Slow magnetic relaxation in mononuclear octa-coordinate Fe(ii) and Co(ii) complexes from a Bpybox ligand
Li, Rui-Xia; Sun, Hui-Ying; Liang, Hai-Chao; Yi, Cheng; Yao, Nian-Tao; Meng, Yin-Shan; Xiong, Jin; Liu, Tao; Zhu, Yuan-Yuan; Dalton Transactions  (2022) –; doi:10.1039/D2DT00865C

data_7710369
_publ_section_title
;
 Slow magnetic relaxation in mononuclear octa-coordinate Fe(ii) and Co(ii)
 complexes from a Bpybox ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00865C
_journal_year                    2022
_chemical_compound_source        none
_chemical_formula_moiety         'C32 H28 Fe N8 O4, 2(Cl O4), 0.5(C2 H3 N)'
_chemical_formula_sum            'C33 H29.5 Cl2 Fe N8.5 O12'
_chemical_formula_weight         863.90
_chemical_name_common            1-Fe
_chemical_name_systematic        1-Fe
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-02-25 deposited with the CCDC.	2022-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.692(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.844(3)
_cell_length_b                   8.7570(11)
_cell_length_c                   31.467(3)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.29
_cell_volume                     6973.7(14)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            90316
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.606
_diffrn_reflns_theta_min         2.280
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6579
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1382 before and 0.0670 after correction.
The Ratio of minimum to maximum transmission is 0.8824.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_description       needle
_exptl_crystal_F_000             3544
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         16122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0338P)^2^+7.4866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0902
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11308
_reflns_number_total             16122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00865c2.cif
_cod_data_source_block           1-Fe
_cod_depositor_comments
;

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C66 H59 Cl4 Fe2 N17 O24'
_cod_original_formula_weight         1727.80
_cod_original_formula_moiety         '2(C32 H28 Fe N8 O4), 4(Cl O4), C2 H3 N'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        6973.6(14)
_cod_database_code               7710369
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C63(H63A,
 H63B), C64(H64A,H64B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C21(H21), C22(H22),
 C23(H23), C26(H26), C27(H27), C28(H28), C37(H37), C38(H38), C39(H39), C42(H42),
  C43(H43), C44(H44), C53(H53), C54(H54), C55(H55), C58(H58), C59(H59), C60(H60)
2.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C)
;
_olex2_submission_special_instructions 'No special instructions were received'