#------------------------------------------------------------------------------
#$Date: 2021-07-05 19:17:08 +0300 (Mon, 05 Jul 2021) $
#$Revision: 267020 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/83/7128317.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_7128317
loop_
_publ_author_name
'Taher, Deeb'
'Wilson, Jessica R.'
'Ritch, Grayson'
'Zeller, Matthias'
'Szymczak, Nathaniel K.'
_publ_section_title
;
 Late-stage ligand functionalization via the Staudinger reaction
 using phosphine-appended 2,2'-bipyridine.
;
_journal_issue                   46
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5718
_journal_page_last               5721
_journal_paper_doi               10.1039/d1cc01407b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'C48 H34 Cl F6 Fe N4 P2, F6 P, 1.155(C4 H10 O), 0.734(C2 H3 N)'
_chemical_formula_sum            'C54.09 H47.75 Cl F12 Fe N4.73 O1.16 P3'
_chemical_formula_weight         1194.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-03-13 deposited with the CCDC.	2021-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.1160(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0420(2)
_cell_length_b                   18.7721(2)
_cell_length_c                   17.1927(2)
_cell_measurement_reflns_used    26681
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      69.0820
_cell_measurement_theta_min      3.5260
_cell_volume                     5394.50(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1005 (Hübschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
'Rigaku AFC10K Saturn 944+ CCD-based X-ray diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81879
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         69.327
_diffrn_reflns_theta_min         2.643
_diffrn_source                   'Cu-target micro-focus rotating anode'
_diffrn_source_type
'Micromax-007HF (Cu) micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    4.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63688
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       plate
_exptl_crystal_F_000             2442.6
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         10032
_refine_ls_number_restraints     427
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0441
_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)+(0.0681P)²+3.3905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9083
_reflns_number_total             10032
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc01407b2.cif
_cod_data_source_block           gr5174
_cod_depositor_comments
'Adding full bibliography for 7128313--7128317.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7128317
_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_min   0.605
_shelx_estimated_absorpt_t_max   0.699
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.31867(2) 0.55948(2) 0.31538(2) 0.02830(11) Uani 1 1 d . . . . .
Cl2 Cl 0.26892(3) 0.48466(3) 0.39415(3) 0.03432(14) Uani 1 1 d . . . . .
P1 P 0.32372(3) 0.43084(3) 0.20022(3) 0.02834(14) Uani 1 1 d . . . . .
P2 P 0.30315(3) 0.70672(4) 0.40032(4) 0.03040(15) Uani 1 1 d . . . . .
P3 P 0.48486(4) 0.65637(4) 0.21078(4) 0.03647(16) Uani 1 1 d . . . . .
F4 F -0.11623(9) 0.63354(11) 0.12555(13) 0.0638(5) Uani 1 1 d D . . . .
F5 F -0.10208(9) 0.74524(11) 0.10606(13) 0.0650(5) Uani 1 1 d D . . . .
F6 F -0.07994(10) 0.66680(11) 0.02642(11) 0.0651(5) Uani 1 1 d D . . . .
F7 F 0.53651(10) 0.67292(10) 0.30696(9) 0.0513(4) Uani 1 1 d . . . . .
F8 F 0.50376(9) 0.57350(9) 0.22684(10) 0.0453(4) Uani 1 1 d . . . . .
F9 F 0.43250(12) 0.64058(9) 0.11419(10) 0.0577(5) Uani 1 1 d . . . . .
F10 F 0.46598(11) 0.73981(9) 0.19455(10) 0.0522(4) Uani 1 1 d . . . . .
F11 F 0.40681(9) 0.64791(10) 0.23265(11) 0.0516(4) Uani 1 1 d . . . . .
F12 F 0.56220(12) 0.66618(11) 0.18857(13) 0.0645(5) Uani 1 1 d . . . . .
N1 N 0.42522(11) 0.49959(11) 0.33093(11) 0.0276(4) Uani 1 1 d . . . . .
N2 N 0.41673(11) 0.61373(11) 0.40896(11) 0.0283(4) Uani 1 1 d . . . . .
N3 N 0.28149(11) 0.50651(11) 0.19794(12) 0.0295(4) Uani 1 1 d . . . . .
N4 N 0.26042(11) 0.65697(11) 0.31974(12) 0.0306(4) Uani 1 1 d . . . . .
C1 C 0.42178(13) 0.44270(13) 0.28362(14) 0.0283(5) Uani 1 1 d . . . . .
C2 C 0.48770(14) 0.39974(14) 0.29562(15) 0.0325(5) Uani 1 1 d . . . . .
H2 H 0.483795 0.359009 0.261503 0.039 Uiso 1 1 calc R U . . .
C3 C 0.55999(14) 0.41827(15) 0.35945(15) 0.0339(5) Uani 1 1 d . . . . .
H3 H 0.606239 0.389779 0.369742 0.041 Uiso 1 1 calc R U . . .
C4 C 0.56412(13) 0.47813(14) 0.40760(14) 0.0319(5) Uani 1 1 d . . . . .
H4 H 0.613113 0.491675 0.450729 0.038 Uiso 1 1 calc R U . . .
C5 C 0.49512(13) 0.51816(13) 0.39167(13) 0.0280(5) Uani 1 1 d . . . . .
C6 C 0.49050(13) 0.58431(14) 0.43613(13) 0.0285(5) Uani 1 1 d . . . . .
C7 C 0.55486(14) 0.61608(14) 0.49973(14) 0.0321(5) Uani 1 1 d . . . . .
H7 H 0.606207 0.594395 0.519316 0.038 Uiso 1 1 calc R U . . .
C8 C 0.54284(14) 0.67938(15) 0.53371(14) 0.0342(5) Uani 1 1 d . . . . .
H8 H 0.586143 0.701757 0.576971 0.041 Uiso 1 1 calc R U . . .
C9 C 0.46729(14) 0.71066(15) 0.50474(14) 0.0338(5) Uani 1 1 d . . . . .
H9 H 0.458068 0.754636 0.526924 0.041 Uiso 1 1 calc R U . . .
C10 C 0.40601(14) 0.67522(14) 0.44229(14) 0.0312(5) Uani 1 1 d . . . . .
C11 C 0.27564(14) 0.35603(14) 0.22649(14) 0.0316(5) Uani 1 1 d . . . . .
C12 C 0.30971(15) 0.28805(15) 0.23724(15) 0.0378(6) Uani 1 1 d . . . . .
H12 H 0.359893 0.281012 0.232280 0.045 Uiso 1 1 calc R U . . .
C13 C 0.27000(16) 0.23088(16) 0.25518(17) 0.0427(6) Uani 1 1 d . . . . .
H13 H 0.293037 0.184637 0.262645 0.051 Uiso 1 1 calc R U . . .
C14 C 0.19675(17) 0.24128(17) 0.26221(18) 0.0486(7) Uani 1 1 d . . . . .
H14 H 0.169408 0.201964 0.273840 0.058 Uiso 1 1 calc R U . . .
C15 C 0.16309(16) 0.30872(17) 0.25237(18) 0.0447(7) Uani 1 1 d . . . . .
H15 H 0.113038 0.315581 0.257675 0.054 Uiso 1 1 calc R U . . .
C16 C 0.20258(14) 0.36614(15) 0.23476(15) 0.0366(6) Uani 1 1 d . . . . .
H16 H 0.179717 0.412410 0.228340 0.044 Uiso 1 1 calc R U . . .
C17 C 0.34208(14) 0.40718(14) 0.10780(14) 0.0321(5) Uani 1 1 d . . . . .
C18 C 0.39882(17) 0.44598(15) 0.08830(16) 0.0411(6) Uani 1 1 d . . . . .
H18 H 0.425945 0.484860 0.122592 0.049 Uiso 1 1 calc R U . . .
C19 C 0.41520(18) 0.42719(18) 0.01832(17) 0.0471(7) Uani 1 1 d . . . . .
H19 H 0.454579 0.452805 0.005500 0.056 Uiso 1 1 calc R U . . .
C20 C 0.37504(17) 0.37186(17) -0.03271(16) 0.0436(6) Uani 1 1 d . . . . .
H20 H 0.386893 0.359442 -0.080343 0.052 Uiso 1 1 calc R U . . .
C21 C 0.31767(16) 0.33448(16) -0.01481(17) 0.0420(6) Uani 1 1 d . . . . .
H21 H 0.289392 0.296834 -0.050638 0.050 Uiso 1 1 calc R U . . .
C22 C 0.30112(15) 0.35176(15) 0.05561(15) 0.0361(6) Uani 1 1 d . . . . .
H22 H 0.261824 0.325709 0.068084 0.043 Uiso 1 1 calc R U . . .
C23 C 0.26473(14) 0.69338(15) 0.48214(15) 0.0350(5) Uani 1 1 d . . . . .
C24 C 0.29428(15) 0.73194(15) 0.55702(15) 0.0361(6) Uani 1 1 d . . . . .
H24 H 0.329742 0.770773 0.562849 0.043 Uiso 1 1 calc R U . . .
C25 C 0.27149(17) 0.71313(16) 0.62296(16) 0.0415(6) Uani 1 1 d . . . . .
H25 H 0.291865 0.738887 0.674254 0.050 Uiso 1 1 calc R U . . .
C26 C 0.21913(18) 0.65693(17) 0.61421(18) 0.0465(7) Uani 1 1 d . . . . .
H26 H 0.203982 0.644165 0.659626 0.056 Uiso 1 1 calc R U . . .
C27 C 0.18891(18) 0.61945(18) 0.53980(19) 0.0492(7) Uani 1 1 d . . . . .
H27 H 0.152208 0.581592 0.533766 0.059 Uiso 1 1 calc R U . . .
C28 C 0.21201(16) 0.63693(16) 0.47365(17) 0.0417(6) Uani 1 1 d . . . . .
H28 H 0.191947 0.610510 0.422824 0.050 Uiso 1 1 calc R U . . .
C29 C 0.31182(14) 0.80045(15) 0.38481(14) 0.0348(5) Uani 1 1 d . . . . .
C30 C 0.36314(16) 0.82275(15) 0.34527(16) 0.0387(6) Uani 1 1 d . . . . .
H30 H 0.393715 0.788734 0.329242 0.046 Uiso 1 1 calc R U . . .
C31 C 0.36911(19) 0.89425(17) 0.32970(18) 0.0502(7) Uani 1 1 d . . . . .
H31 H 0.403386 0.909220 0.302305 0.060 Uiso 1 1 calc R U . . .
C32 C 0.3252(2) 0.94459(18) 0.3539(2) 0.0570(8) Uani 1 1 d . . . . .
H32 H 0.329428 0.993707 0.342877 0.068 Uiso 1 1 calc R U . . .
C33 C 0.2754(2) 0.92266(18) 0.3941(2) 0.0536(8) Uani 1 1 d . . . . .
H33 H 0.246141 0.956975 0.411458 0.064 Uiso 1 1 calc R U . . .
C34 C 0.26814(17) 0.85116(16) 0.40893(17) 0.0421(6) Uani 1 1 d . . . . .
H34 H 0.233232 0.836490 0.435699 0.051 Uiso 1 1 calc R U . . .
C35 C 0.21968(13) 0.53134(14) 0.12388(14) 0.0288(5) Uani 1 1 d . . . . .
C36 C 0.21309(13) 0.60470(14) 0.10885(14) 0.0303(5) Uani 1 1 d . . . . .
H36 H 0.250427 0.635997 0.147433 0.036 Uiso 1 1 calc R U . . .
C37 C 0.15317(14) 0.63246(15) 0.03879(15) 0.0333(5) Uani 1 1 d . . . . .
H37 H 0.148817 0.682502 0.029995 0.040 Uiso 1 1 calc R U . . .
C38 C 0.09918(13) 0.58676(15) -0.01887(15) 0.0336(5) Uani 1 1 d . . . . .
C39 C 0.10453(14) 0.51416(15) -0.00501(15) 0.0359(6) Uani 1 1 d . . . . .
H39 H 0.067406 0.483124 -0.044222 0.043 Uiso 1 1 calc R U . . .
C40 C 0.16396(14) 0.48636(15) 0.06602(15) 0.0336(5) Uani 1 1 d . . . . .
H40 H 0.166848 0.436389 0.075448 0.040 Uiso 1 1 calc R U . . .
C41 C 0.03730(15) 0.61677(16) -0.09681(16) 0.0398(6) Uani 0.464(11) 1 d D U P A
1
F1 F -0.0070(5) 0.5649(4) -0.1505(4) 0.0600(19) Uani 0.464(11) 1 d D U P A 1
F2 F -0.0192(3) 0.6513(5) -0.0787(3) 0.063(2) Uani 0.464(11) 1 d D U P A 1
F3 F 0.0639(3) 0.6581(4) -0.1390(4) 0.0557(19) Uani 0.464(11) 1 d D U P A 1
C41B C 0.03730(15) 0.61677(16) -0.09681(16) 0.0398(6) Uani 0.536(11) 1 d D U P
A 2
F1B F -0.0281(3) 0.5816(4) -0.1258(5) 0.071(2) Uani 0.536(11) 1 d D U P A 2
F2B F 0.0176(4) 0.6862(3) -0.0893(3) 0.0641(19) Uani 0.536(11) 1 d D U P A 2
F3B F 0.0658(3) 0.6218(5) -0.1590(3) 0.0668(17) Uani 0.536(11) 1 d D U P A 2
C42 C 0.17729(13) 0.66581(14) 0.26967(14) 0.0315(5) Uani 1 1 d . . . . .
C43 C 0.14351(14) 0.73154(15) 0.23969(16) 0.0361(6) Uani 1 1 d . . . . .
H43 H 0.175635 0.773219 0.255045 0.043 Uiso 1 1 calc R U . . .
C44 C 0.06271(15) 0.73740(16) 0.18710(17) 0.0416(6) Uani 1 1 d . . . . .
H44 H 0.040191 0.782685 0.166817 0.050 Uiso 1 1 calc R U . . .
C45 C 0.01610(14) 0.67679(16) 0.16501(16) 0.0393(6) Uani 1 1 d . . . . .
C46 C 0.04881(15) 0.61060(16) 0.19514(16) 0.0397(6) Uani 1 1 d . . . . .
H46 H 0.016362 0.569094 0.180257 0.048 Uiso 1 1 calc R U . . .
C47 C 0.12891(14) 0.60525(15) 0.24699(16) 0.0367(6) Uani 1 1 d . . . . .
H47 H 0.151121 0.559876 0.267291 0.044 Uiso 1 1 calc R U . . .
C48 C -0.06974(16) 0.68094(17) 0.1061(2) 0.0515(8) Uani 1 1 d D . . . .
O1 O -0.0206(2) 0.4136(2) 0.4149(2) 0.0691(9) Uani 0.728(2) 1 d D U P B 1
C49 C -0.0104(3) 0.4634(4) 0.3579(4) 0.0679(13) Uani 0.728(2) 1 d D U P B 1
H49A H 0.027031 0.444454 0.333097 0.081 Uiso 0.728(2) 1 calc R U P B 1
H49B H 0.011564 0.508650 0.387025 0.081 Uiso 0.728(2) 1 calc R U P B 1
C50 C -0.0926(3) 0.4758(4) 0.2896(4) 0.0834(17) Uani 0.728(2) 1 d D U P B 1
H50A H -0.127566 0.498766 0.314067 0.125 Uiso 0.728(2) 1 calc R U P B 1
H50B H -0.115846 0.429977 0.264908 0.125 Uiso 0.728(2) 1 calc R U P B 1
H50C H -0.087402 0.506509 0.245863 0.125 Uiso 0.728(2) 1 calc R U P B 1
C51 C 0.0491(4) 0.4025(4) 0.4827(4) 0.0858(17) Uani 0.728(2) 1 d D U P B 1
H51A H 0.068100 0.448616 0.511233 0.103 Uiso 0.728(2) 1 calc R U P B 1
H51B H 0.090359 0.384490 0.462726 0.103 Uiso 0.728(2) 1 calc R U P B 1
C52 C 0.0396(5) 0.3486(5) 0.5475(5) 0.100(3) Uani 0.728(2) 1 d D U P B 1
H52A H 0.021780 0.302490 0.519997 0.149 Uiso 0.728(2) 1 calc R U P B 1
H52B H -0.000097 0.366694 0.568779 0.149 Uiso 0.728(2) 1 calc R U P B 1
H52C H 0.091124 0.342683 0.594229 0.149 Uiso 0.728(2) 1 calc R U P B 1
N5 N 0.2690(4) 0.4577(3) 0.6585(4) 0.0699(14) Uani 0.573(3) 1 d D U P C 1
C53 C 0.2722(5) 0.4126(6) 0.6164(6) 0.0559(19) Uani 0.573(3) 1 d D U P C 1
C54 C 0.2729(8) 0.3553(8) 0.5626(9) 0.055(3) Uani 0.573(3) 1 d D U P C 1
H54A H 0.258728 0.373173 0.505269 0.083 Uiso 0.573(3) 1 calc R U P C 1
H54B H 0.233895 0.319207 0.563352 0.083 Uiso 0.573(3) 1 calc R U P C 1
H54C H 0.326389 0.334087 0.582162 0.083 Uiso 0.573(3) 1 calc R U P C 1
O2 O 0.2147(5) 0.4113(5) 0.6492(6) 0.0614(19) Uani 0.272(2) 1 d D U P B 2
C55 C 0.1949(9) 0.4718(7) 0.6826(8) 0.069(3) Uani 0.272(2) 1 d D U P B 2
H55A H 0.154679 0.499023 0.636599 0.082 Uiso 0.272(2) 1 calc R U P B 2
H55B H 0.243170 0.502028 0.706546 0.082 Uiso 0.272(2) 1 calc R U P B 2
C56 C 0.1622(10) 0.4579(8) 0.7492(9) 0.077(4) Uani 0.272(2) 1 d D U P B 2
H56A H 0.113630 0.428919 0.725923 0.115 Uiso 0.272(2) 1 calc R U P B 2
H56B H 0.149339 0.503312 0.769380 0.115 Uiso 0.272(2) 1 calc R U P B 2
H56C H 0.202208 0.432434 0.796044 0.115 Uiso 0.272(2) 1 calc R U P B 2
C57 C 0.2518(13) 0.4206(12) 0.5949(12) 0.061(3) Uani 0.272(2) 1 d D U P B 2
H57A H 0.306039 0.440218 0.625058 0.074 Uiso 0.272(2) 1 calc R U P B 2
H57B H 0.221341 0.455075 0.550927 0.074 Uiso 0.272(2) 1 calc R U P B 2
C58 C 0.258(2) 0.3473(19) 0.553(3) 0.065(6) Uani 0.272(2) 1 d D U P B 2
H58A H 0.272544 0.356035 0.504183 0.098 Uiso 0.272(2) 1 calc R U P B 2
H58B H 0.206578 0.322596 0.534853 0.098 Uiso 0.272(2) 1 calc R U P B 2
H58C H 0.299397 0.317700 0.593728 0.098 Uiso 0.272(2) 1 calc R U P B 2
O3 O 0.1110(11) 0.3225(10) 0.5517(13) 0.098(4) Uani 0.155(2) 1 d D U P D 3
C59 C 0.1588(11) 0.3799(11) 0.5937(14) 0.062(3) Uani 0.155(2) 1 d D U P D 3
H59A H 0.165609 0.377658 0.653521 0.074 Uiso 0.155(2) 1 calc R U P D 3
H59B H 0.129683 0.424565 0.570251 0.074 Uiso 0.155(2) 1 calc R U P D 3
C60 C 0.2403(14) 0.3841(19) 0.589(2) 0.072(5) Uani 0.155(2) 1 d D U P D 3
H60A H 0.234613 0.390466 0.530645 0.108 Uiso 0.155(2) 1 calc R U P D 3
H60B H 0.269694 0.339999 0.611324 0.108 Uiso 0.155(2) 1 calc R U P D 3
H60C H 0.269644 0.424610 0.622681 0.108 Uiso 0.155(2) 1 calc R U P D 3
C61 C 0.0306(14) 0.335(3) 0.5238(18) 0.091(5) Uani 0.155(2) 1 d D U P D 3
H61A H 0.000711 0.298776 0.481975 0.109 Uiso 0.155(2) 1 calc R U P D 3
H61B H 0.017782 0.382772 0.497494 0.109 Uiso 0.155(2) 1 calc R U P D 3
C62 C 0.0086(15) 0.3309(16) 0.6034(17) 0.079(6) Uani 0.155(2) 1 d D U P D 3
H62A H -0.049448 0.326073 0.586059 0.118 Uiso 0.155(2) 1 calc R U P D 3
H62B H 0.026510 0.374421 0.636671 0.118 Uiso 0.155(2) 1 calc R U P D 3
H62C H 0.035104 0.289553 0.637278 0.118 Uiso 0.155(2) 1 calc R U P D 3
N6 N -0.0574(14) 0.3994(14) 0.3486(17) 0.090(5) Uani 0.161(6) 1 d D U P E 2
C63 C 0.0039(15) 0.4263(17) 0.370(2) 0.079(4) Uani 0.161(6) 1 d D U P E 2
C64 C 0.0673(15) 0.4717(15) 0.394(2) 0.087(6) Uani 0.161(6) 1 d D U P E 2
H64A H 0.055305 0.511999 0.354764 0.130 Uiso 0.161(6) 1 calc R U P E 2
H64B H 0.114690 0.446539 0.393148 0.130 Uiso 0.161(6) 1 calc R U P E 2
H64C H 0.077592 0.489155 0.450591 0.130 Uiso 0.161(6) 1 calc R U P E 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Cl Cl 0.3639 0.7018 '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'
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 N4 117.00(7) . . ?
N3 Fe1 N2 144.28(7) . . ?
N4 Fe1 N2 81.03(7) . . ?
N3 Fe1 N1 79.70(7) . . ?
N4 Fe1 N1 150.99(8) . . ?
N2 Fe1 N1 73.12(7) . . ?
N3 Fe1 Cl2 102.47(6) . . ?
N4 Fe1 Cl2 101.12(6) . . ?
N2 Fe1 Cl2 103.72(5) . . ?
N1 Fe1 Cl2 97.65(5) . . ?
N3 P1 C11 115.36(11) . . ?
N3 P1 C17 116.17(11) . . ?
C11 P1 C17 107.25(12) . . ?
N3 P1 C1 102.84(10) . . ?
C11 P1 C1 108.37(10) . . ?
C17 P1 C1 106.16(11) . . ?
N4 P2 C29 118.82(11) . . ?
N4 P2 C23 113.01(12) . . ?
C29 P2 C23 109.42(12) . . ?
N4 P2 C10 103.87(11) . . ?
C29 P2 C10 104.17(12) . . ?
C23 P2 C10 106.24(11) . . ?
F12 P3 F7 90.20(10) . . ?
F12 P3 F8 90.27(10) . . ?
F7 P3 F8 90.41(9) . . ?
F12 P3 F11 179.03(12) . . ?
F7 P3 F11 89.89(9) . . ?
F8 P3 F11 90.70(9) . . ?
F12 P3 F9 90.05(11) . . ?
F7 P3 F9 179.36(12) . . ?
F8 P3 F9 90.18(9) . . ?
F11 P3 F9 89.86(10) . . ?
F12 P3 F10 89.62(11) . . ?
F7 P3 F10 89.60(10) . . ?
F8 P3 F10 179.89(11) . . ?
F11 P3 F10 89.42(10) . . ?
F9 P3 F10 89.81(9) . . ?
C1 N1 C5 119.8(2) . . ?
C1 N1 Fe1 120.60(15) . . ?
C5 N1 Fe1 119.53(16) . . ?
C10 N2 C6 119.2(2) . . ?
C10 N2 Fe1 121.34(15) . . ?
C6 N2 Fe1 119.43(16) . . ?
C35 N3 P1 121.21(16) . . ?
C35 N3 Fe1 124.09(16) . . ?
P1 N3 Fe1 114.49(10) . . ?
C42 N4 P2 120.36(17) . . ?
C42 N4 Fe1 119.94(16) . . ?
P2 N4 Fe1 116.60(10) . . ?
N1 C1 C2 122.4(2) . . ?
N1 C1 P1 112.77(16) . . ?
C2 C1 P1 124.74(19) . . ?
C1 C2 C3 117.9(2) . . ?
C1 C2 H2 121.1 . . ?
C3 C2 H2 121.1 . . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 118.7(2) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 121.4(2) . . ?
N1 C5 C6 113.60(19) . . ?
C4 C5 C6 125.0(2) . . ?
N2 C6 C7 121.1(2) . . ?
N2 C6 C5 113.88(19) . . ?
C7 C6 C5 125.0(2) . . ?
C8 C7 C6 119.0(2) . . ?
C8 C7 H7 120.5 . . ?
C6 C7 H7 120.5 . . ?
C7 C8 C9 120.1(2) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 117.5(2) . . ?
C10 C9 H9 121.2 . . ?
C8 C9 H9 121.2 . . ?
N2 C10 C9 123.0(2) . . ?
N2 C10 P2 113.71(16) . . ?
C9 C10 P2 123.2(2) . . ?
C16 C11 C12 119.8(2) . . ?
C16 C11 P1 119.0(2) . . ?
C12 C11 P1 121.13(19) . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.4(3) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C16 119.9(3) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C11 120.0(3) . . ?
C15 C16 H16 120.0 . . ?
C11 C16 H16 120.0 . . ?
C22 C17 C18 119.7(2) . . ?
C22 C17 P1 121.69(19) . . ?
C18 C17 P1 118.64(19) . . ?
C19 C18 C17 119.3(3) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 120.8(3) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C19 C20 C21 120.1(3) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C22 120.1(3) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C17 120.0(2) . . ?
C21 C22 H22 120.0 . . ?
C17 C22 H22 120.0 . . ?
C28 C23 C24 119.9(2) . . ?
C28 C23 P2 118.10(19) . . ?
C24 C23 P2 121.4(2) . . ?
C25 C24 C23 119.5(3) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C26 C25 C24 120.3(3) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C27 C26 C25 120.3(3) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C26 C27 C28 120.2(3) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C27 C28 C23 119.8(3) . . ?
C27 C28 H28 120.1 . . ?
C23 C28 H28 120.1 . . ?
C34 C29 C30 119.3(3) . . ?
C34 C29 P2 122.3(2) . . ?
C30 C29 P2 118.3(2) . . ?
C31 C30 C29 119.9(3) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 120.5(3) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C33 C32 C31 119.7(3) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C34 C33 C32 120.3(3) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C29 120.3(3) . . ?
C33 C34 H34 119.9 . . ?
C29 C34 H34 119.9 . . ?
C36 C35 C40 118.3(2) . . ?
C36 C35 N3 118.2(2) . . ?
C40 C35 N3 123.4(2) . . ?
C37 C36 C35 121.1(2) . . ?
C37 C36 H36 119.4 . . ?
C35 C36 H36 119.4 . . ?
C36 C37 C38 119.7(2) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C39 C38 C37 120.0(2) . . ?
C39 C38 C41B 120.5(2) . . ?
C37 C38 C41B 119.5(2) . . ?
C39 C38 C41 120.5(2) . . ?
C37 C38 C41 119.5(2) . . ?
C38 C39 C40 120.2(2) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C39 C40 C35 120.6(2) . . ?
C39 C40 H40 119.7 . . ?
C35 C40 H40 119.7 . . ?
F3 C41 F2 108.6(4) . . ?
F3 C41 F1 107.4(4) . . ?
F2 C41 F1 101.4(4) . . ?
F3 C41 C38 115.2(3) . . ?
F2 C41 C38 110.6(3) . . ?
F1 C41 C38 112.6(4) . . ?
F1B C41B F3B 107.3(4) . . ?
F1B C41B F2B 107.1(4) . . ?
F3B C41B F2B 101.3(4) . . ?
F1B C41B C38 115.0(4) . . ?
F3B C41B C38 110.9(3) . . ?
F2B C41B C38 114.0(3) . . ?
C43 C42 C47 118.7(2) . . ?
C43 C42 N4 122.8(2) . . ?
C47 C42 N4 118.5(2) . . ?
C42 C43 C44 121.0(3) . . ?
C42 C43 H43 119.5 . . ?
C44 C43 H43 119.5 . . ?
C45 C44 C43 119.4(3) . . ?
C45 C44 H44 120.3 . . ?
C43 C44 H44 120.3 . . ?
C44 C45 C46 120.4(2) . . ?
C44 C45 C48 120.7(3) . . ?
C46 C45 C48 118.9(3) . . ?
C47 C46 C45 119.9(3) . . ?
C47 C46 H46 120.1 . . ?
C45 C46 H46 120.1 . . ?
C46 C47 C42 120.7(3) . . ?
C46 C47 H47 119.6 . . ?
C42 C47 H47 119.6 . . ?
F6 C48 F5 106.6(3) . . ?
F6 C48 F4 105.3(2) . . ?
F5 C48 F4 106.5(2) . . ?
F6 C48 C45 112.9(2) . . ?
F5 C48 C45 112.7(2) . . ?
F4 C48 C45 112.3(3) . . ?
C51 O1 C49 111.9(5) . . ?
O1 C49 C50 106.9(4) . . ?
O1 C49 H49A 110.3 . . ?
C50 C49 H49A 110.3 . . ?
O1 C49 H49B 110.3 . . ?
C50 C49 H49B 110.3 . . ?
H49A C49 H49B 108.6 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O1 C51 C52 113.1(6) . . ?
O1 C51 H51A 108.9 . . ?
C52 C51 H51A 108.9 . . ?
O1 C51 H51B 108.9 . . ?
C52 C51 H51B 108.9 . . ?
H51A C51 H51B 107.8 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N5 C53 C54 177.7(9) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C57 O2 C55 117.1(13) . . ?
O2 C55 C56 114.4(11) . . ?
O2 C55 H55A 108.7 . . ?
C56 C55 H55A 108.7 . . ?
O2 C55 H55B 108.7 . . ?
C56 C55 H55B 108.7 . . ?
H55A C55 H55B 107.6 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
O2 C57 C58 110(2) . . ?
O2 C57 H57A 109.6 . . ?
C58 C57 H57A 109.6 . . ?
O2 C57 H57B 109.6 . . ?
C58 C57 H57B 109.6 . . ?
H57A C57 H57B 108.2 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C61 O3 C59 114(2) . . ?
O3 C59 C60 116.0(19) . . ?
O3 C59 H59A 108.3 . . ?
C60 C59 H59A 108.3 . . ?
O3 C59 H59B 108.3 . . ?
C60 C59 H59B 108.3 . . ?
H59A C59 H59B 107.4 . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
O3 C61 C62 106(2) . . ?
O3 C61 H61A 110.6 . . ?
C62 C61 H61A 110.6 . . ?
O3 C61 H61B 110.6 . . ?
C62 C61 H61B 110.6 . . ?
H61A C61 H61B 108.8 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
N6 C63 C64 167(4) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 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 N3 2.120(2) . ?
Fe1 N4 2.126(2) . ?
Fe1 N2 2.1477(19) . ?
Fe1 N1 2.1549(19) . ?
Fe1 Cl2 2.3511(7) . ?
P1 N3 1.605(2) . ?
P1 C11 1.796(3) . ?
P1 C17 1.797(2) . ?
P1 C1 1.824(2) . ?
P2 N4 1.607(2) . ?
P2 C29 1.795(3) . ?
P2 C23 1.805(3) . ?
P2 C10 1.818(2) . ?
P3 F12 1.5899(18) . ?
P3 F7 1.5935(16) . ?
P3 F8 1.5943(18) . ?
P3 F11 1.5965(17) . ?
P3 F9 1.5989(16) . ?
P3 F10 1.6049(19) . ?
F4 C48 1.348(4) . ?
F5 C48 1.341(3) . ?
F6 C48 1.339(4) . ?
N1 C1 1.330(3) . ?
N1 C5 1.346(3) . ?
N2 C10 1.335(3) . ?
N2 C6 1.352(3) . ?
N3 C35 1.419(3) . ?
N4 C42 1.430(3) . ?
C1 C2 1.387(3) . ?
C2 C3 1.396(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.477(4) . ?
C6 C7 1.394(3) . ?
C7 C8 1.377(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.393(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(3) . ?
C9 H9 0.9500 . ?
C11 C16 1.391(4) . ?
C11 C12 1.398(4) . ?
C12 C13 1.388(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.387(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 C22 1.391(4) . ?
C17 C18 1.396(4) . ?
C18 C19 1.388(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.376(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.394(4) . ?
C23 C24 1.396(4) . ?
C24 C25 1.389(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.380(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.395(4) . ?
C29 C30 1.403(4) . ?
C30 C31 1.381(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.393(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.386(5) . ?
C32 H32 0.9500 . ?
C33 C34 1.382(4) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.398(4) . ?
C35 C40 1.400(3) . ?
C36 C37 1.382(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.393(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.381(4) . ?
C38 C41B 1.494(3) . ?
C38 C41 1.494(3) . ?
C39 C40 1.389(3) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 F3 1.273(6) . ?
C41 F2 1.340(5) . ?
C41 F1 1.372(6) . ?
C41B F1B 1.278(6) . ?
C41B F3B 1.352(5) . ?
C41B F2B 1.370(5) . ?
C42 C43 1.387(4) . ?
C42 C47 1.397(4) . ?
C43 C44 1.401(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.380(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.389(4) . ?
C45 C48 1.500(3) . ?
C46 C47 1.387(3) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
O1 C51 1.371(6) . ?
O1 C49 1.416(7) . ?
C49 C50 1.524(8) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.561(13) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
N5 C53 1.130(11) . ?
C53 C54 1.420(13) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
O2 C57 1.349(16) . ?
O2 C55 1.380(13) . ?
C55 C56 1.496(15) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C58 1.58(2) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
O3 C61 1.367(19) . ?
O3 C59 1.399(17) . ?
C59 C60 1.503(18) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.56(2) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
N6 C63 1.142(19) . ?
C63 C64 1.36(2) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
