#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:50:28 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228947 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/11/7231117.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_7231117
loop_
_publ_author_name
'Pino-Cuevas, Arantxa'
'Graña, Ana'
'Abram, Ulrich'
'Carballo, Rosa'
'Vázquez-López, Ezequiel M.'
_publ_section_title
;
 Structural study of mono-, di- and tetranuclear complexes of the
 {Re(CO)3}+ fragment with thiosemicarbazone/thiosemicarbazonate ligands
 containing benzothiazole or benzoxazole groups
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4781
_journal_paper_doi               10.1039/C8CE00874D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C26 H24 N4 O8 Re2 S2'
_chemical_formula_weight         957.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-03-09 deposited with the CCDC.
2018-07-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.892(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5694(7)
_cell_length_b                   14.1822(10)
_cell_length_c                   20.5737(14)
_cell_measurement_reflns_used    9690
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      67.81
_cell_measurement_theta_min      3.80
_cell_volume                     3046.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker CCD Smart 6000'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            40059
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.114
_diffrn_reflns_theta_min         3.800
_exptl_absorpt_coefficient_mu    17.043
_exptl_absorpt_correction_T_max  0.7530
_exptl_absorpt_correction_T_min  0.4194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.966
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5426
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0394
_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)+(0.0779P)²+2.7790P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4766
_reflns_number_total             5426
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00874d2.cif
_cod_data_source_block           2d
_cod_depositor_comments
'Adding full bibliography for 7231102--7231118.cif.'
_cod_database_code               7231117
_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. 
;
_shelx_estimated_absorpt_t_min   0.178
_shelx_estimated_absorpt_t_max   0.477
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C3S C 0.0988(14) 0.8459(8) 0.3092(6) 0.145(4) Uani 1 1 d . U
H3S1 H 0.0189 0.8694 0.3207 0.174 Uiso 1 1 calc R U
H3S2 H 0.0829 0.8270 0.2633 0.174 Uiso 1 1 calc R U
O21 O -0.1871(5) 0.7858(4) 0.1225(3) 0.1004(17) Uani 1 1 d . U
Re1 Re -0.06141(2) 0.96451(2) 0.08024(2) 0.04843(12) Uani 1 1 d . U
Re2 Re 0.41128(2) 0.97001(2) 0.17778(2) 0.05961(12) Uani 1 1 d . U
S1 S 0.06776(12) 1.09321(8) 0.03781(6) 0.0513(3) Uani 1 1 d . U
N2 N 0.1506(4) 0.9399(3) 0.0957(2) 0.0499(8) Uani 1 1 d . U
C1 C 0.1953(5) 1.0264(3) 0.0821(3) 0.0490(10) Uani 1 1 d . U
N1 N 0.3092(4) 1.0564(3) 0.1031(2) 0.0563(9) Uani 1 1 d . U
N3 N 0.2408(4) 0.8903(3) 0.1392(2) 0.0547(9) Uani 1 1 d . U
O20 O -0.3207(5) 1.0616(4) 0.0473(3) 0.0907(14) Uani 1 1 d . U
C3 C 0.1301(5) 0.7361(4) 0.1151(3) 0.0595(11) Uani 1 1 d . U
C6 C -0.0541(6) 0.6113(4) 0.0538(3) 0.0626(12) Uani 1 1 d . U
C8 C 0.0860(6) 0.6630(4) 0.1506(3) 0.0680(14) Uani 1 1 d . U
H8 H 0.1193 0.6552 0.1949 0.082 Uiso 1 1 calc R U
C20 C -0.2270(6) 1.0223(4) 0.0600(3) 0.0595(12) Uani 1 1 d . U
C5 C -0.0024(6) 0.6790(4) 0.0178(3) 0.0627(12) Uani 1 1 d . U
H5 H -0.0298 0.6830 -0.0273 0.075 Uiso 1 1 calc R U
C2 C 0.2252(5) 0.8015(4) 0.1487(3) 0.0597(12) Uani 1 1 d . U
H2 H 0.2836 0.7750 0.1822 0.072 Uiso 1 1 calc R U
C4 C 0.0891(6) 0.7408(4) 0.0475(3) 0.0605(12) Uani 1 1 d . U
H4 H 0.1236 0.7858 0.0223 0.073 Uiso 1 1 calc R U
S2 S -0.2198(2) 0.56048(15) -0.06007(10) 0.0935(6) Uani 1 1 d . U
O1 O 0.2765(5) 1.0350(3) 0.2352(2) 0.0769(11) Uani 1 1 d . U
H1 H 0.2086 0.9971 0.2429 0.092 Uiso 1 1 calc R U
O22 O -0.0546(7) 1.0327(4) 0.2208(3) 0.0994(18) Uani 1 1 d . U
N4 N -0.2159(7) 0.4864(4) 0.0538(3) 0.0788(14) Uani 1 1 d . U
C9 C -0.1592(7) 0.5501(4) 0.0236(3) 0.0678(13) Uani 1 1 d . U
O24 O 0.6380(5) 1.1035(5) 0.2197(3) 0.114(2) Uani 1 1 d . U
C7 C -0.0064(6) 0.6021(4) 0.1209(3) 0.0693(14) Uani 1 1 d . U
H7 H -0.0373 0.5546 0.1454 0.083 Uiso 1 1 calc R U
C22 C -0.0534(6) 1.0086(5) 0.1685(3) 0.0663(13) Uani 1 1 d . U
C25 C 0.5104(6) 0.9089(5) 0.1207(4) 0.0786(15) Uani 1 1 d . U
C21 C -0.1380(5) 0.8508(4) 0.1067(3) 0.0658(13) Uani 1 1 d . U
C23 C 0.4800(7) 0.8865(6) 0.2488(4) 0.0896(19) Uani 1 1 d . U
O23 O 0.5193(7) 0.8373(5) 0.2903(4) 0.141(3) Uani 1 1 d . U
C1S C 0.2786(11) 1.1270(7) 0.2623(6) 0.125(3) Uani 1 1 d . U
H1S1 H 0.2507 1.1227 0.3049 0.150 Uiso 1 1 calc R U
H1S2 H 0.3668 1.1485 0.2697 0.150 Uiso 1 1 calc R U
O1S O 0.1926(7) 0.9207(4) 0.3173(3) 0.1045(17) Uani 1 1 d . U
H1S H 0.2058 0.9373 0.3559 0.157 Uiso 1 1 calc R U
O25 O 0.5661(6) 0.8718(5) 0.0852(4) 0.120(2) Uani 1 1 d . U
C11 C -0.3132(8) 0.4418(5) 0.0121(4) 0.0849(18) Uani 1 1 d . U
C24 C 0.5547(7) 1.0530(6) 0.2040(4) 0.0815(17) Uani 1 1 d . U
C10 C -0.3260(9) 0.4706(5) -0.0521(4) 0.088(2) Uani 1 1 d . U
C12 C -0.3907(10) 0.3708(7) 0.0306(5) 0.120(3) Uani 1 1 d . U
H12 H -0.3832 0.3515 0.0743 0.144 Uiso 1 1 calc R U
C15 C -0.4172(11) 0.4313(8) -0.0996(5) 0.125(4) Uani 1 1 d . U
H15 H -0.4282 0.4517 -0.1430 0.150 Uiso 1 1 calc R U
C13 C -0.4783(12) 0.3300(8) -0.0169(6) 0.144(4) Uani 1 1 d . U
H13 H -0.5293 0.2809 -0.0058 0.173 Uiso 1 1 calc R U
C16 C 0.3536(6) 1.1453(5) 0.0784(3) 0.0732(16) Uani 1 1 d . U
H16A H 0.2814 1.1811 0.0577 0.110 Uiso 1 1 calc R U
H16B H 0.4095 1.1322 0.0469 0.110 Uiso 1 1 calc R U
H16C H 0.3992 1.1808 0.1143 0.110 Uiso 1 1 calc R U
C14 C -0.4915(12) 0.3599(8) -0.0794(6) 0.142(4) Uani 1 1 d . U
H14 H -0.5530 0.3316 -0.1105 0.171 Uiso 1 1 calc R U
C4S C 0.1388(18) 0.7656(8) 0.3488(8) 0.201(8) Uani 1 1 d . U
H4S1 H 0.1987 0.7295 0.3284 0.302 Uiso 1 1 calc R U
H4S2 H 0.0657 0.7273 0.3532 0.302 Uiso 1 1 calc R U
H4S3 H 0.1790 0.7860 0.3916 0.302 Uiso 1 1 calc R U
C2S C 0.204(2) 1.1972(10) 0.2253(9) 0.249(11) Uani 1 1 d . U
H2S1 H 0.1654 1.1713 0.1838 0.373 Uiso 1 1 calc R U
H2S2 H 0.2573 1.2495 0.2180 0.373 Uiso 1 1 calc R U
H2S3 H 0.1378 1.2182 0.2492 0.373 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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_3
C4S C3S O1S 112.5(12) .
C22 Re1 C20 88.4(3) .
C22 Re1 C21 87.9(3) .
C20 Re1 C21 90.6(2) .
C22 Re1 N2 91.1(2) .
C20 Re1 N2 162.8(2) .
C21 Re1 N2 106.5(2) .
C22 Re1 S1 98.4(2) .
C20 Re1 S1 98.06(18) .
C21 Re1 S1 169.40(18) .
N2 Re1 S1 65.03(11) .
C22 Re1 S1 178.9(2) 3_575
C20 Re1 S1 92.37(19) 3_575
C21 Re1 S1 92.9(2) 3_575
N2 Re1 S1 87.90(11) 3_575
S1 Re1 S1 80.70(4) 3_575
C25 Re2 C24 88.1(3) .
C25 Re2 C23 90.5(4) .
C24 Re2 C23 88.6(3) .
C25 Re2 N1 94.8(3) .
C24 Re2 N1 98.0(3) .
C23 Re2 N1 171.7(3) .
C25 Re2 N3 92.4(2) .
C24 Re2 N3 172.7(3) .
C23 Re2 N3 98.7(2) .
N1 Re2 N3 74.70(16) .
C25 Re2 O1 173.0(2) .
C24 Re2 O1 98.1(3) .
C23 Re2 O1 92.9(3) .
N1 Re2 O1 81.20(18) .
N3 Re2 O1 81.03(18) .
C1 S1 Re1 81.06(16) .
C1 S1 Re1 102.89(17) 3_575
Re1 S1 Re1 99.30(4) 3_575
C1 N2 N3 111.2(4) .
C1 N2 Re1 101.7(3) .
N3 N2 Re1 137.7(3) .
N1 C1 N2 124.6(5) .
N1 C1 S1 126.2(4) .
N2 C1 S1 109.0(4) .
C1 N1 C16 120.1(5) .
C1 N1 Re2 113.3(3) .
C16 N1 Re2 126.4(4) .
C2 N3 N2 120.0(5) .
C2 N3 Re2 124.8(4) .
N2 N3 Re2 114.8(3) .
C8 C3 C4 118.9(5) .
C8 C3 C2 119.2(5) .
C4 C3 C2 121.8(5) .
C5 C6 C7 118.9(5) .
C5 C6 C9 121.4(6) .
C7 C6 C9 119.7(5) .
C7 C8 C3 120.5(5) .
O20 C20 Re1 175.6(6) .
C6 C5 C4 121.1(5) .
N3 C2 C3 130.0(5) .
C5 C4 C3 120.1(5) .
C10 S2 C9 89.3(4) .
C1S O1 Re2 128.9(6) .
C9 N4 C11 112.1(6) .
N4 C9 C6 125.8(6) .
N4 C9 S2 113.9(5) .
C6 C9 S2 120.3(5) .
C8 C7 C6 120.2(5) .
O22 C22 Re1 176.5(7) .
O25 C25 Re2 177.8(7) .
O21 C21 Re1 177.4(5) .
O23 C23 Re2 179.5(8) .
C2S C1S O1 117.5(11) .
C10 C11 C12 120.4(7) .
C10 C11 N4 114.5(7) .
C12 C11 N4 125.0(7) .
O24 C24 Re2 178.7(8) .
C11 C10 C15 121.1(8) .
C11 C10 S2 110.1(6) .
C15 C10 S2 128.8(8) .
C13 C12 C11 118.3(9) .
C10 C15 C14 116.8(10) .
C14 C13 C12 120.7(9) .
C13 C14 C15 122.7(9) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C3S C4S 1.426(17) .
C3S O1S 1.444(12) .
O21 C21 1.129(7) .
Re1 C22 1.909(6) .
Re1 C20 1.919(6) .
Re1 C21 1.921(6) .
Re1 N2 2.241(4) .
Re1 S1 2.5152(12) .
Re1 S1 2.5541(13) 3_575
Re2 C25 1.900(7) .
Re2 C24 1.929(7) .
Re2 C23 1.933(7) .
Re2 N1 2.124(4) .
Re2 N3 2.171(4) .
Re2 O1 2.190(5) .
S1 C1 1.780(5) .
S1 Re1 2.5541(13) 3_575
N2 C1 1.359(6) .
N2 N3 1.393(6) .
C1 N1 1.287(7) .
N1 C16 1.464(7) .
N3 C2 1.288(7) .
O20 C20 1.131(7) .
C3 C8 1.390(8) .
C3 C4 1.394(8) .
C3 C2 1.461(8) .
C6 C5 1.377(8) .
C6 C7 1.401(9) .
C6 C9 1.470(9) .
C8 C7 1.374(9) .
C5 C4 1.376(8) .
S2 C10 1.723(8) .
S2 C9 1.748(7) .
O1 C1S 1.417(10) .
O22 C22 1.132(8) .
N4 C9 1.295(8) .
N4 C11 1.385(9) .
O24 C24 1.142(8) .
C25 O25 1.135(9) .
C23 O23 1.130(9) .
C1S C2S 1.417(18) .
C11 C10 1.370(11) .
C11 C12 1.387(11) .
C10 C15 1.380(12) .
C12 C13 1.368(12) .
C15 C14 1.382(14) .
C13 C14 1.341(15) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O1S 0.93 1.90 2.594(7) 129.3 .
O1S H1S N4 0.82 1.97 2.785(8) 172.3 2
C16 H16A S1 0.96 2.56 3.097(6) 115.8 .
