Electronic Conductivity, Ferrimagnetic Ordering, and Reductive Insertion Mediated by Organic Mixed-Valence in a Ferric Semiquinoid Metal-Organic Framework.
Darago, Lucy E.; Aubrey, Michael L.; Yu, Chung Jui; Gonzalez, Miguel I.; Long, Jeffrey R.; Journal of the American Chemical Society 137 (2015) 15703–15711; doi:10.1021/jacs.5b10385

data_4129764
_publ_section_title
;
 Electronic Conductivity, Ferrimagnetic Ordering, and Reductive Insertion
 Mediated by Organic Mixed-Valence in a Ferric Semiquinoid Metal-Organic
 Framework.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15703
_journal_page_last               15711
_journal_paper_doi               10.1021/jacs.5b10385
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         '0.25(C72 H24 Fe8 O48), 2(C16 H36 N)'
_chemical_formula_sum            'C50 H78 Fe2 N2 O12'
_chemical_formula_weight         1010.84
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1401(5)
_cell_length_b                   22.1401(5)
_cell_length_c                   22.1401(5)
_cell_measurement_reflns_used    9406
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.15
_cell_measurement_theta_min      3.24
_cell_volume                     10852.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46510
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        30.185
_diffrn_reflns_theta_max         30.185
_diffrn_reflns_theta_min         2.808
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0952 before and 0.0766 after correction.
The Ratio of minimum to maximum transmission is 0.8754.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         1397
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0733
_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^)+(0.0770P)^2^+82.0727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2064
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1268
_reflns_number_total             1397
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10385_si_002.cif
_cod_data_source_block           led015s
_cod_original_cell_volume        10852.7(7)
_cod_database_code               4129764
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.979
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49 0.51
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-C4 = N1-C11 = N1-C8 = N1-C15
 1.47 with sigma of 0.02
 C1AA-C8 = C12-C11 = C15-C16 = C5-C4 = C1AA-C9 = C5-C6 = C17-C16 = C12-C13 =
 C9-C10 = C7-C6 = C17-C18 = C14-C13
 1.54 with sigma of 0.02
4. Rigid body (RIGU) restrains
 N1, C8, C1AA, C11, C15, C4, C9, C12, C16, C5, C10, C13, C17, C6, C14, C18, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C8(0.33333) H8A(0.33333) H8B(0.33333) N1(0.33333) C11(0.33333)
 H11A(0.33333) H11B(0.33333) C9(0.33333) H9A(0.33333) H9B(0.33333) C12(0.33333)
 H12A(0.33333) H12B(0.33333) C16(0.33333) H16A(0.33333) H16B(0.33333)
 C15(0.33333) H15A(0.33333) H15B(0.33333) C17(0.33333) H17A(0.33333)
 H17B(0.33333) C1AA(0.33333) H1AA(0.33333) H1AB(0.33333) C4(0.33333)
 H4A(0.33333) H4B(0.33333) C5(0.33333) H5A(0.33333) H5B(0.33333) C10(0.33333)
 H10A(0.33333) H10B(0.33333) H10C(0.33333) C7(0.33333) H7A(0.33333)
 H7B(0.33333) H7C(0.33333) C13(0.33333) H13A(0.33333) H13B(0.33333) C6(0.33333)
 H6A(0.33333) H6B(0.33333) C14(0.33333) H14A(0.33333) H14B(0.33333)
 H14C(0.33333) C18(0.33333) H18A(0.33333) H18B(0.33333) H18C(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C11(H11A,H11B), C9(H9A,H9B), C12(H12A,H12B), C16(H16A,H16B),
 C15(H15A,H15B), C17(H17A,H17B), C1AA(H1AA,H1AB), C4(H4A,H4B), C5(H5A,H5B),
 C13(H13A,H13B), C6(H6A,H6B)
6.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_shelx_res_checksum              98593
_shelx_hkl_checksum              20848
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'