#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:14:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179237 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/57/4315768.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_4315768
loop_
_publ_author_name
'Theshini Perera'
'Patricia A. Marzilli'
'Frank R. Fronczek'
'Luigi G. Marzilli'
_publ_section_title
;
 NH NMR Shifts of New Structurally Characterized
 fac-[Re(CO)3(polyamine)]n+ Complexes Probed via Outer-Sphere
 Hydrogen-Bonding Interactions to Anions, Including the Paramagnetic
 [ReIVBr6]2- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5560
_journal_page_last               5572
_journal_paper_doi               10.1021/ic100386c
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C10 H19 N3 O3 Re, P F6'
_chemical_formula_sum            'C10 H19 F6 N3 O3 P Re'
_chemical_formula_weight         560.45
_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                87.892(7)
_cell_angle_beta                 84.975(6)
_cell_angle_gamma                89.380(7)
_cell_formula_units_Z            2
_cell_length_a                   8.3290(10)
_cell_length_b                   8.4008(10)
_cell_length_c                   11.8149(15)
_cell_measurement_reflns_used    5933
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      33.1
_cell_measurement_theta_min      2.5
_cell_volume                     822.93(17)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius 1999)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
'Direct_methods (SIR, Altomare, et al., 1994)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Nonius KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       'ω and φ 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  0.030
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24821
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         33.2
_diffrn_reflns_theta_min         2.8
_exptl_absorpt_coefficient_mu    7.559
_exptl_absorpt_correction_T_max  0.589
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle fragment'
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.66
_refine_diff_density_min         -1.89
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         6238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.026
_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)+(0.0245P)²+0.3934P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.054
_refine_ls_wR_factor_ref         0.055
_reflns_number_gt                5634
_reflns_number_total             6238
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic100386c_si_002_2.cif
_cod_data_source_block           Theshini52
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4315768
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 0.286141(11) 0.616605(11) 0.214281(8) 0.00884(4) Uani 1 1 d . . .
O1 O -0.0639(3) 0.6416(3) 0.1512(2) 0.0217(4) Uani 1 1 d . . .
O2 O 0.3440(3) 0.3737(2) 0.02682(17) 0.0160(4) Uani 1 1 d . . .
O3 O 0.1897(3) 0.3386(2) 0.38168(18) 0.0184(4) Uani 1 1 d . . .
N1 N 0.5477(3) 0.5950(3) 0.2469(2) 0.0135(4) Uani 1 1 d . . .
H21N H 0.549(4) 0.503(5) 0.269(3) 0.016 Uiso 1 1 d . . .
H22N H 0.604(4) 0.610(4) 0.179(3) 0.016 Uiso 1 1 d . . .
N2 N 0.2403(3) 0.8007(3) 0.35288(19) 0.0111(4) Uani 1 1 d . . .
N3 N 0.3674(3) 0.8253(3) 0.1031(2) 0.0127(4) Uani 1 1 d . . .
H31N H 0.461(4) 0.855(4) 0.120(3) 0.015 Uiso 1 1 d . . .
H32N H 0.386(4) 0.781(4) 0.031(3) 0.015 Uiso 1 1 d . . .
C1 C 0.0674(3) 0.6327(3) 0.1762(2) 0.0138(5) Uani 1 1 d . . .
C2 C 0.3243(3) 0.4667(3) 0.0966(2) 0.0126(5) Uani 1 1 d . . .
C3 C 0.2254(3) 0.4429(3) 0.3180(2) 0.0133(5) Uani 1 1 d . . .
C4 C 0.6250(3) 0.6853(3) 0.3342(3) 0.0160(5) Uani 1 1 d . . .
H4A H 0.6728 0.7840 0.2980 0.019 Uiso 1 1 calc R . .
H4B H 0.7134 0.6199 0.3629 0.019 Uiso 1 1 calc R . .
C5 C 0.5069(3) 0.7289(3) 0.4338(2) 0.0152(5) Uani 1 1 d . . .
H5A H 0.5680 0.7654 0.4960 0.018 Uiso 1 1 calc R . .
H5B H 0.4467 0.6324 0.4622 0.018 Uiso 1 1 calc R . .
C6 C 0.3870(3) 0.8583(3) 0.4038(2) 0.0128(5) Uani 1 1 d . . .
H6A H 0.3516 0.9152 0.4737 0.015 Uiso 1 1 calc R . .
H6B H 0.4431 0.9361 0.3496 0.015 Uiso 1 1 calc R . .
C7 C 0.1500(3) 0.9445(3) 0.3110(2) 0.0129(5) Uani 1 1 d . . .
H7A H 0.1252 1.0144 0.3760 0.015 Uiso 1 1 calc R . .
H7B H 0.0458 0.9077 0.2874 0.015 Uiso 1 1 calc R . .
C8 C 0.2313(3) 1.0452(3) 0.2134(2) 0.0133(5) Uani 1 1 d . . .
H8A H 0.3385 1.0774 0.2345 0.016 Uiso 1 1 calc R . .
H8B H 0.1666 1.1435 0.2036 0.016 Uiso 1 1 calc R . .
C9 C 0.2538(3) 0.9646(3) 0.0998(2) 0.0135(5) Uani 1 1 d . . .
H9A H 0.1479 0.9279 0.0793 0.016 Uiso 1 1 calc R . .
H9B H 0.2961 1.0429 0.0402 0.016 Uiso 1 1 calc R . .
C10 C 0.1301(3) 0.7294(3) 0.4481(2) 0.0160(5) Uani 1 1 d . . .
H10A H 0.1838 0.6382 0.4832 0.024 Uiso 1 1 calc R . .
H10B H 0.0310 0.6939 0.4182 0.024 Uiso 1 1 calc R . .
H10C H 0.1037 0.8095 0.5052 0.024 Uiso 1 1 calc R . .
P1 P 0.73784(8) 0.18263(8) 0.21950(6) 0.01156(12) Uani 1 1 d . . .
F1 F 0.6903(2) 0.3095(2) 0.12176(15) 0.0198(4) Uani 1 1 d . . .
F2 F 0.8895(2) 0.1263(2) 0.13932(16) 0.0231(4) Uani 1 1 d . . .
F3 F 0.7792(2) 0.0556(2) 0.31738(15) 0.0201(4) Uani 1 1 d . . .
F4 F 0.5806(2) 0.2383(2) 0.29889(15) 0.0197(4) Uani 1 1 d . . .
F5 F 0.6285(2) 0.0510(2) 0.16615(15) 0.0178(3) Uani 1 1 d . . .
F6 F 0.8418(2) 0.3145(2) 0.27254(16) 0.0249(4) 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'
P P 0.1023 0.0942 '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
C2 Re1 C3 88.60(11) . . ?
C2 Re1 C1 88.04(11) . . ?
C3 Re1 C1 89.13(12) . . ?
C2 Re1 N3 94.29(10) . . ?
C3 Re1 N3 175.89(10) . . ?
C1 Re1 N3 93.89(10) . . ?
C2 Re1 N1 88.79(10) . . ?
C3 Re1 N1 92.82(11) . . ?
C1 Re1 N1 176.23(10) . . ?
N3 Re1 N1 84.32(9) . . ?
C2 Re1 N2 178.85(10) . . ?
C3 Re1 N2 92.51(10) . . ?
C1 Re1 N2 91.66(10) . . ?
N3 Re1 N2 84.63(8) . . ?
N1 Re1 N2 91.47(8) . . ?
C4 N1 Re1 124.41(17) . . ?
C4 N1 H21N 106(3) . . ?
Re1 N1 H21N 99(3) . . ?
C4 N1 H22N 109(2) . . ?
Re1 N1 H22N 106(2) . . ?
H21N N1 H22N 112(3) . . ?
C10 N2 C6 107.3(2) . . ?
C10 N2 C7 104.6(2) . . ?
C6 N2 C7 107.9(2) . . ?
C10 N2 Re1 108.81(16) . . ?
C6 N2 Re1 115.86(16) . . ?
C7 N2 Re1 111.70(16) . . ?
C9 N3 Re1 116.75(17) . . ?
C9 N3 H31N 111(2) . . ?
Re1 N3 H31N 109(2) . . ?
C9 N3 H32N 111(2) . . ?
Re1 N3 H32N 103(2) . . ?
H31N N3 H32N 105(3) . . ?
O1 C1 Re1 178.8(3) . . ?
O2 C2 Re1 178.2(2) . . ?
O3 C3 Re1 179.1(3) . . ?
N1 C4 C5 112.7(2) . . ?
N1 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
N1 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 C6 113.4(2) . . ?
C4 C5 H5A 108.9 . . ?
C6 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C6 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N2 C6 C5 115.2(2) . . ?
N2 C6 H6A 108.5 . . ?
C5 C6 H6A 108.5 . . ?
N2 C6 H6B 108.5 . . ?
C5 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
N2 C7 C8 117.7(2) . . ?
N2 C7 H7A 107.9 . . ?
C8 C7 H7A 107.9 . . ?
N2 C7 H7B 107.9 . . ?
C8 C7 H7B 107.9 . . ?
H7A C7 H7B 107.2 . . ?
C7 C8 C9 115.3(2) . . ?
C7 C8 H8A 108.5 . . ?
C9 C8 H8A 108.5 . . ?
C7 C8 H8B 108.5 . . ?
C9 C8 H8B 108.5 . . ?
H8A C8 H8B 107.5 . . ?
N3 C9 C8 112.0(2) . . ?
N3 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
N3 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
N2 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
F2 P1 F6 91.48(11) . . ?
F2 P1 F3 91.25(11) . . ?
F6 P1 F3 90.81(10) . . ?
F2 P1 F1 90.13(10) . . ?
F6 P1 F1 90.27(10) . . ?
F3 P1 F1 178.22(11) . . ?
F2 P1 F4 178.58(11) . . ?
F6 P1 F4 89.80(11) . . ?
F3 P1 F4 89.34(10) . . ?
F1 P1 F4 89.26(10) . . ?
F2 P1 F5 89.66(10) . . ?
F6 P1 F5 178.71(11) . . ?
F3 P1 F5 89.77(10) . . ?
F1 P1 F5 89.12(10) . . ?
F4 P1 F5 89.05(10) . . ?
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 1.914(3) . ?
Re1 C3 1.914(3) . ?
Re1 C1 1.917(3) . ?
Re1 N3 2.226(2) . ?
Re1 N1 2.249(2) . ?
Re1 N2 2.299(2) . ?
O1 C1 1.159(3) . ?
O2 C2 1.157(3) . ?
O3 C3 1.157(3) . ?
N1 C4 1.496(4) . ?
N1 H21N 0.81(4) . ?
N1 H22N 0.90(4) . ?
N2 C10 1.500(3) . ?
N2 C6 1.501(3) . ?
N2 C7 1.507(4) . ?
N3 C9 1.498(4) . ?
N3 H31N 0.86(4) . ?
N3 H32N 0.94(4) . ?
C4 C5 1.519(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.521(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.520(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.521(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
P1 F2 1.5896(18) . ?
P1 F6 1.5931(19) . ?
P1 F3 1.6019(19) . ?
P1 F1 1.6145(19) . ?
P1 F4 1.6180(18) . ?
P1 F5 1.6198(18) . ?
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
N1 H21N F4 0.81(4) 2.25(4) 3.051(3) 169(4) .
N1 H22N O2 0.90(4) 2.43(4) 3.282(3) 158(3) 2_665
N3 H31N F5 0.86(4) 2.28(4) 3.059(3) 150(3) 1_565
N3 H32N F1 0.94(4) 2.13(4) 3.005(3) 154(3) 2_665
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 C4 179.0(2) . . . . ?
C3 Re1 N1 C4 -92.5(2) . . . . ?
N3 Re1 N1 C4 84.6(2) . . . . ?
N2 Re1 N1 C4 0.1(2) . . . . ?
C3 Re1 N2 C10 -20.64(19) . . . . ?
C1 Re1 N2 C10 68.57(19) . . . . ?
N3 Re1 N2 C10 162.32(18) . . . . ?
N1 Re1 N2 C10 -113.52(18) . . . . ?
C3 Re1 N2 C6 100.24(19) . . . . ?
C1 Re1 N2 C6 -170.55(19) . . . . ?
N3 Re1 N2 C6 -76.80(18) . . . . ?
N1 Re1 N2 C6 7.36(19) . . . . ?
C3 Re1 N2 C7 -135.63(18) . . . . ?
C1 Re1 N2 C7 -46.42(18) . . . . ?
N3 Re1 N2 C7 47.33(17) . . . . ?
N1 Re1 N2 C7 131.49(17) . . . . ?
C2 Re1 N3 C9 127.4(2) . . . . ?
C1 Re1 N3 C9 39.1(2) . . . . ?
N1 Re1 N3 C9 -144.26(19) . . . . ?
N2 Re1 N3 C9 -52.24(19) . . . . ?
Re1 N1 C4 C5 27.7(3) . . . . ?
N1 C4 C5 C6 -71.5(3) . . . . ?
C10 N2 C6 C5 77.0(3) . . . . ?
C7 N2 C6 C5 -170.7(2) . . . . ?
Re1 N2 C6 C5 -44.7(3) . . . . ?
C4 C5 C6 N2 84.8(3) . . . . ?
C10 N2 C7 C8 179.6(2) . . . . ?
C6 N2 C7 C8 65.6(3) . . . . ?
Re1 N2 C7 C8 -62.9(3) . . . . ?
N2 C7 C8 C9 67.3(3) . . . . ?
Re1 N3 C9 C8 66.6(3) . . . . ?
C7 C8 C9 N3 -65.2(3) . . . . ?
