A 2D Semiquinone Radical-Containing Microporous Magnet with Solvent-Induced Switching from Tc = 26 to 80 K.
Jeon, Ie-Rang; Negru, Bogdan; Van Duyne, Richard P.; Harris, T. David; Journal of the American Chemical Society 137 (2015) 15699–15702; doi:10.1021/jacs.5b10382

data_4129762
_publ_section_title
;
 A 2D Semiquinone Radical-Containing Microporous Magnet with
 Solvent-Induced Switching from Tc = 26 to 80 K.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15699
_journal_page_last               15702
_journal_paper_doi               10.1021/jacs.5b10382
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'6(C0.67 H2.67 N0.33), C18 Cl6 Fe2 O12, 0.67(O3)'
_chemical_formula_sum            'C40 H62 Cl6 Fe2 N8 O20'
_chemical_formula_weight         1299.37
_space_group_crystal_system      trigonal
_space_group_IT_number           162
_space_group_name_Hall           '-P 3 2'
_space_group_name_H-M_alt        'P -3 1 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   13.5632(5)
_cell_length_b                   13.5632(5)
_cell_length_c                   8.7449(5)
_cell_measurement_reflns_used    3246
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.046
_cell_measurement_theta_min      3.76
_cell_volume                     1393.19(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5182
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        65.174
_diffrn_reflns_theta_max         65.173
_diffrn_reflns_theta_min         5.057
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.504
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0750 before and 0.0224 after correction.
The Ratio of minimum to maximum transmission is 0.8262.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         831
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0954
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2481
_refine_ls_wR_factor_ref         0.2651
_reflns_Friedel_coverage         0.000
_reflns_number_gt                701
_reflns_number_total             831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10382_si_002.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        1393.19(13)
_cod_database_code               4129762
_chemw03_alert_2_a
;
PROBLEM: The ratio of given/expected molecular weight 
as calculated from the _atom_site* data lies outside 
the range 0.90 <> 1.10
RESPONSE:Residual electron density found in the difference 
Fourier map was removed using the solvent mask protocol 
included in Olex2. This residual electron density likely 
arises from either residual DMF solvent molecules. 6 DMF 
solvent molecules are confirmed by elemental and thermal 
analyses and are taken into consideration for the molecular 
formula. Hydrogen atoms for water molecule were not introduced 
but are also taken into consideration for the molecular formula. 
Therefore, there is a hugh difference in given and expected 
molecular weight.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N3 \\sim C4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N3(0.16667) H3A(0.16667) H3B(0.16667) C4(0.33333) H4A(0.33333)
 H4B(0.33333) H4C(0.33333) O1(0.16667)
6.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B)
6.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_shelx_res_checksum              65550
_shelx_hkl_checksum              66775
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'