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_4303748
_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_moiety         'C77 H100 K2 N4 O5, C6 H14'
_chemical_formula_sum            'C83 H114 K2 N4 O5'
_chemical_formula_weight         1325.98
_chemical_name_common            '[Xanthdim][K(THF)2]'
_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                90.00
_cell_angle_beta                 106.6950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9189(2)
_cell_length_b                   27.2842(5)
_cell_length_c                   21.1070(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     7677.8(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2002)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Berndt, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Stoe IPDS-2t diffractometer'
_diffrn_measurement_method       '\w-rotation,\w-incr.=1\%,258 exposures'
_diffrn_radiation_collimation    '0.5 mm diameter monocapillary'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'long fine focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            79266
_diffrn_reflns_theta_full        26.82
_diffrn_reflns_theta_max         26.82
_diffrn_reflns_theta_min         2.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.782
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0016(3)
_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   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     888
_refine_ls_number_reflns         16196
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0762P)^2^+2.4678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                12067
_reflns_number_total             16196
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic9017536_si_005.cif
_cod_data_source_block           c:\ziemer\chris120
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4303748