Thermally-induced hysteretic valence tautomeric conversions in the solid state <i>via</i> two-step labile electron transfers in manganese-nitronyl nitroxide 2D-frameworks.
Lecourt, Constance; Izumi, Yuuta; Khrouz, Lhoussain; Toche, François; Chiriac, Rodica; Bélanger-Desmarais, Nicolas; Reber, Christian; Fabelo, Oscar; Inoue, Katsuya; Desroches, Cédric; Luneau, Dominique; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15646–15662; doi:10.1039/d0dt03243c

data_7706274
_publ_section_title
;
 Thermally-induced hysteretic valence tautomeric conversions in the solid
 state <i>via</i> two-step labile electron transfers in manganese-nitronyl
 nitroxide 2D-frameworks.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15646
_journal_page_last               15662
_journal_paper_doi               10.1039/d0dt03243c
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         ' C30 H42 Mn2 N12 O6, P F6'
_chemical_formula_sum            'C30 H42 F6 Mn2 N12 O6 P'
_chemical_formula_weight         921.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-07 deposited with the CCDC.	2020-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.362(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.850(2)
_cell_length_b                   17.085(4)
_cell_length_c                   11.085(3)
_cell_measurement_reflns_used    3821
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.2
_cell_measurement_theta_min      2.6
_cell_volume                     2048.9(8)
_computing_cell_refinement       SAINT
_computing_data_collection       SAINT
_computing_data_reduction        SAINT
_computing_molecular_graphics    'VESTA (Momma & Izumi, 2006)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  '8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.1365
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18850
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.646
_diffrn_reflns_theta_min         3.999
_diffrn_source                   'ImS 3.0 micro source'
_exptl_absorpt_coefficient_mu    6.120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
;
_exptl_crystal_colour            Dark-black
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       Plate-like
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.753
_exptl_transmission_factor_min   0.443
_refine_diff_density_max         2.431
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.158
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         6880
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.1227
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2936
_refine_ls_wR_factor_ref         0.3399
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    0.881
_reflns_Friedel_fraction_max     0.863
_reflns_number_gt                3859
_reflns_number_total             6880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03243c2.cif
_cod_data_source_block           ([Mn2(NITIm)3]PF6)n
_cod_original_cell_volume        2049.0(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7706274
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.750
_shelx_estimated_absorpt_t_max   0.750
_shelx_res_checksum              55860