#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:25:18 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263699 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/01/1560175.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_1560175
loop_
_publ_author_name
'Wang, Chi-Hsien'
'Chen, Kai-Jen'
'Wu, Tsung-Huan'
'Chang, Hung-Kai'
'Tsuchido, Yoshitaka'
'Sei, Yoshihisa'
'Chen, Pei-Lin'
'Horie, Masaki'
_publ_section_title
;
 Ring rotation of ferrocene in interlocked molecules in single crystals
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              3871
_journal_page_last               3875
_journal_paper_doi               10.1039/D0SC06876D
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C12 H16 Fe N, F6 P, C H2 Cl2, C20 H24 O6'
_chemical_formula_sum            'C33 H42 Cl2 F6 Fe N O6 P'
_chemical_formula_weight         820.39
_chemical_name_systematic
'[ferrocenylmethyl(methy) ammonium hexafluorophosphate][dibenzo[18]crown-6 ether]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-09-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-24 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                95.673(2)
_cell_angle_beta                 94.963(2)
_cell_angle_gamma                104.636(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6910(3)
_cell_length_b                   11.3787(3)
_cell_length_c                   16.6251(4)
_cell_measurement_reflns_used    15007
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      76.0400
_cell_measurement_theta_min      3.9880
_cell_volume                     1753.22(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      93
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -89.00   0.50    0.05    --  -46.57-153.00 141.00   52
  2  ω    -84.00 -55.00   0.50    0.05    --  -46.57-153.00 141.00   58
  3  ω   -133.00-108.00   0.50    0.05    -- -102.00-153.00 141.00   50
  4  ω   -173.00 -90.00   0.50    0.05    -- -102.00 -45.00 150.00  166
  5  ω    -22.00  12.00   0.50    0.05    --  -46.57  19.00 150.00   68
  6  ω    -23.00  28.00   0.50    0.05    --  -46.57  19.00  90.00  102
  7  ω    -60.00 -33.00   0.50    0.05    -- -102.00 121.00  23.00   54
  8  ω    -75.00 -30.00   0.50    0.05    -- -102.00 125.00  60.00   90
  9  ω    -71.00 -45.00   0.50    0.05    --  -46.57 121.00  23.00   52
 10  ω    -68.00 -36.00   0.50    0.05    -- -102.00  61.00  30.00   64
 11  ω    -64.00 -30.00   0.50    0.05    -- -102.00  61.00  60.00   68
 12  ω    -72.00 -32.00   0.50    0.05    -- -102.00  77.00 -30.00   80
 13  ω    -83.00 -58.00   0.50    0.05    --  -46.57 153.00-177.00   50
 14  ω    -54.00 -29.00   0.50    0.05    -- -102.00 153.00-177.00   50
 15  ω   -107.00 -37.00   0.50    0.05    -- -102.00 125.00 -30.00  140
 16  ω   -107.00 -65.00   0.50    0.05    -- -102.00 121.00  23.00   84
 17  ω   -112.00 -81.00   0.50    0.05    -- -102.00 125.00  60.00   62
 18  ω   -108.00 -45.00   0.50    0.05    -- -102.00 110.00 166.13  126
 19  ω   -124.00 -91.00   0.50    0.05    -- -102.00 -30.00   0.00   66
 20  ω   -159.00-133.00   0.50    0.05    -- -102.00 -30.00   0.00   52
 21  ω   -166.00 -89.00   0.50    0.05    -- -102.00 -15.00-120.00  154
 22  ω   -119.00 -37.00   0.50    0.05    --  -46.57 -77.00-150.00  164
 23  ω    -17.00  20.00   0.50    0.05    --  -46.57  19.00-180.00   74
 24  ω     31.00  87.00   0.50    0.05    --   46.57-121.00 -59.00  112
 25  ω     73.00  99.00   0.50    0.05    --  104.61-121.00 -59.00   52
 26  ω     32.00  57.00   0.50    0.05    --  104.61 -61.00-180.00   50
 27  ω     33.00 102.00   0.50    0.05    --  104.61-125.00-150.00  138
 28  ω     37.00  62.00   0.50    0.05    --  104.61 -61.00 -60.00   50
 29  ω    144.00 171.00   0.50    0.05    --  104.61  45.00   0.00   54
 30  ω    128.00 154.00   0.50    0.05    --  104.61 121.00  23.00   52
 31  ω     89.00 114.00   0.50    0.05    --  104.61 121.00  23.00   50
 32  ω     96.00 129.00   0.50    0.05    --  104.61  45.00   0.00   66
 33  ω     92.00 164.00   0.50    0.05    --  104.61  45.00 -60.00  144
 34  ω     98.00 124.00   0.50    0.05    --  104.61 153.00-177.00   52
 35  ω     60.00  88.00   0.50    0.05    --   46.57 153.00-177.00   56
 36  ω     35.00  69.00   0.50    0.05    --  104.61 -61.00  90.00   68
 37  ω     79.00 104.00   0.50    0.05    --  104.61 -77.00  90.00   50
 38  ω     73.00 108.00   0.50    0.05    --  104.61 -77.00 150.00   70
 39  ω     81.00 106.00   0.50    0.05    --  104.61-153.00 141.00   50
 40  ω     73.00  98.00   0.50    0.05    --   46.57-153.00 141.00   50
 41  ω     39.00  72.00   0.50    0.05    --  104.61 -77.00  90.00   66
 42  ω   -116.00 -88.00   0.50    0.05    --  -46.57-125.00-180.00   56
 43  ω   -147.00 -92.00   0.50    0.05    -- -102.00 -45.00-150.00  110
 44  ω   -120.00 -95.00   0.50    0.05    -- -102.00-121.00 -59.00   50
 45  ω   -108.00 -57.00   0.50    0.05    -- -102.00 115.00 -94.58  102
 46  ω   -125.00 -60.00   0.50    0.05    -- -102.00 153.00-177.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0644651000
_diffrn_orient_matrix_UB_12      -0.0483315000
_diffrn_orient_matrix_UB_13      -0.0886867000
_diffrn_orient_matrix_UB_21      -0.0934081000
_diffrn_orient_matrix_UB_22      -0.1156853000
_diffrn_orient_matrix_UB_23      0.0285566000
_diffrn_orient_matrix_UB_31      -0.1203355000
_diffrn_orient_matrix_UB_32      0.0646030000
_diffrn_orient_matrix_UB_33      0.0104203000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21543
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.316
_diffrn_reflns_theta_min         4.047
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.971
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, diethylether'
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.597
_refine_diff_density_min         -1.059
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0596
_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)+(0.1381P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6566
_reflns_number_total             7022
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc06876d3.cif
_cod_data_source_block           200317_horie_1_-180
_cod_depositor_comments
'Adding full bibliography for 1560152--1560177.cif.'
_cod_original_cell_volume        1753.22(8)
_cod_database_code               1560175
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20O8FePF6Cl
_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   0.460
_shelx_estimated_absorpt_t_min   0.215
_diffrn_oxdiff_digest_frames
;
01a9357df5f57df434707e553f0940fff3000524756
;
_diffrn_oxdiff_digest_hkl
;
0100c5c0fa17579dc290ff6c0d3136f8f7f07c
;
_reflns_odcompleteness_completeness 99.92
_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 C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C15(H15A,H15B), C27(H27A,H27B), C14(H14A,H14B), C43(H43A,H43B),
 C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C18(H18A,H18B), C17(H17A,H17B),
  C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C34(H34), C42(H42), C37(H37), C48(H48), C35(H35), C21(H21), C41(H41),
 C39(H39), C23(H23), C36(H36), C24(H24), C47(H47), C40(H40), C22(H22), C46(H46),
  C49(H49), C50(H50)
2.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
;
_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 4.988
_oxdiff_exptl_absorpt_empirical_full_min 0.496
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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 0.79121(4) 0.24813(3) 0.93117(2) 0.01198(14) Uani 1 1 d . . . . .
P2 P 0.71221(7) 0.76217(6) 0.77911(4) 0.01456(17) Uani 1 1 d . . . . .
Cl9 Cl 0.81914(9) 0.52029(7) 0.57020(5) 0.0320(2) Uani 1 1 d . . . . .
Cl11 Cl 1.03915(8) 0.52162(7) 0.70232(5) 0.0342(2) Uani 1 1 d . . . . .
F6 F 0.60665(18) 0.68857(15) 0.70004(10) 0.0224(4) Uani 1 1 d . . . . .
F4 F 0.6955(2) 0.88844(15) 0.74953(12) 0.0291(4) Uani 1 1 d . . . . .
F3 F 0.72838(19) 0.63496(15) 0.80717(10) 0.0242(4) Uani 1 1 d . . . . .
F8 F 0.84496(19) 0.76798(18) 0.72743(13) 0.0316(4) Uani 1 1 d . . . . .
O32 O 0.22642(19) 0.12183(16) 0.79964(10) 0.0137(4) Uani 1 1 d . . . . .
O19 O 0.31236(19) 0.08556(16) 0.51411(11) 0.0153(4) Uani 1 1 d . . . . .
O13 O 0.33503(19) 0.32472(15) 0.73905(11) 0.0135(4) Uani 1 1 d . . . . .
O29 O 0.30639(19) -0.08863(16) 0.74590(11) 0.0150(4) Uani 1 1 d . . . . .
F5 F 0.5772(2) 0.75413(19) 0.82874(11) 0.0316(4) Uani 1 1 d . . . . .
O16 O 0.48444(19) 0.31406(16) 0.60394(11) 0.0145(4) Uani 1 1 d . . . . .
O26 O 0.27002(19) -0.12185(16) 0.57570(11) 0.0157(4) Uani 1 1 d . . . . .
F7 F 0.8176(2) 0.83578(17) 0.85665(12) 0.0349(5) Uani 1 1 d . . . . .
N1 N 0.4952(2) 0.11832(18) 0.70483(13) 0.0127(4) Uani 1 1 d . . . . .
H1A H 0.411757 0.061278 0.696930 0.015 Uiso 1 1 calc R . . . .
H1B H 0.477735 0.189268 0.695734 0.015 Uiso 1 1 calc R . . . .
C38 C 0.6919(3) 0.2303(2) 0.81660(15) 0.0124(5) Uani 1 1 d . . . . .
C12 C 0.3174(2) 0.3370(2) 0.82081(15) 0.0125(5) Uani 1 1 d . . . . .
C34 C 0.2461(3) 0.2322(2) 0.93578(16) 0.0160(5) Uani 1 1 d . . . . .
H34 H 0.211592 0.160146 0.958134 0.019 Uiso 1 1 calc R . . . .
C33 C 0.2601(2) 0.2273(2) 0.85324(15) 0.0126(5) Uani 1 1 d . . . . .
C42 C 0.8373(3) 0.2223(2) 0.81462(15) 0.0145(5) Uani 1 1 d . . . . .
H42 H 0.865740 0.155996 0.790914 0.017 Uiso 1 1 calc R . . . .
C20 C 0.1993(3) -0.0077(2) 0.47621(15) 0.0135(5) Uani 1 1 d . . . . .
C37 C 0.3531(3) 0.4484(2) 0.87040(16) 0.0148(5) Uani 1 1 d . . . . .
H37 H 0.389093 0.520830 0.848771 0.018 Uiso 1 1 calc R . . . .
C48 C 0.9103(3) 0.2195(3) 1.03168(17) 0.0210(6) Uani 1 1 d . . . . .
H48 H 1.009410 0.248094 1.044124 0.025 Uiso 1 1 calc R . . . .
C15 C 0.4106(3) 0.4063(2) 0.61919(15) 0.0158(5) Uani 1 1 d . . . . .
H15A H 0.312718 0.377964 0.592823 0.019 Uiso 1 1 calc R . . . .
H15B H 0.457979 0.479809 0.597123 0.019 Uiso 1 1 calc R . . . .
C27 C 0.2282(3) -0.2258(2) 0.61866(16) 0.0171(5) Uani 1 1 d . . . . .
H27A H 0.243191 -0.297806 0.588150 0.020 Uiso 1 1 calc R . . . .
H27B H 0.127391 -0.241461 0.626300 0.020 Uiso 1 1 calc R . . . .
C14 C 0.4100(3) 0.4342(2) 0.70910(15) 0.0141(5) Uani 1 1 d . . . . .
H14A H 0.507681 0.461813 0.735737 0.017 Uiso 1 1 calc R . . . .
H14B H 0.362504 0.498558 0.720356 0.017 Uiso 1 1 calc R . . . .
C43 C 0.5588(3) 0.1285(2) 0.79205(16) 0.0150(5) Uani 1 1 d . . . . .
H43A H 0.487083 0.139647 0.827194 0.018 Uiso 1 1 calc R . . . .
H43B H 0.580588 0.051809 0.801058 0.018 Uiso 1 1 calc R . . . .
C35 C 0.2835(3) 0.3443(3) 0.98554(16) 0.0201(6) Uani 1 1 d . . . . .
H35 H 0.273842 0.346660 1.040797 0.024 Uiso 1 1 calc R . . . .
C21 C 0.1093(3) 0.0025(3) 0.40902(16) 0.0172(5) Uani 1 1 d . . . . .
H21 H 0.119850 0.077456 0.389060 0.021 Uiso 1 1 calc R . . . .
C28 C 0.3193(3) -0.1972(2) 0.69976(16) 0.0156(5) Uani 1 1 d . . . . .
H28A H 0.291206 -0.265532 0.730725 0.019 Uiso 1 1 calc R . . . .
H28B H 0.418959 -0.187590 0.691010 0.019 Uiso 1 1 calc R . . . .
C30 C 0.1657(3) -0.0950(2) 0.76839(17) 0.0168(5) Uani 1 1 d . . . . .
H30A H 0.126658 -0.172374 0.788430 0.020 Uiso 1 1 calc R . . . .
H30B H 0.102010 -0.088457 0.721679 0.020 Uiso 1 1 calc R . . . .
C41 C 0.9303(3) 0.3341(2) 0.85547(16) 0.0155(5) Uani 1 1 d . . . . .
H41 H 1.029986 0.353198 0.863462 0.019 Uiso 1 1 calc R . . . .
C45 C 0.5901(3) 0.0866(2) 0.64536(16) 0.0160(5) Uani 1 1 d . . . . .
H45A H 0.537961 0.066708 0.591899 0.024 Uiso 1 1 calc GR . . . .
H45B H 0.621946 0.017456 0.660073 0.024 Uiso 1 1 calc GR . . . .
H45C H 0.671815 0.155177 0.645708 0.024 Uiso 1 1 calc GR . . . .
C39 C 0.6970(3) 0.3481(2) 0.85859(16) 0.0155(5) Uani 1 1 d . . . . .
H39 H 0.618374 0.377811 0.868739 0.019 Uiso 1 1 calc R . . . .
C23 C -0.0131(3) -0.2117(3) 0.40084(17) 0.0204(6) Uani 1 1 d . . . . .
H23 H -0.082225 -0.280238 0.374666 0.024 Uiso 1 1 calc R . . . .
C36 C 0.3346(3) 0.4512(3) 0.95308(16) 0.0179(5) Uani 1 1 d . . . . .
H36 H 0.357022 0.525815 0.986215 0.022 Uiso 1 1 calc R . . . .
C31 C 0.1791(3) 0.0094(2) 0.83373(16) 0.0171(5) Uani 1 1 d . . . . .
H31A H 0.087149 0.004521 0.853909 0.021 Uiso 1 1 calc R . . . .
H31B H 0.247923 0.005731 0.878794 0.021 Uiso 1 1 calc R . . . .
C18 C 0.3404(3) 0.1967(2) 0.47847(16) 0.0182(5) Uani 1 1 d . . . . .
H18A H 0.264178 0.236515 0.486107 0.022 Uiso 1 1 calc R . . . .
H18B H 0.344556 0.179736 0.420526 0.022 Uiso 1 1 calc R . . . .
C24 C 0.0743(3) -0.2215(2) 0.46955(17) 0.0171(5) Uani 1 1 d . . . . .
H24 H 0.062117 -0.296287 0.489834 0.020 Uiso 1 1 calc R . . . .
C47 C 0.8075(3) 0.2813(3) 1.05570(17) 0.0232(6) Uani 1 1 d . . . . .
H47 H 0.827486 0.357633 1.086527 0.028 Uiso 1 1 calc R . . . .
C40 C 0.8437(3) 0.4112(2) 0.88187(16) 0.0160(5) Uani 1 1 d . . . . .
H40 H 0.877466 0.489817 0.909702 0.019 Uiso 1 1 calc R . . . .
C17 C 0.4820(3) 0.2789(2) 0.51890(16) 0.0173(5) Uani 1 1 d . . . . .
H17A H 0.556408 0.237014 0.511099 0.021 Uiso 1 1 calc R . . . .
H17B H 0.504894 0.352167 0.492086 0.021 Uiso 1 1 calc R . . . .
C25 C 0.1795(3) -0.1198(2) 0.50789(15) 0.0138(5) Uani 1 1 d . . . . .
C22 C 0.0031(3) -0.1000(3) 0.37159(17) 0.0210(6) Uani 1 1 d . . . . .
H22 H -0.057285 -0.093155 0.326662 0.025 Uiso 1 1 calc R . . . .
C46 C 0.6690(3) 0.2063(3) 1.02448(18) 0.0264(6) Uani 1 1 d . . . . .
H46 H 0.582234 0.224770 1.031302 0.032 Uiso 1 1 calc R . . . .
C49 C 0.8349(3) 0.1060(3) 0.98513(18) 0.0227(6) Uani 1 1 d . . . . .
H49 H 0.876334 0.047628 0.961649 0.027 Uiso 1 1 calc R . . . .
C50 C 0.6861(3) 0.0973(3) 0.98077(18) 0.0258(6) Uani 1 1 d . . . . .
H50 H 0.612600 0.032321 0.954169 0.031 Uiso 1 1 calc R . . . .
C10 C 0.8546(3) 0.4765(3) 0.6674(2) 0.0267(6) Uani 1 1 d . . . . .
H10A H 0.803051 0.513305 0.705756 0.032 Uiso 1 1 calc R . . . .
H10B H 0.819886 0.388244 0.664757 0.032 Uiso 1 1 calc R . . . .
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'
Cl Cl 0.3639 0.7018 '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'
Fe Fe -1.1336 3.1974 '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'
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_
_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
C38 Fe1 C42 41.48(9) . . ?
C38 Fe1 C48 162.03(11) . . ?
C38 Fe1 C41 69.11(10) . . ?
C38 Fe1 C39 41.29(10) . . ?
C38 Fe1 C47 154.79(11) . . ?
C38 Fe1 C40 68.69(10) . . ?
C38 Fe1 C46 119.05(11) . . ?
C38 Fe1 C49 123.83(11) . . ?
C38 Fe1 C50 105.61(12) . . ?
C42 Fe1 C48 124.95(11) . . ?
C42 Fe1 C41 40.80(10) . . ?
C42 Fe1 C39 69.26(10) . . ?
C42 Fe1 C47 163.38(11) . . ?
C42 Fe1 C40 68.44(10) . . ?
C42 Fe1 C46 153.30(12) . . ?
C42 Fe1 C49 105.44(11) . . ?
C42 Fe1 C50 117.66(12) . . ?
C48 Fe1 C41 108.14(11) . . ?
C48 Fe1 C47 40.49(11) . . ?
C48 Fe1 C40 121.49(12) . . ?
C48 Fe1 C46 68.13(11) . . ?
C48 Fe1 C50 68.31(12) . . ?
C41 Fe1 C40 40.41(10) . . ?
C39 Fe1 C48 155.74(12) . . ?
C39 Fe1 C41 68.55(10) . . ?
C39 Fe1 C47 121.26(11) . . ?
C39 Fe1 C40 40.42(10) . . ?
C39 Fe1 C46 108.52(11) . . ?
C39 Fe1 C50 125.87(12) . . ?
C47 Fe1 C41 127.50(12) . . ?
C47 Fe1 C40 110.25(12) . . ?
C47 Fe1 C46 40.44(13) . . ?
C46 Fe1 C41 165.07(13) . . ?
C46 Fe1 C40 128.08(12) . . ?
C49 Fe1 C48 40.77(12) . . ?
C49 Fe1 C41 119.08(11) . . ?
C49 Fe1 C39 162.41(12) . . ?
C49 Fe1 C47 68.32(12) . . ?
C49 Fe1 C40 154.80(12) . . ?
C49 Fe1 C46 68.26(12) . . ?
C49 Fe1 C50 40.48(13) . . ?
C50 Fe1 C41 152.91(12) . . ?
C50 Fe1 C47 68.29(13) . . ?
C50 Fe1 C40 164.30(12) . . ?
C50 Fe1 C46 40.72(13) . . ?
F4 P2 F6 89.33(9) . . ?
F3 P2 F6 89.84(9) . . ?
F3 P2 F4 179.07(10) . . ?
F8 P2 F6 88.78(10) . . ?
F8 P2 F4 89.72(10) . . ?
F8 P2 F3 89.85(10) . . ?
F5 P2 F6 89.77(10) . . ?
F5 P2 F4 90.44(10) . . ?
F5 P2 F3 89.97(10) . . ?
F5 P2 F8 178.53(11) . . ?
F7 P2 F6 179.38(12) . . ?
F7 P2 F4 90.30(10) . . ?
F7 P2 F3 90.52(9) . . ?
F7 P2 F8 90.73(11) . . ?
F7 P2 F5 90.73(11) . . ?
C33 O32 C31 116.27(19) . . ?
C20 O19 C18 116.4(2) . . ?
C12 O13 C14 115.46(18) . . ?
C28 O29 C30 114.44(19) . . ?
C15 O16 C17 111.86(19) . . ?
C25 O26 C27 115.82(19) . . ?
H1A N1 H1B 107.8 . . ?
C43 N1 H1A 109.0 . . ?
C43 N1 H1B 109.0 . . ?
C45 N1 H1A 109.0 . . ?
C45 N1 H1B 109.0 . . ?
C45 N1 C43 113.09(19) . . ?
C42 C38 Fe1 69.64(14) . . ?
C42 C38 C43 126.4(2) . . ?
C43 C38 Fe1 118.24(18) . . ?
C39 C38 Fe1 70.14(14) . . ?
C39 C38 C42 107.6(2) . . ?
C39 C38 C43 125.2(2) . . ?
O13 C12 C33 115.9(2) . . ?
O13 C12 C37 123.9(2) . . ?
C37 C12 C33 120.2(2) . . ?
C33 C34 H34 119.7 . . ?
C33 C34 C35 120.5(3) . . ?
C35 C34 H34 119.7 . . ?
O32 C33 C12 116.2(2) . . ?
O32 C33 C34 124.7(2) . . ?
C34 C33 C12 119.0(2) . . ?
Fe1 C42 H42 126.2 . . ?
C38 C42 Fe1 68.88(14) . . ?
C38 C42 H42 126.1 . . ?
C41 C42 Fe1 70.35(15) . . ?
C41 C42 C38 107.8(2) . . ?
C41 C42 H42 126.1 . . ?
O19 C20 C21 124.2(2) . . ?
O19 C20 C25 116.0(2) . . ?
C21 C20 C25 119.9(2) . . ?
C12 C37 H37 120.2 . . ?
C12 C37 C36 119.7(2) . . ?
C36 C37 H37 120.2 . . ?
Fe1 C48 H48 126.2 . . ?
C47 C48 Fe1 69.92(15) . . ?
C47 C48 H48 126.1 . . ?
C47 C48 C49 107.9(3) . . ?
C49 C48 Fe1 69.36(15) . . ?
C49 C48 H48 126.1 . . ?
O16 C15 H15A 109.8 . . ?
O16 C15 H15B 109.8 . . ?
O16 C15 C14 109.25(19) . . ?
H15A C15 H15B 108.3 . . ?
C14 C15 H15A 109.8 . . ?
C14 C15 H15B 109.8 . . ?
O26 C27 H27A 110.2 . . ?
O26 C27 H27B 110.2 . . ?
O26 C27 C28 107.4(2) . . ?
H27A C27 H27B 108.5 . . ?
C28 C27 H27A 110.2 . . ?
C28 C27 H27B 110.2 . . ?
O13 C14 C15 108.24(19) . . ?
O13 C14 H14A 110.1 . . ?
O13 C14 H14B 110.1 . . ?
C15 C14 H14A 110.1 . . ?
C15 C14 H14B 110.1 . . ?
H14A C14 H14B 108.4 . . ?
N1 C43 H43A 108.5 . . ?
N1 C43 H43B 108.5 . . ?
C38 C43 N1 114.9(2) . . ?
C38 C43 H43A 108.5 . . ?
C38 C43 H43B 108.5 . . ?
H43A C43 H43B 107.5 . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.2(2) . . ?
C36 C35 H35 119.9 . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C22 119.8(3) . . ?
C22 C21 H21 120.1 . . ?
O29 C28 C27 112.7(2) . . ?
O29 C28 H28A 109.1 . . ?
O29 C28 H28B 109.1 . . ?
C27 C28 H28A 109.1 . . ?
C27 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
O29 C30 H30A 110.2 . . ?
O29 C30 H30B 110.2 . . ?
O29 C30 C31 107.4(2) . . ?
H30A C30 H30B 108.5 . . ?
C31 C30 H30A 110.2 . . ?
C31 C30 H30B 110.2 . . ?
Fe1 C41 H41 126.6 . . ?
C42 C41 Fe1 68.85(14) . . ?
C42 C41 H41 126.0 . . ?
C40 C41 Fe1 70.20(15) . . ?
C40 C41 C42 108.1(2) . . ?
C40 C41 H41 126.0 . . ?
N1 C45 H45A 109.5 . . ?
N1 C45 H45B 109.5 . . ?
N1 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
Fe1 C39 H39 126.4 . . ?
C38 C39 Fe1 68.57(14) . . ?
C38 C39 H39 126.1 . . ?
C40 C39 Fe1 70.54(14) . . ?
C40 C39 C38 107.8(2) . . ?
C40 C39 H39 126.1 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 119.9(2) . . ?
C37 C36 H36 119.8 . . ?
C35 C36 C37 120.3(2) . . ?
C35 C36 H36 119.8 . . ?
O32 C31 C30 108.3(2) . . ?
O32 C31 H31A 110.0 . . ?
O32 C31 H31B 110.0 . . ?
C30 C31 H31A 110.0 . . ?
C30 C31 H31B 110.0 . . ?
H31A C31 H31B 108.4 . . ?
O19 C18 H18A 110.0 . . ?
O19 C18 H18B 110.0 . . ?
O19 C18 C17 108.4(2) . . ?
H18A C18 H18B 108.4 . . ?
C17 C18 H18A 110.0 . . ?
C17 C18 H18B 110.0 . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.2(3) . . ?
C25 C24 H24 119.9 . . ?
Fe1 C47 H47 126.2 . . ?
C48 C47 Fe1 69.60(15) . . ?
C48 C47 H47 125.9 . . ?
C48 C47 C46 108.1(3) . . ?
C46 C47 Fe1 69.82(16) . . ?
C46 C47 H47 125.9 . . ?
Fe1 C40 H40 127.5 . . ?
C41 C40 Fe1 69.39(14) . . ?
C41 C40 H40 125.7 . . ?
C39 C40 Fe1 69.04(15) . . ?
C39 C40 C41 108.6(2) . . ?
C39 C40 H40 125.7 . . ?
O16 C17 C18 114.3(2) . . ?
O16 C17 H17A 108.7 . . ?
O16 C17 H17B 108.7 . . ?
C18 C17 H17A 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
O26 C25 C20 116.5(2) . . ?
O26 C25 C24 123.8(2) . . ?
C24 C25 C20 119.7(2) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H22 119.8 . . ?
Fe1 C46 H46 126.3 . . ?
C47 C46 Fe1 69.74(16) . . ?
C47 C46 H46 126.0 . . ?
C47 C46 C50 108.0(3) . . ?
C50 C46 Fe1 69.52(16) . . ?
C50 C46 H46 126.0 . . ?
Fe1 C49 H49 125.7 . . ?
C48 C49 Fe1 69.87(15) . . ?
C48 C49 H49 125.9 . . ?
C50 C49 Fe1 70.09(16) . . ?
C50 C49 C48 108.2(3) . . ?
C50 C49 H49 125.9 . . ?
Fe1 C50 H50 126.3 . . ?
C46 C50 Fe1 69.76(17) . . ?
C46 C50 H50 126.1 . . ?
C49 C50 Fe1 69.43(16) . . ?
C49 C50 C46 107.8(3) . . ?
C49 C50 H50 126.1 . . ?
Cl9 C10 H10A 109.2 . . ?
Cl9 C10 H10B 109.2 . . ?
Cl11 C10 Cl9 111.83(16) . . ?
Cl11 C10 H10A 109.2 . . ?
Cl11 C10 H10B 109.2 . . ?
H10A C10 H10B 107.9 . . ?
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 C38 2.026(2) . ?
Fe1 C42 2.036(3) . ?
Fe1 C48 2.048(3) . ?
Fe1 C41 2.056(3) . ?
Fe1 C39 2.047(3) . ?
Fe1 C47 2.052(3) . ?
Fe1 C40 2.067(3) . ?
Fe1 C46 2.053(3) . ?
Fe1 C49 2.041(3) . ?
Fe1 C50 2.050(3) . ?
P2 F6 1.6101(17) . ?
P2 F4 1.6051(17) . ?
P2 F3 1.6040(16) . ?
P2 F8 1.5991(18) . ?
P2 F5 1.5941(18) . ?
P2 F7 1.5917(18) . ?
Cl9 C10 1.768(3) . ?
Cl11 C10 1.759(3) . ?
O32 C33 1.372(3) . ?
O32 C31 1.436(3) . ?
O19 C20 1.372(3) . ?
O19 C18 1.423(3) . ?
O13 C12 1.382(3) . ?
O13 C14 1.434(3) . ?
O29 C28 1.427(3) . ?
O29 C30 1.431(3) . ?
O16 C15 1.427(3) . ?
O16 C17 1.427(3) . ?
O26 C27 1.431(3) . ?
O26 C25 1.373(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C43 1.507(3) . ?
N1 C45 1.486(3) . ?
C38 C42 1.438(3) . ?
C38 C43 1.495(3) . ?
C38 C39 1.436(3) . ?
C12 C33 1.411(4) . ?
C12 C37 1.389(3) . ?
C34 H34 0.9300 . ?
C34 C33 1.388(4) . ?
C34 C35 1.396(4) . ?
C42 H42 0.9300 . ?
C42 C41 1.426(4) . ?
C20 C21 1.390(4) . ?
C20 C25 1.403(4) . ?
C37 H37 0.9300 . ?
C37 C36 1.400(4) . ?
C48 H48 0.9300 . ?
C48 C47 1.419(4) . ?
C48 C49 1.424(4) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 C14 1.498(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.505(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C35 H35 0.9300 . ?
C35 C36 1.374(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.396(4) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C31 1.500(4) . ?
C41 H41 0.9300 . ?
C41 C40 1.424(4) . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C39 H39 0.9300 . ?
C39 C40 1.421(4) . ?
C23 H23 0.9300 . ?
C23 C24 1.393(4) . ?
C23 C22 1.383(4) . ?
C36 H36 0.9300 . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 C17 1.509(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.389(4) . ?
C47 H47 0.9300 . ?
C47 C46 1.419(4) . ?
C40 H40 0.9300 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C22 H22 0.9300 . ?
C46 H46 0.9300 . ?
C46 C50 1.428(5) . ?
C49 H49 0.9300 . ?
C49 C50 1.416(4) . ?
C50 H50 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
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 C38 C42 C41 -59.81(18) . . . . ?
Fe1 C38 C43 N1 -177.49(15) . . . . ?
Fe1 C38 C39 C40 59.85(18) . . . . ?
Fe1 C42 C41 C40 -59.44(18) . . . . ?
Fe1 C48 C47 C46 59.4(2) . . . . ?
Fe1 C48 C49 C50 -59.84(19) . . . . ?
Fe1 C41 C40 C39 -58.01(19) . . . . ?
Fe1 C39 C40 C41 58.22(18) . . . . ?
Fe1 C47 C46 C50 59.2(2) . . . . ?
Fe1 C46 C50 C49 59.2(2) . . . . ?
Fe1 C49 C50 C46 -59.4(2) . . . . ?
O19 C20 C21 C22 175.8(2) . . . . ?
O19 C20 C25 O26 3.5(3) . . . . ?
O19 C20 C25 C24 -175.3(2) . . . . ?
O19 C18 C17 O16 -62.6(3) . . . . ?
O13 C12 C33 O32 -1.1(3) . . . . ?
O13 C12 C33 C34 176.9(2) . . . . ?
O13 C12 C37 C36 -178.4(2) . . . . ?
O29 C30 C31 O32 64.3(3) . . . . ?
O16 C15 C14 O13 -61.4(3) . . . . ?
O26 C27 C28 O29 57.3(3) . . . . ?
C38 C42 C41 Fe1 58.89(17) . . . . ?
C38 C42 C41 C40 -0.6(3) . . . . ?
C38 C39 C40 Fe1 -58.62(18) . . . . ?
C38 C39 C40 C41 -0.4(3) . . . . ?
C12 O13 C14 C15 -176.28(19) . . . . ?
C12 C37 C36 C35 1.0(4) . . . . ?
C34 C35 C36 C37 -1.7(4) . . . . ?
C33 O32 C31 C30 -172.9(2) . . . . ?
C33 C12 C37 C36 1.3(4) . . . . ?
C33 C34 C35 C36 0.0(4) . . . . ?
C42 C38 C43 N1 -92.9(3) . . . . ?
C42 C38 C39 Fe1 -59.80(17) . . . . ?
C42 C38 C39 C40 0.1(3) . . . . ?
C42 C41 C40 Fe1 58.60(18) . . . . ?
C42 C41 C40 C39 0.6(3) . . . . ?
C20 O19 C18 C17 -170.1(2) . . . . ?
C20 C21 C22 C23 -0.1(4) . . . . ?
C37 C12 C33 O32 179.2(2) . . . . ?
C37 C12 C33 C34 -2.8(3) . . . . ?
C48 C47 C46 Fe1 -59.3(2) . . . . ?
C48 C47 C46 C50 -0.1(3) . . . . ?
C48 C49 C50 Fe1 59.70(19) . . . . ?
C48 C49 C50 C46 0.3(3) . . . . ?
C15 O16 C17 C18 -76.1(3) . . . . ?
C27 O26 C25 C20 165.6(2) . . . . ?
C27 O26 C25 C24 -15.7(3) . . . . ?
C14 O13 C12 C33 -172.3(2) . . . . ?
C14 O13 C12 C37 7.4(3) . . . . ?
C43 C38 C42 Fe1 -110.7(3) . . . . ?
C43 C38 C42 C41 -170.5(2) . . . . ?
C43 C38 C39 Fe1 111.2(2) . . . . ?
C43 C38 C39 C40 171.0(2) . . . . ?
C35 C34 C33 O32 179.9(2) . . . . ?
C35 C34 C33 C12 2.2(4) . . . . ?
C21 C20 C25 O26 -178.2(2) . . . . ?
C21 C20 C25 C24 3.0(4) . . . . ?
C28 O29 C30 C31 165.0(2) . . . . ?
C30 O29 C28 C27 63.4(3) . . . . ?
C45 N1 C43 C38 64.9(3) . . . . ?
C39 C38 C42 Fe1 60.11(17) . . . . ?
C39 C38 C42 C41 0.3(3) . . . . ?
C39 C38 C43 N1 97.8(3) . . . . ?
C23 C24 C25 O26 -179.9(2) . . . . ?
C23 C24 C25 C20 -1.2(4) . . . . ?
C31 O32 C33 C12 175.1(2) . . . . ?
C31 O32 C33 C34 -2.7(3) . . . . ?
C18 O19 C20 C21 -3.1(3) . . . . ?
C18 O19 C20 C25 175.2(2) . . . . ?
C24 C23 C22 C21 1.9(4) . . . . ?
C47 C48 C49 Fe1 59.53(19) . . . . ?
C47 C48 C49 C50 -0.3(3) . . . . ?
C47 C46 C50 Fe1 -59.3(2) . . . . ?
C47 C46 C50 C49 -0.1(3) . . . . ?
C17 O16 C15 C14 176.9(2) . . . . ?
C25 O26 C27 C28 -166.9(2) . . . . ?
C25 C20 C21 C22 -2.4(4) . . . . ?
C22 C23 C24 C25 -1.2(4) . . . . ?
C49 C48 C47 Fe1 -59.18(19) . . . . ?
C49 C48 C47 C46 0.2(3) . . . . ?
