#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:21:06 +0100 (lun 21 de mar de 2016) $
#$Revision: 178779 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/33/4103316.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_4103316
loop_
_publ_author_name
'Elsa Quartapelle Procopio'
'Matteo Mauro'
'Monica Panigati'
'Daniela Donghi'
'Pierluigi Mercandelli'
'Angelo Sironi'
'Giuseppe D'Alfonso'
'Luisa De Cola'
_publ_section_title
;
 Highly Emitting Concomitant Polymorphic Crystals of a Dinuclear Rhenium
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14397
_journal_page_last               14399
_journal_paper_doi               10.1021/ja106772v
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C16 H20 Cl2 N2 O6 Re2 Si2'
_chemical_formula_sum            'C16 H20 Cl2 N2 O6 Re2 Si2'
_chemical_formula_weight         835.82
_chemical_name_systematic
;
hexacarbonyldi-μ-chloro(μ-4,5-bis(trimethylsilyl)pyridazine-\kN1:\kN2)
dirhenium
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 101.80(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.990(2)
_cell_length_b                   12.734(2)
_cell_length_c                   18.542(2)
_cell_measurement_reflns_used    8191
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.5
_cell_volume                     2540.1(7)
_computing_structure_refinement
;
Sheldrick, G. M. (1997). SHELX97. Universität Göttingen, Germany.
;
_computing_structure_solution
;
SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L.,
Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. &
Spagna, R. (1999). J. Appl. Crystallogr. 32, 115-119.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
A full sphere of reciprocal space was scanned by 0.3° ω steps, collecting
2400 frames each at 10 s exposure keeping the detector at 6.6 cm from the
sample. Intensity decay was monitored by recollecting the initial 50 frames
at the end of data collection and analysing the duplicate reflections.
;
_diffrn_measurement_device_type  'Brucker APEX II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19242
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.859
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.258
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996). SADABS. Universität Göttingen, Germany.
Reflections employed for parameter determination: 13714
Maximum odd and even orders for spherical harmonics: 7 and 8
Effective data to parameter ratio: 4.8
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1560
_exptl_crystal_preparation
;
Crystals were obtained by slow diffusion of n-hexane in a dichloromethane
solution at 248 K.
;
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.015P)²+4.1P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0348
_refine_ls_wR_factor_ref         0.0359
_reflns_number_gt                2760
_reflns_number_total             3042
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja106772v_si_002.cif
_cod_data_source_block           1yellow
_cod_database_code               4103316
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
Re1 Re 0.160969(9) 0.644379(9) 0.908731(6) 0.01250(4) Uani 1 1 d .
C1 C 0.1249(2) 0.7818(2) 0.86623(16) 0.0172(6) Uani 1 1 d .
C2 C 0.1989(3) 0.6022(2) 0.81741(17) 0.0188(6) Uani 1 1 d .
C3 C -0.0065(3) 0.6047(2) 0.87173(17) 0.0176(6) Uani 1 1 d .
C4 C 0.1820(2) 0.4026(2) 0.93341(16) 0.0145(6) Uani 1 1 d .
H1 H 0.1322 0.4044 0.8851 0.017 Uiso 1 1 calc R
C5 C 0.2140(2) 0.3030(2) 0.96401(15) 0.0136(6) Uani 1 1 d .
C6 C 0.0479(3) 0.2389(3) 0.81789(17) 0.0256(7) Uani 1 1 d .
H2 H 0.0159 0.1807 0.7848 0.038 Uiso 1 1 calc R
H3 H 0.0890 0.2901 0.7914 0.038 Uiso 1 1 calc R
H4 H -0.0212 0.2729 0.8349 0.038 Uiso 1 1 calc R
C7 C 0.3005(3) 0.1409(3) 0.8650(2) 0.0290(8) Uani 1 1 d .
H5 H 0.3665 0.1227 0.9071 0.043 Uiso 1 1 calc R
H6 H 0.3297 0.1967 0.8362 0.043 Uiso 1 1 calc R
H7 H 0.2783 0.0789 0.8338 0.043 Uiso 1 1 calc R
C8 C 0.0848(3) 0.0819(2) 0.94265(19) 0.0257(7) Uani 1 1 d .
H8 H 0.0431 0.0329 0.9048 0.038 Uiso 1 1 calc R
H9 H 0.0234 0.1132 0.9679 0.038 Uiso 1 1 calc R
H10 H 0.1475 0.0441 0.9785 0.038 Uiso 1 1 calc R
N1 N 0.21468(19) 0.49469(19) 0.96566(12) 0.0130(5) Uani 1 1 d .
O1 O 0.1055(2) 0.86369(17) 0.84142(13) 0.0266(5) Uani 1 1 d .
O2 O 0.2179(2) 0.57819(19) 0.76084(12) 0.0292(5) Uani 1 1 d .
O3 O -0.10854(19) 0.58105(19) 0.84894(12) 0.0271(5) Uani 1 1 d .
Si1 Si 0.16160(7) 0.18765(7) 0.89860(5) 0.01795(18) Uani 1 1 d .
Cl1 Cl 0.37789(6) 0.69392(6) 0.96784(4) 0.01678(14) Uani 1 1 d .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.01299(6) 0.01138(6) 0.01339(6) 0.00099(5) 0.00330(4) 0.00089(4)
C1 0.0161(13) 0.0173(16) 0.0183(16) -0.0014(13) 0.0041(11) -0.0003(11)
C2 0.0190(14) 0.0151(15) 0.0223(18) 0.0069(13) 0.0043(12) 0.0029(11)
C3 0.0216(15) 0.0141(15) 0.0187(16) 0.0005(13) 0.0080(12) 0.0008(11)
C4 0.0147(13) 0.0180(16) 0.0110(14) -0.0006(12) 0.0035(10) -0.0015(11)
C5 0.0125(12) 0.0133(15) 0.0161(15) -0.0016(12) 0.0057(10) -0.0020(10)
C6 0.0322(16) 0.0244(19) 0.0200(18) -0.0074(14) 0.0052(13) -0.0074(14)
C7 0.0306(17) 0.0272(19) 0.035(2) -0.0085(16) 0.0203(15) -0.0029(14)
C8 0.0267(16) 0.0156(17) 0.037(2) -0.0043(15) 0.0124(14) -0.0064(12)
N1 0.0126(10) 0.0140(13) 0.0125(13) 0.0011(10) 0.0028(9) 0.0007(9)
O1 0.0338(12) 0.0156(13) 0.0313(14) 0.0049(10) 0.0092(10) 0.0054(9)
O2 0.0377(13) 0.0339(15) 0.0181(13) 0.0014(11) 0.0103(10) 0.0105(11)
O3 0.0189(11) 0.0326(15) 0.0287(13) -0.0017(11) 0.0025(9) -0.0052(9)
Si1 0.0207(4) 0.0143(4) 0.0207(5) -0.0048(4) 0.0085(3) -0.0034(3)
Cl1 0.0149(3) 0.0193(4) 0.0169(4) 0.0018(3) 0.0051(2) -0.0026(3)
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'
Si Si 0.0817 0.0704 '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'
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
C1 Re1 C2 87.55(13) . .
C1 Re1 C3 89.46(12) . .
C1 Re1 N1 174.60(10) . .
C1 Re1 Cl1 92.77(8) . .
C1 Re1 Cl1 94.93(9) . 2_557
C2 Re1 C3 88.60(13) . .
C2 Re1 N1 95.51(11) . .
C2 Re1 Cl1 95.68(9) . .
C2 Re1 Cl1 176.66(9) . 2_557
C3 Re1 N1 95.05(11) . .
C3 Re1 Cl1 175.25(9) . .
C3 Re1 Cl1 93.66(9) . 2_557
N1 Re1 Cl1 82.52(6) . .
N1 Re1 Cl1 81.85(6) . 2_557
Cl1 Re1 Cl1 81.98(3) . 2_557
Re1 C1 O1 178.8(3) . .
Re1 C2 O2 177.5(3) . .
Re1 C3 O3 179.6(3) . .
C5 C4 N1 126.2(3) . .
C4 C5 C5 115.44(16) . 2_557
C4 C5 Si1 114.7(2) . .
C5 C5 Si1 129.70(9) 2_557 .
Re1 N1 C4 121.73(18) . .
Re1 N1 N1 119.93(6) . 2_557
C4 N1 N1 118.31(16) . 2_557
C5 Si1 C6 107.79(14) . .
C5 Si1 C7 107.24(14) . .
C5 Si1 C8 112.35(14) . .
C6 Si1 C7 107.76(16) . .
C6 Si1 C8 108.44(15) . .
C7 Si1 C8 113.05(16) . .
Re1 Cl1 Re1 90.66(2) . 2_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Re1 C1 1.927(3) .
Re1 C2 1.903(3) .
Re1 C3 1.897(3) .
Re1 N1 2.201(2) .
Re1 Cl1 2.4928(8) .
Re1 Cl1 2.4936(9) 2_557
C1 O1 1.142(4) .
C2 O2 1.151(4) .
C3 O3 1.154(3) .
C4 N1 1.332(4) .
C4 C5 1.404(4) .
C5 C5 1.406(5) 2_557
C5 Si1 1.917(3) .
C6 Si1 1.861(3) .
C7 Si1 1.860(3) .
C8 Si1 1.864(3) .
N1 N1 1.349(4) 2_557
