New Monodentate Amidine Superbasic Ligands with a Single Configuration in fac-[Re(CO)3(5,5'- or 6,6'-Me2bipyridine)(amidine)]BF4 Complexes
Pramuditha Abhayawardhana; Patricia A. Marzilli; Theshini Perera; Frank R. Fronczek; Luigi G. Marzilli; Inorganic Chemistry 51 (2012) 7271–7283; doi:10.1021/ic300625n

data_4329626
_publ_section_title
;
 New Monodentate Amidine Superbasic Ligands with a Single Configuration in
 fac-[Re(CO)3(5,5'- or 6,6'-Me2bipyridine)(amidine)]BF4 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7271
_journal_page_last               7283
_journal_paper_doi               10.1021/ic300625n
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C23 H28 N4 O3 Re, 0.95(B F4), Br0.05'
_chemical_formula_sum            'C23 H28 B0.95 Br0.05 F3.8 N4 O3 Re'
_chemical_formula_weight         681.16
_chemical_name_systematic
; 
 ? 
;
_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
_cell_angle_beta                 105.347(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3550(15)
_cell_length_b                   13.2081(14)
_cell_length_c                   14.7562(18)
_cell_measurement_reflns_used    6739
_cell_measurement_temperature    150.0(5)
_cell_measurement_theta_max      30.508
_cell_measurement_theta_min      2.546
_cell_volume                     2510.1(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare  et al., 1999)'
_diffrn_ambient_temperature      150.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       ' \w and \f scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38056
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.5
_diffrn_reflns_theta_min         2.8
_exptl_absorpt_coefficient_mu    4.981
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.802
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1335
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.083
_refine_diff_density_min         -1.854
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00146(12)
_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   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+3.5449P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                5702
_reflns_number_total             7045
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic300625n_si_002_02.cif
_cod_data_source_block           Pram17
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C23 H28 B0.95 Br0.05 F3.80 N4 O3 Re'
_cod_database_code               4329626