Diimine Triscarbonyl Re(I) of Isomeric Pyridyl-fulvene Ligands: an Electrochemical, Spectroscopic, and Computational Investigation
Daniel Chartrand; Carlos A. Castro Ruiz; Garry S. Hanan; Inorganic Chemistry 51 (2012) 12738–12747; doi:10.1021/ic301559s

data_4331141
_publ_contact_author_address
;
    D\'epartement de Chimie
    Universit\'e de Montr\'eal
    C.P. 6128, Succ. Centre-ville
    Montr\'eal, Qu\'ebec
    Canada H3C 3J7
;
_publ_contact_author_email       garry.Hanan@umontreal.ca
_publ_contact_author_fax         '+1 514 343 2468'
_publ_contact_author_name        'Dr. Garry Hanan'
_publ_contact_author_phone       '+1 514 343 7056'
_publ_section_title
;
 Diimine Triscarbonyl Re(I) of Isomeric Pyridyl-fulvene Ligands: an
 Electrochemical, Spectroscopic, and Computational Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12738
_journal_page_last               12747
_journal_paper_doi               10.1021/ic301559s
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C32 H21 N3 O3 Re, F6 P, C H2 Cl2'
_chemical_formula_sum            'C33 H23 Cl2 F6 N3 O3 P Re'
_chemical_formula_weight         911.61
_chemical_name_systematic
; 
 4-Fluoren-9-ylidenemethyl-pyridine-2,2-bipyridinetricarbony-rhenium(I)
 hexafluorophosphate dichloromethane monosolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.429(1)
_cell_angle_beta                 90.852(2)
_cell_angle_gamma                102.281(2)
_cell_formula_units_Z            2
_cell_length_a                   8.1758(3)
_cell_length_b                   14.2872(5)
_cell_length_c                   14.8093(5)
_cell_measurement_reflns_used    23686
_cell_measurement_temperature    150
_cell_measurement_theta_max      68.53
_cell_measurement_theta_min      5.98
_cell_volume                     1689.99(10)
_computing_cell_refinement       'SAINT V7.60A(Bruker AXS, 2008)'
_computing_data_collection       'APEX2  (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.60A(Bruker AXS, 2008)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25055
_diffrn_reflns_theta_full        68.78
_diffrn_reflns_theta_max         68.78
_diffrn_reflns_theta_min         4.33
_exptl_absorpt_coefficient_mu    9.581
_exptl_absorpt_correction_T_max  0.6194
_exptl_absorpt_correction_T_min  0.3303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.579
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         6078
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+3.3741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0833
_reflns_number_gt                6061
_reflns_number_total             6078
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301559s_si_001_1.cif
_cod_data_source_block           2pFpyRe
_cod_database_code               4331141