Slow Magnetic Relaxation in 8-Coordinate Mn(II) Compounds
Wang, Li-Xin; Wu, Xiao-Fan; Jin, Xinxin; Li, Jia-Yi; Wang, Bingwu; Liu, Jiyan; Xiang, Jing; Gao, Song; Dalton Transactions  (2023) –; doi:10.1039/D3DT02307A

data_7714079
_publ_section_title
;
 Slow Magnetic Relaxation in 8-Coordinate Mn(II) Compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02307A
_journal_year                    2023
_chemical_formula_moiety
'C40 H48 Mn N20, 2(Cl O4), [+ solvents]1[C2H5OC2H5], 1[]'
_chemical_formula_sum            'C40 H48 Cl2 Mn N20 O8'
_chemical_formula_weight         1062.82
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2022-09-17 deposited with the CCDC.	2023-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.80(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.937(2)
_cell_length_b                   39.707(8)
_cell_length_c                   12.853(3)
_cell_measurement_reflns_used    6436
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      25.6570
_cell_measurement_theta_min      2.2280
_cell_volume                     5218(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5368
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -11.00  28.00   1.00   10.00    --  -11.59 -99.00-120.00   39
  2  \w     -4.00  22.00   1.00   10.00    --  -11.59 -99.00 -60.00   26
  3  \w    -56.00  67.00   1.00   10.00    --   11.74   0.00-180.00  123
  4  \w     68.00  99.00   1.00   10.00    --   11.74-178.00 150.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0387648000
_diffrn_orient_matrix_UB_12      -0.0148222000
_diffrn_orient_matrix_UB_13      0.0121309000
_diffrn_orient_matrix_UB_21      -0.0559806000
_diffrn_orient_matrix_UB_22      -0.0097547000
_diffrn_orient_matrix_UB_23      -0.0293192000
_diffrn_orient_matrix_UB_31      0.0132599000
_diffrn_orient_matrix_UB_32      0.0020952000
_diffrn_orient_matrix_UB_33      -0.0497558000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0752
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25913
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.981
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             2204
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         9174
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.0975
_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/[\s^2^(Fo^2^)+(0.0189P)^2^+27.3117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1865
_refine_ls_wR_factor_ref         0.1958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6912
_reflns_number_total             9174
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02307a2.cif
_cod_data_source_block           mnbpy_sq
_cod_database_code               7714079
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.947
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C23(H23), C24(H24), C25(H25),
 C28(H28), C29(H29), C30(H30)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C)
;
_shelx_res_checksum              78692
_shelx_fab_checksum              88196
_platon_squeeze_special_details
;
A solvent mask was calculated and 188 electrons were 
found in a volume of 658\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
[+ solvents]1[C2H5OC2H5], 1[] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.289
_oxdiff_exptl_absorpt_empirical_full_min 0.756