Dihalogen-substituted [Mn<sup>III</sup>(3,5-diHal-sal<sub>2</sub>323)]BPh<sub>4</sub> salts: so similar but so different.
Korchagin, D. V.; Shilov, G. V.; Zhidkov, M. V.; Dmitriev, A. I.; Palii, A. V.; Yagubskii, E. B.; Aldoshin, S. M.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 5064–5074; doi:10.1039/d5dt03065j

data_7720325
_publ_section_title
;
 Dihalogen-substituted
 [Mn<sup>III</sup>(3,5-diHal-sal<sub>2</sub>323)]BPh<sub>4</sub> salts: so
 similar but so different.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5064
_journal_page_last               5074
_journal_paper_doi               10.1039/d5dt03065j
_journal_volume                  55
_journal_year                    2026
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C22 H24 Br2 Cl2 Mn N4 O2, C24 H20 B'
_chemical_formula_sum            'C46 H44 B Br2 Cl2 Mn N4 O2'
_chemical_formula_weight         981.32
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2026-02-03
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2026-02-17 deposited with the CCDC.	2026-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                79.988(3)
_cell_angle_beta                 86.273(3)
_cell_angle_gamma                76.064(2)
_cell_formula_units_Z            4
_cell_length_a                   13.5019(4)
_cell_length_b                   14.1532(4)
_cell_length_c                   23.1498(7)
_cell_measurement_reflns_used    15839
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      30.4860
_cell_measurement_theta_min      3.1020
_cell_volume                     4227.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2060
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0832
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47701
_diffrn_reflns_point_group_measured_fraction_full 0.780
_diffrn_reflns_point_group_measured_fraction_max 0.744
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.500
_diffrn_reflns_theta_min         2.852
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       prism
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.451(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2090
_refine_ls_number_reflns         47701
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0624P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.490
_reflns_Friedel_fraction_full    0.562
_reflns_Friedel_fraction_max     0.490
_reflns_number_gt                34315
_reflns_number_total             47701
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9534\% 
around [0.69 -0.01 0.72] (reciprocal) or [0.90 -0.30 0.30] (direct)

_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.4593 23974 25981 ref  1.0000  0.0000  0.0000  0.0000  1.0000  0.0000  0.0000  0.0000  1.0000
2 0.5407 23978 25981 nmt  0.4834 -0.4951  0.4943 -0.0145 -0.9963 -0.0056  1.5393 -0.5121 -0.4877
_oxdiff_twin_integration_method simultaneous
;
_cod_data_source_file            d5dt03065j2.cif
_cod_data_source_block           3_100_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7720322--7720333.cif.'
_cod_database_code               7720325
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.648
_shelx_estimated_absorpt_t_min   0.490
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4694(5)
 0.5306(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
4.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N7(H7), N8(H8A), N10(H10), N11(H11A), N14(H14), N15(H15)
4.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,
 H19B), C20(H20A,H20B), C85(H85A,H85B), C86(H86A,H86B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C87(H87A,H87B), C88(H88A,H88B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,
 H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B),
 C62(H62A,H62B), C77(H77A,H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B),
  C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C4(H4), C6(H6), C8(H8), C11(H11), C13(H13), C21(H21), C24(H24),
 C26(H26), C28(H28), C32(H32), C34(H34), C43(H43), C45(H45), C47(H47), C50(H50),
  C51(H51), C53(H53), C65(H65), C67(H67), C69(H69), C70(H70), C73(H73),
 C75(H75), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96), C97(H97),
  C98(H98), C99(H99), C100(H100), C102(H102), C103(H103), C104(H104),
 C105(H105), C106(H106), C108(H108), C109(H109), C110(H110), C111(H111),
 C112(H112), C114(H114), C115(H115), C116(H116), C117(H117), C118(H118),
 C120(H120), C121(H121), C122(H122), C123(H123), C124(H124), C126(H126),
 C127(H127), C128(H128), C129(H129), C130(H130), C132(H132), C133(H133),
 C134(H134), C135(H135), C136(H136), C138(H138), C139(H139), C140(H140),
 C141(H141), C142(H142), C144(H144), C145(H145), C146(H146), C147(H147),
 C148(H148), C150(H150), C151(H151), C152(H152), C153(H153), C154(H154),
 C156(H156), C157(H157), C158(H158), C159(H159), C160(H160), C162(H162),
 C163(H163), C164(H164), C165(H165), C166(H166), C168(H168), C169(H169),
 C170(H170), C171(H171), C172(H172), C174(H174), C175(H175), C176(H176),
 C177(H177), C178(H178), C180(H180), C181(H181), C182(H182), C183(H183),
 C184(H184)
;
_shelx_res_checksum              11766
_shelx_hkl_checksum              34090
_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 1.300
_oxdiff_exptl_absorpt_empirical_full_min 0.798