#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:03:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179877 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/73/7017325.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_7017325
loop_
_publ_author_name
'Fujinami, Takeshi'
'Nishi, Koshiro'
'Matsumoto, Naohide'
'Iijima, Seiichiro'
'Halcrow, Malcolm A.'
'Sunatsuki, Yukinari'
'Kojima, Masaaki'
_publ_section_title
;
 1D and 2D assembly structures by imidazolechloride hydrogen bonds of
 iron(ii) complexes [Fe(II)(HL(n-Pr))(3)]Cl·Y (HL(n-Pr) =
 2-methylimidazol-4-yl-methylideneamino-n-propyl; Y = AsF(6), BF(4)) and
 their spin states.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12301
_journal_page_last               12309
_journal_paper_doi               10.1039/c1dt11063b
_journal_volume                  40
_journal_year                    2011
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C24 H39 B Cl F4 Fe N9'
_chemical_formula_sum            'C24 H39 B Cl F4 Fe N9'
_chemical_formula_weight         631.74
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      161
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            6
_cell_length_a                   10.699(4)
_cell_length_b                   10.699(4)
_cell_length_c                   47.49(2)
_cell_measurement_reflns_used    10414
_cell_measurement_temperature    296
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.07
_cell_volume                     4708(3)
_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    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 1.064
_diffrn_measured_fraction_theta_max 1.064
_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  0.0219
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            14211
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.619
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1980.00
_exptl_crystal_size_max          0.688
_exptl_crystal_size_mid          0.449
_exptl_crystal_size_min          0.394
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.482
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1052 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1910
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0018Fo² + 1.0700σ(Fo²)]/(4Fo²)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                1910
_reflns_number_total             2251
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c1dt11063b.txt
_cod_data_source_block           Fe(HL2Me(Pr))3ClBF4
_cod_original_cell_volume        4707(3)
_cod_original_sg_symbol_H-M      'R 3 c:H'
_cod_database_code               7017325
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -Y,+X-Y,+Z
3 -X+Y,-X,+Z
4 -X+Y,+Y,1/2+Z
5 +X,+X-Y,1/2+Z
6 -Y,-X,1/2+Z
7 2/3+X,1/3+Y,1/3+Z
8 2/3-Y,1/3+X-Y,1/3+Z
9 2/3-X+Y,1/3-X,1/3+Z
10 2/3-X+Y,1/3+Y,5/6+Z
11 2/3+X,1/3+X-Y,5/6+Z
12 2/3-Y,1/3-X,5/6+Z
13 1/3+X,2/3+Y,2/3+Z
14 1/3-Y,2/3+X-Y,2/3+Z
15 1/3-X+Y,2/3-X,2/3+Z
16 1/3-X+Y,2/3+Y,1/6+Z
17 1/3+X,2/3+X-Y,1/6+Z
18 1/3-Y,2/3-X,1/6+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
Fe1 Fe 0.6667 0.3333 0.39981(11) 0.04681(13) Uani 1.0 6 d .
Cl1 Cl 0.3333 0.6667 0.47847(11) 0.0626(3) Uani 1.0 6 d .
F1 F 0.3333 0.6667 0.3389(3) 0.262(8) Uani 0.6000 6 d .
F2 F 0.3333 0.6667 0.3900(7) 0.287(18) Uani 0.4000 6 d .
F3 F 0.437(7) 0.753(7) 0.3361(12) 0.102(14) Uiso 0.0500 18 d .
F4 F 0.420(4) 0.653(3) 0.3465(7) 0.090(7) Uiso 0.1000 18 d .
F5 F 0.441(3) 0.637(3) 0.3678(8) 0.055(6) Uiso 0.1000 18 d .
F6 F 0.4605(17) 0.6698(18) 0.3593(5) 0.078(4) Uiso 0.2000 18 d .
F7 F 0.426(3) 0.652(4) 0.3839(7) 0.058(7) Uiso 0.1000 18 d .
F8 F 0.454(3) 0.686(3) 0.3840(5) 0.078(6) Uiso 0.2000 18 d .
F9 F 0.349(6) 0.820(6) 0.3786(11) 0.055(12) Uiso 0.0500 18 d .
F10 F 0.2140(18) 0.5345(15) 0.3732(5) 0.056(4) Uiso 0.2000 18 d .
N1 N 0.2702(3) 0.1946(3) 0.35110(12) 0.0684(7) Uani 1.0 18 d .
N2 N 0.4684(3) 0.2655(3) 0.37591(11) 0.0510(6) Uani 1.0 18 d .
N3 N 0.5601(3) 0.4355(3) 0.42337(12) 0.0567(7) Uani 1.0 18 d .
C1 C 0.4247(4) 0.0931(4) 0.33636(12) 0.0851(11) Uani 1.0 18 d .
C2 C 0.3901(3) 0.1834(3) 0.35443(12) 0.0568(7) Uani 1.0 18 d .
C3 C 0.2712(3) 0.2867(4) 0.37109(12) 0.0710(9) Uani 1.0 18 d .
C4 C 0.3939(3) 0.3302(3) 0.38629(12) 0.0571(7) Uani 1.0 18 d .
C5 C 0.4473(3) 0.4189(3) 0.41092(12) 0.0599(8) Uani 1.0 18 d .
C6 C 0.6037(5) 0.5185(5) 0.44959(13) 0.0823(11) Uani 1.0 18 d .
C7 C 0.7343(5) 0.6622(5) 0.44709(13) 0.0960(13) Uani 1.0 18 d .
C8 C 0.7188(7) 0.7586(5) 0.42828(15) 0.136(2) Uani 1.0 18 d .
B1 B 0.3333 0.6667 0.3652(2) 0.0736(16) Uani 1.0 6 d .
H1 H 0.1988 0.1469 0.3370 0.0810 Uiso 1.0 18 calc R
H2 H 0.1999 0.3132 0.3744 0.0901 Uiso 1.0 18 calc R
H3 H 0.3979 0.4652 0.4181 0.0754 Uiso 1.0 18 calc R
H4 H 0.5266 0.5315 0.4558 0.1029 Uiso 1.0 18 calc R
H5 H 0.6211 0.4636 0.4631 0.1031 Uiso 1.0 18 calc R
H6 H 0.7593 0.7035 0.4654 0.1197 Uiso 1.0 18 calc R
H7 H 0.8103 0.6502 0.4398 0.1194 Uiso 1.0 18 calc R
H8 H 0.4825 0.1470 0.3208 0.1061 Uiso 1.0 18 calc R
H9 H 0.3367 0.0146 0.3297 0.1059 Uiso 1.0 18 calc R
H10 H 0.4751 0.0573 0.3471 0.1059 Uiso 1.0 18 calc R
H11 H 0.7442 0.7492 0.4096 0.1562 Uiso 1.0 18 calc R
H12 H 0.7791 0.8549 0.4346 0.1560 Uiso 1.0 18 calc R
H13 H 0.6209 0.7359 0.4288 0.1563 Uiso 1.0 18 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)
;
B B 0.0013 0.0007
;
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Fe1 N2 95.5(2) yes . 2_655
N2 Fe1 N2 95.5(2) yes . 3_665
N2 Fe1 N3 76.98(16) yes . .
N2 Fe1 N3 91.11(13) yes . 2_655
N2 Fe1 N3 170.45(10) yes . 3_665
N2 Fe1 N2 95.5(2) yes 2_655 3_665
N2 Fe1 N3 170.45(10) yes 2_655 .
N2 Fe1 N3 76.98(16) yes 2_655 2_655
N2 Fe1 N3 91.11(13) yes 2_655 3_665
N2 Fe1 N3 91.12(13) yes 3_665 .
N2 Fe1 N3 170.45(10) yes 3_665 2_655
N2 Fe1 N3 76.98(16) yes 3_665 3_665
N3 Fe1 N3 97.1(2) yes . 2_655
N3 Fe1 N3 97.1(2) yes . 3_665
N3 Fe1 N3 97.1(2) yes 2_655 3_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Fe1 N2 2.185(5) yes .
Fe1 N2 2.185(5) yes 2_655
Fe1 N2 2.185(5) yes 3_665
Fe1 N3 2.234(5) yes .
Fe1 N3 2.234(5) yes 2_655
Fe1 N3 2.234(5) yes 3_665
F1 F3 1.04(5) yes .
F1 F3 1.04(5) yes 2_665
F1 F3 1.04(5) yes 3_565
F1 F4 1.08(4) yes .
F1 F4 1.08(4) yes 2_665
F1 F4 1.08(4) yes 3_565
F1 F6 1.66(3) yes .
F1 F6 1.66(3) yes 2_665
F1 F6 1.66(3) yes 3_565
F1 B1 1.249(18) yes .
F2 F5 1.70(4) yes .
F2 F5 1.70(4) yes 2_665
F2 F5 1.70(4) yes 3_565
F2 F7 1.12(4) yes .
F2 F7 1.12(4) yes 2_665
F2 F7 1.12(4) yes 3_565
F2 F8 1.23(3) yes .
F2 F8 1.23(3) yes 2_665
F2 F8 1.23(3) yes 3_565
F2 F9 1.66(7) yes .
F2 F9 1.66(7) yes 2_665
F2 F9 1.66(7) yes 3_565
F2 F10 1.57(3) yes .
F2 F10 1.57(3) yes 2_665
F2 F10 1.57(3) yes 3_565
F2 B1 1.18(4) yes .
F3 F3 1.79(9) yes 2_665
F3 F3 1.79(9) yes 3_565
F3 F4 1.11(8) yes .
F3 F4 1.16(8) yes 2_665
F3 F6 1.51(7) yes .
F3 F6 1.78(8) yes 2_665
F3 B1 1.72(6) yes .
F4 F4 1.75(6) yes 2_665
F4 F4 1.75(6) yes 3_565
F4 F5 1.07(5) yes .
F4 F6 0.71(4) yes .
F4 F7 1.78(5) yes .
F4 F9 1.62(7) yes 3_565
F4 F10 1.34(4) yes 2_665
F4 B1 1.35(4) yes .
F5 F6 0.51(4) yes .
F5 F7 0.81(5) yes .
F5 F8 0.90(4) yes .
F5 F9 0.59(7) yes 3_565
F5 F10 0.47(4) yes 2_665
F5 B1 1.34(4) yes .
F6 F7 1.21(4) yes .
F6 F8 1.19(4) yes .
F6 F9 0.96(6) yes 3_565
F6 F10 0.67(3) yes 2_665
F6 B1 1.37(2) yes .
F7 F8 0.34(3) yes .
F7 F8 1.79(4) yes 3_565
F7 F9 0.55(7) yes 3_565
F7 F10 0.63(4) yes 2_665
F7 B1 1.40(4) yes .
F8 F9 0.56(6) yes 3_565
F8 F10 0.54(4) yes 2_665
F8 B1 1.49(3) yes .
F9 F10 0.43(5) yes 3_565
F9 B1 1.69(6) yes .
F10 B1 1.403(14) yes .
N1 C2 1.356(5) yes .
N1 C3 1.365(7) yes .
N2 C2 1.334(7) yes .
N2 C4 1.382(6) yes .
N3 C5 1.274(6) yes .
N3 C6 1.463(8) yes .
C1 C2 1.471(7) yes .
C3 C4 1.360(6) yes .
C4 C5 1.433(7) yes .
C6 C7 1.477(5) yes .
C7 C8 1.435(9) 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
N2 H1 Cl1 10_444 3.187(5) 0.950 2.254 166.8 no
N2 H1 Cl1 11_454 3.187(5) 0.950 2.255 166.8 no
N2 H1 Cl1 12_554 3.187(5) 0.950 2.254 166.8 no
