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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/7/04/51/7045101.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_7045101
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(C6 N5), 2(H2O)'
_chemical_formula_sum            'C36 H28 Co N22 O4'
_chemical_formula_weight         891.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                103.655(8)
_cell_angle_beta                 103.501(8)
_cell_angle_gamma                97.011(8)
_cell_formula_units_Z            1
_cell_length_a                   8.0992(8)
_cell_length_b                   11.4165(10)
_cell_length_c                   11.7630(11)
_cell_measurement_reflns_used    5660
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.9430
_cell_measurement_theta_min      3.5220
_cell_volume                     1009.48(18)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10541
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.970
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.853
_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    1.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             457
_exptl_crystal_size_max          0.4556
_exptl_crystal_size_mid          0.3384
_exptl_crystal_size_min          0.2188
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0178(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         4180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0306
_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)+(0.0232P)²+0.3145P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3586
_reflns_number_total             4180
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt04256f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7045101--7045106.cif.'
_cod_original_cell_volume        1009.48(17)
_cod_database_code               7045101
_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, -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
Co1 Co 0.5000 0.5000 0.5000 0.01946(10) Uani 1 2 d S . P
O2 O 0.24359(17) 0.80343(11) 0.47599(13) 0.0309(3) Uani 1 1 d . . .
O1 O 0.27217(16) 0.56253(12) 0.43496(11) 0.0260(3) Uani 1 1 d . . .
N30 N 0.77110(16) 0.67575(11) 0.31188(11) 0.0203(3) Uani 1 1 d . . .
N60 N 0.81767(18) 0.63863(13) 0.07070(12) 0.0287(3) Uani 1 1 d . . .
N1 N 0.29123(17) 0.90034(12) 0.73781(12) 0.0248(3) Uani 1 1 d . . .
N10 N 0.60326(17) 0.54970(11) 0.36818(11) 0.0208(3) Uani 1 1 d . . .
N3 N 0.1615(2) 0.87860(14) 1.00262(15) 0.0443(4) Uani 1 1 d . . .
N20 N 0.60635(17) 0.49091(12) 0.25265(11) 0.0220(3) Uani 1 1 d . . .
N50 N 0.36320(16) 0.31355(11) 0.41019(11) 0.0205(3) Uani 1 1 d . . .
N40 N 0.8824(2) 0.78349(12) 0.31397(15) 0.0270(3) Uani 1 1 d . . .
N5 N 0.4106(2) 1.14856(13) 1.00824(14) 0.0382(4) Uani 1 1 d . . .
C61 C 0.7438(2) 0.54223(14) 0.10014(14) 0.0221(3) Uani 1 1 d . . .
N6 N 0.5293(2) 1.11633(14) 0.65827(14) 0.0379(4) Uani 1 1 d . . .
C7 C 0.7004(2) 0.66065(13) 0.40275(14) 0.0199(3) Uani 1 1 d . . .
N2 N 0.0428(2) 0.61469(13) 0.64849(15) 0.0382(4) Uani 1 1 d . . .
C62 C 0.6971(2) 0.42331(15) 0.02342(15) 0.0290(4) Uani 1 1 d . . .
H62 H 0.6447 0.3578 0.0478 0.035 Uiso 1 1 calc R U .
C51 C 0.2788(2) 0.25771(14) 0.47607(14) 0.0205(3) Uani 1 1 d . . .
C1 C 0.2046(2) 0.82917(14) 0.78687(15) 0.0250(4) Uani 1 1 d . . .
C54 C 0.2578(2) 0.13156(15) 0.24310(15) 0.0280(4) Uani 1 1 d . . .
H54 H 0.2507 0.0900 0.1615 0.034 Uiso 1 1 calc R U .
C21 C 0.7087(2) 0.56803(14) 0.21985(14) 0.0202(3) Uani 1 1 d . . .
C53 C 0.1751(2) 0.07531(15) 0.31152(15) 0.0303(4) Uani 1 1 d . . .
H53 H 0.1114 -0.0062 0.2777 0.036 Uiso 1 1 calc R U .
C3 C 0.1832(2) 0.85931(15) 0.90724(17) 0.0291(4) Uani 1 1 d . . .
C2 C 0.1165(2) 0.70994(15) 0.70974(16) 0.0278(4) Uani 1 1 d . . .
C4 C 0.3780(2) 1.01469(14) 0.79065(14) 0.0248(4) Uani 1 1 d . . .
C52 C 0.1852(2) 0.13822(14) 0.43011(15) 0.0269(4) Uani 1 1 d . . .
H52 H 0.1296 0.1006 0.4787 0.032 Uiso 1 1 calc R U .
C55 C 0.3521(2) 0.25051(14) 0.29596(14) 0.0244(4) Uani 1 1 d . . .
H55 H 0.4109 0.2886 0.2493 0.029 Uiso 1 1 calc R U .
C6 C 0.4618(2) 1.07171(15) 0.71753(15) 0.0279(4) Uani 1 1 d . . .
C64 C 0.8040(2) 0.50139(18) -0.12166(16) 0.0364(4) Uani 1 1 d . . .
H64 H 0.8267 0.4899 -0.1988 0.044 Uiso 1 1 calc R U .
C63 C 0.7293(2) 0.40334(17) -0.08948(16) 0.0356(4) Uani 1 1 d . . .
H63 H 0.7004 0.3233 -0.1440 0.043 Uiso 1 1 calc R U .
C5 C 0.3951(2) 1.08774(14) 0.91189(16) 0.0263(4) Uani 1 1 d . . .
C65 C 0.8451(2) 0.61639(18) -0.04010(16) 0.0355(4) Uani 1 1 d . . .
H65 H 0.8954 0.6834 -0.0635 0.043 Uiso 1 1 calc R U .
H1N H 0.989(3) 0.7816(18) 0.3596(18) 0.046(6) Uiso 1 1 d . . .
H1O1 H 0.180(3) 0.520(2) 0.4285(19) 0.051(7) Uiso 1 1 d . . .
H2O1 H 0.265(3) 0.635(2) 0.454(2) 0.057(7) Uiso 1 1 d . . .
H2N H 0.887(3) 0.7747(19) 0.236(2) 0.051(6) Uiso 1 1 d . . .
H1O2 H 0.316(3) 0.834(2) 0.446(2) 0.058(7) Uiso 1 1 d . . .
H2O2 H 0.262(3) 0.835(2) 0.548(2) 0.069(9) 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'
Co Co 0.3494 0.9721 '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
N10 Co1 N10 180.00(6) . 2_666
N10 Co1 O1 89.32(5) . 2_666
N10 Co1 O1 90.68(5) 2_666 2_666
N10 Co1 O1 90.68(5) . .
N10 Co1 O1 89.32(5) 2_666 .
O1 Co1 O1 180.0 2_666 .
N10 Co1 N50 103.27(5) . .
N10 Co1 N50 76.73(5) 2_666 .
O1 Co1 N50 91.15(5) 2_666 .
O1 Co1 N50 88.86(5) . .
N10 Co1 N50 76.72(5) . 2_666
N10 Co1 N50 103.27(5) 2_666 2_666
O1 Co1 N50 88.86(5) 2_666 2_666
O1 Co1 N50 91.14(5) . 2_666
N50 Co1 N50 180.0 . 2_666
H1O2 O2 H2O2 112(2) . .
Co1 O1 H1O1 117.8(15) . .
Co1 O1 H2O1 122.3(16) . .
H1O1 O1 H2O1 110(2) . .
C7 N30 C21 105.60(12) . .
C7 N30 N40 125.60(13) . .
C21 N30 N40 128.78(13) . .
C65 N60 C61 116.71(15) . .
C1 N1 C4 127.13(14) . .
C7 N10 N20 109.42(12) . .
C7 N10 Co1 115.28(10) . .
N20 N10 Co1 135.10(10) . .
C21 N20 N10 106.20(12) . .
C55 N50 C51 117.99(13) . .
C55 N50 Co1 125.92(10) . .
C51 N50 Co1 116.07(10) . .
N30 N40 H1N 106.4(13) . .
N30 N40 H2N 105.8(14) . .
H1N N40 H2N 107.9(18) . .
N60 C61 C62 123.75(15) . .
N60 C61 C21 116.40(14) . .
C62 C61 C21 119.83(14) . .
N10 C7 N30 108.59(13) . .
N10 C7 C51 120.45(13) . 2_666
N30 C7 C51 130.92(14) . 2_666
C63 C62 C61 118.03(16) . .
C63 C62 H62 121.0 . .
C61 C62 H62 121.0 . .
N50 C51 C52 122.45(14) . .
N50 C51 C7 111.38(13) . 2_666
C52 C51 C7 126.17(14) . 2_666
N1 C1 C3 127.33(15) . .
N1 C1 C2 116.69(15) . .
C3 C1 C2 115.93(14) . .
C53 C54 C55 118.70(15) . .
C53 C54 H54 120.6 . .
C55 C54 H54 120.6 . .
N20 C21 N30 110.18(13) . .
N20 C21 C61 123.91(14) . .
N30 C21 C61 125.87(13) . .
C54 C53 C52 119.75(15) . .
C54 C53 H53 120.1 . .
C52 C53 H53 120.1 . .
N3 C3 C1 177.05(18) . .
N2 C2 C1 178.65(19) . .
N1 C4 C6 116.13(14) . .
N1 C4 C5 127.39(15) . .
C6 C4 C5 116.47(14) . .
C53 C52 C51 118.37(15) . .
C53 C52 H52 120.8 . .
C51 C52 H52 120.8 . .
N50 C55 C54 122.72(15) . .
N50 C55 H55 118.6 . .
C54 C55 H55 118.6 . .
N6 C6 C4 179.33(18) . .
C63 C64 C65 119.00(16) . .
C63 C64 H64 120.5 . .
C65 C64 H64 120.5 . .
C64 C63 C62 119.05(17) . .
C64 C63 H63 120.5 . .
C62 C63 H63 120.5 . .
N5 C5 C4 178.37(17) . .
N60 C65 C64 123.46(16) . .
N60 C65 H65 118.3 . .
C64 C65 H65 118.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N10 2.0810(12) .
Co1 N10 2.0811(12) 2_666
Co1 O1 2.1024(12) 2_666
Co1 O1 2.1024(12) .
Co1 N50 2.1658(13) .
Co1 N50 2.1658(13) 2_666
O2 H1O2 0.83(2) .
O2 H2O2 0.80(3) .
O1 H1O1 0.82(2) .
O1 H2O1 0.82(2) .
N30 C7 1.3600(18) .
N30 C21 1.3799(19) .
N30 N40 1.4250(17) .
N60 C65 1.343(2) .
N60 C61 1.344(2) .
N1 C1 1.325(2) .
N1 C4 1.332(2) .
N10 C7 1.3239(19) .
N10 N20 1.3738(17) .
N3 C3 1.150(2) .
N20 C21 1.3200(19) .
N50 C55 1.3426(19) .
N50 C51 1.3595(19) .
N40 H1N 0.91(2) .
N40 H2N 0.91(2) .
N5 C5 1.150(2) .
C61 C62 1.392(2) .
C61 C21 1.470(2) .
N6 C6 1.150(2) .
C7 C51 1.467(2) 2_666
N2 C2 1.153(2) .
C62 C63 1.385(2) .
C62 H62 0.9500 .
C51 C52 1.391(2) .
C51 C7 1.467(2) 2_666
C1 C3 1.433(2) .
C1 C2 1.436(2) .
C54 C53 1.378(2) .
C54 C55 1.393(2) .
C54 H54 0.9500 .
C53 C52 1.388(2) .
C53 H53 0.9500 .
C4 C6 1.433(2) .
C4 C5 1.438(2) .
C52 H52 0.9500 .
C55 H55 0.9500 .
C64 C63 1.380(3) .
C64 C65 1.380(3) .
C64 H64 0.9500 .
C63 H63 0.9500 .
C65 H65 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 N3 0.95 2.58 3.393(2) 143.8 1_544
C54 H54 N5 0.95 2.61 3.315(2) 131.2 1_544
C52 H52 N40 0.95 2.52 3.127(2) 122.2 2_666
C55 H55 N20 0.95 2.62 3.436(2) 143.9 .
C64 H64 O1 0.95 2.60 3.472(2) 152.2 2_665
N40 H1N O2 0.91(2) 2.14(2) 3.045(2) 172.3(18) 1_655
O1 H1O1 N2 0.82(2) 2.08(2) 2.863(2) 160(2) 2_566
O1 H2O1 O2 0.82(2) 1.91(2) 2.7261(18) 173(2) .
N40 H2N N60 0.91(2) 2.09(2) 2.838(2) 139.1(18) .
O2 H1O2 N6 0.83(2) 2.07(2) 2.889(2) 169(2) 2_676
O2 H2O2 N1 0.80(3) 2.13(3) 2.931(2) 173(2) .
