#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179278 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/98/4319876.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_4319876
loop_
_publ_author_name
'Yi Han'
'C. Jeff Harlan'
'Philipp Stoessel'
'Brian J. Frost'
'Jack R. Norton'
'Susie Miller'
'Brian Bridgewater'
'Qiang Xu'
_publ_section_title
;
 Rhenium Oxo Complexes of a Chelating Diyne Ligand. Synthesis and Study of
 the Kinetics of Protonation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2942
_journal_page_last               2952
_journal_paper_doi               10.1021/ic0100931
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C15 H21 B2 F8 I N3 Re'
_chemical_formula_weight         730.07
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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            8
_cell_length_a                   23.889(2)
_cell_length_b                   23.889(2)
_cell_length_c                   9.7525(11)
_cell_measurement_temperature    228(2)
_cell_volume                     5565.6(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      228(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1264
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            18516
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         1.21
_exptl_absorpt_coefficient_mu    5.534
_exptl_absorpt_correction_T_max  0.4041
_exptl_absorpt_correction_T_min  0.2876
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.869
_refine_diff_density_min         -2.232
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       0.00000(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          1.447
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1047P)²+54.8483P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1932
_reflns_number_gt                2591
_reflns_number_total             3438
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0100931_3.cif
_cod_data_source_block           res10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_database_code               4319876
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Re Re 0.004320(19) 0.246471(19) 0.0000 0.0418(2) Uani 1 2 d S . .
I I 0.02493(4) 0.13304(4) 0.0000 0.0685(4) Uani 1 2 d S . .
N1 N 0.0261(4) 0.3310(5) 0.0000 0.048(2) Uani 1 2 d S . .
N2 N 0.0752(3) 0.2442(3) -0.1413(9) 0.0509(18) Uani 1 1 d . . .
C1 C -0.0417(5) 0.3193(5) 0.2631(12) 0.066(3) Uani 1 1 d . . .
H1A H -0.0589 0.3508 0.2163 0.099 Uiso 1 1 calc R . .
H1B H -0.0044 0.3297 0.2929 0.099 Uiso 1 1 calc R . .
H1C H -0.0642 0.3092 0.3422 0.099 Uiso 1 1 calc R . .
C2 C -0.0382(4) 0.2716(4) 0.1694(10) 0.049(2) Uani 1 1 d . . .
C3 C -0.0564(4) 0.2235(4) 0.1332(11) 0.053(2) Uani 1 1 d . . .
C4 C -0.1026(5) 0.1803(5) 0.1331(13) 0.066(3) Uani 1 1 d . . .
H4A H -0.1267 0.1855 0.2135 0.080 Uiso 1 1 calc R . .
H4B H -0.0865 0.1426 0.1368 0.080 Uiso 1 1 calc R . .
C5 C -0.1372(7) 0.1875(7) 0.0000 0.078(5) Uani 1 2 d S . .
H5A H -0.1542 0.2249 0.0000 0.094 Uiso 1 2 calc SR . .
H5B H -0.1677 0.1600 0.0000 0.094 Uiso 1 2 calc SR . .
C11 C 0.0584(9) 0.4327(7) 0.0000 0.097(7) Uani 1 2 d S . .
H11A H 0.0370 0.4532 -0.0680 0.145 Uiso 0.50 1 calc PR . .
H11B H 0.0980 0.4351 -0.0220 0.145 Uiso 0.50 1 calc PR . .
H11C H 0.0519 0.4487 0.0899 0.145 Uiso 0.50 1 calc PR . .
C12 C 0.0411(6) 0.3741(6) 0.0000 0.059(4) Uani 1 2 d S . .
C21 C 0.1598(5) 0.2609(6) -0.3001(11) 0.073(3) Uani 1 1 d . . .
H21A H 0.1535 0.2943 -0.3543 0.109 Uiso 1 1 calc R . .
H21B H 0.1645 0.2290 -0.3606 0.109 Uiso 1 1 calc R . .
H21C H 0.1932 0.2656 -0.2450 0.109 Uiso 1 1 calc R . .
C22 C 0.1121(4) 0.2514(4) -0.2111(10) 0.050(2) Uani 1 1 d . . .
F11 F 0.2501(5) 0.3433(4) -0.1181(13) 0.137(4) Uani 1 1 d . . .
F12 F 0.1694(5) 0.3417(6) 0.0000 0.100(4) Uani 1 2 d S . .
F13 F 0.2258(6) 0.2672(4) 0.0000 0.098(4) Uani 1 2 d S . .
F21 F 0.1706(6) 0.5655(6) 0.0000 0.117(5) Uani 1 2 d S . .
F22 F 0.0857(6) 0.5633(5) 0.104(2) 0.208(8) Uani 1 1 d . . .
F23 F 0.1176(5) 0.6411(5) 0.0000 0.098(4) Uani 1 2 d S . .
B1 B 0.2257(8) 0.3233(8) 0.0000 0.062(4) Uani 1 2 d S . .
B2 B 0.1184(10) 0.5822(9) 0.0000 0.088(7) 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'
B B 0.0013 0.0007 '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'
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'
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
C3 Re C3 79.9(6) 10 . ?
C3 Re C2 36.7(4) 10 10 ?
C3 Re C2 104.1(4) . 10 ?
C3 Re C2 104.1(4) 10 . ?
C3 Re C2 36.7(4) . . ?
C2 Re C2 108.9(5) 10 . ?
C3 Re N1 116.2(3) 10 . ?
C3 Re N1 116.2(3) . . ?
C2 Re N1 80.7(3) 10 . ?
C2 Re N1 80.7(3) . . ?
C3 Re N2 162.6(4) 10 10 ?
C3 Re N2 98.3(4) . 10 ?
C2 Re N2 155.4(3) 10 10 ?
C2 Re N2 83.2(3) . 10 ?
N1 Re N2 80.2(3) . 10 ?
C3 Re N2 98.3(4) 10 . ?
C3 Re N2 162.6(4) . . ?
C2 Re N2 83.2(3) 10 . ?
C2 Re N2 155.4(3) . . ?
N1 Re N2 80.2(3) . . ?
N2 Re N2 78.2(4) 10 . ?
C3 Re I 82.0(3) 10 . ?
C3 Re I 82.0(3) . . ?
C2 Re I 112.3(3) 10 . ?
C2 Re I 112.3(3) . . ?
N1 Re I 155.2(3) . . ?
N2 Re I 80.6(2) 10 . ?
N2 Re I 80.6(2) . . ?
C12 N1 Re 175.4(11) . . ?
C22 N2 Re 169.7(8) . . ?
C3 C2 C1 148.6(10) . . ?
C3 C2 Re 71.3(6) . . ?
C1 C2 Re 140.1(7) . . ?
C2 C3 C4 149.6(10) . . ?
C2 C3 Re 71.9(6) . . ?
C4 C3 Re 135.1(8) . . ?
C3 C4 C5 108.4(10) . . ?
C4 C5 C4 113.8(13) . 10 ?
N1 C12 C11 177.4(17) . . ?
N2 C22 C21 179.6(13) . . ?
F13 B1 F11 110.3(10) . 10 ?
F13 B1 F11 110.3(10) . . ?
F11 B1 F11 113.6(18) 10 . ?
F13 B1 F12 108.2(16) . . ?
F11 B1 F12 107.1(10) 10 . ?
F11 B1 F12 107.1(10) . . ?
F21 B2 F22 116.6(14) . 10 ?
F21 B2 F22 116.6(14) . . ?
F22 B2 F22 97(2) 10 . ?
F21 B2 F23 108.5(19) . . ?
F22 B2 F23 109.0(13) 10 . ?
F22 B2 F23 109.0(13) . . ?
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
Re C3 2.023(10) 10 ?
Re C3 2.023(10) . ?
Re C2 2.030(10) 10 ?
Re C2 2.030(10) . ?
Re N1 2.085(11) . ?
Re N2 2.185(8) 10 ?
Re N2 2.185(8) . ?
Re I 2.7540(11) . ?
N1 C12 1.090(18) . ?
N2 C22 1.127(12) . ?
C1 C2 1.465(14) . ?
C2 C3 1.277(13) . ?
C3 C4 1.511(13) . ?
C4 C5 1.549(15) . ?
C5 C4 1.549(15) 10 ?
C11 C12 1.46(2) . ?
C21 C22 1.449(14) . ?
F11 B1 1.376(15) . ?
F12 B1 1.41(2) . ?
F13 B1 1.34(2) . ?
F21 B2 1.31(3) . ?
F22 B2 1.35(2) . ?
F23 B2 1.41(2) . ?
B1 F11 1.376(15) 10 ?
B2 F22 1.35(2) 10 ?
