Near Room Temperature Stepwise Spin State Switching and Photomagnetic Effect in a Mixed-Valence Molecular Square
Kamilya, Sujit; Mehta, Sakshi; Lescouezec, Rodrigue; Li, Yanling; Pechousek, Jiri; Semwal, Mohini; Mondal, Abhishake; Dalton Transactions  (2023) –; doi:10.1039/D3DT01615C

data_7713460
_publ_section_title
;
 Near Room Temperature Stepwise Spin State Switching and Photomagnetic
 Effect in a Mixed-Valence Molecular Square
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT01615C
_journal_year                    2023
_chemical_formula_moiety
'C74 H82 B2 Fe4 N38 O4, 2(C15 H13 B Fe N11), 4(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C108 H128 B4 Fe6 N60 O10'
_chemical_formula_weight         2805.04
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-03-29 deposited with the CCDC.	2023-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                87.675(4)
_cell_angle_beta                 78.345(3)
_cell_angle_gamma                79.489(3)
_cell_formula_units_Z            1
_cell_length_a                   11.9811(5)
_cell_length_b                   14.8759(6)
_cell_length_c                   18.5704(8)
_cell_measurement_reflns_used    3846
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      2.7
_cell_volume                     3187.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.906
_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  0.1109
_diffrn_reflns_av_unetI/netI     0.1757
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38481
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.594
_diffrn_reflns_theta_min         2.240
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.287
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         17770
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1985
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1220P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2059
_refine_ls_wR_factor_ref         0.2638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7812
_reflns_number_total             17770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01615c2.cif
_cod_data_source_block           test_1_a
_cod_database_code               7713460
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O4(H4A,H4B)
2.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C23(H23A,H23B), C25(H25A,H25B), C34(H34A,H34B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C43(H43), N11(H11), C42(H42), C49(H49), C9(H9), C13(H13), C5(H5),
 C12(H12), C50(H50), C47(H47), C32(H32), C21(H21), C33(H33), C17(H17), C16(H16),
  C27(H27), C22(H22), C45(H45), C14(H14), C51(H51), C4(H4), C6(H6), C10(H10),
 C41(H41), C7(H7), C48(H48), C46(H46), C11(H11A), C44(H44), N30(H30), C15(H15),
 C52(H52), C28(H28)
2.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C35(H35A,H35B,H35C), C24(H24A,H24B,H24C), C37(H37A,H37B,
 H37C), C26(H26A,H26B,H26C), C55(H55A,H55B,H55C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O5(H5A)
;
_shelx_res_checksum              92776
_olex2_submission_special_instructions 'No special instructions were received'