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_4331142
_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         'C19 H13 N'
_chemical_formula_sum            'C19 H13 N'
_chemical_formula_weight         255.30
_chemical_name_systematic
; 
   3-Fluoren-9-ylidenemethyl-pyridine
;
_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                90.475(3)
_cell_angle_beta                 96.308(3)
_cell_angle_gamma                105.025(3)
_cell_formula_units_Z            4
_cell_length_a                   6.2909(4)
_cell_length_b                   11.8465(7)
_cell_length_c                   18.5314(11)
_cell_measurement_reflns_used    4413
_cell_measurement_temperature    200
_cell_measurement_theta_max      71.52
_cell_measurement_theta_min      2.40
_cell_volume                     1324.79(14)
_computing_cell_refinement       'SAINT V7.34A (Bruker AXS, 2006b)'
_computing_data_collection       'APEX2 v2.1-0 (Bruker AXS, 2006a)'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006b)'
_computing_molecular_graphics    'SHELXTL v6.12 (Bruker AXS, 2001)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Bruker Smart 6000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Montel 200 optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17194
_diffrn_reflns_theta_full        72.48
_diffrn_reflns_theta_max         72.48
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        25.00
_diffrn_standards_interval_time  900
_diffrn_standards_number         113
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.8728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0075(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1227
_reflns_number_gt                3347
_reflns_number_total             5031
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic301559s_si_001_2.cif
_cod_data_source_block           mFpy
_cod_database_code               4331142