#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/79/4307966.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_4307966
loop_
_publ_author_name
'Rongmin Yu'
'Kuppuswamy Arumugam'
'Ashok Manepalli'
'Yvon Tran'
'Russell Schmehl'
'Heiko Jacobsen'
'James P. Donahue'
_publ_contact_author_email       donahue@tulane.edu
_publ_contact_author_fax         504-865-5596
_publ_contact_author_phone       504-862-3562
_publ_section_title
;
Reversible, Electrochemically Controlled Binding of Phosphine to Iron and
Cobalt Bis(dithiolene) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5131
_journal_page_last               5133
_journal_paper_doi               10.1021/ic0624569
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C80.5 H93 Cl Fe2 N O8 S8'
_chemical_formula_weight         1606.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.7460(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.9619(18)
_cell_length_b                   11.4244(7)
_cell_length_c                   23.0118(14)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2670
_cell_measurement_theta_min      2.2685
_cell_volume                     7708.0(8)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX'
_diffrn_measurement_method       'phi and 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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54075
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.8754
_exptl_absorpt_correction_T_min  0.7958
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         18167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0411
_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)+(0.0544P)²+2.3699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                14917
_reflns_number_total             18167
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic0624569-file006_02.cif
_cod_data_source_block
'[Bu4N][Fe(S2C2(C6H4-p-OCH3)2)2]2.0.5(CH2Cl2)_[Bu4N].2a.0.5(CH2Cl2)'
_cod_original_formula_sum        'C80.50 H93 Cl Fe2 N O8 S8'
_cod_database_code               4307966
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
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 0.243616(8) 0.27854(2) 0.301126(12) 0.01388(7) Uani 1 1 d . . .
Fe2 Fe 0.260775(9) 0.25070(2) 0.190970(12) 0.01417(7) Uani 1 1 d . . .
S1 S 0.277706(16) 0.13062(4) 0.35994(2) 0.01716(10) Uani 1 1 d . . .
S2 S 0.259272(16) 0.38432(4) 0.38525(2) 0.01684(10) Uani 1 1 d . . .
S3 S 0.181612(15) 0.38807(4) 0.26478(2) 0.01695(10) Uani 1 1 d . . .
S4 S 0.210925(15) 0.14830(4) 0.22782(2) 0.01507(10) Uani 1 1 d . . .
S5 S 0.316102(16) 0.12144(4) 0.22736(2) 0.01720(10) Uani 1 1 d . . .
S6 S 0.298714(15) 0.37050(4) 0.26496(2) 0.01440(10) Uani 1 1 d . . .
S7 S 0.224767(15) 0.40433(4) 0.14081(2) 0.01608(10) Uani 1 1 d . . .
S8 S 0.248617(16) 0.16739(4) 0.10237(2) 0.01777(10) Uani 1 1 d . . .
O1 O 0.41925(5) -0.10286(13) 0.61784(7) 0.0316(4) Uani 1 1 d . . .
O2 O 0.39956(5) 0.58586(13) 0.64139(6) 0.0251(3) Uani 1 1 d . . .
O3 O -0.02023(5) 0.54958(14) 0.09104(8) 0.0359(4) Uani 1 1 d . . .
O4 O 0.04221(5) -0.13798(15) 0.03241(8) 0.0392(4) Uani 1 1 d . . .
O5 O 0.50834(5) -0.09120(14) 0.41086(8) 0.0335(4) Uani 1 1 d . . .
O6 O 0.49325(5) 0.60204(13) 0.44016(7) 0.0292(4) Uani 1 1 d . . .
O7 O 0.09271(5) 0.68296(13) -0.10845(7) 0.0285(3) Uani 1 1 d . . .
O8 O 0.10921(5) -0.01474(14) -0.15611(7) 0.0320(4) Uani 1 1 d . . .
N1 N 0.25401(6) 0.23103(15) 0.72693(9) 0.0263(4) Uani 1 1 d . . .
C1 C 0.30595(6) 0.18929(16) 0.43250(9) 0.0170(4) Uani 1 1 d . . .
C2 C 0.29910(6) 0.30457(17) 0.44249(8) 0.0168(4) Uani 1 1 d . . .
C3 C 0.14314(6) 0.30544(16) 0.20749(8) 0.0158(4) Uani 1 1 d . . .
C4 C 0.15472(6) 0.19882(16) 0.19069(8) 0.0150(4) Uani 1 1 d . . .
C5 C 0.35831(6) 0.19238(16) 0.28472(8) 0.0153(4) Uani 1 1 d . . .
C6 C 0.35227(6) 0.30530(16) 0.29971(8) 0.0150(4) Uani 1 1 d . . .
C7 C 0.20052(6) 0.36344(16) 0.06513(8) 0.0157(4) Uani 1 1 d . . .
C8 C 0.20958(6) 0.25205(16) 0.04860(8) 0.0168(4) Uani 1 1 d . . .
C9 C 0.33386(6) 0.10787(17) 0.47981(9) 0.0187(4) Uani 1 1 d . . .
C10 C 0.35789(7) 0.01630(17) 0.46447(9) 0.0220(4) Uani 1 1 d . . .
H10 H 0.3548 0.0035 0.4225 0.026 Uiso 1 1 calc R . .
C11 C 0.38632(7) -0.05702(18) 0.50881(10) 0.0246(4) Uani 1 1 d . . .
H11 H 0.4028 -0.1177 0.4972 0.029 Uiso 1 1 calc R . .
C12 C 0.39033(7) -0.04089(18) 0.56984(10) 0.0244(4) Uani 1 1 d . . .
C13 C 0.36468(7) 0.04532(19) 0.58602(10) 0.0263(5) Uani 1 1 d . . .
H13 H 0.3659 0.0533 0.6276 0.032 Uiso 1 1 calc R . .
C14 C 0.33735(7) 0.11954(18) 0.54192(9) 0.0218(4) Uani 1 1 d . . .
H14 H 0.3206 0.1795 0.5538 0.026 Uiso 1 1 calc R . .
C15 C 0.44630(8) -0.1916(2) 0.60219(12) 0.0350(6) Uani 1 1 d . . .
H15A H 0.4262 -0.2516 0.5770 0.052 Uiso 1 1 calc R . .
H15B H 0.4665 -0.2274 0.6398 0.052 Uiso 1 1 calc R . .
H15C H 0.4646 -0.1564 0.5791 0.052 Uiso 1 1 calc R . .
C16 C 0.32401(6) 0.37330(16) 0.49763(8) 0.0167(4) Uani 1 1 d . . .
C17 C 0.37178(6) 0.37465(17) 0.51806(9) 0.0187(4) Uani 1 1 d . . .
H17 H 0.3879 0.3261 0.4985 0.022 Uiso 1 1 calc R . .
C18 C 0.39574(7) 0.44534(18) 0.56603(9) 0.0210(4) Uani 1 1 d . . .
H18 H 0.4281 0.4452 0.5793 0.025 Uiso 1 1 calc R . .
C19 C 0.37267(7) 0.51684(17) 0.59509(8) 0.0196(4) Uani 1 1 d . . .
C20 C 0.32536(7) 0.51579(17) 0.57646(9) 0.0203(4) Uani 1 1 d . . .
H20 H 0.3095 0.5631 0.5969 0.024 Uiso 1 1 calc R . .
C21 C 0.30138(7) 0.44482(17) 0.52759(9) 0.0196(4) Uani 1 1 d . . .
H21 H 0.2690 0.4451 0.5144 0.024 Uiso 1 1 calc R . .
C22 C 0.37660(8) 0.67488(19) 0.66401(10) 0.0289(5) Uani 1 1 d . . .
H22A H 0.3581 0.7227 0.6297 0.043 Uiso 1 1 calc R . .
H22B H 0.3992 0.7246 0.6932 0.043 Uiso 1 1 calc R . .
H22C H 0.3569 0.6383 0.6847 0.043 Uiso 1 1 calc R . .
C23 C 0.09884(6) 0.36390(16) 0.17800(9) 0.0178(4) Uani 1 1 d . . .
C24 C 0.07414(7) 0.41208(18) 0.21288(10) 0.0234(4) Uani 1 1 d . . .
H24 H 0.0849 0.4031 0.2562 0.028 Uiso 1 1 calc R . .
C25 C 0.03370(7) 0.47362(19) 0.18532(10) 0.0273(5) Uani 1 1 d . . .
H25 H 0.0169 0.5050 0.2097 0.033 Uiso 1 1 calc R . .
C26 C 0.01835(7) 0.48855(18) 0.12228(10) 0.0258(5) Uani 1 1 d . . .
C27 C 0.04237(7) 0.43999(18) 0.08658(10) 0.0260(5) Uani 1 1 d . . .
H27 H 0.0316 0.4496 0.0433 0.031 Uiso 1 1 calc R . .
C28 C 0.08203(7) 0.37745(17) 0.11416(9) 0.0208(4) Uani 1 1 d . . .
H28 H 0.0980 0.3433 0.0894 0.025 Uiso 1 1 calc R . .
C29 C -0.04530(8) 0.6006(2) 0.12687(13) 0.0405(6) Uani 1 1 d . . .
H29A H -0.0537 0.5396 0.1512 0.061 Uiso 1 1 calc R . .
H29B H -0.0730 0.6375 0.0996 0.061 Uiso 1 1 calc R . .
H29C H -0.0264 0.6597 0.1544 0.061 Uiso 1 1 calc R . .
C30 C 0.12373(6) 0.11507(16) 0.14818(9) 0.0172(4) Uani 1 1 d . . .
C31 C 0.07907(7) 0.09678(19) 0.14793(10) 0.0248(4) Uani 1 1 d . . .
H31 H 0.0677 0.1419 0.1745 0.030 Uiso 1 1 calc R . .
C32 C 0.05084(7) 0.0142(2) 0.10981(10) 0.0305(5) Uani 1 1 d . . .
H32 H 0.0205 0.0042 0.1102 0.037 Uiso 1 1 calc R . .
C33 C 0.06696(7) -0.05362(19) 0.07119(10) 0.0264(5) Uani 1 1 d . . .
C34 C 0.11096(7) -0.03570(18) 0.07011(10) 0.0255(5) Uani 1 1 d . . .
H34 H 0.1221 -0.0807 0.0432 0.031 Uiso 1 1 calc R . .
C35 C 0.13876(7) 0.04719(17) 0.10787(9) 0.0216(4) Uani 1 1 d . . .
H35 H 0.1688 0.0583 0.1064 0.026 Uiso 1 1 calc R . .
C36 C -0.00107(8) -0.1688(2) 0.03762(12) 0.0436(7) Uani 1 1 d . . .
H36A H 0.0030 -0.1967 0.0793 0.065 Uiso 1 1 calc R . .
H36B H -0.0149 -0.2308 0.0081 0.065 Uiso 1 1 calc R . .
H36C H -0.0210 -0.1000 0.0290 0.065 Uiso 1 1 calc R . .
C37 C 0.39917(6) 0.12108(16) 0.31583(9) 0.0177(4) Uani 1 1 d . . .
C38 C 0.41982(6) 0.05016(17) 0.28326(9) 0.0218(4) Uani 1 1 d . . .
H38 H 0.4086 0.0505 0.2397 0.026 Uiso 1 1 calc R . .
C39 C 0.45666(7) -0.02128(18) 0.31330(10) 0.0254(5) Uani 1 1 d . . .
H39 H 0.4707 -0.0682 0.2903 0.030 Uiso 1 1 calc R . .
C40 C 0.47283(7) -0.02364(18) 0.37685(10) 0.0255(5) Uani 1 1 d . . .
C41 C 0.45269(7) 0.04699(18) 0.41014(10) 0.0253(5) Uani 1 1 d . . .
H41 H 0.4638 0.0455 0.4537 0.030 Uiso 1 1 calc R . .
C42 C 0.41670(7) 0.11914(17) 0.38017(9) 0.0209(4) Uani 1 1 d . . .
H42 H 0.4036 0.1682 0.4034 0.025 Uiso 1 1 calc R . .
C43 C 0.52865(8) -0.1683(2) 0.37812(12) 0.0392(6) Uani 1 1 d . . .
H43A H 0.5056 -0.2232 0.3537 0.059 Uiso 1 1 calc R . .
H43B H 0.5535 -0.2120 0.4073 0.059 Uiso 1 1 calc R . .
H43C H 0.5408 -0.1226 0.3508 0.059 Uiso 1 1 calc R . .
C44 C 0.38834(6) 0.38296(16) 0.33818(8) 0.0163(4) Uani 1 1 d . . .
C45 C 0.43171(6) 0.38487(17) 0.33081(9) 0.0199(4) Uani 1 1 d . . .
H45 H 0.4379 0.3335 0.3019 0.024 Uiso 1 1 calc R . .
C46 C 0.46543(7) 0.45930(18) 0.36442(9) 0.0226(4) Uani 1 1 d . . .
H46 H 0.4944 0.4599 0.3583 0.027 Uiso 1 1 calc R . .
C47 C 0.45692(7) 0.53423(17) 0.40771(9) 0.0213(4) Uani 1 1 d . . .
C48 C 0.41448(7) 0.53456(17) 0.41530(9) 0.0200(4) Uani 1 1 d . . .
H48 H 0.4085 0.5858 0.4443 0.024 Uiso 1 1 calc R . .
C49 C 0.38049(6) 0.46005(16) 0.38054(9) 0.0182(4) Uani 1 1 d . . .
H49 H 0.3513 0.4618 0.3858 0.022 Uiso 1 1 calc R . .
C50 C 0.48620(8) 0.6789(2) 0.48511(11) 0.0315(5) Uani 1 1 d . . .
H50A H 0.4630 0.7371 0.4649 0.047 Uiso 1 1 calc R . .
H50B H 0.5149 0.7187 0.5069 0.047 Uiso 1 1 calc R . .
H50C H 0.4759 0.6336 0.5144 0.047 Uiso 1 1 calc R . .
C51 C 0.17272(6) 0.45052(16) 0.02119(9) 0.0175(4) Uani 1 1 d . . .
C52 C 0.14303(6) 0.52606(16) 0.03752(9) 0.0181(4) Uani 1 1 d . . .
H52 H 0.1416 0.5236 0.0781 0.022 Uiso 1 1 calc R . .
C53 C 0.11539(7) 0.60491(17) -0.00442(9) 0.0199(4) Uani 1 1 d . . .
H53 H 0.0948 0.6541 0.0072 0.024 Uiso 1 1 calc R . .
C54 C 0.11832(7) 0.61061(17) -0.06324(9) 0.0209(4) Uani 1 1 d . . .
C55 C 0.14921(7) 0.53998(17) -0.07954(9) 0.0206(4) Uani 1 1 d . . .
H55 H 0.1520 0.5466 -0.1193 0.025 Uiso 1 1 calc R . .
C56 C 0.17570(6) 0.46048(17) -0.03824(9) 0.0187(4) Uani 1 1 d . . .
H56 H 0.1963 0.4117 -0.0501 0.022 Uiso 1 1 calc R . .
C57 C 0.06242(8) 0.7625(2) -0.09233(11) 0.0327(5) Uani 1 1 d . . .
H57A H 0.0406 0.7180 -0.0783 0.049 Uiso 1 1 calc R . .
H57B H 0.0459 0.8093 -0.1283 0.049 Uiso 1 1 calc R . .
H57C H 0.0801 0.8145 -0.0594 0.049 Uiso 1 1 calc R . .
C58 C 0.18487(6) 0.19166(16) -0.00966(9) 0.0170(4) Uani 1 1 d . . .
C59 C 0.20749(7) 0.12518(17) -0.04161(9) 0.0214(4) Uani 1 1 d . . .
H59 H 0.2399 0.1260 -0.0288 0.026 Uiso 1 1 calc R . .
C60 C 0.18353(7) 0.05738(18) -0.09206(9) 0.0230(4) Uani 1 1 d . . .
H60 H 0.1994 0.0142 -0.1141 0.028 Uiso 1 1 calc R . .
C61 C 0.13620(7) 0.05362(18) -0.10981(9) 0.0230(4) Uani 1 1 d . . .
C62 C 0.11331(7) 0.12158(18) -0.07912(10) 0.0245(5) Uani 1 1 d . . .
H62 H 0.0809 0.1210 -0.0921 0.029 Uiso 1 1 calc R . .
C63 C 0.13715(7) 0.18993(17) -0.02998(9) 0.0207(4) Uani 1 1 d . . .
H63 H 0.1210 0.2365 -0.0096 0.025 Uiso 1 1 calc R . .
C64 C 0.13171(8) -0.0964(2) -0.18374(11) 0.0367(6) Uani 1 1 d . . .
H64A H 0.1487 -0.0537 -0.2064 0.055 Uiso 1 1 calc R . .
H64B H 0.1090 -0.1471 -0.2120 0.055 Uiso 1 1 calc R . .
H64C H 0.1529 -0.1442 -0.1517 0.055 Uiso 1 1 calc R . .
C65 C 0.21173(8) 0.30042(19) 0.72554(11) 0.0317(5) Uani 1 1 d . . .
H65A H 0.2191 0.3491 0.7631 0.038 Uiso 1 1 calc R . .
H65B H 0.2039 0.3541 0.6899 0.038 Uiso 1 1 calc R . .
C66 C 0.17026(8) 0.2264(2) 0.72154(14) 0.0424(6) Uani 1 1 d . B .
H66A H 0.1782 0.1691 0.7556 0.051 Uiso 1 1 calc R . .
H66B H 0.1611 0.1822 0.6825 0.051 Uiso 1 1 calc R . .
C67 C 0.13050(9) 0.3008(2) 0.72480(15) 0.0507(8) Uani 1 1 d . . .
H67A H 0.1308 0.3768 0.7043 0.061 Uiso 1 1 calc R A 1
H67B H 0.1014 0.2607 0.7031 0.061 Uiso 1 1 calc R A 1
C68A C 0.13376(19) 0.3205(5) 0.7887(2) 0.0443(15) Uani 0.510(5) 1 d P B 1
H68A H 0.1076 0.3672 0.7904 0.067 Uiso 0.510(5) 1 calc PR B 1
H68B H 0.1621 0.3625 0.8097 0.067 Uiso 0.510(5) 1 calc PR B 1
H68C H 0.1337 0.2450 0.8090 0.067 Uiso 0.510(5) 1 calc PR B 1
C68B C 0.09090(17) 0.2372(4) 0.7292(3) 0.0442(16) Uani 0.490(5) 1 d P B 2
H68D H 0.0992 0.1948 0.7683 0.066 Uiso 0.490(5) 1 calc PR B 2
H68E H 0.0806 0.1814 0.6952 0.066 Uiso 0.490(5) 1 calc PR B 2
H68F H 0.0663 0.2927 0.7272 0.066 Uiso 0.490(5) 1 calc PR B 2
C69 C 0.26883(8) 0.14992(18) 0.78292(10) 0.0286(5) Uani 1 1 d . . .
H69A H 0.2477 0.0823 0.7743 0.034 Uiso 1 1 calc R . .
H69B H 0.2995 0.1193 0.7865 0.034 Uiso 1 1 calc R . .
C70 C 0.27088(8) 0.1997(2) 0.84518(11) 0.0350(5) Uani 1 1 d . . .
H70A H 0.2414 0.2391 0.8399 0.042 Uiso 1 1 calc R . .
H70B H 0.2727 0.1325 0.8731 0.042 Uiso 1 1 calc R . .
C71 C 0.30775(10) 0.2834(3) 0.87750(13) 0.0504(7) Uani 1 1 d . . .
H71A H 0.3023 0.3592 0.8555 0.060 Uiso 1 1 calc R . .
H71B H 0.3374 0.2526 0.8766 0.060 Uiso 1 1 calc R . .
C72 C 0.31018(9) 0.3032(2) 0.94399(11) 0.0390(6) Uani 1 1 d . . .
H72A H 0.2809 0.3341 0.9452 0.059 Uiso 1 1 calc R . .
H72B H 0.3345 0.3595 0.9632 0.059 Uiso 1 1 calc R . .
H72C H 0.3167 0.2289 0.9664 0.059 Uiso 1 1 calc R . .
C73 C 0.29141(8) 0.31820(18) 0.72817(11) 0.0283(5) Uani 1 1 d . . .
H73A H 0.2787 0.3766 0.6953 0.034 Uiso 1 1 calc R . .
H73B H 0.3000 0.3604 0.7678 0.034 Uiso 1 1 calc R . .
C74 C 0.33436(8) 0.26754(19) 0.72009(12) 0.0352(6) Uani 1 1 d . . .
H74A H 0.3277 0.2394 0.6774 0.042 Uiso 1 1 calc R . .
H74B H 0.3448 0.2000 0.7480 0.042 Uiso 1 1 calc R . .
C75 C 0.37159(8) 0.35973(19) 0.73400(11) 0.0305(5) Uani 1 1 d . . .
H75A H 0.3598 0.4298 0.7085 0.037 Uiso 1 1 calc R . .
H75B H 0.3795 0.3832 0.7776 0.037 Uiso 1 1 calc R . .
C76 C 0.41440(8) 0.3177(2) 0.72194(12) 0.0400(6) Uani 1 1 d . . .
H76A H 0.4268 0.2497 0.7479 0.060 Uiso 1 1 calc R . .
H76B H 0.4371 0.3806 0.7314 0.060 Uiso 1 1 calc R . .
H76C H 0.4070 0.2955 0.6787 0.060 Uiso 1 1 calc R . .
C77 C 0.24406(8) 0.15338(17) 0.67051(10) 0.0273(5) Uani 1 1 d . . .
H77A H 0.2206 0.0953 0.6717 0.033 Uiso 1 1 calc R . .
H77B H 0.2722 0.1097 0.6727 0.033 Uiso 1 1 calc R . .
C78 C 0.22758(9) 0.21736(19) 0.60934(11) 0.0340(5) Uani 1 1 d . . .
H78A H 0.1971 0.2514 0.6038 0.041 Uiso 1 1 calc R . .
H78B H 0.2488 0.2823 0.6095 0.041 Uiso 1 1 calc R . .
C79 C 0.22477(8) 0.13600(18) 0.55650(10) 0.0284(5) Uani 1 1 d . . .
H79A H 0.2029 0.0724 0.5557 0.034 Uiso 1 1 calc R . .
H79B H 0.2550 0.1000 0.5630 0.034 Uiso 1 1 calc R . .
C80 C 0.20982(8) 0.1987(2) 0.49529(11) 0.0331(5) Uani 1 1 d . . .
H80A H 0.1770 0.2148 0.4831 0.050 Uiso 1 1 calc R . .
H80B H 0.2162 0.1492 0.4642 0.050 Uiso 1 1 calc R . .
H80C H 0.2266 0.2726 0.4989 0.050 Uiso 1 1 calc R . .
Cl1 Cl 0.0000 0.11269(9) 0.2500 0.0513(3) Uani 1 2 d S . .
Cl2 Cl 0.01899(7) -0.13727(16) 0.23274(9) 0.0731(5) Uani 0.50 1 d P . .
C1S C -0.0023(3) -0.0343(5) 0.2698(3) 0.0594(17) Uani 0.50 1 d P . .
H1S1 H -0.0241 0.0269 0.2730 0.071 Uiso 0.50 1 calc PR . .
H1S2 H 0.0268 -0.0258 0.3040 0.071 Uiso 0.50 1 calc PR . .
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'
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
S2 Fe1 S1 87.384(19) . . ?
S2 Fe1 S3 86.624(19) . . ?
S1 Fe1 S3 147.95(2) . . ?
S2 Fe1 S4 161.62(2) . . ?
S1 Fe1 S4 87.966(19) . . ?
S3 Fe1 S4 87.925(18) . . ?
S2 Fe1 S6 94.91(2) . . ?
S1 Fe1 S6 107.34(2) . . ?
S3 Fe1 S6 104.53(2) . . ?
S4 Fe1 S6 103.46(2) . . ?
S2 Fe1 Fe2 144.627(19) . . ?
S1 Fe1 Fe2 106.160(18) . . ?
S3 Fe1 Fe2 96.721(17) . . ?
S4 Fe1 Fe2 53.552(15) . . ?
S6 Fe1 Fe2 50.086(13) . . ?
S8 Fe2 S7 87.21(2) . . ?
S8 Fe2 S6 152.33(2) . . ?
S7 Fe2 S6 87.953(19) . . ?
S8 Fe2 S5 86.70(2) . . ?
S7 Fe2 S5 158.81(2) . . ?
S6 Fe2 S5 88.081(18) . . ?
S8 Fe2 S4 100.87(2) . . ?
S7 Fe2 S4 108.18(2) . . ?
S6 Fe2 S4 106.53(2) . . ?
S5 Fe2 S4 92.90(2) . . ?
S8 Fe2 Fe1 152.067(19) . . ?
S7 Fe2 Fe1 100.067(17) . . ?
S6 Fe2 Fe1 55.507(15) . . ?
S5 Fe2 Fe1 94.769(17) . . ?
S4 Fe2 Fe1 51.211(14) . . ?
C1 S1 Fe1 106.58(6) . . ?
C2 S2 Fe1 106.26(7) . . ?
C3 S3 Fe1 106.14(6) . . ?
C4 S4 Fe1 106.49(6) . . ?
C4 S4 Fe2 109.12(6) . . ?
Fe1 S4 Fe2 75.237(17) . . ?
C5 S5 Fe2 106.20(6) . . ?
C6 S6 Fe2 106.18(6) . . ?
C6 S6 Fe1 109.42(6) . . ?
Fe2 S6 Fe1 74.408(17) . . ?
C7 S7 Fe2 107.27(6) . . ?
C8 S8 Fe2 107.37(7) . . ?
C12 O1 C15 116.44(18) . . ?
C19 O2 C22 116.28(16) . . ?
C26 O3 C29 116.70(19) . . ?
C33 O4 C36 117.58(19) . . ?
C40 O5 C43 117.13(18) . . ?
C47 O6 C50 116.90(17) . . ?
C54 O7 C57 116.97(17) . . ?
C61 O8 C64 117.11(17) . . ?
C77 N1 C73 110.02(17) . . ?
C77 N1 C65 110.44(17) . . ?
C73 N1 C65 107.70(16) . . ?
C77 N1 C69 106.79(15) . . ?
C73 N1 C69 111.08(16) . . ?
C65 N1 C69 110.84(18) . . ?
C2 C1 C9 124.59(17) . . ?
C2 C1 S1 118.23(14) . . ?
C9 C1 S1 117.10(14) . . ?
C1 C2 C16 126.12(16) . . ?
C1 C2 S2 119.16(14) . . ?
C16 C2 S2 114.67(13) . . ?
C4 C3 C23 124.32(16) . . ?
C4 C3 S3 121.43(13) . . ?
C23 C3 S3 114.19(14) . . ?
C3 C4 C30 126.35(16) . . ?
C3 C4 S4 117.55(13) . . ?
C30 C4 S4 115.86(13) . . ?
C6 C5 C37 124.27(16) . . ?
C6 C5 S5 120.29(13) . . ?
C37 C5 S5 115.41(13) . . ?
C5 C6 C44 125.52(16) . . ?
C5 C6 S6 118.14(13) . . ?
C44 C6 S6 116.03(13) . . ?
C8 C7 C51 123.73(17) . . ?
C8 C7 S7 117.79(14) . . ?
C51 C7 S7 118.45(14) . . ?
C7 C8 C58 125.84(16) . . ?
C7 C8 S8 118.48(14) . . ?
C58 C8 S8 115.30(14) . . ?
C10 C9 C14 117.15(18) . . ?
C10 C9 C1 121.21(18) . . ?
C14 C9 C1 121.63(18) . . ?
C11 C10 C9 121.9(2) . . ?
C12 C11 C10 119.6(2) . . ?
O1 C12 C11 124.81(19) . . ?
O1 C12 C13 115.53(19) . . ?
C11 C12 C13 119.65(18) . . ?
C14 C13 C12 120.4(2) . . ?
C13 C14 C9 121.15(19) . . ?
C21 C16 C17 118.15(17) . . ?
C21 C16 C2 121.89(17) . . ?
C17 C16 C2 119.77(18) . . ?
C18 C17 C16 120.96(19) . . ?
C17 C18 C19 120.19(18) . . ?
O2 C19 C20 124.18(18) . . ?
O2 C19 C18 115.75(17) . . ?
C20 C19 C18 120.06(18) . . ?
C19 C20 C21 119.38(19) . . ?
C20 C21 C16 121.24(18) . . ?
C24 C23 C28 118.32(18) . . ?
C24 C23 C3 121.04(17) . . ?
C28 C23 C3 120.55(18) . . ?
C23 C24 C25 121.1(2) . . ?
C26 C25 C24 119.5(2) . . ?
O3 C26 C25 124.1(2) . . ?
O3 C26 C27 115.80(19) . . ?
C25 C26 C27 120.13(18) . . ?
C28 C27 C26 119.9(2) . . ?
C27 C28 C23 120.9(2) . . ?
C31 C30 C35 117.01(17) . . ?
C31 C30 C4 122.03(18) . . ?
C35 C30 C4 120.91(17) . . ?
C32 C31 C30 121.7(2) . . ?
C33 C32 C31 120.1(2) . . ?
O4 C33 C34 116.1(2) . . ?
O4 C33 C32 124.7(2) . . ?
C34 C33 C32 119.16(18) . . ?
C35 C34 C33 120.5(2) . . ?
C34 C35 C30 121.61(19) . . ?
C38 C37 C42 118.05(17) . . ?
C38 C37 C5 121.93(17) . . ?
C42 C37 C5 119.93(18) . . ?
C37 C38 C39 121.26(19) . . ?
C40 C39 C38 119.7(2) . . ?
O5 C40 C39 124.6(2) . . ?
O5 C40 C41 115.68(19) . . ?
C39 C40 C41 119.75(18) . . ?
C42 C41 C40 120.3(2) . . ?
C41 C42 C37 120.9(2) . . ?
C49 C44 C45 117.58(17) . . ?
C49 C44 C6 122.08(17) . . ?
C45 C44 C6 120.28(17) . . ?
C46 C45 C44 121.55(19) . . ?
C45 C46 C47 119.68(19) . . ?
O6 C47 C48 125.23(18) . . ?
O6 C47 C46 115.03(18) . . ?
C48 C47 C46 119.74(17) . . ?
C47 C48 C49 120.07(18) . . ?
C48 C49 C44 121.36(18) . . ?
C52 C51 C56 117.81(17) . . ?
C52 C51 C7 121.29(18) . . ?
C56 C51 C7 120.89(18) . . ?
C53 C52 C51 121.55(19) . . ?
C54 C53 C52 119.21(19) . . ?
O7 C54 C53 124.62(19) . . ?
O7 C54 C55 115.26(18) . . ?
C53 C54 C55 120.12(17) . . ?
C56 C55 C54 120.30(19) . . ?
C55 C56 C51 120.91(19) . . ?
C59 C58 C63 118.17(17) . . ?
C59 C58 C8 122.01(17) . . ?
C63 C58 C8 119.43(18) . . ?
C58 C59 C60 121.28(18) . . ?
C61 C60 C59 119.37(19) . . ?
O8 C61 C62 115.57(18) . . ?
O8 C61 C60 124.70(19) . . ?
C62 C61 C60 119.73(18) . . ?
C63 C62 C61 120.56(19) . . ?
C62 C63 C58 120.81(19) . . ?
C66 C65 N1 114.64(18) . . ?
C65 C66 C67 111.7(2) . . ?
C68B C67 C68A 78.1(4) . . ?
C68B C67 C66 116.0(3) . . ?
C68A C67 C66 110.0(3) . . ?
C70 C69 N1 118.40(18) . . ?
C71 C70 C69 120.1(2) . . ?
C70 C71 C72 112.3(2) . . ?
C74 C73 N1 116.14(17) . . ?
C73 C74 C75 110.24(18) . . ?
C76 C75 C74 113.0(2) . . ?
N1 C77 C78 115.19(17) . . ?
C79 C78 C77 111.38(18) . . ?
C78 C79 C80 112.29(18) . . ?
C1S Cl1 C1S 32.1(4) . 2 ?
C1S Cl2 Cl2 71.1(3) 2 2 ?
C1S Cl2 C1S 34.2(4) 2 . ?
Cl2 Cl2 C1S 45.2(2) 2 . ?
C1S C1S Cl2 97.8(5) 2 2 ?
C1S C1S Cl2 48.0(3) 2 . ?
Cl2 C1S Cl2 63.8(3) 2 . ?
C1S C1S Cl1 73.93(19) 2 . ?
Cl2 C1S Cl1 157.1(6) 2 . ?
Cl2 C1S Cl1 118.5(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 S2 2.1999(5) . ?
Fe1 S1 2.2098(5) . ?
Fe1 S3 2.2178(5) . ?
Fe1 S4 2.2331(5) . ?
Fe1 S6 2.3705(6) . ?
Fe1 Fe2 2.7703(4) . ?
Fe2 S8 2.1705(5) . ?
Fe2 S7 2.1974(5) . ?
Fe2 S6 2.2060(5) . ?
Fe2 S5 2.2123(5) . ?
Fe2 S4 2.3045(6) . ?
S1 C1 1.7502(19) . ?
S2 C2 1.7440(18) . ?
S3 C3 1.7432(18) . ?
S4 C4 1.7708(18) . ?
S5 C5 1.7315(18) . ?
S6 C6 1.7583(18) . ?
S7 C7 1.7247(19) . ?
S8 C8 1.7222(18) . ?
O1 C12 1.374(2) . ?
O1 C15 1.432(3) . ?
O2 C19 1.371(2) . ?
O2 C22 1.431(3) . ?
O3 C26 1.370(2) . ?
O3 C29 1.426(3) . ?
O4 C33 1.369(2) . ?
O4 C36 1.427(3) . ?
O5 C40 1.365(2) . ?
O5 C43 1.430(3) . ?
O6 C47 1.372(2) . ?
O6 C50 1.426(3) . ?
O7 C54 1.365(2) . ?
O7 C57 1.438(3) . ?
O8 C61 1.368(2) . ?
O8 C64 1.430(3) . ?
N1 C77 1.520(3) . ?
N1 C73 1.521(3) . ?
N1 C65 1.522(3) . ?
N1 C69 1.533(3) . ?
C1 C2 1.365(3) . ?
C1 C9 1.481(3) . ?
C2 C16 1.481(3) . ?
C3 C4 1.360(3) . ?
C3 C23 1.480(2) . ?
C4 C30 1.480(2) . ?
C5 C6 1.364(3) . ?
C5 C37 1.481(2) . ?
C6 C44 1.477(2) . ?
C7 C8 1.383(3) . ?
C7 C51 1.481(2) . ?
C8 C58 1.483(3) . ?
C9 C10 1.393(3) . ?
C9 C14 1.405(3) . ?
C10 C11 1.393(3) . ?
C11 C12 1.382(3) . ?
C12 C13 1.389(3) . ?
C13 C14 1.383(3) . ?
C16 C21 1.394(3) . ?
C16 C17 1.401(3) . ?
C17 C18 1.376(3) . ?
C18 C19 1.390(3) . ?
C19 C20 1.388(3) . ?
C20 C21 1.392(3) . ?
C23 C24 1.388(3) . ?
C23 C28 1.400(3) . ?
C24 C25 1.398(3) . ?
C25 C26 1.384(3) . ?
C26 C27 1.389(3) . ?
C27 C28 1.386(3) . ?
C30 C31 1.397(3) . ?
C30 C35 1.399(3) . ?
C31 C32 1.390(3) . ?
C32 C33 1.387(3) . ?
C33 C34 1.386(3) . ?
C34 C35 1.383(3) . ?
C37 C38 1.391(3) . ?
C37 C42 1.404(3) . ?
C38 C39 1.392(3) . ?
C39 C40 1.386(3) . ?
C40 C41 1.391(3) . ?
C41 C42 1.379(3) . ?
C44 C49 1.392(3) . ?
C44 C45 1.407(3) . ?
C45 C46 1.376(3) . ?
C46 C47 1.401(3) . ?
C47 C48 1.380(3) . ?
C48 C49 1.390(3) . ?
C51 C52 1.398(3) . ?
C51 C56 1.405(3) . ?
C52 C53 1.394(3) . ?
C53 C54 1.387(3) . ?
C54 C55 1.392(3) . ?
C55 C56 1.378(3) . ?
C58 C59 1.393(3) . ?
C58 C63 1.399(3) . ?
C59 C60 1.395(3) . ?
C60 C61 1.390(3) . ?
C61 C62 1.388(3) . ?
C62 C63 1.377(3) . ?
C65 C66 1.515(3) . ?
C66 C67 1.518(4) . ?
C67 C68B 1.456(5) . ?
C67 C68A 1.459(6) . ?
C69 C70 1.523(3) . ?
C70 C71 1.492(3) . ?
C71 C72 1.525(4) . ?
C73 C74 1.515(3) . ?
C74 C75 1.518(3) . ?
C75 C76 1.517(3) . ?
C77 C78 1.521(3) . ?
C78 C79 1.511(3) . ?
C79 C80 1.514(3) . ?
Cl1 C1S 1.748(6) . ?
Cl1 C1S 1.748(6) 2 ?
Cl2 C1S 1.279(6) 2 ?
Cl2 Cl2 1.617(4) 2 ?
Cl2 C1S 1.705(6) . ?
C1S C1S 0.968(11) 2 ?
C1S Cl2 1.279(6) 2 ?
