Bulk spin-crossover in the complex [FeL(NCS)2] of a tris(pyridyl)ethane-derived N4-ligand-a temperature-dependent crystallographic study.
Wiedemann, Dennis; Grohmann, Andreas; Dalton transactions (Cambridge, England : 2003) 43 (2014) 2406–2417; doi:10.1039/c3dt53070a

data_7028752
_publ_section_title
;
 Bulk spin-crossover in the complex [FeL(NCS)2] of a
 tris(pyridyl)ethane-derived N4-ligand-a temperature-dependent
 crystallographic study.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2406
_journal_page_last               2417
_journal_paper_doi               10.1039/c3dt53070a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_iupac          '[Fe (C20 H22 N4) Cl2](P F6)'
_chemical_formula_moiety         'C20 H22 Cl2 Fe N4 1+, F6 P 1-'
_chemical_formula_sum            'C20 H22 Cl2 F6 Fe N4 P'
_chemical_formula_weight         590.14
_chemical_name_systematic
;dichlorido(1-{6-[1,1-di(pyridin-2-yl)ethyl]pyridin-2-yl}-
        N,N-dimethylmethanamine)iron(III) hexafluorophosphate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-09-13T18:33:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                92.040(5)
_cell_angle_beta                 106.526(5)
_cell_angle_gamma                93.255(5)
_cell_formula_units_Z            2
_cell_length_a                   8.9533(5)
_cell_length_b                   10.8208(7)
_cell_length_c                   12.7219(7)
_cell_measurement_reflns_used    3783
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      32.3926
_cell_measurement_theta_min      3.3389
_cell_volume                     1177.98(12)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_detector_type            'Agilent Sapphire 3'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.039
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9564
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         3.35
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.78828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             598
_exptl_crystal_recrystallization_method
'precipitation (vapour diffusion): acetonitrile, diethyl ether, r. t., 2 d'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+0.4573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.095
_reflns_number_gt                4042
_reflns_number_total             4620
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3dt53070a.txt
_cod_data_source_block           compound3
_cod_database_code               7028752
_restr_special_details
;
 Additionally, equal-1,2- and equal-1,3-distance restraints (generated using
 SHELXL-97 SAME intructions with standard weights) have been applied to the
 whole hexafluorophosphate moiety in both orientations of disorder.
;