Room-Temperature Spin Crossover Observed for [(TPyA)FeII(DBQ2-)FeII(TPyA)]2+ [TPyA = Tris(2-pyridylmethyl)amine; DBQ2-= 2,5-Di-tert-butyl-3,6-dihydroxy-1,4-benzoquinonate]
Kil Sik Min; Antonio DiPasquale; Arnold L. Rheingold; Joel S. Miller; Inorganic Chemistry 46 (2007) 1048–1050; doi:10.1021/ic062400e

data_4307881
_publ_section_title
;
Room-Temperature Spin Crossover Observed for
[(TPyA)FeII(DBQ2-)FeII(TPyA)]2+ [TPyA = Tris(2-pyridylmethyl)amine; DBQ2-=
2,5-Di-tert-butyl-3,6-dihydroxy-1,4-benzoquinonate]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1048
_journal_page_last               1050
_journal_paper_doi               10.1021/ic062400e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C50 H54 B2 F8 Fe2 N8 O4'
_chemical_formula_weight         1116.33
_chemical_name_common            KS-129-03
_chemical_name_systematic
;
 ?
;
_space_group.centring_type       P
_space_group_IT_number           14
_space_group.IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.824(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3981(16)
_cell_length_b                   18.5528(19)
_cell_length_c                   19.548(2)
_cell_measurement_reflns_used    6942
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.90
_cell_measurement_theta_min      2.60
_cell_volume                     5316.4(9)
_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    SHELXS-97
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_refln_scan_rate          20
_diffrn_refln_scan_width         0.5
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52789
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.8853
_exptl_absorpt_correction_T_min  0.8348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
; 
 SQUEEZE (PLATON, A.Spek) was used to treat disordered
 anion contributions.  Total electron count found = 303/unit cell.
 Calculated for 8 BF4- (the anion) = 336/unit cell.  The 
 intensive properties (density, F(000), etc.)
 reflect these contributions.
;
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1134P)^2^+1.0834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1883
_reflns_number_gt                7068
_reflns_number_total             9383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062400esi20061215_085058.cif
_cod_data_source_block           jsm135
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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 
;
_cod_database_code               4307881