re1 N3 73.9(3) . . ?
C2 Re1 N1 92.4(4) . . ?
C1 Re1 N1 104.3(4) . . ?
C3 Re1 N1 172.6(4) . . ?
N2 Re1 N1 89.5(3) . . ?
N3 Re1 N1 77.3(3) . . ?
C5 N1 C9 119.0(9) . . ?
C5 N1 Re1 114.5(6) . . ?
C9 N1 Re1 126.5(7) . . ?
C15 N2 C19 117.2(9) . . ?
C15 N2 Re1 113.5(7) . . ?
C19 N2 Re1 127.4(6) . . ?
C24 N3 C4 111.3(8) . . ?
C24 N3 C14 111.6(8) . . ?
C4 N3 C14 104.9(8) . . ?
C24 N3 Re1 113.7(6) . . ?
C4 N3 Re1 110.2(6) . . ?
C14 N3 Re1 104.5(6) . . ?
C29 N4 C32 119.8(10) . . ?
C29 N4 C28 118.2(9) . . ?
C32 N4 C28 122.0(11) . . ?
C29 N5 C30 127.3(10) . . ?
C29 N5 H5A 116.3 . . ?
C30 N5 H5A 116.3 . . ?
C28 O4 C25 105.5(8) . . ?
C26 O5 H5 109.5 . . ?
O1 C1 Re1 177.8(10) . . ?
O2 C2 Re1 177.8(9) . . ?
O3 C3 Re1 175.7(10) . . ?
N3 C4 C5 111.1(8) . . ?
N3 C4 H4A 109.4 . . ?
C5 C4 H4A 109.4 . . ?
N3 C4 H4B 109.4 . . ?
C5 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N1 C5 C6 123.5(9) . . ?
N1 C5 C4 121.3(9) . . ?
C6 C5 C4 115.2(8) . . ?
C7 C6 C5 118.7(9) . . ?
C7 C6 H6 120.7 . . ?
C5 C6 H6 120.7 . . ?
C8 C7 C6 119.0(9) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C7 C8 C9 119.8(9) . . ?
C7 C8 C13 122.7(10) . . ?
C9 C8 C13 117.5(10) . . ?
N1 C9 C10 121.2(9) . . ?
N1 C9 C8 120.0(9) . . ?
C10 C9 C8 118.7(9) . . ?
C11 C10 C9 120.1(10) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 119.3(12) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C13 C12 C11 124.0(14) . . ?
C13 C12 H12 118.0 . . ?
C11 C12 H12 118.0 . . ?
C12 C13 C8 120.2(12) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
C15 C14 N3 110.2(8) . . ?
C15 C14 H14A 109.6 . . ?
N3 C14 H14A 109.6 . . ?
C15 C14 H14B 109.6 . . ?
N3 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
N2 C15 C16 123.5(10) . . ?
N2 C15 C14 116.8(9) . . ?
C16 C15 C14 119.7(9) . . ?
C17 C16 C15 118.7(10) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.6 . . ?
C16 C17 C18 120.0(11) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C19 C18 C23 118.8(10) . . ?
C19 C18 C17 118.7(10) . . ?
C23 C18 C17 122.4(11) . . ?
C18 C19 C20 119.7(10) . . ?
C18 C19 N2 121.3(9) . . ?
C20 C19 N2 119.0(10) . . ?
C21 C20 C19 119.7(10) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 120.1(10) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C23 C22 C21 119.9(10) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C18 121.7(11) . . ?
C22 C23 H23 119.2 . . ?
C18 C23 H23 119.2 . . ?
N3 C24 C25 118.8(8) . . ?
N3 C24 H24A 107.6 . . ?
C25 C24 H24A 107.6 . . ?
N3 C24 H24B 107.6 . . ?
C25 C24 H24B 107.6 . . ?
H24A C24 H24B 107.0 . . ?
O4 C25 C24 109.4(9) . . ?
O4 C25 C26 106.9(8) . . ?
C24 C25 C26 113.1(9) . . ?
O4 C25 H25 109.1 . . ?
C24 C25 H25 109.1 . . ?
C26 C25 H25 109.1 . . ?
O5 C26 C27 107.4(8) . . ?
O5 C26 C25 111.5(10) . . ?
C27 C26 C25 105.0(9) . . ?
O5 C26 H26 110.9 . . ?
C27 C26 H26 110.9 . . ?
C25 C26 H26 110.9 . . ?
C26 C27 C28 99.6(9) . . ?
C26 C27 H27A 111.9 . . ?
C28 C27 H27A 111.9 . . ?
C26 C27 H27B 111.9 . . ?
C28 C27 H27B 111.9 . . ?
H27A C27 H27B 109.6 . . ?
O4 C28 N4 108.0(10) . . ?
O4 C28 C27 104.9(9) . . ?
N4 C28 C27 115.1(10) . . ?
O4 C28 H28 109.6 . . ?
N4 C28 H28 109.6 . . ?
C27 C28 H28 109.6 . . ?
O6 C29 N4 123.9(9) . . ?
O6 C29 N5 121.9(10) . . ?
N4 C29 N5 114.2(9) . . ?
O7 C30 N5 119.4(11) . . ?
O7 C30 C31 125.4(11) . . ?
N5 C30 C31 115.0(10) . . ?
C32 C31 C30 117.6(11) . . ?
C32 C31 C33 125.5(11) . . ?
C30 C31 C33 117.0(10) . . ?
C31 C32 N4 126.1(13) . . ?
C31 C32 H32 117.0 . . ?
N4 C32 H32 117.0 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O8 Na1 O8 84(2) . 2_756 ?
O8 Na1 O9 147(4) . 2_756 ?
O8 Na1 O9 128(4) 2_756 2_756 ?
O8 Na1 O9 128(4) . . ?
O8 Na1 O9 147(4) 2_756 . ?
O9 Na1 O9 24(6) 2_756 . ?
O8 Na1 O5 90.5(5) . 2_756 ?
O8 Na1 O5 82.7(6) 2_756 2_756 ?
O9 Na1 O5 87.2(7) 2_756 2_756 ?
O9 Na1 O5 101.9(6) . 2_756 ?
F2 P1 F2 99.4(16) . 2_757 ?
F2 P1 F1 93.6(8) . 2_757 ?
F2 P1 F1 92.4(7) 2_757 2_757 ?
F2 P1 F1 92.4(7) . . ?
F2 P1 F1 93.6(8) 2_757 . ?
F1 P1 F1 170.8(12) 2_757 . ?
F2 P1 F3 83.9(12) . . ?
F2 P1 F3 176.2(14) 2_757 . ?
F1 P1 F3 85.5(9) 2_757 . ?
F1 P1 F3 88.2(9) . . ?
F2 P1 F3 176.2(14) . 2_757 ?
F2 P1 F3 83.9(12) 2_757 2_757 ?
F1 P1 F3 88.2(9) 2_757 2_757 ?
F1 P1 F3 85.5(9) . 2_757 ?
F3 P1 F3 93(2) . 2_757 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 C2 1.869(11) . ?
Re1 C1 1.899(10) . ?
Re1 C3 1.918(11) . ?
Re1 N2 2.210(9) . ?
Re1 N3 2.232(8) . ?
Re1 N1 2.236(9) . ?
N1 C5 1.294(12) . ?
N1 C9 1.392(12) . ?
N2 C15 1.320(12) . ?
N2 C19 1.416(14) . ?
N3 C24 1.452(13) . ?
N3 C4 1.514(13) . ?
N3 C14 1.524(13) . ?
N4 C29 1.369(13) . ?
N4 C32 1.386(12) . ?
N4 C28 1.466(16) . ?
N5 C29 1.373(13) . ?
N5 C30 1.373(15) . ?
N5 H5A 0.8600 . ?
O1 C1 1.172(13) . ?
O2 C2 1.188(13) . ?
O3 C3 1.139(14) . ?
O4 C28 1.439(13) . ?
O4 C25 1.458(12) . ?
O5 C26 1.436(14) . ?
O5 H5 0.8200 . ?
O6 C29 1.219(13) . ?
O7 C30 1.235(14) . ?
C4 C5 1.527(17) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.417(13) . ?
C6 C7 1.392(14) . ?
C6 H6 0.9300 . ?
C7 C8 1.367(16) . ?
C7 H7 0.9300 . ?
C8 C9 1.430(14) . ?
C8 C13 1.447(13) . ?
C9 C10 1.415(15) . ?
C10 C11 1.390(15) . ?
C10 H10 0.9300 . ?
C11 C12 1.365(19) . ?
C11 H11 0.9300 . ?
C12 C13 1.305(15) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.504(15) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.421(15) . ?
C16 C17 1.357(17) . ?
C16 H16 0.9300 . ?
C17 C18 1.408(16) . ?
C17 H17 0.9300 . ?
C18 C19 1.390(15) . ?
C18 C23 1.399(15) . ?
C19 C20 1.409(13) . ?
C20 C21 1.350(16) . ?
C20 H20 0.9300 . ?
C21 C22 1.428(16) . ?
C21 H21 0.9300 . ?
C22 C23 1.319(17) . ?
C22 H22 0.9300 . ?
C23 H23 0.9300 . ?
C24 C25 1.523(15) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.540(15) . ?
C25 H25 0.9800 . ?
C26 C27 1.518(15) . ?
C26 H26 0.9800 . ?
C27 C28 1.545(17) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28 0.9800 . ?
C30 C31 1.444(16) . ?
C31 C32 1.282(19) . ?
C31 C33 1.469(16) . ?
C32 H32 0.9300 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
Na1 O8 2.301(19) . ?
Na1 O8 2.301(19) 2_756 ?
Na1 O9 2.39(4) 2_756 ?
Na1 O9 2.39(4) . ?
Na1 O5 2.412(8) 2_756 ?
P1 F2 1.528(11) . ?
P1 F2 1.528(11) 2_757 ?
P1 F1 1.555(10) 2_757 ?
P1 F1 1.555(10) . ?
P1 F3 1.581(13) . ?
P1 F3 1.581(13) 2_757 ?
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
N5 H5A Br1 0.86 2.50 3.354(10) 175.3 .
O5 H5 Br1 0.82 3.10 3.263(9) 94.4 1_545
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
C2 Re1 N1 C5 -110.1(7) . . . . ?
C1 Re1 N1 C5 164.2(7) . . . . ?
C3 Re1 N1 C5 -6(3) . . . . ?
N2 Re1 N1 C5 62.6(7) . . . . ?
N3 Re1 N1 C5 -11.0(7) . . . . ?
C2 Re1 N1 C9 67.5(8) . . . . ?
C1 Re1 N1 C9 -18.2(9) . . . . ?
C3 Re1 N1 C9 172(3) . . . . ?
N2 Re1 N1 C9 -119.8(8) . . . . ?
N3 Re1 N1 C9 166.6(9) . . . . ?
C2 Re1 N2 C15 -5(3) . . . . ?
C1 Re1 N2 C15 146.2(8) . . . . ?
C3 Re1 N2 C15 63.8(8) . . . . ?
N3 Re1 N2 C15 -32.4(7) . . . . ?
N1 Re1 N2 C15 -109.3(7) . . . . ?
C2 Re1 N2 C19 -169(3) . . . . ?
C1 Re1 N2 C19 -17.9(9) . . . . ?
C3 Re1 N2 C19 -100.3(9) . . . . ?
N3 Re1 N2 C19 163.5(9) . . . . ?
N1 Re1 N2 C19 86.6(9) . . . . ?
C2 Re1 N3 C24 -15.9(7) . . . . ?
C1 Re1 N3 C24 145(5) . . . . ?
C3 Re1 N3 C24 74.5(7) . . . . ?
N2 Re1 N3 C24 160.6(7) . . . . ?
N1 Re1 N3 C24 -106.2(7) . . . . ?
C2 Re1 N3 C4 109.9(7) . . . . ?
C1 Re1 N3 C4 -90(5) . . . . ?
C3 Re1 N3 C4 -159.8(7) . . . . ?
N2 Re1 N3 C4 -73.6(7) . . . . ?
N1 Re1 N3 C4 19.6(6) . . . . ?
C2 Re1 N3 C14 -137.8(6) . . . . ?
C1 Re1 N3 C14 23(5) . . . . ?
C3 Re1 N3 C14 -47.5(7) . . . . ?
N2 Re1 N3 C14 38.7(6) . . . . ?
N1 Re1 N3 C14 131.9(6) . . . . ?
C2 Re1 C1 O1 75(25) . . . . ?
C3 Re1 C1 O1 -15(25) . . . . ?
N2 Re1 C1 O1 -101(25) . . . . ?
N3 Re1 C1 O1 -86(27) . . . . ?
N1 Re1 C1 O1 166(25) . . . . ?
C1 Re1 C2 O2 39(25) . . . . ?
C3 Re1 C2 O2 122(25) . . . . ?
N2 Re1 C2 O2 -169(23) . . . . ?
N3 Re1 C2 O2 -142(25) . . . . ?
N1 Re1 C2 O2 -65(25) . . . . ?
C2 Re1 C3 O3 -166(14) . . . . ?
C1 Re1 C3 O3 -81(14) . . . . ?
N2 Re1 C3 O3 21(14) . . . . ?
N3 Re1 C3 O3 94(14) . . . . ?
N1 Re1 C3 O3 89(14) . . . . ?
C24 N3 C4 C5 101.8(9) . . . . ?
C14 N3 C4 C5 -137.3(8) . . . . ?
Re1 N3 C4 C5 -25.3(9) . . . . ?
C9 N1 C5 C6 4.3(14) . . . . ?
Re1 N1 C5 C6 -177.9(8) . . . . ?
C9 N1 C5 C4 -178.2(9) . . . . ?
Re1 N1 C5 C4 -0.4(11) . . . . ?
N3 C4 C5 N1 17.9(13) . . . . ?
N3 C4 C5 C6 -164.4(8) . . . . ?
N1 C5 C6 C7 -4.0(16) . . . . ?
C4 C5 C6 C7 178.5(10) . . . . ?
C5 C6 C7 C8 0.8(17) . . . . ?
C6 C7 C8 C9 1.5(17) . . . . ?
C6 C7 C8 C13 -176.9(11) . . . . ?
C5 N1 C9 C10 174.2(10) . . . . ?
Re1 N1 C9 C10 -3.3(14) . . . . ?
C5 N1 C9 C8 -1.8(14) . . . . ?
Re1 N1 C9 C8 -179.3(7) . . . . ?
C7 C8 C9 N1 -1.1(16) . . . . ?
C13 C8 C9 N1 177.3(10) . . . . ?
C7 C8 C9 C10 -177.2(11) . . . . ?
C13 C8 C9 C10 1.2(16) . . . . ?
N1 C9 C10 C11 -178.5(11) . . . . ?
C8 C9 C10 C11 -2.4(17) . . . . ?
C9 C10 C11 C12 1(2) . . . . ?
C10 C11 C12 C13 3(2) . . . . ?
C11 C12 C13 C8 -4.2(19) . . . . ?
C7 C8 C13 C12 -179.6(11) . . . . ?
C9 C8 C13 C12 2.0(17) . . . . ?
C24 N3 C14 C15 -166.2(8) . . . . ?
C4 N3 C14 C15 73.1(10) . . . . ?
Re1 N3 C14 C15 -42.9(9) . . . . ?
C19 N2 C15 C16 3.1(16) . . . . ?
Re1 N2 C15 C16 -162.8(9) . . . . ?
C19 N2 C15 C14 -177.1(9) . . . . ?
Re1 N2 C15 C14 17.1(12) . . . . ?
N3 C14 C15 N2 18.6(13) . . . . ?
N3 C14 C15 C16 -161.5(10) . . . . ?
N2 C15 C16 C17 2.7(19) . . . . ?
C14 C15 C16 C17 -177.2(12) . . . . ?
C15 C16 C17 C18 -4(2) . . . . ?
C16 C17 C18 C19 0(2) . . . . ?
C16 C17 C18 C23 -178.2(13) . . . . ?
C23 C18 C19 C20 3.8(17) . . . . ?
C17 C18 C19 C20 -174.7(11) . . . . ?
C23 C18 C19 N2 -175.8(11) . . . . ?
C17 C18 C19 N2 5.7(18) . . . . ?
C15 N2 C19 C18 -7.3(16) . . . . ?
Re1 N2 C19 C18 156.3(9) . . . . ?
C15 N2 C19 C20 173.1(9) . . . . ?
Re1 N2 C19 C20 -23.3(13) . . . . ?
C18 C19 C20 C21 -2.9(16) . . . . ?
N2 C19 C20 C21 176.8(10) . . . . ?
C19 C20 C21 C22 -0.8(17) . . . . ?
C20 C21 C22 C23 4(2) . . . . ?
C21 C22 C23 C18 -3(2) . . . . ?
C19 C18 C23 C22 -1(2) . . . . ?
C17 C18 C23 C22 177.4(14) . . . . ?
C4 N3 C24 C25 62.4(12) . . . . ?
C14 N3 C24 C25 -54.5(12) . . . . ?
Re1 N3 C24 C25 -172.4(7) . . . . ?
C28 O4 C25 C24 141.8(9) . . . . ?
C28 O4 C25 C26 18.9(12) . . . . ?
N3 C24 C25 O4 72.0(12) . . . . ?
N3 C24 C25 C26 -168.9(9) . . . . ?
O4 C25 C26 O5 -107.8(10) . . . . ?
C24 C25 C26 O5 131.7(9) . . . . ?
O4 C25 C26 C27 8.2(12) . . . . ?
C24 C25 C26 C27 -112.3(10) . . . . ?
O5 C26 C27 C28 89.3(10) . . . . ?
C25 C26 C27 C28 -29.5(11) . . . . ?
C25 O4 C28 N4 -161.9(9) . . . . ?
C25 O4 C28 C27 -38.8(12) . . . . ?
C29 N4 C28 O4 -122.1(11) . . . . ?
C32 N4 C28 O4 61.3(13) . . . . ?
C29 N4 C28 C27 121.2(11) . . . . ?
C32 N4 C28 C27 -55.5(14) . . . . ?
C26 C27 C28 O4 42.5(12) . . . . ?
C26 C27 C28 N4 160.9(10) . . . . ?
C32 N4 C29 O6 -177.8(11) . . . . ?
C28 N4 C29 O6 5.4(18) . . . . ?
C32 N4 C29 N5 1.2(15) . . . . ?
C28 N4 C29 N5 -175.5(10) . . . . ?
C30 N5 C29 O6 179.6(13) . . . . ?
C30 N5 C29 N4 0.6(19) . . . . ?
C29 N5 C30 O7 176.0(12) . . . . ?
C29 N5 C30 C31 -0.6(19) . . . . ?
O7 C30 C31 C32 -177.6(12) . . . . ?
N5 C30 C31 C32 -1.3(16) . . . . ?
O7 C30 C31 C33 3.1(19) . . . . ?
N5 C30 C31 C33 179.3(12) . . . . ?
C30 C31 C32 N4 3.2(16) . . . . ?
C33 C31 C32 N4 -177.4(11) . . . . ?
C29 N4 C32 C31 -3.3(16) . . . . ?
C28 N4 C32 C31 173.3(11) . . . . ?
O8 Na1 O9 O9 -153(9) . . . 2_756 ?
O8 Na1 O9 O9 42(9) 2_756 . . 2_756 ?
O5 Na1 O9 O9 -53(10) 2_756 . . 2_756 ?
