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_7706275
_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, B F4'
_chemical_formula_sum            'C30 H42 B F4 Mn2 N12 O6'
_chemical_formula_weight         863.44
_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
_audit_creation_date             2020-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-07 deposited with the CCDC.	2020-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.077(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.308(3)
_cell_length_b                   17.943(5)
_cell_length_c                   11.085(3)
_cell_measurement_reflns_used    5518
_cell_measurement_temperature    293.(2)
_cell_measurement_theta_max      22.7554
_cell_measurement_theta_min      2.2887
_cell_volume                     2045.1(10)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayered confocal mirror'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.1015
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24033
_diffrn_reflns_point_group_measured_fraction_full 0.496
_diffrn_reflns_point_group_measured_fraction_max 0.496
_diffrn_reflns_theta_full        23.644
_diffrn_reflns_theta_max         23.644
_diffrn_reflns_theta_min         2.16
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Bruker Turbo X-ray Source'
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            'clear dark blue-green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue-green
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             890
_exptl_crystal_recrystallization_method
'Methanol diffusion in water solution of the constituants'
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.032
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         3059
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                1916
_reflns_number_total             3059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03243c2.cif
_cod_data_source_block           ([Mn2(NITIm)3](BF4))n_293k
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7706275
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9A(H9A), C10A(H10A), C9B(H9B), C10B(H10B), C9C(H9C), C10C(H10C)
2.b Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C7A(H7AA,H7AB,
 H7AC), C4B(H4BA,H4BB,H4BC), C5B(H5BA,H5BB,H5BC), C6B(H6BA,H6BB,H6BC), C7B(H7BA,
 H7BB,H7BC), C4C(H4CA,H4CB,H4CC), C5C(H5CA,H5CB,H5CC), C6C(H6CA,H6CB,H6CC),
 C7C(H7CA,H7CB,H7CC)
;
_olex2_submission_special_instructions 'No special instructions were received'