#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:29:58 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179020 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/18/4121819.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_4121819
loop_
_publ_author_name
'Fitzpatrick, Jessica'
'Kalyvas, Harris'
'Filipovic, Milos R.'
'Ivanović-Burmazović, Ivana'
'MacDonald, John C.'
'Shearer, Jason'
'Kim, Eunsuk'
_publ_section_title
;
 Transformation of a Mononitrosyl Iron Complex to a [2Fe-2S] Cluster by a
 Cysteine Analogue.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7229
_journal_page_last               7232
_journal_paper_doi               10.1021/ja5024207
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C44 H44 Fe N O4 P2 S3'
_chemical_formula_weight         864.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 94.529(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8998(11)
_cell_length_b                   12.7903(13)
_cell_length_c                   30.046(3)
_cell_measurement_reflns_used    322
_cell_measurement_temperature    100(2)
_cell_volume                     4175.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker Kappa Apex 2'
_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  0.0733
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            84387
_diffrn_reflns_theta_full        26.52
_diffrn_reflns_theta_max         26.52
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.9691
_exptl_absorpt_correction_T_min  0.7864
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0478P)²+6.4672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                6053
_reflns_number_total             8524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5024207_si_002.cif
_cod_data_source_block           camly5_0m
_cod_depositor_comments          'Adding full bibliography for 4121819.cif.'
_cod_original_cell_volume        4175.6(7)
_cod_database_code               4121819
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'
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
Fe1 Fe 0.01994(4) 0.40529(4) 0.019850(15) 0.03163(14) Uani 1 1 d .
P2 P 0.23672(7) 0.84189(6) 0.22343(2) 0.02088(17) Uani 1 1 d .
P1 P 0.47131(7) 0.84594(6) 0.18111(2) 0.02255(18) Uani 1 1 d .
S3 S -0.10641(8) 0.52904(7) 0.03830(3) 0.0330(2) Uani 1 1 d .
S1 S 0.16897(9) 0.36994(9) 0.07689(3) 0.0447(3) Uani 1 1 d .
S2 S -0.09303(10) 0.25593(9) 0.00552(4) 0.0524(3) Uani 1 1 d .
C31 C 0.1239(3) 0.7598(2) 0.19427(10) 0.0233(6) Uani 1 1 d .
C19 C 0.1979(3) 0.9754(2) 0.20938(10) 0.0240(7) Uani 1 1 d .
C13 C 0.5307(3) 0.7345(2) 0.15311(10) 0.0246(7) Uani 1 1 d .
C20 C 0.1177(3) 1.0004(3) 0.17268(11) 0.0315(7) Uani 1 1 d .
H20 H 0.0759 0.9465 0.1558 0.038 Uiso 1 1 calc R
C24 C 0.2578(3) 1.0552(3) 0.23375(11) 0.0338(8) Uani 1 1 d .
H24 H 0.3128 1.0390 0.2589 0.041 Uiso 1 1 calc R
C14 C 0.5942(3) 0.7480(3) 0.11504(11) 0.0327(8) Uani 1 1 d .
H14 H 0.6033 0.8159 0.1030 0.039 Uiso 1 1 calc R
C15 C 0.6441(3) 0.6622(3) 0.09477(12) 0.0368(8) Uani 1 1 d .
H15 H 0.6876 0.6715 0.0689 0.044 Uiso 1 1 calc R
C16 C 0.6310(3) 0.5645(3) 0.11189(11) 0.0346(8) Uani 1 1 d .
H16 H 0.6656 0.5061 0.0979 0.042 Uiso 1 1 calc R
C32 C 0.1566(3) 0.6949(3) 0.16017(10) 0.0312(7) Uani 1 1 d .
H32 H 0.2396 0.6921 0.1527 0.037 Uiso 1 1 calc R
C17 C 0.5675(3) 0.5497(3) 0.14952(12) 0.0339(8) Uani 1 1 d .
H17 H 0.5583 0.4813 0.1612 0.041 Uiso 1 1 calc R
C18 C 0.5174(3) 0.6350(3) 0.17024(10) 0.0286(7) Uani 1 1 d .
H18 H 0.4741 0.6251 0.1961 0.034 Uiso 1 1 calc R
C36 C 0.0023(3) 0.7612(3) 0.20519(11) 0.0373(8) Uani 1 1 d .
H36 H -0.0209 0.8040 0.2290 0.045 Uiso 1 1 calc R
C22 C 0.1583(4) 1.1823(3) 0.18501(13) 0.0467(10) Uani 1 1 d .
H22 H 0.1448 1.2532 0.1766 0.056 Uiso 1 1 calc R
C34 C -0.0514(3) 0.6374(3) 0.14763(11) 0.0335(8) Uani 1 1 d .
H34 H -0.1118 0.5957 0.1315 0.040 Uiso 1 1 calc R
C35 C -0.0848(3) 0.7005(3) 0.18150(12) 0.0410(9) Uani 1 1 d .
H35 H -0.1680 0.7024 0.1887 0.049 Uiso 1 1 calc R
C33 C 0.0677(3) 0.6341(3) 0.13691(11) 0.0383(8) Uani 1 1 d .
H33 H 0.0899 0.5900 0.1134 0.046 Uiso 1 1 calc R
C21 C 0.0989(3) 1.1040(3) 0.16087(13) 0.0425(9) Uani 1 1 d .
H21 H 0.0442 1.1211 0.1357 0.051 Uiso 1 1 calc R
C23 C 0.2375(4) 1.1580(3) 0.22137(13) 0.0435(9) Uani 1 1 d .
H23 H 0.2786 1.2124 0.2381 0.052 Uiso 1 1 calc R
C12 C 0.3470(3) 0.9002(3) 0.10104(11) 0.0359(8) Uani 1 1 d .
H12 H 0.3336 0.8273 0.0972 0.043 Uiso 1 1 calc R
C7 C 0.4176(3) 0.9372(3) 0.13834(10) 0.0273(7) Uani 1 1 d .
C10 C 0.3159(4) 1.0754(4) 0.07540(14) 0.0556(12) Uani 1 1 d .
H10 H 0.2813 1.1230 0.0536 0.067 Uiso 1 1 calc R
C9 C 0.3841(4) 1.1131(3) 0.11206(14) 0.0487(10) Uani 1 1 d .
H9 H 0.3963 1.1862 0.1157 0.058 Uiso 1 1 calc R
C11 C 0.2966(4) 0.9701(4) 0.06957(12) 0.0489(11) Uani 1 1 d .
H11 H 0.2486 0.9453 0.0440 0.059 Uiso 1 1 calc R
C8 C 0.4356(3) 1.0442(3) 0.14404(12) 0.0358(8) Uani 1 1 d .
H8 H 0.4828 1.0700 0.1696 0.043 Uiso 1 1 calc R
C25 C 0.2222(3) 0.8257(2) 0.28215(10) 0.0233(6) Uani 1 1 d .
C26 C 0.1334(3) 0.8802(3) 0.30375(10) 0.0312(7) Uani 1 1 d .
H26 H 0.0842 0.9317 0.2881 0.037 Uiso 1 1 calc R
C30 C 0.2948(3) 0.7529(3) 0.30562(11) 0.0381(8) Uani 1 1 d .
H30 H 0.3557 0.7155 0.2912 0.046 Uiso 1 1 calc R
C27 C 0.1172(3) 0.8588(3) 0.34811(11) 0.0364(8) Uani 1 1 d .
H27 H 0.0558 0.8951 0.3627 0.044 Uiso 1 1 calc R
C28 C 0.1887(4) 0.7861(3) 0.37097(11) 0.0449(9) Uani 1 1 d .
H28 H 0.1762 0.7712 0.4013 0.054 Uiso 1 1 calc R
C29 C 0.2787(4) 0.7344(4) 0.35020(12) 0.0527(11) Uani 1 1 d .
H29 H 0.3302 0.6856 0.3665 0.063 Uiso 1 1 calc R
C1 C 0.5985(3) 0.9045(3) 0.21374(11) 0.0291(7) Uani 1 1 d .
C6 C 0.6997(3) 0.9432(3) 0.19310(14) 0.0433(9) Uani 1 1 d .
H6 H 0.7005 0.9405 0.1615 0.052 Uiso 1 1 calc R
C2 C 0.5995(3) 0.9070(3) 0.25977(12) 0.0394(9) Uani 1 1 d .
H2 H 0.5314 0.8806 0.2741 0.047 Uiso 1 1 calc R
C4 C 0.7987(4) 0.9878(4) 0.26373(18) 0.0651(15) Uani 1 1 d .
H4 H 0.8671 1.0169 0.2810 0.078 Uiso 1 1 calc R
C5 C 0.7987(4) 0.9854(4) 0.21856(18) 0.0605(13) Uani 1 1 d .
H5 H 0.8668 1.0128 0.2045 0.073 Uiso 1 1 calc R
C3 C 0.7008(4) 0.9484(4) 0.28505(15) 0.0582(12) Uani 1 1 d .
H3 H 0.7024 0.9497 0.3167 0.070 Uiso 1 1 calc R
N1 N 0.3713(2) 0.8079(2) 0.21290(8) 0.0256(6) Uani 1 1 d .
C37 C 0.2760(4) 0.4801(3) 0.07403(13) 0.0492(10) Uani 1 1 d .
H37A H 0.2279 0.5445 0.0671 0.059 Uiso 1 1 calc R
H37B H 0.3208 0.4895 0.1037 0.059 Uiso 1 1 calc R
C41 C 0.0230(4) 0.1610(3) -0.00839(14) 0.0569(11) Uani 1 1 d .
H41A H 0.0989 0.1728 0.0113 0.068 Uiso 1 1 calc R
H41B H -0.0072 0.0898 -0.0023 0.068 Uiso 1 1 calc R
C38 C 0.3677(3) 0.4669(3) 0.04001(13) 0.0448(9) Uani 1 1 d .
H38A H 0.3232 0.4600 0.0101 0.054 Uiso 1 1 calc R
H38B H 0.4192 0.5306 0.0397 0.054 Uiso 1 1 calc R
C42 C 0.0532(4) 0.1669(4) -0.05567(14) 0.0581(12) Uani 1 1 d .
H42A H 0.0889 0.2366 -0.0608 0.070 Uiso 1 1 calc R
H42B H -0.0243 0.1614 -0.0750 0.070 Uiso 1 1 calc R
C43 C 0.1409(4) 0.0851(3) -0.06990(13) 0.0491(10) Uani 1 1 d .
O4 O 0.2366(3) 0.0703(3) -0.04015(10) 0.0655(9) Uani 1 1 d .
O3 O 0.1337(3) 0.0398(3) -0.10417(11) 0.0837(11) Uani 1 1 d .
O1 O 0.4903(3) 0.3434(2) 0.08447(10) 0.0596(8) Uani 1 1 d .
O2 O 0.4766(3) 0.3312(3) 0.01030(11) 0.0711(9) Uani 1 1 d .
C39 C 0.4492(3) 0.3745(3) 0.04830(13) 0.0432(9) Uani 1 1 d .
C40 C 0.5618(6) 0.2454(6) 0.0133(2) 0.117(3) Uani 1 1 d .
H40A H 0.6366 0.2661 0.0314 0.176 Uiso 1 1 calc R
H40B H 0.5830 0.2262 -0.0168 0.176 Uiso 1 1 calc R
H40C H 0.5241 0.1854 0.0272 0.176 Uiso 1 1 calc R
C44 C 0.3198(5) -0.0117(4) -0.04983(16) 0.0696(14) Uani 1 1 d .
H44A H 0.2754 -0.0784 -0.0519 0.104 Uiso 1 1 calc R
H44B H 0.3863 -0.0157 -0.0260 0.104 Uiso 1 1 calc R
H44C H 0.3545 0.0028 -0.0783 0.104 Uiso 1 1 calc R
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'
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
S3 Fe1 S3 103.88(3) . 3_565
S3 Fe1 S2 108.01(4) . .
S3 Fe1 S2 115.03(4) 3_565 .
S3 Fe1 S1 111.82(4) . .
S3 Fe1 S1 109.95(4) 3_565 .
S2 Fe1 S1 108.15(5) . .
S3 Fe1 Fe1 52.23(3) . 3_565
S3 Fe1 Fe1 51.65(3) 3_565 3_565
S2 Fe1 Fe1 126.46(4) . 3_565
S1 Fe1 Fe1 125.31(4) . 3_565
N1 P2 C31 110.60(14) . .
N1 P2 C25 108.61(14) . .
C31 P2 C25 107.62(14) . .
N1 P2 C19 114.61(14) . .
C31 P2 C19 107.55(14) . .
C25 P2 C19 107.60(14) . .
N1 P1 C1 109.71(15) . .
N1 P1 C7 115.44(13) . .
C1 P1 C7 108.24(16) . .
N1 P1 C13 109.23(14) . .
C1 P1 C13 107.11(14) . .
C7 P1 C13 106.76(15) . .
Fe1 S3 Fe1 76.12(3) . 3_565
C37 S1 Fe1 103.14(13) . .
C41 S2 Fe1 103.03(16) . .
C32 C31 C36 119.2(3) . .
C32 C31 P2 120.4(2) . .
C36 C31 P2 120.5(2) . .
C24 C19 C20 119.3(3) . .
C24 C19 P2 118.8(2) . .
C20 C19 P2 121.7(2) . .
C18 C13 C14 119.4(3) . .
C18 C13 P1 120.1(2) . .
C14 C13 P1 120.4(3) . .
C21 C20 C19 119.7(3) . .
C23 C24 C19 120.0(3) . .
C15 C14 C13 120.0(3) . .
C16 C15 C14 120.2(3) . .
C15 C16 C17 120.5(3) . .
C31 C32 C33 119.9(3) . .
C16 C17 C18 119.9(3) . .
C13 C18 C17 119.9(3) . .
C35 C36 C31 120.0(3) . .
C21 C22 C23 119.8(4) . .
C33 C34 C35 120.5(3) . .
C34 C35 C36 120.2(3) . .
C34 C33 C32 120.3(3) . .
C22 C21 C20 120.7(3) . .
C22 C23 C24 120.5(4) . .
C11 C12 C7 119.7(4) . .
C12 C7 C8 119.8(3) . .
C12 C7 P1 118.9(3) . .
C8 C7 P1 121.0(3) . .
C9 C10 C11 121.1(4) . .
C10 C9 C8 119.9(4) . .
C10 C11 C12 119.9(4) . .
C9 C8 C7 119.6(4) . .
C30 C25 C26 119.4(3) . .
C30 C25 P2 119.2(2) . .
C26 C25 P2 121.2(2) . .
C27 C26 C25 119.7(3) . .
C25 C30 C29 119.9(3) . .
C28 C27 C26 120.5(3) . .
C27 C28 C29 120.0(3) . .
C28 C29 C30 120.4(4) . .
C2 C1 C6 119.4(3) . .
C2 C1 P1 120.0(3) . .
C6 C1 P1 120.5(3) . .
C5 C6 C1 120.1(4) . .
C1 C2 C3 119.8(4) . .
C5 C4 C3 121.1(4) . .
C4 C5 C6 120.0(4) . .
C4 C3 C2 119.5(4) . .
P1 N1 P2 136.81(17) . .
C38 C37 S1 114.1(3) . .
C42 C41 S2 113.3(3) . .
C39 C38 C37 113.4(3) . .
C41 C42 C43 115.6(4) . .
O3 C43 O4 120.7(4) . .
O3 C43 C42 126.2(4) . .
O4 C43 C42 113.0(4) . .
C43 O4 C44 116.3(3) . .
C39 O2 C40 117.1(4) . .
O1 C39 O2 123.0(4) . .
O1 C39 C38 125.8(4) . .
O2 C39 C38 111.1(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 S3 2.1976(10) .
Fe1 S3 2.2149(10) 3_565
Fe1 S2 2.2951(12) .
Fe1 S1 2.3109(10) .
Fe1 Fe1 2.7202(10) 3_565
P2 N1 1.586(3) .
P2 C31 1.792(3) .
P2 C25 1.796(3) .
P2 C19 1.801(3) .
P1 N1 1.581(2) .
P1 C1 1.797(3) .
P1 C7 1.799(3) .
P1 C13 1.801(3) .
S3 Fe1 2.2149(10) 3_565
S1 C37 1.835(4) .
S2 C41 1.825(4) .
C31 C32 1.387(4) .
C31 C36 1.391(4) .
C19 C24 1.389(4) .
C19 C20 1.389(4) .
C13 C18 1.385(5) .
C13 C14 1.394(4) .
C20 C21 1.383(5) .
C24 C23 1.379(5) .
C14 C15 1.387(5) .
C15 C16 1.362(5) .
C16 C17 1.384(5) .
C32 C33 1.388(5) .
C17 C18 1.389(5) .
C36 C35 1.379(5) .
C22 C21 1.369(6) .
C22 C23 1.373(6) .
C34 C33 1.362(5) .
C34 C35 1.370(5) .
C12 C11 1.384(5) .
C12 C7 1.391(5) .
C7 C8 1.391(5) .
C10 C9 1.367(6) .
C10 C11 1.372(6) .
C9 C8 1.389(5) .
C25 C30 1.380(4) .
C25 C26 1.394(4) .
C26 C27 1.386(4) .
C30 C29 1.385(5) .
C27 C28 1.363(5) .
C28 C29 1.373(5) .
C1 C2 1.383(5) .
C1 C6 1.398(5) .
C6 C5 1.382(5) .
C2 C3 1.394(5) .
C4 C5 1.357(7) .
C4 C3 1.382(7) .
C37 C38 1.495(5) .
C41 C42 1.485(6) .
C38 C39 1.488(5) .
C42 C43 1.502(6) .
C43 O3 1.179(5) .
C43 O4 1.333(5) .
O4 C44 1.431(5) .
O1 C39 1.209(4) .
O2 C39 1.324(5) .
O2 C40 1.436(6) .
