# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_1
_database_code_depnum_ccdc_archive 'CCDC 1054574'
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_audit_creation_date 2018-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C16 H28 Fe3 N28 O2 S4, 2(C N S), H2 O'
_chemical_formula_sum 'C18 H30 Fe3 N30 O3 S6'
_chemical_formula_weight 1074.63
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Fe Fe 0.3463 0.8444 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_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'
_cell_length_a 10.8419(3)
_cell_length_b 11.7415(4)
_cell_length_c 31.5503(9)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4016.4(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9901
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 25.267
_cell_measurement_theta_min 2.28
_shelx_estimated_absorpt_T_max 0.868
_shelx_estimated_absorpt_T_min 0.812
_exptl_absorpt_coefficient_mu 1.451
_exptl_absorpt_correction_T_max 0.6985
_exptl_absorpt_correction_T_min 0.5947
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Sheldrick,1996)'
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.777
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2184
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0581
_diffrn_reflns_av_unetI/netI 0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_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 40
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 64948
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.595
_diffrn_reflns_theta_min 1.851
_diffrn_ambient_temperature 150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_reflns_Friedel_coverage 0.789
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 0.988
_reflns_number_gt 8126
_reflns_number_total 9202
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'Bruker SHELXTL'
_refine_diff_density_max 0.495
_refine_diff_density_min -0.489
_refine_diff_density_rms 0.067
_refine_ls_abs_structure_details
;
Flack x determined using 3282 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.015(6)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.029
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 541
_refine_ls_number_reflns 9202
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0406
_refine_ls_R_factor_gt 0.0322
_refine_ls_restrained_S_all 1.029
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+1.5114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0726
_refine_ls_wR_factor_ref 0.0763
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups, All O(H,H,H,H,H,H,H,H,H,H) groups
At 1.5 times of:
All O(H,H,H,H,H,H) groups
2.a Riding coordinates:
O3(H8A,H8B,H4A,H4B,H12A,H12B,H20A,H20B,H2A,H2B,H1A,H1B,H16A,H16B,H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
C10(H10), C11(H11), C12(H12)
2.c X=CH2 refined with riding coordinates:
N24(H24A,H24B)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.19625(5) 0.07730(5) 0.12057(2) 0.01793(12) Uani 1 1 d . . . . .
Fe2 Fe 0.32770(5) 0.11443(5) 0.23279(2) 0.02104(13) Uani 1 1 d . . . . .
Fe3 Fe 0.07153(6) 0.06240(5) 0.00701(2) 0.02338(13) Uani 1 1 d . . . . .
N1 N 0.3295(3) 0.1920(3) 0.13683(10) 0.0219(7) Uani 1 1 d . . . . .
N2 N 0.3751(3) 0.2120(3) 0.17682(10) 0.0229(7) Uani 1 1 d . . . . .
N3 N 0.4396(3) 0.3468(3) 0.13501(10) 0.0237(7) Uani 1 1 d . . . . .
N4 N 0.4916(3) 0.4519(3) 0.12316(12) 0.0290(8) Uani 1 1 d . . . . .
N5 N 0.0938(3) 0.1157(3) 0.17266(10) 0.0211(7) Uani 1 1 d . . . . .
N6 N 0.1395(3) 0.1355(3) 0.21278(10) 0.0207(7) Uani 1 1 d . . . . .
N7 N -0.0593(3) 0.1572(3) 0.21370(11) 0.0254(7) Uani 1 1 d . . . . .
N8 N -0.1775(3) 0.1835(3) 0.22925(12) 0.0329(8) Uani 1 1 d . . . . .
N9 N 0.2813(3) -0.0502(3) 0.15259(10) 0.0204(7) Uani 1 1 d . . . . .
N10 N 0.3281(3) -0.0395(3) 0.19317(10) 0.0212(7) Uani 1 1 d . . . . .
N11 N 0.3512(3) -0.2153(3) 0.17266(11) 0.0214(7) Uani 1 1 d . . . . .
N12 N 0.3872(3) -0.3312(3) 0.17424(12) 0.0289(8) Uani 1 1 d . . . . .
N13 N 0.1087(3) 0.2059(3) 0.09131(11) 0.0241(7) Uani 1 1 d . . . . .
N14 N 0.0654(4) 0.2049(3) 0.05116(11) 0.0277(8) Uani 1 1 d . . . . .
N15 N 0.0245(3) 0.3698(3) 0.07824(11) 0.0273(8) Uani 1 1 d . . . . .
N16 N -0.0206(4) 0.4816(3) 0.08122(12) 0.0358(9) Uani 1 1 d . . . . .
N17 N 0.0619(3) -0.0332(3) 0.10178(10) 0.0222(7) Uani 1 1 d . . . . .
N18 N 0.0159(3) -0.0432(3) 0.06065(11) 0.0252(8) Uani 1 1 d . . . . .
N19 N -0.0623(3) -0.1780(3) 0.09889(12) 0.0281(8) Uani 1 1 d . . . . .
N20 N -0.1254(4) -0.2799(3) 0.10872(14) 0.0389(10) Uani 1 1 d . . . . .
N21 N 0.2984(3) 0.0380(3) 0.06952(11) 0.0252(8) Uani 1 1 d . . . . .
N22 N 0.2543(3) 0.0252(3) 0.02913(11) 0.0286(8) Uani 1 1 d . . . . .
N23 N 0.4476(4) -0.0193(4) 0.02991(13) 0.0377(10) Uani 1 1 d . . . . .
N24 N 0.5656(4) -0.0471(4) 0.01524(14) 0.0534(13) Uani 1 1 d . . . . .
H24A H 0.577504 -0.061189 -0.011848 0.064 Uiso 1 1 calc R . . . .
H24B H 0.627809 -0.050478 0.033087 0.064 Uiso 1 1 calc R . . . .
N25 N 0.2789(4) 0.0128(4) 0.28427(12) 0.0412(10) Uani 1 1 d . . . . .
N26 N 0.3317(3) 0.2638(3) 0.27021(11) 0.0292(8) Uani 1 1 d . . . . .
N27 N 0.0687(4) -0.0760(3) -0.03458(11) 0.0300(8) Uani 1 1 d . . . . .
N28 N 0.1326(4) 0.1802(3) -0.03991(12) 0.0348(9) Uani 1 1 d . . . . .
N29 N 0.2705(4) 0.5259(4) 0.07360(12) 0.0355(9) Uani 1 1 d . . . . .
N30 N 0.0710(4) 0.6309(4) 0.16244(13) 0.0444(10) Uani 1 1 d . . . . .
S1 S 0.22193(12) -0.13431(12) 0.35069(4) 0.0394(3) Uani 1 1 d . . . . .
S2 S 0.31910(12) 0.45001(9) 0.32548(3) 0.0306(2) Uani 1 1 d . . . . .
S3 S 0.22783(13) 0.36970(11) -0.08220(4) 0.0394(3) Uani 1 1 d . . . . .
S4 S 0.07266(11) -0.25240(10) -0.09392(4) 0.0319(2) Uani 1 1 d . . . . .
S5 S 0.17300(12) 0.44459(11) 0.20549(4) 0.0379(3) Uani 1 1 d . . . . .
S6 S 0.23027(13) 0.73753(11) 0.03630(4) 0.0413(3) Uani 1 1 d . . . . .
C1 C 0.3715(4) 0.2737(4) 0.11223(13) 0.0244(9) Uani 1 1 d . . . . .
H1 H 0.355863 0.280010 0.082691 0.029 Uiso 1 1 calc R . . . .
C2 C 0.4390(4) 0.3066(4) 0.17494(13) 0.0247(9) Uani 1 1 d . . . . .
H2 H 0.478916 0.341684 0.198349 0.030 Uiso 1 1 calc R . . . .
C3 C -0.0249(4) 0.1290(4) 0.17407(13) 0.0241(8) Uani 1 1 d . . . . .
H3 H -0.079272 0.120284 0.150688 0.029 Uiso 1 1 calc R . . . .
C4 C 0.0452(4) 0.1606(4) 0.23673(14) 0.0261(9) Uani 1 1 d . . . . .
H4 H 0.049648 0.178608 0.266044 0.031 Uiso 1 1 calc R . . . .
C5 C 0.2975(4) -0.1563(3) 0.14075(12) 0.0238(8) Uani 1 1 d . . . . .
H5 H 0.275018 -0.186922 0.113975 0.029 Uiso 1 1 calc R . . . .
C6 C 0.3686(4) -0.1407(4) 0.20414(13) 0.0247(9) Uani 1 1 d . . . . .
H6 H 0.405014 -0.158480 0.230711 0.030 Uiso 1 1 calc R . . . .
C7 C 0.0105(4) -0.1147(3) 0.12395(14) 0.0245(8) Uani 1 1 d . . . . .
H7 H 0.022997 -0.127212 0.153393 0.029 Uiso 1 1 calc R . . . .
C8 C -0.0561(4) -0.1321(4) 0.06006(14) 0.0285(9) Uani 1 1 d . . . . .
H8 H -0.097892 -0.160169 0.035746 0.034 Uiso 1 1 calc R . . . .
C9 C 0.4148(4) 0.0097(4) 0.06938(14) 0.0309(10) Uani 1 1 d . . . . .
H9 H 0.467667 0.009773 0.093386 0.037 Uiso 1 1 calc R . . . .
C10 C 0.3458(4) -0.0113(4) 0.00618(15) 0.0357(11) Uani 1 1 d . . . . .
H10 H 0.341034 -0.029628 -0.023103 0.043 Uiso 1 1 calc R . . . .
C11 C 0.0841(4) 0.3073(4) 0.10729(13) 0.0263(9) Uani 1 1 d . . . . .
H11 H 0.105321 0.332058 0.135013 0.032 Uiso 1 1 calc R . . . .
C12 C 0.0138(5) 0.3033(4) 0.04368(15) 0.0342(11) Uani 1 1 d . . . . .
H12 H -0.025160 0.324639 0.017904 0.041 Uiso 1 1 calc R . . . .
C13 C 0.2533(4) -0.0457(4) 0.31211(14) 0.0302(10) Uani 1 1 d . . . . .
C14 C 0.3249(4) 0.3403(3) 0.29350(12) 0.0241(8) Uani 1 1 d . . . . .
C15 C 0.0703(4) -0.1495(4) -0.05875(13) 0.0244(9) Uani 1 1 d . . . . .
C16 C 0.1721(4) 0.2581(4) -0.05771(12) 0.0281(9) Uani 1 1 d . . . . .
C17 C 0.2561(4) 0.6135(5) 0.05885(15) 0.0346(11) Uani 1 1 d . . . . .
C18 C 0.1110(4) 0.5520(4) 0.18016(14) 0.0327(10) Uani 1 1 d . . . . .
O1 O 0.5221(3) 0.0960(3) 0.24400(10) 0.0450(10) Uani 1 1 d . . . . .
O2 O -0.1196(3) 0.1038(3) -0.00708(10) 0.0346(7) Uani 1 1 d . . . . .
O3 O 0.9592(4) 0.3829(4) 0.27758(13) 0.0647(12) Uani 1 1 d . . . . .
H8A H -0.210264 0.119847 0.236634 0.078 Uiso 1 1 d R . . . .
H8B H -0.216824 0.213097 0.208704 0.078 Uiso 1 1 d R . . . .
H4A H 0.567526 0.442347 0.115654 0.078 Uiso 1 1 d R . . . .
H4B H 0.441326 0.487457 0.107614 0.078 Uiso 1 1 d R . . . .
H12A H 0.451986 -0.339474 0.159094 0.078 Uiso 1 1 d R . . . .
H12B H 0.328476 -0.373593 0.169014 0.078 Uiso 1 1 d R . . . .
H20A H -0.087684 -0.313963 0.131354 0.078 Uiso 1 1 d R . . . .
H20B H -0.198724 -0.267514 0.117794 0.078 Uiso 1 1 d R . . . .
H2A H -0.153524 0.060347 -0.024826 0.097 Uiso 1 1 d R . . . .
H2B H -0.165254 0.106357 0.014744 0.097 Uiso 1 1 d R . . . .
H1A H 0.548586 0.093647 0.269234 0.097 Uiso 1 1 d R . . . .
H1B H 0.559056 0.046647 0.227964 0.097 Uiso 1 1 d R . . . .
H16A H 0.043566 0.527776 0.087534 0.078 Uiso 1 1 d R . . . .
H16B H -0.064264 0.481637 0.105714 0.078 Uiso 1 1 d R . . . .
H3A H 0.905706 0.410547 0.267944 0.097 Uiso 1 1 d R . . . .
H3B H 1.028046 0.394297 0.262084 0.097 Uiso 1 1 d R . . . .
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 0.0203(3) 0.0165(3) 0.0170(3) -0.0009(2) -0.0011(2) 0.0006(2)
Fe2 0.0260(3) 0.0204(3) 0.0167(3) -0.0009(2) -0.0019(2) -0.0009(2)
Fe3 0.0319(3) 0.0208(3) 0.0175(3) -0.0024(2) -0.0026(2) 0.0022(2)
N1 0.0278(19) 0.0217(17) 0.0164(16) -0.0009(13) -0.0015(13) 0.0027(14)
N2 0.0229(18) 0.0268(19) 0.0189(18) -0.0007(14) -0.0023(13) -0.0003(14)
N3 0.0250(18) 0.0235(18) 0.0227(17) 0.0029(14) 0.0015(14) -0.0007(14)
N4 0.0291(19) 0.0239(19) 0.034(2) 0.0047(16) 0.0015(15) -0.0028(14)
N5 0.0247(18) 0.0221(17) 0.0165(16) -0.0019(14) -0.0011(13) -0.0013(13)
N6 0.0239(18) 0.0215(18) 0.0169(16) -0.0015(14) 0.0008(13) -0.0017(13)
N7 0.0235(18) 0.0232(18) 0.0296(19) -0.0023(15) 0.0057(15) 0.0010(14)
N8 0.025(2) 0.037(2) 0.036(2) -0.0010(17) 0.0092(16) 0.0034(16)
N9 0.0237(17) 0.0212(18) 0.0163(15) 0.0005(13) -0.0009(12) -0.0009(13)
N10 0.0251(17) 0.0211(17) 0.0175(16) -0.0007(13) -0.0040(13) 0.0005(13)
N11 0.0233(18) 0.0174(17) 0.0236(17) -0.0006(14) -0.0006(13) 0.0006(12)
N12 0.032(2) 0.0184(18) 0.036(2) -0.0028(16) -0.0010(16) 0.0013(14)
N13 0.0267(19) 0.0226(18) 0.0228(18) -0.0033(14) -0.0013(14) -0.0010(14)
N14 0.036(2) 0.0229(18) 0.0240(18) 0.0008(15) -0.0009(16) 0.0063(16)
N15 0.037(2) 0.0209(18) 0.0237(18) -0.0066(15) -0.0031(15) 0.0043(15)
N16 0.056(3) 0.0203(19) 0.031(2) -0.0026(16) -0.0025(18) 0.0100(17)
N17 0.0278(18) 0.0201(17) 0.0188(16) -0.0005(13) -0.0008(13) 0.0031(14)
N18 0.0263(19) 0.0243(19) 0.0250(19) -0.0007(15) -0.0024(14) 0.0025(14)
N19 0.0253(19) 0.0193(18) 0.040(2) 0.0027(15) 0.0011(16) 0.0019(14)
N20 0.031(2) 0.024(2) 0.062(3) 0.0082(19) 0.0029(18) -0.0085(16)
N21 0.0218(19) 0.0200(18) 0.0339(19) -0.0036(14) -0.0037(14) 0.0008(14)
N22 0.031(2) 0.0254(19) 0.029(2) 0.0050(15) 0.0097(15) 0.0029(15)
N23 0.029(2) 0.042(2) 0.041(2) 0.0105(19) 0.0085(17) 0.0076(17)
N24 0.032(2) 0.090(4) 0.039(2) 0.010(2) 0.0175(19) 0.019(2)
N25 0.064(3) 0.035(2) 0.025(2) 0.0014(18) -0.0041(19) -0.006(2)
N26 0.036(2) 0.0263(19) 0.0251(18) -0.0033(16) -0.0030(16) -0.0001(16)
N27 0.040(2) 0.0282(19) 0.0214(18) -0.0040(16) -0.0048(15) 0.0052(17)
N28 0.054(3) 0.029(2) 0.022(2) 0.0001(16) -0.0001(17) -0.0035(18)
N29 0.036(2) 0.037(2) 0.034(2) 0.0079(19) 0.0022(17) -0.0007(17)
N30 0.055(3) 0.040(3) 0.038(2) 0.003(2) -0.007(2) 0.009(2)
S1 0.0408(7) 0.0465(8) 0.0310(6) 0.0129(5) -0.0020(5) -0.0121(5)
S2 0.0445(7) 0.0236(5) 0.0238(5) -0.0043(4) 0.0019(5) 0.0025(5)
S3 0.0497(8) 0.0322(7) 0.0363(7) 0.0029(5) 0.0056(5) -0.0074(5)
S4 0.0348(6) 0.0297(6) 0.0314(6) -0.0118(5) -0.0009(5) -0.0006(5)
S5 0.0490(7) 0.0313(6) 0.0336(6) -0.0022(5) -0.0067(5) 0.0078(6)
S6 0.0536(8) 0.0306(6) 0.0396(7) -0.0042(5) -0.0125(6) 0.0058(5)
C1 0.029(2) 0.024(2) 0.020(2) 0.0000(17) -0.0014(16) 0.0037(16)
C2 0.025(2) 0.027(2) 0.023(2) 0.0013(17) -0.0033(17) -0.0019(17)
C3 0.024(2) 0.026(2) 0.022(2) -0.0032(18) 0.0005(15) -0.0010(16)
C4 0.031(2) 0.024(2) 0.023(2) -0.0033(17) 0.0038(17) -0.0040(17)
C5 0.027(2) 0.026(2) 0.0177(19) -0.0028(16) -0.0031(16) 0.0007(17)
C6 0.029(2) 0.023(2) 0.022(2) -0.0015(17) -0.0048(16) 0.0015(16)
C7 0.028(2) 0.020(2) 0.025(2) -0.0007(18) 0.0020(16) 0.0019(16)
C8 0.029(2) 0.025(2) 0.031(2) 0.0015(19) -0.0022(18) 0.0012(18)
C9 0.029(3) 0.030(2) 0.033(2) 0.0004(19) 0.0011(18) 0.0000(19)
C10 0.038(3) 0.041(3) 0.028(2) 0.005(2) 0.007(2) 0.002(2)
C11 0.028(2) 0.027(2) 0.024(2) -0.0052(17) -0.0015(17) 0.0015(17)
C12 0.055(3) 0.025(2) 0.023(2) -0.0012(19) -0.008(2) 0.005(2)
C13 0.034(2) 0.033(3) 0.024(2) -0.0008(19) -0.0050(17) -0.0014(19)
C14 0.027(2) 0.026(2) 0.020(2) 0.0036(17) 0.0008(16) 0.0011(17)
C15 0.025(2) 0.026(2) 0.023(2) 0.0022(18) -0.0018(16) 0.0019(17)
C16 0.036(2) 0.030(2) 0.019(2) -0.0035(18) -0.0027(17) 0.001(2)
C17 0.023(2) 0.047(3) 0.033(3) -0.011(2) -0.0048(18) 0.006(2)
C18 0.033(2) 0.040(3) 0.025(2) -0.007(2) 0.0020(17) -0.001(2)
O1 0.0361(19) 0.066(3) 0.0331(18) -0.0208(17) -0.0129(14) 0.0177(17)
O2 0.0351(17) 0.0393(19) 0.0295(16) -0.0079(14) -0.0058(13) 0.0092(14)
O3 0.074(3) 0.061(3) 0.059(3) -0.007(2) 0.001(2) 0.013(2)
_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 N1 2.041(4) . ?
Fe1 N5 2.034(3) . ?
Fe1 N9 2.028(3) . ?
Fe1 N13 2.008(4) . ?
Fe1 N17 2.039(4) . ?
Fe1 N21 2.009(4) . ?
Fe2 N2 2.167(3) . ?
Fe2 N6 2.150(3) . ?
Fe2 N10 2.198(3) . ?
Fe2 N25 2.084(4) . ?
Fe2 N26 2.114(4) . ?
Fe2 O1 2.148(3) . ?
Fe3 N14 2.178(4) . ?
Fe3 N18 2.183(4) . ?
Fe3 N22 2.146(4) . ?
Fe3 N27 2.089(4) . ?
Fe3 N28 2.131(4) . ?
Fe3 O2 2.175(3) . ?
N1 N2 1.376(4) . ?
N1 C1 1.315(5) . ?
N2 C2 1.310(5) . ?
N3 N4 1.406(5) . ?
N3 C1 1.341(5) . ?
N3 C2 1.346(5) . ?
N4 H4A 0.8637 . ?
N4 H4B 0.8441 . ?
N5 N6 1.379(4) . ?
N5 C3 1.297(5) . ?
N6 C4 1.305(5) . ?
N7 N8 1.406(5) . ?
N7 C3 1.346(5) . ?
N7 C4 1.347(6) . ?
N8 H8A 0.8597 . ?
N8 H8B 0.8506 . ?
N9 N10 1.383(4) . ?
N9 C5 1.312(5) . ?
N10 C6 1.313(5) . ?
N11 N12 1.417(5) . ?
N11 C5 1.353(5) . ?
N11 C6 1.337(5) . ?
N12 H12A 0.8556 . ?
N12 H12B 0.8246 . ?
N13 N14 1.351(5) . ?
N13 C11 1.320(5) . ?
N14 C12 1.305(6) . ?
N15 N16 1.404(5) . ?
N15 C11 1.340(5) . ?
N15 C12 1.346(6) . ?
N16 H16A 0.9045 . ?
N16 H16B 0.9062 . ?
N17 N18 1.395(5) . ?
N17 C7 1.310(5) . ?
N18 C8 1.303(5) . ?
N19 N20 1.413(5) . ?
N19 C7 1.342(5) . ?
N19 C8 1.340(6) . ?
N20 H20A 0.9148 . ?
N20 H20B 0.8570 . ?
N21 N22 1.369(5) . ?
N21 C9 1.304(6) . ?
N22 C10 1.301(6) . ?
N23 N24 1.398(5) . ?
N23 C9 1.339(6) . ?
N23 C10 1.337(6) . ?
N24 H24A 0.8800 . ?
N24 H24B 0.8800 . ?
N25 C13 1.149(6) . ?
N26 C14 1.163(5) . ?
N27 C15 1.151(5) . ?
N28 C16 1.155(6) . ?
N29 C17 1.139(6) . ?
N30 C18 1.165(6) . ?
S1 C13 1.637(5) . ?
S2 C14 1.637(4) . ?
S3 C16 1.637(5) . ?
S4 C15 1.641(4) . ?
S5 C18 1.638(5) . ?
S6 C17 1.645(6) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
O1 H1A 0.8469 . ?
O1 H1B 0.8670 . ?
O2 H2A 0.8421 . ?
O2 H2B 0.8482 . ?
O3 H3A 0.7304 . ?
O3 H3B 0.9027 . ?
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
N5 Fe1 N1 92.15(13) . . ?
N5 Fe1 N17 89.17(13) . . ?
N9 Fe1 N1 92.32(13) . . ?
N9 Fe1 N5 90.55(13) . . ?
N9 Fe1 N17 90.00(13) . . ?
N13 Fe1 N1 87.33(14) . . ?
N13 Fe1 N5 86.95(14) . . ?
N13 Fe1 N9 177.46(14) . . ?
N13 Fe1 N17 90.41(13) . . ?
N13 Fe1 N21 93.72(14) . . ?
N17 Fe1 N1 177.32(13) . . ?
N21 Fe1 N1 87.88(13) . . ?
N21 Fe1 N5 179.34(14) . . ?
N21 Fe1 N9 88.79(13) . . ?
N21 Fe1 N17 90.83(13) . . ?
N2 Fe2 N10 88.32(12) . . ?
N6 Fe2 N2 85.71(12) . . ?
N6 Fe2 N10 85.97(12) . . ?
N25 Fe2 N2 176.61(15) . . ?
N25 Fe2 N6 93.09(15) . . ?
N25 Fe2 N10 88.44(14) . . ?
N25 Fe2 N26 92.60(15) . . ?
N25 Fe2 O1 93.61(17) . . ?
N26 Fe2 N2 90.67(13) . . ?
N26 Fe2 N6 95.05(13) . . ?
N26 Fe2 N10 178.50(15) . . ?
N26 Fe2 O1 88.38(14) . . ?
O1 Fe2 N2 87.39(14) . . ?
O1 Fe2 N6 172.33(13) . . ?
O1 Fe2 N10 90.48(13) . . ?
N14 Fe3 N18 86.11(13) . . ?
N22 Fe3 N14 88.67(14) . . ?
N22 Fe3 N18 83.55(13) . . ?
N22 Fe3 O2 172.78(13) . . ?
N27 Fe3 N14 177.28(16) . . ?
N27 Fe3 N18 92.36(14) . . ?
N27 Fe3 N22 93.39(15) . . ?
N27 Fe3 N28 94.19(14) . . ?
N27 Fe3 O2 91.82(13) . . ?
N28 Fe3 N14 87.43(14) . . ?
N28 Fe3 N18 173.16(14) . . ?
N28 Fe3 N22 94.08(15) . . ?
N28 Fe3 O2 90.51(15) . . ?
O2 Fe3 N14 85.97(13) . . ?
O2 Fe3 N18 91.26(13) . . ?
N2 N1 Fe1 126.7(3) . . ?
C1 N1 Fe1 125.3(3) . . ?
C1 N1 N2 107.0(3) . . ?
N1 N2 Fe2 124.9(3) . . ?
C2 N2 Fe2 127.6(3) . . ?
C2 N2 N1 107.0(3) . . ?
C1 N3 N4 129.8(3) . . ?
C1 N3 C2 105.9(3) . . ?
C2 N3 N4 124.0(4) . . ?
N3 N4 H4A 110.0 . . ?
N3 N4 H4B 109.3 . . ?
H4A N4 H4B 121.3 . . ?
N6 N5 Fe1 125.6(2) . . ?
C3 N5 Fe1 126.6(3) . . ?
C3 N5 N6 107.7(3) . . ?
N5 N6 Fe2 126.2(2) . . ?
C4 N6 Fe2 126.8(3) . . ?
C4 N6 N5 106.7(3) . . ?
C3 N7 N8 129.1(4) . . ?
C3 N7 C4 106.0(3) . . ?
C4 N7 N8 124.9(4) . . ?
N7 N8 H8A 106.3 . . ?
N7 N8 H8B 106.3 . . ?
H8A N8 H8B 110.7 . . ?
N10 N9 Fe1 124.1(2) . . ?
C5 N9 Fe1 128.3(3) . . ?
C5 N9 N10 107.5(3) . . ?
N9 N10 Fe2 126.9(2) . . ?
C6 N10 Fe2 126.5(3) . . ?
C6 N10 N9 106.5(3) . . ?
C5 N11 N12 129.5(3) . . ?
C6 N11 N12 124.3(3) . . ?
C6 N11 C5 106.1(3) . . ?
N11 N12 H12A 108.4 . . ?
N11 N12 H12B 111.1 . . ?
H12A N12 H12B 117.0 . . ?
N14 N13 Fe1 126.1(3) . . ?
C11 N13 Fe1 126.7(3) . . ?
C11 N13 N14 107.2(3) . . ?
N13 N14 Fe3 126.6(3) . . ?
C12 N14 Fe3 125.3(3) . . ?
C12 N14 N13 108.1(4) . . ?
C11 N15 N16 129.3(4) . . ?
C11 N15 C12 106.1(4) . . ?
C12 N15 N16 124.5(4) . . ?
N15 N16 H16A 107.9 . . ?
N15 N16 H16B 103.9 . . ?
H16A N16 H16B 102.3 . . ?
N18 N17 Fe1 125.4(3) . . ?
C7 N17 Fe1 127.8(3) . . ?
C7 N17 N18 106.4(3) . . ?
N17 N18 Fe3 125.0(3) . . ?
C8 N18 Fe3 127.5(3) . . ?
C8 N18 N17 107.1(3) . . ?
C7 N19 N20 128.6(4) . . ?
C8 N19 N20 124.5(4) . . ?
C8 N19 C7 106.6(4) . . ?
N19 N20 H20A 108.9 . . ?
N19 N20 H20B 112.2 . . ?
H20A N20 H20B 103.2 . . ?
N22 N21 Fe1 125.4(3) . . ?
C9 N21 Fe1 126.5(3) . . ?
C9 N21 N22 107.8(4) . . ?
N21 N22 Fe3 127.1(3) . . ?
C10 N22 Fe3 126.2(3) . . ?
C10 N22 N21 106.7(4) . . ?
C9 N23 N24 127.6(4) . . ?
C10 N23 N24 125.9(4) . . ?
C10 N23 C9 106.5(4) . . ?
N23 N24 H24A 120.0 . . ?
N23 N24 H24B 120.0 . . ?
H24A N24 H24B 120.0 . . ?
C13 N25 Fe2 178.2(4) . . ?
C14 N26 Fe2 172.8(4) . . ?
C15 N27 Fe3 177.0(4) . . ?
C16 N28 Fe3 165.1(4) . . ?
N1 C1 N3 110.0(4) . . ?
N1 C1 H1 125.0 . . ?
N3 C1 H1 125.0 . . ?
N2 C2 N3 110.0(4) . . ?
N2 C2 H2 125.0 . . ?
N3 C2 H2 125.0 . . ?
N5 C3 N7 109.7(4) . . ?
N5 C3 H3 125.2 . . ?
N7 C3 H3 125.2 . . ?
N6 C4 N7 109.9(4) . . ?
N6 C4 H4 125.1 . . ?
N7 C4 H4 125.1 . . ?
N9 C5 N11 109.4(3) . . ?
N9 C5 H5 125.3 . . ?
N11 C5 H5 125.3 . . ?
N10 C6 N11 110.5(3) . . ?
N10 C6 H6 124.8 . . ?
N11 C6 H6 124.8 . . ?
N17 C7 N19 109.9(4) . . ?
N17 C7 H7 125.1 . . ?
N19 C7 H7 125.1 . . ?
N18 C8 N19 109.8(4) . . ?
N18 C8 H8 125.1 . . ?
N19 C8 H8 125.1 . . ?
N21 C9 N23 109.0(4) . . ?
N21 C9 H9 125.5 . . ?
N23 C9 H9 125.5 . . ?
N22 C10 N23 109.9(4) . . ?
N22 C10 H10 125.0 . . ?
N23 C10 H10 125.0 . . ?
N13 C11 N15 109.3(4) . . ?
N13 C11 H11 125.4 . . ?
N15 C11 H11 125.4 . . ?
N14 C12 N15 109.3(4) . . ?
N14 C12 H12 125.4 . . ?
N15 C12 H12 125.4 . . ?
N25 C13 S1 176.8(5) . . ?
N26 C14 S2 178.1(4) . . ?
N27 C15 S4 178.9(4) . . ?
N28 C16 S3 179.0(4) . . ?
N29 C17 S6 177.4(5) . . ?
N30 C18 S5 177.4(5) . . ?
Fe2 O1 H1A 119.4 . . ?
Fe2 O1 H1B 115.1 . . ?
H1A O1 H1B 111.7 . . ?
Fe3 O2 H2A 114.6 . . ?
Fe3 O2 H2B 113.4 . . ?
H2A O2 H2B 107.9 . . ?
H3A O3 H3B 111.4 . . ?
_iucr_refine_instructions_details
;
TITL 1 in P2(1)2(1)2(1)
1.res
created by SHELXL-2018/1 at 11:57:59 on 08-Feb-2018
CELL 0.71073 10.8419 11.7415 31.5503 90 90 90
ZERR 4 0.0003 0.0004 0.0009 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Fe N O S
UNIT 72 120 12 120 12 24
L.S. 100
PLAN 5
SIZE 0.15 0.13 0.1
TEMP -123
BOND $H
HTAB
fmap 2
acta
OMIT 2 0 0
OMIT 0 0 2
OMIT 1 0 1
REM
REM
REM
WGHT 0.037900 1.511400
FVAR 0.30095
FE1 3 0.196254 0.077295 0.120572 11.00000 0.02025 0.01653 =
0.01702 -0.00091 -0.00115 0.00060
FE2 3 0.327698 0.114435 0.232795 11.00000 0.02598 0.02041 =
0.01672 -0.00087 -0.00191 -0.00090
FE3 3 0.071532 0.062400 0.007008 11.00000 0.03190 0.02077 =
0.01748 -0.00240 -0.00256 0.00219
N1 4 0.329469 0.192041 0.136826 11.00000 0.02777 0.02168 =
0.01636 -0.00094 -0.00155 0.00274
N2 4 0.375146 0.212006 0.176821 11.00000 0.02292 0.02677 =
0.01895 -0.00071 -0.00233 -0.00035
N3 4 0.439635 0.346830 0.135005 11.00000 0.02504 0.02347 =
0.02273 0.00289 0.00148 -0.00070
N4 4 0.491612 0.451856 0.123159 11.00000 0.02911 0.02387 =
0.03396 0.00474 0.00152 -0.00284
N5 4 0.093761 0.115651 0.172662 11.00000 0.02466 0.02209 =
0.01654 -0.00188 -0.00115 -0.00130
N6 4 0.139490 0.135512 0.212780 11.00000 0.02389 0.02148 =
0.01686 -0.00150 0.00083 -0.00167
N7 4 -0.059343 0.157198 0.213698 11.00000 0.02347 0.02325 =
0.02963 -0.00225 0.00568 0.00102
N8 4 -0.177455 0.183483 0.229253 11.00000 0.02520 0.03699 =
0.03649 -0.00097 0.00922 0.00335
N9 4 0.281337 -0.050241 0.152586 11.00000 0.02365 0.02119 =
0.01631 0.00052 -0.00086 -0.00092
N10 4 0.328142 -0.039506 0.193166 11.00000 0.02511 0.02109 =
0.01754 -0.00075 -0.00395 0.00052
N11 4 0.351163 -0.215278 0.172658 11.00000 0.02327 0.01740 =
0.02358 -0.00065 -0.00057 0.00065
N12 4 0.387153 -0.331180 0.174245 11.00000 0.03211 0.01839 =
0.03627 -0.00277 -0.00101 0.00129
N13 4 0.108722 0.205913 0.091314 11.00000 0.02673 0.02261 =
0.02285 -0.00328 -0.00129 -0.00102
N14 4 0.065398 0.204925 0.051160 11.00000 0.03624 0.02293 =
0.02397 0.00080 -0.00091 0.00627
N15 4 0.024466 0.369776 0.078236 11.00000 0.03733 0.02088 =
0.02367 -0.00657 -0.00307 0.00434
N16 4 -0.020628 0.481591 0.081216 11.00000 0.05636 0.02028 =
0.03081 -0.00256 -0.00253 0.01002
N17 4 0.061889 -0.033197 0.101776 11.00000 0.02777 0.02014 =
0.01880 -0.00052 -0.00081 0.00306
N18 4 0.015856 -0.043208 0.060650 11.00000 0.02630 0.02428 =
0.02501 -0.00068 -0.00239 0.00249
N19 4 -0.062323 -0.177994 0.098889 11.00000 0.02526 0.01930 =
0.03960 0.00273 0.00110 0.00186
N20 4 -0.125438 -0.279943 0.108724 11.00000 0.03098 0.02386 =
0.06197 0.00820 0.00294 -0.00845
N21 4 0.298419 0.037973 0.069519 11.00000 0.02182 0.02004 =
0.03386 -0.00362 -0.00366 0.00077
N22 4 0.254344 0.025169 0.029127 11.00000 0.03124 0.02540 =
0.02909 0.00497 0.00971 0.00288
N23 4 0.447625 -0.019284 0.029908 11.00000 0.02937 0.04231 =
0.04134 0.01048 0.00852 0.00756
N24 4 0.565551 -0.047086 0.015236 11.00000 0.03151 0.09001 =
0.03861 0.00994 0.01750 0.01860
AFIX 93
H24A 2 0.577504 -0.061189 -0.011848 11.00000 -1.20000
H24B 2 0.627809 -0.050478 0.033087 11.00000 -1.20000
AFIX 0
N25 4 0.278908 0.012755 0.284269 11.00000 0.06359 0.03491 =
0.02520 0.00142 -0.00413 -0.00629
N26 4 0.331720 0.263772 0.270205 11.00000 0.03635 0.02629 =
0.02508 -0.00330 -0.00304 -0.00007
N27 4 0.068738 -0.076010 -0.034585 11.00000 0.04034 0.02824 =
0.02137 -0.00404 -0.00478 0.00519
N28 4 0.132578 0.180197 -0.039909 11.00000 0.05354 0.02899 =
0.02176 0.00009 -0.00008 -0.00352
N29 4 0.270509 0.525924 0.073596 11.00000 0.03558 0.03741 =
0.03352 0.00793 0.00221 -0.00069
N30 4 0.070968 0.630863 0.162441 11.00000 0.05549 0.03989 =
0.03780 0.00254 -0.00667 0.00856
S1 6 0.221929 -0.134313 0.350691 11.00000 0.04084 0.04646 =
0.03101 0.01287 -0.00203 -0.01207
S2 6 0.319102 0.450009 0.325477 11.00000 0.04450 0.02362 =
0.02376 -0.00434 0.00187 0.00249
S3 6 0.227828 0.369697 -0.082196 11.00000 0.04965 0.03221 =
0.03625 0.00290 0.00564 -0.00740
S4 6 0.072656 -0.252403 -0.093916 11.00000 0.03478 0.02968 =
0.03137 -0.01179 -0.00085 -0.00062
S5 6 0.173000 0.444590 0.205486 11.00000 0.04896 0.03132 =
0.03355 -0.00215 -0.00670 0.00779
S6 6 0.230273 0.737527 0.036301 11.00000 0.05363 0.03057 =
0.03957 -0.00422 -0.01254 0.00585
C1 1 0.371477 0.273717 0.112227 11.00000 0.02891 0.02398 =
0.02031 -0.00002 -0.00138 0.00375
AFIX 43
H1 2 0.355863 0.280010 0.082691 11.00000 -1.20000
AFIX 0
C2 1 0.438963 0.306610 0.174944 11.00000 0.02460 0.02676 =
0.02263 0.00127 -0.00326 -0.00193
AFIX 43
H2 2 0.478916 0.341684 0.198349 11.00000 -1.20000
AFIX 0
C3 1 -0.024900 0.129033 0.174075 11.00000 0.02418 0.02594 =
0.02213 -0.00323 0.00050 -0.00100
AFIX 43
H3 2 -0.079272 0.120284 0.150688 11.00000 -1.20000
AFIX 0
C4 1 0.045213 0.160608 0.236727 11.00000 0.03132 0.02408 =
0.02283 -0.00334 0.00382 -0.00395
AFIX 43
H4 2 0.049648 0.178608 0.266044 11.00000 -1.20000
AFIX 0
C5 1 0.297489 -0.156301 0.140755 11.00000 0.02734 0.02628 =
0.01775 -0.00280 -0.00307 0.00067
AFIX 43
H5 2 0.275018 -0.186922 0.113975 11.00000 -1.20000
AFIX 0
C6 1 0.368551 -0.140715 0.204141 11.00000 0.02896 0.02282 =
0.02225 -0.00146 -0.00477 0.00149
AFIX 43
H6 2 0.405014 -0.158480 0.230711 11.00000 -1.20000
AFIX 0
C7 1 0.010529 -0.114730 0.123953 11.00000 0.02788 0.02040 =
0.02514 -0.00072 0.00201 0.00191
AFIX 43
H7 2 0.022997 -0.127212 0.153393 11.00000 -1.20000
AFIX 0
C8 1 -0.056101 -0.132103 0.060064 11.00000 0.02900 0.02502 =
0.03149 0.00145 -0.00218 0.00124
AFIX 43
H8 2 -0.097892 -0.160169 0.035746 11.00000 -1.20000
AFIX 0
C9 1 0.414781 0.009745 0.069379 11.00000 0.02947 0.02982 =
0.03346 0.00036 0.00109 0.00000
AFIX 43
H9 2 0.467667 0.009773 0.093386 11.00000 -1.20000
AFIX 0
C10 1 0.345835 -0.011330 0.006182 11.00000 0.03797 0.04148 =
0.02760 0.00478 0.00707 0.00222
AFIX 43
H10 2 0.341034 -0.029628 -0.023103 11.00000 -1.20000
AFIX 0
C11 1 0.084110 0.307285 0.107291 11.00000 0.02807 0.02712 =
0.02381 -0.00519 -0.00152 0.00154
AFIX 43
H11 2 0.105321 0.332058 0.135013 11.00000 -1.20000
AFIX 0
C12 1 0.013796 0.303305 0.043680 11.00000 0.05455 0.02512 =
0.02292 -0.00118 -0.00764 0.00549
AFIX 43
H12 2 -0.025160 0.324639 0.017904 11.00000 -1.20000
AFIX 0
C13 1 0.253275 -0.045677 0.312107 11.00000 0.03352 0.03306 =
0.02395 -0.00082 -0.00498 -0.00140
C14 1 0.324930 0.340288 0.293503 11.00000 0.02654 0.02589 =
0.01982 0.00364 0.00078 0.00110
C15 1 0.070274 -0.149475 -0.058751 11.00000 0.02452 0.02567 =
0.02304 0.00225 -0.00179 0.00192
C16 1 0.172069 0.258061 -0.057715 11.00000 0.03616 0.02959 =
0.01864 -0.00349 -0.00266 0.00105
C17 1 0.256144 0.613475 0.058849 11.00000 0.02348 0.04690 =
0.03334 -0.01145 -0.00484 0.00564
C18 1 0.110978 0.552049 0.180164 11.00000 0.03321 0.04033 =
0.02456 -0.00654 0.00202 -0.00058
O1 5 0.522096 0.095960 0.243996 11.00000 0.03608 0.06589 =
0.03313 -0.02080 -0.01289 0.01771
O2 5 -0.119636 0.103819 -0.007078 11.00000 0.03508 0.03930 =
0.02947 -0.00788 -0.00581 0.00920
O3 5 0.959156 0.382937 0.277584 11.00000 0.07442 0.06062 =
0.05902 -0.00679 0.00054 0.01300
AFIX 3
H8A 2 -0.210264 0.119847 0.236634 11.00000 -1.20000
H8B 2 -0.216824 0.213097 0.208704 11.00000 -1.20000
H4A 2 0.567526 0.442347 0.115654 11.00000 -1.20000
H4B 2 0.441326 0.487457 0.107614 11.00000 -1.20000
H12A 2 0.451986 -0.339474 0.159094 11.00000 -1.20000
H12B 2 0.328476 -0.373593 0.169014 11.00000 -1.20000
H20A 2 -0.087684 -0.313963 0.131354 11.00000 -1.20000
H20B 2 -0.198724 -0.267514 0.117794 11.00000 -1.20000
H2A 2 -0.153524 0.060347 -0.024826 11.00000 -1.50000
H2B 2 -0.165254 0.106357 0.014744 11.00000 -1.50000
H1A 2 0.548586 0.093647 0.269234 11.00000 -1.50000
H1B 2 0.559056 0.046647 0.227964 11.00000 -1.50000
H16A 2 0.043566 0.527776 0.087534 11.00000 -1.20000
H16B 2 -0.064264 0.481637 0.105714 11.00000 -1.20000
H3A 2 0.905706 0.410547 0.267944 11.00000 -1.50000
H3B 2 1.028046 0.394297 0.262084 11.00000 -1.50000
AFIX 0
HKLF 4
REM 1 in P2(1)2(1)2(1)
REM R1 = 0.0322 for 8126 Fo > 4sig(Fo) and 0.0406 for all 9202 data
REM 541 parameters refined using 0 restraints
END
WGHT 0.0381 1.4890
REM Instructions for potential hydrogen bonds
EQIV $1 x+1/2, -y+1/2, -z
HTAB N24 N16_$1
HTAB N24 S6_$1
HTAB N24 S3_$1
EQIV $2 x-1/2, -y+1/2, -z
HTAB C3 S3_$2
EQIV $3 -x, y-1/2, -z+1/2
HTAB C4 N30_$3
EQIV $4 x, y-1, z
HTAB C5 S6_$4
EQIV $5 -x+1, y-1/2, -z+1/2
HTAB C7 O3_$5
HTAB C10 N16_$1
HTAB C11 S5
HTAB N8 S5_$3
EQIV $6 -x, y+1/2, -z+1/2
HTAB N8 S1_$6
EQIV $7 -x+1, y+1/2, -z+1/2
HTAB N4 S1_$7
HTAB N4 N29
EQIV $8 x+1/2, -y-1/2, -z
HTAB N12 S4_$8
HTAB N12 S5_$4
HTAB N20 N30_$4
EQIV $9 x-1/2, -y-1/2, -z
HTAB N20 S4_$9
HTAB O2 N29_$2
HTAB O2 S3_$2
HTAB O1 N12_$7
HTAB O1 S2_$5
HTAB N16 N29
HTAB N16 N30
HTAB N16 S1_$6
EQIV $10 x+1, y, z
HTAB O3 S5_$10
REM Highest difference peak 0.495, deepest hole -0.489, 1-sigma level 0.067
Q1 1 0.3022 0.0694 0.0447 11.00000 0.05 0.50
Q2 1 0.2038 -0.0628 0.3633 11.00000 0.05 0.44
Q3 1 0.5294 -0.1252 0.0060 11.00000 0.05 0.38
Q4 1 0.1733 0.3968 -0.0678 11.00000 0.05 0.36
Q5 1 0.3510 0.1756 0.1980 11.00000 0.05 0.31
REM The information below was added by Olex2.
REM
REM R1 = 0.0322 for 8126 Fo > 4sig(Fo) and 0.0406 for all 65079 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.50, deepest hole -0.49
REM Mean Shift 0, Max Shift 0.001.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0406
REM R1_gt = 0.0322
REM wR_ref = 0.0763
REM GOOF = 1.029
REM Shift_max = 0.001
REM Shift_mean = 0
REM Reflections_all = 65079
REM Reflections_gt = 8126
REM Parameters = n/a
REM Hole = -0.49
REM Peak = 0.50
REM Flack = 0.015(6)
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1054575'
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_audit_creation_date 2018-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C16 H28 Fe3 N28 O2 S4, 2(C N S), H2 O'
_chemical_formula_sum 'C18 H30 Fe3 N30 O3 S6'
_chemical_formula_weight 1074.63
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Fe Fe 0.3463 0.8444 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_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'
_cell_length_a 11.025(10)
_cell_length_b 11.863(11)
_cell_length_c 32.15(3)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4205(7)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2110
_cell_measurement_temperature 296(2)
_cell_measurement_theta_max 23.512
_cell_measurement_theta_min 3.159
_shelx_estimated_absorpt_T_max 0.874
_shelx_estimated_absorpt_T_min 0.819
_exptl_absorpt_coefficient_mu 1.386
_exptl_absorpt_correction_T_max 0.6972
_exptl_absorpt_correction_T_min 0.5932
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'SADABS (Sheldrick,1996)'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.698
_exptl_crystal_density_meas .
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2184
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0453
_diffrn_reflns_av_unetI/netI 0.0939
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -8
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_l_max 41
_diffrn_reflns_limit_l_min -31
_diffrn_reflns_number 12897
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.475
_diffrn_reflns_theta_min 3.159
_diffrn_ambient_temperature 296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type 'CCD area detector'
_diffrn_measurement_method 'phi and omega scans'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.658
_reflns_Friedel_fraction_full 0.834
_reflns_Friedel_fraction_max 0.797
_reflns_number_gt 5649
_reflns_number_total 8554
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection 'Bruker SMART'
_computing_data_reduction 'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'Bruker SHELXTL'
_refine_diff_density_max 0.418
_refine_diff_density_min -0.348
_refine_diff_density_rms 0.074
_refine_ls_abs_structure_details
;
Flack x determined using 1720 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.047(18)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.989
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 541
_refine_ls_number_reflns 8554
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0934
_refine_ls_R_factor_gt 0.0494
_refine_ls_restrained_S_all 0.989
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0916
_refine_ls_wR_factor_ref 0.1070
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups, All O(H,H,H,H,H,H,H,H) groups
At 1.5 times of:
All O(H,H) groups, All O(H,H,H,H) groups
2.a Riding coordinates:
N12(H12A,H12B), O1(H1A,H1B), O3(H3A,H3B), O3(H8A,H8B,H2A,H2B,H4A,H4B,H16A,
H16B,H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
C10(H10), C11(H11), C12(H12)
2.c X=CH2 refined with riding coordinates:
N24(H24A,H24B)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.18840(10) 0.07446(7) 0.11999(3) 0.0303(2) Uani 1 1 d . . . . .
Fe2 Fe 0.31965(10) 0.11483(8) 0.23238(3) 0.0349(2) Uani 1 1 d . . . . .
Fe3 Fe 0.06026(10) 0.06243(8) 0.00642(3) 0.0382(3) Uani 1 1 d . . . . .
N1 N 0.3324(6) 0.1938(5) 0.13739(16) 0.0367(14) Uani 1 1 d . . . . .
N2 N 0.3690(5) 0.2147(5) 0.17781(17) 0.0353(14) Uani 1 1 d . . . . .
N3 N 0.4323(6) 0.3513(4) 0.13772(17) 0.0366(14) Uani 1 1 d . . . . .
N4 N 0.4814(6) 0.4567(5) 0.1264(2) 0.0497(17) Uani 1 1 d . . . . .
N5 N 0.0836(6) 0.1180(5) 0.17518(16) 0.0360(14) Uani 1 1 d . . . . .
N6 N 0.1300(5) 0.1364(5) 0.21463(17) 0.0354(14) Uani 1 1 d . . . . .
N7 N -0.0658(6) 0.1603(5) 0.21665(18) 0.0423(15) Uani 1 1 d . . . . .
N8 N -0.1833(7) 0.1855(6) 0.2323(2) 0.0610(19) Uani 1 1 d . . . . .
N9 N 0.2770(5) -0.0596(5) 0.15447(16) 0.0375(14) Uani 1 1 d . . . . .
N10 N 0.3232(6) -0.0431(4) 0.19438(15) 0.0341(13) Uani 1 1 d . . . . .
N11 N 0.3485(5) -0.2193(4) 0.17696(16) 0.0327(13) Uani 1 1 d . . . . .
N12 N 0.3858(6) -0.3330(5) 0.17994(18) 0.0430(16) Uani 1 1 d . . . . .
H12A H 0.440631 -0.345299 0.159725 0.052 Uiso 1 1 d R . . . .
H12B H 0.320911 -0.376349 0.174285 0.052 Uiso 1 1 d R . . . .
N13 N 0.0969(6) 0.2109(5) 0.08846(17) 0.0378(15) Uani 1 1 d . . . . .
N14 N 0.0512(7) 0.2061(5) 0.04946(17) 0.0428(16) Uani 1 1 d . . . . .
N15 N 0.0103(6) 0.3699(5) 0.07583(17) 0.0414(15) Uani 1 1 d . . . . .
N16 N -0.0348(8) 0.4812(5) 0.0791(2) 0.060(2) Uani 1 1 d . . . . .
N17 N 0.0432(6) -0.0388(4) 0.09951(16) 0.0364(14) Uani 1 1 d . . . . .
N18 N 0.0000(6) -0.0453(5) 0.05856(17) 0.0385(14) Uani 1 1 d . . . . .
N19 N -0.0773(6) -0.1811(5) 0.0943(2) 0.0433(15) Uani 1 1 d . . . . .
N20 N -0.1388(6) -0.2846(5) 0.1030(2) 0.061(2) Uani 1 1 d . . . . .
N21 N 0.2927(5) 0.0361(5) 0.06493(18) 0.0379(14) Uani 1 1 d . . . . .
N22 N 0.2436(6) 0.0194(5) 0.02606(17) 0.0415(15) Uani 1 1 d . . . . .
N23 N 0.4309(7) -0.0364(6) 0.0251(2) 0.0560(18) Uani 1 1 d . . . . .
N24 N 0.5434(8) -0.0742(9) 0.0113(2) 0.109(4) Uani 1 1 d . . . . .
H24A H 0.552152 -0.096011 -0.014051 0.130 Uiso 1 1 calc R . . . .
H24B H 0.604116 -0.075682 0.028056 0.130 Uiso 1 1 calc R . . . .
N25 N 0.2722(7) 0.0153(6) 0.2839(2) 0.060(2) Uani 1 1 d . . . . .
N26 N 0.3283(7) 0.2633(5) 0.26902(19) 0.0500(16) Uani 1 1 d . . . . .
N27 N 0.0568(7) -0.0754(5) -0.03520(18) 0.0503(16) Uani 1 1 d . . . . .
N28 N 0.1221(8) 0.1779(7) -0.0396(2) 0.061(2) Uani 1 1 d . . . . .
N29 N 0.2603(7) 0.5211(7) 0.0736(2) 0.062(2) Uani 1 1 d . . . . .
N30 N 0.0531(9) 0.6279(7) 0.1599(2) 0.078(2) Uani 1 1 d . . . . .
S1 S 0.2318(2) -0.1334(2) 0.34944(7) 0.0707(7) Uani 1 1 d . . . . .
S2 S 0.3207(2) 0.44683(17) 0.32372(6) 0.0570(6) Uani 1 1 d . . . . .
S3 S 0.2110(3) 0.3683(2) -0.08011(8) 0.0716(7) Uani 1 1 d . . . . .
S4 S 0.0616(2) -0.24620(18) -0.09513(6) 0.0560(6) Uani 1 1 d . . . . .
S5 S 0.1632(3) 0.4493(2) 0.20154(7) 0.0681(7) Uani 1 1 d . . . . .
S6 S 0.2216(3) 0.7338(2) 0.04143(8) 0.0698(7) Uani 1 1 d . . . . .
C1 C 0.3732(7) 0.2761(6) 0.1138(2) 0.0375(17) Uani 1 1 d . . . . .
H1 H 0.362740 0.281552 0.085128 0.045 Uiso 1 1 calc R . . . .
C2 C 0.4276(7) 0.3115(6) 0.1771(2) 0.0373(17) Uani 1 1 d . . . . .
H2 H 0.460747 0.347155 0.200193 0.045 Uiso 1 1 calc R . . . .
C3 C -0.0347(7) 0.1330(6) 0.1773(2) 0.0401(17) Uani 1 1 d . . . . .
H3 H -0.088406 0.125968 0.155108 0.048 Uiso 1 1 calc R . . . .
C4 C 0.0386(7) 0.1633(6) 0.2385(2) 0.0431(19) Uani 1 1 d . . . . .
H4 H 0.044558 0.181802 0.266521 0.052 Uiso 1 1 calc R . . . .
C5 C 0.2930(7) -0.1655(6) 0.1449(2) 0.0347(17) Uani 1 1 d . . . . .
H5 H 0.269903 -0.199001 0.120015 0.042 Uiso 1 1 calc R . . . .
C6 C 0.3651(7) -0.1407(6) 0.2065(2) 0.0374(17) Uani 1 1 d . . . . .
H6 H 0.401544 -0.154017 0.232121 0.045 Uiso 1 1 calc R . . . .
C7 C -0.0071(7) -0.1205(6) 0.1201(2) 0.0380(16) Uani 1 1 d . . . . .
H7 H 0.003659 -0.134792 0.148316 0.046 Uiso 1 1 calc R . . . .
C8 C -0.0694(8) -0.1344(6) 0.0568(2) 0.0460(19) Uani 1 1 d . . . . .
H8 H -0.107556 -0.161110 0.032997 0.055 Uiso 1 1 calc R . . . .
C9 C 0.4056(8) 0.0022(7) 0.0638(3) 0.049(2) Uani 1 1 d . . . . .
H9 H 0.459710 0.004280 0.085948 0.058 Uiso 1 1 calc R . . . .
C10 C 0.3265(8) -0.0282(7) 0.0035(3) 0.054(2) Uani 1 1 d . . . . .
H10 H 0.315531 -0.053035 -0.023722 0.065 Uiso 1 1 calc R . . . .
C11 C 0.0711(8) 0.3122(6) 0.1039(2) 0.0426(18) Uani 1 1 d . . . . .
H11 H 0.092557 0.337957 0.130241 0.051 Uiso 1 1 calc R . . . .
C12 C -0.0013(9) 0.3033(6) 0.0422(2) 0.052(2) Uani 1 1 d . . . . .
H12 H -0.040343 0.323109 0.017612 0.062 Uiso 1 1 calc R . . . .
C13 C 0.2539(8) -0.0441(7) 0.3116(2) 0.050(2) Uani 1 1 d . . . . .
C14 C 0.3230(8) 0.3392(6) 0.2920(2) 0.0430(18) Uani 1 1 d . . . . .
C15 C 0.0593(7) -0.1456(6) -0.0601(2) 0.0414(17) Uani 1 1 d . . . . .
C16 C 0.1600(8) 0.2557(8) -0.0564(2) 0.048(2) Uani 1 1 d . . . . .
C17 C 0.2472(8) 0.6101(9) 0.0607(3) 0.057(2) Uani 1 1 d . . . . .
C18 C 0.0990(8) 0.5525(8) 0.1767(2) 0.051(2) Uani 1 1 d . . . . .
O1 O 0.5118(5) 0.0898(5) 0.24334(16) 0.0684(18) Uani 1 1 d . . . . .
H1A H 0.540382 0.032460 0.230884 0.103 Uiso 1 1 d R . . . .
H1B H 0.530352 0.088570 0.268994 0.103 Uiso 1 1 d R . . . .
O2 O -0.1300(5) 0.1034(5) -0.00684(15) 0.0565(15) Uani 1 1 d . . . . .
O3 O 0.9696(11) 0.3847(7) 0.2790(3) 0.149(4) Uani 1 1 d . . . . .
H3A H 0.905688 0.411568 0.268026 0.223 Uiso 1 1 d R . . . .
H3B H 1.028018 0.395318 0.262166 0.223 Uiso 1 1 d R . . . .
H8A H -0.199772 0.121658 0.238016 0.178 Uiso 1 1 d R . . . .
H8B H -0.206322 0.214908 0.210086 0.178 Uiso 1 1 d R . . . .
H2A H -0.143042 0.062148 -0.023454 0.223 Uiso 1 1 d R . . . .
H2B H -0.154772 0.108158 0.016146 0.223 Uiso 1 1 d R . . . .
H4A H 0.557148 0.453748 0.117276 0.178 Uiso 1 1 d R . . . .
H4B H 0.441518 0.490518 0.106356 0.178 Uiso 1 1 d R . . . .
H16A H 0.024458 0.522848 0.089666 0.178 Uiso 1 1 d R . . . .
H16B H -0.083272 0.470768 0.100916 0.178 Uiso 1 1 d R . . . .
H20A H -0.096122 -0.318922 0.123696 0.178 Uiso 1 1 d R . . . .
H20B H -0.210262 -0.276632 0.115216 0.178 Uiso 1 1 d R . . . .
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 0.0336(5) 0.0299(5) 0.0274(4) -0.0015(4) -0.0031(4) 0.0019(4)
Fe2 0.0411(6) 0.0353(5) 0.0281(5) -0.0019(4) -0.0035(5) -0.0008(5)
Fe3 0.0501(6) 0.0363(6) 0.0283(5) -0.0048(4) -0.0049(5) 0.0052(5)
N1 0.044(4) 0.036(3) 0.031(3) -0.003(2) -0.002(3) -0.005(3)
N2 0.035(3) 0.038(4) 0.032(3) -0.001(3) -0.004(3) -0.001(3)
N3 0.038(3) 0.034(3) 0.038(3) 0.005(3) -0.001(3) -0.004(3)
N4 0.058(4) 0.031(3) 0.061(4) 0.002(3) 0.003(4) -0.015(3)
N5 0.039(4) 0.040(3) 0.030(3) -0.006(3) -0.003(3) 0.001(3)
N6 0.037(3) 0.041(4) 0.028(3) -0.006(3) 0.000(3) 0.001(3)
N7 0.042(4) 0.039(3) 0.045(3) -0.001(3) 0.011(3) 0.005(3)
N8 0.045(4) 0.069(4) 0.069(4) -0.001(4) 0.029(4) 0.008(4)
N9 0.045(4) 0.036(3) 0.031(3) -0.005(3) -0.008(3) 0.001(3)
N10 0.040(3) 0.032(3) 0.030(3) -0.003(2) -0.012(3) 0.005(3)
N11 0.038(4) 0.025(3) 0.034(3) 0.000(2) -0.004(3) 0.001(2)
N12 0.052(4) 0.028(3) 0.048(4) -0.003(3) -0.006(3) 0.004(3)
N13 0.049(4) 0.032(3) 0.032(3) -0.003(3) -0.007(3) 0.006(3)
N14 0.063(5) 0.032(3) 0.034(3) 0.001(3) -0.006(3) 0.009(3)
N15 0.054(4) 0.034(3) 0.036(3) -0.004(3) -0.007(3) 0.012(3)
N16 0.095(6) 0.033(4) 0.053(4) -0.005(3) -0.009(4) 0.024(4)
N17 0.045(4) 0.033(3) 0.031(3) -0.003(2) -0.005(3) -0.003(3)
N18 0.047(4) 0.036(3) 0.033(3) -0.005(3) -0.005(3) 0.003(3)
N19 0.036(4) 0.033(3) 0.060(4) 0.000(3) -0.003(3) -0.004(3)
N20 0.053(4) 0.040(4) 0.089(5) 0.003(4) 0.000(4) -0.018(3)
N21 0.030(4) 0.041(3) 0.042(3) -0.008(3) -0.004(3) 0.001(3)
N22 0.047(4) 0.044(4) 0.033(3) 0.003(3) 0.008(3) -0.002(3)
N23 0.042(4) 0.072(5) 0.054(4) 0.013(3) 0.015(4) 0.014(4)
N24 0.067(6) 0.194(10) 0.065(5) 0.017(6) 0.027(5) 0.067(7)
N25 0.093(6) 0.053(4) 0.035(3) 0.004(3) 0.001(4) -0.008(4)
N26 0.059(4) 0.048(4) 0.042(3) -0.008(3) -0.004(4) -0.001(4)
N27 0.070(5) 0.045(4) 0.036(3) -0.008(3) -0.008(3) 0.004(4)
N28 0.091(6) 0.056(5) 0.037(4) 0.002(3) 0.003(4) -0.004(4)
N29 0.068(5) 0.060(5) 0.057(5) 0.005(4) 0.005(4) -0.003(4)
N30 0.106(7) 0.073(6) 0.053(4) 0.005(4) -0.015(5) 0.007(5)
S1 0.0703(17) 0.0844(18) 0.0575(13) 0.0296(13) -0.0088(12) -0.0222(13)
S2 0.0813(16) 0.0430(12) 0.0465(10) -0.0113(9) 0.0073(12) 0.0014(13)
S3 0.086(2) 0.0580(14) 0.0706(15) 0.0112(12) 0.0040(14) -0.0149(13)
S4 0.0571(13) 0.0578(13) 0.0530(11) -0.0235(10) -0.0006(12) -0.0016(11)
S5 0.0831(19) 0.0610(15) 0.0600(13) -0.0049(12) -0.0097(13) 0.0152(14)
S6 0.084(2) 0.0542(14) 0.0713(15) -0.0063(12) -0.0242(14) 0.0038(12)
C1 0.048(5) 0.034(4) 0.030(3) -0.003(3) -0.004(3) 0.000(3)
C2 0.038(4) 0.040(4) 0.034(4) -0.001(3) -0.006(4) -0.007(3)
C3 0.038(4) 0.044(4) 0.038(4) -0.005(3) -0.002(4) -0.002(3)
C4 0.046(5) 0.050(5) 0.033(4) -0.005(3) 0.004(4) 0.000(4)
C5 0.040(5) 0.038(4) 0.026(3) -0.007(3) -0.003(3) 0.004(3)
C6 0.046(4) 0.032(4) 0.034(4) -0.004(3) -0.010(3) -0.003(3)
C7 0.038(4) 0.041(4) 0.035(4) -0.003(4) -0.001(3) -0.002(3)
C8 0.052(5) 0.040(4) 0.045(4) -0.005(4) -0.010(4) 0.000(4)
C9 0.040(5) 0.060(5) 0.046(5) 0.002(4) 0.001(4) 0.006(4)
C10 0.054(5) 0.065(5) 0.043(4) 0.000(4) 0.011(5) 0.011(4)
C11 0.054(5) 0.042(4) 0.032(4) -0.007(3) -0.007(4) 0.005(4)
C12 0.082(7) 0.044(5) 0.030(4) -0.005(3) -0.019(4) 0.015(4)
C13 0.058(5) 0.051(5) 0.043(4) 0.000(4) -0.008(4) -0.004(4)
C14 0.053(5) 0.044(4) 0.032(4) 0.002(3) 0.007(4) -0.003(4)
C15 0.041(4) 0.045(4) 0.038(4) -0.001(3) -0.011(4) 0.001(4)
C16 0.058(6) 0.059(5) 0.028(4) -0.008(4) -0.001(4) -0.001(4)
C17 0.047(5) 0.062(6) 0.061(5) -0.017(5) -0.001(4) -0.001(5)
C18 0.054(5) 0.068(6) 0.032(4) -0.006(4) -0.002(4) -0.004(5)
O1 0.055(4) 0.099(5) 0.051(3) -0.031(3) -0.019(3) 0.023(3)
O2 0.059(4) 0.068(4) 0.043(3) -0.009(3) -0.008(3) 0.017(3)
O3 0.190(11) 0.127(7) 0.128(7) -0.008(6) 0.018(7) 0.030(7)
_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 N1 2.200(6) . ?
Fe1 N5 2.179(6) . ?
Fe1 N9 2.170(6) . ?
Fe1 N13 2.160(6) . ?
Fe1 N17 2.191(6) . ?
Fe1 N21 2.159(6) . ?
Fe2 N2 2.185(6) . ?
Fe2 N6 2.182(6) . ?
Fe2 N10 2.237(5) . ?
Fe2 N25 2.102(7) . ?
Fe2 N26 2.121(6) . ?
Fe2 O1 2.168(6) . ?
Fe3 N14 2.198(6) . ?
Fe3 N18 2.210(6) . ?
Fe3 N22 2.178(7) . ?
Fe3 N27 2.113(6) . ?
Fe3 N28 2.129(8) . ?
Fe3 O2 2.195(6) . ?
N1 N2 1.383(7) . ?
N1 C1 1.316(8) . ?
N2 C2 1.318(9) . ?
N3 N4 1.410(7) . ?
N3 C1 1.347(8) . ?
N3 C2 1.351(8) . ?
N4 H4A 0.8859 . ?
N4 H4B 0.8760 . ?
N5 N6 1.385(7) . ?
N5 C3 1.319(9) . ?
N6 C4 1.306(9) . ?
N7 N8 1.422(9) . ?
N7 C3 1.351(8) . ?
N7 C4 1.348(9) . ?
N8 H8A 0.8004 . ?
N8 H8B 0.8339 . ?
N9 N10 1.394(7) . ?
N9 C5 1.306(8) . ?
N10 C6 1.306(8) . ?
N11 N12 1.413(7) . ?
N11 C5 1.357(8) . ?
N11 C6 1.343(8) . ?
N12 H12A 0.8997 . ?
N12 H12B 0.8999 . ?
N13 N14 1.352(7) . ?
N13 C11 1.331(8) . ?
N14 C12 1.311(9) . ?
N15 N16 1.414(8) . ?
N15 C11 1.317(9) . ?
N15 C12 1.346(9) . ?
N16 H16A 0.8864 . ?
N16 H16B 0.8899 . ?
N17 N18 1.403(7) . ?
N17 C7 1.298(8) . ?
N18 C8 1.306(9) . ?
N19 N20 1.431(8) . ?
N19 C7 1.344(9) . ?
N19 C8 1.327(9) . ?
N20 H20A 0.9113 . ?
N20 H20B 0.8858 . ?
N21 N22 1.376(8) . ?
N21 C9 1.309(10) . ?
N22 C10 1.297(9) . ?
N23 N24 1.391(10) . ?
N23 C9 1.354(9) . ?
N23 C10 1.349(11) . ?
N24 H24A 0.8600 . ?
N24 H24B 0.8600 . ?
N25 C13 1.152(9) . ?
N26 C14 1.166(8) . ?
N27 C15 1.155(8) . ?
N28 C16 1.149(9) . ?
N29 C17 1.143(10) . ?
N30 C18 1.160(10) . ?
S1 C13 1.631(9) . ?
S2 C14 1.634(8) . ?
S3 C16 1.637(10) . ?
S4 C15 1.641(8) . ?
S5 C18 1.625(10) . ?
S6 C17 1.617(11) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
O1 H1A 0.8502 . ?
O1 H1B 0.8497 . ?
O2 H2A 0.7382 . ?
O2 H2B 0.7900 . ?
O3 H3A 0.8498 . ?
O3 H3B 0.8498 . ?
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
N5 Fe1 N1 91.3(2) . . ?
N5 Fe1 N17 90.1(2) . . ?
N9 Fe1 N1 91.0(2) . . ?
N9 Fe1 N5 89.8(2) . . ?
N9 Fe1 N17 91.9(2) . . ?
N13 Fe1 N1 88.5(2) . . ?
N13 Fe1 N5 87.5(2) . . ?
N13 Fe1 N9 177.3(2) . . ?
N13 Fe1 N17 88.7(2) . . ?
N17 Fe1 N1 176.8(2) . . ?
N21 Fe1 N1 87.7(2) . . ?
N21 Fe1 N5 178.5(2) . . ?
N21 Fe1 N9 91.4(2) . . ?
N21 Fe1 N13 91.2(2) . . ?
N21 Fe1 N17 90.8(2) . . ?
N2 Fe2 N10 90.6(2) . . ?
N6 Fe2 N2 88.0(2) . . ?
N6 Fe2 N10 88.4(2) . . ?
N25 Fe2 N2 178.6(2) . . ?
N25 Fe2 N6 91.9(3) . . ?
N25 Fe2 N10 88.0(2) . . ?
N25 Fe2 N26 92.3(3) . . ?
N25 Fe2 O1 92.2(3) . . ?
N26 Fe2 N2 89.1(2) . . ?
N26 Fe2 N6 95.2(2) . . ?
N26 Fe2 N10 176.4(3) . . ?
N26 Fe2 O1 88.8(2) . . ?
O1 Fe2 N2 87.8(2) . . ?
O1 Fe2 N6 174.1(2) . . ?
O1 Fe2 N10 87.5(2) . . ?
N14 Fe3 N18 87.6(2) . . ?
N22 Fe3 N14 92.4(2) . . ?
N22 Fe3 N18 85.6(2) . . ?
N22 Fe3 O2 174.2(2) . . ?
N27 Fe3 N14 176.4(3) . . ?
N27 Fe3 N18 91.6(2) . . ?
N27 Fe3 N22 91.1(3) . . ?
N27 Fe3 N28 93.6(3) . . ?
N27 Fe3 O2 91.8(2) . . ?
N28 Fe3 N14 87.3(3) . . ?
N28 Fe3 N18 174.7(2) . . ?
N28 Fe3 N22 93.2(3) . . ?
N28 Fe3 O2 91.7(3) . . ?
O2 Fe3 N14 84.7(2) . . ?
O2 Fe3 N18 89.3(2) . . ?
N2 N1 Fe1 124.4(4) . . ?
C1 N1 Fe1 125.3(5) . . ?
C1 N1 N2 108.1(5) . . ?
N1 N2 Fe2 125.8(4) . . ?
C2 N2 Fe2 127.5(5) . . ?
C2 N2 N1 106.4(5) . . ?
C1 N3 N4 128.7(6) . . ?
C1 N3 C2 106.6(6) . . ?
C2 N3 N4 124.5(6) . . ?
N3 N4 H4A 114.3 . . ?
N3 N4 H4B 113.8 . . ?
H4A N4 H4B 104.4 . . ?
N6 N5 Fe1 125.9(4) . . ?
C3 N5 Fe1 126.7(5) . . ?
C3 N5 N6 107.3(6) . . ?
N5 N6 Fe2 125.1(4) . . ?
C4 N6 Fe2 127.9(5) . . ?
C4 N6 N5 106.9(6) . . ?
C3 N7 N8 127.8(7) . . ?
C4 N7 N8 126.0(6) . . ?
C4 N7 C3 106.2(6) . . ?
N7 N8 H8A 95.1 . . ?
N7 N8 H8B 93.6 . . ?
H8A N8 H8B 121.6 . . ?
N10 N9 Fe1 122.1(4) . . ?
C5 N9 Fe1 130.3(4) . . ?
C5 N9 N10 107.5(5) . . ?
N9 N10 Fe2 127.9(4) . . ?
C6 N10 Fe2 125.9(4) . . ?
C6 N10 N9 106.2(5) . . ?
C5 N11 N12 129.2(5) . . ?
C6 N11 N12 125.1(6) . . ?
C6 N11 C5 105.8(5) . . ?
N11 N12 H12A 107.6 . . ?
N11 N12 H12B 107.5 . . ?
H12A N12 H12B 107.2 . . ?
N14 N13 Fe1 125.3(4) . . ?
C11 N13 Fe1 126.9(5) . . ?
C11 N13 N14 107.7(5) . . ?
N13 N14 Fe3 126.8(4) . . ?
C12 N14 Fe3 126.1(5) . . ?
C12 N14 N13 107.1(5) . . ?
C11 N15 N16 127.8(6) . . ?
C11 N15 C12 107.1(6) . . ?
C12 N15 N16 125.1(6) . . ?
N15 N16 H16A 106.9 . . ?
N15 N16 H16B 98.1 . . ?
H16A N16 H16B 102.6 . . ?
N18 N17 Fe1 124.4(4) . . ?
C7 N17 Fe1 128.1(4) . . ?
C7 N17 N18 107.0(5) . . ?
N17 N18 Fe3 125.3(4) . . ?
C8 N18 Fe3 127.8(5) . . ?
C8 N18 N17 106.5(6) . . ?
C7 N19 N20 127.6(6) . . ?
C8 N19 N20 124.5(7) . . ?
C8 N19 C7 107.5(6) . . ?
N19 N20 H20A 106.4 . . ?
N19 N20 H20B 114.6 . . ?
H20A N20 H20B 100.5 . . ?
N22 N21 Fe1 124.4(5) . . ?
C9 N21 Fe1 126.5(5) . . ?
C9 N21 N22 107.7(6) . . ?
N21 N22 Fe3 126.5(5) . . ?
C10 N22 Fe3 126.4(5) . . ?
C10 N22 N21 107.1(7) . . ?
C9 N23 N24 125.9(8) . . ?
C10 N23 N24 128.2(7) . . ?
C10 N23 C9 105.9(7) . . ?
N23 N24 H24A 120.0 . . ?
N23 N24 H24B 120.0 . . ?
H24A N24 H24B 120.0 . . ?
C13 N25 Fe2 174.8(8) . . ?
C14 N26 Fe2 172.2(6) . . ?
C15 N27 Fe3 174.8(6) . . ?
C16 N28 Fe3 164.0(6) . . ?
N1 C1 N3 109.1(6) . . ?
N1 C1 H1 125.5 . . ?
N3 C1 H1 125.5 . . ?
N2 C2 N3 109.9(6) . . ?
N2 C2 H2 125.1 . . ?
N3 C2 H2 125.1 . . ?
N5 C3 N7 109.3(6) . . ?
N5 C3 H3 125.3 . . ?
N7 C3 H3 125.3 . . ?
N6 C4 N7 110.3(6) . . ?
N6 C4 H4 124.9 . . ?
N7 C4 H4 124.9 . . ?
N9 C5 N11 109.6(6) . . ?
N9 C5 H5 125.2 . . ?
N11 C5 H5 125.2 . . ?
N10 C6 N11 110.9(6) . . ?
N10 C6 H6 124.6 . . ?
N11 C6 H6 124.6 . . ?
N17 C7 N19 109.2(6) . . ?
N17 C7 H7 125.4 . . ?
N19 C7 H7 125.4 . . ?
N18 C8 N19 109.7(7) . . ?
N18 C8 H8 125.1 . . ?
N19 C8 H8 125.1 . . ?
N21 C9 N23 109.0(7) . . ?
N21 C9 H9 125.5 . . ?
N23 C9 H9 125.5 . . ?
N22 C10 N23 110.1(7) . . ?
N22 C10 H10 124.9 . . ?
N23 C10 H10 124.9 . . ?
N13 C11 H11 125.6 . . ?
N15 C11 N13 108.8(6) . . ?
N15 C11 H11 125.6 . . ?
N14 C12 N15 109.3(6) . . ?
N14 C12 H12 125.3 . . ?
N15 C12 H12 125.3 . . ?
N25 C13 S1 176.9(8) . . ?
N26 C14 S2 177.9(8) . . ?
N27 C15 S4 179.2(8) . . ?
N28 C16 S3 178.6(9) . . ?
N29 C17 S6 176.8(9) . . ?
N30 C18 S5 178.1(7) . . ?
Fe2 O1 H1A 113.3 . . ?
Fe2 O1 H1B 113.3 . . ?
H1A O1 H1B 110.7 . . ?
Fe3 O2 H2A 100.4 . . ?
Fe3 O2 H2B 99.5 . . ?
H2A O2 H2B 131.1 . . ?
H3A O3 H3B 108.0 . . ?
_iucr_refine_instructions_details
;
TITL 1 in P2(1)2(1)2(1)
1.res
created by SHELXL-2018/1 at 11:41:35 on 08-Feb-2018
CELL 0.71073 11.0249 11.8626 32.1485 90 90 90
ZERR 4 0.0104 0.0107 0.029 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Fe N O S
UNIT 72 120 12 120 12 24
L.S. 100
PLAN 5
SIZE 0.15 0.13 0.1
TEMP 23
BOND $H
HTAB
fmap 2
acta
REM
REM
REM
WGHT 0.037000
FVAR 0.34756
FE1 3 0.188402 0.074458 0.119994 11.00000 0.03362 0.02991 =
0.02743 -0.00155 -0.00308 0.00186
FE2 3 0.319652 0.114834 0.232384 11.00000 0.04112 0.03534 =
0.02813 -0.00186 -0.00347 -0.00076
FE3 3 0.060260 0.062428 0.006421 11.00000 0.05009 0.03631 =
0.02830 -0.00476 -0.00488 0.00520
N1 4 0.332415 0.193801 0.137390 11.00000 0.04377 0.03556 =
0.03075 -0.00292 -0.00155 -0.00526
N2 4 0.368976 0.214674 0.177813 11.00000 0.03530 0.03819 =
0.03236 -0.00118 -0.00436 -0.00134
N3 4 0.432325 0.351322 0.137721 11.00000 0.03810 0.03394 =
0.03767 0.00496 -0.00106 -0.00364
N4 4 0.481361 0.456729 0.126367 11.00000 0.05794 0.03052 =
0.06065 0.00242 0.00250 -0.01469
N5 4 0.083612 0.117977 0.175182 11.00000 0.03864 0.03975 =
0.02970 -0.00617 -0.00286 0.00121
N6 4 0.130045 0.136446 0.214635 11.00000 0.03657 0.04110 =
0.02840 -0.00588 0.00014 0.00143
N7 4 -0.065758 0.160316 0.216647 11.00000 0.04209 0.03918 =
0.04550 -0.00072 0.01070 0.00507
N8 4 -0.183304 0.185512 0.232288 11.00000 0.04486 0.06878 =
0.06947 -0.00126 0.02910 0.00814
N9 4 0.277003 -0.059566 0.154467 11.00000 0.04548 0.03604 =
0.03104 -0.00549 -0.00769 0.00078
N10 4 0.323211 -0.043086 0.194381 11.00000 0.04009 0.03179 =
0.03032 -0.00312 -0.01178 0.00476
N11 4 0.348508 -0.219282 0.176959 11.00000 0.03842 0.02533 =
0.03447 0.00038 -0.00375 0.00140
N12 4 0.385801 -0.332959 0.179945 11.00000 0.05246 0.02829 =
0.04832 -0.00335 -0.00633 0.00418
AFIX 3
H12A 2 0.440631 -0.345299 0.159725 11.00000 -1.20000
H12B 2 0.320911 -0.376349 0.174285 11.00000 -1.20000
AFIX 0
N13 4 0.096897 0.210877 0.088458 11.00000 0.04934 0.03181 =
0.03238 -0.00303 -0.00714 0.00599
N14 4 0.051196 0.206133 0.049459 11.00000 0.06251 0.03178 =
0.03412 0.00079 -0.00629 0.00945
N15 4 0.010281 0.369922 0.075832 11.00000 0.05354 0.03435 =
0.03619 -0.00417 -0.00671 0.01200
N16 4 -0.034789 0.481195 0.079121 11.00000 0.09509 0.03288 =
0.05288 -0.00527 -0.00917 0.02420
N17 4 0.043205 -0.038794 0.099514 11.00000 0.04520 0.03260 =
0.03130 -0.00308 -0.00474 -0.00282
N18 4 -0.000041 -0.045323 0.058556 11.00000 0.04651 0.03615 =
0.03290 -0.00460 -0.00542 0.00334
N19 4 -0.077287 -0.181072 0.094252 11.00000 0.03618 0.03337 =
0.06029 0.00018 -0.00284 -0.00381
N20 4 -0.138793 -0.284627 0.102977 11.00000 0.05291 0.03970 =
0.08938 0.00303 -0.00032 -0.01825
N21 4 0.292658 0.036087 0.064928 11.00000 0.03040 0.04124 =
0.04216 -0.00786 -0.00412 0.00097
N22 4 0.243558 0.019377 0.026060 11.00000 0.04716 0.04431 =
0.03300 0.00336 0.00752 -0.00178
N23 4 0.430933 -0.036397 0.025116 11.00000 0.04246 0.07165 =
0.05390 0.01276 0.01495 0.01427
N24 4 0.543379 -0.074171 0.011280 11.00000 0.06742 0.19416 =
0.06467 0.01732 0.02732 0.06681
AFIX 93
H24A 2 0.552152 -0.096011 -0.014051 11.00000 -1.20000
H24B 2 0.604116 -0.075682 0.028056 11.00000 -1.20000
AFIX 0
N25 4 0.272174 0.015272 0.283946 11.00000 0.09288 0.05295 =
0.03474 0.00439 0.00142 -0.00782
N26 4 0.328307 0.263306 0.269023 11.00000 0.05926 0.04845 =
0.04234 -0.00764 -0.00442 -0.00141
N27 4 0.056798 -0.075441 -0.035200 11.00000 0.06973 0.04499 =
0.03624 -0.00819 -0.00776 0.00450
N28 4 0.122142 0.177887 -0.039608 11.00000 0.09062 0.05556 =
0.03699 0.00190 0.00334 -0.00449
N29 4 0.260269 0.521136 0.073585 11.00000 0.06763 0.06031 =
0.05741 0.00540 0.00479 -0.00320
N30 4 0.053116 0.627899 0.159941 11.00000 0.10649 0.07282 =
0.05344 0.00486 -0.01539 0.00651
S1 6 0.231822 -0.133359 0.349440 11.00000 0.07034 0.08435 =
0.05755 0.02963 -0.00881 -0.02219
S2 6 0.320719 0.446826 0.323722 11.00000 0.08133 0.04304 =
0.04649 -0.01127 0.00730 0.00138
S3 6 0.211030 0.368341 -0.080114 11.00000 0.08620 0.05803 =
0.07063 0.01121 0.00401 -0.01486
S4 6 0.061591 -0.246198 -0.095134 11.00000 0.05708 0.05783 =
0.05297 -0.02352 -0.00060 -0.00164
S5 6 0.163234 0.449290 0.201537 11.00000 0.08312 0.06103 =
0.06004 -0.00490 -0.00970 0.01516
S6 6 0.221634 0.733762 0.041426 11.00000 0.08374 0.05421 =
0.07133 -0.00631 -0.02420 0.00376
C1 1 0.373151 0.276149 0.113766 11.00000 0.04847 0.03444 =
0.02962 -0.00259 -0.00424 -0.00045
AFIX 43
H1 2 0.362740 0.281552 0.085128 11.00000 -1.20000
AFIX 0
C2 1 0.427588 0.311522 0.177071 11.00000 0.03825 0.03977 =
0.03376 -0.00098 -0.00619 -0.00722
AFIX 43
H2 2 0.460747 0.347155 0.200193 11.00000 -1.20000
AFIX 0
C3 1 -0.034727 0.133030 0.177271 11.00000 0.03765 0.04449 =
0.03802 -0.00477 -0.00183 -0.00203
AFIX 43
H3 2 -0.088406 0.125968 0.155108 11.00000 -1.20000
AFIX 0
C4 1 0.038566 0.163290 0.238486 11.00000 0.04622 0.05014 =
0.03282 -0.00525 0.00367 -0.00023
AFIX 43
H4 2 0.044558 0.181802 0.266521 11.00000 -1.20000
AFIX 0
C5 1 0.293011 -0.165508 0.144941 11.00000 0.04048 0.03759 =
0.02605 -0.00710 -0.00328 0.00386
AFIX 43
H5 2 0.269903 -0.199001 0.120015 11.00000 -1.20000
AFIX 0
C6 1 0.365116 -0.140709 0.206496 11.00000 0.04552 0.03241 =
0.03440 -0.00384 -0.00963 -0.00302
AFIX 43
H6 2 0.401544 -0.154017 0.232121 11.00000 -1.20000
AFIX 0
C7 1 -0.007128 -0.120473 0.120116 11.00000 0.03803 0.04113 =
0.03483 -0.00337 -0.00089 -0.00208
AFIX 43
H7 2 0.003659 -0.134792 0.148316 11.00000 -1.20000
AFIX 0
C8 1 -0.069414 -0.134401 0.056842 11.00000 0.05242 0.04037 =
0.04534 -0.00547 -0.00964 0.00001
AFIX 43
H8 2 -0.107556 -0.161110 0.032997 11.00000 -1.20000
AFIX 0
C9 1 0.405587 0.002189 0.063773 11.00000 0.04049 0.05954 =
0.04583 0.00176 0.00108 0.00592
AFIX 43
H9 2 0.459710 0.004280 0.085948 11.00000 -1.20000
AFIX 0
C10 1 0.326477 -0.028194 0.003458 11.00000 0.05355 0.06539 =
0.04340 0.00011 0.01131 0.01097
AFIX 43
H10 2 0.315531 -0.053035 -0.023722 11.00000 -1.20000
AFIX 0
C11 1 0.071125 0.312190 0.103927 11.00000 0.05443 0.04169 =
0.03155 -0.00684 -0.00691 0.00533
AFIX 43
H11 2 0.092557 0.337957 0.130241 11.00000 -1.20000
AFIX 0
C12 1 -0.001260 0.303301 0.042184 11.00000 0.08215 0.04355 =
0.02951 -0.00523 -0.01914 0.01509
AFIX 43
H12 2 -0.040343 0.323109 0.017612 11.00000 -1.20000
AFIX 0
C13 1 0.253893 -0.044076 0.311616 11.00000 0.05787 0.05090 =
0.04271 0.00003 -0.00767 -0.00384
C14 1 0.323027 0.339236 0.291986 11.00000 0.05346 0.04352 =
0.03191 0.00197 0.00744 -0.00311
C15 1 0.059309 -0.145559 -0.060107 11.00000 0.04081 0.04512 =
0.03837 -0.00112 -0.01108 0.00141
C16 1 0.160019 0.255706 -0.056433 11.00000 0.05841 0.05857 =
0.02841 -0.00782 -0.00149 -0.00108
C17 1 0.247204 0.610149 0.060744 11.00000 0.04724 0.06234 =
0.06057 -0.01718 -0.00077 -0.00126
C18 1 0.098953 0.552504 0.176668 11.00000 0.05420 0.06767 =
0.03194 -0.00630 -0.00225 -0.00439
O1 5 0.511822 0.089830 0.243344 11.00000 0.05507 0.09909 =
0.05092 -0.03096 -0.01946 0.02341
AFIX 3
H1A 2 0.540382 0.032460 0.230884 11.00000 -1.50000
H1B 2 0.530352 0.088570 0.268994 11.00000 -1.50000
AFIX 0
O2 5 -0.129994 0.103364 -0.006842 11.00000 0.05890 0.06763 =
0.04282 -0.00927 -0.00818 0.01734
O3 5 0.969628 0.384728 0.278976 11.00000 0.19049 0.12718 =
0.12809 -0.00828 0.01808 0.03028
AFIX 3
H3A 2 0.905688 0.411568 0.268026 11.00000 -1.50000
H3B 2 1.028018 0.395318 0.262166 11.00000 -1.50000
AFIX 3
H8A 2 -0.199772 0.121658 0.238016 11.00000 -1.20000
H8B 2 -0.206322 0.214908 0.210086 11.00000 -1.20000
H2A 2 -0.143042 0.062148 -0.023454 11.00000 -1.50000
H2B 2 -0.154772 0.108158 0.016146 11.00000 -1.50000
H4A 2 0.557148 0.453748 0.117276 11.00000 -1.20000
H4B 2 0.441518 0.490518 0.106356 11.00000 -1.20000
H16A 2 0.024458 0.522848 0.089666 11.00000 -1.20000
H16B 2 -0.083272 0.470768 0.100916 11.00000 -1.20000
H20A 2 -0.096122 -0.318922 0.123696 11.00000 -1.20000
H20B 2 -0.210262 -0.276632 0.115216 11.00000 -1.20000
AFIX 0
HKLF 4
REM 1 in P2(1)2(1)2(1)
REM R1 = 0.0494 for 5649 Fo > 4sig(Fo) and 0.0934 for all 8554 data
REM 541 parameters refined using 0 restraints
END
WGHT 0.0370 0.0000
REM Instructions for potential hydrogen bonds
EQIV $1 x, y-1, z
HTAB N12 N4_$1
EQIV $2 x+1/2, -y-1/2, -z
HTAB N12 S4_$2
HTAB N12 S5_$1
EQIV $3 x+1/2, -y+1/2, -z
HTAB N24 N16_$3
HTAB N24 S6_$3
EQIV $4 -x, y-1/2, -z+1/2
HTAB C4 N30_$4
EQIV $5 x-1, y, z
HTAB C4 O3_$5
HTAB C5 S6_$1
EQIV $6 -x+1, y-1/2, -z+1/2
HTAB C7 O3_$6
HTAB C10 N16_$3
HTAB C11 S5
HTAB O1 S2_$6
EQIV $7 -x+1, y+1/2, -z+1/2
HTAB O1 N12_$7
EQIV $8 x+1, y, z
HTAB O3 S5_$8
HTAB N8 S5_$4
EQIV $9 -x, y+1/2, -z+1/2
HTAB N8 S1_$9
EQIV $10 x-1/2, -y+1/2, -z
HTAB O2 N29_$10
HTAB O2 S3_$10
HTAB N4 S1_$7
HTAB N4 N29
HTAB N16 N29
HTAB N16 N30
HTAB N16 S1_$9
HTAB N20 N30_$1
EQIV $11 x-1/2, -y-1/2, -z
HTAB N20 S4_$11
REM Highest difference peak 0.418, deepest hole -0.348, 1-sigma level 0.074
Q1 1 0.2074 -0.0586 0.3600 11.00000 0.05 0.40
Q2 1 0.2228 0.6393 0.0246 11.00000 0.05 0.31
Q3 1 0.2805 0.0763 0.0458 11.00000 0.05 0.30
Q4 1 0.3718 0.1417 0.1912 11.00000 0.05 0.30
Q5 1 0.1130 0.0493 0.2130 11.00000 0.05 0.29
REM The information below was added by Olex2.
REM
REM R1 = 0.0494 for 5649 Fo > 4sig(Fo) and 0.0934 for all 12919 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.42, deepest hole -0.35
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0934
REM R1_gt = 0.0494
REM wR_ref = 0.1070
REM GOOF = 0.989
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 12919
REM Reflections_gt = 5649
REM Parameters = n/a
REM Hole = -0.35
REM Peak = 0.42
REM Flack = 0.047(18)
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_d
_database_code_depnum_ccdc_archive 'CCDC 1578879'
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_audit_creation_date 2018-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C17 H26 Fe3 N29 O S5, C N S'
_chemical_formula_sum 'C18 H26 Fe3 N30 O S6'
_chemical_formula_weight 1038.60
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Fe Fe 0.3463 0.8444 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_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'
_cell_length_a 10.972(4)
_cell_length_b 11.475(6)
_cell_length_c 31.878(11)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4014(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9879
_cell_measurement_temperature 150(2)
_cell_measurement_theta_max 24.666
_cell_measurement_theta_min 2.561
_shelx_estimated_absorpt_T_max 0.867
_shelx_estimated_absorpt_T_min 0.735
_exptl_absorpt_coefficient_mu 1.446
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_correction_T_min 0.6194
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0791 before and 0.0696 after correction. The Ratio of minimum to maximum transmission is 0.8312. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.719
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2104
_exptl_crystal_size_max 0.227
_exptl_crystal_size_mid 0.186
_exptl_crystal_size_min 0.102
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0672
_diffrn_reflns_av_unetI/netI 0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 38
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_number 40781
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full 25.518
_diffrn_reflns_theta_max 25.518
_diffrn_reflns_theta_min 2.556
_diffrn_ambient_temperature 150.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.778
_reflns_Friedel_fraction_full 0.993
_reflns_Friedel_fraction_max 0.993
_reflns_number_gt 6008
_reflns_number_total 7423
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.955
_refine_diff_density_min -0.695
_refine_diff_density_rms 0.109
_refine_ls_abs_structure_details
;
Flack x determined using 2137 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.042(9)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 528
_refine_ls_number_reflns 7423
_refine_ls_number_restraints 24
_refine_ls_R_factor_all 0.0873
_refine_ls_R_factor_gt 0.0650
_refine_ls_restrained_S_all 1.079
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+26.4198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1262
_refine_ls_wR_factor_ref 0.1340
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups
At 1.5 times of:
All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(N23) \\sim Ueq, Uanis(N24) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(N3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Riding coordinates:
N16(H16A,H16B), O1(H1A,H1B)
3.b Rotating group:
N4(H4A,H4B), N8(H8A,H8B), N12(H12A,H12B), N20(H20A,H20B), N24(H24A,H24B)
3.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
C10(H10), C11(H11), C12(H12)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.17965(15) 0.07182(12) 0.12003(4) 0.0248(3) Uani 1 1 d . . . . .
Fe2 Fe 0.31936(17) 0.11635(12) 0.23052(4) 0.0311(4) Uani 1 1 d . . . . .
Fe3 Fe 0.0519(2) 0.04907(16) 0.00608(5) 0.0500(5) Uani 1 1 d . . . . .
N1 N 0.3153(11) 0.1959(7) 0.1351(2) 0.038(2) Uani 1 1 d . . . . .
N2 N 0.3621(8) 0.2146(7) 0.1752(2) 0.026(2) Uani 1 1 d . . . . .
N3 N 0.4245(8) 0.3535(7) 0.1338(2) 0.028(2) Uani 1 1 d . U . . .
N4 N 0.4807(9) 0.4583(7) 0.1219(3) 0.041(2) Uani 1 1 d . U . . .
H4A H 0.552260 0.444388 0.112499 0.049 Uiso 1 1 d GR . . . .
H4B H 0.439200 0.491839 0.102508 0.049 Uiso 1 1 d GR . . . .
N5 N 0.0795(8) 0.1133(7) 0.1750(2) 0.0258(19) Uani 1 1 d . . . . .
N6 N 0.1305(8) 0.1331(7) 0.2144(2) 0.026(2) Uani 1 1 d . . . . .
N7 N -0.0633(9) 0.1608(7) 0.2182(3) 0.031(2) Uani 1 1 d . . . . .
N8 N -0.1801(10) 0.1860(8) 0.2349(3) 0.049(3) Uani 1 1 d . . . . .
H8A H -0.215344 0.122785 0.242886 0.059 Uiso 1 1 d GR . . . .
H8B H -0.171041 0.231209 0.256213 0.059 Uiso 1 1 d GR . . . .
N9 N 0.2677(8) -0.0649(8) 0.1542(2) 0.028(2) Uani 1 1 d . . . . .
N10 N 0.3224(9) -0.0444(7) 0.1931(2) 0.0278(19) Uani 1 1 d . . . . .
N11 N 0.3427(8) -0.2277(7) 0.1764(2) 0.027(2) Uani 1 1 d . . . . .
N12 N 0.3807(10) -0.3459(8) 0.1796(3) 0.039(2) Uani 1 1 d . . . . .
H12A H 0.319397 -0.393574 0.180179 0.047 Uiso 1 1 d GR . . . .
H12B H 0.425791 -0.365276 0.158416 0.047 Uiso 1 1 d GR . . . .
N13 N 0.0845(8) 0.2049(8) 0.0887(3) 0.031(2) Uani 1 1 d . . . . .
N14 N 0.0293(10) 0.1907(8) 0.0501(3) 0.039(3) Uani 1 1 d . . . . .
N15 N -0.0233(9) 0.3585(7) 0.0757(2) 0.036(2) Uani 1 1 d . . . . .
N16 N -0.0772(10) 0.4676(8) 0.0785(3) 0.047(3) Uani 1 1 d . . . . .
H16A H -0.019579 0.521432 0.082291 0.056 Uiso 1 1 d R . . . .
H16B H -0.125679 0.468952 0.100981 0.056 Uiso 1 1 d R . . . .
N17 N 0.0415(9) -0.0479(7) 0.1007(3) 0.034(2) Uani 1 1 d . . . . .
N18 N -0.0027(10) -0.0603(9) 0.0600(3) 0.045(3) Uani 1 1 d . . . . .
N19 N -0.0912(9) -0.1896(8) 0.0987(4) 0.050(3) Uani 1 1 d . . . . .
N20 N -0.1606(12) -0.2875(9) 0.1102(5) 0.090(5) Uani 1 1 d . . . . .
H20A H -0.124944 -0.323666 0.130209 0.109 Uiso 1 1 d GR . . . .
H20B H -0.230695 -0.265560 0.118414 0.109 Uiso 1 1 d GR . . . .
N21 N 0.2828(9) 0.0323(8) 0.0659(3) 0.042(3) Uani 1 1 d . . . . .
N22 N 0.2307(11) 0.0077(9) 0.0281(3) 0.051(3) Uani 1 1 d . . . . .
N23 N 0.4184(14) -0.0422(13) 0.0255(4) 0.079(4) Uani 1 1 d . U . . .
N24 N 0.5296(19) -0.088(2) 0.0103(6) 0.156(8) Uani 1 1 d . U . . .
H24A H 0.592556 -0.048672 0.021599 0.188 Uiso 1 1 d GR . . . .
H24B H 0.545501 -0.162984 0.016871 0.188 Uiso 1 1 d GR . . . .
N25 N 0.2808(10) 0.0149(8) 0.2835(3) 0.045(3) Uani 1 1 d . . . . .
N26 N 0.3246(11) 0.2707(8) 0.2671(3) 0.042(2) Uani 1 1 d . . . . .
N27 N 0.0679(13) -0.0970(9) -0.0352(3) 0.063(4) Uani 1 1 d . . . . .
N28 N 0.1178(12) 0.1715(10) -0.0378(3) 0.059(4) Uani 1 1 d . . . . .
N29 N -0.1334(13) 0.0610(13) -0.0153(3) 0.077(4) Uani 1 1 d . . . . .
N30 N 0.0407(12) 0.6283(10) 0.1584(3) 0.061(3) Uani 1 1 d . . . . .
C1 C 0.3571(11) 0.2795(9) 0.1111(3) 0.039(3) Uani 1 1 d . . . . .
H1 H 0.341788 0.286632 0.081925 0.047 Uiso 1 1 calc R . . . .
C2 C 0.4259(11) 0.3121(9) 0.1729(3) 0.032(3) Uani 1 1 d . . . . .
H2 H 0.466793 0.347677 0.195805 0.039 Uiso 1 1 calc R . . . .
C3 C -0.0352(11) 0.1293(8) 0.1789(3) 0.027(2) Uani 1 1 d . . . . .
H3 H -0.092846 0.120073 0.156895 0.033 Uiso 1 1 calc R . . . .
C4 C 0.0402(13) 0.1620(9) 0.2390(3) 0.037(3) Uani 1 1 d . . . . .
H4 H 0.048148 0.181329 0.267841 0.045 Uiso 1 1 calc R . . . .
C5 C 0.2823(10) -0.1754(9) 0.1451(3) 0.029(3) Uani 1 1 d . . . . .
H5 H 0.254562 -0.212547 0.120187 0.035 Uiso 1 1 calc R . . . .
C6 C 0.3656(10) -0.1442(9) 0.2046(3) 0.030(3) Uani 1 1 d . . . . .
H6 H 0.408693 -0.156696 0.230035 0.037 Uiso 1 1 calc R . . . .
C7 C -0.0161(11) -0.1258(10) 0.1237(4) 0.041(3) Uani 1 1 d . . . . .
H7 H -0.006629 -0.135795 0.153056 0.050 Uiso 1 1 calc R . . . .
C8 C -0.0803(13) -0.1454(12) 0.0595(5) 0.057(4) Uani 1 1 d . . . . .
H8 H -0.122764 -0.172568 0.035437 0.069 Uiso 1 1 calc R . . . .
C9 C 0.3996(15) 0.0024(11) 0.0639(6) 0.067(5) Uani 1 1 d . . . . .
H9 H 0.458530 0.010874 0.085497 0.080 Uiso 1 1 calc R . . . .
C10 C 0.3142(15) -0.0400(15) 0.0047(4) 0.079(5) Uani 1 1 d . . . . .
H10 H 0.302074 -0.068831 -0.022893 0.094 Uiso 1 1 calc R . . . .
C11 C 0.0483(11) 0.3066(9) 0.1031(3) 0.032(3) Uani 1 1 d . . . . .
H11 H 0.070579 0.338226 0.129521 0.038 Uiso 1 1 calc R . . . .
C12 C -0.0379(13) 0.2853(10) 0.0433(3) 0.041(3) Uani 1 1 d . . . . .
H12 H -0.087908 0.298710 0.019445 0.050 Uiso 1 1 calc R . . . .
C13 C 0.2672(13) -0.0502(11) 0.3100(4) 0.047(3) Uani 1 1 d . . . . .
C14 C 0.3196(12) 0.3465(10) 0.2901(3) 0.035(3) Uani 1 1 d . . . . .
C15 C 0.0610(15) -0.1644(11) -0.0613(4) 0.056(4) Uani 1 1 d . . . . .
C16 C 0.1461(13) 0.2535(13) -0.0554(4) 0.049(4) Uani 1 1 d . . . . .
C17 C -0.2007(16) 0.0074(14) -0.0367(4) 0.065(5) Uani 1 1 d . . . . .
C18 C 0.0871(12) 0.5484(10) 0.1755(3) 0.040(3) Uani 1 1 d . . . . .
O1 O 0.5127(8) 0.1010(8) 0.2404(2) 0.057(3) Uani 1 1 d . . . . .
H1A H 0.549330 0.056031 0.227756 0.085 Uiso 1 1 d R . . . .
H1B H 0.535200 0.108571 0.266956 0.085 Uiso 1 1 d R . . . .
S1 S 0.2524(3) -0.1487(3) 0.34683(9) 0.0474(8) Uani 1 1 d . . . . .
S2 S 0.3166(4) 0.4561(2) 0.32355(8) 0.0418(7) Uani 1 1 d . . . . .
S3 S 0.1903(5) 0.3690(3) -0.08228(11) 0.0702(11) Uani 1 1 d . . . . .
S4 S 0.0524(4) -0.2605(3) -0.09917(10) 0.0527(9) Uani 1 1 d . . . . .
S5 S -0.2811(4) -0.0602(4) -0.07136(12) 0.0704(11) Uani 1 1 d . . . . .
S6 S 0.1530(3) 0.4432(3) 0.20058(9) 0.0456(8) Uani 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 0.0365(8) 0.0191(7) 0.0187(6) -0.0015(5) -0.0085(7) 0.0031(7)
Fe2 0.0511(10) 0.0229(7) 0.0193(7) -0.0018(6) -0.0133(8) 0.0007(8)
Fe3 0.0890(15) 0.0403(10) 0.0207(8) -0.0124(7) -0.0125(9) 0.0274(10)
N1 0.074(7) 0.023(5) 0.018(4) -0.010(4) -0.014(5) 0.011(5)
N2 0.035(5) 0.026(5) 0.016(4) -0.003(4) -0.012(4) 0.004(4)
N3 0.038(4) 0.022(4) 0.024(4) -0.002(3) -0.003(3) 0.001(4)
N4 0.056(6) 0.030(5) 0.036(5) 0.001(4) -0.003(5) 0.004(4)
N5 0.037(6) 0.020(4) 0.021(4) 0.002(4) -0.002(4) 0.002(4)
N6 0.046(6) 0.021(4) 0.011(4) -0.007(3) -0.002(4) -0.004(4)
N7 0.039(6) 0.025(5) 0.028(5) -0.001(4) 0.009(4) 0.000(4)
N8 0.061(7) 0.037(5) 0.050(6) -0.007(5) 0.035(6) -0.002(6)
N9 0.043(5) 0.029(5) 0.014(4) 0.001(4) -0.009(4) -0.006(4)
N10 0.042(5) 0.020(4) 0.022(4) -0.001(3) -0.021(4) 0.000(5)
N11 0.034(6) 0.020(4) 0.025(4) -0.010(3) -0.008(4) 0.000(4)
N12 0.055(7) 0.027(5) 0.036(5) -0.011(4) -0.018(5) 0.008(5)
N13 0.039(6) 0.032(5) 0.022(4) -0.010(4) -0.010(4) 0.009(4)
N14 0.063(7) 0.033(5) 0.020(5) -0.005(4) -0.001(5) 0.020(5)
N15 0.069(7) 0.028(5) 0.013(4) 0.002(4) 0.005(4) 0.008(5)
N16 0.076(8) 0.027(5) 0.038(5) -0.002(4) 0.012(6) 0.015(5)
N17 0.047(6) 0.023(5) 0.031(5) 0.002(4) 0.005(5) 0.004(5)
N18 0.058(7) 0.034(5) 0.043(6) -0.018(5) -0.015(5) 0.011(5)
N19 0.034(6) 0.027(5) 0.090(9) -0.020(6) 0.000(6) 0.002(5)
N20 0.056(9) 0.033(6) 0.182(16) -0.035(8) 0.031(10) -0.021(6)
N21 0.035(6) 0.023(5) 0.069(7) -0.002(5) 0.002(5) 0.002(4)
N22 0.080(9) 0.036(6) 0.036(6) 0.011(5) 0.014(6) 0.022(6)
N23 0.077(6) 0.088(6) 0.071(6) 0.030(5) 0.029(5) 0.010(5)
N24 0.136(12) 0.196(13) 0.138(11) 0.049(11) 0.060(10) 0.040(11)
N25 0.082(9) 0.032(5) 0.021(5) 0.000(4) -0.016(5) -0.011(5)
N26 0.069(7) 0.033(5) 0.024(4) -0.001(4) -0.008(6) -0.006(6)
N27 0.102(10) 0.045(7) 0.041(6) -0.022(5) -0.023(7) 0.028(7)
N28 0.106(11) 0.055(7) 0.016(5) -0.003(5) -0.009(6) 0.035(7)
N29 0.095(11) 0.101(10) 0.035(6) -0.011(7) -0.025(7) 0.027(9)
N30 0.091(9) 0.037(6) 0.054(7) 0.012(5) 0.009(7) 0.004(7)
C1 0.061(9) 0.029(6) 0.027(6) -0.010(5) -0.007(6) 0.008(6)
C2 0.050(7) 0.030(6) 0.017(5) -0.009(4) -0.007(5) 0.010(6)
C3 0.047(8) 0.015(5) 0.020(5) 0.001(4) -0.003(5) -0.007(5)
C4 0.081(10) 0.020(5) 0.010(5) -0.002(4) 0.004(6) 0.002(6)
C5 0.033(6) 0.033(6) 0.021(5) -0.008(4) -0.009(4) -0.003(5)
C6 0.037(6) 0.032(6) 0.022(5) 0.001(5) -0.019(5) 0.002(5)
C7 0.047(8) 0.034(6) 0.043(7) -0.013(6) -0.008(6) 0.014(6)
C8 0.057(9) 0.043(8) 0.071(10) -0.018(7) -0.027(8) 0.012(7)
C9 0.070(12) 0.030(7) 0.101(13) 0.018(8) 0.012(9) -0.002(7)
C10 0.078(11) 0.109(13) 0.049(8) 0.044(9) 0.036(9) 0.047(11)
C11 0.047(7) 0.028(6) 0.022(5) -0.006(4) -0.007(5) 0.001(5)
C12 0.063(9) 0.034(6) 0.027(6) -0.006(5) -0.013(6) 0.019(6)
C13 0.078(10) 0.037(7) 0.026(6) -0.005(6) -0.016(6) -0.001(7)
C14 0.052(7) 0.040(6) 0.013(5) 0.005(5) -0.004(5) -0.002(7)
C15 0.095(12) 0.036(7) 0.037(7) -0.009(6) -0.002(8) 0.002(8)
C16 0.062(10) 0.062(9) 0.023(6) -0.013(6) -0.012(6) 0.034(7)
C17 0.083(12) 0.087(11) 0.025(6) 0.005(7) 0.007(7) 0.025(10)
C18 0.057(8) 0.032(7) 0.030(6) -0.001(5) 0.007(6) 0.010(6)
O1 0.065(6) 0.068(6) 0.038(5) -0.026(4) -0.021(4) 0.027(5)
S1 0.069(2) 0.0487(19) 0.0245(14) 0.0088(13) -0.0092(15) -0.0065(17)
S2 0.078(2) 0.0268(14) 0.0203(12) -0.0066(11) -0.0009(15) 0.0062(17)
S3 0.106(3) 0.054(2) 0.051(2) 0.0039(17) -0.011(2) 0.023(2)
S4 0.074(3) 0.0459(19) 0.0379(17) -0.0218(15) 0.0120(18) -0.0104(18)
S5 0.068(3) 0.082(3) 0.061(2) -0.001(2) 0.012(2) -0.004(2)
S6 0.074(2) 0.0300(15) 0.0329(15) -0.0052(13) -0.0075(15) 0.0051(16)
_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 N1 2.115(10) . ?
Fe1 N5 2.122(8) . ?
Fe1 N9 2.141(9) . ?
Fe1 N13 2.101(9) . ?
Fe1 N17 2.136(9) . ?
Fe1 N21 2.113(11) . ?
Fe2 N2 2.146(8) . ?
Fe2 N6 2.143(9) . ?
Fe2 N10 2.196(8) . ?
Fe2 N25 2.095(10) . ?
Fe2 N26 2.123(9) . ?
Fe2 O1 2.152(9) . ?
Fe3 N14 2.162(9) . ?
Fe3 N18 2.210(11) . ?
Fe3 N22 2.138(12) . ?
Fe3 N27 2.139(10) . ?
Fe3 N28 2.111(13) . ?
Fe3 N29 2.148(13) . ?
N1 N2 1.395(11) . ?
N1 C1 1.308(14) . ?
N2 C2 1.321(14) . ?
N3 N4 1.404(12) . ?
N3 C1 1.337(13) . ?
N3 C2 1.335(12) . ?
N4 H4A 0.8557 . ?
N4 H4B 0.8588 . ?
N5 N6 1.396(11) . ?
N5 C3 1.278(14) . ?
N6 C4 1.306(14) . ?
N7 N8 1.417(13) . ?
N7 C3 1.340(12) . ?
N7 C4 1.315(15) . ?
N8 H8A 0.8607 . ?
N8 H8B 0.8614 . ?
N9 N10 1.399(10) . ?
N9 C5 1.311(13) . ?
N10 C6 1.291(13) . ?
N11 N12 1.422(12) . ?
N11 C5 1.341(13) . ?
N11 C6 1.337(13) . ?
N12 H12A 0.8679 . ?
N12 H12B 0.8662 . ?
N13 N14 1.381(12) . ?
N13 C11 1.315(13) . ?
N14 C12 1.330(14) . ?
N15 N16 1.388(12) . ?
N15 C11 1.316(14) . ?
N15 C12 1.341(13) . ?
N16 H16A 0.8922 . ?
N16 H16B 0.8915 . ?
N17 N18 1.395(12) . ?
N17 C7 1.315(15) . ?
N18 C8 1.295(17) . ?
N19 N20 1.406(15) . ?
N19 C7 1.360(15) . ?
N19 C8 1.354(18) . ?
N20 H20A 0.8550 . ?
N20 H20B 0.8502 . ?
N21 N22 1.363(14) . ?
N21 C9 1.328(18) . ?
N22 C10 1.301(16) . ?
N23 N24 1.41(2) . ?
N23 C9 1.34(2) . ?
N23 C10 1.32(2) . ?
N24 H24A 0.8990 . ?
N24 H24B 0.9052 . ?
N25 C13 1.136(14) . ?
N26 C14 1.136(13) . ?
N27 C15 1.139(15) . ?
N28 C16 1.139(17) . ?
N29 C17 1.178(19) . ?
N30 C18 1.182(15) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 S1 1.639(13) . ?
C14 S2 1.651(11) . ?
C15 S4 1.636(12) . ?
C16 S3 1.650(16) . ?
C17 S5 1.614(17) . ?
C18 S6 1.619(12) . ?
O1 H1A 0.7688 . ?
O1 H1B 0.8852 . ?
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
N1 Fe1 N5 91.5(3) . . ?
N1 Fe1 N9 93.5(3) . . ?
N1 Fe1 N17 176.1(3) . . ?
N5 Fe1 N9 88.8(3) . . ?
N5 Fe1 N17 90.8(3) . . ?
N13 Fe1 N1 88.1(4) . . ?
N13 Fe1 N5 88.4(3) . . ?
N13 Fe1 N9 176.7(4) . . ?
N13 Fe1 N17 88.8(3) . . ?
N13 Fe1 N21 92.0(4) . . ?
N17 Fe1 N9 89.7(3) . . ?
N21 Fe1 N1 87.3(4) . . ?
N21 Fe1 N5 178.8(4) . . ?
N21 Fe1 N9 90.9(4) . . ?
N21 Fe1 N17 90.4(3) . . ?
N2 Fe2 N10 89.5(3) . . ?
N2 Fe2 O1 87.0(3) . . ?
N6 Fe2 N2 88.1(3) . . ?
N6 Fe2 N10 87.7(3) . . ?
N6 Fe2 O1 174.6(3) . . ?
N25 Fe2 N2 177.8(4) . . ?
N25 Fe2 N6 92.7(4) . . ?
N25 Fe2 N10 88.5(3) . . ?
N25 Fe2 N26 91.5(4) . . ?
N25 Fe2 O1 92.0(4) . . ?
N26 Fe2 N2 90.4(3) . . ?
N26 Fe2 N6 94.8(4) . . ?
N26 Fe2 N10 177.5(4) . . ?
N26 Fe2 O1 87.8(4) . . ?
O1 Fe2 N10 89.8(3) . . ?
N14 Fe3 N18 83.7(3) . . ?
N22 Fe3 N14 93.4(4) . . ?
N22 Fe3 N18 82.4(4) . . ?
N22 Fe3 N27 87.3(4) . . ?
N22 Fe3 N29 170.8(5) . . ?
N27 Fe3 N14 176.7(5) . . ?
N27 Fe3 N18 93.2(4) . . ?
N27 Fe3 N29 86.1(5) . . ?
N28 Fe3 N14 88.3(4) . . ?
N28 Fe3 N18 170.5(4) . . ?
N28 Fe3 N22 92.9(4) . . ?
N28 Fe3 N27 94.9(4) . . ?
N28 Fe3 N29 94.1(5) . . ?
N29 Fe3 N14 92.9(5) . . ?
N29 Fe3 N18 91.5(5) . . ?
N2 N1 Fe1 124.8(7) . . ?
C1 N1 Fe1 127.5(7) . . ?
C1 N1 N2 107.0(9) . . ?
N1 N2 Fe2 126.3(7) . . ?
C2 N2 Fe2 127.3(6) . . ?
C2 N2 N1 105.9(8) . . ?
C1 N3 N4 130.0(9) . . ?
C2 N3 N4 123.5(9) . . ?
C2 N3 C1 106.5(9) . . ?
N3 N4 H4A 109.7 . . ?
N3 N4 H4B 110.2 . . ?
H4A N4 H4B 108.5 . . ?
N6 N5 Fe1 124.9(7) . . ?
C3 N5 Fe1 128.6(7) . . ?
C3 N5 N6 106.5(8) . . ?
N5 N6 Fe2 126.1(6) . . ?
C4 N6 Fe2 127.8(7) . . ?
C4 N6 N5 106.1(9) . . ?
C3 N7 N8 127.9(10) . . ?
C4 N7 N8 126.1(9) . . ?
C4 N7 C3 106.0(9) . . ?
N7 N8 H8A 110.2 . . ?
N7 N8 H8B 108.4 . . ?
H8A N8 H8B 109.0 . . ?
N10 N9 Fe1 121.5(6) . . ?
C5 N9 Fe1 130.6(7) . . ?
C5 N9 N10 107.9(8) . . ?
N9 N10 Fe2 128.0(6) . . ?
C6 N10 Fe2 126.6(6) . . ?
C6 N10 N9 105.0(8) . . ?
C5 N11 N12 128.6(8) . . ?
C6 N11 N12 125.5(8) . . ?
C6 N11 C5 105.8(8) . . ?
N11 N12 H12A 112.0 . . ?
N11 N12 H12B 110.9 . . ?
H12A N12 H12B 107.3 . . ?
N14 N13 Fe1 123.7(6) . . ?
C11 N13 Fe1 129.1(7) . . ?
C11 N13 N14 106.3(8) . . ?
N13 N14 Fe3 128.1(7) . . ?
C12 N14 Fe3 124.8(7) . . ?
C12 N14 N13 107.1(8) . . ?
C11 N15 N16 128.2(9) . . ?
C11 N15 C12 107.4(9) . . ?
C12 N15 N16 124.4(10) . . ?
N15 N16 H16A 109.4 . . ?
N15 N16 H16B 108.8 . . ?
H16A N16 H16B 107.6 . . ?
N18 N17 Fe1 125.5(7) . . ?
C7 N17 Fe1 128.1(8) . . ?
C7 N17 N18 106.3(9) . . ?
N17 N18 Fe3 124.9(7) . . ?
C8 N18 Fe3 126.7(9) . . ?
C8 N18 N17 108.4(11) . . ?
C7 N19 N20 127.3(13) . . ?
C8 N19 N20 126.1(13) . . ?
C8 N19 C7 106.5(11) . . ?
N19 N20 H20A 109.6 . . ?
N19 N20 H20B 109.5 . . ?
H20A N20 H20B 109.2 . . ?
N22 N21 Fe1 122.8(8) . . ?
C9 N21 Fe1 127.7(11) . . ?
C9 N21 N22 108.0(12) . . ?
N21 N22 Fe3 129.0(8) . . ?
C10 N22 Fe3 123.5(10) . . ?
C10 N22 N21 107.3(12) . . ?
C9 N23 N24 125.8(17) . . ?
C10 N23 N24 125.7(16) . . ?
C10 N23 C9 108.4(14) . . ?
N23 N24 H24A 110.0 . . ?
N23 N24 H24B 116.2 . . ?
H24A N24 H24B 103.6 . . ?
C13 N25 Fe2 172.0(11) . . ?
C14 N26 Fe2 172.1(10) . . ?
C15 N27 Fe3 167.6(12) . . ?
C16 N28 Fe3 166.0(10) . . ?
C17 N29 Fe3 138.1(12) . . ?
N1 C1 N3 110.2(9) . . ?
N1 C1 H1 124.9 . . ?
N3 C1 H1 124.9 . . ?
N2 C2 N3 110.3(9) . . ?
N2 C2 H2 124.8 . . ?
N3 C2 H2 124.8 . . ?
N5 C3 N7 110.9(10) . . ?
N5 C3 H3 124.6 . . ?
N7 C3 H3 124.6 . . ?
N6 C4 N7 110.5(8) . . ?
N6 C4 H4 124.7 . . ?
N7 C4 H4 124.8 . . ?
N9 C5 N11 109.1(8) . . ?
N9 C5 H5 125.5 . . ?
N11 C5 H5 125.5 . . ?
N10 C6 N11 112.2(8) . . ?
N10 C6 H6 123.9 . . ?
N11 C6 H6 123.9 . . ?
N17 C7 N19 109.4(11) . . ?
N17 C7 H7 125.3 . . ?
N19 C7 H7 125.3 . . ?
N18 C8 N19 109.3(12) . . ?
N18 C8 H8 125.4 . . ?
N19 C8 H8 125.4 . . ?
N21 C9 N23 106.9(16) . . ?
N21 C9 H9 126.6 . . ?
N23 C9 H9 126.6 . . ?
N22 C10 N23 109.3(15) . . ?
N22 C10 H10 125.4 . . ?
N23 C10 H10 125.4 . . ?
N13 C11 N15 110.6(9) . . ?
N13 C11 H11 124.7 . . ?
N15 C11 H11 124.7 . . ?
N14 C12 N15 108.6(10) . . ?
N14 C12 H12 125.7 . . ?
N15 C12 H12 125.7 . . ?
N25 C13 S1 177.0(13) . . ?
N26 C14 S2 178.4(13) . . ?
N27 C15 S4 179.3(17) . . ?
N28 C16 S3 177.7(12) . . ?
N29 C17 S5 171.9(14) . . ?
N30 C18 S6 177.2(12) . . ?
Fe2 O1 H1A 119.5 . . ?
Fe2 O1 H1B 114.0 . . ?
H1A O1 H1B 115.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 N2 Fe2 4.5(12) . . . . ?
Fe1 N1 N2 C2 -168.4(7) . . . . ?
Fe1 N1 C1 N3 168.2(7) . . . . ?
Fe1 N5 N6 Fe2 -4.1(11) . . . . ?
Fe1 N5 N6 C4 176.6(7) . . . . ?
Fe1 N5 C3 N7 -176.4(6) . . . . ?
Fe1 N9 N10 Fe2 5.9(11) . . . . ?
Fe1 N9 N10 C6 179.9(7) . . . . ?
Fe1 N9 C5 N11 -179.4(7) . . . . ?
Fe1 N13 N14 Fe3 -13.3(13) . . . . ?
Fe1 N13 N14 C12 170.1(8) . . . . ?
Fe1 N13 C11 N15 -171.1(8) . . . . ?
Fe1 N17 N18 Fe3 -4.0(12) . . . . ?
Fe1 N17 N18 C8 176.3(8) . . . . ?
Fe1 N17 C7 N19 -175.9(7) . . . . ?
Fe1 N21 N22 Fe3 20.5(13) . . . . ?
Fe1 N21 N22 C10 -164.5(9) . . . . ?
Fe1 N21 C9 N23 164.9(9) . . . . ?
Fe2 N2 C2 N3 -174.6(7) . . . . ?
Fe2 N6 C4 N7 -178.6(7) . . . . ?
Fe2 N10 C6 N11 173.6(7) . . . . ?
Fe3 N14 C12 N15 -175.1(8) . . . . ?
Fe3 N18 C8 N19 -178.8(8) . . . . ?
Fe3 N22 C10 N23 172.7(9) . . . . ?
N1 N2 C2 N3 -1.7(12) . . . . ?
N2 N1 C1 N3 -2.3(13) . . . . ?
N4 N3 C1 N1 -175.7(10) . . . . ?
N4 N3 C2 N2 177.6(9) . . . . ?
N5 N6 C4 N7 0.7(11) . . . . ?
N6 N5 C3 N7 1.3(11) . . . . ?
N8 N7 C3 N5 -179.9(9) . . . . ?
N8 N7 C4 N6 179.1(9) . . . . ?
N9 N10 C6 N11 -0.5(12) . . . . ?
N10 N9 C5 N11 0.6(12) . . . . ?
N12 N11 C5 N9 -178.5(10) . . . . ?
N12 N11 C6 N10 178.6(10) . . . . ?
N13 N14 C12 N15 1.7(14) . . . . ?
N14 N13 C11 N15 -1.7(13) . . . . ?
N16 N15 C11 N13 -178.1(10) . . . . ?
N16 N15 C12 N14 178.1(10) . . . . ?
N17 N18 C8 N19 0.9(14) . . . . ?
N18 N17 C7 N19 2.3(12) . . . . ?
N20 N19 C7 N17 174.2(11) . . . . ?
N20 N19 C8 N18 -175.6(11) . . . . ?
N21 N22 C10 N23 -2.7(16) . . . . ?
N22 N21 C9 N23 -1.1(14) . . . . ?
N24 N23 C9 N21 -178.3(17) . . . . ?
N24 N23 C10 N22 179.8(17) . . . . ?
C1 N1 N2 Fe2 175.4(7) . . . . ?
C1 N1 N2 C2 2.4(12) . . . . ?
C1 N3 C2 N2 0.4(13) . . . . ?
C2 N3 C1 N1 1.2(13) . . . . ?
C3 N5 N6 Fe2 178.1(7) . . . . ?
C3 N5 N6 C4 -1.2(10) . . . . ?
C3 N7 C4 N6 0.1(11) . . . . ?
C4 N7 C3 N5 -0.9(11) . . . . ?
C5 N9 N10 Fe2 -174.1(8) . . . . ?
C5 N9 N10 C6 -0.1(11) . . . . ?
C5 N11 C6 N10 0.9(13) . . . . ?
C6 N11 C5 N9 -0.9(12) . . . . ?
C7 N17 N18 Fe3 177.7(7) . . . . ?
C7 N17 N18 C8 -2.0(12) . . . . ?
C7 N19 C8 N18 0.5(14) . . . . ?
C8 N19 C7 N17 -1.8(13) . . . . ?
C9 N21 N22 Fe3 -172.7(9) . . . . ?
C9 N21 N22 C10 2.3(14) . . . . ?
C9 N23 C10 N22 2.0(18) . . . . ?
C10 N23 C9 N21 -0.5(17) . . . . ?
C11 N13 N14 Fe3 176.6(8) . . . . ?
C11 N13 N14 C12 -0.1(13) . . . . ?
C11 N15 C12 N14 -2.7(14) . . . . ?
C12 N15 C11 N13 2.7(14) . . . . ?
_iucr_refine_instructions_details
;
TITL D_a.res in P2(1)2(1)2(1)
d.res
created by SHELXL-2018/1 at 11:01:26 on 08-Feb-2018
REM Old TITL D in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.183, Rweak 0.056, Alpha 0.007, Orientation as input
REM Flack x = 0.108 ( 0.008 ) from Parsons' quotients
REM Formula found by SHELXT: C36 N13 S6 Fe3
CELL 0.71073 10.9722 11.4751 31.8776 90 90 90
ZERR 4 0.0042 0.0057 0.0108 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Fe N O S
UNIT 72 104 12 120 4 24
ISOR 0.005 0.01 N4 N23 N24
ISOR 0.005 0.01 N3
L.S. 100
PLAN 2
SIZE 0.102 0.186 0.227
TEMP -123
BOND $H
htab
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.000000 26.419800
FVAR 0.09976
FE1 3 0.179645 0.071823 0.120034 11.00000 0.03654 0.01911 =
0.01874 -0.00154 -0.00846 0.00311
FE2 3 0.319363 0.116353 0.230517 11.00000 0.05111 0.02288 =
0.01930 -0.00179 -0.01327 0.00068
FE3 3 0.051865 0.049073 0.006084 11.00000 0.08902 0.04032 =
0.02067 -0.01244 -0.01253 0.02739
N1 4 0.315257 0.195943 0.135061 11.00000 0.07375 0.02288 =
0.01818 -0.01050 -0.01395 0.01054
N2 4 0.362117 0.214615 0.175179 11.00000 0.03514 0.02608 =
0.01560 -0.00267 -0.01217 0.00368
N3 4 0.424525 0.353452 0.133752 11.00000 0.03769 0.02200 =
0.02378 -0.00165 -0.00304 0.00090
N4 4 0.480697 0.458340 0.121909 11.00000 0.05625 0.02981 =
0.03613 0.00054 -0.00343 0.00384
AFIX 7
H4A 2 0.552260 0.444388 0.112499 11.00000 -1.20000
H4B 2 0.439200 0.491839 0.102508 11.00000 -1.20000
AFIX 0
N5 4 0.079456 0.113308 0.174964 11.00000 0.03680 0.02004 =
0.02059 0.00178 -0.00178 0.00242
N6 4 0.130534 0.133085 0.214435 11.00000 0.04628 0.02106 =
0.01138 -0.00733 -0.00164 -0.00410
N7 4 -0.063273 0.160754 0.218187 11.00000 0.03864 0.02537 =
0.02760 -0.00050 0.00866 0.00027
N8 4 -0.180081 0.185981 0.234872 11.00000 0.06065 0.03667 =
0.04987 -0.00734 0.03506 -0.00216
AFIX 7
H8A 2 -0.215344 0.122785 0.242886 11.00000 -1.20000
H8B 2 -0.171041 0.231209 0.256213 11.00000 -1.20000
AFIX 0
N9 4 0.267750 -0.064909 0.154197 11.00000 0.04311 0.02874 =
0.01352 0.00106 -0.00883 -0.00606
N10 4 0.322399 -0.044407 0.193144 11.00000 0.04190 0.01996 =
0.02164 -0.00148 -0.02116 -0.00047
N11 4 0.342714 -0.227724 0.176426 11.00000 0.03437 0.02046 =
0.02536 -0.00964 -0.00776 -0.00003
N12 4 0.380743 -0.345853 0.179607 11.00000 0.05513 0.02686 =
0.03580 -0.01078 -0.01796 0.00771
AFIX 7
H12A 2 0.319397 -0.393574 0.180179 11.00000 -1.20000
H12B 2 0.425791 -0.365276 0.158416 11.00000 -1.20000
AFIX 0
N13 4 0.084548 0.204877 0.088742 11.00000 0.03854 0.03222 =
0.02167 -0.01008 -0.00962 0.00850
N14 4 0.029269 0.190659 0.050148 11.00000 0.06315 0.03334 =
0.01980 -0.00451 -0.00051 0.02014
N15 4 -0.023276 0.358469 0.075693 11.00000 0.06876 0.02754 =
0.01312 0.00156 0.00468 0.00828
N16 4 -0.077209 0.467582 0.078541 11.00000 0.07574 0.02679 =
0.03842 -0.00155 0.01154 0.01451
AFIX 3
H16A 2 -0.019579 0.521432 0.082291 11.00000 -1.20000
H16B 2 -0.125679 0.468952 0.100981 11.00000 -1.20000
AFIX 0
N17 4 0.041500 -0.047921 0.100743 11.00000 0.04707 0.02315 =
0.03074 0.00204 0.00494 0.00413
N18 4 -0.002746 -0.060349 0.059951 11.00000 0.05754 0.03417 =
0.04259 -0.01786 -0.01535 0.01136
N19 4 -0.091211 -0.189609 0.098701 11.00000 0.03378 0.02709 =
0.09007 -0.01957 0.00038 0.00200
N20 4 -0.160598 -0.287481 0.110231 11.00000 0.05609 0.03346 =
0.18189 -0.03519 0.03060 -0.02134
AFIX 7
H20A 2 -0.124944 -0.323666 0.130209 11.00000 -1.20000
H20B 2 -0.230695 -0.265560 0.118414 11.00000 -1.20000
AFIX 0
N21 4 0.282792 0.032309 0.065883 11.00000 0.03518 0.02321 =
0.06878 -0.00230 0.00219 0.00163
N22 4 0.230729 0.007694 0.028100 11.00000 0.08039 0.03609 =
0.03560 0.01055 0.01372 0.02180
N23 4 0.418369 -0.042191 0.025473 11.00000 0.07749 0.08804 =
0.07096 0.02958 0.02882 0.01010
N24 4 0.529568 -0.087761 0.010314 11.00000 0.13551 0.19576 =
0.13792 0.04878 0.05954 0.04040
AFIX 7
H24A 2 0.592556 -0.048672 0.021599 11.00000 -1.20000
H24B 2 0.545501 -0.162984 0.016871 11.00000 -1.20000
AFIX 0
N25 4 0.280802 0.014900 0.283512 11.00000 0.08229 0.03171 =
0.02091 -0.00036 -0.01603 -0.01061
N26 4 0.324577 0.270743 0.267143 11.00000 0.06850 0.03274 =
0.02409 -0.00057 -0.00774 -0.00592
N27 4 0.067922 -0.097048 -0.035200 11.00000 0.10225 0.04547 =
0.04125 -0.02184 -0.02331 0.02773
N28 4 0.117757 0.171532 -0.037801 11.00000 0.10614 0.05527 =
0.01639 -0.00278 -0.00908 0.03493
N29 4 -0.133358 0.061019 -0.015319 11.00000 0.09490 0.10065 =
0.03539 -0.01127 -0.02547 0.02679
N30 4 0.040708 0.628321 0.158403 11.00000 0.09110 0.03736 =
0.05369 0.01162 0.00876 0.00381
C1 1 0.357110 0.279523 0.111144 11.00000 0.06113 0.02859 =
0.02669 -0.00985 -0.00694 0.00767
AFIX 43
H1 2 0.341788 0.286632 0.081925 11.00000 -1.20000
AFIX 0
C2 1 0.425859 0.312101 0.172879 11.00000 0.05036 0.02969 =
0.01707 -0.00889 -0.00700 0.01034
AFIX 43
H2 2 0.466793 0.347677 0.195805 11.00000 -1.20000
AFIX 0
C3 1 -0.035221 0.129280 0.178889 11.00000 0.04701 0.01476 =
0.02032 0.00120 -0.00312 -0.00708
AFIX 43
H3 2 -0.092846 0.120073 0.156895 11.00000 -1.20000
AFIX 0
C4 1 0.040209 0.162039 0.238989 11.00000 0.08096 0.02029 =
0.01036 -0.00230 0.00419 0.00182
AFIX 43
H4 2 0.048148 0.181329 0.267841 11.00000 -1.20000
AFIX 0
C5 1 0.282327 -0.175435 0.145053 11.00000 0.03282 0.03302 =
0.02057 -0.00776 -0.00897 -0.00318
AFIX 43
H5 2 0.254562 -0.212547 0.120187 11.00000 -1.20000
AFIX 0
C6 1 0.365624 -0.144151 0.204580 11.00000 0.03662 0.03249 =
0.02228 0.00119 -0.01942 0.00228
AFIX 43
H6 2 0.408693 -0.156696 0.230035 11.00000 -1.20000
AFIX 0
C7 1 -0.016071 -0.125752 0.123654 11.00000 0.04670 0.03392 =
0.04316 -0.01260 -0.00808 0.01395
AFIX 43
H7 2 -0.006629 -0.135795 0.153056 11.00000 -1.20000
AFIX 0
C8 1 -0.080264 -0.145424 0.059492 11.00000 0.05713 0.04335 =
0.07104 -0.01787 -0.02742 0.01174
AFIX 43
H8 2 -0.122764 -0.172568 0.035437 11.00000 -1.20000
AFIX 0
C9 1 0.399573 0.002380 0.063887 11.00000 0.07008 0.02960 =
0.10065 0.01753 0.01153 -0.00170
AFIX 43
H9 2 0.458530 0.010874 0.085497 11.00000 -1.20000
AFIX 0
C10 1 0.314183 -0.040046 0.004736 11.00000 0.07770 0.10940 =
0.04896 0.04404 0.03644 0.04714
AFIX 43
H10 2 0.302074 -0.068831 -0.022893 11.00000 -1.20000
AFIX 0
C11 1 0.048259 0.306589 0.103074 11.00000 0.04667 0.02787 =
0.02160 -0.00580 -0.00704 0.00113
AFIX 43
H11 2 0.070579 0.338226 0.129521 11.00000 -1.20000
AFIX 0
C12 1 -0.037926 0.285267 0.043294 11.00000 0.06294 0.03394 =
0.02748 -0.00588 -0.01275 0.01887
AFIX 43
H12 2 -0.087908 0.298710 0.019445 11.00000 -1.20000
AFIX 0
C13 1 0.267214 -0.050156 0.309961 11.00000 0.07809 0.03723 =
0.02618 -0.00462 -0.01585 -0.00141
C14 1 0.319605 0.346462 0.290058 11.00000 0.05169 0.03957 =
0.01333 0.00532 -0.00408 -0.00168
C15 1 0.060988 -0.164436 -0.061346 11.00000 0.09496 0.03591 =
0.03672 -0.00937 -0.00199 0.00234
C16 1 0.146123 0.253518 -0.055430 11.00000 0.06242 0.06177 =
0.02269 -0.01254 -0.01210 0.03380
C17 1 -0.200742 0.007387 -0.036651 11.00000 0.08315 0.08740 =
0.02476 0.00458 0.00676 0.02540
C18 1 0.087147 0.548405 0.175452 11.00000 0.05716 0.03203 =
0.02971 -0.00094 0.00725 0.01017
O1 5 0.512730 0.101031 0.240426 11.00000 0.06452 0.06793 =
0.03836 -0.02590 -0.02064 0.02715
AFIX 3
H1A 2 0.549330 0.056031 0.227756 11.00000 -1.50000
H1B 2 0.535200 0.108571 0.266956 11.00000 -1.50000
AFIX 0
S1 6 0.252369 -0.148711 0.346833 11.00000 0.06892 0.04871 =
0.02446 0.00882 -0.00915 -0.00647
S2 6 0.316650 0.456132 0.323547 11.00000 0.07837 0.02679 =
0.02030 -0.00660 -0.00094 0.00619
S3 6 0.190311 0.368956 -0.082278 11.00000 0.10616 0.05351 =
0.05096 0.00386 -0.01149 0.02294
S4 6 0.052352 -0.260494 -0.099170 11.00000 0.07429 0.04593 =
0.03791 -0.02184 0.01196 -0.01040
S5 6 -0.281089 -0.060219 -0.071363 11.00000 0.06795 0.08218 =
0.06109 -0.00054 0.01186 -0.00443
S6 6 0.153029 0.443182 0.200578 11.00000 0.07390 0.03000 =
0.03288 -0.00516 -0.00748 0.00512
HKLF 4
REM D_a.res in P2(1)2(1)2(1)
REM R1 = 0.0650 for 6008 Fo > 4sig(Fo) and 0.0873 for all 7423 data
REM 528 parameters refined using 24 restraints
END
WGHT 0.0000 26.4262
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, y+1/2, -z+1/2
HTAB N4 S1_$1
EQIV $2 x+1/2, -y+1/2, -z
HTAB N4 S5_$2
EQIV $3 -x, y-1/2, -z+1/2
HTAB N8 S6_$3
EQIV $4 x, y-1, z
HTAB N12 S6_$4
HTAB N12 N4_$4
EQIV $5 x+1/2, -y-1/2, -z
HTAB N12 S4_$5
HTAB N16 S5_$2
EQIV $6 -x, y+1/2, -z+1/2
HTAB N16 S1_$6
HTAB N20 N30_$4
EQIV $7 x-1/2, -y-1/2, -z
HTAB N20 S4_$7
HTAB N24 S3_$2
HTAB N24 S4_$5
HTAB C4 N30_$3
HTAB C9 S3_$2
HTAB C10 N16_$2
HTAB C11 S6
EQIV $8 -x+1, y-1/2, -z+1/2
HTAB O1 S2_$8
HTAB O1 N12_$1
REM Highest difference peak 0.955, deepest hole -0.695, 1-sigma level 0.109
Q1 1 0.5014 -0.1336 0.0033 11.00000 0.05 0.96
Q2 1 -0.3256 -0.0978 -0.0348 11.00000 0.05 0.81
REM The information below was added by Olex2.
REM
REM R1 = 0.0650 for 6008 Fo > 4sig(Fo) and 0.0873 for all 40879 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.96, deepest hole -0.69
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0873
REM R1_gt = 0.0650
REM wR_ref = 0.1340
REM GOOF = 1.068
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 40879
REM Reflections_gt = 6008
REM Parameters = n/a
REM Hole = -0.69
REM Peak = 0.96
REM Flack = 0.042(9)
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_a
_database_code_depnum_ccdc_archive 'CCDC 1578877'
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_audit_creation_date 2018-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2018/1
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C16 H28 Fe3 N28 O2 S4, 2(C N S), H2 O'
_chemical_formula_sum 'C18 H30 Fe3 N30 O3 S6'
_chemical_formula_weight 1074.63
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Fe Fe 0.3463 0.8444 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_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'
_cell_length_a 10.8323(4)
_cell_length_b 11.6921(4)
_cell_length_c 31.5984(11)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4002.0(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9844
_cell_measurement_temperature 100
_cell_measurement_theta_max 27.38
_cell_measurement_theta_min 2.56
_shelx_estimated_absorpt_T_max 0.868
_shelx_estimated_absorpt_T_min 0.811
_exptl_absorpt_coefficient_mu 1.457
_exptl_absorpt_correction_T_max 0.7456
_exptl_absorpt_correction_T_min 0.6468
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0917 before and 0.0588 after correction. The Ratio of minimum to maximum transmission is 0.8675. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.784
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2184
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.13
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0428
_diffrn_reflns_av_unetI/netI 0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 40
_diffrn_reflns_limit_l_min -40
_diffrn_reflns_number 44718
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.487
_diffrn_reflns_theta_min 2.280
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.789
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 0.996
_reflns_number_gt 8138
_reflns_number_total 9133
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution ?
_refine_diff_density_max 0.480
_refine_diff_density_min -0.608
_refine_diff_density_rms 0.073
_refine_ls_abs_structure_details
;
Flack x determined using 3252 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.000(5)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.022
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 541
_refine_ls_number_reflns 9133
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0398
_refine_ls_R_factor_gt 0.0308
_refine_ls_restrained_S_all 1.022
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+2.0406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0603
_refine_ls_wR_factor_ref 0.0626
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups, All O(H,H,H,H,H,H,H,H,H,H) groups
At 1.5 times of:
All O(H,H,H,H,H,H) groups
2.a Riding coordinates:
O3(H8A,H8B,H4A,H4B,H12A,H12B,H20A,H20B,H2A,H2B,H1A,H1B,H16A,H16B,H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
C10(H10), C11(H11), C12(H12)
2.c X=CH2 refined with riding coordinates:
N24(H24A,H24B)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.19880(5) 0.07664(4) 0.12106(2) 0.00781(11) Uani 1 1 d . . . . .
Fe2 Fe 0.33188(5) 0.11296(4) 0.23278(2) 0.00963(12) Uani 1 1 d . . . . .
Fe3 Fe 0.07585(5) 0.06191(4) 0.00726(2) 0.01092(12) Uani 1 1 d . . . . .
N1 N 0.3292(3) 0.1902(2) 0.13670(9) 0.0092(6) Uani 1 1 d . . . . .
N2 N 0.3777(3) 0.2106(3) 0.17662(9) 0.0108(7) Uani 1 1 d . . . . .
N3 N 0.4417(3) 0.3450(3) 0.13459(10) 0.0109(7) Uani 1 1 d . . . . .
N4 N 0.4943(3) 0.4501(2) 0.12209(11) 0.0147(7) Uani 1 1 d . . . . .
N5 N 0.0981(3) 0.1137(3) 0.17212(9) 0.0092(6) Uani 1 1 d . . . . .
N6 N 0.1438(3) 0.1330(3) 0.21253(9) 0.0101(7) Uani 1 1 d . . . . .
N7 N -0.0555(3) 0.1556(3) 0.21353(10) 0.0114(7) Uani 1 1 d . . . . .
N8 N -0.1739(3) 0.1828(3) 0.22929(10) 0.0153(7) Uani 1 1 d . . . . .
N9 N 0.2830(3) -0.0499(2) 0.15224(9) 0.0089(6) Uani 1 1 d . . . . .
N10 N 0.3305(3) -0.0406(2) 0.19300(9) 0.0101(6) Uani 1 1 d . . . . .
N11 N 0.3518(3) -0.2167(2) 0.17169(10) 0.0095(7) Uani 1 1 d . . . . .
N12 N 0.3870(3) -0.3335(3) 0.17271(11) 0.0149(7) Uani 1 1 d . . . . .
N13 N 0.1126(3) 0.2042(3) 0.09228(9) 0.0096(7) Uani 1 1 d . . . . .
N14 N 0.0694(3) 0.2032(3) 0.05101(9) 0.0123(7) Uani 1 1 d . . . . .
N15 N 0.0284(3) 0.3690(3) 0.07897(9) 0.0103(7) Uani 1 1 d . . . . .
N16 N -0.0175(3) 0.4819(3) 0.08191(10) 0.0161(7) Uani 1 1 d . . . . .
N17 N 0.0663(3) -0.0330(2) 0.10236(9) 0.0098(6) Uani 1 1 d . . . . .
N18 N 0.0204(3) -0.0426(3) 0.06131(9) 0.0111(7) Uani 1 1 d . . . . .
N19 N -0.0591(3) -0.1778(2) 0.09974(10) 0.0117(7) Uani 1 1 d . . . . .
N20 N -0.1230(3) -0.2797(3) 0.10977(11) 0.0192(8) Uani 1 1 d . . . . .
N21 N 0.3003(3) 0.0375(2) 0.07084(9) 0.0106(7) Uani 1 1 d . . . . .
N22 N 0.2584(3) 0.0256(3) 0.02971(9) 0.0109(7) Uani 1 1 d . . . . .
N23 N 0.4529(3) -0.0163(3) 0.03113(10) 0.0129(7) Uani 1 1 d . . . . .
N24 N 0.5721(3) -0.0418(3) 0.01590(10) 0.0214(8) Uani 1 1 d . . . . .
H24A H 0.583989 -0.053202 -0.011328 0.026 Uiso 1 1 calc R . . . .
H24B H 0.634536 -0.046435 0.033619 0.026 Uiso 1 1 calc R . . . .
N25 N 0.2864(3) 0.0094(3) 0.28408(11) 0.0209(8) Uani 1 1 d . . . . .
N26 N 0.3330(3) 0.2625(3) 0.27061(10) 0.0151(7) Uani 1 1 d . . . . .
N27 N 0.0723(3) -0.0767(3) -0.03420(10) 0.0147(7) Uani 1 1 d . . . . .
N28 N 0.1371(3) 0.1811(3) -0.03968(10) 0.0164(8) Uani 1 1 d . . . . .
N29 N 0.2741(3) 0.5257(3) 0.07367(11) 0.0192(8) Uani 1 1 d . . . . .
N30 N 0.0748(4) 0.6311(3) 0.16328(11) 0.0241(8) Uani 1 1 d . . . . .
S1 S 0.21935(10) -0.13610(9) 0.35055(3) 0.0195(2) Uani 1 1 d . . . . .
S2 S 0.31681(10) 0.44994(8) 0.32593(3) 0.0160(2) Uani 1 1 d . . . . .
S3 S 0.23501(10) 0.37040(9) -0.08244(3) 0.0193(2) Uani 1 1 d . . . . .
S4 S 0.07445(10) -0.25344(8) -0.09409(3) 0.0158(2) Uani 1 1 d . . . . .
S5 S 0.17361(10) 0.44208(9) 0.20688(3) 0.0199(2) Uani 1 1 d . . . . .
S6 S 0.23493(10) 0.73828(9) 0.03482(3) 0.0204(2) Uani 1 1 d . . . . .
C1 C 0.3713(3) 0.2725(3) 0.11176(12) 0.0112(8) Uani 1 1 d . . . . .
H1 H 0.354613 0.279316 0.082360 0.013 Uiso 1 1 calc R . . . .
C2 C 0.4433(4) 0.3043(3) 0.17429(12) 0.0127(8) Uani 1 1 d . . . . .
H2 H 0.485778 0.338515 0.197335 0.015 Uiso 1 1 calc R . . . .
C3 C -0.0218(3) 0.1268(3) 0.17371(11) 0.0101(8) Uani 1 1 d . . . . .
H3 H -0.076615 0.117597 0.150498 0.012 Uiso 1 1 calc R . . . .
C4 C 0.0493(3) 0.1586(3) 0.23663(12) 0.0123(8) Uani 1 1 d . . . . .
H4 H 0.053784 0.176597 0.265910 0.015 Uiso 1 1 calc R . . . .
C5 C 0.2977(3) -0.1569(3) 0.14003(11) 0.0097(8) Uani 1 1 d . . . . .
H5 H 0.274053 -0.187200 0.113330 0.012 Uiso 1 1 calc R . . . .
C6 C 0.3702(3) -0.1428(3) 0.20340(12) 0.0123(8) Uani 1 1 d . . . . .
H6 H 0.406983 -0.161678 0.229784 0.015 Uiso 1 1 calc R . . . .
C7 C 0.0152(3) -0.1144(3) 0.12467(12) 0.0110(8) Uani 1 1 d . . . . .
H7 H 0.028380 -0.127037 0.154021 0.013 Uiso 1 1 calc R . . . .
C8 C -0.0527(4) -0.1319(3) 0.06074(12) 0.0145(8) Uani 1 1 d . . . . .
H8 H -0.094695 -0.160041 0.036487 0.017 Uiso 1 1 calc R . . . .
C9 C 0.4179(4) 0.0104(3) 0.07068(12) 0.0128(8) Uani 1 1 d . . . . .
H9 H 0.470194 0.009823 0.094813 0.015 Uiso 1 1 calc R . . . .
C10 C 0.3519(4) -0.0074(3) 0.00677(12) 0.0138(8) Uani 1 1 d . . . . .
H10 H 0.348980 -0.022843 -0.022728 0.017 Uiso 1 1 calc R . . . .
C11 C 0.0872(3) 0.3055(3) 0.10829(12) 0.0112(8) Uani 1 1 d . . . . .
H11 H 0.107268 0.329902 0.136133 0.013 Uiso 1 1 calc R . . . .
C12 C 0.0190(4) 0.3030(3) 0.04409(12) 0.0151(9) Uani 1 1 d . . . . .
H12 H -0.018652 0.325708 0.018278 0.018 Uiso 1 1 calc R . . . .
C13 C 0.2568(4) -0.0491(3) 0.31189(13) 0.0152(8) Uani 1 1 d . . . . .
C14 C 0.3245(4) 0.3396(3) 0.29378(12) 0.0127(8) Uani 1 1 d . . . . .
C15 C 0.0727(4) -0.1505(3) -0.05878(12) 0.0120(8) Uani 1 1 d . . . . .
C16 C 0.1776(4) 0.2590(3) -0.05762(12) 0.0142(8) Uani 1 1 d . . . . .
C17 C 0.2593(3) 0.6147(4) 0.05787(12) 0.0150(9) Uani 1 1 d . . . . .
C18 C 0.1130(4) 0.5513(4) 0.18100(12) 0.0172(9) Uani 1 1 d . . . . .
O1 O 0.5283(3) 0.1005(2) 0.24364(9) 0.0229(7) Uani 1 1 d . . . . .
O2 O -0.1156(2) 0.1051(2) -0.00734(9) 0.0179(6) Uani 1 1 d . . . . .
O3 O 0.9560(4) 0.3798(3) 0.27784(11) 0.0514(10) Uani 1 1 d . . . . .
H8A H -0.213385 0.116729 0.236890 0.062 Uiso 1 1 d R . . . .
H8B H -0.219955 0.209979 0.208960 0.062 Uiso 1 1 d R . . . .
H4A H 0.564385 0.439229 0.115910 0.062 Uiso 1 1 d R . . . .
H4B H 0.438205 0.484329 0.107870 0.062 Uiso 1 1 d R . . . .
H12A H 0.448865 -0.342601 0.159350 0.062 Uiso 1 1 d R . . . .
H12B H 0.325345 -0.376711 0.169270 0.062 Uiso 1 1 d R . . . .
H20A H -0.090825 -0.317091 0.131610 0.062 Uiso 1 1 d R . . . .
H20B H -0.201855 -0.270631 0.118050 0.062 Uiso 1 1 d R . . . .
H2A H -0.156655 0.057219 -0.024570 0.077 Uiso 1 1 d R . . . .
H2B H -0.168385 0.103239 0.015000 0.077 Uiso 1 1 d R . . . .
H1A H 0.545455 0.090529 0.269490 0.077 Uiso 1 1 d R . . . .
H1B H 0.555925 0.043529 0.228220 0.077 Uiso 1 1 d R . . . .
H16A H 0.040445 0.524649 0.087790 0.062 Uiso 1 1 d R . . . .
H16B H -0.067395 0.478519 0.105970 0.062 Uiso 1 1 d R . . . .
H3A H 0.905675 0.410359 0.267980 0.077 Uiso 1 1 d R . . . .
H3B H 1.028005 0.394109 0.262120 0.077 Uiso 1 1 d R . . . .
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 0.0091(3) 0.0092(2) 0.0052(2) -0.0001(2) -0.0006(2) 0.0005(2)
Fe2 0.0116(3) 0.0109(3) 0.0064(3) 0.0001(2) -0.0015(2) -0.0005(2)
Fe3 0.0149(3) 0.0109(3) 0.0069(3) -0.0008(2) -0.0012(2) 0.0012(2)
N1 0.0100(16) 0.0113(15) 0.0063(15) -0.0012(12) -0.0005(13) 0.0012(13)
N2 0.0111(16) 0.0146(16) 0.0066(16) -0.0003(13) -0.0032(13) -0.0006(14)
N3 0.0107(17) 0.0120(16) 0.0099(16) 0.0015(12) 0.0003(13) -0.0001(14)
N4 0.0149(17) 0.0101(16) 0.0191(18) 0.0031(14) -0.0002(14) -0.0023(14)
N5 0.0135(17) 0.0100(14) 0.0040(15) -0.0017(12) -0.0016(12) -0.0006(13)
N6 0.0110(16) 0.0137(16) 0.0055(15) -0.0008(13) -0.0015(12) -0.0016(13)
N7 0.0087(16) 0.0136(15) 0.0118(16) -0.0025(13) 0.0022(13) 0.0016(13)
N8 0.0104(17) 0.0204(17) 0.0150(17) -0.0002(14) 0.0058(14) 0.0017(14)
N9 0.0075(15) 0.0128(16) 0.0063(14) 0.0011(12) 0.0008(12) -0.0007(13)
N10 0.0117(16) 0.0119(16) 0.0067(15) 0.0004(12) -0.0033(13) 0.0014(13)
N11 0.0105(16) 0.0080(15) 0.0101(16) 0.0002(12) -0.0013(13) 0.0006(12)
N12 0.0191(18) 0.0065(15) 0.0190(18) 0.0006(13) 0.0001(15) 0.0026(13)
N13 0.0114(16) 0.0106(15) 0.0068(16) 0.0004(13) -0.0012(13) -0.0007(13)
N14 0.0169(18) 0.0156(16) 0.0046(15) -0.0013(13) -0.0028(14) 0.0025(15)
N15 0.0128(16) 0.0105(16) 0.0076(16) -0.0014(13) -0.0015(13) 0.0024(13)
N16 0.024(2) 0.0095(15) 0.0149(18) -0.0006(14) -0.0008(15) 0.0058(14)
N17 0.0118(16) 0.0107(15) 0.0067(15) -0.0007(12) 0.0000(13) 0.0022(14)
N18 0.0112(16) 0.0155(17) 0.0066(16) -0.0026(13) -0.0017(13) 0.0007(14)
N19 0.0110(17) 0.0128(16) 0.0112(17) 0.0007(13) 0.0011(13) -0.0013(14)
N20 0.0182(19) 0.0140(17) 0.025(2) 0.0045(15) -0.0010(15) -0.0048(14)
N21 0.0133(17) 0.0090(15) 0.0096(15) -0.0013(12) -0.0003(13) 0.0003(14)
N22 0.0134(17) 0.0114(15) 0.0079(15) 0.0000(12) -0.0007(13) -0.0016(13)
N23 0.0113(18) 0.0146(16) 0.0129(17) 0.0014(13) 0.0045(13) 0.0024(14)
N24 0.0123(17) 0.043(2) 0.0088(17) 0.0018(15) 0.0062(14) 0.0088(17)
N25 0.030(2) 0.0200(18) 0.0127(17) 0.0005(15) -0.0038(16) -0.0071(17)
N26 0.0170(18) 0.0145(16) 0.0136(16) -0.0001(14) -0.0029(14) 0.0007(15)
N27 0.0177(18) 0.0159(16) 0.0106(16) 0.0010(14) -0.0045(14) 0.0014(15)
N28 0.024(2) 0.0144(17) 0.0103(17) -0.0002(14) -0.0006(15) -0.0035(15)
N29 0.0162(19) 0.0227(19) 0.0186(18) 0.0045(16) -0.0003(15) 0.0010(15)
N30 0.030(2) 0.0232(19) 0.0190(19) -0.0002(16) -0.0063(17) 0.0042(18)
S1 0.0218(6) 0.0232(5) 0.0135(5) 0.0059(4) 0.0001(4) -0.0069(5)
S2 0.0241(6) 0.0131(5) 0.0109(5) -0.0021(4) 0.0011(4) 0.0015(4)
S3 0.0253(6) 0.0169(5) 0.0156(5) 0.0006(4) 0.0044(4) -0.0043(4)
S4 0.0180(5) 0.0157(5) 0.0138(5) -0.0056(4) -0.0006(4) -0.0008(4)
S5 0.0271(6) 0.0168(5) 0.0157(5) -0.0006(4) -0.0046(4) 0.0042(5)
S6 0.0277(6) 0.0157(5) 0.0177(5) -0.0013(4) -0.0070(5) 0.0025(5)
C1 0.0105(19) 0.0135(19) 0.0097(19) -0.0002(15) -0.0019(15) 0.0011(16)
C2 0.013(2) 0.0153(19) 0.0101(19) -0.0010(16) -0.0018(16) 0.0005(16)
C3 0.0109(19) 0.0113(18) 0.0079(18) -0.0010(16) 0.0000(15) 0.0019(16)
C4 0.014(2) 0.0134(18) 0.0099(19) -0.0006(15) -0.0005(16) -0.0021(16)
C5 0.0089(19) 0.0121(18) 0.0081(17) -0.0008(14) -0.0002(15) -0.0014(16)
C6 0.013(2) 0.015(2) 0.0097(19) -0.0017(16) -0.0020(16) -0.0019(16)
C7 0.0115(19) 0.0120(17) 0.0095(18) -0.0029(16) -0.0019(15) 0.0005(16)
C8 0.016(2) 0.017(2) 0.0105(19) -0.0023(16) -0.0002(16) 0.0025(18)
C9 0.017(2) 0.0103(18) 0.0112(19) -0.0003(15) -0.0001(17) 0.0020(17)
C10 0.019(2) 0.0136(19) 0.0088(18) -0.0007(16) 0.0008(16) -0.0003(16)
C11 0.012(2) 0.0139(18) 0.0080(18) -0.0009(15) -0.0035(16) 0.0010(16)
C12 0.024(2) 0.016(2) 0.0055(19) -0.0015(16) -0.0038(17) 0.0021(18)
C13 0.013(2) 0.018(2) 0.015(2) -0.0031(17) -0.0064(16) -0.0002(17)
C14 0.013(2) 0.0155(19) 0.0100(19) 0.0039(16) -0.0002(16) 0.0016(17)
C15 0.0093(19) 0.0149(19) 0.0118(19) 0.0033(16) -0.0019(16) -0.0003(16)
C16 0.016(2) 0.017(2) 0.0098(18) -0.0032(16) -0.0024(16) 0.0030(18)
C17 0.009(2) 0.023(2) 0.013(2) -0.0056(18) 0.0012(16) -0.0001(18)
C18 0.018(2) 0.023(2) 0.011(2) -0.0048(18) -0.0005(16) -0.0006(18)
O1 0.0193(16) 0.0335(17) 0.0159(15) -0.0096(13) -0.0067(12) 0.0088(14)
O2 0.0157(15) 0.0217(15) 0.0163(14) -0.0037(12) -0.0010(12) 0.0032(12)
O3 0.060(3) 0.053(2) 0.041(2) -0.0022(19) -0.0015(19) 0.010(2)
_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 N1 2.001(3) . ?
Fe1 N5 1.995(3) . ?
Fe1 N9 1.998(3) . ?
Fe1 N13 1.981(3) . ?
Fe1 N17 2.013(3) . ?
Fe1 N21 1.984(3) . ?
Fe2 N2 2.167(3) . ?
Fe2 N6 2.148(3) . ?
Fe2 N10 2.192(3) . ?
Fe2 N25 2.082(3) . ?
Fe2 N26 2.118(3) . ?
Fe2 O1 2.160(3) . ?
Fe3 N14 2.155(3) . ?
Fe3 N18 2.184(3) . ?
Fe3 N22 2.144(3) . ?
Fe3 N27 2.084(3) . ?
Fe3 N28 2.141(3) . ?
Fe3 O2 2.184(3) . ?
N1 N2 1.387(4) . ?
N1 C1 1.324(5) . ?
N2 C2 1.308(5) . ?
N3 N4 1.411(4) . ?
N3 C1 1.349(5) . ?
N3 C2 1.342(5) . ?
N4 H4A 0.7944 . ?
N4 H4B 0.8549 . ?
N5 N6 1.388(4) . ?
N5 C3 1.309(5) . ?
N6 C4 1.311(5) . ?
N7 N8 1.412(4) . ?
N7 C3 1.353(5) . ?
N7 C4 1.350(5) . ?
N8 H8A 0.9149 . ?
N8 H8B 0.8737 . ?
N9 N10 1.391(4) . ?
N9 C5 1.319(5) . ?
N10 C6 1.311(5) . ?
N11 N12 1.419(4) . ?
N11 C5 1.354(5) . ?
N11 C6 1.338(5) . ?
N12 H12A 0.7993 . ?
N12 H12B 0.8443 . ?
N13 N14 1.386(4) . ?
N13 C11 1.317(5) . ?
N14 C12 1.306(5) . ?
N15 N16 1.413(4) . ?
N15 C11 1.348(5) . ?
N15 C12 1.350(5) . ?
N16 H16A 0.8238 . ?
N16 H16B 0.9338 . ?
N17 N18 1.394(4) . ?
N17 C7 1.308(5) . ?
N18 C8 1.311(5) . ?
N19 N20 1.414(4) . ?
N19 C7 1.348(5) . ?
N19 C8 1.346(5) . ?
N20 H20A 0.8885 . ?
N20 H20B 0.8993 . ?
N21 N22 1.384(4) . ?
N21 C9 1.312(5) . ?
N22 C10 1.303(5) . ?
N23 N24 1.410(4) . ?
N23 C9 1.343(5) . ?
N23 C10 1.341(5) . ?
N24 H24A 0.8800 . ?
N24 H24B 0.8800 . ?
N25 C13 1.159(5) . ?
N26 C14 1.165(5) . ?
N27 C15 1.161(5) . ?
N28 C16 1.159(5) . ?
N29 C17 1.165(5) . ?
N30 C18 1.164(5) . ?
S1 C13 1.640(4) . ?
S2 C14 1.644(4) . ?
S3 C16 1.643(4) . ?
S4 C15 1.642(4) . ?
S5 C18 1.653(4) . ?
S6 C17 1.640(4) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
O1 H1A 0.8457 . ?
O1 H1B 0.8777 . ?
O2 H2A 0.8985 . ?
O2 H2B 0.9086 . ?
O3 H3A 0.7226 . ?
O3 H3B 0.9395 . ?
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
N1 Fe1 N17 176.88(12) . . ?
N5 Fe1 N1 92.40(12) . . ?
N5 Fe1 N9 90.65(12) . . ?
N5 Fe1 N17 89.19(12) . . ?
N9 Fe1 N1 92.73(12) . . ?
N9 Fe1 N17 89.93(12) . . ?
N13 Fe1 N1 86.92(12) . . ?
N13 Fe1 N5 87.15(12) . . ?
N13 Fe1 N9 177.75(13) . . ?
N13 Fe1 N17 90.49(12) . . ?
N13 Fe1 N21 93.89(12) . . ?
N21 Fe1 N1 87.68(12) . . ?
N21 Fe1 N5 178.97(13) . . ?
N21 Fe1 N9 88.31(12) . . ?
N21 Fe1 N17 90.78(12) . . ?
N2 Fe2 N10 87.91(11) . . ?
N6 Fe2 N2 85.16(11) . . ?
N6 Fe2 N10 84.94(11) . . ?
N6 Fe2 O1 171.42(11) . . ?
N25 Fe2 N2 176.09(13) . . ?
N25 Fe2 N6 94.07(13) . . ?
N25 Fe2 N10 88.20(12) . . ?
N25 Fe2 N26 92.40(13) . . ?
N25 Fe2 O1 94.01(13) . . ?
N26 Fe2 N2 91.49(12) . . ?
N26 Fe2 N6 94.80(12) . . ?
N26 Fe2 N10 179.36(12) . . ?
N26 Fe2 O1 87.72(12) . . ?
O1 Fe2 N2 86.57(12) . . ?
O1 Fe2 N10 92.44(11) . . ?
N14 Fe3 N18 85.31(12) . . ?
N14 Fe3 O2 85.84(11) . . ?
N18 Fe3 O2 91.90(11) . . ?
N22 Fe3 N14 88.27(12) . . ?
N22 Fe3 N18 83.34(11) . . ?
N22 Fe3 O2 172.72(11) . . ?
N27 Fe3 N14 176.92(14) . . ?
N27 Fe3 N18 92.96(12) . . ?
N27 Fe3 N22 94.06(12) . . ?
N27 Fe3 N28 94.39(12) . . ?
N27 Fe3 O2 91.69(12) . . ?
N28 Fe3 N14 87.44(12) . . ?
N28 Fe3 N18 172.39(12) . . ?
N28 Fe3 N22 94.15(13) . . ?
N28 Fe3 O2 89.87(12) . . ?
N2 N1 Fe1 127.3(2) . . ?
C1 N1 Fe1 125.3(3) . . ?
C1 N1 N2 106.6(3) . . ?
N1 N2 Fe2 124.6(2) . . ?
C2 N2 Fe2 127.7(3) . . ?
C2 N2 N1 107.4(3) . . ?
C1 N3 N4 128.7(3) . . ?
C2 N3 N4 124.5(3) . . ?
C2 N3 C1 106.5(3) . . ?
N3 N4 H4A 108.4 . . ?
N3 N4 H4B 105.6 . . ?
H4A N4 H4B 128.7 . . ?
N6 N5 Fe1 125.8(2) . . ?
C3 N5 Fe1 126.8(2) . . ?
C3 N5 N6 107.4(3) . . ?
N5 N6 Fe2 126.5(2) . . ?
C4 N6 Fe2 126.4(2) . . ?
C4 N6 N5 107.0(3) . . ?
C3 N7 N8 129.0(3) . . ?
C4 N7 N8 124.5(3) . . ?
C4 N7 C3 106.4(3) . . ?
N7 N8 H8A 109.1 . . ?
N7 N8 H8B 110.0 . . ?
H8A N8 H8B 103.5 . . ?
N10 N9 Fe1 124.6(2) . . ?
C5 N9 Fe1 127.8(2) . . ?
C5 N9 N10 107.5(3) . . ?
N9 N10 Fe2 126.7(2) . . ?
C6 N10 Fe2 126.9(2) . . ?
C6 N10 N9 106.4(3) . . ?
C5 N11 N12 129.0(3) . . ?
C6 N11 N12 124.4(3) . . ?
C6 N11 C5 106.5(3) . . ?
N11 N12 H12A 109.9 . . ?
N11 N12 H12B 111.2 . . ?
H12A N12 H12B 121.0 . . ?
N14 N13 Fe1 125.8(2) . . ?
C11 N13 Fe1 126.8(3) . . ?
C11 N13 N14 107.4(3) . . ?
N13 N14 Fe3 126.8(2) . . ?
C12 N14 Fe3 126.2(3) . . ?
C12 N14 N13 106.9(3) . . ?
C11 N15 N16 129.5(3) . . ?
C11 N15 C12 106.3(3) . . ?
C12 N15 N16 124.2(3) . . ?
N15 N16 H16A 108.3 . . ?
N15 N16 H16B 102.6 . . ?
H16A N16 H16B 106.4 . . ?
N18 N17 Fe1 125.4(2) . . ?
C7 N17 Fe1 127.4(3) . . ?
C7 N17 N18 107.0(3) . . ?
N17 N18 Fe3 125.8(2) . . ?
C8 N18 Fe3 127.0(2) . . ?
C8 N18 N17 107.0(3) . . ?
C7 N19 N20 128.6(3) . . ?
C8 N19 N20 124.5(3) . . ?
C8 N19 C7 106.6(3) . . ?
N19 N20 H20A 113.4 . . ?
N19 N20 H20B 115.5 . . ?
H20A N20 H20B 101.8 . . ?
N22 N21 Fe1 126.4(2) . . ?
C9 N21 Fe1 126.6(3) . . ?
C9 N21 N22 106.9(3) . . ?
N21 N22 Fe3 126.4(2) . . ?
C10 N22 Fe3 126.3(3) . . ?
C10 N22 N21 107.3(3) . . ?
C9 N23 N24 128.7(3) . . ?
C10 N23 N24 124.6(3) . . ?
C10 N23 C9 106.6(3) . . ?
N23 N24 H24A 120.0 . . ?
N23 N24 H24B 120.0 . . ?
H24A N24 H24B 120.0 . . ?
C13 N25 Fe2 177.3(3) . . ?
C14 N26 Fe2 173.2(3) . . ?
C15 N27 Fe3 176.7(3) . . ?
C16 N28 Fe3 165.4(3) . . ?
N1 C1 N3 109.5(3) . . ?
N1 C1 H1 125.3 . . ?
N3 C1 H1 125.3 . . ?
N2 C2 N3 110.1(3) . . ?
N2 C2 H2 125.0 . . ?
N3 C2 H2 125.0 . . ?
N5 C3 N7 109.5(3) . . ?
N5 C3 H3 125.3 . . ?
N7 C3 H3 125.3 . . ?
N6 C4 N7 109.7(3) . . ?
N6 C4 H4 125.2 . . ?
N7 C4 H4 125.2 . . ?
N9 C5 N11 109.0(3) . . ?
N9 C5 H5 125.5 . . ?
N11 C5 H5 125.5 . . ?
N10 C6 N11 110.6(3) . . ?
N10 C6 H6 124.7 . . ?
N11 C6 H6 124.7 . . ?
N17 C7 N19 109.7(3) . . ?
N17 C7 H7 125.1 . . ?
N19 C7 H7 125.1 . . ?
N18 C8 N19 109.6(3) . . ?
N18 C8 H8 125.2 . . ?
N19 C8 H8 125.2 . . ?
N21 C9 N23 109.5(3) . . ?
N21 C9 H9 125.3 . . ?
N23 C9 H9 125.3 . . ?
N22 C10 N23 109.7(3) . . ?
N22 C10 H10 125.1 . . ?
N23 C10 H10 125.1 . . ?
N13 C11 N15 109.3(3) . . ?
N13 C11 H11 125.4 . . ?
N15 C11 H11 125.4 . . ?
N14 C12 N15 110.1(3) . . ?
N14 C12 H12 125.0 . . ?
N15 C12 H12 125.0 . . ?
N25 C13 S1 177.5(4) . . ?
N26 C14 S2 178.1(4) . . ?
N27 C15 S4 179.0(4) . . ?
N28 C16 S3 179.2(4) . . ?
N29 C17 S6 178.3(4) . . ?
N30 C18 S5 177.0(4) . . ?
Fe2 O1 H1A 112.3 . . ?
Fe2 O1 H1B 107.4 . . ?
H1A O1 H1B 110.9 . . ?
Fe3 O2 H2A 117.0 . . ?
Fe3 O2 H2B 115.3 . . ?
H2A O2 H2B 98.3 . . ?
H3A O3 H3B 108.1 . . ?
_iucr_refine_instructions_details
;
TITL A_a.res in P2(1)2(1)2(1)
a.res
created by SHELXL-2018/1 at 11:50:52 on 08-Feb-2018
REM Old TITL A in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.072, Rweak 0.026, Alpha 0.004, Orientation as input
REM Flack x = 0.016 ( 0.005 ) from Parsons' quotients
REM Formula found by SHELXT: C40 N11 S6 Fe3
CELL 0.71073 10.8323 11.6921 31.5984 90 90 90
ZERR 4 0.0004 0.0004 0.0011 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Fe N O S
UNIT 72 120 12 120 12 24
L.S. 100
PLAN 5
SIZE 0.15 0.13 0.1
TEMP -173.15
BOND $H
HTAB
fmap 2
acta
OMIT 0 2 0
REM
REM
REM
WGHT 0.026000 2.040600
FVAR 0.09246
FE1 3 0.198798 0.076637 0.121060 11.00000 0.00908 0.00916 =
0.00519 -0.00009 -0.00060 0.00053
FE2 3 0.331881 0.112963 0.232780 11.00000 0.01160 0.01090 =
0.00639 0.00013 -0.00150 -0.00048
FE3 3 0.075850 0.061914 0.007257 11.00000 0.01493 0.01091 =
0.00693 -0.00080 -0.00125 0.00120
N1 4 0.329164 0.190228 0.136700 11.00000 0.00997 0.01130 =
0.00631 -0.00123 -0.00048 0.00118
N2 4 0.377654 0.210584 0.176622 11.00000 0.01113 0.01463 =
0.00664 -0.00034 -0.00324 -0.00063
N3 4 0.441726 0.344977 0.134591 11.00000 0.01074 0.01196 =
0.00988 0.00151 0.00035 -0.00010
N4 4 0.494266 0.450081 0.122086 11.00000 0.01492 0.01009 =
0.01915 0.00310 -0.00018 -0.00227
N5 4 0.098150 0.113686 0.172120 11.00000 0.01346 0.01002 =
0.00399 -0.00169 -0.00158 -0.00063
N6 4 0.143813 0.132978 0.212529 11.00000 0.01098 0.01372 =
0.00549 -0.00081 -0.00153 -0.00161
N7 4 -0.055511 0.155647 0.213529 11.00000 0.00868 0.01364 =
0.01185 -0.00255 0.00216 0.00157
N8 4 -0.173868 0.182767 0.229293 11.00000 0.01043 0.02035 =
0.01497 -0.00025 0.00585 0.00168
N9 4 0.282973 -0.049895 0.152240 11.00000 0.00746 0.01284 =
0.00634 0.00111 0.00082 -0.00073
N10 4 0.330484 -0.040635 0.192997 11.00000 0.01167 0.01189 =
0.00670 0.00036 -0.00331 0.00137
N11 4 0.351842 -0.216671 0.171695 11.00000 0.01050 0.00799 =
0.01012 0.00018 -0.00133 0.00063
N12 4 0.386989 -0.333515 0.172712 11.00000 0.01910 0.00646 =
0.01903 0.00059 0.00011 0.00261
N13 4 0.112626 0.204193 0.092282 11.00000 0.01139 0.01057 =
0.00680 0.00041 -0.00117 -0.00073
N14 4 0.069375 0.203223 0.051008 11.00000 0.01690 0.01556 =
0.00456 -0.00128 -0.00282 0.00253
N15 4 0.028352 0.369043 0.078968 11.00000 0.01276 0.01049 =
0.00760 -0.00138 -0.00155 0.00243
N16 4 -0.017491 0.481860 0.081907 11.00000 0.02394 0.00948 =
0.01493 -0.00063 -0.00080 0.00585
N17 4 0.066262 -0.032963 0.102363 11.00000 0.01184 0.01074 =
0.00671 -0.00066 0.00002 0.00225
N18 4 0.020408 -0.042563 0.061305 11.00000 0.01123 0.01552 =
0.00662 -0.00262 -0.00174 0.00072
N19 4 -0.059106 -0.177754 0.099738 11.00000 0.01103 0.01275 =
0.01118 0.00071 0.00113 -0.00132
N20 4 -0.123035 -0.279676 0.109767 11.00000 0.01819 0.01397 =
0.02537 0.00448 -0.00096 -0.00480
N21 4 0.300327 0.037482 0.070838 11.00000 0.01328 0.00899 =
0.00960 -0.00126 -0.00032 0.00028
N22 4 0.258448 0.025556 0.029708 11.00000 0.01345 0.01136 =
0.00788 0.00005 -0.00068 -0.00162
N23 4 0.452859 -0.016305 0.031125 11.00000 0.01125 0.01457 =
0.01290 0.00139 0.00453 0.00240
N24 4 0.572064 -0.041848 0.015898 11.00000 0.01227 0.04312 =
0.00884 0.00181 0.00616 0.00879
AFIX 93
H24A 2 0.583989 -0.053202 -0.011328 11.00000 -1.20000
H24B 2 0.634536 -0.046435 0.033619 11.00000 -1.20000
AFIX 0
N25 4 0.286440 0.009444 0.284081 11.00000 0.02995 0.02000 =
0.01267 0.00051 -0.00383 -0.00705
N26 4 0.333031 0.262518 0.270607 11.00000 0.01704 0.01449 =
0.01363 -0.00013 -0.00295 0.00074
N27 4 0.072314 -0.076677 -0.034197 11.00000 0.01772 0.01586 =
0.01057 0.00098 -0.00446 0.00137
N28 4 0.137117 0.181122 -0.039678 11.00000 0.02449 0.01443 =
0.01031 -0.00021 -0.00063 -0.00351
N29 4 0.274069 0.525696 0.073669 11.00000 0.01616 0.02274 =
0.01862 0.00451 -0.00034 0.00101
N30 4 0.074754 0.631093 0.163282 11.00000 0.03014 0.02316 =
0.01902 -0.00015 -0.00628 0.00421
S1 6 0.219353 -0.136095 0.350547 11.00000 0.02184 0.02322 =
0.01346 0.00592 0.00013 -0.00695
S2 6 0.316810 0.449938 0.325930 11.00000 0.02407 0.01307 =
0.01092 -0.00214 0.00110 0.00153
S3 6 0.235010 0.370399 -0.082445 11.00000 0.02528 0.01688 =
0.01564 0.00059 0.00436 -0.00434
S4 6 0.074452 -0.253442 -0.094090 11.00000 0.01802 0.01568 =
0.01384 -0.00558 -0.00063 -0.00078
S5 6 0.173612 0.442082 0.206881 11.00000 0.02711 0.01685 =
0.01568 -0.00063 -0.00464 0.00421
S6 6 0.234926 0.738281 0.034822 11.00000 0.02773 0.01567 =
0.01770 -0.00127 -0.00700 0.00247
C1 1 0.371333 0.272453 0.111764 11.00000 0.01049 0.01345 =
0.00966 -0.00024 -0.00187 0.00112
AFIX 43
H1 2 0.354613 0.279316 0.082360 11.00000 -1.20000
AFIX 0
C2 1 0.443261 0.304281 0.174291 11.00000 0.01266 0.01531 =
0.01014 -0.00099 -0.00179 0.00049
AFIX 43
H2 2 0.485778 0.338515 0.197335 11.00000 -1.20000
AFIX 0
C3 1 -0.021776 0.126843 0.173710 11.00000 0.01094 0.01130 =
0.00793 -0.00104 0.00005 0.00190
AFIX 43
H3 2 -0.076615 0.117597 0.150498 11.00000 -1.20000
AFIX 0
C4 1 0.049251 0.158633 0.236630 11.00000 0.01359 0.01339 =
0.00989 -0.00064 -0.00051 -0.00208
AFIX 43
H4 2 0.053784 0.176597 0.265910 11.00000 -1.20000
AFIX 0
C5 1 0.297667 -0.156926 0.140029 11.00000 0.00893 0.01212 =
0.00815 -0.00079 -0.00018 -0.00142
AFIX 43
H5 2 0.274053 -0.187200 0.113330 11.00000 -1.20000
AFIX 0
C6 1 0.370231 -0.142778 0.203398 11.00000 0.01260 0.01472 =
0.00972 -0.00170 -0.00196 -0.00185
AFIX 43
H6 2 0.406983 -0.161678 0.229784 11.00000 -1.20000
AFIX 0
C7 1 0.015152 -0.114419 0.124669 11.00000 0.01149 0.01196 =
0.00951 -0.00290 -0.00194 0.00047
AFIX 43
H7 2 0.028380 -0.127037 0.154021 11.00000 -1.20000
AFIX 0
C8 1 -0.052675 -0.131924 0.060739 11.00000 0.01618 0.01685 =
0.01049 -0.00234 -0.00018 0.00250
AFIX 43
H8 2 -0.094695 -0.160041 0.036487 11.00000 -1.20000
AFIX 0
C9 1 0.417902 0.010417 0.070678 11.00000 0.01683 0.01028 =
0.01123 -0.00031 -0.00005 0.00204
AFIX 43
H9 2 0.470194 0.009823 0.094813 11.00000 -1.20000
AFIX 0
C10 1 0.351918 -0.007426 0.006773 11.00000 0.01911 0.01361 =
0.00875 -0.00070 0.00075 -0.00029
AFIX 43
H10 2 0.348980 -0.022843 -0.022728 11.00000 -1.20000
AFIX 0
C11 1 0.087241 0.305466 0.108294 11.00000 0.01177 0.01388 =
0.00804 -0.00094 -0.00354 0.00102
AFIX 43
H11 2 0.107268 0.329902 0.136133 11.00000 -1.20000
AFIX 0
C12 1 0.019029 0.302972 0.044090 11.00000 0.02355 0.01614 =
0.00554 -0.00153 -0.00382 0.00210
AFIX 43
H12 2 -0.018652 0.325708 0.018278 11.00000 -1.20000
AFIX 0
C13 1 0.256770 -0.049125 0.311889 11.00000 0.01317 0.01771 =
0.01472 -0.00306 -0.00639 -0.00018
C14 1 0.324452 0.339595 0.293785 11.00000 0.01262 0.01554 =
0.00997 0.00393 -0.00024 0.00158
C15 1 0.072656 -0.150482 -0.058776 11.00000 0.00930 0.01487 =
0.01184 0.00335 -0.00187 -0.00028
C16 1 0.177588 0.259013 -0.057622 11.00000 0.01562 0.01730 =
0.00979 -0.00315 -0.00243 0.00302
C17 1 0.259265 0.614690 0.057870 11.00000 0.00906 0.02343 =
0.01251 -0.00563 0.00122 -0.00010
C18 1 0.112989 0.551341 0.181003 11.00000 0.01822 0.02264 =
0.01084 -0.00484 -0.00047 -0.00063
O1 5 0.528335 0.100499 0.243638 11.00000 0.01928 0.03351 =
0.01585 -0.00958 -0.00668 0.00877
O2 5 -0.115605 0.105072 -0.007339 11.00000 0.01568 0.02175 =
0.01629 -0.00367 -0.00104 0.00324
O3 5 0.956025 0.379809 0.277840 11.00000 0.05977 0.05303 =
0.04144 -0.00219 -0.00150 0.00963
AFIX 3
H8A 2 -0.213385 0.116729 0.236890 11.00000 -1.20000
H8B 2 -0.219955 0.209979 0.208960 11.00000 -1.20000
H4A 2 0.564385 0.439229 0.115910 11.00000 -1.20000
H4B 2 0.438205 0.484329 0.107870 11.00000 -1.20000
H12A 2 0.448865 -0.342601 0.159350 11.00000 -1.20000
H12B 2 0.325345 -0.376711 0.169270 11.00000 -1.20000
H20A 2 -0.090825 -0.317091 0.131610 11.00000 -1.20000
H20B 2 -0.201855 -0.270631 0.118050 11.00000 -1.20000
H2A 2 -0.156655 0.057219 -0.024570 11.00000 -1.50000
H2B 2 -0.168385 0.103239 0.015000 11.00000 -1.50000
H1A 2 0.545455 0.090529 0.269490 11.00000 -1.50000
H1B 2 0.555925 0.043529 0.228220 11.00000 -1.50000
H16A 2 0.040445 0.524649 0.087790 11.00000 -1.20000
H16B 2 -0.067395 0.478519 0.105970 11.00000 -1.20000
H3A 2 0.905675 0.410359 0.267980 11.00000 -1.50000
H3B 2 1.028005 0.394109 0.262120 11.00000 -1.50000
AFIX 0
HKLF 4
REM A_a.res in P2(1)2(1)2(1)
REM R1 = 0.0308 for 8138 Fo > 4sig(Fo) and 0.0398 for all 9133 data
REM 541 parameters refined using 0 restraints
END
WGHT 0.0261 2.0314
REM Instructions for potential hydrogen bonds
EQIV $1 x+1/2, -y+1/2, -z
HTAB N24 N16_$1
HTAB N24 S6_$1
HTAB N24 S3_$1
EQIV $2 x-1/2, -y+1/2, -z
HTAB C3 S3_$2
EQIV $3 -x, y-1/2, -z+1/2
HTAB C4 N30_$3
EQIV $4 x, y-1, z
HTAB C5 S6_$4
EQIV $5 -x+1, y-1/2, -z+1/2
HTAB C7 O3_$5
HTAB C10 N16_$1
HTAB C11 S5
HTAB N8 S2_$3
HTAB N8 S5_$3
EQIV $6 -x, y+1/2, -z+1/2
HTAB N8 S1_$6
EQIV $7 -x+1, y+1/2, -z+1/2
HTAB N4 S1_$7
HTAB N4 N29
EQIV $8 x+1/2, -y-1/2, -z
HTAB N12 S4_$8
HTAB N12 S5_$4
HTAB N20 N30_$4
EQIV $9 x-1/2, -y-1/2, -z
HTAB N20 S4_$9
HTAB O2 N29_$2
HTAB O2 S3_$2
HTAB O1 N12_$7
HTAB O1 S2_$5
HTAB N16 N29
HTAB N16 S1_$6
EQIV $10 x+1, y, z
HTAB O3 S5_$10
REM Highest difference peak 0.480, deepest hole -0.608, 1-sigma level 0.073
Q1 1 0.5788 -0.1238 0.0157 11.00000 0.05 0.48
Q2 1 0.2211 -0.0511 0.3611 11.00000 0.05 0.30
Q3 1 0.1585 0.7032 0.0289 11.00000 0.05 0.30
Q4 1 0.1819 0.1602 0.1311 11.00000 0.05 0.28
Q5 1 0.6351 0.0196 0.0285 11.00000 0.05 0.28
REM The information below was added by Olex2.
REM
REM R1 = 0.0308 for 8138 Fo > 4sig(Fo) and 0.0398 for all 44818 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.48, deepest hole -0.61
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0398
REM R1_gt = 0.0308
REM wR_ref = 0.0626
REM GOOF = 1.022
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 44818
REM Reflections_gt = 8138
REM Parameters = n/a
REM Hole = -0.61
REM Peak = 0.48
REM Flack = 0.000(5)
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_c
_database_code_depnum_ccdc_archive 'CCDC 1578880'
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_audit_creation_date 2018-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C17 H26 Fe3 N29 O S5, C N S'
_chemical_formula_sum 'C18 H26 Fe3 N30 O S6'
_chemical_formula_weight 1038.60
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Fe Fe 0.3463 0.8444 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_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'
_cell_length_a 11.131(3)
_cell_length_b 11.508(5)
_cell_length_c 32.090(9)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 4110(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9884
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 23.534
_cell_measurement_theta_min 2.541
_shelx_estimated_absorpt_T_max 0.869
_shelx_estimated_absorpt_T_min 0.740
_exptl_absorpt_coefficient_mu 1.412
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_correction_T_min 0.6314
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0702 before and 0.0641 after correction. The Ratio of minimum to maximum transmission is 0.8473. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.678
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2104
_exptl_crystal_size_max 0.227
_exptl_crystal_size_mid 0.186
_exptl_crystal_size_min 0.102
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0564
_diffrn_reflns_av_unetI/netI 0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 38
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_number 42839
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.414
_diffrn_reflns_theta_max 25.414
_diffrn_reflns_theta_min 2.539
_diffrn_ambient_temperature 293.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.779
_reflns_Friedel_fraction_full 0.997
_reflns_Friedel_fraction_max 0.997
_reflns_number_gt 5852
_reflns_number_total 7567
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution ?
_refine_diff_density_max 0.608
_refine_diff_density_min -0.540
_refine_diff_density_rms 0.070
_refine_ls_abs_structure_details
;
Flack x determined using 2133 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.023(8)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.019
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 529
_refine_ls_number_reflns 7567
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0718
_refine_ls_R_factor_gt 0.0475
_refine_ls_restrained_S_all 1.019
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+7.5545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0993
_refine_ls_wR_factor_ref 0.1073
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups, All O(H,H) groups
2.a Riding coordinates:
N16(H16A,H16B)
2.b Rotating group:
N4(H4A,H4B), N8(H8A,H8B), N12(H12A,H12B), N20(H20A,H20B), N24(H24A,H24B),
O1(H1A,H1B)
2.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
C10(H10), C11(H11), C12(H12)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.17854(10) 0.06672(8) 0.11962(3) 0.0333(2) Uani 1 1 d . . . . .
Fe2 Fe 0.31911(11) 0.11195(9) 0.23007(3) 0.0380(3) Uani 1 1 d . . . . .
Fe3 Fe 0.05151(13) 0.04677(12) 0.00546(3) 0.0589(4) Uani 1 1 d . . . . .
N1 N 0.3176(6) 0.1923(5) 0.13528(17) 0.0415(15) Uani 1 1 d . . . . .
N2 N 0.3621(5) 0.2123(5) 0.17512(17) 0.0327(14) Uani 1 1 d . . . . .
N3 N 0.4242(6) 0.3495(5) 0.13403(17) 0.0365(14) Uani 1 1 d . . . . .
N4 N 0.4795(6) 0.4554(5) 0.1225(2) 0.0514(17) Uani 1 1 d . . . . .
H4A H 0.5484 0.4409 0.1110 0.062 Uiso 1 1 d GR . . . .
H4B H 0.4347 0.4918 0.1047 0.062 Uiso 1 1 d GR . . . .
N5 N 0.0788(6) 0.1091(5) 0.17602(17) 0.0367(14) Uani 1 1 d . . . . .
N6 N 0.1310(6) 0.1292(5) 0.21492(17) 0.0385(15) Uani 1 1 d . . . . .
N7 N -0.0606(6) 0.1582(5) 0.21973(19) 0.0423(15) Uani 1 1 d . . . . .
N8 N -0.1738(7) 0.1850(7) 0.2367(2) 0.066(2) Uani 1 1 d . . . . .
H8A H -0.2077 0.1221 0.2456 0.079 Uiso 1 1 d GR . . . .
H8B H -0.1650 0.2325 0.2574 0.079 Uiso 1 1 d GR . . . .
N9 N 0.2665(5) -0.0723(5) 0.15472(16) 0.0363(14) Uani 1 1 d . . . . .
N10 N 0.3222(6) -0.0511(5) 0.19249(17) 0.0383(13) Uani 1 1 d . . . . .
N11 N 0.3424(5) -0.2339(5) 0.17717(17) 0.0334(14) Uani 1 1 d . . . . .
N12 N 0.3797(7) -0.3515(5) 0.1812(2) 0.0502(18) Uani 1 1 d . . . . .
H12A H 0.3184 -0.3992 0.1811 0.060 Uiso 1 1 d GR . . . .
H12B H 0.4263 -0.3703 0.1603 0.060 Uiso 1 1 d GR . . . .
N13 N 0.0815(6) 0.2032(5) 0.08800(18) 0.0422(16) Uani 1 1 d . . . . .
N14 N 0.0271(6) 0.1879(6) 0.04939(18) 0.0480(18) Uani 1 1 d . . . . .
N15 N -0.0266(6) 0.3544(5) 0.07543(18) 0.0462(17) Uani 1 1 d . . . . .
N16 N -0.0823(8) 0.4625(6) 0.0780(2) 0.068(2) Uani 1 1 d . . . . .
H16A H -0.0247 0.5164 0.0817 0.082 Uiso 1 1 d R . . . .
H16B H -0.1308 0.4639 0.1004 0.082 Uiso 1 1 d R . . . .
N17 N 0.0378(6) -0.0548(6) 0.09917(18) 0.0431(15) Uani 1 1 d . . . . .
N18 N -0.0048(6) -0.0638(6) 0.0585(2) 0.0523(18) Uani 1 1 d . . . . .
N19 N -0.0931(6) -0.1934(6) 0.0965(3) 0.058(2) Uani 1 1 d . . . . .
N20 N -0.1628(8) -0.2917(7) 0.1075(3) 0.092(3) Uani 1 1 d . . . . .
H20A H -0.1335 -0.3215 0.1300 0.110 Uiso 1 1 d GR . . . .
H20B H -0.2361 -0.2710 0.1119 0.110 Uiso 1 1 d GR . . . .
N21 N 0.2829(6) 0.0277(5) 0.0644(2) 0.0461(17) Uani 1 1 d . . . . .
N22 N 0.2298(7) 0.0023(6) 0.02716(19) 0.0539(19) Uani 1 1 d . . . . .
N23 N 0.4154(8) -0.0491(8) 0.0240(2) 0.075(3) Uani 1 1 d . . . . .
N24 N 0.5258(10) -0.0898(14) 0.0093(3) 0.158(6) Uani 1 1 d . . . . .
H24A H 0.5563 -0.1402 0.0271 0.189 Uiso 1 1 d GR . . . .
H24B H 0.5179 -0.1260 -0.0148 0.189 Uiso 1 1 d GR . . . .
N25 N 0.2820(8) 0.0106(7) 0.2827(2) 0.067(2) Uani 1 1 d . . . . .
N26 N 0.3245(7) 0.2663(6) 0.2667(2) 0.0549(17) Uani 1 1 d . . . . .
N27 N 0.0668(9) -0.0973(7) -0.0362(2) 0.078(3) Uani 1 1 d . . . . .
N28 N 0.1160(9) 0.1710(8) -0.0379(2) 0.078(3) Uani 1 1 d . . . . .
N29 N -0.1337(9) 0.0599(10) -0.0156(2) 0.092(3) Uani 1 1 d . . . . .
N30 N 0.0331(9) 0.6208(8) 0.1576(3) 0.082(3) Uani 1 1 d . . . . .
C1 C 0.3585(7) 0.2768(7) 0.1120(2) 0.044(2) Uani 1 1 d . . . . .
H1 H 0.3432 0.2846 0.0836 0.053 Uiso 1 1 calc R . . . .
C2 C 0.4247(7) 0.3088(6) 0.1730(2) 0.0411(18) Uani 1 1 d . . . . .
H2 H 0.4637 0.3437 0.1954 0.049 Uiso 1 1 calc R . . . .
C3 C -0.0354(7) 0.1263(6) 0.1803(2) 0.0406(18) Uani 1 1 d . . . . .
H3 H -0.0920 0.1178 0.1592 0.049 Uiso 1 1 calc R . . . .
C4 C 0.0437(8) 0.1589(7) 0.2397(2) 0.048(2) Uani 1 1 d . . . . .
H4 H 0.0532 0.1780 0.2677 0.058 Uiso 1 1 calc R . . . .
C5 C 0.2809(6) -0.1825(6) 0.1465(2) 0.0356(17) Uani 1 1 d . . . . .
H5 H 0.2525 -0.2199 0.1227 0.043 Uiso 1 1 calc R . . . .
C6 C 0.3672(7) -0.1498(7) 0.2041(2) 0.0426(19) Uani 1 1 d . . . . .
H6 H 0.4114 -0.1603 0.2284 0.051 Uiso 1 1 calc R . . . .
C7 C -0.0183(7) -0.1316(7) 0.1214(3) 0.049(2) Uani 1 1 d . . . . .
H7 H -0.0087 -0.1426 0.1499 0.059 Uiso 1 1 calc R . . . .
C8 C -0.0800(9) -0.1476(9) 0.0582(3) 0.066(3) Uani 1 1 d . . . . .
H8 H -0.1204 -0.1735 0.0346 0.080 Uiso 1 1 calc R . . . .
C9 C 0.3944(9) -0.0033(8) 0.0621(3) 0.058(2) Uani 1 1 d . . . . .
H9 H 0.4510 0.0047 0.0832 0.069 Uiso 1 1 calc R . . . .
C10 C 0.3119(10) -0.0436(9) 0.0039(3) 0.072(3) Uani 1 1 d . . . . .
H10 H 0.2998 -0.0692 -0.0233 0.086 Uiso 1 1 calc R . . . .
C11 C 0.0456(8) 0.3033(6) 0.1022(2) 0.045(2) Uani 1 1 d . . . . .
H11 H 0.0681 0.3346 0.1278 0.054 Uiso 1 1 calc R . . . .
C12 C -0.0393(9) 0.2805(8) 0.0432(3) 0.059(3) Uani 1 1 d . . . . .
H12 H -0.0878 0.2931 0.0201 0.071 Uiso 1 1 calc R . . . .
C13 C 0.2682(8) -0.0547(8) 0.3091(2) 0.055(2) Uani 1 1 d . . . . .
C14 C 0.3180(8) 0.3416(7) 0.2892(2) 0.0418(17) Uani 1 1 d . . . . .
C15 C 0.0591(9) -0.1635(8) -0.0623(3) 0.059(2) Uani 1 1 d . . . . .
C16 C 0.1425(10) 0.2545(11) -0.0548(3) 0.068(3) Uani 1 1 d . . . . .
C17 C -0.1988(10) 0.0100(10) -0.0364(3) 0.071(3) Uani 1 1 d . . . . .
C18 C 0.0823(8) 0.5445(8) 0.1748(2) 0.053(2) Uani 1 1 d . . . . .
O1 O 0.5103(5) 0.0953(6) 0.23970(18) 0.074(2) Uani 1 1 d . . . . .
H1A H 0.5516 0.0661 0.2249 0.089 Uiso 1 1 d GR . . . .
H1B H 0.5338 0.0953 0.2675 0.089 Uiso 1 1 d GR . . . .
S1 S 0.2542(3) -0.1515(2) 0.34546(7) 0.0719(8) Uani 1 1 d . . . . .
S2 S 0.3127(3) 0.45182(19) 0.32161(6) 0.0604(6) Uani 1 1 d . . . . .
S3 S 0.1814(4) 0.3699(3) -0.08090(10) 0.0966(9) Uani 1 1 d . . . . .
S4 S 0.0499(3) -0.2586(2) -0.10001(7) 0.0674(7) Uani 1 1 d . . . . .
S5 S -0.2827(3) -0.0553(4) -0.07011(11) 0.1031(11) Uani 1 1 d . . . . .
S6 S 0.1508(3) 0.4419(2) 0.19878(7) 0.0700(7) Uani 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 0.0443(5) 0.0305(5) 0.0250(5) -0.0029(4) -0.0057(4) 0.0031(5)
Fe2 0.0525(6) 0.0350(5) 0.0263(5) -0.0013(4) -0.0069(5) -0.0011(5)
Fe3 0.0903(10) 0.0584(8) 0.0281(6) -0.0132(6) -0.0136(6) 0.0242(7)
N1 0.058(4) 0.041(4) 0.026(3) -0.003(3) -0.003(3) -0.007(4)
N2 0.039(3) 0.031(3) 0.029(3) 0.000(3) -0.004(3) -0.001(3)
N3 0.052(4) 0.028(3) 0.030(3) 0.001(3) 0.002(3) -0.005(3)
N4 0.071(5) 0.032(4) 0.051(4) 0.007(3) -0.002(4) -0.010(3)
N5 0.046(4) 0.034(3) 0.030(3) -0.001(3) -0.003(3) 0.003(3)
N6 0.051(4) 0.039(4) 0.026(3) -0.005(3) 0.001(3) -0.002(3)
N7 0.044(4) 0.042(4) 0.041(4) 0.001(3) 0.008(3) 0.005(3)
N8 0.069(5) 0.068(5) 0.060(5) -0.003(4) 0.034(4) 0.013(4)
N9 0.051(3) 0.032(3) 0.026(3) -0.003(3) -0.009(3) 0.002(3)
N10 0.045(3) 0.035(3) 0.035(3) -0.003(3) -0.012(3) 0.004(3)
N11 0.038(4) 0.029(3) 0.033(3) -0.006(3) -0.007(3) 0.007(3)
N12 0.071(5) 0.033(4) 0.046(4) -0.007(3) -0.016(3) 0.013(3)
N13 0.055(4) 0.041(4) 0.030(3) -0.005(3) -0.007(3) 0.008(3)
N14 0.073(5) 0.044(4) 0.027(3) -0.006(3) -0.008(3) 0.019(4)
N15 0.078(5) 0.034(4) 0.026(3) -0.002(3) -0.006(3) 0.017(3)
N16 0.098(6) 0.044(4) 0.062(5) -0.002(4) -0.007(4) 0.032(4)
N17 0.053(4) 0.037(4) 0.040(3) -0.004(3) -0.009(3) 0.000(3)
N18 0.065(5) 0.045(4) 0.047(4) -0.017(4) -0.021(3) 0.004(4)
N19 0.043(4) 0.034(4) 0.096(6) -0.020(4) -0.008(4) -0.002(3)
N20 0.068(6) 0.051(5) 0.156(9) -0.022(5) 0.010(6) -0.020(5)
N21 0.050(4) 0.042(4) 0.047(4) -0.009(3) 0.003(3) 0.005(3)
N22 0.078(5) 0.055(4) 0.029(4) 0.001(3) 0.007(4) 0.020(4)
N23 0.076(6) 0.097(6) 0.052(5) 0.028(5) 0.033(4) 0.031(5)
N24 0.131(10) 0.254(16) 0.088(7) 0.050(10) 0.066(7) 0.103(11)
N25 0.105(7) 0.059(5) 0.037(4) 0.003(4) -0.010(4) -0.019(5)
N26 0.080(5) 0.046(4) 0.039(4) -0.006(3) -0.006(4) -0.003(4)
N27 0.115(7) 0.070(6) 0.050(4) -0.024(4) -0.016(5) 0.025(5)
N28 0.128(8) 0.076(6) 0.029(4) 0.001(4) -0.002(4) 0.020(6)
N29 0.103(7) 0.124(8) 0.048(5) -0.014(6) -0.029(5) 0.026(7)
N30 0.116(7) 0.064(6) 0.065(5) 0.002(5) 0.001(5) 0.015(6)
C1 0.059(5) 0.045(5) 0.030(4) -0.005(4) -0.005(4) -0.004(4)
C2 0.050(5) 0.039(4) 0.033(4) -0.001(3) -0.007(4) 0.000(4)
C3 0.051(5) 0.036(4) 0.034(4) -0.004(3) -0.001(4) -0.002(4)
C4 0.069(6) 0.053(5) 0.023(4) -0.003(3) 0.008(4) -0.001(4)
C5 0.045(4) 0.033(4) 0.029(4) -0.005(3) -0.011(3) 0.000(3)
C6 0.047(5) 0.041(5) 0.039(4) -0.002(4) -0.014(4) 0.002(4)
C7 0.056(5) 0.041(5) 0.050(5) -0.007(4) -0.007(4) 0.002(4)
C8 0.068(6) 0.061(6) 0.070(7) -0.016(5) -0.024(5) 0.005(5)
C9 0.068(7) 0.053(5) 0.052(5) 0.007(4) 0.013(5) 0.006(5)
C10 0.096(8) 0.082(7) 0.039(5) 0.007(5) 0.016(6) 0.029(7)
C11 0.071(6) 0.036(4) 0.027(4) -0.006(3) -0.009(4) 0.006(4)
C12 0.080(7) 0.055(6) 0.043(5) -0.005(4) -0.031(5) 0.018(5)
C13 0.074(6) 0.057(5) 0.034(4) 0.000(4) -0.009(4) -0.001(5)
C14 0.057(5) 0.042(4) 0.026(4) 0.003(3) -0.001(4) -0.002(4)
C15 0.081(7) 0.056(5) 0.041(5) -0.004(4) -0.011(5) 0.004(5)
C16 0.085(8) 0.086(8) 0.033(5) -0.014(5) -0.011(5) 0.027(6)
C17 0.080(8) 0.097(8) 0.037(5) 0.003(5) 0.007(5) 0.027(6)
C18 0.075(6) 0.044(5) 0.041(5) -0.004(4) 0.008(4) 0.006(5)
O1 0.064(4) 0.109(6) 0.049(4) -0.031(4) -0.019(3) 0.027(4)
S1 0.0937(19) 0.0767(18) 0.0452(13) 0.0203(12) -0.0099(13) -0.0251(15)
S2 0.0948(17) 0.0451(12) 0.0412(11) -0.0121(10) 0.0040(12) 0.0072(14)
S3 0.128(3) 0.0688(18) 0.092(2) 0.0074(16) -0.009(2) 0.015(2)
S4 0.0877(18) 0.0619(15) 0.0527(13) -0.0236(12) 0.0018(13) -0.0089(14)
S5 0.079(2) 0.127(3) 0.103(2) -0.015(2) 0.0060(17) -0.011(2)
S6 0.100(2) 0.0508(13) 0.0593(14) -0.0065(12) -0.0159(13) 0.0106(14)
_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 N1 2.177(6) . ?
Fe1 N5 2.179(6) . ?
Fe1 N9 2.188(6) . ?
Fe1 N13 2.159(6) . ?
Fe1 N17 2.200(6) . ?
Fe1 N21 2.166(6) . ?
Fe2 N2 2.161(6) . ?
Fe2 N6 2.158(6) . ?
Fe2 N10 2.231(6) . ?
Fe2 N25 2.093(7) . ?
Fe2 N26 2.131(7) . ?
Fe2 O1 2.159(6) . ?
Fe3 N14 2.168(6) . ?
Fe3 N18 2.217(8) . ?
Fe3 N22 2.165(8) . ?
Fe3 N27 2.138(8) . ?
Fe3 N28 2.119(10) . ?
Fe3 N29 2.175(9) . ?
N1 N2 1.390(8) . ?
N1 C1 1.308(9) . ?
N2 C2 1.313(9) . ?
N3 N4 1.415(8) . ?
N3 C1 1.317(9) . ?
N3 C2 1.335(9) . ?
N4 H4A 0.8662 . ?
N4 H4B 0.8658 . ?
N5 N6 1.396(8) . ?
N5 C3 1.294(10) . ?
N6 C4 1.301(10) . ?
N7 N8 1.407(9) . ?
N7 C3 1.347(9) . ?
N7 C4 1.325(10) . ?
N8 H8A 0.8651 . ?
N8 H8B 0.8658 . ?
N9 N10 1.383(7) . ?
N9 C5 1.306(9) . ?
N10 C6 1.296(9) . ?
N11 N12 1.420(8) . ?
N11 C5 1.338(8) . ?
N11 C6 1.327(9) . ?
N12 H12A 0.8761 . ?
N12 H12B 0.8739 . ?
N13 N14 1.390(8) . ?
N13 C11 1.302(9) . ?
N14 C12 1.311(10) . ?
N15 N16 1.392(9) . ?
N15 C11 1.315(10) . ?
N15 C12 1.346(10) . ?
N16 H16A 0.9000 . ?
N16 H16B 0.8999 . ?
N17 N18 1.391(8) . ?
N17 C7 1.296(10) . ?
N18 C8 1.277(12) . ?
N19 N20 1.416(10) . ?
N19 C7 1.356(10) . ?
N19 C8 1.344(12) . ?
N20 H20A 0.8611 . ?
N20 H20B 0.8611 . ?
N21 N22 1.364(9) . ?
N21 C9 1.294(11) . ?
N22 C10 1.293(11) . ?
N23 N24 1.398(11) . ?
N23 C9 1.351(11) . ?
N23 C10 1.322(12) . ?
N24 H24A 0.8815 . ?
N24 H24B 0.8826 . ?
N25 C13 1.143(10) . ?
N26 C14 1.130(9) . ?
N27 C15 1.133(11) . ?
N28 C16 1.142(13) . ?
N29 C17 1.140(13) . ?
N30 C18 1.174(11) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 S1 1.622(9) . ?
C14 S2 1.641(8) . ?
C15 S4 1.636(9) . ?
C16 S3 1.629(13) . ?
C17 S5 1.615(12) . ?
C18 S6 1.602(10) . ?
O1 H1A 0.7414 . ?
O1 H1B 0.9311 . ?
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
N1 Fe1 N5 91.3(2) . . ?
N1 Fe1 N9 92.8(2) . . ?
N1 Fe1 N17 175.8(2) . . ?
N5 Fe1 N9 87.9(2) . . ?
N5 Fe1 N17 91.5(2) . . ?
N9 Fe1 N17 90.4(2) . . ?
N13 Fe1 N1 88.9(2) . . ?
N13 Fe1 N5 88.4(2) . . ?
N13 Fe1 N9 176.0(2) . . ?
N13 Fe1 N17 88.0(2) . . ?
N13 Fe1 N21 92.0(2) . . ?
N21 Fe1 N1 86.9(2) . . ?
N21 Fe1 N5 178.1(3) . . ?
N21 Fe1 N9 91.7(2) . . ?
N21 Fe1 N17 90.3(2) . . ?
N2 Fe2 N10 90.3(2) . . ?
N6 Fe2 N2 89.0(2) . . ?
N6 Fe2 N10 88.3(2) . . ?
N25 Fe2 N2 178.0(3) . . ?
N25 Fe2 N6 92.4(3) . . ?
N25 Fe2 N10 88.3(3) . . ?
N25 Fe2 N26 91.4(3) . . ?
N25 Fe2 O1 91.7(3) . . ?
N26 Fe2 N2 89.9(2) . . ?
N26 Fe2 N6 94.3(3) . . ?
N26 Fe2 N10 177.4(3) . . ?
N26 Fe2 O1 88.1(3) . . ?
O1 Fe2 N2 86.9(2) . . ?
O1 Fe2 N6 175.2(2) . . ?
O1 Fe2 N10 89.3(2) . . ?
N14 Fe3 N18 84.0(2) . . ?
N14 Fe3 N29 91.8(3) . . ?
N22 Fe3 N14 94.7(3) . . ?
N22 Fe3 N18 82.9(3) . . ?
N22 Fe3 N29 170.3(4) . . ?
N27 Fe3 N14 176.7(3) . . ?
N27 Fe3 N18 93.3(3) . . ?
N27 Fe3 N22 86.8(3) . . ?
N27 Fe3 N29 86.3(4) . . ?
N28 Fe3 N14 87.9(3) . . ?
N28 Fe3 N18 170.8(3) . . ?
N28 Fe3 N22 93.5(3) . . ?
N28 Fe3 N27 94.9(3) . . ?
N28 Fe3 N29 94.0(4) . . ?
N29 Fe3 N18 90.6(3) . . ?
N2 N1 Fe1 125.1(4) . . ?
C1 N1 Fe1 127.5(5) . . ?
C1 N1 N2 106.2(6) . . ?
N1 N2 Fe2 125.7(4) . . ?
C2 N2 Fe2 127.7(5) . . ?
C2 N2 N1 106.3(6) . . ?
C1 N3 N4 130.4(6) . . ?
C1 N3 C2 106.4(6) . . ?
C2 N3 N4 123.1(6) . . ?
N3 N4 H4A 109.3 . . ?
N3 N4 H4B 109.9 . . ?
H4A N4 H4B 108.8 . . ?
N6 N5 Fe1 124.6(5) . . ?
C3 N5 Fe1 128.6(5) . . ?
C3 N5 N6 106.8(6) . . ?
N5 N6 Fe2 126.2(4) . . ?
C4 N6 Fe2 127.7(5) . . ?
C4 N6 N5 106.2(6) . . ?
C3 N7 N8 127.5(7) . . ?
C4 N7 N8 126.6(7) . . ?
C4 N7 C3 105.9(6) . . ?
N7 N8 H8A 109.7 . . ?
N7 N8 H8B 109.5 . . ?
H8A N8 H8B 108.8 . . ?
N10 N9 Fe1 121.5(4) . . ?
C5 N9 Fe1 131.3(5) . . ?
C5 N9 N10 107.1(6) . . ?
N9 N10 Fe2 128.0(4) . . ?
C6 N10 Fe2 126.0(5) . . ?
C6 N10 N9 105.7(6) . . ?
C5 N11 N12 129.5(6) . . ?
C6 N11 N12 125.1(6) . . ?
C6 N11 C5 105.3(6) . . ?
N11 N12 H12A 111.7 . . ?
N11 N12 H12B 109.9 . . ?
H12A N12 H12B 107.7 . . ?
N14 N13 Fe1 123.0(5) . . ?
C11 N13 Fe1 129.3(5) . . ?
C11 N13 N14 106.8(6) . . ?
N13 N14 Fe3 128.3(5) . . ?
C12 N14 Fe3 125.5(5) . . ?
C12 N14 N13 106.1(6) . . ?
C11 N15 N16 129.3(7) . . ?
C11 N15 C12 106.4(6) . . ?
C12 N15 N16 124.3(7) . . ?
N15 N16 H16A 107.8 . . ?
N15 N16 H16B 109.2 . . ?
H16A N16 H16B 108.0 . . ?
N18 N17 Fe1 124.7(5) . . ?
C7 N17 Fe1 127.8(5) . . ?
C7 N17 N18 107.5(6) . . ?
N17 N18 Fe3 125.5(5) . . ?
C8 N18 Fe3 127.8(6) . . ?
C8 N18 N17 106.7(8) . . ?
C7 N19 N20 127.4(9) . . ?
C8 N19 N20 127.0(8) . . ?
C8 N19 C7 105.4(8) . . ?
N19 N20 H20A 108.6 . . ?
N19 N20 H20B 109.8 . . ?
H20A N20 H20B 109.4 . . ?
N22 N21 Fe1 121.9(5) . . ?
C9 N21 Fe1 128.2(6) . . ?
C9 N21 N22 107.8(7) . . ?
N21 N22 Fe3 128.9(5) . . ?
C10 N22 Fe3 124.0(6) . . ?
C10 N22 N21 106.7(8) . . ?
C9 N23 N24 126.0(10) . . ?
C10 N23 N24 128.1(9) . . ?
C10 N23 C9 105.8(8) . . ?
N23 N24 H24A 109.9 . . ?
N23 N24 H24B 111.5 . . ?
H24A N24 H24B 107.3 . . ?
C13 N25 Fe2 172.3(8) . . ?
C14 N26 Fe2 171.8(7) . . ?
C15 N27 Fe3 167.5(8) . . ?
C16 N28 Fe3 165.1(8) . . ?
C17 N29 Fe3 138.6(9) . . ?
N1 C1 N3 111.0(6) . . ?
N1 C1 H1 124.5 . . ?
N3 C1 H1 124.5 . . ?
N2 C2 N3 110.1(6) . . ?
N2 C2 H2 125.0 . . ?
N3 C2 H2 125.0 . . ?
N5 C3 N7 110.2(7) . . ?
N5 C3 H3 124.9 . . ?
N7 C3 H3 124.9 . . ?
N6 C4 N7 110.9(6) . . ?
N6 C4 H4 124.5 . . ?
N7 C4 H4 124.5 . . ?
N9 C5 N11 110.0(6) . . ?
N9 C5 H5 125.0 . . ?
N11 C5 H5 125.0 . . ?
N10 C6 N11 111.8(6) . . ?
N10 C6 H6 124.1 . . ?
N11 C6 H6 124.1 . . ?
N17 C7 N19 109.2(8) . . ?
N17 C7 H7 125.4 . . ?
N19 C7 H7 125.4 . . ?
N18 C8 N19 111.1(8) . . ?
N18 C8 H8 124.4 . . ?
N19 C8 H8 124.4 . . ?
N21 C9 N23 109.0(9) . . ?
N21 C9 H9 125.5 . . ?
N23 C9 H9 125.5 . . ?
N22 C10 N23 110.7(8) . . ?
N22 C10 H10 124.7 . . ?
N23 C10 H10 124.7 . . ?
N13 C11 N15 110.8(6) . . ?
N13 C11 H11 124.6 . . ?
N15 C11 H11 124.6 . . ?
N14 C12 N15 109.8(7) . . ?
N14 C12 H12 125.1 . . ?
N15 C12 H12 125.1 . . ?
N25 C13 S1 177.0(10) . . ?
N26 C14 S2 178.3(9) . . ?
N27 C15 S4 179.2(11) . . ?
N28 C16 S3 177.2(9) . . ?
N29 C17 S5 173.6(10) . . ?
N30 C18 S6 179.0(9) . . ?
Fe2 O1 H1A 124.1 . . ?
Fe2 O1 H1B 114.5 . . ?
H1A O1 H1B 116.0 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 N2 Fe2 7.1(8) . . . . ?
Fe1 N1 N2 C2 -167.2(5) . . . . ?
Fe1 N1 C1 N3 167.3(5) . . . . ?
Fe1 N5 N6 Fe2 -4.6(8) . . . . ?
Fe1 N5 N6 C4 176.0(5) . . . . ?
Fe1 N5 C3 N7 -175.8(5) . . . . ?
Fe1 N9 N10 Fe2 8.2(8) . . . . ?
Fe1 N9 N10 C6 -178.4(5) . . . . ?
Fe1 N9 C5 N11 179.2(5) . . . . ?
Fe1 N13 N14 Fe3 -13.6(9) . . . . ?
Fe1 N13 N14 C12 169.6(6) . . . . ?
Fe1 N13 C11 N15 -170.1(5) . . . . ?
Fe1 N17 N18 Fe3 -3.1(9) . . . . ?
Fe1 N17 N18 C8 176.1(6) . . . . ?
Fe1 N17 C7 N19 -176.4(5) . . . . ?
Fe1 N21 N22 Fe3 22.7(9) . . . . ?
Fe1 N21 N22 C10 -164.8(6) . . . . ?
Fe1 N21 C9 N23 163.5(6) . . . . ?
Fe2 N2 C2 N3 -175.3(5) . . . . ?
Fe2 N6 C4 N7 -178.8(5) . . . . ?
Fe2 N10 C6 N11 172.2(5) . . . . ?
Fe3 N14 C12 N15 -175.2(6) . . . . ?
Fe3 N18 C8 N19 -179.0(6) . . . . ?
Fe3 N22 C10 N23 172.9(6) . . . . ?
N1 N2 C2 N3 -1.2(8) . . . . ?
N2 N1 C1 N3 -0.7(9) . . . . ?
N4 N3 C1 N1 -175.8(7) . . . . ?
N4 N3 C2 N2 176.9(6) . . . . ?
N5 N6 C4 N7 0.6(9) . . . . ?
N6 N5 C3 N7 0.9(8) . . . . ?
N8 N7 C3 N5 179.8(7) . . . . ?
N8 N7 C4 N6 179.6(7) . . . . ?
N9 N10 C6 N11 -1.4(9) . . . . ?
N10 N9 C5 N11 0.4(8) . . . . ?
N12 N11 C5 N9 -179.2(7) . . . . ?
N12 N11 C6 N10 179.7(7) . . . . ?
N13 N14 C12 N15 1.8(10) . . . . ?
N14 N13 C11 N15 -0.7(9) . . . . ?
N16 N15 C11 N13 -178.5(8) . . . . ?
N16 N15 C12 N14 178.0(8) . . . . ?
N17 N18 C8 N19 1.8(10) . . . . ?
N18 N17 C7 N19 2.1(8) . . . . ?
N20 N19 C7 N17 174.2(7) . . . . ?
N20 N19 C8 N18 -175.8(7) . . . . ?
N21 N22 C10 N23 -0.1(11) . . . . ?
N22 N21 C9 N23 -0.3(10) . . . . ?
N24 N23 C9 N21 178.4(10) . . . . ?
N24 N23 C10 N22 -178.1(11) . . . . ?
C1 N1 N2 Fe2 175.5(5) . . . . ?
C1 N1 N2 C2 1.2(8) . . . . ?
C1 N3 C2 N2 0.8(9) . . . . ?
C2 N3 C1 N1 0.0(9) . . . . ?
C3 N5 N6 Fe2 178.5(5) . . . . ?
C3 N5 N6 C4 -0.9(8) . . . . ?
C3 N7 C4 N6 -0.1(9) . . . . ?
C4 N7 C3 N5 -0.6(8) . . . . ?
C5 N9 N10 Fe2 -172.9(5) . . . . ?
C5 N9 N10 C6 0.6(8) . . . . ?
C5 N11 C6 N10 1.7(9) . . . . ?
C6 N11 C5 N9 -1.2(8) . . . . ?
C7 N17 N18 Fe3 178.3(5) . . . . ?
C7 N17 N18 C8 -2.4(9) . . . . ?
C7 N19 C8 N18 -0.5(10) . . . . ?
C8 N19 C7 N17 -1.1(9) . . . . ?
C9 N21 N22 Fe3 -172.3(6) . . . . ?
C9 N21 N22 C10 0.3(10) . . . . ?
C9 N23 C10 N22 0.0(12) . . . . ?
C10 N23 C9 N21 0.2(11) . . . . ?
C11 N13 N14 Fe3 176.2(6) . . . . ?
C11 N13 N14 C12 -0.7(9) . . . . ?
C11 N15 C12 N14 -2.2(11) . . . . ?
C12 N15 C11 N13 1.8(10) . . . . ?
_iucr_refine_instructions_details
;
c.res created by SHELXL-2014/7
TITL C_a.res in P2(1)2(1)2(1)
REM Old TITL C in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.163, Rweak 0.044, Alpha 0.006, Orientation as input
REM Flack x = 0.067 ( 0.008 ) from Parsons' quotients
REM Formula found by SHELXT: C8CA N14 O S6 Fe3
REM C_a.res in P2(1)2(1)2(1)
REM 514 parameters refined using 0 restraints
CELL 0.71073 11.1307 11.5076 32.0901 90 90 90
ZERR 4 0.0033 0.0047 0.0087 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Fe N O S
UNIT 72 104 12 120 4 24
L.S. 100
PLAN 2
SIZE 0.102 0.186 0.227
TEMP 20
BOND $H
htab
LIST 6
MORE -1
CONF
fmap 2
acta 52
REM
REM
REM
WGHT 0.035600 7.554501
FVAR 0.10110
FE1 3 0.178540 0.066722 0.119623 11.00000 0.04425 0.03047 =
0.02505 -0.00287 -0.00573 0.00306
FE2 3 0.319106 0.111955 0.230068 11.00000 0.05255 0.03500 =
0.02633 -0.00130 -0.00695 -0.00109
FE3 3 0.051513 0.046769 0.005456 11.00000 0.09025 0.05844 =
0.02813 -0.01320 -0.01361 0.02419
N1 4 0.317647 0.192326 0.135277 11.00000 0.05775 0.04121 =
0.02568 -0.00287 -0.00278 -0.00682
N2 4 0.362063 0.212264 0.175117 11.00000 0.03861 0.03056 =
0.02899 -0.00049 -0.00356 -0.00142
N3 4 0.424185 0.349476 0.134029 11.00000 0.05171 0.02764 =
0.03026 0.00140 0.00150 -0.00457
N4 4 0.479480 0.455375 0.122466 11.00000 0.07098 0.03195 =
0.05127 0.00658 -0.00235 -0.01014
AFIX 7
H4A 2 0.548358 0.440914 0.111025 11.00000 -1.20000
H4B 2 0.434748 0.491846 0.104687 11.00000 -1.20000
AFIX 0
N5 4 0.078771 0.109077 0.176023 11.00000 0.04579 0.03422 =
0.03009 -0.00109 -0.00277 0.00338
N6 4 0.131014 0.129164 0.214919 11.00000 0.05063 0.03922 =
0.02569 -0.00464 0.00079 -0.00159
N7 4 -0.060560 0.158227 0.219728 11.00000 0.04387 0.04185 =
0.04129 0.00120 0.00800 0.00450
N8 4 -0.173789 0.184965 0.236699 11.00000 0.06879 0.06754 =
0.06036 -0.00265 0.03407 0.01338
AFIX 7
H8A 2 -0.207744 0.122113 0.245645 11.00000 -1.20000
H8B 2 -0.164987 0.232455 0.257402 11.00000 -1.20000
AFIX 0
N9 4 0.266521 -0.072297 0.154718 11.00000 0.05104 0.03233 =
0.02559 -0.00282 -0.00942 0.00236
N10 4 0.322235 -0.051094 0.192493 11.00000 0.04516 0.03461 =
0.03523 -0.00295 -0.01245 0.00402
N11 4 0.342420 -0.233934 0.177172 11.00000 0.03761 0.02948 =
0.03323 -0.00566 -0.00695 0.00664
N12 4 0.379666 -0.351455 0.181163 11.00000 0.07116 0.03325 =
0.04615 -0.00705 -0.01558 0.01278
AFIX 7
H12A 2 0.318385 -0.399234 0.181050 11.00000 -1.20000
H12B 2 0.426319 -0.370302 0.160329 11.00000 -1.20000
AFIX 0
N13 4 0.081509 0.203158 0.087999 11.00000 0.05509 0.04126 =
0.03014 -0.00489 -0.00744 0.00792
N14 4 0.027134 0.187946 0.049390 11.00000 0.07319 0.04383 =
0.02686 -0.00589 -0.00805 0.01871
N15 4 -0.026631 0.354379 0.075434 11.00000 0.07789 0.03417 =
0.02646 -0.00199 -0.00647 0.01663
N16 4 -0.082306 0.462500 0.077983 11.00000 0.09836 0.04366 =
0.06176 -0.00206 -0.00680 0.03211
AFIX 3
H16A 2 -0.024676 0.516350 0.081733 11.00000 -1.20000
H16B 2 -0.130776 0.463870 0.100423 11.00000 -1.20000
AFIX 0
N17 4 0.037759 -0.054814 0.099175 11.00000 0.05267 0.03683 =
0.03976 -0.00388 -0.00869 0.00013
N18 4 -0.004848 -0.063785 0.058548 11.00000 0.06512 0.04479 =
0.04713 -0.01665 -0.02099 0.00382
N19 4 -0.093065 -0.193448 0.096483 11.00000 0.04267 0.03435 =
0.09559 -0.01955 -0.00775 -0.00231
N20 4 -0.162794 -0.291651 0.107532 11.00000 0.06795 0.05127 =
0.15643 -0.02237 0.00994 -0.02003
AFIX 7
H20A 2 -0.133512 -0.321452 0.129952 11.00000 -1.20000
H20B 2 -0.236063 -0.270960 0.111903 11.00000 -1.20000
AFIX 0
N21 4 0.282851 0.027666 0.064386 11.00000 0.04966 0.04206 =
0.04672 -0.00906 0.00335 0.00529
N22 4 0.229821 0.002308 0.027162 11.00000 0.07782 0.05464 =
0.02932 0.00121 0.00653 0.02003
N23 4 0.415365 -0.049078 0.024012 11.00000 0.07595 0.09667 =
0.05210 0.02849 0.03295 0.03141
N24 4 0.525838 -0.089842 0.009318 11.00000 0.13105 0.25361 =
0.08817 0.04995 0.06627 0.10291
AFIX 7
H24A 2 0.556300 -0.140158 0.027133 11.00000 -1.20000
H24B 2 0.517905 -0.126026 -0.014777 11.00000 -1.20000
AFIX 0
N25 4 0.282019 0.010581 0.282656 11.00000 0.10456 0.05898 =
0.03656 0.00256 -0.00983 -0.01875
N26 4 0.324509 0.266310 0.266717 11.00000 0.07969 0.04608 =
0.03895 -0.00569 -0.00557 -0.00305
N27 4 0.066842 -0.097340 -0.036233 11.00000 0.11529 0.06990 =
0.04988 -0.02364 -0.01625 0.02492
N28 4 0.115955 0.171016 -0.037873 11.00000 0.12819 0.07599 =
0.02868 0.00101 -0.00206 0.02041
N29 4 -0.133678 0.059931 -0.015628 11.00000 0.10345 0.12361 =
0.04773 -0.01412 -0.02874 0.02642
N30 4 0.033139 0.620848 0.157553 11.00000 0.11616 0.06428 =
0.06550 0.00239 0.00062 0.01464
C1 1 0.358520 0.276833 0.111986 11.00000 0.05865 0.04529 =
0.02954 -0.00548 -0.00482 -0.00449
AFIX 43
H1 2 0.343227 0.284568 0.083630 11.00000 -1.20000
AFIX 0
C2 1 0.424686 0.308765 0.172990 11.00000 0.05038 0.03944 =
0.03337 -0.00100 -0.00717 -0.00001
AFIX 43
H2 2 0.463695 0.343667 0.195355 11.00000 -1.20000
AFIX 0
C3 1 -0.035450 0.126263 0.180308 11.00000 0.05117 0.03640 =
0.03426 -0.00355 -0.00081 -0.00224
AFIX 43
H3 2 -0.092044 0.117766 0.159206 11.00000 -1.20000
AFIX 0
C4 1 0.043683 0.158867 0.239693 11.00000 0.06911 0.05277 =
0.02291 -0.00269 0.00794 -0.00128
AFIX 43
H4 2 0.053152 0.177981 0.267659 11.00000 -1.20000
AFIX 0
C5 1 0.280859 -0.182548 0.146451 11.00000 0.04512 0.03296 =
0.02873 -0.00529 -0.01072 -0.00008
AFIX 43
H5 2 0.252465 -0.219866 0.122706 11.00000 -1.20000
AFIX 0
C6 1 0.367152 -0.149769 0.204127 11.00000 0.04749 0.04079 =
0.03938 -0.00166 -0.01401 0.00236
AFIX 43
H6 2 0.411368 -0.160349 0.228423 11.00000 -1.20000
AFIX 0
C7 1 -0.018287 -0.131624 0.121395 11.00000 0.05596 0.04059 =
0.04989 -0.00669 -0.00679 0.00221
AFIX 43
H7 2 -0.008732 -0.142605 0.149915 11.00000 -1.20000
AFIX 0
C8 1 -0.080004 -0.147603 0.058234 11.00000 0.06807 0.06112 =
0.07015 -0.01551 -0.02381 0.00547
AFIX 43
H8 2 -0.120408 -0.173527 0.034632 11.00000 -1.20000
AFIX 0
C9 1 0.394406 -0.003310 0.062079 11.00000 0.06844 0.05264 =
0.05223 0.00702 0.01313 0.00573
AFIX 43
H9 2 0.450987 0.004653 0.083211 11.00000 -1.20000
AFIX 0
C10 1 0.311901 -0.043593 0.003887 11.00000 0.09550 0.08165 =
0.03893 0.00707 0.01583 0.02936
AFIX 43
H10 2 0.299814 -0.069225 -0.023276 11.00000 -1.20000
AFIX 0
C11 1 0.045645 0.303340 0.102181 11.00000 0.07064 0.03624 =
0.02701 -0.00622 -0.00936 0.00622
AFIX 43
H11 2 0.068100 0.334550 0.127754 11.00000 -1.20000
AFIX 0
C12 1 -0.039287 0.280463 0.043229 11.00000 0.07978 0.05513 =
0.04348 -0.00520 -0.03070 0.01781
AFIX 43
H12 2 -0.087846 0.293108 0.020086 11.00000 -1.20000
AFIX 0
C13 1 0.268183 -0.054686 0.309057 11.00000 0.07403 0.05652 =
0.03385 -0.00038 -0.00906 -0.00095
C14 1 0.317996 0.341649 0.289200 11.00000 0.05700 0.04191 =
0.02644 0.00330 -0.00070 -0.00246
C15 1 0.059138 -0.163515 -0.062251 11.00000 0.08087 0.05630 =
0.04088 -0.00436 -0.01084 0.00433
C16 1 0.142468 0.254536 -0.054773 11.00000 0.08486 0.08559 =
0.03254 -0.01369 -0.01142 0.02714
C17 1 -0.198825 0.009987 -0.036365 11.00000 0.08001 0.09687 =
0.03692 0.00328 0.00722 0.02712
C18 1 0.082262 0.544461 0.174797 11.00000 0.07485 0.04362 =
0.04106 -0.00448 0.00774 0.00571
O1 5 0.510265 0.095323 0.239695 11.00000 0.06375 0.10883 =
0.04941 -0.03053 -0.01944 0.02732
AFIX 7
H1A 2 0.551610 0.066106 0.224919 11.00000 -1.20000
H1B 2 0.533811 0.095265 0.267536 11.00000 -1.20000
AFIX 0
S1 6 0.254154 -0.151538 0.345464 11.00000 0.09369 0.07667 =
0.04522 0.02028 -0.00986 -0.02507
S2 6 0.312747 0.451822 0.321607 11.00000 0.09483 0.04514 =
0.04119 -0.01213 0.00401 0.00721
S3 6 0.181378 0.369882 -0.080902 11.00000 0.12840 0.06884 =
0.09243 0.00735 -0.00876 0.01469
S4 6 0.049934 -0.258614 -0.100014 11.00000 0.08774 0.06189 =
0.05271 -0.02363 0.00181 -0.00889
S5 6 -0.282721 -0.055305 -0.070108 11.00000 0.07877 0.12722 =
0.10325 -0.01503 0.00596 -0.01102
S6 6 0.150757 0.441873 0.198775 11.00000 0.09984 0.05078 =
0.05933 -0.00653 -0.01588 0.01057
HKLF 4
REM C_a.res in P2(1)2(1)2(1)
REM R1 = 0.0475 for 5852 Fo > 4sig(Fo) and 0.0718 for all 7567 data
REM 529 parameters refined using 0 restraints
END
WGHT 0.0357 7.5435
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, y+1/2, -z+1/2
HTAB N4 S1_$1
EQIV $2 x+1/2, -y+1/2, -z
HTAB N4 S5_$2
EQIV $3 -x, y-1/2, -z+1/2
HTAB N8 S6_$3
EQIV $4 x, y-1, z
HTAB N12 S6_$4
HTAB N12 N4_$4
EQIV $5 x+1/2, -y-1/2, -z
HTAB N12 S4_$5
HTAB N16 S5_$2
EQIV $6 -x, y+1/2, -z+1/2
HTAB N16 S1_$6
HTAB N20 N30_$4
EQIV $7 x-1/2, -y-1/2, -z
HTAB N20 S4_$7
HTAB N24 S4_$5
HTAB C4 N30_$3
HTAB C9 S3_$2
HTAB C10 N16_$2
HTAB C11 S6
EQIV $8 -x+1, y-1/2, -z+1/2
HTAB O1 S2_$8
HTAB O1 N12_$1
REM Highest difference peak 0.608, deepest hole -0.540, 1-sigma level 0.070
Q1 1 0.0083 -0.0174 0.0171 11.00000 0.05 0.61
Q2 1 -0.3166 -0.0987 -0.0379 11.00000 0.05 0.49
REM The information below was added by Olex2.
REM
REM R1 = 0.0475 for 5852 Fo > 4sig(Fo) and 0.0718 for all 42943 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.61, deepest hole -0.54
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0718
REM R1_gt = 0.0475
REM wR_ref = 0.1073
REM GOOF = 1.019
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 42943
REM Reflections_gt = 5852
REM Parameters = n/a
REM Hole = -0.54
REM Peak = 0.61
REM Flack = 0.023(8)
;
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_e
_database_code_depnum_ccdc_archive 'CCDC 1578878'
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-02-09 downloaded from the CCDC.
;
_audit_creation_date 2018-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C17 H26 Fe3 N29 O S5, C N S'
_chemical_formula_sum 'C18 H26 Fe3 N30 O S6'
_chemical_formula_weight 1038.60
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
Fe Fe 0.3463 0.8444 '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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_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'
_cell_length_a 10.799(3)
_cell_length_b 11.407(5)
_cell_length_c 31.847(9)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 3923(2)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 9921
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 25.191
_cell_measurement_theta_min 2.584
_shelx_estimated_absorpt_T_max 0.864
_shelx_estimated_absorpt_T_min 0.730
_exptl_absorpt_coefficient_mu 1.479
_exptl_absorpt_correction_T_max 0.7452
_exptl_absorpt_correction_T_min 0.6643
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1091 before and 0.0653 after correction. The Ratio of minimum to maximum transmission is 0.8914. The \l/2 correction factor is Not present.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.758
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2104
_exptl_crystal_size_max 0.227
_exptl_crystal_size_mid 0.186
_exptl_crystal_size_min 0.102
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0519
_diffrn_reflns_av_unetI/netI 0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 38
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_number 40886
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 25.495
_diffrn_reflns_theta_max 25.495
_diffrn_reflns_theta_min 2.279
_diffrn_ambient_temperature 100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.777
_reflns_Friedel_fraction_full 0.997
_reflns_Friedel_fraction_max 0.997
_reflns_number_gt 6348
_reflns_number_total 7268
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection ?
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2008)'
_computing_structure_solution 'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max 0.837
_refine_diff_density_min -0.522
_refine_diff_density_rms 0.083
_refine_ls_abs_structure_details
;
Flack x determined using 2454 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.004(7)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.037
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 528
_refine_ls_number_reflns 7268
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0524
_refine_ls_R_factor_gt 0.0416
_refine_ls_restrained_S_all 1.037
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^+6.8838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0925
_refine_ls_wR_factor_ref 0.0968
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H,H) groups
At 1.5 times of:
All O(H,H) groups
2.a Riding coordinates:
N16(H16A,H16B), O1(H1A,H1B)
2.b Rotating group:
N4(H4A,H4B), N8(H8A,H8B), N12(H12A,H12B), N20(H20A,H20B), N24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
C10(H10), C11(H11), C12(H12)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.17919(9) 0.07783(7) 0.12189(3) 0.01751(19) Uani 1 1 d . . . . .
Fe2 Fe 0.31974(9) 0.12358(8) 0.23117(3) 0.0211(2) Uani 1 1 d . . . . .
Fe3 Fe 0.05078(11) 0.04727(9) 0.00878(3) 0.0340(3) Uani 1 1 d . . . . .
N1 N 0.3090(5) 0.2004(4) 0.13590(15) 0.0218(12) Uani 1 1 d . . . . .
N2 N 0.3622(5) 0.2179(5) 0.17515(15) 0.0201(12) Uani 1 1 d . . . . .
N3 N 0.4237(5) 0.3564(5) 0.13275(15) 0.0202(12) Uani 1 1 d . . . . .
N4 N 0.4800(5) 0.4616(5) 0.12022(17) 0.0280(13) Uani 1 1 d . . . . .
H4A H 0.5512 0.4479 0.1102 0.034 Uiso 1 1 d GR . . . .
H4B H 0.4377 0.4962 0.1012 0.034 Uiso 1 1 d GR . . . .
N5 N 0.0800(5) 0.1183(4) 0.17411(15) 0.0182(11) Uani 1 1 d . . . . .
N6 N 0.1296(5) 0.1400(5) 0.21362(15) 0.0185(11) Uani 1 1 d . . . . .
N7 N -0.0676(5) 0.1645(5) 0.21665(16) 0.0212(12) Uani 1 1 d . . . . .
N8 N -0.1856(5) 0.1891(5) 0.23344(18) 0.0299(13) Uani 1 1 d . . . . .
H8A H -0.2296 0.1266 0.2353 0.036 Uiso 1 1 d GR . . . .
H8B H -0.1771 0.2180 0.2583 0.036 Uiso 1 1 d GR . . . .
N9 N 0.2683(5) -0.0523(5) 0.15400(15) 0.0191(11) Uani 1 1 d . . . . .
N10 N 0.3203(5) -0.0362(4) 0.19343(15) 0.0194(11) Uani 1 1 d . . . . .
N11 N 0.3451(5) -0.2170(4) 0.17463(15) 0.0186(12) Uani 1 1 d . . . . .
N12 N 0.3840(5) -0.3348(5) 0.17709(17) 0.0253(13) Uani 1 1 d . . . . .
H12A H 0.3229 -0.3831 0.1773 0.030 Uiso 1 1 d GR . . . .
H12B H 0.4300 -0.3540 0.1561 0.030 Uiso 1 1 d GR . . . .
N13 N 0.0854(5) 0.2040(5) 0.09161(16) 0.0217(12) Uani 1 1 d . . . . .
N14 N 0.0310(6) 0.1916(5) 0.05229(17) 0.0282(14) Uani 1 1 d . . . . .
N15 N -0.0162(5) 0.3616(5) 0.07748(16) 0.0244(12) Uani 1 1 d . . . . .
N16 N -0.0695(6) 0.4749(5) 0.07913(17) 0.0289(13) Uani 1 1 d . . . . .
H16A H -0.0119 0.5288 0.0829 0.035 Uiso 1 1 d R . . . .
H16B H -0.1180 0.4763 0.1016 0.035 Uiso 1 1 d R . . . .
N17 N 0.0471(5) -0.0415(5) 0.10464(17) 0.0246(12) Uani 1 1 d . . . . .
N18 N 0.0034(5) -0.0578(5) 0.06424(18) 0.0306(14) Uani 1 1 d . . . . .
N19 N -0.0832(6) -0.1854(5) 0.1046(2) 0.0371(16) Uani 1 1 d . . . . .
N20 N -0.1525(6) -0.2849(6) 0.1170(3) 0.0518(19) Uani 1 1 d . . . . .
H20A H -0.1153 -0.3239 0.1361 0.062 Uiso 1 1 d GR . . . .
H20B H -0.2212 -0.2623 0.1263 0.062 Uiso 1 1 d GR . . . .
N21 N 0.2820(5) 0.0373(5) 0.07209(19) 0.0278(13) Uani 1 1 d . . . . .
N22 N 0.2367(6) 0.0193(5) 0.03285(19) 0.0382(16) Uani 1 1 d . . . . .
N23 N 0.4330(6) -0.0128(7) 0.0338(2) 0.0485(19) Uani 1 1 d . . . . .
N24 N 0.5518(7) -0.0368(8) 0.0182(3) 0.071(3) Uani 1 1 d . . . . .
H24A H 0.5937 -0.0308 0.0420 0.085 Uiso 1 1 d GR . . . .
H24B H 0.5608 -0.1110 0.0097 0.085 Uiso 1 1 d GR . . . .
N25 N 0.2809(6) 0.0219(5) 0.28349(18) 0.0351(16) Uani 1 1 d . . . . .
N26 N 0.3267(6) 0.2772(5) 0.26776(17) 0.0290(13) Uani 1 1 d . . . . .
N27 N 0.0749(7) -0.0992(6) -0.0315(2) 0.0457(18) Uani 1 1 d . . . . .
N28 N 0.1133(7) 0.1688(6) -0.03664(19) 0.0402(17) Uani 1 1 d . . . . .
N29 N -0.1382(7) 0.0490(7) -0.0123(2) 0.053(2) Uani 1 1 d . . . . .
N30 N 0.0591(6) 0.6391(6) 0.1622(2) 0.0428(16) Uani 1 1 d . . . . .
C1 C 0.3495(6) 0.2834(5) 0.11140(19) 0.0234(15) Uani 1 1 d . . . . .
H1 H 0.3293 0.2910 0.0825 0.028 Uiso 1 1 calc R . . . .
C2 C 0.4292(6) 0.3143(6) 0.1720(2) 0.0228(15) Uani 1 1 d . . . . .
H2 H 0.4747 0.3489 0.1943 0.027 Uiso 1 1 calc R . . . .
C3 C -0.0391(6) 0.1332(5) 0.17703(19) 0.0200(13) Uani 1 1 d . . . . .
H3 H -0.0967 0.1236 0.1548 0.024 Uiso 1 1 calc R . . . .
C4 C 0.0374(6) 0.1677(5) 0.23787(19) 0.0215(14) Uani 1 1 d . . . . .
H4 H 0.0445 0.1874 0.2668 0.026 Uiso 1 1 calc R . . . .
C5 C 0.2860(5) -0.1605(6) 0.14342(19) 0.0196(14) Uani 1 1 d . . . . .
H5 H 0.2610 -0.1948 0.1176 0.024 Uiso 1 1 calc R . . . .
C6 C 0.3652(6) -0.1368(6) 0.20430(19) 0.0210(14) Uani 1 1 d . . . . .
H6 H 0.4070 -0.1515 0.2300 0.025 Uiso 1 1 calc R . . . .
C7 C -0.0078(6) -0.1192(6) 0.1286(2) 0.0326(17) Uani 1 1 d . . . . .
H7 H 0.0037 -0.1275 0.1580 0.039 Uiso 1 1 calc R . . . .
C8 C -0.0741(7) -0.1452(7) 0.0650(3) 0.0398(19) Uani 1 1 d . . . . .
H8 H -0.1172 -0.1757 0.0414 0.048 Uiso 1 1 calc R . . . .
C9 C 0.4008(7) 0.0167(7) 0.0720(3) 0.0385(19) Uani 1 1 d . . . . .
H9 H 0.4546 0.0222 0.0955 0.046 Uiso 1 1 calc R . . . .
C10 C 0.3299(9) -0.0155(8) 0.0107(3) 0.050(2) Uani 1 1 d . . . . .
H10 H 0.3257 -0.0395 -0.0179 0.061 Uiso 1 1 calc R . . . .
C11 C 0.0543(6) 0.3073(6) 0.10534(19) 0.0230(15) Uani 1 1 d . . . . .
H11 H 0.0787 0.3392 0.1316 0.028 Uiso 1 1 calc R . . . .
C12 C -0.0308(7) 0.2883(6) 0.0451(2) 0.0318(17) Uani 1 1 d . . . . .
H12 H -0.0785 0.3039 0.0206 0.038 Uiso 1 1 calc R . . . .
C13 C 0.2649(6) -0.0418(6) 0.3102(2) 0.0267(15) Uani 1 1 d . . . . .
C14 C 0.3225(6) 0.3526(6) 0.29144(19) 0.0249(14) Uani 1 1 d . . . . .
C15 C 0.0692(8) -0.1672(7) -0.0578(2) 0.0344(18) Uani 1 1 d . . . . .
C16 C 0.1478(7) 0.2478(8) -0.0561(2) 0.0364(19) Uani 1 1 d . . . . .
C17 C -0.1994(8) -0.0040(8) -0.0357(2) 0.042(2) Uani 1 1 d . . . . .
C18 C 0.0995(6) 0.5571(6) 0.1790(2) 0.0267(15) Uani 1 1 d . . . . .
O1 O 0.5167(4) 0.1130(5) 0.24098(15) 0.0374(13) Uani 1 1 d . . . . .
H1A H 0.5499 0.0566 0.2276 0.056 Uiso 1 1 d R . . . .
H1B H 0.5358 0.1091 0.2668 0.056 Uiso 1 1 d R . . . .
S1 S 0.24856(17) -0.14046(18) 0.34745(5) 0.0330(4) Uani 1 1 d . . . . .
S2 S 0.32395(18) 0.46150(14) 0.32540(5) 0.0272(4) Uani 1 1 d . . . . .
S3 S 0.1961(2) 0.35860(19) -0.08424(6) 0.0460(5) Uani 1 1 d . . . . .
S4 S 0.05833(19) -0.26358(17) -0.09579(6) 0.0364(5) Uani 1 1 d . . . . .
S5 S -0.27527(19) -0.0723(2) -0.07282(7) 0.0452(5) Uani 1 1 d . . . . .
S6 S 0.15755(18) 0.44471(16) 0.20309(5) 0.0332(4) Uani 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 0.0219(4) 0.0153(4) 0.0153(4) -0.0010(3) -0.0026(4) 0.0005(4)
Fe2 0.0282(5) 0.0189(5) 0.0162(4) -0.0014(4) -0.0039(4) -0.0006(4)
Fe3 0.0550(7) 0.0291(6) 0.0178(5) -0.0085(4) -0.0069(5) 0.0129(5)
N1 0.035(3) 0.017(3) 0.014(3) -0.006(2) -0.002(2) 0.006(3)
N2 0.028(3) 0.021(3) 0.012(3) -0.005(2) -0.003(2) 0.000(2)
N3 0.028(3) 0.018(3) 0.014(3) 0.000(2) -0.002(2) 0.000(2)
N4 0.035(3) 0.024(3) 0.025(3) 0.001(3) -0.001(3) 0.003(3)
N5 0.023(3) 0.019(3) 0.013(3) 0.001(2) 0.002(2) -0.001(2)
N6 0.029(3) 0.017(3) 0.010(2) -0.003(2) -0.001(2) -0.003(2)
N7 0.025(3) 0.017(3) 0.022(3) 0.001(2) 0.009(2) -0.001(2)
N8 0.030(3) 0.031(3) 0.029(3) -0.007(3) 0.015(3) 0.001(3)
N9 0.024(3) 0.022(3) 0.012(2) -0.002(2) -0.003(2) -0.005(2)
N10 0.024(3) 0.017(3) 0.017(2) 0.002(2) -0.007(2) -0.001(3)
N11 0.018(3) 0.016(3) 0.021(3) -0.003(2) -0.001(2) 0.001(2)
N12 0.031(3) 0.018(3) 0.027(3) -0.004(2) -0.004(3) 0.007(2)
N13 0.023(3) 0.023(3) 0.019(3) -0.007(2) 0.000(2) 0.002(2)
N14 0.042(4) 0.024(3) 0.018(3) -0.002(2) 0.000(3) 0.008(3)
N15 0.038(3) 0.019(3) 0.016(3) -0.004(2) 0.004(2) 0.001(3)
N16 0.040(3) 0.022(3) 0.025(3) -0.004(2) 0.005(3) 0.008(3)
N17 0.030(3) 0.019(3) 0.025(3) 0.000(2) 0.004(2) 0.006(3)
N18 0.038(3) 0.020(3) 0.033(3) -0.006(3) -0.005(3) 0.007(3)
N19 0.029(3) 0.020(3) 0.062(5) -0.008(3) 0.000(3) 0.000(3)
N20 0.039(4) 0.027(4) 0.089(6) -0.008(4) 0.007(4) -0.004(3)
N21 0.029(3) 0.018(3) 0.037(4) -0.003(3) -0.001(3) -0.002(2)
N22 0.055(4) 0.028(3) 0.031(4) 0.009(3) 0.020(3) 0.013(3)
N23 0.037(4) 0.055(5) 0.053(5) 0.016(4) 0.014(4) 0.008(3)
N24 0.059(5) 0.097(7) 0.057(5) -0.006(5) 0.036(4) 0.006(5)
N25 0.058(4) 0.027(3) 0.020(3) -0.003(3) -0.007(3) -0.013(3)
N26 0.043(3) 0.025(3) 0.019(3) -0.003(3) -0.007(3) -0.002(3)
N27 0.068(5) 0.037(4) 0.032(4) -0.013(3) -0.009(3) 0.013(3)
N28 0.066(5) 0.038(4) 0.018(3) -0.004(3) -0.004(3) 0.015(3)
N29 0.061(5) 0.071(5) 0.026(3) -0.010(4) -0.012(3) 0.015(4)
N30 0.052(4) 0.038(4) 0.038(4) 0.010(3) 0.004(3) 0.011(4)
C1 0.038(4) 0.019(3) 0.013(3) -0.006(3) -0.001(3) 0.002(3)
C2 0.026(4) 0.025(4) 0.017(3) -0.007(3) 0.000(3) 0.002(3)
C3 0.023(3) 0.017(3) 0.020(3) -0.002(3) 0.003(3) -0.004(3)
C4 0.032(4) 0.019(3) 0.014(3) 0.001(3) 0.006(3) 0.001(3)
C5 0.020(3) 0.027(4) 0.012(3) -0.001(3) 0.000(2) 0.000(3)
C6 0.022(3) 0.023(4) 0.017(3) 0.001(3) -0.005(3) -0.003(3)
C7 0.031(4) 0.024(4) 0.042(4) -0.002(4) 0.002(3) 0.005(3)
C8 0.046(5) 0.031(4) 0.042(5) -0.006(4) -0.005(4) 0.009(4)
C9 0.038(5) 0.035(4) 0.043(5) 0.010(4) 0.013(4) -0.002(4)
C10 0.066(6) 0.058(6) 0.028(4) 0.010(4) 0.014(5) 0.002(5)
C11 0.031(4) 0.024(4) 0.014(3) -0.004(3) 0.001(3) -0.001(3)
C12 0.044(5) 0.032(4) 0.020(4) -0.003(3) -0.007(3) 0.011(4)
C13 0.033(4) 0.029(4) 0.018(3) -0.002(3) -0.006(3) -0.001(3)
C14 0.028(3) 0.028(4) 0.019(3) 0.006(3) 0.000(3) 0.004(3)
C15 0.051(5) 0.029(4) 0.023(4) 0.000(3) -0.003(3) 0.001(4)
C16 0.046(5) 0.043(5) 0.020(4) -0.013(4) -0.014(3) 0.018(4)
C17 0.045(5) 0.051(5) 0.031(4) 0.005(4) 0.007(4) 0.017(4)
C18 0.026(4) 0.028(4) 0.026(4) -0.004(3) 0.003(3) 0.000(3)
O1 0.036(3) 0.049(3) 0.027(3) -0.016(2) -0.008(2) 0.013(2)
S1 0.0396(10) 0.0385(11) 0.0208(9) 0.0059(8) -0.0031(8) -0.0084(9)
S2 0.0419(10) 0.0224(8) 0.0174(7) -0.0039(7) 0.0013(8) 0.0033(8)
S3 0.0581(14) 0.0425(12) 0.0373(11) 0.0027(9) -0.0022(10) 0.0102(11)
S4 0.0449(11) 0.0329(11) 0.0315(10) -0.0137(8) -0.0002(9) 0.0006(9)
S5 0.0412(11) 0.0515(13) 0.0428(11) -0.0018(11) 0.0046(9) 0.0004(10)
S6 0.0459(11) 0.0261(10) 0.0278(9) -0.0040(8) -0.0053(8) 0.0067(9)
_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 N1 2.030(6) . ?
Fe1 N5 2.031(5) . ?
Fe1 N9 2.043(5) . ?
Fe1 N13 2.007(5) . ?
Fe1 N17 2.047(6) . ?
Fe1 N21 1.990(6) . ?
Fe2 N2 2.133(5) . ?
Fe2 N6 2.136(5) . ?
Fe2 N10 2.184(5) . ?
Fe2 N25 2.073(6) . ?
Fe2 N26 2.106(6) . ?
Fe2 O1 2.153(5) . ?
Fe3 N14 2.163(6) . ?
Fe3 N18 2.195(6) . ?
Fe3 N22 2.173(7) . ?
Fe3 N27 2.122(6) . ?
Fe3 N28 2.114(7) . ?
Fe3 N29 2.148(7) . ?
N1 N2 1.390(7) . ?
N1 C1 1.302(8) . ?
N2 C2 1.320(8) . ?
N3 N4 1.403(7) . ?
N3 C1 1.341(8) . ?
N3 C2 1.340(8) . ?
N4 H4A 0.8471 . ?
N4 H4B 0.8555 . ?
N5 N6 1.390(7) . ?
N5 C3 1.301(8) . ?
N6 C4 1.299(8) . ?
N7 N8 1.410(7) . ?
N7 C3 1.347(8) . ?
N7 C4 1.321(8) . ?
N8 H8A 0.8589 . ?
N8 H8B 0.8630 . ?
N9 N10 1.388(7) . ?
N9 C5 1.294(8) . ?
N10 C6 1.292(8) . ?
N11 N12 1.411(7) . ?
N11 C5 1.345(8) . ?
N11 C6 1.333(8) . ?
N12 H12A 0.8592 . ?
N12 H12B 0.8616 . ?
N13 N14 1.391(8) . ?
N13 C11 1.301(8) . ?
N14 C12 1.309(9) . ?
N15 N16 1.416(7) . ?
N15 C11 1.324(8) . ?
N15 C12 1.338(9) . ?
N16 H16A 0.8825 . ?
N16 H16B 0.8860 . ?
N17 N18 1.383(8) . ?
N17 C7 1.311(9) . ?
N18 C8 1.302(10) . ?
N19 N20 1.416(9) . ?
N19 C7 1.348(9) . ?
N19 C8 1.346(10) . ?
N20 H20A 0.8553 . ?
N20 H20B 0.8403 . ?
N21 N22 1.358(9) . ?
N21 C9 1.304(9) . ?
N22 C10 1.292(10) . ?
N23 N24 1.404(9) . ?
N23 C9 1.310(10) . ?
N23 C10 1.336(11) . ?
N24 H24A 0.8869 . ?
N24 H24B 0.8938 . ?
N25 C13 1.132(9) . ?
N26 C14 1.145(8) . ?
N27 C15 1.145(9) . ?
N28 C16 1.155(10) . ?
N29 C17 1.167(10) . ?
N30 C18 1.163(9) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 S1 1.645(7) . ?
C14 S2 1.647(7) . ?
C15 S4 1.638(8) . ?
C16 S3 1.635(10) . ?
C17 S5 1.635(9) . ?
C18 S6 1.621(7) . ?
O1 H1A 0.8499 . ?
O1 H1B 0.8500 . ?
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
N1 Fe1 N5 91.6(2) . . ?
N1 Fe1 N9 93.7(2) . . ?
N1 Fe1 N17 176.9(2) . . ?
N5 Fe1 N9 90.2(2) . . ?
N5 Fe1 N17 90.2(2) . . ?
N9 Fe1 N17 88.8(2) . . ?
N13 Fe1 N1 87.7(2) . . ?
N13 Fe1 N5 88.0(2) . . ?
N13 Fe1 N9 177.7(2) . . ?
N13 Fe1 N17 89.8(2) . . ?
N21 Fe1 N1 87.1(2) . . ?
N21 Fe1 N5 177.8(2) . . ?
N21 Fe1 N9 88.1(2) . . ?
N21 Fe1 N13 93.7(2) . . ?
N21 Fe1 N17 91.2(2) . . ?
N2 Fe2 N6 86.8(2) . . ?
N2 Fe2 N10 87.72(19) . . ?
N2 Fe2 O1 86.4(2) . . ?
N6 Fe2 N10 86.1(2) . . ?
N6 Fe2 O1 172.9(2) . . ?
N25 Fe2 N2 176.3(2) . . ?
N25 Fe2 N6 93.7(2) . . ?
N25 Fe2 N10 88.6(2) . . ?
N25 Fe2 N26 91.6(2) . . ?
N25 Fe2 O1 93.0(2) . . ?
N26 Fe2 N2 92.0(2) . . ?
N26 Fe2 N6 96.1(2) . . ?
N26 Fe2 N10 177.8(2) . . ?
N26 Fe2 O1 86.1(2) . . ?
O1 Fe2 N10 91.73(19) . . ?
N14 Fe3 N18 82.9(2) . . ?
N14 Fe3 N22 88.7(2) . . ?
N22 Fe3 N18 81.4(2) . . ?
N27 Fe3 N14 177.1(2) . . ?
N27 Fe3 N18 94.9(2) . . ?
N27 Fe3 N22 89.1(3) . . ?
N27 Fe3 N29 86.3(3) . . ?
N28 Fe3 N14 88.3(2) . . ?
N28 Fe3 N18 169.4(2) . . ?
N28 Fe3 N22 92.4(3) . . ?
N28 Fe3 N27 93.7(3) . . ?
N28 Fe3 N29 94.8(3) . . ?
N29 Fe3 N14 95.7(3) . . ?
N29 Fe3 N18 92.0(3) . . ?
N29 Fe3 N22 171.6(3) . . ?
N2 N1 Fe1 125.6(4) . . ?
C1 N1 Fe1 126.9(4) . . ?
C1 N1 N2 107.2(5) . . ?
N1 N2 Fe2 126.2(4) . . ?
C2 N2 Fe2 127.0(4) . . ?
C2 N2 N1 106.1(5) . . ?
C1 N3 N4 130.2(5) . . ?
C2 N3 N4 123.5(5) . . ?
C2 N3 C1 106.1(5) . . ?
N3 N4 H4A 110.0 . . ?
N3 N4 H4B 111.4 . . ?
H4A N4 H4B 107.6 . . ?
N6 N5 Fe1 125.4(4) . . ?
C3 N5 Fe1 127.6(4) . . ?
C3 N5 N6 107.0(5) . . ?
N5 N6 Fe2 126.3(4) . . ?
C4 N6 Fe2 127.0(4) . . ?
C4 N6 N5 106.7(5) . . ?
C3 N7 N8 127.9(6) . . ?
C4 N7 N8 125.2(5) . . ?
C4 N7 C3 106.9(5) . . ?
N7 N8 H8A 111.1 . . ?
N7 N8 H8B 109.1 . . ?
H8A N8 H8B 108.2 . . ?
N10 N9 Fe1 123.2(4) . . ?
C5 N9 Fe1 129.2(4) . . ?
C5 N9 N10 107.6(5) . . ?
N9 N10 Fe2 127.4(4) . . ?
C6 N10 Fe2 126.5(4) . . ?
C6 N10 N9 106.1(5) . . ?
C5 N11 N12 129.7(5) . . ?
C6 N11 N12 124.5(5) . . ?
C6 N11 C5 105.8(5) . . ?
N11 N12 H12A 112.5 . . ?
N11 N12 H12B 111.7 . . ?
H12A N12 H12B 106.6 . . ?
N14 N13 Fe1 125.0(4) . . ?
C11 N13 Fe1 128.2(4) . . ?
C11 N13 N14 106.6(5) . . ?
N13 N14 Fe3 127.8(4) . . ?
C12 N14 Fe3 125.4(5) . . ?
C12 N14 N13 106.7(5) . . ?
C11 N15 N16 129.5(5) . . ?
C11 N15 C12 107.0(5) . . ?
C12 N15 N16 123.5(5) . . ?
N15 N16 H16A 110.7 . . ?
N15 N16 H16B 106.6 . . ?
H16A N16 H16B 107.2 . . ?
N18 N17 Fe1 125.2(4) . . ?
C7 N17 Fe1 127.5(5) . . ?
C7 N17 N18 107.2(6) . . ?
N17 N18 Fe3 126.6(4) . . ?
C8 N18 Fe3 125.6(5) . . ?
C8 N18 N17 107.8(6) . . ?
C7 N19 N20 127.7(7) . . ?
C8 N19 N20 124.9(7) . . ?
C8 N19 C7 107.2(6) . . ?
N19 N20 H20A 111.6 . . ?
N19 N20 H20B 108.6 . . ?
H20A N20 H20B 108.7 . . ?
N22 N21 Fe1 124.6(4) . . ?
C9 N21 Fe1 126.3(6) . . ?
C9 N21 N22 109.0(6) . . ?
N21 N22 Fe3 129.4(4) . . ?
C10 N22 Fe3 124.9(6) . . ?
C10 N22 N21 105.6(7) . . ?
C9 N23 N24 128.5(8) . . ?
C9 N23 C10 107.3(7) . . ?
C10 N23 N24 124.2(8) . . ?
N23 N24 H24A 98.4 . . ?
N23 N24 H24B 113.0 . . ?
H24A N24 H24B 106.2 . . ?
C13 N25 Fe2 173.8(6) . . ?
C14 N26 Fe2 171.2(5) . . ?
C15 N27 Fe3 165.9(7) . . ?
C16 N28 Fe3 168.8(6) . . ?
C17 N29 Fe3 137.1(7) . . ?
N1 C1 N3 110.4(5) . . ?
N1 C1 H1 124.8 . . ?
N3 C1 H1 124.8 . . ?
N2 C2 N3 110.2(6) . . ?
N2 C2 H2 124.9 . . ?
N3 C2 H2 124.9 . . ?
N5 C3 N7 109.1(6) . . ?
N5 C3 H3 125.4 . . ?
N7 C3 H3 125.4 . . ?
N6 C4 N7 110.3(5) . . ?
N6 C4 H4 124.8 . . ?
N7 C4 H4 124.8 . . ?
N9 C5 N11 109.5(5) . . ?
N9 C5 H5 125.2 . . ?
N11 C5 H5 125.2 . . ?
N10 C6 N11 111.0(5) . . ?
N10 C6 H6 124.5 . . ?
N11 C6 H6 124.5 . . ?
N17 C7 N19 108.8(7) . . ?
N17 C7 H7 125.6 . . ?
N19 C7 H7 125.6 . . ?
N18 C8 N19 108.9(7) . . ?
N18 C8 H8 125.5 . . ?
N19 C8 H8 125.5 . . ?
N21 C9 N23 108.0(8) . . ?
N21 C9 H9 126.0 . . ?
N23 C9 H9 126.0 . . ?
N22 C10 N23 109.9(7) . . ?
N22 C10 H10 125.1 . . ?
N23 C10 H10 125.1 . . ?
N13 C11 N15 110.3(6) . . ?
N13 C11 H11 124.8 . . ?
N15 C11 H11 124.8 . . ?
N14 C12 N15 109.4(6) . . ?
N14 C12 H12 125.3 . . ?
N15 C12 H12 125.3 . . ?
N25 C13 S1 176.0(7) . . ?
N26 C14 S2 177.1(7) . . ?
N27 C15 S4 178.9(8) . . ?
N28 C16 S3 179.1(7) . . ?
N29 C17 S5 173.6(8) . . ?
N30 C18 S6 178.7(7) . . ?
Fe2 O1 H1A 112.7 . . ?
Fe2 O1 H1B 112.5 . . ?
H1A O1 H1B 110.1 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 N1 N2 Fe2 -1.2(7) . . . . ?
Fe1 N1 N2 C2 -172.2(4) . . . . ?
Fe1 N1 C1 N3 172.5(4) . . . . ?
Fe1 N5 N6 Fe2 -5.2(7) . . . . ?
Fe1 N5 N6 C4 177.1(4) . . . . ?
Fe1 N5 C3 N7 -177.1(4) . . . . ?
Fe1 N9 N10 Fe2 1.0(7) . . . . ?
Fe1 N9 N10 C6 178.4(4) . . . . ?
Fe1 N9 C5 N11 -177.6(4) . . . . ?
Fe1 N13 N14 Fe3 -9.3(8) . . . . ?
Fe1 N13 N14 C12 174.1(5) . . . . ?
Fe1 N13 C11 N15 -174.6(4) . . . . ?
Fe1 N17 N18 Fe3 -5.3(7) . . . . ?
Fe1 N17 N18 C8 176.4(5) . . . . ?
Fe1 N17 C7 N19 -176.3(4) . . . . ?
Fe1 N21 N22 Fe3 8.2(8) . . . . ?
Fe1 N21 N22 C10 -174.1(5) . . . . ?
Fe1 N21 C9 N23 176.7(5) . . . . ?
Fe2 N2 C2 N3 -172.6(4) . . . . ?
Fe2 N6 C4 N7 -177.3(4) . . . . ?
Fe2 N10 C6 N11 177.1(4) . . . . ?
Fe3 N14 C12 N15 -175.6(4) . . . . ?
Fe3 N18 C8 N19 -177.7(4) . . . . ?
Fe3 N22 C10 N23 173.9(5) . . . . ?
N1 N2 C2 N3 -1.7(7) . . . . ?
N2 N1 C1 N3 -1.8(7) . . . . ?
N4 N3 C1 N1 -174.6(6) . . . . ?
N4 N3 C2 N2 176.4(5) . . . . ?
N5 N6 C4 N7 0.4(7) . . . . ?
N6 N5 C3 N7 0.5(7) . . . . ?
N8 N7 C3 N5 -179.9(6) . . . . ?
N8 N7 C4 N6 179.6(6) . . . . ?
N9 N10 C6 N11 -0.4(7) . . . . ?
N10 N9 C5 N11 1.3(6) . . . . ?
N12 N11 C5 N9 -179.7(6) . . . . ?
N12 N11 C6 N10 179.4(6) . . . . ?
N13 N14 C12 N15 1.1(8) . . . . ?
N14 N13 C11 N15 0.0(7) . . . . ?
N16 N15 C11 N13 -179.3(6) . . . . ?
N16 N15 C12 N14 178.9(6) . . . . ?
N17 N18 C8 N19 0.7(8) . . . . ?
N18 N17 C7 N19 1.1(7) . . . . ?
N20 N19 C7 N17 174.7(6) . . . . ?
N20 N19 C8 N18 -175.5(6) . . . . ?
N21 N22 C10 N23 -3.9(9) . . . . ?
N22 N21 C9 N23 0.6(9) . . . . ?
N24 N23 C9 N21 176.4(8) . . . . ?
N24 N23 C10 N22 -175.0(8) . . . . ?
C1 N1 N2 Fe2 173.1(4) . . . . ?
C1 N1 N2 C2 2.1(7) . . . . ?
C1 N3 C2 N2 0.7(7) . . . . ?
C2 N3 C1 N1 0.7(7) . . . . ?
C3 N5 N6 Fe2 177.1(4) . . . . ?
C3 N5 N6 C4 -0.5(7) . . . . ?
C3 N7 C4 N6 -0.1(7) . . . . ?
C4 N7 C3 N5 -0.3(7) . . . . ?
C5 N9 N10 Fe2 -178.0(4) . . . . ?
C5 N9 N10 C6 -0.6(6) . . . . ?
C5 N11 C6 N10 1.1(7) . . . . ?
C6 N11 C5 N9 -1.5(7) . . . . ?
C7 N17 N18 Fe3 177.3(4) . . . . ?
C7 N17 N18 C8 -1.1(7) . . . . ?
C7 N19 C8 N18 -0.1(8) . . . . ?
C8 N19 C7 N17 -0.6(8) . . . . ?
C9 N21 N22 Fe3 -175.6(5) . . . . ?
C9 N21 N22 C10 2.0(8) . . . . ?
C9 N23 C10 N22 4.4(10) . . . . ?
C10 N23 C9 N21 -3.0(9) . . . . ?
C11 N13 N14 Fe3 175.9(5) . . . . ?
C11 N13 N14 C12 -0.6(7) . . . . ?
C11 N15 C12 N14 -1.1(8) . . . . ?
C12 N15 C11 N13 0.7(8) . . . . ?
_iucr_refine_instructions_details
;
e.res created by SHELXL-2014/7
TITL E_a.res in P2(1)2(1)2(1)
REM Old TITL E in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.114, Rweak 0.032, Alpha 0.003, Orientation as input
REM Flack x = 0.040 ( 0.007 ) from Parsons' quotients
REM Formula found by SHELXT: C38 N11 S6 Fe3
CELL 0.71073 10.799 11.4073 31.8466 90 90 90
ZERR 4 0.003 0.0054 0.0091 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H Fe N O S
UNIT 72 104 12 120 4 24
L.S. 100
PLAN 1
SIZE 0.102 0.186 0.227
TEMP -173
BOND $H
htab
LIST 6
MORE -1
CONF
fmap 2
acta 52
OMIT 0 0 6
OMIT 1 0 8
OMIT 0 1 8
OMIT 8 0 1
REM
REM
REM
WGHT 0.041600 6.883800
FVAR 0.09089
FE1 3 0.179189 0.077831 0.121886 11.00000 0.02191 0.01528 =
0.01535 -0.00103 -0.00255 0.00055
FE2 3 0.319743 0.123580 0.231170 11.00000 0.02821 0.01886 =
0.01621 -0.00144 -0.00392 -0.00065
FE3 3 0.050778 0.047269 0.008781 11.00000 0.05503 0.02908 =
0.01781 -0.00847 -0.00694 0.01287
N1 4 0.309023 0.200426 0.135905 11.00000 0.03493 0.01673 =
0.01365 -0.00633 -0.00210 0.00560
N2 4 0.362246 0.217931 0.175155 11.00000 0.02767 0.02063 =
0.01191 -0.00503 -0.00275 -0.00003
N3 4 0.423715 0.356383 0.132748 11.00000 0.02824 0.01830 =
0.01412 -0.00028 -0.00168 0.00019
N4 4 0.479966 0.461586 0.120217 11.00000 0.03523 0.02422 =
0.02467 0.00136 -0.00124 0.00282
AFIX 7
H4A 2 0.551194 0.447888 0.110212 11.00000 -1.20000
H4B 2 0.437705 0.496193 0.101176 11.00000 -1.20000
AFIX 0
N5 4 0.080031 0.118299 0.174110 11.00000 0.02254 0.01888 =
0.01316 0.00083 0.00198 -0.00065
N6 4 0.129608 0.140009 0.213616 11.00000 0.02859 0.01693 =
0.00986 -0.00274 -0.00146 -0.00316
N7 4 -0.067599 0.164532 0.216654 11.00000 0.02460 0.01725 =
0.02164 0.00066 0.00862 -0.00085
N8 4 -0.185603 0.189113 0.233443 11.00000 0.02951 0.03135 =
0.02891 -0.00711 0.01523 0.00146
AFIX 7
H8A 2 -0.229571 0.126582 0.235299 11.00000 -1.20000
H8B 2 -0.177087 0.218016 0.258320 11.00000 -1.20000
AFIX 0
N9 4 0.268299 -0.052273 0.154003 11.00000 0.02371 0.02181 =
0.01190 -0.00180 -0.00301 -0.00514
N10 4 0.320312 -0.036232 0.193426 11.00000 0.02423 0.01685 =
0.01712 0.00170 -0.00740 -0.00145
N11 4 0.345124 -0.216952 0.174630 11.00000 0.01847 0.01611 =
0.02122 -0.00282 -0.00112 0.00144
N12 4 0.383978 -0.334809 0.177089 11.00000 0.03055 0.01787 =
0.02747 -0.00426 -0.00419 0.00713
AFIX 7
H12A 2 0.322912 -0.383084 0.177254 11.00000 -1.20000
H12B 2 0.430031 -0.353962 0.156086 11.00000 -1.20000
AFIX 0
N13 4 0.085437 0.204009 0.091610 11.00000 0.02308 0.02315 =
0.01897 -0.00677 -0.00016 0.00172
N14 4 0.030975 0.191629 0.052291 11.00000 0.04235 0.02403 =
0.01831 -0.00216 -0.00031 0.00827
N15 4 -0.016239 0.361639 0.077477 11.00000 0.03809 0.01854 =
0.01643 -0.00448 0.00423 0.00114
N16 4 -0.069522 0.474931 0.079127 11.00000 0.04028 0.02155 =
0.02481 -0.00425 0.00453 0.00825
AFIX 3
H16A 2 -0.011902 0.528782 0.082877 11.00000 -1.20000
H16B 2 -0.118002 0.476301 0.101567 11.00000 -1.20000
AFIX 0
N17 4 0.047146 -0.041550 0.104642 11.00000 0.03014 0.01879 =
0.02486 0.00027 0.00364 0.00586
N18 4 0.003414 -0.057782 0.064240 11.00000 0.03817 0.02026 =
0.03344 -0.00557 -0.00459 0.00735
N19 4 -0.083165 -0.185402 0.104608 11.00000 0.02894 0.02014 =
0.06220 -0.00821 0.00011 0.00048
N20 4 -0.152472 -0.284944 0.116959 11.00000 0.03883 0.02739 =
0.08920 -0.00778 0.00680 -0.00360
AFIX 7
H20A 2 -0.115345 -0.323906 0.136145 11.00000 -1.20000
H20B 2 -0.221182 -0.262318 0.126320 11.00000 -1.20000
AFIX 0
N21 4 0.282033 0.037332 0.072088 11.00000 0.02923 0.01760 =
0.03666 -0.00253 -0.00073 -0.00156
N22 4 0.236739 0.019282 0.032849 11.00000 0.05549 0.02828 =
0.03088 0.00916 0.02032 0.01325
N23 4 0.433010 -0.012785 0.033798 11.00000 0.03737 0.05477 =
0.05331 0.01554 0.01404 0.00819
N24 4 0.551840 -0.036848 0.018160 11.00000 0.05878 0.09708 =
0.05701 -0.00569 0.03602 0.00590
AFIX 7
H24A 2 0.593674 -0.030779 0.042026 11.00000 -1.20000
H24B 2 0.560782 -0.111045 0.009669 11.00000 -1.20000
AFIX 0
N25 4 0.280933 0.021878 0.283493 11.00000 0.05791 0.02733 =
0.02019 -0.00274 -0.00708 -0.01298
N26 4 0.326718 0.277203 0.267762 11.00000 0.04349 0.02505 =
0.01854 -0.00303 -0.00679 -0.00160
N27 4 0.074909 -0.099200 -0.031461 11.00000 0.06781 0.03703 =
0.03222 -0.01283 -0.00892 0.01281
N28 4 0.113345 0.168756 -0.036642 11.00000 0.06552 0.03766 =
0.01756 -0.00402 -0.00427 0.01514
N29 4 -0.138224 0.049018 -0.012251 11.00000 0.06134 0.07139 =
0.02599 -0.00954 -0.01248 0.01503
N30 4 0.059056 0.639119 0.162165 11.00000 0.05236 0.03802 =
0.03812 0.00961 0.00391 0.01094
C1 1 0.349497 0.283352 0.111405 11.00000 0.03831 0.01850 =
0.01330 -0.00555 -0.00109 0.00172
AFIX 43
H1 2 0.329317 0.291044 0.082501 11.00000 -1.20000
AFIX 0
C2 1 0.429181 0.314319 0.172007 11.00000 0.02590 0.02535 =
0.01704 -0.00691 -0.00004 0.00232
AFIX 43
H2 2 0.474664 0.348898 0.194335 11.00000 -1.20000
AFIX 0
C3 1 -0.039054 0.133240 0.177031 11.00000 0.02297 0.01737 =
0.01963 -0.00221 0.00265 -0.00408
AFIX 43
H3 2 -0.096721 0.123619 0.154769 11.00000 -1.20000
AFIX 0
C4 1 0.037426 0.167702 0.237875 11.00000 0.03186 0.01892 =
0.01361 0.00088 0.00634 0.00063
AFIX 43
H4 2 0.044543 0.187420 0.266757 11.00000 -1.20000
AFIX 0
C5 1 0.285983 -0.160514 0.143421 11.00000 0.01956 0.02737 =
0.01197 -0.00054 0.00002 -0.00010
AFIX 43
H5 2 0.261045 -0.194841 0.117592 11.00000 -1.20000
AFIX 0
C6 1 0.365236 -0.136768 0.204300 11.00000 0.02200 0.02346 =
0.01741 0.00130 -0.00498 -0.00298
AFIX 43
H6 2 0.407020 -0.151545 0.230011 11.00000 -1.20000
AFIX 0
C7 1 -0.007762 -0.119201 0.128580 11.00000 0.03108 0.02435 =
0.04235 -0.00227 0.00222 0.00471
AFIX 43
H7 2 0.003707 -0.127469 0.158008 11.00000 -1.20000
AFIX 0
C8 1 -0.074091 -0.145231 0.064973 11.00000 0.04596 0.03115 =
0.04238 -0.00565 -0.00533 0.00891
AFIX 43
H8 2 -0.117214 -0.175720 0.041377 11.00000 -1.20000
AFIX 0
C9 1 0.400837 0.016749 0.072009 11.00000 0.03797 0.03492 =
0.04276 0.01036 0.01291 -0.00153
AFIX 43
H9 2 0.454596 0.022221 0.095540 11.00000 -1.20000
AFIX 0
C10 1 0.329890 -0.015504 0.010651 11.00000 0.06624 0.05760 =
0.02762 0.00998 0.01418 0.00186
AFIX 43
H10 2 0.325679 -0.039450 -0.017884 11.00000 -1.20000
AFIX 0
C11 1 0.054298 0.307315 0.105341 11.00000 0.03122 0.02368 =
0.01409 -0.00357 0.00088 -0.00075
AFIX 43
H11 2 0.078717 0.339207 0.131624 11.00000 -1.20000
AFIX 0
C12 1 -0.030769 0.288309 0.045078 11.00000 0.04377 0.03174 =
0.01981 -0.00298 -0.00650 0.01070
AFIX 43
H12 2 -0.078456 0.303946 0.020644 11.00000 -1.20000
AFIX 0
C13 1 0.264891 -0.041785 0.310211 11.00000 0.03295 0.02871 =
0.01837 -0.00209 -0.00590 -0.00145
C14 1 0.322455 0.352641 0.291436 11.00000 0.02775 0.02769 =
0.01915 0.00593 0.00024 0.00437
C15 1 0.069169 -0.167221 -0.057824 11.00000 0.05108 0.02926 =
0.02287 0.00024 -0.00278 0.00066
C16 1 0.147755 0.247834 -0.056066 11.00000 0.04614 0.04316 =
0.01983 -0.01258 -0.01430 0.01779
C17 1 -0.199409 -0.003971 -0.035733 11.00000 0.04538 0.05085 =
0.03094 0.00498 0.00673 0.01691
C18 1 0.099513 0.557135 0.178963 11.00000 0.02619 0.02783 =
0.02600 -0.00352 0.00349 0.00022
O1 5 0.516716 0.112952 0.240984 11.00000 0.03629 0.04878 =
0.02704 -0.01564 -0.00811 0.01339
AFIX 3
H1A 2 0.549896 0.056582 0.227644 11.00000 -1.50000
H1B 2 0.535766 0.109122 0.266844 11.00000 -1.50000
AFIX 0
S1 6 0.248559 -0.140464 0.347455 11.00000 0.03962 0.03847 =
0.02077 0.00592 -0.00309 -0.00843
S2 6 0.323945 0.461500 0.325401 11.00000 0.04190 0.02236 =
0.01736 -0.00388 0.00128 0.00326
S3 6 0.196144 0.358605 -0.084235 11.00000 0.05812 0.04252 =
0.03731 0.00267 -0.00224 0.01024
S4 6 0.058332 -0.263579 -0.095794 11.00000 0.04487 0.03294 =
0.03152 -0.01369 -0.00024 0.00062
S5 6 -0.275273 -0.072260 -0.072824 11.00000 0.04123 0.05154 =
0.04275 -0.00182 0.00461 0.00037
S6 6 0.157553 0.444713 0.203091 11.00000 0.04589 0.02609 =
0.02776 -0.00402 -0.00530 0.00670
HKLF 4
REM E_a.res in P2(1)2(1)2(1)
REM R1 = 0.0416 for 6348 Fo > 4sig(Fo) and 0.0524 for all 7268 data
REM 528 parameters refined using 0 restraints
END
WGHT 0.0415 6.8821
REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, y+1/2, -z+1/2
HTAB N4 S1_$1
EQIV $2 x+1/2, -y+1/2, -z
HTAB N4 S5_$2
EQIV $3 -x, y-1/2, -z+1/2
HTAB N8 S2_$3
HTAB N8 S6_$3
EQIV $4 x, y-1, z
HTAB N12 S6_$4
HTAB N12 N4_$4
EQIV $5 x+1/2, -y-1/2, -z
HTAB N12 S4_$5
HTAB N16 S5_$2
EQIV $6 -x, y+1/2, -z+1/2
HTAB N16 S1_$6
HTAB N20 N30_$4
EQIV $7 x-1/2, -y-1/2, -z
HTAB N20 S4_$7
HTAB N24 S3_$2
HTAB N24 S4_$5
HTAB C4 N30_$3
HTAB C9 S3_$2
HTAB C10 N16_$2
HTAB C11 S6
EQIV $8 -x+1, y-1/2, -z+1/2
HTAB O1 S2_$8
HTAB O1 N12_$1
REM Highest difference peak 0.837, deepest hole -0.522, 1-sigma level 0.083
Q1 1 -0.3173 -0.0943 -0.0291 11.00000 0.05 0.84
REM The information below was added by Olex2.
REM
REM R1 = 0.0416 for 6348 Fo > 4sig(Fo) and 0.0524 for all 41013 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 0.84, deepest hole -0.52
REM Mean Shift 0, Max Shift 0.000.
REM +++ Tabular Listing of Refinement Information +++
REM R1_all = 0.0524
REM R1_gt = 0.0416
REM wR_ref = 0.0968
REM GOOF = 1.037
REM Shift_max = 0.000
REM Shift_mean = 0
REM Reflections_all = 41013
REM Reflections_gt = 6348
REM Parameters = n/a
REM Hole = -0.52
REM Peak = 0.84
REM Flack = 0.004(7)
;
_olex2_submission_special_instructions 'No special instructions were received'