Xanthene-Based Ligand with Two Adjacent β-Diiminato Binding Sites
Maurice Frederic Pilz; Christian Limberg; Burkhard Ziemer; Journal of Organic Chemistry 71 (2006) 4559–4564; doi:10.1021/jo060394y

data_4021741
_publ_section_title
;
 Xanthene-Based Ligand with Two Adjacent \b-Diiminato
 Binding Sites
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4559
_journal_page_last               4564
_journal_paper_doi               10.1021/jo060394y
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C69 H88 Li2 N4 O3, C4 H10 O'
_chemical_formula_sum            'C73 H98 Li2 N4 O4'
_chemical_formula_weight         1109.43
_chemical_name_systematic
; 
 Dilithium 2,7-Bis(1,1-dimethylethyl)9,9-dimethyl-4,5-bis(1-(2,3-dimethyl
phenylamido)-3-(2,3-dimethylphenylimino)iso-propenyl)-xanthene 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.470(2)
_cell_length_b                   28.695(4)
_cell_length_c                   27.500(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.5
_cell_volume                     13786(3)
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-oscill.,\f-incr.=1.0\%,247 exposures'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.064
_diffrn_reflns_av_sigmaI/netI    0.1279
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            111441
_diffrn_reflns_theta_full        24.15
_diffrn_reflns_theta_max         24.15
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9696
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             4816
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0010(2)
_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   0.870
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         10675
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.0907
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1370P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2299
_refine_ls_wR_factor_ref         0.2549
_reflns_number_gt                4318
_reflns_number_total             10675
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jo060394ysi20060301_035558.cif
_cod_database_code               4021741