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_4129763
_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
'C18 Cl6 O12 Zn2, 6(C0.67 H2.67 N0.33), 0.67(O3)'
_chemical_formula_sum            'C40 H62 Cl6 N8 O20 Zn2'
_chemical_formula_weight         1318.41
_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                   13.6682(6)
_cell_length_b                   13.6682(6)
_cell_length_c                   8.8870(5)
_cell_measurement_reflns_used    3679
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.93
_cell_measurement_theta_min      3.73
_cell_volume                     1437.83(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0296
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6412
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        58.927
_diffrn_reflns_theta_max         58.927
_diffrn_reflns_theta_min         3.734
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.251
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1124 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.7858.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.119
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         736
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0939
_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^)+(0.1977P)^2^+0.0891P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2327
_refine_ls_wR_factor_ref         0.2469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                628
_reflns_number_total             736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b10382_si_002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        1437.83(15)
_cod_database_code               4129763
_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.
;
_thetm01_alert_3_b
;
PROBLEM: The value of sine(theta_max)/wavelength is less 
than 0.575 Calculated sin(theta_max)/wavelength =    0.5555
RESPONSE: This crystals did not diffract out far, however, 
the structure was solved with out ambiguity.
;
_plat051_alert_1_b
;
PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by 7.38%
RESPONSE: Same reason as the one for CHEMW03_ALERT_2_A 
;
_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. Restrained distances
 N2-C1
 1.45 with sigma of 0.02
3. Rigid bond restraints
 N2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N2 \\sim C1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Fixed Sof: C1(0.33333) H1A(0.33333) H1B(0.33333) H1C(0.33333) N2(0.16667)
 H2A(0.16667) H2B(0.16667) O1(0.16667)
6.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B)
6.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              71607
_shelx_hkl_checksum              70832
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'