#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:07:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179277 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/97/4319712.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_4319712
loop_
_publ_author_name
'Xiaoyuan Chen'
'Frank J. Femia'
'John W. Babich'
'Jon A. Zubieta'
_publ_section_title
;
 Rhenium(I) Carbonyl Complexes of 2,4,6-Tris(2-pyridyl)-1,3,5-triazine
 (TPT). Rhenium(I)-Promoted Methoxylation of the Triazine Ring Carbon Atom
 in Dinuclear Rhenium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2769
_journal_page_last               2777
_journal_paper_doi               10.1021/ic000446g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C25 H15 Br2 Cl2 N6 O7 Re2'
_chemical_formula_weight         1114.55
_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                 111.179(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.555(4)
_cell_length_b                   15.277(3)
_cell_length_c                   13.093(3)
_cell_measurement_temperature    90(2)
_cell_volume                     3274.2(12)
_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      90(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10653
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    10.042
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.885
_refine_diff_density_min         -2.614
_refine_diff_density_rms         0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0651P)²+29.9910P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                3271
_reflns_number_total             3939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000446g_5.cif
_cod_data_source_block           (mu-TPT)[ReBr(CO)3]2CH2Cl20.5H2O_(4')
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        3274.1(12)
_cod_database_code               4319712
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
Re1 Re 0.328115(16) 0.459664(18) 0.04254(2) 0.01870(12) Uani 1 1 d . . .
Br1 Br 0.26067(5) 0.52953(5) 0.17070(7) 0.0299(2) Uani 1 1 d . . .
O3 O 0.1629(4) 0.4261(5) -0.1371(5) 0.0410(15) Uani 1 1 d . . .
O2 O 0.3082(4) 0.2766(4) 0.1286(5) 0.0335(13) Uani 1 1 d . . .
O1 O 0.4151(4) 0.3786(5) -0.0972(5) 0.0486(18) Uani 1 1 d . . .
N1 N 0.3380(4) 0.5949(4) -0.0044(5) 0.0210(12) Uani 1 1 d . . .
N2 N 0.4411(4) 0.5104(4) 0.1695(5) 0.0188(12) Uani 1 1 d . . .
N3 N 0.5000 0.6452(6) 0.2500 0.0194(17) Uani 1 2 d S . .
C4 C 0.3937(5) 0.7356(5) 0.0648(6) 0.0256(16) Uani 1 1 d . . .
H4 H 0.4292 0.7694 0.1211 0.031 Uiso 1 1 calc R . .
C8 C 0.5000 0.3709(7) 0.2500 0.022(2) Uani 1 2 d S . .
C14 C 0.2251(5) 0.4372(5) -0.0701(6) 0.0265(16) Uani 1 1 d . . .
C1 C 0.2907(5) 0.6332(5) -0.0974(6) 0.0243(16) Uani 1 1 d . . .
H1 H 0.2554 0.5988 -0.1530 0.029 Uiso 1 1 calc R . .
C7 C 0.5000 0.4680(7) 0.2500 0.021(2) Uani 1 2 d S . .
C9 C 0.5146(4) 0.3299(5) 0.1668(6) 0.0251(15) Uani 1.08 1 d P . .
H9 H 0.5243 0.3608 0.1116 0.030 Uiso 1.08 1 calc PR . .
C6 C 0.4461(4) 0.5984(5) 0.1715(6) 0.0197(14) Uani 1 1 d . . .
C5 C 0.3904(4) 0.6457(5) 0.0757(6) 0.0216(15) Uani 1 1 d . . .
C13 C 0.3181(5) 0.3453(5) 0.0977(6) 0.0243(16) Uani 1 1 d . . .
C10 C 0.5139(5) 0.2396(6) 0.1691(8) 0.037(2) Uani 1 1 d . . .
H10 H 0.5234 0.2090 0.1134 0.044 Uiso 1 1 calc R . .
C12 C 0.3824(6) 0.4103(6) -0.0476(6) 0.034(2) Uani 1 1 d . . .
C11 C 0.5000 0.1934(9) 0.2500 0.043(3) Uani 1 2 d S . .
H11 H 0.5000 0.1325 0.2500 0.051 Uiso 1 2 calc SR . .
C3 C 0.3431(5) 0.7746(5) -0.0318(6) 0.0262(16) Uani 1 1 d . . .
H3 H 0.3434 0.8349 -0.0408 0.031 Uiso 1 1 calc R . .
C2 C 0.2928(5) 0.7227(5) -0.1134(6) 0.0262(16) Uani 1 1 d . . .
H2 H 0.2599 0.7474 -0.1796 0.031 Uiso 1 1 calc R . .
Cl1S Cl -0.0982(3) 0.6685(4) -0.1448(4) 0.0514(13) Uani 0.50 1 d P . .
Cl2S Cl 0.0265(5) 0.5376(4) -0.0824(11) 0.117(5) Uani 0.50 1 d P . .
C1S C -0.0686(12) 0.5712(18) -0.141(2) 0.076(9) Uani 0.50 1 d P . .
H1S1 H -0.0865 0.5516 -0.2160 0.092 Uiso 0.50 1 calc PR . .
H1S2 H -0.1001 0.5380 -0.1063 0.092 Uiso 0.50 1 calc PR . .
O1S O 0.0000 0.619(3) -0.2500 0.29(2) Uiso 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C14 Re1 C12 89.8(4) . . ?
C14 Re1 C13 86.4(3) . . ?
C12 Re1 C13 90.4(4) . . ?
C14 Re1 N1 95.9(3) . . ?
C12 Re1 N1 95.2(3) . . ?
C13 Re1 N1 174.0(3) . . ?
C14 Re1 N2 169.8(3) . . ?
C12 Re1 N2 95.2(3) . . ?
C13 Re1 N2 102.4(3) . . ?
N1 Re1 N2 74.9(2) . . ?
C14 Re1 Br1 92.7(2) . . ?
C12 Re1 Br1 177.4(3) . . ?
C13 Re1 Br1 90.4(2) . . ?
N1 Re1 Br1 83.93(15) . . ?
N2 Re1 Br1 82.25(16) . . ?
C1 N1 C5 118.5(6) . . ?
C1 N1 Re1 125.9(5) . . ?
C5 N1 Re1 115.1(5) . . ?
C6 N2 C7 116.0(6) . . ?
C6 N2 Re1 113.5(5) . . ?
C7 N2 Re1 130.1(5) . . ?
C6 N3 C6 114.7(9) . 2_655 ?
C5 C4 C3 118.8(7) . . ?
C9 C8 C9 125.0(10) . 2_655 ?
C9 C8 C7 117.5(5) . . ?
C9 C8 C7 117.5(5) 2_655 . ?
O3 C14 Re1 178.1(8) . . ?
N1 C1 C2 121.9(7) . . ?
N2 C7 N2 122.4(9) 2_655 . ?
N2 C7 C8 118.8(5) 2_655 . ?
N2 C7 C8 118.8(5) . . ?
C8 C9 C10 116.0(8) . . ?
N3 C6 N2 125.2(7) . . ?
N3 C6 C5 117.6(7) . . ?
N2 C6 C5 117.1(6) . . ?
N1 C5 C4 121.9(7) . . ?
N1 C5 C6 115.6(6) . . ?
C4 C5 C6 122.4(7) . . ?
O2 C13 Re1 176.8(7) . . ?
C11 C10 C9 122.6(9) . . ?
O1 C12 Re1 177.0(8) . . ?
C10 C11 C10 117.8(12) 2_655 . ?
C2 C3 C4 118.9(7) . . ?
C3 C2 C1 120.0(7) . . ?
Cl1S C1S Cl2S 125.4(15) . . ?
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 C14 1.907(8) . ?
Re1 C12 1.919(9) . ?
Re1 C13 1.923(8) . ?
Re1 N1 2.180(6) . ?
Re1 N2 2.217(6) . ?
Re1 Br1 2.6062(9) . ?
O3 C14 1.139(10) . ?
O2 C13 1.160(10) . ?
O1 C12 1.121(10) . ?
N1 C1 1.335(9) . ?
N1 C5 1.361(9) . ?
N2 C6 1.346(10) . ?
N2 C7 1.347(8) . ?
N3 C6 1.327(8) . ?
N3 C6 1.327(8) 2_655 ?
C4 C5 1.384(10) . ?
C4 C3 1.390(11) . ?
C8 C9 1.358(8) . ?
C8 C9 1.358(8) 2_655 ?
C8 C7 1.483(14) . ?
C1 C2 1.385(11) . ?
C7 N2 1.347(8) 2_655 ?
C9 C10 1.379(12) . ?
C6 C5 1.472(10) . ?
C10 C11 1.367(12) . ?
C11 C10 1.367(12) 2_655 ?
C3 C2 1.366(11) . ?
Cl1S C1S 1.57(3) . ?
Cl2S C1S 1.65(2) . ?
