The effect of fluorine substituents on the crystal structure and spin crossover behavior of the cation [MnIII(3,5-diHal-sal2323)]+ complex family with BPh4 anions
Tiunova, A. V.; Kazakova, A. V.; Korchagin, D. V.; Shilov, G. V.; Zakharov, K. V.; Vasiliev, A. N.; Yagubskii, E. B.; New Journal of Chemistry 46 (2022) 16880–16888; doi:10.1039/D2NJ02872G

data_7061711
_publ_section_title
;
 The effect of fluorine substituents on the crystal structure and spin
 crossover behavior of the cation [MnIII(3,5-diHal-sal2323)]+ complex
 family with BPh4 anions
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16880
_journal_page_last               16888
_journal_paper_doi               10.1039/D2NJ02872G
_journal_volume                  46
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C22 H24 Br2 F2 Mn N4 O2, C24 H20 B'
_chemical_formula_sum            'C46 H44 B Br2 F2 Mn N4 O2'
_chemical_formula_weight         948.42
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-29 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                105.613(7)
_cell_angle_beta                 102.473(6)
_cell_angle_gamma                111.889(8)
_cell_formula_units_Z            2
_cell_length_a                   13.1318(9)
_cell_length_b                   13.4997(13)
_cell_length_c                   14.3197(10)
_cell_measurement_reflns_used    3516
_cell_measurement_temperature    240.0(1)
_cell_measurement_theta_max      29.107
_cell_measurement_theta_min      2.9581
_cell_volume                     2121.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      240.00(10)
_diffrn_detector_area_resol_mean 16.2060
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0754
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17180
_diffrn_reflns_point_group_measured_fraction_full 0.703
_diffrn_reflns_point_group_measured_fraction_max 0.574
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.049
_diffrn_reflns_theta_min         2.964
_exptl_absorpt_coefficient_mu    2.246
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.130
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 2117 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.040(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         13019
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0797
_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^)+(0.1309P)^2^+2.5294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2103
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.341
_reflns_Friedel_fraction_full    0.407
_reflns_Friedel_fraction_max     0.292
_reflns_number_gt                9196
_reflns_number_total             13019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02872g2.cif
_cod_data_source_block           6_240
_cod_depositor_comments
;
Adding full bibliography for 7061703--7061711.cif.

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C92 H88 B2 Br4 F4 Mn2 N8 O4'
_cod_original_formula_weight         1896.84
_cod_original_formula_moiety         '2(C22 H24 Br2 F2 Mn N4 O2), 2(C24 H20 B)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2121.7(3)
_cod_database_code               7061711
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              4650