#------------------------------------------------------------------------------
#$Date: 2025-08-18 17:33:07 +0200 (Mon 18 de Aug de 2025) $
#$Revision: 301779 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/34/1543487.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_1543487
loop_
_publ_author_name
'Zhang, Yuan-Zhu'
'Gómez-Coca, Silvia'
'Brown, Andrew J.'
'Saber, Mohamed R.'
'Zhang, Xuan'
'Dunbar, Kim R.'
_publ_section_title
;
 Trigonal antiprismatic Co(ii) single molecule magnets with large uniaxial
 anisotropies: importance of Raman and tunneling mechanisms
;
_journal_issue                   10
_journal_name_full               'Chem. Sci.'
_journal_page_first              6519
_journal_paper_doi               10.1039/C6SC02035F
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C20 H20 Cl2 Co N12 O8'
_chemical_formula_weight         686.31
_chemical_name_common            Co(Tpm)2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-04 deposited with the CCDC.
2016-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.529(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.500(8)
_cell_length_b                   7.818(6)
_cell_length_c                   16.997(13)
_cell_measurement_reflns_used    3339
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.46
_cell_volume                     1356.6(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13000
_diffrn_reflns_theta_full        25.84
_diffrn_reflns_theta_max         25.84
_diffrn_reflns_theta_min         2.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_correction_T_min  0.7495
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             698
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.988
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0602
_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)+(0.1046P)²+2.5815P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1760
_reflns_number_gt                2092
_reflns_number_total             2603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6sc02035f2.cif
_cod_data_source_block           p21n
_cod_depositor_comments
'Adding full bibliography for 1543487--1543488.cif.'
_cod_original_cell_volume        1356.5(18)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               1543487
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 1.0000 1.0000 0.0000 0.0170(3) Uani 1 2 d S
N1 N 0.7529(3) 1.2010(4) -0.01205(19) 0.0191(7) Uani 1 1 d .
N2 N 0.8423(3) 1.1592(4) -0.0560(2) 0.0214(7) Uani 1 1 d .
N3 N 0.8915(3) 1.2019(4) 0.11907(19) 0.0202(7) Uani 1 1 d .
N4 N 1.0071(3) 1.1606(4) 0.1005(2) 0.0209(7) Uani 1 1 d .
N5 N 0.7666(3) 0.9536(4) 0.0705(2) 0.0207(7) Uani 1 1 d .
N6 N 0.8575(3) 0.8634(4) 0.04347(19) 0.0201(7) Uani 1 1 d .
C1 C 0.8059(4) 1.2467(5) -0.1243(2) 0.0250(9) Uani 1 1 d .
H1A H 0.8493 1.2428 -0.1674 0.030 Uiso 1 1 calc R
C2 C 0.6953(4) 1.3454(6) -0.1242(3) 0.0295(10) Uani 1 1 d .
H2A H 0.6505 1.4194 -0.1659 0.035 Uiso 1 1 calc R
C3 C 0.6651(4) 1.3138(5) -0.0523(2) 0.0234(9) Uani 1 1 d .
H3A H 0.5945 1.3625 -0.0338 0.028 Uiso 1 1 calc R
C4 C 1.0976(4) 1.2519(5) 0.1516(3) 0.0257(9) Uani 1 1 d .
H4A H 1.1888 1.2488 0.1535 0.031 Uiso 1 1 calc R
C5 C 1.0404(4) 1.3522(6) 0.2015(3) 0.0283(10) Uani 1 1 d .
H5A H 1.0838 1.4289 0.2424 0.034 Uiso 1 1 calc R
C6 C 0.9103(4) 1.3182(5) 0.1799(2) 0.0231(9) Uani 1 1 d .
H6A H 0.8446 1.3668 0.2031 0.028 Uiso 1 1 calc R
C7 C 0.8259(4) 0.7006(5) 0.0523(3) 0.0259(9) Uani 1 1 d .
H7A H 0.8721 0.6054 0.0381 0.031 Uiso 1 1 calc R
C8 C 0.7165(4) 0.6882(6) 0.0850(3) 0.0280(10) Uani 1 1 d .
H8A H 0.6754 0.5865 0.0971 0.034 Uiso 1 1 calc R
C9 C 0.6804(4) 0.8527(5) 0.0959(3) 0.0249(9) Uani 1 1 d .
H9A H 0.6088 0.8887 0.1172 0.030 Uiso 1 1 calc R
C10 C 0.7703(4) 1.1389(5) 0.0693(2) 0.0187(8) Uani 1 1 d .
H10A H 0.6966 1.1831 0.0917 0.022 Uiso 1 1 calc R
Cl1 Cl 1.51099(12) 0.25160(16) 0.17786(8) 0.0404(4) Uani 1 1 d .
O1 O 1.4656(8) 0.3409(8) 0.2345(3) 0.137(3) Uani 1 1 d .
O2 O 1.5346(3) 0.3574(4) 0.11455(18) 0.0305(7) Uani 1 1 d .
O3 O 1.6237(3) 0.1522(4) 0.21213(18) 0.0305(7) Uani 1 1 d .
O4 O 1.4076(4) 0.1326(8) 0.1408(4) 0.117(3) 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'
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'
Co Co 0.3494 0.9721 '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
N6 Co1 N6 180.00(15) . 3_775
N6 Co1 N4 84.91(13) . .
N6 Co1 N4 95.09(13) 3_775 .
N6 Co1 N4 95.09(13) . 3_775
N6 Co1 N4 84.91(13) 3_775 3_775
N4 Co1 N4 180.00(11) . 3_775
N6 Co1 N2 95.11(14) . 3_775
N6 Co1 N2 84.89(14) 3_775 3_775
N4 Co1 N2 96.32(13) . 3_775
N4 Co1 N2 83.68(13) 3_775 3_775
N6 Co1 N2 84.89(14) . .
N6 Co1 N2 95.11(14) 3_775 .
N4 Co1 N2 83.68(13) . .
N4 Co1 N2 96.32(13) 3_775 .
N2 Co1 N2 180.0 3_775 .
C3 N1 N2 110.8(3) . .
C3 N1 C10 129.1(3) . .
N2 N1 C10 119.8(3) . .
C1 N2 N1 105.2(3) . .
C1 N2 Co1 137.3(3) . .
N1 N2 Co1 117.3(2) . .
C6 N3 N4 110.9(3) . .
C6 N3 C10 128.9(3) . .
N4 N3 C10 119.8(3) . .
C4 N4 N3 105.1(3) . .
C4 N4 Co1 137.0(3) . .
N3 N4 Co1 117.7(2) . .
C9 N5 N6 112.6(3) . .
C9 N5 C10 127.7(3) . .
N6 N5 C10 119.6(3) . .
C7 N6 N5 104.2(3) . .
C7 N6 Co1 137.7(3) . .
N5 N6 Co1 118.1(3) . .
N2 C1 C2 110.8(4) . .
C3 C2 C1 105.7(4) . .
N1 C3 C2 107.6(4) . .
N4 C4 C5 110.8(4) . .
C6 C5 C4 106.1(4) . .
C5 C6 N3 107.2(4) . .
N6 C7 C8 111.2(4) . .
C9 C8 C7 105.6(4) . .
N5 C9 C8 106.2(4) . .
N1 C10 N3 110.2(3) . .
N1 C10 N5 110.7(3) . .
N3 C10 N5 110.8(3) . .
O1 Cl1 O3 112.7(3) . .
O1 Cl1 O2 112.8(3) . .
O3 Cl1 O2 110.58(19) . .
O1 Cl1 O4 106.5(5) . .
O3 Cl1 O4 107.0(3) . .
O2 Cl1 O4 106.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N6 2.107(3) .
Co1 N6 2.107(3) 3_775
Co1 N4 2.107(3) .
Co1 N4 2.107(3) 3_775
Co1 N2 2.112(3) 3_775
Co1 N2 2.112(3) .
N1 C3 1.342(5) .
N1 N2 1.369(5) .
N1 C10 1.437(5) .
N2 C1 1.323(5) .
N3 C6 1.357(5) .
N3 N4 1.363(5) .
N3 C10 1.440(5) .
N4 C4 1.334(5) .
N5 C9 1.346(5) .
N5 N6 1.351(5) .
N5 C10 1.450(5) .
N6 C7 1.332(5) .
C1 C2 1.394(6) .
C2 C3 1.355(6) .
C4 C5 1.391(6) .
C5 C6 1.355(6) .
C7 C8 1.392(6) .
C8 C9 1.365(6) .
Cl1 O1 1.362(5) .
Cl1 O3 1.422(3) .
Cl1 O2 1.424(3) .
Cl1 O4 1.457(6) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139048751
