#------------------------------------------------------------------------------
#$Date: 2025-08-21 14:03:24 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301848 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/25/7022597.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_7022597
loop_
_publ_author_name
'Bhargavi, G.'
'Rajasekharan, M. V.'
'Costes, J.-P.'
'Tuchagues, J.-P.'
_publ_section_title
;
 A new end-on azido bridged Mn(III) single-chain magnet and its dimeric
 single molecule magnet polymorph. Synthesis, structure and magnetic
 properties of [Mn(5-Clsalpn)N3]n and phenoxo bridged [Mn(5-Clsalpn)N3]2.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8113
_journal_page_last               8123
_journal_paper_doi               10.1039/c3dt31966k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C17 H14 Cl2 Mn N5 O2'
_chemical_formula_sum            'C17 H14 Cl2 Mn N5 O2'
_chemical_formula_weight         446.17
_chemical_name_common            '[Mn(5-Clsalpn)N3]n'
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.162(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.035(4)
_cell_length_b                   8.5326(14)
_cell_length_c                   19.386(3)
_cell_measurement_reflns_used    7175
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.29
_cell_volume                     3627.4(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20426
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.736
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0491P)²+3.5042P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                3921
_reflns_number_total             4344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt31966k.txt
_cod_data_source_block           compound-1a
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7022597
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Mn Mn 0.248976(11) 0.30068(3) 0.244061(13) 0.02321(9) Uani 1 1 d .
Cl1 Cl 0.04803(3) -0.03568(9) 0.38932(4) 0.0625(2) Uani 1 1 d .
Cl2 Cl 0.54915(3) -0.02603(11) 0.39917(5) 0.0794(3) Uani 1 1 d .
O1 O 0.21507(6) 0.35388(14) 0.31291(7) 0.0283(3) Uani 1 1 d .
O2 O 0.32771(5) 0.35033(15) 0.31815(7) 0.0296(3) Uani 1 1 d .
N1 N 0.16536(7) 0.22090(17) 0.17180(8) 0.0275(3) Uani 1 1 d .
N2 N 0.28854(7) 0.22236(17) 0.17580(8) 0.0285(3) Uani 1 1 d .
N3 N 0.23297(7) 0.53988(17) 0.19522(8) 0.0286(3) Uani 1 1 d .
N4 N 0.21230(7) 0.56416(17) 0.12821(9) 0.0302(3) Uani 1 1 d .
N5 N 0.19267(10) 0.5909(2) 0.06459(10) 0.0478(5) Uani 1 1 d .
C1 C 0.17682(8) 0.2648(2) 0.32826(10) 0.0267(3) Uani 1 1 d .
C2 C 0.17809(9) 0.2678(2) 0.40112(10) 0.0321(4) Uani 1 1 d .
H2 H 0.2064 0.3341 0.4384 0.039 Uiso 1 1 calc R
C3 C 0.13903(9) 0.1763(2) 0.41956(11) 0.0360(4) Uani 1 1 d .
H3 H 0.1407 0.1787 0.4694 0.043 Uiso 1 1 calc R
C4 C 0.09714(9) 0.0803(3) 0.36496(12) 0.0386(4) Uani 1 1 d .
C5 C 0.09308(9) 0.0771(2) 0.29238(12) 0.0376(4) Uani 1 1 d .
H5 H 0.0633 0.0137 0.2553 0.045 Uiso 1 1 calc R
C6 C 0.13325(8) 0.1683(2) 0.27329(10) 0.0300(4) Uani 1 1 d .
C7 C 0.12704(8) 0.1664(2) 0.19608(10) 0.0315(4) Uani 1 1 d .
H7 H 0.0910 0.1203 0.1597 0.038 Uiso 1 1 calc R
C8 C 0.14742(9) 0.2156(2) 0.08940(10) 0.0343(4) Uani 1 1 d .
H8A H 0.1418 0.3239 0.0695 0.041 Uiso 1 1 calc R
H8B H 0.1078 0.1606 0.0651 0.041 Uiso 1 1 calc R
C9 C 0.19422(10) 0.1329(2) 0.06855(10) 0.0367(4) Uani 1 1 d .
H9A H 0.2017 0.0273 0.0917 0.044 Uiso 1 1 calc R
H9B H 0.1770 0.1191 0.0130 0.044 Uiso 1 1 calc R
C10 C 0.25473(10) 0.2173(2) 0.09303(10) 0.0359(4) Uani 1 1 d .
H10A H 0.2800 0.1638 0.0707 0.043 Uiso 1 1 calc R
H10B H 0.2474 0.3258 0.0732 0.043 Uiso 1 1 calc R
C11 C 0.34323(9) 0.1685(2) 0.20257(11) 0.0334(4) Uani 1 1 d .
H11 H 0.3568 0.1232 0.1674 0.040 Uiso 1 1 calc R
C12 C 0.38606(9) 0.1698(2) 0.28057(11) 0.0337(4) Uani 1 1 d .
C13 C 0.43986(10) 0.0816(3) 0.30090(13) 0.0433(5) Uani 1 1 d .
H13 H 0.4466 0.0207 0.2640 0.052 Uiso 1 1 calc R
C14 C 0.48248(10) 0.0836(3) 0.37389(14) 0.0475(5) Uani 1 1 d .
C15 C 0.47392(10) 0.1738(3) 0.42840(13) 0.0452(5) Uani 1 1 d .
H15 H 0.5038 0.1738 0.4790 0.054 Uiso 1 1 calc R
C16 C 0.42206(9) 0.2632(3) 0.40890(11) 0.0377(4) Uani 1 1 d .
H16 H 0.4169 0.3264 0.4462 0.045 Uiso 1 1 calc R
C17 C 0.37651(8) 0.2627(2) 0.33470(10) 0.0291(4) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
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
_geom_angle_publ_flag
O1 Mn O2 89.80(6) . y
O1 Mn N2 174.10(6) . y
O2 Mn N2 88.78(6) . y
O1 Mn N1 88.66(6) . y
O2 Mn N1 172.62(6) . y
N2 Mn N1 92.01(6) . y
O1 Mn N3 91.78(6) . y
O2 Mn N3 93.59(6) . y
N2 Mn N3 94.03(6) . y
N1 Mn N3 93.67(6) . y
O1 Mn N3 85.53(5) 4_545 y
O2 Mn N3 85.08(5) 4_545 y
N2 Mn N3 88.64(6) 4_545 y
N1 Mn N3 87.60(6) 4_545 y
N3 Mn N3 177.00(3) 4_545 y
C1 O1 Mn 124.45(11) . ?
C17 O2 Mn 124.84(12) . ?
C7 N1 C8 116.83(15) . ?
C7 N1 Mn 121.54(12) . ?
C8 N1 Mn 121.55(12) . ?
C11 N2 C10 116.53(16) . ?
C11 N2 Mn 121.91(13) . ?
C10 N2 Mn 121.49(12) . ?
N4 N3 Mn 122.84(12) . y
N4 N3 Mn 105.87(11) 4 y
Mn N3 Mn 131.29(7) 4 y
N5 N4 N3 178.46(19) . y
O1 C1 C2 119.20(16) . ?
O1 C1 C6 122.43(16) . ?
C2 C1 C6 118.36(17) . ?
C3 C2 C1 121.06(18) . ?
C3 C2 H2 119.5 . ?
C1 C2 H2 119.5 . ?
C2 C3 C4 119.68(18) . ?
C2 C3 H3 120.2 . ?
C4 C3 H3 120.2 . ?
C5 C4 C3 121.22(18) . ?
C5 C4 Cl1 119.63(17) . ?
C3 C4 Cl1 119.14(16) . ?
C4 C5 C6 119.52(19) . ?
C4 C5 H5 120.2 . ?
C6 C5 H5 120.2 . ?
C5 C6 C1 120.12(17) . ?
C5 C6 C7 118.55(17) . ?
C1 C6 C7 121.27(17) . ?
N1 C7 C6 126.36(17) . ?
N1 C7 H7 116.8 . ?
C6 C7 H7 116.8 . ?
N1 C8 C9 112.53(15) . ?
N1 C8 H8A 109.1 . ?
C9 C8 H8A 109.1 . ?
N1 C8 H8B 109.1 . ?
C9 C8 H8B 109.1 . ?
H8A C8 H8B 107.8 . ?
C10 C9 C8 114.67(16) . ?
C10 C9 H9A 108.6 . ?
C8 C9 H9A 108.6 . ?
C10 C9 H9B 108.6 . ?
C8 C9 H9B 108.6 . ?
H9A C9 H9B 107.6 . ?
N2 C10 C9 112.71(15) . ?
N2 C10 H10A 109.0 . ?
C9 C10 H10A 109.0 . ?
N2 C10 H10B 109.0 . ?
C9 C10 H10B 109.0 . ?
H10A C10 H10B 107.8 . ?
N2 C11 C12 126.52(18) . ?
N2 C11 H11 116.7 . ?
C12 C11 H11 116.7 . ?
C13 C12 C17 120.31(19) . ?
C13 C12 C11 118.06(19) . ?
C17 C12 C11 121.55(17) . ?
C14 C13 C12 119.8(2) . ?
C14 C13 H13 120.1 . ?
C12 C13 H13 120.1 . ?
C13 C14 C15 120.9(2) . ?
C13 C14 Cl2 119.84(19) . ?
C15 C14 Cl2 119.25(18) . ?
C16 C15 C14 119.9(2) . ?
C16 C15 H15 120.1 . ?
C14 C15 H15 120.1 . ?
C15 C16 C17 121.2(2) . ?
C15 C16 H16 119.4 . ?
C17 C16 H16 119.4 . ?
O2 C17 C16 119.39(17) . ?
O2 C17 C12 122.67(17) . ?
C16 C17 C12 117.93(18) . ?
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
Mn O1 1.8820(12) . y
Mn O2 1.8969(13) . y
Mn N2 2.0328(15) . y
Mn N1 2.0397(15) . y
Mn N3 2.2163(15) . y
Mn N3 2.4714(15) 4_545 y
Cl1 C4 1.747(2) . ?
Cl2 C14 1.744(2) . ?
O1 C1 1.317(2) . ?
O2 C17 1.315(2) . ?
N1 C7 1.281(2) . ?
N1 C8 1.475(2) . ?
N2 C11 1.285(2) . ?
N2 C10 1.473(2) . ?
N3 N4 1.204(2) . y
N3 Mn 2.4714(15) 4 ?
N4 N5 1.149(2) . y
C1 C2 1.400(2) . ?
C1 C6 1.413(3) . ?
C2 C3 1.376(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.370(3) . ?
C5 C6 1.402(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.442(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.516(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.514(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.439(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.406(3) . ?
C12 C17 1.407(3) . ?
C13 C14 1.366(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.389(3) . ?
C15 C16 1.376(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.407(3) . ?
C16 H16 0.9500 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168347925
