#------------------------------------------------------------------------------
#$Date: 2019-11-23 00:16:37 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231637 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/61/4346166.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4346166
loop_
_publ_author_name
'Fujinami, Takeshi'
'Nishi, Koshiro'
'Hamada, Daisuke'
'Murakami, Keishiro'
'Matsumoto, Naohide'
'Iijima, Seiichiro'
'Kojima, Masaaki'
'Sunatsuki, Yukinari'
_publ_section_title
;
 Scan Rate Dependent Spin Crossover Iron(II) Complex with Two Different
 Relaxations and Thermal Hysteresis fac-[Fe(II)(HL(n-Pr))3]Cl·PF6
 (HL(n-Pr) = 2-Methylimidazol-4-yl-methylideneamino-n-propyl).
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7291
_journal_page_last               7300
_journal_paper_doi               10.1021/acs.inorgchem.5b00701
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C24 H39 Cl F6 Fe N9 P'
_chemical_formula_sum            'C24 H39 Cl F6 Fe N9 P'
_chemical_formula_weight         689.90
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                85.29(3)
_cell_angle_beta                 69.45(3)
_cell_angle_gamma                83.72(3)
_cell_formula_units_Z            2
_cell_length_a                   10.504(10)
_cell_length_b                   12.701(9)
_cell_length_c                   12.861(10)
_cell_measurement_reflns_used    10402
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      3.10
_cell_volume                     1595(2)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'CRYSTALS (Carruthers, et al., 1999)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.2353
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14949
_diffrn_reflns_theta_full        27.38
_diffrn_reflns_theta_max         27.38
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716.00
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.152
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.663
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     283
_refine_ls_number_reflns         1786
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0010Fo² + 1.0000σ(Fo²)]/(4Fo²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2062
_reflns_number_gt                1786
_reflns_number_total             7009
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic5b00701_si_001.cif
_cod_data_source_block           Fe(Pr)ClPF6-110K-slow
_cod_original_cell_volume        1595(3)
_cod_database_code               4346166
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,-Y,-Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe(1) Fe 0.3811(2) 0.23217(16) 0.25683(18) 0.0274(7) Uani 1.0 2 d .
Cl(1) Cl 0.1417(4) 0.3726(3) 0.8291(3) 0.0328(13) Uani 1.0 2 d .
P(1) P 0.2446(5) 0.7575(4) 0.4177(4) 0.0354(15) Uani 1.0 2 d .
F(1) F 0.1253(8) 0.7375(7) 0.5353(7) 0.050(4) Uani 1.0 2 d .
F(2) F 0.3633(8) 0.7788(8) 0.3020(7) 0.060(4) Uani 1.0 2 d .
F(3) F 0.3240(8) 0.8152(7) 0.4803(7) 0.048(3) Uani 1.0 2 d .
F(4) F 0.1622(8) 0.7002(7) 0.3567(7) 0.048(3) Uani 1.0 2 d .
F(5) F 0.1644(8) 0.8689(6) 0.4014(7) 0.045(3) Uani 1.0 2 d .
F(6) F 0.3228(8) 0.6452(6) 0.4373(8) 0.049(4) Uani 1.0 2 d .
N(1) N 0.1106(12) 0.4680(9) 0.1778(10) 0.031(4) Uiso 1.0 2 d .
N(2) N 0.2581(10) 0.3481(8) 0.2137(10) 0.022(4) Uani 1.0 2 d .
N(3) N 0.4444(10) 0.2150(8) 0.0926(9) 0.023(4) Uani 1.0 2 d .
N(4) N 0.2039(12) 0.2728(9) 0.5996(10) 0.035(4) Uiso 1.0 2 d .
N(5) N 0.2944(11) 0.2499(9) 0.4203(10) 0.034(4) Uani 1.0 2 d .
N(6) N 0.2345(11) 0.1321(9) 0.2890(10) 0.031(4) Uani 1.0 2 d .
N(7) N 0.6848(12) 0.4284(9) 0.2380(9) 0.033(4) Uiso 1.0 2 d .
N(8) N 0.5306(11) 0.3236(9) 0.2424(9) 0.024(4) Uani 1.0 2 d .
N(9) N 0.5123(12) 0.1196(9) 0.2924(10) 0.034(4) Uani 1.0 2 d .
C(1) C 0.0918(14) 0.4498(11) 0.3767(11) 0.033(4) Uiso 1.0 2 d .
C(2) C 0.1560(14) 0.4178(11) 0.2575(12) 0.027(4) Uiso 1.0 2 d .
C(3) C 0.1862(14) 0.4261(11) 0.0787(13) 0.038(4) Uiso 1.0 2 d .
C(4) C 0.2800(14) 0.3520(11) 0.1009(12) 0.027(4) Uiso 1.0 2 d .
C(5) C 0.3817(14) 0.2759(11) 0.0368(13) 0.027(4) Uiso 1.0 2 d .
C(6) C 0.5573(13) 0.1387(11) 0.0271(12) 0.032(4) Uiso 1.0 2 d .
C(7) C 0.6974(15) 0.1765(12) 0.0033(13) 0.039(5) Uiso 1.0 2 d .
C(8) C 0.7241(16) 0.2787(12) -0.0585(13) 0.049(5) Uiso 1.0 2 d .
C(9) C 0.3975(14) 0.3871(11) 0.4989(12) 0.037(5) Uiso 1.0 2 d .
C(10) C 0.3027(14) 0.3038(11) 0.5031(13) 0.030(4) Uiso 1.0 2 d .
C(11) C 0.1325(15) 0.1972(11) 0.5807(12) 0.032(4) Uiso 1.0 2 d .
C(12) C 0.1883(14) 0.1851(11) 0.4687(12) 0.023(4) Uiso 1.0 2 d .
C(13) C 0.1586(14) 0.1226(11) 0.3910(12) 0.029(4) Uiso 1.0 2 d .
C(14) C 0.1919(14) 0.0762(11) 0.2112(12) 0.031(4) Uiso 1.0 2 d .
C(15) C 0.0672(14) 0.1363(11) 0.1888(12) 0.035(4) Uiso 1.0 2 d .
C(16) C 0.0263(15) 0.0861(12) 0.1057(13) 0.051(5) Uiso 1.0 2 d .
C(17) C 0.4862(14) 0.5111(11) 0.1868(12) 0.038(5) Uiso 1.0 2 d .
C(18) C 0.5648(16) 0.4212(12) 0.2217(13) 0.032(4) Uiso 1.0 2 d .
C(19) C 0.7312(15) 0.3349(12) 0.2690(12) 0.037(4) Uiso 1.0 2 d .
C(20) C 0.6352(15) 0.2678(11) 0.2727(12) 0.026(4) Uiso 1.0 2 d .
C(21) C 0.6177(16) 0.1543(12) 0.3029(12) 0.034(4) Uiso 1.0 2 d .
C(22) C 0.4821(15) 0.0072(11) 0.3253(13) 0.040(5) Uiso 1.0 2 d .
C(23) C 0.6022(14) -0.0739(12) 0.3177(12) 0.041(5) Uiso 1.0 2 d .
C(24) C 0.7038(15) -0.0862(11) 0.1994(12) 0.046(5) Uiso 1.0 2 d .
H(1) H 0.0375 0.5220 0.1902 0.0368 Uiso 1.0 2 calc R
H(2) H 0.1880 0.3000 0.6701 0.0420 Uiso 1.0 2 calc R
H(3) H 0.7289 0.4916 0.2294 0.0397 Uiso 1.0 2 calc R
H(4) H 0.1400 0.5042 0.3882 0.0396 Uiso 1.0 2 calc R
H(5) H 0.0979 0.3900 0.4248 0.0396 Uiso 1.0 2 calc R
H(6) H -0.0012 0.4749 0.3923 0.0396 Uiso 1.0 2 calc R
H(7) H 0.1774 0.4440 0.0082 0.0459 Uiso 1.0 2 calc R
H(8) H 0.4031 0.2701 -0.0408 0.0326 Uiso 1.0 2 calc R
H(9) H 0.5505 0.0732 0.0692 0.0382 Uiso 1.0 2 calc R
H(10) H 0.5471 0.1287 -0.0419 0.0382 Uiso 1.0 2 calc R
H(11) H 0.7057 0.1850 0.0733 0.0470 Uiso 1.0 2 calc R
H(12) H 0.7653 0.1240 -0.0355 0.0471 Uiso 1.0 2 calc R
H(13) H 0.7640 0.2653 -0.1353 0.0583 Uiso 1.0 2 calc R
H(14) H 0.7844 0.3150 -0.0367 0.0583 Uiso 1.0 2 calc R
H(15) H 0.6402 0.3212 -0.0455 0.0583 Uiso 1.0 2 calc R
H(16) H 0.3578 0.4546 0.4833 0.0443 Uiso 1.0 2 calc R
H(17) H 0.4832 0.3724 0.4421 0.0443 Uiso 1.0 2 calc R
H(18) H 0.4103 0.3871 0.5684 0.0443 Uiso 1.0 2 calc R
H(19) H 0.0580 0.1633 0.6326 0.0385 Uiso 1.0 2 calc R
H(20) H 0.0887 0.0753 0.4155 0.0351 Uiso 1.0 2 calc R
H(21) H 0.2649 0.0715 0.1421 0.0373 Uiso 1.0 2 calc R
H(22) H 0.1710 0.0069 0.2417 0.0373 Uiso 1.0 2 calc R
H(23) H -0.0081 0.1346 0.2566 0.0417 Uiso 1.0 2 calc R
H(24) H 0.0854 0.2079 0.1661 0.0417 Uiso 1.0 2 calc R
H(25) H 0.0734 0.1177 0.0349 0.0609 Uiso 1.0 2 calc R
H(26) H -0.0692 0.0961 0.1200 0.0609 Uiso 1.0 2 calc R
H(27) H 0.0540 0.0124 0.1066 0.0609 Uiso 1.0 2 calc R
H(28) H 0.4227 0.5442 0.2504 0.0453 Uiso 1.0 2 calc R
H(29) H 0.4387 0.4874 0.1436 0.0452 Uiso 1.0 2 calc R
H(30) H 0.5478 0.5605 0.1434 0.0452 Uiso 1.0 2 calc R
H(31) H 0.8128 0.3157 0.2847 0.0442 Uiso 1.0 2 calc R
H(32) H 0.6831 0.1089 0.3245 0.0412 Uiso 1.0 2 calc R
H(33) H 0.4192 0.0057 0.3994 0.0482 Uiso 1.0 2 calc R
H(34) H 0.4404 -0.0147 0.2769 0.0483 Uiso 1.0 2 calc R
H(35) H 0.6486 -0.0508 0.3620 0.0498 Uiso 1.0 2 calc R
H(36) H 0.5702 -0.1412 0.3458 0.0498 Uiso 1.0 2 calc R
H(37) H 0.6791 -0.1403 0.1653 0.0554 Uiso 1.0 2 calc R
H(38) H 0.7940 -0.1035 0.1998 0.0554 Uiso 1.0 2 calc R
H(39) H 0.6999 -0.0206 0.1589 0.0554 Uiso 1.0 2 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
P P 0.1023 0.0942
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Fe Fe 0.3463 0.8444
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N(2) Fe(1) N(3) 79.9(5) yes
N(2) Fe(1) N(5) 95.3(5) yes
N(2) Fe(1) N(6) 89.5(5) yes
N(2) Fe(1) N(8) 96.0(5) yes
N(2) Fe(1) N(9) 176.8(4) yes
N(3) Fe(1) N(5) 172.9(5) yes
N(3) Fe(1) N(6) 93.2(5) yes
N(3) Fe(1) N(8) 92.5(5) yes
N(3) Fe(1) N(9) 97.8(5) yes
N(5) Fe(1) N(6) 81.5(5) yes
N(5) Fe(1) N(8) 93.2(5) yes
N(5) Fe(1) N(9) 87.2(5) yes
N(6) Fe(1) N(8) 172.7(6) yes
N(6) Fe(1) N(9) 93.0(5) yes
N(8) Fe(1) N(9) 81.8(5) yes
F(1) P(1) F(2) 179.2(7) yes
F(1) P(1) F(3) 89.4(5) yes
F(1) P(1) F(4) 89.6(5) yes
F(1) P(1) F(5) 89.3(5) yes
F(1) P(1) F(6) 89.3(5) yes
F(2) P(1) F(3) 89.8(5) yes
F(2) P(1) F(4) 91.1(6) yes
F(2) P(1) F(5) 90.4(5) yes
F(2) P(1) F(6) 91.0(5) yes
F(3) P(1) F(4) 178.9(5) yes
F(3) P(1) F(5) 89.8(5) yes
F(3) P(1) F(6) 89.9(6) yes
F(4) P(1) F(5) 89.7(6) yes
F(4) P(1) F(6) 90.6(5) yes
F(5) P(1) F(6) 178.5(5) yes
C(2) N(1) C(3) 108.2(12) yes
Fe(1) N(2) C(2) 141.3(11) yes
Fe(1) N(2) C(4) 111.9(8) yes
C(2) N(2) C(4) 106.5(12) yes
Fe(1) N(3) C(5) 117.1(9) yes
Fe(1) N(3) C(6) 126.7(10) yes
C(5) N(3) C(6) 116.2(12) yes
C(10) N(4) C(11) 110.9(13) yes
Fe(1) N(5) C(10) 141.8(10) yes
Fe(1) N(5) C(12) 112.0(10) yes
C(10) N(5) C(12) 106.3(11) yes
Fe(1) N(6) C(13) 115.0(12) yes
Fe(1) N(6) C(14) 129.9(8) yes
C(13) N(6) C(14) 114.8(12) yes
C(18) N(7) C(19) 110.4(13) yes
Fe(1) N(8) C(18) 143.2(11) yes
Fe(1) N(8) C(20) 111.9(9) yes
C(18) N(8) C(20) 104.7(13) yes
Fe(1) N(9) C(21) 115.0(10) yes
Fe(1) N(9) C(22) 124.0(10) yes
C(21) N(9) C(22) 120.1(13) yes
N(1) C(2) N(2) 110.6(13) yes
N(1) C(2) C(1) 119.9(12) yes
N(2) C(2) C(1) 129.4(15) yes
N(1) C(3) C(4) 105.6(14) yes
N(2) C(4) C(3) 109.0(12) yes
N(2) C(4) C(5) 116.3(13) yes
C(3) C(4) C(5) 134.5(16) yes
N(3) C(5) C(4) 114.7(14) yes
N(3) C(6) C(7) 112.6(12) yes
C(6) C(7) C(8) 116.6(14) yes
N(4) C(10) N(5) 107.9(13) yes
N(4) C(10) C(9) 122.6(14) yes
N(5) C(10) C(9) 129.5(12) yes
N(4) C(11) C(12) 104.1(12) yes
N(5) C(12) C(11) 110.8(14) yes
N(5) C(12) C(13) 114.9(12) yes
C(11) C(12) C(13) 134.3(13) yes
N(6) C(13) C(12) 116.6(13) yes
N(6) C(14) C(15) 111.9(11) yes
C(14) C(15) C(16) 113.5(12) yes
N(7) C(18) N(8) 110.1(14) yes
N(7) C(18) C(17) 124.2(14) yes
N(8) C(18) C(17) 125.7(16) yes
N(7) C(19) C(20) 104.7(15) yes
N(8) C(20) C(19) 110.1(12) yes
N(8) C(20) C(21) 114.9(14) yes
C(19) C(20) C(21) 135.0(15) yes
N(9) C(21) C(20) 115.9(14) yes
N(9) C(22) C(23) 117.3(12) yes
C(22) C(23) C(24) 113.7(13) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Fe(1) N(2) 2.024(11) yes
Fe(1) N(3) 2.002(12) yes
Fe(1) N(5) 1.997(12) yes
Fe(1) N(6) 2.013(12) yes
Fe(1) N(8) 2.002(12) yes
Fe(1) N(9) 2.014(12) yes
P(1) F(1) 1.612(9) yes
P(1) F(2) 1.596(9) yes
P(1) F(3) 1.607(12) yes
P(1) F(4) 1.614(12) yes
P(1) F(5) 1.603(9) yes
P(1) F(6) 1.614(9) yes
N(1) C(2) 1.36(2) yes
N(1) C(3) 1.359(18) yes
N(2) C(2) 1.304(16) yes
N(2) C(4) 1.38(2) yes
N(3) C(5) 1.29(2) yes
N(3) C(6) 1.496(15) yes
N(4) C(10) 1.370(17) yes
N(4) C(11) 1.37(2) yes
N(5) C(10) 1.35(3) yes
N(5) C(12) 1.392(18) yes
N(6) C(13) 1.278(17) yes
N(6) C(14) 1.48(3) yes
N(7) C(18) 1.36(3) yes
N(7) C(19) 1.318(19) yes
N(8) C(18) 1.309(19) yes
N(8) C(20) 1.40(2) yes
N(9) C(21) 1.29(3) yes
N(9) C(22) 1.492(18) yes
C(1) C(2) 1.513(19) yes
C(3) C(4) 1.38(2) yes
C(4) C(5) 1.429(18) yes
C(6) C(7) 1.52(2) yes
C(7) C(8) 1.47(2) yes
C(9) C(10) 1.52(3) yes
C(11) C(12) 1.37(2) yes
C(12) C(13) 1.46(3) yes
C(14) C(15) 1.55(2) yes
C(15) C(16) 1.49(3) yes
C(17) C(18) 1.47(2) yes
C(19) C(20) 1.38(3) yes
C(20) C(21) 1.48(2) yes
C(22) C(23) 1.52(2) yes
C(23) C(24) 1.530(18) yes
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N(1) H(1) Cl(1) 2_566 3.201(13) 0.950 2.288 161.0 no
N(4) H(2) Cl(1) . 3.146(16) 0.950 2.198 175.7 no
N(7) H(3) Cl(1) 2_666 3.168(14) 0.950 2.234 167.4 no
