Metal-to-metal communication during the spin state transition of a [2 × 2] Fe(ii) metallogrid at equilibrium and out-of-equilibrium conditions
Velazquez-Garcia, Jose de Jesus; Basuroy, Krishnayan; Storozhuk, Darina; Wong, Joanne; Demeshko, Serhiy; Meyer, Franc; Henning, Robert; Techert, Simone; Dalton Transactions  (2022) –; doi:10.1039/D1DT04255F

data_7709882
_publ_section_title
;
 Metal-to-metal communication during the spin state transition of a [2
 \\times 2] Fe(ii) metallogrid at equilibrium and out-of-equilibrium
 conditions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04255F
_journal_year                    2022
_chemical_formula_moiety         'C92 H62 Fe3 N24, 4(B F4)'
_chemical_formula_sum            'C92 H62 B4 F16 Fe2.09 N24'
_chemical_formula_weight         1967.34
_chemical_name_common
'[Fe3(3,5-Bis{6(2,2'-dipyridyl)}H-pyrazole)2(3,5-Bis{6(2,2'-dipyridyl)}pyrazole)2](BF4)4(C2NH3)'
_chemical_name_systematic
'[Fe3(3,5-Bis{6(2,2'-dipyridyl)}H-pyrazole)2(3,5-Bis{6(2,2'-dipyridyl)}pyrazole)2](BF4)4(C2NH3)'
_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
_audit_creation_date             2019-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-21 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.7330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5550(4)
_cell_length_b                   15.3500(4)
_cell_length_c                   26.2590(4)
_cell_measurement_reflns_used    8017
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      23.408
_cell_measurement_theta_min      1.473
_cell_volume                     8879.6(3)
_computing_cell_refinement       Precognition
_computing_data_collection       'Laue collect'
_computing_data_reduction        Epinorm
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ShelX
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.674
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type
'Standard Huber 515.2 kappa model (APS 14 ID Beamline)'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3116
_diffrn_reflns_av_unetI/netI     0.3707
_diffrn_reflns_Laue_measured_fraction_full 0.674
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            121706
_diffrn_reflns_point_group_measured_fraction_full 0.674
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        23.013
_diffrn_reflns_theta_max         23.013
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'undulator radiation'
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4001
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0028(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         8341
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.2511
_refine_ls_R_factor_gt           0.0845
_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^)+(0.1359P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.2003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4993
_reflns_number_total             8341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04255f3.cif
_cod_data_source_block           tr_2013_fe3_200k_50ps
_cod_database_code               7709882
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.811
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N11(H11), C1(H1), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11A),
 C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
  C23(H23), C31(H31), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41),
 C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52),
  C53(H53), C61(H61), C65(H65), C66(H66), C67(H67), C70(H70), C71(H71),
 C72(H72), C73(H73), C75(H75), C76(H76), C77(H77), C80(H80), C81(H81), C82(H82),
  C83(H83), C91(H91), C95(H95), C96(H96), C97(H97), C11A(H11B), C12A(H12A),
 C10B(H10B), C105(H105), C106(H106), C107(H107), C110(H110), C111(H111),
 C112(H112), C113(H113), C0AA(H0AA)
;
_shelx_res_checksum              27809
_olex2_submission_special_instructions 'No special instructions were received'