#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:07:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179094 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/56/4305605.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_4305605
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            'C26 H46 B2 Cl6 Fe N12 O6 S18'
_chemical_formula_weight         1490.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                116.0080(10)
_cell_angle_beta                 94.4850(10)
_cell_angle_gamma                115.0470(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0552(2)
_cell_length_b                   12.4970(2)
_cell_length_c                   13.3489(2)
_cell_measurement_reflns_used    5231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66
_cell_measurement_theta_min      4
_cell_volume                     1549.09(5)
_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 0.918
_diffrn_measured_fraction_theta_max 0.968
_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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12780
_diffrn_reflns_theta_full        67.17
_diffrn_reflns_theta_max         67.17
_diffrn_reflns_theta_min         3.89
_exptl_absorpt_coefficient_mu    10.409
_exptl_absorpt_correction_T_max  0.2300
_exptl_absorpt_correction_T_min  0.0891
_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            'pale orange'
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00133(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5074
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0271P)²+1.1561P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0555
_reflns_number_gt                4999
_reflns_number_total             5074
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8005794-file003_7.cif
_cod_data_source_block           7-2CHCl3
_cod_original_cell_volume        1549.09(4)
_cod_database_code               4305605
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.0000 0.5000 0.01358(9) Uani 1 2 d S . .
S1A S 0.21571(4) -0.07394(4) 0.33105(4) 0.01896(10) Uani 1 1 d . . .
S2A S 0.51221(4) -0.27230(4) 0.36364(4) 0.01772(10) Uani 1 1 d . . .
S3A S 0.62305(4) 0.13809(4) 0.35914(4) 0.01684(10) Uani 1 1 d . . .
O1 O 0.36110(12) 0.00186(12) 0.38835(11) 0.0208(3) Uani 1 1 d . . .
O2 O 0.42124(11) -0.21694(12) 0.39742(11) 0.0184(3) Uani 1 1 d . . .
O3 O 0.62527(12) 0.04535(13) 0.40440(11) 0.0195(3) Uani 1 1 d . . .
C1A C 0.1589(2) -0.2509(2) 0.2834(2) 0.0303(5) Uani 1 1 d . . .
C2A C 0.1494(2) -0.0327(3) 0.4480(2) 0.0307(5) Uani 1 1 d . . .
C3A C 0.5127(2) -0.3543(2) 0.44481(19) 0.0298(4) Uani 1 1 d . . .
C4A C 0.4179(2) -0.4244(2) 0.22144(17) 0.0255(4) Uani 1 1 d . . .
C5A C 0.7800(2) 0.2905(2) 0.43466(19) 0.0272(4) Uani 1 1 d . . .
C6A C 0.6402(2) 0.0621(2) 0.21723(17) 0.0232(4) Uani 1 1 d . . .
H1A H 0.187(3) -0.285(3) 0.219(3) 0.054(8) Uiso 1 1 d . . .
H1B H 0.065(2) -0.299(2) 0.263(2) 0.033(6) Uiso 1 1 d . . .
H1C H 0.199(3) -0.253(3) 0.351(2) 0.046(7) Uiso 1 1 d . . .
H2A H 0.173(2) 0.061(3) 0.481(2) 0.041(7) Uiso 1 1 d . . .
H2B H 0.183(3) -0.045(3) 0.503(3) 0.047(8) Uiso 1 1 d . . .
H2C H 0.057(3) -0.093(3) 0.412(2) 0.037(6) Uiso 1 1 d . . .
H3A H 0.423(2) -0.420(2) 0.433(2) 0.031(6) Uiso 1 1 d . . .
H3B H 0.554(2) -0.281(3) 0.524(2) 0.038(7) Uiso 1 1 d . . .
H3C H 0.556(2) -0.403(3) 0.418(2) 0.036(6) Uiso 1 1 d . . .
H4A H 0.337(2) -0.484(2) 0.2261(19) 0.028(6) Uiso 1 1 d . . .
H4B H 0.467(2) -0.469(3) 0.197(2) 0.036(6) Uiso 1 1 d . . .
H4C H 0.399(2) -0.396(3) 0.168(2) 0.037(6) Uiso 1 1 d . . .
H5A H 0.841(3) 0.264(3) 0.432(2) 0.039(7) Uiso 1 1 d . . .
H5B H 0.785(2) 0.342(3) 0.518(2) 0.042(7) Uiso 1 1 d . . .
H5C H 0.790(2) 0.343(3) 0.401(2) 0.038(7) Uiso 1 1 d . . .
H6A H 0.646(2) 0.121(3) 0.187(2) 0.037(6) Uiso 1 1 d . . .
H6B H 0.713(2) 0.052(2) 0.224(2) 0.032(6) Uiso 1 1 d . . .
H6C H 0.564(2) -0.023(2) 0.1708(19) 0.025(5) Uiso 1 1 d . . .
S1 S 1.22471(4) 0.28265(4) 0.73222(4) 0.01962(10) Uani 1 1 d . . .
S2 S 1.10098(4) 0.28401(4) 0.91977(4) 0.01857(10) Uani 1 1 d . . .
S3 S 1.01531(4) 0.57860(4) 0.74144(4) 0.02065(10) Uani 1 1 d . . .
S4 S 1.13904(4) 0.85955(4) 0.96289(4) 0.02331(11) Uani 1 1 d . . .
S5 S 1.49193(4) 0.71304(4) 0.74332(4) 0.02022(10) Uani 1 1 d . . .
S6 S 1.66394(4) 0.77558(4) 0.96067(4) 0.01988(10) Uani 1 1 d . . .
N1 N 1.20068(13) 0.49082(15) 0.89605(12) 0.0157(3) Uani 1 1 d . . .
N2 N 1.15773(14) 0.53229(15) 0.99143(13) 0.0193(3) Uani 1 1 d . . .
N3 N 1.24439(14) 0.71468(14) 0.91309(13) 0.0169(3) Uani 1 1 d . . .
N4 N 1.32855(15) 0.83253(16) 1.02016(14) 0.0235(3) Uani 1 1 d . . .
N5 N 1.42105(14) 0.65646(15) 0.91063(13) 0.0171(3) Uani 1 1 d . . .
N6 N 1.46504(15) 0.66525(16) 1.01447(14) 0.0224(3) Uani 1 1 d . . .
B1 B 1.27390(19) 0.5948(2) 0.85729(18) 0.0175(4) Uani 1 1 d . . .
C1 C 1.18161(16) 0.36196(18) 0.84580(15) 0.0159(3) Uani 1 1 d . . .
C2 C 1.10396(17) 0.43494(19) 1.01272(16) 0.0193(4) Uani 1 1 d . . .
C3 C 1.13648(17) 0.70810(18) 0.86723(16) 0.0180(4) Uani 1 1 d . . .
C4 C 1.28548(19) 0.9165(2) 1.05599(18) 0.0257(4) Uani 1 1 d . . .
C5 C 1.51229(16) 0.70920(17) 0.86637(15) 0.0162(3) Uani 1 1 d . . .
C6 C 1.58892(19) 0.7244(2) 1.04966(17) 0.0228(4) Uani 1 1 d . . .
H1 H 1.2426(19) 0.545(2) 0.7619(18) 0.018(5) Uiso 1 1 d . . .
H2 H 1.068(2) 0.445(2) 1.073(2) 0.024(5) Uiso 1 1 d . . .
H4 H 1.331(2) 1.001(3) 1.126(2) 0.035(6) Uiso 1 1 d . . .
H6 H 1.636(2) 0.739(2) 1.119(2) 0.034(6) Uiso 1 1 d . . .
Cl1 Cl 2.03992(5) 0.94568(5) 0.70574(5) 0.03237(12) Uani 1 1 d . . .
Cl2 Cl 1.78903(5) 0.77399(6) 0.71303(5) 0.03612(13) Uani 1 1 d . . .
Cl3 Cl 1.86589(5) 0.66833(6) 0.50878(4) 0.03735(13) Uani 1 1 d . . .
C1S C 1.92086(19) 0.7753(2) 0.66300(17) 0.0240(4) Uani 1 1 d . . .
H1S H 1.957(2) 0.738(2) 0.6946(18) 0.020(5) 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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
O3 Fe1 O3 180.0 . 2_656 ?
O3 Fe1 O2 85.23(5) . 2_656 ?
O3 Fe1 O2 94.78(5) 2_656 2_656 ?
O3 Fe1 O2 94.77(5) . . ?
O3 Fe1 O2 85.22(5) 2_656 . ?
O2 Fe1 O2 180.0 2_656 . ?
O3 Fe1 O1 87.92(5) . . ?
O3 Fe1 O1 92.08(5) 2_656 . ?
O2 Fe1 O1 85.10(5) 2_656 . ?
O2 Fe1 O1 94.91(5) . . ?
O3 Fe1 O1 92.08(5) . 2_656 ?
O3 Fe1 O1 87.92(5) 2_656 2_656 ?
O2 Fe1 O1 94.91(5) 2_656 2_656 ?
O2 Fe1 O1 85.09(5) . 2_656 ?
O1 Fe1 O1 180.0 . 2_656 ?
O1 S1A C1A 105.69(9) . . ?
O1 S1A C2A 106.48(9) . . ?
C1A S1A C2A 98.76(12) . . ?
O2 S2A C4A 103.69(9) . . ?
O2 S2A C3A 105.65(9) . . ?
C4A S2A C3A 98.23(10) . . ?
O3 S3A C6A 103.60(8) . . ?
O3 S3A C5A 105.35(9) . . ?
C6A S3A C5A 98.43(10) . . ?
S1A O1 Fe1 139.00(7) . . ?
S2A O2 Fe1 118.94(7) . . ?
S3A O3 Fe1 118.09(7) . . ?
S1A C1A H1A 105.8(18) . . ?
S1A C1A H1B 108.3(14) . . ?
H1A C1A H1B 113(2) . . ?
S1A C1A H1C 107.4(15) . . ?
H1A C1A H1C 112(2) . . ?
H1B C1A H1C 110(2) . . ?
S1A C2A H2A 106.7(16) . . ?
S1A C2A H2B 109.3(17) . . ?
H2A C2A H2B 111(2) . . ?
S1A C2A H2C 106.1(15) . . ?
H2A C2A H2C 111(2) . . ?
H2B C2A H2C 113(2) . . ?
S2A C3A H3A 110.6(13) . . ?
S2A C3A H3B 104.5(15) . . ?
H3A C3A H3B 110(2) . . ?
S2A C3A H3C 109.2(15) . . ?
H3A C3A H3C 109(2) . . ?
H3B C3A H3C 113(2) . . ?
S2A C4A H4A 108.7(13) . . ?
S2A C4A H4B 108.4(15) . . ?
H4A C4A H4B 111.9(19) . . ?
S2A C4A H4C 107.8(15) . . ?
H4A C4A H4C 109.2(19) . . ?
H4B C4A H4C 111(2) . . ?
S3A C5A H5A 108.6(16) . . ?
S3A C5A H5B 107.0(15) . . ?
H5A C5A H5B 108(2) . . ?
S3A C5A H5C 109.4(16) . . ?
H5A C5A H5C 112(2) . . ?
H5B C5A H5C 111(2) . . ?
S3A C6A H6A 106.8(14) . . ?
S3A C6A H6B 109.1(14) . . ?
H6A C6A H6B 114(2) . . ?
S3A C6A H6C 105.8(13) . . ?
H6A C6A H6C 109(2) . . ?
H6B C6A H6C 111.5(19) . . ?
C2 S2 C1 89.03(8) . . ?
C4 S4 C3 89.16(9) . . ?
C6 S6 C5 89.33(9) . . ?
C1 N1 N2 116.33(14) . . ?
C1 N1 B1 123.81(14) . . ?
N2 N1 B1 119.76(14) . . ?
C2 N2 N1 110.93(15) . . ?
C3 N3 N4 116.48(14) . . ?
C3 N3 B1 124.25(15) . . ?
N4 N3 B1 119.14(14) . . ?
C4 N4 N3 110.73(16) . . ?
C5 N5 N6 116.34(14) . . ?
C5 N5 B1 124.89(14) . . ?
N6 N5 B1 118.69(14) . . ?
C6 N6 N5 110.96(15) . . ?
N5 B1 N1 107.49(14) . . ?
N5 B1 N3 108.21(14) . . ?
N1 B1 N3 107.53(14) . . ?
N5 B1 H1 112.3(11) . . ?
N1 B1 H1 111.2(11) . . ?
N3 B1 H1 109.9(10) . . ?
N1 C1 S1 128.15(13) . . ?
N1 C1 S2 108.57(12) . . ?
S1 C1 S2 123.28(10) . . ?
N2 C2 S2 115.12(14) . . ?
N2 C2 H2 122.2(13) . . ?
S2 C2 H2 122.7(13) . . ?
N3 C3 S3 127.83(14) . . ?
N3 C3 S4 108.67(13) . . ?
S3 C3 S4 123.50(11) . . ?
N4 C4 S4 114.97(15) . . ?
N4 C4 H4 121.6(15) . . ?
S4 C4 H4 123.4(15) . . ?
N5 C5 S5 128.34(13) . . ?
N5 C5 S6 108.39(12) . . ?
S5 C5 S6 123.26(10) . . ?
N6 C6 S6 114.98(14) . . ?
N6 C6 H6 122.7(15) . . ?
S6 C6 H6 122.4(15) . . ?
Cl3 C1S Cl2 109.72(11) . . ?
Cl3 C1S Cl1 109.62(10) . . ?
Cl2 C1S Cl1 110.87(10) . . ?
Cl3 C1S H1S 107.4(13) . . ?
Cl2 C1S H1S 109.1(12) . . ?
Cl1 C1S H1S 110.0(13) . . ?
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
Fe1 O3 2.1075(12) . ?
Fe1 O3 2.1075(12) 2_656 ?
Fe1 O2 2.1184(11) 2_656 ?
Fe1 O2 2.1184(11) . ?
Fe1 O1 2.1676(12) . ?
Fe1 O1 2.1677(12) 2_656 ?
S1A O1 1.5177(13) . ?
S1A C1A 1.7833(19) . ?
S1A C2A 1.783(2) . ?
S2A O2 1.5267(12) . ?
S2A C4A 1.7825(19) . ?
S2A C3A 1.789(2) . ?
S3A O3 1.5320(12) . ?
S3A C6A 1.7841(19) . ?
S3A C5A 1.786(2) . ?
C1A H1A 0.94(3) . ?
C1A H1B 0.97(2) . ?
C1A H1C 1.01(3) . ?
C2A H2A 0.95(3) . ?
C2A H2B 0.91(3) . ?
C2A H2C 0.97(3) . ?
C3A H3A 0.99(2) . ?
C3A H3B 0.94(3) . ?
C3A H3C 0.94(3) . ?
C4A H4A 0.97(2) . ?
C4A H4B 0.95(3) . ?
C4A H4C 0.96(3) . ?
C5A H5A 0.92(3) . ?
C5A H5B 0.99(3) . ?
C5A H5C 0.93(3) . ?
C6A H6A 0.96(3) . ?
C6A H6B 0.94(2) . ?
C6A H6C 0.93(2) . ?
S1 C1 1.6710(17) . ?
S2 C2 1.7267(18) . ?
S2 C1 1.7494(17) . ?
S3 C3 1.6746(19) . ?
S4 C4 1.728(2) . ?
S4 C3 1.7431(18) . ?
S5 C5 1.6663(18) . ?
S6 C6 1.7271(19) . ?
S6 C5 1.7479(18) . ?
N1 C1 1.346(2) . ?
N1 N2 1.382(2) . ?
N1 B1 1.557(2) . ?
N2 C2 1.283(2) . ?
N3 C3 1.347(2) . ?
N3 N4 1.380(2) . ?
N3 B1 1.562(2) . ?
N4 C4 1.288(3) . ?
N5 C5 1.350(2) . ?
N5 N6 1.385(2) . ?
N5 B1 1.553(2) . ?
N6 C6 1.284(3) . ?
B1 H1 1.09(2) . ?
C2 H2 0.93(2) . ?
C4 H4 0.92(3) . ?
C6 H6 0.94(3) . ?
Cl1 C1S 1.772(2) . ?
Cl2 C1S 1.768(2) . ?
Cl3 C1S 1.757(2) . ?
C1S H1S 0.95(2) . ?
