#------------------------------------------------------------------------------
#$Date: 2022-02-19 01:15:19 +0200 (Sat, 19 Feb 2022) $
#$Revision: 273036 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/63/1566392.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_1566392
loop_
_publ_author_name
'Birchall, Lee'
'Truccolo, Giada'
'Jackson, Lewis'
'Shepherd, Helena Jane'
_publ_section_title
;
 Co-crystallisation as a Modular Approach to the Discovery of
 Spin-Crossover Materials
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04956A
_journal_year                    2022
_chemical_formula_moiety         'C22 H18 Fe N10, 2(F6 P), 2(C10 H8 N2)'
_chemical_formula_sum            'C42 H34 F12 Fe N14 P2'
_chemical_formula_weight         1080.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.4899(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9529(3)
_cell_length_b                   14.8247(3)
_cell_length_c                   21.0093(3)
_cell_measurement_reflns_used    6715
_cell_measurement_temperature    298.00(13)
_cell_measurement_theta_max      71.8650
_cell_measurement_theta_min      4.2000
_cell_volume                     4635.82(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -27.00  -2.00   1.00    1.00    --  -42.16 125.00-180.00   25
  2  ω    -87.00 -59.00   1.00    1.00    --  -42.16 125.00-180.00   28
  3  ω   -115.00 -19.00   1.00    1.00    --  -42.16 -38.00  60.00   96
  4  ω   -116.00 -18.00   1.00    1.00    --  -42.16 -38.00 150.00   98
  5  ω      2.00  80.00   1.00    1.00    --   42.16 -99.00  30.00   78
  6  ω     29.00  56.00   1.00    1.00    --   42.16-125.00 -30.00   27
  7  ω      3.00  46.00   1.00    1.00    --   42.16 -99.00 -60.00   43
  8  ω     31.00  82.00   1.00    4.00    --  103.72 -61.00  90.00   51
  9  ω     33.00  58.00   1.00    4.00    --  103.72-125.00 -90.00   25
 10  ω     64.00 107.00   1.00    4.00    --  103.72 -94.00  90.00   43
 11  ω     94.00 127.00   1.00    4.00    --  103.72 125.00  30.00   33
 12  ω     75.00 118.00   1.00    4.00    --  103.72-125.00 -90.00   43
 13  ω     39.00  66.00   1.00    4.00    --  103.72 -45.00 -60.00   27
 14  ω     37.00 118.00   1.00    4.00    --  103.72-125.00  60.00   81
 15  ω     75.00 137.00   1.00    4.00    --  103.72  61.00  90.00   62
 16  ω     97.00 166.00   1.00    4.00    --  103.72 125.00-180.00   69
 17  ω    119.00 177.00   1.00    4.00    --  103.72 125.00 -60.00   58
 18  ω     44.00 116.00   1.00    4.00    --  103.72 -30.00-150.00   72
 19  ω    107.00 133.00   1.00    4.00    --  103.72 -61.00  90.00   26
 20  ω     30.00 117.00   1.00    4.00    --  103.72 -77.00-120.00   87
 21  ω     51.00 178.00   1.00    4.00    --  103.72  15.00-150.00  127
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0445973000
_diffrn_orient_matrix_UB_12      -0.0775932000
_diffrn_orient_matrix_UB_13      -0.0402356000
_diffrn_orient_matrix_UB_21      0.0075887000
_diffrn_orient_matrix_UB_22      -0.0611760000
_diffrn_orient_matrix_UB_23      0.0595574000
_diffrn_orient_matrix_UB_31      -0.0930664000
_diffrn_orient_matrix_UB_32      0.0321731000
_diffrn_orient_matrix_UB_33      0.0162513000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17455
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.043
_diffrn_reflns_theta_min         4.209
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.138
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4687
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0623
_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)+(0.1351P)²+2.5431P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.1981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4072
_reflns_number_total             4687
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-97-002r_298_red_ref
_cod_original_cell_volume        4635.81(15)
_cod_database_code               1566392
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 P2 F12 N14'
_chemical_oxdiff_usercomment     '298 K Red crystal'
_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.
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid body (RIGU) restrains
 P2, F6, F5, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, F3, F2, F1, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), N8(H8), C5(H5), C6(H6), C13(H13), C2(H2), C1(H1A), C11(H11),
 C8(H8A), C12(H12), C16(H16), C17(H17), C7(H7), C19(H19), C22(H22), C18(H18),
 C23(H23), C26(H26), C27(H27), C24(H24), C25(H25)
;
_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 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.872
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Fe1 Fe 0.75911(4) 0.5000 0.25370(3) 0.0478(2) Uani 1 2 d S T P . .
P1 P 0.25307(10) 0.5000 0.12275(7) 0.0847(5) Uani 1 2 d S TU P . .
P2 P 0.5000 0.21975(10) 0.5000 0.0918(6) Uani 1 2 d S TU P . .
N3 N 0.6837(2) 0.5000 0.32220(14) 0.0471(7) Uani 1 2 d S T P . .
F6 F 0.5000 0.1139(2) 0.5000 0.0971(11) Uani 1 2 d S TU P . .
N6 N 0.8345(2) 0.5000 0.18557(16) 0.0520(8) Uani 1 2 d S T P . .
N2 N 0.74340(17) 0.63130(19) 0.26529(12) 0.0560(6) Uani 1 1 d . . . . .
F5 F 0.4231(2) 0.21986(18) 0.54705(16) 0.1174(12) Uani 1 1 d . U . . .
N7 N 0.8783(2) 0.5000 0.30276(16) 0.0568(8) Uani 1 2 d S T P . .
N5 N 0.6677(2) 0.5000 0.17995(16) 0.0567(8) Uani 1 2 d S T P . .
N1 N 0.76280(19) 0.7084(2) 0.23631(13) 0.0632(7) Uani 1 1 d . . . . .
H1 H 0.7967 0.7121 0.2056 0.076 Uiso 1 1 calc R U . . .
F7 F 0.5000 0.3278(2) 0.5000 0.144(2) Uani 1 2 d S TU P . .
N4 N 0.5776(3) 0.5000 0.16904(18) 0.0679(11) Uani 1 2 d S T P . .
H4 H 0.5415 0.5000 0.1985 0.081 Uiso 1 2 calc R U P . .
C4 C 0.65678(19) 0.5785(2) 0.34564(13) 0.0509(6) Uani 1 1 d . . . . .
N8 N 0.9132(3) 0.5000 0.36440(18) 0.0693(11) Uani 1 2 d S T P . .
H8 H 0.8818 0.5000 0.3966 0.083 Uiso 1 2 calc R U P . .
C14 C 0.9242(3) 0.5000 0.1989(2) 0.0556(9) Uani 1 2 d S T P . .
C3 C 0.6897(2) 0.6547(2) 0.31051(14) 0.0551(7) Uani 1 1 d . . . . .
C15 C 0.9491(3) 0.5000 0.2680(2) 0.0586(10) Uani 1 2 d S T P . .
F8 F 0.5745(3) 0.2191(3) 0.55967(19) 0.1370(12) Uani 1 1 d . U . . .
C10 C 0.7965(3) 0.5000 0.12431(19) 0.0602(11) Uani 1 2 d S T P . .
C9 C 0.6990(3) 0.5000 0.1218(2) 0.0636(11) Uani 1 2 d S T P . .
C5 C 0.6034(2) 0.5807(2) 0.39607(14) 0.0579(7) Uani 1 1 d . . . . .
H5 H 0.5855 0.6352 0.4126 0.069 Uiso 1 1 calc R U . . .
N9 N 0.8040(3) 0.5000 0.4700(2) 0.0914(17) Uani 1 2 d S T P . .
N10 N 0.5391(3) 0.5000 0.7334(2) 0.0919(18) Uani 1 2 d S T P . .
N11 N 0.6178(3) 0.2268(3) 0.86144(18) 0.0900(11) Uani 1 1 d . . . . .
C28 C 0.5249(3) 0.2386(2) 0.97091(17) 0.0696(9) Uani 1 1 d . . . . .
C6 C 0.5778(3) 0.5000 0.4210(2) 0.0598(11) Uani 1 2 d S T P . .
H6 H 0.5427 0.5000 0.4552 0.072 Uiso 1 2 calc R U P . .
F1 F 0.2119(4) 0.5000 0.1894(2) 0.1465(19) Uani 1 2 d S TU P . .
C13 C 0.9807(3) 0.5000 0.1502(2) 0.0659(12) Uani 1 2 d S T P . .
H13 H 1.0428 0.5000 0.1596 0.079 Uiso 1 2 calc R U P . .
C20 C 0.7063(3) 0.5000 0.5774(2) 0.0693(14) Uani 1 2 d S T P . .
C21 C 0.6498(3) 0.5000 0.6327(2) 0.0732(15) Uani 1 2 d S T P . .
C2 C 0.6747(3) 0.7473(3) 0.30964(18) 0.0692(9) Uani 1 1 d . . . . .
H2 H 0.6401 0.7803 0.3358 0.083 Uiso 1 1 calc R U . . .
C1 C 0.7224(3) 0.7795(3) 0.26154(18) 0.0719(9) Uani 1 1 d . . . . .
H1A H 0.7261 0.8393 0.2488 0.086 Uiso 1 1 calc R U . . .
C11 C 0.8517(4) 0.5000 0.0743(2) 0.0730(14) Uani 1 2 d S T P . .
H11 H 0.8265 0.5000 0.0321 0.088 Uiso 1 2 calc R U P . .
C8 C 0.6279(4) 0.5000 0.0744(2) 0.0831(16) Uani 1 2 d S T P . .
H8A H 0.6308 0.5000 0.0304 0.100 Uiso 1 2 calc R U P . .
C12 C 0.9430(4) 0.5000 0.0878(2) 0.0712(13) Uani 1 2 d S T P . .
H12 H 0.9798 0.5000 0.0546 0.085 Uiso 1 2 calc R U P . .
C16 C 1.0290(3) 0.5000 0.3077(3) 0.0753(14) Uani 1 2 d S T P . .
H16 H 1.0873 0.5000 0.2957 0.090 Uiso 1 2 calc R U P . .
F4 F 0.3240(3) 0.4286(4) 0.1527(2) 0.1742(19) Uani 1 1 d . U . . .
C17 C 1.0027(4) 0.5000 0.3688(3) 0.0865(18) Uani 1 2 d S T P . .
H17 H 1.0407 0.5000 0.4065 0.104 Uiso 1 2 calc R U P . .
C7 C 0.5516(4) 0.5000 0.1068(2) 0.0852(17) Uani 1 2 d S T P . .
H7 H 0.4926 0.5000 0.0883 0.102 Uiso 1 2 calc R U P . .
C19 C 0.7309(3) 0.4201(4) 0.54956(19) 0.0924(14) Uani 1 1 d . . . . .
H19 H 0.7150 0.3648 0.5660 0.111 Uiso 1 1 calc R U . . .
C22 C 0.6213(3) 0.4206(4) 0.65898(19) 0.0871(13) Uani 1 1 d . . . . .
H22 H 0.6386 0.3653 0.6432 0.105 Uiso 1 1 calc R U . . .
C18 C 0.7798(3) 0.4242(4) 0.4967(2) 0.0958(15) Uani 1 1 d . . . . .
H18 H 0.7966 0.3701 0.4789 0.115 Uiso 1 1 calc R U . . .
C23 C 0.5670(3) 0.4238(4) 0.7088(2) 0.0975(16) Uani 1 1 d . . . . .
H23 H 0.5492 0.3695 0.7259 0.117 Uiso 1 1 calc R U . . .
C26 C 0.4810(4) 0.2403(4) 0.9097(2) 0.0950(14) Uani 1 1 d . . . . .
H26 H 0.4187 0.2453 0.9040 0.114 Uiso 1 1 calc R U . . .
F2 F 0.1804(3) 0.4343(5) 0.0990(3) 0.237(3) Uani 1 1 d . U . . .
C27 C 0.6165(3) 0.2277(5) 0.9751(3) 0.120(2) Uani 1 1 d . . . . .
H27 H 0.6498 0.2242 1.0148 0.144 Uiso 1 1 calc R U . . .
C24 C 0.5299(4) 0.2345(4) 0.8571(2) 0.1017(15) Uani 1 1 d . . . . .
H24 H 0.4989 0.2360 0.8166 0.122 Uiso 1 1 calc R U . . .
C25 C 0.6585(4) 0.2222(5) 0.9194(3) 0.124(2) Uani 1 1 d . . . . .
H25 H 0.7205 0.2145 0.9233 0.149 Uiso 1 1 calc R U . . .
F3 F 0.2938(4) 0.5000 0.0616(3) 0.263(5) Uani 1 2 d S TU P . .
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
Fe Fe -1.1336 3.1974 '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 8 -4 0.1162
0 8 -8 0.1215
8 2 -8 0.1158
-9 3 3 0.1466
7 3 7 0.0387
7 3 8 0.0392
9 -3 -4 0.1497
-9 -1 7 0.1348
2 -8 6 0.1131
3 -8 5 0.1071
-9 -1 -3 0.1084
-6 -4 -9 0.0849
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
N3 Fe1 N2 79.74(7) . 6_565 ?
N3 Fe1 N2 79.74(7) . . ?
N3 Fe1 N7 100.08(13) . . ?
N3 Fe1 N5 100.23(14) . . ?
N6 Fe1 N3 179.86(15) . . ?
N6 Fe1 N2 100.27(7) . . ?
N6 Fe1 N2 100.27(7) . 6_565 ?
N6 Fe1 N7 79.78(14) . . ?
N6 Fe1 N5 79.91(15) . . ?
N2 Fe1 N2 159.38(14) . 6_565 ?
N7 Fe1 N2 92.73(8) . 6_565 ?
N7 Fe1 N2 92.73(8) . . ?
N5 Fe1 N2 90.87(8) . 6_565 ?
N5 Fe1 N2 90.87(8) . . ?
N5 Fe1 N7 159.69(14) . . ?
F1 P1 F4 87.2(3) . 6_565 ?
F1 P1 F4 87.2(3) . . ?
F4 P1 F4 83.8(4) . 6_565 ?
F2 P1 F1 87.9(3) . . ?
F2 P1 F1 88.0(3) 6_565 . ?
F2 P1 F4 174.8(3) . 6_565 ?
F2 P1 F4 174.8(3) 6_565 . ?
F2 P1 F4 97.7(4) 6_565 6_565 ?
F2 P1 F4 97.7(4) . . ?
F2 P1 F2 80.4(6) . 6_565 ?
F3 P1 F1 178.5(4) . . ?
F3 P1 F4 91.7(3) . . ?
F3 P1 F4 91.7(3) . 6_565 ?
F3 P1 F2 93.2(3) . . ?
F3 P1 F2 93.2(3) . 6_565 ?
F6 P2 F5 90.06(11) . . ?
F6 P2 F5 90.06(11) . 2_656 ?
F6 P2 F7 180.0 . . ?
F6 P2 F8 89.68(15) . 2_656 ?
F6 P2 F8 89.68(15) . . ?
F5 P2 F5 179.9(2) 2_656 . ?
F5 P2 F7 89.94(11) 2_656 . ?
F5 P2 F7 89.94(11) . . ?
F5 P2 F8 90.2(2) 2_656 2_656 ?
F5 P2 F8 90.2(2) . . ?
F5 P2 F8 89.8(2) 2_656 . ?
F5 P2 F8 89.8(2) . 2_656 ?
F8 P2 F7 90.32(15) 2_656 . ?
F8 P2 F7 90.32(15) . . ?
F8 P2 F8 179.4(3) 2_656 . ?
C4 N3 Fe1 119.75(16) 6_565 . ?
C4 N3 Fe1 119.75(16) . . ?
C4 N3 C4 120.5(3) . 6_565 ?
C14 N6 Fe1 119.6(3) . . ?
C14 N6 C10 121.1(4) . . ?
C10 N6 Fe1 119.3(3) . . ?
N1 N2 Fe1 138.6(2) . . ?
N1 N2 C3 105.7(3) . . ?
C3 N2 Fe1 115.2(2) . . ?
N8 N7 Fe1 138.5(3) . . ?
C15 N7 Fe1 115.9(3) . . ?
C15 N7 N8 105.6(4) . . ?
N4 N5 Fe1 138.1(3) . . ?
N4 N5 C9 106.0(4) . . ?
C9 N5 Fe1 115.9(3) . . ?
N2 N1 H1 124.3 . . ?
N2 N1 C1 111.3(3) . . ?
C1 N1 H1 124.3 . . ?
N5 N4 H4 124.4 . . ?
C7 N4 N5 111.2(4) . . ?
C7 N4 H4 124.4 . . ?
N3 C4 C3 111.0(2) . . ?
N3 C4 C5 121.1(3) . . ?
C5 C4 C3 127.9(3) . . ?
N7 N8 H8 124.4 . . ?
C17 N8 N7 111.1(4) . . ?
C17 N8 H8 124.4 . . ?
N6 C14 C15 111.2(3) . . ?
N6 C14 C13 120.8(4) . . ?
C13 C14 C15 128.0(4) . . ?
N2 C3 C4 114.2(3) . . ?
N2 C3 C2 110.5(3) . . ?
C2 C3 C4 135.1(3) . . ?
N7 C15 C14 113.6(4) . . ?
N7 C15 C16 110.5(4) . . ?
C16 C15 C14 135.9(4) . . ?
N6 C10 C9 111.2(3) . . ?
N6 C10 C11 119.3(4) . . ?
C11 C10 C9 129.5(4) . . ?
N5 C9 C10 113.7(4) . . ?
N5 C9 C8 109.9(4) . . ?
C8 C9 C10 136.4(4) . . ?
C4 C5 H5 120.9 . . ?
C6 C5 C4 118.2(3) . . ?
C6 C5 H5 120.9 . . ?
C18 N9 C18 116.5(5) . 6_565 ?
C23 N10 C23 116.8(5) . 6_565 ?
C25 N11 C24 116.2(4) . . ?
C26 C28 C28 122.1(5) . 2_657 ?
C27 C28 C28 121.4(5) . 2_657 ?
C27 C28 C26 116.2(4) . . ?
C5 C6 C5 120.9(4) 6_565 . ?
C5 C6 H6 119.6 . . ?
C5 C6 H6 119.6 6_565 . ?
C14 C13 H13 120.7 . . ?
C12 C13 C14 118.6(5) . . ?
C12 C13 H13 120.7 . . ?
C19 C20 C21 121.2(2) . . ?
C19 C20 C21 121.2(2) 6_565 . ?
C19 C20 C19 117.4(5) 6_565 . ?
C22 C21 C20 121.7(3) 6_565 . ?
C22 C21 C20 121.7(3) . . ?
C22 C21 C22 116.5(5) . 6_565 ?
C3 C2 H2 127.5 . . ?
C1 C2 C3 104.9(3) . . ?
C1 C2 H2 127.5 . . ?
N1 C1 C2 107.5(3) . . ?
N1 C1 H1A 126.3 . . ?
C2 C1 H1A 126.3 . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(5) . . ?
C12 C11 H11 120.2 . . ?
C9 C8 H8A 127.5 . . ?
C7 C8 C9 105.0(4) . . ?
C7 C8 H8A 127.5 . . ?
C13 C12 H12 119.7 . . ?
C11 C12 C13 120.5(4) . . ?
C11 C12 H12 119.7 . . ?
C15 C16 H16 127.7 . . ?
C17 C16 C15 104.7(4) . . ?
C17 C16 H16 127.7 . . ?
N8 C17 C16 108.0(5) . . ?
N8 C17 H17 126.0 . . ?
C16 C17 H17 126.0 . . ?
N4 C7 C8 107.9(5) . . ?
N4 C7 H7 126.1 . . ?
C8 C7 H7 126.1 . . ?
C20 C19 H19 120.6 . . ?
C20 C19 C18 118.8(5) . . ?
C18 C19 H19 120.6 . . ?
C21 C22 H22 120.1 . . ?
C21 C22 C23 119.8(5) . . ?
C23 C22 H22 120.1 . . ?
N9 C18 C19 124.3(5) . . ?
N9 C18 H18 117.9 . . ?
C19 C18 H18 117.9 . . ?
N10 C23 C22 123.5(5) . . ?
N10 C23 H23 118.2 . . ?
C22 C23 H23 118.2 . . ?
C28 C26 H26 120.0 . . ?
C24 C26 C28 119.9(5) . . ?
C24 C26 H26 120.0 . . ?
C28 C27 H27 120.5 . . ?
C28 C27 C25 118.9(5) . . ?
C25 C27 H27 120.5 . . ?
N11 C24 C26 123.5(5) . . ?
N11 C24 H24 118.3 . . ?
C26 C24 H24 118.3 . . ?
N11 C25 C27 125.2(5) . . ?
N11 C25 H25 117.4 . . ?
C27 C25 H25 117.4 . . ?
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 N3 1.911(3) . ?
Fe1 N6 1.905(3) . ?
Fe1 N2 1.978(3) 6_565 ?
Fe1 N2 1.978(3) . ?
Fe1 N7 1.971(4) . ?
Fe1 N5 1.966(4) . ?
P1 F1 1.584(5) . ?
P1 F4 1.585(4) . ?
P1 F4 1.585(4) 6_565 ?
P1 F2 1.509(4) 6_565 ?
P1 F2 1.509(4) . ?
P1 F3 1.473(5) . ?
P2 F6 1.569(4) . ?
P2 F5 1.586(2) 2_656 ?
P2 F5 1.586(2) . ?
P2 F7 1.602(4) . ?
P2 F8 1.595(4) . ?
P2 F8 1.595(4) 2_656 ?
N3 C4 1.341(3) . ?
N3 C4 1.341(3) 6_565 ?
N6 C14 1.344(6) . ?
N6 C10 1.356(6) . ?
N2 N1 1.340(4) . ?
N2 C3 1.347(4) . ?
N7 N8 1.349(5) . ?
N7 C15 1.343(5) . ?
N5 N4 1.344(5) . ?
N5 C9 1.350(5) . ?
N1 H1 0.8600 . ?
N1 C1 1.348(5) . ?
N4 H4 0.8600 . ?
N4 C7 1.328(7) . ?
C4 C3 1.460(4) . ?
C4 C5 1.386(4) . ?
N8 H8 0.8600 . ?
N8 C17 1.332(7) . ?
C14 C15 1.463(6) . ?
C14 C13 1.388(5) . ?
C3 C2 1.391(5) . ?
C15 C16 1.390(7) . ?
C10 C9 1.454(7) . ?
C10 C11 1.396(6) . ?
C9 C8 1.386(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.375(4) . ?
N9 C18 1.322(6) 6_565 ?
N9 C18 1.322(6) . ?
N10 C23 1.327(6) 6_565 ?
N10 C23 1.327(6) . ?
N11 C24 1.314(7) . ?
N11 C25 1.309(7) . ?
C28 C28 1.491(6) 2_657 ?
C28 C26 1.387(6) . ?
C28 C27 1.374(6) . ?
C6 C5 1.375(4) 6_565 ?
C6 H6 0.9300 . ?
C13 H13 0.9300 . ?
C13 C12 1.377(7) . ?
C20 C21 1.501(6) . ?
C20 C19 1.386(6) . ?
C20 C19 1.386(6) 6_565 ?
C21 C22 1.385(5) . ?
C21 C22 1.385(5) 6_565 ?
C2 H2 0.9300 . ?
C2 C1 1.376(5) . ?
C1 H1A 0.9300 . ?
C11 H11 0.9300 . ?
C11 C12 1.367(8) . ?
C8 H8A 0.9300 . ?
C8 C7 1.382(8) . ?
C12 H12 0.9300 . ?
C16 H16 0.9300 . ?
C16 C17 1.378(7) . ?
C17 H17 0.9300 . ?
C7 H7 0.9300 . ?
C19 H19 0.9300 . ?
C19 C18 1.388(5) . ?
C22 H22 0.9300 . ?
C22 C23 1.385(5) . ?
C18 H18 0.9300 . ?
C23 H23 0.9300 . ?
C26 H26 0.9300 . ?
C26 C24 1.385(6) . ?
C27 H27 0.9300 . ?
C27 C25 1.383(6) . ?
C24 H24 0.9300 . ?
C25 H25 0.9300 . ?
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 N3 C4 C3 2.2(4) . . . . ?
Fe1 N3 C4 C5 -178.8(2) . . . . ?
Fe1 N6 C14 C15 0.000(0) . . . . ?
Fe1 N6 C14 C13 180.000(0) . . . . ?
Fe1 N6 C10 C9 0.000(0) . . . . ?
Fe1 N6 C10 C11 180.000(0) . . . . ?
Fe1 N2 N1 C1 170.5(3) . . . . ?
Fe1 N2 C3 C4 3.5(3) . . . . ?
Fe1 N2 C3 C2 -173.0(2) . . . . ?
Fe1 N7 N8 C17 180.000(1) . . . . ?
Fe1 N7 C15 C14 0.000(1) . . . . ?
Fe1 N7 C15 C16 180.000(1) . . . . ?
Fe1 N5 N4 C7 180.000(0) . . . . ?
Fe1 N5 C9 C10 0.000(0) . . . . ?
Fe1 N5 C9 C8 180.000(0) . . . . ?
N3 C4 C3 N2 -3.6(4) . . . . ?
N3 C4 C3 C2 171.7(4) . . . . ?
N3 C4 C5 C6 -0.8(5) . . . . ?
N6 C14 C15 N7 0.000(1) . . . . ?
N6 C14 C15 C16 180.000(1) . . . . ?
N6 C14 C13 C12 0.000(1) . . . . ?
N6 C10 C9 N5 0.000(0) . . . . ?
N6 C10 C9 C8 180.000(0) . . . . ?
N6 C10 C11 C12 0.000(0) . . . . ?
N2 N1 C1 C2 0.4(4) . . . . ?
N2 C3 C2 C1 -0.2(4) . . . . ?
N7 N8 C17 C16 0.000(1) . . . . ?
N7 C15 C16 C17 0.000(1) . . . . ?
N5 N4 C7 C8 0.000(0) . . . . ?
N5 C9 C8 C7 0.000(0) . . . . ?
N1 N2 C3 C4 176.9(3) . . . . ?
N1 N2 C3 C2 0.4(4) . . . . ?
N4 N5 C9 C10 180.000(0) . . . . ?
N4 N5 C9 C8 0.000(0) . . . . ?
C4 N3 C4 C3 -176.5(2) 6_565 . . . ?
C4 N3 C4 C5 2.5(6) 6_565 . . . ?
C4 C3 C2 C1 -175.6(4) . . . . ?
C4 C5 C6 C5 -0.8(6) . . . 6_565 ?
N8 N7 C15 C14 180.000(0) . . . . ?
N8 N7 C15 C16 0.000(1) . . . . ?
C14 N6 C10 C9 180.000(0) . . . . ?
C14 N6 C10 C11 0.000(0) . . . . ?
C14 C15 C16 C17 180.000(1) . . . . ?
C14 C13 C12 C11 0.000(0) . . . . ?
C3 N2 N1 C1 -0.5(4) . . . . ?
C3 C4 C5 C6 178.0(3) . . . . ?
C3 C2 C1 N1 -0.1(4) . . . . ?
C15 N7 N8 C17 0.000(1) . . . . ?
C15 C14 C13 C12 180.000(0) . . . . ?
C15 C16 C17 N8 0.000(1) . . . . ?
C10 N6 C14 C15 180.000(0) . . . . ?
C10 N6 C14 C13 0.000(1) . . . . ?
C10 C9 C8 C7 180.000(0) . . . . ?
C10 C11 C12 C13 0.000(0) . . . . ?
C9 N5 N4 C7 0.000(0) . . . . ?
C9 C10 C11 C12 180.000(0) . . . . ?
C9 C8 C7 N4 0.000(0) . . . . ?
C5 C4 C3 N2 177.5(3) . . . . ?
C5 C4 C3 C2 -7.2(6) . . . . ?
C28 C28 C26 C24 -175.9(4) 2_657 . . . ?
C28 C28 C27 C25 175.7(5) 2_657 . . . ?
C28 C26 C24 N11 0.3(9) . . . . ?
C28 C27 C25 N11 0.3(11) . . . . ?
C13 C14 C15 N7 180.000(0) . . . . ?
C13 C14 C15 C16 0.000(1) . . . . ?
C20 C21 C22 C23 -178.0(4) . . . . ?
C20 C19 C18 N9 -0.9(7) . . . . ?
C21 C20 C19 C18 177.2(4) . . . . ?
C21 C22 C23 N10 0.5(7) . . . . ?
C11 C10 C9 N5 180.000(0) . . . . ?
C11 C10 C9 C8 0.000(0) . . . . ?
C19 C20 C21 C22 -1.1(7) 6_565 . . 6_565 ?
C19 C20 C21 C22 1.1(7) . . . . ?
C19 C20 C21 C22 177.0(4) 6_565 . . . ?
C19 C20 C21 C22 -177.0(4) . . . 6_565 ?
C19 C20 C19 C18 1.2(8) 6_565 . . . ?
C22 C21 C22 C23 0.1(7) 6_565 . . . ?
C18 N9 C18 C19 0.5(8) 6_565 . . . ?
C23 N10 C23 C22 -1.2(8) 6_565 . . . ?
C26 C28 C27 C25 2.0(9) . . . . ?
C27 C28 C26 C24 -2.3(8) . . . . ?
C24 N11 C25 C27 -2.3(10) . . . . ?
C25 N11 C24 C26 2.0(8) . . . . ?
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
-4.5131 7.9325 -3.7804 -0.2621 -0.7447 0.6138
0.4107 7.9836 -7.6125 -0.3315 -0.9387 0.0949
7.9486 2.2657 -8.1816 -0.2011 -0.5656 -0.7998
-9.2025 2.6344 3.4623 0.0667 -0.0248 0.9975
6.9680 3.1411 7.4041 -0.8524 0.3017 -0.4271
6.7620 3.2859 7.6492 -0.8643 0.3059 -0.3993
8.9476 -3.0328 -4.2866 0.0088 -0.0019 -1.0000
-8.6299 -0.6926 7.3066 0.1446 0.4120 0.8996
2.1191 -8.2921 5.9337 0.3102 0.8768 -0.3676
3.4379 -8.1850 4.8159 0.2880 0.8136 -0.5050
-9.2705 -0.5425 -2.7050 0.5644 -0.1983 0.8014
-5.5676 -4.0054 -8.8214 0.9140 -0.3226 0.2459
