Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_publ_contact_author_name 'Mei Wang'
_publ_contact_author_address
;
DUT-KTH joint Education and Research Centre
Dalian University of Technology
Dalian
116012
CHINA
;
_publ_contact_author_email SYMBUENO@DLUT.EDU.CN
_publ_section_title
;
Protonation, electrochemical properties and molecular
structures of halogen-functionalized diiron azadithiolate complexes
related to the active site of iron-only hydrogenases
;
_publ_contact_author
;Mei Wang
Dalian University of technology,
Zhongshan Road 158-46, 116012 Dalian, P. R. China,
Fax: +86-411-83702185
;
loop_
_publ_author_name
'Mei Wang'
'Weibing Dong'
'Kun Jin'
'Xiaoyang Liu'
'Licheng Sun'
;
Fujun Wang
;
# Copyright The Royal Society of Chemistry, 2007
# CCDC Number: 644460
data_4
_database_code_depnum_ccdc_archive 'CCDC 644460'
#------------------------------------------------------------------------------
_audit_creation_date 'Dec 15 14:01:24 2004'
_audit_creation_method SHELXL-97
_audit_update_record ?
#------------------------------------------------------------------------------
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
#------------------------------------------------------------------------------
_chemical_compound_source ?
_chemical_name_common ?
_chemical_formula_weight 652.09
_chemical_formula_analytical ?
_chemical_formula_sum 'C19 H28 Br Fe2 N O4 P2 S2'
_chemical_formula_moiety 'C19 H28 Br Fe2 N O4 P2 S2'
_chemical_formula_structural ?
_chemical_melting_point ?
#------------------------------------------------------------------------------
_cell_length_a 20.2633(8)
_cell_length_b 10.2848(4)
_cell_length_c 13.4463(5)
_cell_angle_alpha 90.00
_cell_angle_beta 106.989(2)
_cell_angle_gamma 90.00
_cell_volume 2679.97(18)
_cell_formula_units_Z 4
_cell_measurement_temperature 273(2)
_cell_measurement_reflns_used 6023
_cell_measurement_theta_min 2.56
_cell_measurement_theta_max 29.38
#------------------------------------------------------------------------------
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P2(1)/c '
_symmetry_Int_Tables_number ?
_symmetry_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_exptl_crystal_description block
_exptl_crystal_colour red
_exptl_crystal_size_max 0.52
_exptl_crystal_size_mid 0.43
_exptl_crystal_size_min 0.30
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.616
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1320
_exptl_absorpt_coefficient_mu 2.873
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.240
_exptl_absorpt_correction_T_max 0.422
_exptl_absorpt_process_details SADABS
_exptl_special_details
;
?
;
#------------------------------------------------------------------------------
_diffrn_special_details
;
?
;
_diffrn_ambient_temperature 273(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_detector 'Imaging Plate'
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_standards_number none
_diffrn_standards_interval_count none
_diffrn_standards_decay_% none
_diffrn_reflns_number 18897
_reflns_number_total 5805
_reflns_number_gt 4583
_reflns_threshold_expression >2sigma(I)
_diffrn_reflns_av_R_equivalents 0.0303
_diffrn_reflns_av_sigmaI/netI 0.0316
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 2.56
_diffrn_reflns_theta_max 27.00
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 27.00
_diffrn_measured_fraction_theta_full 0.993
#------------------------------------------------------------------------------
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'
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'
P P 0.1023 0.0942 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#------------------------------------------------------------------------------
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 0.224904(16) 1.01191(3) 0.37008(2) 0.03106(10) Uani 1 1 d . . .
Fe2 Fe 0.196968(17) 0.83071(3) 0.48501(2) 0.03168(10) Uani 1 1 d . A .
S1 S 0.29694(3) 0.94125(6) 0.52088(4) 0.03464(14) Uani 1 1 d . . .
S2 S 0.21368(3) 0.80069(6) 0.32892(4) 0.03268(14) Uani 1 1 d . . .
Br1 Br 0.547968(19) 0.78060(4) 0.50492(3) 0.07325(13) Uani 1 1 d . . .
N1 N 0.34244(10) 0.7170(2) 0.44960(15) 0.0366(5) Uani 1 1 d . . .
P1 P 0.21198(4) 1.20184(7) 0.44150(5) 0.04095(17) Uani 1 1 d . . .
P2 P 0.08869(3) 0.76702(8) 0.42147(5) 0.04327(17) Uani 1 1 d . . .
C1 C 0.28762(13) 1.0615(3) 0.31060(18) 0.0384(6) Uani 1 1 d . . .
C2 C 0.15180(14) 1.0485(3) 0.2669(2) 0.0459(6) Uani 1 1 d . . .
C3 C 0.22334(14) 0.6804(3) 0.5496(2) 0.0439(6) Uani 1 1 d . . .
C4 C 0.17276(15) 0.9191(3) 0.5802(2) 0.0463(6) Uani 1 1 d . . .
C5 C 0.36467(12) 0.8431(3) 0.4942(2) 0.0399(6) Uani 1 1 d . . .
H5A H 0.3839 0.8908 0.4470 0.048 Uiso 1 1 calc R . .
H5B H 0.4012 0.8308 0.5587 0.048 Uiso 1 1 calc R . .
C6 C 0.29767(13) 0.7251(3) 0.34446(19) 0.0389(6) Uani 1 1 d . . .
H6A H 0.2901 0.6378 0.3160 0.047 Uiso 1 1 calc R . .
H6B H 0.3213 0.7737 0.3033 0.047 Uiso 1 1 calc R . .
C7 C 0.40158(14) 0.6319(3) 0.4511(2) 0.0478(7) Uani 1 1 d . . .
H7A H 0.4267 0.6694 0.4068 0.057 Uiso 1 1 calc R . .
H7B H 0.3843 0.5477 0.4226 0.057 Uiso 1 1 calc R . .
C8 C 0.45048(13) 0.6131(3) 0.5587(2) 0.0412(6) Uani 1 1 d . . .
C9 C 0.43097(15) 0.5352(3) 0.6292(3) 0.0559(8) Uani 1 1 d . . .
H9A H 0.3873 0.4978 0.6096 0.067 Uiso 1 1 calc R . .
C10 C 0.47437(19) 0.5113(3) 0.7278(3) 0.0656(9) Uani 1 1 d . . .
H10A H 0.4596 0.4596 0.7739 0.079 Uiso 1 1 calc R . .
C11 C 0.53922(16) 0.5641(3) 0.7573(2) 0.0572(8) Uani 1 1 d . . .
H11A H 0.5691 0.5459 0.8228 0.069 Uiso 1 1 calc R . .
C12 C 0.56035(14) 0.6440(3) 0.6903(2) 0.0483(7) Uani 1 1 d . . .
H12A H 0.6040 0.6817 0.7105 0.058 Uiso 1 1 calc R . .
C13 C 0.51566(13) 0.6672(3) 0.5925(2) 0.0415(6) Uani 1 1 d . . .
C14 C 0.0250(4) 0.8722(10) 0.3408(10) 0.099(3) Uani 0.710(18) 1 d PU A 1
H14A H -0.0188 0.8287 0.3207 0.148 Uiso 0.710(18) 1 calc PR A 1
H14B H 0.0381 0.8944 0.2797 0.148 Uiso 0.710(18) 1 calc PR A 1
H14C H 0.0217 0.9499 0.3785 0.148 Uiso 0.710(18) 1 calc PR A 1
C15 C 0.0760(5) 0.6182(10) 0.3420(11) 0.094(3) Uani 0.710(18) 1 d PU A 1
H15A H 0.0277 0.5979 0.3178 0.141 Uiso 0.710(18) 1 calc PR A 1
H15B H 0.1004 0.5474 0.3834 0.141 Uiso 0.710(18) 1 calc PR A 1
H15C H 0.0933 0.6315 0.2836 0.141 Uiso 0.710(18) 1 calc PR A 1
C16 C 0.0475(9) 0.7157(19) 0.5177(13) 0.102(5) Uani 0.710(18) 1 d PU A 1
H16A H 0.0008 0.6902 0.4834 0.153 Uiso 0.710(18) 1 calc PR A 1
H16B H 0.0476 0.7863 0.5644 0.153 Uiso 0.710(18) 1 calc PR A 1
H16C H 0.0722 0.6433 0.5561 0.153 Uiso 0.710(18) 1 calc PR A 1
C14A C 0.0266(9) 0.904(2) 0.405(3) 0.094(6) Uani 0.290(18) 1 d PU A 2
H14D H -0.0196 0.8717 0.3777 0.140 Uiso 0.290(18) 1 calc PR A 2
H14E H 0.0356 0.9664 0.3570 0.140 Uiso 0.290(18) 1 calc PR A 2
H14F H 0.0318 0.9451 0.4707 0.140 Uiso 0.290(18) 1 calc PR A 2
C15A C 0.0613(11) 0.691(3) 0.3007(19) 0.093(6) Uani 0.290(18) 1 d PU A 2
H15D H 0.0130 0.6706 0.2846 0.140 Uiso 0.290(18) 1 calc PR A 2
H15E H 0.0869 0.6118 0.3025 0.140 Uiso 0.290(18) 1 calc PR A 2
H15F H 0.0687 0.7475 0.2483 0.140 Uiso 0.290(18) 1 calc PR A 2
C16A C 0.061(2) 0.668(5) 0.511(4) 0.113(10) Uani 0.290(18) 1 d PU A 2
H16D H 0.0135 0.6425 0.4796 0.170 Uiso 0.290(18) 1 calc PR A 2
H16E H 0.0644 0.7158 0.5732 0.170 Uiso 0.290(18) 1 calc PR A 2
H16F H 0.0891 0.5914 0.5269 0.170 Uiso 0.290(18) 1 calc PR A 2
C17 C 0.2305(2) 1.3412(3) 0.3709(3) 0.0803(12) Uani 1 1 d . . .
H17A H 0.2241 1.4198 0.4055 0.120 Uiso 1 1 calc R . .
H17B H 0.1999 1.3410 0.3013 0.120 Uiso 1 1 calc R . .
H17C H 0.2774 1.3365 0.3687 0.120 Uiso 1 1 calc R . .
C18 C 0.2646(2) 1.2381(3) 0.5727(2) 0.0717(10) Uani 1 1 d . . .
H18A H 0.2531 1.3230 0.5923 0.108 Uiso 1 1 calc R . .
H18B H 0.3124 1.2360 0.5755 0.108 Uiso 1 1 calc R . .
H18C H 0.2560 1.1745 0.6197 0.108 Uiso 1 1 calc R . .
C19 C 0.12564(19) 1.2397(4) 0.4493(3) 0.0753(11) Uani 1 1 d . . .
H19A H 0.1261 1.3232 0.4813 0.113 Uiso 1 1 calc R . .
H19B H 0.1116 1.1746 0.4901 0.113 Uiso 1 1 calc R . .
H19C H 0.0938 1.2411 0.3806 0.113 Uiso 1 1 calc R . .
O1 O 0.32905(10) 1.0894(2) 0.27185(16) 0.0600(6) Uani 1 1 d . . .
O2 O 0.10548(12) 1.0772(3) 0.19698(17) 0.0786(7) Uani 1 1 d . . .
O3 O 0.23951(13) 0.5834(2) 0.59053(17) 0.0710(7) Uani 1 1 d . A .
O4 O 0.15546(14) 0.9766(2) 0.64164(18) 0.0764(7) Uani 1 1 d . A .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.02776(18) 0.0335(2) 0.02935(16) -0.00019(13) 0.00430(13) 0.00282(14)
Fe2 0.03301(19) 0.0335(2) 0.02730(16) -0.00031(13) 0.00683(13) 0.00316(15)
S1 0.0324(3) 0.0340(4) 0.0312(3) -0.0067(2) -0.0007(2) 0.0046(3)
S2 0.0286(3) 0.0386(4) 0.0277(3) -0.0054(2) 0.0033(2) -0.0007(3)
Br1 0.0690(2) 0.0821(3) 0.0722(2) 0.01715(19) 0.02622(18) -0.01218(19)
N1 0.0324(11) 0.0341(12) 0.0391(11) -0.0071(9) 0.0040(8) 0.0053(9)
P1 0.0454(4) 0.0352(4) 0.0425(3) 0.0003(3) 0.0133(3) 0.0083(3)
P2 0.0336(4) 0.0513(5) 0.0456(4) 0.0015(3) 0.0127(3) -0.0006(3)
C1 0.0356(13) 0.0420(16) 0.0336(12) -0.0017(11) 0.0040(10) 0.0027(12)
C2 0.0361(14) 0.0522(18) 0.0452(14) -0.0002(13) 0.0056(11) 0.0062(13)
C3 0.0492(16) 0.0468(18) 0.0347(12) -0.0008(12) 0.0109(11) 0.0064(13)
C4 0.0558(17) 0.0443(17) 0.0410(13) 0.0001(12) 0.0175(12) 0.0000(13)
C5 0.0277(12) 0.0374(16) 0.0470(14) -0.0081(11) -0.0008(10) 0.0052(11)
C6 0.0336(13) 0.0426(16) 0.0381(12) -0.0100(11) 0.0070(10) 0.0051(11)
C7 0.0392(15) 0.0509(18) 0.0490(14) -0.0101(13) 0.0060(12) 0.0129(13)
C8 0.0352(13) 0.0363(15) 0.0503(14) -0.0034(12) 0.0095(11) 0.0104(11)
C9 0.0409(16) 0.051(2) 0.0744(19) 0.0055(15) 0.0156(14) -0.0027(14)
C10 0.066(2) 0.066(2) 0.0670(19) 0.0227(17) 0.0220(17) 0.0064(18)
C11 0.0526(18) 0.062(2) 0.0515(16) 0.0084(15) 0.0064(13) 0.0147(16)
C12 0.0371(15) 0.0514(19) 0.0518(15) -0.0036(13) 0.0056(12) 0.0047(13)
C13 0.0406(14) 0.0376(15) 0.0483(14) 0.0009(12) 0.0163(11) 0.0062(12)
C14 0.047(3) 0.086(6) 0.136(8) 0.031(6) -0.017(5) -0.002(3)
C15 0.062(5) 0.079(6) 0.146(9) -0.059(5) 0.039(5) -0.036(4)
C16 0.065(6) 0.173(15) 0.077(4) 0.024(7) 0.034(4) -0.020(7)
C14A 0.027(6) 0.089(12) 0.153(16) 0.021(13) 0.007(10) 0.015(7)
C15A 0.049(8) 0.137(17) 0.100(13) -0.062(12) 0.032(8) -0.038(11)
C16A 0.064(14) 0.17(2) 0.112(14) 0.057(15) 0.029(11) -0.043(16)
C17 0.127(3) 0.039(2) 0.089(3) 0.0117(18) 0.054(3) 0.011(2)
C18 0.095(3) 0.050(2) 0.0580(19) -0.0181(16) 0.0035(18) 0.0086(19)
C19 0.064(2) 0.069(3) 0.099(3) -0.005(2) 0.035(2) 0.0254(19)
O1 0.0503(12) 0.0783(17) 0.0561(11) 0.0011(11) 0.0226(10) -0.0125(11)
O2 0.0516(13) 0.101(2) 0.0638(13) 0.0124(13) -0.0134(11) 0.0188(13)
O3 0.0992(18) 0.0513(15) 0.0657(13) 0.0232(11) 0.0289(13) 0.0250(13)
O4 0.111(2) 0.0696(16) 0.0660(13) -0.0172(12) 0.0531(14) 0.0040(14)
#------------------------------------------------------------------------------
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
SIMU 0.01 C14 C15 C16 C14a C15a C16a was used to make the anisotropic
displacement parameters similar for the disordered methyl carbon atoms
(closer than 1.7 \%A with each other) on phosphors atoms.
The H atoms attached to C wereplaced in geometrically calculated
positions (C---H = 0.93--0.97 \%A) and refined as riding,
with U~iso~(H) = 1.2U~eq~(C).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.2512P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5805
_refine_ls_number_parameters 308
_refine_ls_number_restraints 18
_refine_ls_R_factor_all 0.0496
_refine_ls_R_factor_gt 0.0343
_refine_ls_wR_factor_ref 0.0859
_refine_ls_wR_factor_gt 0.0813
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_restrained_S_all 1.050
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.639
_refine_diff_density_min -0.896
_refine_diff_density_rms 0.069
#------------------------------------------------------------------------------
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C2 1.749(3) . ?
Fe1 C1 1.763(3) . ?
Fe1 P1 2.2257(8) . ?
Fe1 S2 2.2369(7) . ?
Fe1 S1 2.2451(6) . ?
Fe1 Fe2 2.5870(5) . ?
Fe2 C4 1.753(3) . ?
Fe2 C3 1.777(3) . ?
Fe2 P2 2.2085(8) . ?
Fe2 S2 2.2428(6) . ?
Fe2 S1 2.2489(7) . ?
S1 C5 1.822(2) . ?
S2 C6 1.827(2) . ?
Br1 C13 1.904(3) . ?
N1 C6 1.442(3) . ?
N1 C5 1.445(3) . ?
N1 C7 1.479(3) . ?
P1 C18 1.813(3) . ?
P1 C17 1.818(3) . ?
P1 C19 1.825(3) . ?
P2 C15A 1.74(2) . ?
P2 C14 1.787(8) . ?
P2 C16A 1.79(4) . ?
P2 C16 1.811(16) . ?
P2 C15 1.841(8) . ?
P2 C14A 1.859(19) . ?
C1 O1 1.146(3) . ?
C2 O2 1.156(3) . ?
C3 O3 1.140(3) . ?
C4 O4 1.151(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.508(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C13 1.382(4) . ?
C8 C9 1.385(4) . ?
C9 C10 1.382(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.369(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.377(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(4) . ?
C12 H12A 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C14A H14D 0.9600 . ?
C14A H14E 0.9600 . ?
C14A H14F 0.9600 . ?
C15A H15D 0.9600 . ?
C15A H15E 0.9600 . ?
C15A H15F 0.9600 . ?
C16A H16D 0.9600 . ?
C16A H16E 0.9600 . ?
C16A H16F 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
#------------------------------------------------------------------------------
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
C2 Fe1 C1 97.67(12) . . ?
C2 Fe1 P1 88.51(10) . . ?
C1 Fe1 P1 97.65(9) . . ?
C2 Fe1 S2 90.67(10) . . ?
C1 Fe1 S2 101.73(9) . . ?
P1 Fe1 S2 160.54(3) . . ?
C2 Fe1 S1 164.25(10) . . ?
C1 Fe1 S1 97.97(8) . . ?
P1 Fe1 S1 91.25(3) . . ?
S2 Fe1 S1 84.34(2) . . ?
C2 Fe1 Fe2 110.28(10) . . ?
C1 Fe1 Fe2 142.36(9) . . ?
P1 Fe1 Fe2 107.50(2) . . ?
S2 Fe1 Fe2 54.833(18) . . ?
S1 Fe1 Fe2 54.92(2) . . ?
C4 Fe2 C3 101.72(12) . . ?
C4 Fe2 P2 88.74(10) . . ?
C3 Fe2 P2 93.09(10) . . ?
C4 Fe2 S2 154.91(10) . . ?
C3 Fe2 S2 103.38(8) . . ?
P2 Fe2 S2 90.10(3) . . ?
C4 Fe2 S1 90.44(10) . . ?
C3 Fe2 S1 102.22(10) . . ?
P2 Fe2 S1 164.51(3) . . ?
S2 Fe2 S1 84.11(2) . . ?
C4 Fe2 Fe1 102.65(9) . . ?
C3 Fe2 Fe1 146.25(9) . . ?
P2 Fe2 Fe1 110.40(2) . . ?
S2 Fe2 Fe1 54.618(19) . . ?
S1 Fe2 Fe1 54.786(18) . . ?
C5 S1 Fe1 109.27(8) . . ?
C5 S1 Fe2 111.14(9) . . ?
Fe1 S1 Fe2 70.29(2) . . ?
C6 S2 Fe1 111.17(9) . . ?
C6 S2 Fe2 110.00(8) . . ?
Fe1 S2 Fe2 70.55(2) . . ?
C6 N1 C5 112.7(2) . . ?
C6 N1 C7 108.84(19) . . ?
C5 N1 C7 111.9(2) . . ?
C18 P1 C17 101.14(19) . . ?
C18 P1 C19 101.60(19) . . ?
C17 P1 C19 102.11(19) . . ?
C18 P1 Fe1 119.37(11) . . ?
C17 P1 Fe1 113.49(12) . . ?
C19 P1 Fe1 116.58(13) . . ?
C15A P2 C14 74.3(9) . . ?
C15A P2 C16A 106.8(17) . . ?
C14 P2 C16A 116.0(15) . . ?
C15A P2 C16 116.5(10) . . ?
C14 P2 C16 102.0(6) . . ?
C16A P2 C16 18.6(18) . . ?
C15A P2 C15 29.8(9) . . ?
C14 P2 C15 101.4(4) . . ?
C16A P2 C15 84.0(15) . . ?
C16 P2 C15 99.0(6) . . ?
C15A P2 C14A 102.0(9) . . ?
C14 P2 C14A 28.9(7) . . ?
C16A P2 C14A 100.3(15) . . ?
C16 P2 C14A 82.6(9) . . ?
C15 P2 C14A 125.8(8) . . ?
C15A P2 Fe2 120.3(6) . . ?
C14 P2 Fe2 121.0(3) . . ?
C16A P2 Fe2 112.6(15) . . ?
C16 P2 Fe2 115.1(6) . . ?
C15 P2 Fe2 115.2(3) . . ?
C14A P2 Fe2 112.5(7) . . ?
O1 C1 Fe1 177.7(3) . . ?
O2 C2 Fe1 176.6(3) . . ?
O3 C3 Fe2 179.2(3) . . ?
O4 C4 Fe2 178.6(3) . . ?
N1 C5 S1 114.71(17) . . ?
N1 C5 H5A 108.6 . . ?
S1 C5 H5A 108.6 . . ?
N1 C5 H5B 108.6 . . ?
S1 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N1 C6 S2 115.79(17) . . ?
N1 C6 H6A 108.3 . . ?
S2 C6 H6A 108.3 . . ?
N1 C6 H6B 108.3 . . ?
S2 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
N1 C7 C8 113.0(2) . . ?
N1 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
N1 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C13 C8 C9 116.4(2) . . ?
C13 C8 C7 124.1(3) . . ?
C9 C8 C7 119.5(3) . . ?
C10 C9 C8 122.1(3) . . ?
C10 C9 H9A 119.0 . . ?
C8 C9 H9A 119.0 . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C10 C11 C12 120.2(3) . . ?
C10 C11 H11A 119.9 . . ?
C12 C11 H11A 119.9 . . ?
C11 C12 C13 118.9(3) . . ?
C11 C12 H12A 120.6 . . ?
C13 C12 H12A 120.6 . . ?
C12 C13 C8 122.7(3) . . ?
C12 C13 Br1 116.5(2) . . ?
C8 C13 Br1 120.8(2) . . ?
P2 C14 H14A 109.5 . . ?
P2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
P2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P2 C15 H15A 109.5 . . ?
P2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
P2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P2 C16 H16A 109.5 . . ?
P2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
P2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P2 C14A H14D 109.5 . . ?
P2 C14A H14E 109.5 . . ?
H14D C14A H14E 109.5 . . ?
P2 C14A H14F 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
P2 C15A H15D 109.5 . . ?
P2 C15A H15E 109.5 . . ?
H15D C15A H15E 109.5 . . ?
P2 C15A H15F 109.5 . . ?
H15D C15A H15F 109.5 . . ?
H15E C15A H15F 109.5 . . ?
P2 C16A H16D 109.5 . . ?
P2 C16A H16E 109.5 . . ?
H16D C16A H16E 109.5 . . ?
P2 C16A H16F 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
P1 C17 H17A 109.5 . . ?
P1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P1 C18 H18A 109.5 . . ?
P1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
P1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P1 C19 H19A 109.5 . . ?
P1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
#===END
# Copyright The Royal Society of Chemistry, 2007
# CCDC Number: 644461
data_4FeHFe
_database_code_depnum_ccdc_archive 'CCDC 644461'
#------------------------------------------------------------------------------
_audit_creation_date 'Jan 15 11:01:24 2005'
_audit_creation_method SHELXL-97
_audit_update_record ?
#------------------------------------------------------------------------------
_computing_data_collection 'Bruker XSCANS'
_computing_cell_refinement 'Bruker XSCANS'
_computing_data_reduction 'Bruker SHELXTL'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
#------------------------------------------------------------------------------
_chemical_compound_source ?
_chemical_name_common ?
_chemical_formula_weight 883.00
_chemical_formula_analytical 'C20 H31 Br Cl2 F6 Fe2 N O4 P3 S2'
_chemical_formula_sum 'C20 H31 Br Cl2 F6 Fe2 N O4 P3 S2'
_chemical_formula_moiety 'C19 H29 Br Fe2 N O4 P2 S2 ,PF6, CH2Cl2'
_chemical_formula_structural ?
_chemical_melting_point ?
#------------------------------------------------------------------------------
_cell_length_a 11.621(2)
_cell_length_b 12.590(3)
_cell_length_c 13.505(3)
_cell_angle_alpha 80.32(3)
_cell_angle_beta 65.34(3)
_cell_angle_gamma 76.92(3)
_cell_volume 1743.1(6)
_cell_formula_units_Z 2
_cell_measurement_temperature 273(2)
_cell_measurement_reflns_used 3562
_cell_measurement_theta_min 3.21
_cell_measurement_theta_max 17.50
#------------------------------------------------------------------------------
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M 'P-1 '
_symmetry_Int_Tables_number ?
_symmetry_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_exptl_crystal_description prism
_exptl_crystal_colour red
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.682
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 884
_exptl_absorpt_coefficient_mu 2.448
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6149
_exptl_absorpt_correction_T_max 0.7918
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
#------------------------------------------------------------------------------
_diffrn_special_details
;
?
;
_diffrn_ambient_temperature 273(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_detector 'Imaging Plate'
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_standards_number none
_diffrn_standards_interval_count none
_diffrn_standards_decay_% none
_diffrn_reflns_number 17215
_reflns_number_total 7858
_reflns_number_gt 5720
_reflns_threshold_expression >2sigma(I)
_diffrn_reflns_av_R_equivalents 0.0279
_diffrn_reflns_av_sigmaI/netI 0.0390
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_theta_min 3.03
_diffrn_reflns_theta_max 27.48
_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full 27.48
_diffrn_measured_fraction_theta_full 0.982
#------------------------------------------------------------------------------
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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#------------------------------------------------------------------------------
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 0.34395(5) 0.26107(4) 0.34890(4) 0.04214(13) Uani 1 1 d . B .
Fe2 Fe 0.32034(5) 0.25472(4) 0.16732(3) 0.03905(13) Uani 1 1 d . . .
S1 S 0.49015(8) 0.16492(7) 0.20791(7) 0.04260(19) Uani 1 1 d . . .
S2 S 0.20172(8) 0.17577(7) 0.33114(6) 0.04101(19) Uani 1 1 d . . .
P1 P 0.48678(11) 0.36723(9) 0.32594(9) 0.0616(3) Uani 1 1 d . . .
P2 P 0.13936(10) 0.36544(8) 0.16631(8) 0.0507(2) Uani 1 1 d . . .
P3 P -0.25860(10) -0.31595(9) 0.23408(9) 0.0553(3) Uani 1 1 d . . .
F1 F -0.1799(3) -0.3059(3) 0.3017(3) 0.1084(11) Uani 1 1 d . A .
F2 F -0.3338(3) -0.3245(3) 0.1628(3) 0.1071(11) Uani 1 1 d . A .
F3 F -0.1290(13) -0.3556(16) 0.1465(13) 0.122(6) Uani 0.60(3) 1 d P A 1
F4 F -0.2650(16) -0.4356(12) 0.2898(18) 0.134(6) Uani 0.60(3) 1 d P A 1
F5 F -0.260(2) -0.1956(12) 0.1878(14) 0.126(6) Uani 0.60(3) 1 d P A 1
F6 F -0.3901(9) -0.2768(16) 0.3297(8) 0.117(5) Uani 0.60(3) 1 d P A 1
F3' F -0.136(3) -0.303(3) 0.1196(18) 0.138(10) Uani 0.40(3) 1 d P A 2
F4' F -0.214(3) -0.4421(14) 0.221(3) 0.129(9) Uani 0.40(3) 1 d P A 2
F5' F -0.300(3) -0.1947(15) 0.238(3) 0.142(12) Uani 0.40(3) 1 d P A 2
F6' F -0.373(3) -0.335(3) 0.3325(15) 0.188(11) Uani 0.40(3) 1 d P A 2
Br1 Br 0.16395(7) -0.24441(5) 0.44749(5) 0.1057(2) Uani 1 1 d . . .
N1 N 0.3695(3) -0.0121(2) 0.2441(2) 0.0414(6) Uani 1 1 d . . .
O3 O 0.4811(3) 0.3840(3) -0.0179(2) 0.0768(9) Uani 1 1 d . . .
O4 O 0.3172(4) 0.1053(2) 0.0256(2) 0.0808(10) Uani 1 1 d . . .
O1 O 0.1361(3) 0.4079(3) 0.5006(2) 0.0769(9) Uani 1 1 d . B .
O2 O 0.3996(4) 0.1103(3) 0.5172(3) 0.0960(12) Uani 1 1 d . B .
C3 C 0.4189(4) 0.3337(3) 0.0544(3) 0.0530(9) Uani 1 1 d . . .
C4 C 0.3178(4) 0.1612(3) 0.0827(3) 0.0518(9) Uani 1 1 d . . .
C1 C 0.2176(4) 0.3506(3) 0.4417(3) 0.0530(9) Uani 1 1 d . . .
C2 C 0.3776(4) 0.1710(3) 0.4523(3) 0.0602(10) Uani 1 1 d . . .
C5 C 0.4837(3) 0.0192(3) 0.2410(3) 0.0455(8) Uani 1 1 d . . .
H5A H 0.5601 -0.0222 0.1862 0.055 Uiso 1 1 calc R . .
H5B H 0.4888 -0.0027 0.3132 0.055 Uiso 1 1 calc R . .
C6 C 0.2541(3) 0.0283(3) 0.3356(3) 0.0449(8) Uani 1 1 d . . .
H6A H 0.2688 0.0038 0.4036 0.054 Uiso 1 1 calc R . .
H6B H 0.1833 -0.0061 0.3400 0.054 Uiso 1 1 calc R . .
C7 C 0.3891(4) -0.1334(3) 0.2484(3) 0.0511(9) Uani 1 1 d . . .
H7A H 0.3821 -0.1648 0.3226 0.061 Uiso 1 1 calc R . .
H7B H 0.4768 -0.1608 0.1960 0.061 Uiso 1 1 calc R . .
C8 C 0.2925(3) -0.1710(3) 0.2215(3) 0.0507(9) Uani 1 1 d . . .
C9 C 0.3037(4) -0.1558(3) 0.1139(3) 0.0630(10) Uani 1 1 d . . .
H9A H 0.3693 -0.1189 0.0609 0.076 Uiso 1 1 calc R . .
C10 C 0.2234(5) -0.1921(4) 0.0815(5) 0.0845(15) Uani 1 1 d . . .
H10A H 0.2340 -0.1814 0.0071 0.101 Uiso 1 1 calc R . .
C11 C 0.1270(5) -0.2445(5) 0.1583(6) 0.0943(18) Uani 1 1 d . . .
H11A H 0.0709 -0.2699 0.1363 0.113 Uiso 1 1 calc R . .
C12 C 0.1112(5) -0.2602(4) 0.2649(5) 0.0874(17) Uani 1 1 d . . .
H12A H 0.0442 -0.2961 0.3173 0.105 Uiso 1 1 calc R . .
C13 C 0.1934(4) -0.2235(3) 0.2962(4) 0.0661(11) Uani 1 1 d . . .
C14 C 0.0423(5) 0.4336(4) 0.2902(3) 0.0793(14) Uani 1 1 d . . .
H14A H -0.0342 0.4799 0.2828 0.119 Uiso 1 1 calc R . .
H14B H 0.0926 0.4790 0.3025 0.119 Uiso 1 1 calc R . .
H14C H 0.0160 0.3787 0.3523 0.119 Uiso 1 1 calc R . .
C15 C 0.0293(5) 0.2984(5) 0.1466(5) 0.0892(15) Uani 1 1 d . . .
H15A H -0.0466 0.3521 0.1472 0.134 Uiso 1 1 calc R . .
H15B H 0.0029 0.2407 0.2057 0.134 Uiso 1 1 calc R . .
H15C H 0.0720 0.2661 0.0762 0.134 Uiso 1 1 calc R . .
C16 C 0.1620(5) 0.4776(4) 0.0615(3) 0.0720(12) Uani 1 1 d . . .
H16A H 0.0781 0.5209 0.0678 0.108 Uiso 1 1 calc R . .
H16B H 0.2064 0.4489 -0.0106 0.108 Uiso 1 1 calc R . .
H16C H 0.2137 0.5241 0.0703 0.108 Uiso 1 1 calc R . .
C17 C 0.4171(12) 0.4893(12) 0.3963(16) 0.110(5) Uani 0.60(2) 1 d PU B 1
H17A H 0.4845 0.5314 0.3823 0.166 Uiso 0.60(2) 1 calc PR B 1
H17B H 0.3758 0.4698 0.4750 0.166 Uiso 0.60(2) 1 calc PR B 1
H17C H 0.3528 0.5336 0.3700 0.166 Uiso 0.60(2) 1 calc PR B 1
C17' C 0.4181(17) 0.5188(11) 0.312(3) 0.112(7) Uani 0.40(2) 1 d PU B 2
H17D H 0.4831 0.5623 0.3014 0.168 Uiso 0.40(2) 1 calc PR B 2
H17E H 0.3420 0.5380 0.3785 0.168 Uiso 0.40(2) 1 calc PR B 2
H17F H 0.3940 0.5341 0.2489 0.168 Uiso 0.40(2) 1 calc PR B 2
C18 C 0.5871(8) 0.3188(9) 0.4010(6) 0.171(4) Uani 1 1 d . B .
H18A H 0.6455 0.3701 0.3858 0.257 Uiso 1 1 calc R . .
H18B H 0.6373 0.2467 0.3787 0.257 Uiso 1 1 calc R . .
H18C H 0.5332 0.3130 0.4794 0.257 Uiso 1 1 calc R . .
C19 C 0.6052(6) 0.3880(5) 0.1913(4) 0.108(2) Uani 1 1 d . B .
H19A H 0.6609 0.4354 0.1922 0.162 Uiso 1 1 calc R . .
H19B H 0.5626 0.4226 0.1419 0.162 Uiso 1 1 calc R . .
H19C H 0.6570 0.3173 0.1659 0.162 Uiso 1 1 calc R . .
C20 C 0.8722(11) -0.0186(7) 0.2527(7) 0.160(3) Uani 0.50 1 d P C 1
H20A H 0.9177 -0.0952 0.2438 0.192 Uiso 0.50 1 calc PR C 1
H20B H 0.7791 -0.0209 0.2827 0.192 Uiso 0.50 1 calc PR C 1
Cl1 Cl 0.9095(8) 0.0451(6) 0.1286(5) 0.179(3) Uani 0.50 1 d P C 1
C20A C 0.8722(11) -0.0186(7) 0.2527(7) 0.160(3) Uani 0.50 1 d P C 2
H20C H 0.9546 -0.0537 0.1985 0.192 Uiso 0.50 1 calc PR C 2
H20D H 0.8162 -0.0745 0.2867 0.192 Uiso 0.50 1 calc PR C 2
Cl1' Cl 0.8071(7) 0.0754(4) 0.1935(7) 0.181(3) Uani 0.50 1 d P C 2
Cl2 Cl 0.9007(3) 0.0267(2) 0.35084(19) 0.1742(10) Uani 1 1 d . . .
H1 H 0.315(4) 0.371(3) 0.240(3) 0.062(11) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0492(3) 0.0375(3) 0.0395(3) -0.00701(18) -0.0173(2) -0.0047(2)
Fe2 0.0412(3) 0.0348(2) 0.0362(2) -0.00508(17) -0.01128(19) -0.00349(19)
S1 0.0369(4) 0.0402(4) 0.0486(5) -0.0079(3) -0.0134(4) -0.0065(3)
S2 0.0380(4) 0.0377(4) 0.0401(4) -0.0061(3) -0.0093(3) -0.0027(3)
P1 0.0619(7) 0.0581(6) 0.0716(7) -0.0224(5) -0.0244(5) -0.0148(5)
P2 0.0510(6) 0.0462(5) 0.0491(5) -0.0033(4) -0.0202(4) 0.0028(4)
P3 0.0533(6) 0.0536(6) 0.0674(6) -0.0111(5) -0.0340(5) -0.0011(5)
F1 0.117(3) 0.129(3) 0.125(2) -0.007(2) -0.092(2) -0.023(2)
F2 0.103(2) 0.118(3) 0.140(3) -0.057(2) -0.088(2) 0.0173(19)
F3 0.061(5) 0.181(14) 0.105(9) -0.054(8) -0.019(6) 0.024(8)
F4 0.130(10) 0.077(7) 0.218(13) 0.048(8) -0.103(10) -0.042(7)
F5 0.176(13) 0.080(8) 0.164(10) 0.051(8) -0.118(10) -0.046(9)
F6 0.068(5) 0.190(12) 0.086(5) -0.054(6) -0.032(4) 0.027(6)
F3' 0.095(14) 0.23(3) 0.081(8) 0.003(12) -0.015(7) -0.074(16)
F4' 0.161(19) 0.048(7) 0.24(2) -0.043(12) -0.148(19) 0.022(9)
F5' 0.20(2) 0.057(10) 0.24(3) -0.070(14) -0.16(2) 0.041(12)
F6' 0.163(19) 0.21(2) 0.122(11) 0.010(12) 0.037(11) -0.111(18)
Br1 0.1236(5) 0.0829(4) 0.0768(4) 0.0104(3) -0.0063(3) -0.0313(3)
N1 0.0358(15) 0.0340(14) 0.0511(16) -0.0084(11) -0.0134(12) -0.0039(11)
O3 0.079(2) 0.0697(19) 0.0623(18) 0.0178(15) -0.0106(15) -0.0266(17)
O4 0.132(3) 0.0619(18) 0.0647(18) -0.0162(14) -0.0528(19) -0.0113(19)
O1 0.081(2) 0.080(2) 0.0558(17) -0.0288(15) -0.0179(15) 0.0118(17)
O2 0.152(4) 0.070(2) 0.079(2) -0.0023(17) -0.073(2) 0.009(2)
C3 0.056(2) 0.046(2) 0.051(2) -0.0045(16) -0.0187(18) -0.0028(18)
C4 0.063(2) 0.047(2) 0.0440(19) -0.0011(15) -0.0218(17) -0.0065(18)
C1 0.063(2) 0.052(2) 0.046(2) -0.0076(16) -0.0227(18) -0.0085(19)
C2 0.082(3) 0.050(2) 0.055(2) -0.0104(17) -0.036(2) -0.003(2)
C5 0.0409(19) 0.0405(18) 0.056(2) -0.0083(14) -0.0206(16) -0.0032(15)
C6 0.0432(19) 0.0374(17) 0.0476(18) -0.0048(13) -0.0119(15) -0.0058(15)
C7 0.049(2) 0.0355(18) 0.068(2) -0.0079(15) -0.0231(18) -0.0013(15)
C8 0.045(2) 0.0323(17) 0.066(2) -0.0142(15) -0.0114(17) -0.0026(15)
C9 0.057(2) 0.058(2) 0.068(3) -0.0222(19) -0.014(2) -0.008(2)
C10 0.080(3) 0.091(4) 0.092(4) -0.037(3) -0.035(3) -0.009(3)
C11 0.074(4) 0.083(4) 0.143(5) -0.052(4) -0.045(4) -0.011(3)
C12 0.060(3) 0.061(3) 0.128(5) -0.029(3) -0.009(3) -0.025(2)
C13 0.056(2) 0.042(2) 0.085(3) -0.0142(19) -0.009(2) -0.0093(19)
C14 0.073(3) 0.083(3) 0.056(2) -0.014(2) -0.019(2) 0.032(2)
C15 0.069(3) 0.088(4) 0.126(4) -0.008(3) -0.055(3) -0.009(3)
C16 0.085(3) 0.057(2) 0.062(2) 0.0019(19) -0.030(2) 0.007(2)
C17 0.101(7) 0.084(8) 0.145(11) -0.056(8) -0.019(8) -0.039(6)
C17' 0.088(9) 0.045(7) 0.173(16) -0.024(9) -0.011(12) -0.022(6)
C18 0.166(8) 0.292(12) 0.121(6) 0.063(6) -0.096(6) -0.147(8)
C19 0.145(5) 0.128(5) 0.073(3) 0.010(3) -0.033(3) -0.100(5)
C20 0.238(11) 0.102(6) 0.156(7) -0.022(5) -0.094(8) -0.019(6)
Cl1 0.242(8) 0.168(5) 0.133(4) -0.005(3) -0.095(5) -0.009(5)
C20A 0.238(11) 0.102(6) 0.156(7) -0.022(5) -0.094(8) -0.019(6)
Cl1' 0.213(6) 0.107(3) 0.303(9) -0.009(4) -0.201(7) 0.009(4)
Cl2 0.199(3) 0.215(3) 0.1249(16) -0.0273(16) -0.0547(16) -0.076(2)
#------------------------------------------------------------------------------
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
SIMU 0.01 C14 C15 C16 and SIMU 0.01 C17 C17' C18 C19 were used to make the
anisotropic displacement parameters similar for carbon atoms C14, C15, C16
and C17, C18, C19 (closer than 1.7 \%A with each other) on phosphors atoms.
The H atoms attached to C were placed in geometrically calculated
positions (C---H = 0.93--0.97 \%A) and refined as riding,
with U~iso~(H) = 1.2U~eq~(C).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+1.6851P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7858
_refine_ls_number_parameters 430
_refine_ls_number_restraints 6
_refine_ls_R_factor_all 0.0693
_refine_ls_R_factor_gt 0.0456
_refine_ls_wR_factor_ref 0.1163
_refine_ls_wR_factor_gt 0.1046
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_restrained_S_all 1.034
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.740
_refine_diff_density_min -0.677
_refine_diff_density_rms 0.069
#------------------------------------------------------------------------------
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C2 1.764(4) . ?
Fe1 C1 1.786(4) . ?
Fe1 P1 2.2524(13) . ?
Fe1 S1 2.2632(14) . ?
Fe1 S2 2.2723(11) . ?
Fe1 Fe2 2.5948(8) . ?
Fe1 H1 1.93(4) . ?
Fe2 C3 1.782(4) . ?
Fe2 C4 1.786(4) . ?
Fe2 P2 2.2489(13) . ?
Fe2 S2 2.2623(13) . ?
Fe2 S1 2.2711(12) . ?
Fe2 H1 1.86(4) . ?
S1 C5 1.825(3) . ?
S2 C6 1.818(3) . ?
P1 C19 1.784(5) . ?
P1 C17 1.791(10) . ?
P1 C18 1.792(7) . ?
P1 C17' 1.905(16) . ?
P2 C16 1.804(4) . ?
P2 C15 1.808(5) . ?
P2 C14 1.810(4) . ?
P3 F6' 1.466(16) . ?
P3 F5' 1.496(17) . ?
P3 F3 1.513(12) . ?
P3 F5 1.538(12) . ?
P3 F4 1.570(11) . ?
P3 F4' 1.572(14) . ?
P3 F6 1.572(9) . ?
P3 F1 1.573(3) . ?
P3 F2 1.575(3) . ?
P3 F3' 1.62(2) . ?
Br1 C13 1.907(5) . ?
N1 C5 1.449(4) . ?
N1 C6 1.450(4) . ?
N1 C7 1.487(4) . ?
O3 C3 1.134(4) . ?
O4 C4 1.131(4) . ?
O1 C1 1.142(4) . ?
O2 C2 1.136(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.502(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.387(6) . ?
C8 C13 1.391(5) . ?
C9 C10 1.368(6) . ?
C9 H9A 0.9500 . ?
C10 C11 1.378(8) . ?
C10 H10A 0.9500 . ?
C11 C12 1.358(8) . ?
C11 H11A 0.9500 . ?
C12 C13 1.382(7) . ?
C12 H12A 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17' H17D 0.9800 . ?
C17' H17E 0.9800 . ?
C17' H17F 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 Cl1 1.655(10) . ?
C20 Cl2 1.702(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
#------------------------------------------------------------------------------
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
C2 Fe1 C1 94.57(18) . . ?
C2 Fe1 P1 94.58(15) . . ?
C1 Fe1 P1 90.85(13) . . ?
C2 Fe1 S1 95.85(14) . . ?
C1 Fe1 S1 169.34(12) . . ?
P1 Fe1 S1 90.58(5) . . ?
C2 Fe1 S2 99.24(15) . . ?
C1 Fe1 S2 91.94(13) . . ?
P1 Fe1 S2 165.63(4) . . ?
S1 Fe1 S2 84.15(4) . . ?
C2 Fe1 Fe2 139.67(12) . . ?
C1 Fe1 Fe2 114.57(12) . . ?
P1 Fe1 Fe2 111.32(5) . . ?
S1 Fe1 Fe2 55.23(3) . . ?
S2 Fe1 Fe2 54.92(3) . . ?
C2 Fe1 H1 174.0(11) . . ?
C1 Fe1 H1 83.4(11) . . ?
P1 Fe1 H1 79.8(11) . . ?
S1 Fe1 H1 86.5(11) . . ?
S2 Fe1 H1 86.5(11) . . ?
Fe2 Fe1 H1 45.8(11) . . ?
C3 Fe2 C4 93.45(17) . . ?
C3 Fe2 P2 92.02(13) . . ?
C4 Fe2 P2 93.94(13) . . ?
C3 Fe2 S2 168.47(13) . . ?
C4 Fe2 S2 97.97(12) . . ?
P2 Fe2 S2 88.78(5) . . ?
C3 Fe2 S1 92.29(13) . . ?
C4 Fe2 S1 100.08(13) . . ?
P2 Fe2 S1 165.06(4) . . ?
S2 Fe2 S1 84.20(4) . . ?
C3 Fe2 Fe1 113.94(13) . . ?
C4 Fe2 Fe1 141.76(12) . . ?
P2 Fe2 Fe1 110.36(4) . . ?
S2 Fe2 Fe1 55.28(3) . . ?
S1 Fe2 Fe1 54.95(4) . . ?
C3 Fe2 H1 80.5(11) . . ?
C4 Fe2 H1 170.2(12) . . ?
P2 Fe2 H1 78.8(12) . . ?
S2 Fe2 H1 88.4(11) . . ?
S1 Fe2 H1 87.9(12) . . ?
Fe1 Fe2 H1 47.9(11) . . ?
C5 S1 Fe1 110.26(12) . . ?
C5 S1 Fe2 110.73(12) . . ?
Fe1 S1 Fe2 69.82(4) . . ?
C6 S2 Fe2 110.04(11) . . ?
C6 S2 Fe1 111.02(12) . . ?
Fe2 S2 Fe1 69.81(4) . . ?
C19 P1 C17 113.6(6) . . ?
C19 P1 C18 100.6(3) . . ?
C17 P1 C18 92.1(7) . . ?
C19 P1 C17' 86.7(8) . . ?
C17 P1 C17' 35.5(7) . . ?
C18 P1 C17' 121.0(10) . . ?
C19 P1 Fe1 117.44(17) . . ?
C17 P1 Fe1 114.1(4) . . ?
C18 P1 Fe1 115.5(3) . . ?
C17' P1 Fe1 111.8(6) . . ?
C16 P2 C15 103.2(3) . . ?
C16 P2 C14 102.7(2) . . ?
C15 P2 C14 104.2(3) . . ?
C16 P2 Fe2 115.60(17) . . ?
C15 P2 Fe2 114.65(18) . . ?
C14 P2 Fe2 114.84(16) . . ?
F6' P3 F5' 91.2(13) . . ?
F6' P3 F3 151.8(13) . . ?
F5' P3 F3 116.6(13) . . ?
F6' P3 F5 114.3(13) . . ?
F5' P3 F5 24.4(14) . . ?
F3 P3 F5 93.9(9) . . ?
F6' P3 F4 61.6(12) . . ?
F5' P3 F4 151.2(12) . . ?
F3 P3 F4 90.2(7) . . ?
F5 P3 F4 175.7(8) . . ?
F6' P3 F4' 91.5(11) . . ?
F5' P3 F4' 175.8(11) . . ?
F3 P3 F4' 61.0(11) . . ?
F5 P3 F4' 151.9(11) . . ?
F4 P3 F4' 32.4(8) . . ?
F6' P3 F6 26.9(12) . . ?
F5' P3 F6 64.4(13) . . ?
F3 P3 F6 177.0(7) . . ?
F5 P3 F6 87.5(7) . . ?
F4 P3 F6 88.4(7) . . ?
F4' P3 F6 118.2(11) . . ?
F6' P3 F1 93.1(10) . . ?
F5' P3 F1 85.7(10) . . ?
F3 P3 F1 85.3(7) . . ?
F5 P3 F1 92.5(7) . . ?
F4 P3 F1 86.3(7) . . ?
F4' P3 F1 97.3(7) . . ?
F6 P3 F1 91.9(3) . . ?
F6' P3 F2 88.8(10) . . ?
F5' P3 F2 93.9(10) . . ?
F3 P3 F2 93.2(7) . . ?
F5 P3 F2 86.4(7) . . ?
F4 P3 F2 94.9(7) . . ?
F4' P3 F2 83.0(7) . . ?
F6 P3 F2 89.5(3) . . ?
F1 P3 F2 178.1(2) . . ?
F6' P3 F3' 174.5(14) . . ?
F5' P3 F3' 92.2(14) . . ?
F3 P3 F3' 25.8(11) . . ?
F5 P3 F3' 68.6(12) . . ?
F4 P3 F3' 115.6(10) . . ?
F4' P3 F3' 84.8(11) . . ?
F6 P3 F3' 156.0(11) . . ?
F1 P3 F3' 91.4(10) . . ?
F2 P3 F3' 86.7(10) . . ?
C5 N1 C6 112.7(3) . . ?
C5 N1 C7 108.8(3) . . ?
C6 N1 C7 110.3(3) . . ?
O3 C3 Fe2 179.5(4) . . ?
O4 C4 Fe2 177.1(3) . . ?
O1 C1 Fe1 179.4(4) . . ?
O2 C2 Fe1 177.9(4) . . ?
N1 C5 S1 114.7(2) . . ?
N1 C5 H5A 108.6 . . ?
S1 C5 H5A 108.6 . . ?
N1 C5 H5B 108.6 . . ?
S1 C5 H5B 108.6 . . ?
H5A C5 H5B 107.6 . . ?
N1 C6 S2 115.9(2) . . ?
N1 C6 H6A 108.3 . . ?
S2 C6 H6A 108.3 . . ?
N1 C6 H6B 108.3 . . ?
S2 C6 H6B 108.3 . . ?
H6A C6 H6B 107.4 . . ?
N1 C7 C8 112.0(3) . . ?
N1 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N1 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 C13 116.6(4) . . ?
C9 C8 C7 118.5(3) . . ?
C13 C8 C7 124.8(4) . . ?
C10 C9 C8 122.3(4) . . ?
C10 C9 H9A 118.9 . . ?
C8 C9 H9A 118.9 . . ?
C9 C10 C11 119.1(5) . . ?
C9 C10 H10A 120.4 . . ?
C11 C10 H10A 120.4 . . ?
C12 C11 C10 120.9(5) . . ?
C12 C11 H11A 119.6 . . ?
C10 C11 H11A 119.6 . . ?
C11 C12 C13 119.3(5) . . ?
C11 C12 H12A 120.3 . . ?
C13 C12 H12A 120.3 . . ?
C12 C13 C8 121.8(5) . . ?
C12 C13 Br1 117.5(4) . . ?
C8 C13 Br1 120.7(3) . . ?
P2 C14 H14A 109.5 . . ?
P2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
P2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
P2 C15 H15A 109.5 . . ?
P2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
P2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P2 C16 H16A 109.5 . . ?
P2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
P2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P1 C17 H17A 109.5 . . ?
P1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P1 C17' H17D 109.5 . . ?
P1 C17' H17E 109.5 . . ?
H17D C17' H17E 109.5 . . ?
P1 C17' H17F 109.5 . . ?
H17D C17' H17F 109.5 . . ?
H17E C17' H17F 109.5 . . ?
P1 C18 H18A 109.5 . . ?
P1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
P1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P1 C19 H19A 109.5 . . ?
P1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Cl1 C20 Cl2 121.6(6) . . ?
Cl1 C20 H20A 106.9 . . ?
Cl2 C20 H20A 106.9 . . ?
Cl1 C20 H20B 106.9 . . ?
Cl2 C20 H20B 106.9 . . ?
H20A C20 H20B 106.7 . . ?
#===END
data_1
_database_code_depnum_ccdc_archive 'CCDC 651097'
#------------------------------------------------------------------------------
_audit_creation_date 'Jul 10 10:01:24 2004'
_audit_creation_method SHELXL-97
_audit_update_record ?
#------------------------------------------------------------------------------
_computing_data_collection 'SMART (Bruker, 1997)'
_computing_cell_refinement 'SMART (Bruker, 1997)'
_computing_data_reduction 'SAINT (Bruker, 1997)'
_computing_structure_solution 'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)'
_computing_molecular_graphics 'SHELXP97 (Sheldrick, 1997)'
_computing_publication_material 'SHELXTL (Bruker, 1997)'
#------------------------------------------------------------------------------
_chemical_compound_source ?
_chemical_name_common ?
_chemical_formula_weight 555.97
_chemical_formula_analytical ?
_chemical_formula_sum 'C15 H10 Br Fe2 N O6 S2'
_chemical_formula_moiety 'C15 H10 Br Fe2 N O6 S2'
_chemical_formula_structural ?
_chemical_melting_point ?
#------------------------------------------------------------------------------
_cell_length_a 13.3549(9)
_cell_length_b 14.8313(10)
_cell_length_c 19.7845(11)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 3918.7(4)
_cell_formula_units_Z 8
_cell_measurement_temperature 273(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
#------------------------------------------------------------------------------
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'Pbca '
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'
_exptl_crystal_description block
_exptl_crystal_colour 'black red'
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.885
_exptl_crystal_F_000 2192
_exptl_absorpt_coefficient_mu 3.764
_exptl_absorpt_correction_type empirical
_exptl_absorpt_correction_T_min 0.7281
_exptl_absorpt_correction_T_max 0.8341
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
#------------------------------------------------------------------------------
_diffrn_special_details
;
?
;
_diffrn_ambient_temperature 273(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker CCD area-detector'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 27109
_reflns_number_total 4888
_reflns_number_gt 1801
_reflns_threshold_expression >2sigma(I)
_diffrn_reflns_av_R_equivalents 0.1567
_diffrn_reflns_av_sigmaI/netI 0.1484
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 2.06
_diffrn_reflns_theta_max 28.39
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full 28.39
_diffrn_measured_fraction_theta_full 0.995
#------------------------------------------------------------------------------
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'
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'
Br Br -0.2901 2.4595 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#------------------------------------------------------------------------------
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 0.13622(5) 0.11229(4) 0.58564(3) 0.0422(2) Uani 1 1 d . . .
Fe2 Fe 0.31957(5) 0.06864(4) 0.58780(3) 0.0426(2) Uani 1 1 d . . .
S1 S 0.19157(10) -0.03126(7) 0.58696(6) 0.0452(3) Uani 1 1 d . . .
S2 S 0.23902(10) 0.13301(8) 0.67538(6) 0.0442(3) Uani 1 1 d . . .
Br1 Br 0.47761(5) -0.24339(4) 0.77392(3) 0.0694(2) Uani 1 1 d . . .
O1 O 0.1223(3) 0.3080(2) 0.56783(19) 0.0869(14) Uani 1 1 d . . .
O2 O 0.0813(3) 0.0824(3) 0.44299(19) 0.0881(15) Uani 1 1 d . . .
O3 O -0.0566(3) 0.0813(3) 0.6534(2) 0.0822(14) Uani 1 1 d . . .
O4 O 0.3662(4) -0.0042(3) 0.4544(2) 0.1068(18) Uani 1 1 d . . .
O5 O 0.4898(3) -0.0068(3) 0.6623(2) 0.0831(14) Uani 1 1 d . . .
O6 O 0.4072(3) 0.2446(3) 0.55430(17) 0.0751(12) Uani 1 1 d . . .
N1 N 0.2244(4) -0.0442(3) 0.7258(2) 0.0603(13) Uani 1 1 d . . .
C1 C 0.1297(4) 0.2313(4) 0.5746(2) 0.0554(15) Uani 1 1 d . . .
C2 C 0.1025(4) 0.0937(3) 0.4983(3) 0.0570(16) Uani 1 1 d . . .
C3 C 0.0189(4) 0.0949(3) 0.6268(3) 0.0511(14) Uani 1 1 d . . .
C4 C 0.3478(4) 0.0261(3) 0.5058(3) 0.0637(17) Uani 1 1 d . . .
C5 C 0.4234(5) 0.0200(4) 0.6326(3) 0.0580(16) Uani 1 1 d . . .
C6 C 0.3728(4) 0.1767(4) 0.5679(2) 0.0492(14) Uani 1 1 d . . .
C7 C 0.3540(4) -0.2320(3) 0.8212(2) 0.0442(13) Uani 1 1 d . . .
C8 C 0.2866(4) -0.1647(3) 0.8029(2) 0.0400(13) Uani 1 1 d . . .
C9 C 0.1967(4) -0.1622(3) 0.8383(2) 0.0561(16) Uani 1 1 d . . .
H9 H 0.1490 -0.1191 0.8269 0.080 Uiso 1 1 calc . . .
C10 C 0.1766(4) -0.2224(4) 0.8899(2) 0.0563(15) Uani 1 1 d . . .
H10 H 0.1165 -0.2187 0.9135 0.080 Uiso 1 1 calc . . .
C11 C 0.2436(5) -0.2862(4) 0.9062(3) 0.0679(18) Uani 1 1 d . . .
H11 H 0.2293 -0.3270 0.9405 0.080 Uiso 1 1 calc . . .
C12 C 0.3338(5) -0.2915(3) 0.8723(3) 0.0591(16) Uani 1 1 d . . .
H12 H 0.3805 -0.3353 0.8841 0.080 Uiso 1 1 calc . . .
C13 C 0.3118(5) -0.0953(3) 0.7484(2) 0.0583(15) Uani 1 1 d . . .
H13A H 0.3614 -0.0537 0.7660 0.080 Uiso 1 1 calc . . .
H13B H 0.3411 -0.1260 0.7099 0.080 Uiso 1 1 calc . . .
C14 C 0.1662(4) -0.0796(3) 0.6722(3) 0.0561(15) Uani 1 1 d . . .
H14A H 0.0961 -0.0701 0.6827 0.080 Uiso 1 1 calc . . .
H14B H 0.1773 -0.1442 0.6701 0.080 Uiso 1 1 calc . . .
C15 C 0.2114(4) 0.0482(3) 0.7425(2) 0.0574(16) Uani 1 1 d . . .
H15A H 0.2538 0.0615 0.7811 0.080 Uiso 1 1 calc . . .
H15B H 0.1426 0.0567 0.7568 0.080 Uiso 1 1 calc . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0407(5) 0.0366(4) 0.0494(5) 0.0003(3) -0.0019(4) -0.0021(4)
Fe2 0.0398(5) 0.0392(4) 0.0487(4) -0.0054(4) 0.0075(4) -0.0011(4)
S1 0.0514(10) 0.0348(7) 0.0493(8) -0.0040(6) 0.0000(7) -0.0032(6)
S2 0.0462(10) 0.0397(8) 0.0466(8) -0.0067(6) 0.0018(6) -0.0009(7)
Br1 0.0486(4) 0.0729(4) 0.0867(4) -0.0154(3) -0.0019(3) 0.0029(3)
O1 0.106(4) 0.041(2) 0.114(4) 0.006(2) 0.003(3) 0.002(3)
O2 0.116(4) 0.092(3) 0.056(3) 0.002(2) -0.027(3) -0.022(3)
O3 0.054(3) 0.081(3) 0.112(4) 0.000(2) 0.024(3) 0.001(3)
O4 0.163(5) 0.083(3) 0.074(3) -0.028(2) 0.051(3) -0.010(3)
O5 0.049(3) 0.096(3) 0.104(4) 0.036(2) 0.002(2) 0.009(3)
O6 0.097(4) 0.056(3) 0.073(3) 0.003(2) -0.008(2) -0.028(2)
N1 0.076(4) 0.047(3) 0.058(3) 0.010(2) -0.013(3) 0.003(3)
C1 0.053(4) 0.057(4) 0.055(4) 0.002(3) -0.007(3) -0.003(3)
C2 0.060(4) 0.041(3) 0.070(4) 0.005(3) -0.006(3) -0.010(3)
C3 0.046(4) 0.038(3) 0.068(4) 0.001(3) -0.009(3) 0.002(3)
C4 0.064(5) 0.053(4) 0.075(5) -0.003(3) 0.014(3) -0.007(3)
C5 0.054(5) 0.061(4) 0.059(4) 0.016(3) 0.016(3) 0.003(3)
C6 0.056(4) 0.055(4) 0.036(3) -0.006(3) -0.003(3) 0.002(3)
C7 0.046(4) 0.044(3) 0.043(3) -0.008(3) -0.009(2) -0.005(3)
C8 0.047(4) 0.040(3) 0.034(3) -0.005(2) -0.002(2) -0.001(3)
C9 0.060(5) 0.060(4) 0.048(4) 0.000(3) -0.001(3) 0.008(3)
C10 0.064(5) 0.066(4) 0.038(3) 0.004(3) 0.016(3) -0.012(3)
C11 0.085(6) 0.070(4) 0.049(4) 0.017(3) -0.006(4) -0.016(4)
C12 0.072(5) 0.044(3) 0.062(4) 0.007(3) -0.018(3) 0.000(3)
C13 0.068(5) 0.054(4) 0.053(4) 0.008(3) 0.006(3) -0.003(3)
C14 0.057(4) 0.037(3) 0.074(4) 0.009(3) -0.001(3) -0.004(3)
C15 0.064(5) 0.055(4) 0.053(4) -0.001(3) 0.008(3) 0.008(3)
#------------------------------------------------------------------------------
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0184P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 4888
_refine_ls_number_parameters 244
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1522
_refine_ls_R_factor_gt 0.0403
_refine_ls_wR_factor_ref 0.0793
_refine_ls_wR_factor_gt 0.0607
_refine_ls_goodness_of_fit_ref 0.786
_refine_ls_restrained_S_all 0.786
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.445
_refine_diff_density_min -0.519
_refine_diff_density_rms 0.093
#------------------------------------------------------------------------------
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 C1 1.781(6) . ?
Fe1 C3 1.785(6) . ?
Fe1 C2 1.806(6) . ?
Fe1 S1 2.2539(13) . ?
Fe1 S2 2.2652(14) . ?
Fe1 Fe2 2.5330(10) . ?
Fe2 C4 1.781(6) . ?
Fe2 C5 1.797(6) . ?
Fe2 C6 1.797(6) . ?
Fe2 S2 2.2518(13) . ?
Fe2 S1 2.2622(14) . ?
S1 C14 1.863(5) . ?
S2 C15 1.866(5) . ?
Br1 C7 1.905(5) . ?
O1 C1 1.150(5) . ?
O2 C2 1.143(5) . ?
O3 C3 1.155(6) . ?
O4 C4 1.139(5) . ?
O5 C5 1.135(6) . ?
O6 C6 1.139(5) . ?
N1 C14 1.416(6) . ?
N1 C15 1.420(5) . ?
N1 C13 1.462(6) . ?
C7 C12 1.369(6) . ?
C7 C8 1.392(6) . ?
C8 C9 1.391(7) . ?
C8 C13 1.528(6) . ?
C9 C10 1.384(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.341(7) . ?
C10 H10 0.9300 . ?
C11 C12 1.380(7) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
#------------------------------------------------------------------------------
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
C1 Fe1 C3 99.0(2) . . ?
C1 Fe1 C2 91.3(2) . . ?
C3 Fe1 C2 101.3(2) . . ?
C1 Fe1 S1 162.54(18) . . ?
C3 Fe1 S1 98.40(15) . . ?
C2 Fe1 S1 87.06(16) . . ?
C1 Fe1 S2 89.48(16) . . ?
C3 Fe1 S2 101.19(17) . . ?
C2 Fe1 S2 157.12(18) . . ?
S1 Fe1 S2 85.43(5) . . ?
C1 Fe1 Fe2 107.63(18) . . ?
C3 Fe1 Fe2 143.52(16) . . ?
C2 Fe1 Fe2 102.60(18) . . ?
S1 Fe1 Fe2 56.04(4) . . ?
S2 Fe1 Fe2 55.64(4) . . ?
C4 Fe2 C5 98.3(3) . . ?
C4 Fe2 C6 91.9(2) . . ?
C5 Fe2 C6 99.2(2) . . ?
C4 Fe2 S2 162.2(2) . . ?
C5 Fe2 S2 99.15(18) . . ?
C6 Fe2 S2 88.84(15) . . ?
C4 Fe2 S1 85.48(18) . . ?
C5 Fe2 S1 108.89(18) . . ?
C6 Fe2 S1 151.83(17) . . ?
S2 Fe2 S1 85.54(5) . . ?
C4 Fe2 Fe1 106.25(19) . . ?
C5 Fe2 Fe1 148.95(18) . . ?
C6 Fe2 Fe1 98.69(17) . . ?
S2 Fe2 Fe1 56.14(4) . . ?
S1 Fe2 Fe1 55.73(4) . . ?
C14 S1 Fe1 108.34(16) . . ?
C14 S1 Fe2 112.51(18) . . ?
Fe1 S1 Fe2 68.23(4) . . ?
C15 S2 Fe2 110.87(16) . . ?
C15 S2 Fe1 110.29(17) . . ?
Fe2 S2 Fe1 68.22(4) . . ?
C14 N1 C15 117.8(4) . . ?
C14 N1 C13 118.3(4) . . ?
C15 N1 C13 121.7(4) . . ?
O1 C1 Fe1 177.9(5) . . ?
O2 C2 Fe1 179.7(5) . . ?
O3 C3 Fe1 178.2(5) . . ?
O4 C4 Fe2 177.5(5) . . ?
O5 C5 Fe2 176.7(6) . . ?
O6 C6 Fe2 178.9(5) . . ?
C12 C7 C8 121.8(5) . . ?
C12 C7 Br1 118.5(4) . . ?
C8 C7 Br1 119.7(4) . . ?
C9 C8 C7 116.5(4) . . ?
C9 C8 C13 121.8(5) . . ?
C7 C8 C13 121.7(5) . . ?
C10 C9 C8 121.4(5) . . ?
C10 C9 H9 119.3 . . ?
C8 C9 H9 119.3 . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.4(5) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C7 C12 C11 119.6(5) . . ?
C7 C12 H12 120.2 . . ?
C11 C12 H12 120.2 . . ?
N1 C13 C8 112.9(5) . . ?
N1 C13 H13A 109.0 . . ?
C8 C13 H13A 109.0 . . ?
N1 C13 H13B 109.0 . . ?
C8 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
N1 C14 S1 115.8(4) . . ?
N1 C14 H14A 108.3 . . ?
S1 C14 H14A 108.3 . . ?
N1 C14 H14B 108.3 . . ?
S1 C14 H14B 108.3 . . ?
H14A C14 H14B 107.4 . . ?
N1 C15 S2 117.4(3) . . ?
N1 C15 H15A 107.9 . . ?
S2 C15 H15A 107.9 . . ?
N1 C15 H15B 107.9 . . ?
S2 C15 H15B 107.9 . . ?
H15A C15 H15B 107.2 . . ?
#===END
# Copyright The Royal Society of Chemistry, 2007
# CCDC Number: 651098
data_1NH
_database_code_depnum_ccdc_archive 'CCDC 651098'
#------------------------------------------------------------------------------
_audit_creation_date 'Aug 15 14:01:24 2004'
_audit_creation_method SHELXL-97
_audit_update_record ?
#------------------------------------------------------------------------------
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics SHELXP-97
_computing_publication_material SHELXTL
#------------------------------------------------------------------------------
_chemical_compound_source ?
_chemical_name_common ?
_chemical_formula_weight 656.43
_chemical_formula_analytical ?
_chemical_formula_sum 'C15 H11 Br Cl Fe2 N O10 S2'
_chemical_formula_moiety 'C15 H11 Br Cl Fe2 N O10 S2'
_chemical_formula_structural ?
_chemical_melting_point ?
#------------------------------------------------------------------------------
_cell_length_a 22.953(10)
_cell_length_b 6.611(3)
_cell_length_c 15.033(6)
_cell_angle_alpha 90.00
_cell_angle_beta 104.63(3)
_cell_angle_gamma 90.00
_cell_volume 2207.2(16)
_cell_formula_units_Z 4
_cell_measurement_temperature 273(2)
_cell_measurement_reflns_used ?
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
#------------------------------------------------------------------------------
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/c
_symmetry_Int_Tables_number 14
_symmetry_space_group_name_Hall ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_exptl_crystal_description block
_exptl_crystal_colour 'black red'
_exptl_crystal_size_max 0.27
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.16
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.975
_exptl_crystal_F_000 1296
_exptl_absorpt_coefficient_mu 3.488
_exptl_absorpt_correction_type empirical
_exptl_absorpt_correction_T_min 0.428
_exptl_absorpt_correction_T_max 0.572
_exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)'
_exptl_special_details
;
?
;
#------------------------------------------------------------------------------
_diffrn_special_details
;
?
;
_diffrn_ambient_temperature 273(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_detector 'Imaging Plate'
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_% 0.00
_diffrn_reflns_number 14151
_reflns_number_total 5515
_reflns_number_gt 2403
_reflns_threshold_expression >2sigma(I)
_diffrn_reflns_av_R_equivalents 0.2544
_diffrn_reflns_av_sigmaI/netI 0.2231
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_h_max 30
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 8
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.72
_diffrn_reflns_theta_max 28.82
_diffrn_measured_fraction_theta_max 0.958
_diffrn_reflns_theta_full 28.82
_diffrn_measured_fraction_theta_full 0.958
#------------------------------------------------------------------------------
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'
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'
Cl Cl 0.1484 0.1585 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#------------------------------------------------------------------------------
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
N1 N 0.2035(2) 0.0113(11) 0.3208(4) 0.0267(16) Uani 1 1 d . . .
H1 H 0.2093 0.0631 0.3785 0.080 Uiso 1 1 calc . . .
Cl1 Cl 0.16705(9) -0.3377(4) 0.06221(15) 0.0388(6) Uani 1 1 d . . .
Fe1 Fe 0.36801(5) -0.0032(2) 0.30550(9) 0.0344(4) Uani 1 1 d . . .
Fe2 Fe 0.34667(5) 0.12214(19) 0.45080(9) 0.0303(3) Uani 1 1 d . . .
Br1 Br 0.12671(5) 0.35784(19) 0.40548(8) 0.0577(4) Uani 1 1 d . . .
S1 S 0.31625(8) -0.1801(3) 0.38682(15) 0.0297(5) Uani 1 1 d . . .
S2 S 0.30221(8) 0.2453(3) 0.31000(16) 0.0298(5) Uani 1 1 d . . .
O1 O 0.4448(4) 0.3079(16) 0.2569(8) 0.100(4) Uani 1 1 d . . .
O2 O 0.4729(3) -0.2608(14) 0.3712(7) 0.092(3) Uani 1 1 d . . .
O3 O 0.3265(3) -0.1967(17) 0.1243(6) 0.094(3) Uani 1 1 d . . .
O4 O 0.4389(3) -0.0983(12) 0.5854(6) 0.075(3) Uani 1 1 d . . .
O5 O 0.2742(3) 0.2562(15) 0.5736(6) 0.080(3) Uani 1 1 d . . .
O6 O 0.4246(3) 0.4750(12) 0.4880(6) 0.072(3) Uani 1 1 d . . .
O7 O 0.1052(3) -0.3471(14) 0.0164(6) 0.081(3) Uani 1 1 d . . .
O8 O 0.2012(3) -0.3919(13) 0.0003(5) 0.065(2) Uani 1 1 d . . .
O9 O 0.1812(4) -0.4649(14) 0.1395(5) 0.082(3) Uani 1 1 d . . .
O10 O 0.1825(3) -0.1337(11) 0.0940(6) 0.066(2) Uani 1 1 d . . .
C1 C 0.4166(4) 0.193(2) 0.2765(8) 0.059(3) Uani 1 1 d . . .
C2 C 0.4312(4) -0.1616(18) 0.3458(8) 0.053(3) Uani 1 1 d . . .
C3 C 0.3420(4) -0.1157(16) 0.1949(7) 0.044(3) Uani 1 1 d . . .
C4 C 0.4021(4) -0.0141(18) 0.5336(8) 0.054(3) Uani 1 1 d . . .
C5 C 0.3002(4) 0.1989(17) 0.5258(7) 0.045(3) Uani 1 1 d . . .
C6 C 0.3936(4) 0.3416(18) 0.4712(7) 0.048(3) Uani 1 1 d . . .
C7 C 0.0867(4) 0.3059(16) 0.2809(7) 0.044(3) Uani 1 1 d . . .
C8 C 0.0971(3) 0.1317(14) 0.2396(6) 0.032(2) Uani 1 1 d . . .
C9 C 0.0662(3) 0.1067(15) 0.1413(8) 0.047(3) Uani 1 1 d . . .
H9 H 0.0726 -0.0080 0.1092 0.080 Uiso 1 1 calc . . .
C10 C 0.0282(4) 0.255(2) 0.0987(7) 0.056(3) Uani 1 1 d . . .
H8 H 0.0089 0.2427 0.0367 0.080 Uiso 1 1 calc . . .
C11 C 0.0180(4) 0.4219(17) 0.1457(8) 0.051(3) Uani 1 1 d . . .
H7 H -0.0093 0.5188 0.1156 0.080 Uiso 1 1 calc . . .
C12 C 0.0469(4) 0.4500(15) 0.2359(8) 0.049(3) Uani 1 1 d . . .
H6 H 0.0397 0.5657 0.2667 0.080 Uiso 1 1 calc . . .
C13 C 0.1361(3) -0.0394(13) 0.2847(6) 0.031(2) Uani 1 1 d . . .
H3A H 0.1321 -0.1493 0.2408 0.080 Uiso 1 1 calc . . .
H3B H 0.1212 -0.0876 0.3357 0.080 Uiso 1 1 calc . . .
C14 C 0.2366(3) -0.1905(12) 0.3284(6) 0.0245(18) Uani 1 1 d . . .
H1A H 0.2325 -0.2435 0.2670 0.080 Uiso 1 1 calc . . .
H1B H 0.2171 -0.2851 0.3609 0.080 Uiso 1 1 calc . . .
C15 C 0.2254(3) 0.1588(15) 0.2650(6) 0.034(2) Uani 1 1 d . . .
H2A H 0.1991 0.2757 0.2567 0.080 Uiso 1 1 calc . . .
H2B H 0.2222 0.1003 0.2048 0.080 Uiso 1 1 calc . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.017(3) 0.039(5) 0.023(4) 0.002(3) 0.003(3) 0.001(3)
Cl1 0.0406(11) 0.0469(16) 0.0282(12) -0.0001(11) 0.0072(9) 0.0052(10)
Fe1 0.0260(6) 0.0435(9) 0.0346(7) 0.0049(7) 0.0094(5) 0.0027(5)
Fe2 0.0294(6) 0.0300(8) 0.0277(7) 0.0028(6) 0.0004(5) -0.0071(5)
Br1 0.0653(7) 0.0597(8) 0.0475(7) -0.0161(6) 0.0129(5) 0.0012(5)
S1 0.0247(9) 0.0282(12) 0.0325(12) 0.0017(10) 0.0006(8) -0.0008(8)
S2 0.0286(10) 0.0285(13) 0.0312(12) 0.0054(10) 0.0056(9) -0.0013(8)
O1 0.086(6) 0.098(8) 0.137(9) 0.035(7) 0.065(6) -0.022(5)
O2 0.044(4) 0.078(7) 0.156(10) 0.061(6) 0.028(5) 0.023(4)
O3 0.082(5) 0.128(9) 0.069(6) -0.056(6) 0.018(5) 0.024(5)
O4 0.087(5) 0.038(5) 0.068(6) 0.014(4) -0.041(4) -0.008(4)
O5 0.080(5) 0.097(8) 0.076(6) -0.036(5) 0.045(5) -0.031(5)
O6 0.046(4) 0.054(6) 0.100(6) 0.016(5) -0.013(4) -0.023(4)
O7 0.037(4) 0.099(8) 0.099(7) -0.007(6) 0.003(4) -0.014(4)
O8 0.081(5) 0.084(7) 0.040(4) -0.011(4) 0.034(4) 0.007(4)
O9 0.117(6) 0.084(7) 0.043(5) 0.035(5) 0.018(5) 0.019(5)
O10 0.076(5) 0.048(5) 0.073(6) -0.032(4) 0.016(4) -0.005(4)
C1 0.047(6) 0.080(9) 0.059(8) 0.008(7) 0.029(5) 0.012(6)
C2 0.039(5) 0.071(9) 0.054(7) 0.003(6) 0.020(5) -0.009(5)
C3 0.038(5) 0.056(7) 0.044(6) -0.014(5) 0.019(4) 0.010(4)
C4 0.039(5) 0.055(8) 0.058(7) -0.007(6) -0.008(5) -0.013(5)
C5 0.050(5) 0.056(7) 0.028(5) -0.006(5) 0.009(5) -0.022(5)
C6 0.030(5) 0.062(8) 0.045(6) 0.015(6) -0.008(4) -0.002(5)
C7 0.037(5) 0.050(7) 0.047(6) -0.013(5) 0.014(4) -0.007(4)
C8 0.019(4) 0.048(6) 0.028(5) 0.005(5) 0.005(3) 0.006(4)
C9 0.025(4) 0.043(6) 0.074(8) 0.009(6) 0.016(5) 0.009(4)
C10 0.043(5) 0.081(9) 0.037(6) 0.008(6) -0.003(5) 0.009(5)
C11 0.048(6) 0.044(7) 0.058(7) 0.020(6) 0.008(5) 0.013(5)
C12 0.026(4) 0.041(6) 0.083(8) 0.005(6) 0.020(5) 0.009(4)
C13 0.019(4) 0.032(5) 0.037(5) -0.001(4) 0.000(3) -0.006(3)
C14 0.018(3) 0.020(4) 0.030(5) 0.001(4) -0.004(3) 0.002(3)
C15 0.028(4) 0.046(6) 0.024(5) 0.008(4) 0.001(3) -0.003(4)
#------------------------------------------------------------------------------
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 5515
_refine_ls_number_parameters 290
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.2075
_refine_ls_R_factor_gt 0.0865
_refine_ls_wR_factor_ref 0.1947
_refine_ls_wR_factor_gt 0.1479
_refine_ls_goodness_of_fit_ref 0.961
_refine_ls_restrained_S_all 0.961
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.834
_refine_diff_density_min -0.903
_refine_diff_density_rms 0.157
#------------------------------------------------------------------------------
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
N1 C15 1.456(11) . ?
N1 C14 1.525(10) . ?
N1 C13 1.542(9) . ?
N1 H1 0.9100 . ?
Cl1 O9 1.404(8) . ?
Cl1 O8 1.405(7) . ?
Cl1 O7 1.414(6) . ?
Cl1 O10 1.445(7) . ?
Fe1 C2 1.767(11) . ?
Fe1 C3 1.781(10) . ?
Fe1 C1 1.831(13) . ?
Fe1 S1 2.237(3) . ?
Fe1 S2 2.244(3) . ?
Fe1 Fe2 2.498(2) . ?
Fe2 C4 1.782(11) . ?
Fe2 C6 1.787(11) . ?
Fe2 C5 1.810(11) . ?
Fe2 S1 2.251(3) . ?
Fe2 S2 2.257(3) . ?
Br1 C7 1.897(10) . ?
S1 C14 1.819(7) . ?
S2 C15 1.813(8) . ?
O1 C1 1.089(13) . ?
O2 C2 1.144(11) . ?
O3 C3 1.162(11) . ?
O4 C4 1.140(11) . ?
O5 C5 1.110(12) . ?
O6 C6 1.120(11) . ?
C7 C8 1.358(13) . ?
C7 C12 1.375(13) . ?
C8 C9 1.478(13) . ?
C8 C13 1.495(11) . ?
C9 C10 1.362(13) . ?
C9 H9 0.9300 . ?
C10 C11 1.360(16) . ?
C10 H8 0.9300 . ?
C11 C12 1.363(14) . ?
C11 H7 0.9300 . ?
C12 H6 0.9300 . ?
C13 H3A 0.9700 . ?
C13 H3B 0.9700 . ?
C14 H1A 0.9700 . ?
C14 H1B 0.9700 . ?
C15 H2A 0.9700 . ?
C15 H2B 0.9700 . ?
#------------------------------------------------------------------------------
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
C15 N1 C14 113.1(6) . . ?
C15 N1 C13 113.8(6) . . ?
C14 N1 C13 105.8(6) . . ?
C15 N1 H1 108.0 . . ?
C14 N1 H1 108.0 . . ?
C13 N1 H1 108.0 . . ?
O9 Cl1 O8 110.1(5) . . ?
O9 Cl1 O7 111.8(5) . . ?
O8 Cl1 O7 109.0(5) . . ?
O9 Cl1 O10 107.4(5) . . ?
O8 Cl1 O10 109.0(5) . . ?
O7 Cl1 O10 109.5(5) . . ?
C2 Fe1 C3 97.2(5) . . ?
C2 Fe1 C1 90.3(5) . . ?
C3 Fe1 C1 98.8(5) . . ?
C2 Fe1 S1 90.3(3) . . ?
C3 Fe1 S1 101.1(3) . . ?
C1 Fe1 S1 159.8(4) . . ?
C2 Fe1 S2 157.5(4) . . ?
C3 Fe1 S2 105.3(3) . . ?
C1 Fe1 S2 86.8(4) . . ?
S1 Fe1 S2 84.95(9) . . ?
C2 Fe1 Fe2 102.8(4) . . ?
C3 Fe1 Fe2 149.4(3) . . ?
C1 Fe1 Fe2 103.8(4) . . ?
S1 Fe1 Fe2 56.44(7) . . ?
S2 Fe1 Fe2 56.54(7) . . ?
C4 Fe2 C6 89.8(4) . . ?
C4 Fe2 C5 97.8(5) . . ?
C6 Fe2 C5 95.2(5) . . ?
C4 Fe2 S1 86.5(3) . . ?
C6 Fe2 S1 154.5(4) . . ?
C5 Fe2 S1 110.3(3) . . ?
C4 Fe2 S2 155.6(4) . . ?
C6 Fe2 S2 88.8(3) . . ?
C5 Fe2 S2 106.6(3) . . ?
S1 Fe2 S2 84.35(9) . . ?
C4 Fe2 Fe1 100.4(4) . . ?
C6 Fe2 Fe1 100.2(4) . . ?
C5 Fe2 Fe1 156.2(3) . . ?
S1 Fe2 Fe1 55.93(7) . . ?
S2 Fe2 Fe1 56.06(7) . . ?
C14 S1 Fe1 111.3(3) . . ?
C14 S1 Fe2 113.9(3) . . ?
Fe1 S1 Fe2 67.63(8) . . ?
C15 S2 Fe1 110.9(3) . . ?
C15 S2 Fe2 113.7(3) . . ?
Fe1 S2 Fe2 67.41(8) . . ?
O1 C1 Fe1 178.2(12) . . ?
O2 C2 Fe1 178.4(10) . . ?
O3 C3 Fe1 176.9(10) . . ?
O4 C4 Fe2 177.8(10) . . ?
O5 C5 Fe2 175.4(10) . . ?
O6 C6 Fe2 176.5(9) . . ?
C8 C7 C12 122.3(9) . . ?
C8 C7 Br1 120.5(7) . . ?
C12 C7 Br1 117.2(8) . . ?
C7 C8 C9 117.2(8) . . ?
C7 C8 C13 126.1(8) . . ?
C9 C8 C13 116.7(8) . . ?
C10 C9 C8 118.5(10) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C11 C10 C9 121.0(10) . . ?
C11 C10 H8 119.5 . . ?
C9 C10 H8 119.5 . . ?
C10 C11 C12 121.5(9) . . ?
C10 C11 H7 119.3 . . ?
C12 C11 H7 119.3 . . ?
C11 C12 C7 119.5(10) . . ?
C11 C12 H6 120.3 . . ?
C7 C12 H6 120.3 . . ?
C8 C13 N1 115.4(7) . . ?
C8 C13 H3A 108.4 . . ?
N1 C13 H3A 108.4 . . ?
C8 C13 H3B 108.4 . . ?
N1 C13 H3B 108.4 . . ?
H3A C13 H3B 107.5 . . ?
N1 C14 S1 115.1(5) . . ?
N1 C14 H1A 108.5 . . ?
S1 C14 H1A 108.5 . . ?
N1 C14 H1B 108.5 . . ?
S1 C14 H1B 108.5 . . ?
H1A C14 H1B 107.5 . . ?
N1 C15 S2 116.2(5) . . ?
N1 C15 H2A 108.2 . . ?
S2 C15 H2A 108.2 . . ?
N1 C15 H2B 108.2 . . ?
S2 C15 H2B 108.2 . . ?
H2A C15 H2B 107.4 . . ?
#------------------------------------------------------------------------------
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
N1 H1 O8 0.91 2.20 2.826(9) 125.2 4_556
N1 H1 Br1 0.91 2.82 3.334(7) 117.2 .