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_7710909
_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         'C64 H58 N2 O4 P4 Re, I, 4.5(C6 H14)'
_chemical_formula_sum            'C91 H121 I N2 O4 P4 Re'
_chemical_formula_weight         1743.87
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   30.4077(5)
_cell_length_b                   30.4077(5)
_cell_length_c                   23.4090(4)
_cell_measurement_reflns_used    5465
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.2800
_cell_measurement_theta_min      2.7930
_cell_volume                     18744.8(5)
_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 0.988
_diffrn_measured_fraction_theta_max 0.794
_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  0.0210
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.794
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12109
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.794
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         2.610
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.957
_exptl_absorpt_correction_T_max  0.740
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) 
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            Orange-brown
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       blocks
_exptl_crystal_F_000             8109
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.343
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         8249
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0391P)^2^+20.5407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6695
_reflns_number_total             8249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02157a2.cif
_cod_data_source_block           Re-1
_cod_original_cell_volume        18744.8(8)
_cod_database_code               7710909
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              88451
_shelx_hkl_checksum              13572
_shelx_fab_checksum              48236