Magnetic ordering in TCNQ-based metal‒organic frameworks with host‒guest interactions
Zhang, Xuan; Saber, Mohamed R.; Prosvirin, Andrey P.; Reibenspies, Joseph H.; Sun, Lei; Ballesteros-Rivas, Maria; Zhao, Hanhua; Dunbar, Kim R.; Inorganic Chemistry Frontiers 2 (2015) 904–; doi:10.1039/C5QI00128E

data_4348961
_publ_section_title
;
 Magnetic ordering in TCNQ-based metal--organic frameworks with
 host--guest interactions
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              904
_journal_paper_doi               10.1039/C5QI00128E
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety         '0.25(C88 H48 Fe4 N24), 2(C6 H7 N)'
_chemical_formula_sum            'C34 H26 Fe N8'
_chemical_formula_weight         602.48
_chemical_name_common            FeTCNQ(4,4'-bpy)_aniline
_chemical_name_systematic
'Iron(II) tetracyanoquinodimethane 4,4'-bipyridyl aniline'
_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-22 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.340(2)
_cell_length_b                   12.340(2)
_cell_length_c                   22.852(4)
_cell_measurement_temperature    110
_cell_volume                     3479.8(10)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0112
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15663
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.782
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0507 before and 0.0431 after correction. The Ratio of minimum to maximum transmission is 0.8856. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.296
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     60
_refine_ls_number_reflns         838
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1192P)^2^+18.2775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2003
_refine_ls_wR_factor_ref         0.2258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                715
_reflns_number_total             838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00128e2.cif
_cod_data_source_block           i4mcm
_cod_original_cell_volume        3480.0(13)
_cod_database_code               4348961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Rigid bond restraints
 Fe1, N1, C1, C2, C3, C4, N2, C5, C6, C7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Fe1 \\sim N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim N2 \\sim C5 \\sim C6
\\sim C7: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.01
Uiso(N1A) = Uiso(C1A) = Uiso(C2A) = Uiso(C3A) = Uiso(C4A) = Uiso(C5A) =
Uiso(C6A)
4. Others
 Fixed Sof: C5(0.5) H5(0.5) C6(0.5) H6(0.5) N1A(0.25) H1AA(0.25) H1AB(0.25)
 C1A(0.25) C2A(0.25) H2A(0.25) C3A(0.25) H3A(0.25) C4A(0.25) H4A(0.25)
 C5A(0.25) H5A(0.25) C6A(0.25) H6A(0.25)
5.a Free rotating group:
 N1A(C1A,C2A,C3A,C4A,C5A,C6A)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A)
5.c X=CH2 refined with riding coordinates:
 N1A(H1AA,H1AB)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'