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#$Date: 2019-11-17 10:51:01 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229438 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/77/7047721.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_7047721
loop_
_publ_author_name
'Vráblová, Anna'
'Černák, Juraj'
'Rajnák, Cyril'
'Dlháň, Ľubor'
'Tomás, Milagros'
'Falvello, Larry R.'
'Boča, Roman'
_publ_section_title
;
 Exceptionally slow magnetic relaxation in cobalt(ii) benzoate trihydrate.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15523
_journal_page_last               15529
_journal_paper_doi               10.1039/c8dt03610a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C7 H9 Co O4, C7 H5 O2, H2 O'
_chemical_formula_sum            'C14 H16 Co O7'
_chemical_formula_weight         355.20
_chemical_name_systematic        'cobalt(II) benzoate trihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-03-06 deposited with the CCDC.
2018-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.703(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2318(4)
_cell_length_b                   34.130(3)
_cell_length_c                   6.9115(4)
_cell_measurement_reflns_used    1719
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      28.1500
_cell_measurement_theta_min      3.0690
_cell_volume                     1462.74(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
Brandenburg, K. (2007). DIAMOND. Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution
;
SIR-92
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
;
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4782
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         3.022
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Multi-scan absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       irregular
_exptl_crystal_F_000             732
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method 'Crystallization from mother liquer'
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0426
_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)+(0.0563P)²+0.0997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1323
_reflns_number_total             1636
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03610a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7047721.cif.'
_cod_original_cell_volume        1462.72(17)
_cod_database_code               7047721
_shelx_shelxl_version_number     20/6
_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.
;
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.950
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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 0.500000 0.500000 0.000000 0.01796(18) Uani 1 2 d S . P
O2 O 0.2767(3) 0.48858(5) 0.2096(3) 0.0200(4) Uani 1 1 d . . .
H2A H 0.296(5) 0.4663(8) 0.263(4) 0.030 Uiso 1 1 d . U .
H2B H 0.276(5) 0.5065(8) 0.278(5) 0.030 Uiso 1 1 d . U .
O4 O 0.250000 0.53981(7) 0.500000 0.0261(6) Uani 1 2 d S T P
H4A H 0.137(5) 0.5527(8) 0.464(4) 0.039 Uiso 1 1 d . U .
O1 O 0.5686(3) 0.44358(5) -0.0148(2) 0.0228(4) Uani 1 1 d . . .
C1 C 0.750000 0.42623(9) 0.000000 0.0204(7) Uani 1 2 d S T P
C2 C 0.750000 0.38278(9) 0.000000 0.0203(7) Uani 1 2 d S T P
C3 C 0.5616(4) 0.36237(7) -0.0562(4) 0.0278(6) Uani 1 1 d . . .
H3 H 0.431668 0.376260 -0.092317 0.033 Uiso 1 1 calc R U .
C4 C 0.5624(5) 0.32193(8) -0.0596(4) 0.0353(7) Uani 1 1 d . . .
H4 H 0.434551 0.307992 -0.102803 0.042 Uiso 1 1 calc R U .
C5 C 0.750000 0.30175(11) 0.000000 0.0372(10) Uani 1 2 d S T P
H5 H 0.750005 0.273916 0.000003 0.045 Uiso 1 2 calc R U P
O3 O 0.3772(3) 0.42299(5) 0.3967(3) 0.0305(5) Uani 1 1 d . . .
C6 C 0.250000 0.40566(10) 0.500000 0.0244(8) Uani 1 2 d S T P
C7 C 0.250000 0.36171(10) 0.500000 0.0237(8) Uani 1 2 d S T P
C8 C 0.4124(5) 0.34126(8) 0.4210(4) 0.0320(6) Uani 1 1 d . . .
H8 H 0.523863 0.355063 0.365838 0.038 Uiso 1 1 calc R U .
C9 C 0.4123(6) 0.30075(8) 0.4225(4) 0.0417(8) Uani 1 1 d . . .
H9 H 0.524875 0.286791 0.369812 0.050 Uiso 1 1 calc R U .
C10 C 0.250000 0.28056(11) 0.500000 0.0452(12) Uani 1 2 d S T P
H10 H 0.249997 0.252725 0.500002 0.054 Uiso 1 2 calc R U P
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'
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
O1 Co1 O1 180.0 . 5_665
O1 Co1 O2 90.93(7) . .
O1 Co1 O2 89.07(7) 5_665 .
O1 Co1 O2 89.07(7) . 5_665
O1 Co1 O2 90.93(7) 5_665 5_665
O2 Co1 O2 180.00(9) . 5_665
O1 Co1 O2 87.25(7) . 2
O1 Co1 O2 92.75(7) 5_665 2
O2 Co1 O2 83.83(7) . 2
O2 Co1 O2 96.17(7) 5_665 2
O1 Co1 O2 92.75(7) . 6_665
O1 Co1 O2 87.25(7) 5_665 6_665
O2 Co1 O2 96.17(7) . 6_665
O2 Co1 O2 83.83(7) 5_665 6_665
O2 Co1 O2 180.00(9) 2 6_665
Co1 O2 Co1 92.42(7) . 2
Co1 O2 H2A 113(2) . .
Co1 O2 H2A 121.2(19) 2 .
Co1 O2 H2B 108(2) . .
Co1 O2 H2B 102(2) 2 .
H2A O2 H2B 117(3) . .
H4A O4 H4A 118(4) . 2_556
C1 O1 Co1 130.13(18) . .
O1 C1 O1 124.5(3) 2_655 .
O1 C1 C2 117.76(15) 2_655 .
O1 C1 C2 117.76(15) . .
C3 C2 C3 119.7(3) 2_655 .
C3 C2 C1 120.15(16) 2_655 .
C3 C2 C1 120.15(16) . .
C4 C3 C2 120.2(3) . .
C4 C3 H3 119.9 . .
C2 C3 H3 119.9 . .
C3 C4 C5 119.8(3) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C4 C5 C4 120.3(3) . 2_655
C4 C5 H5 119.8 . .
C4 C5 H5 119.8 2_655 .
O3 C6 O3 124.2(3) . 2_556
O3 C6 C7 117.88(16) . .
O3 C6 C7 117.88(16) 2_556 .
C8 C7 C8 119.5(3) 2_556 .
C8 C7 C6 120.26(16) 2_556 .
C8 C7 C6 120.26(16) . .
C9 C8 C7 120.0(3) . .
C9 C8 H8 120.0 . .
C7 C8 H8 120.0 . .
C10 C9 C8 120.3(3) . .
C10 C9 H9 119.8 . .
C8 C9 H9 119.8 . .
C9 C10 C9 119.9(4) . 2_556
C9 C10 H10 120.1 . .
C9 C10 H10 120.1 2_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 1.9775(16) .
Co1 O1 1.9776(16) 5_665
Co1 O2 2.1418(18) .
Co1 O2 2.1418(18) 5_665
Co1 O2 2.1745(18) 2
Co1 O2 2.1745(18) 6_665
O2 H2A 0.85(3) .
O2 H2B 0.77(3) .
O4 H4A 0.85(3) .
O4 H4A 0.85(3) 2_556
O1 C1 1.271(2) .
C1 C2 1.483(4) .
C2 C3 1.387(3) 2_655
C2 C3 1.387(3) .
C3 C4 1.381(4) .
C3 H3 0.9500 .
C4 C5 1.384(3) .
C4 H4 0.9500 .
C5 H5 0.9500 .
O3 C6 1.265(2) .
C6 C7 1.500(5) .
C7 C8 1.386(3) 2_556
C7 C8 1.386(3) .
C8 C9 1.383(4) .
C8 H8 0.9500 .
C9 C10 1.376(4) .
C9 H9 0.9500 .
C10 H10 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
O2 H2A O3 0.85(3) 1.79(3) 2.630(2) 170(3) .
O2 H2B O4 0.77(3) 1.93(3) 2.679(2) 163(3) .
O4 H4A O3 0.85(3) 1.84(3) 2.681(2) 175(3) 6_565
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
Co1 O1 C1 O1 -5.36(8) . 2_655
Co1 O1 C1 C2 174.63(8) . .
O1 C1 C2 C3 13.57(16) 2_655 2_655
O1 C1 C2 C3 -166.43(16) . 2_655
O1 C1 C2 C3 -166.43(16) 2_655 .
O1 C1 C2 C3 13.57(16) . .
C3 C2 C3 C4 -1.2(2) 2_655 .
C1 C2 C3 C4 178.8(2) . .
C2 C3 C4 C5 2.4(4) . .
C3 C4 C5 C4 -1.2(2) . 2_655
O3 C6 C7 C8 -167.57(16) . 2_556
O3 C6 C7 C8 12.43(16) 2_556 2_556
O3 C6 C7 C8 12.43(16) . .
O3 C6 C7 C8 -167.57(16) 2_556 .
C8 C7 C8 C9 -0.4(2) 2_556 .
C6 C7 C8 C9 179.6(2) . .
C7 C8 C9 C10 0.8(4) . .
C8 C9 C10 C9 -0.4(2) . 2_556
