#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:56:30 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289501 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/48/7714877.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_7714877
loop_
_publ_author_name
'Besmer, Manuel Luca'
'Schwitter, Flurina'
'Battistin, Federica'
'Braband, Henrik'
'Fox, Thomas'
'Spingler, Bernhard'
'Alberto, Roger'
_publ_section_title
;
 Induced fac-mer rearrangements in
 {M(CO)₃}⁺ complexes (M = Re, 99(m)Tc) by
 a PNP ligand.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1434
_journal_page_last               1438
_journal_paper_doi               10.1039/d3dt03992g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'(C18 H11 Br0.17 F1.66 N3 O4.66 P0.83 Re)(C18 H11 Br0.09 F1.83 N3 O4.83 P0.91 Re)'
_chemical_formula_sum            'C36 H22 Br0.26 F3.49 N6 O9.48 P1.74 Re2'
_chemical_formula_weight         1203.63
_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             2023-10-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2023-11-13 deposited with the CCDC.	2023-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                96.4300(10)
_cell_angle_beta                 97.0310(10)
_cell_angle_gamma                104.920(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4380(2)
_cell_length_b                   9.6908(2)
_cell_length_c                   27.1602(4)
_cell_measurement_reflns_used    39320
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      73.5900
_cell_measurement_theta_min      3.3070
_cell_volume                     2105.92(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      160.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -1.00  26.00   0.50    1.08    --    0.00  46.00 -58.00   54
  2  ω    -15.00  11.00   0.50    1.08    --    0.00 -46.00 152.00   52
  3  ω   -162.00-118.00   0.50    4.31    --  -86.25 -46.00 152.00   88
  4  ω    -50.00 -11.00   0.50    4.31    --  -86.25  46.00 -58.00   78
  5  ω    112.00 172.00   0.50    4.31    --   96.41  46.00 -58.00  120
  6  ω     21.00 102.00   0.50    4.31    --   96.41 -46.00 152.00  162
  7  ω    -58.00 -33.00   0.50    1.08    --   10.00 158.00  16.50   50
  8  ω    -19.00   7.00   0.50    1.08    --   14.00 100.00 150.38   52
  9  ω      2.00  29.00   0.50    1.08    --   22.00  72.00-150.43   54
 10  ω     25.00  51.00   0.50    1.08    --   22.00-101.00 -45.86   52
 11  ω      6.00  31.00   0.50    1.08    --   26.00  71.00 111.25   50
 12  ω      6.00  32.00   0.50    1.08    --   26.00  71.00  29.88   52
 13  ω    -37.00 -12.00   0.50    1.08    --  -30.00 -67.00 -64.25   50
 14  ω     12.00  37.00   0.50    1.08    --   30.00  66.00-142.62   50
 15  ω     13.00  38.00   0.50    1.08    --   30.00  66.00 -75.42   50
 16  ω    -33.00  42.00   0.50    1.08    --   30.00 -43.00-152.60  150
 17  ω     22.00  47.00   0.50    1.08    --   38.00  60.00-178.01   50
 18  ω    -48.00 -22.00   0.50    1.08    --  -38.00 -61.00  17.00   52
 19  ω     17.00  50.00   0.50    1.08    --   38.00 -40.00  23.43   66
 20  ω     22.00  47.00   0.50    1.08    --   38.00  60.00  24.66   50
 21  ω    -48.00 -23.00   0.50    1.08    --  -38.00 -61.00 -12.58   50
 22  ω    -33.00  10.00   0.50    1.08    --   38.00 -40.00  23.43   86
 23  ω     22.00  47.00   0.50    1.08    --   38.00  60.00 -89.54   50
 24  ω     22.00  47.00   0.50    1.08    --   38.00  61.00 -43.09   50
 25  ω    -73.00 -37.00   0.50    4.31    --  -50.00 -55.00-137.50   72
 26  ω    -62.00 -35.00   0.50    4.31    --  -50.00 -56.00 -59.96   54
 27  ω    -96.00 -41.00   0.50    4.31    --  -54.00 -56.00 163.74  110
 28  ω     43.00  70.00   0.50    4.31    --   58.00  56.00 -48.78   54
 29  ω     96.00 123.00   0.50    4.31    --   58.00  56.00  64.04   54
 30  ω     45.00  72.00   0.50    4.31    --   58.00  56.00  64.04   54
 31  ω    -82.00 -44.00   0.50    4.31    --  -58.00 -54.00 -71.38   76
 32  ω    -73.00 -43.00   0.50    4.31    --  -58.00 -56.00 100.49   60
 33  ω    -74.00 -48.00   0.50    4.31    --  -62.00 -54.00  82.38   52
 34  ω    -75.00 -47.00   0.50    4.31    --  -62.00 -55.00-167.76   56
 35  ω    -74.00 -47.00   0.50    4.31    --  -62.00 -55.00 -29.03   54
 36  ω    -78.00 -52.00   0.50    4.31    --  -66.00 -53.00 143.50   52
 37  ω    -84.00 -51.00   0.50    4.31    --  -66.00 -55.00  30.31   66
 38  ω    -84.00 -57.00   0.50    4.31    --  -70.00 -53.00  -0.73   54
 39  ω    -81.00 -55.00   0.50    4.31    --  -70.00 -56.00 -63.94   52
 40  ω     57.00  83.00   0.50    4.31    --   70.00  56.00 -55.81   52
 41  ω    -82.00 -55.00   0.50    4.31    --  -70.00 -56.00  80.73   54
 42  ω    -89.00 -63.00   0.50    4.31    --  -78.00 -56.00  33.90   52
 43  ω    -89.00 -63.00   0.50    4.31    --  -78.00 -55.00 140.97   52
 44  ω    -89.00 -63.00   0.50    4.31    --  -78.00 -55.00  -9.24   52
 45  ω    -89.00 -63.00   0.50    4.31    --  -78.00 -56.00 -84.29   52
 46  ω    -99.00 -63.00   0.50    4.31    --  -78.00 -56.00-171.87   72
 47  ω    -89.00 -63.00   0.50    4.31    --  -78.00 -56.00  60.27   52
 48  ω    -98.00 -68.00   0.50    4.31    --  -82.00 -54.00 -40.28   60
 49  ω    -93.00 -67.00   0.50    4.31    --  -82.00 -55.00-131.59   52
 50  ω    -97.00 -71.00   0.50    4.31    --  -86.00 -55.00 170.85   52
 51  ω   -158.00-109.00   0.50    4.31    --  -86.00 -55.00 170.85   98
 52  ω    -98.00 -72.00   0.50    4.31    --  -86.25 -55.00-132.42   52
 53  ω   -158.00-114.00   0.50    4.31    --  -86.25 -55.00-132.42   88
 54  ω   -134.00-108.00   0.50    4.31    --  -86.25 -54.00   0.70   52
 55  ω   -137.00 -75.00   0.50    4.31    --  -86.25 -55.00  65.61  124
 56  ω   -158.00 -72.00   0.50    4.31    --  -86.25 -55.00 -85.43  172
 57  ω   -108.00 -76.00   0.50    4.31    --  -86.25 -53.00-156.89   64
 58  ω   -110.00 -72.00   0.50    4.31    --  -86.25 -54.00 -48.23   76
 59  ω   -154.00 -72.00   0.50    4.31    --  -86.25 -55.00 -61.95  164
 60  ω   -159.00-115.00   0.50    4.31    --  -86.25 -54.00-105.08   88
 61  ω   -101.00 -72.00   0.50    4.31    --  -86.25 -53.00-175.41   58
 62  ω   -145.00-116.00   0.50    4.31    --  -86.25 -53.00-175.41   58
 63  ω   -145.00 -72.00   0.50    4.31    --  -86.25 -55.00  25.27  146
 64  ω   -102.00 -72.00   0.50    4.31    --  -86.25 -54.00   0.70   60
 65  ω   -107.00 -72.00   0.50    4.31    --  -86.25 -55.00 155.30   70
 66  ω   -152.00 -72.00   0.50    4.31    --  -86.25 -55.00 -15.42  160
 67  ω   -112.00 -72.00   0.50    4.31    --  -86.25 -55.00 113.21   80
 68  ω   -159.00-122.00   0.50    4.31    --  -86.25 -55.00 104.70   74
 69  ω   -118.00 -73.00   0.50    4.31    --  -86.25 -54.00-114.81   90
 70  ω   -153.00-128.00   0.50    4.31    --  -86.25 -55.00 113.21   50
 71  ω    -97.00 -72.00   0.50    4.31    --  -86.25 -54.00-105.08   50
 72  ω   -100.00 -72.00   0.50    4.31    --  -86.25 -54.00  75.62   56
 73  ω   -160.00-117.00   0.50    4.31    --  -86.25 -54.00  75.62   86
 74  ω   -101.00 -72.00   0.50    4.31    --  -86.25 -54.00 131.22   58
 75  ω   -152.00-119.00   0.50    4.31    --  -86.25 -54.00 131.22   66
 76  ω    -97.00 -72.00   0.50    4.31    --  -86.25 -54.00-146.60   50
 77  ω   -160.00-117.00   0.50    4.31    --  -86.25 -54.00-146.60   86
 78  ω   -105.00 -72.00   0.50    4.31    --  -86.25 -55.00 104.70   66
 79  ω   -159.00-128.00   0.50    4.31    --  -86.25 -56.00  46.81   62
 80  ω   -109.00 -80.00   0.50    4.31    --  -86.25 -56.00  46.81   58
 81  ω    -81.00 -47.00   0.50    4.31    --  -86.25 111.00  90.00   68
 82  ω     20.00  62.00   0.50    4.31    --   96.41 -94.00  30.00   84
 83  ω     90.00 118.00   0.50    4.31    --   96.41 -77.00 120.00   56
 84  ω     23.00  57.00   0.50    4.31    --   96.41 -77.00 120.00   68
 85  ω     82.00 107.00   0.50    4.31    --   96.41 -61.00-120.00   50
 86  ω     25.00  81.00   0.50    4.31    --   96.41 -61.00-120.00  112
 87  ω     23.00 101.00   0.50    4.31    --   96.41 -94.00-180.00  156
 88  ω     84.00 119.00   0.50    4.31    --   96.41 -77.00-120.00   70
 89  ω     44.00  70.00   0.50    4.31    --   96.41 -77.00-120.00   52
 90  ω     23.00 106.00   0.50    4.31    --   96.41 -94.00 120.00  166
 91  ω     37.00 109.00   0.50    4.31    --   96.41-111.00-120.00  144
 92  ω     80.00 109.00   0.50    4.31    --   96.41-111.00  90.00   58
 93  ω     28.00  73.00   0.50    4.31    --   96.41-111.00  90.00   90
 94  ω     26.00 118.00   0.50    4.31    --   96.41 -77.00  30.00  184
 95  ω     69.00  95.00   0.50    4.31    --   96.41 -94.00  30.00   52
 96  ω     36.00 108.00   0.50    4.31    --   96.41-111.00   0.00  144
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            53308
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.899
_diffrn_reflns_theta_min         3.316
_exptl_absorpt_coefficient_mu    12.643
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       plate
_exptl_crystal_F_000             1145
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.328
_refine_diff_density_min         -2.638
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         8152
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0468P)²+9.8041P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7569
_reflns_number_total             8152
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03992g2.cif
_cod_data_source_block           mlb_fs1_017_auto_sq
_cod_depositor_comments
'Adding full bibliography for 7714872--7714877.cif.'
_cod_database_code               7714877
_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   0.804
_shelx_estimated_absorpt_t_min   0.312
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Br2-Re2
 2.6 with sigma of 0.01
3. Others
 Sof(Br1)=1-FVAR(1)
 Sof(P1)=Sof(F1)=Sof(F2)=Sof(O7)=Sof(O8)=FVAR(1)
 Sof(Br2)=1-FVAR(2)
 Sof(P2)=Sof(F3)=Sof(F4)=Sof(O9)=Sof(O10)=FVAR(2)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26),
  C27(H27), C30(H30), C31(H31), C32(H32), C33(H33)
;
_platon_squeeze_void_probe_radius 1.20
_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
;
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
Re1 Re 0.45190(4) 0.16848(3) 0.18087(2) 0.04456(9) Uani 1 1 d . . . . .
O1 O 0.4621(9) 0.2194(8) 0.0711(2) 0.088(2) Uani 1 1 d . . . . .
O2 O 0.2427(7) 0.3820(6) 0.1880(2) 0.0752(16) Uani 1 1 d . . . . .
O3 O 0.7604(7) 0.4236(6) 0.2094(2) 0.0694(15) Uani 1 1 d . . . . .
N1 N 0.4438(6) 0.1198(5) 0.25656(19) 0.0416(11) Uani 1 1 d . . . . .
N2 N 0.5737(6) -0.0076(6) 0.1857(2) 0.0431(11) Uani 1 1 d . . . . .
N3 N 0.8113(8) 0.1541(8) 0.1289(2) 0.0649(16) Uani 1 1 d . . . . .
C1 C 0.4038(8) 0.2018(7) 0.2935(2) 0.0485(15) Uani 1 1 d . . . . .
H1 H 0.375325 0.286964 0.286365 0.058 Uiso 1 1 calc R U . . .
C2 C 0.4023(8) 0.1674(8) 0.3415(3) 0.0539(17) Uani 1 1 d . . . . .
H2 H 0.375877 0.228687 0.367139 0.065 Uiso 1 1 calc R U . . .
C3 C 0.4403(8) 0.0417(8) 0.3512(3) 0.0545(17) Uani 1 1 d . . . . .
H3 H 0.439333 0.013985 0.383694 0.065 Uiso 1 1 calc R U . . .
C4 C 0.4792(8) -0.0419(7) 0.3131(3) 0.0501(16) Uani 1 1 d . . . . .
H4 H 0.506029 -0.128426 0.319374 0.060 Uiso 1 1 calc R U . . .
C5 C 0.4804(7) -0.0038(6) 0.2662(2) 0.0411(13) Uani 1 1 d . . . . .
C6 C 0.5357(8) -0.0795(7) 0.2246(3) 0.0455(14) Uani 1 1 d . . . . .
C7 C 0.5556(9) -0.2181(7) 0.2264(3) 0.0567(18) Uani 1 1 d . . . . .
H7 H 0.526370 -0.268366 0.253470 0.068 Uiso 1 1 calc R U . . .
C8 C 0.6190(11) -0.2802(9) 0.1875(4) 0.073(2) Uani 1 1 d . . . . .
H8 H 0.629902 -0.375496 0.186772 0.087 Uiso 1 1 calc R U . . .
C9 C 0.6658(10) -0.2019(9) 0.1500(3) 0.063(2) Uani 1 1 d . . . . .
H9 H 0.712619 -0.241924 0.123663 0.076 Uiso 1 1 calc R U . . .
C10 C 0.6451(8) -0.0662(8) 0.1505(3) 0.0530(16) Uani 1 1 d . . . . .
C11 C 0.7078(9) 0.0216(9) 0.1112(3) 0.0589(18) Uani 1 1 d . . . . .
C12 C 0.6720(12) -0.0351(11) 0.0608(3) 0.077(2) Uani 1 1 d . . . . .
H12 H 0.602973 -0.130570 0.049812 0.092 Uiso 1 1 calc R U . . .
C13 C 0.7380(15) 0.0488(15) 0.0273(4) 0.103(4) Uani 1 1 d . . . . .
H13 H 0.709803 0.014886 -0.007672 0.124 Uiso 1 1 calc R U . . .
C14 C 0.8461(15) 0.1835(16) 0.0448(4) 0.112(4) Uani 1 1 d . . . . .
H14 H 0.897644 0.241905 0.022149 0.135 Uiso 1 1 calc R U . . .
C15 C 0.8778(12) 0.2318(13) 0.0957(4) 0.092(3) Uani 1 1 d . . . . .
H15 H 0.950845 0.325268 0.107524 0.110 Uiso 1 1 calc R U . . .
C16 C 0.4588(10) 0.1960(9) 0.1124(3) 0.065(2) Uani 1 1 d . . . . .
C17 C 0.3218(10) 0.3025(8) 0.1845(3) 0.0567(17) Uani 1 1 d . . . . .
C18 C 0.6459(9) 0.3265(8) 0.1991(3) 0.0532(16) Uani 1 1 d . . . . .
P1 P 0.1488(3) -0.1244(3) 0.12109(9) 0.0576(7) Uani 0.828(5) 1 d . . P A 1
F1 F 0.0893(9) -0.0356(10) 0.0825(2) 0.103(2) Uani 0.828(5) 1 d . . P A 1
F2 F 0.0135(9) -0.2448(9) 0.1260(3) 0.110(3) Uani 0.828(5) 1 d . . P A 1
O7 O 0.2391(8) -0.0200(7) 0.1677(3) 0.0498(14) Uani 0.828(5) 1 d . . P A 1
O8 O 0.2769(8) -0.1690(8) 0.0922(3) 0.072(2) Uani 0.828(5) 1 d . . P A 1
Br1 Br 0.1935(7) -0.0404(7) 0.1423(3) 0.060(2) Uiso 0.172(5) 1 d . . P A 2
Re2 Re 0.95525(3) 0.90213(3) 0.39604(2) 0.03385(8) Uani 1 1 d D . . . .
O4 O 0.9770(6) 0.7165(6) 0.48057(19) 0.0573(12) Uani 1 1 d . . . . .
O5 O 0.7281(6) 1.0380(5) 0.45316(18) 0.0536(11) Uani 1 1 d . . . . .
O6 O 1.2594(5) 1.1326(5) 0.45381(17) 0.0478(10) Uani 1 1 d . . . . .
N4 N 0.9394(5) 1.0240(5) 0.33402(17) 0.0319(9) Uani 1 1 d . . . . .
N5 N 1.0760(5) 0.8043(5) 0.33900(17) 0.0332(9) Uani 1 1 d . . . . .
N6 N 1.3169(7) 0.7812(6) 0.4228(2) 0.0475(12) Uani 1 1 d . . . . .
C19 C 0.8958(7) 1.1490(6) 0.3364(2) 0.0381(12) Uani 1 1 d . . . . .
H19 H 0.866542 1.186636 0.366789 0.046 Uiso 1 1 calc R U . . .
C20 C 0.8924(7) 1.2234(6) 0.2963(2) 0.0409(13) Uani 1 1 d . . . . .
H20 H 0.860542 1.310792 0.298783 0.049 Uiso 1 1 calc R U . . .
C21 C 0.9363(8) 1.1691(7) 0.2522(2) 0.0439(13) Uani 1 1 d . . . . .
H21 H 0.934362 1.218316 0.223868 0.053 Uiso 1 1 calc R U . . .
C22 C 0.9826(7) 1.0428(7) 0.2500(2) 0.0398(13) Uani 1 1 d . . . . .
H22 H 1.014807 1.004903 0.220149 0.048 Uiso 1 1 calc R U . . .
C23 C 0.9823(7) 0.9715(6) 0.2909(2) 0.0348(12) Uani 1 1 d . . . . .
C24 C 1.0383(6) 0.8379(6) 0.2922(2) 0.0317(11) Uani 1 1 d . . . . .
C25 C 1.0555(7) 0.7589(7) 0.2489(2) 0.0425(13) Uani 1 1 d . . . . .
H25 H 1.027039 0.785594 0.217053 0.051 Uiso 1 1 calc R U . . .
C26 C 1.1148(8) 0.6400(7) 0.2526(2) 0.0455(14) Uani 1 1 d . . . . .
H26 H 1.122403 0.580452 0.223241 0.055 Uiso 1 1 calc R U . . .
C27 C 1.1631(7) 0.6084(7) 0.2993(3) 0.0448(14) Uani 1 1 d . . . . .
H27 H 1.208995 0.529363 0.302442 0.054 Uiso 1 1 calc R U . . .
C28 C 1.1442(7) 0.6932(6) 0.3422(2) 0.0374(12) Uani 1 1 d . . . . .
C29 C 1.2105(7) 0.6667(7) 0.3927(2) 0.0415(13) Uani 1 1 d . . . . .
C30 C 1.1735(9) 0.5275(7) 0.4049(3) 0.0522(16) Uani 1 1 d . . . . .
H30 H 1.101864 0.447535 0.382392 0.063 Uiso 1 1 calc R U . . .
C31 C 1.2475(11) 0.5115(9) 0.4524(4) 0.070(2) Uani 1 1 d . . . . .
H31 H 1.221770 0.419807 0.463401 0.084 Uiso 1 1 calc R U . . .
C32 C 1.3568(10) 0.6282(10) 0.4828(3) 0.067(2) Uani 1 1 d . . . . .
H32 H 1.410059 0.617560 0.514477 0.080 Uiso 1 1 calc R U . . .
C33 C 1.3877(9) 0.7586(8) 0.4670(3) 0.0558(17) Uani 1 1 d . . . . .
H33 H 1.463848 0.838544 0.488372 0.067 Uiso 1 1 calc R U . . .
C34 C 0.9696(8) 0.7808(7) 0.4492(3) 0.0467(15) Uani 1 1 d . . . . .
C35 C 0.8167(8) 0.9863(7) 0.4331(2) 0.0427(13) Uani 1 1 d . . . . .
C36 C 1.1462(8) 1.0446(7) 0.4320(2) 0.0402(13) Uani 1 1 d . . . . .
P2 P 0.6509(2) 0.6003(2) 0.34688(7) 0.0426(5) Uani 0.914(4) 1 d . . P B 3
F3 F 0.6111(7) 0.5783(6) 0.4002(2) 0.0769(15) Uani 0.914(4) 1 d . . P B 3
F4 F 0.7755(5) 0.5084(5) 0.3451(2) 0.0671(14) Uani 0.914(4) 1 d . . P B 3
O9 O 0.7440(6) 0.7563(6) 0.3486(2) 0.0456(12) Uani 0.914(4) 1 d . . P B 3
O10 O 0.5034(7) 0.5363(6) 0.3098(3) 0.0669(17) Uani 0.914(4) 1 d . . P B 3
Br2 Br 0.6989(11) 0.6913(12) 0.3473(4) 0.058(4) Uiso 0.086(4) 1 d D . P B 4
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'
Br Br -0.6763 1.2805 '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 0 17 0.0069
2 5 -5 0.0182
0 4 -15 0.0138
-3 -1 15 0.0382
3 1 -15 0.0256
-5 5 -2 0.0542
0 5 5 0.0153
-5 -1 1 0.0541
5 1 -1 0.0312
0 -6 0 0.0489
0 0 -17 0.0069
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
N1 Re1 N2 74.98(19) . . ?
N1 Re1 O7 79.6(2) . . ?
N1 Re1 Br1 94.1(2) . . ?
N2 Re1 Br1 83.48(18) . . ?
C16 Re1 N1 175.5(3) . . ?
C16 Re1 N2 101.0(3) . . ?
C16 Re1 O7 97.6(3) . . ?
C16 Re1 Br1 83.2(3) . . ?
C17 Re1 N1 96.5(3) . . ?
C17 Re1 N2 169.6(3) . . ?
C17 Re1 C16 87.3(3) . . ?
C17 Re1 O7 94.3(3) . . ?
C17 Re1 Br1 91.4(3) . . ?
C18 Re1 N1 94.5(3) . . ?
C18 Re1 N2 97.7(2) . . ?
C18 Re1 C16 88.1(3) . . ?
C18 Re1 C17 88.7(3) . . ?
C18 Re1 O7 173.7(3) . . ?
C18 Re1 Br1 171.3(3) . . ?
O7 Re1 N2 78.6(2) . . ?
C1 N1 Re1 124.5(4) . . ?
C1 N1 C5 118.9(6) . . ?
C5 N1 Re1 116.6(4) . . ?
C6 N2 Re1 112.0(4) . . ?
C10 N2 Re1 127.7(5) . . ?
C10 N2 C6 118.6(6) . . ?
C15 N3 C11 117.4(7) . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.6(7) . . ?
C2 C1 H1 118.7 . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.4(7) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.8 . . ?
C4 C3 C2 118.5(7) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 H4 119.3 . . ?
C5 C4 C3 121.4(7) . . ?
C5 C4 H4 119.3 . . ?
N1 C5 C4 120.2(6) . . ?
N1 C5 C6 114.6(5) . . ?
C4 C5 C6 124.9(6) . . ?
N2 C6 C5 117.4(5) . . ?
N2 C6 C7 121.6(6) . . ?
C7 C6 C5 121.0(7) . . ?
C6 C7 H7 120.9 . . ?
C8 C7 C6 118.3(8) . . ?
C8 C7 H7 120.9 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.1(7) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0(7) . . ?
C10 C9 H9 120.0 . . ?
N2 C10 C9 122.1(7) . . ?
N2 C10 C11 118.7(6) . . ?
C9 C10 C11 119.2(7) . . ?
N3 C11 C10 115.4(6) . . ?
N3 C11 C12 122.8(8) . . ?
C12 C11 C10 121.6(8) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 C11 118.6(9) . . ?
C13 C12 H12 120.7 . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.3(10) . . ?
C14 C13 H13 120.3 . . ?
C13 C14 H14 120.7 . . ?
C13 C14 C15 118.6(10) . . ?
C15 C14 H14 120.7 . . ?
N3 C15 C14 123.2(11) . . ?
N3 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
O1 C16 Re1 176.8(8) . . ?
O2 C17 Re1 178.0(7) . . ?
O3 C18 Re1 178.3(6) . . ?
F2 P1 F1 109.9(5) . . ?
F2 P1 O7 118.6(4) . . ?
F2 P1 O8 113.0(5) . . ?
O7 P1 F1 107.6(4) . . ?
O7 P1 O8 108.8(3) . . ?
O8 P1 F1 96.6(4) . . ?
P1 O7 Re1 132.9(4) . . ?
N4 Re2 N5 75.28(17) . . ?
N4 Re2 Br2 89.8(3) . . ?
N5 Re2 Br2 79.6(3) . . ?
C34 Re2 N4 176.3(2) . . ?
C34 Re2 N5 101.5(2) . . ?
C34 Re2 O9 97.1(2) . . ?
C34 Re2 Br2 87.8(3) . . ?
C35 Re2 N4 95.5(2) . . ?
C35 Re2 N5 167.6(2) . . ?
C35 Re2 C34 87.5(3) . . ?
C35 Re2 O9 91.5(2) . . ?
C35 Re2 Br2 92.3(3) . . ?
C36 Re2 N4 92.7(2) . . ?
C36 Re2 N5 98.5(2) . . ?
C36 Re2 C34 89.5(3) . . ?
C36 Re2 C35 90.0(2) . . ?
C36 Re2 O9 173.4(2) . . ?
C36 Re2 Br2 176.4(3) . . ?
O9 Re2 N4 80.71(18) . . ?
O9 Re2 N5 79.06(18) . . ?
C19 N4 Re2 124.6(4) . . ?
C19 N4 C23 118.9(5) . . ?
C23 N4 Re2 116.4(4) . . ?
C24 N5 Re2 113.2(3) . . ?
C28 N5 Re2 127.5(4) . . ?
C28 N5 C24 117.2(5) . . ?
C33 N6 C29 117.5(6) . . ?
N4 C19 H19 119.0 . . ?
N4 C19 C20 122.0(5) . . ?
C20 C19 H19 119.0 . . ?
C19 C20 H20 120.5 . . ?
C19 C20 C21 118.9(6) . . ?
C21 C20 H20 120.5 . . ?
C20 C21 H21 120.5 . . ?
C22 C21 C20 119.0(6) . . ?
C22 C21 H21 120.5 . . ?
C21 C22 H22 120.1 . . ?
C23 C22 C21 119.9(6) . . ?
C23 C22 H22 120.1 . . ?
N4 C23 C22 121.3(5) . . ?
N4 C23 C24 115.6(5) . . ?
C22 C23 C24 123.0(5) . . ?
N5 C24 C23 115.4(4) . . ?
N5 C24 C25 123.5(5) . . ?
C25 C24 C23 121.1(5) . . ?
C24 C25 H25 120.8 . . ?
C24 C25 C26 118.5(6) . . ?
C26 C25 H25 120.8 . . ?
C25 C26 H26 120.3 . . ?
C27 C26 C25 119.4(6) . . ?
C27 C26 H26 120.3 . . ?
C26 C27 H27 120.2 . . ?
C26 C27 C28 119.6(6) . . ?
C28 C27 H27 120.2 . . ?
N5 C28 C27 121.6(6) . . ?
N5 C28 C29 119.0(5) . . ?
C27 C28 C29 119.3(5) . . ?
N6 C29 C28 116.2(5) . . ?
N6 C29 C30 123.3(6) . . ?
C30 C29 C28 120.4(6) . . ?
C29 C30 H30 121.7 . . ?
C29 C30 C31 116.5(7) . . ?
C31 C30 H30 121.7 . . ?
C30 C31 H31 120.0 . . ?
C32 C31 C30 120.0(7) . . ?
C32 C31 H31 120.0 . . ?
C31 C32 H32 120.5 . . ?
C33 C32 C31 119.0(8) . . ?
C33 C32 H32 120.5 . . ?
N6 C33 C32 123.6(7) . . ?
N6 C33 H33 118.2 . . ?
C32 C33 H33 118.2 . . ?
O4 C34 Re2 177.2(6) . . ?
O5 C35 Re2 176.3(5) . . ?
O6 C36 Re2 178.5(5) . . ?
F4 P2 F3 97.1(3) . . ?
O9 P2 F3 108.1(3) . . ?
O9 P2 F4 108.6(3) . . ?
O10 P2 F3 110.2(4) . . ?
O10 P2 F4 111.1(3) . . ?
O10 P2 O9 119.4(3) . . ?
P2 O9 Re2 134.5(3) . . ?
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
Re1 N1 2.165(5) . ?
Re1 N2 2.215(5) . ?
Re1 C16 1.915(9) . ?
Re1 C17 1.906(7) . ?
Re1 C18 1.900(8) . ?
Re1 O7 2.167(6) . ?
Re1 Br1 2.577(7) . ?
O1 C16 1.169(10) . ?
O2 C17 1.146(9) . ?
O3 C18 1.142(9) . ?
N1 C1 1.339(8) . ?
N1 C5 1.356(8) . ?
N2 C6 1.355(9) . ?
N2 C10 1.341(9) . ?
N3 C11 1.350(10) . ?
N3 C15 1.324(11) . ?
C1 H1 0.9500 . ?
C1 C2 1.383(10) . ?
C2 H2 0.9500 . ?
C2 C3 1.382(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.367(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.366(9) . ?
C5 C6 1.466(9) . ?
C6 C7 1.402(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(12) . ?
C8 H8 0.9500 . ?
C8 C9 1.373(12) . ?
C9 H9 0.9500 . ?
C9 C10 1.369(10) . ?
C10 C11 1.501(11) . ?
C11 C12 1.383(11) . ?
C12 H12 0.9500 . ?
C12 C13 1.362(14) . ?
C13 H13 0.9500 . ?
C13 C14 1.380(16) . ?
C14 H14 0.9500 . ?
C14 C15 1.380(14) . ?
C15 H15 0.9500 . ?
P1 F1 1.544(7) . ?
P1 F2 1.439(7) . ?
P1 O7 1.512(7) . ?
P1 O8 1.532(6) . ?
Re2 N4 2.173(5) . ?
Re2 N5 2.212(4) . ?
Re2 C34 1.972(8) . ?
Re2 C35 1.908(7) . ?
Re2 C36 1.904(7) . ?
Re2 O9 2.137(5) . ?
Re2 Br2 2.650(9) . ?
O4 C34 1.116(8) . ?
O5 C35 1.157(8) . ?
O6 C36 1.148(8) . ?
N4 C19 1.351(7) . ?
N4 C23 1.351(7) . ?
N5 C24 1.367(7) . ?
N5 C28 1.351(7) . ?
N6 C29 1.346(8) . ?
N6 C33 1.340(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.374(9) . ?
C20 H20 0.9500 . ?
C20 C21 1.385(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.375(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.374(8) . ?
C23 C24 1.491(8) . ?
C24 C25 1.375(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.378(9) . ?
C26 H26 0.9500 . ?
C26 C27 1.376(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.398(8) . ?
C28 C29 1.491(9) . ?
C29 C30 1.392(9) . ?
C30 H30 0.9500 . ?
C30 C31 1.405(11) . ?
C31 H31 0.9500 . ?
C31 C32 1.370(13) . ?
C32 H32 0.9500 . ?
C32 C33 1.352(11) . ?
C33 H33 0.9500 . ?
P2 F3 1.551(5) . ?
P2 F4 1.545(4) . ?
P2 O9 1.507(6) . ?
P2 O10 1.451(6) . ?
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
Re1 N1 C1 C2 -179.1(5) . . . . ?
Re1 N1 C5 C4 179.6(4) . . . . ?
Re1 N1 C5 C6 5.5(7) . . . . ?
Re1 N2 C6 C5 -22.4(7) . . . . ?
Re1 N2 C6 C7 160.5(5) . . . . ?
Re1 N2 C10 C9 -157.4(5) . . . . ?
Re1 N2 C10 C11 24.2(8) . . . . ?
N1 C1 C2 C3 -1.4(10) . . . . ?
N1 C5 C6 N2 11.9(8) . . . . ?
N1 C5 C6 C7 -171.0(6) . . . . ?
N2 C6 C7 C8 1.3(10) . . . . ?
N2 C10 C11 N3 52.6(9) . . . . ?
N2 C10 C11 C12 -132.5(8) . . . . ?
N3 C11 C12 C13 -3.1(15) . . . . ?
C1 N1 C5 C4 -1.1(9) . . . . ?
C1 N1 C5 C6 -175.2(5) . . . . ?
C1 C2 C3 C4 0.7(10) . . . . ?
C2 C3 C4 C5 -0.3(10) . . . . ?
C3 C4 C5 N1 0.5(9) . . . . ?
C3 C4 C5 C6 173.9(6) . . . . ?
C4 C5 C6 N2 -161.8(6) . . . . ?
C4 C5 C6 C7 15.3(10) . . . . ?
C5 N1 C1 C2 1.6(9) . . . . ?
C5 C6 C7 C8 -175.7(7) . . . . ?
C6 N2 C10 C9 6.5(9) . . . . ?
C6 N2 C10 C11 -172.0(6) . . . . ?
C6 C7 C8 C9 2.5(12) . . . . ?
C7 C8 C9 C10 -1.9(12) . . . . ?
C8 C9 C10 N2 -2.7(11) . . . . ?
C8 C9 C10 C11 175.8(7) . . . . ?
C9 C10 C11 N3 -125.8(8) . . . . ?
C9 C10 C11 C12 49.1(11) . . . . ?
C10 N2 C6 C5 171.3(6) . . . . ?
C10 N2 C6 C7 -5.7(9) . . . . ?
C10 C11 C12 C13 -177.6(9) . . . . ?
C11 N3 C15 C14 0.0(16) . . . . ?
C11 C12 C13 C14 4.0(18) . . . . ?
C12 C13 C14 C15 -3(2) . . . . ?
C13 C14 C15 N3 1(2) . . . . ?
C15 N3 C11 C10 175.9(8) . . . . ?
C15 N3 C11 C12 1.1(13) . . . . ?
F1 P1 O7 Re1 -57.5(6) . . . . ?
F2 P1 O7 Re1 177.1(5) . . . . ?
O8 P1 O7 Re1 46.1(6) . . . . ?
Re2 N4 C19 C20 178.1(4) . . . . ?
Re2 N4 C23 C22 -177.6(4) . . . . ?
Re2 N4 C23 C24 -1.2(6) . . . . ?
Re2 N5 C24 C23 22.4(6) . . . . ?
Re2 N5 C24 C25 -159.9(4) . . . . ?
Re2 N5 C28 C27 156.9(4) . . . . ?
Re2 N5 C28 C29 -27.0(7) . . . . ?
N4 C19 C20 C21 -0.5(9) . . . . ?
N4 C23 C24 N5 -14.5(7) . . . . ?
N4 C23 C24 C25 167.7(5) . . . . ?
N5 C24 C25 C26 -0.5(9) . . . . ?
N5 C28 C29 N6 -51.4(7) . . . . ?
N5 C28 C29 C30 134.0(6) . . . . ?
N6 C29 C30 C31 2.9(10) . . . . ?
C19 N4 C23 C22 0.1(8) . . . . ?
C19 N4 C23 C24 176.6(5) . . . . ?
C19 C20 C21 C22 -0.3(9) . . . . ?
C20 C21 C22 C23 1.0(9) . . . . ?
C21 C22 C23 N4 -0.9(9) . . . . ?
C21 C22 C23 C24 -177.1(5) . . . . ?
C22 C23 C24 N5 161.8(5) . . . . ?
C22 C23 C24 C25 -15.9(8) . . . . ?
C23 N4 C19 C20 0.6(8) . . . . ?
C23 C24 C25 C26 177.1(5) . . . . ?
C24 N5 C28 C27 -5.2(8) . . . . ?
C24 N5 C28 C29 170.9(5) . . . . ?
C24 C25 C26 C27 -3.4(9) . . . . ?
C25 C26 C27 C28 2.9(9) . . . . ?
C26 C27 C28 N5 1.5(9) . . . . ?
C26 C27 C28 C29 -174.6(6) . . . . ?
C27 C28 C29 N6 124.8(6) . . . . ?
C27 C28 C29 C30 -49.8(8) . . . . ?
C28 N5 C24 C23 -173.0(5) . . . . ?
C28 N5 C24 C25 4.7(8) . . . . ?
C28 C29 C30 C31 177.1(6) . . . . ?
C29 N6 C33 C32 -0.6(11) . . . . ?
C29 C30 C31 C32 -3.4(11) . . . . ?
C30 C31 C32 C33 2.0(12) . . . . ?
C31 C32 C33 N6 0.1(12) . . . . ?
C33 N6 C29 C28 -175.4(6) . . . . ?
C33 N6 C29 C30 -1.0(9) . . . . ?
F3 P2 O9 Re2 49.8(5) . . . . ?
F4 P2 O9 Re2 -54.4(5) . . . . ?
O10 P2 O9 Re2 176.8(4) . . . . ?
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.015 0.500 0.000 233 57 ' '
2 0.152 0.609 0.564 11 0 ' '
3 0.847 0.391 0.436 10 0 ' '
