Solid-State Redox Switching of Magnetic Exchange and Electronic Conductivity in a Benzoquinoid-Bridged Mn(II) Chain Compound.
Jeon, Ie-Rang; Sun, Lei; Negru, Bogdan; Van Duyne, Richard P.; Dincă, Mircea; Harris, T. David; Journal of the American Chemical Society 138 (2016) 6583–6590; doi:10.1021/jacs.6b02485

data_4130349
_publ_section_title
;
 Solid-State Redox Switching of Magnetic Exchange and Electronic
 Conductivity in a Benzoquinoid-Bridged Mn(II) Chain Compound.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6583
_journal_page_last               6590
_journal_paper_doi               10.1021/jacs.6b02485
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C20 H16 Mn N4 O5 S'
_chemical_formula_sum            'C20 H16 Mn N4 O5 S'
_chemical_formula_weight         479.37
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   9.1358(2)
_cell_length_b                   9.1358(2)
_cell_length_c                   21.2002(6)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.14
_cell_measurement_theta_min      5.59
_cell_volume                     1532.37(6)
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.95
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12254
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.135
_diffrn_reflns_theta_min         5.591
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.576
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
? was used for absorption correction.
wR2(int) was 0.0821 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.8370.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             735
_exptl_crystal_size_max          0.164
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1371 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.012(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         3164
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0320P)^2^+0.6530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0615
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.773
_reflns_Friedel_fraction_max     0.815
_reflns_number_gt                3130
_reflns_number_total             3164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b02485_si_002.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        1532.37(8)
_cod_database_code               4130349
_plat019_alert_1_b
;
PROBLEM: diffrn_measured_fraction_theta_full/_max < 1.0
RESPONSE: The crystal diffracted weakly at high resolution 
although this was the best crystal we could obtain.
;
_shelxl_version_number           2013-4
_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:
 C12(H12), C16(H16), C18(H18), C21(H21), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28), C29(H29)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              42448
_shelx_hkl_checksum              26565
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'