#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:40:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179388 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/85/4328506.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_4328506
loop_
_publ_author_name
'Alessio Raimondi'
'Monica Panigati'
'Daniela Maggioni'
'Laura D'Alfonso'
'Pierluigi Mercandelli'
'Patrizia Mussini'
'Giuseppe D'Alfonso'
_publ_section_title
;
 Electrochemical, Computational, and Photophysical Characterization of New
 Luminescent Dirhenium-Pyridazine Complexes Containing Bridging OR or SR
 Anions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2966
_journal_page_last               2975
_journal_paper_doi               10.1021/ic202284a
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C22 H14 N2 O6 Re2 S2, C1 H2 Cl2'
_chemical_formula_sum            'C23 H16 Cl2 N2 O6 Re2 S2'
_chemical_formula_weight         923.80
_chemical_name_systematic
;
hexacarbonylbis(μ-benzenethiolato)(μ-pyridazine-\kN1:\kN2)dirhenium
dichloromethane solvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.041(2)
_cell_length_b                   14.442(2)
_cell_length_c                   20.886(2)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      3.3
_cell_volume                     5441.8(11)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
A full sphere of reciprocal space was scanned by 0.5° ω steps, collecting
1440 frames each at 10 s exposure, keeping the detector at 60 mm 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  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0191
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            68104
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    9.281
_exptl_absorpt_correction_T_max  0.224
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Sheldrick, G. M. (1996). SADABS. Universität Göttingen, Germany.
Reflections employed for parameter determination: 49183
Maximum odd and even orders for spherical harmonics: 7 and 8
Effective data to parameter ratio: 28.8
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             3456
_exptl_crystal_preparation
;
Crystals were obtained by slow evaporation of a dichloromethane solution at RT.
;
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0277
_refine_ls_R_factor_gt           0.0231
_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)+(0.025P)²+1.3P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0530
_refine_ls_wR_factor_ref         0.0545
_reflns_number_gt                7133
_reflns_number_total             7883
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic202284a_si_003_1.cif
_cod_data_source_block           2-SPh
_cod_database_code               4328506
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'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 0.390974(6) 0.233938(8) 0.171315(6) 0.01329(3) Uani 1 1 d .
Re2 Re 0.542427(6) 0.364297(8) 0.108863(6) 0.01337(3) Uani 1 1 d .
C1 C 0.30729(19) 0.2129(2) 0.11671(15) 0.0190(6) Uani 1 1 d .
C2 C 0.38832(17) 0.1062(2) 0.19597(15) 0.0167(6) Uani 1 1 d .
C3 C 0.32205(19) 0.2661(2) 0.23762(16) 0.0197(6) Uani 1 1 d .
C4 C 0.53722(19) 0.3964(2) 0.01960(16) 0.0196(6) Uani 1 1 d .
C5 C 0.6420(2) 0.3249(2) 0.09249(16) 0.0208(6) Uani 1 1 d .
C6 C 0.57661(18) 0.4874(2) 0.12894(15) 0.0179(6) Uani 1 1 d .
C7 C 0.60673(18) 0.3255(2) 0.24457(16) 0.0186(6) Uani 1 1 d .
C8 C 0.61283(19) 0.2912(2) 0.30680(17) 0.0219(7) Uani 1 1 d .
C9 C 0.5552(2) 0.2413(3) 0.33049(17) 0.0238(7) Uani 1 1 d .
C10 C 0.49369(19) 0.2283(2) 0.29092(15) 0.0187(6) Uani 1 1 d .
C11 C 0.45733(17) 0.1892(2) 0.01271(14) 0.0159(6) Uani 1 1 d .
C12 C 0.4883(2) 0.1152(3) -0.02078(17) 0.0261(8) Uani 1 1 d .
C13 C 0.4601(3) 0.0918(3) -0.08042(18) 0.0356(10) Uani 1 1 d .
C14 C 0.4030(2) 0.1430(3) -0.10752(17) 0.0269(8) Uani 1 1 d .
C15 C 0.37527(19) 0.2193(3) -0.07566(16) 0.0217(7) Uani 1 1 d .
C16 C 0.40227(18) 0.2423(2) -0.01526(16) 0.0183(6) Uani 1 1 d .
C17 C 0.38760(17) 0.4715(2) 0.19387(16) 0.0171(6) Uani 1 1 d .
C18 C 0.44079(18) 0.5008(2) 0.23749(15) 0.0164(6) Uani 1 1 d .
C19 C 0.42098(18) 0.5586(2) 0.28777(15) 0.0178(6) Uani 1 1 d .
C20 C 0.3489(2) 0.5871(2) 0.29546(18) 0.0245(7) Uani 1 1 d .
C21 C 0.2954(2) 0.5577(3) 0.2522(2) 0.0337(9) Uani 1 1 d .
C22 C 0.3144(2) 0.5006(3) 0.20177(19) 0.0286(8) Uani 1 1 d .
H1 H 0.6470 0.3596 0.2273 0.022 Uiso 1 1 calc R
H2 H 0.6559 0.3023 0.3318 0.026 Uiso 1 1 calc R
H3 H 0.5567 0.2161 0.3725 0.029 Uiso 1 1 calc R
H4 H 0.4531 0.1933 0.3069 0.022 Uiso 1 1 calc R
H5 H 0.5282 0.0811 -0.0029 0.031 Uiso 1 1 calc R
H6 H 0.4801 0.0404 -0.1029 0.043 Uiso 1 1 calc R
H7 H 0.3830 0.1255 -0.1479 0.032 Uiso 1 1 calc R
H8 H 0.3378 0.2561 -0.0949 0.026 Uiso 1 1 calc R
H9 H 0.3829 0.2945 0.0068 0.022 Uiso 1 1 calc R
H10 H 0.4908 0.4813 0.2329 0.020 Uiso 1 1 calc R
H11 H 0.4577 0.5786 0.3172 0.021 Uiso 1 1 calc R
H12 H 0.3357 0.6265 0.3300 0.029 Uiso 1 1 calc R
H13 H 0.2454 0.5769 0.2573 0.040 Uiso 1 1 calc R
H14 H 0.2774 0.4811 0.1723 0.034 Uiso 1 1 calc R
N1 N 0.48912(15) 0.26289(18) 0.23158(13) 0.0146(5) Uani 1 1 d .
N2 N 0.54690(14) 0.31256(18) 0.20838(13) 0.0147(5) Uani 1 1 d .
O1 O 0.25530(15) 0.20154(19) 0.08570(13) 0.0278(5) Uani 1 1 d .
O2 O 0.38625(13) 0.02881(17) 0.20927(12) 0.0233(5) Uani 1 1 d .
O3 O 0.27950(14) 0.2846(2) 0.27669(12) 0.0277(6) Uani 1 1 d .
O4 O 0.53647(16) 0.41080(18) -0.03443(12) 0.0275(6) Uani 1 1 d .
O5 O 0.70180(15) 0.3026(2) 0.08176(14) 0.0342(6) Uani 1 1 d .
O6 O 0.59733(14) 0.56040(17) 0.13994(13) 0.0260(5) Uani 1 1 d .
S1 S 0.49159(4) 0.20575(5) 0.09187(4) 0.01413(14) Uani 1 1 d .
S2 S 0.40757(4) 0.39462(5) 0.12888(4) 0.01476(14) Uani 1 1 d .
C23 C 0.2352(3) 0.5116(4) 0.0103(3) 0.0554(14) Uani 1 1 d .
H15 H 0.2153 0.5676 -0.0110 0.066 Uiso 1 1 calc R
H16 H 0.2810 0.5298 0.0332 0.066 Uiso 1 1 calc R
Cl1 Cl 0.25737(11) 0.43232(13) -0.04676(8) 0.0812(5) Uani 1 1 d .
Cl2 Cl 0.17012(6) 0.47278(9) 0.06666(5) 0.0424(3) 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'
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'
S S 0.1246 0.1234 '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
C1 Re1 C2 89.28(14)
C1 Re1 C3 87.56(14)
C1 Re1 N1 177.59(12)
C1 Re1 S1 98.72(10)
C1 Re1 S2 91.75(10)
C2 Re1 C3 91.32(14)
C2 Re1 N1 92.82(11)
C2 Re1 S1 92.28(10)
C2 Re1 S2 172.41(10)
C3 Re1 N1 93.57(12)
C3 Re1 S1 172.79(10)
C3 Re1 S2 96.24(10)
N1 Re1 S1 80.02(7)
N1 Re1 S2 86.01(7)
S1 Re1 S2 80.13(3)
C4 Re2 C5 86.81(14)
C4 Re2 C6 90.24(14)
C4 Re2 N2 174.15(12)
C4 Re2 S1 93.75(10)
C4 Re2 S2 94.14(10)
C5 Re2 C6 90.72(14)
C5 Re2 N2 91.91(12)
C5 Re2 S1 92.69(11)
C5 Re2 S2 172.72(10)
C6 Re2 N2 95.48(12)
C6 Re2 S1 174.88(9)
C6 Re2 S2 96.49(10)
N2 Re2 S1 80.60(7)
N2 Re2 S2 86.42(7)
S1 Re2 S2 80.05(3)
Re1 C1 O1 177.4(3)
Re1 C2 O2 178.3(3)
Re1 C3 O3 178.6(3)
Re2 C4 O4 175.9(3)
Re2 C5 O5 178.7(3)
Re2 C6 O6 179.0(3)
C8 C7 N2 122.9(3)
C7 C8 C9 117.9(3)
C8 C9 C10 117.6(3)
C9 C10 N1 123.2(3)
C12 C11 C16 120.0(3)
C12 C11 S1 115.5(2)
C16 C11 S1 124.5(2)
C11 C12 C13 119.4(3)
C12 C13 C14 120.5(4)
C13 C14 C15 119.8(3)
C14 C15 C16 120.0(3)
C11 C16 C15 120.1(3)
C18 C17 C22 118.9(3)
C18 C17 S2 123.2(2)
C22 C17 S2 117.8(2)
C17 C18 C19 120.1(3)
C18 C19 C20 120.8(3)
C19 C20 C21 119.3(3)
C20 C21 C22 120.5(3)
C17 C22 C21 120.3(3)
Re1 N1 C10 120.4(2)
Re1 N1 N2 120.82(19)
C10 N1 N2 118.8(3)
Re2 N2 C7 121.1(2)
Re2 N2 N1 119.16(19)
C7 N2 N1 119.7(3)
Re1 S1 Re2 91.33(3)
Re1 S1 C11 112.77(11)
Re2 S1 C11 112.54(11)
Re1 S2 Re2 90.76(2)
Re1 S2 C17 106.40(11)
Re2 S2 C17 115.47(11)
Cl1 C23 Cl2 114.4(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Re1 C1 1.916(3)
Re1 C2 1.916(3)
Re1 C3 1.918(3)
Re1 N1 2.212(3)
Re1 S1 2.4927(8)
Re1 S2 2.5021(8)
Re2 C4 1.923(3)
Re2 C5 1.915(4)
Re2 C6 1.928(3)
Re2 N2 2.210(3)
Re2 S1 2.4919(8)
Re2 S2 2.5071(8)
C1 O1 1.152(4)
C2 O2 1.152(4)
C3 O3 1.152(4)
C4 O4 1.148(4)
C5 O5 1.148(4)
C6 O6 1.142(4)
C7 C8 1.396(5)
C7 N2 1.331(4)
C8 C9 1.358(5)
C9 C10 1.397(5)
C10 N1 1.339(4)
C11 C12 1.394(5)
C11 C16 1.384(4)
C11 S1 1.781(3)
C12 C13 1.387(5)
C13 C14 1.389(5)
C14 C15 1.381(5)
C15 C16 1.392(5)
C17 C18 1.389(4)
C17 C22 1.396(5)
C17 S2 1.790(3)
C18 C19 1.388(4)
C19 C20 1.374(5)
C20 C21 1.387(5)
C21 C22 1.381(5)
N1 N2 1.355(4)
C23 Cl1 1.701(5)
C23 Cl2 1.754(5)
