Superbasic Amidine Monodentate Ligands in fac-[Re(CO)3(5,5'-Me2bipy)(Amidine)]BF4 Complexes: Dependence of Amidine Configuration on the Remote Nitrogen Substituents
Theshini Perera; Frank R. Fronczek; Patricia A. Marzilli; Luigi G. Marzilli; Inorganic Chemistry 49 (2010) 7035–7045; doi:10.1021/ic100714m

data_4316126
_publ_section_title
;
 Superbasic Amidine Monodentate Ligands in
 fac-[Re(CO)3(5,5'-Me2bipy)(Amidine)]BF4 Complexes: Dependence of Amidine
 Configuration on the Remote Nitrogen Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7035
_journal_page_last               7045
_journal_paper_doi               10.1021/ic100714m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'C21 H26 N4 O3 Re, 0.96(B F4), Br0.04, 0.33(C2 H3 N)'
_chemical_formula_sum
'C21.66 H27.99 B0.96 Br0.04 F3.83 N4.33 O3 Re'
_chemical_formula_weight         669.73
_chemical_name_systematic
;
 ?
;
_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                106.934(3)
_cell_angle_beta                 91.331(4)
_cell_angle_gamma                103.427(5)
_cell_formula_units_Z            4
_cell_length_a                   8.5566(5)
_cell_length_b                   17.5817(14)
_cell_length_c                   18.8096(3)
_cell_measurement_reflns_used    16691
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.5
_cell_volume                     2620.4(3)
_computing_cell_refinement
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'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      100.0(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'KappaCCD (with Oxford Cryostream)'
_diffrn_measurement_method       ' \w scans with \k offsets'
_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  0.032
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32739
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         32.0
_diffrn_reflns_theta_min         2.6
_exptl_absorpt_coefficient_mu    4.759
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_correction_T_min  0.360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
29 electrons were removed from from the void centered at 1/2, 1/2, 1/2,
corresponding to approximately 4/3 acetonitrile molecules per unit
cell, or 1/3 molecule of acetonitrile per formula unit. The solvent
contribution is included in the formula, density, etc., but coordinates
for the solvent are not included in the model.
;
_refine_diff_density_max         1.52
_refine_diff_density_min         -2.00
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.00046(8)
_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   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         18182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.054
_refine_ls_R_factor_gt           0.034
_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^)+(0.0341P)^2^+0.9602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.073
_refine_ls_wR_factor_ref         0.078
_reflns_number_gt                13724
_reflns_number_total             18182
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100714m_si_002_2.cif
_cod_data_source_block           Theshini51
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4316126