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_7714875
_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 Cl N3 O3 Tc'
_chemical_formula_sum            'C18 H11 Cl N3 O3 Tc'
_chemical_formula_weight         450.75
_chemical_name_common            '[Tc(CO)3Cl(terPy)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-11-13 deposited with the CCDC.	2023-12-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.168(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6643(3)
_cell_length_b                   7.04490(10)
_cell_length_c                   29.6513(6)
_cell_measurement_reflns_used    18664
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      29.6630
_cell_measurement_theta_min      2.4910
_cell_volume                     3402.81(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      159.99(10)
_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 0.892
_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    -21.00   5.00   0.50    1.54    --  -16.37  95.00-124.00   52
  2  \w     -9.00  17.00   0.50    1.54    --  -16.37 -95.00 124.00   52
  3  \w    -31.00  64.00   0.50    1.54    --   17.15 -95.00 124.00  190
  4  \w    -14.00  14.00   0.50    1.54    --  -16.37 -57.00 -30.00   56
  5  \w    -14.00  14.00   0.50    1.54    --  -16.37 -57.00 -60.00   56
  6  \w    -40.00  22.00   0.50    1.54    --   17.15 -38.00-150.00  124
  7  \w    -37.00   0.00   0.50    1.54    --   17.15 -38.00   0.00   74
  8  \w    -14.00  15.00   0.50    1.54    --   17.15  57.00 -60.00   58
  9  \w    -14.00  15.00   0.50    1.54    --   17.15  57.00  60.00   58
 10  \w     -7.00  18.00   0.50    1.54    --   17.15 -95.00 124.00   50
 11  \w    -32.00   7.00   0.50    1.54    --  -16.37 -38.00 -90.00   78
 12  \w    -15.00  10.00   0.50    1.54    --  -16.37 -57.00-180.00   50
 13  \w    -33.00  -3.00   0.50    1.54    --  -16.37  77.00   0.00   60
 14  \w    -42.00 -15.00   0.50    1.54    --  -16.37  77.00 -30.00   54
 15  \w     70.00 100.00   0.50    1.54    --   17.15 178.00-180.00   60
 16  \w     16.00  66.00   0.50    1.54    --   17.15 -99.00 -30.00  100
 17  \w      0.00  25.00   0.50    1.54    --   17.15 -77.00 120.00   50
 18  \w    -25.00  33.00   0.50    1.54    --   17.15  38.00-150.00  116
 19  \w    -14.00  11.00   0.50    1.54    --   17.15  57.00 120.00   50
 20  \w    -10.00  15.00   0.50    1.54    --   17.15  57.00  30.00   50
 21  \w    -14.00  11.00   0.50    1.54    --   17.15  57.00-180.00   50
;
_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      0.0112718000
_diffrn_orient_matrix_UB_12      -0.0936864000
_diffrn_orient_matrix_UB_13      0.0075257000
_diffrn_orient_matrix_UB_21      -0.0307708000
_diffrn_orient_matrix_UB_22      0.0000026000
_diffrn_orient_matrix_UB_23      0.0132826000
_diffrn_orient_matrix_UB_31      -0.0286983000
_diffrn_orient_matrix_UB_32      -0.0368516000
_diffrn_orient_matrix_UB_33      -0.0191155000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            24908
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.572
_diffrn_reflns_theta_min         2.501
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.224
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.74a (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            green
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       palte
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0202P)^2^+4.0550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4032
_reflns_number_total             4254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03992g2.cif
_cod_data_source_block           ra061222_mo_auto
_cod_depositor_comments
'Adding full bibliography for 7714872--7714877.cif.'
_cod_database_code               7714875
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C18 H11 N3 O3 Cl1 Tc1'
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.592
_exptl_absorpt_special_details   none
_diffrn_oxdiff_digest_frames
;
01abb5817a32f1b6ada6e4039b5f7b2395014884cdb
;
_diffrn_oxdiff_digest_hkl
;
01f13a22f407ccf34403ecf996d46b1a9cfe18
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1.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)
;
_shelx_res_checksum              84043
_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.907