Slow Magnetic Relaxation in Weak Easy-Plane Anisotropy: the Case of a Combined Magnetic and HFEPR Study.
Zhu, Yuan-Yuan; Liu, Fang; Liu, Jia-Jia; Meng, Yin-Shan; Jiang, Shang-Da; Barra, Anne-Laure; Wernsdorfer, Wolfgang; Gao, Song; Inorganic chemistry 56 (2017) 697–700; doi:10.1021/acs.inorgchem.6b01972

data_4344927
_publ_section_title
;
 Slow Magnetic Relaxation in Weak Easy-Plane Anisotropy: the Case of a
 Combined Magnetic and HFEPR Study.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              697
_journal_page_last               700
_journal_paper_doi               10.1021/acs.inorgchem.6b01972
_journal_volume                  56
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C4 Co N4 S4, 2(C12 H24 K O6)'
_chemical_formula_sum            'C28 H48 Co K2 N4 O12 S4'
_chemical_formula_weight         898.07
_chemical_name_common            1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4838(6)
_cell_length_b                   13.9373(5)
_cell_length_c                   17.5812(7)
_cell_measurement_reflns_used    5937
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      27.2800
_cell_measurement_theta_min      3.8870
_cell_volume                     4284.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega    6.00   48.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -        8.8002  -99.0000  -30.0000 42

  2 omega  -59.00   21.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -        8.8002  -57.0000   60.0000 80

  3 omega   26.00   51.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -        8.8002  -99.0000 -180.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0085678000
_diffrn_orient_matrix_UB_12      -0.0486017000
_diffrn_orient_matrix_UB_13      0.0084461000
_diffrn_orient_matrix_UB_21      -0.0201232000
_diffrn_orient_matrix_UB_22      -0.0040419000
_diffrn_orient_matrix_UB_23      -0.0348682000
_diffrn_orient_matrix_UB_31      0.0341645000
_diffrn_orient_matrix_UB_32      -0.0145381000
_diffrn_orient_matrix_UB_33      -0.0184642000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14692
_diffrn_reflns_point_group_measured_fraction_full 0.854
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.923
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 2272 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         7003
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+0.9613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.624
_reflns_Friedel_fraction_full    0.700
_reflns_Friedel_fraction_max     0.660
_reflns_number_gt                6281
_reflns_number_total             7003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01972_si_002.cif
_cod_data_source_block           1498514
_cod_depositor_comments
'Adding full bibliography for 4344927--4344928.cif.'
_cod_database_code               4344927
_chemical_oxdiff_formula         'C46 H40 Co1 N1 O1 S1'
_exptl_absorpt_special_details   SADABS
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
  C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
;
_shelx_res_checksum              66918
_shelx_hkl_checksum              14130
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'