#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/86/2018651.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2018651
loop_
_publ_author_name
'Zhong, Kai-Long'
_publ_section_title
;
 Tris(1,10-phenanthroline-κ²N,N')iron(II)
 bis(2,4,5-tricarboxybenzoate) monohydrate and
 tris(2,2'-bipyridine-κ²N,N')iron(II)
 2,5-dicarboxybenzene-1,4-dicarboxylate--benzene-1,2,4,5-tetracarboxylic
 acid--water (1/1/2)
;
_journal_coeditor_code           SF3175
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m259
_journal_page_last               m264
_journal_paper_doi               10.1107/S0108270112034567
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Fe (C10 H8 N2)3] (C10 H4 O8) , C10 H6 O8 , 2H2 O'
_chemical_formula_moiety
'C30 H24 Fe N6 2+, C10 H4 O8 2-, C10 H6 O8, 2(H2 O)'
_chemical_formula_sum            'C50 H38 Fe N6 O18'
_chemical_formula_weight         1066.71
_chemical_name_systematic
;
tris(2,2'-bipyridine-κ²N,N')iron(II)
2,5-dicarboxybenzene-1,4-dicarboxylate--benzene-1,2,4,5-tetracarboxylic
acid--water (1/1/2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.767(3)
_cell_length_b                   13.911(3)
_cell_length_c                   24.202(5)
_cell_measurement_reflns_used    19949
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      27.5165
_cell_measurement_theta_min      3.0334
_cell_volume                     4521.9(18)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22163
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.9588
_exptl_absorpt_correction_T_min  0.8488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.329
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         7925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0932
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0284P)²+7.0361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                6272
_reflns_number_total             7925
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sf3175.cif
_cod_data_source_block           II
_cod_original_cell_volume        4521.7(16)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               2018651
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Fe Fe1 0.90033(5) 0.67650(5) 0.23293(3) 0.0288(2) Uani d . 1 1
N N1 1.0281(3) 0.6191(3) 0.27004(18) 0.0328(10) Uani d . 1 1
N N2 0.8860(3) 0.5532(3) 0.19218(18) 0.0332(10) Uani d . 1 1
N N3 0.8288(3) 0.6213(3) 0.28746(17) 0.0302(10) Uani d . 1 1
N N4 0.7653(3) 0.7216(3) 0.19734(17) 0.0300(10) Uani d . 1 1
N N5 0.9282(3) 0.7985(3) 0.27426(18) 0.0317(10) Uani d . 1 1
N N6 0.9633(3) 0.7439(3) 0.17877(17) 0.0289(10) Uani d . 1 1
O O1 0.1022(4) 0.4288(3) -0.0236(2) 0.0778(16) Uani d . 1 1
O O2 0.0607(4) 0.3355(3) 0.03997(19) 0.0691(14) Uani d . 1 1
H H2 0.0685 0.3330 0.0749 0.104 Uiso calc R 1 1
O O3 0.1306(4) 0.3003(3) 0.13913(19) 0.0637(13) Uani d . 1 1
O O4 0.2504(4) 0.3572(3) 0.20825(19) 0.0571(12) Uani d . 1 1
O O5 0.3743(3) 0.7088(3) 0.21193(17) 0.0509(11) Uani d . 1 1
O O6 0.2149(3) 0.7459(3) 0.20569(15) 0.0418(10) Uani d . 1 1
H H6 0.2389 0.7862 0.2302 0.063 Uiso calc R 1 1
O O7 0.2831(3) 0.7999(2) 0.09331(15) 0.0417(10) Uani d . 1 1
O O8 0.2010(2) 0.7494(2) 0.00846(15) 0.0340(8) Uani d . 1 1
O O9 0.1418(3) 1.1331(3) 0.04668(16) 0.0450(10) Uani d . 1 1
H H9 0.0854 1.1088 0.0396 0.068 Uiso calc R 1 1
O O10 0.1505(3) 1.0687(3) -0.03662(16) 0.0408(9) Uani d . 1 1
O O11 0.2891(3) 0.9612(2) 0.04911(16) 0.0395(9) Uani d . 1 1
H H11 0.2935 0.9048 0.0606 0.059 Uiso calc R 1 1
O O12 0.4554(3) 0.9543(3) 0.07071(18) 0.0460(10) Uani d . 1 1
O O13 0.6496(3) 1.2180(3) 0.03636(17) 0.0463(10) Uani d . 1 1
H H13 0.7032 1.2433 0.0340 0.069 Uiso calc R 1 1
O O14 0.5871(3) 1.3554(3) -0.00258(19) 0.0535(12) Uani d . 1 1
O O15 0.4067(3) 1.4551(3) 0.03123(17) 0.0500(11) Uani d . 1 1
H H15 0.4069 1.5117 0.0204 0.075 Uiso calc R 1 1
O O16 0.3747(3) 1.4231(3) -0.06068(18) 0.0591(12) Uani d . 1 1
C C1 0.1054(5) 0.4115(4) 0.0261(3) 0.0492(16) Uani d . 1 1
C C2 0.1912(5) 0.3649(4) 0.1610(3) 0.0454(15) Uani d . 1 1
C C3 0.2868(4) 0.7002(4) 0.1894(2) 0.0334(13) Uani d . 1 1
C C4 0.2343(4) 0.7381(4) 0.0607(2) 0.0338(13) Uani d . 1 1
C C5 0.1598(4) 0.4775(4) 0.0719(2) 0.0340(13) Uani d . 1 1
C C6 0.1945(4) 0.4591(3) 0.1300(2) 0.0335(13) Uani d . 1 1
C C7 0.2367(4) 0.5343(3) 0.1652(2) 0.0334(13) Uani d . 1 1
H H7A 0.2591 0.5223 0.2041 0.040 Uiso calc R 1 1
C C8 0.2469(4) 0.6261(3) 0.1450(2) 0.0276(11) Uani d . 1 1
C C9 0.2197(4) 0.6428(3) 0.0870(2) 0.0285(12) Uani d . 1 1
C C10 0.1751(4) 0.5683(4) 0.0523(2) 0.0349(13) Uani d . 1 1
H H10A 0.1542 0.5804 0.0132 0.042 Uiso calc R 1 1
C C11 0.1877(4) 1.1121(4) 0.0056(2) 0.0317(12) Uani d . 1 1
C C12 0.3780(4) 0.9963(4) 0.0527(2) 0.0303(12) Uani d . 1 1
C C13 0.5767(4) 1.2775(4) 0.0173(2) 0.0333(12) Uani d . 1 1
C C14 0.3908(4) 1.3976(4) -0.0129(3) 0.0375(13) Uani d . 1 1
C C15 0.2904(4) 1.1536(3) 0.0153(2) 0.0270(11) Uani d . 1 1
C C16 0.3766(4) 1.0996(3) 0.0325(2) 0.0279(11) Uani d . 1 1
C C17 0.4685(4) 1.1420(3) 0.0340(2) 0.0285(11) Uani d . 1 1
H H17A 0.5267 1.1050 0.0449 0.034 Uiso calc R 1 1
C C18 0.4761(4) 1.2383(4) 0.0197(2) 0.0305(12) Uani d . 1 1
C C19 0.3898(4) 1.2933(3) 0.0046(2) 0.0305(12) Uani d . 1 1
C C20 0.2983(4) 1.2505(4) 0.0022(2) 0.0339(12) Uani d . 1 1
H H20A 0.2401 1.2877 -0.0084 0.041 Uiso calc R 1 1
C C21 1.1038(4) 0.6620(5) 0.3061(2) 0.0468(15) Uani d . 1 1
H H21A 1.0984 0.7277 0.3141 0.056 Uiso calc R 1 1
C C22 1.1904(4) 0.6128(5) 0.3320(3) 0.0553(18) Uani d . 1 1
H H22A 1.2436 0.6451 0.3557 0.066 Uiso calc R 1 1
C C23 1.1956(5) 0.5164(5) 0.3220(3) 0.0564(18) Uani d . 1 1
H H23A 1.2516 0.4812 0.3405 0.068 Uiso calc R 1 1
C C24 1.1197(5) 0.4707(5) 0.2852(3) 0.0526(17) Uani d . 1 1
H H24A 1.1227 0.4044 0.2784 0.063 Uiso calc R 1 1
C C25 1.0390(4) 0.5246(4) 0.2584(2) 0.0391(14) Uani d . 1 1
C C26 0.9578(4) 0.4868(4) 0.2131(3) 0.0436(14) Uani d . 1 1
C C27 0.9556(5) 0.3933(4) 0.1918(3) 0.0579(18) Uani d . 1 1
H H27A 1.0034 0.3476 0.2085 0.069 Uiso calc R 1 1
C C28 0.8810(5) 0.3702(5) 0.1456(3) 0.063(2) Uani d . 1 1
H H28A 0.8791 0.3088 0.1293 0.076 Uiso calc R 1 1
C C29 0.8106(5) 0.4362(4) 0.1237(3) 0.0581(18) Uani d . 1 1
H H29A 0.7597 0.4210 0.0922 0.070 Uiso calc R 1 1
C C30 0.8148(4) 0.5263(4) 0.1485(3) 0.0463(15) Uani d . 1 1
H H30A 0.7645 0.5708 0.1336 0.056 Uiso calc R 1 1
C C31 0.8664(4) 0.5707(4) 0.3345(2) 0.0388(14) Uani d . 1 1
H H31A 0.9351 0.5575 0.3431 0.047 Uiso calc R 1 1
C C32 0.8099(5) 0.5372(4) 0.3706(2) 0.0456(15) Uani d . 1 1
H H32A 0.8395 0.5027 0.4034 0.055 Uiso calc R 1 1
C C33 0.7097(5) 0.5550(4) 0.3581(3) 0.0481(16) Uani d . 1 1
H H33A 0.6696 0.5322 0.3821 0.058 Uiso calc R 1 1
C C34 0.6679(4) 0.6059(4) 0.3103(3) 0.0485(16) Uani d . 1 1
H H34A 0.5991 0.6186 0.3010 0.058 Uiso calc R 1 1
C C35 0.7297(4) 0.6384(4) 0.2759(2) 0.0341(13) Uani d . 1 1
C C36 0.6932(4) 0.6951(4) 0.2245(2) 0.0336(13) Uani d . 1 1
C C37 0.5943(4) 0.7203(4) 0.2045(3) 0.0455(15) Uani d . 1 1
H H37A 0.5458 0.7011 0.2242 0.055 Uiso calc R 1 1
C C38 0.5677(4) 0.7732(4) 0.1559(3) 0.0450(15) Uani d . 1 1
H H38A 0.5008 0.7899 0.1417 0.054 Uiso calc R 1 1
C C39 0.6393(4) 0.8016(4) 0.1284(2) 0.0421(14) Uani d . 1 1
H H39A 0.6224 0.8386 0.0951 0.050 Uiso calc R 1 1
C C40 0.7375(4) 0.7750(4) 0.1500(2) 0.0367(13) Uani d . 1 1
H H40A 0.7865 0.7951 0.1309 0.044 Uiso calc R 1 1
C C41 0.9079(4) 0.8224(4) 0.3237(2) 0.0444(14) Uani d . 1 1
H H41A 0.8725 0.7783 0.3412 0.053 Uiso calc R 1 1
C C42 0.9363(5) 0.9093(4) 0.3507(3) 0.0498(16) Uani d . 1 1
H H42A 0.9203 0.9230 0.3857 0.060 Uiso calc R 1 1
C C43 0.9875(5) 0.9742(4) 0.3263(3) 0.0514(16) Uani d . 1 1
H H43A 1.0092 1.0325 0.3447 0.062 Uiso calc R 1 1
C C44 1.0071(4) 0.9529(4) 0.2738(2) 0.0440(15) Uani d . 1 1
H H44A 1.0407 0.9975 0.2555 0.053 Uiso calc R 1 1
C C45 0.9767(4) 0.8652(4) 0.2485(2) 0.0362(13) Uani d . 1 1
C C46 0.9941(3) 0.8351(4) 0.1929(2) 0.0305(12) Uani d . 1 1
C C47 1.0360(4) 0.8936(4) 0.1586(2) 0.0364(13) Uani d . 1 1
H H47A 1.0570 0.9561 0.1702 0.044 Uiso calc R 1 1
C C48 1.0464(4) 0.8588(4) 0.1072(2) 0.0407(14) Uani d . 1 1
H H48A 1.0746 0.8975 0.0829 0.049 Uiso calc R 1 1
C C49 1.0156(4) 0.7676(4) 0.0915(2) 0.0351(13) Uani d . 1 1
H H49A 1.0216 0.7433 0.0562 0.042 Uiso calc R 1 1
C C50 0.9753(4) 0.7110(4) 0.1280(2) 0.0375(13) Uani d . 1 1
H H50A 0.9557 0.6478 0.1171 0.045 Uiso calc R 1 1
O O1W -0.0520(3) 1.1110(3) 0.03642(17) 0.0473(10) Uani d . 1 1
H H1WA -0.0960 1.1531 0.0182 0.071 Uiso d R 1 1
H H1WB -0.0807 1.0602 0.0331 0.071 Uiso d R 1 1
O O2W 0.0498(4) 0.1267(3) 0.1672(2) 0.0772(15) Uani d . 1 1
H H2WA 0.0718 0.1326 0.2013 0.116 Uiso d R 1 1
H H2WB 0.0610 0.1753 0.1504 0.116 Uiso d R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N1 Fe1 N2 81.71(18) y
N3 Fe1 N4 81.64(17) y
N5 Fe1 N6 82.06(17) y
N1 Fe1 N6 90.98(17) ?
N1 Fe1 N5 93.62(18) ?
N6 Fe1 N2 95.27(17) ?
N5 Fe1 N2 174.60(17) ?
N1 Fe1 N3 93.70(17) ?
N6 Fe1 N3 173.95(17) ?
N5 Fe1 N3 93.79(17) ?
N2 Fe1 N3 89.22(17) ?
N1 Fe1 N4 174.02(18) ?
N6 Fe1 N4 93.94(17) ?
N5 Fe1 N4 90.44(17) ?
N2 Fe1 N4 94.43(18) ?
C21 N1 C25 117.3(5) ?
C21 N1 Fe1 127.4(4) ?
C25 N1 Fe1 115.3(4) ?
C30 N2 C26 116.9(5) ?
C30 N2 Fe1 128.3(4) ?
C26 N2 Fe1 114.8(4) ?
C31 N3 C35 116.9(5) ?
C31 N3 Fe1 128.1(4) ?
C35 N3 Fe1 115.1(3) ?
C40 N4 C36 117.3(4) ?
C40 N4 Fe1 127.7(4) ?
C36 N4 Fe1 115.0(3) ?
C41 N5 C45 117.4(5) ?
C41 N5 Fe1 128.2(4) ?
C45 N5 Fe1 114.4(3) ?
C50 N6 C46 116.7(4) ?
C50 N6 Fe1 127.2(4) ?
C46 N6 Fe1 116.0(3) ?
C1 O2 H2 109.5 ?
C3 O6 H6 109.5 ?
C11 O9 H9 109.5 ?
C12 O11 H11 109.5 ?
C13 O13 H13 109.5 ?
C14 O15 H15 109.5 ?
O1 C1 O2 119.8(6) ?
O1 C1 C5 120.7(6) ?
O2 C1 C5 119.4(6) ?
O4 C2 O3 124.0(5) ?
O4 C2 C6 116.2(5) ?
O3 C2 C6 119.8(6) ?
O5 C3 O6 124.0(5) ?
O5 C3 C8 124.0(5) ?
O6 C3 C8 111.5(4) ?
O7 C4 O8 124.9(5) ?
O7 C4 C9 116.2(5) ?
O8 C4 C9 118.9(5) ?
C10 C5 C6 117.8(5) ?
C10 C5 C1 113.2(5) ?
C6 C5 C1 129.1(5) ?
C7 C6 C5 118.7(5) ?
C7 C6 C2 113.6(5) ?
C5 C6 C2 127.7(5) ?
C8 C7 C6 122.5(5) ?
C8 C7 H7A 118.7 ?
C6 C7 H7A 118.7 ?
C7 C8 C9 118.9(5) ?
C7 C8 C3 115.4(5) ?
C9 C8 C3 125.7(4) ?
C10 C9 C8 118.2(5) ?
C10 C9 C4 118.9(5) ?
C8 C9 C4 122.9(5) ?
C5 C10 C9 123.6(5) ?
C5 C10 H10A 118.2 ?
C9 C10 H10A 118.2 ?
O10 C11 O9 124.5(5) ?
O10 C11 C15 122.6(5) ?
O9 C11 C15 112.8(5) ?
O12 C12 O11 125.7(5) ?
O12 C12 C16 121.4(5) ?
O11 C12 C16 112.9(4) ?
O14 C13 O13 124.1(5) ?
O14 C13 C18 122.2(5) ?
O13 C13 C18 113.6(4) ?
O16 C14 O15 125.1(5) ?
O16 C14 C19 123.3(5) ?
O15 C14 C19 111.6(5) ?
C16 C15 C20 119.1(5) ?
C16 C15 C11 123.6(4) ?
C20 C15 C11 117.1(4) ?
C17 C16 C15 119.5(4) ?
C17 C16 C12 116.5(4) ?
C15 C16 C12 123.9(4) ?
C16 C17 C18 121.3(5) ?
C16 C17 H17A 119.4 ?
C18 C17 H17A 119.4 ?
C19 C18 C17 119.2(5) ?
C19 C18 C13 122.1(4) ?
C17 C18 C13 118.6(5) ?
C20 C19 C18 119.4(4) ?
C20 C19 C14 117.7(5) ?
C18 C19 C14 122.7(5) ?
C19 C20 C15 121.4(5) ?
C19 C20 H20A 119.3 ?
C15 C20 H20A 119.3 ?
N1 C21 C22 122.5(6) ?
N1 C21 H21A 118.7 ?
C22 C21 H21A 118.7 ?
C23 C22 C21 118.3(6) ?
C23 C22 H22A 120.9 ?
C21 C22 H22A 120.9 ?
C22 C23 C24 120.5(6) ?
C22 C23 H23A 119.7 ?
C24 C23 H23A 119.7 ?
C23 C24 C25 118.3(6) ?
C23 C24 H24A 120.9 ?
C25 C24 H24A 120.9 ?
N1 C25 C24 122.9(6) ?
N1 C25 C26 113.4(5) ?
C24 C25 C26 123.7(6) ?
N2 C26 C27 122.5(6) ?
N2 C26 C25 113.6(5) ?
C27 C26 C25 123.8(6) ?
C28 C27 C26 117.9(6) ?
C28 C27 H27A 121.0 ?
C26 C27 H27A 121.0 ?
C29 C28 C27 120.0(6) ?
C29 C28 H28A 120.0 ?
C27 C28 H28A 120.0 ?
C28 C29 C30 119.0(6) ?
C28 C29 H29A 120.5 ?
C30 C29 H29A 120.5 ?
N2 C30 C29 123.6(6) ?
N2 C30 H30A 118.2 ?
C29 C30 H30A 118.2 ?
N3 C31 C32 123.4(5) ?
N3 C31 H31A 118.3 ?
C32 C31 H31A 118.3 ?
C33 C32 C31 118.8(6) ?
C33 C32 H32A 120.6 ?
C31 C32 H32A 120.6 ?
C32 C33 C34 119.8(6) ?
C32 C33 H33A 120.1 ?
C34 C33 H33A 120.1 ?
C33 C34 C35 118.3(6) ?
C33 C34 H34A 120.8 ?
C35 C34 H34A 120.8 ?
N3 C35 C34 122.8(5) ?
N3 C35 C36 114.3(4) ?
C34 C35 C36 122.9(5) ?
N4 C36 C37 121.9(5) ?
N4 C36 C35 114.0(4) ?
C37 C36 C35 124.1(5) ?
C38 C37 C36 119.6(6) ?
C38 C37 H37A 120.2 ?
C36 C37 H37A 120.2 ?
C39 C38 C37 119.4(5) ?
C39 C38 H38A 120.3 ?
C37 C38 H38A 120.3 ?
C38 C39 C40 119.1(5) ?
C38 C39 H39A 120.5 ?
C40 C39 H39A 120.5 ?
N4 C40 C39 122.6(5) ?
N4 C40 H40A 118.7 ?
C39 C40 H40A 118.7 ?
N5 C41 C42 123.3(6) ?
N5 C41 H41A 118.4 ?
C42 C41 H41A 118.4 ?
C43 C42 C41 119.5(6) ?
C43 C42 H42A 120.2 ?
C41 C42 H42A 120.2 ?
C42 C43 C44 118.7(6) ?
C42 C43 H43A 120.7 ?
C44 C43 H43A 120.7 ?
C45 C44 C43 119.4(6) ?
C45 C44 H44A 120.3 ?
C43 C44 H44A 120.3 ?
N5 C45 C44 121.6(5) ?
N5 C45 C46 114.5(5) ?
C44 C45 C46 123.9(5) ?
N6 C46 C47 123.4(5) ?
N6 C46 C45 113.0(4) ?
C47 C46 C45 123.6(5) ?
C48 C47 C46 118.7(5) ?
C48 C47 H47A 120.7 ?
C46 C47 H47A 120.7 ?
C49 C48 C47 119.4(5) ?
C49 C48 H48A 120.3 ?
C47 C48 H48A 120.3 ?
C48 C49 C50 119.7(5) ?
C48 C49 H49A 120.1 ?
C50 C49 H49A 120.1 ?
N6 C50 C49 122.1(5) ?
N6 C50 H50A 119.0 ?
C49 C50 H50A 119.0 ?
H1WA O1W H1WB 105.3 ?
H2WA O2W H2WB 110.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 N1 1.961(4) y
Fe1 N2 1.966(4) y
Fe1 N3 1.967(4) y
Fe1 N4 1.971(4) y
Fe1 N5 1.964(4) y
Fe1 N6 1.961(4) y
N1 C21 1.343(7) ?
N1 C25 1.360(7) ?
N2 C30 1.328(7) ?
N2 C26 1.367(7) ?
N3 C31 1.341(6) ?
N3 C35 1.352(6) ?
N4 C40 1.349(6) ?
N4 C36 1.357(6) ?
N5 C41 1.328(6) ?
N5 C45 1.371(7) ?
N6 C50 1.356(6) ?
N6 C46 1.357(6) ?
O1 C1 1.217(7) ?
O2 C1 1.305(7) ?
O2 H2 0.8300 ?
O3 C2 1.261(7) ?
O4 C2 1.255(7) ?
O5 C3 1.214(6) ?
O6 C3 1.308(6) ?
O6 H6 0.8300 ?
O7 C4 1.257(6) ?
O8 C4 1.257(6) ?
O9 C11 1.322(6) ?
O9 H9 0.8300 ?
O10 C11 1.201(6) ?
O11 C12 1.302(6) ?
O11 H11 0.8300 ?
O12 C12 1.210(6) ?
O13 C13 1.305(6) ?
O13 H13 0.8300 ?
O14 C13 1.206(6) ?
O15 C14 1.313(6) ?
O15 H15 0.8300 ?
O16 C14 1.184(6) ?
C1 C5 1.506(8) ?
C2 C6 1.516(7) ?
C3 C8 1.503(7) ?
C4 C9 1.503(7) ?
C5 C10 1.382(7) ?
C5 C6 1.406(7) ?
C6 C7 1.393(7) ?
C7 C8 1.385(6) ?
C7 H7A 0.9400 ?
C8 C9 1.391(7) ?
C9 C10 1.389(7) ?
C10 H10A 0.9400 ?
C11 C15 1.497(7) ?
C12 C16 1.516(7) ?
C13 C18 1.501(7) ?
C14 C19 1.512(7) ?
C15 C16 1.389(7) ?
C15 C20 1.395(7) ?
C16 C17 1.389(7) ?
C17 C18 1.394(7) ?
C17 H17A 0.9400 ?
C18 C19 1.393(7) ?
C19 C20 1.384(7) ?
C20 H20A 0.9400 ?
C21 C22 1.398(8) ?
C21 H21A 0.9400 ?
C22 C23 1.367(9) ?
C22 H22A 0.9400 ?
C23 C24 1.371(9) ?
C23 H23A 0.9400 ?
C24 C25 1.379(8) ?
C24 H24A 0.9400 ?
C25 C26 1.480(8) ?
C26 C27 1.396(8) ?
C27 C28 1.380(9) ?
C27 H27A 0.9400 ?
C28 C29 1.355(9) ?
C28 H28A 0.9400 ?
C29 C30 1.386(8) ?
C29 H29A 0.9400 ?
C30 H30A 0.9400 ?
C31 C32 1.374(8) ?
C31 H31A 0.9400 ?
C32 C33 1.369(8) ?
C32 H32A 0.9400 ?
C33 C34 1.371(8) ?
C33 H33A 0.9400 ?
C34 C35 1.390(7) ?
C34 H34A 0.9400 ?
C35 C36 1.466(7) ?
C36 C37 1.386(7) ?
C37 C38 1.367(8) ?
C37 H37A 0.9400 ?
C38 C39 1.364(8) ?
C38 H38A 0.9400 ?
C39 C40 1.388(7) ?
C39 H39A 0.9400 ?
C40 H40A 0.9400 ?
C41 C42 1.390(8) ?
C41 H41A 0.9400 ?
C42 C43 1.358(8) ?
C42 H42A 0.9400 ?
C43 C44 1.389(8) ?
C43 H43A 0.9400 ?
C44 C45 1.388(7) ?
C44 H44A 0.9400 ?
C45 C46 1.479(7) ?
C46 C47 1.376(7) ?
C47 C48 1.372(7) ?
C47 H47A 0.9400 ?
C48 C49 1.365(8) ?
C48 H48A 0.9400 ?
C49 C50 1.386(7) ?
C49 H49A 0.9400 ?
C50 H50A 0.9400 ?
O1W H1WA 0.8872 ?
O1W H1WB 0.8050 ?
O2W H2WA 0.8201 ?
O2W H2WB 0.8202 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O2 H2 O3 . 0.83 1.66 2.431(6) 152.7
O6 H6 O4 2 0.83 1.77 2.555(5) 157.8
O9 H9 O1W . 0.83 1.88 2.643(5) 153.0
O11 H11 O7 . 0.83 1.68 2.495(5) 166.0
O13 H13 O8 3_675 0.83 1.84 2.567(5) 144.7
O15 H15 O14 3_685 0.83 1.90 2.732(5) 174.8
O1W H1WA O8 3_575 0.89 1.98 2.861(5) 169.2
O1W H1WB O10 3_575 0.81 2.04 2.844(5) 172.1
O2W H2WA O5 2_545 0.82 2.32 3.101(7) 158.6
O2W H2WB O3 . 0.82 2.03 2.803(6) 156.6
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
N6 Fe1 N1 C21 76.7(5)
N5 Fe1 N1 C21 -5.4(5)
N2 Fe1 N1 C21 171.8(5)
N3 Fe1 N1 C21 -99.5(5)
N6 Fe1 N1 C25 -104.8(4)
N5 Fe1 N1 C25 173.1(4)
N2 Fe1 N1 C25 -9.6(4)
N3 Fe1 N1 C25 79.0(4)
N1 Fe1 N2 C30 -173.1(5)
N6 Fe1 N2 C30 -82.9(5)
N3 Fe1 N2 C30 93.0(5)
N4 Fe1 N2 C30 11.5(5)
N1 Fe1 N2 C26 8.9(4)
N6 Fe1 N2 C26 99.1(4)
N3 Fe1 N2 C26 -84.9(4)
N4 Fe1 N2 C26 -166.5(4)
N1 Fe1 N3 C31 5.0(4)
N5 Fe1 N3 C31 -88.9(4)
N2 Fe1 N3 C31 86.6(4)
N4 Fe1 N3 C31 -178.8(5)
N1 Fe1 N3 C35 -176.1(4)
N5 Fe1 N3 C35 90.0(4)
N2 Fe1 N3 C35 -94.5(4)
N4 Fe1 N3 C35 0.1(4)
N6 Fe1 N4 C40 3.5(4)
N5 Fe1 N4 C40 85.6(4)
N2 Fe1 N4 C40 -92.1(4)
N3 Fe1 N4 C40 179.3(4)
N6 Fe1 N4 C36 -176.3(4)
N5 Fe1 N4 C36 -94.2(4)
N2 Fe1 N4 C36 88.1(4)
N3 Fe1 N4 C36 -0.5(4)
N1 Fe1 N5 C41 -89.7(5)
N6 Fe1 N5 C41 179.8(5)
N3 Fe1 N5 C41 4.3(5)
N4 Fe1 N5 C41 85.9(5)
N1 Fe1 N5 C45 88.8(4)
N6 Fe1 N5 C45 -1.7(3)
N3 Fe1 N5 C45 -177.3(4)
N4 Fe1 N5 C45 -95.6(4)
N1 Fe1 N6 C50 89.4(4)
N5 Fe1 N6 C50 -177.0(4)
N2 Fe1 N6 C50 7.7(4)
N4 Fe1 N6 C50 -87.1(4)
N1 Fe1 N6 C46 -93.8(4)
N5 Fe1 N6 C46 -0.2(3)
N2 Fe1 N6 C46 -175.5(3)
N4 Fe1 N6 C46 89.7(4)
O1 C1 C5 C10 19.5(9)
O2 C1 C5 C10 -160.1(5)
O1 C1 C5 C6 -161.3(6)
O2 C1 C5 C6 19.1(9)
C10 C5 C6 C7 3.9(8)
C1 C5 C6 C7 -175.3(5)
C10 C5 C6 C2 -176.9(5)
C1 C5 C6 C2 4.0(9)
O4 C2 C6 C7 -20.6(7)
O3 C2 C6 C7 158.9(5)
O4 C2 C6 C5 160.1(5)
O3 C2 C6 C5 -20.4(9)
C5 C6 C7 C8 -0.9(8)
C2 C6 C7 C8 179.8(5)
C6 C7 C8 C9 -4.0(8)
C6 C7 C8 C3 175.5(5)
O5 C3 C8 C7 79.2(7)
O6 C3 C8 C7 -92.9(5)
O5 C3 C8 C9 -101.3(7)
O6 C3 C8 C9 86.6(6)
C7 C8 C9 C10 5.6(7)
C3 C8 C9 C10 -173.9(5)
C7 C8 C9 C4 -175.8(5)
C3 C8 C9 C4 4.7(8)
O7 C4 C9 C10 -173.7(5)
O8 C4 C9 C10 3.8(7)
O7 C4 C9 C8 7.7(7)
O8 C4 C9 C8 -174.8(5)
C6 C5 C10 C9 -2.2(8)
C1 C5 C10 C9 177.0(5)
C8 C9 C10 C5 -2.6(8)
C4 C9 C10 C5 178.8(5)
O10 C11 C15 C16 -78.8(7)
O9 C11 C15 C16 104.8(6)
O10 C11 C15 C20 96.7(6)
O9 C11 C15 C20 -79.6(6)
C20 C15 C16 C17 -2.9(7)
C11 C15 C16 C17 172.5(5)
C20 C15 C16 C12 174.4(5)
C11 C15 C16 C12 -10.2(8)
O12 C12 C16 C17 2.1(7)
O11 C12 C16 C17 -178.8(4)
O12 C12 C16 C15 -175.3(5)
O11 C12 C16 C15 3.8(7)
C15 C16 C17 C18 1.4(7)
C12 C16 C17 C18 -176.1(5)
C16 C17 C18 C19 1.2(8)
C16 C17 C18 C13 -174.8(5)
O14 C13 C18 C19 -6.9(8)
O13 C13 C18 C19 175.8(5)
O14 C13 C18 C17 169.0(5)
O13 C13 C18 C17 -8.3(7)
C17 C18 C19 C20 -2.3(8)
C13 C18 C19 C20 173.6(5)
C17 C18 C19 C14 -178.6(5)
C13 C18 C19 C14 -2.7(8)
O16 C14 C19 C20 -79.0(7)
O15 C14 C19 C20 97.8(6)
O16 C14 C19 C18 97.4(7)
O15 C14 C19 C18 -85.8(6)
C18 C19 C20 C15 0.7(8)
C14 C19 C20 C15 177.3(5)
C16 C15 C20 C19 1.9(8)
C11 C15 C20 C19 -173.8(5)
C25 N1 C21 C22 -1.3(8)
Fe1 N1 C21 C22 177.2(4)
N1 C21 C22 C23 -2.9(9)
C21 C22 C23 C24 3.2(9)
C22 C23 C24 C25 0.5(9)
C21 N1 C25 C24 5.3(8)
Fe1 N1 C25 C24 -173.4(4)
C21 N1 C25 C26 -172.8(5)
Fe1 N1 C25 C26 8.5(6)
C23 C24 C25 N1 -5.0(9)
C23 C24 C25 C26 172.9(5)
C30 N2 C26 C27 -2.5(8)
Fe1 N2 C26 C27 175.7(5)
C30 N2 C26 C25 175.0(5)
Fe1 N2 C26 C25 -6.8(6)
N1 C25 C26 N2 -1.1(7)
C24 C25 C26 N2 -179.2(5)
N1 C25 C26 C27 176.4(5)
C24 C25 C26 C27 -1.7(9)
N2 C26 C27 C28 4.1(9)
C25 C26 C27 C28 -173.2(6)
C26 C27 C28 C29 -2.7(10)
C27 C28 C29 C30 -0.1(10)
C26 N2 C30 C29 -0.4(8)
Fe1 N2 C30 C29 -178.3(5)
C28 C29 C30 N2 1.7(10)
C35 N3 C31 C32 -0.6(8)
Fe1 N3 C31 C32 178.3(4)
N3 C31 C32 C33 0.8(9)
C31 C32 C33 C34 -0.4(9)
C32 C33 C34 C35 -0.2(9)
C31 N3 C35 C34 -0.1(8)
Fe1 N3 C35 C34 -179.1(4)
C31 N3 C35 C36 179.2(4)
Fe1 N3 C35 C36 0.2(6)
C33 C34 C35 N3 0.4(9)
C33 C34 C35 C36 -178.8(5)
C40 N4 C36 C37 0.8(7)
Fe1 N4 C36 C37 -179.3(4)
C40 N4 C36 C35 -179.1(4)
Fe1 N4 C36 C35 0.7(6)
N3 C35 C36 N4 -0.6(7)
C34 C35 C36 N4 178.7(5)
N3 C35 C36 C37 179.5(5)
C34 C35 C36 C37 -1.2(9)
N4 C36 C37 C38 0.2(8)
C35 C36 C37 C38 -179.9(5)
C36 C37 C38 C39 -1.0(9)
C37 C38 C39 C40 0.7(8)
C36 N4 C40 C39 -1.1(7)
Fe1 N4 C40 C39 179.1(4)
C38 C39 C40 N4 0.3(8)
C45 N5 C41 C42 -2.3(8)
Fe1 N5 C41 C42 176.1(4)
N5 C41 C42 C43 0.0(10)
C41 C42 C43 C44 2.1(10)
C42 C43 C44 C45 -1.9(9)
C41 N5 C45 C44 2.5(8)
Fe1 N5 C45 C44 -176.1(4)
C41 N5 C45 C46 -178.2(5)
Fe1 N5 C45 C46 3.2(5)
C43 C44 C45 N5 -0.5(8)
C43 C44 C45 C46 -179.7(5)
C50 N6 C46 C47 -0.2(7)
Fe1 N6 C46 C47 -177.3(4)
C50 N6 C46 C45 179.1(4)
Fe1 N6 C46 C45 2.0(5)
N5 C45 C46 N6 -3.4(6)
C44 C45 C46 N6 175.9(5)
N5 C45 C46 C47 175.9(5)
C44 C45 C46 C47 -4.8(8)
N6 C46 C47 C48 0.8(8)
C45 C46 C47 C48 -178.4(5)
C46 C47 C48 C49 -0.3(8)
C47 C48 C49 C50 -0.8(8)
C46 N6 C50 C49 -0.9(7)
Fe1 N6 C50 C49 175.8(4)
C48 C49 C50 N6 1.4(8)
