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_4329625
_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         'C22 H26 N4 O3 Re, B F4'
_chemical_formula_sum            'C22 H26 B F4 N4 O3 Re'
_chemical_formula_weight         667.48
_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
_audit_update_record
;
2012-03-22 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.502(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4576(10)
_cell_length_b                   13.4757(15)
_cell_length_c                   15.9875(15)
_cell_measurement_reflns_used    14272
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2447.3(4)
_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
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Nonius KappaCCD diffractometer (with an Oxford Cryosystems cryostream cooler)
;
_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  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27934
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.13
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    5.027
_exptl_absorpt_correction_T_max  0.6333
_exptl_absorpt_correction_T_min  0.2383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.227
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       0.00086(10)
_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   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         7180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0315P)^2^+2.4602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0726
_reflns_number_gt                5569
_reflns_number_total             7180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300625n_si_002_01.cif
_cod_data_source_block           Revised_pram13
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4329625