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#$Date: 2016-03-22 23:43:21 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179074 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/36/4303691.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_4303691
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            'C18 H14 F10 N3 O Re'
_chemical_formula_weight         664.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9091(4)
_cell_length_b                   21.1485(6)
_cell_length_c                   7.2240(2)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.14
_cell_measurement_theta_min      2.98
_cell_volume                     1972.21(10)
_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    SIR92
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            61364
_diffrn_reflns_theta_full        32.93
_diffrn_reflns_theta_max         32.93
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    6.272
_exptl_absorpt_correction_T_max  0.6338
_exptl_absorpt_correction_T_min  0.2388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.312
_refine_diff_density_min         -2.426
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         3772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0298
_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)+(0.0091P)²+7.7212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                3014
_reflns_number_total             3772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901434u_si_001_1.cif
_cod_data_source_block           x08062
_cod_database_code               4303691
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, z+1/2'
'x, -y+1/2, z'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, -z-1/2'
'-x, y-1/2, -z'
'x-1/2, y, -z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.203261(13) 0.2500 0.57106(3) 0.02359(5) Uani 1 2 d S . .
O1 O 0.2724(2) 0.2500 0.7689(5) 0.0359(9) Uani 1 2 d S . .
N1 N 0.0381(3) 0.2500 0.6207(6) 0.0286(9) Uani 1 2 d S . .
N2 N 0.1650(2) 0.16434(14) 0.4875(4) 0.0280(6) Uani 1 1 d . . .
C1 C 0.3171(3) 0.2500 0.3591(7) 0.0273(9) Uani 1 2 d S . .
H1A H 0.2829 0.2500 0.2379 0.041 Uiso 1 2 calc SR . .
H1B H 0.3604 0.2122 0.3707 0.041 Uiso 0.50 1 calc PR . .
H1C H 0.3604 0.2878 0.3707 0.041 Uiso 0.50 1 calc PR . .
C2 C 0.0270(4) 0.2500 0.8245(8) 0.0494(17) Uani 1 2 d S . .
H2A H 0.0602 0.2879 0.8757 0.074 Uiso 0.50 1 calc PR . .
H2B H 0.0603 0.2122 0.8757 0.074 Uiso 0.50 1 calc PR . .
H2C H -0.0466 0.2500 0.8572 0.074 Uiso 1 2 calc SR . .
C3 C -0.0117(3) 0.19240(18) 0.5407(6) 0.0371(9) Uani 1 1 d . . .
H3A H -0.0739 0.1811 0.6135 0.045 Uiso 1 1 calc R . .
H3B H -0.0333 0.2008 0.4115 0.045 Uiso 1 1 calc R . .
C4 C 0.0634(2) 0.13996(19) 0.5450(6) 0.0382(9) Uani 1 1 d . . .
H4A H 0.0679 0.1223 0.6716 0.046 Uiso 1 1 calc R . .
H4B H 0.0410 0.1059 0.4600 0.046 Uiso 1 1 calc R . .
C5 C 0.2188(2) 0.12514(16) 0.3635(5) 0.0284(7) Uani 1 1 d . . .
C6 C 0.1838(3) 0.11515(17) 0.1857(6) 0.0319(8) Uani 1 1 d . . .
C7 C 0.2360(3) 0.07880(17) 0.0592(6) 0.0350(8) Uani 1 1 d . . .
C8 C 0.3283(3) 0.05073(17) 0.1078(7) 0.0380(9) Uani 1 1 d . . .
C9 C 0.3666(3) 0.05937(17) 0.2825(6) 0.0348(8) Uani 1 1 d . . .
C10 C 0.3126(2) 0.09569(17) 0.4095(6) 0.0307(7) Uani 1 1 d . . .
F6 F 0.09467(16) 0.14301(10) 0.1317(3) 0.0374(5) Uani 1 1 d . . .
F7 F 0.1990(2) 0.07142(12) -0.1146(4) 0.0483(6) Uani 1 1 d . . .
F8 F 0.38026(19) 0.01539(11) -0.0153(4) 0.0507(7) Uani 1 1 d . . .
F9 F 0.45616(16) 0.03193(11) 0.3311(4) 0.0457(6) Uani 1 1 d . . .
F10 F 0.35342(16) 0.10381(12) 0.5777(3) 0.0410(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'
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 113.08(9) . . ?
O1 Re1 N2 113.08(9) . 3 ?
N2 Re1 N2 133.43(17) . 3 ?
O1 Re1 C1 104.20(18) . . ?
N2 Re1 C1 87.27(10) . . ?
N2 Re1 C1 87.27(10) 3 . ?
O1 Re1 N1 112.43(17) . . ?
N2 Re1 N1 78.70(9) . . ?
N2 Re1 N1 78.70(9) 3 . ?
C1 Re1 N1 143.36(18) . . ?
C2 N1 C3 110.1(3) . . ?
C2 N1 C3 110.1(3) . 3 ?
C3 N1 C3 109.3(4) . 3 ?
C2 N1 Re1 105.1(3) . . ?
C3 N1 Re1 111.1(2) . . ?
C3 N1 Re1 111.1(2) 3 . ?
C5 N2 C4 114.5(3) . . ?
C5 N2 Re1 127.9(2) . . ?
C4 N2 Re1 117.3(2) . . ?
Re1 C1 H1A 109.5 . . ?
Re1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Re1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 N1 108.8(3) . . ?
C4 C3 H3A 109.9 . . ?
N1 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
N1 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N2 C4 C3 108.5(3) . . ?
N2 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
N2 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
C6 C5 C10 115.9(3) . . ?
C6 C5 N2 121.5(3) . . ?
C10 C5 N2 122.6(3) . . ?
F6 C6 C7 118.1(4) . . ?
F6 C6 C5 118.8(3) . . ?
C7 C6 C5 123.1(3) . . ?
F7 C7 C6 120.6(3) . . ?
F7 C7 C8 119.5(4) . . ?
C6 C7 C8 119.8(4) . . ?
F8 C8 C9 120.4(4) . . ?
F8 C8 C7 120.3(4) . . ?
C9 C8 C7 119.4(4) . . ?
F9 C9 C8 119.7(4) . . ?
F9 C9 C10 120.1(4) . . ?
C8 C9 C10 120.2(3) . . ?
F10 C10 C9 118.4(3) . . ?
F10 C10 C5 119.9(3) . . ?
C9 C10 C5 121.6(4) . . ?
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 1.685(4) . ?
Re1 N2 1.972(3) . ?
Re1 N2 1.972(3) 3 ?
Re1 C1 2.122(5) . ?
Re1 N1 2.162(4) . ?
N1 C2 1.479(7) . ?
N1 C3 1.493(4) . ?
N1 C3 1.493(4) 3 ?
N2 C5 1.404(5) . ?
N2 C4 1.469(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.473(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.378(5) . ?
C5 C10 1.402(4) . ?
C6 F6 1.350(4) . ?
C6 C7 1.372(5) . ?
C7 F7 1.353(5) . ?
C7 C8 1.377(5) . ?
C8 F8 1.341(4) . ?
C8 C9 1.368(6) . ?
C9 F9 1.340(4) . ?
C9 C10 1.385(5) . ?
C10 F10 1.335(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 C2 0.0 . . . . ?
N2 Re1 N1 C2 110.49(9) . . . . ?
N2 Re1 N1 C2 -110.49(9) 3 . . . ?
C1 Re1 N1 C2 180.0 . . . . ?
O1 Re1 N1 C3 -119.1(3) . . . . ?
N2 Re1 N1 C3 -8.6(3) . . . . ?
N2 Re1 N1 C3 130.5(3) 3 . . . ?
C1 Re1 N1 C3 60.9(3) . . . . ?
O1 Re1 N1 C3 119.1(3) . . . 3 ?
N2 Re1 N1 C3 -130.5(3) . . . 3 ?
N2 Re1 N1 C3 8.6(3) 3 . . 3 ?
C1 Re1 N1 C3 -60.9(3) . . . 3 ?
O1 Re1 N2 C5 -93.0(3) . . . . ?
N2 Re1 N2 C5 94.9(3) 3 . . . ?
C1 Re1 N2 C5 11.2(3) . . . . ?
N1 Re1 N2 C5 157.2(3) . . . . ?
O1 Re1 N2 C4 93.7(3) . . . . ?
N2 Re1 N2 C4 -78.3(4) 3 . . . ?
C1 Re1 N2 C4 -162.0(3) . . . . ?
N1 Re1 N2 C4 -16.0(3) . . . . ?
C2 N1 C3 C4 -85.6(4) . . . . ?
C3 N1 C3 C4 153.3(3) 3 . . . ?
Re1 N1 C3 C4 30.4(4) . . . . ?
C5 N2 C4 C3 -136.4(4) . . . . ?
Re1 N2 C4 C3 37.8(4) . . . . ?
N1 C3 C4 N2 -42.4(5) . . . . ?
C4 N2 C5 C6 67.3(4) . . . . ?
Re1 N2 C5 C6 -106.1(3) . . . . ?
C4 N2 C5 C10 -115.1(4) . . . . ?
Re1 N2 C5 C10 71.5(4) . . . . ?
C10 C5 C6 F6 -179.0(3) . . . . ?
N2 C5 C6 F6 -1.2(5) . . . . ?
C10 C5 C6 C7 0.1(5) . . . . ?
N2 C5 C6 C7 177.9(3) . . . . ?
F6 C6 C7 F7 0.2(5) . . . . ?
C5 C6 C7 F7 -178.9(3) . . . . ?
F6 C6 C7 C8 178.6(3) . . . . ?
C5 C6 C7 C8 -0.5(6) . . . . ?
F7 C7 C8 F8 -1.2(5) . . . . ?
C6 C7 C8 F8 -179.6(3) . . . . ?
F7 C7 C8 C9 178.7(3) . . . . ?
C6 C7 C8 C9 0.2(6) . . . . ?
F8 C8 C9 F9 -0.5(5) . . . . ?
C7 C8 C9 F9 179.7(3) . . . . ?
F8 C8 C9 C10 -179.8(3) . . . . ?
C7 C8 C9 C10 0.4(6) . . . . ?
F9 C9 C10 F10 1.8(5) . . . . ?
C8 C9 C10 F10 -178.9(3) . . . . ?
F9 C9 C10 C5 179.9(3) . . . . ?
C8 C9 C10 C5 -0.8(5) . . . . ?
C6 C5 C10 F10 178.7(3) . . . . ?
N2 C5 C10 F10 0.9(5) . . . . ?
C6 C5 C10 C9 0.6(5) . . . . ?
N2 C5 C10 C9 -177.2(3) . . . . ?
