#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:18:38 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232842 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/82/4348242.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_4348242
loop_
_publ_author_name
'Roy, Subhadip'
'Oyarzabal, Itziar'
'Vallejo, Julia'
'Cano, Joan'
'Colacio, Enrique'
'Bauza, Antonio'
'Frontera, Antonio'
'Kirillov, Alexander M.'
'Drew, Michael G. B.'
'Das, Subrata'
_publ_section_title
;
 Two Polymorphic Forms of a Six-Coordinate Mononuclear Cobalt(II) Complex
 with Easy-Plane Anisotropy: Structural Features, Theoretical
 Calculations, and Field-Induced Slow Relaxation of the Magnetization.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8502
_journal_page_last               8513
_journal_paper_doi               10.1021/acs.inorgchem.6b01087
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C24 H20 Co N6 O14'
_chemical_formula_sum            'C24 H20 Co N6 O14'
_chemical_formula_weight         675.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        '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                 97.205(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.228(4)
_cell_length_b                   17.200(4)
_cell_length_c                   7.4727(16)
_cell_measurement_reflns_used    23024
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.50
_cell_volume                     2834.4(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII 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  0.1516
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            23024
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.50
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.9864
_exptl_absorpt_correction_T_min  0.8749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.857
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2490
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0865
_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)+(0.1260P)²+11.2130P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2189
_refine_ls_wR_factor_ref         0.2525
_reflns_number_gt                1875
_reflns_number_total             2490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01087_si_002.cif
_cod_data_source_block           1
_cod_original_cell_volume        2834.4(11)
_cod_database_code               4348242
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
Co1 Co 1.0000 0.75368(6) 0.2500 0.0371(4) Uani 1 2 d S
O1 O 0.91432(17) 0.7497(2) 0.3432(5) 0.0422(10) Uani 1 1 d .
O2 O 0.9432(2) 0.7062(4) 0.6224(6) 0.0704(16) Uani 1 1 d .
O10 O 0.7046(2) 0.7039(4) 0.0767(7) 0.088(2) Uani 1 1 d .
O11 O 0.6422(2) 0.6452(4) 0.2250(8) 0.0829(18) Uani 1 1 d .
O12 O 0.7084(3) 0.5474(4) 0.8197(9) 0.096(2) Uani 1 1 d .
O13 O 0.7997(3) 0.5664(5) 0.9387(9) 0.108(3) Uani 1 1 d .
N10 N 0.6926(2) 0.6689(3) 0.2086(7) 0.0520(13) Uani 1 1 d .
N11 N 0.7586(3) 0.5726(4) 0.8168(8) 0.0672(17) Uani 1 1 d .
C10 C 0.9053(2) 0.7170(4) 0.4865(7) 0.0402(13) Uani 1 1 d .
C11 C 0.8421(2) 0.6843(3) 0.4940(7) 0.0372(13) Uani 1 1 d .
C12 C 0.7973(2) 0.6904(3) 0.3481(7) 0.0379(13) Uani 1 1 d .
H12 H 0.8053 0.7156 0.2436 0.045 Uiso 1 1 calc R
C13 C 0.7411(2) 0.6589(3) 0.3584(8) 0.0395(13) Uani 1 1 d .
C14 C 0.7267(3) 0.6206(4) 0.5109(8) 0.0456(14) Uani 1 1 d .
H14 H 0.6883 0.6002 0.5169 0.055 Uiso 1 1 calc R
C15 C 0.7723(3) 0.6147(4) 0.6524(8) 0.0472(15) Uani 1 1 d .
C16 C 0.8292(2) 0.6460(3) 0.6499(7) 0.0403(13) Uani 1 1 d .
H16 H 0.8585 0.6418 0.7499 0.048 Uiso 1 1 calc R
N1 N 1.0000 0.6286(4) 0.2500 0.0498(18) Uani 1 2 d S
C1A C 0.9510(3) 0.5879(4) 0.1811(9) 0.0571(17) Uani 1 1 d .
H1A H 0.9166 0.6151 0.1323 0.068 Uiso 1 1 calc R
C2A C 0.9491(4) 0.5086(5) 0.1793(11) 0.078(2) Uani 1 1 d .
H2A H 0.9141 0.4826 0.1312 0.094 Uiso 1 1 calc R
C3A C 1.0000 0.4675(7) 0.2500 0.091(4) Uani 1 2 d S
H3A H 1.0000 0.4135 0.2500 0.109 Uiso 1 2 calc SR
N2 N 1.0000 0.8775(4) 0.2500 0.0511(18) Uani 1 2 d S
C1B C 0.9481(3) 0.9182(5) 0.2327(12) 0.068(2) Uani 1 1 d .
H1B H 0.9116 0.8912 0.2207 0.082 Uiso 1 1 calc R
C2B C 0.9466(5) 0.9978(5) 0.2317(16) 0.098(3) Uani 1 1 d .
H2B H 0.9097 1.0241 0.2189 0.117 Uiso 1 1 calc R
C3B C 1.0000 1.0376(8) 0.2500 0.110(5) Uani 1 2 d S
H3B H 1.0000 1.0917 0.2500 0.132 Uiso 1 2 calc SR
O1W O 1.0499(2) 0.7508(3) 0.5076(6) 0.0609(14) Uani 1 1 d D
H1 H 1.075(3) 0.784(4) 0.561(9) 0.091 Uiso 1 1 d D
H2 H 1.028(3) 0.730(4) 0.579(8) 0.091 Uiso 1 1 d 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'
Co Co 0.3494 0.9721 '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_1
_geom_angle_site_symmetry_3
O1W Co1 O1W 177.3(3) 2_755 .
O1W Co1 O1 95.27(17) 2_755 2_755
O1W Co1 O1 84.64(17) . 2_755
O1W Co1 O1 84.64(17) 2_755 .
O1W Co1 O1 95.27(17) . .
O1 Co1 O1 176.3(2) 2_755 .
O1W Co1 N2 91.35(15) 2_755 .
O1W Co1 N2 91.35(15) . .
O1 Co1 N2 91.86(11) 2_755 .
O1 Co1 N2 91.86(11) . .
O1W Co1 N1 88.65(15) 2_755 .
O1W Co1 N1 88.65(15) . .
O1 Co1 N1 88.14(11) 2_755 .
O1 Co1 N1 88.14(11) . .
N2 Co1 N1 180.000(1) . .
C10 O1 Co1 123.2(3) . .
O11 N10 O10 123.3(5) . .
O11 N10 C13 119.0(5) . .
O10 N10 C13 117.6(5) . .
O12 N11 O13 124.7(6) . .
O12 N11 C15 118.5(6) . .
O13 N11 C15 116.7(6) . .
O1 C10 O2 126.8(5) . .
O1 C10 C11 116.6(4) . .
O2 C10 C11 116.6(5) . .
C12 C11 C16 119.2(5) . .
C12 C11 C10 121.3(5) . .
C16 C11 C10 119.5(5) . .
C13 C12 C11 119.7(5) . .
C13 C12 H12 120.1 . .
C11 C12 H12 120.1 . .
C12 C13 C14 122.6(5) . .
C12 C13 N10 120.0(5) . .
C14 C13 N10 117.3(5) . .
C15 C14 C13 116.3(5) . .
C15 C14 H14 121.8 . .
C13 C14 H14 121.8 . .
C14 C15 C16 123.4(6) . .
C14 C15 N11 117.6(6) . .
C16 C15 N11 119.0(5) . .
C15 C16 C11 118.7(5) . .
C15 C16 H16 120.7 . .
C11 C16 H16 120.7 . .
C1A N1 C1A 117.2(9) 2_755 .
C1A N1 Co1 121.4(4) 2_755 .
C1A N1 Co1 121.4(4) . .
N1 C1A C2A 123.1(8) . .
N1 C1A H1A 118.4 . .
C2A C1A H1A 118.4 . .
C1A C2A C3A 119.1(9) . .
C1A C2A H2A 120.5 . .
C3A C2A H2A 120.5 . .
C2A C3A C2A 118.4(11) 2_755 .
C2A C3A H3A 120.8 2_755 .
C2A C3A H3A 120.8 . .
C1B N2 C1B 117.0(9) 2_755 .
C1B N2 Co1 121.5(4) 2_755 .
C1B N2 Co1 121.5(4) . .
N2 C1B C2B 122.9(8) . .
N2 C1B H1B 118.5 . .
C2B C1B H1B 118.5 . .
C3B C2B C1B 118.7(9) . .
C3B C2B H2B 120.6 . .
C1B C2B H2B 120.6 . .
C2B C3B C2B 119.7(12) . 2_755
C2B C3B H3B 120.2 . .
C2B C3B H3B 120.2 2_755 .
Co1 O1W H1 130(5) . .
Co1 O1W H2 108(5) . .
H1 O1W H2 112(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1W 2.099(4) 2_755
Co1 O1W 2.099(4) .
Co1 O1 2.109(4) 2_755
Co1 O1 2.109(4) .
Co1 N2 2.129(8) .
Co1 N1 2.152(8) .
O1 C10 1.248(7) .
O2 C10 1.250(7) .
O10 N10 1.213(7) .
O11 N10 1.212(7) .
O12 N11 1.200(8) .
O13 N11 1.211(8) .
N10 C13 1.463(7) .
N11 C15 1.490(8) .
C10 C11 1.520(8) .
C11 C12 1.385(7) .
C11 C16 1.399(8) .
C12 C13 1.372(8) .
C12 H12 0.9300 .
C13 C14 1.388(8) .
C14 C15 1.374(8) .
C14 H14 0.9300 .
C15 C16 1.377(8) .
C16 H16 0.9300 .
N1 C1A 1.342(7) 2_755
N1 C1A 1.342(7) .
C1A C2A 1.365(12) .
C1A H1A 0.9300 .
C2A C3A 1.381(11) .
C2A H2A 0.9300 .
C3A C2A 1.381(11) 2_755
C3A H3A 0.9300 .
N2 C1B 1.341(8) 2_755
N2 C1B 1.341(8) .
C1B C2B 1.369(12) .
C1B H1B 0.9300 .
C2B C3B 1.363(11) .
C2B H2B 0.9300 .
C3B C2B 1.363(11) 2_755
C3B H3B 0.9300 .
O1W H1 0.86(2) .
O1W H2 0.84(2) .
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
O1W H1 O11 0.86(2) 2.19(3) 3.036(7) 172(8) 8_566
O1W H2 O2 0.84(2) 2.00(5) 2.732(7) 144(8) .
O1W H2 O2 0.84(2) 2.27(6) 2.854(7) 126(6) 2_756
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1W Co1 O1 C10 147.7(5) 2_755 .
O1W Co1 O1 C10 -29.6(5) . .
O1 Co1 O1 C10 58.8(4) 2_755 .
N2 Co1 O1 C10 -121.2(4) . .
N1 Co1 O1 C10 58.8(4) . .
Co1 O1 C10 O2 26.5(9) . .
Co1 O1 C10 C11 -151.2(4) . .
O1 C10 C11 C12 0.4(8) . .
O2 C10 C11 C12 -177.5(6) . .
O1 C10 C11 C16 179.2(5) . .
O2 C10 C11 C16 1.3(8) . .
C16 C11 C12 C13 0.0(8) . .
C10 C11 C12 C13 178.8(5) . .
C11 C12 C13 C14 0.0(9) . .
C11 C12 C13 N10 176.6(5) . .
O11 N10 C13 C12 -175.2(6) . .
O10 N10 C13 C12 1.5(9) . .
O11 N10 C13 C14 1.6(9) . .
O10 N10 C13 C14 178.3(7) . .
C12 C13 C14 C15 -0.9(9) . .
N10 C13 C14 C15 -177.6(6) . .
C13 C14 C15 C16 1.8(10) . .
C13 C14 C15 N11 -178.9(6) . .
O12 N11 C15 C14 -1.5(10) . .
O13 N11 C15 C14 178.5(7) . .
O12 N11 C15 C16 177.9(7) . .
O13 N11 C15 C16 -2.2(10) . .
C14 C15 C16 C11 -1.7(10) . .
N11 C15 C16 C11 178.9(6) . .
C12 C11 C16 C15 0.8(8) . .
C10 C11 C16 C15 -178.0(5) . .
O1W Co1 N1 C1A 140.9(4) 2_755 2_755
O1W Co1 N1 C1A -39.1(4) . 2_755
O1 Co1 N1 C1A 45.6(4) 2_755 2_755
O1 Co1 N1 C1A -134.4(4) . 2_755
O1W Co1 N1 C1A -39.1(4) 2_755 .
O1W Co1 N1 C1A 140.9(4) . .
O1 Co1 N1 C1A -134.4(4) 2_755 .
O1 Co1 N1 C1A 45.6(4) . .
C1A N1 C1A C2A 0.3(5) 2_755 .
Co1 N1 C1A C2A -179.7(5) . .
N1 C1A C2A C3A -0.5(11) . .
C1A C2A C3A C2A 0.3(5) . 2_755
O1W Co1 N2 C1B -120.9(5) 2_755 2_755
O1W Co1 N2 C1B 59.1(5) . 2_755
O1 Co1 N2 C1B -25.6(5) 2_755 2_755
O1 Co1 N2 C1B 154.4(5) . 2_755
O1W Co1 N2 C1B 59.1(5) 2_755 .
O1W Co1 N2 C1B -120.9(5) . .
O1 Co1 N2 C1B 154.4(5) 2_755 .
O1 Co1 N2 C1B -25.6(5) . .
C1B N2 C1B C2B 0.1(8) 2_755 .
Co1 N2 C1B C2B -179.9(8) . .
N2 C1B C2B C3B -0.3(15) . .
C1B C2B C3B C2B 0.1(7) . 2_755
