Slow Magnetic Relaxation in 8-Coordinate Mn(II) Compounds
Wang, Li-Xin; Wu, Xiao-Fan; Jin, Xinxin; Li, Jia-Yi; Wang, Bingwu; Liu, Jiyan; Xiang, Jing; Gao, Song; Dalton Transactions  (2023) –; doi:10.1039/D3DT02307A

data_7714078
_publ_section_title
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 Slow Magnetic Relaxation in 8-Coordinate Mn(II) Compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02307A
_journal_year                    2023
_chemical_formula_moiety         'C44 H52 Mn N8 O4, 2(Cl O4), H2 O'
_chemical_formula_sum            'C44 H54 Cl2 Mn N8 O13'
_chemical_formula_weight         1028.79
_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   mixed
_audit_creation_date             2021-08-29
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2022-09-17 deposited with the CCDC.	2023-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.152(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8971(2)
_cell_length_b                   21.2744(3)
_cell_length_c                   16.6480(3)
_cell_measurement_reflns_used    11448
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.3930
_cell_measurement_theta_min      4.1450
_cell_volume                     4727.74(14)
_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)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.536
_diffrn_reflns_theta_min         3.457
_exptl_absorpt_coefficient_mu    3.926
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49309
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         9288
_refine_ls_number_restraints     1764
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0432P)^2^+3.4031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8189
_reflns_number_total             9288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02307a2.cif
_cod_data_source_block           1234
_cod_database_code               7714078
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.672
_shelx_estimated_absorpt_t_min   0.650
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 3.8A
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C42(H42A,H42B), C43(H43A,H43B), C26(H26A,H26B), C25(H25A,
 H25B), C4(H4A,H4B), C41(H41A,H41B), C19(H19A,H19B), C21(H21A,H21B), C2(H2A,
 H2B), C24(H24A,H24B), C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 N4(H4), N8(H8), N3(H3), C35(H35), C7(H7), N7(H7A), C36(H36), C29(H29),
 C38(H38), C37(H37), C16(H16), C13(H13), C15(H15), C8(H8A), C14(H14), C30(H30)
3.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              3267
_olex2_submission_special_instructions 'No special instructions were received'