#------------------------------------------------------------------------------
#$Date: 2017-02-19 21:44:26 +0200 (Sun, 19 Feb 2017) $
#$Revision: 192308 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/01/39/2013971.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2013971
loop_
_publ_author_name
'Wang, Shi'
'Li, Yi-Zhi'
'Zuo, Jing-Lin'
'Li, Cheng-Hui'
'You, Xiao-Zeng'
_publ_section_title
;Tris{bis[hydrotris(1-pyrazolyl)borato-κ³N²,N^2'^,N^2''^]iron(III)}
 hexaisothiocyanatoiron(III)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m258
_journal_page_last               m260
_journal_paper_doi               10.1107/S0108270104008741
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Fe (C9 H10 B N6)2]3 [Fe (N C S)6]'
_chemical_formula_moiety         '3(C18 H20 B2 Fe N12), C6 Fe N6 S6'
_chemical_formula_sum            'C60 H60 B6 Fe4 N42 S6'
_chemical_formula_weight         1850.12
_chemical_name_systematic
;
Tris{bis[hydrotris(1-pyrazolyl)borato-κ²N,N']iron(III)}
hexaisothiocyanatoiron(III)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   22.676(2)
_cell_length_b                   22.676(2)
_cell_length_c                   13.5195(18)
_cell_measurement_reflns_used    531
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.01
_cell_measurement_theta_min      2.06
_cell_volume                     6020.4(11)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  'SHELXTL and PLATON (Spek 2003)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11418
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.379
_refine_ls_extinction_coef       0.00035(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0526P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                1915
_reflns_number_total             2638
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fg1750.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking atoms 'Cg1' and 'Cg2' as dummy atoms.

 Antanas Vaitkus,
 2017-02-19

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6020.3(12)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2013971
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Fe1 0.3333 0.1667 0.1667 0.03438(18) Uani d S 1 . . Fe
N1 0.30355(11) 0.06967(10) 0.17187(17) 0.0401(5) Uani d . 1 . . N
N2 0.24385(12) 0.02658(11) 0.21572(18) 0.0456(6) Uani d . 1 . . N
N3 0.24097(11) 0.14203(11) 0.12715(16) 0.0385(5) Uani d . 1 . . N
N4 0.18712(11) 0.09164(11) 0.17580(17) 0.0417(5) Uani d . 1 . . N
N5 0.30681(12) 0.16151(11) 0.30428(16) 0.0401(5) Uani d . 1 . . N
N6 0.24618(11) 0.10961(11) 0.33499(17) 0.0415(5) Uani d . 1 . . N
C1 0.33152(16) 0.03381(15) 0.1414(2) 0.0490(7) Uani d . 1 . . C
H1 0.3728 0.0514 0.1081 0.059 Uiso calc R 1 . . H
C2 0.28999(15) -0.03374(15) 0.1665(3) 0.0568(8) Uani d . 1 . . C
H2 0.2975 -0.0698 0.1539 0.068 Uiso calc R 1 . . H
C3 0.23555(15) -0.03615(14) 0.2136(3) 0.0538(8) Uani d . 1 . . C
H3 0.1987 -0.0750 0.2400 0.065 Uiso calc R 1 . . H
C4 0.21606(16) 0.16781(15) 0.0611(2) 0.0485(7) Uani d . 1 . . C
H4 0.2422 0.2034 0.0179 0.058 Uiso calc R 1 . . H
C5 0.14615(16) 0.13392(18) 0.0665(3) 0.0588(8) Uani d . 1 . . C
H5 0.1163 0.1412 0.0283 0.071 Uiso calc R 1 . . H
C6 0.12995(15) 0.08688(17) 0.1409(2) 0.0516(8) Uani d . 1 . . C
H6 0.0862 0.0567 0.1631 0.062 Uiso calc R 1 . . H
C7 0.33558(16) 0.20125(16) 0.3823(2) 0.0476(7) Uani d . 1 . . C
H7 0.3780 0.2407 0.3824 0.057 Uiso calc R 1 . . H
C8 0.29368(18) 0.17556(18) 0.4624(2) 0.0582(8) Uani d . 1 . . C
H8 0.3017 0.1938 0.5258 0.070 Uiso calc R 1 . . H
C9 0.23720(18) 0.11723(17) 0.4303(2) 0.0535(8) Uani d . 1 . . C
H9 0.1995 0.0883 0.4683 0.064 Uiso calc R 1 . . H
B1 0.20031(17) 0.05481(17) 0.2592(3) 0.0488(8) Uani d . 1 . . B
H11 0.1581 0.0191 0.2890 0.059 Uiso calc R 1 . . H
Fe2 0.0000 0.0000 0.5000 0.0367(2) Uani d S 1 . . Fe
S1 0.15096(4) 0.20524(4) 0.32058(6) 0.0528(2) Uani d . 1 . . S
N7 0.06325(12) 0.08236(12) 0.41285(19) 0.0458(6) Uani d . 1 . . N
C10 0.09926(14) 0.13332(14) 0.37313(18) 0.0375(6) Uani d . 1 . . C
Cg1 0.10449 0.14031 0.36885 0.01 Uiso dum . . . . .
Cg2 0.18405 0.12446 0.11429 0.01 Uiso dum . . . . .
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 Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables 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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N5 Fe1 N5 13 . 180.0
N5 Fe1 N3 13 13 89.39(10)
N5 Fe1 N3 . 13 90.61(10)
N5 Fe1 N1 13 . 91.41(9)
N5 Fe1 N1 . . 88.59(9)
N3 Fe1 N1 13 . 91.71(9)
N5 Fe1 N3 13 . 90.61(10)
N5 Fe1 N3 . . 89.39(10)
N3 Fe1 N3 13 . 180.0
N1 Fe1 N3 . . 88.30(9)
N5 Fe1 N1 13 13 88.59(9)
N5 Fe1 N1 . 13 91.41(9)
N3 Fe1 N1 13 13 88.30(9)
N1 Fe1 N1 . 13 180.0
N3 Fe1 N1 . 13 91.70(9)
C1 N1 N2 . . 107.9(2)
C1 N1 Fe1 . . 132.78(19)
N2 N1 Fe1 . . 119.25(16)
C3 N2 N1 . . 108.5(2)
C3 N2 B1 . . 132.2(2)
N1 N2 B1 . . 119.2(2)
C4 N3 N4 . . 107.1(2)
C4 N3 Fe1 . . 133.2(2)
N4 N3 Fe1 . . 119.61(17)
C6 N4 N3 . . 109.1(2)
C6 N4 B1 . . 132.0(3)
N3 N4 B1 . . 118.8(2)
C7 N5 N6 . . 106.7(2)
C7 N5 Fe1 . . 133.5(2)
N6 N5 Fe1 . . 119.75(18)
C9 N6 N5 . . 109.8(2)
C9 N6 B1 . . 131.5(3)
N5 N6 B1 . . 118.6(2)
N1 C1 C2 . . 109.6(3)
N1 C1 H1 . . 125.2
C2 C1 H1 . . 125.2
C3 C2 C1 . . 105.1(3)
C3 C2 H2 . . 127.5
C1 C2 H2 . . 127.5
N2 C3 C2 . . 108.9(3)
N2 C3 H3 . . 125.6
C2 C3 H3 . . 125.6
N3 C4 C5 . . 110.0(3)
N3 C4 H4 . . 125.0
C5 C4 H4 . . 125.0
C4 C5 C6 . . 105.0(3)
C4 C5 H5 . . 127.5
C6 C5 H5 . . 127.5
N4 C6 C5 . . 108.9(3)
N4 C6 H6 . . 125.5
C5 C6 H6 . . 125.5
N5 C7 C8 . . 109.9(3)
N5 C7 H7 . . 125.1
C8 C7 H7 . . 125.1
C7 C8 C9 . . 106.0(3)
C7 C8 H8 . . 127.0
C9 C8 H8 . . 127.0
N6 C9 C8 . . 107.6(3)
N6 C9 H9 . . 126.2
C8 C9 H9 . . 126.2
N4 B1 N2 . . 106.8(2)
N4 B1 N6 . . 106.8(2)
N2 B1 N6 . . 105.9(2)
N4 B1 H11 . . 112.3
N2 B1 H11 . . 112.3
N6 B1 H11 . . 112.3
N7 Fe2 N7 3 11_556 89.39(10)
N7 Fe2 N7 3 2 90.61(10)
N7 Fe2 N7 11_556 2 180.0
N7 Fe2 N7 3 10_556 89.39(10)
N7 Fe2 N7 11_556 10_556 90.61(10)
N7 Fe2 N7 2 10_556 89.39(10)
N7 Fe2 N7 3 . 90.61(10)
N7 Fe2 N7 11_556 . 89.39(10)
N7 Fe2 N7 2 . 90.61(10)
N7 Fe2 N7 10_556 . 180.0
N7 Fe2 N7 3 12_556 180.0
N7 Fe2 N7 11_556 12_556 90.61(10)
N7 Fe2 N7 2 12_556 89.39(10)
N7 Fe2 N7 10_556 12_556 90.61(10)
N7 Fe2 N7 . 12_556 89.39(10)
C10 N7 Fe2 . . 172.1(2)
N7 C10 S1 . . 178.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N5 13 1.941(2) ?
Fe1 N5 . 1.941(2) ?
Fe1 N3 13 1.953(2) ?
Fe1 N1 . 1.953(2) ?
Fe1 N3 . 1.953(2) ?
Fe1 N1 13 1.953(2) ?
N1 C1 . 1.322(4) ?
N1 N2 . 1.348(3) ?
N2 C3 . 1.339(4) ?
N2 B1 . 1.537(4) ?
N3 C4 . 1.337(4) ?
N3 N4 . 1.354(3) ?
N4 C6 . 1.333(3) ?
N4 B1 . 1.520(4) ?
N5 C7 . 1.328(4) ?
N5 N6 . 1.353(3) ?
N6 C9 . 1.329(4) ?
N6 B1 . 1.543(4) ?
C1 C2 . 1.380(4) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.366(4) ?
C2 H2 . 0.9300 ?
C3 H3 . 0.9300 ?
C4 C5 . 1.375(4) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.375(5) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 C8 . 1.364(4) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.373(5) ?
C8 H8 . 0.9300 ?
C9 H9 . 0.9300 ?
B1 H11 . 0.9800 ?
Fe2 N7 3 2.063(2) ?
Fe2 N7 11_556 2.063(2) ?
Fe2 N7 2 2.063(2) ?
Fe2 N7 10_556 2.063(2) ?
Fe2 N7 . 2.063(2) ?
Fe2 N7 12_556 2.063(2) ?
S1 C10 . 1.621(3) ?
N7 C10 . 1.161(4) ?
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_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C9 H9 Cg1 11_556 0.93 2.54 3.399 153 y
C5 H5 Cg2 12 0.93 2.75 3.654 164 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion
N5 Fe1 N1 C1 13 46.2(3)
N5 Fe1 N1 C1 . -133.8(3)
N3 Fe1 N1 C1 13 -43.2(3)
N3 Fe1 N1 C1 . 136.8(3)
N5 Fe1 N1 N2 13 -135.5(2)
N5 Fe1 N1 N2 . 44.5(2)
N3 Fe1 N1 N2 13 135.1(2)
N3 Fe1 N1 N2 . -44.9(2)
C1 N1 N2 C3 . 1.0(3)
Fe1 N1 N2 C3 . -177.7(2)
C1 N1 N2 B1 . 179.5(3)
Fe1 N1 N2 B1 . 0.8(3)
N5 Fe1 N3 C4 13 -48.0(3)
N5 Fe1 N3 C4 . 132.0(3)
N1 Fe1 N3 C4 . -139.4(3)
N1 Fe1 N3 C4 13 40.6(3)
N5 Fe1 N3 N4 13 136.69(19)
N5 Fe1 N3 N4 . -43.31(19)
N1 Fe1 N3 N4 . 45.30(19)
N1 Fe1 N3 N4 13 -134.70(19)
C4 N3 N4 C6 . -0.6(3)
Fe1 N3 N4 C6 . 175.87(17)
C4 N3 N4 B1 . -177.3(2)
Fe1 N3 N4 B1 . -0.9(3)
N3 Fe1 N5 C7 13 45.1(3)
N1 Fe1 N5 C7 . 136.8(3)
N3 Fe1 N5 C7 . -134.9(3)
N1 Fe1 N5 C7 13 -43.2(3)
N3 Fe1 N5 N6 13 -137.26(19)
N1 Fe1 N5 N6 . -45.57(19)
N3 Fe1 N5 N6 . 42.74(19)
N1 Fe1 N5 N6 13 134.43(19)
C7 N5 N6 C9 . 0.5(3)
Fe1 N5 N6 C9 . -177.73(19)
C7 N5 N6 B1 . 179.5(2)
Fe1 N5 N6 B1 . 1.3(3)
N2 N1 C1 C2 . -0.7(3)
Fe1 N1 C1 C2 . 177.8(2)
N1 C1 C2 C3 . 0.1(4)
N1 N2 C3 C2 . -1.0(4)
B1 N2 C3 C2 . -179.2(3)
C1 C2 C3 N2 . 0.6(4)
N4 N3 C4 C5 . -0.4(3)
Fe1 N3 C4 C5 . -176.1(2)
N3 C4 C5 C6 . 1.1(3)
N3 N4 C6 C5 . 1.3(3)
B1 N4 C6 C5 . 177.5(3)
C4 C5 C6 N4 . -1.4(3)
N6 N5 C7 C8 . -0.5(3)
Fe1 N5 C7 C8 . 177.3(2)
N5 C7 C8 C9 . 0.4(4)
N5 N6 C9 C8 . -0.2(3)
B1 N6 C9 C8 . -179.1(3)
C7 C8 C9 N6 . -0.1(4)
C6 N4 B1 N2 . 128.1(3)
N3 N4 B1 N2 . -56.0(3)
C6 N4 B1 N6 . -118.9(3)
N3 N4 B1 N6 . 57.0(3)
C3 N2 B1 N4 . -125.6(3)
N1 N2 B1 N4 . 56.3(3)
C3 N2 B1 N6 . 120.8(3)
N1 N2 B1 N6 . -57.2(3)
C9 N6 B1 N4 . 121.2(3)
N5 N6 B1 N4 . -57.5(3)
C9 N6 B1 N2 . -125.2(3)
N5 N6 B1 N2 . 56.0(3)
