#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:07:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179094 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/56/4305604.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_4305604
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_moiety         '2(C6 H4 B N6 S6), Fe H12 O6, 6(H2 O)'
_chemical_formula_sum            'C12 H32 B2 Fe N12 O12 S12'
_chemical_formula_weight         998.69
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                115.9180(10)
_cell_angle_beta                 98.7860(10)
_cell_angle_gamma                90.2380(10)
_cell_formula_units_Z            1
_cell_length_a                   7.6358(5)
_cell_length_b                   11.7442(8)
_cell_length_c                   12.4548(8)
_cell_measurement_reflns_used    6639
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      26.391
_cell_measurement_theta_min      2.708
_cell_volume                     989.61(11)
_computing_cell_refinement       'SAINT+ NT V6.22 (Bruker, 2001)'
_computing_data_collection       'SMART NT V5.625 (Bruker, 1998)'
_computing_data_reduction        'SAINT+ NT V6.22'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12037
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4063
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0369P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                3597
_reflns_number_total             4063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8005794-file003_6.cif
_cod_data_source_block           6-6H2O
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_database_code               4305604
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 0.0000 0.0000 0.0000 0.01800(9) Uani 1 2 d S . .
S11 S 0.16690(6) 0.34544(4) 0.38296(4) 0.02852(12) Uani 1 1 d . . .
S12 S 0.49964(6) 0.32147(4) 0.53588(4) 0.02828(12) Uani 1 1 d . . .
S21 S 0.40233(6) -0.01870(4) 0.68125(4) 0.02383(11) Uani 1 1 d . . .
S22 S 0.40284(6) 0.23705(4) 0.89840(4) 0.02326(11) Uani 1 1 d . . .
S31 S -0.18787(6) 0.45721(5) 0.87426(4) 0.03146(12) Uani 1 1 d . . .
S32 S 0.10921(7) 0.58868(4) 0.82581(4) 0.03195(12) Uani 1 1 d . . .
B1 B 0.2093(3) 0.30433(18) 0.69039(17) 0.0200(4) Uani 1 1 d . . .
H1 H 0.322(2) 0.3690(16) 0.7436(14) 0.020(4) Uiso 1 1 d . . .
C11 C 0.2774(2) 0.32350(15) 0.50415(15) 0.0220(4) Uani 1 1 d . . .
C12 C -0.0307(2) 0.33126(17) 0.42755(16) 0.0271(4) Uani 1 1 d . . .
H12 H -0.1420 0.3368 0.3848 0.022(5) Uiso 1 1 calc R . .
C21 C 0.3469(2) 0.13736(16) 0.75004(15) 0.0193(3) Uani 1 1 d . . .
C22 C 0.2903(2) -0.03162(16) 0.54551(15) 0.0234(4) Uani 1 1 d . . .
H22 H 0.2794 -0.1082 0.4726 0.030(5) Uiso 1 1 calc R . .
C31 C 0.0017(2) 0.45786(16) 0.81340(15) 0.0226(4) Uani 1 1 d . . .
C32 C -0.1863(2) 0.29588(18) 0.81868(17) 0.0325(4) Uani 1 1 d . . .
H32 H -0.2729 0.2463 0.8307 0.037(6) Uiso 1 1 calc R . .
N12 N -0.01802(18) 0.31251(13) 0.52297(13) 0.0240(3) Uani 1 1 d . . .
N11 N 0.15833(18) 0.30965(13) 0.56731(12) 0.0199(3) Uani 1 1 d . . .
N22 N 0.22221(18) 0.07003(13) 0.54960(12) 0.0213(3) Uani 1 1 d . . .
N21 N 0.25607(17) 0.16690(13) 0.66553(12) 0.0183(3) Uani 1 1 d . . .
N32 N -0.06059(19) 0.24621(14) 0.75965(13) 0.0263(3) Uani 1 1 d . . .
N31 N 0.04732(18) 0.33854(13) 0.75677(12) 0.0197(3) Uani 1 1 d . . .
O1 O 0.07901(19) 0.17632(13) 0.01258(14) 0.0346(3) Uani 1 1 d D . .
H1A H 0.150(3) 0.190(2) -0.0209(19) 0.055(8) Uiso 1 1 d D . .
H1B H 0.037(3) 0.2385(17) 0.0548(18) 0.055(8) Uiso 1 1 d D . .
O2 O 0.23552(17) 0.00628(13) 0.11943(12) 0.0280(3) Uani 1 1 d D . .
H2A H 0.217(3) 0.019(2) 0.1835(13) 0.046(7) Uiso 1 1 d D . .
H2B H 0.318(2) 0.0483(18) 0.1244(18) 0.035(6) Uiso 1 1 d D . .
O3 O 0.13208(17) -0.09056(12) -0.14705(12) 0.0247(3) Uani 1 1 d D . .
H3A H 0.106(3) -0.081(2) -0.2054(14) 0.038(7) Uiso 1 1 d D . .
H3B H 0.2340(17) -0.102(2) -0.1401(19) 0.048(7) Uiso 1 1 d D . .
O4 O 0.52441(17) 0.14319(13) 0.11243(12) 0.0274(3) Uani 1 1 d D . .
H4A H 0.506(3) 0.145(2) 0.0493(14) 0.047(7) Uiso 1 1 d D . .
H4B H 0.523(3) 0.2131(14) 0.1652(15) 0.037(6) Uiso 1 1 d D . .
O5 O 0.06614(17) 0.01914(13) 0.30736(12) 0.0256(3) Uani 1 1 d D . .
H5A H 0.097(3) 0.052(2) 0.3784(12) 0.050(7) Uiso 1 1 d D . .
H5B H 0.055(3) -0.0543(12) 0.2881(17) 0.033(6) Uiso 1 1 d D . .
O6A O 0.5593(3) 0.36575(19) 0.3074(2) 0.0426(8) Uani 0.797(6) 1 d PD A 1
H6A H 0.551(4) 0.367(3) 0.3696(18) 0.064 Uiso 0.797(6) 1 d PD A 1
H6B H 0.553(5) 0.431(2) 0.305(4) 0.064 Uiso 0.797(6) 1 d PD A 1
O6B O 0.5128(12) 0.3918(9) 0.2421(10) 0.053(3) Uiso 0.203(6) 1 d P A 2
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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 O1 180.00(9) 2 . ?
O1 Fe1 O3 90.15(5) 2 2 ?
O1 Fe1 O3 89.84(5) . 2 ?
O1 Fe1 O3 89.85(5) 2 . ?
O1 Fe1 O3 90.15(5) . . ?
O3 Fe1 O3 180.0 2 . ?
O1 Fe1 O2 89.01(6) 2 . ?
O1 Fe1 O2 90.99(6) . . ?
O3 Fe1 O2 90.55(5) 2 . ?
O3 Fe1 O2 89.45(5) . . ?
O1 Fe1 O2 90.99(6) 2 2 ?
O1 Fe1 O2 89.01(6) . 2 ?
O3 Fe1 O2 89.45(5) 2 2 ?
O3 Fe1 O2 90.56(5) . 2 ?
O2 Fe1 O2 180.0 . 2 ?
C12 S11 C11 88.92(8) . . ?
C22 S21 C21 88.93(8) . . ?
C32 S31 C31 88.70(9) . . ?
N31 B1 N11 108.28(13) . . ?
N31 B1 N21 109.88(13) . . ?
N11 B1 N21 108.70(13) . . ?
N31 B1 H1 110.7(9) . . ?
N11 B1 H1 110.2(9) . . ?
N21 B1 H1 109.1(9) . . ?
N11 C11 S12 126.32(13) . . ?
N11 C11 S11 109.23(12) . . ?
S12 C11 S11 124.45(10) . . ?
N12 C12 S11 115.54(14) . . ?
N12 C12 H12 122.2 . . ?
S11 C12 H12 122.2 . . ?
N21 C21 S22 125.38(13) . . ?
N21 C21 S21 109.24(12) . . ?
S22 C21 S21 125.36(10) . . ?
N22 C22 S21 115.15(13) . . ?
N22 C22 H22 122.4 . . ?
S21 C22 H22 122.4 . . ?
N31 C31 S32 126.17(13) . . ?
N31 C31 S31 109.36(12) . . ?
S32 C31 S31 124.46(10) . . ?
N32 C32 S31 115.65(14) . . ?
N32 C32 H32 122.2 . . ?
S31 C32 H32 122.2 . . ?
C12 N12 N11 110.14(14) . . ?
C11 N11 N12 116.16(13) . . ?
C11 N11 B1 123.83(14) . . ?
N12 N11 B1 119.72(13) . . ?
C22 N22 N21 110.91(13) . . ?
C21 N21 N22 115.71(13) . . ?
C21 N21 B1 123.53(13) . . ?
N22 N21 B1 120.38(13) . . ?
C32 N32 N31 110.55(15) . . ?
C31 N31 N32 115.74(14) . . ?
C31 N31 B1 123.02(14) . . ?
N32 N31 B1 121.24(13) . . ?
Fe1 O1 H1A 126.7(18) . . ?
Fe1 O1 H1B 120.4(18) . . ?
H1A O1 H1B 113(2) . . ?
Fe1 O2 H2A 112.5(17) . . ?
Fe1 O2 H2B 117.9(16) . . ?
H2A O2 H2B 111(2) . . ?
Fe1 O3 H3A 120.4(16) . . ?
Fe1 O3 H3B 123.5(16) . . ?
H3A O3 H3B 108(2) . . ?
H4A O4 H4B 109(2) . . ?
H5A O5 H5B 106(2) . . ?
H6A O6A H6B 116(4) . . ?
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 O1 2.0866(13) 2 ?
Fe1 O1 2.0866(13) . ?
Fe1 O3 2.0912(12) 2 ?
Fe1 O3 2.0912(12) . ?
Fe1 O2 2.1303(13) . ?
Fe1 O2 2.1303(13) 2 ?
S11 C12 1.7169(19) . ?
S11 C11 1.7346(17) . ?
S12 C11 1.6856(18) . ?
S21 C22 1.7163(17) . ?
S21 C21 1.7371(17) . ?
S22 C21 1.6827(17) . ?
S31 C32 1.710(2) . ?
S31 C31 1.7347(18) . ?
S32 C31 1.6738(18) . ?
B1 N31 1.549(2) . ?
B1 N11 1.551(2) . ?
B1 N21 1.559(2) . ?
B1 H1 1.067(17) . ?
C11 N11 1.342(2) . ?
C12 N12 1.290(2) . ?
C12 H12 0.9500 . ?
C21 N21 1.344(2) . ?
C22 N22 1.288(2) . ?
C22 H22 0.9500 . ?
C31 N31 1.341(2) . ?
C32 N32 1.284(2) . ?
C32 H32 0.9500 . ?
N12 N11 1.3816(19) . ?
N22 N21 1.3760(18) . ?
N32 N31 1.3754(19) . ?
O1 H1A 0.786(12) . ?
O1 H1B 0.793(12) . ?
O2 H2A 0.781(12) . ?
O2 H2B 0.777(12) . ?
O3 H3A 0.777(12) . ?
O3 H3B 0.788(12) . ?
O4 H4A 0.786(12) . ?
O4 H4B 0.798(12) . ?
O5 H5A 0.790(12) . ?
O5 H5B 0.788(12) . ?
O6A H6A 0.781(14) . ?
O6A H6B 0.781(14) . ?
O6B H6B 0.72(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2A O5 0.781(12) 2.061(15) 2.7912(19) 156(2) .
O2 H2B O4 0.777(12) 1.987(12) 2.7588(19) 172(2) .
O4 H4B O6A 0.798(12) 1.870(13) 2.655(2) 168(2) .
O4 H4B O6B 0.798(12) 1.896(17) 2.658(9) 160(2) .
O5 H5A N22 0.790(12) 2.119(15) 2.8634(18) 157(2) .
O6A H6A S12 0.781(14) 2.438(16) 3.204(2) 167(3) .
O1 H1A S22 0.786(12) 2.474(13) 3.2545(14) 172(2) 1_554
O4 H4A S22 0.786(12) 2.580(15) 3.3173(14) 157(2) 1_554
O1 H1B S32 0.793(12) 2.339(13) 3.1296(15) 175(2) 2_566
O3 H3A O5 0.777(12) 2.047(15) 2.7445(18) 149(2) 2
O3 H3B O4 0.788(12) 1.929(13) 2.7108(18) 172(2) 2_655
O5 H5B N32 0.788(12) 2.067(13) 2.850(2) 173(2) 2_556
O6A H6A S12 0.781(14) 2.438(16) 3.204(2) 167(3) .
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 S11 C11 N11 -0.92(12) . . . . ?
C12 S11 C11 S12 179.51(12) . . . . ?
C11 S11 C12 N12 0.21(14) . . . . ?
C22 S21 C21 N21 -2.18(12) . . . . ?
C22 S21 C21 S22 179.38(12) . . . . ?
C21 S21 C22 N22 1.50(14) . . . . ?
C32 S31 C31 N31 0.54(13) . . . . ?
C32 S31 C31 S32 -178.98(13) . . . . ?
C31 S31 C32 N32 -0.78(16) . . . . ?
S11 C12 N12 N11 0.55(18) . . . . ?
S12 C11 N11 N12 -178.97(12) . . . . ?
S11 C11 N11 N12 1.47(17) . . . . ?
S12 C11 N11 B1 7.2(2) . . . . ?
S11 C11 N11 B1 -172.34(12) . . . . ?
C12 N12 N11 C11 -1.3(2) . . . . ?
C12 N12 N11 B1 172.75(14) . . . . ?
N31 B1 N11 C11 158.98(14) . . . . ?
N21 B1 N11 C11 -81.68(18) . . . . ?
N31 B1 N11 N12 -14.62(19) . . . . ?
N21 B1 N11 N12 104.71(16) . . . . ?
S21 C22 N22 N21 -0.37(18) . . . . ?
S22 C21 N21 N22 -179.03(11) . . . . ?
S21 C21 N21 N22 2.53(17) . . . . ?
S22 C21 N21 B1 8.0(2) . . . . ?
S21 C21 N21 B1 -170.48(12) . . . . ?
C22 N22 N21 C21 -1.5(2) . . . . ?
C22 N22 N21 B1 171.78(14) . . . . ?
N31 B1 N21 C21 -78.92(19) . . . . ?
N11 B1 N21 C21 162.74(14) . . . . ?
N31 B1 N21 N22 108.38(15) . . . . ?
N11 B1 N21 N22 -10.0(2) . . . . ?
S31 C32 N32 N31 0.8(2) . . . . ?
S32 C31 N31 N32 179.26(12) . . . . ?
S31 C31 N31 N32 -0.25(17) . . . . ?
S32 C31 N31 B1 -1.5(2) . . . . ?
S31 C31 N31 B1 179.03(12) . . . . ?
C32 N32 N31 C31 -0.3(2) . . . . ?
C32 N32 N31 B1 -179.61(16) . . . . ?
N11 B1 N31 C31 -76.74(19) . . . . ?
N21 B1 N31 C31 164.67(14) . . . . ?
N11 B1 N31 N32 102.50(16) . . . . ?
N21 B1 N31 N32 -16.1(2) . . . . ?
