#------------------------------------------------------------------------------
#$Date: 2023-09-05 22:13:01 +0300 (Tue, 05 Sep 2023) $
#$Revision: 286051 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/92/1569244.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_1569244
loop_
_publ_author_name
'Reichl, Stephan'
'Riedlberger, Felix'
'Piesch, Martin'
'Balázs, Gábor'
'Seidl, Michael'
'Scheer, Manfred'
_publ_section_title
;
 Controlled introduction of functional groups at one P atom in
 [Cp*Fe(η⁵-P₅)] and release of
 functionalised phosphines.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              7285
_journal_page_last               7290
_journal_paper_doi               10.1039/d3sc01488f
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '2(C8.5 H15 Br0.5 Fe0.5 P2.5)'
_chemical_formula_sum            'C17 H30 Br Fe P5'
_chemical_formula_weight         525.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-02-19
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6020)
;
_audit_update_record
;
2020-11-02 deposited with the CCDC.	2023-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.764(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2089(5)
_cell_length_b                   11.4407(4)
_cell_length_c                   18.1308(8)
_cell_measurement_reflns_used    5064
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      31.5100
_cell_measurement_theta_min      3.8660
_cell_volume                     2237.60(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.896
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -92.00  -2.00   0.25   50.00    --  -19.91 -38.00-180.00  360
  2  ω    -83.00 -57.00   0.25   50.00    --  -19.91 133.00 143.00  104
  3  ω    -90.00  -3.00   0.25   50.00    --  -19.91 -38.00  90.00  348
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0539627000
_diffrn_orient_matrix_UB_12      0.0025364000
_diffrn_orient_matrix_UB_13      -0.0132671000
_diffrn_orient_matrix_UB_21      0.0375221000
_diffrn_orient_matrix_UB_22      -0.0001476000
_diffrn_orient_matrix_UB_23      0.0383969000
_diffrn_orient_matrix_UB_31      0.0020869000
_diffrn_orient_matrix_UB_32      -0.0619551000
_diffrn_orient_matrix_UB_33      -0.0006606000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            13109
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.281
_diffrn_reflns_theta_min         3.499
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.816
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       needle
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.271
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.046
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         7434
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0355P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6052
_reflns_number_total             7434
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc01488f2.cif
_cod_data_source_block           resp5_tbu_dibr_mp_abs_ana
_cod_depositor_comments
'Adding full bibliography for 1569243--1569247.cif.'
_cod_database_code               1569244
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C17H30BrFeP5
_chemical_oxdiff_usercomment     'green needle'
_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   0.832
_shelx_estimated_absorpt_t_min   0.516
_reflns_odcompleteness_completeness 98.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H6A(0.5) H6B(0.5) H6C(0.5) H10A(0.5) H10B(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) H18A(0.5) H18C(0.5) H12A(0.5) H12B(0.5) H11A(0.5) H11B(0.5)
 H22A(0.5) H22B(0.5) H24A(0.5) H24B(0.5) H23A(0.5) H23B(0.5) H9A(0.5) H9C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C11(H11A,H11B), C22(H22A,H22B), C24(H24A,
 H24B), C23(H23A,H23B)
3.b Me refined with everything fixed:
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C21(H21A,H21B,H21C),
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.332
_oxdiff_exptl_absorpt_empirical_full_min 0.788
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Br1 Br 0.62860(3) 0.750000 0.55866(2) 0.02576(7) Uani 1 2 d S T P . .
Br2 Br 0.36094(3) 0.750000 0.19142(2) 0.02865(8) Uani 1 2 d S T P . .
Fe2 Fe 0.15448(3) 0.750000 0.45994(2) 0.01514(8) Uani 1 2 d S T P . .
Fe1 Fe 0.73337(3) 0.750000 0.89633(2) 0.01423(8) Uani 1 2 d S T P . .
P4 P -0.05766(7) 0.750000 0.30927(4) 0.01802(14) Uani 1 2 d S T P . .
P1 P 0.98062(7) 0.750000 0.85066(4) 0.01849(14) Uani 1 2 d S T P . .
P6 P -0.01474(5) 0.65571(4) 0.48319(3) 0.01833(10) Uani 1 1 d . . . . .
P2 P 0.87385(5) 0.60815(4) 0.87877(3) 0.02062(11) Uani 1 1 d . . . . .
P5 P 0.03214(5) 0.60688(4) 0.38012(3) 0.01902(11) Uani 1 1 d . . . . .
P3 P 0.88033(5) 0.65563(5) 0.99430(3) 0.02382(12) Uani 1 1 d . . . . .
C14 C 0.29615(18) 0.64912(15) 0.52796(11) 0.0184(4) Uani 1 1 d . . . . .
C3 C 0.5826(2) 0.750000 0.94087(15) 0.0174(5) Uani 1 2 d S T P . .
C15 C 0.2739(2) 0.750000 0.56890(15) 0.0170(5) Uani 1 2 d S T P . .
C2 C 0.57820(17) 0.64879(15) 0.89358(11) 0.0169(4) Uani 1 1 d . . . . .
C1 C 0.56914(17) 0.68741(15) 0.81700(11) 0.0173(4) Uani 1 1 d . . . . .
C13 C 0.33288(18) 0.68759(16) 0.46227(11) 0.0197(4) Uani 1 1 d . . . . .
C6 C 0.5845(3) 0.750000 1.02387(16) 0.0226(6) Uani 1 2 d S T P . .
H6A H 0.641228 0.810838 1.050971 0.034 Uiso 0.5 1 calc R U P A -1
H6B H 0.612614 0.673584 1.046392 0.034 Uiso 0.5 1 calc R U P A -1
H6C H 0.500868 0.765578 1.028513 0.034 Uiso 0.5 1 calc R U P A -1
C4 C 0.5507(2) 0.60744(17) 0.74900(11) 0.0232(4) Uani 1 1 d . . . . .
H4A H 0.469052 0.570316 0.738673 0.035 Uiso 1 1 calc R U . . .
H4B H 0.615249 0.547141 0.759916 0.035 Uiso 1 1 calc R U . . .
H4C H 0.555874 0.652748 0.704094 0.035 Uiso 1 1 calc R U . . .
C19 C -0.2308(3) 0.750000 0.27098(16) 0.0206(6) Uani 1 2 d S T P . .
C10 C 0.9524(3) 0.750000 0.74595(16) 0.0270(6) Uani 1 2 d S T P . .
H10A H 0.992548 0.819817 0.731011 0.032 Uiso 0.5 1 calc R U P . .
H10B H 0.992548 0.680183 0.731011 0.032 Uiso 0.5 1 calc R U P . .
C5 C 0.5756(2) 0.52380(16) 0.91780(12) 0.0241(4) Uani 1 1 d . . . . .
H5A H 0.620446 0.475352 0.889632 0.036 Uiso 1 1 calc R U . . .
H5B H 0.489441 0.497145 0.906697 0.036 Uiso 1 1 calc R U . . .
H5C H 0.615183 0.517159 0.972921 0.036 Uiso 1 1 calc R U . . .
C21 C -0.2916(3) 0.750000 0.33690(17) 0.0257(6) Uani 1 2 d S T P . .
H21A H -0.256197 0.813004 0.372804 0.038 Uiso 0.5 1 calc R U P B -1
H21B H -0.276529 0.674742 0.363642 0.038 Uiso 0.5 1 calc R U P B -1
H21C H -0.381069 0.762254 0.316538 0.038 Uiso 0.5 1 calc R U P B -1
C7 C 1.1535(3) 0.750000 0.88763(17) 0.0246(6) Uani 1 2 d S T P . .
C18 C 0.2382(3) 0.750000 0.64279(16) 0.0233(6) Uani 1 2 d S T P . .
H18A H 0.189062 0.819928 0.645397 0.035 Uiso 0.5 1 calc . U P C -1
H18B H 0.313258 0.750024 0.685878 0.035 Uiso 0.5 1 calc . U P D -1
H18C H 0.189104 0.680048 0.645411 0.035 Uiso 0.5 1 calc . U P E -1
C17 C 0.2919(2) 0.52511(15) 0.55422(12) 0.0248(4) Uani 1 1 d . . . . .
H17A H 0.225948 0.516998 0.579943 0.037 Uiso 1 1 calc R U . . .
H17B H 0.371729 0.504712 0.590017 0.037 Uiso 1 1 calc R U . . .
H17C H 0.275340 0.472683 0.509847 0.037 Uiso 1 1 calc R U . . .
C12 C 0.8030(3) 0.750000 0.61605(16) 0.0277(6) Uani 1 2 d S T P . .
H12A H 0.844232 0.679954 0.602291 0.033 Uiso 0.5 1 calc R U P . .
H12B H 0.844232 0.820046 0.602291 0.033 Uiso 0.5 1 calc R U P . .
C16 C 0.3728(2) 0.60872(18) 0.40712(13) 0.0290(5) Uani 1 1 d . . . . .
H16A H 0.373224 0.652717 0.360826 0.043 Uiso 1 1 calc R U . . .
H16B H 0.314840 0.543040 0.393382 0.043 Uiso 1 1 calc R U . . .
H16C H 0.456263 0.578945 0.431191 0.043 Uiso 1 1 calc R U . . .
C11 C 0.8164(3) 0.750000 0.70134(16) 0.0259(6) Uani 1 2 d S T P . .
H11A H 0.775234 0.679950 0.715115 0.031 Uiso 0.5 1 calc R U P . .
H11B H 0.775235 0.820050 0.715115 0.031 Uiso 0.5 1 calc R U P . .
C22 C -0.0008(3) 0.750000 0.22317(16) 0.0264(6) Uani 1 2 d S T P . .
H22A H -0.033682 0.680133 0.192047 0.032 Uiso 0.5 1 calc R U P . .
H22B H -0.033681 0.819867 0.192047 0.032 Uiso 0.5 1 calc R U P . .
C24 C 0.1796(3) 0.750000 0.16739(17) 0.0275(6) Uani 1 2 d S T P . .
H24A H 0.146213 0.820076 0.136660 0.033 Uiso 0.5 1 calc R U P . .
H24B H 0.146213 0.679924 0.136660 0.033 Uiso 0.5 1 calc R U P . .
C23 C 0.1394(3) 0.750000 0.24055(17) 0.0295(7) Uani 1 2 d S T P . .
H23A H 0.173189 0.820028 0.271224 0.035 Uiso 0.5 1 calc R U P . .
H23B H 0.173188 0.679972 0.271224 0.035 Uiso 0.5 1 calc R U P . .
C20 C -0.2700(2) 0.63906(18) 0.22290(13) 0.0302(5) Uani 1 1 d . . . . .
H20A H -0.234814 0.640341 0.178968 0.045 Uiso 1 1 calc R U . . .
H20B H -0.360588 0.635876 0.204568 0.045 Uiso 1 1 calc R U . . .
H20C H -0.239445 0.570113 0.254476 0.045 Uiso 1 1 calc R U . . .
C9 C 1.1893(3) 0.750000 0.97556(19) 0.0367(8) Uani 1 2 d S T P . .
H9A H 1.155541 0.819946 0.993737 0.055 Uiso 0.5 1 calc . U P F -1
H9B H 1.279865 0.749989 0.995363 0.055 Uiso 0.5 1 calc . U P G -1
H9C H 1.155521 0.680065 0.993736 0.055 Uiso 0.5 1 calc . U P H -1
C8 C 1.2052(2) 0.8606(2) 0.85916(15) 0.0374(6) Uani 1 1 d . . . . .
H8A H 1.184484 0.859466 0.803059 0.056 Uiso 1 1 calc R U . . .
H8B H 1.295442 0.862778 0.880246 0.056 Uiso 1 1 calc R U . . .
H8C H 1.168518 0.929933 0.876031 0.056 Uiso 1 1 calc R U . . .
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'
Br Br -0.2901 2.4595 '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'
P P 0.1023 0.0942 '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
-5 -1 -21 0.0329
5 9 -21 0.1102
6 -2 -25 0.0331
-6 0 25 0.0246
5 -8 17 0.0742
-4 13 16 0.1292
9 13 -1 0.1167
14 -1 -17 0.0346
5 2 21 0.0348
-13 -7 16 0.0493
-5 -10 19 0.0548
2 -16 -5 0.1016
-12 -2 21 0.0214
-14 4 17 0.0549
-16 1 5 0.0362
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
P6 Fe2 P6 55.47(3) . 4_575 ?
P6 Fe2 P5 93.81(2) 4_575 . ?
P6 Fe2 P5 54.633(19) 4_575 4_575 ?
P6 Fe2 P5 54.632(19) . . ?
P6 Fe2 P5 93.81(2) . 4_575 ?
P5 Fe2 P5 87.79(3) 4_575 . ?
C14 Fe2 P6 99.49(5) . . ?
C14 Fe2 P6 133.01(6) . 4_575 ?
C14 Fe2 P6 133.01(6) 4_575 . ?
C14 Fe2 P6 99.48(5) 4_575 4_575 ?
C14 Fe2 P5 166.53(6) . 4_575 ?
C14 Fe2 P5 166.53(6) 4_575 . ?
C14 Fe2 P5 101.63(5) 4_575 4_575 ?
C14 Fe2 P5 101.63(5) . . ?
C14 Fe2 C14 67.55(10) 4_575 . ?
C14 Fe2 C13 39.94(7) . . ?
C14 Fe2 C13 66.98(7) 4_575 . ?
C14 Fe2 C13 66.98(7) . 4_575 ?
C14 Fe2 C13 39.94(7) 4_575 4_575 ?
C15 Fe2 P6 100.13(7) . 4_575 ?
C15 Fe2 P6 100.13(7) . . ?
C15 Fe2 P5 134.77(2) . 4_575 ?
C15 Fe2 P5 134.77(2) . . ?
C15 Fe2 C14 40.42(6) . 4_575 ?
C15 Fe2 C14 40.43(6) . . ?
C15 Fe2 C13 67.46(9) . . ?
C15 Fe2 C13 67.45(9) . 4_575 ?
C13 Fe2 P6 166.00(6) 4_575 . ?
C13 Fe2 P6 130.98(5) 4_575 4_575 ?
C13 Fe2 P6 130.98(5) . . ?
C13 Fe2 P6 166.00(6) . 4_575 ?
C13 Fe2 P5 99.61(5) . . ?
C13 Fe2 P5 129.45(6) . 4_575 ?
C13 Fe2 P5 129.45(6) 4_575 . ?
C13 Fe2 P5 99.61(5) 4_575 4_575 ?
C13 Fe2 C13 39.50(10) 4_575 . ?
P2 Fe1 P2 87.70(3) . 4_575 ?
P3 Fe1 P2 54.64(2) . . ?
P3 Fe1 P2 93.58(2) . 4_575 ?
P3 Fe1 P2 54.64(2) 4_575 4_575 ?
P3 Fe1 P2 93.58(2) 4_575 . ?
P3 Fe1 P3 55.12(3) . 4_575 ?
C3 Fe1 P2 134.92(2) . 4_575 ?
C3 Fe1 P2 134.92(2) . . ?
C3 Fe1 P3 100.72(7) . . ?
C3 Fe1 P3 100.72(7) . 4_575 ?
C3 Fe1 C2 40.52(6) . . ?
C3 Fe1 C2 40.52(6) . 4_575 ?
C3 Fe1 C1 67.31(9) . 4_575 ?
C3 Fe1 C1 67.32(9) . . ?
C2 Fe1 P2 101.52(5) . . ?
C2 Fe1 P2 166.31(5) . 4_575 ?
C2 Fe1 P2 166.32(5) 4_575 . ?
C2 Fe1 P2 101.52(5) 4_575 4_575 ?
C2 Fe1 P3 133.56(5) . 4_575 ?
C2 Fe1 P3 100.00(5) 4_575 4_575 ?
C2 Fe1 P3 100.00(5) . . ?
C2 Fe1 P3 133.56(5) 4_575 . ?
C2 Fe1 C2 67.70(10) 4_575 . ?
C2 Fe1 C1 39.84(7) 4_575 4_575 ?
C2 Fe1 C1 66.85(7) 4_575 . ?
C2 Fe1 C1 39.84(7) . . ?
C2 Fe1 C1 66.85(7) . 4_575 ?
C1 Fe1 P2 99.49(5) . . ?
C1 Fe1 P2 129.12(5) . 4_575 ?
C1 Fe1 P2 129.12(5) 4_575 . ?
C1 Fe1 P2 99.49(5) 4_575 4_575 ?
C1 Fe1 P3 131.36(5) . . ?
C1 Fe1 P3 166.43(5) 4_575 . ?
C1 Fe1 P3 166.43(5) . 4_575 ?
C1 Fe1 P3 131.36(5) 4_575 4_575 ?
C1 Fe1 C1 39.31(9) . 4_575 ?
P5 P4 P5 98.93(4) . 4_575 ?
C19 P4 P5 119.31(5) . 4_575 ?
C19 P4 P5 119.31(5) . . ?
C22 P4 P5 107.01(6) . . ?
C22 P4 P5 107.01(6) . 4_575 ?
C22 P4 C19 104.37(13) . . ?
P2 P1 P2 97.53(4) . 4_575 ?
C10 P1 P2 107.04(6) . 4_575 ?
C10 P1 P2 107.04(7) . . ?
C10 P1 C7 103.94(14) . . ?
C7 P1 P2 120.16(5) . . ?
C7 P1 P2 120.16(5) . 4_575 ?
P6 P6 Fe2 62.267(13) 4_575 . ?
P5 P6 Fe2 63.72(2) . . ?
P5 P6 P6 105.076(18) . 4_575 ?
P1 P2 Fe1 86.99(2) . . ?
P3 P2 Fe1 62.46(2) . . ?
P3 P2 P1 99.57(3) . . ?
P4 P5 Fe2 86.44(2) . . ?
P6 P5 Fe2 61.65(2) . . ?
P6 P5 P4 97.82(3) . . ?
P2 P3 Fe1 62.90(2) . . ?
P2 P3 P3 104.662(19) . 4_575 ?
P3 P3 Fe1 62.439(14) 4_575 . ?
C15 C14 Fe2 69.31(12) . . ?
C15 C14 C13 108.29(17) . . ?
C15 C14 C17 124.96(18) . . ?
C13 C14 Fe2 71.41(11) . . ?
C13 C14 C17 126.55(17) . . ?
C17 C14 Fe2 128.96(14) . . ?
C2 C3 Fe1 70.40(13) 4_575 . ?
C2 C3 Fe1 70.40(13) . . ?
C2 C3 C2 107.7(2) . 4_575 ?
C2 C3 C6 126.09(11) . . ?
C2 C3 C6 126.09(11) 4_575 . ?
C6 C3 Fe1 127.2(2) . . ?
C14 C15 Fe2 70.27(13) . . ?
C14 C15 Fe2 70.27(13) 4_575 . ?
C14 C15 C14 107.6(2) 4_575 . ?
C14 C15 C18 126.19(12) . . ?
C14 C15 C18 126.19(12) 4_575 . ?
C18 C15 Fe2 126.50(19) . . ?
C3 C2 Fe1 69.08(13) . . ?
C3 C2 C1 108.18(16) . . ?
C3 C2 C5 126.56(17) . . ?
C1 C2 Fe1 71.96(11) . . ?
C1 C2 C5 125.16(16) . . ?
C5 C2 Fe1 127.40(14) . . ?
C2 C1 Fe1 68.20(10) . . ?
C2 C1 C4 124.34(16) . . ?
C1 C1 Fe1 70.34(5) 4_575 . ?
C1 C1 C2 107.94(10) 4_575 . ?
C1 C1 C4 127.48(10) 4_575 . ?
C4 C1 Fe1 131.26(14) . . ?
C14 C13 Fe2 68.65(11) . . ?
C14 C13 C16 125.03(17) . . ?
C13 C13 Fe2 70.25(5) 4_575 . ?
C13 C13 C14 107.91(10) 4_575 . ?
C13 C13 C16 126.92(11) 4_575 . ?
C16 C13 Fe2 129.85(14) . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C21 C19 P4 110.30(19) . . ?
C21 C19 C20 108.96(17) . 4_575 ?
C21 C19 C20 108.96(17) . . ?
C20 C19 P4 108.52(15) 4_575 . ?
C20 C19 P4 108.52(15) . . ?
C20 C19 C20 111.6(2) 4_575 . ?
P1 C10 H10A 108.6 . . ?
P1 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?
C11 C10 P1 114.6(2) . . ?
C11 C10 H10A 108.6 . . ?
C11 C10 H10B 108.6 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C9 C7 P1 109.0(2) . . ?
C9 C7 C8 109.42(16) . 4_575 ?
C9 C7 C8 109.43(17) . . ?
C8 C7 P1 109.13(15) 4_575 . ?
C8 C7 P1 109.13(15) . . ?
C8 C7 C8 110.7(3) . 4_575 ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Br1 C12 H12A 109.5 . . ?
Br1 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C11 C12 Br1 110.6(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C12 C11 C10 110.5(3) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 108.1 . . ?
P4 C22 H22A 108.8 . . ?
P4 C22 H22B 108.8 . . ?
H22A C22 H22B 107.7 . . ?
C23 C22 P4 113.7(2) . . ?
C23 C22 H22A 108.8 . . ?
C23 C22 H22B 108.8 . . ?
Br2 C24 H24A 109.6 . . ?
Br2 C24 H24B 109.6 . . ?
H24A C24 H24B 108.2 . . ?
C23 C24 Br2 110.1(2) . . ?
C23 C24 H24A 109.6 . . ?
C23 C24 H24B 109.6 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C24 C23 C22 110.9(3) . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 108.0 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 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
Br1 C12 1.950(3) . ?
Br2 C24 1.959(3) . ?
Fe2 P6 2.3181(6) . ?
Fe2 P6 2.3182(6) 4_575 ?
Fe2 P5 2.3617(6) 4_575 ?
Fe2 P5 2.3617(6) . ?
Fe2 C14 2.0762(19) . ?
Fe2 C14 2.0762(19) 4_575 ?
Fe2 C15 2.063(3) . ?
Fe2 C13 2.1128(19) 4_575 ?
Fe2 C13 2.1128(19) . ?
Fe1 P2 2.3425(6) 4_575 ?
Fe1 P2 2.3425(6) . ?
Fe1 P3 2.3334(6) . ?
Fe1 P3 2.3334(6) 4_575 ?
Fe1 C3 2.061(3) . ?
Fe1 C2 2.0786(18) 4_575 ?
Fe1 C2 2.0787(18) . ?
Fe1 C1 2.1288(19) 4_575 ?
Fe1 C1 2.1288(19) . ?
P4 P5 2.1545(7) 4_575 ?
P4 P5 2.1545(7) . ?
P4 C19 1.875(3) . ?
P4 C22 1.839(3) . ?
P1 P2 2.1580(7) 4_575 ?
P1 P2 2.1580(7) . ?
P1 C10 1.838(3) . ?
P1 C7 1.871(3) . ?
P6 P6 2.1576(9) 4_575 ?
P6 P5 2.1479(7) . ?
P2 P3 2.1461(8) . ?
P3 P3 2.1594(11) 4_575 ?
C14 C15 1.430(2) . ?
C14 C13 1.431(3) . ?
C14 C17 1.501(2) . ?
C3 C2 1.434(2) 4_575 ?
C3 C2 1.434(2) . ?
C3 C6 1.499(4) . ?
C15 C18 1.498(4) . ?
C2 C1 1.434(3) . ?
C2 C5 1.499(2) . ?
C1 C1 1.432(3) 4_575 ?
C1 C4 1.504(3) . ?
C13 C13 1.428(4) 4_575 ?
C13 C16 1.502(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C19 C21 1.528(4) . ?
C19 C20 1.535(2) . ?
C19 C20 1.535(2) 4_575 ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.519(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C7 C9 1.535(4) . ?
C7 C8 1.538(3) 4_575 ?
C7 C8 1.538(3) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.513(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.517(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C23 1.512(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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
Br1 C12 C11 C10 180.000(1) . . . . ?
Br2 C24 C23 C22 180.000(0) . . . . ?
Fe2 C14 C15 C14 -60.66(17) . . . 4_575 ?
Fe2 C14 C15 C18 121.4(3) . . . . ?
Fe2 C14 C13 C13 59.49(5) . . . 4_575 ?
Fe2 C14 C13 C16 -124.5(2) . . . . ?
Fe1 C3 C2 C1 -61.67(14) . . . . ?
Fe1 C3 C2 C5 121.7(2) . . . . ?
Fe1 C2 C1 C1 -59.32(5) . . . 4_575 ?
Fe1 C2 C1 C4 125.94(19) . . . . ?
P4 C22 C23 C24 180.000(0) . . . . ?
P1 C10 C11 C12 180.000(1) . . . . ?
P2 P1 C10 C11 51.87(3) . . . . ?
P2 P1 C10 C11 -51.87(3) 4_575 . . . ?
P2 P1 C7 C9 -60.43(6) . . . . ?
P2 P1 C7 C9 60.43(6) 4_575 . . . ?
P2 P1 C7 C8 179.88(14) 4_575 . . 4_575 ?
P2 P1 C7 C8 -179.88(14) . . . . ?
P2 P1 C7 C8 -59.0(2) 4_575 . . . ?
P2 P1 C7 C8 59.0(2) . . . 4_575 ?
P5 P4 C19 C21 60.65(5) . . . . ?
P5 P4 C19 C21 -60.65(5) 4_575 . . . ?
P5 P4 C19 C20 -58.6(2) . . . . ?
P5 P4 C19 C20 -179.94(13) 4_575 . . . ?
P5 P4 C19 C20 58.6(2) 4_575 . . 4_575 ?
P5 P4 C19 C20 179.94(13) . . . 4_575 ?
P5 P4 C22 C23 -52.63(3) . . . . ?
P5 P4 C22 C23 52.63(3) 4_575 . . . ?
C3 C2 C1 Fe1 59.85(15) . . . . ?
C3 C2 C1 C1 0.54(18) . . . 4_575 ?
C3 C2 C1 C4 -174.2(2) . . . . ?
C15 C14 C13 Fe2 -59.75(15) . . . . ?
C15 C14 C13 C13 -0.26(18) . . . 4_575 ?
C15 C14 C13 C16 175.8(2) . . . . ?
C2 C3 C2 Fe1 60.81(18) 4_575 . . . ?
C2 C3 C2 C1 -0.9(3) 4_575 . . . ?
C2 C3 C2 C5 -177.46(13) 4_575 . . . ?
C13 C14 C15 Fe2 61.07(14) . . . . ?
C13 C14 C15 C14 0.4(3) . . . 4_575 ?
C13 C14 C15 C18 -177.6(2) . . . . ?
C6 C3 C2 Fe1 -122.3(3) . . . . ?
C6 C3 C2 C1 176.1(2) . . . . ?
C6 C3 C2 C5 -0.5(4) . . . . ?
C19 P4 C22 C23 180.000(0) . . . . ?
C10 P1 C7 C9 180.000(1) . . . . ?
C10 P1 C7 C8 60.55(17) . . . . ?
C10 P1 C7 C8 -60.55(17) . . . 4_575 ?
C5 C2 C1 Fe1 -123.5(2) . . . . ?
C5 C2 C1 C1 177.18(16) . . . 4_575 ?
C5 C2 C1 C4 2.4(3) . . . . ?
C7 P1 C10 C11 180.000(1) . . . . ?
C17 C14 C15 Fe2 -123.78(19) . . . . ?
C17 C14 C15 C14 175.56(13) . . . 4_575 ?
C17 C14 C15 C18 -2.4(4) . . . . ?
C17 C14 C13 Fe2 125.2(2) . . . . ?
C17 C14 C13 C13 -175.31(16) . . . 4_575 ?
C17 C14 C13 C16 0.7(3) . . . . ?
C22 P4 C19 C21 180.000(0) . . . . ?
C22 P4 C19 C20 -60.71(16) . . . 4_575 ?
C22 P4 C19 C20 60.71(16) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-5.4647 -1.4285 -20.5933 -0.0253 -0.9956 0.0907
5.0104 9.0112 -21.0018 0.5719 -0.6197 -0.5340
5.8004 -1.7996 -25.2685 0.6437 -0.7523 0.1403
-5.7968 0.4763 25.4240 -0.6489 0.7586 -0.0584
4.9848 -8.0082 17.0313 0.0227 0.8422 0.4953
-4.0226 12.9999 16.0241 -0.3967 0.4624 -0.8244
8.9840 13.0070 -0.9556 0.5305 0.2985 -0.7865
14.0066 -0.9931 -16.9775 0.9786 -0.1262 0.1020
5.4127 2.1048 20.5240 0.0251 0.9908 -0.1327
-13.0004 -7.0098 15.9700 -0.9312 0.1264 0.3966
-5.0077 -10.0110 18.9978 -0.5477 0.5430 0.5972
2.0154 -16.0049 -5.0190 0.1347 -0.1147 0.9991
-12.0100 -2.0092 20.9863 -0.9316 0.3555 0.0856
-14.0089 3.9944 16.9810 -0.9711 0.1258 -0.2879
-15.7527 0.7465 5.4432 -0.9204 -0.3822 -0.0827
