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#$Date: 2026-03-17 01:00:13 +0100 (Tue 17 de Mar de 2026) $
#$Revision: 305103 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/07/7720706.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_7720706
loop_
_publ_author_name
'Raza, Arsen'
'Carneiro Neto, José Severiano'
'Lanza, Arianna'
'Bendix, Jesper'
'Briganti, Matteo'
'Sorace, Lorenzo'
'Perfetti, Mauro'
_publ_section_title
;
 Synthesis, structure, and magnetic properties of Fe3+ and Ru3+ metal
 chalcogenide (O,S) complexes with bidentate ligands
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D6DT00055J
_journal_year                    2026
_chemical_formula_sum            'C18 H19 Cl4 N3 O2 Os'
_chemical_formula_weight         641.36
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2026-01-04 deposited with the CCDC.	2026-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.749(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3716(7)
_cell_length_b                   8.8491(6)
_cell_length_c                   20.2098(14)
_cell_measurement_reflns_used    9233
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.5683
_cell_measurement_theta_min      2.4116
_cell_volume                     2180.6(2)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_data_collection       APEX5V2022.8-RC126
_computing_data_reduction        'SAINT V8.40B (Bruker AXS LLC, 2019)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 1503)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'XT, VERSION 2018/2'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55707
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.623
_diffrn_reflns_theta_min         2.412
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.357
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.173
_refine_diff_density_max         2.082
_refine_diff_density_min         -3.066
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         6707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0396
_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)+(0.0269P)²+23.8052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6214
_reflns_number_total             6707
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00055j2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7720706
_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   0.277
_shelx_estimated_absorpt_t_max   0.406
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
Os1 Os 0.24789(2) 0.43900(2) 0.22444(2) 0.01281(6) Uani 1 1 d . . . . .
Cl1 Cl 0.39644(9) 0.51977(14) 0.17370(6) 0.0178(2) Uani 1 1 d . . . . .
Cl2 Cl 0.11682(10) 0.49969(15) 0.12791(6) 0.0198(2) Uani 1 1 d . . . . .
O1 O 0.3475(3) 0.3823(4) 0.31191(17) 0.0160(6) Uani 1 1 d . . . . .
O2 O 0.1297(3) 0.3654(4) 0.27743(18) 0.0175(7) Uani 1 1 d . . . . .
N1 N 0.2630(3) 0.2170(4) 0.1918(2) 0.0162(8) Uani 1 1 d . . . . .
N2 N 0.2343(3) 0.6512(4) 0.2665(2) 0.0139(7) Uani 1 1 d . . . . .
N3 N 0.2729(4) 0.2448(5) 0.4660(2) 0.0213(9) Uani 1 1 d . . . . .
C1 C 0.1769(4) 0.1388(6) 0.1600(3) 0.0211(10) Uani 1 1 d . . . . .
H1 H 0.106729 0.185502 0.152131 0.025 Uiso 1 1 calc R U . . .
C2 C 0.1871(5) -0.0072(6) 0.1384(3) 0.0249(11) Uani 1 1 d . . . . .
H2 H 0.124428 -0.059484 0.115877 0.030 Uiso 1 1 calc R U . . .
C3 C 0.2887(5) -0.0785(6) 0.1493(3) 0.0239(11) Uani 1 1 d . . . . .
H3 H 0.296927 -0.179111 0.134593 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3783(4) 0.0034(6) 0.1828(3) 0.0205(10) Uani 1 1 d . . . . .
H4 H 0.449315 -0.040704 0.191172 0.025 Uiso 1 1 calc R U . . .
C5 C 0.3620(4) 0.1490(6) 0.2034(3) 0.0174(9) Uani 1 1 d . . . . .
H5 H 0.422952 0.203572 0.226687 0.021 Uiso 1 1 calc R U . . .
C6 C 0.3253(4) 0.7221(6) 0.2967(3) 0.0195(9) Uani 1 1 d . . . . .
H6 H 0.394165 0.673922 0.297827 0.023 Uiso 1 1 calc R U . . .
C7 C 0.3225(4) 0.8638(6) 0.3265(3) 0.0231(10) Uani 1 1 d . . . . .
H8 H 0.388398 0.912112 0.346804 0.028 Uiso 1 1 calc R U . . .
C8 C 0.2217(5) 0.9328(6) 0.3261(3) 0.0245(11) Uani 1 1 d . . . . .
H9 H 0.216902 1.029081 0.346142 0.029 Uiso 1 1 calc R U . . .
C9 C 0.1281(4) 0.8574(6) 0.2955(3) 0.0229(10) Uani 1 1 d . . . . .
H10 H 0.058041 0.901855 0.294756 0.027 Uiso 1 1 calc R U . . .
C10 C 0.1367(4) 0.7174(5) 0.2661(3) 0.0171(9) Uani 1 1 d . . . . .
H11 H 0.071974 0.667178 0.245163 0.021 Uiso 1 1 calc R U . . .
C11 C 0.2889(4) 0.3372(5) 0.3577(2) 0.0162(9) Uani 1 1 d . . . . .
C12 C 0.1719(4) 0.3282(5) 0.3386(2) 0.0162(8) Uani 1 1 d . . . . .
C13 C 0.1105(4) 0.2756(5) 0.3860(3) 0.0184(9) Uani 1 1 d . . . . .
H15 H 0.032962 0.267885 0.374818 0.022 Uiso 1 1 calc R U . . .
C14 C 0.1634(5) 0.2353(6) 0.4489(3) 0.0240(11) Uani 1 1 d . . . . .
H16 H 0.121492 0.199903 0.481057 0.029 Uiso 1 1 calc R U . . .
C15 C 0.3246(6) 0.2013(9) 0.5354(3) 0.0378(15) Uani 1 1 d . . . . .
H17A H 0.404305 0.213964 0.540525 0.057 Uiso 1 1 calc R U . . .
H17B H 0.296056 0.265958 0.567865 0.057 Uiso 1 1 calc R U . . .
H17C H 0.307509 0.095503 0.543514 0.057 Uiso 1 1 calc R U . . .
C16 C 0.3383(4) 0.2938(6) 0.4215(3) 0.0198(9) Uani 1 1 d . . . . .
C17 C 0.4599(5) 0.2989(8) 0.4418(3) 0.0299(12) Uani 1 1 d . . . . .
H19A H 0.493113 0.336332 0.404263 0.045 Uiso 1 1 calc R U . . .
H19B H 0.478990 0.366681 0.480396 0.045 Uiso 1 1 calc R U . . .
H19C H 0.487476 0.197184 0.454144 0.045 Uiso 1 1 calc R U . . .
Cl3A Cl 0.0868(5) 0.6294(5) 0.4561(3) 0.0563(14) Uani 0.644(8) 1 d . . P A 1
Cl4A Cl 0.2769(2) 0.8228(4) 0.49281(14) 0.0455(11) Uani 0.644(8) 1 d . . P A 1
C18A C 0.1334(11) 0.8159(15) 0.4741(7) 0.027(2) Uani 0.644(8) 1 d . . P A 1
H6A H 0.107304 0.881471 0.434986 0.032 Uiso 0.644(8) 1 calc R U P A 1
H6B H 0.102284 0.854874 0.512818 0.032 Uiso 0.644(8) 1 calc R U P A 1
Cl4B Cl 0.2849(5) 0.6717(15) 0.4739(3) 0.084(4) Uani 0.356(8) 1 d . . P A 2
C18B C 0.167(3) 0.773(3) 0.4832(18) 0.051(9) Uani 0.356(8) 1 d . . P A 2
H77A H 0.177711 0.821194 0.527969 0.061 Uiso 0.356(8) 1 calc R U P A 2
H77B H 0.153527 0.853060 0.448736 0.061 Uiso 0.356(8) 1 calc R U P A 2
Cl3B Cl 0.0565(7) 0.6538(15) 0.4750(6) 0.062(3) Uani 0.356(8) 1 d . . P A 2
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'
Cl Cl 0.1484 0.1585 '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'
Os Os -1.2165 7.6030 '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
O1 Os1 O2 81.35(14) . . ?
O1 Os1 N2 86.95(15) . . ?
O2 Os1 N2 87.66(14) . . ?
O1 Os1 N1 88.22(15) . . ?
O2 Os1 N1 88.64(16) . . ?
N2 Os1 N1 174.31(16) . . ?
O1 Os1 Cl1 92.88(10) . . ?
O2 Os1 Cl1 174.22(11) . . ?
N2 Os1 Cl1 91.55(11) . . ?
N1 Os1 Cl1 91.70(13) . . ?
O1 Os1 Cl2 174.33(10) . . ?
O2 Os1 Cl2 93.00(11) . . ?
N2 Os1 Cl2 92.31(12) . . ?
N1 Os1 Cl2 92.20(12) . . ?
Cl1 Os1 Cl2 92.76(4) . . ?
C11 O1 Os1 110.9(3) . . ?
C12 O2 Os1 111.6(3) . . ?
C1 N1 C5 118.6(4) . . ?
C1 N1 Os1 122.0(3) . . ?
C5 N1 Os1 119.4(3) . . ?
C10 N2 C6 118.9(4) . . ?
C10 N2 Os1 121.8(3) . . ?
C6 N2 Os1 119.2(3) . . ?
C14 N3 C16 122.1(5) . . ?
C14 N3 C15 118.6(5) . . ?
C16 N3 C15 119.3(5) . . ?
N1 C1 C2 121.9(5) . . ?
C1 C2 C3 120.3(5) . . ?
C2 C3 C4 117.6(5) . . ?
C5 C4 C3 119.0(5) . . ?
N1 C5 C4 122.6(5) . . ?
N2 C6 C7 122.5(5) . . ?
C8 C7 C6 118.7(5) . . ?
C7 C8 C9 118.2(5) . . ?
C10 C9 C8 120.1(5) . . ?
N2 C10 C9 121.5(5) . . ?
O1 C11 C16 121.6(5) . . ?
O1 C11 C12 118.2(4) . . ?
C16 C11 C12 120.1(5) . . ?
O2 C12 C13 123.9(5) . . ?
O2 C12 C11 117.8(4) . . ?
C13 C12 C11 118.3(4) . . ?
C14 C13 C12 119.4(5) . . ?
N3 C14 C13 121.5(5) . . ?
N3 C16 C11 118.7(5) . . ?
N3 C16 C17 120.5(5) . . ?
C11 C16 C17 120.9(5) . . ?
Cl4A C18A Cl3A 111.1(8) . . ?
Cl3B C18B Cl4B 110.1(16) . . ?
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
Os1 O1 2.039(3) . ?
Os1 O2 2.059(3) . ?
Os1 N2 2.080(4) . ?
Os1 N1 2.091(4) . ?
Os1 Cl1 2.3618(12) . ?
Os1 Cl2 2.3775(12) . ?
O1 C11 1.331(6) . ?
O2 C12 1.300(6) . ?
N1 C1 1.340(6) . ?
N1 C5 1.349(6) . ?
N2 C10 1.340(6) . ?
N2 C6 1.342(6) . ?
N3 C14 1.343(7) . ?
N3 C16 1.376(7) . ?
N3 C15 1.491(7) . ?
C1 C2 1.377(8) . ?
C2 C3 1.390(8) . ?
C3 C4 1.399(8) . ?
C4 C5 1.380(7) . ?
C6 C7 1.394(7) . ?
C7 C8 1.387(8) . ?
C8 C9 1.387(8) . ?
C9 C10 1.386(7) . ?
C11 C16 1.385(7) . ?
C11 C12 1.435(7) . ?
C12 C13 1.400(7) . ?
C13 C14 1.375(8) . ?
C16 C17 1.492(8) . ?
Cl3A C18A 1.765(14) . ?
Cl4A C18A 1.754(14) . ?
Cl4B C18B 1.75(3) . ?
C18B Cl3B 1.71(4) . ?
