Induced <i>fac</i>-<i>mer</i> rearrangements in {M(CO)<sub>3</sub>}<sup>+</sup> complexes (M = Re, <sup>99(m)</sup>Tc) by a PNP ligand.
Besmer, Manuel Luca; Schwitter, Flurina; Battistin, Federica; Braband, Henrik; Fox, Thomas; Spingler, Bernhard; Alberto, Roger; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1434–1438; doi:10.1039/d3dt03992g

data_7714877
_publ_section_title
;
 Induced <i>fac</i>-<i>mer</i> rearrangements in
 {M(CO)<sub>3</sub>}<sup>+</sup> complexes (M = Re, <sup>99(m)</sup>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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -1.00  26.00   0.50    1.08    --    0.00  46.00 -58.00   54
  2  \w    -15.00  11.00   0.50    1.08    --    0.00 -46.00 152.00   52
  3  \w   -162.00-118.00   0.50    4.31    --  -86.25 -46.00 152.00   88
  4  \w    -50.00 -11.00   0.50    4.31    --  -86.25  46.00 -58.00   78
  5  \w    112.00 172.00   0.50    4.31    --   96.41  46.00 -58.00  120
  6  \w     21.00 102.00   0.50    4.31    --   96.41 -46.00 152.00  162
  7  \w    -58.00 -33.00   0.50    1.08    --   10.00 158.00  16.50   50
  8  \w    -19.00   7.00   0.50    1.08    --   14.00 100.00 150.38   52
  9  \w      2.00  29.00   0.50    1.08    --   22.00  72.00-150.43   54
 10  \w     25.00  51.00   0.50    1.08    --   22.00-101.00 -45.86   52
 11  \w      6.00  31.00   0.50    1.08    --   26.00  71.00 111.25   50
 12  \w      6.00  32.00   0.50    1.08    --   26.00  71.00  29.88   52
 13  \w    -37.00 -12.00   0.50    1.08    --  -30.00 -67.00 -64.25   50
 14  \w     12.00  37.00   0.50    1.08    --   30.00  66.00-142.62   50
 15  \w     13.00  38.00   0.50    1.08    --   30.00  66.00 -75.42   50
 16  \w    -33.00  42.00   0.50    1.08    --   30.00 -43.00-152.60  150
 17  \w     22.00  47.00   0.50    1.08    --   38.00  60.00-178.01   50
 18  \w    -48.00 -22.00   0.50    1.08    --  -38.00 -61.00  17.00   52
 19  \w     17.00  50.00   0.50    1.08    --   38.00 -40.00  23.43   66
 20  \w     22.00  47.00   0.50    1.08    --   38.00  60.00  24.66   50
 21  \w    -48.00 -23.00   0.50    1.08    --  -38.00 -61.00 -12.58   50
 22  \w    -33.00  10.00   0.50    1.08    --   38.00 -40.00  23.43   86
 23  \w     22.00  47.00   0.50    1.08    --   38.00  60.00 -89.54   50
 24  \w     22.00  47.00   0.50    1.08    --   38.00  61.00 -43.09   50
 25  \w    -73.00 -37.00   0.50    4.31    --  -50.00 -55.00-137.50   72
 26  \w    -62.00 -35.00   0.50    4.31    --  -50.00 -56.00 -59.96   54
 27  \w    -96.00 -41.00   0.50    4.31    --  -54.00 -56.00 163.74  110
 28  \w     43.00  70.00   0.50    4.31    --   58.00  56.00 -48.78   54
 29  \w     96.00 123.00   0.50    4.31    --   58.00  56.00  64.04   54
 30  \w     45.00  72.00   0.50    4.31    --   58.00  56.00  64.04   54
 31  \w    -82.00 -44.00   0.50    4.31    --  -58.00 -54.00 -71.38   76
 32  \w    -73.00 -43.00   0.50    4.31    --  -58.00 -56.00 100.49   60
 33  \w    -74.00 -48.00   0.50    4.31    --  -62.00 -54.00  82.38   52
 34  \w    -75.00 -47.00   0.50    4.31    --  -62.00 -55.00-167.76   56
 35  \w    -74.00 -47.00   0.50    4.31    --  -62.00 -55.00 -29.03   54
 36  \w    -78.00 -52.00   0.50    4.31    --  -66.00 -53.00 143.50   52
 37  \w    -84.00 -51.00   0.50    4.31    --  -66.00 -55.00  30.31   66
 38  \w    -84.00 -57.00   0.50    4.31    --  -70.00 -53.00  -0.73   54
 39  \w    -81.00 -55.00   0.50    4.31    --  -70.00 -56.00 -63.94   52
 40  \w     57.00  83.00   0.50    4.31    --   70.00  56.00 -55.81   52
 41  \w    -82.00 -55.00   0.50    4.31    --  -70.00 -56.00  80.73   54
 42  \w    -89.00 -63.00   0.50    4.31    --  -78.00 -56.00  33.90   52
 43  \w    -89.00 -63.00   0.50    4.31    --  -78.00 -55.00 140.97   52
 44  \w    -89.00 -63.00   0.50    4.31    --  -78.00 -55.00  -9.24   52
 45  \w    -89.00 -63.00   0.50    4.31    --  -78.00 -56.00 -84.29   52
 46  \w    -99.00 -63.00   0.50    4.31    --  -78.00 -56.00-171.87   72
 47  \w    -89.00 -63.00   0.50    4.31    --  -78.00 -56.00  60.27   52
 48  \w    -98.00 -68.00   0.50    4.31    --  -82.00 -54.00 -40.28   60
 49  \w    -93.00 -67.00   0.50    4.31    --  -82.00 -55.00-131.59   52
 50  \w    -97.00 -71.00   0.50    4.31    --  -86.00 -55.00 170.85   52
 51  \w   -158.00-109.00   0.50    4.31    --  -86.00 -55.00 170.85   98
 52  \w    -98.00 -72.00   0.50    4.31    --  -86.25 -55.00-132.42   52
 53  \w   -158.00-114.00   0.50    4.31    --  -86.25 -55.00-132.42   88
 54  \w   -134.00-108.00   0.50    4.31    --  -86.25 -54.00   0.70   52
 55  \w   -137.00 -75.00   0.50    4.31    --  -86.25 -55.00  65.61  124
 56  \w   -158.00 -72.00   0.50    4.31    --  -86.25 -55.00 -85.43  172
 57  \w   -108.00 -76.00   0.50    4.31    --  -86.25 -53.00-156.89   64
 58  \w   -110.00 -72.00   0.50    4.31    --  -86.25 -54.00 -48.23   76
 59  \w   -154.00 -72.00   0.50    4.31    --  -86.25 -55.00 -61.95  164
 60  \w   -159.00-115.00   0.50    4.31    --  -86.25 -54.00-105.08   88
 61  \w   -101.00 -72.00   0.50    4.31    --  -86.25 -53.00-175.41   58
 62  \w   -145.00-116.00   0.50    4.31    --  -86.25 -53.00-175.41   58
 63  \w   -145.00 -72.00   0.50    4.31    --  -86.25 -55.00  25.27  146
 64  \w   -102.00 -72.00   0.50    4.31    --  -86.25 -54.00   0.70   60
 65  \w   -107.00 -72.00   0.50    4.31    --  -86.25 -55.00 155.30   70
 66  \w   -152.00 -72.00   0.50    4.31    --  -86.25 -55.00 -15.42  160
 67  \w   -112.00 -72.00   0.50    4.31    --  -86.25 -55.00 113.21   80
 68  \w   -159.00-122.00   0.50    4.31    --  -86.25 -55.00 104.70   74
 69  \w   -118.00 -73.00   0.50    4.31    --  -86.25 -54.00-114.81   90
 70  \w   -153.00-128.00   0.50    4.31    --  -86.25 -55.00 113.21   50
 71  \w    -97.00 -72.00   0.50    4.31    --  -86.25 -54.00-105.08   50
 72  \w   -100.00 -72.00   0.50    4.31    --  -86.25 -54.00  75.62   56
 73  \w   -160.00-117.00   0.50    4.31    --  -86.25 -54.00  75.62   86
 74  \w   -101.00 -72.00   0.50    4.31    --  -86.25 -54.00 131.22   58
 75  \w   -152.00-119.00   0.50    4.31    --  -86.25 -54.00 131.22   66
 76  \w    -97.00 -72.00   0.50    4.31    --  -86.25 -54.00-146.60   50
 77  \w   -160.00-117.00   0.50    4.31    --  -86.25 -54.00-146.60   86
 78  \w   -105.00 -72.00   0.50    4.31    --  -86.25 -55.00 104.70   66
 79  \w   -159.00-128.00   0.50    4.31    --  -86.25 -56.00  46.81   62
 80  \w   -109.00 -80.00   0.50    4.31    --  -86.25 -56.00  46.81   58
 81  \w    -81.00 -47.00   0.50    4.31    --  -86.25 111.00  90.00   68
 82  \w     20.00  62.00   0.50    4.31    --   96.41 -94.00  30.00   84
 83  \w     90.00 118.00   0.50    4.31    --   96.41 -77.00 120.00   56
 84  \w     23.00  57.00   0.50    4.31    --   96.41 -77.00 120.00   68
 85  \w     82.00 107.00   0.50    4.31    --   96.41 -61.00-120.00   50
 86  \w     25.00  81.00   0.50    4.31    --   96.41 -61.00-120.00  112
 87  \w     23.00 101.00   0.50    4.31    --   96.41 -94.00-180.00  156
 88  \w     84.00 119.00   0.50    4.31    --   96.41 -77.00-120.00   70
 89  \w     44.00  70.00   0.50    4.31    --   96.41 -77.00-120.00   52
 90  \w     23.00 106.00   0.50    4.31    --   96.41 -94.00 120.00  166
 91  \w     37.00 109.00   0.50    4.31    --   96.41-111.00-120.00  144
 92  \w     80.00 109.00   0.50    4.31    --   96.41-111.00  90.00   58
 93  \w     28.00  73.00   0.50    4.31    --   96.41-111.00  90.00   90
 94  \w     26.00 118.00   0.50    4.31    --   96.41 -77.00  30.00  184
 95  \w     69.00  95.00   0.50    4.31    --   96.41 -94.00  30.00   52
 96  \w     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       '\w 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/[\s^2^(Fo^2^)+(0.0468P)^2^+9.8041P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              15397
_shelx_fab_checksum              62140
_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
;