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#$Date: 2016-03-26 00:24:52 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180077 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/23/7052343.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_7052343
loop_
_publ_author_name
'Jorge S. Gancheff'
'Carlos Kremer'
'Oscar N. Ventura'
'Sixto Domínguez'
'Carla Bazzicalupi'
'Antonio Bianchi'
'Leopoldo Suescun'
'Alvaro W. Mombrú'
_publ_section_title
;
 ReO<small>₂</small><small>⁺</small> chelates
 with aliphatic diamines. Structural and proton transfer properties
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1650
_journal_paper_doi               10.1039/b606797b
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C12 H36 I N4 O4 Re'
_chemical_formula_weight         613.56
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 128.293(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8941(17)
_cell_length_b                   19.078(4)
_cell_length_c                   10.2235(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.75
_cell_measurement_theta_min      10.16
_cell_volume                     2126.9(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Software, 1993'
_computing_data_collection       'MSC/AFC Diffractometer Software, 1993'
_computing_data_reduction        'MSC/AFC Diffractometer Software, 1993'
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1995)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0836
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2915
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    7.184
_exptl_absorpt_correction_T_max  0.6332
_exptl_absorpt_correction_T_min  0.2888
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'MSC/AFC Diffractometer Software (1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.915
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.161
_refine_diff_density_min         -2.359
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       0.00073(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0709P)²+6.4164P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1335
_reflns_number_gt                1909
_reflns_number_total             2451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606797b.txt
_cod_data_source_block           jg01
_cod_database_code               7052343
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'
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 0.6771(9) 0.6874(5) 0.1807(12) 0.055(2) Uani 1 1 d . . .
H1A H 0.7601 0.6851 0.2166 0.066 Uiso 1 1 calc R . .
H1B H 0.6205 0.6826 0.0604 0.066 Uiso 1 1 calc R . .
C2 C 0.6565(8) 0.6294(4) 0.2610(10) 0.0499(18) Uani 1 1 d . . .
H2A H 0.5725 0.6307 0.2214 0.060 Uiso 1 1 calc R . .
H2B H 0.6705 0.5843 0.2315 0.060 Uiso 1 1 calc R . .
C3 C 0.6889(9) 0.8156(5) 0.1718(11) 0.053(2) Uani 1 1 d . . .
H3A H 0.7759 0.8135 0.2259 0.064 Uiso 1 1 calc R . .
H3B H 0.6738 0.8589 0.2062 0.064 Uiso 1 1 calc R . .
C4 C 0.6192(10) 0.8179(6) -0.0142(12) 0.068(2) Uani 1 1 d . . .
H4A H 0.6453 0.8578 -0.0423 0.101 Uiso 1 1 calc R . .
H4B H 0.5330 0.8214 -0.0692 0.101 Uiso 1 1 calc R . .
H4C H 0.6351 0.7758 -0.0496 0.101 Uiso 1 1 calc R . .
C5 C 0.8616(8) 0.6038(5) 0.5223(13) 0.062(2) Uani 1 1 d . . .
H5A H 0.9170 0.6171 0.6390 0.075 Uiso 1 1 calc R . .
H5B H 0.8959 0.6214 0.4700 0.075 Uiso 1 1 calc R . .
C6 C 0.8567(11) 0.5256(6) 0.511(2) 0.097(4) Uani 1 1 d . . .
H6A H 0.9377 0.5076 0.5644 0.145 Uiso 1 1 calc R . .
H6B H 0.8039 0.5117 0.3961 0.145 Uiso 1 1 calc R . .
H6C H 0.8254 0.5074 0.5657 0.145 Uiso 1 1 calc R . .
N1 N 0.6569(7) 0.7555(3) 0.2317(9) 0.0396(14) Uani 1 1 d . . .
H1 H 0.5751 0.7587 0.1796 0.047 Uiso 1 1 calc R . .
N2 N 0.7419(5) 0.6385(3) 0.4440(8) 0.0406(13) Uani 1 1 d . . .
H2 H 0.7070 0.6166 0.4843 0.049 Uiso 1 1 calc R . .
O1 O 0.8930(5) 0.7568(2) 0.5405(7) 0.0383(11) Uani 1 1 d . . .
O1W O 0.6444(8) 0.5461(4) 0.5669(11) 0.077(2) Uani 1 1 d . . .
I2 I 0.5000 0.58346(5) 0.7500 0.0645(3) Uani 1 2 d S . .
Re1 Re 0.7500 0.7500 0.5000 0.03396(18) Uani 1 2 d S . .
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'
I I -0.4742 1.8119 '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
N1 C1 C2 108.0(6) . . ?
N1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 . . ?
N1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 . . ?
H1A C1 H1B 108.4 . . ?
N2 C2 C1 109.2(7) . . ?
N2 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N2 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
N1 C3 C4 114.7(8) . . ?
N1 C3 H3A 108.6 . . ?
C4 C3 H3A 108.6 . . ?
N1 C3 H3B 108.6 . . ?
C4 C3 H3B 108.6 . . ?
H3A C3 H3B 107.6 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 C6 115.0(8) . . ?
N2 C5 H5A 108.5 . . ?
C6 C5 H5A 108.5 . . ?
N2 C5 H5B 108.5 . . ?
C6 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 N1 C3 111.0(7) . . ?
C1 N1 Re1 107.6(5) . . ?
C3 N1 Re1 117.1(5) . . ?
C1 N1 H1 106.9 . . ?
C3 N1 H1 106.9 . . ?
Re1 N1 H1 106.9 . . ?
C2 N2 C5 112.5(6) . . ?
C2 N2 Re1 108.5(5) . . ?
C5 N2 Re1 115.8(5) . . ?
C2 N2 H2 106.5 . . ?
C5 N2 H2 106.5 . . ?
Re1 N2 H2 106.5 . . ?
O1 Re1 O1 180.0(4) . 7_666 ?
O1 Re1 N2 90.0(2) . 7_666 ?
O1 Re1 N2 90.0(2) 7_666 7_666 ?
O1 Re1 N2 90.0(2) . . ?
O1 Re1 N2 90.0(2) 7_666 . ?
N2 Re1 N2 180.000(1) 7_666 . ?
O1 Re1 N1 90.3(3) . 7_666 ?
O1 Re1 N1 89.7(3) 7_666 7_666 ?
N2 Re1 N1 79.9(2) 7_666 7_666 ?
N2 Re1 N1 100.1(2) . 7_666 ?
O1 Re1 N1 89.7(3) . . ?
O1 Re1 N1 90.3(3) 7_666 . ?
N2 Re1 N1 100.1(2) 7_666 . ?
N2 Re1 N1 79.9(2) . . ?
N1 Re1 N1 180.000(1) 7_666 . ?
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 N1 1.491(10) . ?
C1 C2 1.507(13) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.479(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.491(10) . ?
C3 C4 1.508(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 N2 1.482(10) . ?
C5 C6 1.494(15) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
N1 Re1 2.193(7) . ?
N1 H1 0.9100 . ?
N2 Re1 2.187(6) . ?
N2 H2 0.9100 . ?
O1 Re1 1.766(5) . ?
Re1 O1 1.766(5) 7_666 ?
Re1 N2 2.187(6) 7_666 ?
Re1 N1 2.193(7) 7_666 ?
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
N1 C1 C2 N2 -58.5(9) . . . . ?
C2 C1 N1 C3 173.9(7) . . . . ?
C2 C1 N1 Re1 44.5(8) . . . . ?
C4 C3 N1 C1 57.7(11) . . . . ?
C4 C3 N1 Re1 -178.2(6) . . . . ?
C1 C2 N2 C5 -87.9(8) . . . . ?
C1 C2 N2 Re1 41.4(7) . . . . ?
C6 C5 N2 C2 -66.1(12) . . . . ?
C6 C5 N2 Re1 168.4(9) . . . . ?
C2 N2 Re1 O1 -102.7(5) . . . . ?
C5 N2 Re1 O1 24.8(6) . . . . ?
C2 N2 Re1 O1 77.3(5) . . . 7_666 ?
C5 N2 Re1 O1 -155.2(6) . . . 7_666 ?
C2 N2 Re1 N2 68(100) . . . 7_666 ?
C5 N2 Re1 N2 -164(100) . . . 7_666 ?
C2 N2 Re1 N1 167.0(5) . . . 7_666 ?
C5 N2 Re1 N1 -65.5(6) . . . 7_666 ?
C2 N2 Re1 N1 -13.0(5) . . . . ?
C5 N2 Re1 N1 114.5(6) . . . . ?
C1 N1 Re1 O1 72.8(5) . . . . ?
C3 N1 Re1 O1 -52.9(6) . . . . ?
C1 N1 Re1 O1 -107.2(5) . . . 7_666 ?
C3 N1 Re1 O1 127.1(6) . . . 7_666 ?
C1 N1 Re1 N2 162.7(5) . . . 7_666 ?
C3 N1 Re1 N2 37.0(6) . . . 7_666 ?
C1 N1 Re1 N2 -17.3(5) . . . . ?
C3 N1 Re1 N2 -143.0(6) . . . . ?
C1 N1 Re1 N1 5(100) . . . 7_666 ?
C3 N1 Re1 N1 -121(100) . . . 7_666 ?
