Synthesis, Structure, and Magnetic Properties of Valence Ambiguous Dinuclear Antiferromagnetically Coupled Cobalt and Ferromagnetically Coupled Iron Complexes Containing the Chloranilate(2-) and the Significantly Stronger Coupling Chloranilate(.3-) Radical Trianion
Kil Sik Min; Antonio G. DiPasquale; James A. Golen; Arnold L. Rheingold; Joel S. Miller; Journal of the American Chemical Society 129 (2007) 2360–2368; doi:10.1021/ja067208q

data_4109116
_publ_section_title
;
 Synthesis, Structure, and Magnetic Properties of Valence Ambiguous
 Dinuclear Antiferromagnetically Coupled Cobalt and Ferromagnetically
 Coupled Iron Complexes Containing the Chloranilate(2-) and the
 Significantly Stronger Coupling Chloranilate(.3-) Radical Trianion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2360
_journal_page_last               2368
_journal_paper_doi               10.1021/ja067208q
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C44 H39 B4 Cl2 Co2 F16 N9 O4'
_chemical_formula_weight         1293.83
_chemical_name_common            KS-108-03
_chemical_name_systematic
;
 ?
;
_space_group.centring_type       P
_space_group_IT_number           2
_space_group.IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.531(4)
_cell_angle_beta                 79.184(4)
_cell_angle_gamma                77.100(4)
_cell_formula_units_Z            1
_cell_length_a                   9.005(2)
_cell_length_b                   10.239(2)
_cell_length_c                   14.930(4)
_cell_measurement_reflns_used    8388
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.36
_cell_volume                     1317.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    DIRDIF-99
_diffrn_ambient_temperature      208(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0561
_diffrn_refln_scan_rate          20
_diffrn_refln_scan_width         0.3
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15518
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.16
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    0.840
_exptl_absorpt_correction_T_max  0.9236
_exptl_absorpt_correction_T_min  0.9236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 SQUEEZE (PLATON, A.Spek) was used to treat diffuse solvent/anion 
 contributions.  Total electron count found = 190/unit cell.  calculated for
 four BF4- and one CH3CN (the re'xtal solvent) = 188/unit cell.  The intensive
 properties (density, F(000), etc.) reflect these contributions.
;
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0675P)^2^+1.4600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                4837
_reflns_number_total             5948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja067208qsi20061008_025137.cif
_cod_data_source_block           jsm123
_cod_depositor_comments
;
The following automatic conversions were performed:

'_space_group.centring_type' value 'primitive' was replaced with the
value 'P' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
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_cod_database_code               4109116