Peculiar Binding Modes of a Ligand with Two Adjacent β-Diiminato Binding Sites in Alkali and Alkaline-Earth Metal Chemistry
Dirk F.-J. Piesik; Peter Haack; Sjoerd Harder; Christian Limberg; Inorganic Chemistry 48 (2009) 11259–11264; doi:10.1021/ic9017536

data_4303745
_publ_section_title
;
Peculiar Binding Modes of a Ligand with Two Adjacent \b-Diiminato Binding
Sites in Alkali and Alkaline-Earth Metal Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11259
_journal_page_last               11264
_journal_paper_doi               10.1021/ic9017536
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C96 H135 Mg2 N6 O3 Si4'
_chemical_formula_weight         1582.08
_chemical_name_common            '[Xanthdim][MgN(SiMe3)2(THF)]2.(C6H6)2.5'
_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                90.00
_cell_angle_beta                 115.644(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.326(2)
_cell_length_b                   27.314(3)
_cell_length_c                   21.130(2)
_cell_measurement_temperature    173(2)
_cell_volume                     9535.0(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens Smart CCD'
_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  0.1097
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            158975
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.125
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_correction_T_min  0.9518
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            light-yellow
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3428
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         16333
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1145
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0915P)^2^+5.1521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1879
_reflns_number_gt                10387
_reflns_number_total             16333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9017536_si_002.cif
_cod_data_source_block           hasj168
_cod_original_cell_volume        9535.1(18)
_cod_database_code               4303745