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_7714872
_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         'C23 H43 N P2'
_chemical_formula_sum            'C23 H43 N P2'
_chemical_formula_weight         395.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-08-10
_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                90
_cell_angle_beta                 96.419(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9398(4)
_cell_length_b                   6.2656(2)
_cell_length_c                   25.0585(8)
_cell_measurement_reflns_used    7117
_cell_measurement_temperature    160.0(2)
_cell_measurement_theta_max      79.6590
_cell_measurement_theta_min      3.5450
_cell_volume                     2486.96(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.57a (Rigaku OD, 2022)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.972
_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   -118.00 -36.00   0.50    1.41    --  -50.63 -65.00  22.00  164
  2  \w    -58.00  21.00   0.50    1.41    --  -50.63  65.00 158.00  158
  3  \w    -10.00  17.00   0.50    1.41    --   50.63 -65.00  22.00   54
  4  \w     55.00  80.00   0.50    1.41    --   50.63  65.00 158.00   50
  5  \w   -158.00-128.00   0.50    5.62    --  -90.00 -65.00  22.00   60
  6  \w    -52.00 -20.00   0.50    5.62    --  -90.00  65.00 158.00   64
  7  \w     42.00  76.00   0.50    5.62    --  111.50 -65.00  22.00   68
  8  \w     98.00 178.00   0.50    5.62    --  111.50  65.00 158.00  160
  9  \w    -25.00  21.00   0.50    1.41    --  -50.63  19.00 -60.00   92
 10  \w    -21.00  26.00   0.50    1.41    --   50.63 -19.00  30.00   94
 11  \w    -51.00 -26.00   0.50    5.62    --  -90.00  45.00 -60.00   50
 12  \w   -161.00-136.00   0.50    5.62    --  -90.00 -95.00 150.00   50
 13  \w     41.00  68.00   0.50    5.62    --  111.50 -61.00 150.00   54
 14  \w    135.00 171.00   0.50    5.62    --  111.50  61.00  30.00   72
 15  \w    127.00 154.00   0.50    5.62    --  111.50  77.00-150.00   54
 16  \w    150.00 177.00   0.50    5.62    --  111.50  61.00-120.00   54
 17  \w     41.00  70.00   0.50    5.62    --  111.50 -61.00 -60.00   58
 18  \w    122.00 177.00   0.50    5.62    --  111.50  45.00  90.00  110
 19  \w     43.00  90.00   0.50    5.62    --  111.50 -95.00 150.00   94
 20  \w     42.00  97.00   0.50    5.62    --  111.50 -95.00  90.00  110
 21  \w     41.00  68.00   0.50    5.62    --  111.50 -61.00-150.00   54
 22  \w     43.00 100.00   0.50    5.62    --  111.50-125.00-120.00  114
 23  \w    123.00 163.00   0.50    5.62    --  111.50  45.00  60.00   80
 24  \w    129.00 178.00   0.50    5.62    --  111.50  61.00-180.00   98
 25  \w     50.00  77.00   0.50    5.62    --  111.50 -77.00-180.00   54
 26  \w     80.00 105.00   0.50    5.62    --  111.50 -77.00-180.00   50
 27  \w    104.00 178.00   0.50    5.62    --  111.50  30.00 -90.00  148
 28  \w     42.00  69.00   0.50    5.62    --  111.50 -61.00  90.00   54
 29  \w     42.00  71.00   0.50    5.62    --  111.50 -61.00 -90.00   58
 30  \w     64.00  89.00   0.50    5.62    --  111.50 -77.00  30.00   50
 31  \w    132.00 161.00   0.50    5.62    --  111.50  77.00   0.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0287963000
_diffrn_orient_matrix_UB_12      -0.0029028000
_diffrn_orient_matrix_UB_13      0.0607228000
_diffrn_orient_matrix_UB_21      -0.0615819000
_diffrn_orient_matrix_UB_22      0.1837035000
_diffrn_orient_matrix_UB_23      0.0083670000
_diffrn_orient_matrix_UB_31      -0.0696514000
_diffrn_orient_matrix_UB_32      -0.1633106000
_diffrn_orient_matrix_UB_33      0.0081247000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10581
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         81.330
_diffrn_reflns_theta_min         3.550
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.57a (Rigaku Oxford Diffraction, 2022)
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            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         2652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0563
_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/[\s^2^(Fo^2^)+(0.1017P)^2^+1.1149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1482
_refine_ls_wR_factor_ref         0.1508
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2452
_reflns_number_total             2652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03992g2.cif
_cod_data_source_block           mlb_ecca_pyrpnptbu_auto
_cod_depositor_comments
'Adding full bibliography for 7714872--7714877.cif.'
_cod_database_code               7714872
_shelx_shelxl_version_number     2018/3
_publcif_funding_html
;
;
_chemical_oxdiff_formula         'C23 H43 N1 P2'
_chemical_oxdiff_usercomment     'HyPix, Cu, 160 K'
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H4a,H4b)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
2.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C10(H10a,H10b,H10c),
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c)
;
_shelx_res_checksum              91773
_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 3.509
_oxdiff_exptl_absorpt_empirical_full_min 0.675