# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013
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# CCDC
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#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
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# fide research purposes only. It may contain copyright material
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data_msb424_0m
#TrackingRef 'MSB-128 compound 12.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Bis{\h^5^-[bis(2-methoxy-4-(3-propenyl)(dichloro(\h^6^-
(4-(2-propyl)toluene)ruthenium(II)phosphino]cylopentadienyl}
iron(II)
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C70 H80 Cl4 Fe O8 P2 Ru2'
_chemical_formula_sum 'C70 H80 Cl4 Fe O8 P2 Ru2'
_chemical_formula_weight 1511.07
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 13.320(3)
_cell_length_b 14.572(3)
_cell_length_c 19.016(4)
_cell_angle_alpha 78.967(3)
_cell_angle_beta 86.074(3)
_cell_angle_gamma 84.913(3)
_cell_volume 3603.6(12)
_cell_formula_units_Z 2
_cell_measurement_temperature 195(2)
_cell_measurement_reflns_used 4626
_cell_measurement_theta_min 2.35
_cell_measurement_theta_max 26.79
_exptl_crystal_description Slab
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.17
_exptl_crystal_size_mid 0.16
_exptl_crystal_size_min 0.07
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.393
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1552
_exptl_absorpt_coefficient_mu 0.856
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.6956
_exptl_absorpt_correction_T_max 0.9425
_exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008a)'
_exptl_special_details
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5 deg. in omega, colllected at phi = 0.00,
90.00 and 180.00 deg. and 2 sets of 800 frames, each of
width 0.45 deg in phi, collected at omega = -30.00 and 210.00
deg. The scan time was 20 sec/frame. From 3410 reflections
chosen from the final data set and having I/sigma(I) > 15 as
well as being well-formed it was determined that the crystal
contained several components with two dominating (CELL_NOW (
Sheldrick 2008b)). These two could be indexed on the basis of
a triclinic cell related by a rotation of 180 deg. about the
(0 1 -1) axis. The raw data were processed using the
multi-component version of SAINT and the 2-component control
file generated by CELL_NOW.
;
_diffrn_ambient_temperature 195(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX-I CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 70854
_diffrn_reflns_av_R_equivalents 0.1013
_diffrn_reflns_av_sigmaI/netI 0.0906
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 2.18
_diffrn_reflns_theta_max 26.87
_reflns_number_total 15313
_reflns_number_gt 10241
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)'
_computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms were placed in
calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding
contributions with isotropic displacement parameters 1.2 - 1.5 times those
of the attached carbon atoms. The 3-propenyl substituents all show evidence
for positional disorder, at least in part because of the centrosymmetry
imposed on the two independent molecules. For two of these, alternate
locatons could be discerned and these were refined subject to constraints
that they approximate ideal geometry.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+5.9787P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 15313
_refine_ls_number_parameters 813
_refine_ls_number_restraints 78
_refine_ls_R_factor_all 0.1048
_refine_ls_R_factor_gt 0.0614
_refine_ls_wR_factor_ref 0.1801
_refine_ls_wR_factor_gt 0.1527
_refine_ls_goodness_of_fit_ref 1.030
_refine_ls_restrained_S_all 1.029
_refine_ls_shift/su_max 0.006
_refine_ls_shift/su_mean 0.000
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
Ru1 Ru 0.16506(6) 0.37825(6) 0.06508(4) 0.0290(2) Uani 1 1 d . . .
Fe1 Fe 0.5000 0.5000 0.0000 0.0259(4) Uani 1 2 d S . .
Cl1 Cl 0.21036(18) 0.46554(19) -0.05155(13) 0.0386(6) Uani 1 1 d . . .
Cl2 Cl 0.18933(18) 0.51652(19) 0.10939(14) 0.0394(6) Uani 1 1 d . . .
P1 P 0.33268(17) 0.32764(17) 0.07966(13) 0.0255(5) Uani 1 1 d . . .
O1 O 0.3440(5) 0.2193(4) 0.0679(3) 0.0337(16) Uani 1 1 d . . .
O2 O 0.4085(5) 0.2008(5) -0.0649(4) 0.0492(18) Uani 1 1 d . A .
O3 O 0.3782(4) 0.3215(5) 0.1579(3) 0.0333(17) Uani 1 1 d . . .
O4 O 0.3212(5) 0.1594(5) 0.2386(4) 0.0368(17) Uani 1 1 d . . .
C1 C 0.4370(7) 0.1703(7) 0.0567(5) 0.031(2) Uani 1 1 d . A .
C2 C 0.4937(7) 0.1282(7) 0.1142(5) 0.038(2) Uani 1 1 d . . .
H2 H 0.4711 0.1341 0.1617 0.045 Uiso 1 1 calc R . .
C3 C 0.5832(7) 0.0776(7) 0.1017(6) 0.045(3) Uani 1 1 d . A .
H3 H 0.6237 0.0517 0.1410 0.054 Uiso 1 1 calc R . .
C4 C 0.6158(6) 0.0635(7) 0.0346(6) 0.045(2) Uani 1 1 d D . .
C5 C 0.5601(8) 0.1068(7) -0.0239(5) 0.046(2) Uani 1 1 d . A .
H5 H 0.5833 0.0998 -0.0711 0.055 Uiso 1 1 calc R . .
C6 C 0.4722(7) 0.1593(7) -0.0130(5) 0.036(2) Uani 1 1 d . . .
C7 C 0.4448(10) 0.2026(9) -0.1365(5) 0.067(3) Uani 1 1 d . . .
H7A H 0.5074 0.2345 -0.1453 0.100 Uiso 1 1 calc R A .
H7B H 0.3942 0.2363 -0.1690 0.100 Uiso 1 1 calc R . .
H7C H 0.4579 0.1383 -0.1449 0.100 Uiso 1 1 calc R . .
C8 C 0.7097(7) 0.0018(8) 0.0204(7) 0.071(3) Uani 0.50 1 d PD A 1
H8A H 0.6952 -0.0645 0.0373 0.085 Uiso 0.50 1 calc PR A 1
H8B H 0.7246 0.0108 -0.0321 0.085 Uiso 0.50 1 calc PR A 1
C9 C 0.8011(14) 0.0189(19) 0.0548(15) 0.082(5) Uani 0.50 1 d PDU A 1
H9 H 0.7854 0.0298 0.1021 0.099 Uiso 0.50 1 calc PR A 1
C10 C 0.8973(18) 0.023(3) 0.0375(19) 0.104(7) Uani 0.50 1 d PDU A 1
H10A H 0.9232 0.0135 -0.0085 0.125 Uiso 0.50 1 calc PR A 1
H10B H 0.9415 0.0358 0.0710 0.125 Uiso 0.50 1 calc PR A 1
C8A C 0.7097(7) 0.0018(8) 0.0204(7) 0.071(3) Uani 0.50 1 d PD A 2
H8A1 H 0.7132 -0.0537 0.0597 0.085 Uiso 0.50 1 calc PR A 2
H8A2 H 0.7021 -0.0210 -0.0246 0.085 Uiso 0.50 1 calc PR A 2
C9A C 0.8081(13) 0.0460(17) 0.0142(15) 0.082(5) Uani 0.50 1 d PDU A 2
H9A H 0.8250 0.0915 -0.0268 0.099 Uiso 0.50 1 calc PR A 2
C10A C 0.872(3) 0.021(3) 0.0670(16) 0.104(7) Uani 0.50 1 d PDU A 2
H10C H 0.8541 -0.0249 0.1078 0.125 Uiso 0.50 1 calc PR A 2
H10D H 0.9342 0.0481 0.0637 0.125 Uiso 0.50 1 calc PR A 2
C11 C 0.3289(7) 0.3188(9) 0.2262(6) 0.042(3) Uani 1 1 d . . .
C12 C 0.3159(8) 0.4035(7) 0.2503(6) 0.040(3) Uani 1 1 d . . .
H12 H 0.3337 0.4600 0.2198 0.048 Uiso 1 1 calc R . .
C13 C 0.2762(8) 0.4041(8) 0.3200(6) 0.047(3) Uani 1 1 d . . .
H13 H 0.2663 0.4615 0.3370 0.057 Uiso 1 1 calc R . .
C14 C 0.2519(8) 0.3239(8) 0.3633(5) 0.047(3) Uani 1 1 d D . .
C15 C 0.2661(7) 0.2397(7) 0.3381(5) 0.036(2) Uani 1 1 d . . .
H15 H 0.2492 0.1829 0.3685 0.043 Uiso 1 1 calc R . .
C16 C 0.3049(7) 0.2388(8) 0.2684(5) 0.034(2) Uani 1 1 d . . .
C17 C 0.2932(8) 0.0750(8) 0.2810(6) 0.048(3) Uani 1 1 d . . .
H17A H 0.3259 0.0646 0.3268 0.073 Uiso 1 1 calc R . .
H17B H 0.3145 0.0231 0.2559 0.073 Uiso 1 1 calc R . .
H17C H 0.2198 0.0783 0.2899 0.073 Uiso 1 1 calc R . .
C18 C 0.2019(8) 0.3254(9) 0.4370(5) 0.060(3) Uani 1 1 d D . .
H18A H 0.2247 0.2676 0.4703 0.071 Uiso 1 1 calc R . .
H18B H 0.2229 0.3797 0.4552 0.071 Uiso 1 1 calc R . .
C19 C 0.0891(10) 0.3320(11) 0.4359(9) 0.089(5) Uani 1 1 d DU . .
H19 H 0.0609 0.2810 0.4220 0.107 Uiso 1 1 calc R . .
C20 C 0.0252(15) 0.3981(13) 0.4514(10) 0.124(7) Uani 1 1 d DU . .
H20A H 0.0485 0.4512 0.4657 0.148 Uiso 1 1 calc R . .
H20B H -0.0451 0.3937 0.4485 0.148 Uiso 1 1 calc R . .
C21 C 0.4412(7) 0.3738(6) 0.0295(5) 0.026(2) Uani 1 1 d . . .
C22 C 0.5393(6) 0.3720(6) 0.0595(5) 0.029(2) Uani 1 1 d . . .
H22 H 0.5530 0.3594 0.1089 0.035 Uiso 1 1 calc R . .
C23 C 0.6111(8) 0.3929(7) -0.0001(6) 0.041(3) Uani 1 1 d . . .
H23 H 0.6815 0.3963 0.0031 0.050 Uiso 1 1 calc R . .
C24 C 0.5600(8) 0.4073(7) -0.0632(6) 0.039(3) Uani 1 1 d . . .
H24 H 0.5906 0.4227 -0.1101 0.047 Uiso 1 1 calc R . .
C25 C 0.4578(7) 0.3960(7) -0.0478(5) 0.035(2) Uani 1 1 d . . .
H25 H 0.4077 0.4018 -0.0820 0.042 Uiso 1 1 calc R . .
C26 C 0.0667(7) 0.3000(7) 0.0119(7) 0.046(3) Uani 1 1 d . . .
C27 C 0.0032(7) 0.3735(8) 0.0348(6) 0.039(3) Uani 1 1 d . . .
H27 H -0.0388 0.4135 0.0016 0.047 Uiso 1 1 calc R . .
C28 C 0.0016(7) 0.3874(9) 0.1037(6) 0.042(3) Uani 1 1 d . . .
H28 H -0.0406 0.4384 0.1165 0.050 Uiso 1 1 calc R . .
C29 C 0.0608(8) 0.3288(9) 0.1582(6) 0.051(3) Uani 1 1 d . . .
C30 C 0.1183(8) 0.2529(9) 0.1373(8) 0.055(4) Uani 1 1 d . . .
H30 H 0.1570 0.2110 0.1716 0.066 Uiso 1 1 calc R . .
C31 C 0.1203(7) 0.2375(8) 0.0683(7) 0.053(3) Uani 1 1 d . . .
H31 H 0.1585 0.1835 0.0570 0.063 Uiso 1 1 calc R . .
C32 C 0.0659(9) 0.2953(9) -0.0678(8) 0.063(3) Uani 1 1 d . . .
H32 H 0.0558 0.3607 -0.0956 0.076 Uiso 1 1 calc R . .
C33 C 0.1608(10) 0.2490(10) -0.0977(8) 0.085(4) Uani 1 1 d . . .
H33A H 0.2193 0.2806 -0.0885 0.127 Uiso 1 1 calc R . .
H33B H 0.1566 0.2534 -0.1495 0.127 Uiso 1 1 calc R . .
H33C H 0.1683 0.1829 -0.0744 0.127 Uiso 1 1 calc R . .
C34 C -0.0321(10) 0.2426(11) -0.0729(9) 0.088(5) Uani 1 1 d . . .
H34A H -0.0259 0.1800 -0.0428 0.132 Uiso 1 1 calc R . .
H34B H -0.0390 0.2368 -0.1228 0.132 Uiso 1 1 calc R . .
H34C H -0.0918 0.2784 -0.0563 0.132 Uiso 1 1 calc R . .
C35 C 0.0582(8) 0.3491(11) 0.2331(6) 0.065(4) Uani 1 1 d . . .
H35A H -0.0120 0.3573 0.2512 0.098 Uiso 1 1 calc R . .
H35B H 0.0917 0.4066 0.2324 0.098 Uiso 1 1 calc R . .
H35C H 0.0934 0.2966 0.2645 0.098 Uiso 1 1 calc R . .
Ru2 Ru 0.66321(6) 0.04981(6) 0.39626(4) 0.0316(2) Uani 1 1 d . . .
Fe2 Fe 1.0000 0.0000 0.5000 0.0310(5) Uani 1 2 d S . .
Cl3 Cl 0.68961(19) 0.1477(2) 0.48015(14) 0.0416(7) Uani 1 1 d . . .
Cl4 Cl 0.70766(18) -0.0811(2) 0.48831(14) 0.0416(7) Uani 1 1 d . . .
P2 P 0.83079(17) 0.05293(19) 0.35740(13) 0.0293(6) Uani 1 1 d . . .
O5 O 0.8757(5) 0.1524(5) 0.3287(4) 0.0393(18) Uani 1 1 d . . .
O6 O 0.8215(5) 0.2135(6) 0.1927(4) 0.047(2) Uani 1 1 d . . .
O7 O 0.8430(5) 0.0031(5) 0.2875(3) 0.0401(18) Uani 1 1 d . . .
O8 O 0.8954(6) -0.1762(6) 0.3181(5) 0.060(2) Uani 1 1 d . B .
C36 C 0.8287(7) 0.2396(8) 0.3099(5) 0.035(3) Uani 1 1 d . . .
C37 C 0.8183(8) 0.3009(8) 0.3580(6) 0.048(3) Uani 1 1 d . . .
H37 H 0.8367 0.2788 0.4060 0.057 Uiso 1 1 calc R . .
C38 C 0.7816(9) 0.3942(8) 0.3376(6) 0.052(3) Uani 1 1 d . . .
H38 H 0.7741 0.4349 0.3714 0.063 Uiso 1 1 calc R . .
C39 C 0.7553(8) 0.4276(7) 0.2653(6) 0.045(3) Uani 1 1 d D . .
C40 C 0.7675(7) 0.3687(7) 0.2176(6) 0.044(3) Uani 1 1 d . . .
H40 H 0.7489 0.3910 0.1697 0.052 Uiso 1 1 calc R . .
C41 C 0.8062(7) 0.2775(8) 0.2370(5) 0.039(3) Uani 1 1 d . . .
C42 C 0.7876(9) 0.2428(8) 0.1207(5) 0.048(3) Uani 1 1 d . . .
H42A H 0.7141 0.2556 0.1226 0.072 Uiso 1 1 calc R . .
H42B H 0.8063 0.1928 0.0932 0.072 Uiso 1 1 calc R . .
H42C H 0.8194 0.2997 0.0974 0.072 Uiso 1 1 calc R . .
C43 C 0.7117(10) 0.5282(7) 0.2432(7) 0.073(4) Uani 1 1 d D . .
H43A H 0.7316 0.5670 0.2766 0.088 Uiso 1 1 calc R . .
H43B H 0.7380 0.5547 0.1942 0.088 Uiso 1 1 calc R . .
C44 C 0.5979(11) 0.5286(11) 0.2449(10) 0.118(7) Uani 1 1 d D . .
H44 H 0.5701 0.4989 0.2113 0.142 Uiso 1 1 calc R . .
C45 C 0.5363(13) 0.5654(15) 0.2877(14) 0.172(12) Uani 1 1 d D . .
H45A H 0.5609 0.5958 0.3222 0.206 Uiso 1 1 calc R . .
H45B H 0.4658 0.5624 0.2851 0.206 Uiso 1 1 calc R . .
C46 C 0.9372(7) -0.0282(8) 0.2589(5) 0.035(2) Uani 1 1 d . B .
C47 C 0.9989(8) 0.0335(8) 0.2161(6) 0.044(3) Uani 1 1 d . . .
H47 H 0.9787 0.0986 0.2052 0.053 Uiso 1 1 calc R . .
C48 C 1.0934(8) -0.0023(8) 0.1886(6) 0.050(3) Uani 1 1 d . B .
H48 H 1.1360 0.0386 0.1576 0.059 Uiso 1 1 calc R . .
C49 C 1.1230(7) -0.0971(8) 0.2072(6) 0.052(3) Uani 1 1 d D . .
C50 C 1.0571(8) -0.1575(8) 0.2500(6) 0.054(3) Uani 1 1 d . B .
H50 H 1.0763 -0.2228 0.2613 0.065 Uiso 1 1 calc R . .
C51 C 0.9636(8) -0.1228(9) 0.2760(6) 0.048(3) Uani 1 1 d . . .
C52 C 0.9241(11) -0.2747(10) 0.3418(10) 0.106(6) Uani 1 1 d . . .
H52A H 0.9180 -0.3085 0.3025 0.158 Uiso 1 1 calc R B .
H52B H 0.8797 -0.3000 0.3828 0.158 Uiso 1 1 calc R . .
H52C H 0.9942 -0.2826 0.3560 0.158 Uiso 1 1 calc R . .
C53 C 1.2161(14) -0.143(2) 0.1740(14) 0.052(6) Uani 0.50 1 d PD B 1
H53A H 1.1970 -0.1682 0.1325 0.063 Uiso 0.50 1 calc PR B 1
H53B H 1.2647 -0.0951 0.1562 0.063 Uiso 0.50 1 calc PR B 1
C54 C 1.2656(19) -0.2205(16) 0.2265(15) 0.079(5) Uani 0.50 1 d PDU B 1
H54 H 1.2815 -0.2158 0.2735 0.094 Uiso 0.50 1 calc PR B 1
C55 C 1.284(3) -0.2970(19) 0.1980(18) 0.091(6) Uani 0.50 1 d PDU B 1
H55A H 1.2659 -0.2964 0.1505 0.109 Uiso 0.50 1 calc PR B 1
H55B H 1.3155 -0.3523 0.2252 0.109 Uiso 0.50 1 calc PR B 1
C53A C 1.2320(10) -0.1256(19) 0.1885(18) 0.052(6) Uani 0.50 1 d PD B 2
H53C H 1.2535 -0.0844 0.1433 0.063 Uiso 0.50 1 calc PR B 2
H53D H 1.2739 -0.1144 0.2266 0.063 Uiso 0.50 1 calc PR B 2
C54A C 1.2534(19) -0.2251(14) 0.1796(15) 0.079(5) Uani 0.50 1 d PDU B 2
H54A H 1.2523 -0.2313 0.1308 0.094 Uiso 0.50 1 calc PR B 2
C55A C 1.273(3) -0.3069(19) 0.2222(17) 0.091(6) Uani 0.50 1 d PDU B 2
H55C H 1.2767 -0.3101 0.2724 0.109 Uiso 0.50 1 calc PR B 2
H55D H 1.2847 -0.3625 0.2026 0.109 Uiso 0.50 1 calc PR B 2
C56 C 0.9405(7) -0.0013(7) 0.4041(5) 0.030(2) Uani 1 1 d . . .
C57 C 1.0379(7) 0.0364(7) 0.3924(5) 0.034(2) Uani 1 1 d . . .
H57 H 1.0509 0.0972 0.3668 0.041 Uiso 1 1 calc R . .
C58 C 1.1099(7) -0.0308(8) 0.4245(5) 0.035(3) Uani 1 1 d . . .
H58 H 1.1800 -0.0237 0.4253 0.042 Uiso 1 1 calc R . .
C59 C 1.0591(7) -0.1125(7) 0.4563(5) 0.036(2) Uani 1 1 d . . .
H59 H 1.0898 -0.1693 0.4820 0.043 Uiso 1 1 calc R . .
C60 C 0.9546(7) -0.0940(7) 0.4427(5) 0.032(2) Uani 1 1 d . . .
H60 H 0.9036 -0.1364 0.4569 0.038 Uiso 1 1 calc R . .
C61 C 0.5631(7) -0.0401(8) 0.3547(6) 0.044(3) Uani 1 1 d . . .
C62 C 0.5037(7) 0.0130(8) 0.4012(5) 0.041(3) Uani 1 1 d . . .
H62 H 0.4644 -0.0200 0.4399 0.049 Uiso 1 1 calc R . .
C63 C 0.5005(7) 0.1084(8) 0.3929(6) 0.037(3) Uani 1 1 d . . .
H63 H 0.4590 0.1399 0.4249 0.045 Uiso 1 1 calc R . .
C64 C 0.5589(7) 0.1607(8) 0.3367(6) 0.042(3) Uani 1 1 d . . .
C65 C 0.6162(8) 0.1112(9) 0.2889(6) 0.043(3) Uani 1 1 d . . .
H65 H 0.6538 0.1449 0.2497 0.052 Uiso 1 1 calc R . .
C66 C 0.6189(7) 0.0116(9) 0.2982(5) 0.048(3) Uani 1 1 d . . .
H66 H 0.6592 -0.0200 0.2657 0.058 Uiso 1 1 calc R . .
C67 C 0.5600(8) -0.1437(8) 0.3660(7) 0.053(3) Uani 1 1 d . . .
H67 H 0.5554 -0.1684 0.4188 0.064 Uiso 1 1 calc R . .
C68 C 0.6526(9) -0.1908(9) 0.3346(9) 0.085(5) Uani 1 1 d . . .
H68A H 0.6507 -0.1785 0.2822 0.127 Uiso 1 1 calc R . .
H68B H 0.6544 -0.2586 0.3527 0.127 Uiso 1 1 calc R . .
H68C H 0.7129 -0.1662 0.3484 0.127 Uiso 1 1 calc R . .
C69 C 0.4641(10) -0.1671(11) 0.3337(9) 0.088(5) Uani 1 1 d . . .
H69A H 0.4055 -0.1295 0.3498 0.131 Uiso 1 1 calc R . .
H69B H 0.4541 -0.2339 0.3496 0.131 Uiso 1 1 calc R . .
H69C H 0.4720 -0.1529 0.2812 0.131 Uiso 1 1 calc R . .
C70 C 0.5570(9) 0.2665(9) 0.3313(8) 0.061(4) Uani 1 1 d . . .
H70A H 0.6039 0.2925 0.2921 0.091 Uiso 1 1 calc R . .
H70B H 0.5771 0.2803 0.3766 0.091 Uiso 1 1 calc R . .
H70C H 0.4885 0.2948 0.3218 0.091 Uiso 1 1 calc 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
Ru1 0.0151(4) 0.0342(5) 0.0332(4) 0.0056(4) -0.0039(3) -0.0014(3)
Fe1 0.0159(9) 0.0286(11) 0.0300(11) 0.0017(9) 0.0016(8) -0.0017(8)
Cl1 0.0254(12) 0.0508(15) 0.0331(13) 0.0087(11) -0.0040(9) -0.0015(11)
Cl2 0.0268(12) 0.0423(15) 0.0479(16) -0.0072(13) 0.0002(11) -0.0005(10)
P1 0.0153(11) 0.0298(13) 0.0277(12) 0.0035(10) -0.0018(9) -0.0006(9)
O1 0.021(3) 0.028(4) 0.050(4) -0.002(3) -0.003(3) 0.000(3)
O2 0.052(4) 0.056(4) 0.038(4) -0.007(3) -0.009(3) 0.006(3)
O3 0.017(3) 0.052(4) 0.026(3) 0.004(3) 0.003(3) -0.001(3)
O4 0.037(4) 0.031(4) 0.038(4) -0.002(3) 0.004(3) 0.004(3)
C1 0.022(5) 0.031(5) 0.038(5) -0.004(4) 0.002(4) -0.004(4)
C2 0.037(5) 0.037(5) 0.037(5) -0.002(4) -0.005(4) 0.001(4)
C3 0.033(5) 0.051(6) 0.049(6) -0.008(5) -0.017(4) 0.012(4)
C4 0.030(5) 0.042(5) 0.064(7) -0.020(5) -0.001(4) 0.002(4)
C5 0.045(6) 0.049(6) 0.042(5) -0.010(5) 0.008(4) 0.000(4)
C6 0.037(5) 0.035(5) 0.034(5) 0.001(4) -0.001(4) -0.006(4)
C7 0.085(9) 0.079(8) 0.032(5) -0.008(5) -0.009(5) 0.010(7)
C8 0.041(6) 0.073(8) 0.100(9) -0.025(7) -0.011(6) 0.013(5)
C9 0.077(6) 0.085(7) 0.085(7) -0.015(5) -0.006(5) -0.004(4)
C10 0.099(8) 0.106(8) 0.107(9) -0.019(5) -0.007(5) -0.005(5)
C8A 0.041(6) 0.073(8) 0.100(9) -0.025(7) -0.011(6) 0.013(5)
C9A 0.077(6) 0.085(7) 0.085(7) -0.015(5) -0.006(5) -0.004(4)
C10A 0.099(8) 0.106(8) 0.107(9) -0.019(5) -0.007(5) -0.005(5)
C11 0.017(5) 0.075(8) 0.039(6) -0.025(6) -0.010(4) 0.009(5)
C12 0.037(6) 0.039(6) 0.040(6) 0.004(5) -0.009(5) -0.006(5)
C13 0.051(7) 0.047(6) 0.045(6) -0.014(5) 0.001(5) -0.001(5)
C14 0.046(7) 0.061(8) 0.027(5) 0.001(5) 0.003(4) 0.005(6)
C15 0.027(5) 0.041(6) 0.032(5) 0.009(5) 0.002(4) -0.003(4)
C16 0.015(4) 0.059(7) 0.022(4) 0.004(5) -0.008(3) 0.006(4)
C17 0.035(6) 0.058(7) 0.047(6) 0.000(6) 0.001(5) 0.001(5)
C18 0.072(8) 0.066(8) 0.037(6) -0.012(5) 0.008(5) 0.013(6)
C19 0.087(7) 0.097(7) 0.083(7) -0.020(6) 0.006(5) -0.006(6)
C20 0.123(9) 0.125(8) 0.127(9) -0.037(6) -0.002(6) -0.007(6)
C21 0.017(4) 0.027(5) 0.027(5) 0.010(4) 0.001(4) 0.001(4)
C22 0.010(4) 0.032(5) 0.040(6) 0.003(4) -0.006(4) 0.001(4)
C23 0.018(5) 0.038(6) 0.061(8) 0.006(6) 0.007(5) -0.005(4)
C24 0.037(6) 0.038(6) 0.039(6) 0.001(5) 0.013(5) -0.011(5)
C25 0.033(5) 0.047(6) 0.026(5) -0.004(5) 0.001(4) -0.007(5)
C26 0.022(5) 0.039(6) 0.080(8) -0.016(6) -0.002(5) -0.010(4)
C27 0.014(4) 0.055(7) 0.046(6) 0.004(5) -0.013(4) -0.010(4)
C28 0.014(5) 0.053(7) 0.053(7) 0.000(5) 0.005(4) 0.002(4)
C29 0.027(6) 0.078(9) 0.043(6) 0.022(6) -0.013(5) -0.033(6)
C30 0.021(5) 0.058(8) 0.076(9) 0.020(7) -0.014(6) -0.013(5)
C31 0.022(5) 0.037(6) 0.097(10) 0.004(6) -0.027(6) -0.009(4)
C32 0.042(6) 0.057(7) 0.097(10) -0.030(6) -0.011(6) -0.006(5)
C33 0.065(9) 0.095(10) 0.099(10) -0.036(8) -0.022(8) 0.015(7)
C34 0.048(8) 0.115(13) 0.114(12) -0.049(10) -0.029(8) 0.005(8)
C35 0.020(5) 0.128(12) 0.036(6) 0.016(7) 0.000(4) -0.012(6)
Ru2 0.0158(4) 0.0482(5) 0.0270(4) 0.0033(4) -0.0040(3) -0.0031(4)
Fe2 0.0169(10) 0.0449(13) 0.0270(11) 0.0043(10) -0.0036(8) -0.0007(9)
Cl3 0.0294(13) 0.0574(17) 0.0362(14) -0.0044(13) -0.0068(10) 0.0000(12)
Cl4 0.0233(12) 0.0541(17) 0.0397(14) 0.0121(12) -0.0041(10) -0.0041(11)
P2 0.0148(11) 0.0417(15) 0.0279(13) 0.0031(11) -0.0044(9) -0.0013(10)
O5 0.024(4) 0.045(4) 0.041(4) 0.014(4) -0.006(3) -0.003(3)
O6 0.034(4) 0.057(5) 0.044(4) 0.009(4) -0.013(3) 0.003(4)
O7 0.017(3) 0.065(5) 0.038(4) -0.008(4) -0.003(3) 0.003(3)
O8 0.044(4) 0.058(5) 0.075(5) -0.007(4) 0.011(4) -0.015(4)
C36 0.020(5) 0.049(7) 0.028(5) 0.013(5) -0.009(4) -0.003(4)
C37 0.033(6) 0.059(8) 0.045(6) 0.005(6) -0.008(5) 0.001(5)
C38 0.059(7) 0.050(7) 0.045(6) 0.003(5) -0.003(5) -0.009(6)
C39 0.041(6) 0.044(7) 0.049(7) -0.003(5) 0.003(5) -0.005(5)
C40 0.028(6) 0.040(6) 0.052(7) 0.017(6) -0.004(5) -0.001(5)
C41 0.027(5) 0.057(7) 0.028(5) 0.001(5) -0.008(4) 0.016(5)
C42 0.052(7) 0.052(7) 0.034(6) 0.006(5) -0.007(5) -0.004(5)
C43 0.084(10) 0.056(8) 0.067(9) 0.009(7) 0.003(7) 0.008(7)
C44 0.108(13) 0.081(11) 0.144(16) 0.013(10) -0.024(12) 0.054(10)
C45 0.048(9) 0.140(17) 0.34(4) -0.09(2) 0.038(14) 0.017(10)
C46 0.023(5) 0.050(6) 0.034(5) -0.014(5) 0.001(4) -0.001(4)
C47 0.034(5) 0.052(7) 0.044(6) -0.006(5) 0.002(4) 0.005(5)
C48 0.035(5) 0.057(7) 0.056(6) -0.015(5) 0.005(4) 0.006(5)
C49 0.038(5) 0.065(7) 0.053(6) -0.020(5) 0.011(4) -0.002(5)
C50 0.042(6) 0.054(7) 0.071(7) -0.024(6) 0.001(5) -0.003(5)
C51 0.036(6) 0.071(8) 0.040(6) -0.019(6) 0.003(4) -0.013(5)
C52 0.080(10) 0.088(11) 0.135(14) -0.003(10) 0.051(9) -0.014(8)
C53 0.038(8) 0.058(12) 0.072(14) -0.045(8) 0.011(8) -0.007(8)
C54 0.075(6) 0.082(6) 0.079(7) -0.017(5) -0.002(5) -0.005(4)
C55 0.089(7) 0.087(7) 0.094(8) -0.015(5) -0.001(5) 0.004(4)
C53A 0.038(8) 0.058(12) 0.072(14) -0.045(8) 0.011(8) -0.007(8)
C54A 0.075(6) 0.082(6) 0.079(7) -0.017(5) -0.002(5) -0.005(4)
C55A 0.089(7) 0.087(7) 0.094(8) -0.015(5) -0.001(5) 0.004(4)
C56 0.020(5) 0.041(6) 0.032(5) -0.010(5) -0.005(4) -0.007(4)
C57 0.027(5) 0.040(6) 0.031(5) 0.003(5) -0.003(4) -0.005(4)
C58 0.019(5) 0.060(7) 0.027(5) -0.010(5) -0.003(4) 0.002(5)
C59 0.025(5) 0.047(6) 0.033(5) -0.003(5) -0.002(4) 0.009(5)
C60 0.021(5) 0.043(6) 0.030(5) -0.001(4) -0.007(4) -0.004(4)
C61 0.019(5) 0.067(7) 0.045(6) -0.003(5) -0.009(4) -0.010(4)
C62 0.012(4) 0.070(8) 0.034(6) 0.005(5) 0.001(4) -0.002(5)
C63 0.016(4) 0.043(6) 0.045(6) 0.017(5) -0.006(4) -0.011(4)
C64 0.017(5) 0.058(7) 0.046(6) 0.007(5) -0.008(4) 0.001(4)
C65 0.028(6) 0.067(8) 0.031(6) 0.008(5) -0.009(4) -0.013(5)
C66 0.019(5) 0.096(10) 0.031(5) -0.017(6) -0.005(4) 0.002(5)
C67 0.033(5) 0.058(7) 0.074(7) -0.021(6) -0.013(5) -0.005(5)
C68 0.038(6) 0.079(9) 0.150(14) -0.050(9) -0.007(7) -0.004(6)
C69 0.055(8) 0.100(11) 0.125(12) -0.052(10) -0.031(8) -0.016(8)
C70 0.041(7) 0.060(8) 0.074(9) 0.009(7) -0.019(6) 0.002(6)
_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
Ru1 C31 2.175(11) . ?
Ru1 C30 2.176(12) . ?
Ru1 C26 2.220(11) . ?
Ru1 C29 2.221(11) . ?
Ru1 C28 2.250(10) . ?
Ru1 C27 2.279(9) . ?
Ru1 P1 2.307(2) . ?
Ru1 Cl2 2.383(3) . ?
Ru1 Cl1 2.403(2) . ?
Fe1 C21 2.028(9) . ?
Fe1 C21 2.028(9) 2_665 ?
Fe1 C22 2.033(9) 2_665 ?
Fe1 C22 2.033(9) . ?
Fe1 C25 2.047(11) 2_665 ?
Fe1 C25 2.047(11) . ?
Fe1 C24 2.051(11) . ?
Fe1 C24 2.051(11) 2_665 ?
Fe1 C23 2.053(10) 2_665 ?
Fe1 C23 2.053(10) . ?
P1 O1 1.628(7) . ?
P1 O3 1.629(7) . ?
P1 C21 1.786(9) . ?
O1 C1 1.398(10) . ?
O2 C6 1.362(11) . ?
O2 C7 1.409(12) . ?
O3 C11 1.409(12) . ?
O4 C16 1.377(12) . ?
O4 C17 1.400(12) . ?
C1 C2 1.385(13) . ?
C1 C6 1.409(13) . ?
C2 C3 1.376(13) . ?
C2 H2 0.9500 . ?
C3 C4 1.366(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.396(14) . ?
C4 C8 1.515(6) . ?
C5 C6 1.367(13) . ?
C5 H5 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.482(12) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.305(13) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9500 . ?
C10 H10B 0.9500 . ?
C9A C10A 1.333(14) . ?
C9A H9A 0.9500 . ?
C10A H10C 0.9500 . ?
C10A H10D 0.9500 . ?
C11 C16 1.334(15) . ?
C11 C12 1.389(15) . ?
C12 C13 1.394(15) . ?
C12 H12 0.9500 . ?
C13 C14 1.345(15) . ?
C13 H13 0.9500 . ?
C14 C15 1.393(15) . ?
C14 C18 1.514(8) . ?
C15 C16 1.392(13) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.498(11) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.292(11) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9500 . ?
C20 H20B 0.9500 . ?
C21 C25 1.450(13) . ?
C21 C22 1.457(12) . ?
C22 C23 1.435(14) . ?
C22 H22 0.9500 . ?
C23 C24 1.392(15) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(13) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C26 C27 1.421(14) . ?
C26 C31 1.452(15) . ?
C26 C32 1.531(17) . ?
C27 C28 1.361(16) . ?
C27 H27 0.9500 . ?
C28 C29 1.442(15) . ?
C28 H28 0.9500 . ?
C29 C30 1.393(17) . ?
C29 C35 1.508(17) . ?
C30 C31 1.371(18) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.508(17) . ?
C32 C34 1.589(18) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
Ru2 C65 2.176(10) . ?
Ru2 C66 2.177(11) . ?
Ru2 C64 2.223(10) . ?
Ru2 C62 2.229(9) . ?
Ru2 C61 2.229(11) . ?
Ru2 C63 2.258(10) . ?
Ru2 P2 2.304(2) . ?
Ru2 Cl4 2.391(3) . ?
Ru2 Cl3 2.396(3) . ?
Fe2 C56 2.041(9) 2_756 ?
Fe2 C56 2.041(9) . ?
Fe2 C59 2.050(10) 2_756 ?
Fe2 C59 2.050(10) . ?
Fe2 C57 2.053(10) . ?
Fe2 C57 2.053(10) 2_756 ?
Fe2 C60 2.059(10) . ?
Fe2 C60 2.059(10) 2_756 ?
Fe2 C58 2.061(10) . ?
Fe2 C58 2.061(10) 2_756 ?
P2 O5 1.601(7) . ?
P2 O7 1.624(7) . ?
P2 C56 1.804(10) . ?
O5 C36 1.359(12) . ?
O6 C41 1.365(12) . ?
O6 C42 1.445(12) . ?
O7 C46 1.406(11) . ?
O8 C51 1.364(13) . ?
O8 C52 1.445(16) . ?
C36 C37 1.389(15) . ?
C36 C41 1.432(12) . ?
C37 C38 1.395(15) . ?
C37 H37 0.9500 . ?
C38 C39 1.425(15) . ?
C38 H38 0.9500 . ?
C39 C40 1.355(15) . ?
C39 C43 1.519(8) . ?
C40 C41 1.373(14) . ?
C40 H40 0.9500 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.514(11) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.272(12) . ?
C44 H44 0.9500 . ?
C45 H45A 0.9500 . ?
C45 H45B 0.9500 . ?
C46 C51 1.374(15) . ?
C46 C47 1.381(15) . ?
C47 C48 1.423(13) . ?
C47 H47 0.9500 . ?
C48 C49 1.387(15) . ?
C48 H48 0.9500 . ?
C49 C50 1.404(15) . ?
C49 C53A 1.513(10) . ?
C49 C53 1.513(10) . ?
C50 C51 1.397(14) . ?
C50 H50 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.496(13) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.326(14) . ?
C54 H54 0.9500 . ?
C55 H55A 0.9500 . ?
C55 H55B 0.9500 . ?
C53A C54A 1.492(12) . ?
C53A H53C 0.9900 . ?
C53A H53D 0.9900 . ?
C54A C55A 1.325(13) . ?
C54A H54A 0.9500 . ?
C55A H55C 0.9500 . ?
C55A H55D 0.9500 . ?
C56 C60 1.411(14) . ?
C56 C57 1.439(13) . ?
C57 C58 1.391(13) . ?
C57 H57 0.9500 . ?
C58 C59 1.432(14) . ?
C58 H58 0.9500 . ?
C59 C60 1.427(12) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 C66 1.398(15) . ?
C61 C62 1.437(14) . ?
C61 C67 1.488(15) . ?
C62 C63 1.366(16) . ?
C62 H62 0.9500 . ?
C63 C64 1.417(14) . ?
C63 H63 0.9500 . ?
C64 C65 1.408(15) . ?
C64 C70 1.524(16) . ?
C65 C66 1.425(16) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 C68 1.502(15) . ?
C67 C69 1.547(15) . ?
C67 H67 1.0000 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
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
C31 Ru1 C30 36.7(5) . . ?
C31 Ru1 C26 38.6(4) . . ?
C30 Ru1 C26 68.7(5) . . ?
C31 Ru1 C29 66.5(5) . . ?
C30 Ru1 C29 36.9(5) . . ?
C26 Ru1 C29 81.1(4) . . ?
C31 Ru1 C28 76.6(5) . . ?
C30 Ru1 C28 65.8(4) . . ?
C26 Ru1 C28 65.6(4) . . ?
C29 Ru1 C28 37.6(4) . . ?
C31 Ru1 C27 65.9(4) . . ?
C30 Ru1 C27 77.9(4) . . ?
C26 Ru1 C27 36.8(4) . . ?
C29 Ru1 C27 66.5(4) . . ?
C28 Ru1 C27 35.0(4) . . ?
C31 Ru1 P1 93.3(3) . . ?
C30 Ru1 P1 90.9(3) . . ?
C26 Ru1 P1 120.6(3) . . ?
C29 Ru1 P1 115.1(3) . . ?
C28 Ru1 P1 152.7(3) . . ?
C27 Ru1 P1 157.2(3) . . ?
C31 Ru1 Cl2 157.3(4) . . ?
C30 Ru1 Cl2 120.8(4) . . ?
C26 Ru1 Cl2 148.5(3) . . ?
C29 Ru1 Cl2 91.7(4) . . ?
C28 Ru1 Cl2 90.1(3) . . ?
C27 Ru1 Cl2 112.5(3) . . ?
P1 Ru1 Cl2 90.32(9) . . ?
C31 Ru1 Cl1 116.2(4) . . ?
C30 Ru1 Cl1 152.9(4) . . ?
C26 Ru1 Cl1 88.0(3) . . ?
C29 Ru1 Cl1 155.5(3) . . ?
C28 Ru1 Cl1 117.9(3) . . ?
C27 Ru1 Cl1 91.7(3) . . ?
P1 Ru1 Cl1 89.39(8) . . ?
Cl2 Ru1 Cl1 86.30(10) . . ?
C21 Fe1 C21 179.999(1) . 2_665 ?
C21 Fe1 C22 138.0(3) . 2_665 ?
C21 Fe1 C22 42.0(3) 2_665 2_665 ?
C21 Fe1 C22 42.0(3) . . ?
C21 Fe1 C22 138.0(3) 2_665 . ?
C22 Fe1 C22 180.0(3) 2_665 . ?
C21 Fe1 C25 138.3(4) . 2_665 ?
C21 Fe1 C25 41.7(4) 2_665 2_665 ?
C22 Fe1 C25 69.6(4) 2_665 2_665 ?
C22 Fe1 C25 110.4(4) . 2_665 ?
C21 Fe1 C25 41.7(4) . . ?
C21 Fe1 C25 138.3(4) 2_665 . ?
C22 Fe1 C25 110.4(4) 2_665 . ?
C22 Fe1 C25 69.6(4) . . ?
C25 Fe1 C25 180.000(1) 2_665 . ?
C21 Fe1 C24 68.5(4) . . ?
C21 Fe1 C24 111.5(4) 2_665 . ?
C22 Fe1 C24 111.7(4) 2_665 . ?
C22 Fe1 C24 68.3(4) . . ?
C25 Fe1 C24 140.3(4) 2_665 . ?
C25 Fe1 C24 39.7(4) . . ?
C21 Fe1 C24 111.5(4) . 2_665 ?
C21 Fe1 C24 68.5(4) 2_665 2_665 ?
C22 Fe1 C24 68.3(4) 2_665 2_665 ?
C22 Fe1 C24 111.7(4) . 2_665 ?
C25 Fe1 C24 39.7(4) 2_665 2_665 ?
C25 Fe1 C24 140.3(4) . 2_665 ?
C24 Fe1 C24 180.000(1) . 2_665 ?
C21 Fe1 C23 110.7(4) . 2_665 ?
C21 Fe1 C23 69.3(4) 2_665 2_665 ?
C22 Fe1 C23 41.1(4) 2_665 2_665 ?
C22 Fe1 C23 138.9(4) . 2_665 ?
C25 Fe1 C23 67.7(4) 2_665 2_665 ?
C25 Fe1 C23 112.3(4) . 2_665 ?
C24 Fe1 C23 140.3(4) . 2_665 ?
C24 Fe1 C23 39.7(4) 2_665 2_665 ?
C21 Fe1 C23 69.3(4) . . ?
C21 Fe1 C23 110.7(4) 2_665 . ?
C22 Fe1 C23 138.9(4) 2_665 . ?
C22 Fe1 C23 41.1(4) . . ?
C25 Fe1 C23 112.3(4) 2_665 . ?
C25 Fe1 C23 67.7(4) . . ?
C24 Fe1 C23 39.7(4) . . ?
C24 Fe1 C23 140.3(4) 2_665 . ?
C23 Fe1 C23 180.0(4) 2_665 . ?
O1 P1 O3 103.6(3) . . ?
O1 P1 C21 101.8(4) . . ?
O3 P1 C21 95.2(4) . . ?
O1 P1 Ru1 106.0(2) . . ?
O3 P1 Ru1 118.6(2) . . ?
C21 P1 Ru1 128.4(3) . . ?
C1 O1 P1 123.4(6) . . ?
C6 O2 C7 116.5(8) . . ?
C11 O3 P1 130.6(6) . . ?
C16 O4 C17 117.1(8) . . ?
C2 C1 O1 120.5(9) . . ?
C2 C1 C6 118.9(9) . . ?
O1 C1 C6 120.5(8) . . ?
C3 C2 C1 119.2(9) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 122.1(9) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 119.1(8) . . ?
C3 C4 C8 123.0(10) . . ?
C5 C4 C8 117.9(9) . . ?
C6 C5 C4 119.7(9) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
O2 C6 C5 125.4(9) . . ?
O2 C6 C1 113.7(9) . . ?
C5 C6 C1 120.8(9) . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C4 115.3(13) . . ?
C9 C8 H8A 108.4 . . ?
C4 C8 H8A 108.4 . . ?
C9 C8 H8B 108.4 . . ?
C4 C8 H8B 108.4 . . ?
H8A C8 H8B 107.5 . . ?
C10 C9 C8 137(3) . . ?
C10 C9 H9 111.4 . . ?
C8 C9 H9 111.4 . . ?
C9 C10 H10A 120.0 . . ?
C9 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?
C10A C9A H9A 120.5 . . ?
C9A C10A H10C 120.0 . . ?
C9A C10A H10D 120.0 . . ?
H10C C10A H10D 120.0 . . ?
C16 C11 C12 121.4(10) . . ?
C16 C11 O3 122.3(10) . . ?
C12 C11 O3 115.9(11) . . ?
C11 C12 C13 118.8(10) . . ?
C11 C12 H12 120.6 . . ?
C13 C12 H12 120.6 . . ?
C14 C13 C12 120.5(10) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C15 119.7(9) . . ?
C13 C14 C18 120.5(11) . . ?
C15 C14 C18 119.6(10) . . ?
C16 C15 C14 120.0(9) . . ?
C16 C15 H15 120.0 . . ?
C14 C15 H15 120.0 . . ?
C11 C16 O4 116.1(9) . . ?
C11 C16 C15 119.5(10) . . ?
O4 C16 C15 124.3(9) . . ?
O4 C17 H17A 109.5 . . ?
O4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C14 112.0(10) . . ?
C19 C18 H18A 109.2 . . ?
C14 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C14 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 C18 128.4(16) . . ?
C20 C19 H19 115.8 . . ?
C18 C19 H19 115.8 . . ?
C19 C20 H20A 120.0 . . ?
C19 C20 H20B 120.0 . . ?
H20A C20 H20B 120.0 . . ?
C25 C21 C22 106.5(8) . . ?
C25 C21 P1 127.8(7) . . ?
C22 C21 P1 123.9(7) . . ?
C25 C21 Fe1 69.9(5) . . ?
C22 C21 Fe1 69.2(5) . . ?
P1 C21 Fe1 137.5(5) . . ?
C23 C22 C21 106.8(9) . . ?
C23 C22 Fe1 70.2(6) . . ?
C21 C22 Fe1 68.8(5) . . ?
C23 C22 H22 126.6 . . ?
C21 C22 H22 126.6 . . ?
Fe1 C22 H22 126.0 . . ?
C24 C23 C22 108.4(9) . . ?
C24 C23 Fe1 70.1(6) . . ?
C22 C23 Fe1 68.7(5) . . ?
C24 C23 H23 125.8 . . ?
C22 C23 H23 125.8 . . ?
Fe1 C23 H23 127.0 . . ?
C25 C24 C23 110.4(9) . . ?
C25 C24 Fe1 70.0(6) . . ?
C23 C24 Fe1 70.3(6) . . ?
C25 C24 H24 124.8 . . ?
C23 C24 H24 124.8 . . ?
Fe1 C24 H24 126.5 . . ?
C24 C25 C21 107.9(9) . . ?
C24 C25 Fe1 70.3(6) . . ?
C21 C25 Fe1 68.5(6) . . ?
C24 C25 H25 126.0 . . ?
C21 C25 H25 126.0 . . ?
Fe1 C25 H25 126.8 . . ?
C27 C26 C31 115.0(11) . . ?
C27 C26 C32 115.9(10) . . ?
C31 C26 C32 129.0(11) . . ?
C27 C26 Ru1 73.9(6) . . ?
C31 C26 Ru1 69.0(6) . . ?
C32 C26 Ru1 128.5(8) . . ?
C28 C27 C26 121.1(10) . . ?
C28 C27 Ru1 71.3(6) . . ?
C26 C27 Ru1 69.3(5) . . ?
C28 C27 H27 119.5 . . ?
C26 C27 H27 119.5 . . ?
Ru1 C27 H27 133.1 . . ?
C27 C28 C29 123.3(11) . . ?
C27 C28 Ru1 73.7(6) . . ?
C29 C28 Ru1 70.1(6) . . ?
C27 C28 H28 118.4 . . ?
C29 C28 H28 118.4 . . ?
Ru1 C28 H28 130.8 . . ?
C30 C29 C28 116.0(11) . . ?
C30 C29 C35 123.0(11) . . ?
C28 C29 C35 121.0(12) . . ?
C30 C29 Ru1 69.8(7) . . ?
C28 C29 Ru1 72.3(6) . . ?
C35 C29 Ru1 128.5(8) . . ?
C31 C30 C29 121.5(11) . . ?
C31 C30 Ru1 71.6(7) . . ?
C29 C30 Ru1 73.3(7) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
Ru1 C30 H30 128.1 . . ?
C30 C31 C26 122.8(12) . . ?
C30 C31 Ru1 71.7(7) . . ?
C26 C31 Ru1 72.4(6) . . ?
C30 C31 H31 118.6 . . ?
C26 C31 H31 118.6 . . ?
Ru1 C31 H31 130.2 . . ?
C33 C32 C26 114.5(10) . . ?
C33 C32 C34 113.2(11) . . ?
C26 C32 C34 103.8(11) . . ?
C33 C32 H32 108.3 . . ?
C26 C32 H32 108.3 . . ?
C34 C32 H32 108.3 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C29 C35 H35A 109.5 . . ?
C29 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C29 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C65 Ru2 C66 38.2(4) . . ?
C65 Ru2 C64 37.3(4) . . ?
C66 Ru2 C64 68.4(4) . . ?
C65 Ru2 C62 77.6(4) . . ?
C66 Ru2 C62 66.2(4) . . ?
C64 Ru2 C62 65.7(4) . . ?
C65 Ru2 C61 67.7(4) . . ?
C66 Ru2 C61 37.0(4) . . ?
C64 Ru2 C61 80.5(4) . . ?
C62 Ru2 C61 37.6(4) . . ?
C65 Ru2 C63 66.1(4) . . ?
C66 Ru2 C63 78.7(4) . . ?
C64 Ru2 C63 36.9(4) . . ?
C62 Ru2 C63 35.4(4) . . ?
C61 Ru2 C63 66.8(4) . . ?
C65 Ru2 P2 91.1(3) . . ?
C66 Ru2 P2 93.1(3) . . ?
C64 Ru2 P2 115.6(3) . . ?
C62 Ru2 P2 157.8(3) . . ?
C61 Ru2 P2 120.3(3) . . ?
C63 Ru2 P2 152.4(2) . . ?
C65 Ru2 Cl4 152.4(3) . . ?
C66 Ru2 Cl4 114.2(3) . . ?
C64 Ru2 Cl4 155.2(3) . . ?
C62 Ru2 Cl4 92.2(3) . . ?
C61 Ru2 Cl4 88.5(3) . . ?
C63 Ru2 Cl4 118.4(2) . . ?
P2 Ru2 Cl4 89.08(9) . . ?
C65 Ru2 Cl3 120.6(3) . . ?
C66 Ru2 Cl3 158.6(3) . . ?
C64 Ru2 Cl3 91.2(3) . . ?
C62 Ru2 Cl3 112.2(3) . . ?
C61 Ru2 Cl3 149.2(3) . . ?
C63 Ru2 Cl3 88.8(3) . . ?
P2 Ru2 Cl3 90.08(10) . . ?
Cl4 Ru2 Cl3 87.04(10) . . ?
C56 Fe2 C56 179.998(1) 2_756 . ?
C56 Fe2 C59 68.2(4) 2_756 2_756 ?
C56 Fe2 C59 111.8(4) . 2_756 ?
C56 Fe2 C59 111.8(4) 2_756 . ?
C56 Fe2 C59 68.2(4) . . ?
C59 Fe2 C59 179.999(1) 2_756 . ?
C56 Fe2 C57 138.8(4) 2_756 . ?
C56 Fe2 C57 41.2(4) . . ?
C59 Fe2 C57 112.5(4) 2_756 . ?
C59 Fe2 C57 67.5(4) . . ?
C56 Fe2 C57 41.2(4) 2_756 2_756 ?
C56 Fe2 C57 138.8(4) . 2_756 ?
C59 Fe2 C57 67.5(4) 2_756 2_756 ?
C59 Fe2 C57 112.5(4) . 2_756 ?
C57 Fe2 C57 179.999(1) . 2_756 ?
C56 Fe2 C60 139.7(4) 2_756 . ?
C56 Fe2 C60 40.3(4) . . ?
C59 Fe2 C60 139.4(4) 2_756 . ?
C59 Fe2 C60 40.6(3) . . ?
C57 Fe2 C60 68.0(4) . . ?
C57 Fe2 C60 112.0(4) 2_756 . ?
C56 Fe2 C60 40.3(4) 2_756 2_756 ?
C56 Fe2 C60 139.7(4) . 2_756 ?
C59 Fe2 C60 40.6(3) 2_756 2_756 ?
C59 Fe2 C60 139.4(3) . 2_756 ?
C57 Fe2 C60 112.0(4) . 2_756 ?
C57 Fe2 C60 68.0(4) 2_756 2_756 ?
C60 Fe2 C60 179.998(1) . 2_756 ?
C56 Fe2 C58 111.6(4) 2_756 . ?
C56 Fe2 C58 68.4(4) . . ?
C59 Fe2 C58 139.2(4) 2_756 . ?
C59 Fe2 C58 40.8(4) . . ?
C57 Fe2 C58 39.5(4) . . ?
C57 Fe2 C58 140.5(4) 2_756 . ?
C60 Fe2 C58 68.4(4) . . ?
C60 Fe2 C58 111.6(4) 2_756 . ?
C56 Fe2 C58 68.4(4) 2_756 2_756 ?
C56 Fe2 C58 111.6(4) . 2_756 ?
C59 Fe2 C58 40.8(4) 2_756 2_756 ?
C59 Fe2 C58 139.2(4) . 2_756 ?
C57 Fe2 C58 140.5(4) . 2_756 ?
C57 Fe2 C58 39.5(4) 2_756 2_756 ?
C60 Fe2 C58 111.6(4) . 2_756 ?
C60 Fe2 C58 68.4(4) 2_756 2_756 ?
C58 Fe2 C58 179.999(2) . 2_756 ?
O5 P2 O7 103.3(4) . . ?
O5 P2 C56 96.0(4) . . ?
O7 P2 C56 100.2(4) . . ?
O5 P2 Ru2 118.7(3) . . ?
O7 P2 Ru2 106.3(3) . . ?
C56 P2 Ru2 128.7(3) . . ?
C36 O5 P2 130.9(6) . . ?
C41 O6 C42 116.9(8) . . ?
C46 O7 P2 122.9(6) . . ?
C51 O8 C52 118.0(9) . . ?
O5 C36 C37 120.4(8) . . ?
O5 C36 C41 121.3(10) . . ?
C37 C36 C41 117.2(10) . . ?
C36 C37 C38 121.7(10) . . ?
C36 C37 H37 119.2 . . ?
C38 C37 H37 119.2 . . ?
C37 C38 C39 119.1(11) . . ?
C37 C38 H38 120.5 . . ?
C39 C38 H38 120.5 . . ?
C40 C39 C38 119.5(9) . . ?
C40 C39 C43 121.0(10) . . ?
C38 C39 C43 119.4(11) . . ?
C39 C40 C41 121.6(10) . . ?
C39 C40 H40 119.2 . . ?
C41 C40 H40 119.2 . . ?
O6 C41 C40 125.6(9) . . ?
O6 C41 C36 113.6(9) . . ?
C40 C41 C36 120.7(11) . . ?
O6 C42 H42A 109.5 . . ?
O6 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
O6 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 C39 108.4(10) . . ?
C44 C43 H43A 110.0 . . ?
C39 C43 H43A 110.0 . . ?
C44 C43 H43B 110.0 . . ?
C39 C43 H43B 110.0 . . ?
H43A C43 H43B 108.4 . . ?
C45 C44 C43 125.6(18) . . ?
C45 C44 H44 117.2 . . ?
C43 C44 H44 117.2 . . ?
C44 C45 H45A 120.0 . . ?
C44 C45 H45B 120.0 . . ?
H45A C45 H45B 120.0 . . ?
C51 C46 C47 122.4(10) . . ?
C51 C46 O7 116.3(9) . . ?
C47 C46 O7 121.3(9) . . ?
C46 C47 C48 118.8(10) . . ?
C46 C47 H47 120.6 . . ?
C48 C47 H47 120.6 . . ?
C49 C48 C47 119.7(10) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C48 C49 C50 119.6(9) . . ?
C48 C49 C53A 116.0(14) . . ?
C50 C49 C53A 123.8(15) . . ?
C48 C49 C53 123.1(15) . . ?
C50 C49 C53 116.5(15) . . ?
C53A C49 C53 18.2(17) . . ?
C51 C50 C49 120.8(11) . . ?
C51 C50 H50 119.6 . . ?
C49 C50 H50 119.6 . . ?
O8 C51 C46 116.6(10) . . ?
O8 C51 C50 124.7(11) . . ?
C46 C51 C50 118.7(10) . . ?
O8 C52 H52A 109.5 . . ?
O8 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
O8 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 C49 111.9(19) . . ?
C54 C53 H53A 109.2 . . ?
C49 C53 H53A 109.2 . . ?
C54 C53 H53B 109.2 . . ?
C49 C53 H53B 109.2 . . ?
H53A C53 H53B 107.9 . . ?
C55 C54 C53 110(3) . . ?
C55 C54 H54 124.8 . . ?
C53 C54 H54 124.8 . . ?
C54 C55 H55A 120.0 . . ?
C54 C55 H55B 120.0 . . ?
H55A C55 H55B 120.0 . . ?
C54A C53A C49 115.4(18) . . ?
C54A C53A H53C 108.4 . . ?
C49 C53A H53C 108.4 . . ?
C54A C53A H53D 108.4 . . ?
C49 C53A H53D 108.4 . . ?
H53C C53A H53D 107.5 . . ?
C55A C54A C53A 136(3) . . ?
C55A C54A H54A 111.8 . . ?
C53A C54A H54A 111.8 . . ?
C54A C55A H55C 120.0 . . ?
C54A C55A H55D 120.0 . . ?
H55C C55A H55D 120.0 . . ?
C60 C56 C57 107.5(8) . . ?
C60 C56 P2 127.4(7) . . ?
C57 C56 P2 123.4(8) . . ?
C60 C56 Fe2 70.6(6) . . ?
C57 C56 Fe2 69.9(5) . . ?
P2 C56 Fe2 136.5(6) . . ?
C58 C57 C56 109.0(9) . . ?
C58 C57 Fe2 70.5(6) . . ?
C56 C57 Fe2 69.0(5) . . ?
C58 C57 H57 125.5 . . ?
C56 C57 H57 125.5 . . ?
Fe2 C57 H57 126.6 . . ?
C57 C58 C59 107.6(9) . . ?
C57 C58 Fe2 69.9(6) . . ?
C59 C58 Fe2 69.2(6) . . ?
C57 C58 H58 126.2 . . ?
C59 C58 H58 126.2 . . ?
Fe2 C58 H58 126.2 . . ?
C60 C59 C58 108.2(8) . . ?
C60 C59 Fe2 70.0(6) . . ?
C58 C59 Fe2 70.0(6) . . ?
C60 C59 H59 125.9 . . ?
C58 C59 H59 125.9 . . ?
Fe2 C59 H59 125.7 . . ?
C56 C60 C59 107.7(8) . . ?
C56 C60 Fe2 69.2(6) . . ?
C59 C60 Fe2 69.3(6) . . ?
C56 C60 H60 126.1 . . ?
C59 C60 H60 126.1 . . ?
Fe2 C60 H60 126.9 . . ?
C66 C61 C62 116.2(11) . . ?
C66 C61 C67 123.4(11) . . ?
C62 C61 C67 120.3(10) . . ?
C66 C61 Ru2 69.5(6) . . ?
C62 C61 Ru2 71.2(6) . . ?
C67 C61 Ru2 131.6(7) . . ?
C63 C62 C61 123.6(10) . . ?
C63 C62 Ru2 73.5(6) . . ?
C61 C62 Ru2 71.2(5) . . ?
C63 C62 H62 118.2 . . ?
C61 C62 H62 118.2 . . ?
Ru2 C62 H62 130.0 . . ?
C62 C63 C64 120.3(11) . . ?
C62 C63 Ru2 71.1(6) . . ?
C64 C63 Ru2 70.2(6) . . ?
C62 C63 H63 119.9 . . ?
C64 C63 H63 119.9 . . ?
Ru2 C63 H63 131.7 . . ?
C65 C64 C63 117.7(11) . . ?
C65 C64 C70 123.7(11) . . ?
C63 C64 C70 118.6(11) . . ?
C65 C64 Ru2 69.5(6) . . ?
C63 C64 Ru2 72.9(6) . . ?
C70 C64 Ru2 128.2(8) . . ?
C64 C65 C66 121.5(10) . . ?
C64 C65 Ru2 73.1(6) . . ?
C66 C65 Ru2 70.9(6) . . ?
C64 C65 H65 119.3 . . ?
C66 C65 H65 119.3 . . ?
Ru2 C65 H65 129.1 . . ?
C61 C66 C65 120.7(11) . . ?
C61 C66 Ru2 73.5(6) . . ?
C65 C66 Ru2 70.8(6) . . ?
C61 C66 H66 119.6 . . ?
C65 C66 H66 119.6 . . ?
Ru2 C66 H66 128.2 . . ?
C61 C67 C68 112.6(10) . . ?
C61 C67 C69 109.2(10) . . ?
C68 C67 C69 110.4(11) . . ?
C61 C67 H67 108.2 . . ?
C68 C67 H67 108.2 . . ?
C69 C67 H67 108.2 . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C64 C70 H70A 109.5 . . ?
C64 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C64 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full 26.87
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max 1.179
_refine_diff_density_min -0.971
_refine_diff_density_rms 0.139
_database_code_depnum_ccdc_archive 'CCDC 933867'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_msb433_0m
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C200 H208 Cu10 Fe4 I10 O32 P8'
_chemical_formula_sum 'C200 H208 Cu10 Fe4 I10 O32 P8'
_chemical_formula_weight 5499.33
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Triclinic
_symmetry_space_group_name_H-M P-1
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 14.6299(14)
_cell_length_b 16.1611(15)
_cell_length_c 24.111(2)
_cell_angle_alpha 71.670(1)
_cell_angle_beta 80.188(1)
_cell_angle_gamma 71.003(1)
_cell_volume 5102.1(8)
_cell_formula_units_Z 1
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9991
_cell_measurement_theta_min 2.23
_cell_measurement_theta_max 27.46
_exptl_crystal_description Plate
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.08
_exptl_crystal_size_min 0.02
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.790
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2708
_exptl_absorpt_coefficient_mu 2.936
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7390
_exptl_absorpt_correction_T_max 0.9436
_exptl_absorpt_process_details 'SADABs (Sheldrick, 2008a)'
_exptl_special_details
;
The diffraction data were collected in three sets of
606 frames (0.3 deg. width in omega) at phi = 0, 120
and 240 deg. A scan time of 80 sec/frame was used.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Smart APEX CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 42697
_diffrn_reflns_av_R_equivalents 0.0642
_diffrn_reflns_av_sigmaI/netI 0.1191
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -20
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -30
_diffrn_reflns_limit_l_max 30
_diffrn_reflns_theta_min 1.39
_diffrn_reflns_theta_max 26.75
_reflns_number_total 21465
_reflns_number_gt 12644
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009a)'
_computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009a)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms were placed in
calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding
contributions with isotropic displacement parameters 1.2 - 1.5 times those
of the attached carbon atoms. The whole allylphenoxy group based on O4 is
disordered over two sites in a 64/36 ratio while the allyl group based on
C95 is disordered over two sites in a 61/39 ratio. Both disordered groups
were refined subject to restraints that the two components of each disorder
have the same geometry. Additionally, Cu5 is disordered over two sites in a
1/1 ratio.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0811P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 21465
_refine_ls_number_parameters 1220
_refine_ls_number_restraints 48
_refine_ls_R_factor_all 0.1275
_refine_ls_R_factor_gt 0.0649
_refine_ls_wR_factor_ref 0.1720
_refine_ls_wR_factor_gt 0.1437
_refine_ls_goodness_of_fit_ref 0.994
_refine_ls_restrained_S_all 0.993
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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
I1 I 0.25324(5) 0.68860(4) 0.21206(3) 0.02531(15) Uani 1 1 d . . .
I2 I 0.32202(5) 0.60428(4) 0.39296(3) 0.02798(16) Uani 1 1 d . . .
I3 I 0.03375(5) 0.75886(5) 0.35111(3) 0.03354(17) Uani 1 1 d . . .
I4 I 0.09709(5) 0.50891(4) 0.31245(3) 0.03346(17) Uani 1 1 d . . .
I5 I 0.39328(5) 0.40230(4) 0.29305(3) 0.03228(17) Uani 1 1 d . . .
Cu1 Cu 0.24211(9) 0.50542(8) 0.23137(5) 0.0306(3) Uani 1 1 d . A .
Cu2 Cu 0.07569(9) 0.68235(8) 0.26382(5) 0.0271(3) Uani 1 1 d . A .
Cu3 Cu 0.21984(8) 0.74163(7) 0.31169(5) 0.0252(3) Uani 1 1 d . A .
Cu4 Cu 0.13818(8) 0.66526(7) 0.44053(5) 0.0225(3) Uani 1 1 d . . .
Cu5 Cu 0.3112(3) 0.5627(3) 0.3042(2) 0.0362(8) Uani 0.502(5) 1 d P A 1
Cu5A Cu 0.2734(3) 0.5449(3) 0.3163(2) 0.0362(8) Uani 0.498(5) 1 d P A 2
Fe1 Fe 0.01240(9) 0.64791(8) 0.09243(5) 0.0191(3) Uani 1 1 d . A .
Fe2 Fe 0.20348(9) 0.94227(8) 0.41181(6) 0.0207(3) Uani 1 1 d . A .
P1 P -0.04523(18) 0.74644(16) 0.20615(10) 0.0210(5) Uani 1 1 d . . .
P2 P 0.22812(17) 0.49897(16) 0.14367(10) 0.0212(5) Uani 1 1 d . . .
P3 P 0.23432(17) 0.88158(16) 0.28573(11) 0.0205(5) Uani 1 1 d . . .
P4 P 0.13457(16) 0.75547(15) 0.49485(10) 0.0175(5) Uani 1 1 d . . .
O1 O -0.1337(5) 0.6990(5) 0.2241(3) 0.0282(15) Uani 1 1 d . A .
O2 O -0.1487(5) 0.5327(4) 0.2543(3) 0.0305(16) Uani 1 1 d . . .
O3 O -0.1018(5) 0.8514(4) 0.2079(3) 0.0338(17) Uani 1 1 d D A .
O5 O 0.2672(4) 0.5669(4) 0.0859(3) 0.0268(15) Uani 1 1 d . A .
O6 O 0.3052(5) 0.6649(5) -0.0184(3) 0.0370(17) Uani 1 1 d . . .
O7 O 0.2876(4) 0.4011(4) 0.1293(3) 0.0285(15) Uani 1 1 d . A .
O8 O 0.1755(4) 0.3306(4) 0.2195(3) 0.0292(16) Uani 1 1 d . . .
O9 O 0.1892(4) 0.9332(4) 0.2226(3) 0.0222(14) Uani 1 1 d . A .
O10 O 0.3028(5) 1.0421(4) 0.1660(3) 0.0379(18) Uani 1 1 d . . .
O11 O 0.3418(4) 0.8947(4) 0.2779(3) 0.0239(14) Uani 1 1 d . A .
O12 O 0.4775(5) 0.7762(5) 0.3459(3) 0.0327(17) Uani 1 1 d . . .
O13 O 0.0307(4) 0.8296(4) 0.5063(3) 0.0188(13) Uani 1 1 d . A .
O14 O -0.1009(4) 0.9296(4) 0.4299(3) 0.0236(14) Uani 1 1 d . . .
O15 O 0.1600(4) 0.6903(4) 0.5604(3) 0.0202(13) Uani 1 1 d . A .
O16 O 0.3492(4) 0.6393(4) 0.5653(3) 0.0325(17) Uani 1 1 d . . .
C1 C -0.0264(7) 0.7537(5) 0.1300(4) 0.021(2) Uani 1 1 d . A .
C2 C -0.0962(7) 0.7662(6) 0.0895(4) 0.025(2) Uani 1 1 d . . .
H2 H -0.1631 0.7707 0.0989 0.031 Uiso 1 1 calc R A .
C3 C -0.0461(7) 0.7705(6) 0.0337(4) 0.021(2) Uani 1 1 d . A .
H3 H -0.0743 0.7798 -0.0013 0.026 Uiso 1 1 calc R . .
C4 C 0.0532(7) 0.7588(6) 0.0381(4) 0.025(2) Uani 1 1 d . . .
H4 H 0.1025 0.7587 0.0069 0.030 Uiso 1 1 calc R A .
C5 C 0.0657(7) 0.7473(5) 0.0969(4) 0.021(2) Uani 1 1 d . A .
H5 H 0.1253 0.7371 0.1122 0.025 Uiso 1 1 calc R . .
C6 C 0.1104(6) 0.5237(6) 0.1194(4) 0.021(2) Uani 1 1 d . A .
C7 C 0.0875(7) 0.5390(5) 0.0613(4) 0.022(2) Uani 1 1 d . . .
H7 H 0.1316 0.5401 0.0275 0.026 Uiso 1 1 calc R A .
C8 C -0.0133(7) 0.5522(6) 0.0635(4) 0.023(2) Uani 1 1 d . A .
H8 H -0.0484 0.5632 0.0310 0.028 Uiso 1 1 calc R . .
C9 C -0.0538(7) 0.5466(6) 0.1220(4) 0.022(2) Uani 1 1 d . . .
H9 H -0.1202 0.5535 0.1352 0.027 Uiso 1 1 calc R A .
C10 C 0.0231(6) 0.5287(6) 0.1576(4) 0.021(2) Uani 1 1 d . A .
H10 H 0.0176 0.5214 0.1986 0.025 Uiso 1 1 calc R . .
C11 C -0.1582(7) 0.6614(7) 0.2825(4) 0.027(2) Uani 1 1 d . . .
C12 C -0.1738(7) 0.7056(6) 0.3247(4) 0.027(2) Uani 1 1 d . A .
H12 H -0.1726 0.7671 0.3139 0.032 Uiso 1 1 calc R . .
C13 C -0.1916(7) 0.6610(6) 0.3836(4) 0.026(2) Uani 1 1 d . . .
H13 H -0.1969 0.6904 0.4129 0.031 Uiso 1 1 calc R A .
C14 C -0.2016(6) 0.5734(6) 0.3993(4) 0.024(2) Uani 1 1 d . A .
C15 C -0.2185(7) 0.5213(6) 0.4620(4) 0.029(2) Uani 1 1 d . . .
H15A H -0.2597 0.4823 0.4640 0.043 Uiso 1 1 calc R A .
H15B H -0.2526 0.5643 0.4855 0.043 Uiso 1 1 calc R . .
C16 C -0.1223(7) 0.4626(6) 0.4866(4) 0.028(2) Uani 1 1 d . . .
H16 H -0.0791 0.4246 0.4644 0.033 Uiso 1 1 calc R . .
C17 C -0.0929(9) 0.4597(7) 0.5370(5) 0.042(3) Uani 1 1 d . . .
H17A H -0.1338 0.4966 0.5606 0.051 Uiso 1 1 calc R A .
H17B H -0.0312 0.4207 0.5492 0.051 Uiso 1 1 calc R . .
C18 C -0.1904(7) 0.5316(6) 0.3551(4) 0.024(2) Uani 1 1 d . . .
H18 H -0.1993 0.4729 0.3647 0.029 Uiso 1 1 calc R A .
C19 C -0.1669(7) 0.5735(7) 0.2981(4) 0.027(2) Uani 1 1 d . A .
C20 C -0.1454(8) 0.4392(7) 0.2711(5) 0.038(3) Uani 1 1 d . . .
H20A H -0.1026 0.4055 0.3031 0.056 Uiso 1 1 calc R . .
H20B H -0.1204 0.4142 0.2376 0.056 Uiso 1 1 calc R . .
H20C H -0.2108 0.4334 0.2843 0.056 Uiso 1 1 calc R . .
O4 O -0.0547(11) 0.9737(8) 0.1224(6) 0.041(4) Uani 0.640(7) 1 d PD A 1
C21 C -0.1732(7) 0.9028(7) 0.1688(5) 0.030(4) Uani 0.640(7) 1 d PGD A 1
C22 C -0.2645(8) 0.8910(7) 0.1741(4) 0.038(4) Uani 0.640(7) 1 d PG A 1
H22 H -0.2825 0.8462 0.2066 0.046 Uiso 0.640(7) 1 calc PR A 1
C23 C -0.3297(6) 0.9446(8) 0.1320(5) 0.049(5) Uani 0.640(7) 1 d PG A 1
H23 H -0.3921 0.9365 0.1356 0.059 Uiso 0.640(7) 1 calc PR A 1
C24 C -0.3035(8) 1.0100(8) 0.0844(5) 0.051(5) Uani 0.640(7) 1 d PGD A 1
C28 C -0.2121(9) 1.0219(7) 0.0790(4) 0.046(5) Uani 0.640(7) 1 d PG A 1
H28 H -0.1942 1.0666 0.0465 0.056 Uiso 0.640(7) 1 calc PR A 1
C29 C -0.1469(7) 0.9682(7) 0.1212(5) 0.031(4) Uani 0.640(7) 1 d PGD A 1
C25 C -0.3722(17) 1.0663(15) 0.0366(8) 0.083(7) Uani 0.640(7) 1 d PD A 1
H25A H -0.4290 1.0427 0.0440 0.100 Uiso 0.640(7) 1 calc PR A 1
H25B H -0.3959 1.1300 0.0389 0.100 Uiso 0.640(7) 1 calc PR A 1
C26 C -0.3273(18) 1.0655(17) -0.0237(9) 0.074(6) Uani 0.640(7) 1 d PDU A 1
H26A H -0.3018 1.0117 -0.0362 0.089 Uiso 0.640(7) 1 calc PR A 1
C27 C -0.327(3) 1.148(2) -0.0583(15) 0.147(13) Uani 0.640(7) 1 d PDU A 1
H27A H -0.3534 1.1995 -0.0435 0.176 Uiso 0.640(7) 1 calc PR A 1
H27B H -0.2999 1.1549 -0.0976 0.176 Uiso 0.640(7) 1 calc PR A 1
C30 C -0.0251(18) 1.0447(13) 0.0770(7) 0.061(6) Uani 0.640(7) 1 d PD A 1
H30A H 0.0410 1.0418 0.0822 0.091 Uiso 0.640(7) 1 calc PR A 1
H30B H -0.0693 1.1042 0.0792 0.091 Uiso 0.640(7) 1 calc PR A 1
H30C H -0.0269 1.0366 0.0386 0.091 Uiso 0.640(7) 1 calc PR A 1
O4A O 0.0069(16) 0.9508(15) 0.1233(10) 0.041(4) Uani 0.360(7) 1 d PD A 2
C21A C -0.1411(16) 0.9209(14) 0.1582(8) 0.030(4) Uani 0.360(7) 1 d PGD A 2
C22A C -0.2386(15) 0.9340(14) 0.1537(8) 0.038(4) Uani 0.360(7) 1 d PG A 2
H22A H -0.2734 0.8987 0.1833 0.046 Uiso 0.360(7) 1 calc PR A 2
C23A C -0.2852(11) 0.9989(16) 0.1060(10) 0.049(5) Uani 0.360(7) 1 d PG A 2
H23A H -0.3518 1.0078 0.1029 0.059 Uiso 0.360(7) 1 calc PR A 2
C24A C -0.2343(16) 1.0505(14) 0.0627(8) 0.051(5) Uani 0.360(7) 1 d PGD A 2
C28A C -0.1368(16) 1.0374(13) 0.0672(8) 0.046(5) Uani 0.360(7) 1 d PG A 2
H28A H -0.1021 1.0727 0.0376 0.056 Uiso 0.360(7) 1 calc PR A 2
C29A C -0.0902(12) 0.9726(16) 0.1150(10) 0.031(4) Uani 0.360(7) 1 d PGD A 2
C25A C -0.275(3) 1.120(2) 0.0065(13) 0.083(7) Uani 0.360(7) 1 d PD A 2
H25C H -0.2388 1.1651 -0.0089 0.100 Uiso 0.360(7) 1 calc PR A 2
H25D H -0.3443 1.1522 0.0144 0.100 Uiso 0.360(7) 1 calc PR A 2
C26A C -0.266(3) 1.065(3) -0.0392(15) 0.074(6) Uani 0.360(7) 1 d PDU A 2
H26D H -0.2676 1.0040 -0.0285 0.089 Uiso 0.360(7) 1 calc PR A 2
C27A C -0.256(5) 1.111(4) -0.0908(18) 0.147(13) Uani 0.360(7) 1 d PDU A 2
H27C H -0.2543 1.1721 -0.0989 0.176 Uiso 0.360(7) 1 calc PR A 2
H27D H -0.2491 1.0849 -0.1220 0.176 Uiso 0.360(7) 1 calc PR A 2
C30A C 0.059(3) 1.009(2) 0.0818(13) 0.061(6) Uani 0.360(7) 1 d PD A 2
H30D H 0.1260 0.9898 0.0916 0.091 Uiso 0.360(7) 1 calc PR A 2
H30E H 0.0279 1.0722 0.0834 0.091 Uiso 0.360(7) 1 calc PR A 2
H30F H 0.0568 1.0053 0.0423 0.091 Uiso 0.360(7) 1 calc PR A 2
C31 C 0.3624(6) 0.5695(6) 0.0734(4) 0.023(2) Uani 1 1 d . . .
C32 C 0.4341(7) 0.5256(7) 0.1113(5) 0.034(2) Uani 1 1 d . A .
H32 H 0.4199 0.4904 0.1496 0.040 Uiso 1 1 calc R . .
C33 C 0.5285(7) 0.5324(7) 0.0937(5) 0.035(3) Uani 1 1 d . . .
H33 H 0.5774 0.5023 0.1205 0.043 Uiso 1 1 calc R A .
C34 C 0.5510(7) 0.5816(7) 0.0385(4) 0.027(2) Uani 1 1 d . A .
C35 C 0.6528(7) 0.5877(8) 0.0178(5) 0.042(3) Uani 1 1 d . . .
H35A H 0.6955 0.5515 0.0501 0.051 Uiso 1 1 calc R A .
H35B H 0.6766 0.5598 -0.0151 0.051 Uiso 1 1 calc R . .
C36 C 0.6611(9) 0.6828(10) -0.0021(5) 0.058(4) Uani 1 1 d . A .
H36 H 0.6152 0.7275 -0.0278 0.069 Uiso 1 1 calc R . .
C37 C 0.7256(9) 0.7092(10) 0.0128(6) 0.068(4) Uani 1 1 d . . .
H37A H 0.7729 0.6667 0.0385 0.081 Uiso 1 1 calc R A .
H37B H 0.7255 0.7711 -0.0018 0.081 Uiso 1 1 calc R . .
C38 C 0.4763(7) 0.6265(7) -0.0003(5) 0.035(3) Uani 1 1 d . . .
H38 H 0.4907 0.6615 -0.0387 0.042 Uiso 1 1 calc R A .
C39 C 0.3823(8) 0.6205(7) 0.0164(5) 0.035(3) Uani 1 1 d . A .
C40 C 0.3257(8) 0.7170(8) -0.0761(5) 0.042(3) Uani 1 1 d . . .
H40A H 0.3576 0.7608 -0.0742 0.063 Uiso 1 1 calc R . .
H40B H 0.2651 0.7499 -0.0952 0.063 Uiso 1 1 calc R . .
H40C H 0.3687 0.6763 -0.0985 0.063 Uiso 1 1 calc R . .
C41 C 0.3297(7) 0.3238(6) 0.1735(4) 0.026(2) Uani 1 1 d . . .
C42 C 0.4280(7) 0.2840(7) 0.1705(5) 0.037(3) Uani 1 1 d . A .
H42 H 0.4680 0.3097 0.1390 0.044 Uiso 1 1 calc R . .
C43 C 0.4693(8) 0.2049(7) 0.2143(5) 0.037(3) Uani 1 1 d . . .
H43 H 0.5367 0.1747 0.2106 0.044 Uiso 1 1 calc R A .
C44 C 0.4127(8) 0.1707(7) 0.2627(5) 0.035(3) Uani 1 1 d . A .
C45 C 0.4589(8) 0.0884(7) 0.3140(5) 0.044(3) Uani 1 1 d . . .
H45A H 0.5068 0.1041 0.3302 0.053 Uiso 1 1 calc R A .
H45B H 0.4076 0.0771 0.3455 0.053 Uiso 1 1 calc R . .
C46 C 0.5059(9) 0.0067(8) 0.2967(6) 0.059(4) Uani 1 1 d . A .
H46 H 0.4704 -0.0095 0.2743 0.071 Uiso 1 1 calc R . .
C47 C 0.5936(10) -0.0485(10) 0.3086(7) 0.086(5) Uani 1 1 d . . .
H47A H 0.6321 -0.0354 0.3308 0.103 Uiso 1 1 calc R A .
H47B H 0.6182 -0.1013 0.2949 0.103 Uiso 1 1 calc R . .
C48 C 0.3141(7) 0.2118(6) 0.2655(5) 0.033(2) Uani 1 1 d . . .
H48 H 0.2745 0.1889 0.2984 0.039 Uiso 1 1 calc R A .
C49 C 0.2713(7) 0.2880(7) 0.2197(5) 0.032(2) Uani 1 1 d . A .
C50 C 0.1145(8) 0.2934(7) 0.2664(5) 0.038(3) Uani 1 1 d . . .
H50A H 0.1145 0.2341 0.2637 0.057 Uiso 1 1 calc R . .
H50B H 0.0484 0.3347 0.2640 0.057 Uiso 1 1 calc R . .
H50C H 0.1386 0.2856 0.3037 0.057 Uiso 1 1 calc R . .
C51 C 0.1777(7) 0.9608(6) 0.3280(4) 0.020(2) Uani 1 1 d . A .
C52 C 0.0898(6) 0.9654(6) 0.3651(4) 0.023(2) Uani 1 1 d . . .
H52 H 0.0495 0.9272 0.3712 0.028 Uiso 1 1 calc R A .
C53 C 0.0732(7) 1.0370(6) 0.3913(4) 0.026(2) Uani 1 1 d . A .
H53 H 0.0200 1.0547 0.4180 0.032 Uiso 1 1 calc R . .
C54 C 0.1494(7) 1.0773(6) 0.3708(4) 0.030(2) Uani 1 1 d . . .
H54 H 0.1565 1.1267 0.3813 0.036 Uiso 1 1 calc R A .
C55 C 0.2140(7) 1.0308(6) 0.3316(4) 0.026(2) Uani 1 1 d . A .
H55 H 0.2714 1.0441 0.3113 0.031 Uiso 1 1 calc R . .
C56 C 0.2111(6) 0.8275(5) 0.4790(4) 0.0150(18) Uani 1 1 d . A .
C57 C 0.1995(7) 0.9055(6) 0.5008(4) 0.024(2) Uani 1 1 d . . .
H57 H 0.1475 0.9291 0.5263 0.029 Uiso 1 1 calc R A .
C58 C 0.2804(7) 0.9397(7) 0.4768(4) 0.031(2) Uani 1 1 d . A .
H58 H 0.2924 0.9896 0.4839 0.037 Uiso 1 1 calc R . .
C59 C 0.3405(6) 0.8853(6) 0.4400(4) 0.025(2) Uani 1 1 d . . .
H59 H 0.3987 0.8939 0.4179 0.030 Uiso 1 1 calc R A .
C60 C 0.2984(6) 0.8165(6) 0.4420(4) 0.025(2) Uani 1 1 d . A .
H60 H 0.3243 0.7709 0.4219 0.030 Uiso 1 1 calc R . .
C61 C 0.1481(6) 1.0286(6) 0.2007(4) 0.021(2) Uani 1 1 d . . .
C62 C 0.0487(7) 1.0635(7) 0.2078(4) 0.030(2) Uani 1 1 d . A .
H62 H 0.0095 1.0253 0.2289 0.036 Uiso 1 1 calc R . .
C63 C 0.0072(7) 1.1567(7) 0.1832(4) 0.033(2) Uani 1 1 d . . .
H63 H -0.0612 1.1814 0.1871 0.039 Uiso 1 1 calc R A .
C64 C 0.0634(7) 1.2141(6) 0.1532(4) 0.025(2) Uani 1 1 d . A .
C65 C 0.0169(8) 1.3156(6) 0.1288(5) 0.037(3) Uani 1 1 d . . .
H65A H -0.0061 1.3433 0.1618 0.044 Uiso 1 1 calc R A .
H65B H 0.0665 1.3434 0.1042 0.044 Uiso 1 1 calc R . .
C66 C -0.0652(8) 1.3370(7) 0.0937(5) 0.036(3) Uani 1 1 d . A .
H66 H -0.0505 1.3204 0.0580 0.043 Uiso 1 1 calc R . .
C67 C -0.1561(8) 1.3766(7) 0.1067(5) 0.047(3) Uani 1 1 d . . .
H67A H -0.1744 1.3945 0.1419 0.056 Uiso 1 1 calc R A .
H67B H -0.2038 1.3874 0.0810 0.056 Uiso 1 1 calc R . .
C68 C 0.1620(7) 1.1767(6) 0.1466(4) 0.031(2) Uani 1 1 d . . .
H68 H 0.2010 1.2148 0.1248 0.037 Uiso 1 1 calc R A .
C69 C 0.2065(6) 1.0840(6) 0.1712(4) 0.024(2) Uani 1 1 d . A .
C70 C 0.3657(8) 1.0942(8) 0.1370(6) 0.053(3) Uani 1 1 d . . .
H70A H 0.3503 1.1229 0.0961 0.079 Uiso 1 1 calc R . .
H70B H 0.4328 1.0547 0.1385 0.079 Uiso 1 1 calc R . .
H70C H 0.3582 1.1414 0.1563 0.079 Uiso 1 1 calc R . .
C71 C 0.4194(6) 0.8352(6) 0.2528(4) 0.024(2) Uani 1 1 d . . .
C72 C 0.4242(6) 0.8399(6) 0.1950(4) 0.025(2) Uani 1 1 d . A .
H72 H 0.3738 0.8818 0.1714 0.029 Uiso 1 1 calc R . .
C73 C 0.5034(7) 0.7830(7) 0.1705(4) 0.029(2) Uani 1 1 d . . .
H73 H 0.5066 0.7854 0.1304 0.035 Uiso 1 1 calc R A .
C74 C 0.5771(7) 0.7233(7) 0.2050(5) 0.033(2) Uani 1 1 d . A .
C75 C 0.6610(8) 0.6610(7) 0.1791(5) 0.038(3) Uani 1 1 d . . .
H75A H 0.7220 0.6644 0.1897 0.046 Uiso 1 1 calc R A .
H75B H 0.6607 0.6826 0.1359 0.046 Uiso 1 1 calc R . .
C76 C 0.6600(8) 0.5637(8) 0.1990(5) 0.043(3) Uani 1 1 d . A .
H76 H 0.7128 0.5219 0.1840 0.052 Uiso 1 1 calc R . .
C77 C 0.5963(9) 0.5299(9) 0.2340(6) 0.055(4) Uani 1 1 d . . .
H77A H 0.5418 0.5683 0.2504 0.067 Uiso 1 1 calc R A .
H77B H 0.6037 0.4665 0.2434 0.067 Uiso 1 1 calc R . .
C78 C 0.5718(7) 0.7198(7) 0.2637(5) 0.034(2) Uani 1 1 d . . .
H78 H 0.6230 0.6790 0.2871 0.040 Uiso 1 1 calc R A .
C79 C 0.4909(7) 0.7763(6) 0.2892(4) 0.028(2) Uani 1 1 d . A .
C80 C 0.5448(7) 0.7100(8) 0.3856(5) 0.047(3) Uani 1 1 d . . .
H80A H 0.5476 0.6489 0.3850 0.070 Uiso 1 1 calc R . .
H80B H 0.5240 0.7165 0.4252 0.070 Uiso 1 1 calc R . .
H80C H 0.6091 0.7191 0.3739 0.070 Uiso 1 1 calc R . .
C81 C -0.0568(6) 0.8050(6) 0.5128(4) 0.0190(19) Uani 1 1 d . . .
C82 C -0.0732(6) 0.7344(6) 0.5575(4) 0.024(2) Uani 1 1 d . A .
H82 H -0.0258 0.6991 0.5849 0.029 Uiso 1 1 calc R . .
C83 C -0.1608(6) 0.7141(7) 0.5629(4) 0.028(2) Uani 1 1 d . . .
H83 H -0.1729 0.6644 0.5938 0.034 Uiso 1 1 calc R A .
C84 C -0.2303(7) 0.7665(7) 0.5231(4) 0.030(2) Uani 1 1 d . A .
C85 C -0.3276(7) 0.7475(7) 0.5301(5) 0.033(2) Uani 1 1 d . . .
H85A H -0.3465 0.7543 0.4910 0.040 Uiso 1 1 calc R A .
H85B H -0.3209 0.6838 0.5538 0.040 Uiso 1 1 calc R . .
C86 C -0.4059(7) 0.8104(8) 0.5590(5) 0.043(3) Uani 1 1 d . A .
H86 H -0.4008 0.8044 0.5989 0.051 Uiso 1 1 calc R . .
C87 C -0.4796(10) 0.8719(11) 0.5341(7) 0.083(5) Uani 1 1 d . . .
H87A H -0.4874 0.8801 0.4942 0.100 Uiso 1 1 calc R A .
H87B H -0.5261 0.9090 0.5556 0.100 Uiso 1 1 calc R . .
C88 C -0.2118(6) 0.8384(6) 0.4789(4) 0.021(2) Uani 1 1 d . . .
H88 H -0.2594 0.8748 0.4518 0.025 Uiso 1 1 calc R A .
C89 C -0.1246(6) 0.8590(6) 0.4729(4) 0.021(2) Uani 1 1 d . A .
C90 C -0.1636(7) 0.9764(7) 0.3832(4) 0.032(2) Uani 1 1 d . . .
H90A H -0.1697 0.9326 0.3648 0.049 Uiso 1 1 calc R . .
H90B H -0.1363 1.0217 0.3541 0.049 Uiso 1 1 calc R . .
H90C H -0.2276 1.0070 0.3989 0.049 Uiso 1 1 calc R . .
C91 C 0.1963(7) 0.7158(6) 0.6004(4) 0.023(2) Uani 1 1 d . . .
C92 C 0.1353(7) 0.7640(6) 0.6378(4) 0.025(2) Uani 1 1 d . A .
H92 H 0.0672 0.7838 0.6348 0.030 Uiso 1 1 calc R . .
C93 C 0.1737(8) 0.7830(6) 0.6792(4) 0.036(3) Uani 1 1 d . . .
H93 H 0.1319 0.8145 0.7054 0.043 Uiso 1 1 calc R A .
C94 C 0.2730(8) 0.7563(7) 0.6824(5) 0.049(3) Uani 1 1 d D A .
C95 C 0.3277(11) 0.7910(14) 0.7164(8) 0.034(5) Uani 0.611(13) 1 d PD A 1
H95A H 0.3902 0.7446 0.7275 0.041 Uiso 0.611(13) 1 calc PR A 1
H95B H 0.3416 0.8476 0.6909 0.041 Uiso 0.611(13) 1 calc PR A 1
C96 C 0.2683(12) 0.8087(12) 0.7691(8) 0.037(4) Uani 0.611(13) 1 d PD A 1
H96 H 0.2542 0.7635 0.8035 0.044 Uiso 0.611(13) 1 d PR A 1
C97 C 0.235(2) 0.8823(13) 0.7853(9) 0.033(5) Uani 0.611(13) 1 d PD A 1
H97A H 0.2414 0.9383 0.7577 0.039 Uiso 0.611(13) 1 d PR A 1
H97B H 0.2056 0.8822 0.8240 0.039 Uiso 0.611(13) 1 d PR A 1
C95A C 0.294(2) 0.7633(18) 0.7420(12) 0.034(5) Uani 0.389(13) 1 d PD A 2
H95C H 0.2470 0.7431 0.7736 0.041 Uiso 0.389(13) 1 calc PR A 2
H95D H 0.3603 0.7240 0.7524 0.041 Uiso 0.389(13) 1 calc PR A 2
C96A C 0.2868(19) 0.8597(17) 0.7350(13) 0.037(4) Uani 0.389(13) 1 d PD A 2
H96A H 0.3128 0.9046 0.7064 0.044 Uiso 0.389(13) 1 d PR A 2
C97A C 0.239(4) 0.913(2) 0.7669(14) 0.033(5) Uani 0.389(13) 1 d PD A 2
H97C H 0.2001 0.8924 0.8017 0.039 Uiso 0.389(13) 1 d PR A 2
H97D H 0.2408 0.9753 0.7550 0.039 Uiso 0.389(13) 1 d PR A 2
C98 C 0.3341(7) 0.7074(7) 0.6449(5) 0.044(3) Uani 1 1 d . . .
H98 H 0.4022 0.6879 0.6478 0.053 Uiso 1 1 calc R A .
C99 C 0.2965(7) 0.6873(6) 0.6039(4) 0.027(2) Uani 1 1 d . A .
C100 C 0.4530(8) 0.6098(9) 0.5668(6) 0.062(4) Uani 1 1 d . . .
H10A H 0.4762 0.6625 0.5615 0.093 Uiso 1 1 calc R . .
H10B H 0.4826 0.5811 0.5352 0.093 Uiso 1 1 calc R . .
H10C H 0.4710 0.5657 0.6046 0.093 Uiso 1 1 calc 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
I1 0.0328(4) 0.0242(3) 0.0256(3) -0.0102(3) -0.0042(3) -0.0129(3)
I2 0.0310(4) 0.0236(3) 0.0261(3) -0.0114(3) -0.0072(3) 0.0034(3)
I3 0.0373(4) 0.0341(4) 0.0351(4) -0.0144(3) -0.0103(3) -0.0097(3)
I4 0.0418(4) 0.0271(4) 0.0316(4) -0.0107(3) -0.0088(3) -0.0046(3)
I5 0.0296(4) 0.0295(4) 0.0399(4) -0.0137(3) -0.0155(3) -0.0010(3)
Cu1 0.0338(7) 0.0310(7) 0.0322(7) -0.0128(6) -0.0142(6) -0.0063(5)
Cu2 0.0321(7) 0.0258(6) 0.0234(6) -0.0080(5) -0.0071(5) -0.0048(5)
Cu3 0.0284(6) 0.0177(6) 0.0306(7) -0.0079(5) -0.0061(5) -0.0049(5)
Cu4 0.0260(6) 0.0231(6) 0.0245(6) -0.0124(5) -0.0084(5) -0.0065(5)
Cu5 0.037(2) 0.0399(17) 0.0394(18) -0.0249(14) -0.0132(17) -0.0023(13)
Cu5A 0.037(2) 0.0399(17) 0.0394(18) -0.0249(14) -0.0132(17) -0.0023(13)
Fe1 0.0243(7) 0.0169(6) 0.0182(7) -0.0071(5) -0.0044(5) -0.0051(5)
Fe2 0.0198(7) 0.0186(7) 0.0285(7) -0.0126(6) -0.0016(6) -0.0063(5)
P1 0.0304(14) 0.0165(11) 0.0180(12) -0.0054(10) -0.0060(10) -0.0066(10)
P2 0.0239(13) 0.0202(12) 0.0241(13) -0.0086(10) -0.0056(10) -0.0083(10)
P3 0.0182(12) 0.0184(12) 0.0257(13) -0.0087(10) -0.0047(10) -0.0026(9)
P4 0.0168(11) 0.0185(11) 0.0207(12) -0.0098(10) -0.0066(9) -0.0028(9)
O1 0.029(4) 0.042(4) 0.022(3) -0.011(3) -0.005(3) -0.017(3)
O2 0.037(4) 0.034(4) 0.029(4) -0.015(3) 0.001(3) -0.017(3)
O3 0.054(5) 0.021(3) 0.026(4) -0.010(3) -0.010(3) -0.004(3)
O5 0.024(4) 0.032(4) 0.027(4) -0.008(3) 0.000(3) -0.014(3)
O6 0.035(4) 0.039(4) 0.037(4) -0.002(3) -0.013(3) -0.014(3)
O7 0.025(4) 0.028(4) 0.032(4) -0.012(3) -0.003(3) -0.003(3)
O8 0.022(4) 0.028(4) 0.037(4) -0.006(3) -0.009(3) -0.005(3)
O9 0.027(3) 0.016(3) 0.025(3) -0.008(3) -0.007(3) -0.004(3)
O10 0.032(4) 0.026(4) 0.051(5) -0.007(3) 0.002(4) -0.008(3)
O11 0.020(3) 0.029(4) 0.027(4) -0.018(3) 0.002(3) -0.006(3)
O12 0.023(4) 0.040(4) 0.033(4) -0.020(3) 0.000(3) 0.000(3)
O13 0.014(3) 0.017(3) 0.030(4) -0.010(3) -0.003(3) -0.005(2)
O14 0.022(3) 0.021(3) 0.026(3) -0.002(3) -0.013(3) -0.003(3)
O15 0.025(3) 0.019(3) 0.023(3) -0.013(3) -0.012(3) -0.003(3)
O16 0.022(4) 0.034(4) 0.049(4) -0.025(3) -0.011(3) 0.000(3)
C1 0.038(6) 0.006(4) 0.020(5) -0.005(4) -0.006(4) -0.006(4)
C2 0.029(5) 0.023(5) 0.030(5) -0.014(4) -0.004(4) -0.007(4)
C3 0.029(5) 0.018(5) 0.017(5) -0.001(4) -0.007(4) -0.008(4)
C4 0.041(6) 0.024(5) 0.008(4) -0.001(4) -0.001(4) -0.011(4)
C5 0.034(5) 0.007(4) 0.025(5) -0.003(4) -0.007(4) -0.009(4)
C6 0.028(5) 0.017(4) 0.024(5) -0.011(4) -0.007(4) -0.007(4)
C7 0.029(5) 0.013(4) 0.026(5) -0.014(4) -0.004(4) -0.002(4)
C8 0.034(5) 0.023(5) 0.014(5) -0.002(4) -0.009(4) -0.012(4)
C9 0.028(5) 0.021(5) 0.026(5) -0.009(4) -0.005(4) -0.014(4)
C10 0.024(5) 0.016(4) 0.021(5) 0.000(4) -0.004(4) -0.008(4)
C11 0.025(5) 0.031(5) 0.026(5) -0.008(4) 0.001(4) -0.012(4)
C12 0.026(5) 0.021(5) 0.037(6) -0.007(4) -0.004(4) -0.010(4)
C13 0.028(5) 0.028(5) 0.027(5) -0.015(4) -0.001(4) -0.007(4)
C14 0.009(4) 0.033(5) 0.029(5) -0.007(4) -0.004(4) -0.003(4)
C15 0.036(6) 0.022(5) 0.025(5) -0.011(4) 0.003(4) -0.003(4)
C16 0.039(6) 0.030(5) 0.020(5) -0.005(4) -0.006(4) -0.018(5)
C17 0.064(8) 0.038(6) 0.041(7) -0.001(5) -0.022(6) -0.038(6)
C18 0.028(5) 0.023(5) 0.024(5) -0.007(4) -0.004(4) -0.010(4)
C19 0.025(5) 0.031(5) 0.021(5) -0.003(4) -0.009(4) -0.004(4)
C20 0.040(6) 0.036(6) 0.040(6) -0.016(5) -0.007(5) -0.008(5)
O4 0.075(11) 0.020(7) 0.027(5) -0.002(5) -0.006(9) -0.017(8)
C21 0.047(12) 0.015(8) 0.026(8) -0.006(6) -0.011(8) -0.002(7)
C22 0.042(10) 0.023(9) 0.047(11) -0.018(8) 0.010(8) -0.005(7)
C23 0.031(10) 0.061(13) 0.058(13) -0.034(10) -0.019(9) 0.009(7)
C24 0.080(15) 0.028(9) 0.028(9) -0.001(7) -0.033(9) 0.013(8)
C28 0.071(13) 0.033(9) 0.038(9) -0.010(7) -0.028(10) -0.007(9)
C29 0.045(12) 0.021(7) 0.029(8) -0.009(6) -0.019(9) -0.002(9)
C25 0.110(18) 0.068(14) 0.071(15) -0.012(12) -0.049(13) -0.010(12)
C26 0.076(7) 0.076(7) 0.072(7) -0.020(4) -0.012(4) -0.022(4)
C27 0.148(13) 0.147(13) 0.147(13) -0.041(5) -0.012(4) -0.044(5)
C30 0.106(18) 0.056(13) 0.025(8) -0.001(8) -0.010(12) -0.038(13)
O4A 0.075(11) 0.020(7) 0.027(5) -0.002(5) -0.006(9) -0.017(8)
C21A 0.047(12) 0.015(8) 0.026(8) -0.006(6) -0.011(8) -0.002(7)
C22A 0.042(10) 0.023(9) 0.047(11) -0.018(8) 0.010(8) -0.005(7)
C23A 0.031(10) 0.061(13) 0.058(13) -0.034(10) -0.019(9) 0.009(7)
C24A 0.080(15) 0.028(9) 0.028(9) -0.001(7) -0.033(9) 0.013(8)
C28A 0.071(13) 0.033(9) 0.038(9) -0.010(7) -0.028(10) -0.007(9)
C29A 0.045(12) 0.021(7) 0.029(8) -0.009(6) -0.019(9) -0.002(9)
C25A 0.110(18) 0.068(14) 0.071(15) -0.012(12) -0.049(13) -0.010(12)
C26A 0.076(7) 0.076(7) 0.072(7) -0.020(4) -0.012(4) -0.022(4)
C27A 0.148(13) 0.147(13) 0.147(13) -0.041(5) -0.012(4) -0.044(5)
C30A 0.106(18) 0.056(13) 0.025(8) -0.001(8) -0.010(12) -0.038(13)
C31 0.020(5) 0.024(5) 0.025(5) -0.003(4) 0.002(4) -0.011(4)
C32 0.035(6) 0.038(6) 0.032(6) -0.008(5) -0.005(5) -0.016(5)
C33 0.023(5) 0.044(6) 0.044(7) -0.017(5) -0.014(5) -0.005(5)
C34 0.028(5) 0.031(5) 0.026(5) -0.006(4) -0.001(4) -0.014(4)
C35 0.028(6) 0.051(7) 0.047(7) -0.013(6) -0.002(5) -0.010(5)
C36 0.037(7) 0.083(10) 0.048(8) 0.013(7) -0.013(6) -0.038(7)
C37 0.042(8) 0.079(10) 0.065(9) 0.018(8) -0.004(7) -0.033(7)
C38 0.028(6) 0.044(6) 0.030(6) -0.005(5) -0.004(5) -0.010(5)
C39 0.038(6) 0.023(5) 0.054(7) -0.017(5) -0.011(5) -0.011(5)
C40 0.039(7) 0.047(7) 0.037(7) 0.005(5) -0.008(5) -0.022(6)
C41 0.021(5) 0.024(5) 0.041(6) -0.018(5) -0.006(4) -0.005(4)
C42 0.031(6) 0.034(6) 0.056(7) -0.023(5) -0.013(5) -0.008(5)
C43 0.030(6) 0.033(6) 0.052(7) -0.014(5) -0.015(5) -0.007(5)
C44 0.039(6) 0.031(6) 0.040(6) -0.012(5) -0.018(5) -0.007(5)
C45 0.033(6) 0.033(6) 0.065(8) -0.006(6) -0.012(6) -0.012(5)
C46 0.056(8) 0.036(7) 0.077(10) -0.010(7) -0.021(7) -0.001(6)
C47 0.056(10) 0.058(10) 0.129(15) -0.018(10) -0.010(10) -0.002(8)
C48 0.030(6) 0.023(5) 0.050(7) -0.005(5) -0.014(5) -0.013(4)
C49 0.028(6) 0.028(5) 0.049(7) -0.017(5) -0.011(5) -0.012(4)
C50 0.037(6) 0.040(6) 0.037(6) -0.004(5) -0.007(5) -0.015(5)
C51 0.032(5) 0.012(4) 0.017(5) -0.003(4) -0.005(4) -0.005(4)
C52 0.022(5) 0.019(5) 0.023(5) 0.000(4) -0.005(4) -0.002(4)
C53 0.029(5) 0.020(5) 0.026(5) -0.009(4) 0.001(4) 0.000(4)
C54 0.035(6) 0.016(5) 0.037(6) -0.013(4) 0.012(5) -0.005(4)
C55 0.025(5) 0.026(5) 0.026(5) -0.012(4) 0.007(4) -0.006(4)
C56 0.007(4) 0.015(4) 0.026(5) -0.012(4) -0.002(3) -0.002(3)
C57 0.026(5) 0.023(5) 0.030(5) -0.016(4) -0.011(4) -0.004(4)
C58 0.030(6) 0.032(6) 0.040(6) -0.022(5) -0.013(5) -0.006(4)
C59 0.016(5) 0.031(5) 0.030(5) -0.012(4) -0.003(4) -0.007(4)
C60 0.023(5) 0.029(5) 0.028(5) -0.012(4) -0.010(4) -0.006(4)
C61 0.022(5) 0.012(4) 0.024(5) -0.002(4) -0.008(4) 0.001(4)
C62 0.028(5) 0.031(6) 0.033(6) -0.004(5) -0.005(4) -0.015(4)
C63 0.017(5) 0.032(6) 0.037(6) -0.004(5) -0.003(4) 0.003(4)
C64 0.025(5) 0.017(5) 0.031(5) -0.013(4) -0.013(4) 0.006(4)
C65 0.042(6) 0.014(5) 0.058(7) -0.012(5) -0.006(6) -0.008(4)
C66 0.039(6) 0.029(6) 0.034(6) -0.005(5) -0.004(5) -0.005(5)
C67 0.046(7) 0.042(7) 0.055(8) -0.011(6) -0.016(6) -0.013(6)
C68 0.041(6) 0.019(5) 0.037(6) -0.006(4) -0.010(5) -0.013(4)
C69 0.018(5) 0.025(5) 0.033(5) -0.017(4) -0.006(4) 0.000(4)
C70 0.029(6) 0.041(7) 0.082(10) -0.008(7) 0.011(6) -0.018(5)
C71 0.021(5) 0.019(5) 0.036(6) -0.012(4) -0.002(4) -0.006(4)
C72 0.020(5) 0.028(5) 0.028(5) -0.012(4) -0.005(4) -0.003(4)
C73 0.026(5) 0.035(6) 0.031(6) -0.019(5) -0.006(4) -0.004(4)
C74 0.028(6) 0.037(6) 0.036(6) -0.022(5) 0.004(5) -0.003(5)
C75 0.035(6) 0.037(6) 0.041(7) -0.023(5) 0.002(5) 0.001(5)
C76 0.020(6) 0.055(7) 0.064(8) -0.045(7) -0.008(5) 0.008(5)
C77 0.037(7) 0.053(8) 0.091(11) -0.046(8) -0.006(7) -0.007(6)
C78 0.029(6) 0.033(6) 0.037(6) -0.010(5) -0.010(5) -0.003(5)
C79 0.026(5) 0.029(5) 0.026(5) -0.008(4) 0.000(4) -0.004(4)
C80 0.025(6) 0.076(9) 0.030(6) -0.019(6) -0.005(5) 0.003(6)
C81 0.011(4) 0.026(5) 0.024(5) -0.015(4) 0.001(4) -0.002(4)
C82 0.022(5) 0.022(5) 0.031(5) -0.009(4) -0.008(4) -0.006(4)
C83 0.016(5) 0.034(6) 0.038(6) -0.020(5) 0.004(4) -0.007(4)
C84 0.031(6) 0.033(6) 0.025(5) -0.012(5) 0.004(4) -0.010(5)
C85 0.033(6) 0.042(6) 0.035(6) -0.016(5) 0.008(5) -0.025(5)
C86 0.025(6) 0.056(7) 0.061(8) -0.028(6) -0.004(5) -0.019(5)
C87 0.048(9) 0.103(13) 0.099(13) -0.036(10) -0.029(9) -0.003(9)
C88 0.013(4) 0.021(5) 0.026(5) -0.007(4) -0.007(4) 0.000(4)
C89 0.022(5) 0.016(4) 0.031(5) -0.014(4) -0.001(4) -0.009(4)
C90 0.030(6) 0.032(6) 0.032(6) -0.002(5) -0.011(5) -0.008(5)
C91 0.033(5) 0.020(5) 0.021(5) -0.010(4) -0.015(4) -0.007(4)
C92 0.024(5) 0.018(5) 0.028(5) -0.007(4) -0.012(4) 0.003(4)
C93 0.051(7) 0.025(5) 0.036(6) -0.021(5) -0.022(5) 0.007(5)
C94 0.050(7) 0.038(6) 0.066(8) -0.030(6) -0.040(6) 0.010(5)
C95 0.014(10) 0.052(12) 0.052(14) -0.041(11) -0.010(8) -0.001(7)
C96 0.032(8) 0.044(11) 0.042(11) -0.016(8) -0.023(8) -0.008(8)
C97 0.061(9) 0.029(13) 0.014(12) -0.010(10) 0.009(11) -0.024(12)
C95A 0.014(10) 0.052(12) 0.052(14) -0.041(11) -0.010(8) -0.001(7)
C96A 0.032(8) 0.044(11) 0.042(11) -0.016(8) -0.023(8) -0.008(8)
C97A 0.061(9) 0.029(13) 0.014(12) -0.010(10) 0.009(11) -0.024(12)
C98 0.025(6) 0.042(6) 0.077(9) -0.037(6) -0.027(6) 0.006(5)
C99 0.026(5) 0.021(5) 0.042(6) -0.021(4) -0.013(4) 0.001(4)
C100 0.026(6) 0.081(10) 0.090(11) -0.054(9) -0.008(7) 0.000(6)
_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
I1 Cu5 2.544(5) . ?
I1 Cu2 2.7021(14) . ?
I1 Cu3 2.7140(13) . ?
I1 Cu5A 2.817(5) . ?
I1 Cu1 2.9031(14) . ?
I2 Cu5 2.479(4) . ?
I2 Cu5A 2.616(4) . ?
I2 Cu3 2.6654(12) . ?
I2 Cu4 2.7304(13) . ?
I3 Cu4 2.6149(13) . ?
I3 Cu2 2.6529(13) . ?
I3 Cu3 2.6803(14) . ?
I4 Cu2 2.6109(13) . ?
I4 Cu1 2.6275(15) . ?
I4 Cu5A 2.845(5) . ?
I5 Cu5 2.556(4) . ?
I5 Cu5A 2.560(4) . ?
I5 Cu1 2.6538(13) . ?
Cu1 P2 2.196(3) . ?
Cu1 Cu5A 2.480(5) . ?
Cu1 Cu5 2.682(4) . ?
Cu2 P1 2.208(3) . ?
Cu3 P3 2.220(3) . ?
Cu3 Cu5 2.813(5) . ?
Cu3 Cu5A 2.986(5) . ?
Cu4 C17 2.207(10) 2_566 ?
Cu4 P4 2.230(2) . ?
Cu4 C16 2.302(9) 2_566 ?
Fe1 C6 2.032(9) . ?
Fe1 C5 2.038(8) . ?
Fe1 C7 2.039(8) . ?
Fe1 C2 2.040(9) . ?
Fe1 C8 2.040(9) . ?
Fe1 C10 2.047(8) . ?
Fe1 C9 2.047(9) . ?
Fe1 C3 2.052(8) . ?
Fe1 C1 2.057(8) . ?
Fe1 C4 2.059(9) . ?
Fe2 C55 2.028(9) . ?
Fe2 C56 2.029(8) . ?
Fe2 C51 2.031(9) . ?
Fe2 C57 2.033(9) . ?
Fe2 C52 2.036(9) . ?
Fe2 C54 2.037(9) . ?
Fe2 C60 2.041(9) . ?
Fe2 C53 2.041(9) . ?
Fe2 C59 2.048(9) . ?
Fe2 C58 2.062(9) . ?
P1 O3 1.637(7) . ?
P1 O1 1.641(7) . ?
P1 C1 1.782(9) . ?
P2 O5 1.628(7) . ?
P2 O7 1.650(7) . ?
P2 C6 1.793(9) . ?
P3 O9 1.623(6) . ?
P3 O11 1.626(6) . ?
P3 C51 1.789(9) . ?
P4 O15 1.626(6) . ?
P4 O13 1.644(6) . ?
P4 C56 1.783(9) . ?
O1 C11 1.383(11) . ?
O2 C19 1.363(11) . ?
O2 C20 1.422(11) . ?
O3 C21 1.396(9) . ?
O3 C21A 1.413(13) . ?
O5 C31 1.385(10) . ?
O6 C39 1.381(12) . ?
O6 C40 1.420(11) . ?
O7 C41 1.401(11) . ?
O8 C49 1.346(11) . ?
O8 C50 1.419(11) . ?
O9 C61 1.417(10) . ?
O10 C69 1.354(10) . ?
O10 C70 1.399(12) . ?
O11 C71 1.414(10) . ?
O12 C79 1.347(11) . ?
O12 C80 1.422(12) . ?
O13 C81 1.429(10) . ?
O14 C89 1.375(10) . ?
O14 C90 1.428(10) . ?
O15 C91 1.395(9) . ?
O16 C99 1.371(11) . ?
O16 C100 1.439(12) . ?
C1 C5 1.433(13) . ?
C1 C2 1.455(12) . ?
C2 C3 1.412(12) . ?
C2 H2 0.9500 . ?
C3 C4 1.421(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.406(11) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.421(12) . ?
C6 C10 1.437(12) . ?
C7 C8 1.412(12) . ?
C7 H7 0.9500 . ?
C8 C9 1.421(12) . ?
C8 H8 0.9500 . ?
C9 C10 1.431(12) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.368(13) . ?
C11 C19 1.392(13) . ?
C12 C13 1.398(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(13) . ?
C13 H13 0.9500 . ?
C14 C18 1.393(13) . ?
C14 C15 1.503(12) . ?
C15 C16 1.515(13) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.338(13) . ?
C16 Cu4 2.302(9) 2_566 ?
C16 H16 0.9500 . ?
C17 Cu4 2.207(10) 2_566 ?
C17 H17A 0.9500 . ?
C17 H17B 0.9500 . ?
C18 C19 1.368(13) . ?
C18 H18 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
O4 C29 1.387(16) . ?
O4 C30 1.441(18) . ?
C21 C22 1.3900 . ?
C21 C29 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22 0.9500 . ?
C23 C24 1.3900 . ?
C23 H23 0.9500 . ?
C24 C28 1.3900 . ?
C24 C25 1.518(17) . ?
C28 C29 1.3900 . ?
C28 H28 0.9500 . ?
C25 C26 1.49(2) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.33(3) . ?
C26 H26A 0.9500 . ?
C27 H27A 0.9500 . ?
C27 H27B 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
O4A C29A 1.38(2) . ?
O4A C30A 1.44(2) . ?
C21A C22A 1.3900 . ?
C21A C29A 1.3900 . ?
C22A C23A 1.3900 . ?
C22A H22A 0.9500 . ?
C23A C24A 1.3900 . ?
C23A H23A 0.9500 . ?
C24A C28A 1.3900 . ?
C24A C25A 1.53(2) . ?
C28A C29A 1.3900 . ?
C28A H28A 0.9500 . ?
C25A C26A 1.58(3) . ?
C25A H25C 0.9900 . ?
C25A H25D 0.9900 . ?
C26A C27A 1.24(3) . ?
C26A H26D 0.9500 . ?
C27A H27C 0.9500 . ?
C27A H27D 0.9500 . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 0.9800 . ?
C31 C32 1.368(13) . ?
C31 C39 1.399(14) . ?
C32 C33 1.403(14) . ?
C32 H32 0.9500 . ?
C33 C34 1.366(14) . ?
C33 H33 0.9500 . ?
C34 C38 1.415(13) . ?
C34 C35 1.512(14) . ?
C35 C36 1.499(16) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 C37 1.294(17) . ?
C36 H36 0.9500 . ?
C37 H37A 0.9500 . ?
C37 H37B 0.9500 . ?
C38 C39 1.392(14) . ?
C38 H38 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.371(13) . ?
C41 C49 1.378(14) . ?
C42 C43 1.407(14) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(15) . ?
C43 H43 0.9500 . ?
C44 C48 1.377(14) . ?
C44 C45 1.556(14) . ?
C45 C46 1.430(16) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.321(17) . ?
C46 H46 0.9500 . ?
C47 H47A 0.9500 . ?
C47 H47B 0.9500 . ?
C48 C49 1.414(14) . ?
C48 H48 0.9500 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C55 1.428(12) . ?
C51 C52 1.431(12) . ?
C52 C53 1.422(13) . ?
C52 H52 0.9500 . ?
C53 C54 1.412(13) . ?
C53 H53 0.9500 . ?
C54 C55 1.425(12) . ?
C54 H54 0.9500 . ?
C55 H55 0.9500 . ?
C56 C60 1.422(12) . ?
C56 C57 1.462(11) . ?
C57 C58 1.426(13) . ?
C57 H57 0.9500 . ?
C58 C59 1.432(13) . ?
C58 H58 0.9500 . ?
C59 C60 1.421(12) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 C62 1.380(12) . ?
C61 C69 1.388(13) . ?
C62 C63 1.398(13) . ?
C62 H62 0.9500 . ?
C63 C64 1.389(13) . ?
C63 H63 0.9500 . ?
C64 C68 1.374(13) . ?
C64 C65 1.517(12) . ?
C65 C66 1.474(14) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 C67 1.306(14) . ?
C66 H66 0.9500 . ?
C67 H67A 0.9500 . ?
C67 H67B 0.9500 . ?
C68 C69 1.400(13) . ?
C68 H68 0.9500 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 C72 1.361(13) . ?
C71 C79 1.382(13) . ?
C72 C73 1.397(12) . ?
C72 H72 0.9500 . ?
C73 C74 1.381(13) . ?
C73 H73 0.9500 . ?
C74 C78 1.389(13) . ?
C74 C75 1.497(13) . ?
C75 C76 1.498(15) . ?
C75 H75A 0.9900 . ?
C75 H75B 0.9900 . ?
C76 C77 1.285(16) . ?
C76 H76 0.9500 . ?
C77 H77A 0.9500 . ?
C77 H77B 0.9500 . ?
C78 C79 1.419(13) . ?
C78 H78 0.9500 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 C82 1.356(12) . ?
C81 C89 1.380(12) . ?
C82 C83 1.399(12) . ?
C82 H82 0.9500 . ?
C83 C84 1.391(13) . ?
C83 H83 0.9500 . ?
C84 C88 1.374(13) . ?
C84 C85 1.522(13) . ?
C85 C86 1.498(14) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 C87 1.287(17) . ?
C86 H86 0.9500 . ?
C87 H87A 0.9500 . ?
C87 H87B 0.9500 . ?
C88 C89 1.394(12) . ?
C88 H88 0.9500 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
C91 C92 1.390(12) . ?
C91 C99 1.395(12) . ?
C92 C93 1.380(12) . ?
C92 H92 0.9500 . ?
C93 C94 1.383(15) . ?
C93 H93 0.9500 . ?
C94 C98 1.398(15) . ?
C94 C95 1.558(16) . ?
C94 C95A 1.57(2) . ?
C95 C96 1.46(2) . ?
C95 H95A 0.9900 . ?
C95 H95B 0.9900 . ?
C96 C97 1.29(2) . ?
C96 H96 0.9600 . ?
C97 H97A 0.9599 . ?
C97 H97B 0.9601 . ?
C95A C96A 1.48(3) . ?
C95A H95C 0.9900 . ?
C95A H95D 0.9900 . ?
C96A C97A 1.30(3) . ?
C96A H96A 0.9600 . ?
C97A H97C 0.9601 . ?
C97A H97D 0.9600 . ?
C98 C99 1.375(13) . ?
C98 H98 0.9500 . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
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
Cu5 I1 Cu2 83.33(11) . . ?
Cu5 I1 Cu3 64.60(10) . . ?
Cu2 I1 Cu3 69.53(4) . . ?
Cu2 I1 Cu5A 70.68(10) . . ?
Cu3 I1 Cu5A 65.32(9) . . ?
Cu5 I1 Cu1 58.56(10) . . ?
Cu2 I1 Cu1 72.23(4) . . ?
Cu3 I1 Cu1 113.41(4) . . ?
Cu5A I1 Cu1 51.35(9) . . ?
Cu5 I2 Cu3 66.18(11) . . ?
Cu5A I2 Cu3 68.85(11) . . ?
Cu5 I2 Cu4 108.15(11) . . ?
Cu5A I2 Cu4 96.03(11) . . ?
Cu3 I2 Cu4 71.27(4) . . ?
Cu4 I3 Cu2 113.87(4) . . ?
Cu4 I3 Cu3 72.84(4) . . ?
Cu2 I3 Cu3 70.77(4) . . ?
Cu2 I4 Cu1 78.31(4) . . ?
Cu2 I4 Cu5A 71.51(10) . . ?
Cu1 I4 Cu5A 53.70(10) . . ?
Cu5 I5 Cu1 61.94(10) . . ?
Cu5A I5 Cu1 56.76(10) . . ?
P2 Cu1 Cu5A 165.78(15) . . ?
P2 Cu1 I4 121.81(8) . . ?
Cu5A Cu1 I4 67.64(12) . . ?
P2 Cu1 I5 123.03(8) . . ?
Cu5A Cu1 I5 59.70(11) . . ?
I4 Cu1 I5 102.31(5) . . ?
P2 Cu1 Cu5 152.18(14) . . ?
I4 Cu1 Cu5 81.65(11) . . ?
I5 Cu1 Cu5 57.24(10) . . ?
P2 Cu1 I1 104.12(8) . . ?
Cu5A Cu1 I1 62.53(12) . . ?
I4 Cu1 I1 98.26(4) . . ?
I5 Cu1 I1 102.97(4) . . ?
Cu5 Cu1 I1 54.01(11) . . ?
P1 Cu2 I4 112.30(8) . . ?
P1 Cu2 I3 108.14(8) . . ?
I4 Cu2 I3 106.04(5) . . ?
P1 Cu2 I1 116.13(8) . . ?
I4 Cu2 I1 103.97(4) . . ?
I3 Cu2 I1 109.79(5) . . ?
P3 Cu3 I2 123.21(8) . . ?
P3 Cu3 I3 105.41(7) . . ?
I2 Cu3 I3 105.27(4) . . ?
P3 Cu3 I1 106.49(8) . . ?
I2 Cu3 I1 107.24(4) . . ?
I3 Cu3 I1 108.61(4) . . ?
P3 Cu3 Cu5 144.27(13) . . ?
I2 Cu3 Cu5 53.74(10) . . ?
I3 Cu3 Cu5 109.44(11) . . ?
I1 Cu3 Cu5 54.77(10) . . ?
P3 Cu3 Cu5A 157.20(13) . . ?
I2 Cu3 Cu5A 54.80(9) . . ?
I3 Cu3 Cu5A 96.37(10) . . ?
I1 Cu3 Cu5A 59.01(10) . . ?
C17 Cu4 P4 130.8(3) 2_566 . ?
C17 Cu4 C16 34.4(3) 2_566 2_566 ?
P4 Cu4 C16 100.0(2) . 2_566 ?
C17 Cu4 I3 98.0(3) 2_566 . ?
P4 Cu4 I3 109.81(7) . . ?
C16 Cu4 I3 128.9(2) 2_566 . ?
C17 Cu4 I2 99.8(3) 2_566 . ?
P4 Cu4 I2 110.27(7) . . ?
C16 Cu4 I2 101.8(3) 2_566 . ?
I3 Cu4 I2 105.26(4) . . ?
I2 Cu5 I1 119.13(18) . . ?
I2 Cu5 I5 122.11(19) . . ?
I1 Cu5 I5 117.10(17) . . ?
I2 Cu5 Cu1 159.3(2) . . ?
I1 Cu5 Cu1 67.43(11) . . ?
I5 Cu5 Cu1 60.82(10) . . ?
I2 Cu5 Cu3 60.09(10) . . ?
I1 Cu5 Cu3 60.63(10) . . ?
I5 Cu5 Cu3 177.7(2) . . ?
Cu1 Cu5 Cu3 117.41(16) . . ?
Cu1 Cu5A I5 63.53(11) . . ?
Cu1 Cu5A I2 170.3(2) . . ?
I5 Cu5A I2 116.72(17) . . ?
Cu1 Cu5A I1 66.12(12) . . ?
I5 Cu5A I1 107.93(17) . . ?
I2 Cu5A I1 105.66(16) . . ?
Cu1 Cu5A I4 58.66(10) . . ?
I5 Cu5A I4 98.98(15) . . ?
I2 Cu5A I4 129.13(18) . . ?
I1 Cu5A I4 95.35(14) . . ?
Cu1 Cu5A Cu3 118.17(18) . . ?
I5 Cu5A Cu3 150.8(2) . . ?
I2 Cu5A Cu3 56.35(9) . . ?
I1 Cu5A Cu3 55.68(9) . . ?
I4 Cu5A Cu3 106.07(14) . . ?
C6 Fe1 C5 110.1(4) . . ?
C6 Fe1 C7 40.9(3) . . ?
C5 Fe1 C7 126.0(4) . . ?
C6 Fe1 C2 164.2(4) . . ?
C5 Fe1 C2 69.3(4) . . ?
C7 Fe1 C2 152.4(4) . . ?
C6 Fe1 C8 68.1(3) . . ?
C5 Fe1 C8 161.6(4) . . ?
C7 Fe1 C8 40.5(4) . . ?
C2 Fe1 C8 117.7(4) . . ?
C6 Fe1 C10 41.3(3) . . ?
C5 Fe1 C10 123.0(4) . . ?
C7 Fe1 C10 69.4(4) . . ?
C2 Fe1 C10 124.9(4) . . ?
C8 Fe1 C10 68.6(3) . . ?
C6 Fe1 C9 68.7(4) . . ?
C5 Fe1 C9 157.3(4) . . ?
C7 Fe1 C9 68.9(4) . . ?
C2 Fe1 C9 105.5(4) . . ?
C8 Fe1 C9 40.7(3) . . ?
C10 Fe1 C9 40.9(3) . . ?
C6 Fe1 C3 155.1(4) . . ?
C5 Fe1 C3 68.0(3) . . ?
C7 Fe1 C3 118.7(4) . . ?
C2 Fe1 C3 40.4(4) . . ?
C8 Fe1 C3 105.5(3) . . ?
C10 Fe1 C3 161.0(4) . . ?
C9 Fe1 C3 123.1(4) . . ?
C6 Fe1 C1 127.6(3) . . ?
C5 Fe1 C1 41.0(4) . . ?
C7 Fe1 C1 164.3(4) . . ?
C2 Fe1 C1 41.6(3) . . ?
C8 Fe1 C1 154.6(4) . . ?
C10 Fe1 C1 108.7(4) . . ?
C9 Fe1 C1 120.6(4) . . ?
C3 Fe1 C1 68.3(3) . . ?
C6 Fe1 C4 121.8(4) . . ?
C5 Fe1 C4 40.2(3) . . ?
C7 Fe1 C4 107.2(4) . . ?
C2 Fe1 C4 68.6(4) . . ?
C8 Fe1 C4 124.0(3) . . ?
C10 Fe1 C4 157.6(4) . . ?
C9 Fe1 C4 160.2(4) . . ?
C3 Fe1 C4 40.4(4) . . ?
C1 Fe1 C4 68.3(4) . . ?
C55 Fe2 C56 163.7(3) . . ?
C55 Fe2 C51 41.2(3) . . ?
C56 Fe2 C51 126.4(3) . . ?
C55 Fe2 C57 152.7(4) . . ?
C56 Fe2 C57 42.2(3) . . ?
C51 Fe2 C57 163.6(4) . . ?
C55 Fe2 C52 68.9(4) . . ?
C56 Fe2 C52 108.6(3) . . ?
C51 Fe2 C52 41.2(4) . . ?
C57 Fe2 C52 124.8(4) . . ?
C55 Fe2 C54 41.0(3) . . ?
C56 Fe2 C54 154.5(3) . . ?
C51 Fe2 C54 69.3(4) . . ?
C57 Fe2 C54 117.1(4) . . ?
C52 Fe2 C54 68.6(4) . . ?
C55 Fe2 C60 126.0(4) . . ?
C56 Fe2 C60 40.9(3) . . ?
C51 Fe2 C60 109.5(3) . . ?
C57 Fe2 C60 69.5(4) . . ?
C52 Fe2 C60 123.4(4) . . ?
C54 Fe2 C60 161.5(4) . . ?
C55 Fe2 C53 68.7(4) . . ?
C56 Fe2 C53 120.7(4) . . ?
C51 Fe2 C53 69.2(4) . . ?
C57 Fe2 C53 105.2(4) . . ?
C52 Fe2 C53 40.8(4) . . ?
C54 Fe2 C53 40.5(4) . . ?
C60 Fe2 C53 157.6(4) . . ?
C55 Fe2 C59 107.0(4) . . ?
C56 Fe2 C59 69.0(3) . . ?
C51 Fe2 C59 121.6(4) . . ?
C57 Fe2 C59 69.0(4) . . ?
C52 Fe2 C59 158.2(4) . . ?
C54 Fe2 C59 123.1(4) . . ?
C60 Fe2 C59 40.7(3) . . ?
C53 Fe2 C59 159.4(4) . . ?
C55 Fe2 C58 118.5(4) . . ?
C56 Fe2 C58 69.5(4) . . ?
C51 Fe2 C58 155.3(4) . . ?
C57 Fe2 C58 40.7(4) . . ?
C52 Fe2 C58 160.4(4) . . ?
C54 Fe2 C58 104.3(4) . . ?
C60 Fe2 C58 68.8(4) . . ?
C53 Fe2 C58 122.2(4) . . ?
C59 Fe2 C58 40.8(4) . . ?
O3 P1 O1 102.2(4) . . ?
O3 P1 C1 103.9(4) . . ?
O1 P1 C1 99.4(4) . . ?
O3 P1 Cu2 112.1(3) . . ?
O1 P1 Cu2 115.3(2) . . ?
C1 P1 Cu2 121.4(3) . . ?
O5 P2 O7 98.7(3) . . ?
O5 P2 C6 95.8(4) . . ?
O7 P2 C6 103.0(4) . . ?
O5 P2 Cu1 119.9(3) . . ?
O7 P2 Cu1 115.4(3) . . ?
C6 P2 Cu1 120.1(3) . . ?
O9 P3 O11 106.0(3) . . ?
O9 P3 C51 103.6(4) . . ?
O11 P3 C51 96.6(4) . . ?
O9 P3 Cu3 106.8(2) . . ?
O11 P3 Cu3 119.0(2) . . ?
C51 P3 Cu3 122.9(3) . . ?
O15 P4 O13 103.2(3) . . ?
O15 P4 C56 103.4(4) . . ?
O13 P4 C56 98.7(3) . . ?
O15 P4 Cu4 107.1(2) . . ?
O13 P4 Cu4 118.1(2) . . ?
C56 P4 Cu4 123.7(3) . . ?
C11 O1 P1 119.8(6) . . ?
C19 O2 C20 116.6(7) . . ?
C21 O3 P1 117.8(7) . . ?
C21A O3 P1 122.8(12) . . ?
C31 O5 P2 124.7(6) . . ?
C39 O6 C40 116.7(8) . . ?
C41 O7 P2 121.2(6) . . ?
C49 O8 C50 117.5(8) . . ?
C61 O9 P3 125.3(5) . . ?
C69 O10 C70 119.3(8) . . ?
C71 O11 P3 118.6(5) . . ?
C79 O12 C80 118.8(7) . . ?
C81 O13 P4 118.9(5) . . ?
C89 O14 C90 117.4(7) . . ?
C91 O15 P4 123.3(6) . . ?
C99 O16 C100 117.2(8) . . ?
C5 C1 C2 106.7(8) . . ?
C5 C1 P1 124.2(7) . . ?
C2 C1 P1 129.0(7) . . ?
C5 C1 Fe1 68.8(5) . . ?
C2 C1 Fe1 68.6(5) . . ?
P1 C1 Fe1 127.3(4) . . ?
C3 C2 C1 107.2(8) . . ?
C3 C2 Fe1 70.3(5) . . ?
C1 C2 Fe1 69.8(5) . . ?
C3 C2 H2 126.4 . . ?
C1 C2 H2 126.4 . . ?
Fe1 C2 H2 125.1 . . ?
C2 C3 C4 109.2(8) . . ?
C2 C3 Fe1 69.4(5) . . ?
C4 C3 Fe1 70.0(5) . . ?
C2 C3 H3 125.4 . . ?
C4 C3 H3 125.4 . . ?
Fe1 C3 H3 126.8 . . ?
C5 C4 C3 108.0(8) . . ?
C5 C4 Fe1 69.1(5) . . ?
C3 C4 Fe1 69.5(5) . . ?
C5 C4 H4 126.0 . . ?
C3 C4 H4 126.0 . . ?
Fe1 C4 H4 126.9 . . ?
C4 C5 C1 108.9(8) . . ?
C4 C5 Fe1 70.7(5) . . ?
C1 C5 Fe1 70.2(5) . . ?
C4 C5 H5 125.6 . . ?
C1 C5 H5 125.6 . . ?
Fe1 C5 H5 125.1 . . ?
C7 C6 C10 109.0(8) . . ?
C7 C6 P2 127.1(7) . . ?
C10 C6 P2 123.9(7) . . ?
C7 C6 Fe1 69.8(5) . . ?
C10 C6 Fe1 69.9(5) . . ?
P2 C6 Fe1 127.6(5) . . ?
C8 C7 C6 107.1(8) . . ?
C8 C7 Fe1 69.8(5) . . ?
C6 C7 Fe1 69.3(5) . . ?
C8 C7 H7 126.5 . . ?
C6 C7 H7 126.5 . . ?
Fe1 C7 H7 126.0 . . ?
C7 C8 C9 109.4(8) . . ?
C7 C8 Fe1 69.7(5) . . ?
C9 C8 Fe1 69.9(5) . . ?
C7 C8 H8 125.3 . . ?
C9 C8 H8 125.3 . . ?
Fe1 C8 H8 126.7 . . ?
C8 C9 C10 107.8(8) . . ?
C8 C9 Fe1 69.4(5) . . ?
C10 C9 Fe1 69.5(5) . . ?
C8 C9 H9 126.1 . . ?
C10 C9 H9 126.1 . . ?
Fe1 C9 H9 126.5 . . ?
C9 C10 C6 106.8(8) . . ?
C9 C10 Fe1 69.6(5) . . ?
C6 C10 Fe1 68.8(5) . . ?
C9 C10 H10 126.6 . . ?
C6 C10 H10 126.6 . . ?
Fe1 C10 H10 126.5 . . ?
C12 C11 O1 123.5(9) . . ?
C12 C11 C19 119.3(9) . . ?
O1 C11 C19 117.1(8) . . ?
C11 C12 C13 120.4(9) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 120.3(9) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C18 C14 C13 118.1(9) . . ?
C18 C14 C15 119.2(8) . . ?
C13 C14 C15 122.6(9) . . ?
C14 C15 C16 109.7(8) . . ?
C14 C15 H15A 109.7 . . ?
C16 C15 H15A 109.7 . . ?
C14 C15 H15B 109.7 . . ?
C16 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 C15 125.7(10) . . ?
C17 C16 Cu4 68.9(6) . 2_566 ?
C15 C16 Cu4 111.7(6) . 2_566 ?
C17 C16 H16 117.2 . . ?
C15 C16 H16 117.2 . . ?
Cu4 C16 H16 89.4 2_566 . ?
C16 C17 Cu4 76.7(6) . 2_566 ?
C16 C17 H17A 120.0 . . ?
Cu4 C17 H17A 107.0 2_566 . ?
C16 C17 H17B 120.0 . . ?
Cu4 C17 H17B 86.4 2_566 . ?
H17A C17 H17B 120.0 . . ?
C19 C18 C14 121.2(9) . . ?
C19 C18 H18 119.4 . . ?
C14 C18 H18 119.4 . . ?
O2 C19 C18 123.1(9) . . ?
O2 C19 C11 116.4(8) . . ?
C18 C19 C11 120.4(9) . . ?
O2 C20 H20A 109.5 . . ?
O2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C29 O4 C30 116.7(14) . . ?
C22 C21 C29 120.0 . . ?
C22 C21 O3 124.6(8) . . ?
C29 C21 O3 115.4(8) . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C28 C24 C23 120.0 . . ?
C28 C24 C25 119.4(12) . . ?
C23 C24 C25 120.6(13) . . ?
C24 C28 C29 120.0 . . ?
C24 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
O4 C29 C28 126.5(9) . . ?
O4 C29 C21 113.5(9) . . ?
C28 C29 C21 120.0 . . ?
C26 C25 C24 113.7(18) . . ?
C26 C25 H25A 108.8 . . ?
C24 C25 H25A 108.8 . . ?
C26 C25 H25B 108.8 . . ?
C24 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C27 C26 C25 113(3) . . ?
C27 C26 H26A 123.4 . . ?
C25 C26 H26A 123.4 . . ?
C26 C27 H27A 120.0 . . ?
C26 C27 H27B 120.0 . . ?
H27A C27 H27B 120.0 . . ?
O4 C30 H30A 109.5 . . ?
O4 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O4 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29A O4A C30A 115(2) . . ?
C22A C21A C29A 120.0 . . ?
C22A C21A O3 114.4(15) . . ?
C29A C21A O3 125.6(15) . . ?
C23A C22A C21A 120.0 . . ?
C23A C22A H22A 120.0 . . ?
C21A C22A H22A 120.0 . . ?
C24A C23A C22A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
C22A C23A H23A 120.0 . . ?
C23A C24A C28A 120.0 . . ?
C23A C24A C25A 125(2) . . ?
C28A C24A C25A 115(2) . . ?
C24A C28A C29A 120.0 . . ?
C24A C28A H28A 120.0 . . ?
C29A C28A H28A 120.0 . . ?
O4A C29A C28A 125.5(17) . . ?
O4A C29A C21A 114.5(17) . . ?
C28A C29A C21A 120.0 . . ?
C24A C25A C26A 107(2) . . ?
C24A C25A H25C 110.2 . . ?
C26A C25A H25C 110.2 . . ?
C24A C25A H25D 110.2 . . ?
C26A C25A H25D 110.2 . . ?
H25C C25A H25D 108.5 . . ?
C27A C26A C25A 113(4) . . ?
C27A C26A H26A 123.6 . . ?
C25A C26A H26A 123.6 . . ?
C26A C27A H27C 120.0 . . ?
C26A C27A H27D 120.0 . . ?
H27C C27A H27D 120.0 . . ?
O4A C30A H30D 109.5 . . ?
O4A C30A H30E 109.5 . . ?
H30D C30A H30E 109.5 . . ?
O4A C30A H30F 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
C32 C31 O5 125.1(8) . . ?
C32 C31 C39 120.7(9) . . ?
O5 C31 C39 114.1(8) . . ?
C31 C32 C33 120.2(10) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 H32 119.9 . . ?
C34 C33 C32 121.0(9) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C38 118.2(9) . . ?
C33 C34 C35 122.2(9) . . ?
C38 C34 C35 119.6(9) . . ?
C36 C35 C34 114.3(9) . . ?
C36 C35 H35A 108.7 . . ?
C34 C35 H35A 108.7 . . ?
C36 C35 H35B 108.7 . . ?
C34 C35 H35B 108.7 . . ?
H35A C35 H35B 107.6 . . ?
C37 C36 C35 125.6(12) . . ?
C37 C36 H36 117.2 . . ?
C35 C36 H36 117.2 . . ?
C36 C37 H37A 120.0 . . ?
C36 C37 H37B 120.0 . . ?
H37A C37 H37B 120.0 . . ?
C39 C38 C34 121.6(10) . . ?
C39 C38 H38 119.2 . . ?
C34 C38 H38 119.2 . . ?
O6 C39 C38 124.7(10) . . ?
O6 C39 C31 117.0(9) . . ?
C38 C39 C31 118.3(9) . . ?
O6 C40 H40A 109.5 . . ?
O6 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
O6 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C49 120.4(10) . . ?
C42 C41 O7 120.2(9) . . ?
C49 C41 O7 119.4(8) . . ?
C41 C42 C43 119.7(11) . . ?
C41 C42 H42 120.1 . . ?
C43 C42 H42 120.1 . . ?
C44 C43 C42 120.7(10) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C48 C44 C43 118.8(10) . . ?
C48 C44 C45 120.0(10) . . ?
C43 C44 C45 121.1(9) . . ?
C46 C45 C44 113.1(10) . . ?
C46 C45 H45A 109.0 . . ?
C44 C45 H45A 109.0 . . ?
C46 C45 H45B 109.0 . . ?
C44 C45 H45B 109.0 . . ?
H45A C45 H45B 107.8 . . ?
C47 C46 C45 126.7(14) . . ?
C47 C46 H46 116.7 . . ?
C45 C46 H46 116.7 . . ?
C46 C47 H47A 120.0 . . ?
C46 C47 H47B 120.0 . . ?
H47A C47 H47B 120.0 . . ?
C44 C48 C49 120.7(10) . . ?
C44 C48 H48 119.7 . . ?
C49 C48 H48 119.7 . . ?
O8 C49 C41 116.9(9) . . ?
O8 C49 C48 123.6(10) . . ?
C41 C49 C48 119.4(9) . . ?
O8 C50 H50A 109.5 . . ?
O8 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
O8 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C55 C51 C52 107.0(8) . . ?
C55 C51 P3 125.7(7) . . ?
C52 C51 P3 127.3(7) . . ?
C55 C51 Fe2 69.3(5) . . ?
C52 C51 Fe2 69.6(5) . . ?
P3 C51 Fe2 125.3(5) . . ?
C53 C52 C51 108.3(8) . . ?
C53 C52 Fe2 69.8(5) . . ?
C51 C52 Fe2 69.2(5) . . ?
C53 C52 H52 125.8 . . ?
C51 C52 H52 125.8 . . ?
Fe2 C52 H52 126.7 . . ?
C54 C53 C52 108.3(8) . . ?
C54 C53 Fe2 69.6(5) . . ?
C52 C53 Fe2 69.4(5) . . ?
C54 C53 H53 125.9 . . ?
C52 C53 H53 125.9 . . ?
Fe2 C53 H53 126.7 . . ?
C53 C54 C55 108.0(8) . . ?
C53 C54 Fe2 69.9(5) . . ?
C55 C54 Fe2 69.1(5) . . ?
C53 C54 H54 126.0 . . ?
C55 C54 H54 126.0 . . ?
Fe2 C54 H54 126.5 . . ?
C54 C55 C51 108.4(8) . . ?
C54 C55 Fe2 69.8(5) . . ?
C51 C55 Fe2 69.5(5) . . ?
C54 C55 H55 125.8 . . ?
C51 C55 H55 125.8 . . ?
Fe2 C55 H55 126.4 . . ?
C60 C56 C57 107.3(8) . . ?
C60 C56 P4 124.2(6) . . ?
C57 C56 P4 128.5(7) . . ?
C60 C56 Fe2 70.0(5) . . ?
C57 C56 Fe2 69.1(5) . . ?
P4 C56 Fe2 126.8(4) . . ?
C58 C57 C56 107.6(8) . . ?
C58 C57 Fe2 70.7(5) . . ?
C56 C57 Fe2 68.7(5) . . ?
C58 C57 H57 126.2 . . ?
C56 C57 H57 126.2 . . ?
Fe2 C57 H57 126.0 . . ?
C57 C58 C59 107.9(8) . . ?
C57 C58 Fe2 68.6(5) . . ?
C59 C58 Fe2 69.1(5) . . ?
C57 C58 H58 126.0 . . ?
C59 C58 H58 126.0 . . ?
Fe2 C58 H58 127.8 . . ?
C60 C59 C58 108.6(8) . . ?
C60 C59 Fe2 69.4(5) . . ?
C58 C59 Fe2 70.1(5) . . ?
C60 C59 H59 125.7 . . ?
C58 C59 H59 125.7 . . ?
Fe2 C59 H59 126.4 . . ?
C59 C60 C56 108.6(8) . . ?
C59 C60 Fe2 70.0(5) . . ?
C56 C60 Fe2 69.1(5) . . ?
C59 C60 H60 125.7 . . ?
C56 C60 H60 125.7 . . ?
Fe2 C60 H60 126.8 . . ?
C62 C61 C69 121.5(8) . . ?
C62 C61 O9 117.9(8) . . ?
C69 C61 O9 120.5(8) . . ?
C61 C62 C63 118.2(9) . . ?
C61 C62 H62 120.9 . . ?
C63 C62 H62 120.9 . . ?
C64 C63 C62 121.8(9) . . ?
C64 C63 H63 119.1 . . ?
C62 C63 H63 119.1 . . ?
C68 C64 C63 118.3(8) . . ?
C68 C64 C65 120.9(9) . . ?
C63 C64 C65 120.8(8) . . ?
C66 C65 C64 113.2(8) . . ?
C66 C65 H65A 108.9 . . ?
C64 C65 H65A 108.9 . . ?
C66 C65 H65B 108.9 . . ?
C64 C65 H65B 108.9 . . ?
H65A C65 H65B 107.7 . . ?
C67 C66 C65 126.4(11) . . ?
C67 C66 H66 116.8 . . ?
C65 C66 H66 116.8 . . ?
C66 C67 H67A 120.0 . . ?
C66 C67 H67B 120.0 . . ?
H67A C67 H67B 120.0 . . ?
C64 C68 C69 121.6(9) . . ?
C64 C68 H68 119.2 . . ?
C69 C68 H68 119.2 . . ?
O10 C69 C61 116.4(8) . . ?
O10 C69 C68 125.0(9) . . ?
C61 C69 C68 118.5(8) . . ?
O10 C70 H70A 109.5 . . ?
O10 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
O10 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C72 C71 C79 122.7(9) . . ?
C72 C71 O11 120.8(8) . . ?
C79 C71 O11 116.4(8) . . ?
C71 C72 C73 119.9(9) . . ?
C71 C72 H72 120.0 . . ?
C73 C72 H72 120.0 . . ?
C74 C73 C72 119.6(9) . . ?
C74 C73 H73 120.2 . . ?
C72 C73 H73 120.2 . . ?
C73 C74 C78 119.9(9) . . ?
C73 C74 C75 119.7(9) . . ?
C78 C74 C75 120.4(9) . . ?
C74 C75 C76 113.7(9) . . ?
C74 C75 H75A 108.8 . . ?
C76 C75 H75A 108.8 . . ?
C74 C75 H75B 108.8 . . ?
C76 C75 H75B 108.8 . . ?
H75A C75 H75B 107.7 . . ?
C77 C76 C75 127.8(10) . . ?
C77 C76 H76 116.1 . . ?
C75 C76 H76 116.1 . . ?
C76 C77 H77A 120.0 . . ?
C76 C77 H77B 120.0 . . ?
H77A C77 H77B 120.0 . . ?
C74 C78 C79 120.8(9) . . ?
C74 C78 H78 119.6 . . ?
C79 C78 H78 119.6 . . ?
O12 C79 C71 117.6(8) . . ?
O12 C79 C78 125.5(8) . . ?
C71 C79 C78 117.0(9) . . ?
O12 C80 H80A 109.5 . . ?
O12 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
O12 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C82 C81 C89 122.1(8) . . ?
C82 C81 O13 121.2(8) . . ?
C89 C81 O13 116.6(8) . . ?
C81 C82 C83 119.2(9) . . ?
C81 C82 H82 120.4 . . ?
C83 C82 H82 120.4 . . ?
C84 C83 C82 120.1(9) . . ?
C84 C83 H83 119.9 . . ?
C82 C83 H83 119.9 . . ?
C88 C84 C83 119.1(9) . . ?
C88 C84 C85 120.3(9) . . ?
C83 C84 C85 120.5(9) . . ?
C86 C85 C84 112.3(8) . . ?
C86 C85 H85A 109.2 . . ?
C84 C85 H85A 109.2 . . ?
C86 C85 H85B 109.2 . . ?
C84 C85 H85B 109.2 . . ?
H85A C85 H85B 107.9 . . ?
C87 C86 C85 125.3(13) . . ?
C87 C86 H86 117.4 . . ?
C85 C86 H86 117.4 . . ?
C86 C87 H87A 120.0 . . ?
C86 C87 H87B 120.0 . . ?
H87A C87 H87B 120.0 . . ?
C84 C88 C89 121.3(8) . . ?
C84 C88 H88 119.4 . . ?
C89 C88 H88 119.4 . . ?
O14 C89 C81 117.3(8) . . ?
O14 C89 C88 124.6(8) . . ?
C81 C89 C88 118.2(8) . . ?
O14 C90 H90A 109.5 . . ?
O14 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
O14 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C92 C91 C99 120.4(8) . . ?
C92 C91 O15 121.7(8) . . ?
C99 C91 O15 117.8(8) . . ?
C93 C92 C91 120.0(9) . . ?
C93 C92 H92 120.0 . . ?
C91 C92 H92 120.0 . . ?
C92 C93 C94 120.0(9) . . ?
C92 C93 H93 120.0 . . ?
C94 C93 H93 120.0 . . ?
C93 C94 C98 119.8(9) . . ?
C93 C94 C95 125.6(10) . . ?
C98 C94 C95 113.6(10) . . ?
C93 C94 C95A 108.7(14) . . ?
C98 C94 C95A 128.9(14) . . ?
C96 C95 C94 109.8(13) . . ?
C96 C95 H95A 109.7 . . ?
C94 C95 H95A 109.7 . . ?
C96 C95 H95B 109.7 . . ?
C94 C95 H95B 109.7 . . ?
H95A C95 H95B 108.2 . . ?
C97 C96 C95 130.5(19) . . ?
C97 C96 H96 102.7 . . ?
C95 C96 H96 126.0 . . ?
C96 C97 H97A 118.4 . . ?
C96 C97 H97B 121.6 . . ?
H97A C97 H97B 120.0 . . ?
C96A C95A C94 108(2) . . ?
C96A C95A H95C 110.1 . . ?
C94 C95A H95C 110.1 . . ?
C96A C95A H95D 110.1 . . ?
C94 C95A H95D 110.1 . . ?
H95C C95A H95D 108.4 . . ?
H97C C97A H97D 120.0 . . ?
C99 C98 C94 120.6(9) . . ?
C99 C98 H98 119.7 . . ?
C94 C98 H98 119.7 . . ?
O16 C99 C98 125.6(9) . . ?
O16 C99 C91 115.2(8) . . ?
C98 C99 C91 119.1(9) . . ?
O16 C100 H10A 109.5 . . ?
O16 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
O16 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full 26.75
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max 1.790
_refine_diff_density_min -2.180
_refine_diff_density_rms 0.194
_database_code_depnum_ccdc_archive 'CCDC 933868'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_msb438_0m
_audit_creation_method SHELXL-2013
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C50 H52 Au2 Cl2 Fe O8 P2'
_chemical_formula_sum 'C50 H52 Au2 Cl2 Fe O8 P2'
_chemical_formula_weight 1363.54
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.4474(10)
_cell_length_b 11.7473(13)
_cell_length_c 14.7451(16)
_cell_angle_alpha 112.484(1)
_cell_angle_beta 103.393(1)
_cell_angle_gamma 104.426(2)
_cell_volume 1363.2(3)
_cell_formula_units_Z 1
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 4677
_cell_measurement_theta_min 2.3433
_cell_measurement_theta_max 28.3430
_exptl_crystal_description block
_exptl_crystal_colour 0.176
_exptl_crystal_density_meas 0.120
_exptl_crystal_density_method 0.102
_exptl_crystal_density_diffrn 1.661
_exptl_crystal_F_000 664
_exptl_transmission_factor_min 0.392
_exptl_transmission_factor_max 0.563
_exptl_crystal_size_max 0.176
_exptl_crystal_size_mid 0.120
_exptl_crystal_size_min 0.102
_exptl_absorpt_coefficient_mu 5.835
_shelx_estimated_absorpt_T_min 0.427
_shelx_estimated_absorpt_T_max 0.588
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.43
_exptl_absorpt_correction_T_max 0.59
_exptl_absorpt_process_details 'TWINABS (Sheldrick, 2008a)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_source 'fine-focus sealed tube'
_diffrn_measurement_device_type 'Bruker Smart APEX CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean 8.3660
_diffrn_reflns_number 12187
_diffrn_reflns_av_unetI/netI 0.0710
_diffrn_reflns_av_R_equivalents 0.0589
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_theta_min 2.025
_diffrn_reflns_theta_max 27.995
_diffrn_reflns_theta_full 27.900
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total 6511
_reflns_number_gt 5219
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_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.
;
_computing_data_collection 'APEX2 (Bruker AXS, 2009)'
_computing_cell_refinement 'SAINT (Bruker AXS, 2009a)'
_computing_data_reduction 'SAINT (Bruker AXS, 2009a)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics 'SHELXTL (Bruker AXS, 2008)'
_computing_publication_material 'SHELXTL (Bruker AXS, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms were placed in
calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding
contributions with isotropic displacement parameters 1.2 - 1.5 times those
of the attached carbon atoms. One 2-methoxy-4-allylphenyl group is
disordered over two sites and was refined with restraints to make the
geometry of the two components comparable. Disordered lattice solvent
was removed with the SQUEEZE option of PLATON (Spek, 2012). The refinement
was performed using the one-component reflection file extracted from the
twinned data with TWINABS.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+11.2955P]
where P=(Fo^2^+2Fc^2^)/3
;
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 6511
_refine_ls_number_parameters 305
_refine_ls_number_restraints 150
_refine_ls_R_factor_all 0.0791
_refine_ls_R_factor_gt 0.0609
_refine_ls_wR_factor_ref 0.1441
_refine_ls_wR_factor_gt 0.1365
_refine_ls_goodness_of_fit_ref 1.073
_refine_ls_restrained_S_all 1.065
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Au1 Au 0.38600(4) 0.85557(4) 0.68604(2) 0.03836(12) Uani 1 1 d . . . . .
Fe1 Fe 0.0000 0.5000 0.5000 0.0498(5) Uani 1 2 d S . P . .
Cl1 Cl 0.3669(3) 1.0540(2) 0.78104(18) 0.0488(5) Uani 1 1 d . . . . .
P1 P 0.3912(3) 0.6578(2) 0.59683(17) 0.0389(5) Uani 1 1 d . . . . .
O1 O 0.5254(8) 0.6618(7) 0.5471(5) 0.0440(15) Uani 1 1 d . . . . .
O2 O 0.4197(9) 0.7330(9) 0.4016(6) 0.066(2) Uani 1 1 d . . . . .
O3 O 0.4249(7) 0.5798(7) 0.6623(5) 0.0438(15) Uani 1 1 d D . . . .
C1 C 0.2172(10) 0.5308(10) 0.4925(7) 0.044(2) Uani 1 1 d . . . . .
C2 C 0.1480(12) 0.3998(12) 0.4749(9) 0.060(3) Uani 1 1 d . . . . .
H2 H 0.1883 0.3617 0.5162 0.071 Uiso 1 1 calc R U . . .
C3 C 0.0062(12) 0.3337(12) 0.3838(9) 0.068(4) Uani 1 1 d . . . . .
H3 H -0.0639 0.2442 0.3539 0.082 Uiso 1 1 calc R U . . .
C4 C -0.0102(12) 0.4238(14) 0.3472(9) 0.070(4) Uani 1 1 d . . . . .
H4 H -0.0944 0.4060 0.2875 0.084 Uiso 1 1 calc R U . . .
C5 C 0.1178(12) 0.5462(12) 0.4123(8) 0.058(3) Uani 1 1 d . . . . .
H5 H 0.1348 0.6244 0.4043 0.069 Uiso 1 1 calc R U . . .
C6 C 0.6174(11) 0.7817(11) 0.5542(7) 0.048(2) Uani 1 1 d . . . . .
C7 C 0.5634(12) 0.8138(12) 0.4751(8) 0.052(3) Uani 1 1 d . . . . .
C8 C 0.6578(13) 0.9292(13) 0.4786(9) 0.059(3) Uani 1 1 d . . . . .
H8 H 0.6203 0.9544 0.4265 0.071 Uiso 1 1 calc R U . . .
C9 C 0.8067(13) 1.0079(11) 0.5576(8) 0.051(2) Uani 1 1 d . . . . .
C10 C 0.8571(13) 0.9705(11) 0.6362(8) 0.053(2) Uani 1 1 d . . . . .
H10 H 0.9576 1.0228 0.6906 0.063 Uiso 1 1 calc R U . . .
C11 C 0.7626(12) 0.8596(10) 0.6349(8) 0.047(2) Uani 1 1 d . . . . .
H11 H 0.7966 0.8364 0.6889 0.057 Uiso 1 1 calc R U . . .
C12 C 0.3723(12) 0.7516(16) 0.3114(9) 0.077(4) Uani 1 1 d . . . . .
H12A H 0.3779 0.8431 0.3336 0.115 Uiso 1 1 calc R U . . .
H12B H 0.2641 0.6897 0.2662 0.115 Uiso 1 1 calc R U . . .
H12C H 0.4419 0.7348 0.2722 0.115 Uiso 1 1 calc R U . . .
C13 C 0.9123(16) 1.1262(13) 0.5570(10) 0.069(3) Uani 1 1 d . . . . .
H13A H 0.9743 1.0960 0.5137 0.082 Uiso 1 1 calc R U . . .
H13B H 0.8460 1.1620 0.5221 0.082 Uiso 1 1 calc R U . . .
C14 C 1.0222(15) 1.2355(15) 0.6618(11) 0.072(3) Uani 1 1 d . . . . .
H14 H 0.9788 1.2704 0.7133 0.087 Uiso 1 1 calc R U . . .
C15 C 1.1732(17) 1.2873(19) 0.6887(16) 0.107(6) Uani 1 1 d . . . . .
H15A H 1.2209 1.2550 0.6394 0.129 Uiso 1 1 calc R U . . .
H15B H 1.2360 1.3574 0.7578 0.129 Uiso 1 1 calc R U . . .
C16 C 0.5545(13) 0.6654(12) 0.7625(7) 0.035(3) Uani 0.5 1 d DG U P A 1
C17 C 0.5258(11) 0.7382(13) 0.8510(10) 0.034(3) Uani 0.5 1 d DG U P A 1
C18 C 0.6470(14) 0.8109(12) 0.9490(8) 0.038(3) Uani 0.5 1 d G U P A 1
H18 H 0.6273 0.8607 1.0095 0.046 Uiso 0.5 1 calc R U P A 1
C19 C 0.7968(12) 0.8109(13) 0.9586(7) 0.048(4) Uani 0.5 1 d DG U P A 1
C20 C 0.8255(11) 0.7381(13) 0.8702(10) 0.044(3) Uani 0.5 1 d G U P A 1
H20 H 0.9279 0.7381 0.8767 0.053 Uiso 0.5 1 calc R U P A 1
C21 C 0.7043(15) 0.6653(12) 0.7721(8) 0.038(3) Uani 0.5 1 d G U P A 1
H21 H 0.7239 0.6156 0.7117 0.045 Uiso 0.5 1 calc R U P A 1
O4 O 0.3761(15) 0.7325(14) 0.8360(13) 0.036(3) Uani 0.5 1 d D U P A 1
C22 C 0.350(3) 0.824(2) 0.9224(19) 0.050(5) Uani 0.5 1 d D U P A 1
H22A H 0.2391 0.8110 0.9016 0.075 Uiso 0.5 1 calc R U P A 1
H22B H 0.4140 0.9150 0.9416 0.075 Uiso 0.5 1 calc R U P A 1
H22C H 0.3807 0.8070 0.9830 0.075 Uiso 0.5 1 calc R U P A 1
C23 C 0.9249(18) 0.900(2) 1.0660(11) 0.060(4) Uani 0.5 1 d D U P A 1
H23A H 0.9543 0.9921 1.0769 0.072 Uiso 0.5 1 calc R U P A 1
H23B H 0.8796 0.8950 1.1193 0.072 Uiso 0.5 1 calc R U P A 1
C24 C 1.070(2) 0.873(3) 1.088(2) 0.090(7) Uani 0.5 1 d D U P A 1
H24 H 1.0503 0.7816 1.0658 0.108 Uiso 0.5 1 d R U P A 1
C25 C 1.207(2) 0.955(3) 1.108(2) 0.073(6) Uani 0.5 1 d D U P A 1
H25A H 1.2699 1.0465 1.1355 0.088 Uiso 0.5 1 d R U P A 1
H25B H 1.2549 0.8916 1.0993 0.088 Uiso 0.5 1 d R U P A 1
C16A C 0.5369(13) 0.6294(13) 0.7592(7) 0.035(3) Uani 0.5 1 d DG U P A 2
C17A C 0.5122(11) 0.6992(13) 0.8504(10) 0.034(3) Uani 0.5 1 d DG U P A 2
C18A C 0.6340(14) 0.7622(12) 0.9478(8) 0.038(3) Uani 0.5 1 d G U P A 2
H18A H 0.6171 0.8099 1.0102 0.046 Uiso 0.5 1 calc R U P A 2
C19A C 0.7804(12) 0.7554(13) 0.9541(7) 0.048(4) Uani 0.5 1 d DG U P A 2
C20A C 0.8051(11) 0.6856(13) 0.8629(10) 0.044(3) Uani 0.5 1 d G U P A 2
H20A H 0.9052 0.6809 0.8671 0.053 Uiso 0.5 1 calc R U P A 2
C21A C 0.6833(15) 0.6226(13) 0.7655(8) 0.038(3) Uani 0.5 1 d G U P A 2
H21A H 0.7002 0.5749 0.7031 0.045 Uiso 0.5 1 calc R U P A 2
O4A O 0.3608(15) 0.6922(15) 0.8320(13) 0.036(3) Uani 0.5 1 d D U P A 2
C22A C 0.330(3) 0.773(2) 0.9213(18) 0.050(5) Uani 0.5 1 d D U P A 2
H22D H 0.2190 0.7600 0.8998 0.075 Uiso 0.5 1 calc R U P A 2
H22E H 0.3944 0.8668 0.9479 0.075 Uiso 0.5 1 calc R U P A 2
H22F H 0.3572 0.7473 0.9769 0.075 Uiso 0.5 1 calc R U P A 2
C23A C 0.9061(19) 0.833(2) 1.0632(11) 0.060(4) Uani 0.5 1 d D U P A 2
H23C H 0.9363 0.9289 1.0825 0.072 Uiso 0.5 1 calc R U P A 2
H23D H 0.8580 0.8189 1.1128 0.072 Uiso 0.5 1 calc R U P A 2
C24A C 1.051(2) 0.806(2) 1.082(2) 0.090(7) Uani 0.5 1 d D U P A 2
H24A H 1.0356 0.7161 1.0641 0.108 Uiso 0.5 1 d R U P A 2
C25A C 1.191(2) 0.897(3) 1.115(2) 0.073(6) Uani 0.5 1 d D U P A 2
H25C H 1.2251 0.9891 1.1362 0.088 Uiso 0.5 1 d R U P A 2
H25D H 1.2662 0.8561 1.1198 0.088 Uiso 0.5 1 d R U P A 2
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
Au1 0.03592(17) 0.0553(2) 0.02542(16) 0.01280(13) 0.01484(12) 0.02581(14)
Fe1 0.0380(9) 0.0693(13) 0.0316(9) 0.0038(8) 0.0162(7) 0.0327(9)
Cl1 0.0551(13) 0.0577(14) 0.0363(11) 0.0148(10) 0.0224(10) 0.0315(11)
P1 0.0374(11) 0.0564(14) 0.0291(10) 0.0153(10) 0.0187(9) 0.0287(10)
O1 0.048(3) 0.061(4) 0.034(3) 0.019(3) 0.025(3) 0.033(3)
O2 0.051(4) 0.108(7) 0.049(4) 0.044(5) 0.019(4) 0.034(4)
O3 0.040(3) 0.065(4) 0.029(3) 0.015(3) 0.016(3) 0.031(3)
C1 0.039(4) 0.064(6) 0.028(4) 0.010(4) 0.015(3) 0.031(4)
C2 0.045(5) 0.072(7) 0.053(6) 0.009(5) 0.025(5) 0.035(5)
C3 0.040(5) 0.068(7) 0.056(7) -0.014(6) 0.023(5) 0.021(5)
C4 0.040(5) 0.101(10) 0.046(6) 0.003(6) 0.021(5) 0.039(6)
C5 0.051(6) 0.085(8) 0.040(5) 0.017(5) 0.026(5) 0.041(6)
C6 0.048(5) 0.077(7) 0.030(4) 0.022(4) 0.023(4) 0.039(5)
C7 0.048(5) 0.084(8) 0.041(5) 0.030(5) 0.027(4) 0.036(5)
C8 0.058(6) 0.096(9) 0.051(6) 0.045(6) 0.035(5) 0.040(6)
C9 0.060(6) 0.069(7) 0.042(5) 0.030(5) 0.032(5) 0.032(5)
C10 0.060(6) 0.068(7) 0.040(5) 0.024(5) 0.025(5) 0.036(5)
C11 0.054(5) 0.064(6) 0.040(5) 0.027(5) 0.026(4) 0.037(5)
C12 0.036(5) 0.137(12) 0.056(7) 0.056(8) 0.016(5) 0.014(6)
C13 0.074(8) 0.088(9) 0.058(7) 0.039(7) 0.037(6) 0.032(7)
C14 0.058(7) 0.102(10) 0.081(9) 0.059(8) 0.030(7) 0.036(7)
C15 0.058(8) 0.155(16) 0.139(16) 0.091(14) 0.032(9) 0.055(10)
C16 0.038(4) 0.036(5) 0.033(4) 0.016(3) 0.017(3) 0.014(4)
C17 0.034(4) 0.039(5) 0.031(4) 0.017(3) 0.013(3) 0.015(4)
C18 0.039(4) 0.045(6) 0.034(4) 0.020(4) 0.018(3) 0.014(4)
C19 0.048(4) 0.052(6) 0.045(4) 0.022(4) 0.017(3) 0.021(4)
C20 0.042(4) 0.047(6) 0.044(4) 0.020(4) 0.019(3) 0.019(4)
C21 0.040(4) 0.041(6) 0.039(4) 0.018(3) 0.021(3) 0.019(4)
O4 0.035(3) 0.040(6) 0.032(3) 0.015(3) 0.017(2) 0.015(4)
C22 0.041(6) 0.059(10) 0.042(5) 0.012(6) 0.023(4) 0.019(7)
C23 0.055(5) 0.065(7) 0.057(5) 0.024(4) 0.021(4) 0.027(5)
C24 0.088(7) 0.095(8) 0.084(7) 0.039(5) 0.034(5) 0.032(5)
C25 0.060(7) 0.081(11) 0.066(8) 0.019(7) 0.040(6) 0.015(7)
C16A 0.038(4) 0.036(5) 0.033(4) 0.016(3) 0.017(3) 0.014(4)
C17A 0.034(4) 0.039(5) 0.031(4) 0.017(3) 0.013(3) 0.015(4)
C18A 0.039(4) 0.045(6) 0.034(4) 0.020(4) 0.018(3) 0.014(4)
C19A 0.048(4) 0.052(6) 0.045(4) 0.022(4) 0.017(3) 0.021(4)
C20A 0.042(4) 0.047(6) 0.044(4) 0.020(4) 0.019(3) 0.019(4)
C21A 0.040(4) 0.041(6) 0.039(4) 0.018(3) 0.021(3) 0.019(4)
O4A 0.035(3) 0.040(6) 0.032(3) 0.015(3) 0.017(2) 0.015(4)
C22A 0.041(6) 0.059(10) 0.042(5) 0.012(6) 0.023(4) 0.019(7)
C23A 0.055(5) 0.065(7) 0.057(5) 0.024(4) 0.021(4) 0.027(5)
C24A 0.088(7) 0.095(8) 0.084(7) 0.039(5) 0.034(5) 0.032(5)
C25A 0.060(7) 0.081(11) 0.066(8) 0.019(7) 0.040(6) 0.015(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
Au1 P1 2.209(2) . ?
Au1 Cl1 2.293(2) . ?
Fe1 C5 2.026(11) . ?
Fe1 C5 2.027(11) 2_566 ?
Fe1 C1 2.029(9) 2_566 ?
Fe1 C1 2.029(9) . ?
Fe1 C4 2.050(11) . ?
Fe1 C4 2.050(11) 2_566 ?
Fe1 C2 2.051(10) . ?
Fe1 C2 2.051(10) 2_566 ?
Fe1 C3 2.073(10) 2_566 ?
Fe1 C3 2.073(10) . ?
P1 O3 1.598(7) . ?
P1 O1 1.604(6) . ?
P1 C1 1.774(10) . ?
O1 C6 1.409(13) . ?
O2 C7 1.345(13) . ?
O2 C12 1.418(13) . ?
O3 C16A 1.363(10) . ?
O3 C16 1.451(9) . ?
C1 C2 1.407(16) . ?
C1 C5 1.431(14) . ?
C2 C3 1.433(15) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(19) . ?
C3 H3 0.9500 . ?
C4 C5 1.411(17) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 C7 1.386(14) . ?
C6 C11 1.386(14) . ?
C7 C8 1.399(16) . ?
C8 C9 1.400(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.414(14) . ?
C9 C13 1.499(16) . ?
C10 C11 1.375(15) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.479(18) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.297(18) . ?
C14 H14 0.9500 . ?
C15 H15A 0.9500 . ?
C15 H15B 0.9500 . ?
C16 C17 1.3900 . ?
C16 C21 1.3900 . ?
C17 O4 1.360(12) . ?
C17 C18 1.3900 . ?
C18 C19 1.3900 . ?
C18 H18 0.9500 . ?
C19 C20 1.3900 . ?
C19 C23 1.509(9) . ?
C20 C21 1.3900 . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
O4 C22 1.434(15) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.470(10) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.297(13) . ?
C24 H24 0.9500 . ?
C25 H25A 0.9500 . ?
C25 H25B 0.9500 . ?
C16A C17A 1.3900 . ?
C16A C21A 1.3900 . ?
C17A O4A 1.368(12) . ?
C17A C18A 1.3900 . ?
C18A C19A 1.3900 . ?
C18A H18A 0.9500 . ?
C19A C20A 1.3900 . ?
C19A C23A 1.511(9) . ?
C20A C21A 1.3900 . ?
C20A H20A 0.9500 . ?
C21A H21A 0.9500 . ?
O4A C22A 1.439(15) . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C23A C24A 1.474(10) . ?
C23A H23C 0.9900 . ?
C23A H23D 0.9900 . ?
C24A C25A 1.310(13) . ?
C24A H24A 0.9500 . ?
C25A H25C 0.9500 . ?
C25A H25D 0.9500 . ?
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
P1 Au1 Cl1 176.18(9) . . ?
C5 Fe1 C5 180.0 . 2_566 ?
C5 Fe1 C1 138.7(4) . 2_566 ?
C5 Fe1 C1 41.3(4) 2_566 2_566 ?
C5 Fe1 C1 41.3(4) . . ?
C5 Fe1 C1 138.7(4) 2_566 . ?
C1 Fe1 C1 180.0 2_566 . ?
C5 Fe1 C4 40.5(5) . . ?
C5 Fe1 C4 139.5(5) 2_566 . ?
C1 Fe1 C4 111.7(4) 2_566 . ?
C1 Fe1 C4 68.3(4) . . ?
C5 Fe1 C4 139.5(5) . 2_566 ?
C5 Fe1 C4 40.5(5) 2_566 2_566 ?
C1 Fe1 C4 68.3(4) 2_566 2_566 ?
C1 Fe1 C4 111.7(4) . 2_566 ?
C4 Fe1 C4 180.0 . 2_566 ?
C5 Fe1 C2 68.2(5) . . ?
C5 Fe1 C2 111.8(5) 2_566 . ?
C1 Fe1 C2 139.7(4) 2_566 . ?
C1 Fe1 C2 40.3(4) . . ?
C4 Fe1 C2 67.4(5) . . ?
C4 Fe1 C2 112.6(5) 2_566 . ?
C5 Fe1 C2 111.8(5) . 2_566 ?
C5 Fe1 C2 68.2(5) 2_566 2_566 ?
C1 Fe1 C2 40.3(4) 2_566 2_566 ?
C1 Fe1 C2 139.7(4) . 2_566 ?
C4 Fe1 C2 112.6(5) . 2_566 ?
C4 Fe1 C2 67.4(5) 2_566 2_566 ?
C2 Fe1 C2 180.0 . 2_566 ?
C5 Fe1 C3 112.4(5) . 2_566 ?
C5 Fe1 C3 67.6(5) 2_566 2_566 ?
C1 Fe1 C3 68.2(4) 2_566 2_566 ?
C1 Fe1 C3 111.8(4) . 2_566 ?
C4 Fe1 C3 140.8(5) . 2_566 ?
C4 Fe1 C3 39.2(5) 2_566 2_566 ?
C2 Fe1 C3 139.4(4) . 2_566 ?
C2 Fe1 C3 40.6(4) 2_566 2_566 ?
C5 Fe1 C3 67.6(5) . . ?
C5 Fe1 C3 112.4(5) 2_566 . ?
C1 Fe1 C3 111.8(4) 2_566 . ?
C1 Fe1 C3 68.2(4) . . ?
C4 Fe1 C3 39.2(5) . . ?
C4 Fe1 C3 140.8(5) 2_566 . ?
C2 Fe1 C3 40.6(4) . . ?
C2 Fe1 C3 139.4(4) 2_566 . ?
C3 Fe1 C3 180.0 2_566 . ?
O3 P1 O1 102.7(3) . . ?
O3 P1 C1 98.2(4) . . ?
O1 P1 C1 105.4(4) . . ?
O3 P1 Au1 116.1(2) . . ?
O1 P1 Au1 113.6(3) . . ?
C1 P1 Au1 118.6(3) . . ?
C6 O1 P1 120.5(5) . . ?
C7 O2 C12 117.7(9) . . ?
C16A O3 P1 127.4(8) . . ?
C16 O3 P1 111.7(7) . . ?
C2 C1 C5 107.4(9) . . ?
C2 C1 P1 127.3(8) . . ?
C5 C1 P1 125.3(9) . . ?
C2 C1 Fe1 70.6(5) . . ?
C5 C1 Fe1 69.2(5) . . ?
P1 C1 Fe1 123.7(4) . . ?
C1 C2 C3 108.1(11) . . ?
C1 C2 Fe1 69.0(5) . . ?
C3 C2 Fe1 70.5(6) . . ?
C1 C2 H2 125.9 . . ?
C3 C2 H2 125.9 . . ?
Fe1 C2 H2 126.1 . . ?
C4 C3 C2 107.7(11) . . ?
C4 C3 Fe1 69.5(6) . . ?
C2 C3 Fe1 68.8(5) . . ?
C4 C3 H3 126.1 . . ?
C2 C3 H3 126.1 . . ?
Fe1 C3 H3 127.1 . . ?
C3 C4 C5 109.3(11) . . ?
C3 C4 Fe1 71.3(7) . . ?
C5 C4 Fe1 68.9(6) . . ?
C3 C4 H4 125.3 . . ?
C5 C4 H4 125.3 . . ?
Fe1 C4 H4 126.1 . . ?
C4 C5 C1 107.5(11) . . ?
C4 C5 Fe1 70.6(7) . . ?
C1 C5 Fe1 69.5(6) . . ?
C4 C5 H5 126.3 . . ?
C1 C5 H5 126.3 . . ?
Fe1 C5 H5 125.2 . . ?
C7 C6 C11 121.6(10) . . ?
C7 C6 O1 118.3(9) . . ?
C11 C6 O1 120.0(8) . . ?
O2 C7 C6 116.9(10) . . ?
O2 C7 C8 124.4(10) . . ?
C6 C7 C8 118.6(10) . . ?
C7 C8 C9 121.0(10) . . ?
C7 C8 H8 119.5 . . ?
C9 C8 H8 119.5 . . ?
C8 C9 C10 118.3(10) . . ?
C8 C9 C13 120.9(10) . . ?
C10 C9 C13 120.8(10) . . ?
C11 C10 C9 120.9(10) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C10 C11 C6 119.5(9) . . ?
C10 C11 H11 120.2 . . ?
C6 C11 H11 120.2 . . ?
O2 C12 H12A 109.5 . . ?
O2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C9 115.5(10) . . ?
C14 C13 H13A 108.4 . . ?
C9 C13 H13A 108.4 . . ?
C14 C13 H13B 108.4 . . ?
C9 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C15 C14 C13 125.0(15) . . ?
C15 C14 H14 117.5 . . ?
C13 C14 H14 117.5 . . ?
C14 C15 H15A 120.0 . . ?
C14 C15 H15B 120.0 . . ?
H15A C15 H15B 120.0 . . ?
C17 C16 C21 120.0 . . ?
C17 C16 O3 119.8(9) . . ?
C21 C16 O3 120.0(9) . . ?
O4 C17 C16 116.8(10) . . ?
O4 C17 C18 123.2(10) . . ?
C16 C17 C18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C20 C19 C18 120.0 . . ?
C20 C19 C23 122.8(11) . . ?
C18 C19 C23 117.1(10) . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C16 120.0 . . ?
C20 C21 H21 120.0 . . ?
C16 C21 H21 120.0 . . ?
C17 O4 C22 117.2(12) . . ?
O4 C22 H22A 109.5 . . ?
O4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
O4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C19 118.5(14) . . ?
C24 C23 H23A 107.7 . . ?
C19 C23 H23A 107.7 . . ?
C24 C23 H23B 107.7 . . ?
C19 C23 H23B 107.7 . . ?
H23A C23 H23B 107.1 . . ?
C25 C24 C23 124(2) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 112.7 . . ?
C24 C25 H25A 144.4 . . ?
C24 C25 H25B 94.6 . . ?
H25A C25 H25B 120.0 . . ?
O3 C16A C17A 120.9(9) . . ?
O3 C16A C21A 118.7(10) . . ?
C17A C16A C21A 120.0 . . ?
O4A C17A C18A 126.8(10) . . ?
O4A C17A C16A 113.1(10) . . ?
C18A C17A C16A 120.0 . . ?
C17A C18A C19A 120.0 . . ?
C17A C18A H18A 120.0 . . ?
C19A C18A H18A 120.0 . . ?
C20A C19A C18A 120.0 . . ?
C20A C19A C23A 124.5(11) . . ?
C18A C19A C23A 115.4(10) . . ?
C19A C20A C21A 120.0 . . ?
C19A C20A H20A 120.0 . . ?
C21A C20A H20A 120.0 . . ?
C20A C21A C16A 120.0 . . ?
C20A C21A H21A 120.0 . . ?
C16A C21A H21A 120.0 . . ?
C17A O4A C22A 116.1(12) . . ?
O4A C22A H22D 109.5 . . ?
O4A C22A H22E 109.5 . . ?
H22D C22A H22E 109.5 . . ?
O4A C22A H22F 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
C24A C23A C19A 118.8(14) . . ?
C24A C23A H23C 107.6 . . ?
C19A C23A H23C 107.6 . . ?
C24A C23A H23D 107.6 . . ?
C19A C23A H23D 107.6 . . ?
H23C C23A H23D 107.0 . . ?
C25A C24A C23A 123(2) . . ?
C25A C24A H24A 122.0 . . ?
C23A C24A H24A 114.6 . . ?
C24A C25A H25C 131.5 . . ?
C24A C25A H25D 108.4 . . ?
H25C C25A H25D 120.0 . . ?
_refine_diff_density_max 1.981
_refine_diff_density_min -1.568
_refine_diff_density_rms 0.194
_shelxl_version_number 2013-2
_shelx_res_file
;
TITL msb438_0m in P-1
CELL 0.71073 9.4474 11.7473 14.7451 112.484 103.393 104.426
ZERR 1.00 0.0010 0.0013 0.0016 0.001 0.001 0.002
LATT 1
SFAC C H O P Cl Fe Au
UNIT 50 52 8 2 2 1 2
OMIT -2 56
L.S. 4
ACTA 55.8
MERG 3
BOND $H
FMAP 2
PLAN 5
SADI C17 C22 C17a C22a
SADI C22 O4 C22a O4a
SADI C17 O4 C17a O4a
SADI C23 C25 C23a C25a
SADI C19 C24 C19a C24a
SADI C24 25 C24a C25a
SADI C23 C24 C23a C24a
SADI C19 C23 C19a C23a
SADI C16 O3 C16a O3
EADP O4 O4a
EADP C25 C25a
EADP C24 C24a
EADP C23 C23a
EADP C22 C22a
EADP C21 C21a
EADP C20 C20a
EADP C19 C19a
EADP C18 C18a
EADP C17 C17a
EADP C16 C16a
DFIX 1.504 0.011 C19 C23 C19a C23a
DFIX 1.481 0.012 C23 C24 C23a C24a
DFIX 1.301 0.013 C24 C25 C24a C25a
DFIX 2.521 0.05 C19 C24 C19a C24a
DFIX 2.464 0.07 C23 C25 C23a C25a
SIZE 0.102 0.12 0.176
ISOR 0.007 C16 > C25A
TEMP -173
ABIN
WGHT 0.050500 11.295500
FVAR 0.12618
MOLE 1
AU1 7 0.385995 0.855571 0.686043 11.00000 0.03592 0.05525 =
0.02542 0.01280 0.01484 0.02581
FE1 6 0.000000 0.500000 0.500000 10.50000 0.03804 0.06930 =
0.03163 0.00384 0.01623 0.03266
CL1 5 0.366921 1.053999 0.781036 11.00000 0.05507 0.05774 =
0.03630 0.01483 0.02235 0.03149
P1 4 0.391227 0.657822 0.596830 11.00000 0.03738 0.05645 =
0.02908 0.01532 0.01867 0.02871
O1 3 0.525414 0.661787 0.547126 11.00000 0.04795 0.06108 =
0.03391 0.01915 0.02542 0.03280
O2 3 0.419704 0.732987 0.401557 11.00000 0.05068 0.10804 =
0.04924 0.04363 0.01946 0.03385
O3 3 0.424914 0.579778 0.662272 11.00000 0.04037 0.06461 =
0.02887 0.01538 0.01562 0.03100
C1 1 0.217196 0.530847 0.492536 11.00000 0.03850 0.06371 =
0.02765 0.00991 0.01487 0.03051
C2 1 0.148000 0.399765 0.474912 11.00000 0.04465 0.07207 =
0.05321 0.00872 0.02466 0.03510
AFIX 43
H2 2 0.188297 0.361681 0.516247 11.00000 -1.20000
AFIX 0
C3 1 0.006226 0.333718 0.383805 11.00000 0.04010 0.06779 =
0.05637 -0.01373 0.02325 0.02125
AFIX 43
H3 2 -0.063914 0.244182 0.353911 11.00000 -1.20000
AFIX 0
C4 1 -0.010215 0.423755 0.347160 11.00000 0.04048 0.10130 =
0.04568 0.00341 0.02067 0.03861
AFIX 43
H4 2 -0.094436 0.405955 0.287519 11.00000 -1.20000
AFIX 0
C5 1 0.117753 0.546154 0.412285 11.00000 0.05096 0.08515 =
0.03958 0.01667 0.02600 0.04100
AFIX 43
H5 2 0.134764 0.624403 0.404305 11.00000 -1.20000
AFIX 0
C6 1 0.617387 0.781682 0.554186 11.00000 0.04800 0.07700 =
0.03023 0.02237 0.02316 0.03901
C7 1 0.563381 0.813845 0.475100 11.00000 0.04814 0.08352 =
0.04068 0.03039 0.02726 0.03629
C8 1 0.657794 0.929194 0.478557 11.00000 0.05784 0.09643 =
0.05055 0.04492 0.03480 0.04007
AFIX 43
H8 2 0.620299 0.954450 0.426534 11.00000 -1.20000
AFIX 0
C9 1 0.806721 1.007929 0.557576 11.00000 0.06024 0.06852 =
0.04238 0.02974 0.03215 0.03233
C10 1 0.857095 0.970546 0.636156 11.00000 0.06036 0.06817 =
0.04029 0.02378 0.02518 0.03625
AFIX 43
H10 2 0.957622 1.022834 0.690580 11.00000 -1.20000
AFIX 0
C11 1 0.762595 0.859568 0.634885 11.00000 0.05434 0.06412 =
0.03980 0.02674 0.02567 0.03670
AFIX 43
H11 2 0.796598 0.836449 0.688934 11.00000 -1.20000
AFIX 0
C12 1 0.372253 0.751569 0.311421 11.00000 0.03572 0.13750 =
0.05559 0.05576 0.01640 0.01396
AFIX 137
H12A 2 0.377903 0.843103 0.333593 11.00000 -1.50000
H12B 2 0.264130 0.689688 0.266158 11.00000 -1.50000
H12C 2 0.441923 0.734762 0.272201 11.00000 -1.50000
AFIX 0
C13 1 0.912296 1.126217 0.557006 11.00000 0.07395 0.08776 =
0.05791 0.03894 0.03662 0.03239
AFIX 23
H13A 2 0.974323 1.096002 0.513734 11.00000 -1.20000
H13B 2 0.846040 1.161951 0.522084 11.00000 -1.20000
AFIX 0
C14 1 1.022169 1.235503 0.661795 11.00000 0.05784 0.10208 =
0.08142 0.05935 0.02986 0.03647
AFIX 43
H14 2 0.978837 1.270449 0.713315 11.00000 -1.20000
AFIX 0
C15 1 1.173180 1.287268 0.688715 11.00000 0.05835 0.15482 =
0.13916 0.09058 0.03239 0.05488
AFIX 93
H15A 2 1.220927 1.255014 0.639384 11.00000 -1.20000
H15B 2 1.236000 1.357425 0.757756 11.00000 -1.20000
PART 1
AFIX 76
C16 1 0.554466 0.665364 0.762509 10.50000 0.03812 0.03608 =
0.03323 0.01579 0.01666 0.01381
C17 1 0.525774 0.738166 0.850962 10.50000 0.03401 0.03862 =
0.03116 0.01746 0.01318 0.01481
C18 1 0.646950 0.810943 0.949019 10.50000 0.03908 0.04474 =
0.03418 0.01985 0.01790 0.01411
AFIX 43
H18 2 0.627340 0.860701 1.009472 10.50000 -1.20000
AFIX 75
C19 1 0.796819 0.810918 0.958624 10.50000 0.04765 0.05211 =
0.04454 0.02243 0.01704 0.02135
C20 1 0.825513 0.738116 0.870173 10.50000 0.04154 0.04742 =
0.04439 0.02004 0.01882 0.01920
AFIX 43
H20 2 0.927942 0.738099 0.876738 10.50000 -1.20000
AFIX 75
C21 1 0.704338 0.665338 0.772115 10.50000 0.03962 0.04050 =
0.03880 0.01829 0.02088 0.01917
AFIX 43
H21 2 0.723949 0.615581 0.711662 10.50000 -1.20000
AFIX 0
O4 3 0.376122 0.732513 0.835973 10.50000 0.03538 0.04026 =
0.03214 0.01490 0.01676 0.01508
C22 1 0.350457 0.823607 0.922413 10.50000 0.04141 0.05938 =
0.04215 0.01170 0.02311 0.01913
AFIX 33
H22A 2 0.239139 0.811032 0.901640 10.50000 -1.50000
H22B 2 0.414014 0.914984 0.941638 10.50000 -1.50000
H22C 2 0.380685 0.807041 0.983015 10.50000 -1.50000
AFIX 0
C23 1 0.924900 0.899513 1.065980 10.50000 0.05518 0.06509 =
0.05712 0.02407 0.02141 0.02682
AFIX 23
H23A 2 0.954301 0.992083 1.076939 10.50000 -1.20000
H23B 2 0.879604 0.895008 1.119287 10.50000 -1.20000
AFIX 0
C24 1 1.069936 0.873270 1.088413 10.50000 0.08849 0.09483 =
0.08428 0.03881 0.03449 0.03225
AFIX 3
H24 2 1.050291 0.781596 1.065807 10.50000 -1.20000
AFIX 0
C25 1 1.207134 0.955380 1.108156 10.50000 0.06031 0.08098 =
0.06595 0.01911 0.04022 0.01530
AFIX 3
H25A 2 1.269912 1.046466 1.135458 10.50000 -1.20000
H25B 2 1.254914 0.891636 1.099309 10.50000 -1.20000
PART 2
AFIX 76
C16A 1 0.536850 0.629426 0.759238 10.50000 0.03812 0.03608 =
0.03323 0.01579 0.01666 0.01381
C17A 1 0.512168 0.699234 0.850431 10.50000 0.03401 0.03862 =
0.03116 0.01746 0.01318 0.01481
C18A 1 0.633967 0.762210 0.947849 10.50000 0.03908 0.04474 =
0.03418 0.01985 0.01790 0.01411
AFIX 43
H18A 2 0.617097 0.809921 1.010175 10.50000 -1.20000
AFIX 75
C19A 1 0.780449 0.755379 0.954076 10.50000 0.04765 0.05211 =
0.04454 0.02243 0.01704 0.02135
C20A 1 0.805133 0.685571 0.862884 10.50000 0.04154 0.04742 =
0.04439 0.02004 0.01882 0.01920
AFIX 43
H20A 2 0.905247 0.680902 0.867140 10.50000 -1.20000
AFIX 75
C21A 1 0.683335 0.622594 0.765464 10.50000 0.03962 0.04050 =
0.03880 0.01829 0.02088 0.01917
AFIX 43
H21A 2 0.700206 0.574884 0.703138 10.50000 -1.20000
AFIX 0
O4A 3 0.360778 0.692181 0.832038 10.50000 0.03538 0.04026 =
0.03214 0.01490 0.01676 0.01508
C22A 1 0.330417 0.773000 0.921266 10.50000 0.04141 0.05938 =
0.04215 0.01170 0.02311 0.01913
AFIX 33
H22D 2 0.218987 0.760017 0.899781 10.50000 -1.50000
H22E 2 0.394371 0.866773 0.947887 10.50000 -1.50000
H22F 2 0.357212 0.747261 0.976912 10.50000 -1.50000
AFIX 0
C23A 1 0.906072 0.833379 1.063198 10.50000 0.05518 0.06509 =
0.05712 0.02407 0.02141 0.02682
AFIX 23
H23C 2 0.936262 0.928886 1.082457 10.50000 -1.20000
H23D 2 0.858010 0.818912 1.112787 10.50000 -1.20000
AFIX 0
C24A 1 1.051401 0.806232 1.081946 10.50000 0.08849 0.09483 =
0.08428 0.03881 0.03449 0.03225
AFIX 3
H24A 2 1.035570 0.716107 1.064141 10.50000 -1.20000
AFIX 0
C25A 1 1.191290 0.896603 1.115210 10.50000 0.06031 0.08098 =
0.06595 0.01911 0.04022 0.01530
AFIX 3
H25C 2 1.225141 0.989096 1.136190 10.50000 -1.20000
H25D 2 1.266204 0.856075 1.119818 10.50000 -1.20000
PART 0
AFIX 0
HKLF 4
REM msb438_0m in P-1
REM R1 = 0.0609 for 5219 Fo > 4sig(Fo) and 0.0791 for all 6511 data
REM 305 parameters refined using 150 restraints
END
WGHT 0.0503 11.3280
REM Highest difference peak 1.981, deepest hole -1.568, 1-sigma level 0.194
Q1 1 0.4141 0.9400 0.6947 11.00000 0.05 1.98
Q2 1 0.3059 0.7792 0.6183 11.00000 0.05 1.91
Q3 1 0.4564 0.9252 0.7475 11.00000 0.05 1.79
Q4 1 0.4460 1.0433 0.7038 11.00000 0.05 1.76
Q5 1 0.4997 1.0005 0.3388 11.00000 0.05 1.66
;
# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.032 0.500 1.000 160 42 ' '
_platon_squeeze_details
;TITL msb438_0m in P-1
CELL 9.4474 11.7473 14.7451 112.48 103.39 104.43
SPGR P-1
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.472 0.533 0.030 ! 3.80 eA-3
C102 0.273 0.562-0.005 ! 2.68 eA-3
Q103 0.586 0.063 0.297 ! 2.46 eA-3
Q104 0.722 0.265 0.283 ! 2.38 eA-3
C105 0.806 0.467-0.001 ! 2.36 eA-3
Q106 0.686 0.204 0.378 ! 2.29 eA-3
Q107 0.454 0.920 0.750 ! 2.23 eA-3
C108 0.030 0.568 0.046 ! 2.10 eA-3
C109 0.221 0.576 0.093 ! 1.84 eA-3
Q110 0.495 1.005 0.328 ! 1.83 eA-3
Q111 0.675 0.351 0.327 ! 1.80 eA-3
Q112 0.625 0.353 0.343 ! 1.79 eA-3
Q113 0.339 0.799 0.700 ! 1.74 eA-3
C114 0.129 0.549 0.013 ! 1.74 eA-3
Q115 0.765 0.130 0.311 ! 1.71 eA-3
Q116 0.529 0.926 0.281 ! 1.66 eA-3
Q117 0.471 0.074 0.719 ! 1.66 eA-3
Q118 0.941 0.268 0.419 ! 1.60 eA-3
Q119 0.499 0.240 0.219 ! 1.55 eA-3
Q120 0.436 0.835 0.667 ! 1.54 eA-3
Q121 0.554 0.094 0.362 ! 1.40 eA-3
Q122 0.848 0.279 0.312 ! 1.37 eA-3
C123 0.284 0.527 0.063 ! 1.33 eA-3
Q124 0.812 0.471 0.263 ! 1.33 eA-3
C125 0.951 0.485 0.062 ! 1.32 eA-3
Q126 0.934 0.392 0.047 ! 1.31 eA-3
Q127 0.094 0.340-0.001 ! 1.27 eA-3
Q128 0.629 0.298 0.250 ! 1.22 eA-3
Q129 0.379 0.956 0.609 ! 1.22 eA-3
Q130 0.052 0.950 0.081 ! 1.21 eA-3
C131 0.152 0.583 0.952 ! 1.18 eA-3
Q132 0.666 0.393 0.455 ! 1.17 eA-3
Q133 0.024 0.371 0.016 ! 1.16 eA-3
Q134 0.969 0.312 0.922 ! 1.16 eA-3
Q135 0.415 0.847 0.326 ! 1.13 eA-3
Q136 0.742 0.388 0.427 ! 1.13 eA-3
Q137 1.000 1.000 0.500 ! 1.10 eA-3
Q138 0.064 0.534 0.546 ! 1.09 eA-3
Q139 0.906 0.362 0.391 ! 1.09 eA-3
Q140 0.418 0.012 0.218 ! 1.08 eA-3
Q141 0.698 0.236 0.907 ! 1.07 eA-3
Q142 0.059 0.607 0.542 ! 1.05 eA-3
C143 0.533 0.645 0.078 ! 1.04 eA-3
Q144 0.402 0.718 0.285 ! 1.04 eA-3
Q145 0.793 0.371 0.394 ! 1.04 eA-3
Q146 0.861 0.306 0.467 ! 1.03 eA-3
Q147 0.911 0.778 0.063 ! 1.03 eA-3
Q148 0.616 0.922 0.406 ! 1.03 eA-3
Q149 0.801 0.437 0.294 ! 1.02 eA-3
Q150 0.663 0.046 0.250 ! 1.01 eA-3
Q151 0.383 0.778 0.769 ! 1.00 eA-3
Q152 0.518 0.968 0.593 ! 0.96 eA-3
Q153 0.543 0.444 0.232 ! 0.96 eA-3
Q154 0.675 0.531 0.358 ! 0.95 eA-3
Q155 0.709 0.483 0.310 ! 0.95 eA-3
Q156 0.232 0.668 0.468 ! 0.94 eA-3
C157 0.852 0.534 0.957 ! 0.94 eA-3
Q158 0.212 0.481 0.125 ! 0.94 eA-3
Q159 0.980 0.424 0.026 ! 0.94 eA-3
Q160 0.908 0.456 0.373 ! 0.93 eA-3
Q161 0.596 0.970 0.373 ! 0.92 eA-3
Q162 0.856 0.060 0.420 ! 0.91 eA-3
Q163 0.495 0.615 0.011 ! 0.91 eA-3
Q164 0.809 0.548 0.301 ! 0.90 eA-3
Q165 0.863 0.328 0.092 ! 0.90 eA-3
Q166 0.996 0.499 0.371 ! 0.90 eA-3
Q167 0.502 0.171 0.204 ! 0.89 eA-3
Q168 0.166 0.595 0.173 ! 0.89 eA-3
Q169 0.918 0.264 0.031 ! 0.88 eA-3
Q170 0.831 0.140 0.450 ! 0.88 eA-3
Q171 0.194 0.100 0.201 ! 0.87 eA-3
Q172 0.088 0.313 0.472 ! 0.87 eA-3
C173 0.613 0.606 0.063 ! 0.87 eA-3
Q174 0.215 0.997 0.671 ! 0.87 eA-3
Q175 0.381 0.144 0.780 ! 0.87 eA-3
Q176 0.320 0.971 0.199 ! 0.87 eA-3
Q177 0.177 0.259 0.096 ! 0.86 eA-3
C178 0.495 0.313 0.845 ! 0.86 eA-3
Q179 0.642 0.595 0.844 ! 0.86 eA-3
Q180 0.364 0.905 0.335 ! 0.85 eA-3
Q181 0.634 0.376 0.170 ! 0.85 eA-3
Q182 0.409 0.256 0.246 ! 0.85 eA-3
Q183 0.428 0.906 0.860 ! 0.85 eA-3
Q184 0.593 0.360 0.028 ! 0.85 eA-3
Q185 0.875 0.611 0.294 ! 0.84 eA-3
Q186 0.331 0.964 0.889 ! 0.84 eA-3
Q187 0.816 0.393 0.284 ! 0.84 eA-3
Q188 0.335 0.734 0.934 ! 0.84 eA-3
Q189 0.743 0.432 0.096 ! 0.84 eA-3
Q190 0.973 0.330 0.435 ! 0.84 eA-3
Q191 0.621 0.772 0.732 ! 0.84 eA-3
Q192 1.005 0.651 0.421 ! 0.83 eA-3
Q193 0.350 0.384 0.269 ! 0.83 eA-3
Q194 0.815 0.372 0.047 ! 0.83 eA-3
Q195 0.509 0.980 0.235 ! 0.82 eA-3
C196 0.157 0.612 0.109 ! 0.82 eA-3
Q197 0.345 0.469 0.249 ! 0.82 eA-3
Q198 0.662 0.252 0.142 ! 0.82 eA-3
Q199 0.338 0.346 0.392 ! 0.81 eA-3
;
_shelx_fab_checksum 44539
_database_code_depnum_ccdc_archive 'CCDC 933869'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_msb484_0m
#TrackingRef 'MSB-128 compound 9.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
cis-Dichloro(1,1'-bis(bis(2-methoxy-4-(3-propenyl)phenyl)
phosphino)ferrocene)platinum(II)
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C50 H52 Cl2 Fe O8 P2 Pt'
_chemical_formula_sum 'C50 H52 Cl2 Fe O8 P2 Pt'
_chemical_formula_weight 1164.70
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/c
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 14.9206(6)
_cell_length_b 19.1288(7)
_cell_length_c 18.0870(7)
_cell_angle_alpha 90.00
_cell_angle_beta 113.3490(10)
_cell_angle_gamma 90.00
_cell_volume 4739.5(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9412
_cell_measurement_theta_min 2.31
_cell_measurement_theta_max 29.10
_exptl_crystal_description Column
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.31
_exptl_crystal_size_mid 0.18
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.632
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2336
_exptl_absorpt_coefficient_mu 3.488
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.4321
_exptl_absorpt_correction_T_max 0.6263
_exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)'
_exptl_special_details
;
The diffraction data were obtained from 3 sets of 400 frames,
each of width 0.5 deg. in omega, colllected at phi = 0.00,
90.00 and 180.00 deg. and 2 sets of 800 frames, each of
width 0.45 deg in phi, collected at omega = -30.00 and 210.00
deg. The scan time was 15 sec/frame.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Smart APEX CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 83317
_diffrn_reflns_av_R_equivalents 0.0372
_diffrn_reflns_av_sigmaI/netI 0.0231
_diffrn_reflns_limit_h_min -19
_diffrn_reflns_limit_h_max 19
_diffrn_reflns_limit_k_min -26
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_theta_min 1.83
_diffrn_reflns_theta_max 29.13
_reflns_number_total 12365
_reflns_number_gt 11281
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2010)'
_computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2009)'
_computing_data_reduction 'Bruker SAINT (Bruker-AXS 2009)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008)'
_computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms were placed in
calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding
contributions with isotropic displacement parameters 1.2 - 1.5 times those
of the attached carbon atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+3.0807P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 12365
_refine_ls_number_parameters 581
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0237
_refine_ls_R_factor_gt 0.0199
_refine_ls_wR_factor_ref 0.0479
_refine_ls_wR_factor_gt 0.0462
_refine_ls_goodness_of_fit_ref 1.043
_refine_ls_restrained_S_all 1.043
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.000
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
Pt1 Pt 0.933817(5) 0.889750(3) 0.167021(4) 0.01048(2) Uani 1 1 d . . .
Fe1 Fe 0.84868(2) 1.003100(14) 0.336474(16) 0.01402(5) Uani 1 1 d . . .
Cl1 Cl 1.07319(3) 0.87383(2) 0.13926(3) 0.01640(9) Uani 1 1 d . . .
Cl2 Cl 0.84816(3) 0.82583(2) 0.04968(3) 0.01773(9) Uani 1 1 d . . .
P1 P 1.02140(3) 0.94960(2) 0.27782(3) 0.01097(8) Uani 1 1 d . . .
P2 P 0.78958(3) 0.90399(2) 0.17368(3) 0.01188(9) Uani 1 1 d . . .
O1 O 1.11248(9) 0.98806(6) 0.26872(7) 0.0131(2) Uani 1 1 d . . .
O2 O 1.08192(10) 1.12776(7) 0.25864(8) 0.0193(3) Uani 1 1 d . . .
O3 O 1.06579(10) 0.90281(6) 0.35791(8) 0.0145(3) Uani 1 1 d . . .
O4 O 1.03646(11) 0.80786(7) 0.44801(8) 0.0202(3) Uani 1 1 d . . .
O5 O 0.72760(9) 0.96601(7) 0.11546(8) 0.0149(3) Uani 1 1 d . . .
O6 O 0.86840(10) 1.03639(7) 0.08579(8) 0.0173(3) Uani 1 1 d . . .
O7 O 0.72427(10) 0.83418(7) 0.14583(8) 0.0162(3) Uani 1 1 d . . .
O8 O 0.74015(11) 0.74512(8) 0.26305(9) 0.0250(3) Uani 1 1 d . . .
C1 C 1.17345(13) 1.03201(9) 0.33136(11) 0.0139(3) Uani 1 1 d . . .
C2 C 1.24996(14) 1.00373(10) 0.39607(11) 0.0167(4) Uani 1 1 d . . .
H2 H 1.2600 0.9546 0.3997 0.020 Uiso 1 1 calc R . .
C3 C 1.31227(14) 1.04734(11) 0.45595(12) 0.0195(4) Uani 1 1 d . . .
H3 H 1.3651 1.0278 0.5003 0.023 Uiso 1 1 calc R . .
C4 C 1.29781(15) 1.11920(11) 0.45132(12) 0.0199(4) Uani 1 1 d . . .
C5 C 1.22052(14) 1.14740(10) 0.38602(12) 0.0184(4) Uani 1 1 d . . .
H5 H 1.2103 1.1965 0.3829 0.022 Uiso 1 1 calc R . .
C6 C 1.15769(14) 1.10439(9) 0.32494(11) 0.0153(4) Uani 1 1 d . . .
C7 C 1.05055(16) 1.19858(10) 0.26107(14) 0.0249(4) Uani 1 1 d . . .
H7A H 1.0420 1.2063 0.3114 0.037 Uiso 1 1 calc R . .
H7B H 0.9884 1.2067 0.2153 0.037 Uiso 1 1 calc R . .
H7C H 1.0999 1.2310 0.2581 0.037 Uiso 1 1 calc R . .
C8 C 1.36942(17) 1.16687(12) 0.51433(13) 0.0287(5) Uani 1 1 d . . .
H8A H 1.3384 1.2128 0.5136 0.034 Uiso 1 1 calc R . .
H8B H 1.3876 1.1461 0.5685 0.034 Uiso 1 1 calc R . .
C9 C 1.45918(17) 1.17676(12) 0.49738(14) 0.0309(5) Uani 1 1 d . . .
H9 H 1.4538 1.2065 0.4537 0.037 Uiso 1 1 calc R . .
C10 C 1.54470(19) 1.14780(15) 0.53782(17) 0.0411(6) Uani 1 1 d . . .
H10A H 1.5533 1.1177 0.5819 0.049 Uiso 1 1 calc R . .
H10B H 1.5979 1.1570 0.5229 0.049 Uiso 1 1 calc R . .
C11 C 1.11941(13) 0.84114(9) 0.36777(11) 0.0135(3) Uani 1 1 d . . .
C12 C 1.18532(14) 0.82965(10) 0.33312(11) 0.0171(4) Uani 1 1 d . . .
H12 H 1.1910 0.8621 0.2954 0.021 Uiso 1 1 calc R . .
C13 C 1.24340(14) 0.77024(10) 0.35373(12) 0.0194(4) Uani 1 1 d . . .
H13 H 1.2875 0.7615 0.3287 0.023 Uiso 1 1 calc R . .
C14 C 1.23798(14) 0.72341(10) 0.41041(12) 0.0203(4) Uani 1 1 d . . .
C15 C 1.16811(15) 0.73410(10) 0.44287(12) 0.0192(4) Uani 1 1 d . . .
H15 H 1.1618 0.7012 0.4799 0.023 Uiso 1 1 calc R . .
C16 C 1.10779(14) 0.79253(9) 0.42138(11) 0.0156(4) Uani 1 1 d . . .
C17 C 1.0197(2) 0.75776(11) 0.50030(15) 0.0309(5) Uani 1 1 d . . .
H17A H 1.0015 0.7127 0.4725 0.046 Uiso 1 1 calc R . .
H17B H 0.9667 0.7743 0.5150 0.046 Uiso 1 1 calc R . .
H17C H 1.0793 0.7521 0.5491 0.046 Uiso 1 1 calc R . .
C18 C 1.31254(17) 0.66545(12) 0.44167(16) 0.0329(5) Uani 1 1 d . . .
H18A H 1.3710 0.6841 0.4862 0.039 Uiso 1 1 calc R . .
H18B H 1.2850 0.6279 0.4641 0.039 Uiso 1 1 calc R . .
C19 C 1.34247(19) 0.63515(13) 0.38090(18) 0.0395(6) Uani 1 1 d . . .
H19 H 1.2984 0.6034 0.3438 0.047 Uiso 1 1 calc R . .
C20 C 1.4254(2) 0.64780(14) 0.37251(19) 0.0433(7) Uani 1 1 d . . .
H20A H 1.4718 0.6792 0.4081 0.052 Uiso 1 1 calc R . .
H20B H 1.4383 0.6254 0.3309 0.052 Uiso 1 1 calc R . .
C21 C 0.72012(14) 0.97405(10) 0.03560(11) 0.0151(3) Uani 1 1 d . . .
C22 C 0.63866(15) 0.94938(11) -0.02658(12) 0.0222(4) Uani 1 1 d . . .
H22 H 0.5888 0.9264 -0.0157 0.027 Uiso 1 1 calc R . .
C23 C 0.62932(15) 0.95824(12) -0.10593(12) 0.0252(4) Uani 1 1 d . . .
H23 H 0.5727 0.9412 -0.1489 0.030 Uiso 1 1 calc R . .
C24 C 0.70153(15) 0.99151(10) -0.12275(12) 0.0194(4) Uani 1 1 d . . .
C25 C 0.78323(14) 1.01745(10) -0.05882(11) 0.0161(4) Uani 1 1 d . . .
H25 H 0.8329 1.0407 -0.0697 0.019 Uiso 1 1 calc R . .
C26 C 0.79296(13) 1.00975(9) 0.02055(11) 0.0144(3) Uani 1 1 d . . .
C27 C 0.95578(14) 1.05502(10) 0.07490(12) 0.0194(4) Uani 1 1 d . . .
H27A H 0.9815 1.0137 0.0579 0.029 Uiso 1 1 calc R . .
H27B H 1.0046 1.0726 0.1258 0.029 Uiso 1 1 calc R . .
H27C H 0.9407 1.0914 0.0336 0.029 Uiso 1 1 calc R . .
C28 C 0.69427(16) 0.99914(12) -0.20855(12) 0.0249(4) Uani 1 1 d . . .
H28A H 0.7247 1.0440 -0.2133 0.030 Uiso 1 1 calc R . .
H28B H 0.7319 0.9610 -0.2198 0.030 Uiso 1 1 calc R . .
C29 C 0.59156(17) 0.99734(13) -0.27073(13) 0.0286(5) Uani 1 1 d . . .
H29 H 0.5479 1.0326 -0.2684 0.034 Uiso 1 1 calc R . .
C30 C 0.5577(2) 0.95030(15) -0.32818(14) 0.0396(6) Uani 1 1 d . . .
H30A H 0.5992 0.9142 -0.3323 0.047 Uiso 1 1 calc R . .
H30B H 0.4916 0.9524 -0.3656 0.047 Uiso 1 1 calc R . .
C31 C 0.64354(14) 0.82544(10) 0.16664(12) 0.0172(4) Uani 1 1 d . . .
C32 C 0.55891(15) 0.86274(11) 0.12849(12) 0.0216(4) Uani 1 1 d . . .
H32 H 0.5541 0.8950 0.0871 0.026 Uiso 1 1 calc R . .
C33 C 0.48038(15) 0.85321(12) 0.15050(13) 0.0250(4) Uani 1 1 d . . .
H33 H 0.4221 0.8793 0.1243 0.030 Uiso 1 1 calc R . .
C34 C 0.48664(16) 0.80587(12) 0.21038(13) 0.0253(4) Uani 1 1 d . . .
C35 C 0.57272(16) 0.76861(11) 0.24905(13) 0.0245(4) Uani 1 1 d . . .
H35 H 0.5773 0.7364 0.2903 0.029 Uiso 1 1 calc R . .
C36 C 0.65271(15) 0.77794(10) 0.22804(12) 0.0198(4) Uani 1 1 d . . .
C37 C 0.7557(2) 0.70279(14) 0.33221(16) 0.0422(6) Uani 1 1 d . . .
H37A H 0.7523 0.7321 0.3755 0.063 Uiso 1 1 calc R . .
H37B H 0.8201 0.6808 0.3503 0.063 Uiso 1 1 calc R . .
H37C H 0.7052 0.6665 0.3182 0.063 Uiso 1 1 calc R . .
C38 C 0.39958(17) 0.79450(14) 0.23190(15) 0.0335(5) Uani 1 1 d . . .
H38A H 0.4233 0.7786 0.2885 0.040 Uiso 1 1 calc R . .
H38B H 0.3660 0.8398 0.2282 0.040 Uiso 1 1 calc R . .
C39 C 0.32682(19) 0.74227(14) 0.17952(16) 0.0379(6) Uani 1 1 d . . .
H39 H 0.2653 0.7409 0.1835 0.045 Uiso 1 1 calc R . .
C40 C 0.33964(19) 0.69862(14) 0.12909(16) 0.0389(6) Uani 1 1 d . . .
H40A H 0.3999 0.6979 0.1228 0.047 Uiso 1 1 calc R . .
H40B H 0.2887 0.6676 0.0986 0.047 Uiso 1 1 calc R . .
C41 C 0.97104(13) 1.01616(9) 0.31814(11) 0.0134(3) Uani 1 1 d . . .
C42 C 0.99145(14) 1.02716(10) 0.40188(11) 0.0165(4) Uani 1 1 d . . .
H42 H 1.0364 1.0013 0.4458 0.020 Uiso 1 1 calc R . .
C43 C 0.93230(15) 1.08363(10) 0.40708(12) 0.0205(4) Uani 1 1 d . . .
H43 H 0.9304 1.1020 0.4552 0.025 Uiso 1 1 calc R . .
C44 C 0.87646(16) 1.10801(10) 0.32765(13) 0.0201(4) Uani 1 1 d . . .
H44 H 0.8309 1.1454 0.3139 0.024 Uiso 1 1 calc R . .
C45 C 0.90030(14) 1.06696(9) 0.27240(11) 0.0154(4) Uani 1 1 d . . .
H45 H 0.8741 1.0723 0.2155 0.019 Uiso 1 1 calc R . .
C46 C 0.77290(13) 0.92766(9) 0.26240(11) 0.0141(3) Uani 1 1 d . . .
C47 C 0.82755(14) 0.89857(10) 0.34106(11) 0.0161(4) Uani 1 1 d . . .
H47 H 0.8762 0.8633 0.3539 0.019 Uiso 1 1 calc R . .
C48 C 0.79515(15) 0.93248(11) 0.39588(12) 0.0208(4) Uani 1 1 d . . .
H48 H 0.8188 0.9239 0.4521 0.025 Uiso 1 1 calc R . .
C49 C 0.72157(15) 0.98128(11) 0.35258(12) 0.0220(4) Uani 1 1 d . . .
H49 H 0.6880 1.0111 0.3751 0.026 Uiso 1 1 calc R . .
C50 C 0.70627(14) 0.97837(10) 0.27020(12) 0.0186(4) Uani 1 1 d . . .
H50 H 0.6603 1.0051 0.2278 0.022 Uiso 1 1 calc 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
Pt1 0.01323(4) 0.01013(3) 0.00988(4) -0.00144(2) 0.00648(3) -0.00155(2)
Fe1 0.01582(13) 0.01615(12) 0.01243(12) -0.00320(10) 0.00806(10) -0.00152(10)
Cl1 0.0163(2) 0.01879(19) 0.0176(2) -0.00404(16) 0.01036(18) -0.00182(16)
Cl2 0.0186(2) 0.0207(2) 0.0151(2) -0.00770(16) 0.00791(17) -0.00320(17)
P1 0.0131(2) 0.01063(19) 0.0102(2) -0.00053(16) 0.00579(17) -0.00149(16)
P2 0.0137(2) 0.0131(2) 0.0106(2) -0.00144(16) 0.00653(18) -0.00251(16)
O1 0.0150(6) 0.0139(6) 0.0117(6) -0.0027(5) 0.0066(5) -0.0048(5)
O2 0.0223(7) 0.0147(6) 0.0162(7) 0.0011(5) 0.0025(6) -0.0020(5)
O3 0.0195(7) 0.0133(6) 0.0119(6) 0.0015(5) 0.0075(5) 0.0016(5)
O4 0.0313(8) 0.0164(6) 0.0198(7) 0.0017(5) 0.0175(6) -0.0023(6)
O5 0.0174(6) 0.0182(6) 0.0110(6) 0.0013(5) 0.0075(5) 0.0001(5)
O6 0.0178(7) 0.0212(7) 0.0137(6) -0.0020(5) 0.0070(5) -0.0057(5)
O7 0.0176(6) 0.0171(6) 0.0178(7) -0.0043(5) 0.0113(5) -0.0058(5)
O8 0.0302(8) 0.0229(7) 0.0246(8) 0.0048(6) 0.0137(7) 0.0009(6)
C1 0.0147(8) 0.0163(8) 0.0128(8) -0.0035(7) 0.0076(7) -0.0052(7)
C2 0.0165(9) 0.0171(8) 0.0171(9) -0.0003(7) 0.0073(8) -0.0025(7)
C3 0.0161(9) 0.0261(10) 0.0143(9) 0.0000(7) 0.0040(7) -0.0017(8)
C4 0.0186(9) 0.0251(10) 0.0160(9) -0.0059(7) 0.0068(8) -0.0057(8)
C5 0.0201(9) 0.0164(8) 0.0181(9) -0.0054(7) 0.0069(8) -0.0039(7)
C6 0.0161(9) 0.0167(8) 0.0134(9) -0.0010(7) 0.0063(7) -0.0030(7)
C7 0.0261(11) 0.0146(9) 0.0279(11) 0.0018(8) 0.0042(9) -0.0003(8)
C8 0.0283(11) 0.0306(11) 0.0211(11) -0.0109(9) 0.0032(9) -0.0063(9)
C9 0.0296(12) 0.0306(11) 0.0252(11) -0.0044(9) 0.0030(10) -0.0128(9)
C10 0.0293(13) 0.0504(16) 0.0356(14) -0.0057(12) 0.0044(11) -0.0089(12)
C11 0.0161(8) 0.0107(7) 0.0111(8) 0.0011(6) 0.0025(7) -0.0007(6)
C12 0.0175(9) 0.0163(8) 0.0172(9) 0.0035(7) 0.0066(8) -0.0001(7)
C13 0.0163(9) 0.0199(9) 0.0215(10) 0.0018(7) 0.0070(8) 0.0009(7)
C14 0.0176(9) 0.0146(8) 0.0236(10) 0.0030(7) 0.0026(8) 0.0003(7)
C15 0.0240(10) 0.0149(8) 0.0159(9) 0.0034(7) 0.0051(8) -0.0041(7)
C16 0.0194(9) 0.0145(8) 0.0123(8) -0.0017(7) 0.0058(7) -0.0049(7)
C17 0.0526(15) 0.0199(10) 0.0348(12) 0.0027(9) 0.0329(12) -0.0065(10)
C18 0.0265(11) 0.0251(11) 0.0429(14) 0.0152(10) 0.0093(10) 0.0073(9)
C19 0.0337(13) 0.0245(11) 0.0505(16) -0.0030(11) 0.0064(12) 0.0083(10)
C20 0.0365(14) 0.0354(13) 0.0557(18) 0.0069(12) 0.0158(13) 0.0172(11)
C21 0.0186(9) 0.0179(8) 0.0106(8) 0.0012(7) 0.0076(7) 0.0005(7)
C22 0.0212(10) 0.0294(10) 0.0179(10) 0.0009(8) 0.0097(8) -0.0082(8)
C23 0.0201(10) 0.0392(12) 0.0144(10) -0.0016(8) 0.0049(8) -0.0122(9)
C24 0.0214(10) 0.0238(9) 0.0138(9) 0.0011(7) 0.0079(8) -0.0026(8)
C25 0.0179(9) 0.0177(8) 0.0147(9) 0.0004(7) 0.0086(7) -0.0024(7)
C26 0.0163(9) 0.0138(8) 0.0120(8) -0.0001(6) 0.0046(7) -0.0001(7)
C27 0.0184(9) 0.0227(9) 0.0169(9) 0.0007(7) 0.0068(8) -0.0063(8)
C28 0.0266(11) 0.0357(12) 0.0144(9) -0.0004(8) 0.0101(9) -0.0091(9)
C29 0.0296(12) 0.0403(13) 0.0155(10) 0.0030(9) 0.0084(9) -0.0051(10)
C30 0.0347(13) 0.0611(17) 0.0217(12) -0.0054(11) 0.0099(10) -0.0140(12)
C31 0.0182(9) 0.0196(9) 0.0172(9) -0.0052(7) 0.0104(8) -0.0079(7)
C32 0.0200(10) 0.0278(10) 0.0173(10) -0.0029(8) 0.0077(8) -0.0077(8)
C33 0.0174(10) 0.0356(12) 0.0219(11) -0.0061(9) 0.0078(8) -0.0041(9)
C34 0.0251(11) 0.0310(11) 0.0258(11) -0.0106(9) 0.0165(9) -0.0123(9)
C35 0.0325(12) 0.0240(10) 0.0231(10) -0.0019(8) 0.0176(9) -0.0101(9)
C36 0.0241(10) 0.0186(9) 0.0189(10) -0.0044(7) 0.0109(8) -0.0063(8)
C37 0.0503(16) 0.0405(14) 0.0399(15) 0.0214(12) 0.0224(13) 0.0112(12)
C38 0.0287(12) 0.0422(13) 0.0386(13) -0.0113(11) 0.0228(11) -0.0146(10)
C39 0.0300(13) 0.0477(15) 0.0400(14) -0.0070(12) 0.0182(11) -0.0186(11)
C40 0.0342(13) 0.0427(14) 0.0372(14) -0.0050(11) 0.0115(11) -0.0150(11)
C41 0.0151(8) 0.0140(8) 0.0131(8) -0.0022(6) 0.0076(7) -0.0026(7)
C42 0.0183(9) 0.0186(9) 0.0133(9) -0.0041(7) 0.0069(7) -0.0043(7)
C43 0.0263(10) 0.0200(9) 0.0182(10) -0.0083(8) 0.0121(8) -0.0050(8)
C44 0.0237(10) 0.0158(9) 0.0239(10) -0.0036(7) 0.0127(9) 0.0008(7)
C45 0.0179(9) 0.0146(8) 0.0155(9) -0.0009(7) 0.0083(7) -0.0006(7)
C46 0.0154(8) 0.0171(8) 0.0114(8) -0.0024(7) 0.0069(7) -0.0034(7)
C47 0.0171(9) 0.0175(8) 0.0141(9) -0.0002(7) 0.0067(7) -0.0038(7)
C48 0.0233(10) 0.0283(10) 0.0143(9) -0.0029(8) 0.0111(8) -0.0080(8)
C49 0.0205(10) 0.0300(10) 0.0212(10) -0.0081(8) 0.0145(8) -0.0052(8)
C50 0.0164(9) 0.0223(9) 0.0190(10) -0.0033(7) 0.0090(8) -0.0011(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
Pt1 P2 2.2194(5) . ?
Pt1 P1 2.2268(5) . ?
Pt1 Cl2 2.3415(4) . ?
Pt1 Cl1 2.3445(4) . ?
Fe1 C46 1.9887(18) . ?
Fe1 C41 1.9963(18) . ?
Fe1 C47 2.0310(18) . ?
Fe1 C45 2.0337(18) . ?
Fe1 C42 2.0375(19) . ?
Fe1 C50 2.039(2) . ?
Fe1 C44 2.0680(19) . ?
Fe1 C49 2.072(2) . ?
Fe1 C43 2.0730(19) . ?
Fe1 C48 2.073(2) . ?
P1 O3 1.6055(13) . ?
P1 O1 1.6100(13) . ?
P1 C41 1.7754(18) . ?
P2 O7 1.6117(13) . ?
P2 O5 1.6122(13) . ?
P2 C46 1.7772(18) . ?
O1 C1 1.415(2) . ?
O2 C6 1.357(2) . ?
O2 C7 1.440(2) . ?
O3 C11 1.396(2) . ?
O4 C16 1.363(2) . ?
O4 C17 1.436(2) . ?
O5 C21 1.412(2) . ?
O6 C26 1.366(2) . ?
O6 C27 1.438(2) . ?
O7 C31 1.407(2) . ?
O8 C36 1.357(3) . ?
O8 C37 1.430(3) . ?
C1 C2 1.381(3) . ?
C1 C6 1.401(2) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.389(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.391(3) . ?
C4 C8 1.519(3) . ?
C5 C6 1.398(3) . ?
C5 H5 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.500(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.315(4) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9500 . ?
C10 H10B 0.9500 . ?
C11 C12 1.377(3) . ?
C11 C16 1.403(2) . ?
C12 C13 1.388(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.400(3) . ?
C14 C18 1.513(3) . ?
C15 C16 1.390(3) . ?
C15 H15 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.460(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.327(4) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9500 . ?
C20 H20B 0.9500 . ?
C21 C22 1.372(3) . ?
C21 C26 1.399(3) . ?
C22 C23 1.396(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.385(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.397(3) . ?
C24 C28 1.519(3) . ?
C25 C26 1.392(2) . ?
C25 H25 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.499(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.315(3) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9500 . ?
C30 H30B 0.9500 . ?
C31 C32 1.374(3) . ?
C31 C36 1.399(3) . ?
C32 C33 1.391(3) . ?
C32 H32 0.9500 . ?
C33 C34 1.386(3) . ?
C33 H33 0.9500 . ?
C34 C35 1.391(3) . ?
C34 C38 1.512(3) . ?
C35 C36 1.400(3) . ?
C35 H35 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.503(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.305(4) . ?
C39 H39 0.9500 . ?
C40 H40A 0.9500 . ?
C40 H40B 0.9500 . ?
C41 C45 1.432(3) . ?
C41 C42 1.437(2) . ?
C42 C43 1.422(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.424(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.422(3) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C50 1.435(3) . ?
C46 C47 1.442(3) . ?
C47 C48 1.420(3) . ?
C47 H47 0.9500 . ?
C48 C49 1.417(3) . ?
C48 H48 0.9500 . ?
C49 C50 1.416(3) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
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
P2 Pt1 P1 97.117(17) . . ?
P2 Pt1 Cl2 85.447(16) . . ?
P1 Pt1 Cl2 177.436(16) . . ?
P2 Pt1 Cl1 171.499(17) . . ?
P1 Pt1 Cl1 90.315(16) . . ?
Cl2 Pt1 Cl1 87.128(16) . . ?
C46 Fe1 C41 106.98(7) . . ?
C46 Fe1 C47 42.03(7) . . ?
C41 Fe1 C47 107.28(8) . . ?
C46 Fe1 C45 107.13(7) . . ?
C41 Fe1 C45 41.62(7) . . ?
C47 Fe1 C45 135.62(7) . . ?
C46 Fe1 C42 137.69(8) . . ?
C41 Fe1 C42 41.73(7) . . ?
C47 Fe1 C42 110.01(8) . . ?
C45 Fe1 C42 69.53(8) . . ?
C46 Fe1 C50 41.74(7) . . ?
C41 Fe1 C50 137.73(8) . . ?
C47 Fe1 C50 69.70(8) . . ?
C45 Fe1 C50 110.25(8) . . ?
C42 Fe1 C50 179.37(8) . . ?
C46 Fe1 C44 136.88(8) . . ?
C41 Fe1 C44 68.98(8) . . ?
C47 Fe1 C44 176.01(8) . . ?
C45 Fe1 C44 40.57(7) . . ?
C42 Fe1 C44 68.30(8) . . ?
C50 Fe1 C44 111.95(8) . . ?
C46 Fe1 C49 68.96(8) . . ?
C41 Fe1 C49 175.40(8) . . ?
C47 Fe1 C49 68.31(8) . . ?
C45 Fe1 C49 140.85(8) . . ?
C42 Fe1 C49 140.21(8) . . ?
C50 Fe1 C49 40.29(8) . . ?
C44 Fe1 C49 115.39(8) . . ?
C46 Fe1 C43 175.46(8) . . ?
C41 Fe1 C43 69.06(7) . . ?
C47 Fe1 C43 140.51(8) . . ?
C45 Fe1 C43 68.49(8) . . ?
C42 Fe1 C43 40.45(8) . . ?
C50 Fe1 C43 140.10(8) . . ?
C44 Fe1 C43 40.21(8) . . ?
C49 Fe1 C43 115.09(8) . . ?
C46 Fe1 C48 69.11(7) . . ?
C41 Fe1 C48 137.16(8) . . ?
C47 Fe1 C48 40.48(8) . . ?
C45 Fe1 C48 175.94(8) . . ?
C42 Fe1 C48 112.04(8) . . ?
C50 Fe1 C48 68.14(8) . . ?
C44 Fe1 C48 143.37(8) . . ?
C49 Fe1 C48 39.98(8) . . ?
C43 Fe1 C48 115.24(8) . . ?
O3 P1 O1 106.49(7) . . ?
O3 P1 C41 96.87(8) . . ?
O1 P1 C41 103.06(8) . . ?
O3 P1 Pt1 114.23(5) . . ?
O1 P1 Pt1 111.16(5) . . ?
C41 P1 Pt1 123.05(6) . . ?
O7 P2 O5 106.64(7) . . ?
O7 P2 C46 102.10(8) . . ?
O5 P2 C46 98.80(8) . . ?
O7 P2 Pt1 111.13(5) . . ?
O5 P2 Pt1 111.87(5) . . ?
C46 P2 Pt1 124.47(6) . . ?
C1 O1 P1 119.39(11) . . ?
C6 O2 C7 116.75(15) . . ?
C11 O3 P1 126.64(12) . . ?
C16 O4 C17 116.97(16) . . ?
C21 O5 P2 122.72(12) . . ?
C26 O6 C27 117.09(14) . . ?
C31 O7 P2 119.37(11) . . ?
C36 O8 C37 117.55(18) . . ?
C2 C1 C6 120.84(17) . . ?
C2 C1 O1 119.95(16) . . ?
C6 C1 O1 119.16(16) . . ?
C1 C2 C3 119.86(18) . . ?
C1 C2 H2 120.1 . . ?
C3 C2 H2 120.1 . . ?
C4 C3 C2 120.43(18) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 119.45(18) . . ?
C3 C4 C8 120.18(19) . . ?
C5 C4 C8 120.27(19) . . ?
C4 C5 C6 120.87(18) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
O2 C6 C5 124.56(17) . . ?
O2 C6 C1 116.90(16) . . ?
C5 C6 C1 118.54(18) . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C4 110.00(18) . . ?
C9 C8 H8A 109.7 . . ?
C4 C8 H8A 109.7 . . ?
C9 C8 H8B 109.7 . . ?
C4 C8 H8B 109.7 . . ?
H8A C8 H8B 108.2 . . ?
C10 C9 C8 125.5(2) . . ?
C10 C9 H9 117.2 . . ?
C8 C9 H9 117.2 . . ?
C9 C10 H10A 120.0 . . ?
C9 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?
C12 C11 O3 123.57(16) . . ?
C12 C11 C16 120.99(17) . . ?
O3 C11 C16 115.26(16) . . ?
C11 C12 C13 119.41(17) . . ?
C11 C12 H12 120.3 . . ?
C13 C12 H12 120.3 . . ?
C14 C13 C12 120.94(19) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C15 119.13(18) . . ?
C13 C14 C18 119.99(19) . . ?
C15 C14 C18 120.67(19) . . ?
C16 C15 C14 120.49(17) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
O4 C16 C15 125.71(17) . . ?
O4 C16 C11 115.43(16) . . ?
C15 C16 C11 118.85(18) . . ?
O4 C17 H17A 109.5 . . ?
O4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C14 114.1(2) . . ?
C19 C18 H18A 108.7 . . ?
C14 C18 H18A 108.7 . . ?
C19 C18 H18B 108.7 . . ?
C14 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C20 C19 C18 126.2(3) . . ?
C20 C19 H19 116.9 . . ?
C18 C19 H19 116.9 . . ?
C19 C20 H20A 120.0 . . ?
C19 C20 H20B 120.0 . . ?
H20A C20 H20B 120.0 . . ?
C22 C21 C26 120.85(17) . . ?
C22 C21 O5 119.10(16) . . ?
C26 C21 O5 119.98(16) . . ?
C21 C22 C23 119.74(18) . . ?
C21 C22 H22 120.1 . . ?
C23 C22 H22 120.1 . . ?
C24 C23 C22 120.81(19) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 118.75(18) . . ?
C23 C24 C28 121.45(18) . . ?
C25 C24 C28 119.79(17) . . ?
C26 C25 C24 121.06(17) . . ?
C26 C25 H25 119.5 . . ?
C24 C25 H25 119.5 . . ?
O6 C26 C25 124.38(16) . . ?
O6 C26 C21 116.86(16) . . ?
C25 C26 C21 118.74(17) . . ?
O6 C27 H27A 109.5 . . ?
O6 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O6 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C24 113.69(17) . . ?
C29 C28 H28A 108.8 . . ?
C24 C28 H28A 108.8 . . ?
C29 C28 H28B 108.8 . . ?
C24 C28 H28B 108.8 . . ?
H28A C28 H28B 107.7 . . ?
C30 C29 C28 124.6(2) . . ?
C30 C29 H29 117.7 . . ?
C28 C29 H29 117.7 . . ?
C29 C30 H30A 120.0 . . ?
C29 C30 H30B 120.0 . . ?
H30A C30 H30B 120.0 . . ?
C32 C31 C36 121.13(18) . . ?
C32 C31 O7 121.17(17) . . ?
C36 C31 O7 117.70(18) . . ?
C31 C32 C33 119.9(2) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 120.4(2) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 119.37(19) . . ?
C33 C34 C38 119.8(2) . . ?
C35 C34 C38 120.9(2) . . ?
C34 C35 C36 120.98(19) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
O8 C36 C31 116.38(17) . . ?
O8 C36 C35 125.41(19) . . ?
C31 C36 C35 118.21(19) . . ?
O8 C37 H37A 109.5 . . ?
O8 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O8 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C34 114.40(19) . . ?
C39 C38 H38A 108.7 . . ?
C34 C38 H38A 108.7 . . ?
C39 C38 H38B 108.7 . . ?
C34 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?
C40 C39 C38 126.6(2) . . ?
C40 C39 H39 116.7 . . ?
C38 C39 H39 116.7 . . ?
C39 C40 H40A 120.0 . . ?
C39 C40 H40B 120.0 . . ?
H40A C40 H40B 120.0 . . ?
C45 C41 C42 108.02(16) . . ?
C45 C41 P1 125.76(14) . . ?
C42 C41 P1 126.19(14) . . ?
C45 C41 Fe1 70.59(10) . . ?
C42 C41 Fe1 70.67(10) . . ?
P1 C41 Fe1 122.84(9) . . ?
C43 C42 C41 107.65(17) . . ?
C43 C42 Fe1 71.12(11) . . ?
C41 C42 Fe1 67.60(10) . . ?
C43 C42 H42 126.2 . . ?
C41 C42 H42 126.2 . . ?
Fe1 C42 H42 126.6 . . ?
C42 C43 C44 108.22(17) . . ?
C42 C43 Fe1 68.43(11) . . ?
C44 C43 Fe1 69.70(11) . . ?
C42 C43 H43 125.9 . . ?
C44 C43 H43 125.9 . . ?
Fe1 C43 H43 127.5 . . ?
C45 C44 C43 108.59(17) . . ?
C45 C44 Fe1 68.42(10) . . ?
C43 C44 Fe1 70.08(11) . . ?
C45 C44 H44 125.7 . . ?
C43 C44 H44 125.7 . . ?
Fe1 C44 H44 127.4 . . ?
C44 C45 C41 107.52(17) . . ?
C44 C45 Fe1 71.01(11) . . ?
C41 C45 Fe1 67.79(10) . . ?
C44 C45 H45 126.2 . . ?
C41 C45 H45 126.2 . . ?
Fe1 C45 H45 126.5 . . ?
C50 C46 C47 107.85(16) . . ?
C50 C46 P2 127.67(15) . . ?
C47 C46 P2 124.46(14) . . ?
C50 C46 Fe1 71.00(11) . . ?
C47 C46 Fe1 70.55(10) . . ?
P2 C46 Fe1 123.20(10) . . ?
C48 C47 C46 107.26(17) . . ?
C48 C47 Fe1 71.35(11) . . ?
C46 C47 Fe1 67.42(10) . . ?
C48 C47 H47 126.4 . . ?
C46 C47 H47 126.4 . . ?
Fe1 C47 H47 126.4 . . ?
C49 C48 C47 108.57(17) . . ?
C49 C48 Fe1 69.98(11) . . ?
C47 C48 Fe1 68.17(11) . . ?
C49 C48 H48 125.7 . . ?
C47 C48 H48 125.7 . . ?
Fe1 C48 H48 127.7 . . ?
C50 C49 C48 108.79(17) . . ?
C50 C49 Fe1 68.58(11) . . ?
C48 C49 Fe1 70.04(11) . . ?
C50 C49 H49 125.6 . . ?
C48 C49 H49 125.6 . . ?
Fe1 C49 H49 127.4 . . ?
C49 C50 C46 107.51(18) . . ?
C49 C50 Fe1 71.12(11) . . ?
C46 C50 Fe1 67.26(10) . . ?
C49 C50 H50 126.2 . . ?
C46 C50 H50 126.2 . . ?
Fe1 C50 H50 126.9 . . ?
_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full 29.13
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 1.743
_refine_diff_density_min -0.814
_refine_diff_density_rms 0.085
_database_code_depnum_ccdc_archive 'CCDC 933870'
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
data_msb418_0m
#TrackingRef 'MSB-128- Compoun 8.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C50 H52 Cl2 Fe O8 P2 Pd'
_chemical_formula_sum 'C50 H52 Cl2 Fe O8 P2 Pd'
_chemical_formula_weight 1076.01
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/c
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 14.9965(13)
_cell_length_b 19.1024(16)
_cell_length_c 18.0574(15)
_cell_angle_alpha 90.00
_cell_angle_beta 113.145(1)
_cell_angle_gamma 90.00
_cell_volume 4756.5(7)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9954
_cell_measurement_theta_min 2.31
_cell_measurement_theta_max 26.40
_exptl_crystal_description Plate
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.16
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.503
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2208
_exptl_absorpt_coefficient_mu 0.916
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7912
_exptl_absorpt_correction_T_max 0.9686
_exptl_absorpt_process_details 'SADABS (Sheldrick, 2008a)'
_exptl_special_details
;
The diffraction data were collected in three sets of
606 frames (0.3 deg. width in omega) at phi = 0, 120
and 240 deg. A scan time of 60 sec/frame was used.
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX-I CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 37771
_diffrn_reflns_av_R_equivalents 0.0644
_diffrn_reflns_av_sigmaI/netI 0.0630
_diffrn_reflns_limit_h_min -18
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 1.48
_diffrn_reflns_theta_max 26.41
_reflns_number_total 9756
_reflns_number_gt 6785
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2009)'
_computing_cell_refinement 'Bruker SAINT (Bruker-AXS 2008)'
_computing_data_reduction 'Bruker SAINT (Bruker-AXS 2008)'
_computing_structure_solution 'SHELXS (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL(Bruker-AXS 2008a)'
_computing_publication_material 'Bruker SHELXTL(Bruker-AXS 2008a)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger. H-atoms were placed in
calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding
contributions with isotropic displacement parameters 1.2 - 1.5 times those
of the attached carbon atoms.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+5.0076P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9756
_refine_ls_number_parameters 581
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0852
_refine_ls_R_factor_gt 0.0507
_refine_ls_wR_factor_ref 0.1260
_refine_ls_wR_factor_gt 0.1100
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_restrained_S_all 1.035
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
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
Pd1 Pd 0.06433(3) 0.388596(17) 0.334015(18) 0.02314(10) Uani 1 1 d . . .
Fe1 Fe 0.14971(5) 0.50129(3) 0.16314(4) 0.02823(17) Uani 1 1 d . . .
Cl1 Cl 0.15295(9) 0.32583(6) 0.45065(6) 0.0323(3) Uani 1 1 d . . .
Cl2 Cl -0.07461(8) 0.37532(6) 0.36163(6) 0.0293(3) Uani 1 1 d . . .
P1 P 0.20868(9) 0.40076(6) 0.32530(6) 0.0255(3) Uani 1 1 d . . .
P2 P -0.02325(9) 0.44921(6) 0.22170(6) 0.0224(2) Uani 1 1 d . . .
O1 O 0.2714(2) 0.46245(16) 0.38348(16) 0.0290(7) Uani 1 1 d . . .
O2 O 0.1289(2) 0.52890(16) 0.41258(17) 0.0294(7) Uani 1 1 d . . .
O3 O 0.2718(2) 0.33034(16) 0.35144(17) 0.0310(7) Uani 1 1 d . . .
O4 O 0.2565(3) 0.24197(18) 0.2339(2) 0.0477(10) Uani 1 1 d . . .
O5 O -0.1137(2) 0.48792(15) 0.23043(16) 0.0251(7) Uani 1 1 d . . .
O6 O -0.0818(2) 0.62740(15) 0.24009(18) 0.0330(8) Uani 1 1 d . . .
O7 O -0.0668(2) 0.40166(15) 0.14222(16) 0.0259(7) Uani 1 1 d . . .
O8 O -0.0378(3) 0.30759(16) 0.05075(18) 0.0348(8) Uani 1 1 d . . .
C1 C 0.2799(4) 0.4719(3) 0.4640(3) 0.0308(11) Uani 1 1 d . . .
C2 C 0.2057(3) 0.5063(2) 0.4785(2) 0.0253(10) Uani 1 1 d . . .
C3 C 0.2167(4) 0.5156(2) 0.5581(3) 0.0310(11) Uani 1 1 d . . .
H3 H 0.1665 0.5376 0.5692 0.037 Uiso 1 1 calc R . .
C4 C 0.2996(4) 0.4934(3) 0.6212(3) 0.0371(12) Uani 1 1 d . . .
C5 C 0.3734(4) 0.4616(3) 0.6051(3) 0.0482(15) Uani 1 1 d . . .
H5 H 0.4311 0.4469 0.6482 0.058 Uiso 1 1 calc R . .
C6 C 0.3624(4) 0.4515(3) 0.5256(3) 0.0414(13) Uani 1 1 d . . .
H6 H 0.4129 0.4301 0.5145 0.050 Uiso 1 1 calc R . .
C7 C 0.0442(3) 0.5523(2) 0.4246(3) 0.0313(11) Uani 1 1 d . . .
H7A H 0.0169 0.5132 0.4439 0.047 Uiso 1 1 calc R . .
H7B H -0.0041 0.5696 0.3735 0.047 Uiso 1 1 calc R . .
H7C H 0.0624 0.5900 0.4645 0.047 Uiso 1 1 calc R . .
C8 C 0.3077(4) 0.5026(3) 0.7076(3) 0.0454(14) Uani 1 1 d . . .
H8A H 0.2778 0.5479 0.7117 0.054 Uiso 1 1 calc R . .
H8B H 0.2700 0.4651 0.7198 0.054 Uiso 1 1 calc R . .
C9 C 0.4086(4) 0.5010(3) 0.7693(3) 0.0502(15) Uani 1 1 d . . .
H9 H 0.4513 0.5368 0.7667 0.060 Uiso 1 1 calc R . .
C10 C 0.4442(5) 0.4547(4) 0.8269(3) 0.069(2) Uani 1 1 d . . .
H10A H 0.4043 0.4179 0.8320 0.083 Uiso 1 1 calc R . .
H10B H 0.5099 0.4579 0.8638 0.083 Uiso 1 1 calc R . .
C11 C 0.3532(4) 0.3208(3) 0.3310(3) 0.0336(12) Uani 1 1 d . . .
C12 C 0.3439(4) 0.2739(3) 0.2695(3) 0.0387(13) Uani 1 1 d . . .
C13 C 0.4250(5) 0.2638(3) 0.2493(3) 0.0520(16) Uani 1 1 d . . .
H13 H 0.4210 0.2312 0.2084 0.062 Uiso 1 1 calc R . .
C14 C 0.5100(5) 0.3008(3) 0.2884(4) 0.0515(16) Uani 1 1 d . . .
C15 C 0.5161(4) 0.3479(3) 0.3484(3) 0.0518(15) Uani 1 1 d . . .
H15 H 0.5741 0.3738 0.3749 0.062 Uiso 1 1 calc R . .
C16 C 0.4377(4) 0.3574(3) 0.3699(3) 0.0424(13) Uani 1 1 d . . .
H16 H 0.4424 0.3893 0.4117 0.051 Uiso 1 1 calc R . .
C17 C 0.2404(6) 0.1986(4) 0.1644(4) 0.079(2) Uani 1 1 d . . .
H17A H 0.2497 0.2265 0.1224 0.119 Uiso 1 1 calc R . .
H17B H 0.1740 0.1803 0.1437 0.119 Uiso 1 1 calc R . .
H17C H 0.2864 0.1595 0.1797 0.119 Uiso 1 1 calc R . .
C18 C 0.5975(5) 0.2896(4) 0.2675(4) 0.073(2) Uani 1 1 d . . .
H18A H 0.5748 0.2722 0.2114 0.088 Uiso 1 1 calc R . .
H18B H 0.6293 0.3354 0.2695 0.088 Uiso 1 1 calc R . .
C19 C 0.6709(6) 0.2396(4) 0.3213(4) 0.077(2) Uani 1 1 d . . .
H19 H 0.7330 0.2407 0.3189 0.092 Uiso 1 1 calc R . .
C20 C 0.6597(5) 0.1953(4) 0.3703(4) 0.073(2) Uani 1 1 d . . .
H20A H 0.5990 0.1918 0.3751 0.088 Uiso 1 1 calc R . .
H20B H 0.7120 0.1659 0.4017 0.088 Uiso 1 1 calc R . .
C21 C -0.1736(3) 0.5319(2) 0.1681(2) 0.0254(10) Uani 1 1 d . . .
C22 C -0.1584(3) 0.6042(2) 0.1744(2) 0.0272(10) Uani 1 1 d . . .
C23 C -0.2201(4) 0.6474(2) 0.1135(3) 0.0322(11) Uani 1 1 d . . .
H23 H -0.2091 0.6964 0.1163 0.039 Uiso 1 1 calc R . .
C24 C -0.2973(4) 0.6195(3) 0.0492(3) 0.0329(11) Uani 1 1 d . . .
C25 C -0.3130(4) 0.5477(3) 0.0443(3) 0.0337(11) Uani 1 1 d . . .
H25 H -0.3660 0.5282 0.0005 0.040 Uiso 1 1 calc R . .
C26 C -0.2500(3) 0.5042(2) 0.1044(3) 0.0290(10) Uani 1 1 d . . .
H26 H -0.2603 0.4550 0.1012 0.035 Uiso 1 1 calc R . .
C27 C -0.0495(4) 0.6978(3) 0.2380(3) 0.0437(13) Uani 1 1 d . . .
H27A H -0.0430 0.7060 0.1868 0.066 Uiso 1 1 calc R . .
H27B H 0.0134 0.7049 0.2826 0.066 Uiso 1 1 calc R . .
H27C H -0.0969 0.7307 0.2432 0.066 Uiso 1 1 calc R . .
C28 C -0.3687(4) 0.6678(3) -0.0136(3) 0.0454(14) Uani 1 1 d . . .
H28A H -0.3381 0.7140 -0.0119 0.054 Uiso 1 1 calc R . .
H28B H -0.3855 0.6477 -0.0681 0.054 Uiso 1 1 calc R . .
C29 C -0.4589(4) 0.6766(3) 0.0021(4) 0.0532(16) Uani 1 1 d . . .
H29 H -0.4537 0.7053 0.0466 0.064 Uiso 1 1 calc R . .
C30 C -0.5434(5) 0.6493(4) -0.0386(4) 0.0652(18) Uani 1 1 d . . .
H30A H -0.5525 0.6202 -0.0837 0.078 Uiso 1 1 calc R . .
H30B H -0.5961 0.6583 -0.0233 0.078 Uiso 1 1 calc R . .
C31 C -0.1199(3) 0.3401(2) 0.1318(2) 0.0263(10) Uani 1 1 d . . .
C32 C -0.1085(3) 0.2912(2) 0.0779(3) 0.0289(10) Uani 1 1 d . . .
C33 C -0.1680(4) 0.2335(2) 0.0570(3) 0.0344(11) Uani 1 1 d . . .
H33 H -0.1623 0.2011 0.0192 0.041 Uiso 1 1 calc R . .
C34 C -0.2361(4) 0.2213(3) 0.0899(3) 0.0352(11) Uani 1 1 d . . .
C35 C -0.2416(4) 0.2683(3) 0.1464(3) 0.0353(11) Uani 1 1 d . . .
H35 H -0.2854 0.2594 0.1716 0.042 Uiso 1 1 calc R . .
C36 C -0.1846(3) 0.3278(2) 0.1670(3) 0.0309(11) Uani 1 1 d . . .
H36 H -0.1901 0.3599 0.2051 0.037 Uiso 1 1 calc R . .
C37 C -0.0198(5) 0.2573(3) -0.0014(3) 0.0523(16) Uani 1 1 d . . .
H37A H -0.0037 0.2119 0.0259 0.078 Uiso 1 1 calc R . .
H37B H 0.0345 0.2734 -0.0143 0.078 Uiso 1 1 calc R . .
H37C H -0.0779 0.2526 -0.0512 0.078 Uiso 1 1 calc R . .
C38 C -0.3081(5) 0.1627(3) 0.0593(4) 0.0594(17) Uani 1 1 d . . .
H38A H -0.3639 0.1798 0.0117 0.071 Uiso 1 1 calc R . .
H38B H -0.2774 0.1243 0.0409 0.071 Uiso 1 1 calc R . .
C39 C -0.3444(6) 0.1342(4) 0.1153(5) 0.073(2) Uani 1 1 d . . .
H39 H -0.3020 0.1017 0.1522 0.088 Uiso 1 1 calc R . .
C40 C -0.4255(5) 0.1451(4) 0.1247(5) 0.078(2) Uani 1 1 d . . .
H40A H -0.4722 0.1769 0.0904 0.094 Uiso 1 1 calc R . .
H40B H -0.4377 0.1211 0.1659 0.094 Uiso 1 1 calc R . .
C41 C 0.2249(3) 0.4252(2) 0.2361(2) 0.0275(10) Uani 1 1 d . . .
C42 C 0.2907(4) 0.4760(3) 0.2286(3) 0.0357(12) Uani 1 1 d . . .
H42 H 0.3362 0.5028 0.2710 0.043 Uiso 1 1 calc R . .
C43 C 0.2757(4) 0.4792(3) 0.1462(3) 0.0395(13) Uani 1 1 d . . .
H43 H 0.3096 0.5086 0.1237 0.047 Uiso 1 1 calc R . .
C44 C 0.2018(4) 0.4310(3) 0.1031(3) 0.0370(12) Uani 1 1 d . . .
H44 H 0.1775 0.4230 0.0467 0.044 Uiso 1 1 calc R . .
C45 C 0.1700(3) 0.3967(2) 0.1581(3) 0.0291(10) Uani 1 1 d . . .
H45 H 0.1216 0.3614 0.1454 0.035 Uiso 1 1 calc R . .
C46 C 0.0275(3) 0.5152(2) 0.1818(2) 0.0240(10) Uani 1 1 d . . .
C47 C 0.0989(3) 0.5656(2) 0.2276(3) 0.0289(10) Uani 1 1 d . . .
H47 H 0.1254 0.5706 0.2845 0.035 Uiso 1 1 calc R . .
C48 C 0.1228(4) 0.6066(2) 0.1725(3) 0.0350(11) Uani 1 1 d . . .
H48 H 0.1680 0.6441 0.1863 0.042 Uiso 1 1 calc R . .
C49 C 0.0679(4) 0.5822(3) 0.0936(3) 0.0339(11) Uani 1 1 d . . .
H49 H 0.0705 0.6003 0.0455 0.041 Uiso 1 1 calc R . .
C50 C 0.0085(4) 0.5266(2) 0.0983(3) 0.0299(11) Uani 1 1 d . . .
H50 H -0.0361 0.5011 0.0540 0.036 Uiso 1 1 calc 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
Pd1 0.0374(2) 0.02373(17) 0.01261(16) 0.00256(13) 0.01448(14) 0.00385(15)
Fe1 0.0389(4) 0.0343(4) 0.0155(3) 0.0043(3) 0.0151(3) 0.0014(3)
Cl1 0.0436(7) 0.0378(6) 0.0184(5) 0.0111(5) 0.0154(5) 0.0078(5)
Cl2 0.0400(7) 0.0313(6) 0.0224(5) 0.0056(4) 0.0185(5) 0.0037(5)
P1 0.0373(7) 0.0302(6) 0.0127(5) 0.0019(4) 0.0137(5) 0.0050(5)
P2 0.0346(7) 0.0227(6) 0.0133(5) 0.0005(4) 0.0130(5) 0.0025(5)
O1 0.0401(19) 0.0374(18) 0.0130(15) -0.0027(13) 0.0141(14) 0.0021(15)
O2 0.0363(19) 0.0389(18) 0.0130(14) 0.0019(13) 0.0096(14) 0.0081(15)
O3 0.046(2) 0.0343(18) 0.0206(16) 0.0045(13) 0.0210(15) 0.0105(15)
O4 0.086(3) 0.039(2) 0.0294(19) -0.0048(16) 0.034(2) 0.001(2)
O5 0.0382(18) 0.0247(16) 0.0160(14) 0.0038(12) 0.0145(14) 0.0068(14)
O6 0.049(2) 0.0246(17) 0.0182(16) -0.0001(13) 0.0055(15) 0.0039(15)
O7 0.0442(19) 0.0246(16) 0.0132(14) -0.0021(12) 0.0160(14) -0.0007(14)
O8 0.061(2) 0.0287(17) 0.0250(17) -0.0023(14) 0.0284(17) 0.0065(16)
C1 0.045(3) 0.039(3) 0.014(2) -0.0018(19) 0.016(2) 0.007(2)
C2 0.031(3) 0.028(2) 0.017(2) -0.0028(18) 0.0097(19) -0.001(2)
C3 0.045(3) 0.035(3) 0.017(2) -0.0024(19) 0.016(2) 0.006(2)
C4 0.046(3) 0.048(3) 0.016(2) -0.004(2) 0.012(2) 0.012(2)
C5 0.050(3) 0.074(4) 0.016(2) -0.001(2) 0.008(2) 0.023(3)
C6 0.044(3) 0.064(4) 0.019(2) 0.001(2) 0.014(2) 0.022(3)
C7 0.038(3) 0.038(3) 0.018(2) -0.003(2) 0.010(2) 0.007(2)
C8 0.050(3) 0.069(4) 0.019(2) -0.004(2) 0.016(2) 0.019(3)
C9 0.061(4) 0.070(4) 0.019(3) -0.008(3) 0.016(3) 0.009(3)
C10 0.065(4) 0.108(6) 0.031(3) 0.013(3) 0.016(3) 0.029(4)
C11 0.051(3) 0.037(3) 0.023(2) 0.006(2) 0.026(2) 0.017(2)
C12 0.061(4) 0.036(3) 0.023(2) 0.004(2) 0.021(3) 0.014(3)
C13 0.082(5) 0.050(4) 0.039(3) 0.007(3) 0.040(3) 0.025(3)
C14 0.055(4) 0.064(4) 0.045(3) 0.016(3) 0.029(3) 0.027(3)
C15 0.046(3) 0.077(4) 0.036(3) 0.012(3) 0.020(3) 0.017(3)
C16 0.048(3) 0.057(3) 0.025(3) 0.001(2) 0.018(3) 0.009(3)
C17 0.132(7) 0.064(4) 0.052(4) -0.030(3) 0.047(5) -0.015(4)
C18 0.070(5) 0.099(6) 0.068(4) 0.029(4) 0.046(4) 0.047(4)
C19 0.084(5) 0.094(6) 0.067(5) 0.025(4) 0.045(4) 0.032(4)
C20 0.081(5) 0.070(5) 0.065(5) 0.004(4) 0.025(4) 0.024(4)
C21 0.035(3) 0.031(2) 0.015(2) 0.0056(18) 0.014(2) 0.008(2)
C22 0.038(3) 0.031(2) 0.012(2) 0.0012(18) 0.0100(19) 0.005(2)
C23 0.048(3) 0.028(2) 0.023(2) 0.0051(19) 0.017(2) 0.009(2)
C24 0.038(3) 0.044(3) 0.017(2) 0.005(2) 0.011(2) 0.008(2)
C25 0.038(3) 0.043(3) 0.020(2) -0.004(2) 0.011(2) 0.001(2)
C26 0.038(3) 0.033(3) 0.022(2) 0.0013(19) 0.018(2) 0.003(2)
C27 0.054(4) 0.032(3) 0.032(3) -0.005(2) 0.003(3) 0.002(3)
C28 0.053(4) 0.052(3) 0.024(3) 0.013(2) 0.008(3) 0.009(3)
C29 0.051(4) 0.048(3) 0.045(3) 0.004(3) 0.002(3) 0.015(3)
C30 0.059(4) 0.076(5) 0.050(4) 0.001(3) 0.010(3) 0.013(4)
C31 0.040(3) 0.020(2) 0.015(2) 0.0007(17) 0.008(2) 0.005(2)
C32 0.039(3) 0.031(3) 0.017(2) 0.0016(19) 0.011(2) 0.008(2)
C33 0.046(3) 0.027(2) 0.025(2) -0.007(2) 0.009(2) 0.003(2)
C34 0.038(3) 0.031(3) 0.030(3) -0.005(2) 0.005(2) -0.002(2)
C35 0.038(3) 0.035(3) 0.034(3) -0.003(2) 0.014(2) -0.002(2)
C36 0.042(3) 0.028(2) 0.022(2) -0.0031(19) 0.012(2) 0.002(2)
C37 0.096(5) 0.039(3) 0.047(3) -0.005(3) 0.054(4) 0.007(3)
C38 0.060(4) 0.044(3) 0.071(4) -0.022(3) 0.023(4) -0.016(3)
C39 0.081(5) 0.050(4) 0.082(5) -0.004(4) 0.025(5) -0.020(4)
C40 0.053(4) 0.080(5) 0.087(6) 0.004(4) 0.013(4) -0.027(4)
C41 0.038(3) 0.033(2) 0.016(2) 0.0022(18) 0.015(2) 0.008(2)
C42 0.042(3) 0.046(3) 0.025(2) 0.003(2) 0.019(2) -0.002(2)
C43 0.043(3) 0.055(3) 0.030(3) 0.011(2) 0.025(2) 0.007(3)
C44 0.046(3) 0.051(3) 0.020(2) 0.010(2) 0.020(2) 0.012(3)
C45 0.040(3) 0.035(3) 0.017(2) 0.0022(19) 0.017(2) 0.007(2)
C46 0.036(3) 0.027(2) 0.0111(19) 0.0046(17) 0.0117(19) 0.007(2)
C47 0.040(3) 0.026(2) 0.024(2) 0.0002(19) 0.016(2) 0.000(2)
C48 0.051(3) 0.030(3) 0.028(3) 0.005(2) 0.019(2) -0.005(2)
C49 0.050(3) 0.037(3) 0.019(2) 0.011(2) 0.018(2) 0.006(2)
C50 0.044(3) 0.033(3) 0.015(2) 0.0024(19) 0.013(2) 0.003(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
Pd1 P1 2.2433(13) . ?
Pd1 P2 2.2551(11) . ?
Pd1 Cl1 2.3323(11) . ?
Pd1 Cl2 2.3390(12) . ?
Fe1 C41 1.989(4) . ?
Fe1 C46 2.006(4) . ?
Fe1 C45 2.030(5) . ?
Fe1 C42 2.034(5) . ?
Fe1 C50 2.034(5) . ?
Fe1 C47 2.035(4) . ?
Fe1 C44 2.062(5) . ?
Fe1 C49 2.065(5) . ?
Fe1 C48 2.072(5) . ?
Fe1 C43 2.073(5) . ?
P1 O3 1.606(3) . ?
P1 O1 1.612(3) . ?
P1 C41 1.783(4) . ?
P2 O7 1.605(3) . ?
P2 O5 1.606(3) . ?
P2 C46 1.767(4) . ?
O1 C1 1.421(5) . ?
O2 C2 1.361(5) . ?
O2 C7 1.441(5) . ?
O3 C11 1.418(5) . ?
O4 C12 1.356(6) . ?
O4 C17 1.444(6) . ?
O5 C21 1.409(5) . ?
O6 C22 1.360(5) . ?
O6 C27 1.436(6) . ?
O7 C31 1.392(5) . ?
O8 C32 1.367(5) . ?
O8 C37 1.443(5) . ?
C1 C6 1.356(6) . ?
C1 C2 1.402(6) . ?
C2 C3 1.393(6) . ?
C3 C4 1.382(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.388(7) . ?
C4 C8 1.528(6) . ?
C5 C6 1.393(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.486(7) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.308(8) . ?
C9 H9 0.9500 . ?
C10 H10A 0.9500 . ?
C10 H10B 0.9500 . ?
C11 C16 1.374(7) . ?
C11 C12 1.391(6) . ?
C12 C13 1.413(7) . ?
C13 C14 1.385(9) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(8) . ?
C14 C18 1.516(8) . ?
C15 C16 1.388(7) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.493(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.283(9) . ?
C19 H19 0.9500 . ?
C20 H20A 0.9500 . ?
C20 H20B 0.9500 . ?
C21 C26 1.372(6) . ?
C21 C22 1.397(6) . ?
C22 C23 1.394(6) . ?
C23 C24 1.385(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(7) . ?
C24 C28 1.526(6) . ?
C25 C26 1.398(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.497(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.299(8) . ?
C29 H29 0.9500 . ?
C30 H30A 0.9500 . ?
C30 H30B 0.9500 . ?
C31 C36 1.373(6) . ?
C31 C32 1.407(6) . ?
C32 C33 1.375(7) . ?
C33 C34 1.388(7) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(7) . ?
C34 C38 1.503(7) . ?
C35 C36 1.383(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.430(9) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C40 1.311(10) . ?
C39 H39 0.9500 . ?
C40 H40A 0.9500 . ?
C40 H40B 0.9500 . ?
C41 C42 1.429(7) . ?
C41 C45 1.431(6) . ?
C42 C43 1.415(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.415(7) . ?
C43 H43 0.9500 . ?
C44 C45 1.420(6) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C46 C47 1.436(6) . ?
C46 C50 1.437(5) . ?
C47 C48 1.418(6) . ?
C47 H47 0.9500 . ?
C48 C49 1.416(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.410(7) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
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
P1 Pd1 P2 96.93(4) . . ?
P1 Pd1 Cl1 83.89(4) . . ?
P2 Pd1 Cl1 179.17(4) . . ?
P1 Pd1 Cl2 172.38(4) . . ?
P2 Pd1 Cl2 89.69(4) . . ?
Cl1 Pd1 Cl2 89.48(4) . . ?
C41 Fe1 C46 107.66(17) . . ?
C41 Fe1 C45 41.71(17) . . ?
C46 Fe1 C45 107.54(18) . . ?
C41 Fe1 C42 41.59(19) . . ?
C46 Fe1 C42 138.04(17) . . ?
C45 Fe1 C42 69.6(2) . . ?
C41 Fe1 C50 138.25(19) . . ?
C46 Fe1 C50 41.65(16) . . ?
C45 Fe1 C50 110.42(19) . . ?
C42 Fe1 C50 179.69(18) . . ?
C41 Fe1 C47 107.76(17) . . ?
C46 Fe1 C47 41.62(17) . . ?
C45 Fe1 C47 135.83(17) . . ?
C42 Fe1 C47 110.40(19) . . ?
C50 Fe1 C47 69.34(18) . . ?
C41 Fe1 C44 68.83(17) . . ?
C46 Fe1 C44 137.2(2) . . ?
C45 Fe1 C44 40.59(17) . . ?
C42 Fe1 C44 68.2(2) . . ?
C50 Fe1 C44 112.06(19) . . ?
C47 Fe1 C44 176.29(18) . . ?
C41 Fe1 C49 175.89(18) . . ?
C46 Fe1 C49 68.84(17) . . ?
C45 Fe1 C49 140.72(19) . . ?
C42 Fe1 C49 139.9(2) . . ?
C50 Fe1 C49 40.23(18) . . ?
C47 Fe1 C49 68.22(18) . . ?
C44 Fe1 C49 115.16(18) . . ?
C41 Fe1 C48 137.22(19) . . ?
C46 Fe1 C48 68.76(18) . . ?
C45 Fe1 C48 176.04(19) . . ?
C42 Fe1 C48 112.0(2) . . ?
C50 Fe1 C48 67.9(2) . . ?
C47 Fe1 C48 40.38(17) . . ?
C44 Fe1 C48 143.23(19) . . ?
C49 Fe1 C48 40.02(18) . . ?
C41 Fe1 C43 68.66(19) . . ?
C46 Fe1 C43 175.74(19) . . ?
C45 Fe1 C43 68.3(2) . . ?
C42 Fe1 C43 40.30(18) . . ?
C50 Fe1 C43 140.01(18) . . ?
C47 Fe1 C43 140.8(2) . . ?
C44 Fe1 C43 40.0(2) . . ?
C49 Fe1 C43 114.92(19) . . ?
C48 Fe1 C43 115.3(2) . . ?
O3 P1 O1 107.17(17) . . ?
O3 P1 C41 102.13(18) . . ?
O1 P1 C41 98.39(19) . . ?
O3 P1 Pd1 111.51(13) . . ?
O1 P1 Pd1 111.21(12) . . ?
C41 P1 Pd1 124.65(16) . . ?
O7 P2 O5 106.63(17) . . ?
O7 P2 C46 97.34(17) . . ?
O5 P2 C46 103.17(18) . . ?
O7 P2 Pd1 113.71(12) . . ?
O5 P2 Pd1 111.34(11) . . ?
C46 P2 Pd1 122.78(15) . . ?
C1 O1 P1 123.7(3) . . ?
C2 O2 C7 117.4(3) . . ?
C11 O3 P1 119.9(3) . . ?
C12 O4 C17 118.1(5) . . ?
C21 O5 P2 119.6(2) . . ?
C22 O6 C27 117.4(3) . . ?
C31 O7 P2 127.6(3) . . ?
C32 O8 C37 116.9(4) . . ?
C6 C1 C2 121.1(4) . . ?
C6 C1 O1 119.3(4) . . ?
C2 C1 O1 119.4(4) . . ?
O2 C2 C3 125.3(4) . . ?
O2 C2 C1 116.5(4) . . ?
C3 C2 C1 118.1(4) . . ?
C4 C3 C2 120.9(4) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 C8 119.4(4) . . ?
C5 C4 C8 120.9(4) . . ?
C4 C5 C6 119.6(5) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 120.4(5) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C4 114.3(4) . . ?
C9 C8 H8A 108.7 . . ?
C4 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
C4 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C10 C9 C8 126.0(7) . . ?
C10 C9 H9 117.0 . . ?
C8 C9 H9 117.0 . . ?
C9 C10 H10A 120.0 . . ?
C9 C10 H10B 120.0 . . ?
H10A C10 H10B 120.0 . . ?
C16 C11 C12 121.3(5) . . ?
C16 C11 O3 121.1(4) . . ?
C12 C11 O3 117.7(5) . . ?
O4 C12 C11 116.3(5) . . ?
O4 C12 C13 125.8(5) . . ?
C11 C12 C13 117.9(5) . . ?
C14 C13 C12 120.8(5) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C15 C14 C13 119.7(5) . . ?
C15 C14 C18 119.3(6) . . ?
C13 C14 C18 121.0(6) . . ?
C14 C15 C16 120.1(6) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C11 C16 C15 120.2(5) . . ?
C11 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
O4 C17 H17A 109.5 . . ?
O4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C14 114.7(6) . . ?
C19 C18 H18A 108.6 . . ?
C14 C18 H18A 108.6 . . ?
C19 C18 H18B 108.6 . . ?
C14 C18 H18B 108.6 . . ?
H18A C18 H18B 107.6 . . ?
C20 C19 C18 127.5(7) . . ?
C20 C19 H19 116.3 . . ?
C18 C19 H19 116.3 . . ?
C19 C20 H20A 120.0 . . ?
C19 C20 H20B 120.0 . . ?
H20A C20 H20B 120.0 . . ?
C26 C21 C22 120.4(4) . . ?
C26 C21 O5 119.9(4) . . ?
C22 C21 O5 119.5(4) . . ?
O6 C22 C23 124.5(4) . . ?
O6 C22 C21 116.6(4) . . ?
C23 C22 C21 118.9(4) . . ?
C24 C23 C22 120.8(4) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 119.9(4) . . ?
C23 C24 C28 120.1(5) . . ?
C25 C24 C28 119.9(4) . . ?
C24 C25 C26 119.5(4) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C21 C26 C25 120.5(4) . . ?
C21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
O6 C27 H27A 109.5 . . ?
O6 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O6 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 C24 110.4(4) . . ?
C29 C28 H28A 109.6 . . ?
C24 C28 H28A 109.6 . . ?
C29 C28 H28B 109.6 . . ?
C24 C28 H28B 109.6 . . ?
H28A C28 H28B 108.1 . . ?
C30 C29 C28 126.9(6) . . ?
C30 C29 H29 116.6 . . ?
C28 C29 H29 116.6 . . ?
C29 C30 H30A 120.0 . . ?
C29 C30 H30B 120.0 . . ?
H30A C30 H30B 120.0 . . ?
C36 C31 O7 123.6(4) . . ?
C36 C31 C32 120.5(4) . . ?
O7 C31 C32 115.8(4) . . ?
O8 C32 C33 126.6(4) . . ?
O8 C32 C31 114.8(4) . . ?
C33 C32 C31 118.6(4) . . ?
C32 C33 C34 121.7(4) . . ?
C32 C33 H33 119.2 . . ?
C34 C33 H33 119.2 . . ?
C35 C34 C33 118.3(4) . . ?
C35 C34 C38 120.7(5) . . ?
C33 C34 C38 120.7(5) . . ?
C36 C35 C34 121.4(5) . . ?
C36 C35 H35 119.3 . . ?
C34 C35 H35 119.3 . . ?
C31 C36 C35 119.4(4) . . ?
C31 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
O8 C37 H37A 109.5 . . ?
O8 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O8 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C34 116.2(5) . . ?
C39 C38 H38A 108.2 . . ?
C34 C38 H38A 108.2 . . ?
C39 C38 H38B 108.2 . . ?
C34 C38 H38B 108.2 . . ?
H38A C38 H38B 107.4 . . ?
C40 C39 C38 131.5(8) . . ?
C40 C39 H39 114.2 . . ?
C38 C39 H39 114.2 . . ?
C39 C40 H40A 120.0 . . ?
C39 C40 H40B 120.0 . . ?
H40A C40 H40B 120.0 . . ?
C42 C41 C45 108.4(4) . . ?
C42 C41 P1 127.5(3) . . ?
C45 C41 P1 124.1(4) . . ?
C42 C41 Fe1 70.9(3) . . ?
C45 C41 Fe1 70.7(3) . . ?
P1 C41 Fe1 123.1(2) . . ?
C43 C42 C41 107.4(4) . . ?
C43 C42 Fe1 71.3(3) . . ?
C41 C42 Fe1 67.5(3) . . ?
C43 C42 H42 126.3 . . ?
C41 C42 H42 126.3 . . ?
Fe1 C42 H42 126.4 . . ?
C44 C43 C42 108.5(4) . . ?
C44 C43 Fe1 69.6(3) . . ?
C42 C43 Fe1 68.4(3) . . ?
C44 C43 H43 125.8 . . ?
C42 C43 H43 125.8 . . ?
Fe1 C43 H43 127.9 . . ?
C43 C44 C45 108.8(4) . . ?
C43 C44 Fe1 70.4(3) . . ?
C45 C44 Fe1 68.5(3) . . ?
C43 C44 H44 125.6 . . ?
C45 C44 H44 125.6 . . ?
Fe1 C44 H44 127.1 . . ?
C44 C45 C41 106.9(4) . . ?
C44 C45 Fe1 70.9(3) . . ?
C41 C45 Fe1 67.6(3) . . ?
C44 C45 H45 126.5 . . ?
C41 C45 H45 126.5 . . ?
Fe1 C45 H45 126.4 . . ?
C47 C46 C50 107.4(4) . . ?
C47 C46 P2 125.9(3) . . ?
C50 C46 P2 126.7(4) . . ?
C47 C46 Fe1 70.3(3) . . ?
C50 C46 Fe1 70.2(3) . . ?
P2 C46 Fe1 122.9(2) . . ?
C48 C47 C46 107.6(4) . . ?
C48 C47 Fe1 71.2(3) . . ?
C46 C47 Fe1 68.1(2) . . ?
C48 C47 H47 126.2 . . ?
C46 C47 H47 126.2 . . ?
Fe1 C47 H47 126.1 . . ?
C49 C48 C47 108.5(4) . . ?
C49 C48 Fe1 69.7(3) . . ?
C47 C48 Fe1 68.4(3) . . ?
C49 C48 H48 125.8 . . ?
C47 C48 H48 125.8 . . ?
Fe1 C48 H48 127.7 . . ?
C50 C49 C48 108.6(4) . . ?
C50 C49 Fe1 68.7(3) . . ?
C48 C49 Fe1 70.3(3) . . ?
C50 C49 H49 125.7 . . ?
C48 C49 H49 125.7 . . ?
Fe1 C49 H49 126.9 . . ?
C49 C50 C46 107.9(4) . . ?
C49 C50 Fe1 71.0(3) . . ?
C46 C50 Fe1 68.1(3) . . ?
C49 C50 H50 126.0 . . ?
C46 C50 H50 126.0 . . ?
Fe1 C50 H50 126.4 . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 26.41
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 1.359
_refine_diff_density_min -1.054
_refine_diff_density_rms 0.106
_database_code_depnum_ccdc_archive 'CCDC 933871'