#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/15/4301574.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4301574
loop_
_publ_author_name
'Jinkui Tang'
'José Sánchez Costa'
'Simon Smulders'
'Gábor Molnár'
'Azzedine Bousseksou'
'Simon J. Teat'
'Yangguang Li'
'Gerard A. van Albada'
'Patrick Gamez'
'Jan Reedijk'
_publ_section_title
;
Two-Step Spin-Transition Iron(III) Compound with a Wide [High Spin-Low
Spin] Plateau
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2128
_journal_page_last               2135
_journal_paper_doi               10.1021/ic801973x
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C26.5 H27 Cl Fe N6 O9'
_chemical_formula_weight         664.84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.397(2)
_cell_angle_beta                 99.435(2)
_cell_angle_gamma                91.806(2)
_cell_formula_units_Z            4
_cell_length_a                   12.932(2)
_cell_length_b                   15.096(2)
_cell_length_c                   15.345(2)
_cell_measurement_reflns_used    4314
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.75
_cell_volume                     2938.7(7)
_computing_cell_refinement       'Bruker SAINT v7.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v7.34a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Advanced Light Source station 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26158
_diffrn_reflns_theta_full        26.85
_diffrn_reflns_theta_max         26.85
_diffrn_reflns_theta_min         2.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2004/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     807
_refine_ls_number_reflns         9670
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0984P)²+1.1922P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1463
_refine_ls_wR_factor_ref         0.1729
_reflns_number_gt                6108
_reflns_number_total             9670
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic801973x_si_002.cif
_cod_data_source_block           jsc363
_cod_original_formula_sum        'C26.50 H27 Cl Fe N6 O9'
_cod_database_code               4301574
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.11049(5) 0.38269(4) 0.80391(4) 0.0324(2) Uani 1 1 d . . .
O1 O 0.0753(2) 0.3748(2) 0.6757(2) 0.0350(8) Uani 1 1 d . . .
C1 C 0.1931(4) 0.4116(4) 1.0105(3) 0.0450(13) Uani 1 1 d . . .
H1A H 0.2152 0.3522 1.0045 0.054 Uiso 1 1 calc R . .
N1 N 0.1385(3) 0.4450(3) 0.9378(3) 0.0396(10) Uani 1 1 d . . .
O2 O 0.0339(3) 0.2992(2) 0.5138(2) 0.0421(8) Uani 1 1 d . . .
C2 C 0.2172(4) 0.4601(4) 1.0918(4) 0.0520(14) Uani 1 1 d . . .
H2A H 0.2561 0.4352 1.1409 0.062 Uiso 1 1 calc R . .
N2 N 0.0473(3) 0.5589(3) 0.8772(3) 0.0411(11) Uani 1 1 d . . .
H2N H 0.027(4) 0.611(4) 0.878(4) 0.051(17) Uiso 1 1 d . . .
N3 N 0.0313(3) 0.5046(3) 0.7992(3) 0.0374(9) Uani 1 1 d . . .
C3 C 0.1838(5) 0.5465(4) 1.1012(4) 0.0541(15) Uani 1 1 d . . .
H3A H 0.2005 0.5813 1.1569 0.065 Uiso 1 1 calc R . .
C4 C 0.1272(4) 0.5816(4) 1.0307(4) 0.0473(13) Uani 1 1 d . . .
H4A H 0.1034 0.6405 1.0366 0.057 Uiso 1 1 calc R . .
C5 C 0.1051(4) 0.5283(3) 0.9494(3) 0.0371(11) Uani 1 1 d . . .
C6 C -0.0327(4) 0.5308(3) 0.7336(3) 0.0368(11) Uani 1 1 d . . .
H6A H -0.0670 0.5846 0.7438 0.044 Uiso 1 1 calc R . .
C7 C -0.0550(4) 0.4838(3) 0.6464(3) 0.0344(11) Uani 1 1 d . . .
C8 C -0.1341(4) 0.5156(3) 0.5832(3) 0.0387(12) Uani 1 1 d . . .
H8A H -0.1716 0.5657 0.6002 0.046 Uiso 1 1 calc R . .
C9 C -0.1574(4) 0.4756(3) 0.4984(3) 0.0419(12) Uani 1 1 d . . .
H9A H -0.2104 0.4980 0.4569 0.050 Uiso 1 1 calc R . .
C10 C -0.1032(4) 0.4016(3) 0.4726(3) 0.0371(11) Uani 1 1 d . . .
H10A H -0.1201 0.3731 0.4138 0.045 Uiso 1 1 calc R . .
C11 C -0.0256(4) 0.3703(3) 0.5323(3) 0.0353(11) Uani 1 1 d . . .
C12 C -0.0001(3) 0.4088(3) 0.6210(3) 0.0328(11) Uani 1 1 d . . .
C13 C 0.0109(5) 0.2523(4) 0.4272(4) 0.0609(17) Uani 1 1 d . . .
H13A H -0.0626 0.2302 0.4154 0.091 Uiso 1 1 calc R . .
H13B H 0.0566 0.2019 0.4238 0.091 Uiso 1 1 calc R . .
H13C H 0.0231 0.2925 0.3830 0.091 Uiso 1 1 calc R . .
O3 O 0.0042(2) 0.3012(2) 0.8218(2) 0.0375(8) Uani 1 1 d . . .
O4 O -0.1815(3) 0.2424(2) 0.8465(2) 0.0450(9) Uani 1 1 d . . .
N4 N 0.2666(3) 0.4346(3) 0.8005(3) 0.0349(9) Uani 1 1 d . . .
N5 N 0.3177(3) 0.2985(3) 0.8428(3) 0.0432(11) Uani 1 1 d . . .
H5N H 0.362(4) 0.263(4) 0.861(4) 0.050(17) Uiso 1 1 d . . .
N6 N 0.2126(3) 0.2773(3) 0.8368(3) 0.0352(9) Uani 1 1 d . . .
C14 C 0.2916(4) 0.5194(3) 0.7853(3) 0.0440(12) Uani 1 1 d . . .
H14A H 0.2360 0.5568 0.7672 0.053 Uiso 1 1 calc R . .
C15 C 0.3910(4) 0.5531(4) 0.7947(4) 0.0521(14) Uani 1 1 d . . .
H15A H 0.4051 0.6127 0.7835 0.063 Uiso 1 1 calc R . .
C16 C 0.4731(4) 0.4980(4) 0.8214(4) 0.0536(15) Uani 1 1 d . . .
H16A H 0.5439 0.5200 0.8281 0.064 Uiso 1 1 calc R . .
C17 C 0.4511(4) 0.4122(4) 0.8379(4) 0.0498(14) Uani 1 1 d . . .
H17A H 0.5059 0.3740 0.8563 0.060 Uiso 1 1 calc R . .
C18 C 0.3461(4) 0.3826(3) 0.8270(3) 0.0385(12) Uani 1 1 d . . .
C19 C 0.1880(4) 0.1978(3) 0.8566(3) 0.0397(12) Uani 1 1 d . . .
H19A H 0.2432 0.1585 0.8690 0.048 Uiso 1 1 calc R . .
C20 C 0.0842(4) 0.1659(3) 0.8608(3) 0.0393(12) Uani 1 1 d . . .
C21 C 0.0701(5) 0.0788(4) 0.8840(4) 0.0561(15) Uani 1 1 d . . .
H21A H 0.1288 0.0426 0.8939 0.067 Uiso 1 1 calc R . .
C22 C -0.0268(5) 0.0455(4) 0.8925(4) 0.0639(17) Uani 1 1 d . . .
H22A H -0.0353 -0.0142 0.9059 0.077 Uiso 1 1 calc R . .
C23 C -0.1135(5) 0.0986(4) 0.8817(4) 0.0544(15) Uani 1 1 d . . .
H23A H -0.1802 0.0759 0.8898 0.065 Uiso 1 1 calc R . .
C24 C -0.1016(4) 0.1849(3) 0.8590(3) 0.0412(12) Uani 1 1 d . . .
C25 C -0.0038(4) 0.2199(3) 0.8463(3) 0.0357(11) Uani 1 1 d . . .
C26 C -0.2781(4) 0.2170(4) 0.8727(4) 0.0543(15) Uani 1 1 d . . .
H26A H -0.3057 0.1603 0.8394 0.081 Uiso 1 1 calc R . .
H26B H -0.3287 0.2630 0.8601 0.081 Uiso 1 1 calc R . .
H26C H -0.2661 0.2104 0.9364 0.081 Uiso 1 1 calc R . .
Fe2 Fe 0.37977(5) 0.12032(4) 0.67305(4) 0.0310(2) Uani 1 1 d . . .
O5 O 0.4066(2) 0.1234(2) 0.8005(2) 0.0343(7) Uani 1 1 d . . .
O6 O 0.4573(3) 0.2027(2) 0.9612(2) 0.0446(9) Uani 1 1 d . . .
N7 N 0.3547(3) 0.0623(3) 0.5362(3) 0.0350(9) Uani 1 1 d . . .
N8 N 0.4248(3) -0.0600(3) 0.5978(3) 0.0412(11) Uani 1 1 d . . .
H8N H 0.447(4) -0.109(4) 0.594(3) 0.044(16) Uiso 1 1 d . . .
N9 N 0.4456(3) -0.0064(3) 0.6764(3) 0.0348(9) Uani 1 1 d . . .
C27 C 0.3099(4) 0.1002(3) 0.4633(3) 0.0392(12) Uani 1 1 d . . .
H27A H 0.2945 0.1613 0.4700 0.047 Uiso 1 1 calc R . .
C28 C 0.2856(4) 0.0546(4) 0.3805(3) 0.0465(13) Uani 1 1 d . . .
H28A H 0.2538 0.0833 0.3311 0.056 Uiso 1 1 calc R . .
C29 C 0.3087(4) -0.0349(4) 0.3707(4) 0.0484(13) Uani 1 1 d . . .
H29A H 0.2920 -0.0681 0.3141 0.058 Uiso 1 1 calc R . .
C30 C 0.3554(4) -0.0752(3) 0.4422(3) 0.0433(13) Uani 1 1 d . . .
H30A H 0.3722 -0.1361 0.4362 0.052 Uiso 1 1 calc R . .
C31 C 0.3778(4) -0.0237(3) 0.5251(3) 0.0364(11) Uani 1 1 d . . .
C32 C 0.5059(4) -0.0369(3) 0.7424(3) 0.0389(12) Uani 1 1 d . . .
H32A H 0.5341 -0.0936 0.7328 0.047 Uiso 1 1 calc R . .
C33 C 0.5316(3) 0.0106(3) 0.8286(3) 0.0345(11) Uani 1 1 d . . .
C34 C 0.6114(4) -0.0230(3) 0.8903(4) 0.0418(12) Uani 1 1 d . . .
H34A H 0.6457 -0.0748 0.8728 0.050 Uiso 1 1 calc R . .
C35 C 0.6394(4) 0.0181(4) 0.9744(4) 0.0472(13) Uani 1 1 d . . .
H35A H 0.6931 -0.0050 1.0147 0.057 Uiso 1 1 calc R . .
C36 C 0.5890(4) 0.0945(3) 1.0015(3) 0.0405(12) Uani 1 1 d . . .
H36A H 0.6080 0.1230 1.0601 0.049 Uiso 1 1 calc R . .
C37 C 0.5118(4) 0.1276(3) 0.9420(3) 0.0379(11) Uani 1 1 d . . .
C38 C 0.4814(3) 0.0873(3) 0.8547(3) 0.0328(11) Uani 1 1 d . . .
C39 C 0.4862(5) 0.2510(4) 1.0481(4) 0.0571(15) Uani 1 1 d . . .
H39A H 0.4675 0.2144 1.0932 0.086 Uiso 1 1 calc R . .
H39B H 0.4486 0.3064 1.0503 0.086 Uiso 1 1 calc R . .
H39C H 0.5619 0.2652 1.0598 0.086 Uiso 1 1 calc R . .
O7 O 0.4936(2) 0.1987(2) 0.6661(2) 0.0361(8) Uani 1 1 d . . .
O8 O 0.6874(2) 0.2588(2) 0.6709(2) 0.0423(8) Uani 1 1 d . . .
N10 N 0.2204(3) 0.0743(3) 0.6724(3) 0.0336(9) Uani 1 1 d . . .
N11 N 0.1799(3) 0.2086(3) 0.6221(3) 0.0415(11) Uani 1 1 d . . .
H11N H 0.146(4) 0.244(3) 0.612(3) 0.028(14) Uiso 1 1 d . . .
N12 N 0.2857(3) 0.2280(3) 0.6345(3) 0.0346(9) Uani 1 1 d . . .
C40 C 0.1894(4) -0.0068(3) 0.6947(3) 0.0403(12) Uani 1 1 d . . .
H40A H 0.2415 -0.0457 0.7170 0.048 Uiso 1 1 calc R . .
C41 C 0.0863(4) -0.0339(4) 0.6858(4) 0.0495(14) Uani 1 1 d . . .
H41A H 0.0670 -0.0907 0.7018 0.059 Uiso 1 1 calc R . .
C42 C 0.0101(4) 0.0227(4) 0.6531(4) 0.0552(15) Uani 1 1 d . . .
H42A H -0.0620 0.0044 0.6458 0.066 Uiso 1 1 calc R . .
C43 C 0.0387(4) 0.1051(4) 0.6314(4) 0.0477(13) Uani 1 1 d . . .
H43A H -0.0125 0.1453 0.6103 0.057 Uiso 1 1 calc R . .
C44 C 0.1458(4) 0.1277(3) 0.6415(3) 0.0367(11) Uani 1 1 d . . .
C45 C 0.3162(4) 0.3058(3) 0.6150(3) 0.0365(11) Uani 1 1 d . . .
H45A H 0.2635 0.3453 0.5955 0.044 Uiso 1 1 calc R . .
C46 C 0.4228(4) 0.3357(3) 0.6210(3) 0.0366(11) Uani 1 1 d . . .
C47 C 0.4444(4) 0.4235(3) 0.6014(4) 0.0471(13) Uani 1 1 d . . .
H47A H 0.3876 0.4598 0.5835 0.057 Uiso 1 1 calc R . .
C48 C 0.5445(5) 0.4572(4) 0.6074(4) 0.0529(14) Uani 1 1 d . . .
H48A H 0.5572 0.5163 0.5941 0.064 Uiso 1 1 calc R . .
C49 C 0.6288(4) 0.4037(3) 0.6335(4) 0.0469(13) Uani 1 1 d . . .
H49A H 0.6988 0.4276 0.6397 0.056 Uiso 1 1 calc R . .
C50 C 0.6108(4) 0.3169(3) 0.6500(3) 0.0369(11) Uani 1 1 d . . .
C51 C 0.5077(4) 0.2817(3) 0.6468(3) 0.0359(11) Uani 1 1 d . . .
C52 C 0.7904(4) 0.2829(4) 0.6553(4) 0.0480(13) Uani 1 1 d . . .
H52A H 0.7863 0.2977 0.5941 0.072 Uiso 1 1 calc R . .
H52B H 0.8359 0.2328 0.6648 0.072 Uiso 1 1 calc R . .
H52C H 0.8193 0.3347 0.6964 0.072 Uiso 1 1 calc R . .
Cl1 Cl 0.79097(13) 0.23410(10) 1.18227(10) 0.0603(4) Uani 1 1 d D . .
O11 O 0.7578(3) 0.2841(3) 1.1092(3) 0.0664(12) Uani 1 1 d D . .
O12 O 0.7033(4) 0.1923(3) 1.2109(3) 0.0827(14) Uani 1 1 d D . .
O13 O 0.8499(4) 0.2920(3) 1.2521(3) 0.1004(18) Uani 1 1 d D . .
O14 O 0.8569(4) 0.1651(3) 1.1541(4) 0.0976(17) Uani 1 1 d D . .
Cl2 Cl -0.30289(14) 0.70863(11) 0.70859(16) 0.0861(6) Uani 1 1 d DU . .
O21 O -0.3388(5) 0.6992(4) 0.6120(4) 0.1067(19) Uani 1 1 d DU A .
O22 O -0.3732(8) 0.6511(7) 0.7524(7) 0.094(3) Uiso 0.50 1 d PDU A 1
O23 O -0.2010(7) 0.6886(7) 0.7469(7) 0.093(3) Uiso 0.50 1 d PDU A 1
O24 O -0.3189(9) 0.7972(6) 0.7540(7) 0.082(3) Uiso 0.50 1 d PDU A 1
O22' O -0.2881(8) 0.6202(6) 0.7275(6) 0.080(3) Uiso 0.50 1 d PDU A 2
O23' O -0.1964(8) 0.7440(8) 0.6991(9) 0.119(4) Uiso 0.50 1 d PDU A 2
O24' O -0.3653(8) 0.7658(7) 0.7418(6) 0.076(3) Uiso 0.50 1 d PDU A 2
O1S O 0.4589(3) -0.2366(3) 0.5698(3) 0.0615(11) Uani 1 1 d . . .
H1S H 0.5199 -0.2550 0.5804 0.092 Uiso 1 1 calc R . .
C1S C 0.3870(6) -0.2966(5) 0.5994(5) 0.085(2) Uani 1 1 d . . .
H1S1 H 0.4182 -0.3145 0.6573 0.128 Uiso 1 1 calc R . .
H1S2 H 0.3718 -0.3494 0.5563 0.128 Uiso 1 1 calc R . .
H1S3 H 0.3217 -0.2669 0.6047 0.128 Uiso 1 1 calc R . .
O1W O -0.0236(4) 0.7331(3) 0.8999(4) 0.0656(15) Uani 0.80 1 d P B 1
O1W' O -0.0918(18) 0.7836(15) 0.8951(15) 0.071(6) Uiso 0.20 1 d P C 2
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
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N 0.0061 0.0033
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
O O 0.0106 0.0060
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Cl Cl 0.1484 0.1585
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Fe Fe 0.3463 0.8444
'WCROMER Program in WinGX L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
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
O1 Fe1 N1 157.35(15) . . ?
O1 Fe1 N3 84.22(14) . . ?
O1 Fe1 O3 96.90(14) . . ?
O1 Fe1 N4 91.34(14) . . ?
O1 Fe1 N6 107.47(14) . . ?
N1 Fe1 N3 74.57(15) . . ?
N1 Fe1 O3 95.33(15) . . ?
N1 Fe1 N4 84.19(15) . . ?
N1 Fe1 N6 92.68(15) . . ?
N3 Fe1 O3 102.36(14) . . ?
N3 Fe1 N4 98.56(15) . . ?
N3 Fe1 N6 166.07(15) . . ?
O3 Fe1 N4 158.16(14) . . ?
O3 Fe1 N6 84.09(14) . . ?
N4 Fe1 N6 74.14(15) . . ?
Fe1 O1 C12 132.8(3) . . ?
N1 C1 C2 122.7(5) . . ?
Fe1 N1 C1 126.7(3) . . ?
Fe1 N1 C5 116.0(3) . . ?
C1 N1 C5 117.2(4) . . ?
C11 O2 C13 117.9(4) . . ?
C1 C2 C3 118.8(5) . . ?
N3 N2 C5 117.8(4) . . ?
Fe1 N3 N2 114.8(3) . . ?
Fe1 N3 C6 128.2(3) . . ?
N2 N3 C6 116.9(4) . . ?
C2 C3 C4 120.3(5) . . ?
C3 C4 C5 118.0(5) . . ?
N1 C5 N2 116.2(4) . . ?
N1 C5 C4 123.0(5) . . ?
N2 C5 C4 120.8(5) . . ?
N3 C6 C7 124.1(4) . . ?
C6 C7 C8 118.1(4) . . ?
C6 C7 C12 122.7(4) . . ?
C8 C7 C12 119.2(5) . . ?
C7 C8 C9 121.2(4) . . ?
C8 C9 C10 120.0(4) . . ?
C9 C10 C11 119.8(5) . . ?
O2 C11 C10 124.8(4) . . ?
O2 C11 C12 113.1(4) . . ?
C10 C11 C12 122.1(4) . . ?
O1 C12 C7 123.2(4) . . ?
O1 C12 C11 119.1(4) . . ?
C7 C12 C11 117.7(4) . . ?
Fe1 O3 C25 138.3(3) . . ?
C24 O4 C26 117.1(4) . . ?
Fe1 N4 C14 125.0(3) . . ?
Fe1 N4 C18 116.7(3) . . ?
C14 N4 C18 117.6(4) . . ?
N6 N5 C18 117.7(4) . . ?
Fe1 N6 N5 115.2(3) . . ?
Fe1 N6 C19 128.3(3) . . ?
N5 N6 C19 116.3(4) . . ?
N4 C14 C15 123.5(5) . . ?
C14 C15 C16 118.4(5) . . ?
C15 C16 C17 119.9(5) . . ?
C16 C17 C18 118.1(5) . . ?
N4 C18 N5 115.8(4) . . ?
N4 C18 C17 122.5(5) . . ?
N5 C18 C17 121.7(5) . . ?
N6 C19 C20 124.7(4) . . ?
C19 C20 C21 118.2(5) . . ?
C19 C20 C25 122.4(4) . . ?
C21 C20 C25 119.4(5) . . ?
C20 C21 C22 121.0(5) . . ?
C21 C22 C23 120.5(5) . . ?
C22 C23 C24 119.6(5) . . ?
O4 C24 C23 124.3(5) . . ?
O4 C24 C25 114.3(4) . . ?
C23 C24 C25 121.3(5) . . ?
O3 C25 C20 122.1(4) . . ?
O3 C25 C24 119.8(4) . . ?
C20 C25 C24 118.1(5) . . ?
O5 Fe2 N7 157.56(14) . . ?
O5 Fe2 N9 84.34(14) . . ?
O5 Fe2 O7 95.43(14) . . ?
O5 Fe2 N10 89.54(14) . . ?
O5 Fe2 N12 109.86(14) . . ?
N7 Fe2 N9 74.61(15) . . ?
N7 Fe2 O7 97.17(15) . . ?
N7 Fe2 N10 85.27(15) . . ?
N7 Fe2 N12 89.77(14) . . ?
N9 Fe2 O7 104.25(14) . . ?
N9 Fe2 N10 96.45(15) . . ?
N9 Fe2 N12 162.71(15) . . ?
O7 Fe2 N10 159.07(14) . . ?
O7 Fe2 N12 84.70(14) . . ?
N10 Fe2 N12 74.51(15) . . ?
Fe2 O5 C38 130.9(3) . . ?
C37 O6 C39 117.8(4) . . ?
Fe2 N7 C27 127.5(3) . . ?
Fe2 N7 C31 114.7(3) . . ?
C27 N7 C31 117.5(4) . . ?
N9 N8 C31 117.7(4) . . ?
Fe2 N9 N8 114.9(3) . . ?
Fe2 N9 C32 127.7(3) . . ?
N8 N9 C32 117.3(4) . . ?
N7 C27 C28 123.3(5) . . ?
C27 C28 C29 118.3(5) . . ?
C28 C29 C30 120.3(5) . . ?
C29 C30 C31 117.9(5) . . ?
N7 C31 N8 117.0(4) . . ?
N7 C31 C30 122.7(5) . . ?
N8 C31 C30 120.4(4) . . ?
N9 C32 C33 123.3(4) . . ?
C32 C33 C34 117.6(4) . . ?
C32 C33 C38 123.2(4) . . ?
C34 C33 C38 119.3(5) . . ?
C33 C34 C35 121.0(5) . . ?
C34 C35 C36 120.2(5) . . ?
C35 C36 C37 119.2(5) . . ?
O6 C37 C36 124.2(5) . . ?
O6 C37 C38 113.7(4) . . ?
C36 C37 C38 122.1(5) . . ?
O5 C38 C33 122.9(4) . . ?
O5 C38 C37 118.9(4) . . ?
C33 C38 C37 118.2(4) . . ?
Fe2 O7 C51 137.4(3) . . ?
C50 O8 C52 117.0(4) . . ?
Fe2 N10 C40 125.8(3) . . ?
Fe2 N10 C44 116.4(3) . . ?
C40 N10 C44 117.7(4) . . ?
N12 N11 C44 118.4(4) . . ?
Fe2 N12 N11 114.3(3) . . ?
Fe2 N12 C45 128.3(3) . . ?
N11 N12 C45 117.1(4) . . ?
N10 C40 C41 122.3(5) . . ?
C40 C41 C42 118.9(5) . . ?
C41 C42 C43 120.2(5) . . ?
C42 C43 C44 117.5(5) . . ?
N10 C44 N11 115.8(4) . . ?
N10 C44 C43 123.4(5) . . ?
N11 C44 C43 120.7(4) . . ?
N12 C45 C46 124.6(4) . . ?
C45 C46 C47 118.5(4) . . ?
C45 C46 C51 122.6(4) . . ?
C47 C46 C51 118.9(5) . . ?
C46 C47 C48 121.7(5) . . ?
C47 C48 C49 119.4(5) . . ?
C48 C49 C50 120.5(5) . . ?
O8 C50 C49 124.6(5) . . ?
O8 C50 C51 114.7(4) . . ?
C49 C50 C51 120.7(5) . . ?
O7 C51 C46 122.3(4) . . ?
O7 C51 C50 119.0(4) . . ?
C46 C51 C50 118.6(4) . . ?
O11 Cl1 O12 111.3(3) . . ?
O11 Cl1 O13 108.6(3) . . ?
O11 Cl1 O14 108.5(3) . . ?
O12 Cl1 O13 111.0(3) . . ?
O12 Cl1 O14 108.1(3) . . ?
O13 Cl1 O14 109.3(4) . . ?
O21 Cl2 O22 109.6(5) . . ?
O21 Cl2 O23 122.4(5) . . ?
O21 Cl2 O24 114.6(5) . . ?
O21 Cl2 O22' 102.9(5) . . ?
O21 Cl2 O23' 92.3(6) . . ?
O21 Cl2 O24' 105.6(5) . . ?
O22 Cl2 O23 103.7(6) . . ?
O22 Cl2 O24 99.6(6) . . ?
O22 Cl2 O22' 53.1(5) . . ?
O22 Cl2 O23' 150.9(7) . . ?
O22 Cl2 O24' 76.1(6) . . ?
O23 Cl2 O24 104.1(6) . . ?
O23 Cl2 O22' 63.4(6) . . ?
O23 Cl2 O23' 47.4(6) . . ?
O23 Cl2 O24' 127.5(7) . . ?
O24 Cl2 O22' 140.0(6) . . ?
O24 Cl2 O23' 87.6(7) . . ?
O24 Cl2 O24' 29.9(5) . . ?
O22' Cl2 O23' 104.6(6) . . ?
O22' Cl2 O24' 127.6(6) . . ?
O23' Cl2 O24' 116.9(7) . . ?
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 O1 1.936(3) . ?
Fe1 N1 2.147(4) . ?
Fe1 N3 2.135(4) . ?
Fe1 O3 1.887(3) . ?
Fe1 N4 2.153(4) . ?
Fe1 N6 2.144(4) . ?
O1 C12 1.328(5) . ?
C1 N1 1.367(6) . ?
C1 C2 1.369(7) . ?
N1 C5 1.348(6) . ?
O2 C11 1.375(5) . ?
O2 C13 1.427(6) . ?
C2 C3 1.389(8) . ?
N2 N3 1.369(5) . ?
N2 C5 1.359(6) . ?
N3 C6 1.295(6) . ?
C3 C4 1.363(8) . ?
C4 C5 1.402(7) . ?
C6 C7 1.434(7) . ?
C7 C8 1.419(6) . ?
C7 C12 1.413(6) . ?
C8 C9 1.364(7) . ?
C9 C10 1.397(7) . ?
C10 C11 1.372(6) . ?
C11 C12 1.411(7) . ?
O3 C25 1.322(6) . ?
O4 C24 1.372(6) . ?
O4 C26 1.425(6) . ?
N4 C14 1.361(6) . ?
N4 C18 1.347(6) . ?
N5 N6 1.372(6) . ?
N5 C18 1.365(7) . ?
N6 C19 1.308(6) . ?
C14 C15 1.348(7) . ?
C15 C16 1.400(8) . ?
C16 C17 1.374(8) . ?
C17 C18 1.394(7) . ?
C19 C20 1.425(7) . ?
C20 C21 1.409(7) . ?
C20 C25 1.421(7) . ?
C21 C22 1.366(8) . ?
C22 C23 1.395(8) . ?
C23 C24 1.390(7) . ?
C24 C25 1.406(7) . ?
Fe2 O5 1.926(3) . ?
Fe2 N7 2.166(4) . ?
Fe2 N9 2.119(4) . ?
Fe2 O7 1.882(3) . ?
Fe2 N10 2.152(4) . ?
Fe2 N12 2.130(4) . ?
O5 C38 1.333(5) . ?
O6 C37 1.386(6) . ?
O6 C39 1.444(6) . ?
N7 C27 1.358(6) . ?
N7 C31 1.344(6) . ?
N8 N9 1.370(6) . ?
N8 C31 1.352(6) . ?
N9 C32 1.304(6) . ?
C27 C28 1.370(7) . ?
C28 C29 1.393(7) . ?
C29 C30 1.368(7) . ?
C30 C31 1.409(7) . ?
C32 C33 1.426(7) . ?
C33 C34 1.422(6) . ?
C33 C38 1.403(6) . ?
C34 C35 1.365(7) . ?
C35 C36 1.405(7) . ?
C36 C37 1.378(7) . ?
C37 C38 1.406(7) . ?
O7 C51 1.328(5) . ?
O8 C50 1.362(6) . ?
O8 C52 1.433(6) . ?
N10 C40 1.368(6) . ?
N10 C44 1.332(6) . ?
N11 N12 1.369(6) . ?
N11 C44 1.360(6) . ?
N12 C45 1.304(6) . ?
C40 C41 1.364(7) . ?
C41 C42 1.387(8) . ?
C42 C43 1.373(8) . ?
C43 C44 1.397(7) . ?
C45 C46 1.423(7) . ?
C46 C47 1.415(7) . ?
C46 C51 1.415(6) . ?
C47 C48 1.361(8) . ?
C48 C49 1.405(7) . ?
C49 C50 1.379(7) . ?
C50 C51 1.411(7) . ?
Cl1 O11 1.426(4) . ?
Cl1 O12 1.431(5) . ?
Cl1 O13 1.416(4) . ?
Cl1 O14 1.446(5) . ?
Cl2 O21 1.470(6) . ?
Cl2 O22 1.515(9) . ?
Cl2 O23 1.406(9) . ?
Cl2 O24 1.485(9) . ?
Cl2 O22' 1.404(8) . ?
Cl2 O23' 1.496(10) . ?
Cl2 O24' 1.324(8) . ?
O1S C1S 1.433(7) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S O21 0.84 1.98 2.815(7) 176.5 1_645
O1S H1S O24' 0.84 2.66 3.185(11) 122.2 1_645
O1S H1S Cl2 0.84 2.87 3.612(4) 148.6 1_645
N5 H5N O6 0.83(6) 2.10(6) 2.870(6) 154(5) .
N5 H5N O5 0.83(6) 2.35(6) 2.975(5) 132(5) .
N11 H11N O2 0.71(5) 2.16(5) 2.786(5) 147(5) .
N11 H11N O1 0.71(5) 2.40(5) 2.999(5) 143(5) .
N8 H8N O1S 0.80(5) 1.94(5) 2.721(6) 164(5) .
N2 H2N O1W 0.84(5) 1.99(6) 2.821(6) 170(5) .
