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#$Date: 2025-04-05 06:44:14 +0300 (Sat, 05 Apr 2025) $
#$Revision: 299015 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/35/7063542.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_7063542
loop_
_publ_author_name
'Das, Akash'
'Guha, Subhabrata'
'Halder, Arpan'
'Gharami, Saswati'
'Naskar, Rahul'
'Das, Gaurav'
'Mondal, Tapan K.'
_publ_section_title
;
 Synthesis, characterization, DNA/protein-binding study and anticancer
 activity of novel tricarbonyl Re(i) complexes with an ONS donor
 azo-thioether pincer ligand
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              559
_journal_page_last               571
_journal_paper_doi               10.1039/D4NJ03255A
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C15 H13 N2 O5 Re S'
_chemical_formula_sum            'C15 H13 N2 O5 Re S'
_chemical_formula_weight         519.53
_chemical_name_systematic        2
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-11-11
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.11.02 svn.r19aeb66f for OlexSys, GUI svn.r7078)
;
_audit_update_record
;
2024-11-11 deposited with the CCDC.	2024-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.4660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7789(3)
_cell_length_b                   28.8370(12)
_cell_length_c                   9.0488(4)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.45
_cell_volume                     1696.34(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker AXS D8 Quest CMOS diffractometer'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            25384
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.160
_diffrn_reflns_theta_min         3.163
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.313
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.1957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1576 before and 0.0763 after correction.
The Ratio of minimum to maximum transmission is 0.2625.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.034
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.090
_refine_diff_density_min         -1.700
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.0033(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0331P)²+2.5186P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3494
_reflns_number_total             3756
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj03255a2.cif
_cod_data_source_block           tkm_ad_re_0m_a
_cod_depositor_comments
'Adding full bibliography for 7063542--7063543.cif.'
_cod_database_code               7063542
_shelx_shelxl_version_number     2019/3
_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_max   0.629
_shelx_estimated_absorpt_t_min   0.427
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13)
;
_olex2_submission_original_sample_id AD88
_olex2_submission_special_instructions 'No special instructions were received'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re 0.58448(2) 0.58189(2) 0.27134(2) 0.02689(9) Uani 1 1 d . . . . .
S1 S 0.61283(16) 0.55440(4) 0.53612(12) 0.0312(2) Uani 1 1 d . . . . .
N1 N 0.7104(5) 0.64073(11) 0.4076(4) 0.0277(7) Uani 1 1 d . . . . .
N2 N 0.6667(5) 0.68376(11) 0.3767(4) 0.0301(7) Uani 1 1 d . . . . .
O1 O 0.9864(6) 0.52997(16) 0.2961(6) 0.0699(13) Uani 1 1 d . . . . .
O2 O 0.3335(6) 0.50097(14) 0.0909(4) 0.0607(11) Uani 1 1 d . . . . .
O3 O 0.6367(6) 0.62103(14) -0.0305(4) 0.0548(9) Uani 1 1 d . . . . .
O4 O 0.3187(4) 0.62338(11) 0.2611(4) 0.0349(7) Uani 1 1 d . . . . .
O5 O 0.3492(7) 0.75597(15) 0.0962(5) 0.0715(13) Uani 1 1 d . . . . .
C1 C 0.8328(7) 0.54882(17) 0.2858(6) 0.0410(11) Uani 1 1 d . . . . .
C2 C 0.4295(7) 0.53034(16) 0.1585(5) 0.0379(10) Uani 1 1 d . . . . .
C3 C 0.6106(7) 0.60711(16) 0.0794(6) 0.0371(10) Uani 1 1 d . . . . .
C4 C 0.3138(7) 0.66646(16) 0.2355(5) 0.0345(9) Uani 1 1 d . . . . .
C5 C 0.1023(8) 0.6878(2) 0.1937(8) 0.0570(15) Uani 1 1 d . . . . .
H5A H 0.112749 0.720472 0.176301 0.085 Uiso 1 1 calc R U . . .
H5B H 0.017801 0.673508 0.101722 0.085 Uiso 1 1 calc R U . . .
H5C H 0.041757 0.683158 0.276433 0.085 Uiso 1 1 calc R U . . .
C6 C 0.4932(7) 0.69492(14) 0.2634(5) 0.0315(9) Uani 1 1 d . . . . .
C7 C 0.4843(8) 0.74347(17) 0.2077(6) 0.0452(12) Uani 1 1 d . . . . .
C8 C 0.6519(11) 0.7757(2) 0.2901(9) 0.0689(18) Uani 1 1 d . . . . .
H8A H 0.744377 0.759805 0.375038 0.103 Uiso 1 1 calc R U . . .
H8B H 0.725884 0.786245 0.220318 0.103 Uiso 1 1 calc R U . . .
H8C H 0.593142 0.801886 0.327908 0.103 Uiso 1 1 calc R U . . .
C9 C 0.8514(6) 0.63260(14) 0.5563(5) 0.0282(8) Uani 1 1 d . . . . .
C10 C 1.0071(6) 0.66336(16) 0.6291(6) 0.0368(10) Uani 1 1 d . . . . .
H10 H 1.028455 0.690493 0.580322 0.044 Uiso 1 1 calc R U . . .
C11 C 1.1292(7) 0.65272(19) 0.7756(6) 0.0453(12) Uani 1 1 d . . . . .
H11 H 1.234883 0.672750 0.825033 0.054 Uiso 1 1 calc R U . . .
C12 C 1.0966(7) 0.61297(18) 0.8490(6) 0.0432(11) Uani 1 1 d . . . . .
H12 H 1.178973 0.606759 0.948113 0.052 Uiso 1 1 calc R U . . .
C13 C 0.9433(8) 0.58207(16) 0.7778(6) 0.0382(10) Uani 1 1 d . . . . .
H13 H 0.922611 0.555052 0.827555 0.046 Uiso 1 1 calc R U . . .
C14 C 0.8208(6) 0.59229(15) 0.6304(5) 0.0292(8) Uani 1 1 d . . . . .
C15 C 0.4049(8) 0.5779(2) 0.6013(7) 0.0516(14) Uani 1 1 d . . . . .
H15A H 0.282118 0.560220 0.557823 0.077 Uiso 1 1 calc R U . . .
H15B H 0.440374 0.576311 0.711670 0.077 Uiso 1 1 calc R U . . .
H15C H 0.381757 0.609626 0.568957 0.077 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 0.0033 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'
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'
Re Re -1.0185 7.2310 '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'
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
_geom_angle_publ_flag
N1 Re1 S1 77.68(10) . . ?
N1 Re1 O4 76.95(12) . . ?
O4 Re1 S1 93.11(9) . . ?
C1 Re1 S1 87.07(16) . . ?
C1 Re1 N1 99.06(17) . . ?
C1 Re1 O4 175.86(16) . . ?
C1 Re1 C2 89.4(2) . . ?
C1 Re1 C3 86.9(2) . . ?
C2 Re1 S1 98.40(14) . . ?
C2 Re1 N1 170.45(16) . . ?
C2 Re1 O4 94.71(17) . . ?
C2 Re1 C3 89.38(19) . . ?
C3 Re1 S1 170.09(13) . . ?
C3 Re1 N1 95.53(16) . . ?
C3 Re1 O4 92.36(15) . . ?
C14 S1 Re1 95.73(15) . . ?
C14 S1 C15 101.3(2) . . ?
C15 S1 Re1 110.0(2) . . ?
N2 N1 Re1 127.8(3) . . ?
N2 N1 C9 114.4(3) . . ?
C9 N1 Re1 117.7(2) . . ?
N1 N2 C6 119.2(3) . . ?
C4 O4 Re1 122.4(3) . . ?
O1 C1 Re1 178.0(5) . . ?
O2 C2 Re1 177.9(5) . . ?
O3 C3 Re1 176.3(4) . . ?
O4 C4 C5 115.0(4) . . ?
O4 C4 C6 123.8(4) . . ?
C6 C4 C5 120.7(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C4 120.5(4) . . ?
N2 C6 C7 115.0(4) . . ?
C4 C6 C7 122.1(4) . . ?
O5 C7 C6 120.9(5) . . ?
O5 C7 C8 121.3(5) . . ?
C6 C7 C8 117.8(5) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N1 123.7(4) . . ?
C14 C9 N1 116.1(3) . . ?
C14 C9 C10 120.1(4) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 C9 118.7(4) . . ?
C11 C10 H10 120.7 . . ?
C10 C11 H11 119.6 . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.6 . . ?
C11 C12 H12 119.5 . . ?
C11 C12 C13 121.1(5) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 H13 120.8 . . ?
C12 C13 C14 118.5(4) . . ?
C14 C13 H13 120.8 . . ?
C9 C14 S1 119.0(3) . . ?
C9 C14 C13 120.8(4) . . ?
C13 C14 S1 120.1(4) . . ?
S1 C15 H15A 109.5 . . ?
S1 C15 H15B 109.5 . . ?
S1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 S1 2.4789(11) . ?
Re1 N1 2.129(3) . ?
Re1 O4 2.143(3) . ?
Re1 C1 1.907(5) . ?
Re1 C2 1.936(5) . ?
Re1 C3 1.937(5) . ?
S1 C14 1.797(4) . ?
S1 C15 1.807(5) . ?
N1 N2 1.288(5) . ?
N1 C9 1.432(5) . ?
N2 C6 1.362(6) . ?
O1 C1 1.155(6) . ?
O2 C2 1.136(6) . ?
O3 C3 1.131(6) . ?
O4 C4 1.262(5) . ?
O5 C7 1.209(6) . ?
C4 C5 1.507(6) . ?
C4 C6 1.429(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.484(6) . ?
C7 C8 1.494(8) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.393(5) . ?
C9 C14 1.387(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.383(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.374(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.382(7) . ?
C13 H13 0.9300 . ?
C13 C14 1.389(7) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Re1 S1 C14 C9 22.7(3) . . . . ?
Re1 S1 C14 C13 -159.9(4) . . . . ?
Re1 N1 N2 C6 15.4(5) . . . . ?
Re1 N1 C9 C10 151.8(3) . . . . ?
Re1 N1 C9 C14 -30.7(5) . . . . ?
Re1 O4 C4 C5 165.6(3) . . . . ?
Re1 O4 C4 C6 -22.7(6) . . . . ?
N1 N2 C6 C4 33.1(6) . . . . ?
N1 N2 C6 C7 -164.3(4) . . . . ?
N1 C9 C10 C11 177.5(4) . . . . ?
N1 C9 C14 S1 0.2(5) . . . . ?
N1 C9 C14 C13 -177.2(4) . . . . ?
N2 N1 C9 C10 -31.9(6) . . . . ?
N2 N1 C9 C14 145.5(4) . . . . ?
N2 C6 C7 O5 171.8(5) . . . . ?
N2 C6 C7 C8 -5.9(7) . . . . ?
O4 C4 C6 N2 -29.3(7) . . . . ?
O4 C4 C6 C7 169.4(4) . . . . ?
C4 C6 C7 O5 -25.9(7) . . . . ?
C4 C6 C7 C8 156.4(5) . . . . ?
C5 C4 C6 N2 142.0(5) . . . . ?
C5 C4 C6 C7 -19.4(7) . . . . ?
C9 N1 N2 C6 -160.4(4) . . . . ?
C9 C10 C11 C12 -0.8(7) . . . . ?
C10 C9 C14 S1 177.8(3) . . . . ?
C10 C9 C14 C13 0.4(6) . . . . ?
C10 C11 C12 C13 1.1(8) . . . . ?
C11 C12 C13 C14 -0.6(7) . . . . ?
C12 C13 C14 S1 -177.5(4) . . . . ?
C12 C13 C14 C9 -0.1(7) . . . . ?
C14 C9 C10 C11 0.1(6) . . . . ?
C15 S1 C14 C9 -89.0(4) . . . . ?
C15 S1 C14 C13 88.4(4) . . . . ?
