Luminescent Low-Valent Rhenium Complexes with 1,2-Bis(dialkylphosphino)ethane Ligands. Synthesis and X-ray Crystallographic, Electrochemical, and Spectroscopic Characterization
Stephania J. Messersmith; Kristin Kirschbaum; Jon R. Kirchhoff; Inorganic Chemistry 49 (2010) 3857–3865; doi:10.1021/ic902549b

data_4315381
_publ_contact_author
;
Kirchhoff, Jon R.    
Department of Chemistry, 
University of Toledo, 
Toledo, OH 43606
;
_publ_contact_author_email       Jon.Kirchhoff@utoledo.edu
_publ_contact_author_fax         'US- 419-530 4033'
_publ_contact_author_phone       'US- 419-530 1515'
_publ_section_title
;
 Luminescent Low-Valent Rhenium Complexes with
 1,2-Bis(dialkylphosphino)ethane Ligands. Synthesis and X-ray
 Crystallographic, Electrochemical, and Spectroscopic Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3857
_journal_page_last               3865
_journal_paper_doi               10.1021/ic902549b
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H56 P6 Re, F6 P'
_chemical_formula_sum            'C22 H56 F6 P7 Re'
_chemical_formula_weight         837.66
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.194(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2719(10)
_cell_length_b                   21.078(2)
_cell_length_c                   15.7963(16)
_cell_measurement_reflns_used    7284
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      1.5
_cell_volume                     3366.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measurement_device_type  'CCD detector Smart 1K'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24587
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    3.989
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Sheldrick1996;Blessing,ActaC.1995,A51,33
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'parallel pipet'
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.878
_refine_diff_density_min         -1.108
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         9094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+5.1535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                7372
_reflns_number_total             9094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902549b_si_001_1.cif
_cod_data_source_block           '[Re(depe)(dmpe)2][PF6]'
_cod_database_code               4315381