An iron(II) complex tripodally chelated with 1,1,1-tris(pyridin-2-yl)ethane showing room-temperature spin-crossover behaviour
Ishida, Takayuki; Kanetomo, Takuya; Yamasaki, Masaru; Acta Crystallographica Section C 72 (2016) 797–801; doi:10.1107/S2053229616004174

data_2020614
_publ_section_title
;
 An iron(II) complex tripodally chelated with
 1,1,1-tris(pyridin-2-yl)ethane showing room-temperature spin-crossover
 behaviour
;
_journal_coeditor_code           YP3112
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              797
_journal_page_last               801
_journal_paper_doi               10.1107/S2053229616004174
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '(C24 H20 P) [Fe (N C S)3 (C17 H15 N3)]'
_chemical_formula_moiety         'C24 H20 P +, C20 H15 Fe N6 S3 -'
_chemical_formula_sum            'C44 H35 Fe N6 P S3'
_chemical_formula_weight         830.78
_chemical_name_systematic
'Tetraphenylphosphonium tris(thiocyanato-\k<i>N</i>)[1,1,1-tris(pyridin-2-yl)ethane-\k^3^<i>N</i>,<i>N</i>',<i>N</i>'']ferrate(II)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.067(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   8.9560(11)
_cell_length_b                   15.7745(16)
_cell_length_c                   28.455(3)
_cell_measurement_reflns_used    17570
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.29
_cell_volume                     4009.9(8)
_computing_cell_refinement
;
CrystalClear (Rigaku/MSC, 2006)
;
_computing_data_collection
;
CrystalClear (Rigaku/MSC, 2006)
;
_computing_data_reduction
;
CrystalClear (Rigaku/MSC, 2006)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2015)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2015) and
CRYSTALS (Carruthers <i>et al.</i>, 1999)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 14.629
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            64292
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         1.435
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1720.00
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.66
_refine_ls_extinction_coef       0.0027(6)
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     497
_refine_ls_number_reflns         9165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.08P)^2^+1.4P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                7802
_reflns_number_total             9165
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            yp3112sup1.cif
_cod_data_source_block           I100K
_cod_depositor_comments
'Adding full bibliography for 2020614--2020615.cif.'
_cod_database_code               2020614
_cod_database_fobs_code          2020614
_shelx_hkl_checksum              70687
_shelx_res_checksum              29833