#------------------------------------------------------------------------------
#$Date: 2022-06-02 02:02:44 +0300 (Thu, 02 Jun 2022) $
#$Revision: 275727 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/03/7710393.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_7710393
loop_
_publ_author_name
'Alberto, Roger'
'Csucker, Joshua'
'Jo, Da Kyung'
'Nadeem, Qaisar'
'Blacque, Olivier'
'Fox, Thomas'
'Braband, Henrik'
_publ_section_title
;
 An Isoindoline Bridged [M(η6-arene)2]+ (M = Re, 99mTc) ansa-Arenophane
 and its Dinuclear Macrocycles with Axial Chirality
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00743F
_journal_year                    2022
_chemical_formula_moiety         'C28 H18 N2 O4 Re, F6 P'
_chemical_formula_sum            'C28 H18 F6 N2 O4 P Re'
_chemical_formula_weight         777.61
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-01-18 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                102.971(4)
_cell_angle_beta                 102.419(4)
_cell_angle_gamma                92.903(4)
_cell_formula_units_Z            2
_cell_length_a                   7.1963(3)
_cell_length_b                   12.2113(5)
_cell_length_c                   14.9263(6)
_cell_measurement_reflns_used    9027
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.4730
_cell_measurement_theta_min      3.0910
_cell_volume                     1241.53(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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  95.80   0.80    3.50    --   43.61-125.00 -60.00   86
  2  ω     13.00  41.00   0.80    3.50    --   43.61  79.00-123.41   35
  3  ω      6.00  82.00   0.80    3.50    --   43.61 -99.00 -60.00   95
  4  ω      6.00  82.00   0.80    3.50    --   43.61 -99.00 -30.00   95
  5  ω      6.00  82.00   0.80    3.50    --   43.61 -99.00 120.00   95
  6  ω    -33.00  76.60   0.80    3.50    --   43.61 -19.00   0.00  137
  7  ω     23.00 115.00   0.80    3.50    --   43.61  37.00   0.00  115
  8  ω     38.00 131.60   0.80   12.00    --  111.00 -30.00   0.00  117
  9  ω    104.00 177.60   0.80   12.00    --  111.00 111.00-180.00   92
 10  ω    103.00 177.40   0.80   12.00    --  111.00  77.00 -60.00   93
 11  ω     41.00 133.00   0.80   12.00    --  111.00 -45.00-120.00  115
 12  ω    103.00 177.40   0.80   12.00    --  111.00  77.00-180.00   93
 13  ω     38.00 108.40   0.80   12.00    --  111.00-111.00 120.00   88
 14  ω     38.00 108.40   0.80   12.00    --  111.00-111.00   0.00   88
 15  ω    104.00 177.60   0.80   12.00    --  111.00 111.00  60.00   92
 16  ω     38.00 108.40   0.80   12.00    --  111.00-111.00-180.00   88
 17  ω     40.00 140.00   0.80   12.00    --  111.00 -77.00-150.00  125
 18  ω     38.00 108.40   0.80   12.00    --  111.00-111.00  60.00   88
 19  ω     43.00 136.60   0.80   12.00    --  111.00 -61.00  60.00  117
 20  ω     89.00 177.00   0.80   12.00    --  111.00  45.00   0.00  110
 21  ω     31.00 107.00   0.80   12.00    --  111.00 -94.00 -90.00   95
 22  ω     90.00 178.00   0.80   12.00    --  111.00  30.00 -30.00  110
 23  ω     31.00 107.00   0.80   12.00    --  111.00 -94.00-150.00   95
 24  ω     31.00 107.00   0.80   12.00    --  111.00 -94.00  30.00   95
 25  ω     38.00 108.40   0.80   12.00    --  111.00-111.00  90.00   88
 26  ω    104.00 177.60   0.80   12.00    --  111.00 111.00 -90.00   92
 27  ω     38.00 131.60   0.80   12.00    --  111.00 -30.00 150.00  117
 28  ω     14.00 114.00   0.80    3.50    --   43.61  74.00   8.44  125
 29  ω     18.00 111.60   0.80    3.50    --   43.61  57.00-180.00  117
 30  ω     18.00 111.60   0.80    3.50    --   43.61  57.00  90.00  117
 31  ω     18.00 111.60   0.80    3.50    --   43.61  57.00 -90.00  117
 32  ω     13.00  41.00   0.80    3.50    --   43.61  79.00 -70.44   35
 33  ω     13.00  41.00   0.80    3.50    --   43.61  78.00 175.90   35
 34  ω     90.00 178.00   0.80   12.00    --  111.00  30.00 150.00  110
 35  ω     85.00 169.00   0.80   12.00    --  111.00  61.00  90.00  105
 36  ω     85.00 177.00   0.80   12.00    --  111.00  61.00 -90.00  115
 37  ω     82.00 178.00   0.80   12.00    --  111.00  71.00 168.85  120
 38  ω     85.00 177.00   0.80   12.00    --  111.00  61.00-115.19  115
 39  ω     71.00 177.40   0.80   12.00    --  111.00  15.00  90.00  133
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1154303000
_diffrn_orient_matrix_UB_12      0.0563559000
_diffrn_orient_matrix_UB_13      0.1009795000
_diffrn_orient_matrix_UB_21      0.1859049000
_diffrn_orient_matrix_UB_22      -0.0023543000
_diffrn_orient_matrix_UB_23      -0.0355005000
_diffrn_orient_matrix_UB_31      -0.0263035000
_diffrn_orient_matrix_UB_32      0.1173119000
_diffrn_orient_matrix_UB_33      -0.0200646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9155
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.319
_diffrn_reflns_theta_min         3.124
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.980
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (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            yellow
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         9155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0332
_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)+(0.0608P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7820
_reflns_number_total             9155
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by 179.9916° 
around [-0.00 1.00 0.00] (reciprocal) or [0.17 0.97 0.20] (direct)
;
_cod_data_source_file            d2dt00743f2.cif
_cod_data_source_block           '[3][PF6]'
_cod_database_code               7710393
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8240(5)
 0.1760(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C25(H25), C26(H26),
  C27(H27), C28(H28)
;
_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 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.611
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
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
C1 C 0.7196(8) 0.3769(4) 0.7591(4) 0.0240(10) Uani 1 1 d . . . . .
C2 C 0.6637(8) 0.2761(5) 0.6860(4) 0.0277(11) Uani 1 1 d . . . . .
H2 H 0.594799 0.279285 0.624907 0.033 Uiso 1 1 calc R U . . .
C3 C 0.7111(9) 0.1713(5) 0.7048(5) 0.0335(13) Uani 1 1 d . . . . .
H3 H 0.677769 0.104016 0.655751 0.040 Uiso 1 1 calc R U . . .
C4 C 0.8081(9) 0.1666(5) 0.7965(5) 0.0356(14) Uani 1 1 d . . . . .
H4 H 0.839527 0.095946 0.808868 0.043 Uiso 1 1 calc R U . . .
C5 C 0.8592(8) 0.2661(6) 0.8704(5) 0.0342(13) Uani 1 1 d . . . . .
H5 H 0.923312 0.262214 0.932091 0.041 Uiso 1 1 calc R U . . .
C6 C 0.8136(8) 0.3717(5) 0.8514(4) 0.0296(11) Uani 1 1 d . . . . .
H6 H 0.846317 0.438831 0.900571 0.035 Uiso 1 1 calc R U . . .
C7 C 0.6430(8) 0.5803(5) 0.8005(4) 0.0253(10) Uani 1 1 d . . . . .
C8 C 0.6277(8) 0.6707(5) 0.7484(4) 0.0254(10) Uani 1 1 d . . . . .
C9 C 0.6510(8) 0.6261(5) 0.6577(4) 0.0255(11) Uani 1 1 d . . . . .
C10 C 0.6905(8) 0.5074(5) 0.6495(4) 0.0256(11) Uani 1 1 d . . . . .
C11 C 0.5989(8) 0.7825(5) 0.7785(4) 0.0302(12) Uani 1 1 d . . . . .
H11 H 0.586382 0.813302 0.841022 0.036 Uiso 1 1 calc R U . . .
C12 C 0.5890(9) 0.8483(5) 0.7124(5) 0.0353(13) Uani 1 1 d . . . . .
H12 H 0.568708 0.925647 0.730307 0.042 Uiso 1 1 calc R U . . .
C13 C 0.6082(9) 0.8029(5) 0.6204(5) 0.0355(13) Uani 1 1 d . . . . .
H13 H 0.597376 0.849233 0.576625 0.043 Uiso 1 1 calc R U . . .
C14 C 0.6429(9) 0.6913(5) 0.5924(4) 0.0315(12) Uani 1 1 d . . . . .
H14 H 0.660484 0.660678 0.530747 0.038 Uiso 1 1 calc R U . . .
C15 C 0.2731(7) 0.3358(4) 0.8107(4) 0.0216(10) Uani 1 1 d . . . . .
C16 C 0.3764(8) 0.3454(4) 0.9052(4) 0.0248(10) Uani 1 1 d . . . . .
H16 H 0.408858 0.417482 0.948248 0.030 Uiso 1 1 calc R U . . .
C17 C 0.4305(8) 0.2470(5) 0.9349(4) 0.0268(11) Uani 1 1 d . . . . .
H17 H 0.497286 0.253291 0.998352 0.032 Uiso 1 1 calc R U . . .
C18 C 0.3862(8) 0.1392(4) 0.8708(4) 0.0264(11) Uani 1 1 d . . . . .
H18 H 0.423686 0.073480 0.890923 0.032 Uiso 1 1 calc R U . . .
C19 C 0.2862(8) 0.1307(4) 0.7772(4) 0.0284(11) Uani 1 1 d . . . . .
H19 H 0.256868 0.058501 0.734256 0.034 Uiso 1 1 calc R U . . .
C20 C 0.2280(7) 0.2273(4) 0.7453(4) 0.0238(10) Uani 1 1 d . . . . .
H20 H 0.160491 0.220255 0.681806 0.029 Uiso 1 1 calc R U . . .
C21 C 0.1829(7) 0.5355(4) 0.8391(4) 0.0230(10) Uani 1 1 d . . . . .
C22 C 0.1533(7) 0.6175(4) 0.7801(4) 0.0219(10) Uani 1 1 d . . . . .
C23 C 0.1700(8) 0.5662(5) 0.6891(4) 0.0248(10) Uani 1 1 d . . . . .
C24 C 0.2160(8) 0.4492(4) 0.6871(4) 0.0233(10) Uani 1 1 d . . . . .
C25 C 0.1145(7) 0.7313(4) 0.8015(4) 0.0228(10) Uani 1 1 d . . . . .
H25 H 0.101134 0.767485 0.862769 0.027 Uiso 1 1 calc R U . . .
C26 C 0.0966(9) 0.7877(5) 0.7313(4) 0.0296(11) Uani 1 1 d . . . . .
H26 H 0.072619 0.864789 0.744786 0.036 Uiso 1 1 calc R U . . .
C27 C 0.1125(9) 0.7358(5) 0.6405(4) 0.0317(12) Uani 1 1 d . . . . .
H27 H 0.096569 0.777379 0.593103 0.038 Uiso 1 1 calc R U . . .
C28 C 0.1516(8) 0.6232(5) 0.6182(4) 0.0285(11) Uani 1 1 d . . . . .
H28 H 0.165044 0.587433 0.556824 0.034 Uiso 1 1 calc R U . . .
N1 N 0.6820(7) 0.4827(4) 0.7378(3) 0.0238(9) Uani 1 1 d . . . . .
N2 N 0.2202(6) 0.4337(4) 0.7795(3) 0.0229(9) Uani 1 1 d . . . . .
O1 O 0.7284(7) 0.4408(4) 0.5845(3) 0.0356(10) Uani 1 1 d . . . . .
O2 O 0.6243(6) 0.5833(3) 0.8799(3) 0.0322(9) Uani 1 1 d . . . . .
O3 O 0.2498(6) 0.3793(3) 0.6233(3) 0.0308(9) Uani 1 1 d . . . . .
O4 O 0.1786(6) 0.5469(3) 0.9205(3) 0.0276(8) Uani 1 1 d . . . . .
Re1 Re 0.54562(3) 0.25407(2) 0.80831(2) 0.02040(8) Uani 1 1 d . . . . .
F1 F 0.2201(7) 0.0411(5) 0.5453(3) 0.0628(13) Uani 1 1 d . . . . .
F2 F 0.0510(9) -0.1261(3) 0.4672(3) 0.0611(14) Uani 1 1 d . . . . .
F3 F -0.0230(7) -0.0217(3) 0.5995(3) 0.0458(10) Uani 1 1 d . . . . .
P1 P 0.000000 0.000000 0.500000 0.0322(4) Uani 1 2 d S . P . .
F4 F 0.9212(7) 0.8702(3) 0.9828(3) 0.0466(10) Uani 1 1 d . . . . .
F5 F 1.2125(6) 0.9683(4) 1.0290(3) 0.0526(11) Uani 1 1 d . . . . .
F6 F 1.0157(7) 0.9787(3) 0.8926(3) 0.0476(10) Uani 1 1 d . . . . .
P2 P 1.000000 1.000000 1.000000 0.0290(4) Uani 1 2 d S . 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'
F F 0.0727 0.0534 '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'
Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 0 0.0108
0 1 0 0.0108
-4 1 -1 0.0369
4 -1 1 0.0369
0 0 1 0.0093
0 0 -1 0.0293
3 2 -5 0.0427
-4 -2 5 0.0265
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
C2 C1 N1 119.1(5) . . ?
C2 C1 Re1 70.9(3) . . ?
C6 C1 C2 120.2(5) . . ?
C6 C1 N1 120.6(5) . . ?
C6 C1 Re1 70.8(3) . . ?
N1 C1 Re1 131.8(4) . . ?
C1 C2 H2 120.2 . . ?
C1 C2 Re1 72.0(3) . . ?
C3 C2 C1 119.7(6) . . ?
C3 C2 H2 120.2 . . ?
C3 C2 Re1 72.0(3) . . ?
Re1 C2 H2 127.9 . . ?
C2 C3 H3 120.0 . . ?
C2 C3 Re1 71.2(3) . . ?
C4 C3 C2 119.9(6) . . ?
C4 C3 H3 120.0 . . ?
C4 C3 Re1 71.3(3) . . ?
Re1 C3 H3 130.0 . . ?
C3 C4 H4 119.6 . . ?
C3 C4 C5 120.7(5) . . ?
C3 C4 Re1 72.0(3) . . ?
C5 C4 H4 119.6 . . ?
C5 C4 Re1 71.3(3) . . ?
Re1 C4 H4 129.6 . . ?
C4 C5 H5 120.3 . . ?
C4 C5 C6 119.4(6) . . ?
C4 C5 Re1 71.7(3) . . ?
C6 C5 H5 120.3 . . ?
C6 C5 Re1 71.3(3) . . ?
Re1 C5 H5 128.9 . . ?
C1 C6 C5 120.0(5) . . ?
C1 C6 H6 120.0 . . ?
C1 C6 Re1 72.3(3) . . ?
C5 C6 H6 120.0 . . ?
C5 C6 Re1 71.5(3) . . ?
Re1 C6 H6 128.3 . . ?
N1 C7 C8 106.4(4) . . ?
O2 C7 C8 129.3(5) . . ?
O2 C7 N1 124.3(5) . . ?
C9 C8 C7 108.6(5) . . ?
C11 C8 C7 129.7(5) . . ?
C11 C8 C9 121.8(5) . . ?
C8 C9 C10 108.7(5) . . ?
C14 C9 C8 121.6(5) . . ?
C14 C9 C10 129.7(5) . . ?
N1 C10 C9 106.4(4) . . ?
O1 C10 C9 129.7(5) . . ?
O1 C10 N1 123.9(5) . . ?
C8 C11 H11 121.6 . . ?
C8 C11 C12 116.7(5) . . ?
C12 C11 H11 121.6 . . ?
C11 C12 H12 119.2 . . ?
C11 C12 C13 121.6(6) . . ?
C13 C12 H12 119.2 . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 120.9(6) . . ?
C14 C13 H13 119.5 . . ?
C9 C14 H14 121.3 . . ?
C13 C14 C9 117.4(6) . . ?
C13 C14 H14 121.3 . . ?
C16 C15 C20 120.1(5) . . ?
C16 C15 Re1 70.9(3) . . ?
C20 C15 Re1 71.6(3) . . ?
N2 C15 C16 120.4(4) . . ?
N2 C15 C20 119.5(5) . . ?
N2 C15 Re1 127.9(3) . . ?
C15 C16 H16 120.2 . . ?
C15 C16 Re1 72.1(3) . . ?
C17 C16 C15 119.7(5) . . ?
C17 C16 H16 120.2 . . ?
C17 C16 Re1 71.6(3) . . ?
Re1 C16 H16 128.3 . . ?
C16 C17 H17 119.7 . . ?
C16 C17 C18 120.7(5) . . ?
C16 C17 Re1 71.5(3) . . ?
C18 C17 H17 119.7 . . ?
C18 C17 Re1 71.9(3) . . ?
Re1 C17 H17 129.5 . . ?
C17 C18 H18 120.4 . . ?
C17 C18 Re1 71.2(3) . . ?
C19 C18 C17 119.2(5) . . ?
C19 C18 H18 120.4 . . ?
C19 C18 Re1 71.4(3) . . ?
Re1 C18 H18 129.3 . . ?
C18 C19 H19 119.2 . . ?
C18 C19 C20 121.6(5) . . ?
C18 C19 Re1 72.1(3) . . ?
C20 C19 H19 119.2 . . ?
C20 C19 Re1 72.3(3) . . ?
Re1 C19 H19 128.9 . . ?
C15 C20 H20 120.7 . . ?
C15 C20 Re1 71.3(3) . . ?
C19 C20 C15 118.7(5) . . ?
C19 C20 H20 120.7 . . ?
C19 C20 Re1 70.9(3) . . ?
Re1 C20 H20 129.5 . . ?
N2 C21 C22 106.0(4) . . ?
O4 C21 C22 129.3(5) . . ?
O4 C21 N2 124.7(5) . . ?
C23 C22 C21 109.1(4) . . ?
C23 C22 C25 119.8(5) . . ?
C25 C22 C21 131.1(5) . . ?
C22 C23 C24 108.5(5) . . ?
C28 C23 C22 122.3(5) . . ?
C28 C23 C24 129.2(5) . . ?
N2 C24 C23 106.1(4) . . ?
O3 C24 C23 128.9(5) . . ?
O3 C24 N2 124.9(5) . . ?
C22 C25 H25 121.0 . . ?
C26 C25 C22 117.9(5) . . ?
C26 C25 H25 121.0 . . ?
C25 C26 H26 119.0 . . ?
C25 C26 C27 122.0(5) . . ?
C27 C26 H26 119.0 . . ?
C26 C27 H27 119.6 . . ?
C26 C27 C28 120.7(5) . . ?
C28 C27 H27 119.6 . . ?
C23 C28 C27 117.3(5) . . ?
C23 C28 H28 121.4 . . ?
C27 C28 H28 121.4 . . ?
C1 N1 C10 123.5(4) . . ?
C7 N1 C1 126.4(4) . . ?
C7 N1 C10 110.0(4) . . ?
C15 N2 C21 124.5(4) . . ?
C15 N2 C24 125.0(4) . . ?
C24 N2 C21 110.2(4) . . ?
C1 Re1 C15 102.2(2) . . ?
C1 Re1 C20 117.1(2) . . ?
C2 Re1 C1 37.0(2) . . ?
C2 Re1 C3 36.8(2) . . ?
C2 Re1 C4 66.3(2) . . ?
C2 Re1 C15 111.6(2) . . ?
C2 Re1 C16 139.2(2) . . ?
C2 Re1 C17 175.4(2) . . ?
C2 Re1 C18 147.5(2) . . ?
C2 Re1 C19 117.3(2) . . ?
C2 Re1 C20 102.3(2) . . ?
C3 Re1 C1 66.2(2) . . ?
C3 Re1 C15 140.0(2) . . ?
C3 Re1 C20 111.8(2) . . ?
C4 Re1 C1 78.0(2) . . ?
C4 Re1 C3 36.7(2) . . ?
C4 Re1 C15 176.4(2) . . ?
C4 Re1 C18 101.7(2) . . ?
C4 Re1 C20 139.6(2) . . ?
C5 Re1 C1 66.5(2) . . ?
C5 Re1 C2 79.0(2) . . ?
C5 Re1 C3 66.6(3) . . ?
C5 Re1 C4 36.9(3) . . ?
C5 Re1 C15 146.4(2) . . ?
C5 Re1 C16 114.9(2) . . ?
C5 Re1 C17 100.5(2) . . ?
C5 Re1 C18 110.1(2) . . ?
C5 Re1 C19 138.8(2) . . ?
C5 Re1 C20 175.5(2) . . ?
C6 Re1 C1 36.8(2) . . ?
C6 Re1 C2 66.9(2) . . ?
C6 Re1 C3 78.7(2) . . ?
C6 Re1 C4 66.5(2) . . ?
C6 Re1 C5 37.2(2) . . ?
C6 Re1 C15 115.8(2) . . ?
C6 Re1 C16 100.4(2) . . ?
C6 Re1 C17 110.0(2) . . ?
C6 Re1 C18 138.3(2) . . ?
C6 Re1 C19 174.8(2) . . ?
C6 Re1 C20 147.3(2) . . ?
C15 Re1 C20 37.12(18) . . ?
C16 Re1 C1 110.7(2) . . ?
C16 Re1 C3 176.0(2) . . ?
C16 Re1 C4 146.4(2) . . ?
C16 Re1 C15 36.99(19) . . ?
C16 Re1 C17 36.9(2) . . ?
C16 Re1 C18 66.7(2) . . ?
C16 Re1 C19 78.5(2) . . ?
C16 Re1 C20 66.9(2) . . ?
C17 Re1 C1 138.6(2) . . ?
C17 Re1 C3 147.1(2) . . ?
C17 Re1 C4 116.0(2) . . ?
C17 Re1 C15 66.3(2) . . ?
C17 Re1 C18 36.9(2) . . ?
C17 Re1 C20 78.5(2) . . ?
C18 Re1 C1 174.8(2) . . ?
C18 Re1 C3 116.6(2) . . ?
C18 Re1 C15 78.5(2) . . ?
C18 Re1 C20 66.5(2) . . ?
C19 Re1 C1 148.4(2) . . ?
C19 Re1 C3 102.9(2) . . ?
C19 Re1 C4 111.7(2) . . ?
C19 Re1 C15 66.3(2) . . ?
C19 Re1 C17 66.0(2) . . ?
C19 Re1 C18 36.6(2) . . ?
C19 Re1 C20 36.8(2) . . ?
F1 P1 F1 180.0 2_556 . ?
F1 P1 F2 90.1(3) 2_556 2_556 ?
F1 P1 F2 90.1(3) . . ?
F1 P1 F2 89.9(3) 2_556 . ?
F1 P1 F2 89.9(3) . 2_556 ?
F1 P1 F3 89.4(2) 2_556 2_556 ?
F1 P1 F3 90.6(2) 2_556 . ?
F1 P1 F3 89.4(2) . . ?
F1 P1 F3 90.6(2) . 2_556 ?
F2 P1 F2 180.0(3) . 2_556 ?
F2 P1 F3 89.1(2) . 2_556 ?
F2 P1 F3 90.9(2) 2_556 2_556 ?
F2 P1 F3 89.1(2) 2_556 . ?
F2 P1 F3 90.9(2) . . ?
F3 P1 F3 180.0(3) 2_556 . ?
F4 P2 F4 180.0 2_777 . ?
F5 P2 F4 89.6(2) 2_777 2_777 ?
F5 P2 F4 89.6(2) . . ?
F5 P2 F4 90.4(2) . 2_777 ?
F5 P2 F4 90.4(2) 2_777 . ?
F5 P2 F5 180.0 2_777 . ?
F5 P2 F6 89.9(2) 2_777 2_777 ?
F5 P2 F6 90.1(2) 2_777 . ?
F5 P2 F6 89.9(2) . . ?
F5 P2 F6 90.1(2) . 2_777 ?
F6 P2 F4 90.3(2) 2_777 2_777 ?
F6 P2 F4 90.3(2) . . ?
F6 P2 F4 89.7(2) . 2_777 ?
F6 P2 F4 89.7(2) 2_777 . ?
F6 P2 F6 180.0 2_777 . ?
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
C1 C2 1.423(8) . ?
C1 C6 1.414(8) . ?
C1 N1 1.424(7) . ?
C1 Re1 2.249(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.414(8) . ?
C2 Re1 2.234(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.412(10) . ?
C3 Re1 2.245(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.416(10) . ?
C4 Re1 2.237(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.421(9) . ?
C5 Re1 2.231(6) . ?
C6 H6 0.9500 . ?
C6 Re1 2.229(6) . ?
C7 C8 1.481(8) . ?
C7 N1 1.421(7) . ?
C7 O2 1.215(7) . ?
C8 C9 1.391(7) . ?
C8 C11 1.380(8) . ?
C9 C10 1.474(8) . ?
C9 C14 1.385(8) . ?
C10 N1 1.429(7) . ?
C10 O1 1.207(7) . ?
C11 H11 0.9500 . ?
C11 C12 1.399(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.400(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.422(7) . ?
C15 C20 1.433(7) . ?
C15 N2 1.418(7) . ?
C15 Re1 2.249(5) . ?
C16 H16 0.9500 . ?
C16 C17 1.415(8) . ?
C16 Re1 2.234(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.418(8) . ?
C17 Re1 2.236(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.406(8) . ?
C18 Re1 2.245(5) . ?
C19 H19 0.9500 . ?
C19 C20 1.418(8) . ?
C19 Re1 2.236(5) . ?
C20 H20 0.9500 . ?
C20 Re1 2.253(5) . ?
C21 C22 1.470(8) . ?
C21 N2 1.432(6) . ?
C21 O4 1.198(7) . ?
C22 C23 1.396(7) . ?
C22 C25 1.410(7) . ?
C23 C24 1.478(8) . ?
C23 C28 1.379(8) . ?
C24 N2 1.427(7) . ?
C24 O3 1.204(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.366(8) . ?
C26 H26 0.9500 . ?
C26 C27 1.393(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.398(8) . ?
C28 H28 0.9500 . ?
F1 P1 1.589(5) . ?
F2 P1 1.594(4) . ?
F3 P1 1.607(4) . ?
F4 P2 1.601(4) . ?
F5 P2 1.590(4) . ?
F6 P2 1.595(4) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C4 H4 F6 0.95 2.35 3.234(7) 154.4 1_545 yes
C5 H5 F4 0.95 2.44 3.238(7) 141.0 2_767 yes
C19 H19 F3 0.95 2.50 3.206(7) 131.4 . yes
C20 H20 F2 0.95 2.41 3.297(7) 155.4 2_556 yes
C26 H26 F6 0.95 2.46 3.130(7) 127.7 1_455 yes
C28 H28 O1 0.95 2.36 3.262(7) 159.3 2_666 yes
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
C1 C2 C3 C4 2.0(8) . . . . ?
C1 C2 C3 Re1 56.1(4) . . . . ?
C2 C1 C6 C5 2.5(8) . . . . ?
C2 C1 C6 Re1 -52.9(4) . . . . ?
C2 C1 N1 C7 148.9(5) . . . . ?
C2 C1 N1 C10 -35.2(7) . . . . ?
C2 C3 C4 C5 -0.1(9) . . . . ?
C2 C3 C4 Re1 54.0(5) . . . . ?
C3 C4 C5 C6 -0.6(9) . . . . ?
C3 C4 C5 Re1 54.4(5) . . . . ?
C4 C5 C6 C1 -0.5(8) . . . . ?
C4 C5 C6 Re1 55.3(5) . . . . ?
C6 C1 C2 C3 -3.2(8) . . . . ?
C6 C1 C2 Re1 52.9(4) . . . . ?
C6 C1 N1 C7 -31.9(8) . . . . ?
C6 C1 N1 C10 143.9(5) . . . . ?
C7 C8 C9 C10 -2.4(6) . . . . ?
C7 C8 C9 C14 179.7(5) . . . . ?
C7 C8 C11 C12 -179.5(6) . . . . ?
C8 C7 N1 C1 176.0(5) . . . . ?
C8 C7 N1 C10 -0.4(6) . . . . ?
C8 C9 C10 N1 2.2(6) . . . . ?
C8 C9 C10 O1 -175.9(6) . . . . ?
C8 C9 C14 C13 -0.8(9) . . . . ?
C8 C11 C12 C13 -0.3(9) . . . . ?
C9 C8 C11 C12 1.7(8) . . . . ?
C9 C10 N1 C1 -177.5(4) . . . . ?
C9 C10 N1 C7 -1.1(6) . . . . ?
C10 C9 C14 C13 -178.1(6) . . . . ?
C11 C8 C9 C10 176.6(5) . . . . ?
C11 C8 C9 C14 -1.2(9) . . . . ?
C11 C12 C13 C14 -1.7(10) . . . . ?
C12 C13 C14 C9 2.2(9) . . . . ?
C14 C9 C10 N1 179.8(6) . . . . ?
C14 C9 C10 O1 1.7(11) . . . . ?
C15 C16 C17 C18 1.3(8) . . . . ?
C15 C16 C17 Re1 55.8(4) . . . . ?
C16 C15 C20 C19 0.8(8) . . . . ?
C16 C15 C20 Re1 -53.8(4) . . . . ?
C16 C15 N2 C21 -29.4(7) . . . . ?
C16 C15 N2 C24 143.8(5) . . . . ?
C16 C17 C18 C19 -0.5(8) . . . . ?
C16 C17 C18 Re1 54.3(5) . . . . ?
C17 C18 C19 C20 -0.2(8) . . . . ?
C17 C18 C19 Re1 54.7(4) . . . . ?
C18 C19 C20 C15 0.0(8) . . . . ?
C18 C19 C20 Re1 54.8(5) . . . . ?
C20 C15 C16 C17 -1.4(8) . . . . ?
C20 C15 C16 Re1 54.1(4) . . . . ?
C20 C15 N2 C21 153.0(5) . . . . ?
C20 C15 N2 C24 -33.8(7) . . . . ?
C21 C22 C23 C24 -1.4(6) . . . . ?
C21 C22 C23 C28 -179.1(5) . . . . ?
C21 C22 C25 C26 179.0(5) . . . . ?
C22 C21 N2 C15 174.3(5) . . . . ?
C22 C21 N2 C24 0.3(6) . . . . ?
C22 C23 C24 N2 1.5(6) . . . . ?
C22 C23 C24 O3 -176.4(6) . . . . ?
C22 C23 C28 C27 -0.9(9) . . . . ?
C22 C25 C26 C27 1.1(9) . . . . ?
C23 C22 C25 C26 -0.8(8) . . . . ?
C23 C24 N2 C15 -175.1(5) . . . . ?
C23 C24 N2 C21 -1.1(6) . . . . ?
C24 C23 C28 C27 -178.1(6) . . . . ?
C25 C22 C23 C24 178.4(5) . . . . ?
C25 C22 C23 C28 0.7(8) . . . . ?
C25 C26 C27 C28 -1.3(9) . . . . ?
C26 C27 C28 C23 1.2(9) . . . . ?
C28 C23 C24 N2 179.0(6) . . . . ?
C28 C23 C24 O3 1.1(10) . . . . ?
N1 C1 C2 C3 176.0(5) . . . . ?
N1 C1 C2 Re1 -127.9(5) . . . . ?
N1 C1 C6 C5 -176.7(5) . . . . ?
N1 C1 C6 Re1 127.9(5) . . . . ?
N1 C7 C8 C9 1.8(6) . . . . ?
N1 C7 C8 C11 -177.2(6) . . . . ?
N2 C15 C16 C17 -179.0(5) . . . . ?
N2 C15 C16 Re1 -123.5(5) . . . . ?
N2 C15 C20 C19 178.4(5) . . . . ?
N2 C15 C20 Re1 123.8(5) . . . . ?
N2 C21 C22 C23 0.7(6) . . . . ?
N2 C21 C22 C25 -179.1(5) . . . . ?
O1 C10 N1 C1 0.7(9) . . . . ?
O1 C10 N1 C7 177.2(5) . . . . ?
O2 C7 C8 C9 -177.1(6) . . . . ?
O2 C7 C8 C11 4.0(10) . . . . ?
O2 C7 N1 C1 -5.1(9) . . . . ?
O2 C7 N1 C10 178.5(6) . . . . ?
O3 C24 N2 C15 2.9(9) . . . . ?
O3 C24 N2 C21 176.9(5) . . . . ?
O4 C21 C22 C23 -179.4(6) . . . . ?
O4 C21 C22 C25 0.9(10) . . . . ?
O4 C21 N2 C15 -5.6(8) . . . . ?
O4 C21 N2 C24 -179.7(5) . . . . ?
Re1 C1 C2 C3 -56.1(5) . . . . ?
Re1 C1 C6 C5 55.4(5) . . . . ?
Re1 C1 N1 C7 59.1(8) . . . . ?
Re1 C1 N1 C10 -125.0(5) . . . . ?
Re1 C2 C3 C4 -54.1(5) . . . . ?
Re1 C3 C4 C5 -54.1(5) . . . . ?
Re1 C4 C5 C6 -55.1(5) . . . . ?
Re1 C5 C6 C1 -55.8(5) . . . . ?
Re1 C15 C16 C17 -55.6(4) . . . . ?
Re1 C15 C20 C19 54.6(4) . . . . ?
Re1 C15 N2 C21 -118.0(5) . . . . ?
Re1 C15 N2 C24 55.1(7) . . . . ?
Re1 C16 C17 C18 -54.5(5) . . . . ?
Re1 C17 C18 C19 -54.8(5) . . . . ?
Re1 C18 C19 C20 -54.9(5) . . . . ?
Re1 C19 C20 C15 -54.8(4) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.8240(5) 14732 10589 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.1760(5) 14755 10589 nmt -1.0010 0.0001 -0.0002 0.3478 0.9995 0.4024 0.0001
0.0021 -1.0014
