#------------------------------------------------------------------------------
#$Date: 2017-03-05 08:35:02 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193934 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/20/2242065.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2242065
loop_
_publ_author_name
'Priyatharsini, Maruthupandiyan'
'Shankar, Bhaskaran'
'Sathiyendiran, Malaichamy'
'Srinivasan, Navaneethakrishnan'
'Krishnakumar, Rajaputi Venkatraman'
_publ_section_title
;
 Crystal structure of the cis and trans polymorphs of
 bis[μ-2-(1,3-benzothiazol-2-yl)phenolato]-κ³N,O:O;κ³O:N,O-bis[fac-tricarbonylrhenium(I)]
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              310
_journal_page_last               313
_journal_paper_doi               10.1107/S2056989017001347
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Re2 (C13 H8 N1 O1 S1)2 (C O)6]'
_chemical_formula_moiety         'C32 H16 N2 O8 Re2 S2'
_chemical_formula_sum            'C32 H16 N2 O8 Re2 S2'
_chemical_formula_weight         992.99
_chemical_name_systematic
cis-Bis[μ-2-(1,3-benzothiazol-2-yl)phenolato]-κ³N,O:O;κ³O:N,O-bis[fac-tricarbonylrhenium(I)]
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1480(7)
_cell_length_b                   11.6519(5)
_cell_length_c                   15.6329(8)
_cell_measurement_reflns_used    2943
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.9
_cell_volume                     2941.4(2)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
PLUTON (Spek, 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11735
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.268
_diffrn_reflns_theta_min         2.895
_exptl_absorpt_coefficient_mu    8.423
_exptl_absorpt_correction_T_max  0.38
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_description       needle
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.093
_refine_diff_density_min         -0.949
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0269
_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)+(0.0263P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0601
_reflns_number_gt                2943
_reflns_number_total             3510
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            rz5204sup1.cif
_cod_data_source_block           II
_cod_database_code               2242065
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Re Re01 -0.00490(2) 0.15435(2) 0.35969(2) 0.01406(6) Uani d 1
S S1 0.07316(6) 0.54284(8) 0.35632(6) 0.0210(2) Uani d 1
O O1 0.07833(17) 0.1789(2) 0.25483(14) 0.0159(6) Uani d 1
O O2 0.13167(17) 0.1285(2) 0.49308(18) 0.0287(7) Uani d 1
O O3 -0.01421(17) -0.1089(3) 0.34887(19) 0.0293(7) Uani d 1
O O4 -0.13228(17) 0.1328(2) 0.50382(18) 0.0302(7) Uani d 1
N N1 0.00453(16) 0.3439(3) 0.36089(19) 0.0158(8) Uani d 1
C C1 -0.0277(2) 0.5344(3) 0.3923(2) 0.0164(8) Uani d 1
C C2 -0.0769(2) 0.6243(3) 0.4226(2) 0.0198(8) Uani d 1
H H2 -0.0566 0.6988 0.4265 0.024 Uiso calc 1
C C3 -0.1569(2) 0.5978(3) 0.4467(2) 0.0212(8) Uani d 1
H H3 -0.1914 0.6555 0.4672 0.025 Uiso calc 1
C C4 -0.1866(2) 0.4861(3) 0.4407(3) 0.0219(9) Uani d 1
H H4 -0.2410 0.4705 0.4562 0.026 Uiso calc 1
C C5 -0.1369(2) 0.3980(3) 0.4121(2) 0.0173(8) Uani d 1
H H5 -0.1576 0.3237 0.4083 0.021 Uiso calc 1
C C6 -0.0555(2) 0.4210(3) 0.3892(2) 0.0142(7) Uani d 1
C C7 0.0748(2) 0.3953(3) 0.3416(2) 0.0159(8) Uani d 1
C C8 0.1503(2) 0.3426(3) 0.3103(2) 0.0167(8) Uani d 1
C C9 0.1499(2) 0.2380(3) 0.2657(2) 0.0165(8) Uani d 1
C C10 0.2230(2) 0.1963(3) 0.2318(2) 0.0213(9) Uani d 1
H H10 0.2227 0.1273 0.2019 0.026 Uiso calc 1
C C11 0.2959(2) 0.2549(4) 0.2414(2) 0.0271(10) Uani d 1
H H11 0.3443 0.2262 0.2173 0.033 Uiso calc 1
C C12 0.2980(2) 0.3564(3) 0.2867(3) 0.0294(10) Uani d 1
H H12 0.3478 0.3950 0.2945 0.035 Uiso calc 1
C C13 0.2258(2) 0.4003(3) 0.3203(3) 0.0237(9) Uani d 1
H H13 0.2272 0.4694 0.3501 0.028 Uiso calc 1
C C14 0.0788(2) 0.1374(3) 0.4440(3) 0.0183(8) Uani d 1
C C15 -0.0848(2) 0.1418(3) 0.4488(3) 0.0197(8) Uani d 1
C C16 -0.0108(2) -0.0097(4) 0.3516(2) 0.0189(9) Uani d 1
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'
Re Re -1.0185 7.2310 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C14 Re01 C15 . . 88.10(18)
C14 Re01 C16 . . 88.70(15)
C15 Re01 C16 . . 86.45(14)
C14 Re01 O1 . . 95.63(14)
C15 Re01 O1 . . 175.25(12)
C16 Re01 O1 . . 96.54(13)
C14 Re01 O1 . 4 167.74(13)
C15 Re01 O1 . 4 104.12(14)
C16 Re01 O1 . 4 92.87(13)
O1 Re01 O1 . 4 72.12(12)
C14 Re01 N1 . . 92.80(12)
C15 Re01 N1 . . 96.72(12)
C16 Re01 N1 . . 176.53(14)
O1 Re01 N1 . . 80.20(10)
O1 Re01 N1 4 . 85.00(10)
C1 S1 C7 . . 90.05(17)
C9 O1 Re01 . . 120.5(2)
C9 O1 Re01 . 4 129.6(2)
Re01 O1 Re01 . 4 105.77(11)
C7 N1 C6 . . 112.3(3)
C7 N1 Re01 . . 120.7(2)
C6 N1 Re01 . . 126.7(2)
C6 C1 C2 . . 122.6(3)
C6 C1 S1 . . 110.2(3)
C2 C1 S1 . . 127.2(3)
C3 C2 C1 . . 117.2(3)
C3 C2 H2 . . 121.4
C1 C2 H2 . . 121.4
C2 C3 C4 . . 120.9(3)
C2 C3 H3 . . 119.6
C4 C3 H3 . . 119.6
C5 C4 C3 . . 121.3(3)
C5 C4 H4 . . 119.4
C3 C4 H4 . . 119.4
C4 C5 C6 . . 119.4(3)
C4 C5 H5 . . 120.3
C6 C5 H5 . . 120.3
C5 C6 N1 . . 128.0(3)
C5 C6 C1 . . 118.5(3)
N1 C6 C1 . . 113.5(3)
N1 C7 C8 . . 127.5(3)
N1 C7 S1 . . 114.0(3)
C8 C7 S1 . . 118.5(3)
C13 C8 C9 . . 118.4(3)
C13 C8 C7 . . 119.4(3)
C9 C8 C7 . . 122.1(3)
O1 C9 C10 . . 120.1(3)
O1 C9 C8 . . 120.5(3)
C10 C9 C8 . . 119.4(3)
C11 C10 C9 . . 121.1(4)
C11 C10 H10 . . 119.4
C9 C10 H10 . . 119.4
C10 C11 C12 . . 120.3(4)
C10 C11 H11 . . 119.8
C12 C11 H11 . . 119.8
C13 C12 C11 . . 119.6(4)
C13 C12 H12 . . 120.2
C11 C12 H12 . . 120.2
C12 C13 C8 . . 121.0(3)
C12 C13 H13 . . 119.5
C8 C13 H13 . . 119.5
O2 C14 Re01 . . 177.6(3)
O4 C15 Re01 . . 178.7(3)
O3 C16 Re01 . . 178.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Re01 C14 . 1.898(4)
Re01 C15 . 1.904(4)
Re01 C16 . 1.918(4)
Re01 O1 . 2.139(2)
Re01 O1 4 2.166(2)
Re01 N1 . 2.214(3)
S1 C1 . 1.726(4)
S1 C7 . 1.735(4)
O1 C9 . 1.355(4)
O1 Re01 4 2.166(2)
O2 C14 . 1.153(4)
O3 C16 . 1.158(5)
O4 C15 . 1.157(5)
N1 C7 . 1.318(4)
N1 C6 . 1.393(4)
C1 C6 . 1.396(5)
C1 C2 . 1.398(5)
C2 C3 . 1.380(5)
C2 H2 . 0.9300
C3 C4 . 1.390(4)
C3 H3 . 0.9300
C4 C5 . 1.377(4)
C4 H4 . 0.9300
C5 C6 . 1.389(5)
C5 H5 . 0.9300
C7 C8 . 1.450(5)
C8 C13 . 1.401(5)
C8 C9 . 1.404(5)
C9 C10 . 1.382(5)
C10 C11 . 1.370(5)
C10 H10 . 0.9300
C11 C12 . 1.378(6)
C11 H11 . 0.9300
C12 C13 . 1.377(5)
C12 H12 . 0.9300
C13 H13 . 0.9300
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C4 H4 O2 3_456 0.93 2.49 3.387(4) 162.8
C2 H2 O3 1_565 0.93 2.64 3.467(5) 148.7
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_site_symmetry_1
_geom_torsion
C7 S1 C1 C6 . -1.5(3)
C7 S1 C1 C2 . 177.1(4)
C6 C1 C2 C3 . -2.7(6)
S1 C1 C2 C3 . 178.8(3)
C1 C2 C3 C4 . 0.0(6)
C2 C3 C4 C5 . 1.2(6)
C3 C4 C5 C6 . 0.2(6)
C4 C5 C6 N1 . 178.4(4)
C4 C5 C6 C1 . -2.8(5)
C7 N1 C6 C5 . 177.8(4)
Re01 N1 C6 C5 . -9.0(5)
C7 N1 C6 C1 . -1.0(4)
Re01 N1 C6 C1 . 172.2(2)
C2 C1 C6 C5 . 4.2(6)
S1 C1 C6 C5 . -177.2(3)
C2 C1 C6 N1 . -176.9(3)
S1 C1 C6 N1 . 1.8(4)
C6 N1 C7 C8 . -180.0(4)
Re01 N1 C7 C8 . 6.3(5)
C6 N1 C7 S1 . -0.2(4)
Re01 N1 C7 S1 . -173.91(16)
C1 S1 C7 N1 . 1.0(3)
C1 S1 C7 C8 . -179.2(3)
N1 C7 C8 C13 . -158.5(4)
S1 C7 C8 C13 . 21.7(5)
N1 C7 C8 C9 . 25.2(6)
S1 C7 C8 C9 . -154.6(3)
Re01 O1 C9 C10 . 135.2(3)
Re01 O1 C9 C10 4 -71.1(4)
Re01 O1 C9 C8 . -45.7(4)
Re01 O1 C9 C8 4 108.0(3)
C13 C8 C9 O1 . 179.7(3)
C7 C8 C9 O1 . -4.0(5)
C13 C8 C9 C10 . -1.2(5)
C7 C8 C9 C10 . 175.1(3)
O1 C9 C10 C11 . 179.5(3)
C8 C9 C10 C11 . 0.4(6)
C9 C10 C11 C12 . 1.1(6)
C10 C11 C12 C13 . -1.8(6)
C11 C12 C13 C8 . 0.9(6)
C9 C8 C13 C12 . 0.5(6)
C7 C8 C13 C12 . -175.9(4)

_cod_database_fobs_code 2242065
