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_7720820
_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         'C21H28BrReN4O32+ 2(F6P-) 0.5(H3C2N)'
_chemical_formula_sum            'C22 H29.5 Cl F12 N4.5 O3 P2 Re'
_chemical_formula_weight         916.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 96.113(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1497(10)
_cell_length_b                   13.5754(9)
_cell_length_c                   12.6756(8)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.76
_cell_measurement_theta_min      2.55
_cell_volume                     3105.4(3)
_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 7.69
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42554
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.321
_diffrn_reflns_theta_min         2.257
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.209
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.961
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1788
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Et2O/MeCN'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         4.880
_refine_diff_density_min         -2.659
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         14868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0306P)^2^+7.3261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10894
_reflns_number_total             14868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02433a2.cif
_cod_data_source_block           V18105
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C22 H29.50 Cl F12 N4.50 O3 P2 Re'
_cod_database_code               7720820
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.817
_shelx_res_checksum              33117
_shelx_hkl_checksum              80321