#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:43:21 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179074 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/36/4303692.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_4303692
loop_
_publ_author_name
'Yuee Feng'
'Joel Aponte'
'Paul J. Houseworth'
'Paul D. Boyle'
'Elon A. Ison'
_publ_section_title
;
Synthesis of Oxorhenium(V) Complexes with Diamido Amine Ancillary Ligands
and Their Role in Oxygen Atom Transfer Catalysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11058
_journal_page_last               11066
_journal_paper_doi               10.1021/ic901434u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C17 H11 F10 I N3 O Re'
_chemical_formula_weight         776.39
_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                96.614(2)
_cell_angle_beta                 92.581(3)
_cell_angle_gamma                106.742(2)
_cell_formula_units_Z            2
_cell_length_a                   6.8210(3)
_cell_length_b                   8.1645(4)
_cell_length_c                   19.3225(10)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    110
_cell_measurement_theta_max      31.81
_cell_measurement_theta_min      2.63
_cell_volume                     1020.13(9)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  XL
_computing_structure_solution    XS
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker-Nonius X8 Apex2'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0348
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28433
_diffrn_reflns_theta_full        32.37
_diffrn_reflns_theta_max         32.37
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    7.575
_exptl_absorpt_correction_T_max  0.6593
_exptl_absorpt_correction_T_min  0.4634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    2.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.691
_refine_diff_density_min         -1.993
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0269
_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)+(0.0327P)²+0.8970P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0622
_reflns_number_gt                5562
_reflns_number_total             6272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901434u_si_001_2.cif
_cod_data_source_block           x09035
_cod_database_code               4303692
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
Re1 Re 0.247805(18) 0.824825(15) 0.253016(6) 0.01227(4) Uani 1 1 d . . .
I1 I -0.06918(3) 0.55608(3) 0.276031(11) 0.01672(5) Uani 1 1 d . . .
O1 O 0.1294(4) 0.9809(3) 0.25624(13) 0.0196(5) Uani 1 1 d . . .
N1 N 0.5438(4) 0.9813(3) 0.23439(14) 0.0138(5) Uani 1 1 d . . .
N2 N 0.4102(4) 0.8028(3) 0.33518(14) 0.0146(5) Uani 1 1 d . . .
N3 N 0.2826(4) 0.7071(3) 0.16235(14) 0.0140(5) Uani 1 1 d . . .
C1 C 0.3564(5) 0.6814(4) 0.38340(17) 0.0159(6) Uani 1 1 d . . .
C2 C 0.3034(5) 0.7305(4) 0.44943(17) 0.0174(7) Uani 1 1 d . . .
C3 C 0.2530(5) 0.6152(5) 0.49738(18) 0.0220(7) Uani 1 1 d . . .
C4 C 0.2528(5) 0.4476(5) 0.48022(19) 0.0218(7) Uani 1 1 d . . .
C5 C 0.3048(5) 0.3946(4) 0.41512(19) 0.0204(7) Uani 1 1 d . . .
C6 C 0.3584(5) 0.5119(4) 0.36809(18) 0.0186(7) Uani 1 1 d . . .
F1 F 0.2969(3) 0.8926(3) 0.46695(11) 0.0244(5) Uani 1 1 d . . .
F2 F 0.2046(3) 0.6681(3) 0.56120(11) 0.0297(5) Uani 1 1 d . . .
F3 F 0.2039(3) 0.3353(3) 0.52669(12) 0.0306(5) Uani 1 1 d . . .
F4 F 0.3075(4) 0.2314(3) 0.39847(13) 0.0307(5) Uani 1 1 d . . .
F5 F 0.4076(3) 0.4569(3) 0.30496(11) 0.0238(5) Uani 1 1 d . . .
C7 C 0.6289(5) 0.9074(4) 0.34856(18) 0.0170(7) Uani 1 1 d . . .
H7A H 0.7193 0.8341 0.3374 0.020 Uiso 1 1 calc R . .
H7B H 0.6591 0.9574 0.3984 0.020 Uiso 1 1 calc R . .
C8 C 0.6667(5) 1.0496(4) 0.30285(17) 0.0168(7) Uani 1 1 d . . .
H8A H 0.6259 1.1481 0.3259 0.020 Uiso 1 1 calc R . .
H8B H 0.8146 1.0906 0.2954 0.020 Uiso 1 1 calc R . .
C9 C 0.5290(6) 1.1299(4) 0.19767(19) 0.0204(7) Uani 1 1 d . . .
H9A H 0.4701 1.2052 0.2279 0.031 Uiso 1 1 calc R . .
H9B H 0.4407 1.0860 0.1541 0.031 Uiso 1 1 calc R . .
H9C H 0.6664 1.1955 0.1871 0.031 Uiso 1 1 calc R . .
C10 C 0.6385(5) 0.8687(4) 0.18851(17) 0.0145(6) Uani 1 1 d . . .
H10A H 0.6799 0.7868 0.2157 0.017 Uiso 1 1 calc R . .
H10B H 0.7618 0.9402 0.1694 0.017 Uiso 1 1 calc R . .
C11 C 0.4780(5) 0.7712(4) 0.12962(17) 0.0162(6) Uani 1 1 d . . .
H11A H 0.4632 0.8486 0.0952 0.019 Uiso 1 1 calc R . .
H11B H 0.5179 0.6735 0.1054 0.019 Uiso 1 1 calc R . .
C12 C 0.1448(5) 0.5572(4) 0.12432(16) 0.0142(6) Uani 1 1 d . . .
C13 C -0.0414(5) 0.5579(4) 0.09302(17) 0.0165(6) Uani 1 1 d . . .
C14 C -0.1835(5) 0.4090(5) 0.06035(18) 0.0198(7) Uani 1 1 d . . .
C15 C -0.1398(6) 0.2539(4) 0.05569(18) 0.0207(7) Uani 1 1 d . . .
C16 C 0.0483(6) 0.2496(4) 0.08468(18) 0.0203(7) Uani 1 1 d . . .
C17 C 0.1856(5) 0.3990(4) 0.11820(17) 0.0171(7) Uani 1 1 d . . .
F6 F -0.0898(3) 0.7060(3) 0.09568(11) 0.0213(4) Uani 1 1 d . . .
F7 F -0.3635(3) 0.4151(3) 0.03149(11) 0.0260(5) Uani 1 1 d . . .
F8 F -0.2763(4) 0.1095(3) 0.02445(12) 0.0313(5) Uani 1 1 d . . .
F9 F 0.0911(4) 0.0988(3) 0.08122(12) 0.0329(6) Uani 1 1 d . . .
F10 F 0.3638(3) 0.3904(3) 0.14769(11) 0.0234(5) 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
Re Re -1.0185 7.2310 '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
O1 Re1 N2 120.04(12) . . ?
O1 Re1 N3 119.63(12) . . ?
N2 Re1 N3 118.44(11) . . ?
O1 Re1 N1 97.10(11) . . ?
N2 Re1 N1 79.39(11) . . ?
N3 Re1 N1 79.84(11) . . ?
O1 Re1 I1 99.66(8) . . ?
N2 Re1 I1 91.77(8) . . ?
N3 Re1 I1 92.18(8) . . ?
N1 Re1 I1 163.23(7) . . ?
C8 N1 C9 109.1(2) . . ?
C8 N1 C10 111.8(3) . . ?
C9 N1 C10 109.2(3) . . ?
C8 N1 Re1 108.7(2) . . ?
C9 N1 Re1 111.2(2) . . ?
C10 N1 Re1 106.91(18) . . ?
C1 N2 C7 111.0(3) . . ?
C1 N2 Re1 128.6(2) . . ?
C7 N2 Re1 119.9(2) . . ?
C12 N3 C11 113.8(3) . . ?
C12 N3 Re1 127.2(2) . . ?
C11 N3 Re1 118.9(2) . . ?
C6 C1 C2 116.9(3) . . ?
C6 C1 N2 122.5(3) . . ?
C2 C1 N2 120.5(3) . . ?
F1 C2 C3 118.9(3) . . ?
F1 C2 C1 119.6(3) . . ?
C3 C2 C1 121.5(3) . . ?
F2 C3 C4 120.1(3) . . ?
F2 C3 C2 119.7(3) . . ?
C4 C3 C2 120.2(3) . . ?
F3 C4 C3 120.3(3) . . ?
F3 C4 C5 119.8(3) . . ?
C3 C4 C5 119.8(3) . . ?
F4 C5 C4 120.0(3) . . ?
F4 C5 C6 120.6(3) . . ?
C4 C5 C6 119.4(3) . . ?
F5 C6 C5 118.2(3) . . ?
F5 C6 C1 119.6(3) . . ?
C5 C6 C1 122.1(3) . . ?
N2 C7 C8 108.1(3) . . ?
N2 C7 H7A 110.1 . . ?
C8 C7 H7A 110.1 . . ?
N2 C7 H7B 110.1 . . ?
C8 C7 H7B 110.1 . . ?
H7A C7 H7B 108.4 . . ?
N1 C8 C7 108.9(3) . . ?
N1 C8 H8A 109.9 . . ?
C7 C8 H8A 109.9 . . ?
N1 C8 H8B 109.9 . . ?
C7 C8 H8B 109.9 . . ?
H8A C8 H8B 108.3 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C11 107.3(2) . . ?
N1 C10 H10A 110.2 . . ?
C11 C10 H10A 110.2 . . ?
N1 C10 H10B 110.2 . . ?
C11 C10 H10B 110.2 . . ?
H10A C10 H10B 108.5 . . ?
N3 C11 C10 106.4(3) . . ?
N3 C11 H11A 110.4 . . ?
C10 C11 H11A 110.4 . . ?
N3 C11 H11B 110.4 . . ?
C10 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
C13 C12 C17 116.3(3) . . ?
C13 C12 N3 121.9(3) . . ?
C17 C12 N3 121.8(3) . . ?
F6 C13 C14 118.2(3) . . ?
F6 C13 C12 119.7(3) . . ?
C14 C13 C12 122.1(3) . . ?
F7 C14 C15 119.5(3) . . ?
F7 C14 C13 120.2(3) . . ?
C15 C14 C13 120.3(3) . . ?
F8 C15 C14 120.7(3) . . ?
F8 C15 C16 120.3(3) . . ?
C14 C15 C16 119.0(3) . . ?
F9 C16 C17 120.9(3) . . ?
F9 C16 C15 119.4(3) . . ?
C17 C16 C15 119.6(3) . . ?
F10 C17 C16 118.5(3) . . ?
F10 C17 C12 118.9(3) . . ?
C16 C17 C12 122.6(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
Re1 O1 1.691(2) . ?
Re1 N2 1.950(3) . ?
Re1 N3 1.957(3) . ?
Re1 N1 2.127(3) . ?
Re1 I1 2.6954(3) . ?
N1 C8 1.491(4) . ?
N1 C9 1.499(4) . ?
N1 C10 1.501(4) . ?
N2 C1 1.421(4) . ?
N2 C7 1.484(4) . ?
N3 C12 1.411(4) . ?
N3 C11 1.484(4) . ?
C1 C6 1.385(5) . ?
C1 C2 1.388(5) . ?
C2 F1 1.341(4) . ?
C2 C3 1.381(5) . ?
C3 F2 1.346(4) . ?
C3 C4 1.370(5) . ?
C4 F3 1.341(4) . ?
C4 C5 1.378(5) . ?
C5 F4 1.339(4) . ?
C5 C6 1.381(5) . ?
C6 F5 1.342(4) . ?
C7 C8 1.509(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.518(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.384(5) . ?
C12 C17 1.391(4) . ?
C13 F6 1.338(4) . ?
C13 C14 1.380(5) . ?
C14 F7 1.342(4) . ?
C14 C15 1.376(5) . ?
C15 F8 1.332(4) . ?
C15 C16 1.388(5) . ?
C16 F9 1.340(4) . ?
C16 C17 1.374(5) . ?
C17 F10 1.342(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 Re1 N1 C8 92.8(2) . . . . ?
N2 Re1 N1 C8 -26.55(19) . . . . ?
N3 Re1 N1 C8 -148.3(2) . . . . ?
I1 Re1 N1 C8 -85.7(3) . . . . ?
O1 Re1 N1 C9 -27.3(2) . . . . ?
N2 Re1 N1 C9 -146.6(2) . . . . ?
N3 Re1 N1 C9 91.7(2) . . . . ?
I1 Re1 N1 C9 154.2(2) . . . . ?
O1 Re1 N1 C10 -146.3(2) . . . . ?
N2 Re1 N1 C10 94.3(2) . . . . ?
N3 Re1 N1 C10 -27.4(2) . . . . ?
I1 Re1 N1 C10 35.2(4) . . . . ?
O1 Re1 N2 C1 102.4(3) . . . . ?
N3 Re1 N2 C1 -93.3(3) . . . . ?
N1 Re1 N2 C1 -165.5(3) . . . . ?
I1 Re1 N2 C1 0.1(3) . . . . ?
O1 Re1 N2 C7 -85.8(2) . . . . ?
N3 Re1 N2 C7 78.5(3) . . . . ?
N1 Re1 N2 C7 6.3(2) . . . . ?
I1 Re1 N2 C7 172.0(2) . . . . ?
O1 Re1 N3 C12 -89.3(3) . . . . ?
N2 Re1 N3 C12 106.3(3) . . . . ?
N1 Re1 N3 C12 178.2(3) . . . . ?
I1 Re1 N3 C12 13.1(3) . . . . ?
O1 Re1 N3 C11 94.7(2) . . . . ?
N2 Re1 N3 C11 -69.7(3) . . . . ?
N1 Re1 N3 C11 2.3(2) . . . . ?
I1 Re1 N3 C11 -162.9(2) . . . . ?
C7 N2 C1 C6 -95.7(4) . . . . ?
Re1 N2 C1 C6 76.7(4) . . . . ?
C7 N2 C1 C2 82.8(4) . . . . ?
Re1 N2 C1 C2 -104.7(3) . . . . ?
C6 C1 C2 F1 -179.4(3) . . . . ?
N2 C1 C2 F1 2.0(5) . . . . ?
C6 C1 C2 C3 -0.6(5) . . . . ?
N2 C1 C2 C3 -179.2(3) . . . . ?
F1 C2 C3 F2 -1.9(5) . . . . ?
C1 C2 C3 F2 179.3(3) . . . . ?
F1 C2 C3 C4 178.2(3) . . . . ?
C1 C2 C3 C4 -0.6(5) . . . . ?
F2 C3 C4 F3 0.2(5) . . . . ?
C2 C3 C4 F3 -180.0(3) . . . . ?
F2 C3 C4 C5 -179.2(3) . . . . ?
C2 C3 C4 C5 0.6(6) . . . . ?
F3 C4 C5 F4 -0.3(5) . . . . ?
C3 C4 C5 F4 179.1(3) . . . . ?
F3 C4 C5 C6 -178.9(3) . . . . ?
C3 C4 C5 C6 0.5(5) . . . . ?
F4 C5 C6 F5 1.7(5) . . . . ?
C4 C5 C6 F5 -179.7(3) . . . . ?
F4 C5 C6 C1 179.7(3) . . . . ?
C4 C5 C6 C1 -1.8(5) . . . . ?
C2 C1 C6 F5 179.7(3) . . . . ?
N2 C1 C6 F5 -1.7(5) . . . . ?
C2 C1 C6 C5 1.8(5) . . . . ?
N2 C1 C6 C5 -179.6(3) . . . . ?
C1 N2 C7 C8 -171.8(3) . . . . ?
Re1 N2 C7 C8 15.0(3) . . . . ?
C9 N1 C8 C7 163.0(3) . . . . ?
C10 N1 C8 C7 -76.1(3) . . . . ?
Re1 N1 C8 C7 41.7(3) . . . . ?
N2 C7 C8 N1 -36.5(4) . . . . ?
C8 N1 C10 C11 165.9(3) . . . . ?
C9 N1 C10 C11 -73.3(3) . . . . ?
Re1 N1 C10 C11 47.0(3) . . . . ?
C12 N3 C11 C10 -153.5(3) . . . . ?
Re1 N3 C11 C10 23.0(3) . . . . ?
N1 C10 C11 N3 -45.0(3) . . . . ?
C11 N3 C12 C13 -113.8(3) . . . . ?
Re1 N3 C12 C13 70.1(4) . . . . ?
C11 N3 C12 C17 68.4(4) . . . . ?
Re1 N3 C12 C17 -107.7(3) . . . . ?
C17 C12 C13 F6 -178.8(3) . . . . ?
N3 C12 C13 F6 3.3(5) . . . . ?
C17 C12 C13 C14 3.0(5) . . . . ?
N3 C12 C13 C14 -174.9(3) . . . . ?
F6 C13 C14 F7 0.8(5) . . . . ?
C12 C13 C14 F7 179.1(3) . . . . ?
F6 C13 C14 C15 179.3(3) . . . . ?
C12 C13 C14 C15 -2.5(5) . . . . ?
F7 C14 C15 F8 -1.7(5) . . . . ?
C13 C14 C15 F8 179.8(3) . . . . ?
F7 C14 C15 C16 178.9(3) . . . . ?
C13 C14 C15 C16 0.4(5) . . . . ?
F8 C15 C16 F9 -0.3(5) . . . . ?
C14 C15 C16 F9 179.1(3) . . . . ?
F8 C15 C16 C17 -178.4(3) . . . . ?
C14 C15 C16 C17 0.9(5) . . . . ?
F9 C16 C17 F10 -0.2(5) . . . . ?
C15 C16 C17 F10 178.0(3) . . . . ?
F9 C16 C17 C12 -178.5(3) . . . . ?
C15 C16 C17 C12 -0.3(5) . . . . ?
C13 C12 C17 F10 -179.9(3) . . . . ?
N3 C12 C17 F10 -2.0(5) . . . . ?
C13 C12 C17 C16 -1.6(5) . . . . ?
N3 C12 C17 C16 176.3(3) . . . . ?
