A combined experimental and theoretical study on a single, unsupported oxo-bridged Mn(III,III) dimer coordinated to two iminobenzosemiquinone π-radical anions.
Paul, Ganesh Chandra; Sarkar, Prasenjit; Sarmah, Amrit; Shaw, Prantick; Maity, Suvendu; Mukherjee, Chandan; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8768–8775; doi:10.1039/d1dt00489a

data_7707394
_publ_section_title
;
 A combined experimental and theoretical study on a single, unsupported
 oxo-bridged Mn(III,III) dimer coordinated to two iminobenzosemiquinone
 \p-radical anions.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8768
_journal_page_last               8775
_journal_paper_doi               10.1039/d1dt00489a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C66 H76 Mn2 N8 O3, 2(Cl O4), 4(C2 H3 N)'
_chemical_formula_sum            'C74 H88 Cl2 Mn2 N12 O11'
_chemical_formula_weight         1502.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-03-09
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2021.02.10 svn.rb'16c95d35' for OlexSys, GUI svn.r6225)
;
_audit_update_record
;
2021-04-20 deposited with the CCDC.	2021-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                71.247(6)
_cell_angle_beta                 78.540(7)
_cell_angle_gamma                82.261(7)
_cell_formula_units_Z            1
_cell_length_a                   11.6558(11)
_cell_length_b                   12.3631(9)
_cell_length_c                   13.9426(9)
_cell_measurement_reflns_used    3919
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      27.8210
_cell_measurement_theta_min      3.0750
_cell_volume                     1859.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00(13)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.172
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75508
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       needle
_exptl_crystal_F_000             788
_exptl_crystal_recrystallization_method
'dichloromethane methanol and acetonitrile mixture'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.532
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         6557
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0280P)^2^+1.5162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5312
_reflns_number_total             6557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00489a2.cif
_cod_data_source_block           exp_6567
_cod_depositor_comments          'Adding full bibliography for 7707394.cif.'
_cod_database_code               7707394
_shelx_shelxl_version_number     2018/3
_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. Uiso/Uaniso restraints and constraints
Cl1 \\sim Cl1A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(O6) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim
Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
3. Rigid body (RIGU) restrains
 O4, Cl1, O5, O3, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Cl1A, O4A, O5A, O3A, O6A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: Cl1(0.75) O4(0.75) O5(0.75) O3(0.75) O6(0.75) Cl1A(0.25) O4A(0.25)
 O5A(0.25) O3A(0.25) O6A(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C21(H21A,H21B), C28(H28A,H28B)
5.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C6(H6), C33(H33), C27(H27), C24(H24), C26(H26), C30(H30), C31(H31),
 C16(H16), C4(H4), C19(H19), C32(H32), C18(H18), C17(H17)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C)
;
_shelx_res_checksum              11197
_olex2_submission_special_instructions 'No special instructions were received'