Unlocking single molecule magnetism: a supramolecular strategy for isolating neutral Mn<sup>III</sup> salen-type dimer in crystalline environments.
Kyoya, Yuri; Takahashi, Kiyonori; Kosaka, Wataru; Huang, Rui-Kang; Xue, Chen; Wu, Jia-Bing; Miyasaka, Hitoshi; Nakamura, Takayoshi; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7517–7521; doi:10.1039/d4dt00323c

data_7715656
_publ_section_title
;
 Unlocking single molecule magnetism: a supramolecular strategy for
 isolating neutral Mn<sup>III</sup> salen-type dimer in crystalline
 environments.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7517
_journal_page_last               7521
_journal_paper_doi               10.1039/d4dt00323c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C24 H32 O8, 2(C18 H18 Cl Mn N2 O4)'
_chemical_formula_sum            'C60 H68 Cl2 Mn2 N4 O16'
_chemical_formula_weight         1281.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-30 deposited with the CCDC.	2024-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.277(4)
_cell_angle_beta                 102.249(5)
_cell_angle_gamma                98.094(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4886(7)
_cell_length_b                   11.1906(6)
_cell_length_c                   12.9544(7)
_cell_measurement_reflns_used    5135
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      71.4050
_cell_measurement_theta_min      4.3250
_cell_volume                     1470.14(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.948
_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    -81.00 -51.00   0.50    9.34    --    0.00  37.00 -60.00   60
  2  \w      6.00  61.00   0.50    9.34    --    0.00  37.00 -60.00  110
  3  \w    -62.00  89.00   0.50    9.34    --    0.00   0.00-180.00  302
  4  \w     32.00  89.00   0.50   37.35    --    5.00  28.00  30.00  114
  5  \w    -54.00 -23.00   0.50   37.35    --  -94.70  55.00   0.54   62
  6  \w   -169.00-143.00   0.50   37.35    --  -94.70  55.00-165.32   52
  7  \w    -45.00  -9.00   0.50   37.35    --  -94.70  55.00 -95.69   72
  8  \w    -73.00  -8.00   0.50   37.35    --  -94.70  55.00 -50.26  130
  9  \w    -94.00 -67.00   0.50   37.35    --  -94.70  55.00   0.54   54
 10  \w   -164.00-138.00   0.50   37.35    --  -94.70  55.00 172.35   52
 11  \w   -170.00-144.00   0.50   37.35    --  -94.70  53.00 100.98   52
 12  \w   -131.00  -5.00   0.50   37.35    --  -94.70  53.00 100.98  252
 13  \w   -170.00 -83.00   0.50   37.35    --  -94.70  55.00 -50.26  174
 14  \w    -68.00 -18.00   0.50   37.35    --  -94.70  55.00  49.58  100
 15  \w   -183.00 -75.00   0.50   37.35    --  -94.70  55.00  49.58  216
 16  \w   -138.00  -8.00   0.50   37.35    --  -94.70  55.00-165.32  260
 17  \w   -182.00  -5.00   0.50   37.35    --  -94.70  55.00 124.92  354
 18  \w   -136.00-111.00   0.50   37.35    --  -94.70  37.00-150.00   50
 19  \w    -88.00 -14.00   0.50   37.35    --  -94.70  37.00-150.00  148
 20  \w   -182.00-108.00   0.50   37.35    --  -94.70  46.00 -60.00  148
 21  \w   -162.00-123.00   0.50   37.35    --  -94.70  55.00   0.54   78
 22  \w    -96.00 -53.00   0.50   37.35    --  -94.70  55.00 -95.69   86
 23  \w    -60.00 -35.00   0.50   37.35    --  -94.70  55.00 172.35   50
 24  \w   -183.00-134.00   0.50   37.35    --  -94.70  55.00 -95.69   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0122782000
_diffrn_orient_matrix_UB_12      -0.1381720000
_diffrn_orient_matrix_UB_13      0.0090715000
_diffrn_orient_matrix_UB_21      -0.1144928000
_diffrn_orient_matrix_UB_22      0.0020891000
_diffrn_orient_matrix_UB_23      0.0570568000
_diffrn_orient_matrix_UB_31      -0.0990817000
_diffrn_orient_matrix_UB_32      -0.0162513000
_diffrn_orient_matrix_UB_33      -0.1071930000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15676
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.205
_diffrn_reflns_theta_min         3.494
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.943
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         5577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1526P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3901
_reflns_number_total             5577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00323c1.cif
_cod_data_source_block           exp_741_auto
_cod_depositor_comments          'Adding full bibliography for 7715656.cif.'
_cod_database_code               7715656
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         MnNOFeHClC
_chemical_oxdiff_usercomment     293k
_reflns_odcompleteness_completeness 98.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C26(H26A,H26B), C10(H10A,H10B), C28(H28A,H28B), C27(H27A,H27B),
 C25(H25A,H25B), C29(H29A,H29B), C30(H30A,H30B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C11(H11), C16(H16), C7(H7), C14(H14), C15(H15), C22(H22), C6(H6),
 C5(H5), C21(H21), C20(H20), C19(H19)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              89383
_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 1.628
_oxdiff_exptl_absorpt_empirical_full_min 0.424