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#$Date: 2023-06-29 13:46:44 +0300 (Thu, 29 Jun 2023) $
#$Revision: 284609 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/32/7713254.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_7713254
loop_
_publ_author_name
'Jakopec, Silvio'
'Gourdon-Grünewaldt, Lisa'
'Čipor, Ivona'
'Meščić Macan, Andrijana'
'Perić, Berislav'
'Piantanida, Ivo'
'Cariou, Kevin'
'Gasser, Gilles'
'Kirin, Srećko I'
'Raić-Malić, Silvana'
_publ_section_title
;
 Synthesis, characterisation and biological evaluation of monometallic
 Re(I) and heterobimetallic Re(I)/Fe(II) complexes with a 1,2,3-triazolyl
 pyridine chelating moiety.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01070h
_journal_year                    2023
_chemical_formula_moiety         'C18 H16 Fe N4'
_chemical_formula_sum            'C18 H16 Fe N4'
_chemical_formula_weight         344.20
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-04-06 deposited with the CCDC.	2023-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.1180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.84340(10)
_cell_length_b                   28.9507(4)
_cell_length_c                   9.35340(10)
_cell_measurement_reflns_used    4194
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.6050
_cell_measurement_theta_min      5.0200
_cell_volume                     1562.33(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.4323
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Xcalibur, Ruby, Nova'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.898
_diffrn_reflns_theta_min         3.053
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    7.763
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       needle
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0421
_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)+(0.0671P)²+0.2576P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2904
_reflns_number_total             3231
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt01070h2.cif
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7713254
_shelx_shelxl_version_number     2018/3
_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.
;
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.1137(4) 0.54127(8) 0.2994(2) 0.0511(5) Uani 1 1 d . . . . .
C2 C 0.0754(6) 0.50548(11) 0.2091(3) 0.0657(8) Uani 1 1 d . . . . .
H2 H 0.189187 0.498196 0.153610 0.079 Uiso 1 1 calc R U . . .
C3 C -0.1210(7) 0.47862(10) 0.1924(4) 0.0713(9) Uani 1 1 d . . . . .
H3 H -0.137834 0.453607 0.129234 0.086 Uiso 1 1 calc R U . . .
C4 C -0.2905(6) 0.48972(10) 0.2712(4) 0.0694(9) Uani 1 1 d . . . . .
H4 H -0.425827 0.472317 0.262029 0.083 Uiso 1 1 calc R U . . .
C5 C -0.2605(5) 0.52680(9) 0.3645(3) 0.0527(6) Uani 1 1 d . . . . .
H5 H -0.374898 0.534991 0.418514 0.063 Uiso 1 1 calc R U . . .
C6 C -0.0551(4) 0.55168(8) 0.3759(2) 0.0407(5) Uani 1 1 d . . . . .
C9 C -0.0068(4) 0.59060(8) 0.4767(2) 0.0397(5) Uani 1 1 d . . . . .
N10 N -0.1752(4) 0.61109(8) 0.5397(2) 0.0515(5) Uani 1 1 d . . . . .
N11 N -0.0781(4) 0.64285(9) 0.6309(2) 0.0548(5) Uani 1 1 d . . . . .
N12 N 0.1491(4) 0.64237(7) 0.62532(19) 0.0447(4) Uani 1 1 d . . . . .
C13 C 0.2003(4) 0.61071(8) 0.5311(2) 0.0426(5) Uani 1 1 d . . . . .
H13 H 0.345380 0.603863 0.507706 0.051 Uiso 1 1 calc R U . . .
C14 C 0.3080(5) 0.66966(8) 0.7317(3) 0.0515(6) Uani 1 1 d . . . . .
H14A H 0.228646 0.697059 0.757949 0.062 Uiso 1 1 calc R U . . .
H14B H 0.440178 0.679510 0.688358 0.062 Uiso 1 1 calc R U . . .
C15 C 0.3903(4) 0.64189(7) 0.8645(2) 0.0372(4) Uani 1 1 d . . . . .
C16 C 0.2655(4) 0.63225(8) 0.9808(3) 0.0443(5) Uani 1 1 d . . . . .
H16 H 0.116171 0.642122 0.987628 0.053 Uiso 1 1 calc R U . . .
C17 C 0.4102(5) 0.60493(9) 1.0838(2) 0.0512(6) Uani 1 1 d . . . . .
H17 H 0.372492 0.594025 1.170678 0.061 Uiso 1 1 calc R U . . .
C18 C 0.6208(5) 0.59711(8) 1.0323(3) 0.0492(6) Uani 1 1 d . . . . .
H18 H 0.745662 0.580117 1.079051 0.059 Uiso 1 1 calc R U . . .
C19 C 0.6093(4) 0.61957(8) 0.8970(2) 0.0422(5) Uani 1 1 d . . . . .
H19 H 0.724968 0.619723 0.839261 0.051 Uiso 1 1 calc R U . . .
Fe20 Fe 0.56433(6) 0.66666(2) 1.05413(3) 0.03615(13) Uani 1 1 d . . . . .
C21 C 0.5849(5) 0.73697(9) 1.0367(3) 0.0620(8) Uani 1 1 d . . . . .
H21 H 0.519029 0.754745 0.958007 0.074 Uiso 1 1 calc R U . . .
C22 C 0.4787(5) 0.72441(11) 1.1588(4) 0.0670(9) Uani 1 1 d . . . . .
H22 H 0.330273 0.732363 1.173984 0.080 Uiso 1 1 calc R U . . .
C23 C 0.6412(6) 0.69764(12) 1.2522(3) 0.0670(8) Uani 1 1 d . . . . .
H23 H 0.618278 0.685028 1.340284 0.080 Uiso 1 1 calc R U . . .
C24 C 0.8412(5) 0.69340(10) 1.1898(3) 0.0605(7) Uani 1 1 d . . . . .
H24 H 0.974309 0.677368 1.229045 0.073 Uiso 1 1 calc R U . . .
C25 C 0.8084(5) 0.71727(9) 1.0585(3) 0.0578(6) Uani 1 1 d . . . . .
H25 H 0.916221 0.719762 0.995631 0.069 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'
Fe Fe -1.1336 3.1974 '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'
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
C2 N1 C6 116.7(3) . . ?
N1 C2 C3 124.4(3) . . ?
C4 C3 C2 118.1(3) . . ?
C3 C4 C5 119.7(3) . . ?
C4 C5 C6 118.3(3) . . ?
N1 C6 C5 122.8(2) . . ?
N1 C6 C9 115.6(2) . . ?
C5 C6 C9 121.6(2) . . ?
N10 C9 C13 108.1(2) . . ?
N10 C9 C6 122.3(2) . . ?
C13 C9 C6 129.4(2) . . ?
N11 N10 C9 108.5(2) . . ?
N10 N11 N12 107.2(2) . . ?
N11 N12 C13 111.1(2) . . ?
N11 N12 C14 119.4(2) . . ?
C13 N12 C14 128.9(2) . . ?
N12 C13 C9 105.1(2) . . ?
N12 C14 C15 110.93(18) . . ?
C19 C15 C16 107.39(19) . . ?
C19 C15 C14 125.6(2) . . ?
C16 C15 C14 127.0(2) . . ?
C19 C15 Fe20 70.41(12) . . ?
C16 C15 Fe20 69.50(12) . . ?
C14 C15 Fe20 125.95(15) . . ?
C17 C16 C15 107.7(2) . . ?
C17 C16 Fe20 69.89(14) . . ?
C15 C16 Fe20 69.30(12) . . ?
C18 C17 C16 108.4(2) . . ?
C18 C17 Fe20 70.48(14) . . ?
C16 C17 Fe20 69.36(13) . . ?
C17 C18 C19 108.2(2) . . ?
C17 C18 Fe20 69.27(14) . . ?
C19 C18 Fe20 69.70(13) . . ?
C18 C19 C15 108.3(2) . . ?
C18 C19 Fe20 70.02(13) . . ?
C15 C19 Fe20 68.80(12) . . ?
C15 Fe20 C16 41.20(9) . . ?
C15 Fe20 C22 125.58(11) . . ?
C16 Fe20 C22 107.51(11) . . ?
C15 Fe20 C17 68.81(9) . . ?
C16 Fe20 C17 40.75(11) . . ?
C22 Fe20 C17 120.38(13) . . ?
C15 Fe20 C25 121.51(11) . . ?
C16 Fe20 C25 156.75(12) . . ?
C22 Fe20 C25 68.01(13) . . ?
C17 Fe20 C25 161.55(13) . . ?
C15 Fe20 C23 162.71(13) . . ?
C16 Fe20 C23 125.08(12) . . ?
C22 Fe20 C23 40.56(14) . . ?
C17 Fe20 C23 107.43(12) . . ?
C25 Fe20 C23 67.31(13) . . ?
C15 Fe20 C24 156.05(12) . . ?
C16 Fe20 C24 161.50(12) . . ?
C22 Fe20 C24 67.76(13) . . ?
C17 Fe20 C24 124.79(12) . . ?
C25 Fe20 C24 39.97(13) . . ?
C23 Fe20 C24 39.82(13) . . ?
C15 Fe20 C21 108.01(10) . . ?
C16 Fe20 C21 121.23(11) . . ?
C22 Fe20 C21 40.97(14) . . ?
C17 Fe20 C21 156.15(13) . . ?
C25 Fe20 C21 40.36(12) . . ?
C23 Fe20 C21 68.19(13) . . ?
C24 Fe20 C21 67.79(12) . . ?
C15 Fe20 C19 40.79(9) . . ?
C16 Fe20 C19 68.48(10) . . ?
C22 Fe20 C19 163.24(13) . . ?
C17 Fe20 C19 67.96(10) . . ?
C25 Fe20 C19 108.84(11) . . ?
C23 Fe20 C19 155.02(13) . . ?
C24 Fe20 C19 121.20(12) . . ?
C21 Fe20 C19 126.01(12) . . ?
C15 Fe20 C18 68.48(9) . . ?
C16 Fe20 C18 68.23(11) . . ?
C22 Fe20 C18 154.98(14) . . ?
C17 Fe20 C18 40.25(12) . . ?
C25 Fe20 C18 125.64(12) . . ?
C23 Fe20 C18 120.30(12) . . ?
C24 Fe20 C18 108.01(11) . . ?
C21 Fe20 C18 162.49(14) . . ?
C19 Fe20 C18 40.28(10) . . ?
C25 C21 C22 106.9(3) . . ?
C25 C21 Fe20 69.57(15) . . ?
C22 C21 Fe20 69.22(16) . . ?
C23 C22 C21 107.4(3) . . ?
C23 C22 Fe20 69.87(16) . . ?
C21 C22 Fe20 69.81(15) . . ?
C24 C23 C22 108.4(3) . . ?
C24 C23 Fe20 70.10(15) . . ?
C22 C23 Fe20 69.57(15) . . ?
C23 C24 C25 108.6(3) . . ?
C23 C24 Fe20 70.07(15) . . ?
C25 C24 Fe20 69.90(15) . . ?
C24 C25 C21 108.8(3) . . ?
C24 C25 Fe20 70.13(16) . . ?
C21 C25 Fe20 70.07(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
N1 C2 1.333(4) . ?
N1 C6 1.341(3) . ?
C2 C3 1.375(5) . ?
C3 C4 1.363(5) . ?
C4 C5 1.377(4) . ?
C5 C6 1.389(3) . ?
C6 C9 1.467(3) . ?
C9 N10 1.361(3) . ?
C9 C13 1.366(3) . ?
N10 N11 1.320(3) . ?
N11 N12 1.337(3) . ?
N12 C13 1.338(3) . ?
N12 C14 1.478(3) . ?
C14 C15 1.494(3) . ?
C15 C19 1.423(3) . ?
C15 C16 1.430(3) . ?
C15 Fe20 2.0302(19) . ?
C16 C17 1.418(4) . ?
C16 Fe20 2.033(2) . ?
C17 C18 1.409(4) . ?
C17 Fe20 2.040(2) . ?
C18 C19 1.414(3) . ?
C18 Fe20 2.056(2) . ?
C19 Fe20 2.052(2) . ?
Fe20 C22 2.039(3) . ?
Fe20 C25 2.041(3) . ?
Fe20 C23 2.043(2) . ?
Fe20 C24 2.044(2) . ?
Fe20 C21 2.047(3) . ?
C21 C25 1.410(4) . ?
C21 C22 1.430(5) . ?
C22 C23 1.415(5) . ?
C23 C24 1.392(5) . ?
C24 C25 1.396(4) . ?
