#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:56:25 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239910 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/05/4350504.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_4350504
loop_
_publ_author_name
'Senda, Shunsuke'
'Ohki, Yasuhiro'
'Hirayama, Tomoko'
'Toda, Daisuke'
'Chen, Jing-Lin'
'Matsumoto, Tsuyoshi'
'Kawaguchi, Hiroyuki'
'Tatsumi, Kazuyuki'
_publ_section_title
;
 Mono{hydrotris(mercaptoimidazolyl)borato} complexes of manganese(II),
 iron(II), cobalt(II), and nickel(II) halides.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9914
_journal_page_last               9925
_journal_paper_doi               10.1021/ic0610132
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C30 H22 B Cl6 I Mn N6 S3'
_chemical_formula_weight         968.09
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      148
_symmetry_space_group_name_H-M   'R -3 :H'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.052(2)
_cell_length_b                   15.052(2)
_cell_length_c                   30.392(4)
_cell_measurement_reflns_used    5101
_cell_measurement_temperature    173.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5963.2(14)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 28.57
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.9977
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            16242
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    1.700
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.13
_refine_diff_density_min         -0.92
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1611
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.0003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00203|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0739
_reflns_number_gt                1611
_reflns_number_total             3047
_reflns_threshold_expression     F²>3.0σ(F²)
_cod_data_source_file            ic0610132si20060906_094900.cif
_cod_data_source_block           PhMnI
_cod_original_cell_volume        5962(1)
_cod_original_sg_symbol_H-M      'R -3         '
_cod_original_formula_sum        'C30 H22 B Cl6 I Mn N6 S3 '
_cod_database_code               4350504
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-y,x-y,z
-x+y,-x,z
-x,-y,-z
y,-x+y,-z
x-y,x,-z
2/3+x,1/3+y,1/3+z
2/3-y,1/3+x-y,1/3+z
2/3-x+y,1/3-x,1/3+z
2/3-x,1/3-y,1/3-z
2/3+y,1/3-x+y,1/3-z
2/3+x-y,1/3+x,1/3-z
1/3+x,2/3+y,2/3+z
1/3-y,2/3+x-y,2/3+z
1/3-x+y,2/3-x,2/3+z
1/3-x,2/3-y,2/3-z
1/3+y,2/3-x+y,2/3-z
1/3+x-y,2/3+x,2/3-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_calc_flag
_atom_site_refinement_flags
I(1) I 1.0000 0.0000 0.16680(3) 0.0582(2) Uani 1.00 d SP
Mn(1) Mn 1.0000 0.0000 0.25320(6) 0.0197(2) Uani 1.00 d SP
Cl(2) Cl 1.1247(7) -0.2386(9) 0.1770(3) 0.101(3) Uani 0.40 d P
Cl(3) Cl 1.1152(4) -0.1794(5) 0.1965(2) 0.083(2) Uani 0.60 d P
Cl(4) Cl 0.9421(9) -0.312(1) 0.1301(6) 0.048(2) Uani 0.40 d P
Cl(5) Cl 0.952(1) -0.326(1) 0.1362(5) 0.098(4) Uani 0.60 d P
S(1) S 0.9594(1) 0.1232(1) 0.28605(6) 0.0210(4) Uani 1.00 d .
N(3) N 0.7845(4) 0.0320(4) 0.3349(2) 0.017(1) Uani 1.00 d .
N(4) N 0.9037(4) 0.0068(4) 0.3623(2) 0.018(1) Uani 1.00 d .
C(6) C 0.7273(4) 0.0623(4) 0.3068(2) 0.019(2) Uani 1.00 d .
C(8) C 0.8178(5) -0.0422(4) 0.3886(2) 0.020(2) Uani 1.00 d .
C(9) C 0.7439(4) -0.0277(5) 0.3718(2) 0.022(2) Uani 1.00 d .
C(10) C 0.5769(5) 0.0112(6) 0.2633(2) 0.032(2) Uani 1.00 d .
C(11) C 0.8830(4) 0.0521(4) 0.3286(2) 0.018(2) Uani 1.00 d .
C(12) C 0.7003(6) 0.1876(6) 0.2713(3) 0.038(2) Uani 1.00 d .
C(13) C 0.7596(5) 0.1631(5) 0.2994(2) 0.027(2) Uani 1.00 d .
C(14) C 0.6358(5) -0.0152(5) 0.2893(2) 0.024(2) Uani 1.00 d .
C(15) C 0.6095(5) 0.1126(6) 0.2540(2) 0.033(2) Uani 1.00 d .
C(16) C 0.9843(7) -0.2600(8) 0.1848(4) 0.071(3) Uani 1.00 d .
B(1) B 1.0000 0.0000 0.3767(4) 0.0167 Uani 1.00 d SP
H(2) H 0.8122 -0.0807 0.4151 0.0248 Uiso 1.00 calc .
H(3) H 0.6750 -0.0542 0.3833 0.0272 Uiso 1.00 calc .
H(4) H 0.5119 -0.0421 0.2515 0.0377 Uiso 1.00 calc .
H(5) H 0.7239 0.2591 0.2639 0.0450 Uiso 1.00 calc .
H(6) H 0.8220 0.2169 0.3125 0.0327 Uiso 1.00 calc .
H(7) H 0.6129 -0.0870 0.2952 0.0291 Uiso 1.00 calc .
H(8) H 0.5685 0.1310 0.2355 0.0402 Uiso 1.00 calc .
H(9) H 1.0000 0.0000 0.4064 0.0548 Uiso 1.00 calc SP
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn Mn 0.337 0.728
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
S S 0.125 0.123
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
I I -0.474 1.812
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
B B 0.001 0.001
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I(1) Mn(1) S(1) 114.18(5) . . yes
I(1) Mn(1) S(1) 114.18(5) . 2_645 yes
I(1) Mn(1) S(1) 114.18(5) . 3_765 yes
S(1) Mn(1) S(1) 104.38(6) . 2_645 yes
S(1) Mn(1) S(1) 104.38(6) . 3_765 yes
S(1) Mn(1) S(1) 104.38(6) 2_645 3_765 yes
Cl(3) Cl(2) C(16) 61.6(7) . . yes
Cl(2) Cl(3) C(16) 83.7(7) . . yes
Cl(5) Cl(4) C(16) 67(4) . . yes
Cl(4) Cl(5) C(16) 101(5) . . yes
Mn(1) S(1) C(11) 100.4(2) . . yes
C(6) N(3) C(9) 123.4(5) . . yes
C(6) N(3) C(11) 126.8(5) . . yes
C(9) N(3) C(11) 109.7(5) . . yes
C(8) N(4) C(11) 108.5(5) . . yes
C(8) N(4) B(1) 117.0(6) . . yes
C(11) N(4) B(1) 134.5(6) . . yes
N(3) C(6) C(13) 121.1(5) . . yes
N(3) C(6) C(14) 117.4(5) . . yes
C(13) C(6) C(14) 121.4(6) . . yes
N(4) C(8) C(9) 109.0(5) . . yes
N(3) C(9) C(8) 106.5(5) . . yes
C(14) C(10) C(15) 120.6(6) . . yes
S(1) C(11) N(3) 124.1(5) . . yes
S(1) C(11) N(4) 129.6(4) . . yes
N(3) C(11) N(4) 106.3(5) . . yes
C(13) C(12) C(15) 121.2(6) . . yes
C(6) C(13) C(12) 118.2(6) . . yes
C(6) C(14) C(10) 119.1(6) . . yes
C(10) C(15) C(12) 119.4(6) . . yes
Cl(2) C(16) Cl(3) 34.7(4) . . yes
Cl(2) C(16) Cl(4) 94.2(8) . . yes
Cl(2) C(16) Cl(5) 88.0(8) . . yes
Cl(3) C(16) Cl(4) 120.8(8) . . yes
Cl(3) C(16) Cl(5) 118.3(9) . . yes
Cl(4) C(16) Cl(5) 11(1) . . yes
N(4) B(1) N(4) 112.5(4) . 2_645 yes
N(4) B(1) N(4) 112.5(4) . 3_765 yes
N(4) B(1) N(4) 112.5(4) 2_645 3_765 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I(1) Mn(1) 2.626(2) . yes
Mn(1) S(1) 2.437(2) . yes
Mn(1) S(1) 2.437(2) 2_645 yes
Mn(1) S(1) 2.437(2) 3_765 yes
Cl(2) Cl(3) 1.14(1) . yes
Cl(2) C(16) 1.99(2) . yes
Cl(3) C(16) 1.76(1) . yes
Cl(4) Cl(5) 0.36(3) . yes
Cl(4) C(16) 1.81(2) . yes
Cl(5) C(16) 1.71(2) . yes
S(1) C(11) 1.707(6) . yes
N(3) C(6) 1.439(8) . yes
N(3) C(9) 1.373(8) . yes
N(3) C(11) 1.369(7) . yes
N(4) C(8) 1.379(8) . yes
N(4) C(11) 1.350(8) . yes
N(4) B(1) 1.565(6) . yes
C(6) C(13) 1.362(8) . yes
C(6) C(14) 1.391(9) . yes
C(8) C(9) 1.337(9) . yes
C(10) C(14) 1.385(10) . yes
C(10) C(15) 1.38(1) . yes
C(12) C(13) 1.410(10) . yes
C(12) C(15) 1.37(1) . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
I(1) Mn(1) 2.626(2) .
Cl(3) Cl(5) 3.47(2) 11_665
Cl(3) C(14) 3.591(9) 2_645
Cl(4) C(16) 3.47(2) 10_645
Cl(4) C(12) 3.56(2) 11_555
N(3) C(10) 3.457(9) 18_545
C(10) C(16) 3.57(1) 3_765
C(10) C(11) 3.580(9) 17_555
C(14) C(16) 3.57(1) 3_765
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
I(1) Mn(1) S(1) C(11) 139.7(2) . . . yes
I(1) Mn(1) S(1) C(11) 139.7(2) . 2_645 2_645 yes
I(1) Mn(1) S(1) C(11) 139.7(2) . 3_765 3_765 yes
Mn(1) S(1) C(11) N(3) -122.9(5) . . . yes
Mn(1) S(1) C(11) N(4) 58.3(6) . . . yes
Mn(1) S(1) C(11) N(3) -122.9(5) 2_645 2_645 2_645 yes
Mn(1) S(1) C(11) N(4) 58.3(6) 2_645 2_645 2_645 yes
Mn(1) S(1) C(11) N(3) -122.9(5) 3_765 3_765 3_765 yes
Mn(1) S(1) C(11) N(4) 58.3(6) 3_765 3_765 3_765 yes
Cl(2) Cl(3) C(16) Cl(4) -44(1) . . . yes
Cl(2) Cl(3) C(16) Cl(5) -32(1) . . . yes
Cl(2) C(16) Cl(4) Cl(5) 55(4) . . . yes
Cl(2) C(16) Cl(5) Cl(4) -124(4) . . . yes
Cl(3) Cl(2) C(16) Cl(4) 142.8(9) . . . yes
Cl(3) Cl(2) C(16) Cl(5) 152.0(9) . . . yes
Cl(3) C(16) Cl(4) Cl(5) 79(4) . . . yes
Cl(3) C(16) Cl(5) Cl(4) -106(4) . . . yes
S(1) Mn(1) S(1) C(11) -94.9(2) . 2_645 2_645 yes
S(1) Mn(1) S(1) C(11) 14.4(2) . 3_765 3_765 yes
S(1) C(11) N(3) C(6) 2.6(9) . . . yes
S(1) C(11) N(3) C(9) 179.5(4) . . . yes
S(1) C(11) N(4) C(8) -180.0(5) . . . yes
S(1) C(11) N(4) B(1) 0(1) . . . yes
N(3) C(6) C(13) C(12) 179.6(6) . . . yes
N(3) C(6) C(14) C(10) 177.8(6) . . . yes
N(3) C(9) C(8) N(4) -0.7(7) . . . yes
N(3) C(11) N(4) C(8) 1.0(6) . . . yes
N(3) C(11) N(4) B(1) -178.5(6) . . . yes
N(4) C(11) N(3) C(6) -178.3(5) . . . yes
N(4) C(11) N(3) C(9) -1.4(7) . . . yes
N(4) B(1) N(4) C(8) -150.1(6) . 2_645 2_645 yes
N(4) B(1) N(4) C(11) 29(1) . 2_645 2_645 yes
N(4) B(1) N(4) C(8) 81.4(10) . 3_765 3_765 yes
N(4) B(1) N(4) C(11) -99.1(6) . 3_765 3_765 yes
C(6) N(3) C(9) C(8) 178.3(6) . . . yes
C(6) C(13) C(12) C(15) 3(1) . . . yes
C(6) C(14) C(10) C(15) 1(1) . . . yes
C(8) C(9) N(3) C(11) 1.3(7) . . . yes
C(9) N(3) C(6) C(13) 121.6(7) . . . yes
C(9) N(3) C(6) C(14) -55.6(8) . . . yes
C(9) C(8) N(4) C(11) -0.2(7) . . . yes
C(9) C(8) N(4) B(1) 179.4(5) . . . yes
C(10) C(14) C(6) C(13) 0(1) . . . yes
C(10) C(15) C(12) C(13) -1(1) . . . yes
C(11) N(3) C(6) C(13) -61.9(9) . . . yes
C(11) N(3) C(6) C(14) 120.9(6) . . . yes
C(12) C(13) C(6) C(14) -3(1) . . . yes
C(12) C(15) C(10) C(14) -1(1) . . . yes
C(12) C(15) C(10) C(14) -1(1) . . . yes
