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#$Date: 2019-11-17 11:00:00 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229473 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/51/7045105.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_7045105
loop_
_publ_author_name
'Váhovská, L'
'Vitushkina, S.'
'Potočňák, I'
'Trávníček, Z'
'Herchel, R.'
_publ_section_title
;
 Effect of linear and non-linear pseudohalides on the structural and
 magnetic properties of Co(ii) hexacoordinate single-molecule magnets.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1498
_journal_page_last               1512
_journal_paper_doi               10.1039/c7dt04256f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C24 H24 Co N12 O2, 2(C3 N3 O2)'
_chemical_formula_sum            'C30 H24 Co N18 O6'
_chemical_formula_weight         791.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-12-18 deposited with the CCDC.
2017-12-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.741(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6946(3)
_cell_length_b                   13.5526(6)
_cell_length_c                   16.7231(8)
_cell_measurement_reflns_used    3703
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.2800
_cell_measurement_theta_min      4.0030
_cell_volume                     1707.43(13)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.3438
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10955
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         3.006
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       needle
_exptl_crystal_F_000             810
_exptl_crystal_size_max          0.5603
_exptl_crystal_size_mid          0.1479
_exptl_crystal_size_min          0.1042
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0356
_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)+(0.0437P)²+1.0184P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2931
_reflns_number_total             3536
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04256f2.cif
_cod_data_source_block           shelx_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7045101--7045106.cif.'
_cod_database_code               7045105
_shelx_shelxl_version_number     2014/7
_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Co1 Co 0.5000 0.5000 0.0000 0.02088(12) Uani 1 2 d S . P
O3 O 0.73673(19) 0.72776(11) 0.12064(10) 0.0332(4) Uani 1 1 d . . .
O1 O 0.6624(2) 0.53148(13) 0.11536(10) 0.0281(3) Uani 1 1 d . . .
N50 N 0.3480(2) 0.63095(12) 0.00839(10) 0.0223(4) Uani 1 1 d . . .
O2 O 0.5582(2) 0.73713(14) 0.20706(12) 0.0535(5) Uani 1 1 d . . .
N4 N 0.6488(2) 0.77665(13) 0.16278(10) 0.0260(4) Uani 1 1 d . . .
N60 N 0.0746(2) 0.16424(14) 0.17759(12) 0.0346(4) Uani 1 1 d . . .
N10 N 0.3652(2) 0.39174(12) 0.05490(10) 0.0225(4) Uani 1 1 d . . .
N20 N 0.2215(2) 0.38827(12) 0.09250(10) 0.0244(4) Uani 1 1 d . . .
N30 N 0.3446(2) 0.24099(12) 0.09675(10) 0.0226(4) Uani 1 1 d . . .
N40 N 0.3912(3) 0.14081(14) 0.11474(15) 0.0363(5) Uani 1 1 d . . .
N3 N 0.8143(4) 0.95425(17) 0.05321(16) 0.0601(7) Uani 1 1 d . . .
N2 N 0.4817(3) 0.97672(16) 0.24537(13) 0.0496(6) Uani 1 1 d . . .
C65 C -0.0509(3) 0.1314(2) 0.21656(15) 0.0411(6) Uani 1 1 d . . .
H65 H -0.0526 0.0630 0.2289 0.049 Uiso 1 1 calc R U .
C53 C 0.1809(3) 0.81069(16) 0.02120(13) 0.0300(5) Uani 1 1 d . . .
H53 H 0.1241 0.8720 0.0261 0.036 Uiso 1 1 calc R U .
C61 C 0.0744(3) 0.26100(16) 0.16104(12) 0.0250(4) Uani 1 1 d . . .
C54 C 0.1190(3) 0.72550(16) 0.05064(13) 0.0286(5) Uani 1 1 d . . .
H54 H 0.0185 0.7272 0.0755 0.034 Uiso 1 1 calc R U .
C1 C 0.6520(3) 0.87697(16) 0.15711(13) 0.0293(5) Uani 1 1 d . . .
C51 C 0.4064(2) 0.71522(14) -0.02124(11) 0.0218(4) Uani 1 1 d . . .
C62 C -0.0474(3) 0.32689(18) 0.18194(14) 0.0338(5) Uani 1 1 d . . .
H62 H -0.0438 0.3950 0.1689 0.041 Uiso 1 1 calc R U .
C21 C 0.2111(2) 0.29669(15) 0.11737(12) 0.0225(4) Uani 1 1 d . . .
C11 C 0.4375(2) 0.30310(14) 0.05810(11) 0.0209(4) Uani 1 1 d . . .
C52 C 0.3276(3) 0.80622(15) -0.01588(13) 0.0267(4) Uani 1 1 d . . .
H52 H 0.3723 0.8640 -0.0368 0.032 Uiso 1 1 calc R U .
C55 C 0.2059(3) 0.63676(16) 0.04343(12) 0.0266(4) Uani 1 1 d . . .
H55 H 0.1631 0.5782 0.0640 0.032 Uiso 1 1 calc R U .
C2 C 0.5577(3) 0.93210(17) 0.20555(13) 0.0339(5) Uani 1 1 d . . .
C3 C 0.7426(3) 0.92042(17) 0.10016(15) 0.0376(5) Uani 1 1 d . . .
C64 C -0.1763(3) 0.1910(2) 0.23949(14) 0.0404(6) Uani 1 1 d . . .
H64 H -0.2628 0.1642 0.2666 0.049 Uiso 1 1 calc R U .
C63 C -0.1745(3) 0.2903(2) 0.22252(15) 0.0417(6) Uani 1 1 d . . .
H63 H -0.2590 0.3334 0.2383 0.050 Uiso 1 1 calc R U .
H2O H 0.685(3) 0.592(2) 0.1242(16) 0.045(8) Uiso 1 1 d . . .
H1O H 0.624(4) 0.520(2) 0.156(2) 0.063(10) Uiso 1 1 d . . .
H2N H 0.301(4) 0.107(2) 0.0791(18) 0.057(9) Uiso 1 1 d . . .
H1N H 0.379(4) 0.134(2) 0.167(2) 0.080(11) Uiso 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'
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
N10 Co1 N10 180.0 3_665 .
N10 Co1 O1 90.30(7) 3_665 .
N10 Co1 O1 89.70(7) . .
N10 Co1 O1 89.70(7) 3_665 3_665
N10 Co1 O1 90.30(7) . 3_665
O1 Co1 O1 180.0 . 3_665
N10 Co1 N50 77.07(6) 3_665 .
N10 Co1 N50 102.93(6) . .
O1 Co1 N50 90.13(6) . .
O1 Co1 N50 89.87(6) 3_665 .
N10 Co1 N50 102.93(6) 3_665 3_665
N10 Co1 N50 77.07(6) . 3_665
O1 Co1 N50 89.87(6) . 3_665
O1 Co1 N50 90.13(6) 3_665 3_665
N50 Co1 N50 180.0 . 3_665
Co1 O1 H2O 114.8(18) . .
Co1 O1 H1O 118(2) . .
H2O O1 H1O 98(3) . .
C55 N50 C51 117.97(17) . .
C55 N50 Co1 125.44(14) . .
C51 N50 Co1 116.53(12) . .
O2 N4 O3 122.61(18) . .
O2 N4 C1 119.60(18) . .
O3 N4 C1 117.77(17) . .
C61 N60 C65 117.0(2) . .
C11 N10 N20 108.70(15) . .
C11 N10 Co1 114.19(12) . .
N20 N10 Co1 137.05(13) . .
C21 N20 N10 106.39(16) . .
C11 N30 C21 105.85(16) . .
C11 N30 N40 124.16(16) . .
C21 N30 N40 129.87(16) . .
N30 N40 H2N 102.4(18) . .
N30 N40 H1N 104(2) . .
H2N N40 H1N 111(3) . .
N60 C65 C64 123.8(2) . .
N60 C65 H65 118.1 . .
C64 C65 H65 118.1 . .
C54 C53 C52 119.5(2) . .
C54 C53 H53 120.3 . .
C52 C53 H53 120.3 . .
N60 C61 C62 123.30(19) . .
N60 C61 C21 116.83(18) . .
C62 C61 C21 119.86(19) . .
C53 C54 C55 119.07(19) . .
C53 C54 H54 120.5 . .
C55 C54 H54 120.5 . .
N4 C1 C2 118.07(19) . .
N4 C1 C3 118.65(19) . .
C2 C1 C3 123.2(2) . .
N50 C51 C52 122.95(18) . .
N50 C51 C11 111.61(16) . 3_665
C52 C51 C11 125.44(18) . 3_665
C61 C62 C63 118.1(2) . .
C61 C62 H62 120.9 . .
C63 C62 H62 120.9 . .
N20 C21 N30 109.98(16) . .
N20 C21 C61 124.03(18) . .
N30 C21 C61 125.98(18) . .
N10 C11 N30 109.08(16) . .
N10 C11 C51 120.48(17) . 3_665
N30 C11 C51 130.44(17) . 3_665
C51 C52 C53 118.13(19) . .
C51 C52 H52 120.9 . .
C53 C52 H52 120.9 . .
N50 C55 C54 122.39(19) . .
N50 C55 H55 118.8 . .
C54 C55 H55 118.8 . .
N2 C2 C1 179.6(3) . .
N3 C3 C1 178.8(3) . .
C65 C64 C63 118.7(2) . .
C65 C64 H64 120.6 . .
C63 C64 H64 120.6 . .
C64 C63 C62 119.1(2) . .
C64 C63 H63 120.4 . .
C62 C63 H63 120.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N10 2.1116(15) 3_665
Co1 N10 2.1116(15) .
Co1 O1 2.1175(15) .
Co1 O1 2.1176(15) 3_665
Co1 N50 2.1458(16) .
Co1 N50 2.1459(16) 3_665
O3 N4 1.260(2) .
O1 H2O 0.84(3) .
O1 H1O 0.80(3) .
N50 C55 1.344(2) .
N50 C51 1.357(3) .
O2 N4 1.237(2) .
N4 C1 1.363(3) .
N60 C61 1.340(3) .
N60 C65 1.345(3) .
N10 C11 1.320(2) .
N10 N20 1.379(2) .
N20 C21 1.317(3) .
N30 C11 1.351(2) .
N30 C21 1.374(3) .
N30 N40 1.421(2) .
N40 H2N 0.94(3) .
N40 H1N 0.91(4) .
N3 C3 1.143(3) .
N2 C2 1.145(3) .
C65 C64 1.372(4) .
C65 H65 0.9500 .
C53 C54 1.377(3) .
C53 C52 1.396(3) .
C53 H53 0.9500 .
C61 C62 1.390(3) .
C61 C21 1.478(3) .
C54 C55 1.393(3) .
C54 H54 0.9500 .
C1 C2 1.407(3) .
C1 C3 1.418(3) .
C51 C52 1.385(3) .
C51 C11 1.479(3) 3_665
C62 C63 1.390(3) .
C62 H62 0.9500 .
C11 C51 1.479(3) 3_665
C52 H52 0.9500 .
C55 H55 0.9500 .
C64 C63 1.377(4) .
C64 H64 0.9500 .
C63 H63 0.9500 .
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
C54 H54 O3 0.95 2.44 3.380(3) 172.2 1_455
C52 H52 N40 0.95 2.45 3.063(3) 122.6 3_665
C64 H64 O2 0.95 2.60 3.301(3) 131.1 2_545
O1 H2O O3 0.84(3) 1.89(3) 2.719(2) 168(3) .
O1 H2O N4 0.84(3) 2.62(3) 3.423(2) 160(2) .
O1 H1O N2 0.80(3) 2.07(4) 2.873(3) 175(3) 2_645
N40 H2N N3 0.94(3) 2.36(3) 3.200(4) 149(2) 3_665
N40 H1N O2 0.91(4) 2.49(4) 3.204(3) 136(3) 2_645
N40 H1N N2 0.91(4) 2.54(3) 3.096(3) 120(3) 1_545
