#------------------------------------------------------------------------------
#$Date: 2022-10-12 03:29:51 +0200 (Wed 12 de Oct de 2022) $
#$Revision: 278542 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/56/7245661.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_7245661
loop_
_publ_author_name
'Darii, Mariana'
'Mikosch, Annabel'
'van Leusen, Jan'
'Kravtsov, Victor Ch.'
'Dvornina, Elena G.'
'Clapco, Steliana T.'
'Ciloci, Alexandra'
'Kögerler, Paul'
'Baca, Svetlana G.'
_publ_section_title
;
 FeII/III and MnII complexes based on 2,4,6-tris(2-pyridyl)-triazine:
 synthesis, structures, magnetic and biological properties
;
_journal_issue                   45
_journal_name_full               'RSC Advances'
_journal_page_first              29034
_journal_page_last               29047
_journal_paper_doi               10.1039/D2RA04868J
_journal_volume                  12
_journal_year                    2022
_chemical_formula_sum            'C18 H16 Cl2 Fe N6 O2'
_chemical_formula_weight         475.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2021-09-09 deposited with the CCDC.	2022-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                106.09(3)
_cell_angle_beta                 99.73(3)
_cell_angle_gamma                100.60(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7197(17)
_cell_length_b                   9.1076(18)
_cell_length_c                   13.374(3)
_cell_measurement_reflns_used    5079
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.44
_cell_measurement_theta_min      1.63
_cell_volume                     975.5(4)
_computing_cell_refinement
; 
   STOE & Cie GmbH 
   Hilpertstr. 10 
   D-64295 Darmstadt 
   Germany 
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
; 
   STOE & Cie GmbH 
   Hilpertstr. 10 
   D-64295 Darmstadt 
   Germany 
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
; 
   STOE & Cie GmbH 
   Hilpertstr. 10 
   D-64295 Darmstadt 
   Germany 
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material
; 
   STOE & Cie GmbH 
   Hilpertstr. 10 
   D-64295 Darmstadt 
   Germany
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.90, Darmstadt 2020 
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12311
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.400
_diffrn_source                   'Genix Mo'
_exptl_absorpt_coefficient_mu    1.075
_exptl_absorpt_correction_T_max  0.1644
_exptl_absorpt_correction_T_min  0.0556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
   STOE & Cie GmbH 
   Hilpertstr. 10 
   D-64295 Darmstadt 
   Germany 
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.682
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[σ²(Fo²)+(0.1821P)²+0.3387P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2299
_refine_ls_wR_factor_ref         0.2377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2976
_reflns_number_total             3438
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ra04868j2.cif
_cod_data_source_block           am-343_a
_cod_database_code               7245661
_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. 
;
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Fe1 Fe 0.56193(7) 0.53631(7) 0.85578(5) 0.0456(3) Uani 1 1 d . . . . .
Cl1 Cl 0.65308(13) 0.59524(14) 0.71422(9) 0.0499(4) Uani 1 1 d . . . . .
Cl2 Cl 0.73477(14) 0.71086(14) 1.00874(9) 0.0537(4) Uani 1 1 d . . . . .
C1 C 0.3557(6) 0.7916(6) 0.8941(4) 0.0507(11) Uani 1 1 d . . . . .
H1 H 0.4544 0.8611 0.9305 0.061 Uiso 1 1 calc R U . . .
C2 C 0.2220(6) 0.8512(6) 0.8847(4) 0.0530(11) Uani 1 1 d . . . . .
H2 H 0.2301 0.9583 0.9146 0.064 Uiso 1 1 calc R U . . .
C3 C 0.0753(6) 0.7489(6) 0.8299(4) 0.0538(11) Uani 1 1 d . . . . .
H3 H -0.0170 0.7861 0.8222 0.065 Uiso 1 1 calc R U . . .
C4 C 0.0674(6) 0.5899(6) 0.7867(4) 0.0493(10) Uani 1 1 d . . . . .
H4 H -0.0302 0.5188 0.7499 0.059 Uiso 1 1 calc R U . . .
C5 C 0.2065(5) 0.5392(5) 0.7991(4) 0.0450(10) Uani 1 1 d . . . . .
C6 C 0.2117(5) 0.3712(5) 0.7593(4) 0.0453(10) Uani 1 1 d . . . . .
C7 C 0.1045(5) 0.1114(5) 0.6805(4) 0.0453(10) Uani 1 1 d . . . . .
C8 C 0.3699(5) 0.1988(5) 0.7559(4) 0.0446(10) Uani 1 1 d . . . . .
C9 C 0.5317(5) 0.1803(5) 0.7930(4) 0.0439(9) Uani 1 1 d . . . . .
C10 C 0.5652(5) 0.0334(6) 0.7755(4) 0.0477(10) Uani 1 1 d . . . . .
H10 H 0.4862 -0.0584 0.7377 0.057 Uiso 1 1 calc R U . . .
C11 C 0.7207(5) 0.0279(6) 0.8163(4) 0.0513(11) Uani 1 1 d . . . . .
H11 H 0.7476 -0.0684 0.8066 0.062 Uiso 1 1 calc R U . . .
C12 C 0.8358(5) 0.1678(6) 0.8717(4) 0.0500(11) Uani 1 1 d . . . . .
H12 H 0.9408 0.1664 0.8990 0.060 Uiso 1 1 calc R U . . .
C13 C 0.7914(5) 0.3085(6) 0.8854(4) 0.0498(11) Uani 1 1 d . . . . .
H13 H 0.8684 0.4017 0.9231 0.060 Uiso 1 1 calc R U . . .
C14 C -0.0315(5) -0.0237(5) 0.6181(4) 0.0460(10) Uani 1 1 d . . . . .
C15 C -0.0102(5) -0.1769(6) 0.5887(4) 0.0475(10) Uani 1 1 d . . . . .
H15 H 0.0896 -0.1963 0.6088 0.057 Uiso 1 1 calc R U . . .
C16 C -0.1405(6) -0.2983(6) 0.5295(4) 0.0517(11) Uani 1 1 d . . . . .
H16 H -0.1300 -0.4015 0.5096 0.062 Uiso 1 1 calc R U . . .
C17 C -0.2871(5) -0.2662(6) 0.4997(4) 0.0501(11) Uani 1 1 d . . . . .
H17 H -0.3766 -0.3467 0.4596 0.060 Uiso 1 1 calc R U . . .
C18 C -0.2966(5) -0.1104(6) 0.5315(4) 0.0496(11) Uani 1 1 d . . . . .
H18 H -0.3951 -0.0885 0.5112 0.059 Uiso 1 1 calc R U . . .
N1 N 0.3505(4) 0.6383(4) 0.8534(3) 0.0472(9) Uani 1 1 d . . . . .
N2 N 0.3586(4) 0.3483(4) 0.7797(3) 0.0458(9) Uani 1 1 d . . . . .
N3 N 0.6426(4) 0.3165(4) 0.8468(3) 0.0456(8) Uani 1 1 d . . . . .
N4 N 0.0805(4) 0.2577(4) 0.7091(3) 0.0452(9) Uani 1 1 d . . . . .
N5 N 0.2468(4) 0.0760(5) 0.7062(3) 0.0466(9) Uani 1 1 d . . . . .
N6 N -0.1726(4) 0.0103(5) 0.5895(3) 0.0473(9) Uani 1 1 d . . . . .
O1 O 0.3202(4) 0.6767(4) 0.6161(3) 0.0589(9) Uani 1 1 d . . . . .
H1A H 0.3326 0.7161 0.5624 0.071 Uiso 1 1 d R U . . .
H1B H 0.4141 0.6614 0.6407 0.071 Uiso 1 1 d R U . . .
O2 O 0.3176(4) 0.7435(4) 0.4255(3) 0.0623(9) Uani 1 1 d . . . . .
H2A H 0.2984 0.6519 0.3727 0.075 Uiso 1 1 d R U . . .
H2B H 0.2484 0.7771 0.3969 0.075 Uiso 1 1 d 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'
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
N2 Fe1 N1 73.07(14) . . ?
N2 Fe1 N3 73.40(14) . . ?
N1 Fe1 N3 144.01(14) . . ?
N2 Fe1 Cl2 150.44(12) . . ?
N1 Fe1 Cl2 100.83(11) . . ?
N3 Fe1 Cl2 101.82(11) . . ?
N2 Fe1 Cl1 103.62(12) . . ?
N1 Fe1 Cl1 100.67(11) . . ?
N3 Fe1 Cl1 99.54(11) . . ?
Cl2 Fe1 Cl1 105.94(5) . . ?
N1 C1 C2 123.1(4) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C1 C2 C3 118.7(5) . . ?
C1 C2 H2 120.6 . . ?
C3 C2 H2 120.6 . . ?
C2 C3 C4 119.1(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 118.8(4) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 122.5(4) . . ?
N1 C5 C6 113.9(4) . . ?
C4 C5 C6 123.5(4) . . ?
N4 C6 N2 124.5(4) . . ?
N4 C6 C5 121.9(4) . . ?
N2 C6 C5 113.6(4) . . ?
N4 C7 N5 124.7(4) . . ?
N4 C7 C14 119.6(4) . . ?
N5 C7 C14 115.7(4) . . ?
N5 C8 N2 123.8(4) . . ?
N5 C8 C9 121.9(4) . . ?
N2 C8 C9 114.2(4) . . ?
N3 C9 C10 123.2(4) . . ?
N3 C9 C8 114.8(4) . . ?
C10 C9 C8 122.0(4) . . ?
C9 C10 C11 117.8(4) . . ?
C9 C10 H10 121.1 . . ?
C11 C10 H10 121.1 . . ?
C10 C11 C12 119.4(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C13 C12 C11 118.8(4) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
N3 C13 C12 122.8(4) . . ?
N3 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
N6 C14 C15 122.9(4) . . ?
N6 C14 C7 116.3(4) . . ?
C15 C14 C7 120.7(4) . . ?
C16 C15 C14 118.4(4) . . ?
C16 C15 H15 120.8 . . ?
C14 C15 H15 120.8 . . ?
C15 C16 C17 119.7(4) . . ?
C15 C16 H16 120.1 . . ?
C17 C16 H16 120.1 . . ?
C16 C17 C18 118.0(4) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
N6 C18 C17 123.8(4) . . ?
N6 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
C1 N1 C5 117.7(4) . . ?
C1 N1 Fe1 125.1(3) . . ?
C5 N1 Fe1 116.9(3) . . ?
C6 N2 C8 116.6(4) . . ?
C6 N2 Fe1 122.1(3) . . ?
C8 N2 Fe1 121.2(3) . . ?
C13 N3 C9 118.0(4) . . ?
C13 N3 Fe1 125.8(3) . . ?
C9 N3 Fe1 116.1(3) . . ?
C6 N4 C7 114.8(4) . . ?
C8 N5 C7 115.2(4) . . ?
C18 N6 C14 117.2(4) . . ?
H1A O1 H1B 105.9 . . ?
H2A O2 H2B 96.2 . . ?
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
Fe1 N2 2.102(4) . ?
Fe1 N1 2.211(4) . ?
Fe1 N3 2.220(4) . ?
Fe1 Cl2 2.2930(17) . ?
Fe1 Cl1 2.3278(14) . ?
C1 N1 1.340(6) . ?
C1 C2 1.375(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.381(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.386(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.375(6) . ?
C4 H4 0.9300 . ?
C5 N1 1.353(6) . ?
C5 C6 1.486(6) . ?
C6 N4 1.323(6) . ?
C6 N2 1.331(6) . ?
C7 N4 1.346(6) . ?
C7 N5 1.351(6) . ?
C7 C14 1.475(6) . ?
C8 N5 1.323(6) . ?
C8 N2 1.337(6) . ?
C8 C9 1.470(6) . ?
C9 N3 1.350(6) . ?
C9 C10 1.387(7) . ?
C10 C11 1.388(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.391(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.379(7) . ?
C12 H12 0.9300 . ?
C13 N3 1.336(6) . ?
C13 H13 0.9300 . ?
C14 N6 1.342(6) . ?
C14 C15 1.397(6) . ?
C15 C16 1.374(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.380(7) . ?
C16 H16 0.9300 . ?
C17 C18 1.387(7) . ?
C17 H17 0.9300 . ?
C18 N6 1.337(6) . ?
C18 H18 0.9300 . ?
O1 H1A 0.9000 . ?
O1 H1B 0.8797 . ?
O2 H2A 0.8966 . ?
O2 H2B 0.8112 . ?
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 H1A O2 0.90 1.90 2.777(6) 163.7 .
O1 H1B Cl1 0.88 2.40 3.278(4) 173.2 .
O2 H2A Cl1 0.90 2.38 3.214(4) 154.8 2_666
O2 H2B N6 0.81 2.13 2.806(5) 140.8 2_566
