2D Conductive Iron-Quinoid Magnets Ordering up to T<sub>c</sub> = 105 K via Heterogenous Redox Chemistry.
DeGayner, Jordan A.; Jeon, Ie-Rang; Sun, Lei; Dincă, Mircea; Harris, T. David; Journal of the American Chemical Society 139 (2017) 4175–4184; doi:10.1021/jacs.7b00705

data_4131227
_publ_section_title
;
 2D Conductive Iron-Quinoid Magnets Ordering up to T<sub>c</sub> = 105 K
 via Heterogenous Redox Chemistry.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4175
_journal_page_last               4184
_journal_paper_doi               10.1021/jacs.7b00705
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         '0.5(C18 Cl6 Fe2 O12), 3(C0.67 H2.67 N0.33)'
_chemical_formula_sum            'C11 H8 Cl3 Fe N O6'
_chemical_formula_weight         412.38
_chemical_name_systematic        (Cp2Co)(Me2NH2)[Fe2(CA)3]
_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     dual
_audit_creation_date             2017-01-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.5835(11)
_cell_length_b                   13.5835(11)
_cell_length_c                   8.6796(13)
_cell_measurement_reflns_used    994
_cell_measurement_temperature    100
_cell_measurement_theta_max      44.74
_cell_measurement_theta_min      3.76
_cell_volume                     1386.9(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.774
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker Kappa 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  0.0799
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.774
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4588
_diffrn_reflns_point_group_measured_fraction_full 0.774
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         58.977
_diffrn_reflns_theta_min         5.096
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    7.169
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.4707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1063 before and 0.0531 after correction. The Ratio of minimum to maximum transmission is 0.6263. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    0.987
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         711
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1602
_refine_ls_R_factor_gt           0.1222
_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          0.2762
_refine_ls_wR_factor_ref         0.3189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                399
_reflns_number_total             711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00705_si_002.cif
_cod_data_source_block           jd_p-31m
_cod_database_code               4131227
_shelxl_version_number           2014-3
_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
 C3_$1-C3
 2.47 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: N1(0.16667) H1A(0.16667) H1B(0.16667) C3(0.33333) H3A(0.33333)
 H3B(0.33333) H3C(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
5.b Me refined with riding coordinates:
 C3(H3A,H3B,H3C)
;
_shelx_res_checksum              32224
_shelx_hkl_checksum              65384
_shelx_fab_checksum              90618
_olex2_submission_original_sample_id Cmpd2
_olex2_submission_special_instructions 'No special instructions were received'