#------------------------------------------------------------------------------
#$Date: 2019-11-17 08:50:28 +0200 (Sun, 17 Nov 2019) $
#$Revision: 228947 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/11/7231116.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_7231116
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            'C50 H34 Cl0 N8 O8 Re2 S2'
_chemical_formula_weight         1311.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.779(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8797(9)
_cell_length_b                   15.0510(13)
_cell_length_c                   18.0200(17)
_cell_measurement_reflns_used    9312
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.48
_cell_volume                     2660.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 Venture Photon 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            83846
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.429
_diffrn_reflns_theta_min         2.247
_exptl_absorpt_coefficient_mu    4.681
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4314
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.637
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.166
_refine_diff_density_min         -2.376
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0168P)²+16.9965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0827
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5843
_reflns_number_total             6640
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00874d2.cif
_cod_data_source_block           9c_sq_s
_cod_depositor_comments
'Adding full bibliography for 7231102--7231118.cif.'
_cod_database_code               7231116
_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   0.548
_shelx_estimated_absorpt_t_max   0.817
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
S S 0.54996(13) 0.09924(9) 0.97631(7) 0.0212(3) Uani 1 1 d . .
Re1 Re 0.67224(2) -0.04396(2) 0.98323(2) 0.01978(6) Uani 1 1 d . .
C1 C 0.5224(5) 0.1024(4) 0.8760(3) 0.0229(11) Uani 1 1 d . .
C2 C 0.5117(6) -0.1145(4) 0.8291(3) 0.0287(12) Uani 1 1 d . .
C3 C 0.4440(6) -0.1033(4) 0.7503(3) 0.0291(12) Uani 1 1 d . .
C4 C 0.3067(7) -0.1182(5) 0.7333(3) 0.0390(15) Uani 1 1 d . .
H4 H 0.2535 -0.1340 0.7719 0.047 Uiso 1 1 calc R U
C5 C 0.2449(6) -0.1106(5) 0.6603(3) 0.0379(14) Uani 1 1 d . .
H5 H 0.1494 -0.1195 0.6495 0.046 Uiso 1 1 calc R U
C6 C 0.3222(6) -0.0899(4) 0.6030(3) 0.0311(13) Uani 1 1 d . .
C7 C 0.4600(7) -0.0752(5) 0.6207(4) 0.0473(18) Uani 1 1 d . .
H7 H 0.5141 -0.0601 0.5823 0.057 Uiso 1 1 calc R U
C8 C 0.5204(7) -0.0822(6) 0.6940(4) 0.0510(19) Uani 1 1 d . .
H8 H 0.6156 -0.0723 0.7053 0.061 Uiso 1 1 calc R U
C9 C 0.2587(6) -0.0834(4) 0.5262(3) 0.0315(13) Uani 1 1 d . .
C10 C 0.1225(7) -0.0743(4) 0.4250(3) 0.0363(14) Uani 1 1 d . .
C11 C 0.0114(8) -0.0654(4) 0.3701(4) 0.0456(17) Uani 1 1 d . .
H11 H -0.0791 -0.0601 0.3824 0.055 Uiso 1 1 calc R U
C12 C 0.0402(9) -0.0646(5) 0.2961(4) 0.052(2) Uani 1 1 d . .
H12 H -0.0323 -0.0556 0.2573 0.063 Uiso 1 1 calc R U
C13 C 0.1699(9) -0.0763(6) 0.2776(4) 0.058(2) Uani 1 1 d . .
H13 H 0.1841 -0.0784 0.2264 0.069 Uiso 1 1 calc R U
C14 C 0.2807(8) -0.0852(6) 0.3321(4) 0.055(2) Uani 1 1 d . .
H14 H 0.3706 -0.0936 0.3197 0.066 Uiso 1 1 calc R U
C15 C 0.2527(7) -0.0811(5) 0.4058(3) 0.0383(14) Uani 1 1 d . .
C16 C 0.5266(7) -0.2085(4) 0.8563(3) 0.0398(15) Uani 1 1 d . .
H16A H 0.5410 -0.2090 0.9110 0.060 Uiso 1 1 calc R U
H16B H 0.6048 -0.2361 0.8366 0.060 Uiso 1 1 calc R U
H16C H 0.4436 -0.2418 0.8389 0.060 Uiso 1 1 calc R U
C17 C 0.4686(8) 0.2091(5) 0.7721(4) 0.0432(17) Uani 1 1 d . .
C18 C 0.3882(9) 0.1573(6) 0.7209(4) 0.059(2) Uani 1 1 d . .
H18 H 0.3505 0.1032 0.7361 0.071 Uiso 1 1 calc R U
C19 C 0.3629(11) 0.1854(8) 0.6463(5) 0.082(3) Uani 1 1 d . .
H19 H 0.3067 0.1506 0.6111 0.098 Uiso 1 1 calc R U
C20 C 0.4192(11) 0.2632(8) 0.6238(5) 0.083(3) Uani 1 1 d . .
H20 H 0.4033 0.2812 0.5730 0.099 Uiso 1 1 calc R U
C21 C 0.4978(10) 0.3146(7) 0.6745(6) 0.078(3) Uani 1 1 d . .
H21 H 0.5352 0.3687 0.6590 0.094 Uiso 1 1 calc R U
C22 C 0.5232(8) 0.2877(5) 0.7492(5) 0.058(2) Uani 1 1 d . .
H22 H 0.5781 0.3235 0.7842 0.069 Uiso 1 1 calc R U
C30 C 0.7561(5) -0.0259(4) 1.0834(3) 0.0266(12) Uani 1 1 d . .
C31 C 0.7600(5) -0.1577(4) 0.9864(3) 0.0252(11) Uani 1 1 d . .
C32 C 0.8284(5) 0.0066(4) 0.9458(3) 0.0276(12) Uani 1 1 d . .
N1 N 0.4950(6) 0.1853(3) 0.8485(3) 0.0367(12) Uani 1 1 d . .
H1 H 0.4934 0.2284 0.8814 0.044 Uiso 1 1 calc R U
N2 N 0.5284(4) 0.0347(3) 0.8329(2) 0.0251(9) Uani 1 1 d . .
N3 N 0.5547(4) -0.0476(3) 0.8701(2) 0.0223(9) Uani 1 1 d . .
N4 N 0.1285(5) -0.0777(3) 0.5031(3) 0.0339(11) Uani 1 1 d . .
O1 O 0.3403(5) -0.0852(3) 0.4707(2) 0.0403(10) Uani 1 1 d . .
O30 O 0.8049(4) -0.0153(3) 1.1443(2) 0.0411(11) Uani 1 1 d . .
O31 O 0.8173(5) -0.2245(3) 0.9906(3) 0.0457(11) Uani 1 1 d . .
O32 O 0.9219(4) 0.0375(3) 0.9234(2) 0.0424(11) 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
_geom_angle_site_symmetry_3
C1 S Re1 95.11(18) .
C1 S Re1 105.33(17) 3_657
Re1 S Re1 97.72(4) 3_657
C32 Re1 C30 89.9(2) .
C32 Re1 C31 89.1(2) .
C30 Re1 C31 87.4(2) .
C32 Re1 N3 92.43(19) .
C30 Re1 N3 171.3(2) .
C31 Re1 N3 101.0(2) .
C32 Re1 S 92.60(18) .
C30 Re1 S 94.51(17) .
C31 Re1 S 177.41(17) .
N3 Re1 S 77.04(12) .
C32 Re1 S 173.81(17) 3_657
C30 Re1 S 93.94(16) 3_657
C31 Re1 S 95.87(17) 3_657
N3 Re1 S 83.06(11) 3_657
S Re1 S 82.28(4) 3_657
N2 C1 N1 121.9(5) .
N2 C1 S 125.1(4) .
N1 C1 S 113.0(4) .
N3 C2 C16 122.4(5) .
N3 C2 C3 122.2(5) .
C16 C2 C3 115.4(5) .
C8 C3 C4 119.2(5) .
C8 C3 C2 120.1(5) .
C4 C3 C2 120.6(5) .
C3 C4 C5 120.7(6) .
C4 C5 C6 120.2(6) .
C7 C6 C5 118.6(5) .
C7 C6 C9 120.8(6) .
C5 C6 C9 120.6(5) .
C6 C7 C8 120.6(6) .
C3 C8 C7 120.6(6) .
N4 C9 O1 114.5(5) .
N4 C9 C6 127.3(6) .
O1 C9 C6 118.2(5) .
C15 C10 C11 120.7(6) .
C15 C10 N4 108.7(5) .
C11 C10 N4 130.6(6) .
C10 C11 C12 116.5(7) .
C13 C12 C11 122.1(7) .
C12 C13 C14 121.5(7) .
C13 C14 C15 116.2(7) .
O1 C15 C10 107.7(5) .
O1 C15 C14 129.5(6) .
C10 C15 C14 122.8(6) .
C22 C17 C18 119.7(7) .
C22 C17 N1 118.2(7) .
C18 C17 N1 122.0(6) .
C17 C18 C19 119.5(9) .
C20 C19 C18 120.4(10) .
C21 C20 C19 120.1(8) .
C20 C21 C22 120.1(9) .
C17 C22 C21 120.2(9) .
O30 C30 Re1 178.9(5) .
O31 C31 Re1 176.9(5) .
O32 C32 Re1 179.6(6) .
C1 N1 C17 126.3(5) .
C1 N2 N3 115.1(4) .
C2 N3 N2 112.4(4) .
C2 N3 Re1 130.2(4) .
N2 N3 Re1 117.3(3) .
C9 N4 C10 104.2(5) .
C9 O1 C15 105.0(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S C1 1.797(5) .
S Re1 2.4667(13) .
S Re1 2.5340(13) 3_657
Re1 C32 1.913(5) .
Re1 C30 1.914(5) .
Re1 C31 1.917(5) .
Re1 N3 2.225(4) .
Re1 S 2.5341(13) 3_657
C1 N2 1.286(7) .
C1 N1 1.357(7) .
C2 N3 1.290(7) .
C2 C16 1.499(8) .
C2 C3 1.506(7) .
C3 C8 1.371(9) .
C3 C4 1.373(8) .
C4 C5 1.388(8) .
C5 C6 1.391(8) .
C6 C7 1.379(8) .
C6 C9 1.453(8) .
C7 C8 1.388(9) .
C9 N4 1.308(8) .
C9 O1 1.356(7) .
C10 C15 1.375(9) .
C10 C11 1.394(9) .
C10 N4 1.403(8) .
C11 C12 1.396(10) .
C12 C13 1.372(12) .
C13 C14 1.388(10) .
C14 C15 1.389(9) .
C15 O1 1.372(7) .
C17 C22 1.384(10) .
C17 C18 1.384(11) .
C17 N1 1.418(8) .
C18 C19 1.404(10) .
C19 C20 1.377(15) .
C20 C21 1.367(15) .
C21 C22 1.399(11) .
C30 O30 1.157(6) .
C31 O31 1.152(7) .
C32 O32 1.150(7) .
N2 N3 1.419(6) .
