#------------------------------------------------------------------------------
#$Date: 2024-08-05 20:57:08 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293740 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571971.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1571971
loop_
_publ_author_name
'Cobb, Caitlyn R.'
'Ngo, Ren K.'
'Dick, Emily J.'
'Lynch, Vincent M.'
'Rose, Michael J.'
_publ_section_title
;
Multi-phosphine-chelated iron-carbide clusters via redox-promoted
ligand exchange on an inert hexa-iron-carbide carbonyl cluster,
[Fe6(μ6-C)(μ2-CO)4(CO)12]2.
;
_journal_issue 29
_journal_name_full 'Chemical science'
_journal_page_first 11455
_journal_page_last 11471
_journal_paper_doi 10.1039/d4sc01370k
_journal_volume 15
_journal_year 2024
_chemical_formula_moiety 'C49 H39 Fe3 O7 P3, 0.5(C7 H8)'
_chemical_formula_sum 'C52.5 H43 Fe3 O7 P3'
_chemical_formula_weight 1046.33
_chemical_name_systematic 10
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_Hall '-P 2yn'
_space_group_name_H-M_alt 'P 1 21/n 1'
_atom_sites_solution_hydrogens geom
_audit_creation_date 2023-06-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2023-06-06 deposited with the CCDC. 2024-06-03 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 98.7080(10)
_cell_angle_gamma 90
_cell_formula_units_Z 4
_cell_length_a 12.22120(10)
_cell_length_b 19.70640(10)
_cell_length_c 19.6407(2)
_cell_measurement_reflns_used 51180
_cell_measurement_temperature 100.0(4)
_cell_measurement_theta_max 75.9810
_cell_measurement_theta_min 2.2360
_cell_volume 4675.66(7)
_computing_cell_refinement 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):
# Type Start End Width t~exp~ \w \q \k \f Frames
#--------------------------------------------------------------------------
1 \w -44.00 24.00 0.50 5.00 -- -48.29 37.00 -23.00 136
2 \w -121.00 -37.00 0.50 5.00 -- -48.29 -37.00-178.00 168
3 \w -24.00 38.00 0.50 5.00 -- 48.29 -37.00-178.00 124
4 \w 38.00 121.00 0.50 5.00 -- 48.29 37.00 -23.00 166
5 \w -177.00 -94.00 0.50 12.00 -- -104.52 -37.00-178.00 166
6 \w 94.00 177.00 0.50 12.00 -- 104.52 37.00 -23.00 166
7 \w -119.00 -87.00 0.50 5.00 -- -48.29-125.00 -60.00 64
8 \w -26.00 26.00 0.50 5.00 -- -48.29 19.00 120.00 104
9 \w -70.00 24.00 0.50 5.00 -- -48.29 77.00 -30.00 188
10 \w 82.00 120.00 0.50 5.00 -- 48.29 57.00 -90.00 76
11 \w -7.00 81.00 0.50 5.00 -- 48.29 -99.00-180.00 176
12 \w -111.00 -32.00 0.50 12.00 -- -104.52 125.00-150.00 158
13 \w -177.00 -94.00 0.50 12.00 -- -104.52 -15.00 -60.00 166
14 \w -111.00 -32.00 0.50 12.00 -- -104.52 125.00 0.00 158
15 \w -107.00 -32.00 0.50 12.00 -- -104.52 103.00 58.92 150
16 \w -177.00-100.00 0.50 12.00 -- -104.52 -77.00 90.00 154
17 \w -75.00 -32.00 0.50 12.00 -- -104.52 61.00 30.00 86
18 \w -177.00-100.00 0.50 12.00 -- -104.52 -77.00 60.00 154
19 \w -108.00 -32.00 0.50 12.00 -- -104.52 114.00 -33.07 152
20 \w -177.00 -94.00 0.50 12.00 -- -104.52 -45.00 150.00 166
21 \w 32.00 105.00 0.50 12.00 -- 104.52 -95.00 -30.00 146
22 \w 32.00 69.00 0.50 12.00 -- 104.52 -61.00 120.00 74
23 \w 32.00 105.00 0.50 12.00 -- 104.52 -95.00 150.00 146
24 \w 32.00 69.00 0.50 12.00 -- 104.52 -61.00 -30.00 74
25 \w 100.00 177.00 0.50 12.00 -- 104.52 77.00-120.00 154
26 \w 32.00 105.00 0.50 12.00 -- 104.52 -95.00-180.00 146
27 \w 32.00 111.00 0.50 12.00 -- 104.52-125.00 -30.00 158
28 \w 32.00 69.00 0.50 12.00 -- 104.52 -61.00 -60.00 74
29 \w 32.00 69.00 0.50 12.00 -- 104.52 -61.00-180.00 74
30 \w 32.00 111.00 0.50 12.00 -- 104.52-125.00 120.00 158
31 \w 100.00 177.00 0.50 12.00 -- 104.52 77.00-150.00 154
32 \w 32.00 69.00 0.50 12.00 -- 104.52 -61.00 0.00 74
33 \w 32.00 105.00 0.50 12.00 -- 104.52 -95.00 -60.00 146
34 \w 32.00 69.00 0.50 12.00 -- 104.52 -61.00-150.00 74
35 \w 35.00 120.00 0.50 5.00 -- 48.29 56.00 160.40 170
36 \w 35.00 120.00 0.50 5.00 -- 48.29 56.00-106.55 170
37 \w 35.00 120.00 0.50 5.00 -- 48.29 55.00 6.94 170
38 \w 35.00 120.00 0.50 5.00 -- 48.29 54.00 68.22 170
;
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0376
_diffrn_reflns_av_unetI/netI 0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_k_min -24
_diffrn_reflns_limit_l_max 24
_diffrn_reflns_limit_l_min -24
_diffrn_reflns_number 88271
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 76.464
_diffrn_reflns_theta_min 3.195
_exptl_absorpt_coefficient_mu 8.770
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.545
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour 'clear yellowish brown'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_modifier yellowish
_exptl_crystal_colour_primary brown
_exptl_crystal_density_diffrn 1.486
_exptl_crystal_description prism
_exptl_crystal_F_000 2148
_exptl_crystal_preparation
'From a solution of 8 in toluene for two months at -20 degrees C.'
_exptl_crystal_recrystallization_method
'From a crude solution in toluene at -20 degrees C.'
_exptl_crystal_size_max 0.223
_exptl_crystal_size_mid 0.103
_exptl_crystal_size_min 0.049
_refine_diff_density_max 0.348
_refine_diff_density_min -0.374
_refine_diff_density_rms 0.054
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.075
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 623
_refine_ls_number_reflns 9727
_refine_ls_number_restraints 21
_refine_ls_restrained_S_all 1.075
_refine_ls_R_factor_all 0.0303
_refine_ls_R_factor_gt 0.0286
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+3.4570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0729
_refine_ls_wR_factor_ref 0.0738
_reflns_Friedel_coverage 0.000
_reflns_number_gt 9255
_reflns_number_total 9727
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d4sc01370k3.cif
_cod_data_source_block compound10
_cod_depositor_comments
'Adding full bibliography for 1571968--1571976.cif.'
_cod_original_formula_sum 'C52.50 H43 Fe3 O7 P3'
_cod_database_code 1571971
_shelx_shelxl_version_number 2018/3
_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.
;
_shelx_estimated_absorpt_t_max 0.673
_shelx_estimated_absorpt_t_min 0.245
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C55-C50
1.39 with sigma of 0.02
C51-C55
2.4 with sigma of 0.03
C55-C54
1.39 with sigma of 0.02
C54-C52
2.4 with sigma of 0.03
C54-C53
1.39 with sigma of 0.02
C55-C52
2.8 with sigma of 0.03
C53-C52
1.39 with sigma of 0.02
C55-C53
2.4 with sigma of 0.03
C52-C51
1.39 with sigma of 0.02
C53-C51
2.4 with sigma of 0.03
C51-C50
1.39 with sigma of 0.02
C50-C53
2.8 with sigma of 0.03
C56-C50
1.52 with sigma of 0.02
C51-C54
2.8 with sigma of 0.03
C50-C54
2.4 with sigma of 0.03
C50-C52
2.4 with sigma of 0.03
C51-C56 \\sim C55-C56
with sigma of 0.02
3. Restrained planarity
C53, C54, C55, C50, C51, C52, C56
with sigma of 0.02
4. Others
Fixed Sof: C50(0.5) C51(0.5) H51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5)
C54(0.5) H54(0.5) C55(0.5) H55(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5)
5.a Secondary CH2 refined with riding coordinates:
C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
5.b Me refined with riding coordinates:
C56(H56A,H56B,H56C)
5.c Aromatic/amide H refined with riding coordinates:
C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C21(H21), C22(H22), C23(H23),
C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33),
C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C51(H51),
C52(H52), C53(H53), C54(H54), C55(H55)
5.d Idealised Me refined as rotating group:
C15(H15A,H15B,H15C)
;
_shelx_res_file
;
TITL fe3cphtriphos(phosphide)
compound10.res
created by SHELXL-2018/3 at 09:04:43 on 03-Jun-2023
REM Old TITL fe3Cphtriphos(phosphide)_yellowprism_5312022_auto in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.077, Rweak 0.008, Alpha 0.045
REM 1.432 for 301 systematic absences, Orientation as input
REM Formula found by SHELXT: C52 O7
CELL 1.54184 12.2212 19.7064 19.6407 90 98.708 90
ZERR 4 0.0001 0.0001 0.0002 0 0.001 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H Fe O P
UNIT 210 172 12 28 12
DFIX 1.39 C55 C50
SADI C51 C56 C55 C56
DFIX 2.4 0.03 C51 C55
DFIX 1.39 C55 C54
DFIX 2.4 0.03 C54 C52
DFIX 1.39 C54 C53
DFIX 2.8 0.03 C55 C52
DFIX 1.39 C53 C52
DFIX 2.4 0.03 C55 C53
DFIX 1.39 C52 C51
DFIX 2.4 0.03 C53 C51
DFIX 1.39 C51 C50
DFIX 2.8 0.03 C50 C53
DFIX 1.52 C56 C50
DFIX 2.8 0.03 C51 C54
DFIX 2.4 0.03 C50 C54
FLAT 0.02 C53 C54 C55 C50 C51 C52 C56
DFIX 2.4 0.03 C50 C52
L.S. 20
PLAN 4
SIZE 0.049 0.103 0.223
TEMP -173
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2 53
acta
REM
REM
REM
WGHT 0.034700 3.457000
FVAR 0.24461
FE1 3 0.787613 0.723682 0.417370 11.00000 0.01861 0.01546 =
0.01563 0.00054 0.00087 -0.00038
FE2 3 0.741670 0.621697 0.491336 11.00000 0.01852 0.01480 =
0.01366 0.00003 0.00021 0.00028
FE3 3 0.859984 0.603944 0.392981 11.00000 0.01968 0.01788 =
0.01718 -0.00015 0.00144 0.00096
P1 5 0.860133 0.808658 0.487893 11.00000 0.02132 0.01570 =
0.01805 0.00083 -0.00008 -0.00119
P2 5 0.742895 0.648402 0.601960 11.00000 0.01998 0.01721 =
0.01417 -0.00047 0.00018 -0.00039
P3 5 0.640256 0.714220 0.468707 11.00000 0.01866 0.01614 =
0.01637 0.00020 0.00034 0.00046
O1 4 0.708483 0.808965 0.298843 11.00000 0.03719 0.02496 =
0.02319 0.00682 -0.00303 -0.00144
O2 4 1.006555 0.736101 0.375318 11.00000 0.02554 0.02528 =
0.03558 0.00243 0.00961 -0.00116
O3 4 0.849896 0.621130 0.244415 11.00000 0.04217 0.04363 =
0.01895 0.00257 0.00262 0.00990
O4 4 1.103607 0.586080 0.433483 11.00000 0.01907 0.03256 =
0.03382 0.00245 0.00214 0.00137
O5 4 0.810848 0.459485 0.374200 11.00000 0.02843 0.01988 =
0.04447 -0.00496 0.00453 -0.00145
O6 4 0.958558 0.565624 0.549144 11.00000 0.02503 0.03079 =
0.01970 0.00249 -0.00015 0.00819
O7 4 0.629743 0.492904 0.509279 11.00000 0.03600 0.02089 =
0.02480 -0.00039 0.00353 -0.00834
C1 1 0.711993 0.635597 0.389487 11.00000 0.02144 0.01678 =
0.01617 0.00051 0.00174 0.00032
C2 1 0.616294 0.615265 0.338204 11.00000 0.01787 0.02050 =
0.01626 -0.00178 0.00073 0.00212
C3 1 0.567190 0.551189 0.341861 11.00000 0.02372 0.01930 =
0.01755 -0.00083 0.00177 0.00073
AFIX 43
H3 2 0.597815 0.520462 0.376906 11.00000 -1.20000
AFIX 0
C4 1 0.475474 0.531522 0.295883 11.00000 0.02434 0.02152 =
0.02294 -0.00266 0.00223 -0.00171
AFIX 43
H4 2 0.444304 0.487781 0.299719 11.00000 -1.20000
AFIX 0
C5 1 0.428752 0.575375 0.244168 11.00000 0.02362 0.02477 =
0.02217 -0.00501 -0.00287 0.00155
AFIX 43
H5 2 0.364088 0.562726 0.213650 11.00000 -1.20000
AFIX 0
C6 1 0.478024 0.637790 0.237878 11.00000 0.02807 0.02559 =
0.02037 0.00064 -0.00310 0.00456
AFIX 43
H6 2 0.447969 0.667666 0.201891 11.00000 -1.20000
AFIX 0
C7 1 0.570861 0.657400 0.283456 11.00000 0.02594 0.02112 =
0.01834 0.00044 0.00014 -0.00034
AFIX 43
H7 2 0.604230 0.700097 0.277484 11.00000 -1.20000
AFIX 0
C8 1 0.737193 0.774850 0.345926 11.00000 0.02353 0.01892 =
0.02293 -0.00143 0.00343 -0.00240
C9 1 0.923057 0.721005 0.392795 11.00000 0.02599 0.01892 =
0.02073 0.00038 0.00014 -0.00052
C10 1 0.856102 0.614180 0.302891 11.00000 0.02366 0.02381 =
0.02805 -0.00185 0.00295 0.00467
C11 1 1.011245 0.593408 0.418632 11.00000 0.03006 0.01799 =
0.02192 0.00036 0.00741 -0.00003
C12 1 0.831237 0.515720 0.382794 11.00000 0.01954 0.03163 =
0.02141 0.00037 0.00262 0.00450
C13 1 0.879134 0.588592 0.517634 11.00000 0.02725 0.01835 =
0.01656 -0.00071 0.00489 -0.00134
C14 1 0.669432 0.544538 0.500393 11.00000 0.02513 0.02288 =
0.01400 -0.00110 0.00049 0.00224
C15 1 0.668156 0.833847 0.648254 11.00000 0.02862 0.02288 =
0.02531 -0.00620 0.00335 0.00060
AFIX 137
H15A 2 0.618278 0.804283 0.669414 11.00000 -1.50000
H15B 2 0.627244 0.873678 0.628297 11.00000 -1.50000
H15C 2 0.729233 0.848514 0.683365 11.00000 -1.50000
AFIX 0
C16 1 0.714798 0.794702 0.591249 11.00000 0.02411 0.01907 =
0.01985 -0.00376 0.00137 0.00015
C17 1 0.785271 0.844054 0.555403 11.00000 0.02596 0.01728 =
0.02313 -0.00156 0.00084 0.00019
AFIX 23
H17A 2 0.840542 0.865102 0.591253 11.00000 -1.20000
H17B 2 0.736213 0.880790 0.534301 11.00000 -1.20000
AFIX 0
C18 1 0.788101 0.735161 0.625651 11.00000 0.02285 0.01959 =
0.01848 -0.00117 0.00060 -0.00152
AFIX 23
H18A 2 0.792984 0.739703 0.676220 11.00000 -1.20000
H18B 2 0.863815 0.741066 0.614428 11.00000 -1.20000
AFIX 0
C19 1 0.615240 0.772774 0.538249 11.00000 0.02158 0.01825 =
0.02072 -0.00033 0.00145 0.00138
AFIX 23
H19A 2 0.580381 0.814320 0.516435 11.00000 -1.20000
H19B 2 0.560474 0.751186 0.563699 11.00000 -1.20000
AFIX 0
C20 1 0.873804 0.884328 0.435683 11.00000 0.02933 0.01787 =
0.01936 -0.00009 0.00010 -0.00289
C21 1 0.779465 0.922545 0.411483 11.00000 0.02927 0.02092 =
0.02900 0.00285 -0.00105 -0.00325
AFIX 43
H21 2 0.711584 0.912963 0.427538 11.00000 -1.20000
AFIX 0
C22 1 0.784323 0.974301 0.364239 11.00000 0.03646 0.02121 =
0.03000 0.00362 -0.00358 0.00032
AFIX 43
H22 2 0.719663 0.999759 0.347881 11.00000 -1.20000
AFIX 0
C23 1 0.882532 0.989047 0.340843 11.00000 0.04984 0.02079 =
0.02507 0.00409 0.00660 0.00012
AFIX 43
H23 2 0.885566 1.024504 0.308411 11.00000 -1.20000
AFIX 0
C24 1 0.976301 0.952049 0.364776 11.00000 0.04249 0.02525 =
0.03052 0.00358 0.01349 -0.00189
AFIX 43
H24 2 1.044020 0.962454 0.348891 11.00000 -1.20000
AFIX 0
C25 1 0.972869 0.899620 0.411952 11.00000 0.03204 0.02235 =
0.02564 0.00087 0.00517 0.00031
AFIX 43
H25 2 1.037872 0.874329 0.427931 11.00000 -1.20000
AFIX 0
C26 1 0.999525 0.797135 0.536621 11.00000 0.02343 0.02127 =
0.01940 0.00160 0.00021 -0.00201
C27 1 1.059979 0.851786 0.568478 11.00000 0.02887 0.02217 =
0.02673 -0.00152 -0.00239 -0.00027
AFIX 43
H27 2 1.031043 0.896516 0.562812 11.00000 -1.20000
AFIX 0
C28 1 1.162100 0.840683 0.608310 11.00000 0.03124 0.02802 =
0.03786 -0.00580 -0.00770 -0.00287
AFIX 43
H28 2 1.203084 0.878087 0.629366 11.00000 -1.20000
AFIX 0
C29 1 1.205097 0.775857 0.617797 11.00000 0.02991 0.03457 =
0.04243 -0.00059 -0.01344 0.00200
AFIX 43
H29 2 1.275161 0.768753 0.645174 11.00000 -1.20000
AFIX 0
C30 1 1.145234 0.721391 0.587083 11.00000 0.03286 0.02390 =
0.04730 0.00136 -0.00959 0.00406
AFIX 43
H30 2 1.173584 0.676622 0.593971 11.00000 -1.20000
AFIX 0
C31 1 1.043873 0.732265 0.546267 11.00000 0.02706 0.02149 =
0.03109 0.00046 -0.00306 -0.00123
AFIX 43
H31 2 1.004058 0.694758 0.524526 11.00000 -1.20000
AFIX 0
C32 1 0.832972 0.596749 0.664652 11.00000 0.02317 0.02336 =
0.01426 0.00020 0.00255 0.00210
C33 1 0.799351 0.530796 0.675582 11.00000 0.02582 0.02399 =
0.01988 0.00141 0.00131 -0.00093
AFIX 43
H33 2 0.729972 0.515081 0.652614 11.00000 -1.20000
AFIX 0
C34 1 0.866260 0.487573 0.719809 11.00000 0.03618 0.02412 =
0.02419 0.00428 0.00527 0.00547
AFIX 43
H34 2 0.842260 0.442736 0.727437 11.00000 -1.20000
AFIX 0
C35 1 0.967999 0.510125 0.752689 11.00000 0.03303 0.03175 =
0.01880 0.00266 0.00008 0.01122
AFIX 43
H35 2 1.014048 0.480645 0.782766 11.00000 -1.20000
AFIX 0
C36 1 1.002648 0.575466 0.741812 11.00000 0.02751 0.03573 =
0.02192 -0.00235 -0.00447 0.00409
AFIX 43
H36 2 1.072445 0.590751 0.764556 11.00000 -1.20000
AFIX 0
C37 1 0.936006 0.618936 0.697810 11.00000 0.02703 0.02546 =
0.02196 -0.00095 -0.00112 0.00107
AFIX 43
H37 2 0.960468 0.663691 0.690279 11.00000 -1.20000
AFIX 0
C38 1 0.612318 0.642385 0.637209 11.00000 0.02441 0.01724 =
0.01857 0.00135 0.00262 0.00017
C39 1 0.610005 0.660416 0.705819 11.00000 0.02956 0.02187 =
0.01928 -0.00156 0.00304 -0.00104
AFIX 43
H39 2 0.676774 0.672509 0.734598 11.00000 -1.20000
AFIX 0
C40 1 0.510895 0.660775 0.732182 11.00000 0.03808 0.02467 =
0.02302 -0.00251 0.01024 0.00035
AFIX 43
H40 2 0.509996 0.673375 0.778781 11.00000 -1.20000
AFIX 0
C41 1 0.413064 0.642765 0.690614 11.00000 0.02808 0.02449 =
0.03327 0.00069 0.01278 0.00427
AFIX 43
H41 2 0.345136 0.643268 0.708581 11.00000 -1.20000
AFIX 0
C42 1 0.414910 0.624052 0.622806 11.00000 0.02450 0.02389 =
0.02848 0.00143 0.00276 0.00104
AFIX 43
H42 2 0.348131 0.611505 0.594289 11.00000 -1.20000
AFIX 0
C43 1 0.513749 0.623581 0.596485 11.00000 0.02249 0.02141 =
0.01850 0.00101 0.00353 0.00052
AFIX 43
H43 2 0.514308 0.610258 0.550054 11.00000 -1.20000
AFIX 0
C44 1 0.500744 0.719382 0.419343 11.00000 0.02228 0.02180 =
0.01535 -0.00055 0.00046 0.00131
C45 1 0.425220 0.666105 0.416966 11.00000 0.02304 0.02401 =
0.01808 0.00145 0.00207 -0.00173
AFIX 43
H45 2 0.447001 0.624348 0.439137 11.00000 -1.20000
AFIX 0
C46 1 0.318206 0.673935 0.382259 11.00000 0.02395 0.03639 =
0.02496 0.00241 0.00090 -0.00722
AFIX 43
H46 2 0.267019 0.637501 0.380908 11.00000 -1.20000
AFIX 0
C47 1 0.285589 0.734648 0.349541 11.00000 0.02143 0.04445 =
0.03063 0.00617 -0.00254 0.00291
AFIX 43
H47 2 0.212026 0.739923 0.326353 11.00000 -1.20000
AFIX 0
C48 1 0.360579 0.787598 0.350762 11.00000 0.02719 0.03071 =
0.03070 0.00607 -0.00305 0.00688
AFIX 43
H48 2 0.338784 0.828960 0.327792 11.00000 -1.20000
AFIX 0
C49 1 0.467493 0.780122 0.385565 11.00000 0.02519 0.02186 =
0.02529 0.00251 0.00095 0.00068
AFIX 43
H49 2 0.518549 0.816580 0.386457 11.00000 -1.20000
AFIX 0
PART -1
C50 1 1.088473 0.467097 1.008958 10.50000 0.07456 0.03714 =
0.04511 0.00644 0.02116 -0.02427
C51 1 1.032460 0.477827 0.943843 10.50000 0.06976 0.07495 =
0.02778 -0.00759 0.01358 -0.03090
AFIX 43
H51 2 1.056197 0.455614 0.905710 10.50000 -1.20000
AFIX 0
C52 1 0.941973 0.520570 0.933192 10.50000 0.06687 0.09862 =
0.02980 0.00049 0.00778 -0.02704
AFIX 43
H52 2 0.905260 0.527761 0.887572 10.50000 -1.20000
AFIX 0
C53 1 0.903076 0.553454 0.987646 10.50000 0.07132 0.06100 =
0.04575 0.00926 0.00564 -0.03209
AFIX 43
H53 2 0.840313 0.582466 0.980317 10.50000 -1.20000
AFIX 0
C54 1 0.960080 0.541811 1.052521 10.50000 0.08369 0.06207 =
0.04378 -0.00627 0.01602 -0.02536
AFIX 43
H54 2 0.936073 0.563580 1.090811 10.50000 -1.20000
AFIX 0
C55 1 1.050799 0.499618 1.063715 10.50000 0.08662 0.06214 =
0.03515 0.00060 0.00820 -0.02428
AFIX 43
H55 2 1.087950 0.492685 1.109275 10.50000 -1.20000
AFIX 0
C56 1 1.186994 0.420701 1.021436 10.50000 0.08559 0.07881 =
0.06627 0.01753 0.03798 0.01070
AFIX 33
H56A 2 1.215660 0.419535 1.070800 10.50000 -1.50000
H56B 2 1.164877 0.374874 1.005556 10.50000 -1.50000
H56C 2 1.244721 0.437425 0.996095 10.50000 -1.50000
AFIX 0
HKLF 4
REM fe3cphtriphos(phosphide)
REM wR2 = 0.0738, GooF = S = 1.075, Restrained GooF = 1.075 for all data
REM R1 = 0.0286 for 9255 Fo > 4sig(Fo) and 0.0303 for all 9727 data
REM 623 parameters refined using 21 restraints
END
WGHT 0.0347 3.4669
REM Highest difference peak 0.348, deepest hole -0.374, 1-sigma level 0.054
Q1 1 0.7622 0.6207 0.3817 11.00000 0.05 0.35
Q2 1 0.7546 0.7016 0.6153 11.00000 0.05 0.31
Q3 1 0.9621 0.6020 0.3822 11.00000 0.05 0.30
Q4 1 0.6644 0.7793 0.5615 11.00000 0.05 0.29
;
_shelx_res_checksum 82606
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.78761(2) 0.72368(2) 0.41737(2) 0.01675(7) Uani 1 1 d . . . . .
Fe2 Fe 0.74167(2) 0.62170(2) 0.49134(2) 0.01589(6) Uani 1 1 d . . . . .
Fe3 Fe 0.85998(2) 0.60394(2) 0.39298(2) 0.01839(7) Uani 1 1 d . . . . .
P1 P 0.86013(4) 0.80866(2) 0.48789(2) 0.01867(9) Uani 1 1 d . . . . .
P2 P 0.74289(4) 0.64840(2) 0.60196(2) 0.01737(9) Uani 1 1 d . . . . .
P3 P 0.64026(4) 0.71422(2) 0.46871(2) 0.01730(9) Uani 1 1 d . . . . .
O1 O 0.70848(12) 0.80896(7) 0.29884(7) 0.0292(3) Uani 1 1 d . . . . .
O2 O 1.00655(11) 0.73610(7) 0.37532(7) 0.0283(3) Uani 1 1 d . . . . .
O3 O 0.84990(13) 0.62113(8) 0.24441(7) 0.0351(3) Uani 1 1 d . . . . .
O4 O 1.10361(11) 0.58608(7) 0.43348(7) 0.0287(3) Uani 1 1 d . . . . .
O5 O 0.81085(11) 0.45949(7) 0.37420(8) 0.0310(3) Uani 1 1 d . . . . .
O6 O 0.95856(11) 0.56562(7) 0.54914(6) 0.0255(3) Uani 1 1 d . . . . .
O7 O 0.62974(12) 0.49290(7) 0.50928(7) 0.0273(3) Uani 1 1 d . . . . .
C1 C 0.71199(14) 0.63560(9) 0.38949(9) 0.0182(3) Uani 1 1 d . . . . .
C2 C 0.61629(14) 0.61527(9) 0.33820(9) 0.0184(3) Uani 1 1 d . . . . .
C3 C 0.56719(15) 0.55119(9) 0.34186(9) 0.0203(3) Uani 1 1 d . . . . .
H3 H 0.597815 0.520462 0.376906 0.024 Uiso 1 1 calc R U . . .
C4 C 0.47547(15) 0.53152(9) 0.29588(9) 0.0231(4) Uani 1 1 d . . . . .
H4 H 0.444304 0.487781 0.299719 0.028 Uiso 1 1 calc R U . . .
C5 C 0.42875(15) 0.57537(10) 0.24417(9) 0.0242(4) Uani 1 1 d . . . . .
H5 H 0.364088 0.562726 0.213650 0.029 Uiso 1 1 calc R U . . .
C6 C 0.47802(16) 0.63779(10) 0.23788(10) 0.0254(4) Uani 1 1 d . . . . .
H6 H 0.447969 0.667666 0.201891 0.030 Uiso 1 1 calc R U . . .
C7 C 0.57086(15) 0.65740(9) 0.28346(9) 0.0221(4) Uani 1 1 d . . . . .
H7 H 0.604230 0.700097 0.277484 0.027 Uiso 1 1 calc R U . . .
C8 C 0.73719(15) 0.77485(9) 0.34593(9) 0.0218(4) Uani 1 1 d . . . . .
C9 C 0.92306(15) 0.72100(9) 0.39279(9) 0.0222(4) Uani 1 1 d . . . . .
C10 C 0.85610(16) 0.61418(10) 0.30289(10) 0.0253(4) Uani 1 1 d . . . . .
C11 C 1.01125(16) 0.59341(9) 0.41863(9) 0.0230(4) Uani 1 1 d . . . . .
C12 C 0.83124(15) 0.51572(10) 0.38279(9) 0.0242(4) Uani 1 1 d . . . . .
C13 C 0.87913(15) 0.58859(9) 0.51763(9) 0.0206(3) Uani 1 1 d . . . . .
C14 C 0.66943(15) 0.54454(9) 0.50039(9) 0.0209(3) Uani 1 1 d . . . . .
C15 C 0.66816(16) 0.83385(10) 0.64825(10) 0.0257(4) Uani 1 1 d . . . . .
H15A H 0.618278 0.804283 0.669414 0.039 Uiso 1 1 calc R U . . .
H15B H 0.627244 0.873678 0.628297 0.039 Uiso 1 1 calc R U . . .
H15C H 0.729233 0.848514 0.683365 0.039 Uiso 1 1 calc R U . . .
C16 C 0.71480(15) 0.79470(9) 0.59125(9) 0.0212(3) Uani 1 1 d . . . . .
C17 C 0.78527(15) 0.84405(9) 0.55540(9) 0.0224(4) Uani 1 1 d . . . . .
H17A H 0.840542 0.865102 0.591253 0.027 Uiso 1 1 calc R U . . .
H17B H 0.736213 0.880790 0.534301 0.027 Uiso 1 1 calc R U . . .
C18 C 0.78810(15) 0.73516(9) 0.62565(9) 0.0206(3) Uani 1 1 d . . . . .
H18A H 0.792984 0.739703 0.676220 0.025 Uiso 1 1 calc R U . . .
H18B H 0.863815 0.741066 0.614428 0.025 Uiso 1 1 calc R U . . .
C19 C 0.61524(15) 0.77277(9) 0.53825(9) 0.0204(3) Uani 1 1 d . . . . .
H19A H 0.580381 0.814320 0.516435 0.024 Uiso 1 1 calc R U . . .
H19B H 0.560474 0.751186 0.563699 0.024 Uiso 1 1 calc R U . . .
C20 C 0.87380(16) 0.88433(9) 0.43568(9) 0.0226(4) Uani 1 1 d . . . . .
C21 C 0.77946(17) 0.92254(10) 0.41148(10) 0.0270(4) Uani 1 1 d . . . . .
H21 H 0.711584 0.912963 0.427538 0.032 Uiso 1 1 calc R U . . .
C22 C 0.78432(18) 0.97430(10) 0.36424(11) 0.0301(4) Uani 1 1 d . . . . .
H22 H 0.719663 0.999759 0.347881 0.036 Uiso 1 1 calc R U . . .
C23 C 0.88253(19) 0.98905(10) 0.34084(10) 0.0318(4) Uani 1 1 d . . . . .
H23 H 0.885566 1.024504 0.308411 0.038 Uiso 1 1 calc R U . . .
C24 C 0.97630(19) 0.95205(10) 0.36478(11) 0.0319(4) Uani 1 1 d . . . . .
H24 H 1.044020 0.962454 0.348891 0.038 Uiso 1 1 calc R U . . .
C25 C 0.97287(17) 0.89962(10) 0.41195(10) 0.0266(4) Uani 1 1 d . . . . .
H25 H 1.037872 0.874329 0.427931 0.032 Uiso 1 1 calc R U . . .
C26 C 0.99953(15) 0.79714(9) 0.53662(9) 0.0217(4) Uani 1 1 d . . . . .
C27 C 1.05998(16) 0.85179(10) 0.56848(10) 0.0266(4) Uani 1 1 d . . . . .
H27 H 1.031043 0.896516 0.562812 0.032 Uiso 1 1 calc R U . . .
C28 C 1.16210(18) 0.84068(11) 0.60831(11) 0.0337(5) Uani 1 1 d . . . . .
H28 H 1.203084 0.878087 0.629366 0.040 Uiso 1 1 calc R U . . .
C29 C 1.20510(19) 0.77586(11) 0.61780(12) 0.0376(5) Uani 1 1 d . . . . .
H29 H 1.275161 0.768753 0.645174 0.045 Uiso 1 1 calc R U . . .
C30 C 1.14523(18) 0.72139(11) 0.58708(13) 0.0363(5) Uani 1 1 d . . . . .
H30 H 1.173584 0.676622 0.593971 0.044 Uiso 1 1 calc R U . . .
C31 C 1.04387(16) 0.73227(10) 0.54627(10) 0.0273(4) Uani 1 1 d . . . . .
H31 H 1.004058 0.694758 0.524526 0.033 Uiso 1 1 calc R U . . .
C32 C 0.83297(15) 0.59675(9) 0.66465(9) 0.0203(3) Uani 1 1 d . . . . .
C33 C 0.79935(16) 0.53080(9) 0.67558(9) 0.0235(4) Uani 1 1 d . . . . .
H33 H 0.729972 0.515081 0.652614 0.028 Uiso 1 1 calc R U . . .
C34 C 0.86626(17) 0.48757(10) 0.71981(10) 0.0281(4) Uani 1 1 d . . . . .
H34 H 0.842260 0.442736 0.727437 0.034 Uiso 1 1 calc R U . . .
C35 C 0.96800(17) 0.51012(10) 0.75269(10) 0.0283(4) Uani 1 1 d . . . . .
H35 H 1.014048 0.480645 0.782766 0.034 Uiso 1 1 calc R U . . .
C36 C 1.00265(17) 0.57547(11) 0.74181(10) 0.0292(4) Uani 1 1 d . . . . .
H36 H 1.072445 0.590751 0.764556 0.035 Uiso 1 1 calc R U . . .
C37 C 0.93601(16) 0.61894(10) 0.69781(10) 0.0253(4) Uani 1 1 d . . . . .
H37 H 0.960468 0.663691 0.690279 0.030 Uiso 1 1 calc R U . . .
C38 C 0.61232(15) 0.64238(9) 0.63721(9) 0.0201(3) Uani 1 1 d . . . . .
C39 C 0.61001(16) 0.66042(9) 0.70582(9) 0.0236(4) Uani 1 1 d . . . . .
H39 H 0.676774 0.672509 0.734598 0.028 Uiso 1 1 calc R U . . .
C40 C 0.51090(17) 0.66078(10) 0.73218(10) 0.0280(4) Uani 1 1 d . . . . .
H40 H 0.509996 0.673375 0.778781 0.034 Uiso 1 1 calc R U . . .
C41 C 0.41306(17) 0.64277(10) 0.69061(11) 0.0278(4) Uani 1 1 d . . . . .
H41 H 0.345136 0.643268 0.708581 0.033 Uiso 1 1 calc R U . . .
C42 C 0.41491(16) 0.62405(10) 0.62281(10) 0.0258(4) Uani 1 1 d . . . . .
H42 H 0.348131 0.611505 0.594289 0.031 Uiso 1 1 calc R U . . .
C43 C 0.51375(15) 0.62358(9) 0.59649(9) 0.0208(3) Uani 1 1 d . . . . .
H43 H 0.514308 0.610258 0.550054 0.025 Uiso 1 1 calc R U . . .
C44 C 0.50074(15) 0.71938(9) 0.41934(9) 0.0201(3) Uani 1 1 d . . . . .
C45 C 0.42522(15) 0.66611(9) 0.41697(9) 0.0218(4) Uani 1 1 d . . . . .
H45 H 0.447001 0.624348 0.439137 0.026 Uiso 1 1 calc R U . . .
C46 C 0.31821(16) 0.67393(11) 0.38226(10) 0.0287(4) Uani 1 1 d . . . . .
H46 H 0.267019 0.637501 0.380908 0.034 Uiso 1 1 calc R U . . .
C47 C 0.28559(17) 0.73465(12) 0.34954(11) 0.0328(4) Uani 1 1 d . . . . .
H47 H 0.212026 0.739923 0.326353 0.039 Uiso 1 1 calc R U . . .
C48 C 0.36058(17) 0.78760(11) 0.35076(11) 0.0303(4) Uani 1 1 d . . . . .
H48 H 0.338784 0.828960 0.327792 0.036 Uiso 1 1 calc R U . . .
C49 C 0.46749(16) 0.78012(9) 0.38557(10) 0.0244(4) Uani 1 1 d . . . . .
H49 H 0.518549 0.816580 0.386457 0.029 Uiso 1 1 calc R U . . .
C50 C 1.0885(13) 0.4671(5) 1.0090(8) 0.051(3) Uani 0.5 1 d D . P A -1
C51 C 1.0325(13) 0.4778(6) 0.9438(7) 0.057(3) Uani 0.5 1 d D . P A -1
H51 H 1.056197 0.455614 0.905710 0.068 Uiso 0.5 1 calc R U P A -1
C52 C 0.9420(13) 0.5206(7) 0.9332(8) 0.065(3) Uani 0.5 1 d D . P A -1
H52 H 0.905260 0.527761 0.887572 0.078 Uiso 0.5 1 calc R U P A -1
C53 C 0.9031(13) 0.5535(6) 0.9876(8) 0.060(3) Uani 0.5 1 d D . P A -1
H53 H 0.840313 0.582466 0.980317 0.072 Uiso 0.5 1 calc R U P A -1
C54 C 0.9601(16) 0.5418(6) 1.0525(9) 0.063(3) Uani 0.5 1 d D . P A -1
H54 H 0.936073 0.563580 1.090811 0.075 Uiso 0.5 1 calc R U P A -1
C55 C 1.0508(15) 0.4996(6) 1.0637(9) 0.061(3) Uani 0.5 1 d D . P A -1
H55 H 1.087950 0.492685 1.109275 0.074 Uiso 0.5 1 calc R U P A -1
C56 C 1.1870(7) 0.4207(4) 1.0214(4) 0.074(2) Uani 0.5 1 d D . P A -1
H56A H 1.215660 0.419535 1.070800 0.111 Uiso 0.5 1 calc R U P A -1
H56B H 1.164877 0.374874 1.005556 0.111 Uiso 0.5 1 calc R U P A -1
H56C H 1.244721 0.437425 0.996095 0.111 Uiso 0.5 1 calc R U P A -1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.01861(13) 0.01546(13) 0.01563(13) 0.00054(10) 0.00087(10) -0.00038(10)
Fe2 0.01852(13) 0.01480(13) 0.01366(13) 0.00003(9) 0.00021(10) 0.00028(10)
Fe3 0.01968(14) 0.01788(13) 0.01718(13) -0.00015(10) 0.00144(10) 0.00096(10)
P1 0.0213(2) 0.0157(2) 0.0181(2) 0.00083(16) -0.00008(16) -0.00119(16)
P2 0.0200(2) 0.0172(2) 0.01417(19) -0.00047(15) 0.00018(15) -0.00039(16)
P3 0.0187(2) 0.0161(2) 0.0164(2) 0.00020(15) 0.00034(16) 0.00046(15)
O1 0.0372(8) 0.0250(7) 0.0232(7) 0.0068(5) -0.0030(6) -0.0014(6)
O2 0.0255(7) 0.0253(7) 0.0356(8) 0.0024(6) 0.0096(6) -0.0012(5)
O3 0.0422(8) 0.0436(9) 0.0190(7) 0.0026(6) 0.0026(6) 0.0099(7)
O4 0.0191(7) 0.0326(7) 0.0338(7) 0.0024(6) 0.0021(5) 0.0014(5)
O5 0.0284(7) 0.0199(7) 0.0445(8) -0.0050(6) 0.0045(6) -0.0014(5)
O6 0.0250(7) 0.0308(7) 0.0197(6) 0.0025(5) -0.0001(5) 0.0082(5)
O7 0.0360(7) 0.0209(7) 0.0248(7) -0.0004(5) 0.0035(6) -0.0083(6)
C1 0.0214(8) 0.0168(8) 0.0162(8) 0.0005(6) 0.0017(6) 0.0003(6)
C2 0.0179(8) 0.0205(8) 0.0163(8) -0.0018(6) 0.0007(6) 0.0021(6)
C3 0.0237(9) 0.0193(8) 0.0175(8) -0.0008(6) 0.0018(7) 0.0007(7)
C4 0.0243(9) 0.0215(9) 0.0229(9) -0.0027(7) 0.0022(7) -0.0017(7)
C5 0.0236(9) 0.0248(9) 0.0222(9) -0.0050(7) -0.0029(7) 0.0016(7)
C6 0.0281(9) 0.0256(9) 0.0204(9) 0.0006(7) -0.0031(7) 0.0046(7)
C7 0.0259(9) 0.0211(9) 0.0183(8) 0.0004(7) 0.0001(7) -0.0003(7)
C8 0.0235(9) 0.0189(8) 0.0229(9) -0.0014(7) 0.0034(7) -0.0024(7)
C9 0.0260(9) 0.0189(8) 0.0207(8) 0.0004(7) 0.0001(7) -0.0005(7)
C10 0.0237(9) 0.0238(9) 0.0280(10) -0.0018(7) 0.0029(7) 0.0047(7)
C11 0.0301(10) 0.0180(8) 0.0219(9) 0.0004(7) 0.0074(7) 0.0000(7)
C12 0.0195(8) 0.0316(11) 0.0214(9) 0.0004(7) 0.0026(7) 0.0045(7)
C13 0.0273(9) 0.0184(8) 0.0166(8) -0.0007(6) 0.0049(7) -0.0013(7)
C14 0.0251(9) 0.0229(9) 0.0140(8) -0.0011(6) 0.0005(6) 0.0022(7)
C15 0.0286(10) 0.0229(9) 0.0253(9) -0.0062(7) 0.0033(7) 0.0006(7)
C16 0.0241(9) 0.0191(8) 0.0198(8) -0.0038(7) 0.0014(7) 0.0001(7)
C17 0.0260(9) 0.0173(8) 0.0231(9) -0.0016(7) 0.0008(7) 0.0002(7)
C18 0.0228(9) 0.0196(8) 0.0185(8) -0.0012(7) 0.0006(7) -0.0015(7)
C19 0.0216(8) 0.0183(8) 0.0207(8) -0.0003(7) 0.0014(7) 0.0014(7)
C20 0.0293(9) 0.0179(8) 0.0194(8) -0.0001(7) 0.0001(7) -0.0029(7)
C21 0.0293(10) 0.0209(9) 0.0290(10) 0.0028(7) -0.0011(8) -0.0033(7)
C22 0.0365(11) 0.0212(9) 0.0300(10) 0.0036(8) -0.0036(8) 0.0003(8)
C23 0.0498(13) 0.0208(9) 0.0251(10) 0.0041(7) 0.0066(9) 0.0001(9)
C24 0.0425(12) 0.0252(10) 0.0305(10) 0.0036(8) 0.0135(9) -0.0019(9)
C25 0.0320(10) 0.0223(9) 0.0256(9) 0.0009(7) 0.0052(8) 0.0003(8)
C26 0.0234(9) 0.0213(9) 0.0194(8) 0.0016(7) 0.0002(7) -0.0020(7)
C27 0.0289(10) 0.0222(9) 0.0267(9) -0.0015(7) -0.0024(8) -0.0003(7)
C28 0.0312(10) 0.0280(10) 0.0379(11) -0.0058(9) -0.0077(9) -0.0029(8)
C29 0.0299(11) 0.0346(11) 0.0424(12) -0.0006(9) -0.0134(9) 0.0020(9)
C30 0.0329(11) 0.0239(10) 0.0473(13) 0.0014(9) -0.0096(9) 0.0041(8)
C31 0.0271(10) 0.0215(9) 0.0311(10) 0.0005(8) -0.0031(8) -0.0012(7)
C32 0.0232(9) 0.0234(9) 0.0143(8) 0.0002(7) 0.0025(6) 0.0021(7)
C33 0.0258(9) 0.0240(9) 0.0199(8) 0.0014(7) 0.0013(7) -0.0009(7)
C34 0.0362(11) 0.0241(9) 0.0242(9) 0.0043(7) 0.0053(8) 0.0055(8)
C35 0.0330(10) 0.0318(10) 0.0188(9) 0.0027(7) 0.0001(7) 0.0112(8)
C36 0.0275(10) 0.0357(11) 0.0219(9) -0.0024(8) -0.0045(7) 0.0041(8)
C37 0.0270(9) 0.0255(9) 0.0220(9) -0.0009(7) -0.0011(7) 0.0011(7)
C38 0.0244(9) 0.0172(8) 0.0186(8) 0.0014(6) 0.0026(7) 0.0002(7)
C39 0.0296(9) 0.0219(9) 0.0193(8) -0.0016(7) 0.0030(7) -0.0010(7)
C40 0.0381(11) 0.0247(9) 0.0230(9) -0.0025(7) 0.0102(8) 0.0004(8)
C41 0.0281(10) 0.0245(9) 0.0333(10) 0.0007(8) 0.0128(8) 0.0043(8)
C42 0.0245(9) 0.0239(9) 0.0285(10) 0.0014(7) 0.0028(7) 0.0010(7)
C43 0.0225(9) 0.0214(8) 0.0185(8) 0.0010(7) 0.0035(7) 0.0005(7)
C44 0.0223(9) 0.0218(9) 0.0153(8) -0.0006(6) 0.0005(6) 0.0013(7)
C45 0.0230(9) 0.0240(9) 0.0181(8) 0.0014(7) 0.0021(7) -0.0017(7)
C46 0.0239(9) 0.0364(11) 0.0250(9) 0.0024(8) 0.0009(7) -0.0072(8)
C47 0.0214(9) 0.0445(12) 0.0306(10) 0.0062(9) -0.0025(8) 0.0029(8)
C48 0.0272(10) 0.0307(10) 0.0307(10) 0.0061(8) -0.0030(8) 0.0069(8)
C49 0.0252(9) 0.0219(9) 0.0253(9) 0.0025(7) 0.0009(7) 0.0007(7)
C50 0.075(5) 0.037(5) 0.045(5) 0.006(4) 0.021(4) -0.024(4)
C51 0.070(7) 0.075(8) 0.028(4) -0.008(5) 0.014(4) -0.031(6)
C52 0.067(6) 0.099(9) 0.030(4) 0.000(6) 0.008(4) -0.027(6)
C53 0.071(6) 0.061(8) 0.046(4) 0.009(6) 0.006(4) -0.032(6)
C54 0.084(7) 0.062(7) 0.044(5) -0.006(4) 0.016(4) -0.025(5)
C55 0.087(8) 0.062(6) 0.035(5) 0.001(4) 0.008(5) -0.024(6)
C56 0.086(5) 0.079(5) 0.066(4) 0.018(4) 0.038(4) 0.011(4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0460
1 -13 1 0.0296
5 10 0 0.0679
-5 -10 -2 0.0437
0 6 -11 0.0427
1 -8 -10 0.0118
-1 9 9 0.0335
7 6 -5 0.0727
0 0 13 0.0518
-3 2 12 0.0445
-1 6 11 0.0305
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
Fe3 Fe1 Fe2 60.398(10) . . ?
P1 Fe1 Fe2 109.170(16) . . ?
P1 Fe1 Fe3 132.322(17) . . ?
P3 Fe1 Fe2 54.238(14) . . ?
P3 Fe1 Fe3 109.485(16) . . ?
P3 Fe1 P1 93.096(19) . . ?
C1 Fe1 Fe2 49.53(5) . . ?
C1 Fe1 Fe3 46.87(5) . . ?
C1 Fe1 P1 158.24(5) . . ?
C1 Fe1 P3 71.11(5) . . ?
C8 Fe1 Fe2 144.22(6) . . ?
C8 Fe1 Fe3 117.53(6) . . ?
C8 Fe1 P1 96.96(6) . . ?
C8 Fe1 P3 101.63(6) . . ?
C8 Fe1 C1 100.77(8) . . ?
C8 Fe1 C9 91.62(8) . . ?
C9 Fe1 Fe2 114.53(6) . . ?
C9 Fe1 Fe3 64.44(6) . . ?
C9 Fe1 P1 83.96(6) . . ?
C9 Fe1 P3 166.69(6) . . ?
C9 Fe1 C1 107.89(8) . . ?
Fe1 Fe2 Fe3 59.786(10) . . ?
P2 Fe2 Fe1 113.118(16) . . ?
P2 Fe2 Fe3 146.105(17) . . ?
P3 Fe2 Fe1 53.857(14) . . ?
P3 Fe2 Fe3 108.583(16) . . ?
P3 Fe2 P2 85.541(18) . . ?
C1 Fe2 Fe1 49.75(5) . . ?
C1 Fe2 Fe3 46.60(5) . . ?
C1 Fe2 P2 156.29(5) . . ?
C1 Fe2 P3 71.00(5) . . ?
C13 Fe2 Fe1 99.77(6) . . ?
C13 Fe2 Fe3 64.30(5) . . ?
C13 Fe2 P2 86.44(6) . . ?
C13 Fe2 P3 145.61(6) . . ?
C13 Fe2 C1 110.89(7) . . ?
C14 Fe2 Fe1 150.61(6) . . ?
C14 Fe2 Fe3 107.37(6) . . ?
C14 Fe2 P2 91.97(6) . . ?
C14 Fe2 P3 116.93(6) . . ?
C14 Fe2 C1 101.51(7) . . ?
C14 Fe2 C13 96.72(8) . . ?
Fe1 Fe3 Fe2 59.816(10) . . ?
C1 Fe3 Fe1 50.15(5) . . ?
C1 Fe3 Fe2 49.63(5) . . ?
C1 Fe3 C9 89.36(7) . . ?
C1 Fe3 C13 91.32(7) . . ?
C9 Fe3 Fe1 41.70(5) . . ?
C9 Fe3 Fe2 94.89(5) . . ?
C9 Fe3 C13 97.85(6) . . ?
C10 Fe3 Fe1 97.04(6) . . ?
C10 Fe3 Fe2 142.18(6) . . ?
C10 Fe3 C1 92.58(8) . . ?
C10 Fe3 C9 81.45(8) . . ?
C10 Fe3 C11 99.14(8) . . ?
C10 Fe3 C12 91.37(9) . . ?
C10 Fe3 C13 176.03(8) . . ?
C11 Fe3 Fe1 113.98(6) . . ?
C11 Fe3 Fe2 117.15(6) . . ?
C11 Fe3 C1 161.72(8) . . ?
C11 Fe3 C9 78.66(7) . . ?
C11 Fe3 C13 76.90(7) . . ?
C12 Fe3 Fe1 147.57(6) . . ?
C12 Fe3 Fe2 95.29(6) . . ?
C12 Fe3 C1 98.38(8) . . ?
C12 Fe3 C9 169.70(8) . . ?
C12 Fe3 C11 95.34(8) . . ?
C12 Fe3 C13 88.80(7) . . ?
C13 Fe3 Fe1 84.90(4) . . ?
C13 Fe3 Fe2 41.70(4) . . ?
C17 P1 Fe1 121.64(6) . . ?
C20 P1 Fe1 108.65(6) . . ?
C20 P1 C17 100.98(8) . . ?
C20 P1 C26 103.67(8) . . ?
C26 P1 Fe1 118.23(6) . . ?
C26 P1 C17 101.11(8) . . ?
C18 P2 Fe2 115.07(6) . . ?
C18 P2 C38 102.12(8) . . ?
C32 P2 Fe2 115.97(6) . . ?
C32 P2 C18 102.72(8) . . ?
C32 P2 C38 100.30(8) . . ?
C38 P2 Fe2 118.24(6) . . ?
Fe1 P3 Fe2 71.905(16) . . ?
C19 P3 Fe1 121.60(6) . . ?
C19 P3 Fe2 121.10(6) . . ?
C44 P3 Fe1 120.88(6) . . ?
C44 P3 Fe2 126.90(6) . . ?
C44 P3 C19 96.41(8) . . ?
Fe2 C1 Fe1 80.72(6) . . ?
Fe3 C1 Fe1 82.97(7) . . ?
Fe3 C1 Fe2 83.77(7) . . ?
C2 C1 Fe1 134.88(13) . . ?
C2 C1 Fe2 130.55(12) . . ?
C2 C1 Fe3 125.78(12) . . ?
C3 C2 C1 120.58(15) . . ?
C3 C2 C7 116.62(16) . . ?
C7 C2 C1 122.79(16) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 121.90(17) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.37(17) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.6 . . ?
C6 C5 C4 118.83(17) . . ?
C6 C5 H5 120.6 . . ?
C5 C6 H6 119.5 . . ?
C5 C6 C7 120.92(17) . . ?
C7 C6 H6 119.5 . . ?
C2 C7 H7 119.4 . . ?
C6 C7 C2 121.22(17) . . ?
C6 C7 H7 119.4 . . ?
O1 C8 Fe1 177.26(17) . . ?
Fe1 C9 Fe3 73.86(6) . . ?
O2 C9 Fe1 163.37(16) . . ?
O2 C9 Fe3 122.36(14) . . ?
O3 C10 Fe3 177.74(18) . . ?
O4 C11 Fe3 178.80(18) . . ?
O5 C12 Fe3 177.78(18) . . ?
Fe2 C13 Fe3 74.00(6) . . ?
O6 C13 Fe2 163.96(15) . . ?
O6 C13 Fe3 121.87(13) . . ?
O7 C14 Fe2 174.89(16) . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C16 C15 H15A 109.5 . . ?
C16 C15 H15B 109.5 . . ?
C16 C15 H15C 109.5 . . ?
C15 C16 C17 108.11(15) . . ?
C15 C16 C18 108.21(15) . . ?
C15 C16 C19 106.92(15) . . ?
C17 C16 C18 110.35(15) . . ?
C17 C16 C19 107.94(15) . . ?
C19 C16 C18 115.06(14) . . ?
P1 C17 H17A 108.0 . . ?
P1 C17 H17B 108.0 . . ?
C16 C17 P1 117.37(12) . . ?
C16 C17 H17A 108.0 . . ?
C16 C17 H17B 108.0 . . ?
H17A C17 H17B 107.2 . . ?
P2 C18 H18A 108.0 . . ?
P2 C18 H18B 108.0 . . ?
C16 C18 P2 117.26(12) . . ?
C16 C18 H18A 108.0 . . ?
C16 C18 H18B 108.0 . . ?
H18A C18 H18B 107.2 . . ?
P3 C19 H19A 107.8 . . ?
P3 C19 H19B 107.8 . . ?
C16 C19 P3 118.22(12) . . ?
C16 C19 H19A 107.8 . . ?
C16 C19 H19B 107.8 . . ?
H19A C19 H19B 107.1 . . ?
C21 C20 P1 119.22(14) . . ?
C25 C20 P1 121.36(14) . . ?
C25 C20 C21 118.86(17) . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.46(19) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 119.8 . . ?
C23 C22 C21 120.37(19) . . ?
C23 C22 H22 119.8 . . ?
C22 C23 H23 120.2 . . ?
C24 C23 C22 119.67(18) . . ?
C24 C23 H23 120.2 . . ?
C23 C24 H24 119.6 . . ?
C23 C24 C25 120.8(2) . . ?
C25 C24 H24 119.6 . . ?
C20 C25 H25 120.1 . . ?
C24 C25 C20 119.86(19) . . ?
C24 C25 H25 120.1 . . ?
C27 C26 P1 121.54(14) . . ?
C31 C26 P1 119.75(14) . . ?
C31 C26 C27 118.58(17) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.02(18) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 119.6 . . ?
C29 C28 C27 120.86(19) . . ?
C29 C28 H28 119.6 . . ?
C28 C29 H29 120.3 . . ?
C28 C29 C30 119.49(19) . . ?
C30 C29 H29 120.3 . . ?
C29 C30 H30 120.0 . . ?
C29 C30 C31 119.93(19) . . ?
C31 C30 H30 120.0 . . ?
C26 C31 H31 119.4 . . ?
C30 C31 C26 121.11(18) . . ?
C30 C31 H31 119.4 . . ?
C33 C32 P2 117.52(14) . . ?
C33 C32 C37 119.17(17) . . ?
C37 C32 P2 123.16(14) . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.65(18) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 H34 120.1 . . ?
C35 C34 C33 119.76(19) . . ?
C35 C34 H34 120.1 . . ?
C34 C35 H35 120.0 . . ?
C36 C35 C34 120.09(18) . . ?
C36 C35 H35 120.0 . . ?
C35 C36 H36 119.8 . . ?
C35 C36 C37 120.40(19) . . ?
C37 C36 H36 119.8 . . ?
C32 C37 H37 120.0 . . ?
C36 C37 C32 119.93(18) . . ?
C36 C37 H37 120.0 . . ?
C39 C38 P2 119.50(14) . . ?
C43 C38 P2 121.76(13) . . ?
C43 C38 C39 118.66(17) . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.48(18) . . ?
C40 C39 H39 119.8 . . ?
C39 C40 H40 119.9 . . ?
C39 C40 C41 120.14(18) . . ?
C41 C40 H40 119.9 . . ?
C40 C41 H41 120.1 . . ?
C42 C41 C40 119.71(18) . . ?
C42 C41 H41 120.1 . . ?
C41 C42 H42 119.9 . . ?
C43 C42 C41 120.20(18) . . ?
C43 C42 H42 119.9 . . ?
C38 C43 H43 119.6 . . ?
C42 C43 C38 120.80(17) . . ?
C42 C43 H43 119.6 . . ?
C45 C44 P3 122.30(14) . . ?
C45 C44 C49 119.03(17) . . ?
C49 C44 P3 118.60(14) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 C44 120.15(17) . . ?
C46 C45 H45 119.9 . . ?
C45 C46 H46 119.8 . . ?
C47 C46 C45 120.41(18) . . ?
C47 C46 H46 119.8 . . ?
C46 C47 H47 120.1 . . ?
C48 C47 C46 119.87(18) . . ?
C48 C47 H47 120.1 . . ?
C47 C48 H48 120.0 . . ?
C47 C48 C49 119.95(19) . . ?
C49 C48 H48 120.0 . . ?
C44 C49 H49 119.7 . . ?
C48 C49 C44 120.58(18) . . ?
C48 C49 H49 119.7 . . ?
C51 C50 C55 118.3(10) . . ?
C51 C50 C56 121.3(9) . . ?
C55 C50 C56 120.4(9) . . ?
C50 C51 H51 119.7 . . ?
C50 C51 C52 120.7(10) . . ?
C52 C51 H51 119.7 . . ?
C51 C52 H52 119.1 . . ?
C51 C52 C53 121.7(11) . . ?
C53 C52 H52 119.1 . . ?
C52 C53 H53 121.7 . . ?
C54 C53 C52 116.7(11) . . ?
C54 C53 H53 121.7 . . ?
C53 C54 H54 119.0 . . ?
C53 C54 C55 122.1(12) . . ?
C55 C54 H54 119.0 . . ?
C50 C55 H55 119.7 . . ?
C54 C55 C50 120.6(11) . . ?
C54 C55 H55 119.7 . . ?
C50 C56 H56A 109.5 . . ?
C50 C56 H56B 109.5 . . ?
C50 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 Fe2 2.5907(4) . ?
Fe1 Fe3 2.5899(4) . ?
Fe1 P1 2.2664(5) . ?
Fe1 P3 2.2010(5) . ?
Fe1 C1 2.0035(17) . ?
Fe1 C8 1.7617(19) . ?
Fe1 C9 1.7938(19) . ?
Fe2 Fe3 2.6059(4) . ?
Fe2 P2 2.2334(5) . ?
Fe2 P3 2.2116(5) . ?
Fe2 C1 1.9971(17) . ?
Fe2 C13 1.8033(19) . ?
Fe2 C14 1.7806(19) . ?
Fe3 C1 1.9046(18) . ?
Fe3 C9 2.4324(18) . ?
Fe3 C10 1.774(2) . ?
Fe3 C11 1.853(2) . ?
Fe3 C12 1.779(2) . ?
Fe3 C13 2.4427(17) . ?
P1 C17 1.8572(19) . ?
P1 C20 1.8316(18) . ?
P1 C26 1.8374(19) . ?
P2 C18 1.8349(18) . ?
P2 C32 1.8313(18) . ?
P2 C38 1.8370(19) . ?
P3 C19 1.8485(18) . ?
P3 C44 1.8322(18) . ?
O1 C8 1.154(2) . ?
O2 C9 1.163(2) . ?
O3 C10 1.148(2) . ?
O4 C11 1.132(2) . ?
O5 C12 1.143(2) . ?
O6 C13 1.161(2) . ?
O7 C14 1.152(2) . ?
C1 C2 1.479(2) . ?
C2 C3 1.405(2) . ?
C2 C7 1.405(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.383(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(3) . ?
C7 H7 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C15 C16 1.538(2) . ?
C16 C17 1.538(3) . ?
C16 C18 1.566(2) . ?
C16 C19 1.539(2) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.399(3) . ?
C20 C25 1.395(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.380(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.379(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.393(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.399(3) . ?
C26 C31 1.390(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.386(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.383(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.385(3) . ?
C30 H30 0.9500 . ?
C30 C31 1.387(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(3) . ?
C32 C37 1.397(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.391(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.385(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.390(3) . ?
C37 H37 0.9500 . ?
C38 C39 1.398(2) . ?
C38 C43 1.392(2) . ?
C39 H39 0.9500 . ?
C39 C40 1.388(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.388(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.385(3) . ?
C42 H42 0.9500 . ?
C42 C43 1.384(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.394(3) . ?
C44 C49 1.399(2) . ?
C45 H45 0.9500 . ?
C45 C46 1.389(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.388(3) . ?
C47 H47 0.9500 . ?
C47 C48 1.387(3) . ?
C48 H48 0.9500 . ?
C48 C49 1.388(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.373(13) . ?
C50 C55 1.389(13) . ?
C50 C56 1.502(13) . ?
C51 H51 0.9500 . ?
C51 C52 1.381(13) . ?
C52 H52 0.9500 . ?
C52 C53 1.394(13) . ?
C53 H53 0.9500 . ?
C53 C54 1.376(14) . ?
C54 H54 0.9500 . ?
C54 C55 1.377(14) . ?
C55 H55 0.9500 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 Fe2 C13 Fe3 -49.49(4) . . . . ?
Fe1 Fe2 C13 O6 138.4(6) . . . . ?
Fe1 P1 C17 C16 34.55(16) . . . . ?
Fe1 P1 C20 C21 76.58(16) . . . . ?
Fe1 P1 C20 C25 -94.82(15) . . . . ?
Fe1 P1 C26 C27 165.16(14) . . . . ?
Fe1 P1 C26 C31 -19.18(18) . . . . ?
Fe1 P3 C19 C16 -39.42(16) . . . . ?
Fe1 P3 C44 C45 119.55(14) . . . . ?
Fe1 P3 C44 C49 -63.48(16) . . . . ?
Fe1 C1 C2 C3 -164.87(14) . . . . ?
Fe1 C1 C2 C7 16.1(3) . . . . ?
Fe2 Fe1 C9 Fe3 34.89(5) . . . . ?
Fe2 Fe1 C9 O2 -157.3(5) . . . . ?
Fe2 P2 C18 C16 63.73(14) . . . . ?
Fe2 P2 C32 C33 -73.16(15) . . . . ?
Fe2 P2 C32 C37 102.31(15) . . . . ?
Fe2 P2 C38 C39 -178.40(12) . . . . ?
Fe2 P2 C38 C43 -1.73(17) . . . . ?
Fe2 P3 C19 C16 47.43(15) . . . . ?
Fe2 P3 C44 C45 29.75(18) . . . . ?
Fe2 P3 C44 C49 -153.28(12) . . . . ?
Fe2 C1 C2 C3 -41.3(2) . . . . ?
Fe2 C1 C2 C7 139.62(16) . . . . ?
Fe3 Fe1 C9 O2 167.9(6) . . . . ?
Fe3 Fe2 C13 O6 -172.1(6) . . . . ?
Fe3 C1 C2 C3 74.8(2) . . . . ?
Fe3 C1 C2 C7 -104.24(19) . . . . ?
P1 Fe1 C9 Fe3 143.24(4) . . . . ?
P1 Fe1 C9 O2 -48.9(6) . . . . ?
P1 C20 C21 C22 -171.03(15) . . . . ?
P1 C20 C25 C24 171.20(15) . . . . ?
P1 C26 C27 C28 176.09(16) . . . . ?
P1 C26 C31 C30 -175.11(17) . . . . ?
P2 Fe2 C13 Fe3 -162.35(3) . . . . ?
P2 Fe2 C13 O6 25.5(6) . . . . ?
P2 C32 C33 C34 176.72(15) . . . . ?
P2 C32 C37 C36 -176.29(15) . . . . ?
P2 C38 C39 C40 175.52(14) . . . . ?
P2 C38 C43 C42 -175.34(14) . . . . ?
P3 Fe1 C9 Fe3 65.4(3) . . . . ?
P3 Fe1 C9 O2 -126.7(5) . . . . ?
P3 Fe2 C13 Fe3 -85.58(9) . . . . ?
P3 Fe2 C13 O6 102.3(6) . . . . ?
P3 C44 C45 C46 176.09(14) . . . . ?
P3 C44 C49 C48 -176.42(15) . . . . ?
C1 Fe1 C9 Fe3 -18.07(7) . . . . ?
C1 Fe1 C9 O2 149.8(5) . . . . ?
C1 Fe2 C13 Fe3 1.01(7) . . . . ?
C1 Fe2 C13 O6 -171.1(6) . . . . ?
C1 C2 C3 C4 177.99(16) . . . . ?
C1 C2 C7 C6 -177.29(17) . . . . ?
C2 C3 C4 C5 -0.1(3) . . . . ?
C3 C2 C7 C6 3.6(3) . . . . ?
C3 C4 C5 C6 2.5(3) . . . . ?
C4 C5 C6 C7 -1.7(3) . . . . ?
C5 C6 C7 C2 -1.4(3) . . . . ?
C7 C2 C3 C4 -2.9(3) . . . . ?
C8 Fe1 C9 Fe3 -119.94(6) . . . . ?
C8 Fe1 C9 O2 47.9(6) . . . . ?
C14 Fe2 C13 Fe3 106.08(6) . . . . ?
C14 Fe2 C13 O6 -66.0(6) . . . . ?
C15 C16 C17 P1 175.88(12) . . . . ?
C15 C16 C18 P2 116.60(14) . . . . ?
C15 C16 C19 P3 -171.67(12) . . . . ?
C17 P1 C20 C21 -52.42(17) . . . . ?
C17 P1 C20 C25 136.18(16) . . . . ?
C17 P1 C26 C27 -59.43(17) . . . . ?
C17 P1 C26 C31 116.23(16) . . . . ?
C17 C16 C18 P2 -125.30(14) . . . . ?
C17 C16 C19 P3 72.22(17) . . . . ?
C18 P2 C32 C33 160.47(14) . . . . ?
C18 P2 C32 C37 -24.07(17) . . . . ?
C18 P2 C38 C39 -51.02(16) . . . . ?
C18 P2 C38 C43 125.65(15) . . . . ?
C18 C16 C17 P1 57.72(18) . . . . ?
C18 C16 C19 P3 -51.49(19) . . . . ?
C19 P3 C44 C45 -107.49(16) . . . . ?
C19 P3 C44 C49 69.48(16) . . . . ?
C19 C16 C17 P1 -68.80(17) . . . . ?
C19 C16 C18 P2 -2.9(2) . . . . ?
C20 P1 C17 C16 154.69(14) . . . . ?
C20 P1 C26 C27 44.90(18) . . . . ?
C20 P1 C26 C31 -139.44(16) . . . . ?
C20 C21 C22 C23 -0.4(3) . . . . ?
C21 C20 C25 C24 -0.2(3) . . . . ?
C21 C22 C23 C24 -0.1(3) . . . . ?
C22 C23 C24 C25 0.5(3) . . . . ?
C23 C24 C25 C20 -0.3(3) . . . . ?
C25 C20 C21 C22 0.6(3) . . . . ?
C26 P1 C17 C16 -98.85(14) . . . . ?
C26 P1 C20 C21 -156.85(15) . . . . ?
C26 P1 C20 C25 31.75(17) . . . . ?
C26 C27 C28 C29 -0.7(3) . . . . ?
C27 C26 C31 C30 0.7(3) . . . . ?
C27 C28 C29 C30 0.0(4) . . . . ?
C28 C29 C30 C31 1.1(4) . . . . ?
C29 C30 C31 C26 -1.4(4) . . . . ?
C31 C26 C27 C28 0.4(3) . . . . ?
C32 P2 C18 C16 -169.32(13) . . . . ?
C32 P2 C38 C39 54.52(16) . . . . ?
C32 P2 C38 C43 -128.81(15) . . . . ?
C32 C33 C34 C35 -0.8(3) . . . . ?
C33 C32 C37 C36 -0.9(3) . . . . ?
C33 C34 C35 C36 0.3(3) . . . . ?
C34 C35 C36 C37 -0.1(3) . . . . ?
C35 C36 C37 C32 0.4(3) . . . . ?
C37 C32 C33 C34 1.1(3) . . . . ?
C38 P2 C18 C16 -65.67(14) . . . . ?
C38 P2 C32 C33 55.42(15) . . . . ?
C38 P2 C32 C37 -129.12(16) . . . . ?
C38 C39 C40 C41 0.4(3) . . . . ?
C39 C38 C43 C42 1.4(3) . . . . ?
C39 C40 C41 C42 0.4(3) . . . . ?
C40 C41 C42 C43 -0.3(3) . . . . ?
C41 C42 C43 C38 -0.6(3) . . . . ?
C43 C38 C39 C40 -1.3(3) . . . . ?
C44 P3 C19 C16 -171.92(14) . . . . ?
C44 C45 C46 C47 0.2(3) . . . . ?
C45 C44 C49 C48 0.7(3) . . . . ?
C45 C46 C47 C48 0.8(3) . . . . ?
C46 C47 C48 C49 -1.0(3) . . . . ?
C47 C48 C49 C44 0.3(3) . . . . ?
C49 C44 C45 C46 -0.9(3) . . . . ?
C50 C51 C52 C53 -1.0(12) . . . . ?
C51 C50 C55 C54 -0.5(9) . . . . ?
C51 C52 C53 C54 0.7(10) . . . . ?
C52 C53 C54 C55 -0.3(5) . . . . ?
C53 C54 C55 C50 0.2(5) . . . . ?
C55 C50 C51 C52 0.8(11) . . . . ?
C56 C50 C51 C52 179.9(8) . . . . ?
C56 C50 C55 C54 -179.6(5) . . . . ?