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_7714077
_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         'C28 H24 Mn N4 O8, 2(Cl O4), 0.4[H2O]'
_chemical_formula_sum            'C28 H24 Cl2 Mn N4 O16'
_chemical_formula_weight         798.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           50
_space_group_name_Hall           '-P 2ab 2b'
_space_group_name_H-M_alt        'P b a n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-30
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9383(13)
_cell_length_b                   16.4561(16)
_cell_length_c                   10.4468(10)
_cell_measurement_reflns_used    1789
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      27.8370
_cell_measurement_theta_min      3.0610
_cell_volume                     1708.5(3)
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -18.00  29.00   1.00    6.50    --   11.74 -99.00 120.00   47
  2  \w      6.00  35.00   1.00    6.50    --   11.74-132.00 -73.00   29
  3  \w    -60.00  13.00   1.00    6.50    --   11.74 -77.00-150.00   73
;
_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      0.0326789000
_diffrn_orient_matrix_UB_12      -0.0180987000
_diffrn_orient_matrix_UB_13      -0.0532382000
_diffrn_orient_matrix_UB_21      0.0429663000
_diffrn_orient_matrix_UB_22      -0.0216443000
_diffrn_orient_matrix_UB_23      0.0421131000
_diffrn_orient_matrix_UB_31      -0.0468214000
_diffrn_orient_matrix_UB_32      -0.0325179000
_diffrn_orient_matrix_UB_33      0.0016184000
_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  0.0537
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5694
_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         26.497
_diffrn_reflns_theta_min         2.394
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.622
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93785
_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    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         1780
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0832P)^2^+1.1785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1322
_reflns_number_total             1780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02307a2.cif
_cod_data_source_block           mn+b_sq
_cod_original_sg_symbol_H-M      'P b a n'
_cod_database_code               7714077
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.929
_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. Restrained distances
 O3-O1
 3 with sigma of 0.01
 Cl1-O5 = Cl1-O4 = Cl1-O6 = Cl1-O3
 1.42 with sigma of 0.01
 O4_$1-O1
 3 with sigma of 0.01
 O3-O4 \\sim O3-O5 \\sim O3-O6 \\sim O5-O6
 with sigma of 0.04
 Cl1-O3 \\sim Cl1-O4 \\sim Cl1-O5 \\sim Cl1-O6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl1 \\sim O3 \\sim O4 \\sim O5 \\sim O6: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
Cl2 \\sim O7 \\sim O8 \\sim O9 \\sim O10: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 Cl2, O8, O7, O10, O9
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Cl1, O3, O4, O5, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Same fragment restrains
{Cl2, O7, O8, O9, O10} sigma for 1-2: 0.02, 1-3: 0.02
as in
{Cl1, O3, O4, O5, O6}
6. Others
 Fixed Sof: Cl1(0.25) O3(0.25) O4(0.25) O5(0.25) O6(0.25) Cl2(0.25) O7(0.25)
 O8(0.25) O9(0.25) O10(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
7.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              96166
_shelx_fab_checksum              61360
_platon_squeeze_special_details
;
A solvent mask was calculated and 8 electrons were 
found in a volume of 52\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.4[H2O] per Asymmetric Unit 
which account for 8 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 1.101
_oxdiff_exptl_absorpt_empirical_full_min 0.918