Pendant-cation assisted spontaneous axial halide substitution in group 7 M(L)(CO)<sub>3</sub>X complexes.
Kramer, Wesley W.; Sheridan, Thomas R.; Pérez-Vázquez, Jorge; Boivin, Christophe A.; Browne, Amanda M.; Logan, Catherine G.; Sanders, Brian C.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 5197–5209; doi:10.1039/d5dt02433a

data_7720819
_publ_section_title
;
 Pendant-cation assisted spontaneous axial halide substitution in group 7
 M(L)(CO)<sub>3</sub>X complexes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5197
_journal_page_last               5209
_journal_paper_doi               10.1039/d5dt02433a
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C23H31N5O3Re2+ 3(F6P-) 0.5(H3C2N) 0.5(H10C2O)'
_chemical_formula_sum            'C28 H40.5 F18 N6.5 O3.5 P3 Re'
_chemical_formula_weight         1145.28
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2025-10-15 deposited with the CCDC.	2026-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                113.8926(17)
_cell_angle_beta                 96.814(2)
_cell_angle_gamma                111.3674(18)
_cell_formula_units_Z            2
_cell_length_a                   13.0356(6)
_cell_length_b                   13.2377(6)
_cell_length_c                   14.7412(7)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.05
_cell_measurement_theta_min      2.24
_cell_volume                     2057.32(18)
_computing_cell_refinement       'SAINT v8.38A (Bruker-AXS, 2013)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker-AXS, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker-AXS, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            60104
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.384
_diffrn_reflns_theta_min         2.243
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.193
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O/MeCN+ tetrabutylammonium hexafluorophosphate'
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.432
_refine_diff_density_min         -1.097
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         19968
_refine_ls_number_restraints     1498
_refine_ls_restrained_S_all      2.507
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+1.2926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15842
_reflns_number_total             19968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02433a2.cif
_cod_data_source_block           P17338
_cod_original_cell_volume        2057.32(17)
_cod_original_formula_sum        'C28 H40.50 F18 N6.50 O3.50 P3 Re'
_cod_database_code               7720819
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.401
_shelx_estimated_absorpt_t_max   0.741
_shelx_res_checksum              8588
_shelx_hkl_checksum              27576