Crystal Structures, Magnetic Properties, and Redox Behaviors of Carboxylato-Bridged Mn(II) Complexes with Ditopic Ligands Featuring N3-Coordination Sites
Sugiyama, Junya; Umemoto, Yusuke; Sato, Sota; Yoneda, Ko; Koikawa, Masayuki; Chemistry 6 (2024) 601–617; doi:10.3390/chemistry6040036

data_1572288
_publ_section_title
;
 Crystal Structures, Magnetic Properties, and Redox Behaviors of
 Carboxylato-Bridged Mn(II) Complexes with Ditopic Ligands Featuring
 N3-Coordination Sites
;
_journal_issue                   4
_journal_name_full               Chemistry
_journal_page_first              601
_journal_page_last               617
_journal_paper_doi               10.3390/chemistry6040036
_journal_volume                  6
_journal_year                    2024
_chemical_formula_moiety         'C34 H42 F Mn2 N6 O4, B F4'
_chemical_formula_sum            'C34 H42 B F5 Mn2 N6 O4'
_chemical_formula_weight         814.42
_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             2024-07-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                84.2060(10)
_cell_angle_beta                 88.346(2)
_cell_angle_gamma                81.786(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3107(2)
_cell_length_b                   11.4913(2)
_cell_length_c                   15.7802(3)
_cell_measurement_reflns_used    13554
_cell_measurement_temperature    301
_cell_measurement_theta_max      30.9850
_cell_measurement_theta_min      2.1000
_cell_volume                     1840.86(6)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      301.00
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.835
_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   -110.00  70.00   0.50    4.00    --  -20.00  45.00   0.00  360
  2  \w   -110.00  70.00   0.50    4.00    --  -20.00  45.00  90.00  360
;
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0116
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16511
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.802
_diffrn_reflns_theta_min         1.996
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87328
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.081(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9644
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0520P)^2^+0.2812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8846
_reflns_number_total             9644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Complex1.cif
_cod_data_source_block           mn2tphnbf4
_cod_database_code               1572288
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.655
_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. Restrained distances
 B1A-F6B = B1A-F3B = B1A-F4B = B1A-F5B
 1.42 with sigma of 0.02
 B1A-F6B \\sim B1A-F3B \\sim B1A-F4B \\sim B1A-F5B
 with sigma of 0.02
 F6B-F3B \\sim F3B-F4B \\sim F4B-F5B \\sim F5B-F6B \\sim F3B-F5B \\sim F6B-F4B
 with sigma of 0.04
 B1A-F6B \\sim B1B-F3A
 with sigma of 0.02
 B1A-F3B \\sim B1B-F6A
 with sigma of 0.02
 B1A-F4B \\sim B1B-F5A
 with sigma of 0.02
 B1A-F5B \\sim B1B-F4A
 with sigma of 0.02
 F6B-F3B \\sim F3A-F6A
 with sigma of 0.04
 F6B-F4B \\sim F3A-F5A
 with sigma of 0.04
 F6B-F5B \\sim F3A-F4A
 with sigma of 0.04
 F3B-F4B \\sim F6A-F5A
 with sigma of 0.04
 F3B-F5B \\sim F6A-F4A
 with sigma of 0.04
 F4B-F5B \\sim F5A-F4A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
F3B \\sim F4B \\sim F5B \\sim F6B \\sim B1A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 F3B, F4B, F5B, F6B, B1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3B, F6B, F4B, B1A, F5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4A, B1B, F6A, F5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(B1B)=1-FVAR(1)
 Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(B1A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C25(H25A,H25B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C21(H21),
 C22(H22), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30)
6.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              26280
_shelx_hkl_checksum              24972
_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
- Detector area scaling
;