Synthesis and anti-microbial activity of a new series of bis(diphosphine) rhenium(v) dioxo complexes
Cooper, Saul M.; Siakalli, Christina; White, Andrew J. P.; Frei, Angelo; Miller, Philip W.; Long, Nicholas J.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02157A

data_7710911
_publ_section_title
;
 Synthesis and anti-microbial activity of a new series of bis(diphosphine)
 rhenium(v) dioxo complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02157A
_journal_year                    2022
_chemical_formula_moiety         'C54 H56 N2 O8 P6 Re, Cl, 2(C6 H14)'
_chemical_formula_sum            'C66 H84 Cl N2 O8 P6 Re'
_chemical_formula_weight         1440.82
_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_method           SHELXL-2018/3
_audit_update_record
;
2022-04-07 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                91.9605(16)
_cell_angle_beta                 101.2884(16)
_cell_angle_gamma                114.1629(19)
_cell_formula_units_Z            2
_cell_length_a                   12.9710(3)
_cell_length_b                   14.1823(3)
_cell_length_c                   18.7894(3)
_cell_measurement_reflns_used    13972
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.1460
_cell_measurement_theta_min      2.5000
_cell_volume                     3067.27(12)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.869
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41145
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.506
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.099
_refine_diff_density_max         1.029
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         13231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0250P)^2^+4.5192P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10719
_reflns_number_total             13231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02157a2.cif
_cod_data_source_block           Re-4
_cod_original_cell_volume        3067.26(11)
_cod_database_code               7710911
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              30606
_shelx_hkl_checksum              50568
_shelx_fab_checksum              71259