#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:07:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179094 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/56/4305600.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_4305600
loop_
_publ_author_name
'Rosalice M. Silva'
'Chengeto Gwengo'
'Sergey V. Lindeman'
'Mark D. Smith'
'Gary J. Long'
'Fernande Grandjean'
'James R. Gardinier'
_publ_section_title
;
A Second-Generation Janus Scorpionate Ligand: Controlling Coordination
Modes in Iron(II) Complexes by Steric Modulation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7233
_journal_page_last               7242
_journal_paper_doi               10.1021/ic8005794
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C7 H8 B K N6 O S6'
_chemical_formula_weight         434.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.0101(5)
_cell_length_b                   15.0958(5)
_cell_length_c                   16.0605(5)
_cell_measurement_reflns_used    6228
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61
_cell_measurement_theta_min      3
_cell_volume                     3396.7(2)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_data_reduction        'SADABS-2004/1 (Bruker, 2005)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)'
_computing_structure_solution    'XS/SHELXTL v6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28097
_diffrn_reflns_theta_full        67.37
_diffrn_reflns_theta_max         61.37
_diffrn_reflns_theta_min         5.11
_exptl_absorpt_coefficient_mu    9.713
_exptl_absorpt_correction_T_max  0.5104
_exptl_absorpt_correction_T_min  0.0678
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical absorption correction based on the actual
 shape of crystal followed by:
 SADABS. Program for empirical absorption correction of
 area-detector data. University of Goetingen. Germany. 
 Sheldrick, G. M. 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         2612
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0422P)²+1.4527P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                2446
_reflns_number_total             2612
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8005794-file003_2.cif
_cod_data_source_block           KHBmtda-MeOH
_cod_database_code               4305600
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.74205(3) 0.22794(3) 0.52005(3) 0.01642(13) Uani 1 1 d . . .
S1 S 0.66694(3) -0.14309(3) 0.66312(3) 0.01592(13) Uani 1 1 d . . .
S2 S 0.75268(3) 0.01361(3) 0.75109(3) 0.01806(14) Uani 1 1 d . . .
S3 S 0.94239(3) -0.15532(3) 0.45021(3) 0.02002(14) Uani 1 1 d . . .
S4 S 0.98716(3) 0.01367(3) 0.36093(3) 0.01823(13) Uani 1 1 d . . .
S5 S 0.61654(3) -0.16466(3) 0.39073(3) 0.01792(14) Uani 1 1 d . . .
S6 S 0.50760(3) 0.00528(3) 0.37616(3) 0.01493(13) Uani 1 1 d . . .
N1 N 0.75805(10) -0.00043(10) 0.59440(10) 0.0119(3) Uani 1 1 d . . .
N2 N 0.80071(11) 0.08032(9) 0.61124(9) 0.0146(3) Uani 1 1 d . . .
N3 N 0.84100(11) 0.00001(9) 0.45200(9) 0.0127(3) Uani 1 1 d . . .
N4 N 0.83868(11) 0.08674(9) 0.42288(9) 0.0150(3) Uani 1 1 d . . .
N5 N 0.66019(11) -0.00416(9) 0.45992(9) 0.0120(3) Uani 1 1 d . . .
N6 N 0.63108(11) 0.08341(9) 0.46740(9) 0.0151(3) Uani 1 1 d . . .
B1 B 0.75468(14) -0.03478(15) 0.50272(13) 0.0125(5) Uani 1 1 d . . .
C1 C 0.72618(13) -0.04638(12) 0.66117(11) 0.0137(4) Uani 1 1 d . . .
C2 C 0.80238(14) 0.09514(13) 0.68975(12) 0.0177(4) Uani 1 1 d . . .
C3 C 0.91564(13) -0.05046(12) 0.42634(11) 0.0143(4) Uani 1 1 d . . .
C4 C 0.91080(14) 0.10165(13) 0.37492(11) 0.0169(4) Uani 1 1 d . . .
C5 C 0.60317(13) -0.05650(11) 0.41375(11) 0.0130(4) Uani 1 1 d . . .
C6 C 0.55342(13) 0.09665(12) 0.42690(11) 0.0153(4) Uani 1 1 d . . .
H1 H 0.7552(11) -0.1042(13) 0.5039(11) 0.007(5) Uiso 1 1 d . . .
H2 H 0.8278(14) 0.1447(14) 0.7115(13) 0.018(5) Uiso 1 1 d . . .
H4 H 0.9208(14) 0.1567(14) 0.3503(12) 0.018(5) Uiso 1 1 d . . .
H6 H 0.5252(14) 0.1502(13) 0.4261(12) 0.012(5) Uiso 1 1 d . . .
O1S O 0.60984(12) 0.21399(11) 0.64729(9) 0.0333(4) Uani 1 1 d . . .
C1S C 0.60365(19) 0.2419(2) 0.73071(15) 0.0399(6) Uani 1 1 d . . .
H1OS H 0.555(2) 0.2010(18) 0.6325(16) 0.042(8) Uiso 1 1 d . . .
H1SA H 0.665(2) 0.2509(16) 0.7520(17) 0.050(8) Uiso 1 1 d . . .
H1SB H 0.563(3) 0.286(2) 0.744(2) 0.098(13) Uiso 1 1 d . . .
H1SC H 0.577(3) 0.198(3) 0.764(3) 0.111(14) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1S K1 N2 75.45(5) . . ?
O1S K1 N6 78.04(5) . . ?
N2 K1 N6 72.59(4) . . ?
O1S K1 N4 129.73(5) . . ?
N2 K1 N4 64.42(4) . . ?
N6 K1 N4 62.39(4) . . ?
O1S K1 S1 77.72(4) . 8_765 ?
N2 K1 S1 89.53(3) . 8_765 ?
N6 K1 S1 152.82(3) . 8_765 ?
N4 K1 S1 128.25(3) . 8_765 ?
O1S K1 S5 154.87(4) . 8_765 ?
N2 K1 S5 123.12(3) . 8_765 ?
N6 K1 S5 121.66(3) . 8_765 ?
N4 K1 S5 75.40(3) . 8_765 ?
S1 K1 S5 85.155(14) 8_765 8_765 ?
O1S K1 S3 76.64(4) . 8_765 ?
N2 K1 S3 146.08(3) . 8_765 ?
N6 K1 S3 83.10(3) . 8_765 ?
N4 K1 S3 123.92(3) . 8_765 ?
S1 K1 S3 102.979(16) 8_765 8_765 ?
S5 K1 S3 89.645(15) 8_765 8_765 ?
O1S K1 C2 62.69(5) . . ?
N2 K1 C2 19.84(4) . . ?
N6 K1 C2 85.58(5) . . ?
N4 K1 C2 83.55(4) . . ?
S1 K1 C2 72.46(3) 8_765 . ?
S5 K1 C2 129.01(4) 8_765 . ?
S3 K1 C2 139.22(4) 8_765 . ?
C1 S1 K1 108.16(6) . 8_755 ?
C2 S2 C1 89.05(9) . . ?
C3 S3 K1 113.92(7) . 8_755 ?
C4 S4 C3 89.57(9) . . ?
C5 S5 K1 113.91(6) . 8_755 ?
C6 S6 C5 88.76(9) . . ?
C1 N1 N2 116.05(15) . . ?
C1 N1 B1 124.55(15) . . ?
N2 N1 B1 119.31(14) . . ?
C2 N2 N1 110.73(15) . . ?
C2 N2 K1 112.49(12) . . ?
N1 N2 K1 118.27(10) . . ?
C3 N3 N4 116.37(15) . . ?
C3 N3 B1 124.77(15) . . ?
N4 N3 B1 118.53(14) . . ?
C4 N4 N3 110.28(15) . . ?
C4 N4 K1 123.08(12) . . ?
N3 N4 K1 120.66(10) . . ?
C5 N5 N6 115.60(14) . . ?
C5 N5 B1 124.87(15) . . ?
N6 N5 B1 119.52(14) . . ?
C6 N6 N5 110.70(15) . . ?
C6 N6 K1 120.05(12) . . ?
N5 N6 K1 127.07(11) . . ?
N3 B1 N5 109.26(15) . . ?
N3 B1 N1 111.06(15) . . ?
N5 B1 N1 110.02(15) . . ?
N3 B1 H1 110.0(9) . . ?
N5 B1 H1 108.1(9) . . ?
N1 B1 H1 108.3(10) . . ?
N1 C1 S1 128.57(14) . . ?
N1 C1 S2 108.65(13) . . ?
S1 C1 S2 122.75(11) . . ?
N2 C2 S2 115.51(15) . . ?
N2 C2 K1 47.68(9) . . ?
S2 C2 K1 139.41(9) . . ?
N2 C2 H2 122.3(13) . . ?
S2 C2 H2 122.2(13) . . ?
K1 C2 H2 85.5(13) . . ?
N3 C3 S3 129.38(14) . . ?
N3 C3 S4 108.28(13) . . ?
S3 C3 S4 122.34(11) . . ?
N4 C4 S4 115.49(14) . . ?
N4 C4 H4 121.8(13) . . ?
S4 C4 H4 122.7(13) . . ?
N5 C5 S5 128.60(14) . . ?
N5 C5 S6 109.46(13) . . ?
S5 C5 S6 121.94(11) . . ?
N6 C6 S6 115.48(14) . . ?
N6 C6 H6 121.3(13) . . ?
S6 C6 H6 123.2(13) . . ?
C1S O1S K1 136.20(15) . . ?
C1S O1S H1OS 106.6(18) . . ?
K1 O1S H1OS 115.4(18) . . ?
O1S C1S H1SA 109.5(17) . . ?
O1S C1S H1SB 119(3) . . ?
H1SA C1S H1SB 113(3) . . ?
O1S C1S H1SC 111(3) . . ?
H1SA C1S H1SC 105(3) . . ?
H1SB C1S H1SC 97(3) . . ?
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
K1 O1S 2.7662(15) . ?
K1 N2 2.7903(15) . ?
K1 N6 2.8094(15) . ?
K1 N4 2.9683(15) . ?
K1 S1 3.2704(6) 8_765 ?
K1 S5 3.2966(6) 8_765 ?
K1 S3 3.3229(6) 8_765 ?
K1 C2 3.4872(19) . ?
S1 C1 1.6797(19) . ?
S1 K1 3.2706(6) 8_755 ?
S2 C2 1.7235(19) . ?
S2 C1 1.7445(18) . ?
S3 C3 1.6713(18) . ?
S3 K1 3.3228(6) 8_755 ?
S4 C4 1.720(2) . ?
S4 C3 1.7449(18) . ?
S5 C5 1.6845(18) . ?
S5 K1 3.2966(6) 8_755 ?
S6 C6 1.7259(19) . ?
S6 C5 1.7398(18) . ?
N1 C1 1.353(2) . ?
N1 N2 1.384(2) . ?
N1 B1 1.562(3) . ?
N2 C2 1.281(2) . ?
N3 C3 1.358(2) . ?
N3 N4 1.391(2) . ?
N3 B1 1.550(2) . ?
N4 C4 1.290(2) . ?
N5 C5 1.346(2) . ?
N5 N6 1.389(2) . ?
N5 B1 1.562(2) . ?
N6 C6 1.283(2) . ?
B1 H1 1.05(2) . ?
C2 H2 0.90(2) . ?
C4 H4 0.93(2) . ?
C6 H6 0.90(2) . ?
O1S C1S 1.407(3) . ?
O1S H1OS 0.83(3) . ?
C1S H1SA 0.94(3) . ?
C1S H1SB 0.91(4) . ?
C1S H1SC 0.93(4) . ?
